#------------------------------------------------------------------------------ #$Date: 2016-10-08 00:56:55 +0300 (Sat, 08 Oct 2016) $ #$Revision: 187044 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/62/7226207.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7226207 loop_ _publ_author_name 'Gholivand, Khodayar' 'Farshadfar, Kaveh' 'Roe, S. Mark' 'Hosseini, Mahdieh' 'Gholami, Akram' _publ_section_title ; Investigation of structure-directing interactions within copper(i)thiocyanate complexes through X-ray analyses and non-covalent interaction (NCI) theoretical approach ; _journal_issue 37 _journal_name_full CrystEngComm _journal_page_first 7104 _journal_paper_doi 10.1039/C6CE01339B _journal_volume 18 _journal_year 2016 _chemical_formula_moiety 'C30 H24 Cu N4 O P S2' _chemical_formula_sum 'C30 H24 Cu N4 O P S2' _chemical_formula_weight 615.16 _chemical_name_common C1N _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2015-04-22 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _audit_update_record ; 2016-03-19 deposited with the CCDC. 2016-08-09 downloaded from the CCDC. ; _cell_angle_alpha 87.742(5) _cell_angle_beta 89.510(4) _cell_angle_gamma 66.545(5) _cell_formula_units_Z 2 _cell_length_a 9.8334(5) _cell_length_b 10.2673(6) _cell_length_c 15.0986(9) _cell_measurement_reflns_used 4813 _cell_measurement_temperature 173.0 _cell_measurement_theta_max 71.0640 _cell_measurement_theta_min 4.6750 _cell_volume 1397.31(15) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2008)' _diffrn_ambient_temperature 173.0 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1033 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_details ; 1 omega -27.00 58.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 36.7513 -19.0000 -90.0000 85 2 omega 40.00 71.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 36.7513 -99.0000 -180.0000 31 3 omega 47.00 82.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -88.0000 -175.6310 35 4 omega 94.00 140.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -88.0000 -175.6310 46 5 omega 105.00 136.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -92.0000 -138.8165 31 6 omega 81.00 120.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -93.0000 -5.0318 39 7 omega 54.00 98.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -92.0000 -138.8165 44 8 omega 39.00 69.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 -120.0000 30 9 omega 37.00 68.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 -90.0000 31 10 omega 69.00 103.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 15.0000 -150.0000 34 11 omega 106.00 176.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 15.0000 -150.0000 70 12 omega 127.00 174.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 45.0000 -90.0000 47 13 omega 109.00 165.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 61.0000 60.0000 56 14 omega 51.00 77.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -45.0000 90.0000 26 15 omega 42.00 69.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 60.0000 27 16 omega 37.00 63.