Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof F Albert Cotton' _publ_contact_author_address ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry Texas A&M University, P.O. Box 30012 College Station, TX 77842-3012, USA ; _publ_contact_author_email cotton@tamu.edu _publ_contact_author_fax '(979) 845 9351' _publ_contact_author_phone '(979) 845 4432' # TITLE AND AUTHOR LIST _publ_section_title ; Isomerization by Ligand Shuffling Along a Cr~2~2^4^ unit: Further Reaction Leading to Clevage of a Quadruple Bond ; loop_ _publ_author_name _publ_author_address 'Rodolphe Clerac' ; Centre de Recherche Paul Pascal, CNRS UPR 8641, avenue du Dr. A. Schweitzer, 33600 Pessac, France ; 'F. Albert Cotton' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, P.O. Box 30012 College Station, TX 77842-3012, USA ; 'Stephen P. Jeffery' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, P.O. Box 30012 College Station, TX 77842-3012, USA ; 'Carlos A. Murillo' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, P.O. Box 30012 College Station, TX 77842-3012, USA ; 'Xiaoping Wang' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, P.O. Box 300012 College Station, TX 77842-3012, USA and ; #============================================================== data_cmpd1 _database_code_CSD 206653 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cr2(DpyF)4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H36 Cr2 N16' _chemical_formula_weight 892.89 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.960(3) _cell_length_b 13.305(3) _cell_length_c 13.510(5) _cell_angle_alpha 66.75(2) _cell_angle_beta 89.96(5) _cell_angle_gamma 88.52(4) _cell_volume 1974.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 9.05 _cell_measurement_theta_max 21.9 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.896 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_process_details 'SORTAV (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'None (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9422 _diffrn_reflns_av_R_equivalents 0.0874 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 22.68 _reflns_number_total 4903 _reflns_number_gt 3584 _reflns_threshold_expression I>2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+12.6113P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4903 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr -0.23672(10) -0.26324(9) 0.05262(9) 0.0257(3) Uani 1 1 d . . . Cr2 Cr -0.23468(10) -0.25849(10) -0.09261(9) 0.0264(3) Uani 1 1 d . . . N1 N -0.1849(5) -0.3871(5) -0.2211(6) 0.0386(17) Uani 1 1 d . . . N2 N -0.1700(5) -0.4133(5) -0.0455(5) 0.0252(14) Uani 1 1 d . . . N3 N -0.1664(5) -0.4205(5) 0.1250(5) 0.0272(15) Uani 1 1 d . . . N4 N -0.1408(7) -0.5920(5) 0.2681(5) 0.054(2) Uani 1 1 d . . . N5 N -0.3074(5) -0.1078(5) 0.0105(5) 0.0258(15) Uani 1 1 d . . . N6 N -0.2966(5) -0.1004(5) -0.1600(5) 0.0272(15) Uani 1 1 d . . . N7 N -0.3034(5) -0.1089(5) -0.3273(5) 0.0322(16) Uani 1 1 d . . . N8 N -0.3130(6) 0.0541(6) -0.4843(5) 0.0392(17) Uani 1 1 d . . . N9 N -0.3945(5) -0.3152(5) -0.0878(5) 0.0271(15) Uani 1 1 d . . . N10 N -0.3952(5) -0.3249(5) 0.0834(5) 0.0287(15) Uani 1 1 d . . . N11 N -0.3917(5) -0.3243(5) 0.2529(5) 0.0349(16) Uani 1 1 d . . . N12 N -0.5632(6) -0.3048(6) 0.3319(6) 0.0471(19) Uani 1 1 d . . . N13 N -0.0753(5) -0.2007(5) -0.1273(5) 0.0247(14) Uani 1 1 d . . . N14 N -0.0829(5) -0.1912(5) 0.0349(5) 0.0268(15) Uani 1 1 d . . . N15 N -0.1056(5) -0.1773(5) 0.1963(5) 0.0308(16) Uani 1 1 d . . . N16 N 0.0492(6) -0.1298(6) 0.2787(5) 0.0420(18) Uani 1 1 d . . . C1 C -0.1875(7) -0.4213(8) -0.3012(7) 0.048(2) Uani 1 1 d . . . H1A H -0.2027 -0.3698 -0.3714 0.058 Uiso 1 1 calc R . . C2 C -0.1689(8) -0.5292(8) -0.2855(7) 0.052(3) Uani 1 1 d . . . H2A H -0.1721 -0.5508 -0.3438 0.063 Uiso 1 1 calc R . . C3 C -0.1458(7) -0.6036(7) -0.1845(7) 0.046(2) Uani 1 1 d . . . H3A H -0.1333 -0.6777 -0.1719 0.055 Uiso 1 1 calc R . . C4 C -0.1408(7) -0.5699(7) -0.1001(7) 0.041(2) Uani 1 1 d . . . H4A H -0.1233 -0.6200 -0.0297 0.049 Uiso 1 1 calc R . . C5 C -0.1624(6) -0.4596(6) -0.1219(6) 0.0305(19) Uani 1 1 d . . . C6 C -0.1471(6) -0.4687(6) 0.0579(6) 0.0299(19) Uani 1 1 d . . . H6A H -0.1177 -0.5407 0.0830 0.036 Uiso 1 1 calc R . . C7 C -0.1470(6) -0.4834(6) 0.2349(6) 0.0292(18) Uani 1 1 d . . . C8 C -0.1374(7) -0.4322(6) 0.3056(6) 0.0334(19) Uani 1 1 d . . . H8A H -0.1460 -0.3557 0.2809 0.040 Uiso 1 1 calc R . . C9 C -0.1185(9) -0.6501(7) 0.3735(7) 0.062(3) Uani 1 1 d . . . H9A H -0.1131 -0.7267 0.3974 0.074 Uiso 1 1 calc R . . C10 C -0.1031(7) -0.6057(7) 0.4486(6) 0.041(2) Uani 1 1 d . . . H10A H -0.0853 -0.6497 0.5209 0.049 Uiso 1 1 calc R . . C11 C -0.1149(6) -0.4949(7) 0.4129(6) 0.036(2) Uani 1 1 d . . . H11A H -0.1077 -0.4609 0.4617 0.044 Uiso 1 1 calc R . . C12 C -0.3346(6) -0.0642(7) 0.0834(7) 0.0330(19) Uani 1 1 d . . . H12A H -0.3277 -0.1088 0.1572 0.040 Uiso 1 1 calc R . . C13 C -0.3711(7) 0.0412(7) 0.0534(7) 0.042(2) Uani 1 1 d . . . H13A H -0.3928 0.0682 0.1053 0.050 Uiso 1 1 calc R . . C14 C -0.3758(7) 0.1070(7) -0.0537(7) 0.046(2) Uani 1 1 d . . . H14A H -0.3963 0.1814 -0.0757 0.056 Uiso 1 1 calc R . . C15 C -0.3514(7) 0.0664(6) -0.1281(7) 0.040(2) Uani 1 1 d . . . H15A H -0.3554 0.1118 -0.2018 0.047 Uiso 1 1 calc R . . C16 C -0.3193(6) -0.0461(6) -0.0941(6) 0.0302(19) Uani 1 1 d . . . C17 C -0.3196(6) -0.0553(6) -0.2668(6) 0.0286(19) Uani 1 1 d . . . H17A H -0.3482 0.0170 -0.2979 0.034 Uiso 1 1 calc R . . C18 C -0.3324(6) -0.0539(7) -0.4363(6) 0.0327(19) Uani 1 1 d . . . C19 C -0.3759(7) -0.1106(8) -0.4905(8) 0.049(2) Uani 1 1 d . . . H19A H -0.3853 -0.1864 -0.4551 0.059 Uiso 1 1 calc R . . C20 C -0.3414(7) 0.1045(7) -0.5876(7) 0.046(2) Uani 1 1 d . . . H20A H -0.3287 0.1798 -0.6220 0.056 Uiso 1 1 calc R . . C21 C -0.3888(7) 0.0526(8) -0.6478(7) 0.048(2) Uani 1 1 d . . . H21A H -0.4081 0.0916 -0.7208 0.058 Uiso 1 1 calc R . . C22 C -0.4065(7) -0.0575(8) -0.5976(8) 0.050(2) Uani 1 1 d . . . H22A H -0.4388 -0.0959 -0.6352 0.059 Uiso 1 1 calc R . . C23 C -0.4397(7) -0.3245(6) -0.1761(6) 0.0337(19) Uani 1 1 d . . . H23A H -0.3963 -0.3083 -0.2382 0.040 Uiso 1 1 calc R . . C24 C -0.5486(7) -0.3574(7) -0.1760(7) 0.044(2) Uani 1 1 d . . . H24A H -0.5801 -0.3635 -0.2371 0.052 Uiso 1 1 calc R . . C25 C -0.6096(7) -0.3812(7) -0.0819(7) 0.045(2) Uani 1 1 d . . . H25A H -0.6838 -0.4038 -0.0794 0.054 Uiso 1 1 calc R . . C26 C -0.5649(6) -0.3724(7) 0.0053(7) 0.041(2) Uani 1 1 d . . . H26A H -0.6074 -0.3880 0.0679 0.049 Uiso 1 1 calc R . . C27 C -0.4522(6) -0.3392(6) 0.0018(6) 0.0291(19) Uani 1 1 d . . . C28 C -0.4444(7) -0.3416(6) 0.1783(6) 0.0309(19) Uani 1 1 d . . . H28A H -0.5181 -0.3661 0.1901 0.037 Uiso 1 1 calc R . . C29 C -0.4531(7) -0.3344(6) 0.3443(6) 0.0322(19) Uani 1 1 d . . . C30 C -0.4009(8) -0.3719(7) 0.4438(7) 0.042(2) Uani 1 1 d . . . H30A H -0.3236 -0.3877 0.4492 0.051 Uiso 1 1 calc R . . C31 C -0.6197(8) -0.3185(8) 0.4215(8) 0.054(3) Uani 1 1 d . . . H31A H -0.6964 -0.2995 0.4142 0.064 Uiso 1 1 calc R . . C32 C -0.5742(8) -0.3581(7) 0.5230(7) 0.048(2) Uani 1 1 d . . . H32A H -0.6185 -0.3659 0.5830 0.058 Uiso 1 1 calc R . . C33 C -0.4608(7) -0.3866(7) 0.5351(7) 0.046(2) Uani 1 1 d . . . H33A H -0.4263 -0.4149 0.6035 0.055 Uiso 1 1 calc R . . C34 C -0.0245(6) -0.1882(6) -0.2206(7) 0.035(2) Uani 1 1 d . . . H34A H -0.0633 -0.2072 -0.2710 0.042 Uiso 1 1 calc R . . C35 C 0.0816(7) -0.1488(7) -0.2450(7) 0.040(2) Uani 1 1 d . . . H35A H 0.1157 -0.1423 -0.3099 0.048 Uiso 1 1 calc R . . C36 C 0.1366(7) -0.1191(7) -0.1715(6) 0.040(2) Uani 1 1 d . . . H36A H 0.2087 -0.0908 -0.1863 0.048 Uiso 1 1 calc R . . C37 C 0.0860(6) -0.1308(6) -0.0772(7) 0.035(2) Uani 1 1 d . . . H37A H 0.1237 -0.1113 -0.0266 0.042 Uiso 1 1 calc R . . C38 C -0.0221(6) -0.1719(6) -0.0555(6) 0.0254(18) Uani 1 1 d . . . C39 C -0.0483(7) -0.1605(6) 0.1134(6) 0.0269(18) Uani 1 1 d . . . H39A H 0.0204 -0.1257 0.1061 0.032 Uiso 1 1 calc R . . C40 C -0.0610(7) -0.1527(6) 0.2806(6) 0.0318(19) Uani 1 1 d . . . C41 C -0.1300(7) -0.1559(7) 0.3624(6) 0.039(2) Uani 1 1 d . . . H41A H -0.2049 -0.1758 0.3632 0.047 Uiso 1 1 calc R . . C42 C 0.0847(8) -0.1038(7) 0.3589(7) 0.049(2) Uani 1 1 d . . . H42A H 0.1599 -0.0849 0.3586 0.058 Uiso 1 1 calc R . . C43 C 0.0202(8) -0.1026(7) 0.4405(7) 0.045(2) Uani 1 1 d . . . H43A H 0.0505 -0.0832 0.4945 0.054 Uiso 1 1 calc R . . C44 C -0.0879(8) -0.1295(7) 0.4440(7) 0.046(2) Uani 1 1 d . . . H44A H -0.1337 -0.1302 0.5008 0.056 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 Cr1 0.0249(7) 0.0264(7) 0.0241(7) -0.0080(5) -0.0007(5) 0.0001(5) Cr2 0.0244(7) 0.0266(7) 0.0267(7) -0.0087(6) -0.0010(6) -0.0018(5) N1 0.031(4) 0.045(4) 0.044(5) -0.021(4) -0.002(3) -0.006(3) N2 0.027(3) 0.023(3) 0.027(4) -0.012(3) -0.003(3) 0.002(3) N3 0.024(3) 0.027(4) 0.027(4) -0.007(3) -0.003(3) 0.003(3) N4 0.103(7) 0.029(4) 0.034(4) -0.018(4) -0.013(4) 0.011(4) N5 0.017(3) 0.030(4) 0.028(4) -0.009(3) -0.003(3) -0.002(3) N6 0.024(3) 0.026(4) 0.027(4) -0.005(3) 0.003(3) 0.001(3) N7 0.037(4) 0.037(4) 0.022(4) -0.011(3) 0.002(3) 0.000(3) N8 0.043(4) 0.044(4) 0.024(4) -0.007(3) -0.001(3) -0.005(3) N9 0.028(3) 0.022(3) 0.028(4) -0.007(3) 0.000(3) -0.002(3) N10 0.024(3) 0.031(4) 0.031(4) -0.012(3) -0.004(3) 0.001(3) N11 0.036(4) 0.038(4) 0.027(4) -0.009(3) -0.002(3) 0.001(3) N12 0.047(5) 0.045(5) 0.043(5) -0.011(4) 0.005(4) 0.005(4) N13 0.024(3) 0.027(4) 0.023(4) -0.009(3) 0.005(3) -0.002(3) N14 0.026(3) 0.033(4) 0.022(4) -0.011(3) -0.004(3) 0.001(3) N15 0.040(4) 0.030(4) 0.023(4) -0.010(3) -0.003(3) 0.001(3) N16 0.038(4) 0.054(5) 0.033(4) -0.015(4) 0.005(3) -0.011(3) C1 0.051(6) 0.060(6) 0.039(5) -0.026(5) -0.003(5) -0.003(5) C2 0.055(6) 0.081(8) 0.036(6) -0.039(5) 0.001(5) -0.004(5) C3 0.056(6) 0.044(5) 0.044(6) -0.025(5) -0.003(5) 0.003(4) C4 0.043(5) 0.038(5) 0.039(5) -0.013(4) -0.009(4) 