data_ras1602BSN _audit_creation_date "17-02-08" _audit_creation_method CRYSTALS_ver_14.40 _audit_update_record ; 2016-06-22 - Report on C40 H44 Cu2 N8 O6 by Anthony C. Willis for Rasoul Vafazadeh and Najmeh Abdollhi 2016-06-22 - passes checkcif tests with minor warnings 2017-02-08 - small change to suit reviewer 2017-02-08 - details of refinement in _refine_special_details below ; _oxford_structure_analysis_title 'Z:\ras1602BSN\Tony_ras1602BSN\To At 17:16 on' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.4016(4) _cell_length_b 15.5626(5) _cell_length_c 16.3803(7) _cell_angle_alpha 101.944(3) _cell_angle_beta 104.296(4) _cell_angle_gamma 102.394(3) _cell_volume 1949.09(15) _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cu -1.9646 0.5888 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C30 H30 Cl2 Cu2 N10 O6 # Dc = 1.41 Fooo = 892.00 Mu = 30.47 M = 824.63 # Found Formula = C40 H44 Cu2 N8 O6 # Dc = 1.47 FOOO = 892.00 Mu = 18.24 M = 859.93 _chemical_formula_sum 'C40 H44 Cu2 N8 O6' _chemical_formula_moiety 'C40 H44 Cu2 N8 O6' _chemical_compound_source ' Yazd University ' _chemical_formula_weight 859.93 _cell_measurement_reflns_used 8578 _cell_measurement_theta_min 3 _cell_measurement_theta_max 72 _cell_measurement_temperature 150 _exptl_crystal_description 'lath' _exptl_crystal_colour 'light brown' _exptl_crystal_size_min 0.013 _exptl_crystal_size_mid 0.074 _exptl_crystal_size_max 0.199 _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.824 # Sheldrick geometric approximatio 0.87 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 0.98 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2' _diffrn_radiation_source 'Supernova (Cu) X-ray Source' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'mirror' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) ; _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2015)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2015)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 21666 _reflns_number_total 7466 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0536 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 7466 # Theoretical number of reflections is about 15351 _diffrn_reflns_theta_min 3.567 _diffrn_reflns_theta_max 72.084 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 67.300 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -10 _reflns_limit_h_max 9 _reflns_limit_k_min -19 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.14 _oxford_diffrn_Wilson_scale 0.14 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.46 _refine_diff_density_max 0.53 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 7466 _refine_ls_number_restraints 25 _refine_ls_number_parameters 530 _oxford_refine_ls_R_factor_ref 0.0431 _refine_ls_wR_factor_ref 0.0894 _refine_ls_goodness_of_fit_ref 0.9865 _refine_ls_shift/su_max 0.0050467 _refine_ls_shift/su_mean 0.0000942 # The values computed with all filters except I/sigma _oxford_reflns_number_all 7466 _refine_ls_R_factor_all 0.0431 _refine_ls_wR_factor_all 0.0894 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6388 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0842 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.31P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 1. SUBMISSION DETAILS _publ_requested_journal ' test ' _publ_requested_category fm _publ_contact_author_name ' Anthony C. Willis ' _publ_contact_author_address ; Research School of Chemistry, Australian National University, Canberra, A. C. T. 2601, Australia ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61 2 6125 4109 ' _publ_contact_author_fax ' 61 2 6125 0750 ' _publ_contact_author_email ' Anthony.Willis@anu.edu.au ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal structure of [Cu(C~18~H~16~N~4~O~2~)(C~2~H~5~OH)]~2~ --- ras1602BSN ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address ' Najmeh Abdollahi ' ; Department of Chemistry, Yazd University, Yazd, Iran ; 'Rasoul Vafazadeh ' ; Department of Chemistry, Yazd University, Yazd, Iran ; ' Anthony C. Willis ' ; Research School of Chemistry, The Australian National University, Canberra, A. C. T. 2601, Australia ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Cu(C~18~H~16~N~4~O~2~)(C~2~H~5~OH)]~2~ is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [Cu(C~18~H~16~N~4~O~2~)(C~2~H~5~OH)]~2~ molecule. There is disorder in the packing of one of the ethanol species. ; _publ_section_acknowledgements # Acknowledgments ; ; _publ_section_figure_captions #Captions to figures ; Figure 1. Structure of the [Cu(C~18~H~16~N~4~O~2~)(C~2~H~5~OH)]~2~ dimer with labelling of selected atoms. Only the major sites of disordered atoms are shown (C39, C40 occupancy 0.572). Anisotropic displacement ellipsoids display 30% probability levels. Hydrogen atoms are drawn as circles with small radii. Figure 2. Structure of the [Cu(C~18~H~16~N~4~O~2~)(C~2~H~5~OH)]~2~ dimer with labelling of selected atoms. Both sites of each disordered atom are shown (C39, C40 occupancy 0.572; C139, C140 occupancy 0.428). Anisotropic displacement ellipsoids display 30% probability levels. Hydrogen atoms are drawn as circles with small radii. ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; ; _publ_section_exptl_prep ; The compound was prepared by NA and recrystallised from dichloromethane/ethanol. The sample identification was N32. The sample contained two types of crystal. The majority were dark brown blocks but they gave very poor diffraction images. The remainder were light brown needles. The crystal used here was one of the latter. ; _refine_special_details #Text of the paper ; There is disorder in the packing of one of the ethanol species. Two sites were used for each of the C atoms of this group. The relative occupancies were refined. Restraints were applied to distances and angles. The H atoms away from the disorder were located in a difference electron density map, but those bonded to C were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98\%A, O---H = 0.83\%A) and with U~iso~(H) in the range 1.2-1.5 times U~eq~ of the parent atom, after which the positions of the H atoms bonded to O were refined (but with a restraint on the O---H distance for O6), and those bonded to C were refined with riding constraints. H atoms within the disorder were included at calculated positions and ride on the atom sites to which they are respectively bonded. Most of the largest peaks in the final difference electron density map are located midway between bonded atoms. There is clearly no H on N1, N4 N5 or N8. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Spek, A.L. (2008). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cu1 Cu 0.42604(4) 0.28591(2) 0.281849(19) 0.0215 1.0000 Uani . . . . . . Cu2 Cu 0.02698(4) 0.24533(2) 0.24304(2) 0.0229 1.0000 Uani . . . . . . O1 O 0.5123(2) 0.17262(10) 0.26294(10) 0.0263 1.0000 Uani . . . . . . O2 O 0.05197(19) 0.34860(10) 0.19714(10) 0.0250 1.0000 Uani . . . . . . O3 O -0.04996(19) 0.28579(10) 0.35118(10) 0.0252 1.0000 Uani . . . . . . O4 O 0.38636(19) 0.30783(10) 0.16928(9) 0.0243 1.0000 Uani . . . . . . O5 O 0.7011(2) 0.37820(11) 0.32879(11) 0.0275 1.0000 Uani . . . . . . O6 O -0.2529(2) 0.18399(13) 0.16453(11) 0.0358 1.0000 Uani D . . . . . N1 N 0.4868(2) 0.17926(12) 0.40212(12) 0.0250 1.0000 Uani . . . . . . N2 N 0.4396(2) 0.25647(11) 0.39117(11) 0.0223 1.0000 Uani . . . . . . N3 N 0.3195(2) 0.37973(12) 0.33999(12) 0.0229 1.0000 Uani . . . . . . N4 N 0.2842(2) 0.45210(12) 0.30961(12) 0.0246 1.0000 Uani . . . . . . N5 N 0.0044(2) 0.15038(12) 0.37294(12) 0.0263 1.0000 Uani . . . . . . N6 N 0.0352(2) 0.14521(12) 0.29416(12) 0.0246 1.0000 Uani . . . . . . N7 N 0.1289(2) 0.16824(12) 0.16228(12) 0.0252 1.0000 Uani . . . . . . N8 N 0.1540(2) 0.18223(12) 0.08515(12) 0.0265 1.0000 Uani . . . . . . C1 C 0.5203(3) 0.14093(14) 0.33010(14) 0.0238 1.0000 Uani . . . . . . C2 C 0.3995(3) 0.30817(14) 0.45064(14) 0.0231 1.0000 Uani . . . . . . C3 C 0.3382(3) 0.38298(14) 0.42179(14) 0.0228 1.0000 Uani . . . . . . C4 C 0.1610(3) 0.42741(14) 0.23481(14) 0.0237 1.0000 Uani . . . . . . C5 C -0.0376(3) 0.22747(14) 0.39664(14) 0.0241 1.0000 Uani . . . . . . C6 C 0.0780(3) 0.07694(14) 0.25527(15) 0.0257 1.0000 Uani . . . . . . C7 C 0.1202(3) 0.08800(14) 0.17487(15) 0.0260 1.0000 Uani . . . . . . C8 C 0.2763(3) 0.25641(14) 0.09702(14) 0.0240 1.0000 Uani . . . . . . C9 C 0.5649(3) 0.05286(14) 0.32797(16) 0.0276 1.0000 Uani . . . . . . C10 C 0.5816(3) 0.00213(16) 0.25182(17) 0.0323 1.0000 Uani . . . . . . C11 C 0.6185(4) -0.08145(17) 0.24904(19) 0.0398 1.0000 Uani . . . . . . C12 C 0.6418(4) -0.11349(18) 0.3224(2) 0.0455 1.0000 Uani . . . . . . C13 C 0.6270(4) -0.06269(19) 0.3991(2) 0.0446 1.0000 Uani . . . . . . C14 C 0.5885(3) 0.02007(17) 0.40189(17) 0.0356 1.0000 Uani . . . . . . C15 C 0.4095(3) 0.29476(17) 0.53901(15) 0.0317 1.0000 Uani . . . . . . C16 C 0.2951(3) 0.45350(15) 0.48240(15) 0.0297 1.0000 Uani . . . . . . C17 C 0.1421(3) 0.50095(15) 0.19029(15) 0.0260 1.0000 Uani . . . . . . C18 C -0.0107(3) 0.49173(17) 0.12781(16) 0.0321 1.0000 Uani . . . . . . C19 C -0.0288(4) 0.55926(19) 0.08557(18) 0.0387 1.0000 Uani . . . . . . C20 C 0.1057(4) 0.63625(18) 0.10463(18) 0.0398 1.0000 Uani . . . . . . C21 C 0.2581(4) 