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 30.0000 26 17 omega 39.00 77.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -45.0000 0.0000 38 18 omega 42.00 68.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -45.0000 -30.0000 26 19 omega 37.00 63.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 -60.0000 26 20 omega 39.00 107.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -90.0000 -94.2956 68 21 omega 48.00 74.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -93.0000 -5.0318 26 22 omega 53.00 78.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -95.0000 30.0000 25 23 omega 41.00 115.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -90.0000 102.5742 74 24 omega 37.00 68.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 150.0000 31 25 omega 41.00 66.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 120.0000 25 26 omega 14.00 78.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 36.7513 77.0000 90.0000 64 27 omega -35.00 64.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 36.7513 -19.0000 -180.0000 99 28 omega -3.00 34.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 36.7513 -99.0000 -180.0000 37 29 omega 38.00 68.00 1.0000 25.0000 omega____ theta____ kappa____ phi______ frames - 107.0000 -30.0000 -180.0000 30 30 omega -74.00 -35.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - -36.7513 97.0000 -37.0000 39 31 omega -106.00 -63.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - -36.7513 178.0000 -90.0000 43 32 omega -103.00 -75.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - -36.7513 178.0000 120.0000 28 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0176689000 _diffrn_orient_matrix_UB_12 0.1557929000 _diffrn_orient_matrix_UB_13 0.0023993000 _diffrn_orient_matrix_UB_21 -0.0567580000 _diffrn_orient_matrix_UB_22 0.0074426000 _diffrn_orient_matrix_UB_23 0.0958645000 _diffrn_orient_matrix_UB_31 0.1601025000 _diffrn_orient_matrix_UB_32 -0.0496636000 _diffrn_orient_matrix_UB_33 0.0350971000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9032 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.243 _diffrn_reflns_theta_min 4.698 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.292 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light orange' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.462 _exptl_crystal_description needle _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.326 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 5283 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0295 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.2495P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.0778 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4509 _reflns_number_total 5283 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; cuscn542_orangeb.res created by SHELXL-2014/7 TITL cuscn542_orangeb_a.res in P-1 CELL 1.54184 9.8334 10.2673 15.0986 87.742 89.51 66.545 ZERR 2 0.0005 0.0006 0.0009 0.005 0.004 0.005 LATT 1 SFAC C H Cu N O P S UNIT 60 48 2 8 2 2 4 L.S. 10 PLAN 5 TEMP -100.15 