# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name E.McInnes _publ_contact_author_name 'McInnes, Eric' _publ_contact_author_email eric.mcinnes@manchester.ac.uk data_pb1 _database_code_depnum_ccdc_archive 'CCDC 810900' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[CrCl2(bpy)2]2[Cr2Cl8(MeCN)2]' _chemical_melting_point ? _chemical_formula_moiety '2(C20 H16 Cl2 Cr N4), (C4 H6 Cl8 Cr2 N2)' _chemical_formula_sum 'C44 H38 Cl12 Cr4 N10' _chemical_formula_weight 1340.24 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' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7320(6) _cell_length_b 11.9168(7) _cell_length_c 12.3731(7) _cell_angle_alpha 67.596(5) _cell_angle_beta 88.605(5) _cell_angle_gamma 75.836(5) _cell_volume 1282.51(13) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6011 _cell_measurement_theta_min 3.0763 _cell_measurement_theta_max 28.5831 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71367 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8346 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5237 _reflns_number_gt 4202 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. All hydrogen atoms were placed geometrically. ; _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^)+(0.0707P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5237 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cr1 Cr Uani 0.15063(4) 0.14277(4) 0.19297(3) 1.000 0.0100(1) . . Cl1 Cl Uani -0.06616(7) 0.24342(6) 0.23088(5) 1.000 0.0149(2) . . Cl2 Cl Uani 0.07505(7) 0.17336(6) 0.00610(5) 1.000 0.0146(2) . . N1 N Uani 0.2241(2) 0.0953(2) 0.36310(19) 1.000 0.0116(6) . . N2 N Uani 0.1013(2) -0.0269(2) 0.27445(19) 1.000 0.0121(6) . . N3 N Uani 0.2259(2) 0.3004(2) 0.12051(18) 1.000 0.0119(6) . . N4 N Uani 0.3565(2) 0.0655(2) 0.16402(18) 1.000 0.0114(6) . . C1 C Uani 0.2867(3) 0.1625(3) 0.4004(2) 1.000 0.0162(8) . . C2 C Uani 0.3423(3) 0.1206(3) 0.5149(2) 1.000 0.0183(8) . . C3 C Uani 0.3345(3) 0.0033(3) 0.5925(2) 1.000 0.0191(8) . . C4 C Uani 0.2670(3) -0.0662(3) 0.5550(2) 1.000 0.0156(8) . . C5 C Uani 0.2105(3) -0.0181(2) 0.4405(2) 1.000 0.0124(7) . . C6 C Uani 0.1309(3) -0.0810(2) 0.3925(2) 1.000 0.0124(7) . . C7 C Uani 0.0855(3) -0.1855(2) 0.4602(2) 1.000 0.0149(8) . . C8 C Uani 0.0098(3) -0.2365(3) 0.4073(3) 1.000 0.0188(8) . . C9 C Uani -0.0166(3) -0.1838(3) 0.2864(3) 1.000 0.0207(9) . . C10 C Uani 0.0306(3) -0.0787(3) 0.2231(2) 1.000 0.0175(8) . . C11 C Uani 0.1528(3) 0.4176(2) 0.1028(2) 1.000 0.0148(8) . . C12 C Uani 0.1965(3) 0.5221(3) 0.0313(2) 1.000 0.0164(8) . . C13 C Uani 0.3166(3) 0.5044(3) -0.0279(2) 1.000 0.0168(8) . . C14 C Uani 0.3949(3) 0.3844(3) -0.0084(2) 1.000 0.0153(8) . . C15 C Uani 0.3494(3) 0.2835(2) 0.0683(2) 1.000 0.0125(7) . . C16 C Uani 0.4275(3) 0.1512(3) 0.1007(2) 1.000 0.0137(7) . . C17 C Uani 0.5658(3) 0.1138(3) 0.0734(2) 1.000 0.0165(8) . . C18 C Uani 0.6300(3) -0.0136(3) 0.1095(2) 1.000 0.0195(8) . . C19 C Uani 0.5564(3) -0.0992(3) 0.1732(2) 1.000 0.0196(8) . . C20 C Uani 0.4205(3) -0.0571(3) 0.1990(2) 1.000 0.0157(8) . . Cr2 Cr Uani 0.43613(5) 0.50837(4) 0.36227(4) 1.000 0.0140(1) . . Cl3 Cl Uani 0.32219(7) 0.67514(6) 0.19751(6) 1.000 0.0197(2) . . Cl4 Cl Uani 0.48542(7) 0.36680(6) 0.27344(6) 1.000 0.0187(2) . . Cl5 Cl Uani 0.22690(7) 0.45988(6) 0.43076(6) 1.000 0.0194(2) . . Cl6 Cl Uani 0.42963(7) 0.64803(6) 0.46105(6) 1.000 0.0176(2) . . N5 N Uani 0.6307(2) 0.5423(2) 0.3107(2) 1.000 0.0176(7) . . C21 C Uani 0.7452(3) 0.5420(3) 0.2965(2) 1.000 0.0192(9) . . C22 C Uani 0.8951(3) 0.5367(3) 0.2818(3) 1.000 0.0258(10) . . H1 H Uiso 0.29340 0.24080 0.34750 1.000 0.0190 calc R H2 H Uiso 0.38410 0.17040 0.53900 1.000 0.0220 calc R H3 H Uiso 0.37430 -0.02850 0.66910 1.000 0.0230 calc R H4 H Uiso 0.25960 -0.14480 0.60660 1.000 0.0190 calc R H7 H Uiso 0.10600 -0.22110 0.54100 1.000 0.0180 calc R H8 H Uiso -0.02350 -0.30560 0.45220 1.000 0.0220 calc R H9 H Uiso -0.06500 -0.21850 0.24870 1.000 0.0250 calc R H10 H Uiso 0.01260 -0.04270 0.14200 1.000 0.0210 calc R H11 H Uiso 0.06950 0.42930 0.14000 1.000 0.0180 calc R H12 H Uiso 0.14610 0.60230 0.02340 1.000 0.0200 calc R H13 H Uiso 0.34450 0.57320 -0.08070 1.000 0.0200 calc R H14 H Uiso 0.47740 0.37140 -0.04630 1.000 0.0180 calc R H17 H Uiso 0.61460 0.17300 0.03150 1.000 0.0200 calc R H18 H Uiso 0.72200 -0.04080 0.09090 1.000 0.0230 calc R H19 H Uiso 0.59830 -0.18490 0.19840 1.000 0.0230 calc R H20 H Uiso 0.37120 -0.11540 0.24200 1.000 0.0190 calc R H22A H Uiso 0.93320 0.55750 0.34050 1.000 0.0390 calc R H22B H Uiso 0.90560 0.59550 0.20540 1.000 0.0390 calc R H22C H Uiso 0.94550 0.45350 0.29000 1.000 0.0390 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 0.0136(2) 0.0091(2) 0.0063(2) -0.0020(2) 0.0011(2) -0.0026(2) Cl1 0.0154(3) 0.0148(3) 0.0119(3) -0.0034(3) 0.0044(2) -0.0023(2) Cl2 0.0182(3) 0.0159(3) 0.0086(3) -0.0047(3) -0.0006(2) -0.0022(3) N1 0.0134(11) 0.0102(10) 0.0092(10) -0.0022(9) 0.0021(8) -0.0022(9) N2 0.0145(11) 0.0107(11) 0.0100(11) -0.0034(9) 0.0006(9) -0.0022(9) N3 0.0156(11) 0.0121(11) 0.0071(10) -0.0029(9) 0.0017(8) -0.0035(9) N4 0.0124(11) 0.0136(11) 0.0090(10) -0.0058(9) -0.0012(8) -0.0024(9) C1 0.0188(14) 0.0142(13) 0.0157(14) -0.0055(11) 0.0017(11) -0.0050(11) C2 0.0212(15) 0.0205(14) 0.0163(14) -0.0092(12) 0.0016(11) -0.0074(12) C3 0.0209(15) 0.0237(15) 0.0096(13) -0.0029(12) -0.0014(11) -0.0057(12) C4 0.0170(13) 0.0165(13) 0.0105(13) -0.0013(11) 0.0025(10) -0.0059(11) C5 0.0117(12) 0.0126(12) 0.0117(13) -0.0037(11) 0.0036(10) -0.0027(10) C6 0.0120(12) 0.0119(12) 0.0102(12) -0.0036(11) 0.0015(10) 0.0015(10) C7 0.0179(14) 0.0131(13) 0.0119(13) -0.0034(11) 0.0026(10) -0.0035(11) C8 0.0234(15) 0.0141(13) 0.0190(14) -0.0053(12) 0.0060(12) -0.0074(12) C9 0.0258(15) 0.0197(15) 0.0197(15) -0.0084(13) -0.0016(12) -0.0098(13) C10 0.0245(15) 0.0164(14) 0.0122(13) -0.0051(12) -0.0001(11) -0.0070(12) C11 0.0164(13) 0.0135(13) 0.0126(13) -0.0040(11) 0.0014(10) -0.0020(11) C12 0.0209(14) 0.0119(13) 0.0149(13) -0.0048(11) -0.0018(11) -0.0021(11) C13 0.0183(14) 0.0160(13) 0.0137(13) -0.0007(11) -0.0021(11) -0.0082(11) C14 0.0154(13) 0.0193(14) 0.0107(13) -0.0039(11) 0.0024(10) -0.0068(11) C15 0.0124(13) 0.0155(13) 0.0086(12) -0.0046(11) -0.0019(10) -0.0015(11) C16 0.0180(13) 0.0159(13) 0.0068(12) -0.0048(11) -0.0012(10) -0.0027(11) C17 0.0168(14) 0.0194(14) 0.0118(13) -0.0057(11) 0.0018(11) -0.0025(11) C18 0.0159(14) 0.0251(15) 0.0162(14) -0.0105(12) -0.0017(11) 0.0013(12) C19 0.0211(15) 0.0147(13) 0.0185(14) -0.0072(12) -0.0052(11) 0.0051(11) C20 0.0210(14) 0.0135(13) 0.0112(13) -0.0043(11) -0.0025(11) -0.0022(11) Cr2 0.0143(2) 0.0144(2) 0.0131(2) -0.0048(2) 0.0014(2) -0.0043(2) Cl3 0.0216(3) 0.0176(3) 0.0168(3) -0.0044(3) 0.0001(3) -0.0029(3) Cl4 0.0218(3) 0.0184(3) 0.0182(3) -0.0089(3) 0.0041(3) -0.0066(3) Cl5 0.0153(3) 0.0212(3) 0.0229(4) -0.0089(3) 0.0030(3) -0.0062(3) Cl6 0.0188(3) 0.0173(3) 0.0160(3) -0.0062(3) 0.0002(3) -0.0037(3) N5 0.0179(13) 0.0218(12) 0.0137(11) -0.0062(10) 0.0026(9) -0.0073(10) C21 0.0285(17) 0.0158(14) 0.0148(14) -0.0060(12) 0.0023(12) -0.0080(12) C22 0.0223(16) 0.0250(16) 0.0339(18) -0.0141(15) 0.0096(13) -0.0089(13) _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 2.056(2) . ? Cr1 N1 2.057(2) . ? Cr1 N2 2.057(2) . ? Cr1 N4 2.075(2) . ? Cr1 Cl1 2.2919(7) . ? Cr1 Cl2 2.3085(8) . ? N1 C1 1.326(4) . ? N1 C5 1.362(3) . ? N4 C20 1.340(3) . ? N4 C16 1.358(3) . ? N2 C10 1.336(4) . ? N2 C6 1.358(3) . ? C14 C13 1.377(4) . ? C14 C15 1.384(4) . ? C14 H14 0.9300 . ? N3 C11 1.340(3) . ? N3 C15 1.358(3) . ? C11 C12 1.383(4) . ? C11 H11 0.9300 . ? C20 C19 1.371(4) . ? C20 H20 0.9300 . ? C16 C17 1.387(4) . ? C16 C15 1.473(4) . ? C4 C5 1.380(4) . ? C4 C3 1.380(4) . ? C4 H4 0.9300 . ? C6 C7 1.379(4) . ? C6 C5 1.470(4) . ? C19 C18 1.376(4) . ? C19 H19 0.9300 . ? C17 C18 1.388(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C10 C9 1.382(4) . ? C10 H10 0.9300 . ? C9 C8 1.386(4) . ? C9 H9 0.9300 . ? C2 C3 1.381(4) . ? C2 C1 1.384(4) . ? C2 H2 0.9300 . ? C13 C12 1.379(4) . ? C13 H13 0.9300 . ? C7 C8 1.373(4) . ? C7 H7 0.9300 . ? C1 H1 0.9300 . ? C3 H3 0.9300 . ? C12 H12 0.9300 . ? C8 H8 0.9300 . ? Cr2 N5 2.068(2) . ? Cr2 Cl4 2.2970(8) . ? Cr2 Cl3 2.2975(8) . ? Cr2 Cl5 2.3058(8) . ? Cr2 Cl6 2.4007(8) . ? Cr2 Cl6 2.4085(8) 2_666 ? Cl6 Cr2 2.4085(8) 2_666 ? N5 C21 1.122(4) . ? C21 C22 1.455(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 N3 Cr1 N1 96.47(9) . . ? N3 Cr1 N2 172.72(9) . . ? N1 Cr1 N2 79.26(9) . . ? N3 Cr1 N4 78.87(9) . . ? N1 Cr1 N4 87.38(8) . . ? N2 Cr1 N4 94.96(9) . . ? N3 Cr1 Cl1 95.94(7) . . ? N1 Cr1 Cl1 89.21(6) . . ? N2 Cr1 Cl1 89.93(6) . . ? N4 Cr1 Cl1 173.43(7) . . ? N3 Cr1 Cl2 88.29(6) . . ? N1 Cr1 Cl2 173.88(6) . . ? N2 Cr1 Cl2 95.60(7) . . ? N4 Cr1 Cl2 89.78(6) . . ? Cl1 Cr1 Cl2 94.13(3) . . ? C1 N1 C5 119.2(2) . . ? C1 N1 Cr1 125.69(18) . . ? C5 N1 Cr1 115.06(18) . . ? C20 N4 C16 119.4(2) . . ? C20 N4 Cr1 126.26(19) . . ? C16 N4 Cr1 114.31(17) . . ? C10 N2 C6 119.0(2) . . ? C10 N2 Cr1 125.41(18) . . ? C6 N2 Cr1 115.18(18) . . ? C13 C14 C15 119.2(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C11 N3 C15 118.6(2) . . ? C11 N3 Cr1 125.55(18) . . ? C15 N3 Cr1 114.71(18) . . ? N3 C11 C12 122.6(2) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? N4 C20 C19 122.0(3) . . ? N4 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? N4 C16 C17 121.0(2) . . ? N4 C16 C15 115.4(2) . . ? C17 C16 C15 123.6(2) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N2 C6 C7 121.3(3) . . ? N2 C6 C5 114.9(2) . . ? C7 C6 C5 123.8(2) . . ? C20 C19 C18 119.4(3) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C16 C17 C18 118.8(3) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? N3 C15 C14 121.4(2) . . ? N3 C15 C16 114.4(2) . . ? C14 C15 C16 124.2(2) . . ? C19 C18 C17 119.4(3) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N2 C10 C9 122.2(3) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C9 C8 118.7(3) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C3 C2 C1 118.6(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C8 C7 C6 119.5(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? N1 C5 C4 120.9(2) . . ? N1 C5 C6 114.9(2) . . ? C4 C5 C6 124.2(2) . . ? N1 C1 C2 122.5(2) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C13 C12 C11 118.4(3) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C7 C8 C9 119.3(3) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? N5 Cr2 Cl4 85.46(7) . . ? N5 Cr2 Cl3 90.69(7) . . ? Cl4 Cr2 Cl3 95.10(3) . . ? N5 Cr2 Cl5 176.25(7) . . ? Cl4 Cr2 Cl5 94.32(3) . . ? Cl3 Cr2 Cl5 93.06(3) . . ? N5 Cr2 Cl6 85.62(7) . . ? Cl4 Cr2 Cl6 169.80(3) . . ? Cl3 Cr2 Cl6 89.93(3) . . ? Cl5 Cr2 Cl6 94.26(3) . . ? N5 Cr2 Cl6 84.70(7) . 2_666 ? Cl4 Cr2 Cl6 90.25(3) . 2_666 ? Cl3 Cr2 Cl6 172.65(3) . 2_666 ? Cl5 Cr2 Cl6 91.56(3) . 2_666 ? Cl6 Cr2 Cl6 84.02(3) . 2_666 ? Cr2 Cl6 Cr2 95.98(3) . 2_666 ? C21 N5 Cr2 168.7(2) . . ? N5 C21 C22 177.8(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cr1 N1 C1 5.2(2) . . . . ? N2 Cr1 N1 C1 179.2(2) . . . . ? N4 Cr1 N1 C1 83.7(2) . . . . ? Cl1 Cr1 N1 C1 -90.7(2) . . . . ? Cl2 Cr1 N1 C1 146.1(5) . . . . ? N3 Cr1 N1 C5 -171.93(18) . . . . ? N2 Cr1 N1 C5 2.11(17) . . . . ? N4 Cr1 N1 C5 -93.44(18) . . . . ? Cl1 Cr1 N1 C5 92.18(17) . . . . ? Cl2 Cr1 N1 C5 -31.0(7) . . . . ? N3 Cr1 N4 C20 173.1(2) . . . . ? N1 Cr1 N4 C20 75.9(2) . . . . ? N2 Cr1 N4 C20 -3.0(2) . . . . ? Cl1 Cr1 N4 C20 134.8(5) . . . . ? Cl2 Cr1 N4 C20 -98.6(2) . . . . ? N3 Cr1 N4 C16 -8.67(18) . . . . ? N1 Cr1 N4 C16 -105.79(18) . . . . ? N2 Cr1 N4 C16 175.23(18) . . . . ? Cl1 Cr1 N4 C16 -46.9(6) . . . . ? Cl2 Cr1 N4 C16 79.63(17) . . . . ? N3 Cr1 N2 C10 -129.7(7) . . . . ? N1 Cr1 N2 C10 175.7(2) . . . . ? N4 Cr1 N2 C10 -97.9(2) . . . . ? Cl1 Cr1 N2 C10 86.5(2) . . . . ? Cl2 Cr1 N2 C10 -7.6(2) . . . . ? N3 Cr1 N2 C6 57.9(8) . . . . ? N1 Cr1 N2 C6 3.30(18) . . . . ? N4 Cr1 N2 C6 89.69(18) . . . . ? Cl1 Cr1 N2 C6 -85.91(18) . . . . ? Cl2 Cr1 N2 C6 179.95(17) . . . . ? N1 Cr1 N3 C11 -92.8(2) . . . . ? N2 Cr1 N3 C11 -146.5(6) . . . . ? N4 Cr1 N3 C11 -178.8(2) . . . . ? Cl1 Cr1 N3 C11 -2.9(2) . . . . ? Cl2 Cr1 N3 C11 91.1(2) . . . . ? N1 Cr1 N3 C15 99.77(19) . . . . ? N2 Cr1 N3 C15 46.1(8) . . . . ? N4 Cr1 N3 C15 13.74(18) . . . . ? Cl1 Cr1 N3 C15 -170.35(17) . . . . ? Cl2 Cr1 N3 C15 -76.37(18) . . . . ? C15 N3 C11 C12 1.6(4) . . . . ? Cr1 N3 C11 C12 -165.4(2) . . . . ? C16 N4 C20 C19 0.2(4) . . . . ? Cr1 N4 C20 C19 178.4(2) . . . . ? C20 N4 C16 C17 -1.0(4) . . . . ? Cr1 N4 C16 C17 -179.4(2) . . . . ? C20 N4 C16 C15 -178.9(2) . . . . ? Cr1 N4 C16 C15 2.7(3) . . . . ? C10 N2 C6 C7 -2.1(4) . . . . ? Cr1 N2 C6 C7 170.88(19) . . . . ? C10 N2 C6 C5 179.2(2) . . . . ? Cr1 N2 C6 C5 -7.8(3) . . . . ? N4 C20 C19 C18 0.0(4) . . . . ? N4 C16 C17 C18 1.5(4) . . . . ? C15 C16 C17 C18 179.2(3) . . . . ? C11 N3 C15 C14 -4.6(4) . . . . ? Cr1 N3 C15 C14 163.8(2) . . . . ? C11 N3 C15 C16 175.3(2) . . . . ? Cr1 N3 C15 C16 -16.3(3) . . . . ? C13 C14 C15 N3 3.0(4) . . . . ? C13 C14 C15 C16 -176.9(3) . . . . ? N4 C16 C15 N3 8.9(3) . . . . ? C17 C16 C15 N3 -168.9(2) . . . . ? N4 C16 C15 C14 -171.2(2) . . . . ? C17 C16 C15 C14 11.1(4) . . . . ? C20 C19 C18 C17 0.5(4) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C6 N2 C10 C9 1.6(4) . . . . ? Cr1 N2 C10 C9 -170.5(2) . . . . ? N2 C10 C9 C8 0.4(5) . . . . ? C15 C14 C13 C12 1.6(4) . . . . ? N2 C6 C7 C8 0.4(4) . . . . ? C5 C6 C7 C8 179.0(3) . . . . ? C1 N1 C5 C4 -3.2(4) . . . . ? Cr1 N1 C5 C4 174.1(2) . . . . ? C1 N1 C5 C6 175.9(2) . . . . ? Cr1 N1 C5 C6 -6.8(3) . . . . ? C3 C4 C5 N1 1.9(4) . . . . ? C3 C4 C5 C6 -177.1(3) . . . . ? N2 C6 C5 N1 9.6(3) . . . . ? C7 C6 C5 N1 -169.0(2) . . . . ? N2 C6 C5 C4 -171.3(2) . . . . ? C7 C6 C5 C4 10.0(4) . . . . ? C5 N1 C1 C2 1.6(4) . . . . ? Cr1 N1 C1 C2 -175.4(2) . . . . ? C3 C2 C1 N1 1.2(4) . . . . ? C5 C4 C3 C2 1.0(4) . . . . ? C1 C2 C3 C4 -2.5(4) . . . . ? C14 C13 C12 C11 -4.5(4) . . . . ? N3 C11 C12 C13 3.0(4) . . . . ? C6 C7 C8 C9 1.6(4) . . . . ? C10 C9 C8 C7 -2.0(4) . . . . ? N5 Cr2 Cl6 Cr2 -85.11(7) . . . 2_666 ? Cl4 Cr2 Cl6 Cr2 -56.11(17) . . . 2_666 ? Cl3 Cr2 Cl6 Cr2 -175.81(3) . . . 2_666 ? Cl5 Cr2 Cl6 Cr2 91.13(3) . . . 2_666 ? Cl6 Cr2 Cl6 Cr2 0.0 2_666 . . 2_666 ? Cl4 Cr2 N5 C21 -71.8(13) . . . . ? Cl3 Cr2 N5 C21 -166.9(13) . . . . ? Cl5 Cr2 N5 C21 15(2) . . . . ? Cl6 Cr2 N5 C21 103.2(13) . . . . ? Cl6 Cr2 N5 C21 18.8(13) 2_666 . . . ? Cr2 N5 C21 C22 -1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.574 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.106 # Attachment '- 2.cif' data_cr4_2 _database_code_depnum_ccdc_archive 'CCDC 810901' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cr4(tmp)2(bpy)3Cl6],2.5(MeCN)' _chemical_melting_point ? _chemical_formula_moiety '(C42 H46 Cl6 Cr4 N6 O6), 2.5(C2 H3 N)' _chemical_formula_sum 'C47 H53.50 Cl6 Cr4 N8.50 O6' _chemical_formula_weight 1254.18 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' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.841(2) _cell_length_b 12.681(3) _cell_length_c 19.725(4) _cell_angle_alpha 83.13(3) _cell_angle_beta 77.85(3) _cell_angle_gamma 64.92(3) _cell_volume 2620.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3802 _cell_measurement_theta_min 2.359 _cell_measurement_theta_max 26.031 _exptl_crystal_description PLATE _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1282 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20926 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10547 _reflns_number_gt 8197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0436P)^2^+4.6126P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10547 _refine_ls_number_parameters 697 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.008 _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 0.75622(6) 0.36965(5) 0.24953(3) 0.01018(14) Uani 1 1 d . . . Cr2 Cr 0.94143(6) 0.26172(5) 0.11886(3) 0.01204(14) Uani 1 1 d . . . Cr3 Cr 0.69040(6) 0.21874(5) 0.36943(3) 0.01124(14) Uani 1 1 d . . . Cr4 Cr 0.64738(6) 0.63116(5) 0.26411(3) 0.01165(14) Uani 1 1 d . . . Cl1 Cl 1.01863(9) 0.40523(8) 0.09973(5) 0.0148(2) Uani 1 1 d . . . Cl2 Cl 1.14764(9) 0.11771(8) 0.09782(5) 0.0186(2) Uani 1 1 d . . . Cl3 Cl 0.88177(9) 0.05594(8) 0.34532(5) 0.0165(2) Uani 1 1 d . . . Cl4 Cl 0.70585(9) 0.19839(8) 0.48594(5) 0.0166(2) Uani 1 1 d . . . Cl5 Cl 0.64212(9) 0.62494(8) 0.38225(5) 0.0157(2) Uani 1 1 d . . . Cl6 Cl 0.73526(10) 0.76690(8) 0.24971(5) 0.0198(2) Uani 1 1 d . . . N1 N 0.9209(3) 0.2642(3) 0.01556(16) 0.0157(7) Uani 1 1 d . . . N2 N 0.8810(3) 0.1317(3) 0.12022(16) 0.0165(7) Uani 1 1 d . . . N3 N 0.5830(3) 0.1191(3) 0.38602(15) 0.0130(7) Uani 1 1 d . . . N4 N 0.5100(3) 0.3414(3) 0.40182(15) 0.0131(7) Uani 1 1 d . . . N5 N 0.4607(3) 0.7558(3) 0.27128(16) 0.0143(7) Uani 1 1 d . . . N6 N 0.6300(3) 0.6741(3) 0.16072(16) 0.0151(7) Uani 1 1 d . . . O1 O 0.9297(2) 0.2563(2) 0.21936(13) 0.0124(5) Uani 1 1 d . . . O2 O 0.7673(2) 0.3307(2) 0.34691(12) 0.0115(5) Uani 1 1 d . . . O3 O 0.8094(2) 0.4955(2) 0.24772(12) 0.0106(5) Uani 1 1 d . . . O4 O 0.7622(2) 0.3710(2) 0.14951(12) 0.0122(5) Uani 1 1 d . . . O5 O 0.6739(2) 0.2608(2) 0.26994(13) 0.0146(6) Uani 1 1 d . . . O6 O 0.5920(2) 0.5038(2) 0.26269(13) 0.0127(5) Uani 1 1 d . . . C1 C 1.0231(4) 0.2512(3) 0.25660(19) 0.0143(8) Uani 1 1 d . . . H1A H 1.0938 0.2572 0.2237 0.017 Uiso 1 1 calc R . . H1B H 1.0545 0.1761 0.2809 0.017 Uiso 1 1 calc R . . C2 C 0.8752(3) 0.3303(3) 0.36937(19) 0.0126(8) Uani 1 1 d . . . H2A H 0.9160 0.2568 0.3937 0.015 Uiso 1 1 calc R . . H2B H 0.8465 0.3920 0.4019 0.015 Uiso 1 1 calc R . . C3 C 0.9200(3) 0.4708(3) 0.27591(19) 0.0128(8) Uani 1 1 d . . . H3A H 0.8996 0.5273 0.3106 0.015 Uiso 1 1 calc R . . H3B H 0.9848 0.4793 0.2392 0.015 Uiso 1 1 calc R . . C4 C 0.9733(3) 0.3475(3) 0.30922(19) 0.0122(8) Uani 1 1 d . . . C5 C 1.0861(4) 0.3338(3) 0.3429(2) 0.0156(8) Uani 1 1 d . . . H5A H 1.0533 0.3844 0.3821 0.019 Uiso 1 1 calc R . . H5B H 1.1234 0.2543 0.3610 0.019 Uiso 1 1 calc R . . C6 C 1.1903(4) 0.3607(4) 0.2957(2) 0.0243(10) Uani 1 1 d . . . H6A H 1.2173 0.3179 0.2540 0.036 Uiso 1 1 calc R . . H6B H 1.2609 0.3387 0.3191 0.036 Uiso 1 1 calc R . . H6C H 1.1588 0.4427 0.2841 0.036 Uiso 1 1 calc R . . C7 C 0.6490(4) 0.3877(3) 0.12718(19) 0.0157(8) Uani 1 1 d . A . H7A H 0.6671 0.3242 0.0979 0.019 Uiso 1 1 calc R . . H7B H 0.6219 0.4594 0.0992 0.019 Uiso 1 1 calc R . . C8 C 0.5743(4) 0.2814(3) 0.2336(2) 0.0169(8) Uani 1 1 d . A . H8A H 0.4996 0.2860 0.2670 0.020 Uiso 1 1 calc R . . H8B H 0.5990 0.2156 0.2048 0.020 Uiso 1 1 calc R . . C9 C 0.4954(4) 0.5010(3) 0.2310(2) 0.0161(8) Uani 1 1 d . A . H9A H 0.4648 0.5706 0.2016 0.019 Uiso 1 1 calc R . . H9B H 0.4250 0.5026 0.2670 0.019 Uiso 1 1 calc R . . C10 C 0.5395(4) 0.3939(3) 0.1873(2) 0.0152(8) Uani 1 1 d . . . C11 C 0.4257(4) 0.4052(4) 0.1554(2) 0.0273(10) Uani 0.718(10) 1 d PD A 1 H11A H 0.4407 0.3278 0.1434 0.033 Uiso 0.718(10) 1 calc PR A 1 H11B H 0.3511 0.4309 0.1915 0.033 Uiso 0.718(10) 1 calc PR A 1 C12 C 0.3947(6) 0.4831(6) 0.0938(3) 0.0310(19) Uani 0.718(10) 1 d P A 1 H12A H 0.4655 0.4573 0.0563 0.046 Uiso 0.718(10) 1 calc PR A 1 H12B H 0.3763 0.5612 0.1046 0.046 Uiso 0.718(10) 1 calc PR A 1 H12C H 0.3221 0.4814 0.0804 0.046 Uiso 0.718(10) 1 calc PR A 1 C11X C 0.4257(4) 0.4052(4) 0.1554(2) 0.0273(10) Uani 0.282(10) 1 d P A 2 H11C H 0.3566 0.4189 0.1945 0.033 Uiso 0.282(10) 1 calc PR A 2 H11D H 0.4038 0.4779 0.1283 0.033 Uiso 0.282(10) 1 calc PR A 2 C12X C 0.4152(16) 0.3294(14) 0.1153(8) 0.033(5) Uani 0.282(10) 1 d PD A 2 H12D H 0.3393 0.3682 0.0958 0.050 Uiso 0.282(10) 1 calc PR A 2 H12E H 0.4115 0.2634 0.1435 0.050 Uiso 0.282(10) 1 calc PR A 2 H12F H 0.4874 0.3037 0.0786 0.050 Uiso 0.282(10) 1 calc PR A 2 C13 C 0.9468(4) 0.3343(4) -0.0361(2) 0.0204(9) Uani 1 1 d . . . H13 H 0.9728 0.3894 -0.0259 0.024 Uiso 1 1 calc R . . C14 C 0.9361(5) 0.3277(4) -0.1031(2) 0.0340(12) Uani 1 1 d . . . H14 H 0.9557 0.3767 -0.1379 0.041 Uiso 1 1 calc R . . C15 C 0.8958(5) 0.2468(4) -0.1182(2) 0.0355(12) Uani 1 1 d . . . H15 H 0.8874 0.2415 -0.1634 0.043 Uiso 1 1 calc R . . C16 C 0.8680(4) 0.1742(4) -0.0661(2) 0.0271(10) Uani 1 1 d . . . H16 H 0.8409 0.1195 -0.0755 0.033 Uiso 1 1 calc R . . C17 C 0.8813(4) 0.1844(4) 0.0007(2) 