0.64614(17) 0.16631(18) 0.0376 1.0000 Uani . . . . . . C22 C 0.2776(3) 0.57951(16) 0.20974(16) 0.0314 1.0000 Uani . . . . . . C23 C -0.0672(3) 0.24666(15) 0.48362(14) 0.0255 1.0000 Uani . . . . . . C24 C -0.1046(3) 0.32732(16) 0.51730(15) 0.0282 1.0000 Uani . . . . . . C25 C -0.1264(3) 0.34583(17) 0.59971(16) 0.0339 1.0000 Uani . . . . . . C26 C -0.1103(4) 0.2846(2) 0.64920(17) 0.0425 1.0000 Uani . . . . . . C27 C -0.0746(4) 0.2042(2) 0.61606(18) 0.0456 1.0000 Uani . . . . . . C28 C -0.0530(3) 0.18477(17) 0.53381(16) 0.0353 1.0000 Uani . . . . . . C29 C 0.0903(3) -0.00371(16) 0.28967(17) 0.0333 1.0000 Uani . . . . . . C30 C 0.1555(3) 0.01277(15) 0.11557(16) 0.0330 1.0000 Uani . . . . . . C31 C 0.2951(3) 0.28093(14) 0.01566(14) 0.0250 1.0000 Uani . . . . . . C32 C 0.4277(3) 0.35510(16) 0.02123(16) 0.0310 1.0000 Uani . . . . . . C33 C 0.4500(4) 0.37671(17) -0.05389(17) 0.0366 1.0000 Uani . . . . . . C34 C 0.3390(4) 0.32492(17) -0.13554(16) 0.0357 1.0000 Uani . . . . . . C35 C 0.2049(4) 0.25245(18) -0.14140(16) 0.0377 1.0000 Uani . . . . . . C36 C 0.1834(3) 0.23010(16) -0.06670(16) 0.0314 1.0000 Uani . . . . . . C37 C 0.7703(3) 0.42937(17) 0.27614(18) 0.0347 1.0000 Uani . . . . . . C38 C 0.6913(3) 0.50670(17) 0.26979(18) 0.0374 1.0000 Uani . . . . . . C39 C -0.3594(9) 0.1667(9) 0.0806(4) 0.0825 0.572(10) Uani D U P . . . C40 C -0.2813(7) 0.1762(5) 0.0143(3) 0.0622 0.572(10) Uani D U P . . . C139 C -0.3151(11) 0.2041(4) 0.0839(4) 0.0355 0.428(10) Uani D U P . . . C140 C -0.4196(18) 0.1192(7) 0.0130(6) 0.1053 0.428(10) Uani D U P . . . H1 H 0.759(4) 0.348(2) 0.338(2) 0.0421 1.0000 Uiso . . . . . . H2 H -0.312(4) 0.185(2) 0.197(2) 0.0541 1.0000 Uiso D . . . . . H101 H 0.5667 0.0234 0.2017 0.0388 1.0000 Uiso R . . . . . H111 H 0.6303 -0.1144 0.1983 0.0465 1.0000 Uiso R . . . . . H121 H 0.6658 -0.1695 0.3205 0.0540 1.0000 Uiso R . . . . . H131 H 0.6454 -0.0839 0.4491 0.0536 1.0000 Uiso R . . . . . H141 H 0.5778 0.0537 0.4528 0.0421 1.0000 Uiso R . . . . . H151 H 0.4575 0.2462 0.5469 0.0478 1.0000 Uiso R . . . . . H152 H 0.4816 0.3492 0.5829 0.0486 1.0000 Uiso R . . . . . H153 H 0.2994 0.2824 0.5461 0.0491 1.0000 Uiso R . . . . . H161 H 0.3641 0.4656 0.5413 0.0452 1.0000 Uiso R . . . . . H162 H 0.3109 0.5092 0.4654 0.0457 1.0000 Uiso R . . . . . H163 H 0.1787 0.4333 0.4811 0.0464 1.0000 Uiso R . . . . . H181 H -0.1002 0.4396 0.1135 0.0390 1.0000 Uiso R . . . . . H191 H -0.1320 0.5530 0.0445 0.0471 1.0000 Uiso R . . . . . H201 H 0.0942 0.6817 0.0750 0.0477 1.0000 Uiso R . . . . . H211 H 0.3486 0.6991 0.1801 0.0445 1.0000 Uiso R . . . . . H221 H 0.3805 0.5870 0.2514 0.0379 1.0000 Uiso R . . . . . H241 H -0.1146 0.3692 0.4846 0.0328 1.0000 Uiso R . . . . . H251 H -0.1511 0.3998 0.6220 0.0403 1.0000 Uiso R . . . . . H261 H -0.1236 0.2974 0.7048 0.0505 1.0000 Uiso R . . . . . H271 H -0.0647 0.1629 0.6498 0.0534 1.0000 Uiso R . . . . . H281 H -0.0295 0.1315 0.5116 0.0414 1.0000 Uiso R . . . . . H291 H 0.0418 -0.0048 0.3350 0.0515 1.0000 Uiso R . . . . . H292 H 0.2037 -0.0042 0.3115 0.0524 1.0000 Uiso R . . . . . H293 H 0.0342 -0.0587 0.2450 0.0520 1.0000 Uiso R . . . . . H301 H 0.2064 -0.0233 0.1488 0.0501 1.0000 Uiso R . . . . . H302 H 0.2282 0.0372 0.0847 0.0505 1.0000 Uiso R . . . . . H303 H 0.0523 -0.0262 0.0738 0.0504 1.0000 Uiso R . . . . . H321 H 0.5020 0.3909 0.0767 0.0365 1.0000 Uiso R . . . . . H331 H 0.5400 0.4267 -0.0486 0.0444 1.0000 Uiso R . . . . . H341 H 0.3524 0.3406 -0.1861 0.0438 1.0000 Uiso R . . . . . H351 H 0.1267 0.2193 -0.1955 0.0450 1.0000 Uiso R . . . . . H361 H 0.0960 0.1811 -0.0707 0.0376 1.0000 Uiso R . . . . . H371 H 0.8947 0.4530 0.3036 0.0430 1.0000 Uiso R . . . . . H372 H 0.7461 0.3874 0.2165 0.0435 1.0000 Uiso R . . . . . H381 H 0.7398 0.5402 0.2327 0.0576 1.0000 Uiso R . . . . . H382 H 0.7186 0.5496 0.3284 0.0584 1.0000 Uiso R . . . . . H383 H 0.5680 0.4841 0.2436 0.0583 1.0000 Uiso R . . . . . H391 H -0.4287 0.2074 0.0821 0.0991 0.572 Uiso R . . . . . H392 H -0.4296 0.1054 0.0641 0.0991 0.572 Uiso R . . . . . H401 H -0.3672 0.1625 -0.0403 0.0744 0.572 Uiso R . . . . . H402 H -0.2116 0.2373 0.0284 0.0744 0.572 Uiso R . . . . . H403 H -0.2125 0.1353 0.0104 0.0744 0.572 Uiso R . . . . . H1391 H -0.3841 0.2443 0.0913 0.0427 0.428 Uiso R . . . . . H1392 H -0.2208 0.2328 0.0676 0.0427 0.428 Uiso R . . . . . H1401 H -0.4596 0.1346 -0.0401 0.1269 0.428 Uiso R . . . . . H1402 H -0.5146 0.0902 0.0288 0.1269 0.428 Uiso R . . . . . H1403 H -0.3512 0.0787 0.0051 0.1269 0.428 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02065(16) 0.02183(15) 0.02361(15) 0.00637(11) 0.00827(12) 0.00753(11) Cu2 0.02077(16) 0.02247(15) 0.02867(16) 