data_ras1305 _audit_creation_date "13-08-21" _audit_creation_method CRYSTALS_ver_14.40 _audit_update_record ; 2013-08-21 - Report on C19 H16 Cu N4 O3 by Anthony C. Willis for Rasoul Vafazadeh 2013-08-21 - passes checkcif tests with minor warnings ; _oxford_structure_analysis_title 'transform axes for std sp gp' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.8983(10) _cell_length_b 8.4055(3) _cell_length_c 20.8417(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3485.9(3) _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,z' 'x+1/2,-y+1/2,-z' 'x,-y+1/2,z+1/2' '-x,y+1/2,-z+1/2' '-x+1/2,-y,z+1/2' 'x+1/2,y,-z+1/2' 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 0.0033 0.0016 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 0.3201 1.2651 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 0.0061 0.0033 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 0.0106 0.0060 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 8 # Given Formula = C19 H16 Cu1 N4 O3 # Dc = 1.57 Fooo = 1688.00 Mu = 12.82 M = 411.91 # Found Formula = C19 H16 Cu1 N4 O3 # Dc = 1.57 FOOO = 1688.00 Mu = 12.82 M = 411.91 _chemical_formula_sum 'C19 H16 Cu N4 O3' _chemical_formula_moiety 'C19 H16 Cu N4 O3' _chemical_compound_source ' Yazd University ' _chemical_formula_weight 411.91 _cell_measurement_reflns_used 60581 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25 _cell_measurement_temperature 200 _exptl_crystal_description 'needle' _exptl_crystal_colour 'green' _exptl_crystal_size_min 0.010 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_max 0.540 _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 1.282 # Sheldrick geometric approximatio 0.95 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.67 # 0.99*9.49/14.06 scalepack ; 0.95 _exptl_absorpt_correction_T_max 0.99 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 0.8 deg at rate 88 sec/frame, crystal-detector distance 40mm, multiple scan sets so over 95 percent of data collected with 4-fold redundancy or more. ; # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 33860 _reflns_number_total 3058 _diffrn_reflns_av_R_equivalents 0.144 # scalepack # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 3058 # Theoretical number of reflections is about 6147 _diffrn_reflns_theta_min 2.806 _diffrn_reflns_theta_max 25.010 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.010 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min 0 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 10 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 2.27 _oxford_diffrn_Wilson_scale 128.26 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.48 _refine_diff_density_max 1.39 # 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 3058 _refine_ls_number_restraints 0 _refine_ls_number_parameters 244 _oxford_refine_ls_R_factor_ref 0.1523 _refine_ls_wR_factor_ref 