#------------------------------------------------------------------------------ #$Date: 2016-10-08 00:56:55 +0300 (Sat, 08 Oct 2016) $ #$Revision: 187044 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/62/7226208.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_7226208 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 C1S _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 2015-04-15 _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 85.195(5) _cell_angle_beta 78.024(5) _cell_angle_gamma 80.116(6) _cell_formula_units_Z 2 _cell_length_a 10.7768(9) _cell_length_b 11.0362(8) _cell_length_c 12.2584(5) _cell_measurement_reflns_used 4129 _cell_measurement_temperature 173.0 _cell_measurement_theta_max 28.2660 _cell_measurement_theta_min 3.7610 _cell_volume 1403.30(17) _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 0.990 _diffrn_measured_fraction_theta_max 0.805 _diffrn_measurement_details ; 1 omega -33.00 51.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.9733 57.0000 -180.0000 84 2 omega -82.00 11.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.9733 -77.0000 -60.0000 93 3 omega -43.00 49.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -15.9733 77.0000 60.0000 92 4 omega 6.00 56.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 16.5983 -99.0000 -120.0000 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0243961000 _diffrn_orient_matrix_UB_12 -0.0257017000 _diffrn_orient_matrix_UB_13 0.0535383000 _diffrn_orient_matrix_UB_21 -0.0512319000 _diffrn_orient_matrix_UB_22 0.0502274000 _diffrn_orient_matrix_UB_23 0.0077521000 _diffrn_orient_matrix_UB_31 -0.0377264000 _diffrn_orient_matrix_UB_32 -0.0329151000 _diffrn_orient_matrix_UB_33 -0.0241044000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_unetI/netI 0.0596 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.805 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9736 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.805 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.466 _diffrn_reflns_theta_min 3.402 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63168 _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 'clear light red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.456 _exptl_crystal_description irregular _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.492 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 6265 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.113 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0444 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.4153P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0951 _refine_ls_wR_factor_ref 0.1072 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4999 _reflns_number_total 6265 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; cuscn542_red.res created by SHELXL-2014/7 TITL cuscn542_red_a.res in P-1 CELL 0.71073 10.776783 11.036157 12.258382 85.195 78.0237 80.1155 ZERR 2 0.000874 0.000784 0.000535 0.0048 0.0052 0.0064 LATT 1 SFAC C H Cu N O P S UNIT 60 48 2 8 2 2 4 L.S. 10 PLAN 20 TEMP -100 REM Old TITL CuSCN542_red in P-1 #2 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 REM C:/XcaliburData/Mark/Modares/CuSCN542_red/struct/olex2_CuSCN542_red/C REM uSCN542_red.hkl WGHT 0.033400 0.415300 FVAR 5.04534 CU1 3 0.303713 0.363605 0.646911 11.00000 0.02540 0.02418 = 0.02261 -0.00052 -0.00305 -0.00257 S1 7 0.147451 0.529193 0.697581 11.00000 0.04321 0.02985 = 0.03035 -0.00058 0.00376 0.00712 S2 7 0.625236 0.370040 0.970497 11.00000 0.03439 0.10293 = 0.03064 -0.00758 -0.00764 -0.00533 P1 6 0.293638 0.191933 0.750906 11.00000 0.02061 0.02235 = 0.02103 -0.00153 -0.00419 -0.00147 O1 5 0.451036 0.406559 0.810301 11.00000 0.02284 0.05009 = 0.03425 -0.00755 -0.00491 -0.00503 N1 4 0.127620 0.656026 0.491073 11.00000 0.03580 0.03588 = 0.03729 -0.00139 -0.00896 0.00143 N2 4 0.327524 0.351945 0.477574 11.00000 0.02479 0.02405 = 0.02330 -0.00034 -0.00502 -0.00454 N3 4 0.509380 0.364322 0.590986 11.00000 0.01947 0.02533 = 0.02574 0.00030 -0.00480 -0.00408 N4 4 0.601344 0.357642 0.654004 11.00000 0.01963 0.03487 = 0.02923 -0.00390 -0.00649 -0.00261 AFIX 43 H4 2 0.683445 0.341987 0.623331 11.00000 -1.20000 AFIX 0 C1 1 0.134688 0.602530 0.575456 11.00000 0.01948 0.02618 = 0.03655 -0.00806 -0.00208 -0.00014 C2 1 0.234364 0.354138 0.419919 11.00000 0.03408 0.03161 = 0.03068 -0.00173 -0.01190 -0.00521 AFIX 43 H2 2 0.147733 0.363696 0.459168 11.00000 -1.20000 AFIX 0 C3 1 0.258977 0.343058 0.305434 11.00000 0.04602 0.04367 = 0.02932 -0.00433 -0.01598 -0.00988 AFIX 43 H3 2 0.190384 0.345174 0.267211 11.00000 -1.20000 AFIX 0 C4 1 0.383740 0.328985 0.247979 11.00000 0.05999 0.03669 = 0.02343 -0.00347 -0.00984 -0.00992 AFIX 43 H4A 2 0.402899 0.319495 0.169659 11.00000 -1.20000 AFIX 0 C5 1 0.481508 0.328813 0.305885 11.00000 0.03818 0.03228 = 0.02887 -0.00591 -0.00098 -0.00441 AFIX 43 H5 2 0.568560 0.320702 0.267797 11.00000 -1.20000 AFIX 0 C6 1 0.449713 0.340714 0.420507 11.00000 0.02661 0.02392 = 0.02458 -0.00192 -0.00292 -0.00272 C7 1 0.547650 0.341481 0.487244 11.00000 0.02280 0.02612 = 0.03138 -0.00298 -0.00215 -0.00175 AFIX 43 H7 2 0.636565 0.325609 0.454880 11.00000 -1.20000 AFIX 0 C8 1 0.562993 0.375831 0.765901 11.00000 0.02683 0.02750 = 0.02962 0.00017 -0.00678 -0.00632 C9 1 0.667444 0.355003 0.829248 11.00000 0.02875 0.03023 = 0.03039 -0.00236 -0.00689 -0.00503 C10 1 0.796520 0.327023 0.797108 11.00000 0.03046 0.06154 = 0.03547 -0.00827 -0.01005 0.00465 AFIX 43 H10 2 0.839072 0.316395 0.721690 11.00000 -1.20000 AFIX 0 C11 1 0.861362 0.315272 0.887248 11.00000 0.03286 0.08443 = 0.04533 -0.01122 -0.01903 0.00670 AFIX 43 H11 2 0.952001 0.295237 0.879308 11.00000 -1.20000 AFIX 0 C12 1 0.780594 0.335578 0.985394 11.00000 0.04100 0.08152 = 0.03993 -0.00407 -0.02086 -0.00015 AFIX 43 H12 2 0.807227 0.331184 1.054991 11.00000 -1.20000 AFIX 0 C13 1 0.451572 0.102265 0.752322 11.00000 0.02222 0.02381 = 0.02929 0.00096 -0.00466 -0.00176 C14 1 0.526332 0.061790 0.651246 11.00000 0.03170 0.02994 = 0.03259 -0.00074 -0.00253 -0.00047 AFIX 43 H14 2 0.491553 0.076671 0.585339 11.00000 -1.20000 AFIX 0 C15 1 0.649657 0.000648 0.645425 11.00000 0.02925 0.03343 = 0.04643 -0.00032 0.00591 -0.00008 AFIX 43 H15 2 0.699134 -0.027682 0.576152 11.00000 -1.20000 AFIX 0 C16 1 0.701250 -0.019407 0.740283 11.00000 0.02054 0.04617 = 0.06345 0.01005 -0.00365 0.00176 AFIX 43 H16 2 0.786507 -0.061681 0.736389 11.00000 -1.20000 AFIX 0 C17 1 0.629934 0.021476 0.840680 11.00000 0.03290 0.06318 = 0.04618 0.01424 -0.01702 -0.00059 AFIX 43 H17 2 0.666357 0.008067 0.905752 11.00000 -1.20000 AFIX 0 C18 1 0.504936 0.082255 0.847244 11.00000 0.02716 0.04632 = 0.03142 0.00661 -0.00721 -0.00291 AFIX 43 H18 2 0.455855 0.110189 0.916789 11.00000 -1.20000 AFIX 0 C19 1 0.208544 0.085257 0.701285 11.00000 0.02387 0.02580 = 0.01955 -0.00266 -0.00205 -0.00484 C20 1 0.099485 0.135746 0.659130 11.00000 0.02707 0.02766 = 0.02321 -0.00209 -0.00377 -0.00225 AFIX 43 H20 2 0.075816 0.222627 0.652579 11.00000 -1.20000 AFIX 0 C21 1 0.025361 0.059637 0.626700 11.00000 0.03056 0.03951 = 0.02764 -0.00278 -0.00846 -0.00751 AFIX 43 H21 2 -0.050247 0.094469 0.599857 11.00000 -1.20000 AFIX 0 C22 1 0.060922 -0.066456 0.633242 11.00000 0.03512 0.04013 = 0.02703 -0.00927 -0.00057 -0.01510 AFIX 43 H22 2 0.010394 -0.118432 0.610296 11.00000 -1.20000 AFIX 0 C23 1 0.170349 -0.117039 0.673299 11.00000 0.03343 0.02454 = 0.03265 -0.00708 0.00143 -0.00681 AFIX 43 H23 2 0.195208 -0.203900 0.677246 11.00000 -1.20000 AFIX 0 C24 1 0.243559 -0.042286 0.707523 11.00000 0.02563 0.02599 = 0.02921 -0.00190 -0.00407 -0.00334 AFIX 43 H24 2 0.318220 -0.077849 0.735491 11.00000 -1.20000 AFIX 0 C25 1 0.211303 0.204478 0.895977 11.00000 0.02069 0.02935 = 0.01933 -0.00065 -0.00638 -0.00104 C26 1 0.156486 0.108664 0.957482 11.00000 0.02726 0.02933 = 0.02507 -0.00212 -0.00650 -0.00414 AFIX 43 H26 2 0.168563 0.030698 0.926007 11.00000 -1.20000 AFIX 0 C27 1 0.084485 0.125635 1.064109 11.00000 0.02649 0.03837 = 0.02702 0.00435 -0.00514 -0.00633 AFIX 43 H27 2 0.047506 0.059621 1.105682 11.00000 -1.20000 AFIX 0 C28 1 0.066690 0.239202 1.109766 11.00000 0.03033 0.04517 = 0.01880 -0.00446 -0.00347 -0.00235 AFIX 43 H28 2 0.016255 0.251361 1.182513 11.00000 -1.20000 AFIX 0 C29 1 0.121139 0.334224 1.051012 11.00000 0.03562 0.03596 = 0.02428 -0.00769 -0.00590 -0.00464 AFIX 43 H29 2 0.108968 0.411717 1.083354 11.00000 -1.20000 AFIX 0 C30 1 0.194091 0.317736 0.944319 11.00000 0.02819 0.03021 = 0.02601 -0.00270 -0.00409 -0.00801 AFIX 43 H30 2 0.232404 0.383723 0.904097 11.00000 -1.20000 AFIX 0 HKLF 4 REM cuscn542_red_a.res in P-1 REM R1 = 0.0444 for 4999 Fo > 4sig(Fo) and 0.0605 for all 6265 data REM 352 parameters refined using 0 restraints END WGHT 0.0351 0.6510 REM Highest difference peak 0.492, deepest hole -0.537, 1-sigma level 0.074 Q1 1 0.2307 0.4454 0.6607 11.00000 0.05 0.49 Q2 1 0.3734 0.1350 0.7536 11.00000 0.05 0.45 Q3 1 0.3749 0.2806 0.6448 11.00000 0.05 0.42 Q4 1 0.6543 0.2851 0.9666 11.00000 0.05 0.39 Q5 1 0.6455 0.3645 0.8848 11.00000 0.05 0.35 Q6 1 0.2370 0.2840 0.7535 11.00000 0.05 0.33 Q7 1 0.3456 0.3066 0.7273 11.00000 0.05 0.31 Q8 1 0.1360 0.1556 0.9156 11.00000 0.05 0.29 Q9 1 0.3355 0.2416 0.6874 11.00000 0.05 0.28 Q10 1 0.0423 0.1847 1.0667 11.00000 0.05 0.28 Q11 1 0.3359 0.4391 0.7050 11.00000 0.05 0.28 Q12 1 0.1456 0.5847 0.5181 11.00000 0.05 0.28 Q13 1 0.2420 0.2669 0.9408 11.00000 0.05 0.27 Q14 1 0.1199 0.1400 1.0070 11.00000 0.05 0.27 Q15 1 0.8196 0.2464 0.7680 11.00000 0.05 0.27 Q16 1 0.3756 0.1965 0.6381 11.00000 0.05 0.26 Q17 1 0.6471 -0.0245 0.7877 11.00000 0.05 0.26 Q18 1 0.3131 0.4408 0.5688 11.00000 0.05 0.26 Q19 1 0.5046 0.0532 0.6283 11.00000 0.05 0.26 Q20 1 0.1257 0.1418 0.6051 11.00000 0.05 0.26 REM The information below was added by Olex2. REM REM R1 = 0.0444 for 4999 Fo > 4sig(Fo) and 0.0605 for all 9736 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.49, deepest hole -0.54 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0605 REM R1_gt = 0.0444 REM wR_ref = 0.1072 REM GOOF = 1.113 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 9736 REM Reflections_gt = 4999 REM Parameters = n/a REM Hole = -0.54 REM Peak = 0.49 REM Flack = n/a ; _cod_data_source_file c6ce01339b2.cif _cod_data_source_block cuscn542_red _cod_depositor_comments 'Adding full bibliography for 7226207--7226210.cif.' _cod_original_cell_volume 1403.28(17) _cod_database_code 7226208 _chemical_oxdiff_formula C30H24N4O1S2P1Cu1 _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 98.