data_ras1505SN _audit_creation_date "15-05-11" _audit_creation_method CRYSTALS_ver_14.40 _audit_update_record ; 2015-05-19 - Report on (C9 H18 Cu N2 O4)2 by Anthony C. Willis for Rasoul Vafazadeh and Mahshad Chvoshiyan 2015-02-02 - passes checkcif tests with minor warnings ; _oxford_structure_analysis_title 'Z:\ras1505SN\Tony_ras1505SN_data At 15: 6 on' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 6.8283(6) _cell_length_b 9.3019(5) _cell_length_c 10.6562(8) _cell_angle_alpha 70.211(6) _cell_angle_beta 80.563(7) _cell_angle_gamma 76.054(6) _cell_volume 615.58(8) _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' 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 1 # Given Formula = C9 H19 Cu1 N2 O4 # Dc = 1.53 Fooo = 294.00 Mu = 25.52 M = 282.81 # Found Formula = C9 H18 Cu1 N2 O4 # Dc = 1.52 FOOO = 294.00 Mu = 25.51 M = 281.80 _chemical_formula_sum 'C18 H36 Cu2 N4 O8' _chemical_formula_moiety 'C18 H36 Cu2 N4 O8' _chemical_compound_source ' Yazd University ' _chemical_formula_weight 563.60 # 281.80 _cell_measurement_reflns_used 7652 _cell_measurement_theta_min 5 _cell_measurement_theta_max 72 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'blue' _exptl_crystal_size_min 0.061 _exptl_crystal_size_mid 0.131 _exptl_crystal_size_max 0.355 _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 294 _exptl_absorpt_coefficient_mu 2.551 # Sheldrick geometric approximatio 0.72 0.86 _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 0.61 _exptl_absorpt_correction_T_max 0.86 _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 9439 _reflns_number_total 2424 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 2424 # Theoretical number of reflections is about 4858 _diffrn_reflns_theta_min 5.157 _diffrn_reflns_theta_max 72.195 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 72.195 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min -10 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 1.78 _oxford_diffrn_Wilson_scale 0.01 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.30 _refine_diff_density_max 0.30 # 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 2424 _refine_ls_number_restraints 0 _refine_ls_number_parameters 199 _oxford_refine_ls_R_factor_ref 0.0240 _refine_ls_wR_factor_ref 0.0613 _refine_ls_goodness_of_fit_ref 1.0107 _refine_ls_shift/su_max 0.0024331 _refine_ls_shift/su_mean 0.0001773 # The values computed with all filters except I/sigma _oxford_reflns_number_all 2424 _refine_ls_R_factor_all 0.0240 _refine_ls_wR_factor_all 0.0613 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2360 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_gt 