0.0186(9) Uani 1 1 d . . . C18 C 0.8576(4) 0.1101(3) 0.06014(19) 0.0162(8) Uani 1 1 d . . . C19 C 0.8149(4) 0.0254(4) 0.0574(2) 0.0251(10) Uani 1 1 d . . . H19 H 0.7982 0.0122 0.0159 0.030 Uiso 1 1 calc R . . C20 C 0.7969(5) -0.0397(4) 0.1166(2) 0.0304(11) Uani 1 1 d . . . H20 H 0.7669 -0.0964 0.1157 0.036 Uiso 1 1 calc R . . C21 C 0.8243(5) -0.0194(4) 0.1772(2) 0.0278(11) Uani 1 1 d . . . H21 H 0.8141 -0.0631 0.2176 0.033 Uiso 1 1 calc R . . C22 C 0.8667(4) 0.0661(3) 0.1773(2) 0.0210(9) Uani 1 1 d . . . H22 H 0.8860 0.0789 0.2180 0.025 Uiso 1 1 calc R . . C23 C 0.6278(4) 0.0041(3) 0.3784(2) 0.0192(9) Uani 1 1 d . . . H23 H 0.7129 -0.0360 0.3597 0.023 Uiso 1 1 calc R . . C24 C 0.5528(4) -0.0577(4) 0.3974(2) 0.0230(10) Uani 1 1 d . . . H24 H 0.5869 -0.1376 0.3915 0.028 Uiso 1 1 calc R . . C25 C 0.4270(4) 0.0015(4) 0.4251(2) 0.0241(10) Uani 1 1 d . . . H25 H 0.3751 -0.0383 0.4388 0.029 Uiso 1 1 calc R . . C26 C 0.3781(4) 0.1199(4) 0.4325(2) 0.0190(9) Uani 1 1 d . . . H26 H 0.2927 0.1610 0.4502 0.023 Uiso 1 1 calc R . . C27 C 0.4577(4) 0.1778(3) 0.41312(19) 0.0149(8) Uani 1 1 d . . . C28 C 0.4169(4) 0.3024(3) 0.42143(19) 0.0144(8) Uani 1 1 d . . . C29 C 0.2947(4) 0.3770(3) 0.4491(2) 0.0178(9) Uani 1 1 d . . . H29 H 0.2313 0.3498 0.4615 0.021 Uiso 1 1 calc R . . C30 C 0.2676(4) 0.4920(4) 0.4580(2) 0.0203(9) Uani 1 1 d . . . H30 H 0.1856 0.5432 0.4758 0.024 Uiso 1 1 calc R . . C31 C 0.3632(4) 0.5301(4) 0.4402(2) 0.0216(9) Uani 1 1 d . . . H31 H 0.3471 0.6069 0.4468 0.026 Uiso 1 1 calc R . . C32 C 0.4835(4) 0.4524(3) 0.41249(19) 0.0176(9) Uani 1 1 d . . . H32 H 0.5481 0.4782 0.4008 0.021 Uiso 1 1 calc R . . C33 C 0.3753(4) 0.7885(3) 0.3300(2) 0.0189(9) Uani 1 1 d . . . H33 H 0.4019 0.7586 0.3721 0.023 Uiso 1 1 calc R . . C34 C 0.2512(4) 0.8634(4) 0.3310(2) 0.0263(10) Uani 1 1 d . . . H34 H 0.1948 0.8831 0.3728 0.032 Uiso 1 1 calc R . . C35 C 0.2113(4) 0.9092(4) 0.2690(2) 0.0278(10) Uani 1 1 d . . . H35 H 0.1272 0.9597 0.2683 0.033 Uiso 1 1 calc R . . C36 C 0.2981(4) 0.8791(4) 0.2077(2) 0.0246(10) Uani 1 1 d . . . H36 H 0.2735 0.9102 0.1653 0.030 Uiso 1 1 calc R . . C37 C 0.4212(4) 0.8025(3) 0.2104(2) 0.0184(9) Uani 1 1 d . . . C38 C 0.5211(4) 0.7629(3) 0.1483(2) 0.0185(9) Uani 1 1 d . . . C39 C 0.5087(4) 0.8127(4) 0.0826(2) 0.0307(11) Uani 1 1 d . . . H39 H 0.4336 0.8743 0.0747 0.037 Uiso 1 1 calc R . . C40 C 0.6092(5) 0.7699(5) 0.0288(2) 0.0391(13) Uani 1 1 d . . . H40 H 0.6025 0.8026 -0.0157 0.047 Uiso 1 1 calc R . . C41 C 0.7193(4) 0.6787(4) 0.0412(2) 0.0308(11) Uani 1 1 d . . . H41 H 0.7876 0.6486 0.0052 0.037 Uiso 1 1 calc R . . C42 C 0.7270(4) 0.6321(4) 0.10808(19) 0.0184(9) Uani 1 1 d . . . H42 H 0.8014 0.5703 0.1167 0.022 Uiso 1 1 calc R . . N1S N 0.4969(7) 0.0784(6) 0.1114(3) 0.091(2) Uani 1 1 d D . . C1S C 0.4690(7) 0.0679(6) 0.1705(4) 0.0615(18) Uani 1 1 d D . . C2S C 0.4375(7) 0.0529(6) 0.2453(3) 0.0646(18) Uani 1 1 d D . . H2S1 H 0.5037 -0.0151 0.2612 0.097 Uiso 1 1 calc R . . H2S2 H 0.3592 0.0439 0.2569 0.097 Uiso 1 1 calc R . . H2S3 H 0.4289 0.1202 0.2673 0.097 Uiso 1 1 calc R . . N2S N 0.9372(10) 0.7146(12) 0.4630(5) 0.079(4) Uani 0.531(11) 1 d PDU B 1 C3S C 0.9571(12) 0.7285(9) 0.4026(6) 0.038(3) Uani 0.531(11) 1 d PDU B 1 C4S C 0.9999(17) 0.7338(13) 0.3313(7) 0.047(4) Uani 0.531(11) 1 d PDU B 1 H4S1 H 1.0875 0.6810 0.3206 0.071 Uiso 0.531(11) 1 calc PR B 1 H4S2 H 0.9910 0.8117 0.3172 0.071 Uiso 0.531(11) 1 calc PR B 1 H4S3 H 0.9508 0.7125 0.3071 0.071 Uiso 0.531(11) 1 calc PR B 1 N2SX N 1.1207(12) 0.6695(10) 0.2870(6) 0.067(4) Uani 0.469(11) 1 d PDU B 2 C3SX C 1.0375(17) 0.6861(15) 0.3328(9) 0.046(4) Uani 0.469(11) 1 d PDU B 2 C4SX C 0.9363(17) 0.7016(19) 0.3905(9) 0.077(6) Uani 0.469(11) 1 d PDU B 2 H4S4 H 0.8742 0.6815 0.3777 0.116 Uiso 0.469(11) 1 calc PR B 2 H4S5 H 0.8976 0.7815 0.4035 0.116 Uiso 0.469(11) 1 calc PR B 2 H4S6 H 0.9691 0.6523 0.4289 0.116 Uiso 0.469(11) 1 calc PR B 2 N3S N 0.0861(8) 1.1179(7) 0.4794(4) 0.035(2) Uani 0.50 1 d PD C -2 C5S C 0.046(3) 1.048(2) 0.489(2) 0.040(6) Uani 0.50 1 d PD C -2 C6S C -0.011(2) 0.961(2) 0.5042(17) 0.032(5) Uani 0.50 1 d PD C -2 H6S H -0.0417 0.9579 0.5532 0.048 Uiso 0.50 1 calc PR C -2 H6T H 0.0517 0.8862 0.4897 0.048 Uiso 0.50 1 calc PR C -2 H6U H -0.0805 0.9842 0.4797 0.048 Uiso 0.50 1 calc PR C -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 Cr1 0.0141(3) 0.0103(3) 0.0097(3) 0.0007(2) -0.0013(2) -0.0090(3) Cr2 0.0188(3) 0.0111(3) 0.0101(3) -0.0004(2) -0.0003(2) -0.0109(3) Cr3 0.0161(3) 0.0096(3) 0.0108(3) 0.0002(2) 0.0000(2) -0.0092(3) Cr4 0.0155(3) 0.0094(3) 0.0113(3) 0.0018(2) -0.0014(2) -0.0072(3) Cl1 0.0188(5) 0.0133(5) 0.0154(5) 0.0001(4) 0.0003(4) -0.0113(4) Cl2 0.0230(5) 0.0139(5) 0.0172(5) -0.0021(4) -0.0014(4) -0.0065(4) Cl3 0.0189(5) 0.0132(5) 0.0163(5) -0.0001(4) -0.0003(4) -0.0071(4) Cl4 0.0260(5) 0.0153(5) 0.0119(5) 0.0017(4) -0.0024(4) -0.0128(4) Cl5 0.0239(5) 0.0142(5) 0.0119(5) 0.0009(4) -0.0023(4) -0.0114(4) Cl6 0.0301(6) 0.0153(5) 0.0202(5) 0.0025(4) -0.0025(4) -0.0169(4) N1 0.0217(18) 0.0193(18) 0.0091(16) -0.0005(13) 0.0006(13) -0.0127(15) N2 0.0263(19) 0.0166(18) 0.0114(16) -0.0019(13) 0.0021(14) -0.0155(15) N3 0.0190(17) 0.0114(16) 0.0113(16) -0.0002(13) -0.0008(13) -0.0097(14) N4 0.0199(17) 0.0130(16) 0.0096(16) 0.0011(13) -0.0028(13) -0.0101(14) N5 0.0165(17) 0.0115(16) 0.0154(17) 0.0025(13) -0.0022(13) -0.0072(14) N6 0.0168(17) 0.0140(17) 0.0148(17) 0.0008(13) -0.0024(13) -0.0073(14) O1 0.0138(13) 0.0110(13) 0.0124(13) 0.0000(10) -0.0025(11) -0.0051(11) O2 0.0153(14) 0.0117(13) 0.0109(13) 0.0017(10) -0.0025(10) -0.0093(11) O3 0.0135(13) 0.0094(13) 0.0128(13) 0.0007(10) -0.0030(10) -0.0084(11) O4 0.0167(14) 0.0137(14) 0.0104(13) 0.0012(10) -0.0031(10) -0.0103(11) O5 0.0208(15) 0.0178(14) 0.0099(13) -0.0009(11) -0.0012(11) -0.0131(12) O6 0.0141(13) 0.0143(14) 0.0130(13) 0.0018(11) -0.0030(11) -0.0093(11) C1 0.016(2) 0.015(2) 0.015(2) 0.0037(15) -0.0036(16) -0.0098(16) C2 0.016(2) 0.0141(19) 0.0123(19) 0.0010(15) -0.0034(15) -0.0108(16) C3 0.0151(19) 0.0113(19) 0.017(2) -0.0008(15) -0.0027(15) -0.0101(16) C4 0.0136(19) 0.0139(19) 0.0132(19) 0.0005(15) -0.0033(15) -0.0093(16) C5 0.016(2) 0.019(2) 0.015(2) 0.0007(16) -0.0048(16) -0.0101(17) C6 0.020(2) 0.036(3) 0.023(2) 0.0043(19) -0.0092(18) -0.016(2) C7 0.020(2) 0.017(2) 0.014(2) -0.0006(16) -0.0036(16) -0.0117(17) C8 0.023(2) 0.019(2) 0.015(2) 0.0010(16) -0.0051(16) -0.0153(18) C9 0.014(2) 0.020(2) 0.017(2) 0.0030(16) -0.0041(16) -0.0098(17) C10 0.018(2) 0.019(2) 0.016(2) 0.0018(16) -0.0055(16) -0.0134(17) C11 0.025(2) 0.050(3) 0.019(2) 0.000(2) -0.0050(18) -0.026(2) C12 0.028(4) 0.036(4) 0.036(4) 0.012(3) -0.020(3) -0.016(3) C11X 0.025(2) 0.050(3) 0.019(2) 0.000(2) -0.0050(18) -0.026(2) C12X 0.036(10) 0.040(11) 0.032(10) -0.024(8) -0.006(8) -0.016(8) C13 0.031(2) 0.021(2) 0.014(2) -0.0005(17) -0.0015(17) -0.0176(19) C14 0.060(3) 0.037(3) 0.018(2) 0.005(2) -0.007(2) -0.035(3) C15 0.069(4) 0.041(3) 0.012(2) 0.003(2) -0.011(2) -0.036(3) C16 0.046(3) 0.030(3) 0.019(2) 0.0018(19) -0.006(2) -0.029(2) C17 0.024(2) 0.021(2) 0.015(2) -0.0025(17) -0.0012(17) -0.0140(19) C18 0.025(2) 0.017(2) 0.0114(19) -0.0009(16) -0.0006(16) -0.0145(18) C19 0.041(3) 0.028(2) 0.018(2) -0.0075(18) 0.0023(19) -0.027(2) C20 0.052(3) 0.025(2) 0.025(2) -0.0055(19) 0.003(2) -0.030(2) C21 0.051(3) 0.025(2) 0.015(2) -0.0010(18) 0.004(2) -0.028(2) C22 0.034(2) 0.015(2) 0.018(2) -0.0027(17) 0.0012(18) -0.0154(19) C23 0.026(2) 0.018(2) 0.019(2) -0.0006(17) -0.0033(17) -0.0147(19) C24 0.037(3) 0.014(2) 0.025(2) -0.0032(17) -0.0032(19) -0.017(2) C25 0.037(3) 0.028(2) 0.021(2) 0.0005(18) -0.0015(19) -0.029(2) C26 0.023(2) 0.023(2) 0.019(2) -0.0002(17) -0.0071(17) -0.0166(19) C27 0.021(2) 0.019(2) 0.0104(19) 0.0019(15) -0.0037(16) -0.0138(17) C28 0.018(2) 0.018(2) 0.0108(19) 0.0022(15) -0.0042(15) -0.0112(17) C29 0.018(2) 0.023(2) 0.015(2) -0.0007(17) -0.0031(16) -0.0114(18) C30 0.020(2) 0.021(2) 0.016(2) -0.0055(17) -0.0025(17) -0.0040(18) C31 0.033(2) 0.013(2) 0.018(2) 0.0004(16) -0.0032(18) -0.0091(19) C32 0.025(2) 0.016(2) 0.014(2) 0.0008(16) -0.0023(17) -0.0116(18) C33 0.021(2) 0.015(2) 0.019(2) -0.0027(16) 0.0018(17) -0.0073(17) C34 0.027(2) 0.026(2) 0.024(2) -0.0051(19) 0.0048(19) -0.012(2) C35 0.020(2) 0.015(2) 0.042(3) -0.005(2) -0.005(2) 0.0003(18) C36 0.026(2) 0.017(2) 0.031(3) 0.0046(19) -0.011(2) -0.0083(19) C37 0.021(2) 0.013(2) 0.021(2) 0.0053(16) -0.0039(17) -0.0073(17) C38 0.022(2) 0.017(2) 0.018(2) 0.0082(17) -0.0057(17) -0.0110(18) C39 0.025(2) 0.037(3) 0.025(2) 0.014(2) -0.0086(19) -0.009(2) C40 0.038(3) 0.061(4) 0.016(2) 0.016(2) -0.007(2) -0.022(3) C41 0.026(3) 0.050(3) 0.016(2) 0.002(2) 0.0004(19) -0.018(2) C42 0.019(2) 0.025(2) 0.014(2) 0.0016(17) -0.0015(16) -0.0130(18) N1S 0.109(6) 0.095(5) 0.066(4) 0.024(4) -0.037(4) -0.035(4) C1S 0.075(5) 0.051(4) 0.061(4) 0.010(3) -0.027(4) -0.026(4) C2S 0.079(5) 0.055(4) 0.070(5) -0.001(3) -0.016(4) -0.036(4) N2S 0.051(7) 0.127(11) 0.067(6) 0.020(7) -0.009(6) -0.050(7) C3S 0.035(6) 0.013(5) 0.060(6) -0.005(5) 0.009(6) -0.013(5) C4S 0.062(10) 0.031(9) 0.057(6) -0.002(7) -0.025(7) -0.022(8) N2SX 0.088(9) 0.071(9) 0.046(7) 0.018(6) -0.009(5) -0.044(8) C3SX 0.063(11) 0.035(10) 0.047(7) 0.011(7) -0.025(6) -0.024(9) C4SX 0.076(11) 0.098(14) 0.085(11) -0.071(11) 0.018(7) -0.058(10) N3S 0.036(5) 0.026(5) 0.046(5) 0.016(4) -0.019(4) -0.015(4) C5S 0.031(15) 0.034(10) 0.033(12) 0.006(7) -0.012(11) 0.008(7) C6S 0.025(12) 0.037(10) 0.012(7) 0.003(8) -0.004(8) 0.007(8) _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 O2 1.943(3) . ? Cr1 O3 1.943(2) . ? Cr1 O1 1.956(3) . ? Cr1 O4 1.957(3) . ? Cr1 O6 1.958(3) . ? Cr1 O5 1.965(3) . ? Cr2 O1 1.953(3) . ? Cr2 O4 1.989(3) . ? Cr2 N2 2.053(3) . ? Cr2 N1 2.097(3) . ? Cr2 Cl1 2.3218(12) . ? Cr2 Cl2 2.3333(15) . ? Cr3 O2 1.953(2) . ? Cr3 O5 1.999(3) . ? Cr3 N4 2.058(3) . ? Cr3 N3 2.099(3) . ? Cr3 Cl4 2.3188(12) . ? Cr3 Cl3 2.3321(15) . ? Cr4 O3 1.954(3) . ? Cr4 O6 1.989(3) . ? Cr4 N6 2.077(3) . ? Cr4 N5 2.089(3) . ? Cr4 Cl5 2.3107(12) . ? Cr4 Cl6 2.3246(12) . ? N1 C13 1.343(5) . ? N1 C17 1.364(5) . ? N2 C22 1.342(5) . ? N2 C18 1.355(5) . ? N3 C23 1.339(5) . ? N3 C27 1.366(5) . ? N4 C32 1.339(5) . ? N4 C28 1.359(5) . ? N5 C33 1.342(5) . ? N5 C37 1.357(5) . ? N6 C42 1.339(5) . ? N6 C38 1.352(5) . ? O1 C1 1.428(4) . ? O2 C2 1.436(4) . ? O3 C3 1.428(4) . ? O4 C7 1.421(4) . ? O5 C8 1.423(4) . ? O6 C9 1.428(4) . ? C1 C4 1.534(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.542(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.538(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.551(5) . ? C5 C6 1.518(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C10 1.543(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C10 1.545(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.533(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.550(5) . ? C11 C12 1.477(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12X H12D 0.9600 . ? C12X H12E 0.9600 . ? C12X H12F 0.9600 . ? C13 C14 1.370(6) . ? C13 H13 0.9300 . ? C14 C15 1.385(6) . ? C14 H14 0.9300 . ? C15 C16 1.379(6) . ? C15 H15 0.9300 . ? C16 C17 1.386(6) . ? C16 H16 0.9300 . ? C17 C18 1.472(5) . ? C18 C19 1.378(5) . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 C21 1.382(6) . ? C20 H20 0.9300 . ? C21 C22 1.375(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.387(5) . ? C23 H23 0.9300 . ? C24 C25 1.375(6) . ? C24 H24 0.9300 . ? C25 C26 1.375(6) . ? C25 H25 0.9300 . ? C26 C27 1.393(5) . ? C26 H26 0.9300 . ? C27 C28 1.463(5) . ? C28 C29 1.385(5) . ? C29 C30 1.378(6) . ? C29 H29 0.9300 . ? C30 C31 1.376(6) . ? C30 H30 0.9300 . ? C31 C32 1.382(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.368(6) . ? C33 H33 0.9300 . ? C34 C35 1.377(6) . ? C34 H34 0.9300 . ? C35 C36 1.386(6) . ? C35 H35 0.9300 . ? C36 C37 1.376(6) . ? C36 H36 0.9300 . ? C37 C38 1.478(6) . ? C38 C39 1.381(6) . ? C39 C40 1.376(6) . ? C39 H39 0.9300 . ? C40 C41 1.373(7) . ? C40 H40 0.9300 . ? C41 C42 1.385(6) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? N1S C1S 1.151(7) . ? C1S C2S 1.454(8) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? N2S C3S 1.171(12) . ? C3S C4S 1.395(13) . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? N2SX C3SX 1.153(13) . ? C3SX C4SX 1.431(14) . ? C4SX H4S4 0.9600 . ? C4SX H4S5 0.9600 . ? C4SX H4S6 0.9600 . ? N3S C5S 1.153(19) . ? C5S C6S 1.490(13) . ? C6S H6S 0.9600 . ? C6S H6T 0.9600 . ? C6S H6U 0.9600 . ? 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 O2 Cr1 O3 92.97(11) . . ? O2 Cr1 O1 92.33(11) . . ? O3 Cr1 O1 92.66(11) . . ? O2 Cr1 O4 167.13(11) . . ? O3 Cr1 O4 96.70(11) . . ? O1 Cr1 O4 78.80(11) . . ? O2 Cr1 O6 97.53(11) . . ? O3 Cr1 O6 79.21(10) . . ? O1 Cr1 O6 167.49(11) . . ? O4 Cr1 O6 92.61(11) . . ? O2 Cr1 O5 78.96(11) . . ? O3 Cr1 O5 166.78(11) . . ? O1 Cr1 O5 98.07(11) . . ? O4 Cr1 O5 92.95(11) . . ? O6 Cr1 O5 91.37(11) . . ? O1 Cr2 O4 78.12(11) . . ? O1 Cr2 N2 94.38(12) . . ? O4 Cr2 N2 88.68(12) . . ? O1 Cr2 N1 168.99(12) . . ? O4 Cr2 N1 94.14(12) . . ? N2 Cr2 N1 77.46(13) . . ? O1 Cr2 Cl1 93.89(8) . . ? O4 Cr2 Cl1 94.87(8) . . ? N2 Cr2 Cl1 171.52(9) . . ? N1 Cr2 Cl1 94.58(9) . . ? O1 Cr2 Cl2 95.02(9) . . ? O4 Cr2 Cl2 171.58(8) . . ? N2 Cr2 Cl2 86.97(10) . . ? N1 Cr2 Cl2 91.94(10) . . ? Cl1 Cr2 Cl2 90.43(5) . . ? O2 Cr3 O5 77.89(11) . . ? O2 Cr3 N4 95.09(12) . . ? O5 Cr3 N4 91.22(12) . . ? O2 Cr3 N3 170.50(12) . . ? O5 Cr3 N3 95.76(11) . . ? N4 Cr3 N3 77.84(12) . . ? O2 Cr3 Cl4 94.84(8) . . ? O5 Cr3 Cl4 171.42(8) . . ? N4 Cr3 Cl4 84.82(10) . . ? N3 Cr3 Cl4 90.86(9) . . ? O2 Cr3 Cl3 94.57(8) . . ? O5 Cr3 Cl3 94.79(9) . . ? N4 Cr3 Cl3 169.51(9) . . ? N3 Cr3 Cl3 92.99(9) . . ? Cl4 Cr3 Cl3 90.31(5) . . ? O3 Cr4 O6 78.20(10) . . ? O3 Cr4 N6 96.93(12) . . ? O6 Cr4 N6 90.29(12) . . ? O3 Cr4 N5 167.88(12) . . ? O6 Cr4 N5 91.01(12) . . ? N6 Cr4 N5 77.42(13) . . ? O3 Cr4 Cl5 93.65(9) . . ? O6 Cr4 Cl5 97.55(8) . . ? N6 Cr4 Cl5 167.93(9) . . ? N5 Cr4 Cl5 93.22(10) . . ? O3 Cr4 Cl6 95.37(8) . . ? O6 Cr4 Cl6 170.76(8) . . ? N6 Cr4 Cl6 83.85(10) . . ? N5 Cr4 Cl6 94.67(9) . . ? Cl5 Cr4 Cl6 89.42(5) . . ? C13 N1 C17 118.7(3) . . ? C13 N1 Cr2 125.6(3) . . ? C17 N1 Cr2 115.7(3) . . ? C22 N2 C18 119.0(3) . . ? C22 N2 Cr2 123.0(3) . . ? C18 N2 Cr2 118.0(2) . . ? C23 N3 C27 118.3(3) . . ? C23 N3 Cr3 126.2(3) . . ? C27 N3 Cr3 115.1(2) . . ? C32 N4 C28 119.0(3) . . ? C32 N4 Cr3 123.6(3) . . ? C28 N4 Cr3 116.9(3) . . ? C33 N5 C37 117.6(3) . . ? C33 N5 Cr4 125.9(3) . . ? C37 N5 Cr4 116.3(3) . . ? C42 N6 C38 119.4(3) . . ? C42 N6 Cr4 123.0(3) . . ? C38 N6 Cr4 116.5(3) . . ? C1 O1 Cr2 127.5(2) . . ? C1 O1 Cr1 116.7(2) . . ? Cr2 O1 Cr1 102.14(12) . . ? C2 O2 Cr1 116.7(2) . . ? C2 O2 Cr3 129.1(2) . . ? Cr1 O2 Cr3 102.76(12) . . ? C3 O3 Cr1 117.4(2) . . ? C3 O3 Cr4 127.4(2) . . ? Cr1 O3 Cr4 102.15(11) . . ? C7 O4 Cr1 117.2(2) . . ? C7 O4 Cr2 131.2(2) . . ? Cr1 O4 Cr2 100.81(12) . . ? C8 O5 Cr1 116.8(2) . . ? C8 O5 Cr3 131.9(2) . . ? Cr1 O5 Cr3 100.35(12) . . ? C9 O6 Cr1 117.0(2) . . ? C9 O6 Cr4 130.1(2) . . ? Cr1 O6 Cr4 100.37(11) . . ? O1 C1 C4 113.4(3) . . ? O1 C1 H1A 108.9 . . ? C4 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C4 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O2 C2 C4 113.3(3) . . ? O2 C2 H2A 108.9 . . ? C4 C2 H2A 108.9 . . ? O2 C2 H2B 108.9 . . ? C4 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O3 C3 C4 112.9(3) . . ? O3 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? O3 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C1 C4 C3 113.1(3) . . ? C1 C4 C2 111.0(3) . . ? C3 C4 C2 111.2(3) . . ? C1 C4 C5 107.3(3) . . ? C3 C4 C5 108.5(3) . . ? C2 C4 C5 105.4(3) . . ? C6 C5 C4 115.9(3) . . ? C6 C5 H5A 108.3 . . ? C4 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C4 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C10 113.7(3) . . ? O4 C7 H7A 108.8 . . ? C10 C7 H7A 108.8 . . ? O4 C7 H7B 108.8 . . ? C10 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O5 C8 C10 113.9(3) . . ? O5 C8 H8A 108.8 . . ? C10 C8 H8A 108.8 . . ? O5 C8 H8B 108.8 . . ? C10 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O6 C9 C10 113.8(3) . . ? O6 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? O6 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C7 111.8(3) . . ? C9 C10 C8 110.7(3) . . ? C7 C10 C8 112.0(3) . . ? C9 C10 C11 107.5(3) . . ? C7 C10 C11 108.0(3) . . ? C8 C10 C11 106.6(3) . . ? C12 C11 C10 119.1(4) . . ? C12 C11 H11A 107.6 . . ? C10 C11 H11A 107.6 . . ? C12 C11 H11B 107.6 . . ? C10 C11 H11B 107.6 . . ? H11A C11 H11B 107.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H12D C12X H12E 109.5 . . ? H12D C12X H12F 109.5 . . ? H12E C12X H12F 109.5 . . ? N1 C13 C14 122.4(4) . . ? N1 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C13 C14 C15 119.0(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 118.7(4) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N1 C17 C16 121.5(4) . . ? N1 C17 C18 114.8(3) . . ? C16 C17 C18 123.7(4) . . ? N2 C18 C19 121.2(4) . . ? N2 C18 C17 114.1(3) . . ? C19 C18 C17 124.7(4) . . ? C18 C19 C20 119.5(4) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C21 119.0(4) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? C22 C21 C20 119.2(4) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N2 C22 C21 122.0(4) . . ? N2 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? N3 C23 C24 122.8(4) . . ? N3 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 118.7(4) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C26 C25 C24 119.7(4) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 119.4(4) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? N3 C27 C26 121.1(4) . . ? N3 C27 C28 115.0(3) . . ? C26 C27 C28 123.9(4) . . ? N4 C28 C29 120.9(4) . . ? N4 C28 C27 114.9(3) . . ? C29 C28 C27 124.1(4) . . ? C30 C29 C28 119.6(4) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 119.3(4) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 119.0(4) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? N4 C32 C31 122.2(4) . . ? N4 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? N5 C33 C34 123.3(4) . . ? N5 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C33 C34 C35 118.8(4) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C34 C35 C36 119.1(4) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 119.0(4) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? N5 C37 C36 122.1(4) . . ? N5 C37 C38 114.3(3) . . ? C36 C37 C38 123.6(4) . . ? N6 C38 C39 121.2(4) . . ? N6 C38 C37 114.6(3) . . ? C39 C38 C37 124.2(4) . . ? C40 C39 C38 119.0(4) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C41 C40 C39 119.8(4) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 118.9(4) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? N6 C42 C41 121.6(4) . . ? N6 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? N1S C1S C2S 178.4(8) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 171.3(15) . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N2SX C3SX C4SX 177.6(19) . . ? C3SX C4SX H4S4 109.5 . . ? C3SX C4SX H4S5 109.5 . . ? H4S4 C4SX H4S5 109.5 . . ? C3SX C4SX H4S6 109.5 . . ? H4S4 C4SX H4S6 109.5 . . ? H4S5 C4SX H4S6 109.5 . . ? N3S C5S C6S 177(2) . . ? C5S C6S H6S 109.5 . . ? C5S C6S H6T 109.5 . . ? H6S C6S H6T 109.5 . . ? C5S C6S H6U 109.5 . . ? H6S C6S H6U 109.5 . . ? H6T C6S H6U 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cr2 N1 C13 138.9(6) . . . . ? O4 Cr2 N1 C13 94.0(3) . . . . ? N2 Cr2 N1 C13 -178.3(4) . . . . ? Cl1 Cr2 N1 C13 -1.2(3) . . . . ? Cl2 Cr2 N1 C13 -91.8(3) . . . . ? O1 Cr2 N1 C17 -43.1(8) . . . . ? O4 Cr2 N1 C17 -88.0(3) . . . . ? N2 Cr2 N1 C17 -0.3(3) . . . . ? Cl1 Cr2 N1 C17 176.8(3) . . . . ? Cl2 Cr2 N1 C17 86.2(3) . . . . ? O1 Cr2 N2 C22 -9.3(3) . . . . ? O4 Cr2 N2 C22 -87.3(3) . . . . ? N1 Cr2 N2 C22 178.2(3) . . . . ? Cl1 Cr2 N2 C22 157.8(5) . . . . ? Cl2 Cr2 N2 C22 85.5(3) . . . . ? O1 Cr2 N2 C18 172.2(3) . . . . ? O4 Cr2 N2 C18 94.2(3) . . . . ? N1 Cr2 N2 C18 -0.3(3) . . . . ? Cl1 Cr2 N2 C18 -20.7(9) . . . . ? Cl2 Cr2 N2 C18 -93.0(3) . . . . ? O2 Cr3 N3 C23 139.4(6) . . . . ? O5 Cr3 N3 C23 91.8(3) . . . . ? N4 Cr3 N3 C23 -178.2(3) . . . . ? Cl4 Cr3 N3 C23 -93.6(3) . . . . ? Cl3 Cr3 N3 C23 -3.3(3) . . . . ? O2 Cr3 N3 C27 -46.9(8) . . . . ? O5 Cr3 N3 C27 -94.5(3) . . . . ? N4 Cr3 N3 C27 -4.5(3) . . . . ? Cl4 Cr3 N3 C27 80.0(3) . . . . ? Cl3 Cr3 N3 C27 170.4(2) . . . . ? O2 Cr3 N4 C32 -10.8(3) . . . . ? O5 Cr3 N4 C32 -88.8(3) . . . . ? N3 Cr3 N4 C32 175.6(3) . . . . ? Cl4 Cr3 N4 C32 83.6(3) . . . . ? Cl3 Cr3 N4 C32 146.2(4) . . . . ? O2 Cr3 N4 C28 177.7(3) . . . . ? O5 Cr3 N4 C28 99.7(3) . . . . ? N3 Cr3 N4 C28 4.1(3) . . . . ? Cl4 Cr3 N4 C28 -87.9(3) . . . . ? Cl3 Cr3 N4 C28 -25.3(7) . . . . ? O3 Cr4 N5 C33 111.8(6) . . . . ? O6 Cr4 N5 C33 85.0(3) . . . . ? N6 Cr4 N5 C33 175.1(3) . . . . ? Cl5 Cr4 N5 C33 -12.6(3) . . . . ? Cl6 Cr4 N5 C33 -102.3(3) . . . . ? O3 Cr4 N5 C37 -64.1(6) . . . . ? O6 Cr4 N5 C37 -91.0(3) . . . . ? N6 Cr4 N5 C37 -0.9(3) . . . . ? Cl5 Cr4 N5 C37 171.4(3) . . . . ? Cl6 Cr4 N5 C37 81.7(3) . . . . ? O3 Cr4 N6 C42 -15.9(3) . . . . ? O6 Cr4 N6 C42 -94.1(3) . . . . ? N5 Cr4 N6 C42 175.0(3) . . . . ? Cl5 Cr4 N6 C42 135.2(4) . . . . ? Cl6 Cr4 N6 C42 78.8(3) . . . . ? O3 Cr4 N6 C38 175.5(3) . . . . ? O6 Cr4 N6 C38 97.3(3) . . . . ? N5 Cr4 N6 C38 6.3(3) . . . . ? Cl5 Cr4 N6 C38 -33.4(6) . . . . ? Cl6 Cr4 N6 C38 -89.8(3) . . . . ? O4 Cr2 O1 C1 -140.9(3) . . . . ? N2 Cr2 O1 C1 131.4(3) . . . . ? N1 Cr2 O1 C1 173.1(6) . . . . ? Cl1 Cr2 O1 C1 -46.7(3) . . . . ? Cl2 Cr2 O1 C1 44.1(3) . . . . ? O4 Cr2 O1 Cr1 -2.80(11) . . . . ? N2 Cr2 O1 Cr1 -90.52(13) . . . . ? N1 Cr2 O1 Cr1 -48.8(7) . . . . ? Cl1 Cr2 O1 Cr1 91.37(10) . . . . ? Cl2 Cr2 O1 Cr1 -177.86(9) . . . . ? O2 Cr1 O1 C1 -42.9(2) . . . . ? O3 Cr1 O1 C1 50.1(2) . . . . ? O4 Cr1 O1 C1 146.5(2) . . . . ? O6 Cr1 O1 C1 99.2(5) . . . . ? O5 Cr1 O1 C1 -122.1(2) . . . . ? O2 Cr1 O1 Cr2 173.44(11) . . . . ? O3 Cr1 O1 Cr2 -93.47(12) . . . . ? O4 Cr1 O1 Cr2 2.84(11) . . . . ? O6 Cr1 O1 Cr2 -44.4(5) . . . . ? O5 Cr1 O1 Cr2 94.26(12) . . . . ? O3 Cr1 O2 C2 -42.2(2) . . . . ? O1 Cr1 O2 C2 50.6(2) . . . . ? O4 Cr1 O2 C2 96.6(5) . . . . ? O6 Cr1 O2 C2 -121.7(2) . . . . ? O5 Cr1 O2 C2 148.4(2) . . . . ? O3 Cr1 O2 Cr3 170.90(11) . . . . ? O1 Cr1 O2 Cr3 -96.32(12) . . . . ? O4 Cr1 O2 Cr3 -50.3(5) . . . . ? O6 Cr1 O2 Cr3 91.39(12) . . . . ? O5 Cr1 O2 Cr3 1.46(11) . . . . ? O5 Cr3 O2 C2 -142.5(3) . . . . ? N4 Cr3 O2 C2 127.3(3) . . . . ? N3 Cr3 O2 C2 168.8(6) . . . . ? Cl4 Cr3 O2 C2 42.1(3) . . . . ? Cl3 Cr3 O2 C2 -48.6(3) . . . . ? O5 Cr3 O2 Cr1 -1.44(11) . . . . ? N4 Cr3 O2 Cr1 -91.60(13) . . . . ? N3 Cr3 O2 Cr1 -50.1(7) . . . . ? Cl4 Cr3 O2 Cr1 -176.81(9) . . . . ? Cl3 Cr3 O2 Cr1 92.49(10) . . . . ? O2 Cr1 O3 C3 49.1(2) . . . . ? O1 Cr1 O3 C3 -43.3(2) . . . . ? O4 Cr1 O3 C3 -122.4(2) . . . . ? O6 Cr1 O3 C3 146.2(2) . . . . ? O5 Cr1 O3 C3 101.0(5) . . . . ? O2 Cr1 O3 Cr4 -95.14(12) . . . . ? O1 Cr1 O3 Cr4 172.38(11) . . . . ? O4 Cr1 O3 Cr4 93.36(12) . . . . ? O6 Cr1 O3 Cr4 1.97(11) . . . . ? O5 Cr1 O3 Cr4 -43.3(5) . . . . ? O6 Cr4 O3 C3 -141.2(3) . . . . ? N6 Cr4 O3 C3 129.9(3) . . . . ? N5 Cr4 O3 C3 -168.7(5) . . . . ? Cl5 Cr4 O3 C3 -44.3(3) . . . . ? Cl6 Cr4 O3 C3 45.5(3) . . . . ? O6 Cr4 O3 Cr1 -1.95(10) . . . . ? N6 Cr4 O3 Cr1 -90.79(13) . . . . ? N5 Cr4 O3 Cr1 -29.4(6) . . . . ? Cl5 Cr4 O3 Cr1 95.01(10) . . . . ? Cl6 Cr4 O3 Cr1 -175.23(9) . . . . ? O2 Cr1 O4 C7 98.6(5) . . . . ? O3 Cr1 O4 C7 -122.9(2) . . . . ? O1 Cr1 O4 C7 145.7(3) . . . . ? O6 Cr1 O4 C7 -43.5(2) . . . . ? O5 Cr1 O4 C7 48.0(3) . . . . ? O2 Cr1 O4 Cr2 -49.9(5) . . . . ? O3 Cr1 O4 Cr2 88.62(12) . . . . ? O1 Cr1 O4 Cr2 -2.77(10) . . . . ? O6 Cr1 O4 Cr2 168.06(11) . . . . ? O5 Cr1 O4 Cr2 -100.42(12) . . . . ? O1 Cr2 O4 C7 -139.0(3) . . . . ? N2 Cr2 O4 C7 -44.3(3) . . . . ? N1 Cr2 O4 C7 33.0(3) . . . . ? Cl1 Cr2 O4 C7 128.0(3) . . . . ? Cl2 Cr2 O4 C7 -103.1(6) . . . . ? O1 Cr2 O4 Cr1 2.78(10) . . . . ? N2 Cr2 O4 Cr1 97.54(13) . . . . ? N1 Cr2 O4 Cr1 174.86(12) . . . . ? Cl1 Cr2 O4 Cr1 -90.17(9) . . . . ? Cl2 Cr2 O4 Cr1 38.7(6) . . . . ? O2 Cr1 O5 C8 147.1(3) . . . . ? O3 Cr1 O5 C8 93.9(5) . . . . ? O1 Cr1 O5 C8 -122.1(2) . . . . ? O4 Cr1 O5 C8 -43.0(3) . . . . ? O6 Cr1 O5 C8 49.7(3) . . . . ? O2 Cr1 O5 Cr3 -1.41(11) . . . . ? O3 Cr1 O5 Cr3 -54.6(5) . . . . ? O1 Cr1 O5 Cr3 89.40(12) . . . . ? O4 Cr1 O5 Cr3 168.50(11) . . . . ? O6 Cr1 O5 Cr3 -98.82(12) . . . . ? O2 Cr3 O5 C8 -139.8(3) . . . . ? N4 Cr3 O5 C8 -44.9(3) . . . . ? N3 Cr3 O5 C8 33.0(3) . . . . ? Cl4 Cr3 O5 C8 -107.2(6) . . . . ? Cl3 Cr3 O5 C8 126.5(3) . . . . ? O2 Cr3 O5 Cr1 1.41(11) . . . . ? N4 Cr3 O5 Cr1 96.35(13) . . . . ? N3 Cr3 O5 Cr1 174.25(12) . . . . ? Cl4 Cr3 O5 Cr1 34.0(6) . . . . ? Cl3 Cr3 O5 Cr1 -92.25(10) . . . . ? O2 Cr1 O6 C9 -124.3(2) . . . . ? O3 Cr1 O6 C9 144.1(2) . . . . ? O1 Cr1 O6 C9 93.9(5) . . . . ? O4 Cr1 O6 C9 47.8(2) . . . . ? O5 Cr1 O6 C9 -45.3(2) . . . . ? O2 Cr1 O6 Cr4 89.68(12) . . . . ? O3 Cr1 O6 Cr4 -1.92(10) . . . . ? O1 Cr1 O6 Cr4 -52.1(5) . . . . ? O4 Cr1 O6 Cr4 -98.25(12) . . . . ? O5 Cr1 O6 Cr4 168.73(11) . . . . ? O3 Cr4 O6 C9 -137.4(3) . . . . ? N6 Cr4 O6 C9 -40.4(3) . . . . ? N5 Cr4 O6 C9 37.0(3) . . . . ? Cl5 Cr4 O6 C9 130.4(3) . . . . ? Cl6 Cr4 O6 C9 -91.0(6) . . . . ? O3 Cr4 O6 Cr1 1.92(10) . . . . ? N6 Cr4 O6 Cr1 98.94(13) . . . . ? N5 Cr4 O6 Cr1 176.36(12) . . . . ? Cl5 Cr4 O6 Cr1 -90.26(10) . . . . ? Cl6 Cr4 O6 Cr1 48.4(6) . . . . ? Cr2 O1 C1 C4 126.0(3) . . . . ? Cr1 O1 C1 C4 -7.1(4) . . . . ? Cr1 O2 C2 C4 -6.8(4) . . . . ? Cr3 O2 C2 C4 129.9(3) . . . . ? Cr1 O3 C3 C4 -4.8(4) . . . . ? Cr4 O3 C3 C4 129.3(3) . . . . ? O1 C1 C4 C3 -58.1(4) . . . . ? O1 C1 C4 C2 67.7(4) . . . . ? O1 C1 C4 C5 -177.6(3) . . . . ? O3 C3 C4 C1 65.4(4) . . . . ? O3 C3 C4 C2 -60.3(4) . . . . ? O3 C3 C4 C5 -175.7(3) . . . . ? O2 C2 C4 C1 -59.3(4) . . . . ? O2 C2 C4 C3 67.5(4) . . . . ? O2 C2 C4 C5 -175.2(3) . . . . ? C1 C4 C5 C6 68.4(4) . . . . ? C3 C4 C5 C6 -54.1(4) . . . . ? C2 C4 C5 C6 -173.2(3) . . . . ? Cr1 O4 C7 C10 -4.0(4) . . . . ? Cr2 O4 C7 C10 132.9(3) . . . . ? Cr1 O5 C8 C10 -4.6(4) . . . . ? Cr3 O5 C8 C10 131.7(3) . . . . ? Cr1 O6 C9 C10 -3.4(4) . . . . ? Cr4 O6 C9 C10 130.6(3) . . . . ? O6 C9 C10 C7 -60.4(4) . . . . ? O6 C9 C10 C8 65.2(4) . . . . ? O6 C9 C10 C11 -178.8(3) . . . . ? O4 C7 C10 C9 65.1(4) . . . . ? O4 C7 C10 C8 -59.8(4) . . . . ? O4 C7 C10 C11 -176.9(3) . . . . ? O5 C8 C10 C9 -60.4(4) . . . . ? O5 C8 C10 C7 65.1(4) . . . . ? O5 C8 C10 C11 -177.0(3) . . . . ? C9 C10 C11 C12 79.1(5) . . . . ? C7 C10 C11 C12 -41.6(6) . . . . ? C8 C10 C11 C12 -162.2(5) . . . . ? C17 N1 C13 C14 -0.7(6) . . . . ? Cr2 N1 C13 C14 177.2(3) . . . . ? N1 C13 C14 C15 0.8(7) . . . . ? C13 C14 C15 C16 -0.5(8) . . . . ? C14 C15 C16 C17 0.1(8) . . . . ? C13 N1 C17 C16 0.3(6) . . . . ? Cr2 N1 C17 C16 -177.8(3) . . . . ? C13 N1 C17 C18 178.9(4) . . . . ? Cr2 N1 C17 C18 0.8(5) . . . . ? C15 C16 C17 N1 0.0(7) . . . . ? C15 C16 C17 C18 -178.5(4) . . . . ? C22 N2 C18 C19 2.5(6) . . . . ? Cr2 N2 C18 C19 -179.0(3) . . . . ? C22 N2 C18 C17 -177.7(4) . . . . ? Cr2 N2 C18 C17 0.8(5) . . . . ? N1 C17 C18 N2 -1.0(5) . . . . ? C16 C17 C18 N2 177.5(4) . . . . ? N1 C17 C18 C19 178.7(4) . . . . ? C16 C17 C18 C19 -2.7(7) . . . . ? N2 C18 C19 C20 -0.8(7) . . . . ? C17 C18 C19 C20 179.5(4) . . . . ? C18 C19 C20 C21 -1.0(7) . . . . ? C19 C20 C21 C22 1.0(7) . . . . ? C18 N2 C22 C21 -2.5(6) . . . . ? Cr2 N2 C22 C21 179.0(3) . . . . ? C20 C21 C22 N2 0.8(7) . . . . ? C27 N3 C23 C24 -0.5(6) . . . . ? Cr3 N3 C23 C24 173.0(3) . . . . ? N3 C23 C24 C25 0.0(6) . . . . ? C23 C24 C25 C26 0.9(6) . . . . ? C24 C25 C26 C27 -1.4(6) . . . . ? C23 N3 C27 C26 0.0(5) . . . . ? Cr3 N3 C27 C26 -174.2(3) . . . . ? C23 N3 C27 C28 178.5(3) . . . . ? Cr3 N3 C27 C28 4.2(4) . . . . ? C25 C26 C27 N3 1.0(6) . . . . ? C25 C26 C27 C28 -177.3(4) . . . . ? C32 N4 C28 C29 3.0(5) . . . . ? Cr3 N4 C28 C29 174.9(3) . . . . ? C32 N4 C28 C27 -175.0(3) . . . . ? Cr3 N4 C28 C27 -3.1(4) . . . . ? N3 C27 C28 N4 -0.8(5) . . . . ? C26 C27 C28 N4 177.6(3) . . . . ? N3 C27 C28 C29 -178.8(3) . . . . ? C26 C27 C28 C29 -0.4(6) . . . . ? N4 C28 C29 C30 -1.2(6) . . . . ? C27 C28 C29 C30 176.6(4) . . . . ? C28 C29 C30 C31 -1.0(6) . . . . ? C29 C30 C31 C32 1.4(6) . . . . ? C28 N4 C32 C31 -2.6(6) . . . . ? Cr3 N4 C32 C31 -174.0(3) . . . . ? C30 C31 C32 N4 0.5(6) . . . . ? C37 N5 C33 C34 1.7(6) . . . . ? Cr4 N5 C33 C34 -174.2(3) . . . . ? N5 C33 C34 C35 -0.8(6) . . . . ? C33 C34 C35 C36 -0.7(6) . . . . ? C34 C35 C36 C37 1.2(6) . . . . ? C33 N5 C37 C36 -1.1(6) . . . . ? Cr4 N5 C37 C36 175.2(3) . . . . ? C33 N5 C37 C38 179.5(3) . . . . ? Cr4 N5 C37 C38 -4.2(4) . . . . ? C35 C36 C37 N5 -0.3(6) . . . . ? C35 C36 C37 C38 179.0(4) . . . . ? C42 N6 C38 C39 -1.2(6) . . . . ? Cr4 N6 C38 C39 167.9(3) . . . . ? C42 N6 C38 C37 -179.4(3) . . . . ? Cr4 N6 C38 C37 -10.4(4) . . . . ? N5 C37 C38 N6 9.5(5) . . . . ? C36 C37 C38 N6 -169.9(4) . . . . ? N5 C37 C38 C39 -168.7(4) . . . . ? C36 C37 C38 C39 11.9(7) . . . . ? N6 C38 C39 C40 0.6(7) . . . . ? C37 C38 C39 C40 178.7(4) . . . . ? C38 C39 C40 C41 0.2(8) . . . . ? C39 C40 C41 C42 -0.5(8) . . . . ? C38 N6 C42 C41 0.9(6) . . . . ? Cr4 N6 C42 C41 -167.4(3) . . . . ? C40 C41 C42 N6 -0.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.926 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.098 # Attachment '- 3.cif' data_pb3 _database_code_depnum_ccdc_archive 'CCDC 810902' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cr4(Hpeol)2(bpy)3Cl6]' _chemical_melting_point ? _chemical_formula_moiety '(C40 H42 Cl6 Cr4 N6 O8), 1.83(C2 H3 N), 0.5(H2O)' _chemical_formula_sum 'C43.66 H48.50 Cl6 Cr4 N7.83 O8.50' _chemical_formula_weight 1239.64 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' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9229(7) _cell_length_b 12.5995(6) _cell_length_c 19.7854(10) _cell_angle_alpha 82.643(4) _cell_angle_beta 77.861(5) _cell_angle_gamma 64.945(5) _cell_volume 2629.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5299 _cell_measurement_theta_min 2.6976 _cell_measurement_theta_max 27.5353 _exptl_crystal_description PLATE _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1263 _exptl_absorpt_coefficient_mu 1.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15616 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.1137 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8944 _reflns_number_gt 5136 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. All hydrogen atoms were placed geometrically, except for the water molecules since these could not be place or located in the difference map and so were omitted from the refinement. Due to disorder in the structure the hydroxy groups O4 and O8 were split over two and three sites respectively. Displacement and geometric restraints were applied to the anisotropic thermal parameters of these atoms and all solvent acetonitrile. The non-H atoms in the solvent acetonitrile N9-C46 and water were left isotropic, several attempts were made to model the solvent molecules but this resulted in persistent npds and since no new chemical information would result these attempts were abandoned. ; _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^)+(0.0529P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8944 _refine_ls_number_parameters 680 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.919 _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 0.26354(8) 0.86374(7) 0.25219(4) 0.0178(2) Uani 1 1 d . . . Cr2 Cr 0.14523(8) 1.12767(7) 0.26445(4) 0.0197(2) Uani 1 1 d . . . Cr3 Cr 0.44426(8) 0.75910(7) 0.12119(4) 0.0191(2) Uani 1 1 d . . . Cr4 Cr 0.20808(8) 0.70885(7) 0.37375(4) 0.0210(2) Uani 1 1 d . . . Cl1 Cl 0.14037(13) 1.12317(11) 0.38221(6) 0.0241(3) Uani 1 1 d . . . Cl2 Cl 0.22290(14) 1.27116(12) 0.24834(6) 0.0325(4) Uani 1 1 d . . . Cl3 Cl 0.51707(12) 0.90591(11) 0.09916(6) 0.0227(3) Uani 1 1 d . . . Cl4 Cl 0.64994(12) 0.61786(11) 0.09699(6) 0.0245(3) Uani 1 1 d . . . Cl5 Cl 0.40279(13) 0.54997(11) 0.35055(6) 0.0285(3) Uani 1 1 d . . . Cl6 Cl 0.22927(14) 0.68787(12) 0.48995(6) 0.0288(4) Uani 1 1 d . . . O1 O 0.3104(3) 0.9948(3) 0.24816(15) 0.0172(8) Uani 1 1 d . . . O2 O 0.4382(3) 0.7544(3) 0.22140(15) 0.0171(8) Uani 1 1 d . . . O3 O 0.2779(3) 0.8267(3) 0.34987(15) 0.0182(8) Uani 1 1 d . . . O4 O 0.6620(7) 0.7297(6) 0.3680(3) 0.068(2) Uani 0.705(4) 1 d PDU A 1 H4 H 0.6254 0.7170 0.4060 0.102 Uiso 0.705(4) 1 calc PR A 1 O4X O 0.5391(13) 0.9383(13) 0.4015(7) 0.053(4) Uani 0.295(4) 1 d PDU A 2 H4X H 0.5926 0.9633 0.4010 0.080 Uiso 0.295(4) 1 calc PR A 2 O5 O 0.0966(3) 0.9949(3) 0.26700(15) 0.0173(8) Uani 1 1 d . . . O6 O 0.2645(3) 0.8652(3) 0.15274(15) 0.0189(8) Uani 1 1 d . . . O7 O 0.1904(3) 0.7467(3) 0.27490(15) 0.0178(8) Uani 1 1 d . . . O8 O -0.1671(5) 0.8807(5) 0.2128(3) 0.0373(15) Uani 0.70 1 d PD B 1 H8 H -0.2201 0.9477 0.2199 0.056 Uiso 0.70 1 calc PR B 1 O8X O -0.043(2) 0.7691(16) 0.1385(11) 0.048(7) Uani 0.17 1 d PDU B 2 H8X H -0.1045 0.7776 0.1226 0.073 Uiso 0.17 1 calc PR B 2 O8Y O -0.096(2) 0.981(2) 0.1050(11) 0.041(8) Uani 0.13 1 d PDU B 3 H8Y H -0.1547 0.9806 0.0899 0.061 Uiso 0.13 1 calc PR B 3 N1 N -0.0407(4) 1.2491(3) 0.2697(2) 0.0201(10) Uani 1 1 d . . . N2 N 0.1286(4) 1.1664(4) 0.16032(19) 0.0225(11) Uani 1 1 d . . . N3 N 0.4143(4) 0.7652(4) 0.02041(19) 0.0221(11) Uani 1 1 d . . . N4 N 0.3904(4) 0.6226(4) 0.12437(19) 0.0193(10) Uani 1 1 d . . . N5 N 0.1082(4) 0.6035(4) 0.38962(19) 0.0237(11) Uani 1 1 d . . . N6 N 0.0274(4) 0.8274(4) 0.40556(19) 0.0206(10) Uani 1 1 d . . . C1 C 0.4188(5) 0.9735(4) 0.2762(3) 0.0230(13) Uani 1 1 d . A . H1A H 0.3964 1.0309 0.3105 0.028 Uiso 1 1 calc R . . H1B H 0.4817 0.9844 0.2395 0.028 Uiso 1 1 calc R . . C2 C 0.5295(5) 0.7549(5) 0.2562(2) 0.0244(13) Uani 1 1 d . A . H2A H 0.5955 0.7668 0.2225 0.029 Uiso 1 1 calc R . . H2B H 0.5669 0.6789 0.2795 0.029 Uiso 1 1 calc R . . C3 C 0.3827(5) 0.8292(5) 0.3702(2) 0.0224(13) Uani 1 1 d . A . H3A H 0.4260 0.7552 0.3940 0.027 Uiso 1 1 calc R . . H3B H 0.3537 0.8906 0.4028 0.027 Uiso 1 1 calc R . . C4 C 0.4762(5) 0.8505(5) 0.3099(2) 0.0212(12) Uani 1 1 d . . . C5 C 0.5865(6) 0.8456(5) 0.3406(3) 0.0359(15) Uani 0.705(4) 1 d PDU A 1 H5A H 0.6405 0.8711 0.3050 0.043 Uiso 0.705(4) 1 calc PR A 1 H5B H 0.5536 0.9003 0.3775 0.043 Uiso 0.705(4) 1 calc PR A 1 C5X C 0.5865(6) 0.8456(5) 0.3406(3) 0.0359(15) Uani 0.295(4) 1 d PDU A 2 H5C H 0.6455 0.8631 0.3042 0.043 Uiso 0.295(4) 1 calc PR A 2 H5D H 0.6300 0.7668 0.3593 0.043 Uiso 0.295(4) 1 calc PR A 2 C6 C 0.0022(5) 0.9867(5) 0.2378(3) 0.0253(13) Uani 1 1 d . . . H6A H -0.0325 1.0564 0.2085 0.030 Uiso 1 1 calc R . . H6B H -0.0651 0.9854 0.2748 0.030 Uiso 1 1 calc R . . C7 C 0.1524(5) 0.8764(5) 0.1334(2) 0.0239(13) Uani 1 1 d . . . H7A H 0.1717 0.8119 0.1047 0.029 Uiso 1 1 calc R . . H7B H 0.1207 0.9485 0.1055 0.029 Uiso 1 1 calc R . . C8 C 0.0909(5) 0.7639(5) 0.2413(3) 0.0254(14) Uani 1 1 d . . . H8A H 0.0195 0.7656 0.2761 0.030 Uiso 1 1 calc R . . H8B H 0.1161 0.6974 0.2131 0.030 Uiso 1 1 calc R . . C9 C 0.0484(5) 0.8777(5) 0.1946(2) 0.0223(13) Uani 1 1 d D B . C10 C -0.0619(5) 0.8846(5) 0.1638(3) 0.0301(14) Uani 1 1 d D . . H10A H -0.0906 0.9568 0.1357 0.036 Uiso 1 1 calc R B 1 H10B H -0.0317 0.8201 0.1333 0.036 Uiso 1 1 calc R B 1 C11 C -0.1273(5) 1.2838(5) 0.3277(3) 0.0269(14) Uani 1 1 d . . . H11 H -0.1025 1.2544 0.3702 0.032 Uiso 1 1 calc R . . C12 C -0.2494(5) 1.3597(5) 0.3272(3) 0.0298(14) Uani 1 1 d . . . H12 H -0.3063 1.3809 0.3684 0.036 Uiso 1 1 calc R . . C13 C -0.2866(6) 1.4044(5) 0.2646(3) 0.0322(14) Uani 1 1 d . . . H13 H -0.3694 1.4563 0.2630 0.039 Uiso 1 1 calc R . . C14 C -0.2005(5) 1.3717(5) 0.2044(3) 0.0274(14) Uani 1 1 d . . . H14 H -0.2245 1.4016 0.1617 0.033 Uiso 1 1 calc R . . C15 C -0.0786(5) 1.2944(5) 0.2081(2) 0.0232(13) Uani 1 1 d . . . C16 C 0.0215(5) 1.2524(5) 0.1468(3) 0.0249(13) Uani 1 1 d . . . C17 C 0.0090(6) 1.3017(5) 0.0805(3) 0.0419(17) Uani 1 1 d . . . H17 H -0.0660 1.3621 0.0717 0.050 Uiso 1 1 calc R . . C18 C 0.1109(7) 1.2587(7) 0.0277(3) 0.055(2) Uani 1 1 d . . . H18 H 0.1051 1.2894 -0.0174 0.067 Uiso 1 1 calc R . . C19 C 0.2205(6) 1.1706(6) 0.0425(3) 0.0407(17) Uani 1 1 d . . . H19 H 0.2898 1.1414 0.0074 0.049 Uiso 1 1 calc R . . C20 C 0.2277(5) 1.1254(5) 0.1092(2) 0.0291(14) Uani 1 1 d . . . H20 H 0.3023 1.0655 0.1190 0.035 Uiso 1 1 calc R . . C21 C 0.4247(5) 0.8445(5) -0.0311(3) 0.0279(14) Uani 1 1 d . . . H21 H 0.4516 0.9001 -0.0227 0.033 Uiso 1 1 calc R . . C22 C 0.3973(6) 0.8456(5) -0.0952(3) 0.0353(16) Uani 1 1 d . . . H22 H 0.4058 0.9011 -0.1294 0.042 Uiso 1 1 calc R . . C23 C 0.3569(6) 0.7639(5) -0.1088(3) 0.0378(16) Uani 1 1 d . . . H23 H 0.3362 0.7645 -0.1517 0.045 Uiso 1 1 calc R . . C24 C 0.3477(6) 0.6809(5) -0.0571(3) 0.0326(15) Uani 1 1 d . . . H24 H 0.3237 0.6231 -0.0654 0.039 Uiso 1 1 calc R . . C25 C 0.3744(5) 0.6850(4) 0.0061(2) 0.0223(13) Uani 1 1 d . . . C26 C 0.3646(5) 0.6010(5) 0.0659(2) 0.0216(13) Uani 1 1 d . . . C27 C 0.3300(5) 0.5118(5) 0.0625(3) 0.0257(13) Uani 1 1 d . . . H27 H 0.3123 0.4987 0.0215 0.031 Uiso 1 1 calc R . . C28 C 0.3216(5) 0.4414(5) 0.1211(3) 0.0302(15) Uani 1 1 d . . . H28 H 0.2965 0.3811 0.1205 0.036 Uiso 1 1 calc R . . C29 C 0.3511(5) 0.4615(5) 0.1806(3) 0.0296(15) Uani 1 1 d . . . H29 H 0.3479 0.4136 0.2202 0.036 Uiso 1 1 calc R . . C30 C 0.3851(5) 0.5525(4) 0.1810(2) 0.0247(13) Uani 1 1 d . . . H30 H 0.4048 0.5660 0.2212 0.030 Uiso 1 1 calc R . . C31 C 0.1565(6) 0.4875(5) 0.3818(3) 0.0346(16) Uani 1 1 d . . . H31 H 0.2421 0.4492 0.3652 0.042 Uiso 1 1 calc R . . C32 C 0.0854(6) 0.4223(5) 0.3970(3) 0.0373(17) Uani 1 1 d . . . H32 H 0.1225 0.3417 0.3916 0.045 Uiso 1 1 calc R . . C33 C -0.0404(6) 0.4786(5) 0.4200(3) 0.0376(17) Uani 1 1 d . . . H33 H -0.0903 0.4365 0.4302 0.045 Uiso 1 1 calc R . . C34 C -0.0937(6) 0.5976(5) 0.4283(3) 0.0337(15) Uani 1 1 d . . . H34 H -0.1795 0.6366 0.4441 0.040 Uiso 1 1 calc R . . C35 C -0.0166(6) 0.6590(5) 0.4127(2) 0.0256(14) Uani 1 1 d . . . C36 C -0.0645(5) 0.7863(5) 0.4206(2) 0.0223(13) Uani 1 1 d . . . C37 C -0.1864(5) 0.8593(5) 0.4431(3) 0.0300(14) Uani 1 1 d . . . H37 H -0.2485 0.8306 0.4521 0.036 Uiso 1 1 calc R . . C38 C -0.2176(5) 0.9752(5) 0.4525(2) 0.0316(15) Uani 1 1 d . . . H38 H -0.3009 1.0256 0.4671 0.038 Uiso 1 1 calc R . . C39 C -0.1254(5) 1.0158(5) 0.4401(2) 0.0285(14) Uani 1 1 d . . . H39 H -0.1443 1.0934 0.4476 0.034 Uiso 1 1 calc R . . C40 C -0.0040(5) 0.9399(5) 0.4164(2) 0.0245(13) Uani 1 1 d . . . H40 H 0.0587 0.9677 0.4076 0.029 Uiso 1 1 calc R . . N7 N 0.3329(7) 0.8971(6) 0.7304(3) 0.0341(19) Uani 0.705(4) 1 d PD A 1 C41 C 0.4164(8) 0.8462(8) 0.6967(4) 0.033(2) Uani 0.705(4) 1 d PDU A 1 C42 C 0.5265(9) 0.7832(9) 0.6492(6) 0.071(3) Uani 0.705(4) 1 d PDU A 1 H42A H 0.5309 0.8309 0.6076 0.107 Uiso 0.705(4) 1 calc PR A 1 H42B H 0.5234 0.7125 0.6383 0.107 Uiso 0.705(4) 1 calc PR A 1 H42C H 0.5995 0.7638 0.6696 0.107 Uiso 0.705(4) 1 calc PR A 1 N8 N 1.0122(8) 0.5735(7) 0.1118(4) 0.073(3) Uani 0.83 1 d PD C 1 C43 C 0.9664(8) 0.5745(8) 0.1644(5) 0.049(2) Uani 0.83 1 d PD C 1 C44 C 0.9115(9) 0.5837(9) 0.2353(5) 0.080(3) Uani 0.83 1 d PD C 1 H44A H 0.9738 0.5351 0.2627 0.121 Uiso 0.83 1 calc PR C 1 H44B H 0.8441 0.5585 0.2435 0.121 Uiso 0.83 1 calc PR C 1 H44C H 0.8793 0.6638 0.2477 0.121 Uiso 0.83 1 calc PR C 1 N9 N 0.5362(13) 0.8153(11) 0.5057(6) 0.022(4) Uiso 0.295(4) 1 d PD A 2 C45 C 0.5529(17) 0.7249(13) 0.5009(8) 0.025(5) Uiso 0.295(4) 1 d PD A 2 C46 C 0.5615(7) 0.6150(6) 0.4906(3) 0.065(2) Uiso 0.295(4) 1 d PD A 2 H46A H 0.4793 0.6195 0.4901 0.097 Uiso 0.295(4) 1 calc PR A 2 H46B H 0.5965 0.5614 0.5273 0.097 Uiso 0.295(4) 1 calc PR A 2 H46C H 0.6148 0.5879 0.4471 0.097 Uiso 0.295(4) 1 calc PR A 2 O1S O 0.5615(7) 0.6150(6) 0.4906(3) 0.065(2) Uiso 0.50 1 d P D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0197(5) 0.0152(5) 0.0190(4) -0.0029(3) 0.0050(4) -0.0107(4) Cr2 0.0240(5) 0.0140(5) 0.0194(4) -0.0014(3) 0.0046(4) -0.0098(4) Cr3 0.0223(5) 0.0144(5) 0.0198(4) -0.0036(3) 0.0065(4) -0.0105(4) Cr4 0.0265(6) 0.0151(5) 0.0200(4) -0.0037(3) 0.0074(4) -0.0115(4) Cl1 0.0351(9) 0.0166(7) 0.0215(7) -0.0024(5) 0.0025(6) -0.0143(7) Cl2 0.0490(10) 0.0241(8) 0.0292(7) -0.0011(6) 0.0076(7) -0.0261(8) Cl3 0.0267(8) 0.0185(7) 0.0230(7) -0.0036(5) 0.0085(6) -0.0145(6) Cl4 0.0236(8) 0.0193(7) 0.0259(7) -0.0047(5) 0.0050(6) -0.0076(6) Cl5 0.0307(9) 0.0209(8) 0.0237(7) -0.0048(6) 0.0064(6) -0.0050(7) Cl6 0.0405(9) 0.0244(8) 0.0194(7) -0.0031(6) 0.0069(6) -0.0163(7) O1 0.017(2) 0.015(2) 