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 0.30371(3) 0.36361(3) 0.64691(2) 0.02451(11) Uani 1 1 d . S1 S 0.14745(9) 0.52919(7) 0.69758(6) 0.0377(2) Uani 1 1 d . S2 S 0.62524(9) 0.37004(11) 0.97050(7) 0.0562(3) Uani 1 1 d . P1 P 0.29364(7) 0.19193(6) 0.75091(5) 0.02152(16) Uani 1 1 d . O1 O 0.4510(2) 0.40656(19) 0.81030(16) 0.0356(5) Uani 1 1 d . N1 N 0.1276(3) 0.6560(2) 0.4911(2) 0.0369(6) Uani 1 1 d . N2 N 0.3275(2) 0.35194(19) 0.47757(17) 0.0240(5) Uani 1 1 d . N3 N 0.5094(2) 0.36432(19) 0.59099(17) 0.0235(5) Uani 1 1 d . N4 N 0.6013(2) 0.3576(2) 0.65400(18) 0.0277(5) Uani 1 1 d . H4 H 0.6834 0.3420 0.6233 0.033 Uiso 1 1 calc R C1 C 0.1347(3) 0.6025(2) 0.5755(2) 0.0279(6) Uani 1 1 d . C2 C 0.2344(3) 0.3541(3) 0.4199(2) 0.0313(7) Uani 1 1 d . H2 H 0.1477 0.3637 0.4592 0.038 Uiso 1 1 calc R C3 C 0.2590(3) 0.3431(3) 0.3054(2) 0.0379(8) Uani 1 1 d . H3 H 0.1904 0.3452 0.2672 0.046 Uiso 1 1 calc R C4 C 0.3837(4) 0.3290(3) 0.2480(2) 0.0394(8) Uani 1 1 d . H4A H 0.4029 0.3195 0.1697 0.047 Uiso 1 1 calc R C5 C 0.4815(3) 0.3288(3) 0.3059(2) 0.0338(7) Uani 1 1 d . H5 H 0.5686 0.3207 0.2678 0.041 Uiso 1 1 calc R C6 C 0.4497(3) 0.3407(2) 0.4205(2) 0.0255(6) Uani 1 1 d . C7 C 0.5477(3) 0.3415(2) 0.4872(2) 0.0274(6) Uani 1 1 d . H7 H 0.6366 0.3256 0.4549 0.033 Uiso 1 1 calc R C8 C 0.5630(3) 0.3758(2) 0.7659(2) 0.0277(6) Uani 1 1 d . C9 C 0.6674(3) 0.3550(3) 0.8292(2) 0.0295(6) Uani 1 1 d . C10 C 0.7965(3) 0.3270(3) 0.7971(3) 0.0431(8) Uani 1 1 d . H10 H 0.8391 0.3164 0.7217 0.052 Uiso 1 1 calc R C11 C 0.8614(4) 0.3153(4) 0.8872(3) 0.0540(10) Uani 1 1 d . H11 H 0.9520 0.2952 0.8793 0.065 Uiso 1 1 calc R C12 C 0.7806(4) 0.3356(4) 0.9854(3) 0.0534(10) Uani 1 1 d . H12 H 0.8072 0.3312 1.0550 0.064 Uiso 1 1 calc R C13 C 0.4516(3) 0.1023(2) 0.7523(2) 0.0255(6) Uani 1 1 d . C14 C 0.5263(3) 0.0618(3) 0.6512(2) 0.0325(7) Uani 1 1 d . H14 H 0.4916 0.0767 0.5853 0.039 Uiso 1 1 calc R C15 C 0.6497(3) 0.0006(3) 0.6454(3) 0.0390(7) Uani 1 1 d . H15 H 0.6991 -0.0277 0.5762 0.047 Uiso 1 1 calc R C16 C 0.7012(3) -0.0194(3) 0.7403(3) 0.0457(8) Uani 1 1 d . H16 H 0.7865 -0.0617 0.7364 0.055 Uiso 1 1 calc R C17 C 0.6299(3) 0.0215(3) 0.8407(3) 0.0479(9) Uani 1 1 d . H17 H 0.6664 0.0081 0.9058 0.057 Uiso 1 1 calc R C18 C 0.5049(3) 0.0823(3) 0.8472(2) 0.0356(7) Uani 1 1 d . H18 H 0.4559 0.1102 0.9168 0.043 Uiso 1 1 calc R C19 C 0.2085(3) 0.0853(2) 0.7013(2) 0.0232(6) Uani 1 1 d . C20 C 0.0995(3) 0.1357(2) 0.6591(2) 0.0264(6) Uani 1 1 d . H20 H 0.0758 0.2226 0.6526 0.032 Uiso 1 1 calc R C21 C 0.0254(3) 0.0596(3) 0.6267(2) 0.0319(7) Uani 1 1 d . H21 H -0.0502 0.0945 0.5999 0.038 Uiso 1 1 calc R C22 C 0.0609(3) -0.0665(3) 0.6332(2) 0.0334(7) Uani 1 1 d . H22 H 0.0104 -0.1184 0.6103 0.040 Uiso 1 1 calc R C23 C 0.1703(3) -0.1170(3) 0.6733(2) 0.0308(6) Uani 1 1 d . H23 H 0.1952 -0.2039 0.6772 0.037 Uiso 1 1 calc R C24 C 0.2436(3) -0.0423(2) 0.7075(2) 0.0272(6) Uani 1 1 d . H24 H 0.3182 -0.0778 0.7355 0.033 Uiso 1 1 calc R C25 C 0.2113(3) 0.2045(2) 0.8960(2) 0.0232(6) Uani 1 1 d . C26 C 0.1565(3) 0.1087(3) 0.9575(2) 0.0270(6) Uani 1 1 d . H26 H 0.1686 0.0307 0.9260 