0.1195 _refine_ls_goodness_of_fit_ref 0.9703 _refine_ls_shift/su_max 0.0003297 _refine_ls_shift/su_mean 0.0000229 # The values computed with all filters except I/sigma _oxford_reflns_number_all 3058 _refine_ls_R_factor_all 0.1523 _refine_ls_wR_factor_all 0.1195 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1540 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_gt 0.0901 # 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 constr #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^ + 9.61P] ,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. 0200, 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 ' willis@rsc.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~19~H~16~N~4~O~3~)] --- ras1305 ; # 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 'N. Hasanzadeh ' ; 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. 0200, Australia ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Cu(C~19~H~16~N~4~O~3~)] is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one [Cu(C~19~H~16~N~4~O~3~)] molecule. ; _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 NH and RV and was recrystallised from ???. The sample identification was H1-new. ; _refine_special_details #Text of the paper ; Crystals of this compound were obtained as very thin needles which diffracted only weakly. Even with long exposure times, the number of reflections with intensities above background is limited. The observation:parameter ratio is therefore lower than we would like but the identity of the compound is clearly established, nonetheless. There do not appear to be any significant refinement anomalies. Owing to the poor quality of the data, hydrogen atoms were not reliably observed in difference electron density maps prior to their inclusion. H atoms attached to C were added at calculated positions and then were 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 U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints and the displacement parameters were held fixed. There is some doubt as to whether or not there should be H atoms on N1 and N4. There were no peaks in the final difference electron density map at these locations, but with such weak intensity data this is no real proof. The C---N---N angles, however, are about 109\%, which seems more consistent with a tetrahedral geometry (i.e. a N with a lone-pair of electrons) than a trigonal geometry. The C---N---N angle for compounds we have studied where the H is clearly observed tend to be about 115\%. The peaks in the final difference electron density map are of similar intensity and are situated randomly through the structure. ; # 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--?. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Johnson, C.K. (1976). ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. ; # 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 0.72681(3) 0.50795(9) 0.31568(3) 0.0400 1.0000 Uani . . . . . . O1 O 0.66920(17) 0.3906(4) 0.37284(18) 0.0417 1.0000 Uani . . . . . . O2 O 0.66081(17) 0.6106(4) 0.26319(17) 0.0386 1.0000 Uani . . . . . . O3 O 0.95135(18) 0.5415(5) 0.3132(2) 0.0577 1.0000 Uani . . . . . . N1 N 0.7708(2) 0.2727(5) 0.4001(2) 0.0395 1.0000 Uani . . . . . . N2 N 0.7958(2) 0.3865(5) 0.3579(2) 0.0361 1.0000 Uani . . . . . . N3 N 0.7876(2) 0.6278(5) 0.2621(2) 0.0354 1.0000 Uani . . . . . . N4 N 0.7554(3) 0.7279(6) 0.2189(2) 0.0434 1.0000 Uani . . . . . . C1 C 0.6016(3) 0.2182(7) 0.4658(3) 0.0444 1.0000 Uani . . . . . . C2 C 0.5697(3) 0.1318(7) 0.5132(3) 0.0546 1.0000 Uani . . . . . . C3 C 0.6041(4) 0.0256(8) 0.5514(3) 0.0600 1.0000 Uani . . . . . . C4 C 0.6722(3) 0.0063(8) 0.5419(3) 0.0564 1.0000 Uani . . . . . . C5 C 0.7049(3) 0.0922(7) 0.4948(3) 0.0458 1.0000 Uani . . . . . . C6 C 0.6706(3) 0.1982(7) 0.4562(3) 0.0375 1.0000 Uani . . . . . . C7 C 0.7047(3) 0.2932(7) 0.4060(3) 0.0350 1.0000 Uani . . . . . . C8 C 0.8607(3) 0.3974(7) 0.3517(3) 0.0369 1.0000 Uani . . . . . . C9 C 0.9077(3) 0.2895(7) 0.3871(3) 0.0508 1.0000 Uani . . . . . . C10 C 0.8904(3) 0.5242(7) 0.3099(3) 0.0420 1.0000 Uani . . . . . . C11 C 0.8530(3) 0.6312(7) 0.2640(3) 0.0401 1.0000 Uani . . . . . . C12 C 0.8943(3) 0.7415(7) 0.2229(3) 0.0519 1.0000 Uani . . . . . . C13 C 0.6895(3) 0.7035(7) 0.2231(3) 0.0368 1.0000 Uani . . . . . . C14 C 0.6459(3) 0.7948(7) 0.1784(3) 0.0386 1.0000 Uani . . . . . . C15 C 0.6735(3) 0.8868(7) 0.1295(3) 0.0499 1.0000 Uani . . . . . . C16 C 0.6314(3) 0.9714(8) 0.0886(3) 0.0588 1.0000 Uani . . . . . . C17 C 0.5625(3) 0.9618(7) 0.0955(3) 0.0567 1.0000 Uani . . . . . . C18 C 0.5356(3) 0.8709(7) 0.1438(3) 0.0543 1.0000 Uani . . . . . . C19 C 0.5764(3) 0.7864(7) 0.1845(3) 0.0437 1.0000 Uani . . . . . . H11 H 0.5778 0.2894 0.4403 0.0528 1.0000 Uiso R . . . . . H21 H 0.5241 0.1458 0.5195 0.0659 1.0000 Uiso R . . . . . H31 H 0.5815 -0.0308 0.5831 0.0718 1.0000 Uiso R . . . . . H41 H 0.6957 -0.0638 0.5677 0.0678 1.0000 Uiso R . . . . . H51 H 0.7509 0.0789 0.4890 0.0548 1.0000 Uiso R . . . . . H91 H 0.9528 0.3110 0.3750 0.0762 1.0000 Uiso R . . . . . H92 H 0.9034 0.3046 0.4326 0.0762 1.0000 Uiso R . . . . . H93 H 0.8978 0.1809 0.3774 0.0758 1.0000 Uiso R . . . . . H121 H 0.9384 0.6979 0.2177 0.0783 1.0000 Uiso R . . . . . H122 H 0.8966 0.8434 0.2427 0.0779 1.0000 Uiso R . . . . . H123 H 0.8737 0.7520 0.1815 0.0778 1.0000 Uiso R . . . . . H151 H 0.7195 0.8911 0.1250 0.0600 1.0000 Uiso R . . . . . H161 H 0.6500 1.0331 0.0569 0.0710 1.0000 Uiso R . . . . . H171 H 0.5348 1.0191 0.0678 0.0678 1.0000 Uiso R . . . . . H181 H 0.4889 0.8679 0.1493 0.0648 1.0000 Uiso R . . . . . H191 H 0.5582 0.7217 0.2158 0.0516 1.0000 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 0.0250(3) 0.0459(4) 0.0492(4) 0.0043(4) 0.0015(4) -0.0019(4) O1 0.022(2) 0.051(3) 