0.0193(18) -0.0050(14) 0.0033(15) -0.0078(17) O2 0.019(2) 0.016(2) 0.0179(17) -0.0045(14) 0.0059(15) -0.0117(17) O3 0.021(2) 0.016(2) 0.0183(18) -0.0025(14) 0.0030(16) -0.0112(17) O4 0.077(5) 0.049(5) 0.088(5) -0.009(4) -0.040(4) -0.022(4) O4X 0.041(8) 0.064(9) 0.076(8) -0.006(6) -0.036(6) -0.030(6) O5 0.016(2) 0.016(2) 0.0201(18) -0.0045(14) 0.0024(15) -0.0085(17) O6 0.016(2) 0.019(2) 0.0210(18) -0.0067(15) 0.0052(16) -0.0089(17) O7 0.020(2) 0.020(2) 0.0148(17) -0.0033(14) 0.0041(16) -0.0123(17) O8 0.036(4) 0.047(4) 0.041(3) -0.004(3) 0.002(3) -0.031(3) O8X 0.045(10) 0.051(11) 0.056(10) -0.026(8) -0.014(8) -0.017(8) O8Y 0.038(11) 0.046(12) 0.056(12) -0.017(9) -0.003(9) -0.032(9) N1 0.019(3) 0.014(2) 0.022(2) 0.0011(18) 0.005(2) -0.005(2) N2 0.027(3) 0.020(3) 0.019(2) 0.0010(19) 0.003(2) -0.011(2) N3 0.027(3) 0.018(3) 0.022(2) -0.0058(19) 0.006(2) -0.013(2) N4 0.019(3) 0.017(3) 0.018(2) -0.0049(18) 0.0099(19) -0.009(2) N5 0.033(3) 0.021(3) 0.020(2) -0.0066(19) 0.010(2) -0.019(2) N6 0.026(3) 0.018(3) 0.018(2) -0.0070(18) 0.007(2) -0.013(2) C1 0.023(3) 0.022(3) 0.028(3) -0.004(2) -0.002(3) -0.014(3) C2 0.017(3) 0.027(3) 0.027(3) 0.002(2) -0.001(2) -0.010(3) C3 0.024(3) 0.020(3) 0.028(3) -0.005(2) -0.008(3) -0.010(3) C4 0.023(3) 0.021(3) 0.023(3) -0.006(2) -0.002(2) -0.011(3) C5 0.035(4) 0.030(4) 0.041(3) -0.006(3) -0.002(3) -0.013(3) C5X 0.035(4) 0.030(4) 0.041(3) -0.006(3) -0.002(3) -0.013(3) C6 0.023(3) 0.023(3) 0.032(3) -0.008(2) 0.002(3) -0.012(3) C7 0.025(3) 0.023(3) 0.026(3) -0.005(2) -0.003(3) -0.010(3) C8 0.026(4) 0.024(3) 0.026(3) -0.010(2) 0.012(3) -0.015(3) C9 0.018(3) 0.031(3) 0.020(3) -0.008(2) 0.006(2) -0.014(3) C10 0.030(4) 0.028(4) 0.035(3) -0.010(3) -0.004(3) -0.013(3) C11 0.035(4) 0.025(3) 0.022(3) -0.002(2) 0.006(3) -0.018(3) C12 0.028(4) 0.027(4) 0.025(3) -0.010(3) 0.012(3) -0.008(3) C13 0.025(4) 0.025(4) 0.041(4) -0.006(3) 0.001(3) -0.007(3) C14 0.030(4) 0.025(3) 0.025(3) -0.002(2) -0.006(3) -0.009(3) C15 0.028(4) 0.019(3) 0.021(3) 0.000(2) 0.001(3) -0.012(3) C16 0.025(3) 0.018(3) 0.027(3) -0.002(2) 0.002(3) -0.007(3) C17 0.041(4) 0.041(4) 0.028(3) 0.006(3) -0.003(3) -0.005(3) C18 0.055(5) 0.072(6) 0.024(3) 0.012(3) -0.001(3) -0.017(4) C19 0.038(4) 0.050(5) 0.020(3) -0.002(3) 0.012(3) -0.013(4) C20 0.026(4) 0.028(3) 0.025(3) -0.002(2) 0.007(3) -0.007(3) C21 0.038(4) 0.019(3) 0.030(3) -0.001(2) 0.005(3) -0.019(3) C22 0.059(5) 0.034(4) 0.023(3) 0.007(3) -0.003(3) -0.032(4) C23 0.063(5) 0.041(4) 0.020(3) 0.002(3) -0.008(3) -0.031(4) C24 0.049(4) 0.035(4) 0.026(3) -0.008(3) 0.001(3) -0.031(3) C25 0.022(3) 0.018(3) 0.025(3) -0.007(2) 0.011(2) -0.011(3) C26 0.023(3) 0.021(3) 0.020(3) -0.006(2) 0.007(2) -0.011(3) C27 0.032(4) 0.026(3) 0.022(3) -0.008(2) 0.006(3) -0.018(3) C28 0.036(4) 0.025(3) 0.034(3) -0.006(3) 0.010(3) -0.022(3) C29 0.042(4) 0.018(3) 0.027(3) -0.001(2) 0.014(3) -0.019(3) C30 0.027(3) 0.023(3) 0.020(3) -0.005(2) 0.012(2) -0.012(3) C31 0.049(4) 0.020(3) 0.029(3) -0.006(3) 0.014(3) -0.017(3) C32 0.064(5) 0.023(4) 0.030(3) -0.006(3) 0.006(3) -0.027(4) C33 0.062(5) 0.034(4) 0.031(3) 0.001(3) 0.002(3) -0.039(4) C34 0.036(4) 0.046(4) 0.027(3) 0.003(3) -0.001(3) -0.028(3) C35 0.041(4) 0.023(3) 0.020(3) 0.003(2) -0.002(3) -0.023(3) C36 0.028(3) 0.027(3) 0.015(3) -0.001(2) 0.002(2) -0.016(3) C37 0.025(4) 0.030(4) 0.033(3) 0.001(3) -0.001(3) -0.012(3) C38 0.024(4) 0.035(4) 0.025(3) -0.003(3) 0.007(3) -0.006(3) C39 0.041(4) 0.019(3) 0.018(3) -0.006(2) 0.009(3) -0.010(3) C40 0.035(4) 0.019(3) 0.026(3) -0.005(2) 0.002(3) -0.019(3) N7 0.042(5) 0.041(5) 0.032(4) 0.013(3) -0.015(4) -0.029(4) C41 0.033(4) 0.026(4) 0.055(4) 0.001(3) -0.022(3) -0.021(3) C42 0.046(6) 0.038(6) 0.145(8) -0.041(5) -0.040(6) -0.010(5) N8 0.077(7) 0.055(6) 0.092(6) 0.018(5) -0.048(5) -0.023(5) C43 0.032(5) 0.053(6) 0.066(6) 0.014(5) -0.018(5) -0.023(5) C44 0.078(8) 0.104(9) 0.092(8) -0.004(6) -0.012(6) -0.069(8) _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 O1 1.942(3) . ? Cr1 O3 1.955(3) . ? Cr1 O6 1.963(3) . ? Cr1 O2 1.964(3) . ? Cr1 O5 1.968(3) . ? Cr1 O7 1.972(3) . ? Cr2 O1 1.966(3) . ? Cr2 O5 1.981(3) . ? Cr2 N1 2.082(4) . ? Cr2 N2 2.087(4) . ? Cr2 Cl1 2.3125(14) . ? Cr2 Cl2 2.3182(14) . ? Cr3 O2 1.963(3) . ? Cr3 O6 1.999(3) . ? Cr3 N4 2.065(4) . ? Cr3 N3 2.085(4) . ? Cr3 Cl3 2.3151(14) . ? Cr3 Cl4 2.3319(16) . ? Cr4 O3 1.956(3) . ? Cr4 O7 1.986(3) . ? Cr4 N6 2.052(4) . ? Cr4 N5 2.086(4) . ? Cr4 Cl6 2.3349(15) . ? Cr4 Cl5 2.3364(16) . ? O1 C1 1.421(6) . ? O2 C2 1.408(6) . ? O3 C3 1.404(5) . ? O4 C5 1.458(8) . ? O4 H4 0.8200 . ? O4X H4X 0.8200 . ? O5 C6 1.414(6) . ? O6 C7 1.413(6) . ? O7 C8 1.405(6) . ? O8 C10 1.429(6) . ? O8 H8 0.8200 . ? O8X C10 1.509(13) . ? O8X H8X 0.8200 . ? O8Y C10 1.550(14) . ? O8Y H8Y 0.8200 . ? N1 C11 1.350(6) . ? N1 C15 1.362(6) . ? N2 C16 1.332(7) . ? N2 C20 1.342(6) . ? N3 C21 1.358(6) . ? N3 C25 1.366(6) . ? N4 C26 1.344(6) . ? N4 C30 1.344(6) . ? N5 C31 1.342(6) . ? N5 C35 1.351(7) . ? N6 C40 1.338(6) . ? N6 C36 1.364(6) . ? C1 C4 1.530(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.541(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.533(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.537(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C9 1.543(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.537(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.551(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.528(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.363(8) . ? C11 H11 0.9300 . ? C12 C13 1.374(7) . ? C12 H12 0.9300 . ? C13 C14 1.377(7) . ? C13 H13 0.9300 . ? C14 C15 1.376(7) . ? C14 H14 0.9300 . ? C15 C16 1.481(7) . ? C16 C17 1.388(7) . ? C17 C18 1.384(8) . ? C17 H17 0.9300 . ? C18 C19 1.369(9) . ? C18 H18 0.9300 . ? C19 C20 1.374(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.372(7) . ? C21 H21 0.9300 . ? C22 C23 1.382(7) . ? C22 H22 0.9300 . ? C23 C24 1.388(7) . ? C23 H23 0.9300 . ? C24 C25 1.366(7) . ? C24 H24 0.9300 . ? C25 C26 1.504(6) . ? C26 C27 1.366(6) . ? C27 C28 1.380(7) . ? C27 H27 0.9300 . ? C28 C29 1.378(7) . ? C28 H28 0.9300 . ? C29 C30 1.369(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.380(7) . ? C31 H31 0.9300 . ? C32 C33 1.362(8) . ? C32 H32 0.9300 . ? C33 C34 1.375(8) . ? C33 H33 0.9300 . ? C34 C35 1.400(7) . ? C34 H34 0.9300 . ? C35 C36 1.475(7) . ? C36 C37 1.363(7) . ? C37 C38 1.374(7) . ? C37 H37 0.9300 . ? C38 C39 1.364(7) . ? C38 H38 0.9300 . ? C39 C40 1.373(7) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? N7 C41 1.066(9) . ? C41 C42 1.424(11) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N8 C43 1.067(8) . ? C43 C44 1.414(10) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? N9 C45 1.084(13) . ? C45 C46 1.383(12) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? 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 O1 Cr1 O3 92.73(13) . . ? O1 Cr1 O6 96.63(13) . . ? O3 Cr1 O6 168.03(14) . . ? O1 Cr1 O2 92.32(13) . . ? O3 Cr1 O2 92.52(14) . . ? O6 Cr1 O2 79.70(14) . . ? O1 Cr1 O5 79.35(14) . . ? O3 Cr1 O5 96.56(13) . . ? O6 Cr1 O5 92.49(14) . . ? O2 Cr1 O5 167.92(12) . . ? O1 Cr1 O7 167.34(13) . . ? O3 Cr1 O7 78.91(13) . . ? O6 Cr1 O7 92.99(13) . . ? O2 Cr1 O7 97.49(13) . . ? O5 Cr1 O7 92.07(13) . . ? O1 Cr2 O5 78.47(13) . . ? O1 Cr2 N1 168.05(15) . . ? O5 Cr2 N1 91.70(15) . . ? O1 Cr2 N2 95.79(15) . . ? O5 Cr2 N2 91.28(14) . . ? N1 Cr2 N2 77.48(16) . . ? O1 Cr2 Cl1 93.85(10) . . ? O5 Cr2 Cl1 96.05(9) . . ? N1 Cr2 Cl1 93.93(12) . . ? N2 Cr2 Cl1 168.89(13) . . ? O1 Cr2 Cl2 95.69(10) . . ? O5 Cr2 Cl2 172.08(10) . . ? N1 Cr2 Cl2 93.41(12) . . ? N2 Cr2 Cl2 83.93(12) . . ? Cl1 Cr2 Cl2 89.64(5) . . ? O2 Cr3 O6 78.85(13) . . ? O2 Cr3 N4 95.15(14) . . ? O6 Cr3 N4 88.98(15) . . ? O2 Cr3 N3 168.44(15) . . ? O6 Cr3 N3 91.81(15) . . ? N4 Cr3 N3 77.73(15) . . ? O2 Cr3 Cl3 93.45(9) . . ? O6 Cr3 Cl3 95.73(10) . . ? N4 Cr3 Cl3 170.85(11) . . ? N3 Cr3 Cl3 94.25(11) . . ? O2 Cr3 Cl4 95.61(11) . . ? O6 Cr3 Cl4 172.13(10) . . ? N4 Cr3 Cl4 85.94(12) . . ? N3 Cr3 Cl4 92.98(13) . . ? Cl3 Cr3 Cl4 90.14(5) . . ? O3 Cr4 O7 78.56(13) . . ? O3 Cr4 N6 94.98(15) . . ? O7 Cr4 N6 91.56(15) . . ? O3 Cr4 N5 169.73(17) . . ? O7 Cr4 N5 94.03(14) . . ? N6 Cr4 N5 77.97(16) . . ? O3 Cr4 Cl6 94.67(10) . . ? O7 Cr4 Cl6 172.66(10) . . ? N6 Cr4 Cl6 86.18(12) . . ? N5 Cr4 Cl6 92.32(11) . . ? O3 Cr4 Cl5 94.34(11) . . ? O7 Cr4 Cl5 94.44(10) . . ? N6 Cr4 Cl5 169.76(11) . . ? N5 Cr4 Cl5 93.32(13) . . ? Cl6 Cr4 Cl5 88.84(6) . . ? C1 O1 Cr1 116.7(3) . . ? C1 O1 Cr2 127.7(3) . . ? Cr1 O1 Cr2 101.80(15) . . ? C2 O2 Cr3 127.9(3) . . ? C2 O2 Cr1 116.8(3) . . ? Cr3 O2 Cr1 101.30(16) . . ? C3 O3 Cr1 116.8(3) . . ? C3 O3 Cr4 128.7(3) . . ? Cr1 O3 Cr4 102.10(15) . . ? C6 O5 Cr1 116.6(3) . . ? C6 O5 Cr2 130.0(3) . . ? Cr1 O5 Cr2 100.36(14) . . ? C7 O6 Cr1 116.7(3) . . ? C7 O6 Cr3 131.5(3) . . ? Cr1 O6 Cr3 100.06(16) . . ? C8 O7 Cr1 116.2(3) . . ? C8 O7 Cr4 130.6(3) . . ? Cr1 O7 Cr4 100.41(14) . . ? C10 O8 H8 109.5 . . ? C10 O8X H8X 109.5 . . ? C10 O8Y H8Y 109.5 . . ? C11 N1 C15 117.4(5) . . ? C11 N1 Cr2 126.5(4) . . ? C15 N1 Cr2 116.1(3) . . ? C16 N2 C20 120.0(4) . . ? C16 N2 Cr2 116.5(3) . . ? C20 N2 Cr2 122.2(4) . . ? C21 N3 C25 117.1(4) . . ? C21 N3 Cr3 126.4(3) . . ? C25 N3 Cr3 116.5(3) . . ? C26 N4 C30 119.1(4) . . ? C26 N4 Cr3 117.8(3) . . ? C30 N4 Cr3 123.0(4) . . ? C31 N5 C35 118.1(4) . . ? C31 N5 Cr4 126.5(4) . . ? C35 N5 Cr4 115.4(3) . . ? C40 N6 C36 118.4(4) . . ? C40 N6 Cr4 124.0(3) . . ? C36 N6 Cr4 117.4(3) . . ? O1 C1 C4 113.6(4) . . ? O1 C1 H1A 108.8 . . ? C4 C1 H1A 108.8 . . ? O1 C1 H1B 108.8 . . ? C4 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O2 C2 C4 113.3(4) . . ? O2 C2 H2A 108.9 . . ? C4 C2 H2A 108.9 . . ? O2 C2 H2B 108.9 . . ? C4 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O3 C3 C4 113.7(4) . . ? O3 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? O3 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C1 C4 C3 111.5(4) . . ? C1 C4 C5 106.5(4) . . ? C3 C4 C5 106.9(4) . . ? C1 C4 C2 111.7(4) . . ? C3 C4 C2 112.3(4) . . ? C5 C4 C2 107.7(4) . . ? O4 C5 C4 114.1(5) . . ? O4 C5 H5A 108.7 . . ? C4 C5 H5A 108.7 . . ? O4 C5 H5B 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? O5 C6 C9 114.2(4) . . ? O5 C6 H6A 108.7 . . ? C9 C6 H6A 108.7 . . ? O5 C6 H6B 108.7 . . ? C9 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O6 C7 C9 114.3(4) . . ? O6 C7 H7A 108.7 . . ? C9 C7 H7A 108.7 . . ? O6 C7 H7B 108.7 . . ? C9 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O7 C8 C9 114.8(4) . . ? O7 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? O7 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C7 106.7(4) . . ? C10 C9 C6 107.9(4) . . ? C7 C9 C6 111.4(4) . . ? C10 C9 C8 108.0(4) . . ? C7 C9 C8 112.0(4) . . ? C6 C9 C8 110.6(4) . . ? O8 C10 O8X 88.2(9) . . ? O8 C10 C9 115.6(4) . . ? O8X C10 C9 113.4(9) . . ? O8 C10 O8Y 114.9(11) . . ? O8X C10 O8Y 109.3(14) . . ? C9 C10 O8Y 112.9(9) . . ? O8 C10 H10A 108.4 . . ? O8X C10 H10A 121.7 . . ? C9 C10 H10A 108.4 . . ? O8Y C10 H10A 13.3 . . ? O8 C10 H10B 108.4 . . ? O8X C10 H10B 21.2 . . ? C9 C10 H10B 108.4 . . ? O8Y C10 H10B 94.2 . . ? H10A C10 H10B 107.5 . . ? N1 C11 C12 123.4(5) . . ? N1 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 118.6(5) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C12 C13 C14 119.6(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 119.2(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N1 C15 C14 121.8(5) . . ? N1 C15 C16 114.3(5) . . ? C14 C15 C16 123.9(5) . . ? N2 C16 C17 121.5(5) . . ? N2 C16 C15 114.9(4) . . ? C17 C16 C15 123.4(5) . . ? C18 C17 C16 118.4(6) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C19 C18 C17 119.4(6) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 119.7(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N2 C20 C19 120.9(6) . . ? N2 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? N3 C21 C22 122.6(5) . . ? N3 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C21 C22 C23 119.6(5) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C24 118.7(5) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C25 C24 C23 119.2(5) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? N3 C25 C24 122.9(4) . . ? N3 C25 C26 113.7(4) . . ? C24 C25 C26 123.4(5) . . ? N4 C26 C27 122.3(5) . . ? N4 C26 C25 114.1(4) . . ? C27 C26 C25 123.6(5) . . ? C26 C27 C28 118.6(5) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C29 C28 C27 119.2(5) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C30 C29 C28 119.5(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N4 C30 C29 121.2(5) . . ? N4 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? N5 C31 C32 123.2(6) . . ? N5 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C33 C32 C31 118.5(6) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 120.0(5) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 118.9(6) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N5 C35 C34 121.3(5) . . ? N5 C35 C36 115.7(4) . . ? C34 C35 C36 123.0(5) . . ? C37 C36 N6 120.8(5) . . ? C37 C36 C35 125.7(5) . . ? N6 C36 C35 113.4(5) . . ? C36 C37 C38 120.0(5) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 119.4(5) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 118.8(5) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N6 C40 C39 122.5(5) . . ? N6 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? N7 C41 C42 177.0(11) . . ? N8 C43 C44 173.9(10) . . ? N9 C45 C46 173(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cr1 O1 C1 48.3(3) . . . . ? O6 Cr1 O1 C1 -124.2(3) . . . . ? O2 Cr1 O1 C1 -44.3(3) . . . . ? O5 Cr1 O1 C1 144.5(3) . . . . ? O7 Cr1 O1 C1 96.6(7) . . . . ? O3 Cr1 O1 Cr2 -95.22(15) . . . . ? O6 Cr1 O1 Cr2 92.25(15) . . . . ? O2 Cr1 O1 Cr2 172.14(14) . . . . ? O5 Cr1 O1 Cr2 0.95(13) . . . . ? O7 Cr1 O1 Cr2 -47.0(7) . . . . ? O5 Cr2 O1 C1 -138.8(3) . . . . ? N1 Cr2 O1 C1 -173.9(6) . . . . ? N2 Cr2 O1 C1 131.1(3) . . . . ? Cl1 Cr2 O1 C1 -43.4(3) . . . . ? Cl2 Cr2 O1 C1 46.6(3) . . . . ? O5 Cr2 O1 Cr1 -0.95(13) . . . . ? N1 Cr2 O1 Cr1 -36.1(7) . . . . ? N2 Cr2 O1 Cr1 -91.08(15) . . . . ? Cl1 Cr2 O1 Cr1 94.45(12) . . . . ? Cl2 Cr2 O1 Cr1 -175.53(11) . . . . ? O6 Cr3 O2 C2 -140.0(4) . . . . ? N4 Cr3 O2 C2 132.1(4) . . . . ? N3 Cr3 O2 C2 -176.5(7) . . . . ? Cl3 Cr3 O2 C2 -44.8(4) . . . . ? Cl4 Cr3 O2 C2 45.7(4) . . . . ? O6 Cr3 O2 Cr1 -2.25(12) . . . . ? N4 Cr3 O2 Cr1 -90.19(16) . . . . ? N3 Cr3 O2 Cr1 -38.8(8) . . . . ? Cl3 Cr3 O2 Cr1 92.91(11) . . . . ? Cl4 Cr3 O2 Cr1 -176.60(10) . . . . ? O1 Cr1 O2 C2 49.5(3) . . . . ? O3 Cr1 O2 C2 -43.4(3) . . . . ? O6 Cr1 O2 C2 145.8(3) . . . . ? O5 Cr1 O2 C2 95.5(7) . . . . ? O7 Cr1 O2 C2 -122.5(3) . . . . ? O1 Cr1 O2 Cr3 -94.03(14) . . . . ? O3 Cr1 O2 Cr3 173.13(14) . . . . ? O6 Cr1 O2 Cr3 2.29(13) . . . . ? O5 Cr1 O2 Cr3 -48.0(7) . . . . ? O7 Cr1 O2 Cr3 93.98(14) . . . . ? O1 Cr1 O3 C3 -43.3(3) . . . . ? O6 Cr1 O3 C3 98.2(7) . . . . ? O2 Cr1 O3 C3 49.1(3) . . . . ? O5 Cr1 O3 C3 -122.9(3) . . . . ? O7 Cr1 O3 C3 146.3(3) . . . . ? O1 Cr1 O3 Cr4 171.15(15) . . . . ? O6 Cr1 O3 Cr4 -47.4(7) . . . . ? O2 Cr1 O3 Cr4 -96.40(15) . . . . ? O5 Cr1 O3 Cr4 91.57(15) . . . . ? O7 Cr1 O3 Cr4 0.74(15) . . . . ? O7 Cr4 O3 C3 -140.4(4) . . . . ? N6 Cr4 O3 C3 129.0(4) . . . . ? N5 Cr4 O3 C3 175.2(7) . . . . ? Cl6 Cr4 O3 C3 42.4(3) . . . . ? Cl5 Cr4 O3 C3 -46.8(3) . . . . ? O7 Cr4 O3 Cr1 -0.73(15) . . . . ? N6 Cr4 O3 Cr1 -91.32(17) . . . . ? N5 Cr4 O3 Cr1 -45.2(8) . . . . ? Cl6 Cr4 O3 Cr1 -177.88(12) . . . . ? Cl5 Cr4 O3 Cr1 92.93(13) . . . . ? O1 Cr1 O5 C6 144.4(3) . . . . ? O3 Cr1 O5 C6 -124.0(3) . . . . ? O6 Cr1 O5 C6 48.1(3) . . . . ? O2 Cr1 O5 C6 97.4(7) . . . . ? O7 Cr1 O5 C6 -45.0(3) . . . . ? O1 Cr1 O5 Cr2 -0.94(13) . . . . ? O3 Cr1 O5 Cr2 90.62(14) . . . . ? O6 Cr1 O5 Cr2 -97.22(14) . . . . ? O2 Cr1 O5 Cr2 -47.9(7) . . . . ? O7 Cr1 O5 Cr2 169.69(13) . . . . ? O1 Cr2 O5 C6 -137.5(4) . . . . ? N1 Cr2 O5 C6 35.7(4) . . . . ? N2 Cr2 O5 C6 -41.8(4) . . . . ? Cl1 Cr2 O5 C6 129.8(3) . . . . ? Cl2 Cr2 O5 C6 -94.5(9) . . . . ? O1 Cr2 O5 Cr1 0.93(13) . . . . ? N1 Cr2 O5 Cr1 174.09(15) . . . . ? N2 Cr2 O5 Cr1 96.58(16) . . . . ? Cl1 Cr2 O5 Cr1 -91.77(11) . . . . ? Cl2 Cr2 O5 Cr1 43.9(9) . . . . ? O1 Cr1 O6 C7 -123.6(3) . . . . ? O3 Cr1 O6 C7 95.2(7) . . . . ? O2 Cr1 O6 C7 145.2(3) . . . . ? O5 Cr1 O6 C7 -44.0(3) . . . . ? O7 Cr1 O6 C7 48.2(3) . . . . ? O1 Cr1 O6 Cr3 88.92(15) . . . . ? O3 Cr1 O6 Cr3 -52.3(7) . . . . ? O2 Cr1 O6 Cr3 -2.24(12) . . . . ? O5 Cr1 O6 Cr3 168.48(13) . . . . ? O7 Cr1 O6 Cr3 -99.31(15) . . . . ? O2 Cr3 O6 C7 -137.8(4) . . . . ? N4 Cr3 O6 C7 -42.4(4) . . . . ? N3 Cr3 O6 C7 35.3(4) . . . . ? Cl3 Cr3 O6 C7 129.8(4) . . . . ? Cl4 Cr3 O6 C7 -92.1(9) . . . . ? O2 Cr3 O6 Cr1 2.24(12) . . . . ? N4 Cr3 O6 Cr1 97.70(15) . . . . ? N3 Cr3 O6 Cr1 175.39(15) . . . . ? Cl3 Cr3 O6 Cr1 -90.16(11) . . . . ? Cl4 Cr3 O6 Cr1 48.0(8) . . . . ? O1 Cr1 O7 C8 95.8(7) . . . . ? O3 Cr1 O7 C8 145.2(3) . . . . ? O6 Cr1 O7 C8 -43.7(3) . . . . ? O2 Cr1 O7 C8 -123.7(3) . . . . ? O5 Cr1 O7 C8 48.9(3) . . . . ? O1 Cr1 O7 Cr4 -50.1(8) . . . . ? O3 Cr1 O7 Cr4 -0.72(14) . . . . ? O6 Cr1 O7 Cr4 170.39(15) . . . . ? O2 Cr1 O7 Cr4 90.39(15) . . . . ? O5 Cr1 O7 Cr4 -97.01(15) . . . . ? O3 Cr4 O7 C8 -137.8(4) . . . . ? N6 Cr4 O7 C8 -43.0(4) . . . . ? N5 Cr4 O7 C8 35.0(4) . . . . ? Cl6 Cr4 O7 C8 -115.0(8) . . . . ? Cl5 Cr4 O7 C8 128.7(4) . . . . ? O3 Cr4 O7 Cr1 0.72(14) . . . . ? N6 Cr4 O7 Cr1 95.49(16) . . . . ? N5 Cr4 O7 Cr1 173.54(17) . . . . ? Cl6 Cr4 O7 Cr1 23.6(10) . . . . ? Cl5 Cr4 O7 Cr1 -92.81(12) . . . . ? O1 Cr2 N1 C11 118.9(7) . . . . ? O5 Cr2 N1 C11 84.6(4) . . . . ? N2 Cr2 N1 C11 175.5(4) . . . . ? Cl1 Cr2 N1 C11 -11.6(4) . . . . ? Cl2 Cr2 N1 C11 -101.5(4) . . . . ? O1 Cr2 N1 C15 -58.7(8) . . . . ? O5 Cr2 N1 C15 -93.1(3) . . . . ? N2 Cr2 N1 C15 -2.1(3) . . . . ? Cl1 Cr2 N1 C15 170.7(3) . . . . ? Cl2 Cr2 N1 C15 80.9(3) . . . . ? O1 Cr2 N2 C16 176.7(4) . . . . ? O5 Cr2 N2 C16 98.2(4) . . . . ? N1 Cr2 N2 C16 6.7(4) . . . . ? Cl1 Cr2 N2 C16 -33.2(9) . . . . ? Cl2 Cr2 N2 C16 -88.2(4) . . . . ? O1 Cr2 N2 C20 -16.6(4) . . . . ? O5 Cr2 N2 C20 -95.1(4) . . . . ? N1 Cr2 N2 C20 173.4(4) . . . . ? Cl1 Cr2 N2 C20 133.5(6) . . . . ? Cl2 Cr2 N2 C20 78.6(4) . . . . ? O2 Cr3 N3 C21 125.1(7) . . . . ? O6 Cr3 N3 C21 89.3(4) . . . . ? N4 Cr3 N3 C21 177.8(5) . . . . ? Cl3 Cr3 N3 C21 -6.6(4) . . . . ? Cl4 Cr3 N3 C21 -97.0(4) . . . . ? O2 Cr3 N3 C25 -51.6(10) . . . . ? O6 Cr3 N3 C25 -87.4(4) . . . . ? N4 Cr3 N3 C25 1.2(4) . . . . ? Cl3 Cr3 N3 C25 176.7(4) . . . . ? Cl4 Cr3 N3 C25 86.4(4) . . . . ? O2 Cr3 N4 C26 171.5(4) . . . . ? O6 Cr3 N4 C26 92.8(4) . . . . ? N3 Cr3 N4 C26 0.7(4) . . . . ? Cl3 Cr3 N4 C26 -28.3(11) . . . . ? Cl4 Cr3 N4 C26 -93.2(4) . . . . ? O2 Cr3 N4 C30 -11.3(4) . . . . ? O6 Cr3 N4 C30 -90.0(4) . . . . ? N3 Cr3 N4 C30 178.0(4) . . . . ? Cl3 Cr3 N4 C30 148.9(7) . . . . ? Cl4 Cr3 N4 C30 84.0(4) . . . . ? O3 Cr4 N5 C31 134.3(8) . . . . ? O7 Cr4 N5 C31 90.8(4) . . . . ? N6 Cr4 N5 C31 -178.5(4) . . . . ? Cl6 Cr4 N5 C31 -92.9(4) . . . . ? Cl5 Cr4 N5 C31 -3.9(4) . . . . ? O3 Cr4 N5 C35 -48.5(9) . . . . ? O7 Cr4 N5 C35 -91.9(4) . . . . ? N6 Cr4 N5 C35 -1.2(4) . . . . ? Cl6 Cr4 N5 C35 84.4(4) . . . . ? Cl5 Cr4 N5 C35 173.4(3) . . . . ? O3 Cr4 N6 C40 -12.0(4) . . . . ? O7 Cr4 N6 C40 -90.6(4) . . . . ? N5 Cr4 N6 C40 175.6(4) . . . . ? Cl6 Cr4 N6 C40 82.4(4) . . . . ? Cl5 Cr4 N6 C40 143.4(6) . . . . ? O3 Cr4 N6 C36 172.4(3) . . . . ? O7 Cr4 N6 C36 93.7(4) . . . . ? N5 Cr4 N6 C36 -0.1(3) . . . . ? Cl6 Cr4 N6 C36 -93.3(3) . . . . ? Cl5 Cr4 N6 C36 -32.2(9) . . . . ? Cr1 O1 C1 C4 -4.0(5) . . . . ? Cr2 O1 C1 C4 128.7(4) . . . . ? Cr3 O2 C2 C4 127.6(4) . . . . ? Cr1 O2 C2 C4 -4.7(5) . . . . ? Cr1 O3 C3 C4 -5.2(5) . . . . ? Cr4 O3 C3 C4 129.7(4) . . . . ? O1 C1 C4 C3 -60.6(5) . . . . ? O1 C1 C4 C5 -176.9(4) . . . . ? O1 C1 C4 C2 65.8(5) . . . . ? O3 C3 C4 C1 66.3(5) . . . . ? O3 C3 C4 C5 -177.7(4) . . . . ? O3 C3 C4 C2 -59.9(6) . . . . ? O2 C2 C4 C1 -60.2(5) . . . . ? O2 C2 C4 C3 65.8(6) . . . . ? O2 C2 C4 C5 -176.8(4) . . . . ? C1 C4 C5 O4 -173.2(5) . . . . ? C3 C4 C5 O4 67.6(6) . . . . ? C2 C4 C5 O4 -53.3(6) . . . . ? Cr1 O5 C6 C9 -3.5(5) . . . . ? Cr2 O5 C6 C9 129.6(4) . . . . ? Cr1 O6 C7 C9 -3.8(5) . . . . ? Cr3 O6 C7 C9 131.2(4) . . . . ? Cr1 O7 C8 C9 -3.6(5) . . . . ? Cr4 