0.032 Uiso 1 1 calc R C27 C 0.0845(3) 0.1256(3) 1.0641(2) 0.0308(6) Uani 1 1 d . H27 H 0.0475 0.0596 1.1057 0.037 Uiso 1 1 calc R C28 C 0.0667(3) 0.2392(3) 1.1098(2) 0.0319(7) Uani 1 1 d . H28 H 0.0163 0.2514 1.1825 0.038 Uiso 1 1 calc R C29 C 0.1211(3) 0.3342(3) 1.0510(2) 0.0317(7) Uani 1 1 d . H29 H 0.1090 0.4117 1.0834 0.038 Uiso 1 1 calc R C30 C 0.1941(3) 0.3177(2) 0.9443(2) 0.0278(6) Uani 1 1 d . H30 H 0.2324 0.3837 0.9041 0.033 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 0.0254(2) 0.02418(18) 0.02261(18) -0.00052(12) -0.00305(14) -0.00257(14) S1 0.0432(5) 0.0299(4) 0.0304(4) -0.0006(3) 0.0038(3) 0.0071(4) S2 0.0344(5) 0.1029(8) 0.0306(4) -0.0076(4) -0.0076(4) -0.0053(5) P1 0.0206(4) 0.0223(3) 0.0210(3) -0.0015(2) -0.0042(3) -0.0015(3) O1 0.0228(12) 0.0501(13) 0.0343(11) -0.0075(9) -0.0049(9) -0.0050(10) N1 0.0358(17) 0.0359(14) 0.0373(15) -0.0014(11) -0.0090(12) 0.0014(12) N2 0.0248(13) 0.0241(11) 0.0233(11) -0.0003(8) -0.0050(10) -0.0045(10) N3 0.0195(13) 0.0253(12) 0.0257(12) 0.0003(9) -0.0048(9) -0.0041(10) N4 0.0196(13) 0.0349(13) 0.0292(12) -0.0039(9) -0.0065(10) -0.0026(10) C1 0.0195(15) 0.0262(14) 0.0366(16) -0.0081(11) -0.0021(12) -0.0001(12) C2 0.0341(18) 0.0316(15) 0.0307(15) -0.0017(11) -0.0119(13) -0.0052(13) C3 0.046(2) 0.0437(18) 0.0293(16) -0.0043(13) -0.0160(15) -0.0099(16) C4 0.060(2) 0.0367(17) 0.0234(15) -0.0035(12) -0.0098(15) -0.0099(16) C5 0.038(2) 0.0323(16) 0.0289(15) -0.0059(11) -0.0010(13) -0.0044(14) C6 0.0266(16) 0.0239(13) 0.0246(14) -0.0019(10) -0.0029(11) -0.0027(12) C7 0.0228(16) 0.0261(14) 0.0314(15) -0.0030(10) -0.0022(12) -0.0017(12) C8 0.0268(17) 0.0275(14) 0.0296(15) 0.0002(11) -0.0068(12) -0.0063(12) C9 0.0287(17) 0.0302(15) 0.0304(15) -0.0024(11) -0.0069(12) -0.0050(13) C10 0.0305(19) 0.062(2) 0.0355(17) -0.0083(15) -0.0101(14) 0.0047(17) C11 0.033(2) 0.084(3) 0.045(2) -0.0112(18) -0.0190(17) 0.007(2) C12 0.041(2) 0.082(3) 0.040(2) -0.0041(17) -0.0209(17) 0.000(2) C13 0.0222(15) 0.0238(13) 0.0293(14) 0.0010(10) -0.0047(11) -0.0018(11) C14 0.0317(18) 0.0299(15) 0.0326(16) -0.0007(11) -0.0025(13) -0.0005(13) C15 0.0293(19) 0.0334(17) 0.0464(19) -0.0003(13) 0.0059(14) -0.0001(14) C16 0.0205(18) 0.046(2) 0.063(2) 0.0100(16) -0.0037(16) 0.0018(15) C17 0.033(2) 0.063(2) 0.046(2) 0.0142(16) -0.0170(16) -0.0006(17) C18 0.0272(18) 0.0463(18) 0.0314(16) 0.0066(13) -0.0072(13) -0.0029(14) C19 0.0239(15) 0.0258(14) 0.0195(13) -0.0027(10) -0.0021(11) -0.0048(11) C20 0.0271(16) 0.0277(14) 0.0232(14) -0.0021(10) -0.0038(11) -0.0022(12) C21 0.0306(18) 0.0395(17) 0.0276(15) -0.0028(12) -0.0085(12) -0.0075(14) C22 0.0351(19) 0.0401(17) 0.0270(15) -0.0093(12) -0.0006(13) -0.0151(14) C23 0.0334(18) 0.0245(14) 0.0327(15) -0.0071(11) 