0.00900(12) 0.01025(13) 0.00729(12) O1 0.0256(8) 0.0245(7) 0.0306(8) 0.0073(6) 0.0103(6) 0.0090(6) O2 0.0236(8) 0.0239(7) 0.0294(7) 0.0094(6) 0.0089(6) 0.0078(6) O3 0.0232(8) 0.0273(7) 0.0286(7) 0.0101(6) 0.0102(6) 0.0089(6) O4 0.0218(7) 0.0265(7) 0.0233(7) 0.0066(6) 0.0061(6) 0.0049(6) O5 0.0211(8) 0.0287(8) 0.0356(8) 0.0126(6) 0.0094(7) 0.0086(6) O6 0.0225(8) 0.0515(10) 0.0311(9) 0.0109(8) 0.0078(7) 0.0066(7) N1 0.0250(9) 0.0219(8) 0.0289(9) 0.0076(7) 0.0071(7) 0.0088(7) N2 0.0200(9) 0.0213(8) 0.0254(8) 0.0065(7) 0.0065(7) 0.0060(7) N3 0.0205(9) 0.0217(8) 0.0281(9) 0.0067(7) 0.0087(7) 0.0076(7) N4 0.0262(9) 0.0203(8) 0.0305(9) 0.0077(7) 0.0115(8) 0.0089(7) N5 0.0243(9) 0.0271(9) 0.0301(9) 0.0095(7) 0.0109(8) 0.0078(7) N6 0.0210(9) 0.0255(8) 0.0283(9) 0.0087(7) 0.0092(7) 0.0052(7) N7 0.0216(9) 0.0242(8) 0.0306(9) 0.0076(7) 0.0105(7) 0.0053(7) N8 0.0260(9) 0.0256(9) 0.0282(9) 0.0063(7) 0.0112(8) 0.0054(7) C1 0.0179(10) 0.0217(9) 0.0300(11) 0.0059(8) 0.0056(8) 0.0048(8) C2 0.0180(10) 0.0232(10) 0.0262(10) 0.0050(8) 0.0069(8) 0.0037(8) C3 0.0158(9) 0.0224(9) 0.0279(10) 0.0048(8) 0.0059(8) 0.0036(7) C4 0.0231(10) 0.0253(10) 0.0298(10) 0.0091(8) 0.0145(9) 0.0123(8) C5 0.0168(10) 0.0260(10) 0.0286(10) 0.0087(8) 0.0067(8) 0.0033(8) C6 0.0187(10) 0.0236(10) 0.0346(11) 0.0081(8) 0.0088(9) 0.0047(8) C7 0.0180(10) 0.0240(10) 0.0331(11) 0.0049(8) 0.0064(9) 0.0045(8) C8 0.0215(10) 0.0236(10) 0.0287(10) 0.0056(8) 0.0087(9) 0.0104(8) C9 0.0219(11) 0.0222(10) 0.0377(12) 0.0066(9) 0.0078(9) 0.0071(8) C10 0.0301(12) 0.0291(11) 0.0383(12) 0.0079(9) 0.0101(10) 0.0114(9) C11 0.0411(15) 0.0292(12) 0.0480(15) 0.0018(10) 0.0138(12) 0.0157(10) C12 0.0506(17) 0.0271(12) 0.0651(18) 0.0145(12) 0.0187(14) 0.0206(11) C13 0.0553(17) 0.0353(13) 0.0527(16) 0.0210(12) 0.0180(14) 0.0216(12) C14 0.0406(14) 0.0300(11) 0.0409(13) 0.0120(10) 0.0147(11) 0.0145(10) C15 0.0335(13) 0.0377(12) 0.0269(11) 0.0098(9) 0.0098(10) 0.0140(10) C16 0.0285(12) 0.0275(10) 0.0324(11) 0.0034(9) 0.0121(9) 0.0076(9) C17 0.0280(11) 0.0274(10) 0.0302(11) 0.0103(8) 0.0153(9) 0.0134(9) C18 0.0312(12) 0.0365(12) 0.0359(12) 0.0146(10) 0.0151(10) 0.0140(10) C19 0.0389(14) 0.0503(15) 0.0412(13) 0.0247(12) 0.0164(11) 0.0252(12) C20 0.0516(16) 0.0415(13) 0.0505(15) 0.0289(12) 0.0312(13) 0.0284(12) C21 0.0431(15) 0.0315(12) 0.0515(15) 0.0191(11) 0.0276(12) 0.0150(11) C22 0.0322(12) 0.0300(11) 0.0381(12) 0.0126(9) 0.0165(10) 0.0112(9) C23 0.0166(10) 0.0310(11) 0.0277(10) 0.0079(8) 0.0067(8) 0.0044(8) C24 0.0226(11) 0.0319(11) 0.0315(11) 0.0104(9) 0.0087(9) 0.0082(9) C25 0.0315(13) 0.0375(12) 0.0332(12) 0.0061(10) 0.0110(10) 0.0126(10) C26 0.0549(17) 0.0498(15) 0.0294(12) 0.0121(11) 0.0183(12) 0.0206(13) C27 0.069(2) 0.0444(14) 0.0342(13) 0.0199(11) 0.0202(13) 0.0243(14) C28 0.0413(14) 0.0334(12) 0.0327(12) 0.0096(10) 0.0115(11) 0.0129(10) C29 0.0343(13) 0.0279(11) 0.0446(13) 0.0141(10) 0.0186(11) 0.0110(9) C30 0.0377(13) 0.0253(10) 0.0359(12) 0.0045(9) 0.0146(10) 0.0085(9) C31 0.0236(11) 0.0264(10) 0.0273(10) 0.0068(8) 0.0095(9) 0.0105(8) C32 0.0301(12) 0.0321(11) 0.0305(11) 0.0076(9) 0.0107(10) 0.0072(9) C33 0.0397(14) 0.0360(12) 0.0374(13) 0.0128(10) 0.0174(11) 0.0086(10) C34 0.0479(15) 0.0402(13) 0.0307(12) 0.0158(10) 0.0196(11) 0.0215(11) C35 0.0458(15) 0.0395(13) 0.0257(11) 0.0052(10) 0.0070(11) 0.0159(11) C36 0.0298(12) 0.0284(11) 0.0325(12) 0.0063(9) 0.0067(10) 0.0062(9) C37 0.0307(13) 0.0336(12) 0.0459(14) 0.0154(10) 0.0182(11) 0.0096(10) C38 0.0362(14) 0.0356(12) 0.0479(14) 0.0170(11) 0.0189(12) 0.0135(10) C39 0.046(4) 0.130(8) 0.041(4) 0.011(5) -0.001(3) -0.009(5) C40 0.042(3) 0.116(6) 0.032(3) 0.022(3) 0.014(2) 0.024(3) C139 0.032(4) 0.025(3) 0.032(3) 0.007(2) -0.011(3) -0.003(3) C140 0.132(10) 0.101(8) 0.043(5) -0.007(5) -0.003(6) 0.011(7) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 2.95(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 . O1 . 2.0402(15) yes Cu1 . O4 . 1.9061(15) yes Cu1 . O5 . 2.2883(16) yes Cu1 . N2 . 1.9212(18) yes Cu1 . N3 . 2.0605(18) yes Cu1 . N7 . 2.7494(18) yes Cu2 . O2 . 1.9042(15) yes Cu2 . O3 . 2.0569(15) yes Cu2 . O6 . 2.2649(17) yes Cu2 . N6 . 1.9213(18) yes Cu2 . N7 . 2.0657(19) yes O1 . C1 . 1.288(3) yes O2 . C4 . 1.284(3) yes O3 . C5 . 1.293(3) yes O4 . C8 . 1.283(3) yes O5 . C37 . 1.431(3) yes O5 . H1 . 0.76(3) no O6 . C39 . 1.378(6) yes O6 . C139 . 1.419(6) yes O6 . H2 . 0.81(2) no N1 . N2 . 1.375(2) yes N1 . C1 . 1.331(3) yes N2 . C2 . 1.290(3) yes N3 . N4 . 1.381(2) yes N3 . C3 . 1.299(3) yes N4 . C4 . 1.315(3) yes N5 . N6 . 1.367(3) yes N5 . C5 . 1.331(3) yes N6 . C6 . 1.289(3) yes N7 . N8 . 1.383(3) yes N7 . C7 . 1.297(3) yes N8 . C8 . 