0.053(3) 0.006(2) -0.002(2) 0.001(2) O2 0.026(2) 0.046(2) 0.044(2) 0.006(2) -0.0014(19) -0.007(2) O3 0.022(2) 0.075(3) 0.076(3) 0.003(3) -0.004(2) -0.009(2) N1 0.028(3) 0.044(3) 0.047(3) 0.002(3) -0.002(2) -0.004(3) N2 0.028(3) 0.034(3) 0.046(3) -0.004(3) -0.004(2) -0.002(2) N3 0.027(3) 0.035(3) 0.044(3) -0.007(2) 0.003(2) -0.003(2) N4 0.032(3) 0.049(3) 0.049(3) 0.005(3) 0.006(3) -0.001(2) C1 0.036(4) 0.052(4) 0.045(4) 0.003(3) -0.004(3) -0.008(3) C2 0.041(4) 0.063(5) 0.061(5) 0.000(4) 0.011(4) -0.013(4) C3 0.068(5) 0.065(5) 0.047(4) 0.004(4) 0.003(4) -0.022(4) C4 0.060(4) 0.060(4) 0.049(4) 0.017(4) -0.012(3) -0.010(5) C5 0.040(4) 0.052(4) 0.045(4) 0.002(3) -0.005(3) -0.004(3) C6 0.034(3) 0.044(4) 0.035(4) 0.001(3) -0.001(3) -0.004(3) C7 0.025(3) 0.042(4) 0.038(4) -0.008(3) -0.007(3) -0.003(3) C8 0.025(3) 0.040(4) 0.046(4) -0.011(3) -0.004(3) 0.002(3) C9 0.024(3) 0.071(5) 0.058(4) -0.002(4) -0.008(3) -0.001(3) C10 0.027(3) 0.053(4) 0.046(4) -0.014(4) 0.002(3) -0.003(3) C11 0.037(4) 0.033(3) 0.050(4) -0.005(3) 0.009(3) 0.002(3) C12 0.035(4) 0.051(4) 0.070(5) -0.001(4) 0.013(4) -0.004(3) C13 0.041(4) 0.027(4) 0.042(4) -0.008(3) 0.005(3) 0.001(3) C14 0.040(3) 0.040(3) 0.035(4) 0.003(3) 0.002(3) 0.001(3) C15 0.049(4) 0.049(4) 0.052(4) 0.005(4) 0.005(4) 0.004(3) C16 0.058(4) 0.067(5) 0.052(4) 0.014(4) 0.008(4) 0.003(4) C17 0.053(4) 0.063(5) 0.055(4) 0.009(4) -0.010(4) 0.007(4) C18 0.044(4) 0.060(5) 0.059(5) 0.005(4) -0.010(4) 0.000(4) C19 0.033(3) 0.051(4) 0.048(4) 0.003(4) 0.000(3) -0.007(3) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.08855(3) 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 . 1.925(4) yes Cu1 . O2 . 1.915(4) yes Cu1 . N2 . 1.923(4) yes Cu1 . N3 . 1.930(4) yes O1 . C7 . 1.283(6) yes O2 . C13 . 1.277(6) yes O3 . C10 . 1.224(6) yes N1 . N2 . 1.391(6) yes N1 . C7 . 1.331(6) yes N2 . C8 . 1.301(6) yes N3 . N4 . 1.389(6) yes N3 . C11 . 1.302(6) yes N4 . C13 . 1.332(7) yes C1 . C2 . 1.380(8) yes C1 . C6 . 1.397(7) yes C1 . H11 . 0.930 no C2 . C3 . 1.378(8) yes C2 . H21 . 0.924 no C3 . C4 . 1.378(8) yes C3 . H31 . 0.931 no C4 . C5 . 1.381(7) yes C4 . H41 . 0.925 no C5 . C6 . 1.380(7) yes C5 . H51 . 0.932 no C6 . C7 . 1.483(7) yes C8 . C9 . 1.498(7) yes C8 . C10 . 1.497(8) yes C9 . H91 . 0.950 no C9 . H92 . 0.959 no C9 . H93 . 0.956 no C10 . C11 . 1.509(8) yes C11 . C12 . 1.506(7) yes C12 . H121 . 0.957 no C12 . H122 . 0.952 no C12 . H123 . 0.960 no C13 . C14 . 1.486(8) yes C14 . C15 . 1.393(7) yes C14 . C19 . 1.391(7) yes C15 . C16 . 1.391(8) yes C15 . H151 . 0.921 no C16 . C17 . 1.381(8) yes C16 . H161 . 0.918 no C17 . C18 . 1.372(8) yes C17 . H171 . 0.931 no C18 . C19 . 1.374(8) yes C18 . H181 . 0.935 no C19 . H191 . 0.923 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 . O2 . 100.13(15) yes O1 . Cu1 . N2 . 82.52(17) yes O2 . Cu1 . N2 . 171.86(18) yes O1 . Cu1 . N3 . 177.03(17) yes O2 . Cu1 . N3 . 