0.0014(13) -0.0068(13) C24 0.0256(16) 0.0260(14) 0.0292(14) -0.0019(10) -0.0041(12) -0.0033(12) C25 0.0207(15) 0.0294(14) 0.0193(13) -0.0007(10) -0.0064(11) -0.0010(11) C26 0.0273(16) 0.0293(14) 0.0251(14) -0.0021(10) -0.0065(12) -0.0041(12) C27 0.0265(17) 0.0384(16) 0.0270(15) 0.0043(11) -0.0051(12) -0.0063(13) C28 0.0303(18) 0.0452(17) 0.0188(13) -0.0045(11) -0.0035(12) -0.0024(14) C29 0.0356(19) 0.0360(16) 0.0243(14) -0.0077(11) -0.0059(13) -0.0046(14) C30 0.0282(17) 0.0302(15) 0.0260(14) -0.0027(11) -0.0041(12) -0.0080(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P1 Cu1 S1 117.60(3) N2 Cu1 S1 107.38(7) N2 Cu1 P1 117.49(6) N2 Cu1 N3 77.64(9) N3 Cu1 S1 127.28(6) N3 Cu1 P1 103.74(6) C1 S1 Cu1 102.46(10) C12 S2 C9 91.99(16) C13 P1 Cu1 112.32(9) C13 P1 C19 103.33(12) C13 P1 C25 106.63(12) C19 P1 Cu1 113.80(8) C25 P1 Cu1 117.45(9) C25 P1 C19 101.87(12) C2 N2 Cu1 126.4(2) C6 N2 Cu1 115.66(18) C6 N2 C2 118.0(2) N4 N3 Cu1 128.58(17) C7 N3 Cu1 112.19(18) C7 N3 N4 117.4(2) N3 N4 H4 120.7 N3 N4 C8 118.6(2) C8 N4 H4 120.7 N1 C1 S1 178.1(3) N2 C2 H2 118.6 N2 C2 C3 122.7(3) C3 C2 H2 118.6 C2 C3 H3 120.4 C4 C3 C2 119.1(3) C4 C3 H3 120.4 C3 C4 H4A 120.5 C3 C4 C5 119.0(3) C5 C4 H4A 120.5 C4 C5 H5 120.6 C4 C5 C6 118.7(3) C6 C5 H5 120.6 N2 C6 C5 122.4(3) N2 C6 C7 115.7(2) C5 C6 C7 121.8(3) N3 C7 C6 117.8(3) N3 C7 H7 121.1 C6 C7 H7 121.1 O1 C8 N4 122.9(3) O1 C8 C9 122.2(2) N4 C8 C9 114.9(3) C8 C9 S2 117.2(2) C10 C9 S2 110.6(2) C10 C9 C8 132.1(3) C9 C10 H10 123.5 C9 C10 C11 113.0(3) C11 C10 H10 123.5 C10 C11 H11 123.8 C12 C11 C10 112.4(3) C12 C11 H11 123.8 S2 C12 H12 124.0 C11 C12 S2 112.0(2) C11 C12 H12 124.0 C14 C13 P1 118.1(2) C14 C13 C18 118.7(3) C18 C13 P1 122.9(2) C13 C14 H14 119.5 C15 C14 C13 121.0(3) C15 C14 H14 119.5 C14 C15 H15 120.1 C14 C15 C16 119.8(3) C16 C15 H15 120.1 C15 C16 H16 119.9 C17 C16 C15 120.3(3) C17 C16 H16 119.9 C16 C17 H17 119.9 C18 C17 C16 120.2(3) C18 C17 H17 119.9 C13 C18 H18 120.0 C17 C18 C13 120.0(3) C17 C18 H18 120.0 C20 C19 P1 117.10(19) C20 C19 C24 119.1(2) C24 C19 P1 123.8(2) C19 C20 H20 119.9 C19 C20 C21 120.2(3) C21 C20 H20 119.9 C20 C21 H21 119.9 C22 C21 C20 120.2(3) C22 C21 H21 119.9 C21 C22 H22 120.1 C23 C22 C21 119.8(3) C23 C22 H22 120.1 C22 C23 H23 119.8 C22 C23 C24 120.4(3) C24 C23 H23 119.8 C19 C24 H24 119.9 C23 C24 C19 120.3(3) C23 C24 H24 119.9 C26 C25 P1 122.5(2) C26 C25 C30 118.8(2) C30 C25 P1 118.5(2) C25 C26 H26 119.7 C27 C26 C25 120.7(3) C27 C26 H26 119.7 C26 C27 H27 120.2 C26 C27 C28 119.6(3) C28 C27 H27 120.2 C27 C28 H28 119.7 C29 C28 C27 120.5(3) C29 C28 H28 119.7 C28 C29 H29 119.9 C28 C29 C30 120.2(3) C30 C29 H29 119.9 C25 C30 H30 119.9 C29 C30 C25 120.2(3) C29 C30 H30 119.