0.010(4) C5 0.024(4) 0.035(5) 0.027(5) -0.006(4) -0.003(4) 0.004(3) C6 0.018(4) 0.029(4) 0.044(5) -0.015(4) 0.004(4) -0.004(3) C7 0.024(4) 0.029(5) 0.032(5) -0.010(4) 0.000(4) 0.007(3) C8 0.042(5) 0.023(4) 0.034(5) -0.010(4) 0.002(4) 0.000(4) C9 0.106(9) 0.030(5) 0.039(6) -0.003(5) -0.017(6) 0.010(5) C10 0.058(6) 0.042(5) 0.015(4) -0.004(4) -0.002(4) 0.013(4) C11 0.034(5) 0.037(5) 0.031(5) -0.006(4) 0.004(4) 0.001(4) C12 0.022(4) 0.043(5) 0.041(5) -0.024(4) -0.010(4) 0.000(4) C13 0.037(5) 0.036(5) 0.061(6) -0.029(5) -0.008(5) 0.008(4) C14 0.053(6) 0.038(5) 0.053(6) -0.022(5) -0.015(5) 0.006(4) C15 0.042(5) 0.031(5) 0.038(5) -0.005(4) -0.005(4) -0.004(4) C16 0.022(4) 0.033(5) 0.036(5) -0.014(4) 0.001(4) -0.004(3) C17 0.016(4) 0.033(4) 0.026(5) 0.000(4) 0.002(3) -0.004(3) C18 0.030(4) 0.041(5) 0.025(5) -0.010(4) 0.008(4) -0.004(4) C19 0.045(5) 0.046(6) 0.060(7) -0.024(5) -0.005(5) -0.002(4) C20 0.044(5) 0.041(5) 0.047(6) -0.011(5) -0.004(5) -0.001(4) C21 0.038(5) 0.064(7) 0.038(5) -0.016(5) 0.005(4) 0.009(5) C22 0.035(5) 0.076(7) 0.052(6) -0.041(6) 0.008(5) -0.009(5) C23 0.038(5) 0.034(5) 0.029(5) -0.013(4) 0.000(4) 0.002(4) C24 0.039(5) 0.048(6) 0.046(6) -0.020(5) -0.007(5) -0.007(4) C25 0.035(5) 0.044(5) 0.061(6) -0.026(5) -0.005(5) -0.007(4) C26 0.023(4) 0.056(6) 0.054(6) -0.031(5) 0.008(4) -0.009(4) C27 0.032(4) 0.019(4) 0.032(5) -0.006(4) 0.000(4) 0.006(3) C28 0.030(4) 0.032(5) 0.024(5) -0.004(4) 0.008(4) 0.001(4) C29 0.039(5) 0.027(4) 0.029(5) -0.009(4) 0.004(4) -0.004(4) C30 0.053(6) 0.041(5) 0.036(5) -0.018(4) 0.003(5) -0.013(4) C31 0.051(6) 0.055(6) 0.050(6) -0.016(5) 0.014(5) 0.000(5) C32 0.071(7) 0.050(6) 0.024(5) -0.016(4) 0.005(5) -0.008(5) C33 0.048(6) 0.055(6) 0.034(5) -0.017(4) 0.003(5) -0.012(5) C34 0.030(5) 0.033(5) 0.037(5) -0.008(4) -0.006(4) -0.002(4) C35 0.041(5) 0.048(5) 0.033(5) -0.017(4) 0.013(4) -0.007(4) C36 0.046(5) 0.044(5) 0.028(5) -0.012(4) 0.005(4) -0.009(4) C37 0.028(4) 0.042(5) 0.037(5) -0.020(4) -0.004(4) -0.002(4) C38 0.026(4) 0.022(4) 0.025(4) -0.005(3) -0.008(4) 0.000(3) C39 0.037(4) 0.024(4) 0.021(4) -0.010(3) 0.006(4) -0.004(3) C40 0.042(5) 0.029(4) 0.018(4) -0.003(3) -0.003(4) 0.001(4) C41 0.038(5) 0.044(5) 0.037(5) -0.019(4) 0.011(4) -0.002(4) C42 0.054(6) 0.056(6) 0.031(5) -0.012(5) -0.017(5) -0.011(5) C43 0.067(7) 0.037(5) 0.029(5) -0.013(4) -0.015(5) 0.004(5) C44 0.052(6) 0.059(6) 0.036(5) -0.028(5) -0.007(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 Cr2 1.9380(18) . ? Cr1 N10 2.061(6) . ? Cr1 N14 2.066(6) . ? Cr1 N5 2.073(6) . ? Cr1 N3 2.083(6) . ? Cr1 N15 3.063(6) . ? Cr1 N11 3.123(7) . ? Cr2 N2 2.032(6) . ? Cr2 N6 2.052(6) . ? Cr2 N13 2.058(6) . ? Cr2 N9 2.065(6) . ? Cr2 N1 2.930(7) . ? Cr2 N7 3.103(6) . ? N1 C5 1.328(10) . ? N1 C1 1.330(10) . ? N2 C6 1.322(9) . ? N2 C5 1.398(9) . ? N3 C6 1.318(9) . ? N3 C7 1.402(9) . ? N4 C7 1.333(10) . ? N4 C9 1.348(11) . ? N5 C16 1.329(9) . ? N5 C12 1.361(9) . ? N6 C17 1.351(9) . ? N6 C16 1.374(9) . ? N7 C17 1.291(9) . ? N7 C18 1.401(9) . ? N8 C20 1.328(10) . ? N8 C18 1.349(10) . ? N9 C27 1.323(9) . ? N9 C23 1.360(9) . ? N10 C28 1.350(9) . ? N10 C27 1.374(9) . ? N11 C28 1.286(9) . ? N11 C29 1.398(10) . ? N12 C31 1.337(11) . ? N12 C29 1.356(10) . ? N13 C38 1.341(9) . ? N13 C34 1.351(10) . ? N14 C39 1.347(9) . ? N14 C38 1.359(9) . ? N15 C39 1.257(9) . ? N15 C40 1.413(9) . ? N16 C42 1.335(10) . ? N16 C40 1.358(10) . ? C1 C2 1.378(13) . ? C2 C3 1.356(12) . ? C3 C4 1.382(11) . ? C4 C5 1.394(11) . ? C7 C8 1.381(10) . ? C8 C11 1.381(11) . ? C9 C10 1.376(12) . ? C10 C11 1.363(11) . ? C12 C13 1.357(11) . ? C13 C14 1.364(12) . ? C14 C15 1.344(11) . ? C15 C16 1.423(11) . ? C18 C19 1.355(11) . ? C19 C22 1.380(12) . ? C20 C21 1.387(12) . ? C21 C22 1.372(12) . ? C23 C24 1.384(11) . ? C24 C25 1.394(12) . ? C25 C26 1.342(11) . ? C26 C27 1.424(10) . ? C29 C30 1.379(11) . ? C30 C33 1.374(12) . ? C31 C32 1.367(12) . ? C32 C33 1.391(13) . ? C34 C35 1.376(11) . ? C35 C36 1.378(11) . ? C36 C37 1.363(11) . ? C37 C38 1.403(10) . ? C40 C41 1.367(11) . ? C41 C44 1.381(11) . ? C42 C43 1.349(12) . ? C43 C44 1.345(12) . ? 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 _geom_angle_publ_flag Cr2 Cr1 N10 93.86(19) . . ? Cr2 Cr1 N14 92.45(18) . . ? N10 Cr1 N14 172.6(3) . . ? Cr2 Cr1 N5 95.54(18) . . ? N10 Cr1 N5 88.5(2) . . ? N14 Cr1 N5 86.9(2) . . ? Cr2 Cr1 N3 95.51(18) . . ? N10 Cr1 N3 90.6(2) . . ? N14 Cr1 N3 92.7(2) . . ? N5 Cr1 N3 169.0(2) . . ? Cr2 Cr1 N15 139.78(14) . . ? N10 Cr1 N15 125.2(2) . . ? N14 Cr1 N15 48.0(2) . . ? N5 Cr1 N15 78.0(2) . . ? N3 Cr1 N15 93.5(2) . . ? Cr2 Cr1 N11 141.07(13) . . ? N10 Cr1 N11 47.2(2) . . ? N14 Cr1 N11 126.3(2) . . ? N5 Cr1 N11 84.2(2) . . ? N3 Cr1 N11 87.1(2) . . ? N15 Cr1 N11 78.40(18) . . ? Cr1 Cr2 N2 93.65(18) . . ? Cr1 Cr2 N6 93.62(18) . . ? N2 Cr2 N6 172.6(2) . . ? Cr1 Cr2 N13 95.88(18) . . ? N2 Cr2 N13 88.9(2) . . ? N6 Cr2 N13 89.2(2) . . ? Cr1 Cr2 N9 95.23(19) . . ? N2 Cr2 N9 90.5(2) . . ? N6 Cr2 N9 89.9(2) . . ? N13 Cr2 N9 168.9(3) . . ? Cr1 Cr2 N1 143.97(15) . . ? N2 Cr2 N1 50.4(2) . . ? N6 Cr2 N1 122.4(2) . . ? N13 Cr2 N1 86.7(2) . . ? N9 Cr2 N1 84.4(2) . . ? Cr1 Cr2 N7 141.52(14) . . ? N2 Cr2 N7 124.7(2) . . ? N6 Cr2 N7 48.1(2) . . ? N13 Cr2 N7 88.2(2) . . ? N9 Cr2 N7 83.0(2) . . ? N1 Cr2 N7 74.35(18) . . ? C5 N1 C1 118.8(7) . . ? C5 N1 Cr2 78.4(5) . . ? C1 N1 Cr2 160.6(6) . . ? C6 N2 C5 123.1(6) . . ? C6 N2 Cr2 118.2(5) . . ? C5 N2 Cr2 118.4(5) . . ? C6 N3 C7 117.1(6) . . ? C6 N3 Cr1 114.1(5) . . ? C7 N3 Cr1 128.5(5) . . ? C7 N4 C9 117.0(7) . . ? C16 N5 C12 119.2(6) . . ? C16 N5 Cr1 117.2(5) . . ? C12 N5 Cr1 123.5(5) . . ? C17 N6 C16 122.1(6) . . ? C17 N6 Cr2 118.9(5) . . ? C16 N6 Cr2 118.9(5) . . ? C17 N7 C18 116.4(6) . . ? C17 N7 Cr2 71.2(4) . . ? C18 N7 Cr2 172.3(5) . . ? C20 N8 C18 117.1(7) . . ? C27 N9 C23 121.3(7) . . ? C27 N9 Cr2 118.3(5) . . ? C23 N9 Cr2 120.4(5) . . ? C28 N10 C27 121.2(6) . . ? C28 N10 Cr1 120.2(5) . . ? C27 N10 Cr1 118.3(5) . . ? C28 N11 C29 116.5(7) . . ? C28 N11 Cr1 71.6(5) . . ? C29 N11 Cr1 169.3(5) . . ? C31 N12 C29 116.7(8) . . ? C38 N13 C34 119.5(6) . . ? C38 N13 Cr2 118.3(5) . . ? C34 N13 Cr2 122.2(5) . . ? C39 N14 C38 121.9(6) . . ? C39 N14 Cr1 117.7(5) . . ? C38 N14 Cr1 120.3(5) . . ? C39 N15 C40 119.5(7) . . ? C39 N15 Cr1 72.7(4) . . ? C40 N15 Cr1 167.2(5) . . ? C42 N16 C40 115.4(8) . . ? N1 C1 C2 122.7(8) . . ? C3 C2 C1 118.8(8) . . ? C2 C3 C4 119.7(8) . . ? C3 C4 C5 118.2(8) . . ? N1 C5 C4 121.8(8) . . ? N1 C5 N2 112.2(7) . . ? C4 C5 N2 125.8(7) . . ? N2 C6 N3 118.4(7) . . ? N4 C7 C8 122.0(7) . . ? N4 C7 N3 118.3(7) . . ? C8 C7 N3 119.7(7) . . ? C11 C8 C7 119.1(7) . . ? N4 C9 C10 124.8(8) . . ? C11 C10 C9 116.6(7) . . ? C10 C11 C8 120.4(8) . . ? C13 C12 N5 122.4(8) . . ? C12 C13 C14 118.6(8) . . ? C15 C14 C13 120.6(8) . . ? C14 C15 C16 119.4(8) . . ? N5 C16 N6 114.2(7) . . ? N5 C16 C15 119.6(7) . . ? N6 C16 C15 126.2(7) . . ? N7 C17 N6 121.8(7) . . ? N8 C18 C19 122.3(7) . . ? N8 C18 N7 118.3(7) . . ? C19 C18 N7 119.4(8) . . ? C18 C19 C22 120.2(9) . . ? N8 C20 C21 123.9(8) . . ? C22 C21 C20 117.8(8) . . ? C21 C22 C19 118.5(8) . . ? N9 C23 C24 121.2(8) . . ? C23 C24 C25 117.4(8) . . ? C26 C25 C24 121.4(8) . . ? C25 C26 C27 119.2(8) . . ? N9 C27 N10 114.2(7) . . ? N9 C27 C26 119.5(7) . . ? N10 C27 C26 126.2(8) . . ? N11 C28 N10 120.9(7) . . ? N12 C29 C30 121.6(8) . . ? N12 C29 N11 118.5(7) . . ? C30 C29 N11 119.9(8) . . ? C33 C30 C29 120.7(9) . . ? N12 C31 C32 124.9(9) . . ? C31 C32 C33 118.2(9) . . ? C30 C33 C32 117.8(8) . . ? N13 C34 C35 122.6(7) . . ? C34 C35 C36 118.1(8) . . ? C37 C36 C35 119.8(8) . . ? C36 C37 C38 120.2(7) . . ? N13 C38 N14 112.6(6) . . ? N13 C38 C37 119.8(7) . . ? N14 C38 C37 127.6(7) . . ? N15 C39 N14 121.7(7) . . ? N16 C40 C41 122.8(7) . . ? N16 C40 N15 118.7(7) . . ? C41 C40 N15 118.5(7) . . ? C40 C41 C44 118.9(8) . . ? N16 C42 C43 124.6(9) . . ? C44 C43 C42 119.5(8) . . ? C43 C44 C41 118.7(9) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 22.68 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.524 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.090 #===END of CIF for Compound 1 =============== data_cmpd2CH3CN _database_code_CSD 206654 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '(Cr2(DpyF)4)(CuCl2)2, CH3CN' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H39 Cl4 Cr2 Cu2 N17' _chemical_formula_weight 1202.82 _chemical_melting_point ? _chemical_compound_source synthesis 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' N N 0.0061 0.0033 '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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9070(11) _cell_length_b 14.005(2) _cell_length_c 20.237(3) _cell_angle_alpha 92.957(2) _cell_angle_beta 97.270(2) _cell_angle_gamma 90.847(2) _cell_volume 2500.