82.19(17) yes N2 . Cu1 . N3 . 95.43(19) yes Cu1 . O1 . C7 . 109.4(3) yes Cu1 . O2 . C13 . 110.1(4) yes N2 . N1 . C7 . 108.8(5) yes N1 . N2 . Cu1 . 113.5(3) yes N1 . N2 . C8 . 117.8(5) yes Cu1 . N2 . C8 . 128.7(4) yes Cu1 . N3 . N4 . 113.7(3) yes Cu1 . N3 . C11 . 128.3(4) yes N4 . N3 . C11 . 117.9(5) yes N3 . N4 . C13 . 108.6(5) yes C2 . C1 . C6 . 119.3(6) yes C2 . C1 . H11 . 121.0 no C6 . C1 . H11 . 119.7 no C1 . C2 . C3 . 121.7(6) yes C1 . C2 . H21 . 119.0 no C3 . C2 . H21 . 119.2 no C2 . C3 . C4 . 118.8(6) yes C2 . C3 . H31 . 120.0 no C4 . C3 . H31 . 121.2 no C3 . C4 . C5 . 120.2(6) yes C3 . C4 . H41 . 119.2 no C5 . C4 . H41 . 120.6 no C4 . C5 . C6 . 121.2(6) yes C4 . C5 . H51 . 119.5 no C6 . C5 . H51 . 119.3 no C1 . C6 . C5 . 118.7(5) yes C1 . C6 . C7 . 119.1(5) yes C5 . C6 . C7 . 122.1(5) yes C6 . C7 . N1 . 116.7(5) yes C6 . C7 . O1 . 118.1(4) yes N1 . C7 . O1 . 125.2(5) yes N2 . C8 . C9 . 121.9(5) yes N2 . C8 . C10 . 120.0(5) yes C9 . C8 . C10 . 118.1(5) yes C8 . C9 . H91 . 110.1 no C8 . C9 . H92 . 110.6 no H91 . C9 . H92 . 108.8 no C8 . C9 . H93 . 110.2 no H91 . C9 . H93 . 108.6 no H92 . C9 . H93 . 108.6 no C8 . C10 . O3 . 116.3(5) yes C8 . C10 . C11 . 126.8(4) yes O3 . C10 . C11 . 116.9(5) yes C10 . C11 . N3 . 119.9(5) yes C10 . C11 . C12 . 117.3(5) yes N3 . C11 . C12 . 122.8(6) yes C11 . C12 . H121 . 109.2 no C11 . C12 . H122 . 109.5 no H121 . C12 . H122 . 110.4 no C11 . C12 . H123 . 109.7 no H121 . C12 . H123 . 108.8 no H122 . C12 . H123 . 109.2 no N4 . C13 . O2 . 125.3(6) yes N4 . C13 . C14 . 117.0(5) yes O2 . C13 . C14 . 117.7(5) yes C13 . C14 . C15 . 121.1(5) yes C13 . C14 . C19 . 119.7(5) yes C15 . C14 . C19 . 119.1(6) yes C14 . C15 . C16 . 119.7(6) yes C14 . C15 . H151 . 119.2 no C16 . C15 . H151 . 121.1 no C15 . C16 . C17 . 120.3(6) yes C15 . C16 . H161 . 119.1 no C17 . C16 . H161 . 120.6 no C16 . C17 . C18 . 119.8(6) yes C16 . C17 . H171 . 119.5 no C18 . C17 . H171 . 120.7 no C17 . C18 . C19 . 120.7(6) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 119.8 no C14 . C19 . C18 . 120.4(6) yes C14 . C19 . H191 . 119.0 no C18 . C19 . H191 . 120.6 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 N1 2.837(4) . 3_655 no Cu1 N4 3.120(5) . 3_645 no Cu1 N2 3.332(4) . 3_655 no Cu1 C7 3.339(6) . 3_655 no Cu1 N3 3.397(4) . 3_645 no O1 C11 3.177(7) . 3_645 no O1 N3 3.308(5) . 3_645 no O1 N1 3.473(5) . 3_655 no O1 C10 3.551(7) . 3_645 no O1 C12 3.596(7) . 3_645 no O2 C8 3.066(7) . 3_655 no O2 N2 3.165(5) . 3_655 no O2 C9 3.285(7) . 3_655 no O2 C12 3.396(7) . 3_645 no O2 N1 3.443(5) . 3_655 no O3 C19 3.230(7) . 8 no O3 C18 3.359(7) . 8 no O3 C19 3.478(7) . 3_645 no N1 N3 3.333(6) . 3_645 no N1 C5 3.368(7) . 3_655 no N2 C13 3.216(7) . 3_645 no N2 C5 3.336(7) . 3_655 no N2 N4 3.348(6) . 3_645 no N2 N3 3.387(6) . 3_645 no N2 C6 3.392(7) . 3_655 no N2 C7 3.562(7) . 3_655 no N3 C7 3.309(7) . 