0.0610 # 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 refxyz #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^) + ( 0.03P)^2^ + 0.52P] ,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~3~H~10~N~2~)(C~2~H~3~O~2~)(C~4~H~5~O~2~)]~2~ --- ras1505SN ; # 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 ' Mahshad Chvoshiyan ' ; 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~3~H~10~N~2~)(C~2~H~3~O~2~)(C~4~H~5~O~2~)]~2~ is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of a [Cu(C~3~H~10~N~2~)(C~2~H~3~O~2~)(C~4~H~5~O~2~)]~2~ molecule centred around a crystallographic inversion symmetry operation. ; _publ_section_acknowledgements # Acknowledgments ; ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; ; _publ_section_exptl_prep ; The compound was prepared by MC and was recrystallised from dichloromethane/n-hexane/toluene (5/1/1 V:V). The sample identification was Cpn1. ; _refine_special_details #Text of the paper ; The H atoms were all located in a difference electron density map, but 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) and with U~iso~(H) in the range 1.2-1.5 times U~eq~ of the parent atom, after which the positions were refined without restraints. The largest peaks in the final difference electron density map are located midway between bonded atoms. ; # 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 0.53117(3) 0.31431(2) 0.51495(2) 0.0179 1.0000 Uani . . . . . . O1 O 0.67616(16) 0.49433(12) 0.55227(11) 0.0195 1.0000 Uani . . . . . . O2 O 0.92934(18) 0.34703(14) 0.67218(13) 0.0274 1.0000 Uani . . . . . . O3 O 0.64084(17) 0.35200(14) 0.32641(11) 0.0252 1.0000 Uani . . . . . . O4 O 0.7902(2) 0.11144(16) 0.32134(13) 0.0360 1.0000 Uani . . . . . . N1 N 0.3659(2) 0.28996(16) 0.69261(14) 0.0206 1.0000 Uani . . . . . . N2 N 0.7476(2) 0.13197(17) 0.58675(15) 0.0234 1.0000 Uani . . . . . . C1 C 0.3706(3) 0.1369(2) 0.79647(18) 0.0281 1.0000 Uani . . . . . . C2 C 0.5842(3) 0.0440(2) 0.81788(19) 0.0347 1.0000 Uani . . . . . . C3 C 0.6935(3) -0.0033(2) 0.69734(19) 0.0299 1.0000 Uani . . . . . . C4 C 0.8209(2) 0.47552(19) 0.62343(15) 0.0195 1.0000 Uani . . . . . . C5 C 0.8546(3) 0.6190(2) 0.6462(2) 0.0283 1.0000 Uani . . . . . . C6 C 0.7365(2) 0.2531(2) 0.26668(17) 0.0238 1.0000 Uani . . . . . . C7 C 0.7828(3) 0.3236(2) 0.11711(18) 0.0304 1.0000 Uani . . . . . . C8 C 0.8636(3) 0.2303(3) 0.0434(2) 0.0399 1.0000 Uani . . . . . . C9 C 0.7346(4) 0.4984(3) 0.0596(2) 0.0417 1.0000 Uani . . . . . . H1 H 0.402(3) 0.353(3) 0.716(2) 0.0313 1.0000 Uiso . . . . . . H2 H 0.245(4) 0.328(3) 0.675(2) 0.0303 1.0000 