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 988 _cell_measurement_theta_min 2.809 _cell_measurement_theta_max 27.402 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method ? _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.529 _exptl_absorpt_correction_type 'multi scans' _exptl_absorpt_correction_T_min 0.6487 _exptl_absorpt_correction_T_max 0.8714 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method 'w/ scans' _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17352 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11106 _reflns_number_observed 8907 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL V. 5.03 (Siemens, 1994)' _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.8289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11106 _refine_ls_number_parameters 643 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_obs 0.0349 _refine_ls_wR_factor_all 0.0993 _refine_ls_wR_factor_obs 0.0921 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.069 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.069 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr 0.17071(4) 0.22308(2) 0.21034(2) 0.02181(8) Uani 1 d . . Cr2 Cr 0.03438(4) 0.01229(2) 0.25967(2) 0.02252(8) Uani 1 d . . N1 N 0.3724(2) 0.24614(13) 0.17617(9) 0.0260(4) Uani 1 d . . N2 N 0.3079(2) 0.10288(12) 0.20582(8) 0.0241(4) Uani 1 d . . N3 N 0.2309(2) -0.04552(13) 0.23698(9) 0.0261(4) Uani 1 d . . N4 N 0.2108(3) -0.19044(15) 0.28611(12) 0.0479(6) Uani 1 d . . N5 N 0.1476(2) 0.31806(14) 0.06970(10) 0.0341(4) Uani 1 d . . N6 N 0.0609(2) 0.18477(12) 0.11755(8) 0.0239(4) Uani 1 d . . N7 N -0.0124(2) 0.04020(12) 0.15638(8) 0.0239(4) Uani 1 d . . N8 N -0.0789(2) -0.09304(12) 0.20019(9) 0.0270(4) Uani 1 d . . N9 N 0.0694(2) 0.35174(12) 0.21133(8) 0.0257(4) Uani 1 d . . N10 N -0.0463(2) 0.22528(12) 0.24384(8) 0.0235(4) Uani 1 d . . N11 N -0.1529(2) 0.08698(12) 0.27851(8) 0.0245(4) Uani 1 d . . N12 N -0.2798(2) -0.04913(14) 0.30335(10) 0.0363(5) Uani 1 d . . N13 N 0.4467(2) 0.36887(15) 0.31507(11) 0.0414(5) Uani 1 d . . N14 N 0.2560(2) 0.25055(12) 0.30757(8) 0.0254(4) Uani 1 d . . N15 N 0.1577(2) 0.10466(12) 0.33440(8) 0.0247(4) Uani 1 d . . N16 N 0.0579(2) -0.03456(13) 0.35330(9) 0.0270(4) Uani 1 d . . C1 C 0.4531(3) 0.3125(2) 0.14979(11) 0.0317(5) Uani 1 d . . H1A H 0.4199(3) 0.3759(2) 0.14885(11) 0.038 Uiso 1 calc R . C2 C 0.5848(3) 0.2884(2) 0.12392(12) 0.0368(5) Uani 1 d . . H2A H 0.6416(3) 0.3348(2) 0.10527(12) 0.044 Uiso 1 calc R . C3 C 0.6314(3) 0.1944(2) 0.12606(12) 0.0379(6) Uani 1 d . . H3A H 0.7203(3) 0.1772(2) 0.10826(12) 0.045 Uiso 1 calc R . C4 C 0.5500(3) 0.1259(2) 0.15378(11) 0.0332(5) Uani 1 d . . H4A H 0.5820(3) 0.0623(2) 0.15582(11) 0.040 Uiso 1 calc R . C5 C 0.4181(2) 0.1551(2) 0.17863(10) 0.0256(4) Uani 1 d . . C6 C 0.3298(2) 0.0109(2) 0.21483(10) 0.0255(4) Uani 1 d . . H6A H 0.4213(2) -0.0154(2) 0.20478(10) 0.031 Uiso 1 calc R . C7 C 0.2654(3) -0.1445(2) 0.23858(11) 0.0300(5) Uani 1 d . . C8 C 0.3490(3) -0.1892(2) 0.19290(13) 0.0426(6) Uani 1 d . . H8A H 0.3821(3) -0.1554(2) 0.15828(13) 0.051 Uiso 1 calc R . C9 C 0.3821(3) -0.2843(2) 0.19962(15) 0.0507(7) Uani 1 d . . H9A H 0.4396(3) -0.3163(2) 0.16984(15) 0.061 Uiso 1 calc R . C10 C 0.3303(3) -0.3318(2) 0.2501(2) 0.0515(7) Uani 1 d . . H10A H 0.3536(3) -0.3962(2) 0.2565(2) 0.062 Uiso 1 calc R . C11 C 0.2444(4) -0.2828(2) 0.2907(2) 0.0618(9) Uani 1 d . . H11A H 0.2061(4) -0.3161(2) 0.3244(2) 0.074 Uiso 1 calc R . C12 C 0.1374(3) 0.3824(2) 0.02260(13) 0.0421(6) Uani 1 d . . H12A H 0.2115(3) 0.4316(2) 0.02617(13) 0.051 Uiso 1 calc R . C13 C 0.0250(3) 0.3805(2) -0.03052(13) 0.0474(7) Uani 1 d . . H13A H 0.0229(3) 0.4262(2) -0.06303(13) 0.057 Uiso 1 calc R . C14 C -0.0842(4) 0.3097(2) -0.03458(13) 0.0493(7) Uani 1 d . . H14A H -0.1633(4) 0.3066(2) -0.07013(13) 0.059 Uiso 1 calc R . C15 C -0.0781(3) 0.2428(2) 0.01358(12) 0.0380(5) Uani 1 d . . H15A H -0.1532(3) 0.1946(2) 0.01192(12) 0.046 Uiso 1 calc R . C16 C 0.0425(2) 0.2490(2) 0.06449(10) 0.0265(4) Uani 1 d . . C17 C -0.0043(2) 0.09936(15) 0.10819(10) 0.0245(4) Uani 1 d . . H17A H -0.0474(2) 0.07939(15) 0.06478(10) 0.029 Uiso 1 calc R . C18 C -0.0849(2) -0.04933(15) 0.14242(10) 0.0255(4) Uani 1 d . . C19 C -0.1573(3) -0.0920(2) 0.08308(12) 0.0372(5) Uani 1 d . . H19A H -0.1600(3) -0.0615(2) 0.04267(12) 0.045 Uiso 1 calc R . C20 C -0.2246(3) -0.1805(2) 0.08563(13) 0.0438(6) Uani 1 d . . H20A H -0.2766(3) -0.2105(2) 0.04655(13) 0.053 Uiso 1 calc R . C21 C -0.2165(3) -0.2265(2) 0.14567(13) 0.0410(6) Uani 1 d . . H21A H -0.2605(3) -0.2877(2) 0.14717(13) 0.049 Uiso 1 calc R . C22 C -0.1431(3) -0.1803(2) 0.20228(12) 0.0333(5) Uani 1 d . . H22A H -0.1375(3) -0.2100(2) 0.24312(12) 0.040 Uiso 1 calc R . C23 C 0.5038(3) 0.4542(2) 0.3407(2) 0.0515(7) Uani 1 d . . H23A H 0.5964(3) 0.4747(2) 0.3280(2) 0.062 Uiso 1 calc R . C24 C 0.4374(3) 0.5132(2) 0.38388(13) 0.0443(6) Uani 1 d . . H24A H 0.4835(3) 0.5718(2) 0.40087(13) 0.053 Uiso 1 calc R . C25 C 0.3017(3) 0.4839(2) 0.40139(13) 0.0454(6) Uani 1 d . . H25A H 0.2516(3) 0.5230(2) 0.43040(13) 0.055 Uiso 1 calc R . C26 C 0.2381(3) 0.3970(2) 0.37648(13) 0.0397(6) Uani 1 d . . H26A H 0.1444(3) 0.3759(2) 0.38782(13) 0.048 Uiso 1 calc R . C27 C 0.3167(2) 0.34140(15) 0.33414(10) 0.0267(4) Uani 1 d . . C28 C 0.2272(2) 0.1888(2) 0.35128(10) 0.0267(4) Uani 1 d . . H28A H 0.2571(2) 0.2048(2) 0.39676(10) 0.032 Uiso 1 calc R . C29 C 0.1415(2) 0.0404(2) 0.38338(10) 0.0259(4) Uani 1 d . . C30 C 0.1984(3) 0.0420(2) 0.45074(11) 0.0323(5) Uani 1 d . . H30A H 0.2555(3) 0.0945(2) 0.47184(11) 0.039 Uiso 1 calc R . C31 C 0.1673(3) -0.0370(2) 0.48525(12) 0.0384(6) Uani 1 d . . H31A H 0.2045(3) -0.0386(2) 0.53076(12) 0.046 Uiso 1 calc R . C32 C 0.0820(3) -0.1143(2) 0.45398(12) 0.0372(5) Uani 1 d . . H32A H 0.0617(3) -0.1679(2) 0.47777(12) 0.045 Uiso 1 calc R . C33 C 0.0278(3) -0.1105(2) 0.38730(12) 0.0323(5) Uani 1 d . . H33A H -0.0309(3) -0.1619(2) 0.36547(12) 0.039 Uiso 1 calc R . C34 C 0.0907(3) 0.4439(2) 0.19822(11) 0.0333(5) Uani 1 d . . H34A H 0.1799(3) 0.4630(2) 0.18171(11) 0.040 Uiso 1 calc R . C35 C -0.0171(3) 0.5106(2) 0.20880(12) 0.0388(6) Uani 1 d . . H35A H -0.0014(3) 0.5751(2) 0.20044(12) 0.047 Uiso 1 calc R . C36 C -0.1494(3) 0.4808(2) 0.23202(12) 0.0383(6) Uani 1 d . . H36A H -0.2247(3) 0.5255(2) 0.23835(12) 0.046 Uiso 1 calc R . C37 C -0.1721(3) 0.3867(2) 0.24593(11) 0.0324(5) Uani 1 d . . H37A H -0.2608(3) 0.3663(2) 0.26225(11) 0.039 Uiso 1 calc R . C38 C -0.0578(2) 0.32288(15) 0.23477(10) 0.0247(4) Uani 1 d . . C39 C -0.1561(2) 0.17915(15) 0.26855(10) 0.0245(4) Uani 1 d . . H39A H -0.2399(2) 0.21385(15) 0.27943(10) 0.029 Uiso 1 calc R . C40 C -0.2702(2) 0.0459(2) 0.31032(10) 0.0251(4) Uani 1 d . . C41 C -0.3626(3) 0.0992(2) 0.34853(11) 0.0303(5) Uani 1 d . . H41A H -0.3546(3) 0.1663(2) 0.35260(11) 0.036 Uiso 1 calc R . C42 C -0.4664(3) 0.0500(2) 0.38022(12) 0.0341(5) Uani 1 d . . H42A H -0.5301(3) 0.0840(2) 0.40627(12) 0.041 Uiso 1 calc R . C43 C -0.4770(3) -0.0480(2) 0.37388(12) 0.0353(5) Uani 1 d . . H43A H -0.5462(3) -0.0822(2) 0.39553(12) 0.042 Uiso 1 calc R . C44 C -0.3824(3) -0.0941(2) 0.33459(13) 0.0391(6) Uani 1 d . . H44A H -0.3901(3) -0.1611(2) 0.32929(13) 0.047 Uiso 1 calc R . Cu1 Cu 0.5000 0.5000 0.0000 0.04948(13) Uani 1 d S . Cu2 Cu 0.5000 0.0000 0.0000 0.0573(2) Uani 1 d S . Cu3 Cu -0.33914(4) -0.70931(2) 0.46763(2) 0.04622(10) Uani 1 d . . Cl1 Cl 0.55970(13) 0.54179(6) 0.10078(4) 0.0726(3) Uani 1 d . . Cl2 Cl 0.31660(10) -0.04246(6) 0.04953(4) 0.0640(2) Uani 1 d . . Cl6 Cl -0.14384(9) -0.68069(6) 0.42202(4) 0.0586(2) Uani 1 d . . Cl7 Cl -0.53112(9) -0.74589(5) 0.51235(4) 0.0515(2) Uani 1 d . . C1S C -0.1661(4) 0.6373(2) 0.3829(2) 0.0566(8) Uani 1 d . . C2S C -0.1545(4) 0.5903(3) 0.4461(2) 0.0683(9) Uani 1 d . . N1S N -0.1774(5) 0.6734(2) 0.3340(2) 0.0925(12) Uani 1 d . . 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 Cr1 0.0226(2) 0.0198(2) 0.0234(2) 0.00307(12) 0.00403(12) -0.00390(12) Cr2 0.0245(2) 0.0196(2) 0.0237(2) 0.00356(12) 0.00382(13) -0.00288(13) N1 0.0227(9) 0.0265(9) 0.0290(9) 0.0041(7) 0.0040(7) -0.0052(7) N2 0.0224(9) 0.0245(9) 0.0255(8) 0.0034(7) 0.0030(7) -0.0037(7) N3 0.0263(9) 0.0232(9) 0.0288(9) 0.0042(7) 0.0021(7) -0.0010(7) N4 0.0589(15) 0.0267(11) 0.0648(15) 0.0135(10) 0.0284(12) 0.0040(10) N5 0.0357(11) 0.0314(11) 0.0360(10) 0.0094(8) 0.0053(8) -0.0055(8) N6 0.0239(9) 0.0253(9) 0.0231(8) 0.0051(7) 0.0039(7) -0.0026(7) N7 0.0247(9) 0.0221(9) 0.0250(8) 0.0019(7) 0.0035(7) -0.0029(7) N8 0.0284(9) 0.0216(9) 0.0317(9) 0.0012(7) 0.0070(8) -0.0038(7) N9 0.0292(9) 0.0223(9) 0.0259(9) 0.0035(7) 0.0043(7) -0.0035(7) N10 0.0255(9) 0.0204(9) 0.0249(8) 0.0011(7) 0.0045(7) -0.0032(7) N11 0.0239(9) 0.0234(9) 0.0270(9) 0.0033(7) 0.0059(7) -0.0035(7) N12 0.0388(11) 0.0254(10) 0.0474(12) 0.0046(8) 0.0157(9) -0.0042(8) N13 0.0396(12) 0.0330(11) 0.0525(13) -0.0101(9) 0.0152(10) -0.0134(9) N14 0.0267(9) 0.0226(9) 0.0260(9) 0.0021(7) 0.0010(7) -0.0045(7) N15 0.0263(9) 0.0241(9) 0.0238(8) 0.0035(7) 0.0032(7) -0.0035(7) N16 0.0304(10) 0.0244(9) 0.0274(9) 0.0065(7) 0.0064(7) -0.0012(7) C1 0.0300(12) 0.0292(12) 0.0359(12) 0.0069(9) 0.0038(9) -0.0083(9) C2 0.0284(12) 0.0440(14) 0.0395(13) 0.0118(11) 0.0080(10) -0.0116(10) C3 0.0238(12) 0.049(2) 0.0419(13) 0.0053(11) 0.0094(10) -0.0033(10) C4 0.0267(12) 0.0375(13) 0.0357(12) 0.0032(10) 0.0043(9) 0.0001(10) C5 0.0225(10) 0.0300(11) 0.0236(10) 0.0029(8) 0.0000(8) -0.0051(8) C6 0.0227(10) 0.0277(11) 0.0255(10) 0.0022(8) 0.0009(8) -0.0001(8) C7 0.0288(11) 0.0247(11) 0.0359(12) 0.0045(9) 0.0000(9) 0.0008(9) C8 0.055(2) 0.0322(13) 0.0426(14) 0.0023(11) 0.0123(12) 0.0040(12) C9 0.056(2) 0.0370(15) 0.060(2) -0.0027(13) 0.0104(14) 0.0105(13) C10 0.059(2) 0.0253(13) 0.071(2) 0.0075(13) 0.0066(15) 0.0080(12) C11 0.080(2) 0.0322(15) 0.081(2) 0.0214(15) 0.033(2) 0.0046(15) C12 0.050(2) 0.0341(14) 0.0447(14) 0.0130(11) 0.0121(12) -0.0073(11) C13 0.067(2) 0.0395(15) 0.0374(13) 0.0183(11) 0.0070(13) 0.0024(13) C14 0.060(2) 0.051(2) 0.0343(13) 0.0121(12) -0.0094(12) -0.0010(14) C15 0.0378(13) 0.0396(14) 0.0352(12) 0.0099(10) -0.0028(10) -0.0068(11) C16 0.0293(11) 0.0272(11) 0.0242(10) 0.0045(8) 0.0068(8) -0.0003(9) C17 0.0241(10) 0.0262(11) 0.0235(10) 0.0017(8) 0.0044(8) -0.0001(8) C18 0.0247(11) 0.0213(10) 0.0309(11) 0.0002(8) 0.0055(8) -0.0006(8) C19 0.0437(14) 0.0350(13) 0.0318(12) -0.0004(10) 0.0021(10) -0.0051(11) C20 0.049(2) 0.0362(14) 0.0424(14) -0.0094(11) -0.0016(12) -0.0108(12) C21 0.0439(15) 0.0262(12) 0.053(2) -0.0047(11) 0.0097(12) -0.0108(10) C22 0.0392(13) 0.0222(11) 0.0400(12) 0.0025(9) 0.0113(10) -0.0055(9) C23 0.046(2) 0.039(2) 0.071(2) -0.0126(13) 0.0183(14) -0.0191(12) C24 0.054(2) 0.0283(13) 0.0486(15) -0.0062(11) 0.0040(13) -0.0121(11) C25 0.058(2) 0.0340(14) 0.0451(14) -0.0091(11) 0.0143(13) -0.0032(12) C26 0.0420(14) 0.0333(13) 0.0450(14) -0.0044(11) 0.0136(11) -0.0080(11) C27 0.0307(11) 0.0232(11) 0.0249(10) 