#------------------------------------------------------------------------------ #$Date: 2019-12-04 09:39:12 +0200 (Wed, 04 Dec 2019) $ #$Revision: 244897 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556425.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_1556425 loop_ _publ_author_name 'Rancan, M.' 'Carlotto, A.' 'Bottaro, G.' 'Armelao, L.' _publ_section_title ; Effect of Coordinating Solvents on the Structure of Cu(II)-4,4'-bipyridine Coordination Polymers ; _journal_name_full Inorganics _journal_page_first 103 _journal_paper_doi 10.3390/inorganics7080103 _journal_volume 7 _journal_year 2019 _chemical_formula_moiety 'C20 H34 Cu N4 O4 S2, 2(Cl O4)' _chemical_formula_sum 'C20 H34 Cl2 Cu N4 O12 S2' _chemical_formula_weight 721.07 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _cell_angle_alpha 90 _cell_angle_beta 100.154(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.9524(17) _cell_length_b 11.0913(7) _cell_length_c 16.3512(15) _cell_measurement_reflns_used 3574 _cell_measurement_temperature 299.6(6) _cell_measurement_theta_max 27.3020 _cell_measurement_theta_min 2.4620 _cell_volume 3204.8(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment air _diffrn_ambient_temperature 299.6(6) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1274 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -54.00 44.00 0.50 10.00 -- 18.52 -38.00 150.00 196 2 \w -52.00 49.00 0.50 10.00 -- 18.52 -77.00 -90.00 202 3 \w -12.00 89.00 0.50 10.00 -- 18.52 77.00 30.00 202 4 \w -26.00 91.00 0.50 10.00 -- 18.52 19.00 -60.00 234 5 \w -73.00 -35.00 0.50 10.00 -- -18.60 121.00 0.00 76 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0049725000 _diffrn_orient_matrix_UB_12 0.0484797000 _diffrn_orient_matrix_UB_13 -0.0286476000 _diffrn_orient_matrix_UB_21 0.0004615000 _diffrn_orient_matrix_UB_22 -0.0411596000 _diffrn_orient_matrix_UB_23 -0.0331333000 _diffrn_orient_matrix_UB_31 -0.0398572000 _diffrn_orient_matrix_UB_32 -0.0066054000 _diffrn_orient_matrix_UB_33 -0.0046070000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_unetI/netI 0.0269 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 13522 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.230 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 1.494 _exptl_crystal_description needle _exptl_crystal_F_000 1492 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.352 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.054 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 229 _refine_ls_number_reflns 3287 _refine_ls_number_restraints 101 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0340 _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^)+(0.0426P)^2^+3.0618P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.0902 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2795 _reflns_number_total 3287 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 6.cif _cod_data_source_block 6 _cod_database_code 1556425 _chemical_oxdiff_formula 'Cu1 N2 C10 H10 Cl2 O8' _chemical_oxdiff_usercomment 'cristallo azzurro chiaro da MR100, dopo un mese, DMF+ DMSO vap Et2O' _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 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O6B-O3B \\sim O6B-O4B \\sim O6B-O5B \\sim O4A-O5A \\sim O4A-O3A \\sim O4A-O6A \\sim O5A-O3A with sigma of 0.04 Cl1-O6B \\sim Cl1-O4A \\sim Cl1-O5A \\sim Cl1-O3B \\sim Cl1-O3A \\sim Cl1-O4B \\sim Cl1-O6A \\sim Cl1-O5B with sigma of 0.02 3. Rigid body (RIGU) restrains O4A, Cl1, O6B, O4B, O3B, O5A, O6A, O3A, O5B with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.004 4. Others Sof(O5B)=Sof(O6B)=Sof(O4B)=Sof(O3B)=1-FVAR(1) Sof(O6A)=Sof(O3A)=Sof(O5A)=Sof(O4A)=FVAR(1) 5.