REM Old TITL CuSCN542_orangeb in P-1 #2 BOND $H LIST 6 fmap 2 MORE -1 CONF ACTA REM C:/XcaliburData/Mark/Modares/CuSCN542_orangeb/struct/olex2_CuSCN542_o REM rangeb/CuSCN542_orangeb.hkl WGHT 0.036500 0.249500 FVAR 5.64432 CU1 3 0.252111 0.569985 0.666757 11.00000 0.02595 0.02849 = 0.02312 -0.00210 0.00418 -0.00925 S1 7 0.429224 0.922816 0.581811 11.00000 0.03496 0.02832 = 0.03713 0.00020 0.00267 -0.01263 S2 7 0.857560 0.148987 0.767221 11.00000 0.03368 0.05424 = 0.02997 -0.00410 -0.00499 -0.00716 P1 6 0.172595 0.528632 0.796260 11.00000 0.01986 0.02501 = 0.02159 -0.00189 0.00236 -0.00787 O1 5 0.557422 0.372717 0.730330 11.00000 0.02937 0.04806 = 0.03481 -0.01508 0.00175 -0.00636 N1 4 0.326975 0.722152 0.651774 11.00000 0.03167 0.03091 = 0.03593 -0.00134 0.00274 -0.01107 N2 4 0.117887 0.611649 0.549970 11.00000 0.02488 0.02557 = 0.02646 -0.00049 0.00089 -0.00740 N3 4 0.392759 0.413439 0.578909 11.00000 0.02125 0.02512 = 0.02816 -0.00254 0.00249 -0.00427 N4 4 0.529726 0.305498 0.592246 11.00000 0.02405 0.03177 = 0.02888 -0.00811 0.00029 0.00128 AFIX 43 H4 2 0.568925 0.243765 0.550808 11.00000 -1.20000 AFIX 0 C1 1 0.367764 0.806991 0.624722 11.00000 0.02183 0.02674 = 0.02538 -0.00388 0.00008 -0.00393 C2 1 -0.019166 0.708906 0.533931 11.00000 0.02627 0.02835 = 0.03677 -0.00182 0.00200 -0.00576 AFIX 43 H2 2 -0.074060 0.761647 0.581981 11.00000 -1.20000 AFIX 0 C3 1 -0.085372 0.736698 0.450352 11.00000 0.02661 0.02994 = 0.04334 0.00579 -0.00790 -0.00743 AFIX 43 H3 2 -0.182819 0.807293 0.441679 11.00000 -1.20000 AFIX 0 C4 1 -0.007006 0.659942 0.380352 11.00000 0.03597 0.03515 = 0.03436 0.00406 -0.01167 -0.01543 AFIX 43 H4A 2 -0.049242 0.677107 0.322494 11.00000 -1.20000 AFIX 0 C5 1 0.134149 0.557536 0.395851 11.00000 0.03586 0.03375 = 0.02838 -0.00438 -0.00090 -0.01277 AFIX 43 H5 2 0.190331 0.502592 0.348908 11.00000 -1.20000 AFIX 0 C6 1 0.192240 0.536434 0.481019 11.00000 0.02702 0.02628 = 0.02728 -0.00072 -0.00018 -0.00991 C7 1 0.339148 0.427700 0.500226 11.00000 0.02847 0.03320 = 0.02633 -0.00592 0.00169 -0.00478 AFIX 43 H7 2 0.394826 0.367866 0.454993 11.00000 -1.20000 AFIX 0 C8 1 0.605741 0.293473 0.669907 11.00000 0.02373 0.03097 = 0.02882 -0.00281 0.00260 -0.00871 C9 1 0.755235 0.176802 0.671909 11.00000 0.02430 0.03096 = 0.02933 0.00044 -0.00167 -0.00985 C10 1 0.835934 0.088448 0.606993 11.00000 0.02207 0.03095 = 0.03011 -0.00633 -0.00086 -0.00505 AFIX 43 H10 2 0.798507 0.086797 0.549438 11.00000 -1.20000 AFIX 0 C11 1 0.980807 0.000649 0.636081 11.00000 0.02574 0.03155 = 0.04978 -0.00656 0.00320 -0.00544 AFIX 43 H11 2 1.052307 -0.065807 0.599709 11.00000 -1.20000 AFIX 0 C12 1 1.007184 0.020873 0.720815 11.00000 0.02729 0.03857 = 0.04923 0.00696 -0.00624 -0.00717 AFIX 43 H12 2 1.098429 -0.030279 0.751067 11.00000 -1.20000 AFIX 0 C13 1 -0.028593 0.583495 0.801601 11.00000 0.02201 0.02880 = 0.02072 -0.00300 0.00149 -0.00747 C14 1 -0.115102 0.718469 0.765196 11.00000 0.02946 0.03170 = 0.03261 0.00268 0.00188 -0.00913 AFIX 43 H14 2 -0.068703 0.777682 0.741922 11.00000 -1.20000 AFIX 0 C15 1 -0.268473 0.766295 