0.0024(8) -0.0012(8) -0.0040(9) C28 0.0267(11) 0.0271(11) 0.0257(10) 0.0006(8) 0.0020(8) -0.0028(8) C29 0.0247(11) 0.0270(11) 0.0270(10) 0.0041(8) 0.0064(8) -0.0011(8) C30 0.0289(12) 0.0410(14) 0.0277(11) 0.0055(9) 0.0060(9) -0.0045(10) C31 0.0356(13) 0.053(2) 0.0279(11) 0.0139(10) 0.0050(10) 0.0008(11) C32 0.0426(14) 0.0358(13) 0.0368(12) 0.0169(10) 0.0123(11) 0.0049(11) C33 0.0360(13) 0.0258(11) 0.0370(12) 0.0085(9) 0.0098(10) -0.0011(9) C34 0.0404(13) 0.0255(11) 0.0353(12) 0.0065(9) 0.0078(10) -0.0065(10) C35 0.053(2) 0.0193(11) 0.0447(14) 0.0070(10) 0.0077(12) -0.0027(10) C36 0.0455(14) 0.0275(12) 0.0428(13) 0.0027(10) 0.0078(11) 0.0082(10) C37 0.0353(13) 0.0276(12) 0.0351(12) 0.0027(9) 0.0073(10) 0.0034(9) C38 0.0287(11) 0.0225(10) 0.0224(9) 0.0016(8) 0.0022(8) -0.0034(8) C39 0.0245(10) 0.0250(11) 0.0243(10) 0.0023(8) 0.0040(8) -0.0011(8) C40 0.0219(10) 0.0287(11) 0.0246(10) 0.0046(8) 0.0015(8) -0.0051(8) C41 0.0307(12) 0.0259(11) 0.0352(12) 0.0017(9) 0.0079(9) -0.0032(9) C42 0.0265(12) 0.0413(14) 0.0361(12) 0.0054(10) 0.0094(9) -0.0023(10) C43 0.0277(12) 0.0414(14) 0.0381(12) 0.0111(10) 0.0063(10) -0.0069(10) C44 0.0388(14) 0.0291(13) 0.0513(15) 0.0085(11) 0.0116(11) -0.0085(10) Cu1 0.0547(3) 0.0347(3) 0.0609(3) -0.0024(2) 0.0174(2) -0.0079(2) Cu2 0.0724(4) 0.0517(3) 0.0433(3) 0.0107(2) -0.0114(2) -0.0192(3) Cu3 0.0510(2) 0.0403(2) 0.0454(2) 0.00060(14) 0.0002(2) -0.0076(2) Cl1 0.1116(8) 0.0407(4) 0.0647(5) -0.0061(4) 0.0137(5) -0.0116(4) Cl2 0.0804(6) 0.0668(5) 0.0403(4) 0.0105(3) -0.0102(4) -0.0260(4) Cl6 0.0557(4) 0.0633(5) 0.0555(4) 0.0073(3) 0.0028(3) -0.0188(4) Cl7 0.0569(4) 0.0466(4) 0.0502(4) -0.0033(3) 0.0066(3) -0.0068(3) C1S 0.070(2) 0.036(2) 0.064(2) -0.0067(14) 0.018(2) -0.0156(14) C2S 0.074(2) 0.072(2) 0.056(2) 0.013(2) -0.005(2) -0.007(2) N1S 0.169(4) 0.044(2) 0.071(2) 0.0068(15) 0.039(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.032(2) . y Cr1 N2 2.100(2) . y Cr1 N6 2.046(2) . y Cr1 N9 2.027(2) . y Cr1 N10 2.128(2) . y Cr1 N14 2.033(2) . y Cr2 N3 2.034(2) . y Cr2 N7 2.137(2) . y Cr2 N8 2.027(2) . y Cr2 N11 2.048(2) . y Cr2 N15 2.122(2) . y Cr2 N16 2.024(2) . y N1 C1 1.339(3) . ? N1 C5 1.346(3) . ? N2 C6 1.325(3) . ? N2 C5 1.399(3) . ? N3 C6 1.311(3) . ? N3 C7 1.425(3) . ? N4 C7 1.323(3) . ? N4 C11 1.337(3) . ? N5 C16 1.327(3) . ? N5 C12 1.341(3) . ? N6 C17 1.316(3) . ? N6 C16 1.431(3) . ? N7 C17 1.320(3) . ? N7 C18 1.401(3) . ? N8 C18 1.343(3) . ? N8 C22 1.347(3) . ? N9 C38 1.347(3) . ? N9 C34 1.347(3) . ? N10 C39 1.327(3) . ? N10 C38 1.392(3) . ? N11 C39 1.317(3) . ? N11 C40 1.424(3) . ? N12 C40 1.332(3) . ? N12 C44 1.342(3) . ? N13 C27 1.324(3) . ? N13 C23 1.344(3) . ? N14 C28 1.314(3) . ? N14 C27 1.427(3) . ? N15 C28 1.331(3) . ? N15 C29 1.392(3) . ? N16 C33 1.338(3) . ? N16 C29 1.350(3) . ? C1 C2 1.384(3) . ? C2 C3 1.387(4) . ? C3 C4 1.378(3) . ? C4 C5 1.394(3) . ? C7 C8 1.389(3) . ? C8 C9 1.378(4) . ? C9 C10 1.371(4) . ? C10 C11 1.359(4) . ? C12 C13 1.372(4) . ? C13 C14 1.371(4) . ? C14 C15 1.383(3) . ? C15 C16 1.390(3) . ? C18 C19 1.390(3) . ? C19 C20 1.375(4) . ? C20 C21 1.399(4) . ? C21 C22 1.371(3) . ? C23 C24 1.366(4) . ? C24 C25 1.365(4) . ? C25 C26 1.379(3) . ? C26 C27 1.389(3) . ? C29 C30 1.392(3) . ? C30 C31 1.381(3) . ? C31 C32 1.389(4) . ? C32 C33 1.378(3) . ? C34 C35 1.377(3) . ? C35 C36 1.389(4) . ? C36 C37 1.379(3) . ? C37 C38 1.396(3) . ? C40 C41 1.397(3) . ? C41 C42 1.384(3) . ? C42 C43 1.373(3) . ? C43 C44 1.376(3) . ? Cu1 Cl1 2.0923(9) 2_665 y Cu1 Cl1 2.0925(9) . y Cu2 Cl2 2.1151(9) 2_655 y Cu2 Cl2 2.1152(9) . y Cu3 Cl7 2.1022(8) . y Cu3 Cl6 2.1125(9) . y C1S N1S 1.127(4) . ? C1S C2S 1.462(5) . ? 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 _geom_angle_publ_flag N1 Cr1 N2 64.70(7) . . y N1 Cr1 N6 93.57(7) . . y N1 Cr1 N9 105.72(7) . . y N1 Cr1 N10 169.82(7) . . y N1 Cr1 N14 93.95(7) . . y N2 Cr1 N6 90.28(7) . . y N2 Cr1 N9 170.31(7) . . y N2 Cr1 N10 125.48(7) . . y N2 Cr1 N14 90.13(7) . . y N6 Cr1 N9 91.93(7) . . y N6 Cr1 N10 86.94(7) . . y N6 Cr1 N14 171.86(7) . . y N9 Cr1 N10 64.09(7) . . y N9 Cr1 N14 89.02(7) . . y N10 Cr1 N14 86.20(7) . . y N3 Cr2 N7 86.58(7) . . y N3 Cr2 N8 88.19(7) . . y N3 Cr2 N11 172.49(7) . . y N3 Cr2 N15 90.22(7) . . y N3 Cr2 N16 94.13(7) . . y N7 Cr2 N8 64.09(7) . . y N7 Cr2 N11 89.90(7) . . y N7 Cr2 N15 125.50(7) . . y N7 Cr2 N16 170.38(7) . . y N8 Cr2 N11 96.24(7) . . y N8 Cr2 N15 170.17(7) . . y N8 Cr2 N16 106.32(7) . . y N11 Cr2 N15 86.42(7) . . y N11 Cr2 N16 90.45(7) . . y N15 Cr2 N16 64.11(7) . . y C1 N1 C5 120.9(2) . . ? C1 N1 Cr1 142.5(2) . . ? C5 N1 Cr1 96.20(13) . . ? C6 N2 C5 118.6(2) . . ? C6 N2 Cr1 149.76(15) . . ? C5 N2 Cr1 91.61(12) . . ? C6 N3 C7 116.8(2) . . ? C6 N3 Cr2 117.96(14) . . ? C7 N3 Cr2 125.05(15) . . ? C7 N4 C11 117.2(2) . . ? C16 N5 C12 117.9(2) . . ? C17 N6 C16 119.0(2) . . ? C17 N6 Cr1 117.93(14) . . ? C16 N6 Cr1 122.92(14) . . ? C17 N7 C18 120.2(2) . . ? C17 N7 Cr2 148.85(15) . . ? C18 N7 Cr2 90.97(12) . . ? C18 N8 C22 120.7(2) . . ? C18 N8 Cr2 97.56(13) . . ? C22 N8 Cr2 141.8(2) . . ? C38 N9 C34 120.7(2) . . ? C38 N9 Cr1 97.20(13) . . ? C34 N9 Cr1 142.1(2) . . ? C39 N10 C38 119.6(2) . . ? C39 N10 Cr1 148.92(15) . . ? C38 N10 Cr1 91.38(12) . . ? C39 N11 C40 118.5(2) . . ? C39 N11 Cr2 118.77(14) . . ? C40 N11 Cr2 122.16(13) . . ? C40 N12 C44 117.9(2) . . ? C27 N13 C23 116.3(2) . . ? C28 N14 C27 116.2(2) . . ? C28 N14 Cr1 118.46(14) . . ? C27 N14 Cr1 123.83(13) . . ? C28 N15 C29 119.6(2) . . ? C28 N15 Cr2 148.53(15) . . ? C29 N15 Cr2 91.69(13) . . ? C33 N16 C29 121.0(2) . . ? C33 N16 Cr2 141.5(2) . . ? C29 N16 Cr2 97.33(13) . . ? N1 C1 C2 120.5(2) . . ? C1 C2 C3 118.6(2) . . ? C4 C3 C2 121.3(2) . . ? C3 C4 C5 117.0(2) . . ? N1 C5 C4 121.7(2) . . ? N1 C5 N2 107.4(2) . . ? C4 C5 N2 130.9(2) . . ? N3 C6 N2 123.5(2) . . ? N4 C7 C8 122.7(2) . . ? N4 C7 N3 115.1(2) . . ? C8 C7 N3 122.1(2) . . ? C9 C8 C7 118.3(3) . . ? C10 C9 C8 119.4(3) . . ? C11 C10 C9 117.9(3) . . ? N4 C11 C10 124.4(3) . . ? N5 C12 C13 123.7(3) . . ? C14 C13 C12 117.7(2) . . ? C13 C14 C15 120.1(2) . . ? C14 C15 C16 118.0(2) . . ? N5 C16 C15 122.6(2) . . ? N5 C16 N6 114.0(2) . . ? C15 C16 N6 123.4(2) . . ? N6 C17 N7 123.6(2) . . ? N8 C18 C19 121.5(2) . . ? N8 C18 N7 107.4(2) . . ? C19 C18 N7 131.1(2) . . ? C20 C19 C18 117.6(2) . . ? C19 C20 C21 120.8(2) . . ? C22 C21 C20 118.5(2) . . ? N8 C22 C21 120.9(2) . . ? N13 C23 C24 124.9(3) . . ? C25 C24 C23 117.4(2) . . ? C24 C25 C26 120.0(2) . . ? C25 C26 C27 118.0(2) . . ? N13 C27 C26 123.4(2) . . ? N13 C27 N14 116.6(2) . . ? C26 C27 N14 120.0(2) . . ? N14 C28 N15 123.3(2) . . ? N16 C29 C30 121.4(2) . . ? N16 C29 N15 106.8(2) . . ? C30 C29 N15 131.7(2) . . ? C31 C30 C29 117.1(2) . . ? C30 C31 C32 121.3(2) . . ? C33 C32 C31 118.5(2) . . ? N16 C33 C32 120.7(2) . . ? N9 C34 C35 120.5(2) . . ? C34 C35 C36 118.9(2) . . ? C37 C36 C35 121.0(2) . . ? C36 C37 C38 117.2(2) . . ? N9 C38 N10 107.3(2) . . ? N9 C38 C37 121.6(2) . . ? N10 C38 C37 131.1(2) . . ? N11 C39 N10 123.0(2) . . ? N12 C40 C41 122.3(2) . . ? N12 C40 N11 114.0(2) . . ? C41 C40 N11 123.6(2) . . ? C42 C41 C40 118.0(2) . . ? C43 C42 C41 120.4(2) . . ? C42 C43 C44 117.4(2) . . ? N12 C44 C43 124.0(2) . . ? Cl1 Cu1 Cl1 180.0 2_665 . y Cl2 Cu2 Cl2 179.997(1) 2_655 . y Cl7 Cu3 Cl6 176.83(4) . . y N1S C1S C2S 178.9(4) . . ? _refine_diff_density_max 0.561 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.063 #===END of CIF for Compound 2.CH3CN ========== data_cmpd2acetone2 _database_code_CSD 206655 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Cr2(DpyF)4)(CuCl2)2, 2acetone' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H48 Cl4 Cr2 Cu2 N16 O2' _chemical_formula_weight 1277.92 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5393(7) _cell_length_b 17.3743(14) _cell_length_c 18.7599(15) _cell_angle_alpha 94.327(2) _cell_angle_beta 96.490(2) _cell_angle_gamma 95.157(2) _cell_volume 2743.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4422 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.89 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6399 _exptl_absorpt_correction_T_max 0.8914 _exptl_absorpt_process_details SADABS _exptl_special_details ; One of the [CuCl2]~-~ anions, and the acetone solvent molecules are disordered. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Buker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15628 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9537 _reflns_number_gt 6507 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+8.8228P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9537 _refine_ls_number_parameters 711 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1552 _refine_ls_wR_factor_gt 0.1351 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr2 Cr 0.62571(9) 0.15134(5) 0.25866(4) 0.0253(2) Uani 1 1 d . A . Cr1 Cr 0.78137(9) 0.33859(5) 0.25589(4) 0.0254(2) Uani 1 1 d . A . N1 N 0.6823(5) 0.4366(2) 0.2842(2) 0.0291(10) Uani 1 1 d . . . N2 N 0.5584(5) 0.3217(2) 0.2948(2) 0.0252(9) Uani 1 1 d . . . N3 N 0.4384(5) 0.1971(2) 0.2999(2) 0.0261(10) Uani 1 1 d . . . N4 N 0.2638(5) 0.0854(3) 0.2899(3) 0.0361(11) Uani 1 1 d . . . N5 N 0.9993(6) 0.4595(3) 0.3800(3) 0.0488(14) Uani 1 1 d . . . N6 N 0.8890(5) 0.3303(2) 0.3576(2) 0.0268(10) Uani 1 1 d . . . N7 N 0.7621(5) 0.2058(2) 0.3542(2) 0.0278(10) Uani 1 1 d . . . N8 N 0.6434(5) 0.0865(2) 0.3441(2) 0.0296(10) Uani 1 1 d . . . N9 N 0.9892(5) 0.3764(2) 0.2212(2) 0.0272(10) Uani 1 1 d . . . N10 N 0.9224(5) 0.2506(2) 0.2222(2) 0.0251(9) Uani 1 1 d . . . N11 N 0.8267(5) 0.1207(2) 0.2189(2) 0.0270(10) Uani 1 1 d . . . N12 N 0.7588(6) -0.0099(3) 0.2271(3) 0.0434(13) Uani 1 1 d . . . N14 N 0.6755(5) 0.3304(2) 0.1523(2) 0.0263(10) Uani 1 1 d . . . N15 N 0.5756(5) 0.2036(2) 0.1615(2) 0.0270(10) Uani 1 1 d . . . N16 N 0.4929(5) 0.0830(2) 0.1771(2) 0.0300(10) Uani 1 1 d . . . C1 C 0.7050(7) 