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C9(H9), C5(H5), C6(H6) 5.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C) ; _shelx_res_file ; TITL 6.res in I2/a 6.res created by SHELXL-2018/3 at 14:38:18 on 18-Jul-2019 REM Old TITL 6 in I2/a REM SHELXT solution in I2/a REM R1 0.172, Rweak 0.135, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C30 N2 O6A Cl4 Cu CELL 0.71073 17.9524 11.0913 16.3512 90 100.154 90 ZERR 4 0.0017 0.0007 0.0015 0 0.008 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Cl Cu N O S UNIT 80 136 8 4 16 48 8 SADI 0.04 O6B O3B O6B O4B O6B O5B O4A O5A O4A O3A O4A O6A O5A O3A SADI Cl1 O6B Cl1 O4A Cl1 O5A Cl1 O3B Cl1 O3A Cl1 O4B Cl1 O6A Cl1 O5B RIGU 0.003 0.004 O4A Cl1 O6B O4B O3B O5A O6A O3A O5B L.S. 50 PLAN 20 BOND $H list 4 MORE -1 CONF fmap 2 ACTA REM REM REM WGHT 0.042600 3.061800 FVAR 0.18771 0.37923 CU1 4 0.750000 0.286591 0.500000 10.50000 0.04751 0.01248 = 0.03649 0.00000 0.01001 0.00000 S1 7 0.624765 0.311908 0.343789 11.00000 0.06319 0.04293 = 0.04287 -0.00334 0.00217 0.00128 CL1 3 0.612695 0.651574 0.728412 11.00000 0.06992 0.07214 = 0.05851 -0.00229 0.02274 -0.00614 O1 6 0.708039 0.283556 0.377544 11.00000 0.05931 0.02736 = 0.04066 -0.00397 0.00751 -0.00225 N1 5 0.750000 0.467257 0.500000 10.50000 0.03809 0.01700 = 0.03539 0.00000 0.00965 0.00000 N2 5 0.750000 1.105876 0.500000 10.50000 0.05069 0.01563 = 0.04164 0.00000 0.01695 0.00000 O2 6 0.626938 0.270453 0.532163 11.00000 0.05220 0.05048 = 0.07457 0.00207 0.02556 0.00436 C3 1 0.750000 0.720479 0.500000 10.50000 0.03119 0.01762 = 0.03632 0.00000 0.00790 0.00000 C4 1 0.750000 0.853953 0.500000 10.50000 0.03462 0.01755 = 0.03586 0.00000 0.00958 0.00000 N3 5 0.508447 0.301717 0.555439 11.00000 0.04535 0.06122 = 0.05393 0.00420 0.01121 -0.00516 C1 1 0.741723 0.531214 0.568300 11.00000 0.04912 0.02100 = 0.03386 0.00301 0.01437 0.00153 AFIX 43 H1 2 0.735087 0.489426 0.615801 11.00000 -1.20000 AFIX 0 C2 1 0.742667 0.654678 0.570709 11.00000 0.04749 0.02034 = 0.03322 -0.00159 0.01302 0.00088 AFIX 43 H2 2 0.738403 0.694655 0.619667 11.00000 -1.20000 AFIX 0 C9 1 0.578979 0.333234 0.555713 11.00000 0.04739 0.04483 = 0.05154 0.00650 0.00912 0.00330 AFIX 43 H9 2 0.593650 0.409786 0.575499 11.00000 -1.20000 AFIX 0 C5 1 0.726478 0.919551 0.563253 11.00000 0.07600 0.01973 = 0.04376 0.00066 0.03151 -0.00144 AFIX 43 H5 2 0.709971 0.879823 0.606860 11.00000 -1.20000 AFIX 0 C6 1 0.727716 1.043177 0.561077 11.00000 0.07827 0.01944 = 0.04681 -0.00264 0.03321 0.00042 AFIX 43 H6 2 0.712264 1.085396 0.604302 11.00000 -1.20000 AFIX 0 PART 2 O5B 6 0.670201 0.561101 0.731705 -21.00000 0.13587 0.11874 = 0.09496 0.03176 0.07391 0.05997 PART 0 C10 1 0.454147 0.384606 0.581162 11.00000 0.05328 0.09294 = 0.09981 0.01421 0.02334 0.01818 AFIX 137 H10A 2 0.479377 0.458027 0.600986 11.00000 -1.50000 H10B 2 0.432304 0.348486 0.624783 11.00000 -1.50000 H10C 2 0.414933 0.401996 0.534690 11.00000 -1.50000 AFIX 0 PART 2 O6B 6 0.566699 0.614528 0.656973 -21.00000 0.13500 0.13109 = 0.15792 -0.05275 -0.02415 -0.01495 O4B 6 0.632298 0.770233 0.718220 -21.00000 0.18827 0.07295 = 0.16155 -0.00291 0.08618 -0.03073 O3B 6 0.559847 0.631181 0.778175 -21.00000 0.14836 0.13937 = 0.19676 0.05607 0.13558 0.03635 PART 0 C8 1 0.582173 0.170320 0.317690 11.00000 0.08238 0.06753 = 0.11844 -0.02431 -0.00314 -0.02542 AFIX 137 H8A 2 0.610281 0.127673 0.282053 11.00000 -1.50000 H8B 2 0.531097 0.181921 0.289414 11.00000 -1.50000 H8C 2 0.581983 0.124387 0.367415 11.00000 -1.50000 AFIX 0 C11 1 0.480621 0.184987 0.523268 11.00000 0.07946 0.09025 = 0.08494 -0.01280 0.02039 -0.03571 AFIX 