1.314(3) yes C1 . C9 . 1.492(3) yes C2 . C3 . 1.486(3) yes C2 . C15 . 1.490(3) yes C3 . C16 . 1.489(3) yes C4 . C17 . 1.494(3) yes C5 . C23 . 1.487(3) yes C6 . C7 . 1.479(3) yes C6 . C29 . 1.491(3) yes C7 . C30 . 1.491(3) yes C8 . C31 . 1.495(3) yes C9 . C10 . 1.388(3) yes C9 . C14 . 1.395(3) yes C10 . C11 . 1.395(3) yes C10 . H101 . 0.936 no C11 . C12 . 1.380(4) yes C11 . H111 . 0.922 no C12 . C13 . 1.388(4) yes C12 . H121 . 0.932 no C13 . C14 . 1.388(4) yes C13 . H131 . 0.936 no C14 . H141 . 0.924 no C15 . H151 . 0.947 no C15 . H152 . 0.957 no C15 . H153 . 0.944 no C16 . H161 . 0.951 no C16 . H162 . 0.957 no C16 . H163 . 0.954 no C17 . C18 . 1.388(3) yes C17 . C22 . 1.398(3) yes C18 . C19 . 1.387(3) yes C18 . H181 . 0.923 no C19 . C20 . 1.379(4) yes C19 . H191 . 0.928 no C20 . C21 . 1.377(4) yes C20 . H201 . 0.946 no C21 . C22 . 1.389(3) yes C21 . H211 . 0.937 no C22 . H221 . 0.927 no C23 . C24 . 1.395(3) yes C23 . C28 . 1.395(3) yes C24 . C25 . 1.387(3) yes C24 . H241 . 0.929 no C25 . C26 . 1.380(4) yes C25 . H251 . 0.931 no C26 . C27 . 1.383(4) yes C26 . H261 . 0.931 no C27 . C28 . 1.384(4) yes C27 . H271 . 0.933 no C28 . H281 . 0.917 no C29 . H291 . 0.932 no C29 . H292 . 0.934 no C29 . H293 . 0.943 no C30 . H301 . 0.954 no C30 . H302 . 0.952 no C30 . H303 . 0.947 no C31 . C32 . 1.391(3) yes C31 . C36 . 1.393(3) yes C32 . C33 . 1.386(3) yes C32 . H321 . 0.941 no C33 . C34 . 1.387(4) yes C33 . H331 . 0.934 no C34 . C35 . 1.381(4) yes C34 . H341 . 0.936 no C35 . C36 . 1.382(4) yes C35 . H351 . 0.928 no C36 . H361 . 0.917 no C37 . C38 . 1.503(3) yes C37 . H371 . 0.982 no C37 . H372 . 1.002 no C38 . H381 . 0.984 no C38 . H382 . 0.990 no C38 . H383 . 0.971 no C39 . C40 . 1.417(7) yes C39 . H391 . 0.950 no C39 . H392 . 0.950 no C40 . H401 . 0.950 no C40 . H402 . 0.950 no C40 . H403 . 0.950 no C139 . C140 . 1.493(8) yes C139 . H1391 . 0.950 no C139 . H1392 . 0.950 no C140 . H1401 . 0.950 no C140 . H1402 . 0.950 no C140 . H1403 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Cu1 . O4 . 101.84(6) yes O1 . Cu1 . O5 . 90.41(6) yes O4 . Cu1 . O5 . 92.04(6) yes O1 . Cu1 . N2 . 78.78(7) yes O4 . Cu1 . N2 . 173.64(7) yes O5 . Cu1 . N2 . 94.29(7) yes O1 . Cu1 . N3 . 157.39(7) yes O4 . Cu1 . N3 . 99.21(7) yes O5 . Cu1 . N3 . 97.02(6) yes N2 . Cu1 . N3 . 79.39(7) yes O1 . Cu1 . N7 . 82.88(6) yes O4 . Cu1 . N7 . 67.42(6) yes O5 . Cu1 . N7 . 156.33(6) yes N2 . Cu1 . N7 . 106.52(6) yes N3 . Cu1 . N7 . 97.80(6) yes O2 . Cu2 . O3 . 104.25(6) yes O2 . Cu2 . O6 . 93.96(7) yes O3 . Cu2 . O6 . 87.94(6) yes O2 . Cu2 . N6 . 172.20(7) yes O3 . Cu2 . N6 . 78.35(7) yes O6 . Cu2 . N6 . 93.49(7) yes O2 . Cu2 . N7 . 97.51(7) yes O3 . Cu2 . N7 . 156.91(7) yes O6 . Cu2 . N7 . 98.29(7) yes N6 . Cu2 . N7 . 79.09(8) yes Cu1 . O1 . C1 . 109.05(13) yes Cu2 . O2 . C4 . 126.42(14) yes Cu2 . O3 . C5 . 108.64(13) yes Cu1 . O4 . C8 . 127.48(14) yes Cu1 . O5 . C37 . 122.52(14) yes Cu1 . O5 . H1 . 107(2) no C37 . O5 . H1 . 105(3) no Cu2 . O6 . C39 . 139.8(3) yes Cu2 . O6 . C139 . 119.2(3) yes Cu2 . O6 . H2 . 110(3) no C39 . O6 . H2 . 107(3) no C139 . O6 . H2 . 117(3) no N2 . N1 . C1 . 108.21(18) yes N1 . N2 . Cu1 . 118.65(14) yes N1 . N2 . C2 . 122.35(18) yes Cu1 . N2 . C2 . 118.97(15) yes Cu1 . N3 . N4 . 125.04(14) yes Cu1 . N3 . C3 . 112.27(14) yes N4 . N3 . C3 . 119.41(18) yes N3 . N4 . C4 . 114.02(17) yes N6 . N5 . C5 . 108.32(18) yes N5 . N6 . Cu2 . 119.25(14) yes N5 . N6 . C6 . 121.73(19) yes Cu2 . N6 . C6 . 118.93(16) yes Cu2 . N7 . Cu1 . 80.32(6) yes Cu2 . N7 . N8 . 126.18(14) yes Cu1 . N7 . N8 . 100.33(12) yes Cu2 . N7 . C7 . 112.25(15) yes Cu1 . N7 . C7 . 106.83(14) yes N8 . N7 . C7 . 118.56(19) yes N7 . N8 . C8 . 113.53(18) yes N1 . C1 . O1 . 125.16(19) yes N1 . C1 . C9 . 115.9(2) yes O1 . C1 . C9 . 118.9(2) yes N2 . C2 . C3 . 113.08(19) yes N2 . C2 . C15 . 124.4(2) yes C3 . C2 . C15 . 122.49(19) yes C2 . C3 . N3 . 115.07(19) yes C2 . C3 . C16 . 121.57(19) yes N3 . C3 . C16 . 123.3(2) yes N4 . C4 . O2 . 127.7(2) yes N4 . C4 . C17 . 115.87(19) yes O2 . C4 . C17 . 116.39(19) yes N5 . C5 . O3 . 125.1(2) yes N5 . C5 . C23 . 115.64(19) yes O3 . C5 . C23 . 119.26(19) yes N6 . C6 . C7 . 113.39(19) yes N6 . C6 . C29 . 123.4(2) yes C7 . C6 . C29 . 123.2(2) yes C6 . C7 . N7 . 114.8(2) yes C6 . C7 . C30 . 121.7(2) yes N7 . C7 . C30 . 123.5(2) yes N8 . C8 . O4 . 128.0(2) yes N8 . C8 . C31 . 115.77(19) yes O4 . C8 . C31 . 116.09(19) yes C1 . C9 . C10 . 120.1(2) yes C1 . C9 . C14 . 120.6(2) yes C10 . C9 . C14 . 119.2(2) yes C9 . C10 . C11 . 120.2(2) yes C9 . C10 . H101 . 120.3 no C11 . C10 . H101 . 119.6 no C10 . C11 . C12 . 120.3(2) yes C10 . C11 . H111 . 