0.5143(3) 0.2874(3) 0.0389(14) Uani 1 1 d . . . H1A H 0.7943 0.5381 0.2698 0.047 Uiso 1 1 calc R . . C2 C 0.6003(8) 0.5592(3) 0.3160(4) 0.0465(16) Uani 1 1 d . . . H2A H 0.6171 0.6136 0.3181 0.056 Uiso 1 1 calc R . . C3 C 0.4694(7) 0.5235(3) 0.3416(4) 0.0445(16) Uani 1 1 d . . . H3A H 0.3975 0.5541 0.3619 0.053 Uiso 1 1 calc R . . C4 C 0.4426(7) 0.4444(3) 0.3379(3) 0.0413(15) Uani 1 1 d . . . H4A H 0.3537 0.4198 0.3553 0.050 Uiso 1 1 calc R . . C5 C 0.5530(6) 0.4017(3) 0.3073(3) 0.0285(12) Uani 1 1 d . . . C6 C 0.4440(6) 0.2724(3) 0.3121(3) 0.0281(12) Uani 1 1 d . . . H6A H 0.3619 0.2929 0.3345 0.034 Uiso 1 1 calc R . . C7 C 0.3190(6) 0.1512(3) 0.3291(3) 0.0282(12) Uani 1 1 d . . . C8 C 0.2687(7) 0.1727(3) 0.3949(3) 0.0408(15) Uani 1 1 d . . . H8A H 0.3138 0.2184 0.4224 0.049 Uiso 1 1 calc R . . C9 C 0.1508(7) 0.1251(4) 0.4190(4) 0.0482(16) Uani 1 1 d . . . H9A H 0.1125 0.1386 0.4629 0.058 Uiso 1 1 calc R . . C10 C 0.0904(7) 0.0578(4) 0.3782(4) 0.0454(16) Uani 1 1 d . . . H10A H 0.0088 0.0249 0.3930 0.055 Uiso 1 1 calc R . . C11 C 0.1514(7) 0.0398(3) 0.3160(3) 0.0401(14) Uani 1 1 d . . . H11A H 0.1129 -0.0075 0.2894 0.048 Uiso 1 1 calc R . . C12 C 1.1046(9) 0.5140(4) 0.4207(5) 0.062(2) Uani 1 1 d . . . H12A H 1.1028 0.5659 0.4098 0.074 Uiso 1 1 calc R . . C13 C 1.2104(9) 0.4988(5) 0.4752(4) 0.065(2) Uani 1 1 d . . . H13A H 1.2773 0.5388 0.5027 0.078 Uiso 1 1 calc R . . C14 C 1.2174(8) 0.4216(5) 0.4893(4) 0.061(2) Uani 1 1 d . . . H14A H 1.2931 0.4085 0.5256 0.073 Uiso 1 1 calc R . . C15 C 1.1141(7) 0.3646(4) 0.4504(3) 0.0397(14) Uani 1 1 d . . . H15A H 1.1181 0.3123 0.4592 0.048 Uiso 1 1 calc R . . C16 C 1.0045(6) 0.3862(3) 0.3982(3) 0.0320(13) Uani 1 1 d . . . C17 C 0.8527(6) 0.2661(3) 0.3879(3) 0.0281(12) Uani 1 1 d . . . H17A H 0.8937 0.2632 0.4362 0.034 Uiso 1 1 calc R . . C18 C 0.7262(6) 0.1410(3) 0.3918(3) 0.0271(11) Uani 1 1 d . . . C19 C 0.7599(7) 0.1293(3) 0.4637(3) 0.0362(13) Uani 1 1 d . . . H19A H 0.8134 0.1688 0.4970 0.043 Uiso 1 1 calc R . . C20 C 0.7120(7) 0.0574(4) 0.4850(3) 0.0451(15) Uani 1 1 d . . . H20A H 0.7337 0.0471 0.5334 0.054 Uiso 1 1 calc R . . C21 C 0.6317(7) 0.0000(3) 0.4347(3) 0.0437(15) Uani 1 1 d . . . H21A H 0.6010 -0.0495 0.4486 0.052 Uiso 1 1 calc R . . C22 C 0.5983(7) 0.0168(3) 0.3651(3) 0.0369(14) Uani 1 1 d . . . H22A H 0.5424 -0.0213 0.3312 0.044 Uiso 1 1 calc R . . C27 C 0.7039(6) 0.3879(3) 0.1043(3) 0.0311(12) Uani 0.39(3) 1 d PGD A 1 N13 N 0.699(2) 0.4642(4) 0.1316(10) 0.046(3) Uani 0.39(3) 1 d PGD A 1 C23 C 0.735(4) 0.5248(4) 0.0901(17) 0.059(5) Uani 0.39(3) 1 d PGD A 1 H23 H 0.7320 0.5764 0.1086 0.070 Uiso 0.39(3) 1 calc PR A 1 C24 C 0.777(4) 0.5092(14) 0.0214(16) 0.059(3) Uani 0.39(3) 1 d PGD A 1 H24 H 0.8023 0.5503 -0.0066 0.070 Uiso 0.39(3) 1 calc PR A 1 C25 C 0.783(4) 0.4330(17) -0.0058(9) 0.050(3) Uani 0.39(3) 1 d PGD A 1 H25 H 0.8111 0.4225 -0.0523 0.060 Uiso 0.39(3) 1 calc PR A 1 C26 C 0.746(3) 0.3723(10) 0.0356(5) 0.032(3) Uani 0.39(3) 1 d PGD A 1 H26 H 0.7494 0.3208 0.0171 0.038 Uiso 0.39(3) 1 calc PR A 1 C27' C 0.7039(6) 0.3879(3) 0.1043(3) 0.0311(12) Uani 0.61(3) 1 d PD A 2 N13' N 0.637(2) 0.4542(6) 0.1198(7) 0.046(3) Uani 0.61(3) 1 d PD A 2 C23' C 0.663(3) 0.5117(7) 0.0756(10) 0.059(5) Uani 0.61(3) 1 d PD A 2 H23' H 0.6226 0.5593 0.0856 0.070 Uiso 0.61(3) 1 calc PR A 2 C24' C 0.746(3) 0.5035(10) 0.0171(11) 0.059(3) Uani 0.61(3) 1 d PD A 2 H24A H 0.7552 0.5437 -0.0135 0.070 Uiso 0.61(3) 1 calc PR A 2 C25' C 0.816(2) 0.4356(11) 0.0036(8) 0.050(3) Uani 0.61(3) 1 d PD A 2 H25A H 0.8759 0.4298 -0.0351 0.060 Uiso 0.61(3) 1 calc PR A 2 C26' C 0.7944(18) 0.3763(8) 0.0483(6) 0.032(3) Uani 0.61(3) 1 d PD A 2 H26' H 0.8401 0.3296 0.0408 0.038 Uiso 0.61(3) 1 calc PR A 2 C28 C 0.6021(6) 0.2642(3) 0.1236(3) 0.0283(12) Uani 1 1 d . A . H28A H 0.5664 0.2592 0.0740 0.034 Uiso 1 1 calc R . . C29 C 0.4940(6) 0.1350(3) 0.1279(3) 0.0311(13) Uani 1 1 d . A . C30 C 0.4229(7) 0.1157(4) 0.0572(3) 0.0413(15) Uani 1 1 d . . . H30A H 0.4235 0.1521 0.0226 0.050 Uiso 1 1 calc R A . C31 C 0.3519(7) 0.0411(4) 0.0402(4) 0.0494(17) Uani 1 1 d . A . H31A H 0.3022 0.0262 -0.0068 0.059 Uiso 1 1 calc R . . C32 C 0.3530(7) -0.0122(4) 0.0916(4) 0.0462(16) Uani 1 1 d . . . H32A H 0.3068 -0.0634 0.0796 0.055 Uiso 1 1 calc R A . C33 C 0.4223(7) 0.0109(3) 0.1599(3) 0.0376(14) Uani 1 1 d . A . H33A H 0.4204 -0.0243 0.1955 0.045 Uiso 1 1 calc R . . C34 C 1.0742(7) 0.4409(3) 0.2072(3) 0.0355(13) Uani 1 1 d . . . H34A H 1.0383 0.4894 0.2186 0.043 Uiso 1 1 calc R . . C35 C 1.2110(6) 0.4380(3) 0.1770(3) 0.0368(14) Uani 1 1 d . . . H35A H 1.2696 0.4837 0.1675 0.044 Uiso 1 1 calc R . . C36 C 1.2622(6) 0.3659(3) 0.1605(3) 0.0390(14) Uani 1 1 d . . . H36A H 1.3567 0.3629 0.1396 0.047 Uiso 1 1 calc R . . C37 C 1.1770(6) 0.2988(3) 0.1743(3) 0.0326(13) Uani 1 1 d . . . H37A H 1.2121 0.2499 0.1637 0.039 Uiso 1 1 calc R . . C38 C 1.0364(6) 0.3058(3) 0.2047(3) 0.0257(11) Uani 1 1 d . . . C39 C 0.9357(6) 0.1755(3) 0.2084(3) 0.0282(12) Uani 1 1 d . . . H39A H 1.0277 0.1609 0.1901 0.034 Uiso 1 1 calc R . . C40 C 0.8449(6) 0.0422(3) 0.1958(3) 0.0330(13) Uani 1 1 d . . . C41 C 0.9380(7) 0.0213(3) 0.1424(3) 0.0376(14) Uani 1 1 d . . . H41A H 0.9959 0.0593 0.1202 0.045 Uiso 1 1 calc R . . C42 C 0.9428(8) -0.0564(3) 0.1231(4) 0.0476(16) Uani 1 1 d . . . H42A H 1.0065 -0.0721 0.0880 0.057 Uiso 1 1 calc R . . C43 C 0.8554(8) -0.1105(4) 0.1548(4) 0.0552(19) Uani 1 1 d . . . H43A H 0.8568 -0.1638 0.1419 0.066 Uiso 1 1 calc R . . C44 C 0.7649(8) -0.0849(4) 0.2062(4) 0.0549(18) Uani 1 1 d . . . H44A H 0.7039 -0.1222 0.2279 0.066 Uiso 1 1 calc R . . Cl3 Cl 0.2956(2) 0.28964(10) -0.02388(10) 0.0598(5) Uani 1 1 d . . . Cu2 Cu 0.08759(10) 0.23198(5) 0.00491(4) 0.0509(2) Uani 1 1 d . . . Cl4 Cl -0.1221(2) 0.17175(9) 0.02962(9) 0.0535(4) Uani 1 1 d . . . Cl1 Cl 0.4759(10) 0.1955(3) 0.6685(3) 0.138(2) Uani 0.526(2) 1 d P B 1 Cu1 Cu 0.5269(3) 0.25482(14) 0.58006(15) 0.0708(6) Uani 0.526(2) 1 d P B 1 Cl2 Cl 0.585(3) 0.3164(15) 0.4928(13) 0.071(3) Uani 0.526(2) 1 d P B 1 Cl1A Cl 0.6513(11) 0.1581(4) 0.6743(3) 0.138(2) Uani 0.474(2) 1 d P B 2 Cu1A Cu 0.6091(4) 0.23377(16) 0.59440(17) 0.0708(6) Uani 0.474(2) 1 d P B 2 Cl2A Cl 0.566(4) 0.3074(17) 0.5104(14) 0.071(3) Uani 0.474(2) 1 d P B 2 O2 O 1.2055(14) 0.6305(6) 0.1962(9) 0.121(5) Uani 0.71 1 d PD C 1 C95 C 1.2807(14) 0.6832(6) 0.1752(5) 0.103(4) Uani 0.71 1 d PDU C 1 C92 C 1.4575(18) 0.685(2) 0.171(2) 0.231(15) Uani 0.71 1 d PDU C 1 H92A H 1.4944 0.6367 0.1867 0.347 Uiso 0.71 1 calc PR C 1 H92B H 1.5129 0.7282 0.2019 0.347 Uiso 0.71 1 calc PR C 1 H92C H 1.4782 0.6898 0.1217 0.347 Uiso 0.71 1 calc PR C 1 C90 C 1.210(3) 0.7550(9) 0.1550(8) 0.243(11) Uani 0.71 1 d PD C 1 H90A H 1.0968 0.7489 0.1587 0.364 Uiso 0.71 1 calc PR C 1 H90B H 1.2262 0.7639 0.1058 0.364 Uiso 0.71 1 calc PR C 1 H90C H 1.2593 0.7989 0.1872 0.364 Uiso 0.71 1 calc PR C 1 C92A C 1.145(6) 0.632(4) 0.195(4) 0.231(15) Uani 0.29 1 d PD D 2 H92D H 1.1810 0.5838 0.2091 0.347 Uiso 0.29 1 calc PR D 2 H92E H 1.0638 0.6220 0.1538 0.347 Uiso 0.29 1 calc PR D 2 H92F H 1.1007 0.6581 0.2347 0.347 Uiso 0.29 1 calc PR D 2 C95A C 1.2807(14) 0.6832(6) 0.1752(5) 0.103(4) Uani 0.29 1 d PD D 2 O2A O 1.420(2) 0.6795(19) 0.167(3) 0.121(5) Uani 0.29 1 d PD D 2 C90A C 1.210(3) 0.7550(9) 0.1550(8) 0.243(11) Uani 0.29 1 d PD D 2 H90D H 1.2911 0.7919 0.1418 0.364 Uiso 0.29 1 calc PR D 2 H90E H 1.1633 0.7776 0.1955 0.364 Uiso 0.29 1 calc PR D 2 H90F H 1.1279 0.7421 0.1144 0.364 Uiso 0.29 1 calc PR D 2 C94 C 1.0500(11) 0.2227(6) 0.6278(5) 0.117(4) Uani 0.50 1 d PD E 1 C93 C 1.028(3) 0.2518(14) 0.5575(9) 0.107(6) Uani 0.50 1 d PDU E 1 H93A H 1.0282 0.2096 0.5206 0.160 Uiso 0.50 1 calc PR E 1 H93B H 1.1140 0.2912 0.5535 0.160 Uiso 0.50 1 calc PR E 1 H93C H 0.9281 0.2742 0.5513 0.160 Uiso 0.50 1 calc PR E 1 C91 C 1.058(3) 0.2874(9) 0.6856(10) 0.270(12) Uani 0.50 1 d PD E 1 H91A H 1.0477 0.2662 0.7315 0.404 Uiso 0.50 1 calc PR E 1 H91B H 0.9717 0.3192 0.6746 0.404 Uiso 0.50 1 calc PR E 1 H91C H 1.1581 0.3190 0.6884 0.404 Uiso 0.50 1 calc PR E 1 O1 O 1.057(3) 0.1555(9) 0.6408(9) 0.261(13) Uani 0.50 1 d PDU E 1 C94A C 1.0500(11) 0.2227(6) 0.6278(5) 0.117(4) Uani 0.50 1 d PD F 2 O1A O 1.064(4) 0.2498(10) 0.5730(8) 0.261(13) Uani 0.50 1 d PD F 2 C91A C 1.058(3) 0.2874(9) 0.6856(10) 0.270(12) Uani 0.50 1 d PD F 2 H91D H 1.1066 0.3346 0.6696 0.404 Uiso 0.50 1 calc PR F 2 H91E H 1.1197 0.2744 0.7288 0.404 Uiso 0.50 1 calc PR F 2 H91F H 0.9512 0.2954 0.6961 0.404 Uiso 0.50 1 calc PR F 2 C93A C 1.022(2) 0.1359(7) 0.6109(13) 0.107(6) Uani 0.50 1 d PD F 2 H93D H 1.0455 0.1226 0.5623 0.160 Uiso 0.50 1 calc PR F 2 H93E H 0.9127 0.1186 0.6147 0.160 Uiso 0.50 1 calc PR F 2 H93F H 1.0910 0.1107 0.6447 0.160 Uiso 0.50 1 calc PR F 2 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 Cr2 0.0257(4) 0.0237(4) 0.0262(5) -0.0006(3) 0.0048(3) 0.0011(3) Cr1 0.0260(4) 0.0238(4) 0.0270(5) 0.0001(3) 0.0072(4) 0.0026(3) N1 0.032(2) 0.026(2) 0.030(2) 0.0009(19) 0.007(2) -0.0010(19) N2 0.026(2) 0.022(2) 0.028(2) 0.0011(18) 0.0040(18) 0.0038(18) N3 0.024(2) 0.026(2) 0.028(2) 0.0000(19) 0.0042(18) -0.0011(18) N4 0.037(3) 0.032(3) 0.038(3) -0.001(2) 0.007(2) -0.004(2) N5 0.048(3) 0.037(3) 0.063(4) 0.001(3) 0.022(3) -0.002(2) N6 0.025(2) 0.028(2) 0.026(2) -0.0045(19) 0.0052(18) 0.0012(18) N7 0.025(2) 0.032(2) 0.025(2) 0.0006(19) 0.0033(18) 0.0011(19) N8 0.032(2) 0.023(2) 0.035(3) 0.003(2) 0.011(2) -0.0001(19) N9 0.029(2) 0.026(2) 0.027(2) 0.0011(19) 0.0071(19) 0.0006(19) N10 0.022(2) 0.026(2) 0.026(2) -0.0018(18) 0.0054(18) -0.0004(18) N11 0.029(2) 0.023(2) 0.030(2) 0.0006(19) 0.0066(19) 0.0043(18) N12 0.048(3) 0.026(3) 0.058(3) 0.001(2) 0.016(3) 0.004(2) N14 0.027(2) 0.029(2) 0.025(2) 0.0029(19) 0.0078(18) 0.0078(19) N15 0.026(2) 0.027(2) 0.027(2) -0.0031(19) 0.0038(18) 0.0034(18) N16 0.031(2) 0.027(2) 0.031(3) -0.004(2) 0.003(2) -0.0005(19) C1 0.037(3) 