137 H11A 2 0.450892 0.194885 0.468835 11.00000 -1.50000 H11B 2 0.449898 0.150136 0.559579 11.00000 -1.50000 H11C 2 0.522681 0.132793 0.520129 11.00000 -1.50000 AFIX 0 C7 1 0.627827 0.368049 0.242548 11.00000 0.12097 0.13910 = 0.05352 0.03349 -0.01118 -0.01253 AFIX 137 H7A 2 0.652352 0.445279 0.246843 11.00000 -1.50000 H7B 2 0.577216 0.376250 0.212151 11.00000 -1.50000 H7C 2 0.655565 0.312922 0.214003 11.00000 -1.50000 AFIX 0 PART 1 O6A 6 0.578292 0.652674 0.644180 21.00000 0.11113 0.17585 = 0.05568 -0.00089 -0.00852 0.00322 O3A 6 0.586379 0.636608 0.803876 21.00000 0.27801 0.11359 = 0.10559 0.02057 0.13154 0.07078 O5A 6 0.679733 0.589131 0.749157 21.00000 0.07348 0.25566 = 0.09986 0.06293 -0.00675 0.03196 O4A 6 0.640288 0.766486 0.744225 21.00000 0.18024 0.14840 = 0.17030 -0.08298 0.02335 -0.09616 HKLF 4 REM 6.res in I2/a REM wR2 = 0.0902, GooF = S = 1.035, Restrained GooF = 1.061 for all data REM R1 = 0.0340 for 2795 Fo > 4sig(Fo) and 0.0427 for all 3287 data REM 229 parameters refined using 101 restraints END WGHT 0.0417 3.1233 REM Highest difference peak 0.352, deepest hole -0.323, 1-sigma level 0.054 Q1 1 0.5559 0.2646 0.5694 11.00000 0.05 0.35 Q2 1 0.6158 0.5590 0.6747 11.00000 0.05 0.30 Q3 1 0.5419 0.5822 0.7654 11.00000 0.05 0.26 Q4 1 0.6597 0.6427 0.8136 11.00000 0.05 0.26 Q5 1 0.5518 0.7007 0.7746 11.00000 0.05 0.25 Q6 1 0.7213 0.8869 0.5205 11.00000 0.05 0.24 Q7 1 0.6630 0.2873 0.2782 11.00000 0.05 0.24 Q8 1 0.5353 0.6883 0.7691 11.00000 0.05 0.24 Q9 1 0.7581 0.5027 0.5358 11.00000 0.05 0.23 Q10 1 0.6077 0.7237 0.7278 11.00000 0.05 0.23 Q11 1 0.6809 0.2940 0.3598 11.00000 0.05 0.22 Q12 1 0.6059 0.3100 0.4988 11.00000 0.05 0.21 Q13 1 0.5985 0.6153 0.8276 11.00000 0.05 0.21 Q14 1 0.7688 0.9060 0.5585 11.00000 0.05 0.21 Q15 1 0.5584 0.6228 0.7313 11.00000 0.05 0.21 Q16 1 0.6222 0.2400 0.3401 11.00000 0.05 0.21 Q17 1 0.6498 0.6920 0.7983 11.00000 0.05 0.20 Q18 1 0.6902 0.3154 0.5125 11.00000 0.05 0.20 Q19 1 0.6743 0.6600 0.7368 11.00000 0.05 0.20 Q20 1 0.8050 0.2817 0.5083 11.00000 0.05 0.19 ; _shelx_res_checksum 98099 _shelx_hkl_file ; 0 0 2 329.68 6.42 0 0 2 339.28 6.29 0 0 -2 340.27 6.39 0 0 4 3265.41 57.45 0 0 4 3244.26 57.08 0 0 -4 3366.73 57.37 0 0 -4 3396.38 57.18 0 0 -6 2.56 0.58 0 0 6 2.40 0.50 0 0 -6 2.81 0.66 0 0 6 2.79 0.69 0 0 6 2.25 0.51 0 0 -8 380.49 9.05 0 0 8 352.09 8.57 0 0 8 364.85 9.03 0 0 -10 74.78 3.67 0 0 10 75.54 3.68 0 0 10 71.77 3.35 0 0 12 257.45 7.82 0 0 12 269.76 8.48 0 0 14 301.66 9.73 0 0 -14 303.14 9.72 0 0 14 299.17 8.99 0 0 16 57.67 4.14 0 0 -16 60.29 4.23 0 0 16 59.64 3.83 0 0 18 109.97 6.18 0 0 -18 107.51 6.10 0 0 20 6.82 1.89 0 0 20 9.33 2.13 0 0 -20 9.99 2.09 0 -1 1 491.25 8.72 0 -1 1 490.52 8.95 0 -1 -1 506.72 8.96 0 1 3 101.73 2.69 0 -1 3 97.21 2.65 0 -1 -3 101.45 2.67 0 1 -3 99.14 2.71 0 -1 3 97.35 2.69 0 -1 -5 10.53 0.98 0 1 5 11.88 1.08 0 1 -5 10.15 0.94 0 -1 -5 10.15 0.88 0 1 -5 11.23 0.99 0 1 5 11.60 0.99 0 -1 5 10.17 1.07 0 -1 5 12.25 1.04 0 -1 7 1.56 0.67 0 1 -7 2.91 0.80 0 1 7 3.15 0.76 0 -1 7 1.52 0.62 0 1 -7 2.42 0.64 0 -1 -7 2.06 0.64 0 1 7 2.98 0.88 0 -1 -7 2.85 0.68 0 1 -9 11.18 1.41 0 1 9 9.18 1.35 0 -1 9 9.62 1.25 0 1 9 11.54 1.27 0 -1 -9 10.59 1.36 0 -1 9 9.11 1.30 0 1 11 13.70 1.56 0 1 -11 14.33 1.74 0 -1 11 15.96 1.66 0 1 11 13.24 1.74 0 -1 -11 16.20 1.80 0 -1 11 16.01 1.87 0 -1 13 91.64 4.36 0 1 13 94.26 4.78 0 -1 -13 99.84 4.84 0 1 13 94.08 4.30 0 -1 13 92.46 4.80 0 1 -13 93.66 4.73 0 -1 15 0.06 0.80 0 -1 15 1.57 1.17 0 1 -15 2.95 1.42 0 1 15 2.19 1.21 0 -1 -15 -0.20 0.91 0 -1 -17 1.59 1.01 0 -1 17 2.51 1.21 0 1 17 0.40 1.09 0 1 17 -1.37 1.33 0 1 -17 1.26 1.04 0 -1 17 1.94 1.07 0 -1 19 0.93 1.21 0 