119.5 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 119.8(2) yes C11 . C12 . H121 . 120.4 no C13 . C12 . H121 . 119.8 no C12 . C13 . C14 . 120.1(3) yes C12 . C13 . H131 . 119.7 no C14 . C13 . H131 . 120.2 no C9 . C14 . C13 . 120.4(2) yes C9 . C14 . H141 . 119.5 no C13 . C14 . H141 . 120.1 no C2 . C15 . H151 . 110.6 no C2 . C15 . H152 . 109.4 no H151 . C15 . H152 . 107.9 no C2 . C15 . H153 . 110.2 no H151 . C15 . H153 . 109.9 no H152 . C15 . H153 . 108.9 no C3 . C16 . H161 . 111.6 no C3 . C16 . H162 . 110.1 no H161 . C16 . H162 . 108.9 no C3 . C16 . H163 . 110.6 no H161 . C16 . H163 . 107.2 no H162 . C16 . H163 . 108.3 no C4 . C17 . C18 . 120.3(2) yes C4 . C17 . C22 . 120.9(2) yes C18 . C17 . C22 . 118.8(2) yes C17 . C18 . C19 . 120.7(2) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 119.8 no C18 . C19 . C20 . 120.3(2) yes C18 . C19 . H191 . 120.1 no C20 . C19 . H191 . 119.6 no C19 . C20 . C21 . 119.7(2) yes C19 . C20 . H201 . 120.3 no C21 . C20 . H201 . 120.0 no C20 . C21 . C22 . 120.7(2) yes C20 . C21 . H211 . 119.6 no C22 . C21 . H211 . 119.7 no C17 . C22 . C21 . 119.9(2) yes C17 . C22 . H221 . 120.0 no C21 . C22 . H221 . 120.1 no C5 . C23 . C24 . 120.9(2) yes C5 . C23 . C28 . 120.0(2) yes C24 . C23 . C28 . 119.1(2) yes C23 . C24 . C25 . 120.4(2) yes C23 . C24 . H241 . 120.1 no C25 . C24 . H241 . 119.5 no C24 . C25 . C26 . 120.1(2) yes C24 . C25 . H251 . 120.1 no C26 . C25 . H251 . 119.8 no C25 . C26 . C27 . 119.9(2) yes C25 . C26 . H261 . 120.0 no C27 . C26 . H261 . 120.1 no C26 . C27 . C28 . 120.6(2) yes C26 . C27 . H271 . 119.4 no C28 . C27 . H271 . 120.0 no C23 . C28 . C27 . 120.0(2) yes C23 . C28 . H281 . 119.2 no C27 . C28 . H281 . 120.8 no C6 . C29 . H291 . 112.0 no C6 . C29 . H292 . 111.9 no H291 . C29 . H292 . 107.1 no C6 . C29 . H293 . 110.8 no H291 . C29 . H293 . 108.0 no H292 . C29 . H293 . 106.8 no C7 . C30 . H301 . 109.8 no C7 . C30 . H302 . 110.3 no H301 . C30 . H302 . 110.6 no C7 . C30 . H303 . 110.4 no H301 . C30 . H303 . 107.7 no H302 . C30 . H303 . 107.9 no C8 . C31 . C32 . 120.0(2) yes C8 . C31 . C36 . 121.3(2) yes C32 . C31 . C36 . 118.7(2) yes C31 . C32 . C33 . 120.5(2) yes C31 . C32 . H321 . 119.3 no C33 . C32 . H321 . 120.1 no C32 . C33 . C34 . 120.2(2) yes C32 . C33 . H331 . 119.1 no C34 . C33 . H331 . 120.8 no C33 . C34 . C35 . 119.6(2) yes C33 . C34 . H341 . 120.1 no C35 . C34 . H341 . 120.3 no C34 . C35 . C36 . 120.4(2) yes C34 . C35 . H351 . 120.2 no C36 . C35 . H351 . 119.4 no C31 . C36 . C35 . 120.6(2) yes C31 . C36 . H361 . 119.0 no C35 . C36 . H361 . 120.4 no O5 . C37 . C38 . 109.9(2) yes O5 . C37 . H371 . 108.2 no C38 . C37 . H371 . 110.5 no O5 . C37 . H372 . 108.8 no C38 . C37 . H372 . 110.4 no H371 . C37 . H372 . 108.9 no C37 . C38 . H381 . 108.2 no C37 . C38 . H382 . 110.7 no H381 . C38 . H382 . 108.3 no C37 . C38 . H383 . 111.2 no H381 . C38 . H383 . 108.8 no H382 . C38 . H383 . 109.4 no O6 . C39 . C40 . 117.4(6) yes O6 . C39 . H391 . 107.5 no C40 . C39 . H391 . 107.5 no O6 . C39 . H392 . 107.5 no C40 . C39 . H392 . 107.5 no H391 . C39 . H392 . 109.5 no C39 . C40 . H401 . 109.5 no C39 . C40 . H402 . 109.4 no H401 . C40 . H402 . 109.5 no C39 . C40 . H403 . 109.5 no H401 . C40 . H403 . 109.5 no H402 . C40 . H403 . 109.5 no O6 . C139 . C140 . 111.3(6) yes O6 . C139 . H1391 . 109.0 no C140 . C139 . H1391 . 109.0 no O6 . C139 . H1392 . 109.1 no C140 . C139 . H1392 . 109.1 no H1391 . C139 . H1392 . 109.5 no C139 . C140 . H1401 . 109.5 no C139 . C140 . H1402 . 109.5 no H1401 . C140 . H1402 . 109.5 no C139 . C140 . H1403 . 109.4 no H1401 . C140 . H1403 . 109.5 no H1402 . C140 . H1403 . 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag O5 . H1 . O3 1_655 166(3) 0.76(3) 2.03(3) 2.776(2) yes O6 . H2 . O1 1_455 171(4) 0.81(2) 2.04(2) 2.839(2) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cu1 O1 C1 -170.29(15) . . . . no O5 Cu1 O1 C1 97.54(16) . . . . no N2 Cu1 O1 C1 3.25(15) . . . . no N3 Cu1 O1 C1 -12.0(3) . . . . no N7 Cu1 O1 C1 -105.22(16) . . . . no O1 Cu1 O4 C8 64.8(2) . . . . no O5 Cu1 O4 C8 155.6(2) . . . . no N3 Cu1 O4 C8 -106.9(2) . . . . no N7 Cu1 O4 C8 -12.28(19) . . . . no O1 Cu1 O5 C37 105.87(18) . . . . no O4 Cu1 O5 C37 4.01(18) . . . . no N2 Cu1 O5 C37 -175.35(18) . . . . no N3 Cu1 O5 C37 -95.53(18) . . . . no N7 Cu1 O5 C37 32.9(3) . . . . no O1 Cu1 N2 N1 -3.04(14) . . . . no O1 Cu1 N2 C2 178.93(19) . . . . no O5 Cu1 N2 N1 -92.59(15) . . . . no O5 Cu1 N2 C2 89.37(18) . . . . no N3 Cu1 N2 N1 171.05(16) . . . . no N3 Cu1 N2 C2 -6.98(17) . . . . no N7 Cu1 N2 N1 76.00(15) . . . . no N7 Cu1 N2 C2 -102.04(18) . . . . no O1 Cu1 N3 Cu2 -79.82(18) . . . . no O1 Cu1 N3 N4 -175.50(16) . . . . no O1 