O7 C8 C9 129.8(3) . . . . ? O6 C7 C9 C10 -177.5(4) . . . . ? O6 C7 C9 C6 65.0(6) . . . . ? O6 C7 C9 C8 -59.4(6) . . . . ? O5 C6 C9 C10 -177.2(4) . . . . ? O5 C6 C9 C7 -60.4(6) . . . . ? O5 C6 C9 C8 64.9(5) . . . . ? O7 C8 C9 C10 -178.5(4) . . . . ? O7 C8 C9 C7 64.3(5) . . . . ? O7 C8 C9 C6 -60.6(5) . . . . ? C7 C9 C10 O8 177.0(5) . . . . ? C6 C9 C10 O8 -63.2(6) . . . . ? C8 C9 C10 O8 56.4(6) . . . . ? C7 C9 C10 O8X 77.2(11) . . . . ? C6 C9 C10 O8X -162.9(10) . . . . ? C8 C9 C10 O8X -43.3(11) . . . . ? C7 C9 C10 O8Y -47.9(13) . . . . ? C6 C9 C10 O8Y 72.0(13) . . . . ? C8 C9 C10 O8Y -168.5(12) . . . . ? C15 N1 C11 C12 0.8(7) . . . . ? Cr2 N1 C11 C12 -176.8(4) . . . . ? N1 C11 C12 C13 -0.5(8) . . . . ? C11 C12 C13 C14 0.0(8) . . . . ? C12 C13 C14 C15 0.3(8) . . . . ? C11 N1 C15 C14 -0.6(7) . . . . ? Cr2 N1 C15 C14 177.3(4) . . . . ? C11 N1 C15 C16 180.0(4) . . . . ? Cr2 N1 C15 C16 -2.2(5) . . . . ? C13 C14 C15 N1 0.1(8) . . . . ? C13 C14 C15 C16 179.5(5) . . . . ? C20 N2 C16 C17 -0.1(8) . . . . ? Cr2 N2 C16 C17 166.9(4) . . . . ? C20 N2 C16 C15 -176.9(4) . . . . ? Cr2 N2 C16 C15 -9.8(6) . . . . ? N1 C15 C16 N2 7.9(6) . . . . ? C14 C15 C16 N2 -171.6(5) . . . . ? N1 C15 C16 C17 -168.8(5) . . . . ? C14 C15 C16 C17 11.7(8) . . . . ? N2 C16 C17 C18 0.6(9) . . . . ? C15 C16 C17 C18 177.0(5) . . . . ? C16 C17 C18 C19 -0.7(10) . . . . ? C17 C18 C19 C20 0.4(10) . . . . ? C16 N2 C20 C19 -0.2(8) . . . . ? Cr2 N2 C20 C19 -166.5(4) . . . . ? C18 C19 C20 N2 0.0(9) . . . . ? C25 N3 C21 C22 -0.1(8) . . . . ? Cr3 N3 C21 C22 -176.7(4) . . . . ? N3 C21 C22 C23 0.2(9) . . . . ? C21 C22 C23 C24 -1.3(9) . . . . ? C22 C23 C24 C25 2.3(9) . . . . ? C21 N3 C25 C24 1.2(8) . . . . ? Cr3 N3 C25 C24 178.1(4) . . . . ? C21 N3 C25 C26 -179.6(4) . . . . ? Cr3 N3 C25 C26 -2.7(6) . . . . ? C23 C24 C25 N3 -2.3(9) . . . . ? C23 C24 C25 C26 178.6(5) . . . . ? C30 N4 C26 C27 1.7(8) . . . . ? Cr3 N4 C26 C27 179.1(4) . . . . ? C30 N4 C26 C25 -179.7(4) . . . . ? Cr3 N4 C26 C25 -2.3(6) . . . . ? N3 C25 C26 N4 3.2(6) . . . . ? C24 C25 C26 N4 -177.6(5) . . . . ? N3 C25 C26 C27 -178.2(5) . . . . ? C24 C25 C26 C27 1.0(8) . . . . ? N4 C26 C27 C28 -0.2(8) . . . . ? C25 C26 C27 C28 -178.7(5) . . . . ? C26 C27 C28 C29 -1.4(8) . . . . ? C27 C28 C29 C30 1.6(8) . . . . ? C26 N4 C30 C29 -1.6(8) . . . . ? Cr3 N4 C30 C29 -178.8(4) . . . . ? C28 C29 C30 N4 -0.1(8) . . . . ? C35 N5 C31 C32 -1.0(8) . . . . ? Cr4 N5 C31 C32 176.2(4) . . . . ? N5 C31 C32 C33 1.1(9) . . . . ? C31 C32 C33 C34 -0.6(9) . . . . ? C32 C33 C34 C35 0.0(8) . . . . ? C31 N5 C35 C34 0.3(7) . . . . ? Cr4 N5 C35 C34 -177.2(4) . . . . ? C31 N5 C35 C36 179.7(4) . . . . ? Cr4 N5 C35 C36 2.2(6) . . . . ? C33 C34 C35 N5 0.1(8) . . . . ? C33 C34 C35 C36 -179.2(5) . . . . ? C40 N6 C36 C37 3.1(7) . . . . ? Cr4 N6 C36 C37 179.0(4) . . . . ? C40 N6 C36 C35 -174.7(4) . . . . ? Cr4 N6 C36 C35 1.2(5) . . . . ? N5 C35 C36 C37 -179.9(5) . . . . ? C34 C35 C36 C37 -0.5(8) . . . . ? N5 C35 C36 N6 -2.3(6) . . . . ? C34 C35 C36 N6 177.1(5) . . . . ? N6 C36 C37 C38 -1.7(8) . . . . ? C35 C36 C37 C38 175.8(5) . . . . ? C36 C37 C38 C39 -1.0(8) . . . . ? C37 C38 C39 C40 2.1(8) . . . . ? C36 N6 C40 C39 -2.0(7) . . . . ? Cr4 N6 C40 C39 -177.6(4) . . . . ? C38 C39 C40 N6 -0.6(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 N9 0.82 2.28 2.915(14) 135.1 . O8 H8 N7 0.82 2.08 2.861(10) 160.4 2_576 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.134 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.097 # Attachment '- 4.cif' data_cr4_4 _database_code_depnum_ccdc_archive 'CCDC 810903' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cr4(tmp)2(t-bu-bpy)3Cl6],4MeCN,0.5Me2CO,0.5H2O' _chemical_melting_point ? _chemical_formula_moiety '(C66 H94 Cl6 Cr4 N6 O6), 4(C2 H3 N), 0.5(C3H6O), 0.5(H2O)' _chemical_formula_sum 'C75.50 H110 Cl6 Cr4 N10 O7' _chemical_formula_weight 1690.43 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' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9679(9) _cell_length_b 19.2804(12) _cell_length_c 19.5271(17) _cell_angle_alpha 60.4850(10) _cell_angle_beta 74.5300(10) _cell_angle_gamma 74.9500(10) _cell_volume 4358.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6447 _cell_measurement_theta_min 2.190 _cell_measurement_theta_max 28.329 _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1774 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.428 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35126 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.37 _reflns_number_total 17589 _reflns_number_gt 14993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0818P)^2^+8.1476P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17589 _refine_ls_number_parameters 1038 _refine_ls_number_restraints 459 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1430 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.050 _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 C1 C 1.1648(2) 0.25849(18) 0.28038(18) 0.0150(6) Uani 1 1 d . . . H1A H 1.1978 0.2743 0.2243 0.018 Uiso 1 1 calc R . . H1B H 1.1876 0.2003 0.3120 0.018 Uiso 1 1 calc R . . C2 C 1.1598(2) 0.27720(18) 0.40219(17) 0.0154(6) Uani 1 1 d . . . H2A H 1.1894 0.2200 0.4313 0.019 Uiso 1 1 calc R . . H2B H 1.1839 0.3090 0.4197 0.019 Uiso 1 1 calc R . . C3 C 1.1663(2) 0.39767(17) 0.26391(18) 0.0151(6) Uani 1 1 d . . . H3A H 1.1977 0.4265 0.2804 0.018 Uiso 1 1 calc R . . H3B H 1.1920 0.4139 0.2065 0.018 Uiso 1 1 calc R . . C4 C 1.1978(2) 0.30635(18) 0.31189(17) 0.0150(6) Uani 1 1 d . . . C5 C 1.3145(2) 0.28711(19) 0.30485(19) 0.0200(6) Uani 1 1 d . . . H5A H 1.3350 0.3143 0.3292 0.024 Uiso 1 1 calc R . . H5B H 1.3329 0.2283 0.3373 0.024 Uiso 1 1 calc R . . C6 C 1.3761(2) 0.3105(2) 0.2223(2) 0.0286(8) Uani 1 1 d . . . H6A H 1.3562 0.2852 0.1963 0.043 Uiso 1 1 calc R . . H6B H 1.4476 0.2921 0.2264 0.043 Uiso 1 1 calc R . . H6C H 1.3645 0.3692 0.1905 0.043 Uiso 1 1 calc R . . C7 C 0.7906(2) 0.38311(18) 0.27330(18) 0.0154(6) Uani 1 1 d . . . H7A H 0.7601 0.3499 0.2616 0.019 Uiso 1 1 calc R . . H7B H 0.7673 0.4405 0.2387 0.019 Uiso 1 1 calc R . . C8 C 0.7857(2) 0.27672(17) 0.41927(18) 0.0159(6) Uani 1 1 d . . . H8A H 0.7525 0.2669 0.4742 0.019 Uiso 1 1 calc R . . H8B H 0.7622 0.2413 0.4058 0.019 Uiso 1 1 calc R . . C9 C 0.7874(2) 0.42389(18) 0.37956(18) 0.0154(6) Uani 1 1 d . . . H9A H 0.7577 0.4797 0.3459 0.018 Uiso 1 1 calc R . . H9B H 0.7606 0.4118 0.4360 0.018 Uiso 1 1 calc R . . C10 C 0.7530(2) 0.36557(17) 0.36110(18) 0.0144(6) Uani 1 1 d . . . C11 C 0.6366(2) 0.38386(19) 0.37381(19) 0.0189(6) Uani 1 1 d . . . H11A H 0.6127 0.3818 0.4272 0.023 Uiso 1 1 calc R . . H11B H 0.6166 0.4398 0.3339 0.023 Uiso 1 1 calc R . . C12 C 0.5820(2) 0.3288(2) 0.3680(2) 0.0290(8) Uani 1 1 d . . . H12A H 0.6048 0.3297 0.3156 0.043 Uiso 1 1 calc R . . H12B H 0.5095 0.3475 0.3748 0.043 Uiso 1 1 calc R . . H12C H 0.5966 0.2736 0.4099 0.043 Uiso 1 1 calc R . . C13 C 0.8831(2) 0.39701(18) 0.04866(18) 0.0189(6) Uani 1 1 d . . . H13 H 0.9333 0.4307 0.0274 0.023 Uiso 1 1 calc R . . C14 C 0.8145(2) 0.41235(19) 0.00146(18) 0.0204(6) Uani 1 1 d . . . H14 H 0.8179 0.4562 -0.0507 0.024 Uiso 1 1 calc R . . C15 C 0.7406(2) 0.36372(19) 0.03016(19) 0.0191(6) Uani 1 1 d . . . C16 C 0.7402(2) 0.30044(19) 0.10825(19) 0.0199(6) Uani 1 1 d . . . H16 H 0.6917 0.2651 0.1304 0.024 Uiso 1 1 calc R . . C17 C 0.8094(2) 0.28919(18) 0.15273(18) 0.0171(6) Uani 1 1 d . . . C18 C 0.8127(2) 0.22376(18) 0.23529(18) 0.0165(6) Uani 1 1 d . . . C19 C 0.7383(2) 0.17570(19) 0.27997(19) 0.0203(6) Uani 1 1 d . . . H19 H 0.6809 0.1840 0.2579 0.024 Uiso 1 1 calc R . . C20 C 0.7473(2) 0.11499(18) 0.35741(19) 0.0199(6) Uani 1 1 d . . . C21 C 0.8367(2) 0.10247(18) 0.38341(18) 0.0186(6) Uani 1 1 d . . . H21 H 0.8493 0.0585 0.4334 0.022 Uiso 1 1 calc R . . C22 C 0.9072(2) 0.15360(17) 0.33698(18) 0.0163(6) Uani 1 1 d . . . H22 H 0.9669 0.1447 0.3566 0.020 Uiso 1 1 calc R . . C23 C 0.6638(2) 0.3752(2) -0.01865(19) 0.0223(7) Uani 1 1 d . . . C24 C 0.6629(3) 0.4562(2) -0.0940(2) 0.0284(8) Uani 1 1 d . . . H24A H 0.6496 0.5000 -0.0793 0.043 Uiso 1 1 calc R . . H24B H 0.6103 0.4630 -0.1224 0.043 Uiso 1 1 calc R . . H24C H 0.7284 0.4574 -0.1287 0.043 Uiso 1 1 calc R . . C25 C 0.6931(3) 0.3063(2) -0.0422(2) 0.0292(8) Uani 1 1 d . . . H25A H 0.7569 0.3126 -0.0794 0.044 Uiso 1 1 calc R . . H25B H 0.6405 0.3079 -0.0678 0.044 Uiso 1 1 calc R . . H25C H 0.7005 0.2545 0.0057 0.044 Uiso 1 1 calc R . . C26 C 0.5584(3) 0.3723(2) 0.0323(2) 0.0318(8) Uani 1 1 d . . . H26A H 0.5561 0.3188 0.0783 0.048 Uiso 1 1 calc R . . H26B H 0.5084 0.3829 0.0000 0.048 Uiso 1 1 calc R . . H26C H 0.5436 0.4133 0.0509 0.048 Uiso 1 1 calc R . . C27 C 0.6630(3) 0.0653(2) 0.4107(2) 0.0264(7) Uani 1 1 d . . . C28 C 0.6923(3) -0.0175(3) 0.4167(3) 0.0549(13) Uani 1 1 d . . . H28A H 0.6462 -0.0528 0.4597 0.082 Uiso 1 1 calc R . . H28B H 0.7611 -0.0388 0.4281 0.082 Uiso 1 1 calc R . . H28C H 0.6889 -0.0151 0.3661 0.082 Uiso 1 1 calc R . . C29 C 0.5632(3) 0.1067(3) 0.3830(3) 0.0578(14) Uani 1 1 d . . . H29A H 0.5674 0.1137 0.3291 0.087 Uiso 1 1 calc R . . H29B H 0.5463 0.1595 0.3824 0.087 Uiso 1 1 calc R . . H29C H 0.5110 0.0737 0.4194 0.087 Uiso 1 1 calc R . . C30 C 0.6483(4) 0.0585(4) 0.4956(3) 0.0598(14) Uani 1 1 d . . . H30A H 0.6347 0.1127 0.4918 0.090 Uiso 1 1 calc R . . H30B H 0.7094 0.0287 0.5188 0.090 Uiso 1 1 calc R . . H30C H 0.5914 0.0299 0.5295 0.090 Uiso 1 1 calc R . . C31 C 0.8745(3) 0.04713(19) 0.59969(19) 0.0222(7) Uani 1 1 d . . . H31 H 0.9274 0.0252 0.5704 0.027 Uiso 1 1 calc R . . C32 C 0.8046(3) -0.00095(19) 0.6555(2) 0.0243(7) Uani 1 1 d . . . H32 H 0.8109 -0.0549 0.6644 0.029 Uiso 1 1 calc R . . C33 C 0.7252(2) 0.02897(19) 0.69885(19) 0.0211(7) Uani 1 1 d . . . C34 C 0.7216(2) 0.10876(18) 0.68270(19) 0.0202(6) Uani 1 1 d . . . H34 H 0.6683 0.1323 0.7104 0.024 Uiso 1 1 calc R . . C35 C 0.7944(2) 0.15388(18) 0.62692(18) 0.0173(6) Uani 1 1 d . . . C36 C 0.7980(2) 0.23753(18) 0.60905(18) 0.0176(6) Uani 1 1 d . . . C37 C 0.7251(2) 0.28231(19) 0.64104(19) 0.0203(6) Uani 1 1 d . . . H37 H 0.6673 0.2600 0.6761 0.024 Uiso 1 1 calc R . . C38 C 0.7358(2) 0.36044(19) 0.62213(19) 0.0200(6) Uani 1 1 d . . . C39 C 0.8249(2) 0.38747(19) 0.57405(18) 0.0195(6) Uani 1 1 d . . . H39 H 0.8379 0.4384 0.5627 0.023 Uiso 1 1 calc R . . C40 C 0.8944(2) 0.34058(18) 0.54277(18) 0.0181(6) Uani 1 1 d . . . H40 H 0.9543 0.3607 0.5094 0.022 Uiso 1 1 calc R . . C41 C 0.6456(3) -0.0205(2) 0.7615(2) 0.0305(8) Uani 1 1 d . . . C42 C 0.6605(3) -0.1048(2) 0.7690(3) 0.0378(10) Uani 1 1 d . . . H42A H 0.6038 -0.1321 0.8058 0.057 Uiso 1 1 calc R . . H42B H 0.7231 -0.1356 0.7894 0.057 Uiso 1 1 calc R . . H42C H 0.6641 -0.1010 0.7164 0.057 Uiso 1 1 calc R . . C43 C 0.5435(3) 0.0238(3) 0.7395(4) 0.0595(15) Uani 1 1 d . . . H43A H 0.5438 0.0382 0.6838 0.089 Uiso 1 1 calc R . . H43B H 0.5278 0.0729 0.7461 0.089 Uiso 1 1 calc R . . H43C H 0.4925 -0.0111 0.7743 0.089 Uiso 1 1 calc R . . C44 C 0.6536(4) -0.0294(3) 0.8431(3) 0.0527(13) Uani 1 1 d . . . H44A H 0.6392 0.0240 0.8412 0.079 Uiso 1 1 calc R . . H44B H 0.7217 -0.0547 0.8548 0.079 Uiso 1 1 calc R . . H44C H 0.6050 -0.0630 0.8850 0.079 Uiso 1 1 calc R . . C45 C 0.6541(3) 0.4111(2) 0.6552(2) 0.0293(8) Uani 1 1 d . . . C46 C 0.5502(3) 0.4039(2) 0.6497(3) 0.0356(9) Uani 1 1 d . . . H46A H 0.5493 0.4146 0.5953 0.053 Uiso 1 1 calc R . . H46B H 0.4993 0.4431 0.6630 0.053 Uiso 1 1 calc R . . H46C H 0.5353 0.3493 0.6873 0.053 Uiso 1 1 calc R . . C47 C 0.6608(3) 0.3761(3) 0.7447(3) 0.0488(12) Uani 1 1 d . . . H47A H 0.6477 0.3203 0.7734 0.073 Uiso 1 1 calc R . . H47B H 0.6108 0.4086 0.7676 0.073 Uiso 1 1 calc R . . H47C H 0.7282 0.3775 0.7497 0.073 Uiso 1 1 calc R . . C48 C 0.6675(4) 0.4998(3) 0.6116(4) 0.0669(18) Uani 1 1 d . . . H48A H 0.7226 0.5065 0.6290 0.100 Uiso 1 1 calc R . . H48B H 0.6052 0.5324 0.6237 0.100 Uiso 1 1 calc R . . H48C H 0.6833 0.5174 0.5539 0.100 Uiso 1 1 calc R . . C49 C 0.8815(2) 0.60004(18) 0.40108(18) 0.0184(6) Uani 1 1 d . . . H49 H 0.9340 0.5705 0.4318 0.022 Uiso 1 1 calc R . . C50 C 0.8099(2) 0.65440(19) 0.42190(18) 0.0186(6) Uani 1 1 d . . . H50 H 0.8145 0.6614 0.4657 0.022 Uiso 1 1 calc R . . C51 C 0.7316(2) 0.69871(18) 0.37884(18) 0.0180(6) Uani 1 1 d . . . C52 C 0.7312(2) 0.68520(18) 0.31463(18) 0.0179(6) Uani 1 1 d . . . H52 H 0.6793 0.7139 0.2832 0.021 Uiso 1 1 calc R . . C53 C 0.8052(2) 0.63073(17) 0.29629(17) 0.0147(6) Uani 1 1 d . . . C54 C 0.8120(2) 0.61560(17) 0.22796(17) 0.0143(6) Uani 1 1 d . . . C55 C 0.7430(2) 0.65280(18) 0.17593(18) 0.0173(6) Uani 1 1 d . . . H55 H 0.6867 0.6896 0.1842 0.021 Uiso 1 1 calc R . . C56 C 0.7555(2) 0.63671(19) 0.11141(18) 0.0185(6) Uani 1 1 d . . . C57 C 0.8416(2) 0.58435(18) 0.10104(18) 0.0172(6) Uani 1 1 d . . . H57 H 0.8551 0.5735 0.0566 0.021 Uiso 1 1 calc R . . C58 C 0.9072(2) 0.54818(18) 0.15573(17) 0.0157(6) Uani 1 1 d . . . H58 H 0.9652 0.5124 0.1479 0.019 Uiso 1 1 calc R . . C59 C 0.6526(2) 0.7614(2) 0.3959(2) 0.0218(7) Uani 1 1 d . . . C60 C 0.6595(3) 0.7599(2) 0.4739(2) 0.0291(8) Uani 1 1 d . . . H60A H 0.6535 0.7057 0.5181 0.044 Uiso 1 1 calc R . . H60B H 0.6049 0.7989 0.4845 0.044 Uiso 1 1 calc R . . H60C H 0.7243 0.7741 0.4689 0.044 Uiso 1 1 calc R . . C61 C 0.5468(3) 0.7468(2) 0.4022(2) 0.0285(8) Uani 1 1 d . . . H61A H 0.5386 0.7541 0.3506 0.043 Uiso 1 1 calc R . . H61B H 0.4964 0.7853 0.4169 0.043 Uiso 1 1 calc R . . H61C H 0.5380 0.6917 0.4430 0.043 Uiso 1 1 calc R . . C62 C 0.6718(3) 0.8445(2) 0.3267(2) 0.0281(8) Uani 1 1 d . . . H62A H 0.7415 0.8509 0.3202 0.042 Uiso 1 1 calc R . . H62B H 0.6261 0.8868 0.3384 0.042 Uiso 1 1 calc R . . H62C H 0.6601 0.8488 0.2774 0.042 Uiso 1 1 calc R . . C63 C 0.6757(2) 0.6762(2) 0.0573(2) 0.0272(8) Uani 1 1 d . . . C64 C 0.5739(3) 0.6544(3) 0.1095(2) 0.0387(10) Uani 1 1 d . . . H64A H 0.5767 0.5957 0.1362 0.058 Uiso 1 1 calc R . . H64B H 0.5213 0.6797 0.0761 0.058 Uiso 1 1 calc R . . H64C H 0.5587 0.6739 0.1497 0.058 Uiso 1 1 calc R . . C65 C 0.6727(3) 0.7688(3) 0.0161(2) 0.0408(10) Uani 1 1 d . . . H65A H 0.6598 0.7874 0.0567 0.061 Uiso 1 1 calc R . . H65B H 0.6191 0.7952 -0.0164 0.061 Uiso 1 1 calc R . . H65C H 0.7374 0.7824 -0.0182 0.061 Uiso 1 1 calc R . . C66 C 0.6982(3) 0.6485(3) -0.0075(2) 0.0349(9) Uani 1 1 d . . . H66A H 0.7626 0.6634 -0.0415 0.052 Uiso 1 1 calc R . . H66B H 0.6446 0.6745 -0.0401 0.052 Uiso 1 1 calc R . . H66C H 0.7017 0.5898 0.0176 0.052 Uiso 1 1 calc R . . Cl1 Cl 1.07277(5) 0.40922(4) 0.10646(4) 0.01479(15) Uani 1 1 d . . . Cl2 Cl 1.08829(6) 0.21706(4) 0.14924(5) 0.02081(16) Uani 1 1 d . . . Cl3 Cl 1.06971(5) 0.10349(4) 0.46404(4) 0.01696(15) Uani 1 1 d . . . Cl4 Cl 1.07544(6) 0.15788(5) 0.60009(4) 0.02239(17) Uani 1 1 d . . . Cl5 Cl 1.07188(5) 0.46134(4) 0.40829(4) 0.01667(15) Uani 1 1 d . . . Cl6 Cl 1.08880(6) 0.59915(4) 0.21819(4) 0.01979(16) Uani 1 1 d . . . Cr1 Cr 0.98445(3) 0.30402(3) 0.19816(3) 0.01222(11) Uani 1 1 d . . . Cr2 Cr 0.97498(4) 0.19943(3) 0.50495(3) 0.01389(11) Uani 1 1 d . . . Cr3 Cr 0.98278(3) 0.50558(3) 0.30550(3) 0.01241(11) Uani 1 1 d . . . Cr4 Cr 0.97595(3) 0.33650(3) 0.33655(3) 0.01151(11) Uani 1 1 d . . . N1 N 0.88191(19) 0.33626(15) 0.12353(15) 0.0154(5) Uani 1 1 d . . . N2 N 0.89392(19) 0.21555(15) 0.26499(15) 0.0152(5) Uani 1 1 d . . . N3 N 0.8709(2) 0.12342(15) 0.58496(15) 0.0182(5) Uani 1 1 d . . . N4 N 0.88074(19) 0.26786(15) 0.55767(14) 0.0159(5) Uani 1 1 d . . . N5 N 0.88041(19) 0.58716(14) 0.34019(14) 0.0147(5) Uani 1 1 d . . . N6 N 0.89225(18) 0.56168(14) 0.21869(14) 0.0142(5) Uani 1 1 d . . . O1 O 1.05796(14) 0.27162(12) 0.28428(12) 0.0130(4) Uani 1 1 d . . . O2 O 1.05294(15) 0.28411(12) 0.42341(12) 0.0141(4) Uani 1 1 d . . . O3 O 1.05951(15) 0.42170(12) 0.27476(12) 0.0131(4) Uani 1 1 d . . . O4 O 0.89690(15) 0.36716(12) 0.25376(12) 0.0133(4) Uani 1 1 d . . . O5 O 0.89137(15) 0.25522(12) 0.41755(12) 0.0138(4) Uani 1 1 d . . . O6 O 0.89326(15) 0.41984(12) 0.36655(12) 0.0141(4) Uani 1 1 d . . . N1S N 1.1125(9) 0.1760(7) 0.8208(7) 0.091(3) Uani 0.521(9) 1 d PDU A 1 C1S C 1.0435(10) 0.2002(8) 0.7867(7) 0.073(3) Uani 0.521(9) 1 d PDU A 1 C2S C 0.9578(12) 0.2286(13) 0.7503(13) 0.068(3) Uani 0.521(9) 1 d PDU A 1 H2S1 H 0.9259 0.2808 0.7491 0.103 Uiso 0.521(9) 1 calc PR A 1 H2S2 H 0.9103 0.1898 0.7808 0.103 Uiso 0.521(9) 1 calc PR A 1 H2S3 H 0.9772 0.2350 0.6957 0.103 Uiso 0.521(9) 1 calc PR A 1 N1SX N 0.8221(14) 0.1489(12) 0.8252(12) 0.155(6) Uani 0.479(9) 1 d PDU A 2 C1SX C 0.8924(15) 0.1804(12) 0.8006(13) 0.125(5) Uani 0.479(9) 1 d PDU A 2 C2SX C 0.9787(16) 0.2219(18) 0.7521(17) 0.091(5) Uani 0.479(9) 1 d PDU A 2 H2S4 H 0.9580 0.2801 0.7330 0.136 Uiso 0.479(9) 1 calc PR A 2 H2S5 H 1.0043 0.2102 0.7064 0.136 Uiso 0.479(9) 1 calc PR A 2 H2S6 H 1.0316 0.2031 0.7845 0.136 Uiso 0.479(9) 1 calc PR A 2 N2S N 1.1600(12) 0.1684(10) 0.8917(10) 0.124(5) Uani 0.482(9) 1 d PDU B 1 C3S C 1.0948(12) 0.1969(9) 0.9258(10) 0.091(4) Uani 0.482(9) 1 d PDU B 1 C4S C 1.0169(16) 0.2414(13) 0.9612(18) 0.069(4) Uani 0.482(9) 1 d PDU B 1 H4S1 H 0.9936 0.2940 0.9190 0.103 Uiso 0.482(9) 1 calc PR B 1 H4S2 H 1.0439 0.2493 0.9979 0.103 Uiso 0.482(9) 1 calc PR B 1 H4S3 H 0.9605 0.2110 0.9905 0.103 Uiso 0.482(9) 1 calc PR B 1 N2SX N 0.9052(10) 0.1474(8) 1.0298(10) 0.126(5) Uani 0.518(9) 1 d PDU B 2 C3SX C 0.9569(9) 0.1957(7) 0.9985(8) 0.080(3) Uani 0.518(9) 1 d PDU B 2 C4SX C 1.0240(15) 0.2549(11) 0.9614(16) 0.059(3) Uani 0.518(9) 1 d PDU B 2 H4S4 H 1.0382 0.2648 1.0021 0.089 Uiso 0.518(9) 1 calc PR B 2 H4S5 H 0.9923 0.3054 0.9216 0.089 Uiso 0.518(9) 1 calc PR B 2 H4S6 H 1.0869 0.2349 0.9353 0.089 Uiso 0.518(9) 1 calc PR B 2 N3S N 0.4801(3) 0.1854(3) 0.8050(2) 0.0051(6) Uiso 0.570(6) 1 d PDU C 1 C5S C 0.5347(8) 0.1761(7) 0.8448(6) 0.074(2) Uiso 0.570(6) 1 d PDU C 1 C6S C 0.5854(12) 0.1317(10) 0.9206(8) 0.143(6) Uani 0.570(6) 1 d PDU C 1 H6S1 H 0.5591 0.0810 0.9571 0.214 Uiso 0.570(6) 1 calc PR C 1 H6S2 H 0.5709 0.1659 0.9473 0.214 Uiso 0.570(6) 1 calc PR C 1 H6S3 H 0.6583 0.1203 0.9052 0.214 Uiso 0.570(6) 1 calc PR C 1 N3SX N 0.5039(4) 0.2028(3) 0.7957(3) 0.0051(6) Uiso 0.430(6) 1 d PDU C 2 C5SX C 0.4605(11) 0.1551(8) 0.8366(8) 0.074(2) Uiso 0.430(6) 1 d PDU C 2 C6SX C 0.4039(15) 0.0881(10) 0.9060(11) 0.133(7) Uani 0.430(6) 1 d PDU C 2 H6S4 H 0.3542 0.1105 0.9390 0.199 Uiso 0.430(6) 1 calc PR C 2 H6S5 H 0.4518 0.0450 0.9386 0.199 Uiso 0.430(6) 1 calc PR C 2 H6S6 H 0.3698 0.0663 0.8848 0.199 Uiso 0.430(6) 1 calc PR C 2 C8S C 0.8764(11) 0.0456(10) 0.8271(11) 0.113(5) Uani 0.50 1 d PDU D 1 H8S1 H 0.8913 0.0484 0.8719 0.170 Uiso 0.50 1 calc PR D 1 H8S2 H 0.8164 0.0200 0.8446 0.170 Uiso 0.50 1 calc PR D 1 H8S3 H 0.8644 0.1002 0.7837 0.170 Uiso 0.50 1 calc PR D 1 C7S C 0.9582(10) 0.0001(9) 0.8000(10) 0.085(3) Uani 0.50 1 d PDU D 1 N4S N 1.0272(10) -0.0342(7) 0.7722(8) 0.082(3) Uani 0.50 1 d PDU D 1 O1SY O 1.0898(10) -0.1098(7) 0.8509(7) 0.139(4) Uani 0.50 1 d PDU E 2 C9SY C 1.1342(10) 0.0121(8) 0.7574(9) 0.097(4) Uani 0.50 1 d PDU E 2 H9S1 H 1.1196 0.0508 0.7790 0.145 Uiso 0.50 1 calc PR E 2 H9S2 H 1.1283 0.0410 0.7007 0.145 Uiso 0.50 1 calc PR E 2 H9S3 H 1.2026 -0.0171 0.7636 0.145 Uiso 0.50 1 calc PR E 2 C7SY C 1.0623(11) -0.0454(9) 0.8008(10) 0.090(3) Uani 0.50 1 d PDU E 2 C8SY C 0.9674(13) -0.0209(11) 0.7645(11) 0.105(4) Uani 0.50 1 d PDU E 2 H8S4 H 0.9401 -0.0693 0.7793 0.158 Uiso 0.50 1 calc PR E 2 H8S5 H 0.9839 0.0084 0.7062 0.158 Uiso 0.50 1 calc PR E 2 H8S6 H 0.9173 0.0138 0.7846 0.158 Uiso 0.50 1 calc PR E 2 O1S O 0.3148(6) 0.8950(4) 0.8431(5) 0.0232(12) Uani 0.50 1 d PU F 1 N5SX N 0.3673(9) 0.8702(7) 0.8329(7) 0.077(3) Uani 0.50 1 d PDU G 2 C9SX C 0.3101(14) 0.9186(10) 0.8450(13) 0.073(4) Uani 0.50 1 d PDU G 2 C10X C 0.2486(13) 0.9809(10) 0.8650(12) 0.128(5) Uani 0.50 1 d PDU G 2 H10D H 0.2048 0.9563 0.9164 0.191 Uiso 0.50 1 calc PR G 2 H10E H 0.2073 1.0175 0.8236 0.191 Uiso 0.50 1 calc PR G 2 H10F H 0.2918 1.0113 0.8686 0.191 Uiso 0.50 1 calc PRU G 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 C1 0.0112(13) 0.0164(14) 0.0166(14) -0.0087(12) -0.0016(11) 0.0008(11) C2 0.0149(14) 0.0155(14) 0.0148(14) -0.0056(12) -0.0052(11) -0.0004(11) C3 0.0120(14) 0.0155(14) 0.0181(14) -0.0087(12) -0.0018(11) -0.0011(11) C4 0.0119(14) 0.0163(14) 0.0164(14) -0.0082(12) -0.0015(11) -0.0005(11) C5 