1 19 -0.60 1.21 0 -1 -19 1.73 1.33 0 -1 19 -1.75 1.16 0 1 19 2.06 1.45 0 1 -19 1.17 1.31 0 2 0 5170.96 87.01 0 -2 0 5184.65 86.91 0 -2 -2 76.79 2.25 0 2 -2 82.96 2.11 0 2 2 83.84 2.22 0 -2 -2 84.33 2.45 0 -2 -2 77.91 2.15 0 -2 2 80.71 2.44 0 -2 2 80.69 2.15 0 2 -4 306.82 6.70 0 2 -4 303.88 6.95 0 -2 -4 311.46 6.81 0 -2 4 307.49 6.91 0 2 -4 324.67 6.94 0 -2 -4 315.16 6.89 0 2 4 309.96 6.79 0 -2 4 310.21 6.78 0 2 4 318.21 6.93 0 -2 -6 918.54 17.50 0 -2 6 865.37 17.41 0 2 -6 914.05 17.41 0 -2 -6 917.07 17.34 0 2 -6 885.31 17.36 0 -2 6 910.99 17.49 0 2 6 888.72 17.45 0 -2 -6 888.94 17.51 0 2 -6 894.16 17.58 0 2 8 395.41 9.78 0 2 -8 405.58 9.83 0 -2 -8 421.42 9.83 0 -2 8 412.62 9.80 0 -2 8 417.90 9.92 0 -2 10 9.60 1.45 0 -2 -10 8.70 1.37 0 -2 10 7.59 1.39 0 2 10 7.33 1.32 0 2 -10 9.41 1.37 0 2 12 19.72 2.15 0 -2 12 20.48 2.00 0 2 -12 18.55 2.05 0 -2 12 21.98 2.25 0 -2 -12 21.39 2.19 0 -2 14 26.10 2.66 0 2 14 23.65 2.65 0 2 14 21.12 2.43 0 2 -14 26.56 2.63 0 -2 -14 29.15 2.71 0 -2 14 26.91 2.39 0 2 16 1.58 1.25 0 2 16 -0.48 1.01 0 -2 16 -0.23 1.02 0 -2 -16 0.52 0.93 0 -2 16 -3.17 1.47 0 2 -16 0.31 0.90 0 2 -18 17.53 2.61 0 -2 -18 17.08 2.59 0 2 18 16.99 2.63 0 -2 18 16.91 2.55 0 -2 18 19.26 2.46 0 2 18 16.66 2.54 0 3 1 1180.06 20.79 0 -3 1 1167.07 20.59 0 3 -1 1194.17 20.74 0 -3 1 1173.29 20.73 0 -3 -1 1188.07 20.73 0 3 -3 26.49 1.20 0 -3 3 23.87 1.28 0 3 3 25.93 1.35 0 -3 -3 25.15 1.49 0 -3 3 25.43 1.55 0 -3 -3 25.45 1.25 0 -3 5 45.53 2.15 0 -3 -5 48.53 2.17 0 -3 5 43.37 2.22 0 3 -5 49.46 2.10 0 3 -5 53.42 2.32 0 -3 -5 48.83 2.26 0 3 5 48.83 2.18 0 3 5 46.02 2.23 0 3 -7 47.68 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-3 17.64 2.77 18 -3 3 14.48 2.44 18 3 5 11.65 1.86 18 -3 5 6.97 1.74 -18 3 -5 8.22 2.23 -18 -3 -5 11.82 2.54 18 3 7 2.27 1.15 18 -3 7 1.32 1.21 -18 3 -7 1.32 1.55 -18 -3 -7 -1.77 1.83 18 -4 -12 -0.35 0.88 -18 4 12 -2.11 1.38 -18 -4 12 0.50 1.12 -18 4 10 2.51 1.56 -18 -4 10 -1.11 1.08 -18 -4 8 1.55 0.95 -18 4 8 1.99 1.46 -18 -4 6 -0.02 0.78 -18 4 6 0.97 1.23 -18 4 4 10.32 2.03 18 -4 -2 -1.85 1.40 -18 4 2 1.34 1.11 -18 4 0 17.52 2.61 -18 -4 0 13.32 2.35 18 -4 0 13.73 2.39 -18 4 0 14.59 2.40 -18 4 -2 2.66 1.41 -18 -4 -2 0.18 1.13 18 -4 2 1.97 1.32 -18 4 -4 14.75 2.62 -18 -4 -4 12.67 2.55 18 -4 4 9.91 2.14 18 -4 6 2.43 1.40 -18 4 -6 1.78 1.56 -18 -4 -6 2.43 1.63 -18 -5 11 6.58 1.75 -18 5 11 5.16 1.85 -18 -5 9 12.99 2.11 -18 5 9 16.90 2.81 -18 -5 7 16.75 2.23 -18 5 7 19.36 2.89 -18 -5 5 0.54 0.97 -18 5 5 -0.31 1.14 -18 5 3 8.81 2.06 18 -5 -1 32.01 3.45 -18 5 1 26.64 3.22 -18 5 -1 4.62 1.75 -18 -5 -1 4.44 1.43 -18 5 -3 28.53 3.42 -18 -5 -3 28.70 3.34 18 -5 3 28.82 3.29 -18 5 -5 23.64 3.15 18 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0 -7 -0.97 1.49 -19 -1 12 0.32 1.09 -19 1 12 -0.08 1.11 -19 -1 10 -0.27 1.03 -19 1 10 0.63 1.20 -19 -1 8 37.82 3.57 -19 1 8 33.80 3.59 -19 -1 6 0.77 0.99 -19 1 6 0.26 1.09 19 1 -4 16.31 2.20 -19 -1 4 19.38 2.45 -19 1 4 19.73 2.70 19 1 -2 4.03 1.28 19 -1 -2 1.28 1.07 -19 1 2 3.95 1.46 -19 1 0 -0.56 1.30 -19 -1 0 -1.34 1.55 19 1 0 1.29 0.86 19 -1 0 1.59 1.14 -19 1 -2 -0.43 1.22 -19 -1 -2 0.56 1.22 19 -1 2 -0.55 1.05 19 1 4 27.19 2.89 19 -1 4 23.14 2.84 -19 1 -4 21.77 3.18 -19 -1 -4 22.50 3.27 19 1 6 2.64 1.30 19 -1 6 3.98 1.82 -19 1 -6 3.17 1.80 -19 -1 -6 0.56 1.44 -19 -2 13 2.28 1.47 -19 -2 13 4.77 1.77 -19 2 13 5.09 1.91 -19 -2 11 4.25 1.54 -19 -2 11 5.46 1.70 -19 2 11 2.11 1.49 -19 -2 9 17.58 2.51 -19 2 9 17.05 2.80 -19 -2 9 14.72 2.28 -19 -2 7 0.45 0.83 -19 2 7 3.62 1.59 -19 -2 7 2.34 0.99 -19 -2 5 4.89 1.39 -19 2 5 3.62 1.42 19 2 -3 11.90 1.86 -19 2 3 13.24 2.37 -19 2 1 -0.35 1.20 -19 -2 1 -1.54 1.34 19 2 -1 