3_655 no N3 C15 3.513(7) . 3_645 no N3 C14 3.554(7) . 3_645 no N3 N4 3.583(7) . 3_645 no C2 C2 3.59(1) . 2_656 no C6 C8 3.395(9) . 3_645 no C6 C10 3.593(9) . 3_645 no C7 C11 3.454(9) . 3_645 no C7 C10 3.564(9) . 3_645 no C8 C13 3.292(9) . 3_645 no C10 C19 3.356(9) . 3_645 no C10 C14 3.428(9) . 3_645 no C11 C14 3.343(9) . 3_645 no C11 C15 3.515(9) . 3_645 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cu1 O1 C7 N1 . . . . -2.2(7) no Cu1 O1 C7 C6 . . . . 176.1(4) no Cu1 O2 C13 N4 . . . . -1.0(7) no Cu1 O2 C13 C14 . . . . -179.6(4) no Cu1 N2 N1 C7 . . . . -8.1(5) no Cu1 N2 C8 C9 . . . . -178.2(4) no Cu1 N2 C8 C10 . . . . 3.9(8) no Cu1 N3 N4 C13 . . . . -5.0(5) no Cu1 N3 C11 C10 . . . . 4.1(8) no Cu1 N3 C11 C12 . . . . -174.5(4) no O1 Cu1 O2 C13 . . . . 176.5(4) no O1 Cu1 N2 N1 . . . . 5.9(3) no O1 Cu1 N2 C8 . . . . -174.4(5) no O1 C7 N1 N2 . . . . 6.9(8) no O1 C7 C6 C1 . . . . -0.2(8) no O1 C7 C6 C5 . . . . -179.1(6) no O2 Cu1 O1 C7 . . . . 170.0(4) no O2 Cu1 N3 N4 . . . . 3.8(3) no O2 Cu1 N3 C11 . . . . -179.9(5) no O2 C13 N4 N3 . . . . 4.1(8) no O2 C13 C14 C15 . . . . -173.9(5) no O2 C13 C14 C19 . . . . 4.9(8) no O3 C10 C8 N2 . . . . 170.3(5) no O3 C10 C8 C9 . . . . -7.7(8) no O3 C10 C11 N3 . . . . -174.4(5) no O3 C10 C11 C12 . . . . 4.3(8) no N1 N2 Cu1 N3 . . . . -176.3(3) no N1 N2 C8 C9 . . . . 1.5(8) no N1 N2 C8 C10 . . . . -176.4(5) no N1 C7 C6 C1 . . . . 178.2(5) no N1 C7 C6 C5 . . . . -0.6(9) no N2 Cu1 O1 C7 . . . . -2.2(4) no N2 Cu1 N3 N4 . . . . 175.9(3) no N2 Cu1 N3 C11 . . . . -7.7(5) no N2 N1 C7 C6 . . . . -171.4(5) no N2 C8 C10 C11 . . . . -10.3(9) no N3 Cu1 O2 C13 . . . . -1.6(4) no N3 Cu1 N2 C8 . . . . 3.5(5) no N3 N4 C13 C14 . . . . -177.4(5) no N3 C11 C10 C8 . . . . 6.2(9) no N4 N3 C11 C10 . . . . -179.7(5) no N4 N3 C11 C12 . . . . 1.7(8) no N4 C13 C14 C15 . . . . 7.4(9) no N4 C13 C14 C19 . . . . -173.8(5) no C1 C2 C3 C4 . . . . 0(1) no C1 C6 C5 C4 . . . . 0.3(9) no C2 C1 C6 C5 . . . . -0.1(9) no C2 C1 C6 C7 . . . . -179.0(6) no C2 C3 C4 C5 . . . . -0(1) no C3 C2 C1 C6 . . . . -0.2(9) no C3 C4 C5 C6 . . . . -0(1) no C4 C5 C6 C7 . . . . 179.2(6) no C7 N1 N2 C8 . . . . 172.2(5) no C8 C10 C11 C12 . . . . -175.2(6) no C9 C8 C10 C11 . . . . 171.7(6) no C11 N3 N4 C13 . . . . 178.3(5) no C13 C14 C15 C16 . . . . -179.7(6) no C13 C14 C19 C18 . . . . 179.6(6) no C14 C15 C16 C17 . . . . -1.3(9) no C14 C19 C18 C17 . . . . 1.6(9) no C15 C14 C19 C18 . . . . -1.6(9) no C15 C16 C17 C18 . . . . 1.4(9) no C16 C15 C14 C19 . . . . 1.5(9) no C16 C17 C18 C19 . . . . -1.5(9) no #------------------------------------------------------------------------------ _iucr_refine_instruction_details_constraints ; # # Punched on 21/08/13 at 14:14:06 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) H ( 123,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 21/08/13 at 14:14:06 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END