0.762921 11.00000 0.02778 0.03799 = 0.03624 0.00284 -0.00046 -0.00060 AFIX 43 H15 2 -0.326599 0.858606 0.738824 11.00000 -1.20000 AFIX 0 C16 1 -0.336971 0.680462 0.795479 11.00000 0.01921 0.05207 = 0.03554 -0.00375 0.00037 -0.00750 AFIX 43 H16 2 -0.441828 0.712732 0.792602 11.00000 -1.20000 AFIX 0 C17 1 -0.252472 0.547381 0.832287 11.00000 0.02816 0.04536 = 0.03373 -0.00464 0.00462 -0.01787 AFIX 43 H17 2 -0.299575 0.488652 0.855360 11.00000 -1.20000 AFIX 0 C18 1 -0.098634 0.498988 0.835709 11.00000 0.02495 0.03129 = 0.02692 -0.00129 0.00089 -0.01090 AFIX 43 H18 2 -0.041332 0.407689 0.861513 11.00000 -1.20000 AFIX 0 C19 1 0.210303 0.626959 0.884385 11.00000 0.02906 0.02880 = 0.02345 -0.00247 0.00360 -0.01355 C20 1 0.102254 0.719244 0.938090 11.00000 0.03156 0.04246 = 0.03171 -0.00914 0.00327 -0.01153 AFIX 43 H20 2 0.001453 0.733534 0.930367 11.00000 -1.20000 AFIX 0 C21 1 0.140817 0.790774 1.003049 11.00000 0.04985 0.04572 = 0.03323 -0.01520 0.00867 -0.01472 AFIX 43 H21 2 0.066093 0.854911 1.038890 11.00000 -1.20000 AFIX 0 C22 1 0.286921 0.769104 1.015712 11.00000 0.05935 0.05318 = 0.03127 -0.01071 0.00537 -0.03661 AFIX 43 H22 2 0.313083 0.817144 1.060759 11.00000 -1.20000 AFIX 0 C23 1 0.395241 0.677430 0.962804 11.00000 0.04292 0.06770 = 0.04330 -0.01691 0.00680 -0.03579 AFIX 43 H23 2 0.496111 0.662000 0.971699 11.00000 -1.20000 AFIX 0 C24 1 0.357100 0.607642 0.896551 11.00000 0.03079 0.04965 = 0.03942 -0.01534 0.00833 -0.02127 AFIX 43 H24 2 0.431781 0.546418 0.859390 11.00000 -1.20000 AFIX 0 C25 1 0.246947 0.346493 0.842039 11.00000 0.02032 0.02767 = 0.02834 0.00014 -0.00129 -0.00815 C26 1 0.243052 0.314170 0.932632 11.00000 0.03020 0.03685 = 0.02872 0.00068 -0.00011 -0.00973 AFIX 43 H26 2 0.202841 0.388716 0.972851 11.00000 -1.20000 AFIX 0 C27 1 0.297223 0.174790 0.963861 11.00000 0.04134 0.04676 = 0.03899 0.01383 -0.00440 -0.01287 AFIX 43 H27 2 0.294789 0.153498 1.025509 11.00000 -1.20000 AFIX 0 C28 1 0.355482 0.065204 0.905195 11.00000 0.04443 0.02987 = 0.05971 0.01158 -0.00391 -0.00500 AFIX 43 H28 2 0.392450 -0.030828 0.926848 11.00000 -1.20000 AFIX 0 C29 1 0.359699 0.095632 0.815697 11.00000 0.03947 0.02900 = 0.05127 -0.00507 0.00258 -0.00524 AFIX 43 H29 2 0.398619 0.020653 0.775671 11.00000 -1.20000 AFIX 0 C30 1 0.307062 0.235808 0.784194 11.00000 0.02597 0.03198 = 0.03202 -0.00366 -0.00036 -0.00738 AFIX 43 H30 2 0.312058 0.256477 0.722664 11.00000 -1.20000 AFIX 0 HKLF 4 REM cuscn542_orangeb_a.res in P-1 REM R1 = 0.0295 for 4509 Fo > 4sig(Fo) and 0.0364 for all 5283 data REM 352 parameters refined using 0 restraints END WGHT 0.0364 0.2522 REM Highest difference peak 0.326, deepest hole -0.307, 1-sigma level 0.050 Q1 1 0.0567 0.5537 0.8012 11.00000 0.05 0.33 Q2 1 0.2122 0.4133 0.8244 11.00000 0.05 0.29 Q3 1 0.7981 0.1132 0.6343 11.00000 0.05 0.28 Q4 1 0.3533 0.5195 0.6996 11.00000 0.05 0.28 Q5 1 0.2016 0.5400 0.7329 11.00000 0.05 0.28 REM The information below was added by Olex2. REM REM R1 = 0.0295 for 4509 Fo > 4sig(Fo) and 0.0364 for all 9032 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.33, deepest