1.13 0.77 19 -2 -1 0.07 0.96 -19 2 1 0.36 0.91 19 2 1 0.44 0.89 -19 2 -1 -2.13 1.48 -19 -2 -1 -1.49 1.54 19 -2 1 -0.71 1.14 19 2 3 -0.80 0.98 -19 2 -3 -0.58 1.28 19 -2 3 0.97 1.26 19 2 5 9.53 1.87 19 -2 5 9.16 2.00 -19 2 -5 11.38 2.61 -19 -2 -5 11.14 2.41 19 2 7 -1.10 1.22 19 -2 7 -0.25 1.18 -19 2 -7 0.31 1.52 -19 -2 -7 -2.34 1.77 -19 3 12 2.07 1.66 -19 -3 12 -0.51 1.07 -19 3 10 6.10 1.92 -19 -3 10 7.32 1.81 -19 3 8 1.12 1.26 -19 -3 8 0.13 0.97 -19 -3 6 0.20 0.83 -19 3 6 1.17 1.26 -19 -3 6 2.05 0.97 19 3 -4 1.91 0.99 -19 3 4 2.44 1.42 19 3 -2 0.90 0.84 19 -3 -2 0.60 1.09 19 3 0 -0.73 0.86 -19 3 0 -0.78 1.24 -19 -3 0 -3.13 1.74 19 -3 0 -1.58 1.10 19 3 2 4.29 1.24 -19 3 -2 7.23 1.94 -19 -3 -2 6.49 1.89 19 -3 2 7.27 1.84 19 3 4 6.30 1.54 -19 3 -4 3.18 1.77 -19 -3 -4 5.28 1.91 19 -3 4 6.28 1.87 19 3 6 2.98 1.23 19 -3 6 1.67 1.39 -19 3 -6 0.09 1.43 -19 -3 -6 -1.53 1.54 -19 4 11 2.03 1.73 -19 -4 11 -0.63 1.08 -19 4 9 24.39 3.30 -19 -4 9 14.80 2.22 -19 4 7 2.44 1.24 -19 -4 7 4.01 1.33 -19 4 5 0.40 1.19 -19 4 3 15.59 2.59 19 -4 -1 -0.25 1.17 -19 4 1 3.33 1.59 -19 4 -1 1.38 1.23 -19 -4 -1 0.91 1.11 19 -4 1 0.80 1.20 -19 4 -3 6.42 2.11 -19 -4 -3 4.30 1.67 19 -4 3 4.15 1.72 19 -4 5 5.53 1.79 -19 -4 -5 9.05 2.28 -19 -5 10 7.57 1.92 -19 5 10 8.03 2.12 -19 -5 8 -2.54 1.29 -19 5 8 0.36 1.24 -19 5 6 9.48 2.15 -19 5 4 -2.31 1.54 19 -5 -2 1.36 1.32 -19 5 2 5.27 1.82 -19 5 0 -0.91 1.23 -19 -5 0 -2.71 1.60 19 -5 0 -0.36 1.13 -19 5 -2 5.12 1.74 -19 -5 -2 9.70 2.14 19 -5 2 8.96 1.97 -19 5 -4 1.60 1.44 -19 -5 -4 2.41 1.51 19 -5 4 2.06 1.45 -19 -6 9 7.93 1.80 -19 6 9 7.41 2.15 -19 6 7 12.65 2.50 -19 6 5 4.76 1.59 19 -6 -3 12.63 2.47 -19 6 3 11.30 2.40 19 -6 -1 8.05 2.09 -19 6 1 6.34 1.92 -19 6 -1 1.75 1.16 -19 -6 -1 1.69 1.27 19 -6 1 3.10 1.57 -19 6 -3 10.45 2.23 -19 -6 -3 5.55 1.68 19 -6 3 10.41 2.30 -19 7 6 4.51 1.88 -19 7 4 1.73 1.41 19 -7 -2 2.09 1.36 -19 7 2 4.40 1.72 19 -7 0 1.57 1.25 -20 0 12 9.74 2.31 -20 0 10 88.33 6.03 -20 0 8 12.50 2.35 -20 0 6 14.70 2.37 20 0 -4 2.81 1.08 -20 0 4 5.13 1.65 20 0 -2 21.71 2.60 -20 0 0 0.10 1.41 20 0 0 4.88 1.47 20 0 2 35.00 3.34 -20 0 -2 29.35 3.67 20 0 4 29.89 3.15 -20 0 -4 33.17 3.98 -20 -1 11 3.15 1.50 -20 1 11 2.76 1.62 -20 -1 9 -1.85 1.34 -20 1 9 -0.37 1.07 -20 -1 7 4.71 1.53 -20 1 7 4.59 1.63 -20 -1 5 0.06 0.91 -20 1 5 0.22 1.06 20 1 -3 0.30 0.90 20 -1 -3 -0.56 1.10 -20 1 3 1.07 1.15 -20 1 1 7.66 1.99 -20 -1 1 4.03 1.46 20 1 -1 6.55 1.59 20 -1 -1 5.81 1.56 -20 1 -1 -0.50 1.20 -20 -1 -1 -2.56 1.65 20 -1 1 -2.26 1.30 20 1 3 12.40 2.08 20 -1 3 9.00 1.97 -20 1 -3 7.84 2.26 -20 -1 -3 10.46 2.44 20 1 5 4.03 1.56 20 -1 5 0.13 1.11 -20 1 -5 1.90 1.66 -20 -1 -5 -1.25 1.50 -20 -2 10 7.06 1.83 -20 -2 10 5.26 1.57 -20 2 10 4.20 1.71 -20 -2 8 4.30 1.34 -20 -2 8 3.52 1.40 -20 2 8 3.17 1.50 -20 -2 6 4.61 1.48 -20 2 6 4.65 1.57 20 2 -4 7.27 1.51 -20 2 4 7.29 1.92 20 2 -2 4.38 1.32 20 -2 -2 4.49 1.55 -20 2 2 7.30 1.88 20 2 0 0.83 0.84 -20 2 0 -0.38 1.32 -20 -2 0 2.74 1.47 20 -2 0 -0.61 1.07 20 2 2 3.97 1.28 -20 2 -2 7.68 2.13 -20 -2 -2 4.88 1.83 20 -2 2 3.59 1.50 20 2 4 4.45 1.34 20 -2 4 6.62 1.88 -20 2 -4 6.06 1.92 -20 -2 -4 5.98 2.08 -20 3 11 -0.57 1.26 -20 -3 11 2.21 1.25 -20 3 9 12.63 2.57 -20 -3 9 8.12 1.80 -20 3 7 3.67 1.64 -20 3 5 9.69 2.11 20 3 -3 -0.03 0.82 -20 3 3 -0.04 1.03 20 3 -1 4.08 1.26 20 -3 -1 5.38 1.71 20 3 1 1.89 1.04 -20 3 -1 1.50 1.45 -20 -3 -1 -1.17 1.39 20 -3 1 1.63 1.20 20 3 3 10.70 1.88 -20 3 -3 10.64 2.39 -20 -3 -3 11.81 2.41 20 -3 3 9.99 2.09 -20 4 10 2.82 1.63 -20 -4 10 -0.02 1.17 -20 4 8 12.08 2.51 -20 4 6 0.53 1.01 -20 4 4 7.53 2.00 20 -4 -2 -1.56 1.32 -20 4 2 -0.12 1.26 -20 4 0 0.45 1.20 -20 -4 0 -0.73 1.43 20 -4 0 1.11 1.20 -20 4 -2 2.40 1.59 -20 -4 -2 1.46 1.25 20 -4 2 2.89 1.51 -20 5 7 9.98 2.27 -20 5 5 19.19 2.97 20 -5 -3 15.03 2.63 -20 5 3 13.56 2.55 20 -5 -1 3.64 1.56 -20 5 1 6.18 1.98 -20 5 -1 5.43 1.85 -20 -5 -1 5.75 1.80 20 -5 1 8.57 2.06 -20 6 4 4.42 1.81 20 -6 -2 1.33 1.35 -20 6 2 2.70 1.74 -21 0 9 0.79 1.19 -21 0 7 -2.32 1.47 -21 0 5 -0.82 1.02 21 0 -3 0.01 1.04 21 0 -1 2.47 1.20 21 0 1 -1.33 1.25 -21 0 -1 0.13 1.42 21 0 3 1.01 1.07 -21 0 -3 -1.59 1.55 -21 -1 10 8.41 2.09 -21 1 10 6.10 1.97 -21 -1 8 6.62 1.80 -21 1 8 6.36 1.92 -21 -1 6 7.67 1.89 -21 1 6 7.35 1.92 21 1 -4 7.38 1.60 21 -1 -4 7.23 1.66 -21 -1 4 9.22 1.92 21 1 -2 1.16 0.99 21 -1 -2 0.23 0.98 21 1 0 2.36 1.30 -21 1 0 -0.17 1.22 -21 -1 0 0.98 1.34 21 -1 0 2.76 1.46 21 1 2 17.52 2.42 21 -1 2 16.57 2.54 -21 1 -2 16.68 3.01 -21 -1 -2 19.15 3.02 -21 2 9 0.77 1.13 -21 -2 7 10.87 2.04 -21 2 7 9.16 2.12 21 2 -5 -0.91 0.99 -21 -2 5 2.03 1.10 -21 2 5 0.62 1.14 21 2 -3 6.47 1.61 21 -2 -3 6.00 1.74 -21 2 3 8.44 2.09 21 2 -1 2.20 1.07 21 -2 -1 0.36 1.12 21 2 1 4.83 1.47 -21 2 -1 4.01 1.82 -21 -2 -1 1.19 1.50 21 -2 1 2.57 1.30 21 2 3 1.19 0.99 21 -2 3 1.32 1.36 -21 2 -3 1.04 1.61 -21 -2 -3 1.54 1.34 -21 3 8 0.10 1.07 -21 3 6 1.30 1.35 21 -3 -4 -0.01 1.26 -21 3 4 3.46 1.59 21 -3 -2 0.59 1.17 -21 3 2 1.19 1.26 -21 3 0 -1.36 1.41 -21 -3 0 3.35 1.72 21 -3 0 2.76 1.36 -21 3 -2 4.26 1.72 -21 -3 -2 3.38 1.78 21 -3 2 4.61 1.76 -21 4 7 0.69 1.29 -21 4 5 6.40 2.03 21 -4 -3 8.13 2.07 -21 4 3 10.40 2.32 21 -4 -1 2.32 1.46 -22 0 6 20.55 2.97 22 0 -4 26.71 3.01 -22 0 4 30.41 3.34 22 0 -2 -1.43 1.12 22 0 0 21.06 2.74 -22 0 0 23.74 3.38 -22 -1 7 -0.86 1.11 -22 1 7 0.34 1.24 22 1 -5 -0.31 0.91 22 -1 -5 -1.00 1.32 -22 -1 5 3.16 1.46 -22 1 5 2.27 1.37 22 1 -3 1.03 1.12 22 -1 -3 1.12 1.12 22 1 -1 -1.02 1.02 22 -1 -1 0.69 1.13 -22 2 6 5.75 1.93 22 2 -4 12.46 2.03 22 -2 -4 9.90 2.06 -22 2 4 13.73 2.55 22 2 -2 0.12 0.86 22 -2 -2 1.63 1.30 0 0 0 0.00 0.00 TITL exp_1028_d08 in I2/a REM I2/a (#15 in standard setting) CELL 0.71073 17.952424 11.091333 16.351191 90.0000 100.1541 90.0000 ZERR 8.00 0.001664 0.000662 0.001469 0.0000 0.0081 0.0000 LATT 2 SYMM -x+1/2, y,-z SFAC C H N O Cl Cu UNIT 80.00 80.00 16.00 64.00 16.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 2544 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.371 _oxdiff_exptl_absorpt_empirical_full_min 0.839 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.750000 0.28659(3) 0.500000 0.03184(12) Uani 1 2 d S T P . . S1 S 0.62477(4) 0.31191(6) 0.34379(4) 0.05053(18) Uani 1 1 d . . . . . Cl1 Cl 0.61270(4) 0.65157(7) 0.72841(4) 0.0655(2) Uani 1 1 d D U . . . O1 O 0.70804(9) 0.28356(13) 0.37754(9) 0.0426(4) Uani 1 1 d . . . . . N1 N 0.750000 0.46726(19) 0.500000 0.0298(5) Uani 1 2 d S T P . . N2 N 0.750000 1.1059(2) 0.500000 0.0349(5) Uani 1 2 d S T P . . O2 O 0.62694(10) 0.27045(17) 0.53216(12) 0.0573(5) Uani 1 1 d . . . . . C3 C 0.750000 0.7205(2) 0.500000 0.0281(5) Uani 1 2 d S T P . . C4 C 0.750000 0.8540(2) 0.500000 0.0289(6) Uani 1 2 d S T P . . N3 N 0.50845(12) 0.3017(2) 0.55544(13) 0.0532(5) Uani 1 1 d . . . . . C1 C 0.74172(12) 0.53121(18) 0.56830(12) 0.0338(4) Uani 1 1 d . . . . . H1 H 0.735087 0.489426 0.615801 0.041 Uiso 1 1 calc R . . . . C2 C 0.74267(12) 0.65468(17) 0.57071(12) 0.0330(4) Uani 1 1 d . . . . . H2 H 0.738403 0.694655 0.619667 0.040 Uiso 1 1 calc R . . . . C9 C 0.57898(14) 0.3332(2) 0.55571(15) 0.0479(6) Uani 1 1 d . . . . . H9 H 0.593650 0.409786 0.575499 0.057 Uiso 1 1 calc R . . . . C5 C 0.72648(14) 0.91955(18) 0.56325(13) 0.0440(6) Uani 1 1 d . . . . . H5 H 0.709971 0.879823 0.606860 0.053 Uiso 1 1 calc R . . . . C6 C 0.72772(14) 1.04318(19) 0.56108(14) 