0.0144(15) 0.0215(16) 0.0238(16) -0.0107(13) -0.0043(12) -0.0002(12) C6 0.0160(16) 0.034(2) 0.0241(17) -0.0070(15) -0.0009(13) -0.0018(14) C7 0.0119(14) 0.0157(14) 0.0180(14) -0.0079(12) -0.0025(11) -0.0003(11) C8 0.0141(14) 0.0145(14) 0.0168(14) -0.0068(12) 0.0002(11) -0.0020(11) C9 0.0130(14) 0.0155(14) 0.0185(14) -0.0098(12) -0.0004(11) -0.0014(11) C10 0.0115(14) 0.0132(14) 0.0176(14) -0.0073(12) -0.0009(11) -0.0013(11) C11 0.0121(14) 0.0203(15) 0.0219(15) -0.0107(13) 0.0005(12) 0.0000(11) C12 0.0137(15) 0.0336(19) 0.045(2) -0.0241(17) -0.0002(15) -0.0040(14) C13 0.0208(15) 0.0180(15) 0.0165(14) -0.0055(12) -0.0017(12) -0.0072(12) C14 0.0217(16) 0.0201(16) 0.0144(14) -0.0027(12) -0.0038(12) -0.0055(12) C15 0.0184(15) 0.0205(15) 0.0187(15) -0.0084(13) -0.0030(12) -0.0046(12) C16 0.0188(15) 0.0204(16) 0.0191(15) -0.0062(13) -0.0020(12) -0.0080(12) C17 0.0191(15) 0.0163(15) 0.0160(14) -0.0065(12) -0.0020(12) -0.0053(12) C18 0.0198(15) 0.0147(14) 0.0165(14) -0.0076(12) -0.0041(12) -0.0029(11) C19 0.0193(15) 0.0201(16) 0.0206(15) -0.0064(13) -0.0035(12) -0.0077(12) C20 0.0200(16) 0.0152(15) 0.0211(16) -0.0058(13) -0.0005(12) -0.0054(12) C21 0.0219(16) 0.0116(14) 0.0178(15) -0.0038(12) -0.0027(12) -0.0022(12) C22 0.0172(15) 0.0133(14) 0.0175(14) -0.0077(12) -0.0022(12) -0.0002(11) C23 0.0196(16) 0.0288(18) 0.0170(15) -0.0069(14) -0.0037(12) -0.0082(13) C24 0.0256(18) 0.0338(19) 0.0215(17) -0.0061(15) -0.0100(14) -0.0053(15) C25 0.0313(19) 0.037(2) 0.0261(18) -0.0148(16) -0.0106(15) -0.0079(15) C26 0.0210(17) 0.047(2) 0.0231(17) -0.0112(16) -0.0035(14) -0.0087(16) C27 0.0232(17) 0.0208(17) 0.0262(17) -0.0017(14) -0.0021(14) -0.0104(13) C28 0.042(3) 0.031(2) 0.085(4) -0.027(2) 0.013(2) -0.0195(19) C29 0.025(2) 0.044(3) 0.063(3) 0.006(2) 0.003(2) -0.0139(19) C30 0.059(3) 0.082(4) 0.042(3) -0.027(3) 0.019(2) -0.045(3) C31 0.0247(17) 0.0168(15) 0.0226(16) -0.0110(13) 0.0036(13) -0.0028(12) C32 0.0287(18) 0.0154(15) 0.0262(17) -0.0101(14) 0.0027(14) -0.0053(13) C33 0.0209(16) 0.0170(15) 0.0192(15) -0.0055(13) -0.0007(13) -0.0016(12) C34 0.0202(16) 0.0169(15) 0.0184(15) -0.0076(13) 0.0008(12) 0.0000(12) C35 0.0203(15) 0.0146(14) 0.0151(14) -0.0063(12) -0.0037(12) 0.0003(11) C36 0.0210(15) 0.0151(14) 0.0139(14) -0.0055(12) -0.0016(12) -0.0021(12) C37 0.0211(16) 0.0201(16) 0.0188(15) -0.0109(13) 0.0005(12) -0.0017(12) C38 0.0223(16) 0.0189(15) 0.0205(15) -0.0117(13) -0.0038(13) 0.0001(12) C39 0.0253(16) 0.0157(15) 0.0194(15) -0.0098(13) -0.0037(13) -0.0023(12) C40 0.0210(15) 0.0168(15) 0.0153(14) -0.0066(12) -0.0013(12) -0.0039(12) C41 0.0259(18) 0.0141(16) 0.037(2) -0.0068(15) 0.0083(15) -0.0031(13) C42 0.0270(19) 0.0199(18) 0.048(2) -0.0063(17) 0.0058(17) -0.0060(14) C43 0.025(2) 0.025(2) 0.095(4) -0.010(2) 0.003(2) 0.0004(16) C44 0.077(3) 0.033(2) 0.033(2) -0.0120(19) 0.018(2) -0.020(2) C45 0.0227(17) 0.0271(18) 0.046(2) -0.0280(17) 0.0037(15) -0.0025(14) C46 0.0253(19) 0.034(2) 0.056(3) -0.031(2) -0.0104(17) 0.0080(15) C47 0.025(2) 0.093(4) 0.058(3) -0.065(3) 0.0030(19) -0.003(2) C48 0.039(3) 0.037(3) 0.122(5) -0.052(3) 0.025(3) -0.008(2) C49 0.0215(16) 0.0169(15) 0.0176(15) -0.0087(12) -0.0065(12) 0.0011(12) C50 0.0234(16) 0.0201(15) 0.0162(14) -0.0115(13) -0.0066(12) 0.0005(12) C51 0.0195(15) 0.0164(15) 0.0196(15) -0.0101(12) -0.0041(12) -0.0004(12) C52 0.0173(15) 0.0188(15) 0.0172(15) -0.0085(12) -0.0066(12) 0.0021(12) C53 0.0151(14) 0.0138(14) 0.0151(14) -0.0061(12) -0.0041(11) -0.0013(11) C54 0.0176(14) 0.0112(13) 0.0141(14) -0.0054(11) -0.0029(11) -0.0024(11) C55 0.0139(14) 0.0196(15) 0.0187(15) -0.0100(13) -0.0042(12) 0.0013(11) C56 0.0155(15) 0.0252(16) 0.0150(14) -0.0091(13) -0.0010(12) -0.0052(12) C57 0.0188(15) 0.0205(15) 0.0142(14) -0.0093(12) -0.0007(12) -0.0052(12) C58 0.0161(14) 0.0149(14) 0.0156(14) -0.0078(12) 0.0000(11) -0.0028(11) C59 0.0198(16) 0.0244(17) 0.0280(17) -0.0193(14) -0.0075(13) 0.0050(13) C60 0.0244(18) 0.039(2) 0.036(2) -0.0299(17) -0.0099(15) 0.0085(15) C61 0.0211(17) 0.037(2) 0.037(2) -0.0269(17) -0.0055(15) 0.0017(14) C62 0.0298(18) 0.0212(17) 0.0337(19) -0.0147(15) -0.0115(15) 0.0065(14) C63 0.0166(16) 0.050(2) 0.0205(16) -0.0218(16) -0.0045(13) 0.0007(15) C64 0.0172(17) 0.079(3) 0.034(2) -0.037(2) -0.0014(15) -0.0077(18) C65 0.039(2) 0.044(2) 0.0263(19) -0.0094(18) -0.0159(17) 0.0112(18) C66 0.0180(17) 0.068(3) 0.0287(19) -0.032(2) -0.0077(14) 0.0011(17) Cl1 0.0154(3) 0.0146(3) 0.0139(3) -0.0067(3) 0.0011(3) -0.0048(3) Cl2 0.0222(4) 0.0191(4) 0.0231(4) -0.0140(3) 0.0018(3) -0.0027(3) Cl3 0.0193(4) 0.0127(3) 0.0157(3) -0.0067(3) -0.0013(3) 0.0014(3) Cl4 0.0237(4) 0.0251(4) 0.0169(4) -0.0091(3) -0.0053(3) -0.0004(3) Cl5 0.0192(3) 0.0158(3) 0.0169(3) -0.0084(3) -0.0070(3) 0.0007(3) Cl6 0.0201(4) 0.0164(3) 0.0211(4) -0.0064(3) -0.0022(3) -0.0059(3) Cr1 0.0132(2) 0.0119(2) 0.0120(2) -0.00585(18) -0.00080(17) -0.00301(17) Cr2 0.0157(2) 0.0118(2) 0.0123(2) -0.00592(19) -0.00004(18) -0.00053(18) Cr3 0.0140(2) 0.0109(2) 0.0124(2) -0.00550(18) -0.00325(18) -0.00054(17) Cr4 0.0112(2) 0.0109(2) 0.0118(2) -0.00568(18) -0.00087(17) -0.00076(17) N1 0.0176(13) 0.0149(12) 0.0146(12) -0.0071(10) -0.0018(10) -0.0037(10) N2 0.0163(12) 0.0136(12) 0.0162(12) -0.0074(10) -0.0007(10) -0.0036(10) N3 0.0218(13) 0.0149(12) 0.0161(12) -0.0078(10) 0.0000(10) -0.0016(10) N4 0.0206(13) 0.0140(12) 0.0120(12) -0.0054(10) -0.0026(10) -0.0020(10) N5 0.0177(13) 0.0119(12) 0.0141(12) -0.0054(10) -0.0044(10) -0.0008(9) N6 0.0163(12) 0.0126(12) 0.0130(12) -0.0046(10) -0.0029(10) -0.0031(9) O1 0.0117(10) 0.0130(10) 0.0145(10) -0.0074(8) -0.0015(8) -0.0002(8) O2 0.0129(10) 0.0148(10) 0.0135(10) -0.0068(8) -0.0010(8) -0.0009(8) O3 0.0117(10) 0.0123(10) 0.0140(10) -0.0054(8) -0.0011(8) -0.0017(8) O4 0.0118(10) 0.0142(10) 0.0139(10) -0.0072(8) -0.0011(8) -0.0013(8) O5 0.0125(10) 0.0122(10) 0.0145(10) -0.0053(8) -0.0004(8) -0.0018(8) O6 0.0135(10) 0.0129(10) 0.0154(10) -0.0071(8) -0.0004(8) -0.0020(8) N1S 0.092(6) 0.097(6) 0.080(6) -0.045(5) -0.007(4) -0.006(5) C1S 0.087(6) 0.070(6) 0.067(6) -0.043(5) -0.002(4) -0.004(5) C2S 0.095(6) 0.065(6) 0.069(6) -0.055(5) -0.008(5) -0.002(5) N1SX 0.144(9) 0.139(9) 0.160(10) -0.057(7) -0.014(7) -0.024(7) C1SX 0.120(7) 0.107(8) 0.119(8) -0.044(6) -0.007(6) 0.000(6) C2SX 0.114(8) 0.084(7) 0.083(7) -0.055(6) -0.017(6) 0.008(6) N2S 0.121(8) 0.120(8) 0.122(8) -0.050(6) -0.015(6) -0.018(6) C3S 0.098(7) 0.082(6) 0.096(7) -0.030(5) -0.028(5) -0.027(5) C4S 0.080(6) 0.067(7) 0.065(6) -0.014(5) -0.038(5) -0.029(5) N2SX 0.098(7) 0.091(7) 0.153(9) -0.021(6) -0.005(6) -0.044(5) C3SX 0.057(5) 0.061(5) 0.093(6) -0.015(5) -0.010(5) -0.010(4) C4SX 0.071(6) 0.059(6) 0.057(5) -0.025(5) -0.023(5) -0.014(4) C6S 0.154(9) 0.110(8) 0.146(9) -0.074(7) 0.012(7) 0.005(7) C6SX 0.124(10) 0.126(9) 0.126(9) -0.057(7) -0.007(8) 0.003(8) C8S 0.110(8) 0.104(8) 0.141(9) -0.070(7) -0.005(6) -0.025(6) C7S 0.086(6) 0.080(5) 0.106(6) -0.047(5) -0.013(5) -0.031(4) N4S 0.108(7) 0.060(5) 0.083(6) -0.035(4) 0.002(5) -0.037(5) O1SY 0.144(7) 0.115(6) 0.108(7) -0.029(5) -0.010(5) 0.003(5) C9SY 0.090(7) 0.108(7) 0.097(7) -0.050(5) -0.016(6) -0.015(5) C7SY 0.094(5) 0.082(5) 0.104(6) -0.051(4) -0.014(5) -0.012(4) C8SY 0.109(7) 0.104(7) 0.108(7) -0.043(5) -0.018(6) -0.036(6) O1S 0.025(3) 0.011(3) 0.032(3) -0.002(3) -0.017(2) -0.004(2) N5SX 0.082(6) 0.068(5) 0.074(6) -0.015(4) -0.007(5) -0.042(4) C9SX 0.064(5) 0.061(6) 0.071(6) -0.003(5) -0.008(4) -0.033(5) C10X 0.116(8) 0.105(7) 0.148(8) -0.053(6) -0.002(7) -0.025(6) _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 C1 O1 1.434(3) . ? C1 C4 1.541(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.428(3) . ? C2 C4 1.545(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.434(3) . ? C3 C4 1.537(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.559(4) . ? C5 C6 1.513(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O4 1.421(3) . ? C7 C10 1.539(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O5 1.421(3) . ? C8 C10 1.545(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O6 1.420(3) . ? C9 C10 1.548(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.550(4) . ? C11 C12 1.519(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N1 1.349(4) . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.407(4) . ? C15 C23 1.524(4) . ? C16 C17 1.374(4) . ? C16 H16 0.9500 . ? C17 N1 1.354(4) . ? C17 C18 1.483(4) . ? C18 N2 1.348(4) . ? C18 C19 1.385(4) . ? C19 C20 1.398(4) . ? C19 H19 0.9500 . ? C20 C21 1.391(4) . ? C20 C27 1.528(4) . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 N2 1.344(4) . ? C22 H22 0.9500 . ? C23 C24 1.530(5) . ? C23 C25 1.537(5) . ? C23 C26 1.538(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.494(5) . ? C27 C29 1.507(5) . ? C27 C30 1.557(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N3 1.342(4) . ? C31 C32 1.381(5) . ? C31 H31 0.9500 . ? C32 C33 1.388(5) . ? C32 H32 0.9500 . ? C33 C34 1.399(4) . ? C33 C41 1.522(4) . ? C34 C35 1.383(4) . ? C34 H34 0.9500 . ? C35 N3 1.356(4) . ? C35 C36 1.484(4) . ? C36 N4 1.355(4) . ? C36 C37 1.381(4) . ? C37 C38 1.403(4) . ? C37 H37 0.9500 . ? C38 C39 1.391(5) . ? C38 C45 1.523(4) . ? C39 C40 1.380(4) . ? C39 H39 0.9500 . ? C40 N4 1.340(4) . ? C40 H40 0.9500 . ? C41 C43 1.511(6) . ? C41 C42 1.522(5) . ? C41 C44 1.548(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48 1.527(6) . ? C45 C46 1.530(5) . ? C45 C47 1.554(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N5 1.333(4) . ? C49 C50 1.386(4) . ? C49 H49 0.9500 . ? C50 C51 1.390(4) . ? C50 H50 0.9500 . ? C51 C52 1.402(4) . ? C51 C59 1.516(4) . ? C52 C53 1.382(4) . ? C52 H52 0.9500 . ? C53 N5 1.362(4) . ? C53 C54 1.475(4) . ? C54 N6 1.357(4) . ? C54 C55 1.386(4) . ? C55 C56 1.398(4) . ? C55 H55 0.9500 . ? C56 C57 1.395(4) . ? C56 C63 1.528(4) . ? C57 C58 1.387(4) . ? C57 H57 0.9500 . ? C58 N6 1.331(4) . ? C58 H58 0.9500 . ? C59 C62 1.538(5) . ? C59 C61 1.537(5) . ? C59 C60 1.538(4) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C66 1.534(5) . ? C63 C64 1.533(5) . ? C63 C65 1.549(6) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? Cl1 Cr1 2.3204(8) . ? Cl2 Cr1 2.3246(8) . ? Cl3 Cr2 2.3304(8) . ? Cl4 Cr2 2.3243(9) . ? Cl5 Cr3 2.3237(8) . ? Cl6 Cr3 2.3163(8) . ? Cr1 O1 1.956(2) . ? Cr1 O4 1.994(2) . ? Cr1 N2 2.064(2) . ? Cr1 N1 2.078(3) . ? Cr2 O2 1.955(2) . ? Cr2 O5 2.009(2) . ? Cr2 N4 2.061(3) . ? Cr2 N3 2.083(3) . ? Cr3 O3 1.959(2) . ? Cr3 O6 2.013(2) . ? Cr3 N6 2.066(2) . ? Cr3 N5 2.084(2) . ? Cr4 O2 1.943(2) . ? Cr4 O3 1.951(2) . ? Cr4 O1 1.952(2) . ? Cr4 O4 1.963(2) . ? Cr4 O6 1.965(2) . ? Cr4 O5 1.969(2) . ? N1S C1S 1.180(12) . ? C1S C2S 1.403(15) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? N1SX C1SX 1.156(10) . ? C1SX C2SX 1.461(11) . ? C2SX H2S4 0.9800 . ? C2SX H2S5 0.9800 . ? C2SX H2S6 0.9800 . ? N2S C3S 1.162(10) . ? C3S C4S 1.447(10) . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? N2SX C3SX 1.147(9) . ? C3SX C4SX 1.444(10) . ? C4SX H4S4 0.9800 . ? C4SX H4S5 0.9800 . ? C4SX H4S6 0.9800 . ? N3S C5S 1.154(8) . ? C5S C6S 1.555(10) . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? N3SX C5SX 1.077(9) . ? C5SX C6SX 1.537(10) . ? C6SX H6S4 0.9800 . ? C6SX H6S5 0.9800 . ? C6SX H6S6 0.9800 . ? C8S C7S 1.403(10) . ? C8S H8S1 0.9800 . ? C8S H8S2 0.9800 . ? C8S H8S3 0.9800 . ? C7S N4S 1.185(10) . ? O1SY C7SY 1.184(14) . ? C9SY C7SY 1.468(14) . ? C9SY H9S1 0.9800 . ? C9SY H9S2 0.9800 . ? C9SY H9S3 0.9800 . ? C7SY C8SY 1.527(14) . ? C8SY H8S4 0.9800 . ? C8SY H8S5 0.9800 . ? C8SY H8S6 0.9800 . ? N5SX C9SX 1.136(10) . ? C9SX C10X 1.444(10) . ? C10X H10D 0.9800 . ? C10X H10E 0.9800 . ? C10X H10F 0.9800 . ? 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 O1 C1 C4 112.9(2) . . ? O1 C1 H1A 109.0 . . ? C4 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C4 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C4 113.8(2) . . ? O2 C2 H2A 108.8 . . ? C4 C2 H2A 108.8 . . ? O2 C2 H2B 108.8 . . ? C4 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? O3 C3 C4 112.9(2) . . ? O3 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? O3 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C1 111.6(2) . . ? C3 C4 C2 111.5(2) . . ? C1 C4 C2 111.9(2) . . ? C3 C4 C5 109.3(2) . . ? C1 C4 C5 108.1(2) . . ? C2 C4 C5 104.1(2) . . ? C6 C5 C4 117.7(3) . . ? C6 C5 H5A 107.9 . . ? C4 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? C4 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C10 113.8(2) . . ? O4 C7 H7A 108.8 . . ? C10 C7 H7A 108.8 . . ? O4 C7 H7B 108.8 . . ? C10 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? O5 C8 C10 113.6(2) . . ? O5 C8 H8A 108.8 . . ? C10 C8 H8A 108.8 . . ? O5 C8 H8B 108.8 . . ? C10 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O6 C9 C10 114.4(2) . . ? O6 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? O6 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C7 C10 C8 112.1(2) . . ? C7 C10 C9 110.9(2) . . ? C8 C10 C9 111.2(2) . . ? C7 C10 C11 107.9(2) . . ? C8 C10 C11 108.8(2) . . ? C9 C10 C11 105.7(2) . . ? C12 C11 C10 116.9(3) . . ? C12 C11 H11A 108.1 . . ? C10 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? C10 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.9(3) . . ? N1 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 116.4(3) . . ? C14 C15 C23 123.5(3) . . ? C16 C15 C23 120.1(3) . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? N1 C17 C16 122.3(3) . . ? N1 C17 C18 114.6(3) . . ? C16 C17 C18 123.1(3) . . ? N2 C18 C19 121.9(3) . . ? N2 C18 C17 114.3(3) . . ? C19 C18 C17 123.8(3) . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 116.5(3) . . ? C21 C20 C27 121.9(3) . . ? C19 C20 C27 121.6(3) . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? N2 C22 C21 122.0(3) . . ? N2 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C15 C23 C24 111.6(3) . . ? C15 C23 C25 107.4(3) . . ? C24 C23 C25 109.4(3) . . ? C15 C23 C26 109.3(3) . . ? C24 C23 C26 108.6(3) . . ? C25 C23 C26 110.6(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 112.8(4) . . ? C28 C27 C20 109.4(3) . . ? C29 C27 C20 112.0(3) . . ? C28 C27 C30 108.8(4) . . ? C29 C27 C30 105.1(4) . . ? C20 C27 C30 108.5(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C32 122.9(3) . . ? N3 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C31 C32 C33 120.5(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C34 116.3(3) . . ? C32 C33 C41 123.4(3) . . ? C34 C33 C41 120.3(3) . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? N3 C35 C34 121.7(3) . . ? N3 C35 C36 114.3(3) . . ? C34 C35 C36 124.0(3) . . ? N4 C36 C37 121.4(3) . . ? N4 C36 C35 114.2(3) . . ? C37 C36 C35 124.4(3) . . ? C36 C37 C38 120.6(3) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 116.6(3) . . ? C39 C38 C45 122.6(3) . . ? C37 C38 C45 120.8(3) . . ? C40 C39 C38 120.2(3) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? N4 C40 C39 122.5(3) . . ? N4 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C43 C41 C42 109.6(4) . . ? C43 C41 C33 108.6(3) . . ? C42 C41 C33 112.6(3) . . ? C43 C41 C44 110.4(4) . . ? C42 C41 C44 107.8(3) . . ? C33 C41 C44 107.9(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C38 C45 C48 112.0(3) . . ? C38 C45 C46 110.4(3) . . ? C48 C45 C46 109.4(4) . . ? C38 C45 C47 107.2(3) . . ? C48 C45 C47 109.5(4) . . ? C46 C45 C47 108.2(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N5 C49 C50 123.3(3) . . ? N5 C49 H49 118.3 . . ? C50 C49 H49 118.3 . . ? C49 C50 C51 120.2(3) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C52 116.1(3) . . ? C50 C51 C59 123.4(3) . . ? C52 C51 C59 120.4(3) . . ? C53 C52 C51 121.0(3) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? N5 C53 C52 121.7(3) . . ? N5 C53 C54 114.2(3) . . ? C52 C53 C54 124.1(3) . . ? N6 C54 C55 121.2(3) . . ? N6 C54 C53 115.0(3) . . ? C55 C54 C53 123.8(3) . . ? C54 C55 C56 120.6(3) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C57 C56 C55 116.8(3) . . ? C57 C56 C63 124.1(3) . . ? C55 C56 C63 119.1(3) . . ? C58 C57 C56 119.9(3) . . ? C58 C57 H57 120.1 . . ? C56 C57 H57 120.1 . . ? N6 C58 C57 122.6(3) . . ? N6 C58 H58 118.7 . . ? C57 C58 H58 118.7 . . ? C51 C59 C62 107.4(3) . . ? C51 C59 C61 110.3(3) . . ? C62 C59 C61 110.4(3) . . ? C51 C59 C60 111.9(3) . . ? C62 C59 C60 108.3(3) . . ? C61 C59 C60 108.6(3) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C56 C63 C66 112.3(3) . . ? C56 C63 C64 108.0(3) . . ? C66 C63 C64 109.7(3) . . ? C56 C63 C65 108.5(3) . . ? C66 C63 C65 108.4(3) . . ? C64 C63 C65 109.9(3) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O1 Cr1 O4 78.83(8) . . ? O1 Cr1 N2 94.44(9) . . ? O4 Cr1 N2 88.51(9) . . ? O1 Cr1 N1 168.93(9) . . ? O4 Cr1 N1 92.83(9) . . ? N2 Cr1 N1 77.93(10) . . ? O1 Cr1 Cl1 94.76(6) . . ? O4 Cr1 Cl1 93.54(6) . . ? N2 Cr1 Cl1 170.80(7) . . ? N1 Cr1 Cl1 92.99(7) . . ? O1 Cr1 Cl2 95.78(6) . . ? O4 Cr1 Cl2 172.79(6) . . ? N2 Cr1 Cl2 87.14(7) . . ? N1 Cr1 Cl2 91.87(7) . . ? Cl1 Cr1 Cl2 91.67(3) . . ? O2 Cr2 O5 78.33(8) . . ? O2 Cr2 N4 96.45(9) . . ? O5 Cr2 N4 87.97(9) . . ? O2 Cr2 N3 170.37(10) . . ? O5 Cr2 N3 93.72(9) . . ? N4 Cr2 N3 77.68(10) . . ? O2 Cr2 Cl4 93.83(6) . . ? O5 Cr2 Cl4 169.80(6) . . ? N4 Cr2 Cl4 86.44(7) . . ? N3 Cr2 Cl4 93.41(8) . . ? O2 Cr2 Cl3 93.21(6) . . ? O5 Cr2 Cl3 95.68(6) . . ? N4 Cr2 Cl3 170.20(7) . . ? N3 Cr2 Cl3 92.98(7) . . ? Cl4 Cr2 Cl3 91.22(3) . . ? O3 Cr3 O6 78.85(8) . . ? O3 Cr3 N6 97.19(9) . . ? O6 Cr3 N6 88.04(9) . . ? O3 Cr3 N5 170.56(9) . . ? O6 Cr3 N5 92.87(9) . . ? N6 Cr3 N5 77.82(10) . . ? O3 Cr3 Cl6 94.13(6) . . ? O6 Cr3 Cl6 170.57(6) . . ? N6 Cr3 Cl6 86.61(7) . . ? N5 Cr3 Cl6 93.57(7) . . ? O3 Cr3 Cl5 92.82(6) . . ? O6 Cr3 Cl5 95.15(6) . . ? N6 Cr3 Cl5 169.92(7) . . ? N5 Cr3 Cl5 92.44(7) . . ? Cl6 Cr3 Cl5 91.44(3) . . ? O2 Cr4 O3 92.16(8) . . ? O2 Cr4 O1 92.99(8) . . ? O3 Cr4 O1 92.19(8) . . ? O2 Cr4 O4 168.45(8) . . ? O3 Cr4 O4 96.99(8) . . ? O1 Cr4 O4 79.69(8) . . ? O2 Cr4 O6 96.36(8) . . ? O3 Cr4 O6 80.21(8) . . ? O1 Cr4 O6 168.14(9) . . ? O4 Cr4 O6 92.14(8) . . ? O2 Cr4 O5 79.61(8) . . ? O3 Cr4 O5 167.89(9) . . ? O1 Cr4 O5 97.05(8) . . ? O4 Cr4 O5 92.36(8) . . ? O6 Cr4 O5 91.81(8) . . ? C13 N1 C17 117.6(3) . . ? C13 N1 Cr1 126.4(2) . . ? C17 N1 Cr1 116.0(2) . . ? C22 N2 C18 118.3(3) . . ? C22 N2 Cr1 124.9(2) . . ? C18 N2 Cr1 116.7(2) . . ? C31 N3 C35 117.7(3) . . ? C31 N3 Cr2 125.9(2) . . ? C35 N3 Cr2 116.4(2) . . ? C40 N4 C36 118.4(3) . . ? C40 N4 Cr2 124.4(2) . . ? C36 N4 Cr2 117.1(2) . . ? C49 N5 C53 117.6(3) . . ? C49 N5 Cr3 126.2(2) . . ? C53 N5 Cr3 116.23(19) . . ? C58 N6 C54 118.8(3) . . ? C58 N6 Cr3 124.7(2) . . ? C54 N6 Cr3 116.53(19) . . ? C1 O1 Cr4 117.40(16) . . ? C1 O1 Cr1 127.67(17) . . ? Cr4 O1 Cr1 101.58(9) . . ? C2 O2 Cr4 117.01(16) . . ? C2 O2 Cr2 126.98(17) . . ? Cr4 O2 Cr2 102.40(9) . . ? C3 O3 Cr4 117.46(16) . . ? C3 O3 Cr3 127.93(17) . . ? Cr4 O3 Cr3 101.63(9) . . ? C7 O4 Cr4 117.34(17) . . ? C7 O4 Cr1 131.45(17) . . ? Cr4 O4 Cr1 99.82(9) . . ? C8 O5 Cr4 117.32(17) . . ? C8 O5 Cr2 131.84(17) . . ? Cr4 O5 Cr2 99.59(9) . . ? C9 O6 Cr4 116.75(16) . . ? C9 O6 Cr3 132.08(17) . . ? Cr4 O6 Cr3 99.25(9) . . ? N1S C1S C2S 176.6(15) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N1SX C1SX C2SX 167(3) . . ? C1SX C2SX H2S4 109.5 . . ? C1SX C2SX H2S5 109.5 . . ? H2S4 C2SX H2S5 109.5 . . ? C1SX C2SX H2S6 109.5 . . ? H2S4 C2SX H2S6 109.5 . . ? H2S5 C2SX H2S6 109.5 . . ? N2S C3S C4S 173(2) . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N2SX C3SX C4SX 178.0(19) . . ? C3SX C4SX H4S4 109.5 . . ? C3SX C4SX H4S5 109.5 . . ? H4S4 C4SX H4S5 109.5 . . ? C3SX C4SX H4S6 109.5 . . ? H4S4 C4SX H4S6 109.5 . . ? H4S5 C4SX H4S6 109.5 . . ? N3S C5S C6S 155.5(12) . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? N3SX C5SX C6SX 170.4(17) . . ? C5SX C6SX H6S4 109.5 . . ? C5SX C6SX H6S5 109.5 . . ? H6S4 C6SX H6S5 109.5 . . ? C5SX C6SX H6S6 109.5 . . ? H6S4 C6SX H6S6 109.5 . . ? H6S5 C6SX H6S6 109.5 . . ? C7S C8S H8S1 109.5 . . ? C7S C8S H8S2 109.5 . . ? H8S1 C8S H8S2 109.5 . . ? C7S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? N4S C7S C8S 175.7(19) . . ? C7SY C9SY H9S1 109.5 . . ? C7SY C9SY H9S2 109.5 . . ? H9S1 C9SY H9S2 109.5 . . ? C7SY C9SY H9S3 109.5 . . ? H9S1 C9SY H9S3 109.5 . . ? H9S2 C9SY H9S3 109.5 . . ? O1SY C7SY C9SY 117.6(13) . . ? O1SY C7SY C8SY 126.4(14) . . ? C9SY C7SY C8SY 114.8(12) . . ? C7SY C8SY H8S4 109.5 . . ? C7SY C8SY H8S5 109.5 . . ? H8S4 C8SY H8S5 109.5 . . ? C7SY C8SY H8S6 109.5 . . ? H8S4 C8SY H8S6 109.5 . . ? H8S5 C8SY H8S6 109.5 . . ? N5SX C9SX C10X 172(2) . . ? C9SX C10X H10D 109.5 . . ? C9SX C10X H10E 109.5 . . ? H10D C10X H10E 109.5 . . ? C9SX C10X H10F 109.5 . . ? H10D C10X H10F 109.5 . . ? H10E C10X H10F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 C3 C4 C1 67.3(3) . . . . ? O3 C3 C4 C2 -58.6(3) . . . . ? O3 C3 C4 C5 -173.2(2) . . . . ? O1 C1 C4 C3 -59.9(3) . . . . ? O1 C1 C4 C2 65.8(3) . . . . ? O1 C1 C4 C5 179.9(2) . . . . ? O2 C2 C4 C3 66.3(3) . . . . ? O2 C2 C4 C1 -59.5(3) . . . . ? O2 C2 C4 C5 -176.0(2) . . . . ? C3 C4 C5 C6 -59.3(4) . . . . ? C1 C4 C5 C6 62.4(4) . . . . ? C2 C4 C5 C6 -178.5(3) . . . . ? O4 C7 C10 C8 -59.0(3) . . . . ? O4 C7 C10 C9 65.9(3) . . . . ? O4 C7 C10 C11 -178.8(2) . . . . ? O5 C8 C10 C7 65.9(3) . . . . ? O5 C8 C10 C9 -58.8(3) . . . . ? O5 C8 C10 C11 -174.9(2) . . . . ? O6 C9 C10 C7 -59.7(3) . . . . ? O6 C9 C10 C8 65.7(3) . . . . ? O6 C9 C10 C11 -176.4(2) . . . . ? C7 C10 C11 C12 67.5(3) . . . . ? C8 C10 C11 C12 -54.3(4) . . . . ? C9 C10 C11 C12 -173.8(3) . . . . ? N1 C13 C14 C15 -0.7(5) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? C13 C14 C15 C23 -178.4(3) . . . . ? C14 C15 C16 C17 0.7(5) . . . . ? C23 C15 C16 C17 179.7(3) . . . . ? C15 C16 C17 N1 -1.8(5) . . . . ? C15 C16 C17 C18 179.9(3) . . . . ? N1 C17 C18 N2 -7.3(4) . . . . ? C16 C17 C18 N2 171.2(3) . . . . ? N1 C17 C18 C19 171.2(3) . . . . ? C16 C17 C18 C19 -10.3(5) . . . . ? N2 C18 C19 C20 -1.9(5) . . . . ? C17 C18 C19 C20 179.8(3) . . . . ? C18 C19 C20 C21 -4.7(5) . . . . ? C18 C19 C20 C27 175.1(3) . . . . ? C19 C20 C21 C22 6.3(5) . . . . ? C27 C20 C21 C22 -173.4(3) . . . . ? C20 C21 C22 N2 -1.6(5) . . . . ? C14 C15 C23 C24 -12.7(5) . . . . ? C16 C15 C23 C24 168.4(3) . . . . ? C14 C15 C23 C25 107.2(4) . . . . ? C16 C15 C23 C25 -71.7(4) . . . . ? C14 C15 C23 C26 -132.8(3) . . . . ? C16 C15 C23 C26 48.3(4) . . . . ? C21 C20 C27 C28 -74.0(4) . . . . ? C19 C20 C27 C28 106.2(4) . . . . ? C21 C20 C27 C29 160.0(4) . . . . ? C19 C20 C27 C29 -19.7(5) . . . . ? C21 C20 C27 C30 44.5(5) . . . . ? C19 C20 C27 C30 -135.3(4) . . . . ? N3 C31 C32 C33 0.9(5) . . . . ? C31 C32 C33 C34 -0.4(5) . . . . ? C31 C32 C33 C41 -179.8(3) . . . . ? C32 C33 C34 C35 -0.6(5) . . . . ? C41 C33 C34 C35 178.8(3) . . . . ? C33 C34 C35 N3 1.1(5) . . . . ? C33 C34 C35 C36 -177.3(3) . . . . ? N3 C35 C36 N4 -4.2(4) . . . . ? C34 C35 C36 N4 174.3(3) . . . . ? N3 C35 C36 C37 176.1(3) . . . . ? C34 C35 C36 C37 -5.5(5) . . . . ? N4 C36 C37 C38 -1.2(5) . . . . ? C35 C36 C37 C38 178.6(3) . . . . ? C36 C37 C38 C39 -3.5(5) . . . . ? C36 C37 C38 C45 178.1(3) . . . . ? C37 C38 C39 C40 4.6(5) . . . . ? C45 C38 C39 C40 -177.1(3) . . . . ? C38 C39 C40 N4 -1.0(5) . . . . ? C32 C33 C41 C43 -123.7(4) . . . . ? C34 C33 C41 C43 56.9(5) . . . . ? C32 C33 C41 C42 -2.2(5) . . . . ? C34 C33 C41 C42 178.4(3) . . . . ? C32 C33 C41 C44 116.6(4) . . . . ? C34 C33 C41 C44 -62.8(4) . . . . ? C39 C38 C45 C48 16.2(5) . . . . ? C37 C38 C45 C48 -165.6(4) . . . . ? C39 C38 C45 C46 138.4(3) . . . . ? C37 C38 C45 C46 -43.3(5) . . . . ? C39 C38 C45 C47 -104.0(4) . . . . ? C37 C38 C45 C47 74.3(4) . . . . ? N5 C49 C50 C51 0.3(5) . . . . ? C49 C50 C51 C52 -0.6(5) . . . . ? C49 C50 C51 C59 -177.7(3) . . . . ? C50 C51 C52 C53 0.0(5) . . . . ? C59 C51 C52 C53 177.2(3) . . . . ? C51 C52 C53 N5 1.0(5) . . . . ? C51 C52 C53 C54 -177.6(3) . . . . ? N5 C53 C54 N6 -0.8(4) . . . . ? C52 C53 C54 N6 177.9(3) . . . . ? N5 C53 C54 C55 179.4(3) . . . . ? C52 C53 C54 C55 -1.9(5) . . . . ? N6 C54 C55 C56 -1.2(5) . . . . ? C53 C54 C55 C56 178.6(3) . . . . ? C54 C55 C56 C57 -2.2(4) . . . . ? C54 C55 C56 C63 177.5(3) . . . . ? C55 C56 C57 C58 3.0(4) . . . . ? C63 C56 C57 C58 -176.7(3) . . . . ? C56 C57 C58 N6 -0.5(5) . . . . ? C50 C51 C59 C62 109.4(3) . . . . ? C52 C51 C59 C62 -67.6(4) . . . . ? C50 C51 C59 C61 -130.3(3) . . . . ? C52 C51 C59 C61 52.7(4) . . . . ? C50 C51 C59 C60 -9.3(5) . . . . ? C52 C51 C59 C60 173.7(3) . . . . ? C57 C56 C63 C66 2.8(5) . . . . ? C55 C56 C63 C66 -176.8(3) . . . . ? C57 C56 C63 C64 123.9(3) . . . . ? C55 C56 C63 C64 -55.8(4) . . . . ? C57 C56 C63 C65 -117.0(3) . . . . ? C55 C56 C63 C65 63.3(4) . . . . ? C14 C13 N1 C17 -0.3(5) . . . . ? C14 C13 N1 Cr1 177.0(2) . . . . ? C16 C17 N1 C13 1.5(4) . . . . ? C18 C17 N1 C13 -180.0(3) . . . . ? C16 C17 N1 Cr1 -176.1(2) . . . . ? C18 C17 N1 Cr1 2.4(3) . . . . ? O1 Cr1 N1 C13 137.1(4) . . . . ? O4 Cr1 N1 C13 96.3(3) . . . . ? N2 Cr1 N1 C13 -175.8(3) . . . . ? Cl1 Cr1 N1 C13 2.6(3) . . . . ? Cl2 Cr1 N1 C13 -89.1(2) . . . . ? O1 Cr1 N1 C17 -45.5(6) . . . . ? O4 Cr1 N1 C17 -86.3(2) . . . . ? N2 Cr1 N1 C17 1.6(2) . . . . ? Cl1 Cr1 N1 C17 -180.0(2) . . . . ? Cl2 Cr1 N1 C17 88.2(2) . . . . ? C21 C22 N2 C18 -5.1(4) . . . . ? C21 C22 N2 Cr1 171.2(2) . . . . ? C19 C18 N2 C22 6.8(4) . . . . ? C17 C18 N2 C22 -174.7(3) . . . . ? C19 C18 N2 Cr1 -169.8(2) . . . . ? C17 C18 N2 Cr1 8.7(3) . . . . ? O1 Cr1 N2 C22 -10.2(2) . . . . ? O4 Cr1 N2 C22 -88.9(2) . . . . ? N1 Cr1 N2 C22 177.9(3) . . . . ? Cl1 Cr1 N2 C22 168.1(3) . . . . ? Cl2 Cr1 N2 C22 85.4(2) . . . . ? O1 Cr1 N2 C18 166.1(2) . . . . ? O4 Cr1 N2 C18 87.4(2) . . . . ? N1 Cr1 N2 C18 -5.8(2) . . . . ? Cl1 Cr1 N2 C18 -15.6(6) . . . . ? Cl2 Cr1 N2 C18 -98.3(2) . . . . ? C32 C31 N3 C35 -0.5(5) . . . . ? C32 C31 N3 Cr2 177.8(3) . . . . ? C34 C35 N3 C31 -0.5(5) . . . . ? C36 C35 N3 C31 178.0(3) . . . . ? C34 C35 N3 Cr2 -179.0(2) . . . . ? C36 C35 N3 Cr2 -0.5(3) . . . . ? O2 Cr2 N3 C31 131.7(5) . . . . ? O5 Cr2 N3 C31 97.7(3) . . . . ? N4 Cr2 N3 C31 -175.2(3) . . . . ? Cl4 Cr2 N3 C31 -89.6(3) . . . . ? Cl3 Cr2 N3 C31 1.8(3) . . . . ? O2 Cr2 N3 C35 -50.0(7) . . . . ? O5 Cr2 N3 C35 -84.0(2) . . . . ? N4 Cr2 N3 C35 3.1(2) . . . . ? Cl4 Cr2 N3 C35 88.7(2) . . . . ? Cl3 Cr2 N3 C35 -179.9(2) . . . . ? C39 C40 N4 C36 -3.8(4) . . . . ? C39 C40 N4 Cr2 174.2(2) . . . . ? C37 C36 N4 C40 4.9(4) . . . . ? C35 C36 N4 C40 -174.9(3) . . . . ? C37 C36 N4 Cr2 -173.3(2) . . . . ? C35 C36 N4 Cr2 7.0(3) . . . . ? O2 Cr2 N4 C40 -11.3(2) . . . . ? O5 Cr2 N4 C40 -89.3(2) . . . . ? N3 Cr2 N4 C40 176.4(3) . . . . ? Cl4 Cr2 N4 C40 82.2(2) . . . . ? Cl3 Cr2 N4 C40 158.6(3) . . . . ? O2 Cr2 N4 C36 166.7(2) . . . . ? O5 Cr2 N4 C36 88.7(2) . . . . ? N3 Cr2 N4 C36 -5.6(2) . . . . ? Cl4 Cr2 N4 C36 -99.8(2) . . . . ? Cl3 Cr2 N4 C36 -23.4(6) . . . . ? C50 C49 N5 C53 0.7(5) . . . . ? C50 C49 N5 Cr3 -178.8(2) . . . . ? C52 C53 N5 C49 -1.3(4) . . . . ? C54 C53 N5 C49 177.4(3) . . . . ? C52 C53 N5 Cr3 178.3(2) . . . . ? C54 C53 N5 Cr3 -3.0(3) . . . . ? O3 Cr3 N5 C49 124.8(5) . . . . ? O6 Cr3 N5 C49 96.2(3) . . . . ? N6 Cr3 N5 C49 -176.4(3) . . . . ? Cl6 Cr3 N5 C49 -90.7(2) . . . . ? Cl5 Cr3 N5 C49 0.9(2) . . . . ? O3 Cr3 N5 C53 -54.8(6) . . . . ? O6 Cr3 N5 C53 -83.3(2) . . . . ? N6 Cr3 N5 C53 4.0(2) . . . . ? Cl6 Cr3 N5 C53 89.8(2) . . . . ? Cl5 Cr3 N5 C53 -178.6(2) . . . . ? C57 C58 N6 C54 -3.0(4) . . . . ? C57 C58 N6 Cr3 176.7(2) . . . . ? C55 C54 N6 C58 3.8(4) . . . . ? C53 C54 N6 C58 -176.1(3) . . . . ? C55 C54 N6 Cr3 -175.9(2) . . . . ? C53 C54 N6 Cr3 4.2(3) . . . . ? O3 Cr3 N6 C58 -12.3(2) . . . . ? O6 Cr3 N6 C58 -90.8(2) . . . . ? N5 Cr3 N6 C58 175.9(2) . . . . ? Cl6 Cr3 N6 C58 81.5(2) . . . . ? Cl5 Cr3 N6 C58 160.6(3) . . . . ? O3 Cr3 N6 C54 167.4(2) . . . . ? O6 Cr3 N6 C54 88.9(2) . . . . ? N5 Cr3 N6 C54 -4.5(2) . . . . ? Cl6 Cr3 N6 C54 -98.9(2) . . . . ? Cl5 Cr3 N6 C54 -19.8(6) . . . . ? C4 C1 O1 Cr4 -5.8(3) . . . . ? C4 C1 O1 Cr1 127.5(2) . . . . ? O2 Cr4 O1 C1 -42.73(19) . . . . ? O3 Cr4 O1 C1 49.55(19) . . . . ? O4 Cr4 O1 C1 146.3(2) . . . . ? O6 Cr4 O1 C1 99.3(4) . . . . ? O5 Cr4 O1 C1 -122.62(19) . . . . ? O2 Cr4 O1 Cr1 173.30(9) . . . . ? O3 Cr4 O1 Cr1 -94.42(9) . . . . ? O4 Cr4 O1 Cr1 2.30(8) . . . . ? O6 Cr4 O1 Cr1 -44.7(4) . . . . ? O5 Cr4 O1 Cr1 93.42(9) . . . . ? O4 Cr1 O1 C1 -141.0(2) . . . . ? N2 Cr1 O1 C1 131.4(2) . . . . ? N1 Cr1 O1 C1 177.3(4) . . . . ? Cl1 Cr1 O1 C1 -48.3(2) . . . . ? Cl2 Cr1 O1 C1 43.9(2) . . . . ? O4 Cr1 O1 Cr4 -2.27(8) . . . . ? N2 Cr1 O1 Cr4 -89.86(10) . . . . ? N1 Cr1 O1 Cr4 -43.9(5) . . . . ? Cl1 Cr1 O1 Cr4 90.41(7) . . . . ? Cl2 Cr1 O1 Cr4 -177.43(7) . . . . ? C4 C2 O2 Cr4 -5.3(3) . . . . ? C4 C2 O2 Cr2 128.0(2) . . . . ? O3 Cr4 O2 C2 -43.43(19) . . . . ? O1 Cr4 O2 C2 48.88(19) . . . . ? O4 Cr4 O2 C2 99.1(4) . . . . ? O6 Cr4 O2 C2 -123.81(19) . . . . ? O5 Cr4 O2 C2 145.5(2) . . . . ? O3 Cr4 O2 Cr2 173.12(9) . . . . ? O1 Cr4 O2 Cr2 -94.57(9) . . . . ? O4 Cr4 O2 Cr2 -44.4(5) . . . . ? O6 Cr4 O2 Cr2 92.73(9) . . . . ? O5 Cr4 O2 Cr2 2.06(8) . . . . ? O5 Cr2 O2 C2 -140.4(2) . . . . ? N4 Cr2 O2 C2 133.0(2) . . . . ? N3 Cr2 O2 C2 -175.2(5) . . . . ? Cl4 Cr2 O2 C2 46.2(2) . . . . ? Cl3 Cr2 O2 C2 -45.3(2) . . . . ? O5 Cr2 O2 Cr4 -2.02(8) . . . . ? N4 Cr2 O2 Cr4 -88.60(10) . . . . ? N3 Cr2 O2 Cr4 -36.8(6) . . . . ? Cl4 Cr2 O2 Cr4 -175.44(7) . . . . ? Cl3 Cr2 O2 Cr4 93.11(8) . . . . ? C4 C3 O3 Cr4 -6.3(3) . . . . ? C4 C3 O3 Cr3 127.6(2) . . . . ? O2 Cr4 O3 C3 50.42(19) . . . . ? O1 Cr4 O3 C3 -42.65(19) . . . . ? O4 Cr4 O3 C3 -122.53(19) . . . . ? O6 Cr4 O3 C3 146.5(2) . . . . ? O5 Cr4 O3 C3 97.2(4) . . . . ? O2 Cr4 O3 Cr3 -94.10(9) . . . . ? O1 Cr4 O3 Cr3 172.83(9) . . . . ? O4 Cr4 O3 Cr3 92.95(9) . . . . ? O6 Cr4 O3 Cr3 1.98(9) . . . . ? O5 Cr4 O3 Cr3 -47.3(4) . . . . ? O6 Cr3 O3 C3 -141.2(2) . . . . ? N6 Cr3 O3 C3 132.3(2) . . . . ? N5 Cr3 O3 C3 -170.3(5) . . . . ? Cl6 Cr3 O3 C3 45.2(2) . . . . ? Cl5 Cr3 O3 C3 -46.5(2) . . . . ? O6 Cr3 O3 Cr4 -1.95(8) . . . . ? N6 Cr3 O3 Cr4 -88.50(10) . . . . ? N5 Cr3 O3 Cr4 -31.1(6) . . . . ? Cl6 Cr3 O3 Cr4 -175.60(7) . . . . ? Cl5 Cr3 O3 Cr4 92.75(8) . . . . ? C10 C7 O4 Cr4 -5.6(3) . . . . ? C10 C7 O4 Cr1 129.9(2) . . . . ? O2 Cr4 O4 C7 94.3(4) . . . . ? O3 Cr4 O4 C7 -123.51(19) . . . . ? O1 Cr4 O4 C7 145.5(2) . . . . ? O6 Cr4 O4 C7 -43.12(19) . . . . ? O5 Cr4 O4 C7 48.78(19) . . . . ? O2 Cr4 O4 Cr1 -53.5(4) . . . . ? O3 Cr4 O4 Cr1 88.73(9) . . . . ? O1 Cr4 O4 Cr1 -2.24(8) . . . . ? O6 Cr4 O4 Cr1 169.12(9) . . . . ? O5 Cr4 O4 Cr1 -98.98(9) . . . . ? O1 Cr1 O4 C7 -138.5(2) . . . . ? N2 Cr1 O4 C7 -43.7(2) . . . . ? N1 Cr1 O4 C7 34.1(2) . . . . ? Cl1 Cr1 O4 C7 127.3(2) . . . . ? Cl2 Cr1 O4 C7 -96.6(5) . . . . ? O1 Cr1 O4 Cr4 2.24(8) . . . . ? N2 Cr1 O4 Cr4 97.06(10) . . . . ? N1 Cr1 O4 Cr4 174.90(9) . . . . ? Cl1 Cr1 O4 Cr4 -91.92(7) . . . . ? Cl2 Cr1 O4 Cr4 44.2(5) . . . . ? C10 C8 O5 Cr4 -5.7(3) . . . . ? C10 C8 O5 Cr2 129.9(2) . . . . ? O2 Cr4 O5 C8 146.1(2) . . . . ? O3 Cr4 O5 C8 98.3(4) . . . . ? O1 Cr4 O5 C8 -122.15(19) . . . . ? O4 Cr4 O5 C8 -42.25(19) . . . . ? O6 Cr4 O5 C8 49.96(19) . . . . ? O2 Cr4 O5 Cr2 -1.98(8) . . . . ? O3 Cr4 O5 Cr2 -49.7(4) . . . . ? O1 Cr4 O5 Cr2 89.78(9) . . . . ? O4 Cr4 O5 Cr2 169.67(9) . . . . ? O6 Cr4 O5 Cr2 -98.12(9) . . . . ? O2 Cr2 O5 C8 -138.9(2) . . . . ? N4 Cr2 O5 C8 -41.9(2) . . . . ? N3 Cr2 O5 C8 35.6(2) . . . . ? Cl4 Cr2 O5 C8 -98.7(4) . . . . ? Cl3 Cr2 O5 C8 129.0(2) . . . . ? O2 Cr2 O5 Cr4 1.98(8) . . . . ? N4 Cr2 O5 Cr4 98.99(10) . . . . ? N3 Cr2 O5 Cr4 176.50(9) . . . . ? Cl4 Cr2 O5 Cr4 42.2(4) . . . . ? Cl3 Cr2 O5 Cr4 -90.14(7) . . . . ? C10 C9 O6 Cr4 -4.8(3) . . . . ? C10 C9 O6 Cr3 129.4(2) . . . . ? O2 Cr4 O6 C9 -123.42(19) . . . . ? O3 Cr4 O6 C9 145.5(2) . . . . ? O1 Cr4 O6 C9 94.8(4) . . . . ? O4 Cr4 O6 C9 48.75(19) . . . . ? O5 Cr4 O6 C9 -43.68(19) . . . . ? O2 Cr4 O6 Cr3 89.19(9) . . . . ? O3 Cr4 O6 Cr3 -1.92(8) . . . . ? O1 Cr4 O6 Cr3 -52.6(4) . . . . ? O4 Cr4 O6 Cr3 -98.65(9) . . . . ? O5 Cr4 O6 Cr3 168.93(9) . . . . ? O3 Cr3 O6 C9 -137.7(2) . . . . ? N6 Cr3 O6 C9 -40.0(2) . . . . ? N5 Cr3 O6 C9 37.7(2) . . . . ? Cl6 Cr3 O6 C9 -95.3(4) . . . . ? Cl5 Cr3 O6 C9 130.5(2) . . . . ? O3 Cr3 O6 Cr4 1.92(8) . . . . ? N6 Cr3 O6 Cr4 99.64(10) . . . . ? N5 Cr3 O6 Cr4 177.33(9) . . . . ? Cl6 Cr3 O6 Cr4 44.2(4) . . . . ? Cl5 Cr3 O6 Cr4 -89.95(7) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.227 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.101 # Attachment '- 5.cif' data_pb5 _database_code_depnum_ccdc_archive 'CCDC 810904' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cr4(tmp)2Cl6(Et-iac)2].2MeCN' _chemical_melting_point ? _chemical_formula_moiety 'C20 H40 Cl6 Cr4 N6 O6, 2(C2 H3 N)' _chemical_formula_sum 'C24 H46 Cl6 Cr4 N8 O6' _chemical_formula_weight 963.39 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' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2643(9) _cell_length_b 10.2700(13) _cell_length_c 10.6796(10) _cell_angle_alpha 62.341(11) _cell_angle_beta 84.353(7) _cell_angle_gamma 71.591(9) _cell_volume 944.55(17) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2218 _cell_measurement_theta_min 2.6216 _cell_measurement_theta_max 28.4752 _exptl_crystal_description Block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 1.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5016 _exptl_absorpt_correction_T_max 0.5016 _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5316 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3823 _reflns_number_gt 2209 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. All hydrogen atoms were placed geometrically, apart from H2N, which was located manually. ; _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^)+(0.0570P)^2^+0.0000P] 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 3823 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 0.855 _refine_ls_restrained_S_all 0.855 _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 C1 C 0.1434(4) 0.3540(6) 0.3029(5) 0.0224(11) Uani 1 1 d . . . H1A H 0.1447 0.4332 0.3278 0.027 Uiso 1 1 calc R . . H1B H 0.2062 0.2572 0.3698 0.027 Uiso 1 1 calc R . . C2 C -0.0057(5) 0.2068(6) 0.2913(5) 0.0236(11) Uani 1 1 d . . . H2A H 0.0585 0.1113 0.3583 0.028 Uiso 1 1 calc R . . H2B H -0.0971 0.1954 0.3068 0.028 Uiso 1 1 calc R . . C3 C 0.1086(4) 0.5076(5) -0.2286(4) 0.0199(11) Uani 1 1 d . . . H3A H 0.1043 0.4310 -0.2557 0.024 Uiso 1 1 calc R . . H3B H 0.1996 0.5196 -0.2466 0.024 Uiso 1 1 calc R . . C4 C -0.0022(4) 0.3391(6) 0.3194(5) 0.0213(11) Uani 1 1 d . . . C5 C -0.0310(5) 0.2965(7) 0.4765(5) 0.0311(13) Uani 1 1 d . . . H5A H 0.0424 0.2049 0.5348 0.037 Uiso 1 1 calc R . . H5B H -0.0260 0.3796 0.4938 0.037 Uiso 1 1 calc R . . C6 C -0.1665(5) 0.2664(7) 0.5265(5) 0.0344(13) Uani 1 1 d . . . H6A H -0.2408 0.3577 0.4736 0.052 Uiso 1 1 calc R . . H6B H -0.1718 0.2395 0.6253 0.052 Uiso 1 1 calc R . . H6C H -0.1729 0.1830 0.5121 0.052 Uiso 1 1 calc R . . C7 C 0.4519(5) 0.2407(6) -0.1041(5) 0.0245(11) Uani 1 1 d . . . C8 C 0.5706(4) 0.2910(6) -0.1764(5) 0.0261(12) Uani 1 1 d . . . H8A H 0.5423 0.3683 -0.2724 0.039 Uiso 1 1 calc R . . H8B H 0.6423 0.2041 -0.1762 0.039 Uiso 1 1 calc R . . H8C H 0.6043 0.3335 -0.1277 0.039 Uiso 1 1 calc R . . C9 C 0.3016(5) 0.0979(6) -0.1088(5) 0.0226(11) Uani 1 1 d . . . C10 C 0.2785(5) 0.0168(6) -0.1860(5) 0.0288(12) Uani 1 1 d . . . H10A H 0.2105 -0.0339 -0.1406 0.043 Uiso 1 1 calc R . . H10B H 0.3631 -0.0585 -0.1849 0.043 Uiso 1 1 calc R . . H10C H 0.2470 0.0905 -0.2822 0.043 Uiso 1 1 calc R . . C11 C 0.4262(6) 0.3169(7) 0.4715(6) 0.0420(15) Uani 1 1 d . . . C12 C 0.4995(6) 0.2616(8) 0.3734(6) 0.0510(17) Uani 1 1 d . . . H12A H 0.5025 0.1563 0.4061 0.077 Uiso 1 1 calc R . . H12B H 0.5916 0.2674 0.3680 0.077 Uiso 1 1 calc R . . H12C H 0.4529 0.3244 0.2813 0.077 Uiso 1 1 calc R . . Cl3 Cl -0.29638(12) 0.36636(15) 0.09027(13) 0.0267(3) Uani 1 1 d . . . Cl4 Cl -0.08883(11) 0.26661(15) -0.12627(14) 0.0292(3) Uani 1 1 d . . . Cl5 Cl 0.33675(11) 0.03524(15) 0.27792(13) 0.0271(3) Uani 1 1 d . . . Cr1 Cr 0.21109(7) 0.24953(9) 0.08243(8) 0.0206(2) Uani 1 1 d . . . Cr2 Cr -0.09448(7) 0.40801(9) -0.00886(8) 0.0196(2) Uani 1 1 d . . . N4 N 0.3680(6) 0.3598(7) 0.5465(6) 0.0600(16) Uani 1 1 d . . . O1 O 0.1931(3) 0.3915(4) 0.1642(3) 0.0172(7) Uani 1 1 d . . . O2 O 0.0288(3) 0.2317(4) 0.1502(3) 0.0205(7) Uani 1 1 d . . . O3 O 0.0876(3) 0.4518(4) -0.0768(3) 0.0164(7) Uani 1 1 d . . . N1 N 0.3833(3) 0.2851(4) -0.0168(4) 0.0195(9) Uani 1 1 d . . . H1N H 0.4169 0.3404 0.0033 0.023 Uiso 1 1 calc R . . N2 N 0.4170(4) 0.1437(5) -0.1403(4) 0.0238(10) Uani 1 1 d . . . N3 N 0.2174(4) 0.1270(4) -0.0210(4) 0.0214(9) Uani 1 1 d . . . H3N H 0.1519 0.0866 -0.0032 0.026 Uiso 1 1 calc R . . H2N H 0.468(5) 0.117(6) -0.194(6) 0.040(17) Uiso 1 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 C1 0.021(2) 0.026(3) 0.017(3) -0.011(2) 0.003(2) -0.002(2) C2 0.017(2) 0.025(3) 0.018(3) -0.006(2) 0.003(2) 0.000(2) C3 0.017(2) 0.028(3) 0.016(2) -0.014(2) 0.0078(19) -0.005(2) C4 0.015(2) 0.026(3) 0.018(3) -0.011(2) 0.001(2) 0.001(2) C5 0.024(3) 0.044(4) 0.023(3) -0.016(3) 0.008(2) -0.007(2) C6 0.034(3) 0.041(4) 0.021(3) -0.012(3) 0.008(2) -0.009(3) C7 0.018(2) 0.023(3) 0.019(3) -0.005(2) 0.000(2) 0.004(2) C8 0.025(3) 0.031(3) 0.026(3) -0.018(3) 0.009(2) -0.008(2) C9 0.018(2) 0.017(3) 0.022(3) -0.003(2) -0.002(2) 0.000(2) C10 0.021(3) 0.034(3) 0.034(3) -0.021(3) 0.000(2) -0.003(2) C11 0.039(3) 0.051(4) 0.030(3) -0.013(3) -0.009(3) -0.010(3) C12 0.041(3) 0.075(5) 0.034(3) -0.022(4) 0.006(3) -0.020(3) Cl3 0.0218(6) 0.0293(8) 0.0310(7) -0.0170(6) 0.0070(5) -0.0071(6) Cl4 0.0209(6) 0.0361(8) 0.0376(8) -0.0254(7) 0.0042(6) -0.0051(6) Cl5 0.0195(6) 0.0263(8) 0.0269(7) -0.0107(6) 0.0013(5) 0.0017(5) Cr1 0.0127(4) 0.0253(5) 0.0217(4) -0.0131(4) 0.0032(3) -0.0003(3) Cr2 0.0129(4) 0.0248(5) 0.0209(4) -0.0133(4) 0.0034(3) -0.0017(3) N4 0.073(4) 0.056(4) 0.034(3) -0.017(3) -0.014(3) 0.002(3) O1 0.0086(15) 0.0206(19) 0.0187(17) -0.0086(16) 0.0039(13) -0.0012(14) O2 0.0140(15) 0.026(2) 0.0192(17) -0.0135(16) -0.0003(13) 0.0021(14) O3 0.0091(14) 0.0213(19) 0.0162(17) -0.0090(15) 0.0005(13) -0.0008(13) N1 0.018(2) 0.017(2) 0.021(2) -0.0098(19) 0.0011(16) -0.0002(17) N2 0.021(2) 0.029(3) 0.026(2) -0.018(2) 0.0066(19) -0.0046(19) N3 0.0155(19) 0.023(2) 0.026(2) -0.014(2) 0.0050(17) -0.0043(18) _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 C1 O1 1.432(5) . ? C1 C4 1.535(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O2 1.434(5) . ? C2 C4 1.533(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O3 1.466(5) . ? C3 C4 1.522(6) 2_565 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C3 1.522(6) 2_565 ? C4 C5 1.548(6) . ? C5 C6 1.512(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N1 1.279(5) . ? C7 N2 1.371(6) . ? C7 C8 1.480(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N3 1.286(5) . ? C9 N2 1.365(6) . ? C9 C10 1.494(6) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N4 1.123(7) . ? C11 C12 1.454(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? Cl3 Cr2 2.3035(13) . ? Cl4 Cr2 2.3039(13) . ? Cl5 Cr1 2.3102(15) . ? Cr1 O2 1.971(3) . ? Cr1 O1 1.976(3) . ? Cr1 N3 2.008(4) . ? Cr1 N1 2.015(4) . ? Cr1 O3 2.072(3) . ? Cr2 O1 1.964(3) 2_565 ? Cr2 O2 1.971(3) . ? Cr2 O3 2.046(3) . ? Cr2 O3 2.053(3) 2_565 ? O1 Cr2 1.964(3) 2_565 ? O3 Cr2 2.053(3) 2_565 ? N1 H1N 0.8600 . ? N2 H2N 0.82(5) . ? N3 H3N 0.8600 . ? 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 O1 C1 C4 114.9(4) . . ? O1 C1 H1A 108.5 . . ? C4 C1 H1A 108.5 . . ? O1 C1 H1B 108.5 . . ? C4 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? O2 C2 C4 112.7(4) . . ? O2 C2 H2A 109.1 . . ? C4 C2 H2A 109.1 . . ? O2 C2 H2B 109.1 . . ? C4 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? O3 C3 C4 112.7(3) . 2_565 ? O3 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 2_565 . ? O3 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 2_565 . ? H3A C3 H3B 107.8 . . ? C3 C4 C2 113.5(4) 2_565 . ? C3 C4 C1 111.4(4) 2_565 . ? C2 C4 C1 110.0(4) . . ? C3 C4 C5 107.8(3) 2_565 . ? C2 C4 C5 108.7(4) . . ? C1 C4 C5 105.1(4) . . ? C6 C5 C4 117.1(4) . . ? C6 C5 H5A 108.0 . . ? C4 C5 H5A 108.0 . . ? C6 C5 H5B 108.0 . . ? C4 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 N2 121.3(4) . . ? N1 C7 C8 123.9(4) . . ? N2 C7 C8 114.8(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 N2 121.5(4) . . ? N3 C9 C10 122.9(4) . . ? N2 C9 C10 115.6(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 C12 179.1(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 Cr1 O1 88.54(12) . . ? O2 Cr1 N3 91.01(13) . . ? O1 Cr1 N3 173.31(15) . . ? O2 Cr1 N1 171.22(14) . . ? O1 Cr1 N1 94.67(13) . . ? N3 Cr1 N1 84.84(15) . . ? O2 Cr1 O3 80.55(12) . . ? O1 Cr1 O3 80.34(12) . . ? N3 Cr1 O3 93.00(14) . . ? N1 Cr1 O3 91.92(14) . . ? O2 Cr1 Cl5 96.09(10) . . ? O1 Cr1 Cl5 93.87(10) . . ? N3 Cr1 Cl5 92.82(12) . . ? N1 Cr1 Cl5 91.85(11) . . ? O3 Cr1 Cl5 173.33(9) . . ? O1 Cr2 O2 167.72(13) 2_565 . ? O1 Cr2 O3 89.50(12) 2_565 . ? O2 Cr2 O3 81.21(12) . . ? O1 Cr2 O3 81.10(12) 2_565 2_565 ? O2 Cr2 O3 89.13(12) . 