Cu1 N3 C3 25.3(3) . . . . no O4 Cu1 N3 Cu2 78.63(6) . . . . no O4 Cu1 N3 N4 -17.05(17) . . . . no O4 Cu1 N3 C3 -176.30(16) . . . . no O5 Cu1 N3 Cu2 171.86(5) . . . . no O5 Cu1 N3 N4 76.18(17) . . . . no O5 Cu1 N3 C3 -83.07(17) . . . . no N2 Cu1 N3 Cu2 -95.07(6) . . . . no N2 Cu1 N3 N4 169.26(17) . . . . no N2 Cu1 N3 C3 10.00(16) . . . . no N7 Cu1 N3 Cu2 10.37(6) . . . . no N7 Cu1 N3 N4 -85.30(16) . . . . no N7 Cu1 N3 C3 115.44(16) . . . . no O1 Cu1 N7 Cu2 143.44(7) . . . . no O1 Cu1 N7 N8 -91.27(12) . . . . no O1 Cu1 N7 C7 32.95(15) . . . . no O4 Cu1 N7 Cu2 -110.56(8) . . . . no O4 Cu1 N7 N8 14.73(12) . . . . no O4 Cu1 N7 C7 138.95(17) . . . . no O5 Cu1 N7 Cu2 -142.03(13) . . . . no O5 Cu1 N7 N8 -16.7(2) . . . . no O5 Cu1 N7 C7 107.5(2) . . . . no N2 Cu1 N7 Cu2 67.41(8) . . . . no N2 Cu1 N7 N8 -167.30(12) . . . . no N2 Cu1 N7 C7 -43.09(16) . . . . no N3 Cu1 N7 Cu2 -13.77(7) . . . . no N3 Cu1 N7 N8 111.52(13) . . . . no N3 Cu1 N7 C7 -124.27(16) . . . . no O3 Cu2 O2 C4 64.9(2) . . . . no O6 Cu2 O2 C4 153.80(19) . . . . no N3 Cu2 O2 C4 -11.19(18) . . . . no N7 Cu2 O2 C4 -107.3(2) . . . . no O2 Cu2 O3 C5 -167.42(15) . . . . no O6 Cu2 O3 C5 99.02(15) . . . . no N3 Cu2 O3 C5 -101.96(15) . . . . no N6 Cu2 O3 C5 5.03(15) . . . . no N7 Cu2 O3 C5 -7.4(3) . . . . no O2 Cu2 O6 C39 45.1(8) . . . . no O3 Cu2 O6 C39 149.2(8) . . . . no N3 Cu2 O6 C39 83.3(8) . . . . no N6 Cu2 O6 C39 -132.6(8) . . . . no N7 Cu2 O6 C39 -53.1(8) . . . . no O2 Cu2 N3 Cu1 -108.68(8) . . . . no O2 Cu2 N3 N4 15.54(12) . . . . no O2 Cu2 N3 C3 140.68(17) . . . . no O3 Cu2 N3 Cu1 142.83(7) . . . . no O3 Cu2 N3 N4 -92.94(12) . . . . no O3 Cu2 N3 C3 32.19(15) . . . . no O6 Cu2 N3 Cu1 -150.29(13) . . . . no O6 Cu2 N3 N4 -26.1(2) . . . . no O6 Cu2 N3 C3 99.1(2) . . . . no N6 Cu2 N3 Cu1 66.98(8) . . . . no N6 Cu2 N3 N4 -168.79(12) . . . . no N6 Cu2 N3 C3 -43.66(16) . . . . no N7 Cu2 N3 Cu1 -13.89(7) . . . . no N7 Cu2 N3 N4 110.34(12) . . . . no N7 Cu2 N3 C3 -124.53(16) . . . . no O3 Cu2 N6 N5 -5.05(15) . . . . no O3 Cu2 N6 C6 178.36(19) . . . . no O6 Cu2 N6 N5 -92.22(15) . . . . no O6 Cu2 N6 C6 91.19(18) . . . . no N3 Cu2 N6 N5 74.12(16) . . . . no N3 Cu2 N6 C6 -102.47(18) . . . . no N7 Cu2 N6 N5 170.01(16) . . . . no N7 Cu2 N6 C6 -6.58(18) . . . . no O2 Cu2 N7 Cu1 79.51(6) . . . . no O2 Cu2 N7 N8 -16.25(17) . . . . no O2 Cu2 N7 C7 -176.18(16) . . . . no O3 Cu2 N7 Cu1 -80.93(18) . . . . no O3 Cu2 N7 N8 -176.69(15) . . . . no O3 Cu2 N7 C7 23.4(3) . . . . no O6 Cu2 N7 Cu1 174.65(6) . . . . no O6 Cu2 N7 N8 78.89(17) . . . . no O6 Cu2 N7 C7 -81.04(17) . . . . no N3 Cu2 N7 Cu1 10.39(6) . . . . no N3 Cu2 N7 N8 -85.38(17) . . . . no N3 Cu2 N7 C7 114.70(16) . . . . no N6 Cu2 N7 Cu1 -93.37(7) . . . . no N6 Cu2 N7 N8 170.87(18) . . . . no N6 Cu2 N7 C7 10.94(16) . . . . no Cu1 O1 C1 N1 -3.5(3) . . . . no Cu1 O1 C1 C9 174.44(18) . . . . no Cu2 O2 C4 N4 4.6(4) . . . . no Cu2 O2 C4 C17 -172.96(16) . . . . no Cu2 O3 C5 N5 -5.1(3) . . . . no Cu2 O3 C5 C23 173.21(18) . . . . no Cu1 O4 C8 N8 8.0(4) . . . . no Cu1 O4 C8 C31 -168.46(16) . . . . no Cu1 O5 C37 C38 71.2(2) . . . . no Cu2 O6 C39 C40 11.7(16) . . . . no C1 N1 N2 Cu1 2.1(2) . . . . no C1 N1 N2 C2 -179.9(2) . . . . no N2 N1 C1 O1 1.2(3) . . . . no N2 N1 C1 C9 -176.81(19) . . . . no Cu1 N2 C2 C3 3.0(3) . . . . no Cu1 N2 C2 C15 -178.04(19) . . . . no N1 N2 C2 C3 -174.97(19) . . . . no N1 N2 C2 C15 4.0(4) . . . . no Cu1 N3 N4 C4 67.8(2) . . . . no Cu2 N3 N4 C4 -18.0(2) . . . . no C3 N3 N4 C4 -134.3(2) . . . . no Cu1 N3 C3 C2 -11.3(3) . . . . no Cu1 N3 C3 C16 171.23(19) . . . . no Cu2 N3 C3 C2 75.9(2) . . . . no Cu2 N3 C3 C16 -101.6(2) . . . . no N4 N3 C3 C2 -171.85(19) . . . . no N4 N3 C3 C16 10.7(3) . . . . no N3 N4 C4 O2 14.5(3) . . . . no N3 N4 C4 C17 -167.98(19) . . . . no C5 N5 N6 Cu2 3.8(2) . . . . no C5 N5 N6 C6 -179.7(2) . . . . no N6 N5 C5 O3 1.3(3) . . . . no N6 N5 C5 C23 -177.06(19) . . . . no Cu2 N6 C6 C7 1.5(3) . . . . no Cu2 N6 C6 C29 179.31(18) . . . . no N5 N6 C6 C7 -174.99(19) . . . . no N5 N6 C6 C29 2.8(4) . . . . no Cu1 N7 N8 C8 -15.6(2) . . . . no Cu2 N7 N8 C8 69.9(2) . . . . no C7 N7 N8 C8 -131.3(2) . . . . no Cu1 N7 C7 C6 73.0(2) . . . . no Cu1 N7 C7 C30 -104.9(2) . . . . no Cu2 N7 C7 C6 -13.2(3) . . . . no Cu2 N7 C7 C30 168.86(19) . . . . no N8 N7 C7 C6 -174.84(19) . . . . no N8 N7 C7 C30 7.2(3) . . . . no N7 N8 C8 O4 10.6(4) . . . . no N7 N8 C8 C31 -173.00(19) . . . . no O1 C1 C9 C10 -5.9(4) . . . . no O1 C1 C9 C14 174.8(2) . . . . no N1 C1 C9 C10 172.2(2) . . . . no N1 C1 C9 C14 -7.1(4) . . . . no N2 C2 C3 N3 6.1(3) . . . . no N2 C2 C3 C16 -176.4(2) . . . . no C15 C2 C3 N3 -172.9(2) . . . . no C15 C2 C3 C16 4.6(4) . . . . no