hole -0.31 REM Mean Shift 0, Max Shift -0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0364 REM R1_gt = 0.0295 REM wR_ref = 0.0778 REM GOOF = 1.022 REM Shift_max = -0.002 REM Shift_mean = 0 REM Reflections_all = 9032 REM Reflections_gt = 4509 REM Parameters = n/a REM Hole = -0.31 REM Peak = 0.33 REM Flack = n/a ; _cod_data_source_file c6ce01339b2.cif _cod_data_source_block cuscn542_orangeb _cod_depositor_comments 'Adding full bibliography for 7226207--7226210.cif.' _cod_database_code 7226207 _chemical_oxdiff_formula C30H24N4O1P1S2Cu1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.76 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 2.a Aromatic/amide H refined with riding coordinates: N4(H4), C2(H2), C3(H3), C4(H4A), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30) ; _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Cu1 Cu 0.25211(3) 0.56999(3) 0.66676(2) 0.02634(8) Uani 1 1 d . S1 S 0.42922(5) 0.92282(5) 0.58181(3) 0.03351(12) Uani 1 1 d . S2 S 0.85756(6) 0.14899(6) 0.76722(3) 0.04245(14) Uani 1 1 d . P1 P 0.17260(5) 0.52863(5) 0.79626(3) 0.02247(10) Uani 1 1 d . O1 O 0.55742(15) 0.37272(17) 0.73033(10) 0.0399(3) Uani 1 1 d . N1 N 0.32698(18) 0.72215(18) 0.65177(11) 0.0333(4) Uani 1 1 d . N2 N 0.11789(17) 0.61165(16) 0.54997(10) 0.0265(3) Uani 1 1 d . N3 N 0.39276(16) 0.41344(16) 0.57891(10) 0.0264(3) Uani 1 1 d . N4 N 0.52973(17) 0.30550(18) 0.59225(11) 0.0319(4) Uani 1 1 d . H4 H 0.5689 0.2438 0.5508 0.038 Uiso 1 1 calc R C1 C 0.36776(19) 0.80699(19) 0.62472(12) 0.0264(4) Uani 1 1 d . C2 C -0.0192(2) 0.7089(2) 0.53393(14) 0.0321(4) Uani 1 1 d . H2 H -0.0741 0.7616 0.5820 0.038 Uiso 1 1 calc R C3 C -0.0854(2) 0.7367(2) 0.45035(14) 0.0347(4) Uani 1 1 d . H3 H -0.1828 0.8073 0.4417 0.042 Uiso 1 1 calc R C4 C -0.0070(2) 0.6599(2) 0.38035(14) 0.0348(4) Uani 1 1 d . H4A H -0.0492 0.6771 0.3225 0.042 Uiso 1 1 calc R C5 C 0.1341(2) 0.5575(2) 0.39585(13) 0.0329(4) Uani 1 1 d . H5 H 0.1903 0.5026 0.3489 0.039 Uiso 1 1 calc R C6 C 0.1922(2) 0.53643(19) 0.48102(12) 0.0271(4) Uani 1 1 d . C7 C 0.3391(2) 0.4277(2) 0.50023(13) 0.0316(4) Uani 1 1 d . H7 H 0.3948 0.3679 0.4550 0.038 Uiso 1 1 calc R C8 C 0.6057(2) 0.2935(2) 0.66991(12) 0.0285(4) Uani 1 1 d . C9 C 0.7552(2) 0.1768(2) 0.67191(13) 0.0286(4) Uani 1 1 d . C10 C 0.8359(2) 0.0884(2) 0.60699(13) 0.0293(4) Uani 1 1 d . H10 H 0.7985 0.0868 0.5494 0.035 Uiso 1 1 calc R C11 C 0.9808(2) 0.0006(2) 0.63608(15) 0.0374(5) Uani 1 1 d . H11 H 1.0523 -0.0658 0.5997 0.045 Uiso 1 1 calc R C12 C 1.0072(2) 0.0209(2) 0.72081(16) 0.0404(5) Uani 1 1 d . H12 H 1.0984 -0.0303 0.7511 0.049 Uiso 1 1 calc R C13 C -0.02859(19) 0.58350(19) 0.80160(11) 0.0246(3) Uani 1 1 d . C14 C -0.1151(2) 0.7185(2) 0.76520(13) 0.0323(4) Uani 1 1 d . H14 H -0.0687 0.7777 0.7419 0.039 Uiso 1 1 calc R C15 C -0.2685(2) 0.7663(2) 0.76292(14) 0.0381(5) Uani 1 1 d . H15 H -0.3266 0.8586 0.7388 0.046 Uiso 1 1 calc R C16 C -0.3370(2) 0.6805(2) 0.79548(14) 0.0377(5) Uani 1 1 d . H16 H -0.4418 0.7127 0.7926 0.045 Uiso 1 1 calc R C17 C -0.2525(2) 0.5474(2) 0.83229(13) 