Uiso . . . . . . H3 H 0.836(4) 0.168(3) 0.609(2) 0.0347 1.0000 Uiso . . . . . . H4 H 0.802(4) 0.105(3) 0.521(2) 0.0351 1.0000 Uiso . . . . . . H11 H 0.300(3) 0.152(2) 0.881(2) 0.0334 1.0000 Uiso . . . . . . H12 H 0.294(3) 0.082(3) 0.767(2) 0.0346 1.0000 Uiso . . . . . . H21 H 0.663(4) 0.101(3) 0.841(2) 0.0407 1.0000 Uiso . . . . . . H22 H 0.578(4) -0.048(3) 0.892(2) 0.0425 1.0000 Uiso . . . . . . H31 H 0.814(4) -0.077(3) 0.721(2) 0.0361 1.0000 Uiso . . . . . . H32 H 0.603(3) -0.047(3) 0.663(2) 0.0358 1.0000 Uiso . . . . . . H51 H 0.975(4) 0.601(3) 0.676(2) 0.0431 1.0000 Uiso . . . . . . H52 H 0.751(4) 0.646(3) 0.707(2) 0.0433 1.0000 Uiso . . . . . . H53 H 0.833(4) 0.709(3) 0.567(2) 0.0427 1.0000 Uiso . . . . . . H81 H 0.893(4) 0.267(3) -0.049(3) 0.0479 1.0000 Uiso . . . . . . H82 H 0.895(4) 0.121(3) 0.084(2) 0.0467 1.0000 Uiso . . . . . . H91 H 0.765(4) 0.532(3) -0.035(3) 0.0624 1.0000 Uiso . . . . . . H92 H 0.815(4) 0.548(3) 0.100(3) 0.0622 1.0000 Uiso . . . . . . H93 H 0.589(5) 0.541(3) 0.080(3) 0.0620 1.0000 Uiso . . . . . . 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 0.01474(13) 0.01773(13) 0.01976(13) -0.00544(9) -0.00252(9) -0.00071(9) O1 0.0162(5) 0.0194(5) 0.0236(6) -0.0066(4) -0.0055(4) -0.0023(4) O2 0.0203(6) 0.0259(6) 0.0335(7) -0.0052(5) -0.0114(5) 0.0003(5) O3 0.0223(6) 0.0296(6) 0.0221(6) -0.0095(5) -0.0002(5) -0.0014(5) O4 0.0463(8) 0.0316(7) 0.0319(7) -0.0160(6) 0.0037(6) -0.0071(6) N1 0.0159(7) 0.0211(7) 0.0235(7) -0.0065(6) -0.0025(5) -0.0014(5) N2 0.0195(7) 0.0231(7) 0.0258(7) -0.0077(6) -0.0016(6) -0.0010(6) C1 0.0254(9) 0.0269(9) 0.0238(9) -0.0011(7) 0.0013(7) -0.0024(7) C2 0.0324(10) 0.0337(10) 0.0261(9) -0.0003(8) -0.0062(8) 0.0045(8) C3 0.0274(9) 0.0199(8) 0.0347(10) -0.0036(7) -0.0041(7) 0.0032(7) C4 0.0130(7) 0.0253(8) 0.0194(7) -0.0066(6) 0.0004(6) -0.0044(6) C5 0.0231(9) 0.0308(9) 0.0363(10) -0.0153(8) -0.0086(8) -0.0044(7) C6 0.0159(7) 0.0341(9) 0.0260(8) -0.0133(7) -0.0006(6) -0.0087(7) C7 0.0238(9) 0.0444(11) 0.0274(9) -0.0145(8) 0.0013(7) -0.0126(8) C8 0.0443(12) 0.0508(13) 0.0308(10) -0.0195(10) 0.0084(9) -0.0189(10) C9 0.0490(13) 0.0443(12) 0.0258(10) -0.0072(9) 0.0011(9) -0.0067(10) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 8.9(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_666 1.9850(11) yes Cu1 . O1 . 2.3069(11) yes Cu1 . O3 . 1.9689(12) yes Cu1 . N1 . 2.0104(14) yes Cu1 . N2 . 1.9825(14) yes O1 . C4 . 1.2867(19) yes O2 . C4 . 1.235(2) yes O3 . C6 . 1.284(2) yes O4 . C6 . 1.236(2) yes N1 . C1 . 1.475(2) yes N1 . H1 . 0.81(2) no N1 . H2 . 0.84(2) no N2 . C3 . 1.478(2) yes N2 . H3 . 0.86(2) no N2 . H4 . 