0.027(3) 0.053(4) 0.001(3) 0.013(3) 0.000(2) C2 0.055(4) 0.022(3) 0.062(4) -0.001(3) 0.009(3) 0.003(3) C3 0.045(4) 0.031(3) 0.060(4) -0.003(3) 0.018(3) 0.014(3) C4 0.033(3) 0.038(3) 0.054(4) -0.005(3) 0.017(3) 0.005(3) C5 0.031(3) 0.032(3) 0.022(3) -0.001(2) 0.003(2) 0.004(2) C6 0.022(3) 0.033(3) 0.030(3) 0.001(2) 0.003(2) 0.003(2) C7 0.021(3) 0.030(3) 0.035(3) 0.005(2) 0.002(2) 0.004(2) C8 0.044(3) 0.037(3) 0.042(4) -0.002(3) 0.017(3) -0.002(3) C9 0.049(4) 0.052(4) 0.048(4) 0.005(3) 0.026(3) 0.001(3) C10 0.035(3) 0.046(4) 0.058(4) 0.015(3) 0.017(3) -0.001(3) C11 0.034(3) 0.032(3) 0.052(4) 0.004(3) 0.001(3) -0.008(3) C12 0.062(5) 0.033(4) 0.092(6) -0.013(4) 0.040(5) -0.008(3) C13 0.050(4) 0.077(6) 0.061(5) -0.037(4) 0.026(4) -0.030(4) C14 0.040(4) 0.099(6) 0.038(4) -0.005(4) 0.001(3) -0.007(4) C15 0.035(3) 0.048(4) 0.034(3) 0.003(3) 0.004(3) -0.003(3) C16 0.034(3) 0.033(3) 0.028(3) -0.008(2) 0.012(2) -0.003(2) C17 0.025(3) 0.032(3) 0.027(3) -0.003(2) 0.002(2) 0.005(2) C18 0.026(3) 0.029(3) 0.028(3) 0.007(2) 0.006(2) 0.006(2) C19 0.037(3) 0.040(3) 0.030(3) 0.005(3) 0.005(3) -0.002(3) C20 0.047(4) 0.055(4) 0.036(4) 0.014(3) 0.010(3) 0.004(3) C21 0.052(4) 0.032(3) 0.051(4) 0.015(3) 0.016(3) -0.001(3) C22 0.037(3) 0.031(3) 0.043(4) 0.004(3) 0.011(3) 0.003(2) C27 0.034(3) 0.031(3) 0.030(3) 0.005(2) 0.005(2) 0.007(2) N13 0.061(9) 0.034(4) 0.051(5) 0.012(3) 0.024(6) 0.015(5) C23 0.093(15) 0.033(5) 0.059(9) 0.016(6) 0.029(10) 0.017(7) C24 0.090(10) 0.045(5) 0.045(5) 0.013(4) 0.018(6) 0.009(5) C25 0.065(9) 0.049(4) 0.037(5) 0.009(4) 0.018(6) -0.003(5) C26 0.025(8) 0.034(4) 0.036(5) 0.003(3) 0.004(5) 0.004(5) C27' 0.034(3) 0.031(3) 0.030(3) 0.005(2) 0.005(2) 0.007(2) N13' 0.061(9) 0.034(4) 0.051(5) 0.012(3) 0.024(6) 0.015(5) C23' 0.093(15) 0.033(5) 0.059(9) 0.016(6) 0.029(10) 0.017(7) C24' 0.090(10) 0.045(5) 0.045(5) 0.013(4) 0.018(6) 0.009(5) C25' 0.065(9) 0.049(4) 0.037(5) 0.009(4) 0.018(6) -0.003(5) C26' 0.025(8) 0.034(4) 0.036(5) 0.003(3) 0.004(5) 0.004(5) C28 0.024(3) 0.037(3) 0.024(3) -0.001(2) 0.003(2) 0.008(2) C29 0.024(3) 0.035(3) 0.033(3) -0.007(3) 0.002(2) 0.008(2) C30 0.041(3) 0.046(4) 0.034(3) -0.005(3) -0.004(3) 0.005(3) C31 0.043(4) 0.057(4) 0.041(4) -0.017(3) -0.007(3) 0.002(3) C32 0.037(3) 0.042(4) 0.055(4) -0.014(3) 0.004(3) -0.004(3) C33 0.037(3) 0.029(3) 0.046(4) -0.006(3) 0.009(3) -0.001(2) C34 0.037(3) 0.030(3) 0.039(3) 0.001(3) 0.009(3) -0.003(2) C35 0.033(3) 0.037(3) 0.039(3) 0.006(3) 0.006(3) -0.007(3) C36 0.026(3) 0.052(4) 0.040(3) 0.004(3) 0.009(3) 0.000(3) C37 0.026(3) 0.033(3) 0.040(3) 0.001(3) 0.007(2) 0.004(2) C38 0.024(3) 0.030(3) 0.022(3) 0.001(2) -0.001(2) 0.001(2) C39 0.027(3) 0.036(3) 0.022(3) 0.000(2) 0.002(2) 0.006(2) C40 0.029(3) 0.028(3) 0.041(3) -0.003(3) -0.002(2) 0.009(2) C41 0.036(3) 0.033(3) 0.044(4) -0.006(3) 0.008(3) 0.005(2) C42 0.051(4) 0.037(4) 0.055(4) -0.011(3) 0.013(3) 0.010(3) C43 0.067(5) 0.027(3) 0.071(5) -0.010(3) 0.008(4) 0.010(3) C44 0.062(4) 0.028(3) 0.076(5) 0.001(3) 0.020(4) 0.001(3) Cl3 0.0661(11) 0.0448(10) 0.0681(12) 0.0075(8) 0.0055(9) 0.0046(8) Cu2 0.0626(5) 0.0408(5) 0.0479(5) -0.0014(4) 0.0024(4) 0.0078(4) Cl4 0.0688(11) 0.0463(9) 0.0438(9) -0.0060(7) 0.0079(8) 0.0033(8) Cl1 0.229(6) 0.087(3) 0.084(3) -0.007(2) 0.030(4) -0.061(3) Cu1 0.0812(17) 0.0491(12) 0.0783(12) -0.0140(9) 0.0198(13) -0.0105(10) Cl2 0.075(6) 0.051(5) 0.086(10) -0.006(5) 0.025(5) -0.007(4) Cl1A 0.229(6) 0.087(3) 0.084(3) -0.007(2) 0.030(4) -0.061(3) Cu1A 0.0812(17) 0.0491(12) 0.0783(12) -0.0140(9) 0.0198(13) -0.0105(10) Cl2A 0.075(6) 0.051(5) 0.086(10) -0.006(5) 0.025(5) -0.007(4) O2 0.113(9) 0.080(7) 0.165(12) -0.031(7) 0.040(8) -0.005(6) C95 0.143(11) 0.103(8) 0.060(6) -0.012(6) -0.006(7) 0.040(8) C92 0.134(18) 0.44(4) 0.14(2) 0.11(2) 0.028(17) 0.05(2) C90 0.40(3) 0.222(18) 0.133(13) 0.061(12) -0.001(16) 0.20(2) C92A 0.134(18) 0.44(4) 0.14(2) 0.11(2) 0.028(17) 0.05(2) C95A 0.143(11) 0.103(8) 0.060(6) -0.012(6) -0.006(7) 0.040(8) O2A 0.113(9) 0.080(7) 0.165(12) -0.031(7) 0.040(8) -0.005(6) C90A 0.40(3) 0.222(18) 0.133(13) 0.061(12) -0.001(16) 0.20(2) C94 0.169(11) 0.114(9) 0.054(6) 0.022(6) -0.029(7) -0.026(8) C93 0.079(10) 0.113(14) 0.115(13) 0.021(10) -0.012(10) -0.040(9) C91 0.34(3) 0.190(18) 0.26(2) -0.071(17) 0.12(2) -0.109(19) O1 0.43(3) 0.148(15) 0.164(16) 0.081(12) -0.108(18) -0.039(17) C94A 0.169(11) 0.114(9) 0.054(6) 0.022(6) -0.029(7) -0.026(8) O1A 0.43(3) 0.148(15) 0.164(16) 0.081(12) -0.108(18) -0.039(17) C91A 0.34(3) 0.190(18) 0.26(2) -0.071(17) 0.12(2) -0.109(19) C93A 0.079(10) 0.113(14) 0.115(13) 0.021(10) -0.012(10) -0.040(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.031(4) . ? Cr1 N2 2.119(4) . ? Cr1 N6 2.044(4) . ? Cr1 N9 2.030(4) . ? Cr1 N10 2.133(4) . ? Cr1 N14 2.037(4) . ? Cr2 N3 2.051(4) . ? Cr2 N7 2.131(4) . ? Cr2 N8 2.027(5) . ? Cr2 N11 2.044(4) . ? Cr2 N15 2.115(5) . ? Cr2 N16 2.032(4) . ? Cr2 Cr1 3.4084(12) . ? N1 C1 1.341(7) . ? N1 C5 1.342(6) . ? N2 C6 1.325(6) . ? N2 C5 1.399(6) . ? N3 C6 1.307(6) . ? N3 C7 1.422(6) . ? N4 C7 1.329(7) . ? N4 C11 1.348(7) . ? N5 C16 1.347(7) . ? N5 C12 1.368(9) . ? N6 C17 1.317(7) . ? N6 C16 1.429(6) . ? N7 C17 1.319(6) . ? N7 C18 1.402(6) . ? N8 C22 1.338(7) . ? N8 C18 1.344(6) . ? N9 C34 1.339(7) . ? N9 C38 1.349(6) . ? N10 C39 1.328(6) . ? N10 C38 1.388(6) . ? N11 C39 1.312(6) . ? N11 C40 1.427(6) . ? N12 C40 1.327(7) . ? N12 C44 1.339(7) . ? N14 C28 1.306(6) . ? N14 C27 1.419(6) . ? N15 C28 1.332(7) . ? N15 C29 1.395(6) . ? N16 C33 1.340(7) . ? N16 C29 1.340(7) . ? C1 C2 1.366(8) . ? C2 C3 1.381(8) . ? C3 C4 1.368(8) . ? C4 C5 1.398(7) . ? C7 C8 1.389(7) . ? C8 C9 1.382(8) . ? C9 C10 1.374(9) . ? C10 C11 1.359(8) . ? C12 C13 1.343(11) . ? C13 C14 1.392(11) . ? C14 C15 1.371(9) . ? C15 C16 1.373(8) . ? C18 C19 1.382(7) . ? C19 C20 1.381(8) . ? C20 C21 1.394(9) . ? C21 C22 1.363(8) . ? C27 N13 1.3900 . ? C27 C26 1.3900 . ? N13 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? N13' C23' 1.365(8) . ? C23' C24' 1.376(8) . ? C24' C25' 1.387(8) . ? C25' C26' 1.388(8) . ? C29 C30 1.398(8) . ? C30 C31 1.379(8) . ? C31 C32 1.387(9) . ? C32 C33 1.364(8) . ? C34 C35 1.358(8) . ? C35 C36 1.388(8) . ? C36 C37 1.376(8) . ? C37 C38 1.397(7) . ? C40 C41 1.395(8) . ? C41 C42 1.377(8) . ? C42 C43 1.362(9) . ? C43 C44 1.374(9) . ? Cl3 Cu2 2.105(2) . ? Cu2 Cl4 2.107(2) . ? Cl1 Cu1 2.084(6) . ? Cu1 Cl2 2.104(16) . ? Cl1A Cu1A 2.090(8) . ? Cu1A Cl2A 2.13(3) . ? O2 C95 1.188(9) . ? C95 C90 1.491(7) . ? C95 C92 1.519(10) . ? C94 O1 1.216(10) . ? C94 C93 1.447(10) . ? C94 C91 1.494(7) . ? 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 _geom_angle_publ_flag N8 Cr2 N16 106.04(18) . . ? N8 Cr2 N11 96.26(17) . . ? N16 Cr2 N11 89.62(17) . . ? N8 Cr2 N3 87.56(17) . . ? N16 Cr2 N3 95.78(17) . . ? N11 Cr2 N3 172.28(17) . . ? N8 Cr2 N15 169.89(17) . . ? N16 Cr2 N15 64.13(17) . . ? N11 Cr2 N15 86.36(16) . . ? N3 Cr2 N15 91.03(16) . . ? N8 Cr2 N7 64.14(17) . . ? N16 Cr2 N7 170.16(18) . . ? N11 Cr2 N7 90.74(16) . . ? N3 Cr2 N7 84.88(16) . . ? N15 Cr2 N7 125.71(17) . . ? N8 Cr2 Cr1 126.35(12) . . ? N16 Cr2 Cr1 127.59(13) . . ? N11 Cr2 Cr1 86.28(12) . . ? N3 Cr2 Cr1 86.06(12) . . ? N15 Cr2 Cr1 63.47(11) . . ? N7 Cr2 Cr1 62.24(12) . . ? N9 Cr1 N1 104.94(17) . . ? N9 Cr1 N14 89.22(17) . . ? N1 Cr1 N14 93.62(17) . . ? N9 Cr1 N6 92.13(17) . . ? N1 Cr1 N6 93.75(17) . . ? N14 Cr1 N6 171.90(17) . . ? N9 Cr1 N2 169.20(16) . . ? N1 Cr1 N2 64.26(16) . . ? N14 Cr1 N2 91.10(16) . . ? N6 Cr1 N2 89.07(16) . . ? N9 Cr1 N10 64.10(16) . . ? N1 Cr1 N10 169.02(16) . . ? N14 Cr1 N10 87.11(16) . . ? N6 Cr1 N10 86.31(16) . . ? N2 Cr1 N10 126.70(16) . . ? N9 Cr1 Cr2 127.39(12) . . ? N1 Cr1 Cr2 127.62(12) . . ? N14 Cr1 Cr2 85.70(12) . . ? N6 Cr1 Cr2 87.14(12) . . ? N2 Cr1 Cr2 63.39(11) . . ? N10 Cr1 Cr2 63.36(11) . . ? C1 N1 C5 120.2(5) . . ? C1 N1 Cr1 142.9(4) . . ? C5 N1 Cr1 97.0(3) . . ? C6 N2 C5 120.5(4) . . ? C6 N2 Cr1 148.0(3) . . ? C5 N2 Cr1 91.3(3) . . ? C6 N3 C7 117.6(4) . . ? C6 N3 Cr2 118.3(3) . . ? C7 N3 Cr2 122.9(3) . . ? C7 N4 C11 116.9(5) . . ? C16 N5 C12 115.6(6) . . ? C17 N6 C16 116.6(5) . . ? C17 N6 Cr1 117.0(3) . . ? C16 N6 Cr1 126.3(4) . . ? C17 N7 C18 119.4(5) . . ? C17 N7 Cr2 149.6(4) . . ? C18 N7 Cr2 91.1(3) . . ? C22 N8 C18 119.8(5) . . ? C22 N8 Cr2 142.7(4) . . ? C18 N8 Cr2 97.4(3) . . ? C34 N9 C38 120.7(4) . . ? C34 N9 Cr1 142.1(4) . . ? C38 N9 Cr1 96.9(3) . . ? C39 N10 C38 120.4(4) . . ? C39 N10 Cr1 148.0(4) . . ? C38 N10 Cr1 91.2(3) . . ? C39 N11 C40 119.0(4) . . ? C39 N11 Cr2 118.9(3) . . ? C40 N11 Cr2 121.8(3) . . ? C40 N12 C44 117.7(5) . . ? C28 N14 C27 116.3(4) . . ? C28 N14 Cr1 119.5(4) . . ? C27 N14 Cr1 122.9(3) . . ? C28 N15 C29 120.0(5) . . ? C28 N15 Cr2 147.9(4) . . ? C29 N15 Cr2 91.6(3) . . ? C33 N16 C29 120.7(5) . . ? C33 N16 Cr2 142.3(4) . . ? C29 N16 Cr2 96.9(3) . . ? N1 C1 C2 121.0(5) . . ? C1 C2 C3 119.0(5) . . ? C4 C3 C2 121.0(5) . . ? C3 C4 C5 117.2(5) . . ? N1 C5 C4 121.6(5) . . ? N1 C5 N2 107.3(4) . . ? C4 C5 N2 131.1(5) . . ? N3 C6 N2 124.0(5) . . ? N4 C7 C8 122.9(5) . . ? N4 C7 N3 115.0(5) . . ? C8 C7 N3 122.0(5) . . ? C9 C8 C7 118.3(5) . . ? C10 C9 C8 119.3(6) . . ? C11 C10 C9 118.3(6) . . ? N4 C11 C10 124.1(5) . . ? C13 C12 N5 124.8(7) . . ? C12 C13 C14 117.5(6) . . ? C15 C14 C13 120.1(7) . . ? C14 C15 C16 118.2(6) . . ? N5 C16 C15 123.6(5) . . ? N5 C16 N6 115.2(5) . . ? C15 C16 N6 121.2(5) . . ? N6 C17 N7 123.6(5) . . ? N8 C18 C19 122.1(5) . . ? N8 C18 N7 107.1(4) . . ? C19 C18 N7 130.8(5) . . ? C20 C19 C18 117.6(5) . . ? C19 C20 C21 120.1(6) . . ? C22 C21 C20 118.9(6) . . ? N8 C22 C21 121.5(6) . . ? N13 C27 C26 120.0 . . ? N13 C27 N14 115.9(8) . . ? C26 C27 N14 124.0(8) . . ? C27 N13 C23 120.0 . . ? C24 C23 N13 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? N13' C23' C24' 123.4(8) . . ? C23' C24' C25' 119.6(8) . . ? C24' C25' C26' 118.6(8) . . ? N14 C28 N15 