0.0347(4) Uani 1 1 d . H17 H -0.2996 0.4887 0.8554 0.042 Uiso 1 1 calc R C18 C -0.0986(2) 0.4990(2) 0.83571(12) 0.0278(4) Uani 1 1 d . H18 H -0.0413 0.4077 0.8615 0.033 Uiso 1 1 calc R C19 C 0.2103(2) 0.6270(2) 0.88439(12) 0.0264(4) Uani 1 1 d . C20 C 0.1023(2) 0.7192(2) 0.93809(13) 0.0361(4) Uani 1 1 d . H20 H 0.0015 0.7335 0.9304 0.043 Uiso 1 1 calc R C21 C 0.1408(3) 0.7908(3) 1.00305(15) 0.0440(5) Uani 1 1 d . H21 H 0.0661 0.8549 1.0389 0.053 Uiso 1 1 calc R C22 C 0.2869(3) 0.7691(3) 1.01571(14) 0.0432(5) Uani 1 1 d . H22 H 0.3131 0.8171 1.0608 0.052 Uiso 1 1 calc R C23 C 0.3952(3) 0.6774(3) 0.96280(16) 0.0466(6) Uani 1 1 d . H23 H 0.4961 0.6620 0.9717 0.056 Uiso 1 1 calc R C24 C 0.3571(2) 0.6076(2) 0.89655(14) 0.0380(5) Uani 1 1 d . H24 H 0.4318 0.5464 0.8594 0.046 Uiso 1 1 calc R C25 C 0.24695(19) 0.34649(19) 0.84204(12) 0.0259(4) Uani 1 1 d . C26 C 0.2431(2) 0.3142(2) 0.93263(13) 0.0331(4) Uani 1 1 d . H26 H 0.2028 0.3887 0.9729 0.040 Uiso 1 1 calc R C27 C 0.2972(3) 0.1748(3) 0.96386(16) 0.0443(5) Uani 1 1 d . H27 H 0.2948 0.1535 1.0255 0.053 Uiso 1 1 calc R C28 C 0.3555(3) 0.0652(2) 0.90520(17) 0.0481(6) Uani 1 1 d . H28 H 0.3924 -0.0308 0.9268 0.058 Uiso 1 1 calc R C29 C 0.3597(2) 0.0956(2) 0.81570(16) 0.0425(5) Uani 1 1 d . H29 H 0.3986 0.0207 0.7757 0.051 Uiso 1 1 calc R C30 C 0.3071(2) 0.2358(2) 0.78419(13) 0.0312(4) Uani 1 1 d . H30 H 0.3121 0.2565 0.7227 0.037 Uiso 1 1 calc 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 0.02595(14) 0.02849(14) 0.02312(14) -0.00210(10) 0.00418(10) -0.00925(11) S1 0.0350(2) 0.0283(2) 0.0371(3) 0.00020(18) 0.00267(19) -0.01263(19) S2 0.0337(3) 0.0542(3) 0.0300(2) -0.0041(2) -0.0050(2) -0.0072(2) P1 0.0199(2) 0.0250(2) 0.0216(2) -0.00189(16) 0.00236(15) -0.00787(16) O1 0.0294(7) 0.0481(9) 0.0348(7) -0.0151(6) 0.0018(6) -0.0064(6) N1 0.0317(8) 0.0309(8) 0.0359(9) -0.0013(7) 0.0027(7) -0.0111(7) N2 0.0249(7) 0.0256(7) 0.0265(7) -0.0005(6) 0.0009(6) -0.0074(6) N3 0.0213(7) 0.0251(7) 0.0282(8) -0.0025(6) 0.0025(6) -0.0043(6) N4 0.0240(8) 0.0318(8) 0.0289(8) -0.0081(6) 0.0003(6) 0.0013(6) C1 0.0218(8) 0.0267(9) 0.0254(8) -0.0039(7) 0.0001(7) -0.0039(7) C2 0.0263(9) 0.0283(9) 0.0368(10) -0.0018(8) 0.0020(8) -0.0058(8) C3 0.0266(9) 0.0299(10) 0.0433(11) 0.0058(8) -0.0079(8) -0.0074(8) C4 0.0360(10) 0.0351(10) 0.0344(10) 0.0041(8) -0.0117(8) -0.0154(8) C5 0.0359(10) 0.0337(10) 0.0284(9) -0.0044(8) -0.0009(8) -0.0128(8) C6 0.0270(9) 0.0263(9) 0.0273(9) -0.0007(7) -0.0002(7) -0.0099(7) C7 0.0285(9) 0.0332(10) 0.0263(9) -0.0059(7) 0.0017(7) -0.0048(8) C8 0.0237(9) 0.0310(9) 0.0288(9) -0.0028(7) 0.0026(7) -0.0087(7) C9 0.0243(9) 0.0310(9) 0.0293(9) 0.0004(7) -0.0017(7) -0.0099(7) C10 0.0221(8) 0.0309(9) 0.0301(9) -0.0063(7) -0.0009(7) -0.0050(7) C11 0.0257(9) 0.0315(10) 0.0498(12) -0.0066(9) 0.0032(8) -0.0054(8) C12 0.0273(10) 0.0386(11) 0.0492(12) 0.0070(9) -0.0062(9) -0.0072(9) C13 0.0220(8) 0.0288(9) 0.0207(8) -0.0030(6) 0.0015(6) -0.0075(7) C14 0.0295(9) 0.0317(10) 0.0326(10) 0.0027(8) 0.0019(8) -0.0091(8) C15 0.0278(10) 0.0380(11) 0.0362(11) 0.0028(8) -0.0005(8) -0.0006(8) C16 