0.82(2) no C1 . C2 . 1.515(3) yes C1 . H11 . 0.98(2) no C1 . H12 . 0.96(2) no C2 . C3 . 1.520(3) yes C2 . H21 . 0.95(2) no C2 . H22 . 0.96(2) no C3 . H31 . 0.94(2) no C3 . H32 . 0.99(2) no C4 . C5 . 1.510(2) yes C5 . H51 . 0.89(3) no C5 . H52 . 0.93(3) no C5 . H53 . 0.97(2) no C6 . C7 . 1.516(2) yes C7 . C8 . 1.328(3) yes C7 . C9 . 1.503(3) yes C8 . H81 . 0.93(3) no C8 . H82 . 0.94(3) no C9 . H91 . 0.95(3) no C9 . H92 . 1.01(3) no C9 . H93 . 0.99(3) 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 2_666 Cu1 . O1 . 80.29(4) yes O1 2_666 Cu1 . O3 . 85.78(5) yes O1 . Cu1 . O3 . 95.73(5) yes O1 2_666 Cu1 . N1 . 85.39(5) yes O1 . Cu1 . N1 . 89.72(5) yes O3 . Cu1 . N1 . 168.70(5) yes O1 2_666 Cu1 . N2 . 175.96(6) yes O1 . Cu1 . N2 . 95.71(5) yes O3 . Cu1 . N2 . 95.21(6) yes N1 . Cu1 . N2 . 94.08(6) yes Cu1 . O1 . Cu1 2_666 99.71(4) yes Cu1 . O1 . C4 . 130.77(10) yes Cu1 2_666 O1 . C4 . 127.74(10) yes Cu1 . O3 . C6 . 129.01(11) yes Cu1 . N1 . C1 . 122.07(11) yes Cu1 . N1 . H1 . 99.8(16) no C1 . N1 . H1 . 113.9(16) no Cu1 . N1 . H2 . 106.0(15) no C1 . N1 . H2 . 107.6(15) no H1 . N1 . H2 . 106(2) no Cu1 . N2 . C3 . 119.19(11) yes Cu1 . N2 . H3 . 106.0(15) no C3 . N2 . H3 . 110.4(15) no Cu1 . N2 . H4 . 104.4(16) no C3 . N2 . H4 . 110.6(16) no H3 . N2 . H4 . 105(2) no N1 . C1 . C2 . 112.48(15) yes N1 . C1 . H11 . 109.4(13) no C2 . C1 . H11 . 110.6(13) no N1 . C1 . H12 . 106.4(13) no C2 . C1 . H12 . 110.3(13) no H11 . C1 . H12 . 107.5(18) no C1 . C2 . C3 . 113.78(16) yes C1 . C2 . H21 . 110.7(14) no C3 . C2 . H21 . 108.6(14) no C1 . C2 . H22 . 108.2(14) no C3 . C2 . H22 . 108.6(14) no H21 . C2 . H22 . 106.7(19) no C2 . C3 . N2 . 111.68(15) yes C2 . C3 . H31 . 110.7(14) no N2 . C3 . H31 . 107.8(14) no C2 . C3 . H32 . 109.5(13) no N2 . C3 . H32 . 106.9(13) no H31 . C3 . H32 . 110.2(18) no O1 . C4 . O2 . 122.65(15) yes O1 . C4 . C5 . 117.01(14) yes O2 . C4 . C5 . 120.34(15) yes C4 . C5 . H51 . 110.5(16) no C4 . C5 . H52 . 107.7(15) no H51 . C5 . H52 . 112(2) no C4 . C5 . H53 . 111.6(14) no H51 . C5 . H53 . 113(2) no H52 . C5 . H53 . 101.9(20) no O3 . C6 . O4 . 125.39(16) yes O3 . C6 . C7 . 114.31(15) yes O4 . C6 . C7 . 120.29(16) yes C6 . C7 . C8 . 119.34(19) yes C6 . C7 . C9 . 117.50(16) yes C8 . C7 . C9 . 123.16(19) yes C7 . C8 . H81 . 122.8(16) no C7 . C8 . H82 . 120.5(15) no H81 . C8 . H82 . 117(2) no C7 . C9 . H91 . 111.8(17) no C7 . C9 . H92 . 110.9(16) no H91 . C9 . H92 . 108(2) no C7 . C9 . H93 . 111.3(16) no H91 . C9 . H93 . 108(2) no H92 . C9 . H93 . 106(2) 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 N1 . H1 . O3 2_666 142.6(19) 0.81(2) 2.58(2) 3.257(3) yes N1 . H2 . O2 1_455 161(2) 0.84(2) 2.12(2) 2.930(3) yes N2 . H3 . O2 . 