122.8(5) . . ? N16 C29 N15 107.3(4) . . ? N16 C29 C30 121.2(5) . . ? N15 C29 C30 131.5(6) . . ? C31 C30 C29 117.4(6) . . ? C30 C31 C32 120.7(6) . . ? C33 C32 C31 118.8(6) . . ? N16 C33 C32 121.2(6) . . ? N9 C34 C35 121.6(5) . . ? C34 C35 C36 118.4(5) . . ? C37 C36 C35 121.1(5) . . ? C36 C37 C38 117.6(5) . . ? N9 C38 N10 107.7(4) . . ? N9 C38 C37 120.6(5) . . ? N10 C38 C37 131.7(5) . . ? N11 C39 N10 123.3(5) . . ? N12 C40 C41 122.3(5) . . ? N12 C40 N11 114.1(5) . . ? C41 C40 N11 123.4(5) . . ? C42 C41 C40 118.2(6) . . ? C43 C42 C41 120.0(6) . . ? C42 C43 C44 118.0(6) . . ? N12 C44 C43 123.7(6) . . ? Cl3 Cu2 Cl4 177.70(8) . . ? Cl1 Cu1 Cl2 178.1(9) . . ? Cl1A Cu1A Cl2A 178.0(9) . . ? O2 C95 C90 122.1(15) . . ? O2 C95 C92 122.7(18) . . ? C90 C95 C92 115.0(19) . . ? O1 C94 C93 126.9(11) . . ? O1 C94 C91 122.6(11) . . ? C93 C94 C91 110.4(18) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.395 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.094 #===END of CIF for Compound 2.2Acetone ========== data_cmpd3CH3CN _database_code_CSD 206656 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '(Cr2(DpyF)4CuCl3)(CuCl2), CH3CN' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H39 Cl5 Cr2 Cu2 N17' _chemical_formula_weight 1238.27 _chemical_melting_point ? _chemical_compound_source synthesis 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' N N 0.0061 0.0033 '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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5665(5) _cell_length_b 12.8413(7) _cell_length_c 18.949(1) _cell_angle_alpha 86.269(1) _cell_angle_beta 75.518(1) _cell_angle_gamma 80.250(1) _cell_volume 2452.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7044 _cell_measurement_theta_min 2.373 _cell_measurement_theta_max 27.466 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1250 _exptl_absorpt_coefficient_mu 1.614 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_method 'w\ scans' _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16189 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10799 _reflns_number_observed 8119 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL V. 5.03 (Siemens, 1994)' _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+1.8440P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10798 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_obs 0.0413 _refine_ls_wR_factor_all 0.1065 _refine_ls_wR_factor_obs 0.0963 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.079 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.079 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr 0.72625(4) 0.60017(4) 0.27352(3) 0.01684(11) Uani 1 d . . Cr2 Cr 0.90363(5) 0.79420(4) 0.21227(3) 0.01691(11) Uani 1 d . . Cu1 Cu 0.79192(4) 0.84990(3) 0.47555(2) 0.02782(10) Uani 1 d . . Cu2 Cu 1.25729(5) 1.24095(4) 0.04617(3) 0.03988(13) Uani 1 d . . Cl1 Cl 0.63117(11) 0.94745(8) 0.55721(6) 0.0479(3) Uani 1 d . . Cl2 Cl 0.72306(9) 0.69457(6) 0.50256(5) 0.0321(2) Uani 1 d . . Cl3 Cl 1.01387(9) 0.80035(7) 0.45604(5) 0.0336(2) Uani 1 d . . Cl4 Cl 1.46320(10) 1.22734(9) 0.02795(8) 0.0590(3) Uani 1 d . . Cl5 Cl 1.05383(10) 1.24570(9) 0.05852(8) 0.0597(3) Uani 1 d . . N1 N 0.8200(3) 0.9702(2) 0.39952(15) 0.0259(6) Uani 1 d . . N2 N 0.7888(2) 0.8798(2) 0.30043(14) 0.0185(5) Uani 1 d . . N3 N 0.6613(2) 0.7460(2) 0.32862(14) 0.0195(5) Uani 1 d . . N4 N 0.5659(2) 0.6039(2) 0.35993(14) 0.0203(5) Uani 1 d . . N5 N 0.8724(2) 0.9093(2) 0.13547(14) 0.0200(5) Uani 1 d . . N6 N 0.7369(2) 0.7920(2) 0.16929(14) 0.0206(5) Uani 1 d . . N7 N 0.6124(2) 0.6571(2) 0.20364(14) 0.0204(5) Uani 1 d . . N8 N 0.5663(3) 0.5471(3) 0.1212(2) 0.0456(9) Uani 1 d . . N9 N 1.0177(2) 0.6925(2) 0.13354(13) 0.0188(5) Uani 1 d . . N10 N 0.8837(2) 0.5648(2) 0.17968(14) 0.0189(5) Uani 1 d . . N11 N 0.7515(2) 0.4539(2) 0.23448(14) 0.0201(5) Uani 1 d . . N12 N 0.6364(3) 0.3393(2) 0.3145(2) 0.0263(6) Uani 1 d . . N13 N 1.1879(3) 0.9369(2) 0.1623(2) 0.0303(6) Uani 1 d . . N14 N 1.0689(2) 0.8218(2) 0.23982(14) 0.0209(5) Uani 1 d . . N15 N 0.9716(2) 0.6871(2) 0.29018(14) 0.0192(5) Uani 1 d . . N16 N 0.8572(2) 0.5488(2) 0.33640(13) 0.0184(5) Uani 1 d . . N17 N 0.0854(4) 0.3553(3) 0.2336(2) 0.0531(9) Uani 1 d . . C1 C 0.8591(4) 1.0529(3) 0.4239(2) 0.0341(8) Uani 1 d . . H1A H 0.8536(4) 1.0558(3) 0.4740(2) 0.041 Uiso 1 calc R . C2 C 0.9066(4) 1.1331(3) 0.3787(2) 0.0353(8) Uani 1 d . . H2A H 0.9346(4) 1.1889(3) 0.3975(2) 0.042 Uiso 1 calc R . C3 C 0.9124(3) 1.1299(3) 0.3053(2) 0.0331(8) Uani 1 d . . H3A H 0.9444(3) 1.1837(3) 0.2731(2) 0.040 Uiso 1 calc R . C4 C 0.8707(3) 1.0473(2) 0.2801(2) 0.0286(7) Uani 1 d . . H4A H 0.8727(3) 1.0447(2) 0.2303(2) 0.034 Uiso 1 calc R . C5 C 0.8254(3) 0.9672(2) 0.3279(2) 0.0212(6) Uani 1 d . . C6 C 0.6886(3) 0.8378(2) 0.3421(2) 0.0193(6) Uani 1 d . . H6A H 0.6350(3) 0.8750(2) 0.3829(2) 0.023 Uiso 1 calc R . C7 C 0.5535(3) 0.7066(2) 0.3748(2) 0.0204(6) Uani 1 d . . C8 C 0.4476(3) 0.7564(3) 0.4274(2) 0.0304(8) Uani 1 d . . H8A H 0.4389(3) 0.8287(3) 0.4366(2) 0.036 Uiso 1 calc R . C9 C 0.3561(3) 0.6958(3) 0.4655(2) 0.0362(8) Uani 1 d . . H9A H 0.2831(3) 0.7268(3) 0.5013(2) 0.043 Uiso 1 calc R . C10 C 0.3712(3) 0.5884(3) 0.4512(2) 0.0320(8) Uani 1 d . . H10A H 0.3098(3) 0.5465(3) 0.4779(2) 0.038 Uiso 1 calc R . C11 C 0.4767(3) 0.5451(2) 0.3978(2) 0.0259(7) Uani 1 d . . H11A H 0.4870(3) 0.4731(2) 0.3875(2) 0.031 Uiso 1 calc R . C12 C 0.9183(3) 0.9944(2) 0.0996(2) 0.0232(6) Uani 1 d . . H12A H 0.9970(3) 1.0128(2) 0.1061(2) 0.028 Uiso 1 calc R . C13 C 0.8522(3) 1.0548(2) 0.0536(2) 0.0264(7) Uani 1 d . . H13A H 0.8851(3) 1.1142(2) 0.0288(2) 0.032 Uiso 1 calc R . C14 C 0.7361(3) 1.0273(3) 0.0442(2) 0.0277(7) Uani 1 d . . H14A H 0.6902(3) 1.0683(3) 0.0128(2) 0.033 Uiso 1 calc R . C15 C 0.6875(3) 0.9399(2) 0.0805(2) 0.0238(6) Uani 1 d . . H15A H 0.6086(3) 0.9209(2) 0.0749(2) 0.029 Uiso 1 calc R . C16 C 0.7604(3) 0.8812(2) 0.1259(2) 0.0200(6) Uani 1 d . . C17 C 0.6439(3) 0.7383(2) 0.1617(2) 0.0224(6) Uani 1 d . . H17A H 0.5993(3) 0.7597(2) 0.1248(2) 0.027 Uiso 1 calc R . C18 C 0.5240(3) 0.5969(2) 0.1845(2) 0.0220(6) Uani 1 d . . C19 C 0.4074(4) 0.5866(3) 0.2328(2) 0.0426(10) Uani 1 d . . H19A H 0.3821(4) 0.6212(3) 0.2775(2) 0.051 Uiso 1 calc R . C20 C 0.3273(4) 0.5239(4) 0.2143(3) 0.0545(12) Uani 1 d . . H20A H 0.2447(4) 0.5179(4) 0.2459(3) 0.065 Uiso 1 calc R . C21 C 0.3669(3) 0.4708(3) 0.1506(2) 0.0350(8) Uani 1 d . . H21A H 0.3149(3) 0.4256(3) 0.1383(2) 0.042 Uiso 1 calc R . C22 C 0.4854(4) 0.4860(3) 0.1055(2) 0.0470(10) Uani 1 d . . H22A H 0.5123(4) 0.4517(3) 0.0606(2) 0.056 Uiso 1 calc R . C23 C 1.1245(3) 0.7244(2) 0.0865(2) 0.0223(6) Uani 1 d . . H23A H 1.1420(3) 0.7928(2) 0.0909(2) 0.027 Uiso 1 calc R . C24 C 1.2077(3) 0.6621(3) 0.0330(2) 0.0281(7) Uani 1 d . . H24A H 1.2818(3) 0.6863(3) 0.0020(2) 0.034 Uiso 1 calc R . C25 C 1.1802(3) 0.5616(3) 0.0256(2) 0.0301(7) Uani 1 d . . H25A H 1.2343(3) 0.5175(3) -0.0115(2) 0.036 Uiso 1 calc R . C26 C 1.0731(3) 0.5275(3) 0.0731(2) 0.0259(7) Uani 1 d . . H26A H 1.0543(3) 0.4596(3) 0.0687(2) 0.031 Uiso 1 calc R . C27 C 0.9922(3) 0.5938(2) 0.1279(2) 0.0189(6) Uani 1 d . . C28 C 0.8529(3) 0.4685(2) 0.1805(2) 0.0213(6) Uani 1 d . . H28 H 0.8984(3) 0.4168(2) 0.1463(2) 0.026 Uiso 1 calc R . C29 C 0.6949(3) 0.3604(2) 0.2453(2) 0.0227(6) Uani 1 d . . C30 C 0.6962(4) 0.2976(3) 0.1881(2) 0.0327(8) Uani 1 d . . H30A H 0.7369(4) 0.3154(3) 0.1399(2) 0.039 Uiso 1 calc R . C31 C 0.6359(4) 0.2080(3) 0.2038(2) 0.0402(9) Uani 1 d . . H31A H 0.6350(4) 0.1640(3) 0.1663(2) 0.048 Uiso 1 calc R . C32 C 0.5772(3) 0.1845(3) 0.2756(2) 0.0371(9) Uani 1 d . . H32A H 0.5369(3) 0.1238(3) 0.2878(2) 0.044 Uiso 1 calc R . C33 C 0.5791(3) 0.2515(3) 0.3285(2) 0.0326(8) Uani 1 d . . H33A H 0.5383(3) 0.2355(3) 0.3771(2) 0.039 Uiso 1 calc R . C34 C 1.2814(4) 0.9999(3) 0.1480(2) 0.0385(9) Uani 1 d . . H34A H 1.2978(4) 1.0352(3) 0.1024(2) 0.046 Uiso 1 calc R . C35 C 1.3540(4) 1.0157(3) 0.1957(2) 0.0426(10) Uani 1 d . . H35A H 1.4206(4) 1.0583(3) 0.1822(2) 0.051 Uiso 1 calc R . C36 C 1.3272(4) 0.9677(3) 0.2641(2) 0.0468(11) Uani 1 d . . H36A H 1.3743(4) 0.9781(3) 0.2983(2) 0.056 Uiso 1 calc R . C37 C 1.2294(4) 0.9036(3) 0.2814(2) 0.0371(9) Uani 1 d . . H37A H 1.2072(4) 0.8714(3) 0.3279(2) 0.045 Uiso 1 calc R . C38 C 1.1654(3) 0.8888(2) 0.2277(2) 0.0243(7) Uani 1 d . . C39 C 1.0702(3) 0.7406(2) 0.2855(2) 0.0210(6) Uani 1 d . . H39 H 1.1349(3) 0.7222(2) 0.3122(2) 0.025 Uiso 1 calc R . C40 C 0.9610(3) 0.5971(2) 0.3349(2) 0.0177(6) Uani 1 d . . C41 C 1.0526(3) 0.5565(2) 0.3763(2) 0.0230(6) Uani 1 d . . H41A H 1.1246(3) 0.5912(2) 0.3754(2) 0.028 Uiso 1 calc R . C42 C 1.0363(3) 0.4663(2) 0.4180(2) 0.0238(6) Uani 1 d . . H42A H 1.0980(3) 0.4377(2) 0.4451(2) 0.029 Uiso 1 calc R . C43 C 0.9275(3) 0.4172(2) 0.4199(2) 0.0230(6) Uani 1 d . . H43A H 0.9137(3) 0.3560(2) 0.4488(2) 0.028 Uiso 1 calc R . C44 C 0.8411(3) 0.4601(2) 0.3787(2) 0.0219(6) Uani 1 d . . H44A H 0.7679(3) 0.4269(2) 0.3797(2) 0.026 Uiso 1 calc R . C45 C 0.1493(4) 0.3095(3) 0.2680(2) 0.0428(10) Uani 1 d . . C46 C 0.2283(6) 0.2497(5) 0.3156(4) 0.085(2) Uani 1 d . . 