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cu1 S1 2.2936(8) Cu1 P1 2.1989(7) Cu1 N2 2.050(2) Cu1 N3 2.181(2) S1 C1 1.661(3) S2 C9 1.711(3) S2 C12 1.696(4) P1 C13 1.819(3) P1 C19 1.822(3) P1 C25 1.820(3) O1 C8 1.219(3) N1 C1 1.157(3) N2 C2 1.338(3) N2 C6 1.347(4) N3 N4 1.367(3) N3 C7 1.285(3) N4 H4 0.8800 N4 C8 1.369(3) C2 H2 0.9500 C2 C3 1.385(4) C3 H3 0.9500 C3 C4 1.372(5) C4 H4A 0.9500 C4 C5 1.387(4) C5 H5 0.9500 C5 C6 1.387(4) C6 C7 1.465(4) C7 H7 0.9500 C8 C9 1.472(4) C9 C10 1.353(4) C10 H10 0.9500 C10 C11 1.411(4) C11 H11 0.9500 C11 C12 1.341(5) C12 H12 0.9500 C13 C14 1.392(4) C13 C18 1.387(4) C14 H14 0.9500 C14 C15 1.374(4) C15 H15 0.9500 C15 C16 1.376(4) C16 H16 0.9500 C16 C17 1.375(5) C17 H17 0.9500 C17 C18 1.387(4) C18 H18 0.9500 C19 C20 1.392(4) C19 C24 1.393(4) C20 H20 0.9500 C20 C21 1.386(4) C21 H21 0.9500 C21 C22 1.379(4) C22 H22 0.9500 C22 C23 1.383(4) C23 H23 0.9500 C23 C24 1.378(4) C24 H24 0.9500 C25 C26 1.390(4) C25 C30 1.395(4) C26 H26 0.9500 C26 C27 1.384(4) C27 H27 0.9500 C27 C28 1.383(4) C28 H28 0.9500 C28 C29 1.368(4) C29 H29 0.9500 C29 C30 1.388(4) 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 -60.5(2) Cu1 P1 C13 C18 113.5(2) Cu1 P1 C19 C20 -39.1(2) Cu1 P1 C19 C24 143.6(2) Cu1 P1 C25 C26 155.3(2) Cu1 P1 C25 C30 -19.6(3) Cu1 N2 C2 C3 -178.6(2) Cu1 N2 C6 C5 178.4(2) Cu1 N2 C6 C7 -1.4(3) Cu1 N3 N4 C8 -13.8(3) Cu1 N3 C7 C6 10.4(3) S2 C9 C10 C11 1.2(4) P1 C13 C14 C15 175.7(2) P1 C13 C18 C17 -174.8(3) P1 C19 C20 C21 -175.8(2) P1 C19 C24 C23 176.7(2) P1 C25 C26 C27 -173.9(2) P1 C25 C30 C29 173.8(2) O1 C8 C9 S2 2.4(4) O1 C8 C9 C10 -176.3(3) N2 C2 C3 C4 0.1(4) N2 C6 C7 N3 -6.5(4) N3 N4 C8 O1 -5.5(4) N3 N4 C8 C9 174.3(2) N4 N3 C7 C6 176.2(2) N4 C8 C9 S2 -177.39(19) N4 C8 C9 C10 3.9(5) C2 N2 C6 C5 -1.4(4) C2 N2 C6 C7 178.7(2) C2 C3 C4 C5 -1.3(4) C3 C4 C5 C6 1.1(4) C4 C5 C6 N2 0.3(4) C4 C5 C6 C7 -179.9(3) C5 C6 C7 N3 173.7(2) C6 N2 C2 C3 1.3(4) C7 N3 N4 C8 -177.0(2) C8 C9 C10 C11 179.9(3) C9 S2 C12 C11 0.9(3) C9 C10 C11 C12 -0.6(5) C10 C11 C12 S2 -0.4(5) C12 S2 C9 C8 179.9(2) C12 S2 C9 C10 -1.2(3) C13 P1 C19 C20 -161.2(2) C13 P1 C19 C24 21.5(3) C13 P1 C25 C26 -77.7(3) C13 P1 C25 C30 107.4(2) C13 C14 C15 C16 -1.0(5) C14 C13 C18 C17 -0.9(4) C14 C15 C16 C17 0.0(5) C15 C16 C17 C18 0.6(5) C16 C17 C18 C13 -0.2(5) C18 C13 C14 C15 1.5(4) C19 P1 C13 C14 62.6(2) C19 P1 C13 C18 -123.4(2) C19 P1 C25 C26 30.3(3) C19 P1 C25 C30 -144.7(2) C19 C20 C21 C22 -1.7(4) C20 C19 C24 C23 -0.6(4) C20 C21 C22 C23 0.6(4) C21 C22 C23 C24 0.5(4) C22 C23 C24 C19 -0.5(4) C24 C19 C20 C21 1.7(4) C25 P1 C13 C14 169.5(2) C25 P1 C13 C18 -16.5(3) C25 P1 C19 C20 88.3(2) C25 P1 C19 C24 -89.0(2) C25 C26 C27 C28 0.2(4) C26 C25 C30 C29 -1.3(4) C26 C27 C28 C29 -0.9(4) C27 C28 C29 C30 0.5(5) C28 C29 C30 C25 0.6(4) C30 C25 C26 C27 1.0(4)