0.0455(6) Uani 1 1 d . . . . . H6 H 0.712264 1.085396 0.604302 0.055 Uiso 1 1 calc R . . . . O5B O 0.6702(5) 0.5611(9) 0.7317(6) 0.110(3) Uani 0.621(19) 1 d D U . A 2 C10 C 0.45415(17) 0.3846(3) 0.5812(2) 0.0808(10) Uani 1 1 d . . . . . H10A H 0.479377 0.458027 0.600986 0.121 Uiso 1 1 calc GR . . . . H10B H 0.432304 0.348486 0.624783 0.121 Uiso 1 1 calc GR . . . . H10C H 0.414933 0.401996 0.534690 0.121 Uiso 1 1 calc GR . . . . O6B O 0.5667(9) 0.6145(14) 0.6570(7) 0.147(5) Uani 0.621(19) 1 d D U . A 2 O4B O 0.6323(8) 0.7702(6) 0.7182(9) 0.134(4) Uani 0.621(19) 1 d D U . A 2 O3B O 0.5598(8) 0.6312(13) 0.7782(8) 0.149(4) Uani 0.621(19) 1 d D U . A 2 C8 C 0.5822(2) 0.1703(3) 0.3177(3) 0.0920(11) Uani 1 1 d . . . . . H8A H 0.610281 0.127673 0.282053 0.138 Uiso 1 1 calc GR . . . . H8B H 0.531097 0.181921 0.289414 0.138 Uiso 1 1 calc GR . . . . H8C H 0.581983 0.124387 0.367415 0.138 Uiso 1 1 calc GR . . . . C11 C 0.4806(2) 0.1850(3) 0.5233(2) 0.0842(10) Uani 1 1 d . . . . . H11A H 0.450892 0.194885 0.468835 0.126 Uiso 1 1 calc GR . . . . H11B H 0.449898 0.150136 0.559579 0.126 Uiso 1 1 calc GR . . . . H11C H 0.522681 0.132793 0.520129 0.126 Uiso 1 1 calc GR . . . . C7 C 0.6278(2) 0.3680(4) 0.2425(2) 0.1078(14) Uani 1 1 d . . . . . H7A H 0.652352 0.445279 0.246843 0.162 Uiso 1 1 calc GR . . . . H7B H 0.577216 0.376250 0.212151 0.162 Uiso 1 1 calc GR . . . . H7C H 0.655565 0.312922 0.214003 0.162 Uiso 1 1 calc GR . . . . O6A O 0.5783(12) 0.653(2) 0.6442(6) 0.117(6) Uani 0.379(19) 1 d D U . A 1 O3A O 0.5864(14) 0.6366(18) 0.8039(11) 0.154(8) Uani 0.379(19) 1 d D U . A 1 O5A O 0.6797(9) 0.589(2) 0.7492(12) 0.146(6) Uani 0.379(19) 1 d D U . A 1 O4A O 0.6403(15) 0.7665(14) 0.7442(14) 0.167(8) Uani 0.379(19) 1 d D U . A 1 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 0.0475(2) 0.01248(17) 0.03649(19) 0.000 0.01001(15) 0.000 S1 0.0632(4) 0.0429(4) 0.0429(3) -0.0033(2) 0.0022(3) 0.0013(3) Cl1 0.0699(5) 0.0721(5) 0.0585(4) -0.0023(3) 0.0227(3) -0.0061(4) O1 0.0593(10) 0.0274(8) 0.0407(8) -0.0040(6) 0.0075(7) -0.0023(7) N1 0.0381(13) 0.0170(11) 0.0354(12) 0.000 0.0097(10) 0.000 N2 0.0507(15) 0.0156(11) 0.0416(13) 0.000 0.0170(11) 0.000 O2 0.0522(10) 0.0505(11) 0.0746(12) 0.0021(9) 0.0256(9) 0.0044(8) C3 0.0312(14) 0.0176(13) 0.0363(14) 0.000 0.0079(11) 0.000 C4 0.0346(15) 0.0175(13) 0.0359(14) 0.000 0.0096(11) 0.000 N3 0.0453(12) 0.0612(14) 0.0539(12) 0.0042(10) 0.0112(9) -0.0052(10) C1 0.0491(12) 0.0210(10) 0.0339(10) 0.0030(7) 0.0144(9) 0.0015(8) C2 0.0475(12) 0.0203(10) 0.0332(10) -0.0016(7) 0.0130(9) 0.0009(8) C9 0.0474(14) 0.0448(14) 0.0515(13) 0.0065(11) 0.0091(11) 0.0033(11) C5 0.0760(16) 0.0197(10) 0.0438(12) 0.0007(8) 0.0315(11) -0.0014(10) C6 0.0783(17) 0.0194(10) 0.0468(12) -0.0026(8) 0.0332(12) 0.0004(10) O5B 0.136(7) 0.119(5) 0.095(5) 0.032(4) 0.074(5) 0.060(5) C10 0.0533(17) 0.093(3) 0.100(2) 0.014(2) 0.0233(17) 0.0182(17) O6B 0.135(7) 0.131(8) 0.158(7) -0.053(7) -0.024(6) -0.015(5) O4B 0.188(10) 0.073(4) 0.162(8) -0.003(4) 0.086(7) -0.031(4) O3B 0.148(7) 0.139(7) 0.197(9) 0.056(7) 0.136(7) 0.036(5) C8 0.082(2) 0.068(2) 0.118(3) -0.024(2) -0.003(2) -0.0254(19) C11 0.079(2) 0.090(3) 0.085(2) -0.0128(19) 0.0204(18) -0.0357(19) C7 0.121(3) 0.139(4) 0.0535(19) 0.033(2) -0.0112(19) -0.013(3) O6A 0.111(9) 0.176(17) 0.056(5) -0.001(6) -0.009(4) 0.003(9) O3A 0.28(2) 0.114(9) 0.106(8) 0.021(6) 0.132(12) 0.071(11) O5A 0.073(6) 0.256(16) 0.100(9) 0.063(10) -0.007(6) 0.032(8) O4A 0.180(14) 0.148(10) 0.170(14) -0.083(9) 0.023(10) -0.096(9) 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' Cl Cl 0.1484 0.1585 '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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Cu1 O1 178.08(8) 2_656 . O1 Cu1 O2 88.74(7) 2_656 . O1 Cu1 O2 91.12(7) . . O1 Cu1 O2 91.12(7) 2_656 2_656 O1 Cu1 O2 88.74(7) . 