0.0192(8) 0.0521(13) 0.0355(10) -0.0037(9) 0.0004(8) -0.0075(8) C17 0.0282(10) 0.0454(11) 0.0337(10) -0.0046(8) 0.0046(8) -0.0179(9) C18 0.0249(9) 0.0313(9) 0.0269(9) -0.0013(7) 0.0009(7) -0.0109(7) C19 0.0291(9) 0.0288(9) 0.0234(8) -0.0025(7) 0.0036(7) -0.0136(7) C20 0.0316(10) 0.0425(11) 0.0317(10) -0.0091(8) 0.0033(8) -0.0115(9) C21 0.0498(13) 0.0457(13) 0.0332(11) -0.0152(9) 0.0087(9) -0.0147(11) C22 0.0594(14) 0.0532(13) 0.0313(10) -0.0107(9) 0.0054(10) -0.0366(12) C23 0.0429(12) 0.0677(16) 0.0433(12) -0.0169(11) 0.0068(10) -0.0358(12) C24 0.0308(10) 0.0496(12) 0.0394(11) -0.0153(9) 0.0083(8) -0.0213(9) C25 0.0203(8) 0.0277(9) 0.0283(9) 0.0001(7) -0.0013(7) -0.0082(7) C26 0.0302(9) 0.0369(10) 0.0287(9) 0.0007(8) -0.0001(7) -0.0097(8) C27 0.0413(11) 0.0468(13) 0.0390(11) 0.0138(10) -0.0044(9) -0.0129(10) C28 0.0444(12) 0.0299(11) 0.0597(15) 0.0116(10) -0.0039(11) -0.0050(9) C29 0.0395(11) 0.0290(10) 0.0513(13) -0.0051(9) 0.0026(10) -0.0052(9) C30 0.0260(9) 0.0320(10) 0.0320(10) -0.0037(8) -0.0004(7) -0.0074(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 Cu1 P1 119.82(5) N1 Cu1 N2 99.81(7) N1 Cu1 N3 101.96(6) N2 Cu1 P1 121.68(4) N2 Cu1 N3 77.57(6) N3 Cu1 P1 126.46(5) C12 S2 C9 91.95(10) C13 P1 Cu1 114.06(6) C19 P1 Cu1 112.95(6) C19 P1 C13 103.11(8) C25 P1 Cu1 118.17(6) C25 P1 C13 104.03(8) C25 P1 C19 102.81(8) C1 N1 Cu1 165.86(16) C2 N2 Cu1 129.80(13) C2 N2 C6 117.17(16) C6 N2 Cu1 112.62(12) N4 N3 Cu1 131.07(12) C7 N3 Cu1 113.24(12) C7 N3 N4 115.66(16) N3 N4 H4 119.9 C8 N4 N3 120.22(15) C8 N4 H4 119.9 N1 C1 S1 177.09(17) N2 C2 H2 118.4 N2 C2 C3 123.24(19) C3 C2 H2 118.4 C2 C3 H3 120.6 C4 C3 C2 118.80(18) C4 C3 H3 120.6 C3 C4 H4A 120.6 C3 C4 C5 118.81(18) C5 C4 H4A 120.6 C4 C5 H5 120.6 C4 C5 C6 118.85(19) C6 C5 H5 120.6 N2 C6 C5 123.11(17) N2 C6 C7 116.47(16) C5 C6 C7 120.41(17) N3 C7 C6 119.30(17) N3 C7 H7 120.4 C6 C7 H7 120.4 O1 C8 N4 123.44(17) O1 C8 C9 122.92(18) N4 C8 C9 113.61(16) C8 C9 S2 117.44(14) C10 C9 S2 111.02(14) C10 C9 C8 131.35(17) C9 C10 H10 124.0 C9 C10 C11 112.02(18) C11 C10 H10 124.0 C10 C11 H11 123.5 C12 C11 C10 113.01(19) C12 C11 H11 123.5 S2 C12 H12 124.0 C11 C12 S2 111.99(16) C11 C12 H12 124.0 C14 C13 P1 116.40(14) C18 C13 P1 124.62(14) C18 C13 C14 118.94(17) C13 C14 H14 119.9 C15 C14 C13 120.29(19) C15 C14 H14 119.9 C14 C15 H15 119.8 C16 C15 C14 120.36(19) C16 C15 H15 119.8 C15 C16 H16 120.1 C15 C16 C17 119.77(18) C17 C16 H16 120.1 C16 C17 H17 119.8 C16 C17 C18 120.31(19) C18 C17 H17 119.8 C13 C18 C17 120.32(18) C13 C18 H18 119.8 C17 C18 H18 119.8 C20 C19 P1 124.21(15) C20 C19 C24 119.00(18) C24 C19 P1 116.78(14) C19 C20 H20 119.8 C19 C20 C21 120.3(2) C21 C20 H20 119.8 C20 C21 H21 119.9 C22 C21 C20 120.3(2) C22 C21 H21 119.9 C21 C22 H22 120.1 C21 C22 C23 119.9(2) C23 C22 H22 120.1 C22 C23 H23 119.9 C22 C23 C24 120.2(2) C24 C23 H23 119.9 C19 C24 C23 120.3(2) C19 C24 H24 119.8 C23 C24 H24 119.8 C26 C25 P1 122.44(15) C30 C25 P1 118.57(14) C30 C25 C26 118.98(18) C25 C26 H26 119.8 C27 C26 C25 120.4(2) C27 C26 H26 119.8 C26 C27 H27 120.0 C26 C27 C28 120.1(2) C28 C27 H27 120.0 C27 C28 H28 119.9 C29 C28 C27 120.2(2) C29 C28 H28 119.9 C28 C29 H29 120.0 C28 C29 C30 119.9(2) C30 C29 H29 120.0 C25 C30 H30 119.7 C29 C30 C25 120.51(19) C29 C30 H30 119.