O2 C4 C17 C18 18.0(3) . . . . no O2 C4 C17 C22 -161.2(2) . . . . no N4 C4 C17 C18 -159.8(2) . . . . no N4 C4 C17 C22 21.0(3) . . . . no O3 C5 C23 C24 -1.3(4) . . . . no O3 C5 C23 C28 -179.5(2) . . . . no N5 C5 C23 C24 177.2(2) . . . . no N5 C5 C23 C28 -1.0(3) . . . . no N6 C6 C7 N7 8.4(3) . . . . no N6 C6 C7 C30 -173.7(2) . . . . no C29 C6 C7 N7 -169.4(2) . . . . no C29 C6 C7 C30 8.5(4) . . . . no O4 C8 C31 C32 0.8(3) . . . . no O4 C8 C31 C36 179.9(2) . . . . no N8 C8 C31 C32 -176.1(2) . . . . no N8 C8 C31 C36 3.1(4) . . . . no C1 C9 C10 C11 -178.2(3) . . . . no C14 C9 C10 C11 1.2(4) . . . . no C1 C9 C14 C13 178.9(3) . . . . no C10 C9 C14 C13 -0.5(4) . . . . no C9 C10 C11 C12 -1.2(5) . . . . no C10 C11 C12 C13 0.6(5) . . . . no C11 C12 C13 C14 0.1(5) . . . . no C12 C13 C14 C9 -0.2(5) . . . . no C4 C17 C18 C19 -179.4(2) . . . . no C22 C17 C18 C19 -0.1(4) . . . . no C4 C17 C22 C21 178.8(2) . . . . no C18 C17 C22 C21 -0.5(4) . . . . no C17 C18 C19 C20 0.6(4) . . . . no C18 C19 C20 C21 -0.4(5) . . . . no C19 C20 C21 C22 -0.2(5) . . . . no C20 C21 C22 C17 0.7(4) . . . . no C5 C23 C24 C25 -177.9(2) . . . . no C28 C23 C24 C25 0.3(4) . . . . no C5 C23 C28 C27 177.7(3) . . . . no C24 C23 C28 C27 -0.5(4) . . . . no C23 C24 C25 C26 0.3(4) . . . . no C24 C25 C26 C27 -0.8(5) . . . . no C25 C26 C27 C28 0.7(5) . . . . no C26 C27 C28 C23 0.0(5) . . . . no C8 C31 C32 C33 177.8(3) . . . . no C36 C31 C32 C33 -1.3(4) . . . . no C8 C31 C36 C35 -178.5(3) . . . . no C32 C31 C36 C35 0.6(4) . . . . no C31 C32 C33 C34 0.6(4) . . . . no C32 C33 C34 C35 0.8(5) . . . . no C33 C34 C35 C36 -1.5(5) . . . . no C34 C35 C36 C31 0.8(4) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu1 O2 3.5323(17) . . no Cu1 N1 2.8490(19) . . no Cu1 N6 3.6113(19) . . no Cu1 N7 2.7496(19) . . no Cu1 N8 3.2919(19) . . no Cu2 C37 3.967(3) . 1_455 no Cu2 N3 2.7254(19) . . no Cu2 O4 3.5426(17) . . no Cu2 N2 3.6536(18) . . no Cu2 N4 3.2577(19) . . no Cu2 N5 2.8509(19) . . no O1 O4 3.065(2) . . no O1 O5 3.076(2) . . no O1 O6 2.839(2) . 1_655 no O1 N1 2.325(2) . . no O1 N2 2.516(2) . . no O1 N7 3.215(2) . . no O1 C7 3.110(3) . . no O1 C39 3.407(7) . 1_655 no O2 N3 2.689(2) . . no O2 C139 3.237(8) . . no O2 N7 2.987(2) . . no O2 O3 3.128(2) . . no O2 O4 3.128(2) . . no O2 O6 3.058(3) . . no O2 N8 3.251(2) . . no O2 N4 2.333(2) . . no O2 C37 3.312(3) . 1_455 no O2 C8 3.164(3) . . no O3 N3 3.202(2) . . no O3 N6 2.515(2) . . no O3 O6 3.004(2) . . no O3 C3 3.091(3) . . no O3 N5 2.328(2) . . no O3 O5 2.776(2) . 1_455 no O3 C37 3.233(3) . 1_455 no O3 C16 3.345(3) . . no O4 N3 3.023(2) . . no O4 O5 3.030(2) . . no O4 C4 3.145(3) . . no O4 N7 2.677(2) . . no O4 N8 2.334(2) . . no O4 C37 3.205(3) . . no O4 C38 3.355(3) . . no O5 N2 3.096(2) . . no O5 N3 3.261(3) . . no O6 N6 3.058(3) . . no N1 O1 2.325(2) . . no N2 C1 2.193(3) . . no N2 C3 2.319(3) . . no N2 N3 2.546(3) . . no N2 N6 3.277(3) . . no N3 C2 2.352(3) . . no N3 C4 2.261(3) . . no N5 C2 3.434(3) . . no N6 N7 2.541(3) . . no N6 C5 2.187(3) . . no N6 C7 2.316(3) . . no N7 C8 2.256(3) . . no N7 C6 2.341(3) . . no C1 C5 3.470(4) . 1_655 no C1 C6 3.458(4) . . no C1 C7 3.488(3) . . no C1 C23 3.547(3) . 1_655 no C2 C5 3.435(4) . . no C3 C5 3.415(3) . . no C3 C16 3.320(3) . 2_666 no C4 C8 3.580(3) . . no C4 C37 3.517(4) . 1_455 no C5 C9 3.576(3) . 1_455 no C14 C28 3.390(4) . 1_655 no C16 C16 3.289(4) . 2_666 no C18 C37 3.556(4) . 1_455 no C18 C19 3.535(4) . 2_565 no C19 C19 3.226(4) . 2_565 no C20 C36 3.545(4) . 2_565 no C20 C35 3.530(5) . 2_565 no C21 C33 3.445(5) . 2_665 no C21 C26 3.594(4) . 2_566 no C21 C34 3.493(5) . 2_665 no C22 C26 3.556(4) . 2_566 no _iucr_refine_instruction_details_constraints ; # # Punched on 08/02/17 at 11:42:12 # #LIST 12 BLOCK SCALE X'S, U'S CONT C(39,OCC) C(40,OCC) C(139,OCC) C(140,OCC) CONT H(1,X'S) H(2,X'S) EQUIV C(39,OCC) C(40,OCC) C(139,OCC) C(140,OCC) WEIGHT -1 C(139,OCC) C(140,OCC) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) H ( 372,X'S) RIDE C ( 38,X'S) H ( 381,X'S) H ( 382,X'S) H ( 383,X'S) RIDE C(39,X'S) H(391,X'S) H(392,X'S) RIDE C(40,X'S) H(401,X'S) H(402,X'S) H(403,X'S) RIDE C(139,X'S) H(1391,X'S) H(1392,X'S) RIDE C(140,X'S) H(1401,X'S) H(1402,X'S) H(1403,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 08/02/17 at 11:42:12 # #LIST 16 DIST 1.43, .01 = O(6) TO C(39), O(6) TO C(139) DIST 1.50, .01 = C(39) TO C(40), C(139) TO C(140) ANGLE 110, 2 = O(6) TO C(39) TO C(40), O(6) TO C(139) TO C(140) U(IJ) 0.0, .01 = C(39) TO C(139) U(IJ) 0.0, .02 = C(139) TO C(140) U(IJ) 0.0, .03 = C(40) TO C(140) REM DIST 0.83 , .02 = O(6) TO H(2) NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END