2_656 N1 Cu1 O1 90.96(4) . . N1 Cu1 O1 90.96(4) . 2_656 N1 Cu1 N2 180.0 . 1_545 N1 Cu1 O2 94.34(5) . 2_656 N1 Cu1 O2 94.34(5) . . N2 Cu1 O1 89.04(4) 1_545 . N2 Cu1 O1 89.04(4) 1_545 2_656 N2 Cu1 O2 85.66(5) 1_545 2_656 N2 Cu1 O2 85.66(5) 1_545 . O2 Cu1 O2 171.32(9) 2_656 . O1 S1 C8 104.95(15) . . O1 S1 C7 102.64(16) . . C8 S1 C7 99.8(2) . . O6B Cl1 O5B 98.3(9) . . O6B Cl1 O4B 108.1(7) . . O6B Cl1 O3B 94.6(11) . . O4B Cl1 O5B 118.3(8) . . O3B Cl1 O5B 115.5(7) . . O3B Cl1 O4B 116.5(8) . . O3A Cl1 O6A 134.6(16) . . O5A Cl1 O6A 117.3(14) . . O5A Cl1 O3A 98.0(12) . . O4A Cl1 O6A 104.9(11) . . O4A Cl1 O3A 96.3(13) . . O4A Cl1 O5A 98.6(13) . . S1 O1 Cu1 121.71(9) . . C1 N1 Cu1 121.62(11) . . C1 N1 Cu1 121.62(11) 2_656 . C1 N1 C1 116.8(2) 2_656 . C6 N2 Cu1 121.40(12) 2_656 1_565 C6 N2 Cu1 121.40(12) . 1_565 C6 N2 C6 117.2(2) 2_656 . C9 O2 Cu1 139.88(18) . . C2 C3 C4 121.60(12) 2_656 . C2 C3 C4 121.60(12) . . C2 C3 C2 116.8(2) . 2_656 C5 C4 C3 121.57(12) 2_656 . C5 C4 C3 121.57(12) . . C5 C4 C5 116.9(2) . 2_656 C9 N3 C10 121.7(3) . . C9 N3 C11 120.6(2) . . C10 N3 C11 117.6(3) . . N1 C1 H1 118.5 . . N1 C1 C2 123.03(18) . . C2 C1 H1 118.5 . . C3 C2 H2 119.9 . . C1 C2 C3 120.15(18) . . C1 C2 H2 119.9 . . O2 C9 N3 125.5(3) . . O2 C9 H9 117.3 . . N3 C9 H9 117.3 . . C4 C5 H5 120.1 . . C6 C5 C4 119.70(19) . . C6 C5 H5 120.1 . . N2 C6 C5 123.26(19) . . N2 C6 H6 118.4 . . C5 C6 H6 118.4 . . N3 C10 H10A 109.5 . . N3 C10 H10B 109.5 . . N3 C10 H10C 109.5 . . H10A C10 H10B 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . S1 C8 H8A 109.5 . . S1 C8 H8B 109.5 . . S1 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . N3 C11 H11A 109.5 . . N3 C11 H11B 109.5 . . N3 C11 H11C 109.5 . . H11A C11 H11B 109.5 . . H11A C11 H11C 109.5 . . H11B C11 H11C 109.5 . . S1 C7 H7A 109.5 . . S1 C7 H7B 109.5 . . S1 C7 H7C 109.5 . . H7A C7 H7B 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 O1 2.0114(15) 2_656 Cu1 O1 2.0115(15) . Cu1 N1 2.004(2) . Cu1 N2 2.004(2) 1_545 Cu1 O2 2.3662(17) . Cu1 O2 2.3662(17) 2_656 S1 O1 1.5322(18) . S1 C8 1.766(3) . S1 C7 1.779(3) . Cl1 O5B 1.434(6) . Cl1 O6B 1.369(8) . Cl1 O4B 1.380(6) . Cl1 O3B 1.373(6) . Cl1 O6A 1.407(9) . Cl1 O3A 1.407(10) . Cl1 O5A 1.378(10) . Cl1 O4A 1.375(11) . N1 C1 1.353(2) 2_656 N1 C1 1.353(2) . N2 C6 1.335(2) . N2 C6 1.335(2) 2_656 O2 C9 1.221(3) . C3 C4 1.480(4) . C3 C2 1.393(2) 2_656 C3 C2 1.393(2) . C4 C5 1.390(2) . C4 C5 1.390(2) 2_656 N3 C9 1.313(3) . N3 C10 1.455(4) . N3 C11 1.453(4) . C1 H1 0.9300 . C1 C2 1.370(3) . C2 H2 0.9300 . C9 H9 0.9300 . C5 H5 0.9300 . C5 C6 1.372(3) . C6 H6 0.9300 . C10 H10A 0.9600 . C10 H10B 0.9600 . C10 H10C 0.9600 . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . C11 H11A 0.9600 . C11 H11B 0.9600 . C11 H11C 0.9600 . C7 H7A 0.9600 . C7 H7B 0.9600 . C7 H7C 0.9600 . 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 Cu1 N1 C1 C2 178.94(15) . . . . Cu1 N2 C6 C5 179.66(19) 1_565 . . . Cu1 O2 C9 N3 168.03(18) . . . . N1 C1 C2 C3 2.1(3) . . . . C3 C4 C5 C6 179.68(18) . . . . C4 C3 C2 C1 179.01(14) . . . . C4 C5 C6 N2 0.7(4) . . . . C1 N1 C1 C2 -1.05(15) 2_656 . . . C2 C3 C4 C5 -14.28(16) . . . . C2 C3 C4 C5 165.71(16) . . . 2_656 C2 C3 C4 C5 -14.28(16) 2_656 . . 2_656 C2 C3 C4 C5 165.72(16) 2_656 . . . C2 C3 C2 C1 -0.99(14) 2_656 . . . C5 C4 C5 C6 -0.32(18) 2_656 . . . C6 N2 C6 C5 -0.35(19) 2_656 . . . C10 N3 C9 O2 -177.1(3) . . . . C8 S1 O1 Cu1 -103.37(17) . . . . C11 N3 C9 O2 -1.8(4) . . . . C7 S1 O1 Cu1 152.76(18) . . . .