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 Cr1 0.0189(2) 0.0169(2) 0.0159(2) 0.0010(2) -0.0041(2) -0.0068(2) Cr2 0.0195(2) 0.0168(2) 0.0164(2) 0.0022(2) -0.0060(2) -0.0068(2) Cu1 0.0358(2) 0.0237(2) 0.0253(2) 0.0017(2) -0.0100(2) -0.0052(2) Cu2 0.0374(2) 0.0335(2) 0.0521(3) -0.0057(2) -0.0162(2) -0.0056(2) Cl1 0.0576(6) 0.0331(5) 0.0422(6) -0.0028(4) 0.0040(5) -0.0005(4) Cl2 0.0394(4) 0.0261(4) 0.0336(5) 0.0045(3) -0.0140(4) -0.0073(3) Cl3 0.0379(4) 0.0330(4) 0.0318(5) 0.0013(4) -0.0139(4) -0.0034(3) Cl4 0.0368(5) 0.0538(6) 0.0909(10) -0.0098(6) -0.0206(6) -0.0091(5) Cl5 0.0397(5) 0.0426(6) 0.1025(10) -0.0258(6) -0.0235(6) -0.0037(4) N1 0.0357(15) 0.0211(13) 0.0241(14) -0.0015(11) -0.0113(12) -0.0074(11) N2 0.0226(12) 0.0159(11) 0.0186(13) -0.0003(10) -0.0070(10) -0.0045(9) N3 0.0189(12) 0.0222(12) 0.0179(13) 0.0015(10) -0.0046(10) -0.0053(10) N4 0.0199(12) 0.0199(12) 0.0210(13) 0.0014(10) -0.0031(10) -0.0058(10) N5 0.0242(12) 0.0199(12) 0.0179(13) 0.0029(10) -0.0072(10) -0.0067(10) N6 0.0237(12) 0.0223(13) 0.0178(13) 0.0055(10) -0.0076(11) -0.0079(10) N7 0.0208(12) 0.0219(12) 0.0207(13) 0.0013(10) -0.0068(10) -0.0073(10) N8 0.045(2) 0.062(2) 0.034(2) -0.015(2) 0.001(2) -0.030(2) N9 0.0216(12) 0.0211(12) 0.0151(12) 0.0024(10) -0.0058(10) -0.0064(10) N10 0.0192(12) 0.0203(12) 0.0181(13) 0.0003(10) -0.0040(10) -0.0063(10) N11 0.0240(12) 0.0194(12) 0.0188(13) -0.0014(10) -0.0049(10) -0.0090(10) N12 0.0266(13) 0.0246(13) 0.0270(15) -0.0008(11) -0.0011(12) -0.0104(11) N13 0.038(2) 0.0310(15) 0.028(2) 0.0065(12) -0.0104(13) -0.0195(13) N14 0.0223(12) 0.0211(12) 0.0222(14) 0.0022(10) -0.0082(11) -0.0082(10) N15 0.0208(12) 0.0212(12) 0.0176(13) 0.0030(10) -0.0073(10) -0.0065(10) N16 0.0210(12) 0.0185(12) 0.0157(12) 0.0023(10) -0.0036(10) -0.0055(10) N17 0.052(2) 0.060(2) 0.051(2) 0.002(2) -0.016(2) -0.014(2) C1 0.049(2) 0.030(2) 0.028(2) -0.0039(15) -0.013(2) -0.014(2) C2 0.048(2) 0.024(2) 0.040(2) -0.009(2) -0.013(2) -0.0129(15) C3 0.037(2) 0.021(2) 0.042(2) 0.0033(15) -0.006(2) -0.0119(14) C4 0.038(2) 0.022(2) 0.027(2) 0.0021(13) -0.0076(15) -0.0103(14) C5 0.0209(14) 0.0172(14) 0.026(2) -0.0022(12) -0.0056(13) -0.0025(11) C6 0.0219(14) 0.0179(14) 0.019(2) 0.0007(12) -0.0083(12) -0.0018(11) C7 0.0215(14) 0.0205(14) 0.021(2) 0.0037(12) -0.0078(12) -0.0063(11) C8 0.026(2) 0.023(2) 0.039(2) -0.0058(15) 0.0000(15) -0.0046(13) C9 0.027(2) 0.034(2) 0.040(2) -0.009(2) 0.008(2) -0.0047(14) C10 0.027(2) 0.031(2) 0.034(2) -0.0001(15) 0.0051(15) -0.0130(14) C11 0.029(2) 0.0210(15) 0.027(2) -0.0019(13) -0.0007(14) -0.0093(13) C12 0.0247(15) 0.025(2) 0.021(2) 0.0028(13) -0.0036(13) -0.0110(12) C13 0.035(2) 0.021(2) 0.021(2) 0.0047(13) -0.0040(14) -0.0066(13) C14 0.035(2) 0.025(2) 0.024(2) 0.0035(13) -0.0124(14) 0.0005(13) C15 0.027(2) 0.024(2) 0.023(2) -0.0002(13) -0.0109(13) -0.0031(12) C16 0.0231(14) 0.0207(14) 0.0164(15) 0.0015(12) -0.0049(12) -0.0050(11) C17 0.0218(14) 0.027(2) 0.021(2) 0.0013(13) -0.0088(12) -0.0077(12) C18 0.0219(14) 0.0222(15) 0.024(2) 0.0019(12) -0.0095(13) -0.0058(12) C19 0.034(2) 0.058(2) 0.037(2) -0.026(2) 0.007(2) -0.023(2) C20 0.036(2) 0.072(3) 0.056(3) -0.023(2) 0.011(2) -0.033(2) C21 0.031(2) 0.037(2) 0.044(2) -0.005(2) -0.014(2) -0.0161(15) C22 0.053(2) 0.059(3) 0.034(2) -0.020(2) -0.004(2) -0.027(2) C23 0.0240(15) 0.0226(15) 0.021(2) 0.0045(12) -0.0049(13) -0.0103(12) C24 0.023(2) 0.035(2) 0.025(2) 0.0037(14) -0.0016(13) -0.0089(13) C25 0.027(2) 0.031(2) 0.028(2) -0.0043(14) 0.0007(14) -0.0041(13) C26 0.026(2) 0.024(2) 0.026(2) -0.0032(13) -0.0016(13) -0.0068(12) C27 0.0198(13) 0.0213(14) 0.0166(15) 0.0020(12) -0.0046(12) -0.0067(11) C28 0.0227(14) 0.0232(15) 0.019(2) -0.0017(12) -0.0040(12) -0.0064(12) C29 0.0208(14) 0.0203(14) 0.027(2) -0.0021(13) -0.0037(13) -0.0062(12) C30 0.038(2) 0.033(2) 0.028(2) -0.0065(15) -0.002(2) -0.0172(15) C31 0.043(2) 0.035(2) 0.044(2) -0.017(2) 0.000(2) -0.021(2) C32 0.033(2) 0.025(2) 0.053(3) -0.003(2) -0.002(2) -0.0149(14) C33 0.032(2) 0.027(2) 0.036(2) 0.0014(15) 0.002(2) -0.0132(14) C34 0.052(2) 0.040(2) 0.029(2) 0.006(2) -0.007(2) -0.029(2) C35 0.042(2) 0.047(2) 0.046(2) 0.001(2) -0.008(2) -0.032(2) C36 0.052(2) 0.060(3) 0.043(2) 0.008(2) -0.024(2) -0.035(2) C37 0.046(2) 0.044(2) 0.031(2) 0.007(2) -0.017(2) -0.025(2) C38 0.0245(15) 0.0219(15) 0.029(2) 0.0018(13) -0.0089(13) -0.0085(12) C39 0.0233(14) 0.0216(14) 0.021(2) 0.0018(12) -0.0103(12) -0.0051(12) C40 0.0228(14) 0.0160(13) 0.0133(14) -0.0010(11) -0.0026(11) -0.0023(11) C41 0.0249(15) 0.024(2) 0.022(2) 0.0006(12) -0.0076(13) -0.0052(12) C42 0.030(2) 0.0212(15) 0.019(2) -0.0007(12) -0.0083(13) 0.0014(12) C43 0.031(2) 0.0163(14) 0.020(2) 0.0025(12) -0.0030(13) -0.0023(12) C44 0.0259(15) 0.0207(14) 0.019(2) 0.0010(12) -0.0036(13) -0.0055(12) C45 0.035(2) 0.044(2) 0.050(3) -0.015(2) -0.006(2) -0.008(2) C46 0.077(4) 0.086(4) 0.098(5) -0.031(4) -0.054(4) 0.034(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N3 2.128(3) . ? Cr1 N4 2.037(2) . ? Cr1 N7 2.027(3) . ? Cr1 N10 2.123(2) . ? Cr1 N11 2.014(3) . ? Cr2 N14 2.034(2) . ? Cr1 N16 2.045(2) . ? Cr2 N2 2.060(3) . ? Cr2 N5 2.051(2) . ? Cr2 N6 2.123(3) . ? Cr2 N9 2.050(3) . ? Cr2 N15 2.126(2) . ? Cu1 N1 2.050(3) . ? Cu1 Cl2 2.2231(9) . ? Cu1 Cl1 2.2507(11) . ? Cu1 Cl3 2.2657(10) . ? Cu2 Cl5 2.0944(11) . ? Cu2 Cl4 2.0945(11) . ? N1 C5 1.346(4) . ? N1 C1 1.349(4) . ? N2 C6 1.325(4) . ? N2 C5 1.416(4) . ? N3 C6 1.315(4) . ? N3 C7 1.400(4) . ? N4 C11 1.343(4) . ? N4 C7 1.344(4) . ? N5 C12 1.346(4) . ? N5 C16 1.350(4) . ? N6 C17 1.331(4) . ? N6 C16 1.387(4) . ? N7 C17 1.307(4) . ? N7 C18 1.432(4) . ? N8 C18 1.335(4) . ? N8 C22 1.348(5) . ? N9 C27 1.357(4) . ? N9 C23 1.357(4) . ? N10 C28 1.330(4) . ? N10 C27 1.395(4) . ? N11 C28 1.313(4) . ? N11 C29 1.411(4) . ? N12 C29 1.334(4) . ? N12 C33 1.349(4) . ? N13 C38 1.333(4) . ? N13 C34 1.346(4) . ? N14 C39 1.311(4) . ? N14 C38 1.409(4) . ? N15 C39 1.324(4) . ? N15 C40 1.391(4) . ? N16 C40 1.343(4) . ? N16 C44 1.358(4) . ? N17 C45 1.123(5) . ? C1 C2 1.375(5) . ? C2 C3 1.381(5) . ? C3 C4 1.371(5) . ? C4 C5 1.392(4) . ? C7 C8 1.393(4) . ? C8 C9 1.376(5) . ? C9 C10 1.398(5) . ? C10 C11 1.369(5) . ? C12 C13 1.372(4) . ? C13 C14 1.388(5) . ? C14 C15 1.384(4) . ? C15 C16 1.397(4) . ? C18 C19 1.359(5) . ? C19 C20 1.379(5) . ? C20 C21 1.361(6) . ? C21 C22 1.365(5) . ? C23 C24 1.364(5) . ? C24 C25 1.393(5) . ? C25 C26 1.373(4) . ? C26 C27 1.400(4) . ? C29 C30 1.388(5) . ? C30 C31 1.388(5) . ? C31 C32 1.383(5) . ? C32 C33 1.369(5) . ? C34 C35 1.366(5) . ? C35 C36 1.383(6) . ? C36 C37 1.390(5) . ? C37 C38 1.393(5) . ? C40 C41 1.406(4) . ? C41 C42 1.370(4) . ? C42 C43 1.393(4) . ? C43 C44 1.370(4) . ? C45 C46 1.473(7) . ? 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 _geom_angle_publ_flag N11 Cr1 N7 90.51(10) . . ? N11 Cr1 N4 103.98(10) . . ? N7 Cr1 N4 92.38(10) . . ? N11 Cr1 N16 90.46(10) . . ? N7 Cr1 N16 173.96(10) . . ? N4 Cr1 N16 93.17(10) . . ? N11 Cr1 N10 64.01(9) . . ? N7 Cr1 N10 86.57(10) . . ? N4 Cr1 N10 167.91(10) . . ? N16 Cr1 N10 88.51(10) . . ? N11 Cr1 N3 167.84(10) . . ? N7 Cr1 N3 88.06(10) . . ? N4 Cr1 N3 64.04(9) . . ? N16 Cr1 N3 92.22(10) . . ? N10 Cr1 N3 127.90(9) . . ? N14 Cr2 N9 90.32(10) . . ? N14 Cr2 N5 104.67(10) . . ? N9 Cr2 N5 91.60(10) . . ? N14 Cr2 N2 89.41(10) . . ? N9 Cr2 N2 172.64(9) . . ? N5 Cr2 N2 95.58(10) . . ? N14 Cr2 N6 168.53(10) . . ? N9 Cr2 N6 90.06(10) . . ? N5 Cr2 N6 63.86(9) . . ? N2 Cr2 N6 91.66(10) . . ? N14 Cr2 N15 63.95(9) . . ? N9 Cr2 N15 87.32(10) . . ? N5 Cr2 N15 168.54(10) . . ? N2 Cr2 N15 85.96(10) . . ? N6 Cr2 N15 127.52(9) . . ? N1 Cu1 Cl2 146.19(8) . . ? N1 Cu1 Cl1 95.16(8) . . ? Cl2 Cu1 Cl1 98.15(4) . . ? N1 Cu1 Cl3 90.28(8) . . ? Cl2 Cu1 Cl3 100.83(3) . . ? Cl1 Cu1 Cl3 136.54(4) . . ? Cl5 Cu2 Cl4 175.65(5) . . ? C5 N1 C1 118.4(3) . . ? C5 N1 Cu1 127.3(2) . . ? C1 N1 Cu1 113.3(2) . . ? C6 N2 C5 117.3(3) . . ? C6 N2 Cr2 117.0(2) . . ? C5 N2 Cr2 124.2(2) . . ? C6 N3 C7 119.5(3) . . ? C6 N3 Cr1 148.0(2) . . ? C7 N3 Cr1 91.3(2) . . ? C11 N4 C7 120.1(3) . . ? C11 N4 Cr1 142.7(2) . . ? C7 N4 Cr1 97.0(2) . . ? C12 N5 C16 120.1(3) . . ? C12 N5 Cr2 143.4(2) . . ? C16 N5 Cr2 96.4(2) . . ? C17 N6 C16 119.7(3) . . ? C17 N6 Cr2 147.3(2) . . ? C16 N6 Cr2 92.1(2) . . ? C17 N7 C18 117.6(3) . . ? C17 N7 Cr1 118.0(2) . . ? C18 N7 Cr1 122.3(2) . . ? C18 N8 C22 116.6(3) . . ? C27 N9 C23 118.9(3) . . ? C27 N9 Cr2 122.4(2) . . ? C23 N9 Cr2 118.7(2) . . ? C28 N10 C27 120.6(3) . . ? C28 N10 Cr1 89.2(2) . . ? C27 N10 Cr1 150.1(2) . . ? C28 N11 C29 123.5(3) . . ? C28 N11 Cr1 94.5(2) . . ? C29 N11 Cr1 141.9(2) . . ? C29 N12 C33 117.6(3) . . ? C38 N13 C34 116.7(3) . . ? C39 N14 C38 121.9(3) . . ? C39 N14 Cr2 93.5(2) . . ? C38 N14 Cr2 144.7(2) . . ? C39 N15 C40 120.5(3) . . ? C39 N15 Cr2 89.1(2) . . ? C40 N15 Cr2 150.4(2) . . ? C40 N16 C44 119.2(3) . . ? C40 N16 Cr1 122.2(2) . . ? C44 N16 Cr1 118.5(2) . . ? N1 C1 C2 123.0(3) . . ? C1 C2 C3 118.5(3) . . ? C4 C3 C2 119.0(3) . . ? C3 C4 C5 120.1(3) . . ? N1 C5 C4 120.9(3) . . ? N1 C5 N2 119.6(3) . . ? C4 C5 N2 119.4(3) . . ? N3 C6 N2 122.5(3) . . ? N4 C7 C8 122.0(3) . . ? N4 C7 N3 107.3(3) . . ? C8 C7 N3 130.7(3) . . ? C9 C8 C7 117.4(3) . . ? C8 C9 C10 120.4(3) . . ? C11 C10 C9 119.0(3) . . ? N4 C11 C10 121.1(3) . . ? N5 C12 C13 121.1(3) . . ? C12 C13 C14 119.2(3) . . ? C15 C14 C13 120.6(3) . . ? C14 C15 C16 117.3(3) . . ? N5 C16 N6 107.6(3) . . ? N5 C16 C15 121.7(3) . . ? N6 C16 C15 130.7(3) . . ? N7 C17 N6 122.5(3) . . ? N8 C18 C19 123.3(3) . . ? N8 C18 N7 117.1(3) . . ? C19 C18 N7 119.5(3) . . ? C18 C19 C20 118.1(4) . . ? C21 C20 C19 120.6(4) . . ? C20 C21 C22 117.1(3) . . ? N8 C22 C21 124.2(4) . . ? N9 C23 C24 123.2(3) . . ? C23 C24 C25 118.3(3) . . ? C26 C25 C24 119.4(3) . . ? C25 C26 C27 120.1(3) . . ? N9 C27 N10 115.8(3) . . ? N9 C27 C26 120.1(3) . . ? N10 C27 C26 124.1(3) . . ? N11 C28 N10 112.3(3) . . ? N12 C29 C30 122.9(3) . . ? N12 C29 N11 114.6(3) . . ? C30 C29 N11 122.5(3) . . ? C31 C30 C29 118.6(3) . . ? C32 C31 C30 118.9(3) . . ? C33 C32 C31 118.7(3) . . ? N12 C33 C32 123.4(3) . . ? N13 C34 C35 124.1(3) . . ? C34 C35 C36 118.6(3) . . ? C35 C36 C37 119.0(4) . . ? C36 C37 C38 117.9(3) . . ? N13 C38 C37 123.6(3) . . ? N13 C38 N14 114.9(3) . . ? C37 C38 N14 121.5(3) . . ? N14 C39 N15 113.5(3) . . ? N16 C40 N15 116.0(3) . . ? N16 C40 C41 120.6(3) . . ? N15 C40 C41 123.3(3) . . ? C42 C41 C40 119.7(3) . . ? C41 C42 C43 119.4(3) . . ? C44 C43 C42 118.6(3) . . ? N16 C44 C43 122.5(3) . . ? N17 C45 C46 177.7(5) . . ? _refine_diff_density_max 1.292 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.082 #===END of CIF for 3.CH3CN ============