152(2) 0.86(2) 2.25(2) 3.028(3) yes N2 . H4 . O4 . 149(2) 0.82(2) 2.13(2) 2.862(3) 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 O3 Cu1 O1 C4 -109.94(13) . . . . no O3 Cu1 O1 Cu1 84.71(5) . . . 2_666 no N1 Cu1 O1 C4 79.97(13) . . . . no N1 Cu1 O1 Cu1 -85.38(6) . . . 2_666 no N2 Cu1 O1 C4 -14.10(14) . . . . no N2 Cu1 O1 Cu1 -179.44(6) . . . 2_666 no O1 Cu1 O1 C4 165.34(13) 2_666 . . . no O1 Cu1 O1 Cu1 0.00(4) 2_666 . . 2_666 no O1 Cu1 O3 C6 129.68(13) . . . . no N2 Cu1 O3 C6 33.39(14) . . . . no O1 Cu1 O3 C6 -150.54(14) 2_666 . . . no O1 Cu1 N1 C1 -124.44(13) . . . . no N2 Cu1 N1 C1 -28.74(14) . . . . no O1 Cu1 N1 C1 155.28(14) 2_666 . . . no O1 Cu1 N2 C3 123.19(13) . . . . no O3 Cu1 N2 C3 -140.49(13) . . . . no N1 Cu1 N2 C3 33.08(14) . . . . no O1 Cu1 O1 Cu1 0.00(4) . . 2_666 2_666 no O1 Cu1 O1 C4 165.98(13) . . 2_666 2_666 no O3 Cu1 O1 Cu1 -96.56(5) . . 2_666 2_666 no O3 Cu1 O1 C4 69.42(13) . . 2_666 2_666 no N1 Cu1 O1 Cu1 90.50(5) . . 2_666 2_666 no N1 Cu1 O1 C4 -103.53(13) . . 2_666 2_666 no Cu1 O1 C4 O2 10.5(2) . . . . no Cu1 O1 C4 C5 -169.37(11) . . . . no Cu1 O1 C4 O2 172.15(11) 2_666 . . . no Cu1 O1 C4 C5 -7.8(2) 2_666 . . . no Cu1 O3 C6 O4 -5.1(2) . . . . no Cu1 O3 C6 C7 175.00(12) . . . . no Cu1 N1 C1 C2 46.45(19) . . . . no Cu1 N2 C3 C2 -56.40(19) . . . . no N1 C1 C2 C3 -65.3(2) . . . . no C1 C2 C3 N2 71.3(2) . . . . no O3 C6 C7 C8 -173.52(18) . . . . no O3 C6 C7 C9 6.7(3) . . . . no O4 C6 C7 C8 6.6(3) . . . . no O4 C6 C7 C9 -173.19(19) . . . . 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 3.5398(13) . . no Cu1 O4 3.2828(15) . . no Cu1 O3 3.8751(13) . 2_666 no Cu1 N1 3.7630(15) . 2_666 no O1 O3 3.1789(17) . . no O1 N1 3.0522(19) . . no O1 N2 3.188(2) . . no O1 O3 2.6911(17) . 2_666 no O1 N1 2.7094(18) . 2_666 no O1 O1 2.7779(16) . 2_666 no O2 C5 3.412(2) . 2_766 no O2 N1 2.9304(19) . 1_655 no O2 C4 3.410(2) . 2_766 no O2 N2 3.028(2) . . no O2 C1 3.372(2) . 1_655 no O3 C5 3.300(2) . 2_666 no O3 N1 3.257(2) . 2_666 no O3 N2 2.9182(19) . . no O3 C4 3.223(2) . 2_666 no O4 N2 2.862(2) . . no O4 C3 3.417(3) . 2_756 no N1 N2 2.922(2) . . no N1 C3 3.074(2) . . no N2 C1 3.122(2) . . no N2 C6 3.217(2) . . no C4 C4 3.275(2) . 2_766 no C4 C5 3.553(3) . 2_766 no _iucr_refine_instruction_details_constraints ; # # Punched on 11/05/15 at 15:31:47 # #LIST 12 BLOCK CONT SCALE CONT CU ( 1 ,X'S,U'S) UNTIL C ( 9 ) CONT H ( 1 ,X'S) UNTIL H ( 93 ) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 11/05/15 at 15:31:47 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END