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cu1 P1 2.1881(5) Cu1 N1 1.9796(18) Cu1 N2 2.1367(15) Cu1 N3 2.1500(15) S1 C1 1.644(2) S2 C9 1.7113(19) S2 C12 1.703(2) P1 C13 1.8307(18) P1 C19 1.8274(19) P1 C25 1.8242(18) O1 C8 1.210(2) N1 C1 1.155(3) N2 C2 1.337(2) N2 C6 1.347(2) N3 N4 1.372(2) N3 C7 1.283(2) N4 H4 0.8800 N4 C8 1.371(2) C2 H2 0.9500 C2 C3 1.391(3) C3 H3 0.9500 C3 C4 1.378(3) C4 H4A 0.9500 C4 C5 1.382(3) C5 H5 0.9500 C5 C6 1.385(3) C6 C7 1.454(3) C7 H7 0.9500 C8 C9 1.481(3) C9 C10 1.377(3) C10 H10 0.9500 C10 C11 1.411(3) C11 H11 0.9500 C11 C12 1.348(3) C12 H12 0.9500 C13 C14 1.398(3) C13 C18 1.388(3) C14 H14 0.9500 C14 C15 1.388(3) C15 H15 0.9500 C15 C16 1.380(3) C16 H16 0.9500 C16 C17 1.382(3) C17 H17 0.9500 C17 C18 1.392(3) C18 H18 0.9500 C19 C20 1.389(3) C19 C24 1.389(3) C20 H20 0.9500 C20 C21 1.389(3) C21 H21 0.9500 C21 C22 1.377(3) C22 H22 0.9500 C22 C23 1.380(3) C23 H23 0.9500 C23 C24 1.390(3) C24 H24 0.9500 C25 C26 1.399(3) C25 C30 1.392(3) C26 H26 0.9500 C26 C27 1.378(3) C27 H27 0.9500 C27 C28 1.391(4) C28 H28 0.9500 C28 C29 1.379(3) C29 H29 0.9500 C29 C30 1.387(3) C30 H30 0.9500 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 Cu1 P1 C13 C14 -46.13(16) Cu1 P1 C13 C18 131.30(14) Cu1 P1 C19 C20 123.25(16) Cu1 P1 C19 C24 -56.01(17) Cu1 P1 C25 C26 158.75(14) Cu1 P1 C25 C30 -22.54(17) Cu1 N2 C2 C3 170.84(15) Cu1 N2 C6 C5 -172.26(16) Cu1 N2 C6 C7 8.7(2) Cu1 N3 N4 C8 -6.9(3) Cu1 N3 C7 C6 -3.9(2) S2 C9 C10 C11 -0.7(2) P1 C13 C14 C15 177.22(16) P1 C13 C18 C17 -176.35(15) P1 C19 C20 C21 -179.37(17) P1 C19 C24 C23 -179.32(19) P1 C25 C26 C27 178.35(16) P1 C25 C30 C29 -177.55(16) O1 C8 C9 S2 3.8(3) O1 C8 C9 C10 -170.8(2) N2 C2 C3 C4 0.5(3) N2 C6 C7 N3 -3.3(3) N3 N4 C8 O1 1.5(3) N3 N4 C8 C9 -176.61(16) N4 N3 C7 C6 177.93(17) N4 C8 C9 S2 -178.07(14) N4 C8 C9 C10 7.3(3) C2 N2 C6 C5 1.2(3) C2 N2 C6 C7 -177.93(17) C2 C3 C4 C5 0.4(3) C3 C4 C5 C6 -0.5(3) C4 C5 C6 N2 -0.3(3) C4 C5 C6 C7 178.74(18) C5 C6 C7 N3 177.56(19) C6 N2 C2 C3 -1.3(3) C7 N3 N4 C8 170.91(18) C8 C9 C10 C11 174.1(2) C9 S2 C12 C11 0.39(19) C9 C10 C11 C12 1.0(3) C10 C11 C12 S2 -0.9(3) C12 S2 C9 C8 -175.45(16) C12 S2 C9 C10 0.20(17) C13 P1 C19 C20 -0.33(19) C13 P1 C19 C24 -179.59(16) C13 P1 C25 C26 -73.63(17) C13 P1 C25 C30 105.08(15) C13 C14 C15 C16 -0.9(3) C14 C13 C18 C17 1.0(3) C14 C15 C16 C17 1.4(3) C15 C16 C17 C18 -0.7(3) C16 C17 C18 C13 -0.5(3) C18 C13 C14 C15 -0.4(3) C19 P1 C13 C14 76.72(16) C19 P1 C13 C18 -105.85(16) C19 P1 C25 C26 33.62(18) C19 P1 C25 C30 -147.66(15) C19 C20 C21 C22 -1.0(4) C20 C19 C24 C23 1.4(3) C20 C21 C22 C23 0.9(4) C21 C22 C23 C24 0.4(4) C22 C23 C24 C19 -1.5(4) C24 C19 C20 C21 -0.1(3) C25 P1 C13 C14 -176.25(15) C25 P1 C13 C18 1.19(17) C25 P1 C19 C20 -108.28(18) C25 P1 C19 C24 72.46(17) C25 C26 C27 C28 -0.4(3) C26 C25 C30 C29 1.2(3) C26 C27 C28 C29 0.2(4) C27 C28 C29 C30 0.6(4) C28 C29 C30 C25 -1.4(3) C30 C25 C26 C27 -0.4(3)