2_565 ? O3 Cr2 O3 78.40(12) . 2_565 ? O1 Cr2 Cl3 92.21(9) 2_565 . ? O2 Cr2 Cl3 96.03(10) . . ? O3 Cr2 Cl3 172.68(9) . . ? O3 Cr2 Cl3 94.83(8) 2_565 . ? O1 Cr2 Cl4 95.46(9) 2_565 . ? O2 Cr2 Cl4 93.49(9) . . ? O3 Cr2 Cl4 95.99(8) . . ? O3 Cr2 Cl4 173.38(10) 2_565 . ? Cl3 Cr2 Cl4 90.94(5) . . ? C1 O1 Cr2 117.4(2) . 2_565 ? C1 O1 Cr1 119.4(3) . . ? Cr2 O1 Cr1 102.03(13) 2_565 . ? C2 O2 Cr1 121.0(3) . . ? C2 O2 Cr2 118.2(3) . . ? Cr1 O2 Cr2 101.66(15) . . ? C3 O3 Cr2 117.0(2) . . ? C3 O3 Cr2 117.0(2) . 2_565 ? Cr2 O3 Cr2 101.60(12) . 2_565 ? C3 O3 Cr1 124.9(2) . . ? Cr2 O3 Cr1 95.85(13) . . ? Cr2 O3 Cr1 95.89(12) 2_565 . ? C7 N1 Cr1 132.0(3) . . ? C7 N1 H1N 114.0 . . ? Cr1 N1 H1N 114.0 . . ? C9 N2 C7 128.0(4) . . ? C9 N2 H2N 116(4) . . ? C7 N2 H2N 116(4) . . ? C9 N3 Cr1 131.8(3) . . ? C9 N3 H3N 114.1 . . ? Cr1 N3 H3N 114.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C2 C4 C3 63.9(5) . . . 2_565 ? O2 C2 C4 C1 -61.6(5) . . . . ? O2 C2 C4 C5 -176.2(3) . . . . ? O1 C1 C4 C3 -64.4(5) . . . 2_565 ? O1 C1 C4 C2 62.4(5) . . . . ? O1 C1 C4 C5 179.2(4) . . . . ? C3 C4 C5 C6 64.0(6) 2_565 . . . ? C2 C4 C5 C6 -59.4(5) . . . . ? C1 C4 C5 C6 -177.1(4) . . . . ? C4 C1 O1 Cr2 63.5(4) . . . 2_565 ? C4 C1 O1 Cr1 -60.6(4) . . . . ? O2 Cr1 O1 C1 44.4(3) . . . . ? N3 Cr1 O1 C1 130.7(11) . . . . ? N1 Cr1 O1 C1 -143.8(3) . . . . ? O3 Cr1 O1 C1 125.1(3) . . . . ? Cl5 Cr1 O1 C1 -51.6(3) . . . . ? O2 Cr1 O1 Cr2 -86.90(14) . . . 2_565 ? N3 Cr1 O1 Cr2 -0.7(12) . . . 2_565 ? N1 Cr1 O1 Cr2 84.91(15) . . . 2_565 ? O3 Cr1 O1 Cr2 -6.25(12) . . . 2_565 ? Cl5 Cr1 O1 Cr2 177.09(10) . . . 2_565 ? C4 C2 O2 Cr1 61.9(4) . . . . ? C4 C2 O2 Cr2 -64.2(4) . . . . ? O1 Cr1 O2 C2 -46.2(3) . . . . ? N3 Cr1 O2 C2 140.5(3) . . . . ? N1 Cr1 O2 C2 -157.8(9) . . . . ? O3 Cr1 O2 C2 -126.6(3) . . . . ? Cl5 Cr1 O2 C2 47.6(3) . . . . ? O1 Cr1 O2 Cr2 87.15(14) . . . . ? N3 Cr1 O2 Cr2 -86.18(15) . . . . ? N1 Cr1 O2 Cr2 -24.5(10) . . . . ? O3 Cr1 O2 Cr2 6.69(12) . . . . ? Cl5 Cr1 O2 Cr2 -179.12(10) . . . . ? O1 Cr2 O2 C2 86.9(6) 2_565 . . . ? O3 Cr2 O2 C2 128.2(3) . . . . ? O3 Cr2 O2 C2 49.8(3) 2_565 . . . ? Cl3 Cr2 O2 C2 -45.0(3) . . . . ? Cl4 Cr2 O2 C2 -136.3(3) . . . . ? O1 Cr2 O2 Cr1 -48.0(6) 2_565 . . . ? O3 Cr2 O2 Cr1 -6.77(12) . . . . ? O3 Cr2 O2 Cr1 -85.16(13) 2_565 . . . ? Cl3 Cr2 O2 Cr1 -179.93(10) . . . . ? Cl4 Cr2 O2 Cr1 88.76(11) . . . . ? C4 C3 O3 Cr2 61.2(4) 2_565 . . . ? C4 C3 O3 Cr2 -59.6(4) 2_565 . . 2_565 ? C4 C3 O3 Cr1 -179.2(3) 2_565 . . . ? O1 Cr2 O3 C3 -47.6(3) 2_565 . . . ? O2 Cr2 O3 C3 140.5(3) . . . . ? O3 Cr2 O3 C3 -128.6(3) 2_565 . . . ? Cl3 Cr2 O3 C3 -151.2(7) . . . . ? Cl4 Cr2 O3 C3 47.9(3) . . . . ? O1 Cr2 O3 Cr2 81.02(14) 2_565 . . 2_565 ? O2 Cr2 O3 Cr2 -90.92(13) . . . 2_565 ? O3 Cr2 O3 Cr2 0.0 2_565 . . 2_565 ? Cl3 Cr2 O3 Cr2 -22.6(9) . . . 2_565 ? Cl4 Cr2 O3 Cr2 176.46(11) . . . 2_565 ? O1 Cr2 O3 Cr1 178.27(12) 2_565 . . . ? O2 Cr2 O3 Cr1 6.34(11) . . . . ? O3 Cr2 O3 Cr1 97.26(14) 2_565 . . . ? Cl3 Cr2 O3 Cr1 74.7(8) . . . . ? Cl4 Cr2 O3 Cr1 -86.29(10) . . . . ? O2 Cr1 O3 C3 -135.2(3) . . . . ? O1 Cr1 O3 C3 134.7(3) . . . . ? N3 Cr1 O3 C3 -44.6(3) . . . . ? N1 Cr1 O3 C3 40.3(3) . . . . ? Cl5 Cr1 O3 C3 164.7(7) . . . . ? O2 Cr1 O3 Cr2 -6.35(11) . . . . ? O1 Cr1 O3 Cr2 -96.47(12) . . . . ? N3 Cr1 O3 Cr2 84.18(14) . . . . ? N1 Cr1 O3 Cr2 169.11(13) . . . . ? Cl5 Cr1 O3 Cr2 -66.5(9) . . . . ? O2 Cr1 O3 Cr2 96.00(12) . . . 2_565 ? O1 Cr1 O3 Cr2 5.88(11) . . . 2_565 ? N3 Cr1 O3 Cr2 -173.47(13) . . . 2_565 ? N1 Cr1 O3 Cr2 -88.54(14) . . . 2_565 ? Cl5 Cr1 O3 Cr2 35.9(9) . . . 2_565 ? N2 C7 N1 Cr1 -4.1(7) . . . . ? C8 C7 N1 Cr1 174.2(3) . . . . ? O2 Cr1 N1 C7 -61.9(11) . . . . ? O1 Cr1 N1 C7 -173.1(4) . . . . ? N3 Cr1 N1 C7 0.2(4) . . . . ? O3 Cr1 N1 C7 -92.7(4) . . . . ? Cl5 Cr1 N1 C7 92.8(4) . . . . ? N3 C9 N2 C7 -9.9(8) . . . . ? C10 C9 N2 C7 168.5(5) . . . . ? N1 C7 N2 C9 9.4(8) . . . . ? C8 C7 N2 C9 -169.0(5) . . . . ? N2 C9 N3 Cr1 4.9(7) . . . . ? C10 C9 N3 Cr1 -173.3(3) . . . . ? O2 Cr1 N3 C9 171.6(4) . . . . ? O1 Cr1 N3 C9 85.5(12) . . . . ? N1 Cr1 N3 C9 -0.6(4) . . . . ? O3 Cr1 N3 C9 91.1(5) . . . . ? Cl5 Cr1 N3 C9 -92.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.662 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.125 # Attachment '- 6.cif' data_brepw52m _database_code_depnum_ccdc_archive 'CCDC 810905' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Cr4(tmp)2Cl6(Pr-iac)2].2EtCN' _chemical_melting_point ? _chemical_formula_moiety 'C24 H48 Cl6 Cr4 N6 O6, 2(C3 H5 N)' _chemical_formula_sum 'C30 H58 Cl6 Cr4 N8 O6' _chemical_formula_weight 1047.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.134(2) _cell_length_b 16.530(3) _cell_length_c 13.389(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.16(3) _cell_angle_gamma 90.00 _cell_volume 2233.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2031 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 23.98 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.354 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12813 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4566 _reflns_number_gt 2865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0214P)^2^+0.0000P] 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 4566 _refine_ls_number_parameters 317 _refine_ls_number_restraints 107 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.849 _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 Cr1 Cr 0.47716(5) 0.13800(3) 0.90330(5) 0.02262(16) Uani 1 1 d . . . Cr2 Cr 0.58465(5) 0.04284(3) 1.08990(5) 0.02052(16) Uani 1 1 d . . . Cl1 Cl 0.34905(8) 0.25089(5) 0.87690(8) 0.0304(2) Uani 1 1 d . . . Cl2 Cl 0.77765(8) 0.11928(5) 1.10463(7) 0.0238(2) Uani 1 1 d . . . Cl3 Cl 0.56661(8) 0.05579(5) 1.25968(7) 0.0269(2) Uani 1 1 d . . . O1 O 0.57721(19) 0.03042(12) 0.93751(17) 0.0184(6) Uani 1 1 d . . . O2 O 0.47483(19) 0.13734(12) 1.05096(18) 0.0202(6) Uani 1 1 d . . . O3 O 0.3259(2) 0.06231(12) 0.89504(18) 0.0203(6) Uani 1 1 d . . . N1 N 0.6421(3) 0.23866(18) 0.7419(3) 0.0301(8) Uani 1 1 d D A . H1N H 0.677(3) 0.262(2) 0.699(2) 0.036 Uiso 1 1 d D . . N2 N 0.6465(3) 0.20199(19) 0.9062(2) 0.0255(8) Uani 1 1 d D A . H2N H 0.682(3) 0.204(2) 0.9608(18) 0.031 Uiso 1 1 d D . . N3 N 0.5017(3) 0.12941(18) 0.7571(3) 0.0260(8) Uani 1 1 d D A . H3N H 0.466(3) 0.0909(17) 0.729(3) 0.031 Uiso 1 1 d D . . C1 C 0.6953(3) 0.2429(2) 0.8383(3) 0.0282(10) Uani 1 1 d . . . C2 C 0.8144(4) 0.2970(2) 0.8566(4) 0.0470(13) Uani 0.62(3) 1 d P A 1 H2A H 0.8622 0.2966 0.7953 0.056 Uiso 0.62(3) 1 calc PR A 1 H2B H 0.7823 0.3529 0.8654 0.056 Uiso 0.62(3) 1 calc PR A 1 C3 C 0.9065(13) 0.2787(9) 0.9391(10) 0.051(4) Uani 0.62(3) 1 d P A 1 H3A H 0.9353 0.2223 0.9344 0.061 Uiso 0.62(3) 1 calc PR A 1 H3B H 0.8648 0.2865 1.0016 0.061 Uiso 0.62(3) 1 calc PR A 1 H3C H 0.9835 0.3145 0.9384 0.061 Uiso 0.62(3) 1 calc PR A 1 C2X C 0.8144(4) 0.2970(2) 0.8566(4) 0.0470(13) Uani 0.38(3) 1 d P A 2 H2X1 H 0.8243 0.3291 0.7953 0.056 Uiso 0.38(3) 1 calc PR A 2 H2X2 H 0.7993 0.3352 0.9113 0.056 Uiso 0.38(3) 1 calc PR A 2 C3X C 0.9359(17) 0.2530(12) 0.883(3) 0.067(8) Uani 0.38(3) 1 d P A 2 H3X1 H 1.0105 0.2909 0.8895 0.080 Uiso 0.38(3) 1 calc PR A 2 H3X2 H 0.9497 0.2133 0.8306 0.080 Uiso 0.38(3) 1 calc PR A 2 H3X3 H 0.9300 0.2249 0.9470 0.080 Uiso 0.38(3) 1 calc PR A 2 C4 C 0.5630(4) 0.1765(2) 0.6999(3) 0.0304(10) Uani 1 1 d . . . C5 C 0.5617(4) 0.1673(2) 0.5901(3) 0.0402(11) Uani 0.556(15) 1 d P A 1 H5A H 0.5114 0.2130 0.5578 0.048 Uiso 0.556(15) 1 calc PR A 1 H5B H 0.6541 0.1716 0.5719 0.048 Uiso 0.556(15) 1 calc PR A 1 C6 C 0.5069(16) 0.0943(5) 0.5492(7) 0.064(5) Uani 0.556(15) 1 d P A 1 H6A H 0.5409 0.0485 0.5904 0.097 Uiso 0.556(15) 1 calc PR A 1 H6B H 0.5317 0.0876 0.4806 0.097 Uiso 0.556(15) 1 calc PR A 1 H6C H 0.4102 0.0962 0.5483 0.097 Uiso 0.556(15) 1 calc PR A 1 C5X C 0.5617(4) 0.1673(2) 0.5901(3) 0.0402(11) Uani 0.444(15) 1 d P A 2 H5X1 H 0.6028 0.2161 0.5633 0.048 Uiso 0.444(15) 1 calc PR A 2 H5X2 H 0.4682 0.1659 0.5614 0.048 Uiso 0.444(15) 1 calc PR A 2 C6X C 0.6300(19) 0.0951(6) 0.5529(8) 0.058(5) Uani 0.444(15) 1 d P A 2 H6X1 H 0.5908 0.0460 0.5785 0.070 Uiso 0.444(15) 1 calc PR A 2 H6X2 H 0.7243 0.0973 0.5763 0.070 Uiso 0.444(15) 1 calc PR A 2 H6X3 H 0.6198 0.0946 0.4794 0.070 Uiso 0.444(15) 1 calc PR A 2 C7 C 0.7478(3) -0.0784(2) 0.9326(3) 0.0215(9) Uani 1 1 d . . . C8 C 0.8779(3) -0.0960(2) 0.8842(3) 0.0273(10) Uani 1 1 d . . . H8A H 0.9438 -0.0547 0.9086 0.033 Uiso 1 1 calc R . . H8B H 0.9118 -0.1491 0.9093 0.033 Uiso 1 1 calc R . . C9 C 0.8719(3) -0.0975(2) 0.7711(3) 0.0401(11) Uani 1 1 d . . . H9A H 0.8069 -0.1379 0.7450 0.060 Uiso 1 1 calc R . . H9B H 0.9593 -0.1114 0.7502 0.060 Uiso 1 1 calc R . . H9C H 0.8455 -0.0440 0.7446 0.060 Uiso 1 1 calc R . . C10 C 0.6976(3) 0.00460(19) 0.8941(3) 0.0214(9) Uani 1 1 d . . . H10A H 0.7679 0.0454 0.9101 0.026 Uiso 1 1 calc R . . H10B H 0.6799 0.0023 0.8202 0.026 Uiso 1 1 calc R . . C11 C 0.2167(3) 0.0778(2) 0.9538(3) 0.0246(9) Uani 1 1 d . . . H11A H 0.1481 0.0360 0.9378 0.030 Uiso 1 1 calc R . . H11B H 0.1775 0.1308 0.9336 0.030 Uiso 1 1 calc R . . C12 C 0.3522(3) 0.14634(19) 1.0962(3) 0.0222(9) Uani 1 1 d . . . H12A H 0.3118 0.1990 1.0755 0.027 Uiso 1 1 calc R . . H12B H 0.3711 0.1472 1.1700 0.027 Uiso 1 1 calc R . . N4 N -0.0935(8) 0.1275(5) 0.7354(9) 0.100(3) Uani 0.641(9) 1 d PDU B 1 C13 C 0.0069(9) 0.1069(7) 0.7167(10) 0.086(3) Uani 0.641(9) 1 d PDU B 1 C14 C 0.1297(8) 0.0712(7) 0.6868(9) 0.077(3) Uani 0.641(9) 1 d PDU B 1 H14C H 0.1990 0.1136 0.6933 0.115 Uiso 0.641(9) 1 calc PR B 1 H14D H 0.1573 0.0282 0.7357 0.115 Uiso 0.641(9) 1 calc PR B 1 C15 C 0.1290(12) 0.0405(8) 0.5981(9) 0.117(4) Uani 0.641(9) 1 d PDU B 1 H15D H 0.1320 0.0841 0.5488 0.140 Uiso 0.641(9) 1 calc PR B 1 H15E H 0.0480 0.0087 0.5833 0.140 Uiso 0.641(9) 1 calc PR B 1 H15F H 0.2065 0.0054 0.5951 0.140 Uiso 0.641(9) 1 calc PR B 1 N4X N -0.0955(13) 0.1318(10) 0.6449(15) 0.109(5) Uani 0.359(9) 1 d PDU B 2 C13X C 0.0117(15) 0.1116(14) 0.6513(17) 0.093(3) Uani 0.359(9) 1 d PDU B 2 C14X C 0.1554(13) 0.1151(14) 0.6586(17) 0.095(4) Uani 0.359(9) 1 d PDU B 2 H14A H 0.1943 0.0862 0.7190 0.142 Uiso 0.359(9) 1 calc PR B 2 H14B H 0.1869 0.1718 0.6611 0.142 Uiso 0.359(9) 1 calc PR B 2 C15X C 0.1929(18) 0.0703(13) 0.5566(13) 0.099(5) Uani 0.359(9) 1 d PDU B 2 H15A H 0.1242 0.0306 0.5355 0.118 Uiso 0.359(9) 1 calc PR B 2 H15B H 0.2784 0.0428 0.5694 0.118 Uiso 0.359(9) 1 calc PR B 2 H15C H 0.1987 0.1106 0.5035 0.118 Uiso 0.359(9) 1 calc PRU B 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 Cr1 0.0154(3) 0.0159(3) 0.0364(4) 0.0020(3) 0.0015(3) 0.0005(2) Cr2 0.0114(3) 0.0155(3) 0.0347(4) 0.0005(3) 0.0024(3) 0.0005(2) Cl1 0.0253(5) 0.0199(5) 0.0455(7) 0.0040(5) 0.0003(5) 0.0058(4) Cl2 0.0137(4) 0.0200(5) 0.0378(6) -0.0023(4) 0.0023(4) -0.0021(3) Cl3 0.0203(5) 0.0229(5) 0.0378(6) 0.0000(4) 0.0038(4) -0.0011(4) O1 0.0083(12) 0.0157(13) 0.0316(16) 0.0021(11) 0.0038(11) 0.0012(9) O2 0.0089(12) 0.0154(13) 0.0368(17) -0.0010(12) 0.0041(11) 0.0012(9) O3 0.0105(12) 0.0157(13) 0.0350(16) -0.0008(11) 0.0027(11) 0.0020(10) N1 0.0260(19) 0.0193(19) 0.047(3) 0.0082(17) 0.0131(17) -0.0018(14) N2 0.0194(18) 0.0217(18) 0.035(2) 0.0044(17) -0.0024(16) -0.0013(13) N3 0.0205(18) 0.0209(19) 0.037(2) 0.0027(16) 0.0047(15) -0.0002(14) C1 0.018(2) 0.016(2) 0.051(3) 0.008(2) 0.003(2) 0.0054(15) C2 0.025(2) 0.034(3) 0.081(4) 0.012(2) -0.002(2) -0.0088(19) C3 0.043(7) 0.055(8) 0.053(7) 0.023(6) -0.011(5) -0.025(6) C2X 0.025(2) 0.034(3) 0.081(4) 0.012(2) -0.002(2) -0.0088(19) C3X 0.024(8) 0.056(12) 0.12(2) 0.039(12) -0.004(11) -0.015(8) C4 0.029(2) 0.019(2) 0.045(3) 0.001(2) 0.010(2) 0.0068(17) C5 0.049(3) 0.030(2) 0.044(3) 0.005(2) 0.020(2) 0.004(2) C6 0.110(12) 0.049(6) 0.037(6) -0.007(5) 0.022(6) -0.025(6) C5X 0.049(3) 0.030(2) 0.044(3) 0.005(2) 0.020(2) 0.004(2) C6X 0.100(14) 0.043(7) 0.036(7) -0.010(6) 0.026(8) 0.006(7) C7 0.0106(18) 0.0191(19) 0.035(3) -0.0016(18) 0.0052(17) 0.0015(15) C8 0.014(2) 0.024(2) 0.044(3) -0.0040(19) 0.0068(18) 0.0014(15) C9 0.020(2) 0.048(3) 0.053(3) -0.006(2) 0.010(2) -0.0009(18) C10 0.0108(18) 0.020(2) 0.034(2) -0.0021(17) 0.0061(17) -0.0007(14) C11 0.0118(18) 0.020(2) 0.043(3) -0.0015(19) 0.0036(18) 0.0016(15) C12 0.0125(18) 0.0153(19) 0.039(3) 0.0003(17) 0.0042(17) 0.0019(14) N4 0.069(5) 0.097(5) 0.135(8) -0.010(6) 0.019(6) 0.028(4) C13 0.058(4) 0.104(5) 0.095(7) -0.007(6) -0.007(5) 0.030(4) C14 0.041(4) 0.101(6) 0.084(6) -0.008(6) -0.019(4) 0.029(4) C15 0.097(8) 0.159(9) 0.093(8) 0.003(7) 0.001(6) 0.056(7) N4X 0.063(5) 0.142(9) 0.116(10) -0.023(10) -0.015(8) 0.047(7) C13X 0.056(5) 0.122(6) 0.096(7) -0.015(7) -0.013(6) 0.031(5) C14X 0.053(5) 0.134(8) 0.092(8) -0.018(7) -0.027(6) 0.031(7) C15X 0.067(9) 0.158(11) 0.071(9) 0.022(8) 0.008(7) 0.018(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 O3 1.974(2) . ? Cr1 O2 1.979(2) . ? Cr1 N3 2.000(3) . ? Cr1 N2 2.013(3) . ? Cr1 O1 2.078(2) . ? Cr1 Cl1 2.2826(10) . ? Cr2 O2 1.961(2) . ? Cr2 O3 1.962(2) 3_657 ? Cr2 O1 2.045(2) 3_657 ? Cr2 O1 2.045(2) . ? Cr2 Cl3 2.3068(13) . ? Cr2 Cl2 2.3219(10) . ? O1 C10 1.462(3) . ? O1 Cr2 2.045(2) 3_657 ? O2 C12 1.438(3) . ? O3 C11 1.437(4) . ? O3 Cr2 1.962(2) 3_657 ? N1 C1 1.355(5) . ? N1 C4 1.391(5) . ? N1 H1N 0.80(2) . ? N2 C1 1.268(5) . ? N2 H2N 0.78(2) . ? N3 C4 1.290(5) . ? N3 H3N 0.80(2) . ? C1 C2 1.504(5) . ? C2 C3 1.414(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3X H3X1 0.9800 . ? C3X H3X2 0.9800 . ? C3X H3X3 0.9800 . ? C4 C5 1.478(5) . ? C5 C6 1.418(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6X H6X1 0.9800 . ? C6X H6X2 0.9800 . ? C6X H6X3 0.9800 . ? C7 C11 1.531(5) 3_657 ? C7 C10 1.537(4) . ? C7 C12 1.538(4) 3_657 ? C7 C8 1.547(4) . ? C8 C9 1.510(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C7 1.531(5) 3_657 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C7 1.538(4) 3_657 ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N4 C13 1.122(8) . ? C13 C14 1.465(10) . ? C14 C15 1.290(14) . ? C14 H14C 0.9900 . ? C14 H14D 0.9900 . ? C15 H15D 0.9800 . ? C15 H15E 0.9800 . ? C15 H15F 0.9800 . ? N4X C13X 1.133(12) . ? C13X C14X 1.452(14) . ? C14X C15X 1.63(3) . ? C14X H14A 0.9900 . ? C14X H14B 0.9900 . ? C15X H15A 0.9800 . ? C15X H15B 0.9800 . ? C15X H15C 0.9800 . ? 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 O3 Cr1 O2 88.48(9) . . ? O3 Cr1 N3 93.69(11) . . ? O2 Cr1 N3 172.21(11) . . ? O3 Cr1 N2 172.01(11) . . ? O2 Cr1 N2 94.05(12) . . ? N3 Cr1 N2 82.83(13) . . ? O3 Cr1 O1 80.26(8) . . ? O2 Cr1 O1 79.89(9) . . ? N3 Cr1 O1 93.09(11) . . ? N2 Cr1 O1 92.71(10) . . ? O3 Cr1 Cl1 94.68(7) . . ? O2 Cr1 Cl1 95.82(7) . . ? N3 Cr1 Cl1 91.46(9) . . ? N2 Cr1 Cl1 92.61(9) . . ? O1 Cr1 Cl1 173.40(7) . . ? O2 Cr2 O3 168.15(10) . 3_657 ? O2 Cr2 O1 89.83(9) . 3_657 ? O3 Cr2 O1 81.35(9) 3_657 3_657 ? O2 Cr2 O1 81.12(9) . . ? O3 Cr2 O1 89.36(9) 3_657 . ? O1 Cr2 O1 78.73(10) 3_657 . ? O2 Cr2 Cl3 95.43(8) . . ? O3 Cr2 Cl3 93.31(8) 3_657 . ? O1 Cr2 Cl3 95.65(8) 3_657 . ? O1 Cr2 Cl3 173.35(6) . . ? O2 Cr2 Cl2 92.45(7) . . ? O3 Cr2 Cl2 95.48(7) 3_657 . ? O1 Cr2 Cl2 173.33(7) 3_657 . ? O1 Cr2 Cl2 95.43(7) . . ? Cl3 Cr2 Cl2 90.38(4) . . ? C10 O1 Cr2 116.14(18) . 3_657 ? C10 O1 Cr2 117.95(19) . . ? Cr2 O1 Cr2 101.27(10) 3_657 . ? C10 O1 Cr1 124.79(18) . . ? Cr2 O1 Cr1 95.72(8) 3_657 . ? Cr2 O1 Cr1 96.17(9) . . ? C12 O2 Cr2 117.50(18) . . ? C12 O2 Cr1 120.55(19) . . ? Cr2 O2 Cr1 102.27(10) . . ? C11 O3 Cr2 118.19(19) . 3_657 ? C11 O3 Cr1 119.25(19) . . ? Cr2 O3 Cr1 101.92(9) 3_657 . ? C1 N1 C4 126.1(3) . . ? C1 N1 H1N 119(3) . . ? C4 N1 H1N 110(3) . . ? C1 N2 Cr1 130.8(3) . . ? C1 N2 H2N 118(3) . . ? Cr1 N2 H2N 111(3) . . ? C4 N3 Cr1 130.3(3) . . ? C4 N3 H3N 115(3) . . ? Cr1 N3 H3N 115(3) . . ? N2 C1 N1 120.5(3) . . ? N2 C1 C2 124.0(4) . . ? N1 C1 C2 115.5(4) . . ? C3 C2 C1 117.6(5) . . ? C3 C2 H2A 107.9 . . ? C1 C2 H2A 107.9 . . ? C3 C2 H2B 107.9 . . ? C1 C2 H2B 107.9 . . ? H2A C2 H2B 107.2 . . ? H3X1 C3X H3X2 109.5 . . ? H3X1 C3X H3X3 109.5 . . ? H3X2 C3X H3X3 109.5 . . ? N3 C4 N1 119.8(4) . . ? N3 C4 C5 124.5(4) . . ? N1 C4 C5 115.6(3) . . ? C6 C5 C4 116.1(5) . . ? C6 C5 H5A 108.3 . . ? C4 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C4 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? H6X1 C6X H6X2 109.5 . . ? H6X1 C6X H6X3 109.5 . . ? H6X2 C6X H6X3 109.5 . . ? C11 C7 C10 111.6(3) 3_657 . ? C11 C7 C12 110.1(3) 3_657 3_657 ? C10 C7 C12 112.1(3) . 3_657 ? C11 C7 C8 106.6(3) 3_657 . ? C10 C7 C8 107.2(3) . . ? C12 C7 C8 109.0(3) 3_657 . ? C9 C8 C7 117.6(3) . . ? C9 C8 H8A 107.9 . . ? C7 C8 H8A 107.9 . . ? C9 C8 H8B 107.9 . . ? C7 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C10 C7 113.0(3) . . ? O1 C10 H10A 109.0 . . ? C7 C10 H10A 109.0 . . ? O1 C10 H10B 109.0 . . ? C7 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? O3 C11 C7 115.0(3) . 3_657 ? O3 C11 H11A 108.5 . . ? C7 C11 H11A 108.5 3_657 . ? O3 C11 H11B 108.5 . . ? C7 C11 H11B 108.5 3_657 . ? H11A C11 H11B 107.5 . . ? O2 C12 C7 113.2(3) . 3_657 ? O2 C12 H12A 108.9 . . ? C7 C12 H12A 108.9 3_657 . ? O2 C12 H12B 108.9 . . ? C7 C12 H12B 108.9 3_657 . ? H12A C12 H12B 107.7 . . ? N4 C13 C14 172.9(13) . . ? C15 C14 C13 118.4(9) . . ? C15 C14 H14C 107.7 . . ? C13 C14 H14C 107.7 . . ? C15 C14 H14D 107.7 . . ? C13 C14 H14D 107.7 . . ? H14C C14 H14D 107.1 . . ? N4X C13X C14X 160(2) . . ? C13X C14X C15X 103.5(15) . . ? C13X C14X H14A 111.1 . . ? C15X C14X H14A 111.1 . . ? C13X C14X H14B 111.1 . . ? C15X C14X H14B 111.1 . . ? H14A C14X H14B 109.0 . . ? C14X C15X H15A 109.5 . . ? C14X C15X H15B 109.5 . . ? H15A C15X H15B 109.5 . . ? C14X C15X H15C 109.5 . . ? H15A C15X H15C 109.5 . . ? H15B C15X H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cr2 O1 C10 140.5(2) . . . . ? O3 Cr2 O1 C10 -46.59(19) 3_657 . . . ? O1 Cr2 O1 C10 -127.9(2) 3_657 . . . ? Cl3 Cr2 O1 C10 -160.3(5) . . . . ? Cl2 Cr2 O1 C10 48.85(19) . . . . ? O2 Cr2 O1 Cr2 -91.61(9) . . . 3_657 ? O3 Cr2 O1 Cr2 81.31(9) 3_657 . . 3_657 ? O1 Cr2 O1 Cr2 0.0 3_657 . . 3_657 ? Cl3 Cr2 O1 Cr2 -32.4(6) . . . 3_657 ? Cl2 Cr2 O1 Cr2 176.75(7) . . . 3_657 ? O2 Cr2 O1 Cr1 5.50(8) . . . . ? O3 Cr2 O1 Cr1 178.42(9) 3_657 . . . ? O1 Cr2 O1 Cr1 97.11(10) 3_657 . . . ? Cl3 Cr2 O1 Cr1 64.7(6) . . . . ? Cl2 Cr2 O1 Cr1 -86.14(7) . . . . ? O3 Cr1 O1 C10 133.9(2) . . . . ? O2 Cr1 O1 C10 -135.9(2) . . . . ? N3 Cr1 O1 C10 40.7(2) . . . . ? N2 Cr1 O1 C10 -42.3(2) . . . . ? Cl1 Cr1 O1 C10 174.1(5) . . . . ? O3 Cr1 O1 Cr2 6.38(10) . . . 3_657 ? O2 Cr1 O1 Cr2 96.56(10) . . . 3_657 ? N3 Cr1 O1 Cr2 -86.84(11) . . . 3_657 ? N2 Cr1 O1 Cr2 -169.80(12) . . . 3_657 ? Cl1 Cr1 O1 Cr2 46.6(7) . . . 3_657 ? O3 Cr1 O1 Cr2 -95.65(10) . . . . ? O2 Cr1 O1 Cr2 -5.47(8) . . . . ? N3 Cr1 O1 Cr2 171.13(10) . . . . ? N2 Cr1 O1 Cr2 88.17(12) . . . . ? Cl1 Cr1 O1 Cr2 -55.4(7) . . . . ? O3 Cr2 O2 C12 91.6(5) 3_657 . . . ? O1 Cr2 O2 C12 49.9(2) 3_657 . . . ? O1 Cr2 O2 C12 128.5(2) . . . . ? Cl3 Cr2 O2 C12 -45.8(2) . . . . ? Cl2 Cr2 O2 C12 -136.4(2) . . . . ? O3 Cr2 O2 Cr1 -42.8(5) 3_657 . . . ? O1 Cr2 O2 Cr1 -84.49(10) 3_657 . . . ? O1 Cr2 O2 Cr1 -5.87(9) . . . . ? Cl3 Cr2 O2 Cr1 179.86(7) . . . . ? Cl2 Cr2 O2 Cr1 89.24(8) . . . . ? O3 Cr1 O2 C12 -46.4(2) . . . . ? N3 Cr1 O2 C12 -152.7(7) . . . . ? N2 Cr1 O2 C12 141.2(2) . . . . ? O1 Cr1 O2 C12 -126.8(2) . . . . ? Cl1 Cr1 O2 C12 48.12(19) . . . . ? O3 Cr1 O2 Cr2 86.18(10) . . . . ? N3 Cr1 O2 Cr2 -20.1(8) . . . . ? N2 Cr1 O2 Cr2 -86.23(12) . . . . ? O1 Cr1 O2 Cr2 5.80(9) . . . . ? Cl1 Cr1 O2 Cr2 -179.27(7) . . . . ? O2 Cr1 O3 C11 45.4(2) . . . . ? N3 Cr1 O3 C11 -142.1(2) . . . . ? N2 Cr1 O3 C11 154.0(8) . . . . ? O1 Cr1 O3 C11 125.4(2) . . . . ? Cl1 Cr1 O3 C11 -50.3(2) . . . . ? O2 Cr1 O3 Cr2 -86.77(11) . . . 3_657 ? N3 Cr1 O3 Cr2 85.74(12) . . . 3_657 ? N2 Cr1 O3 Cr2 21.8(9) . . . 3_657 ? O1 Cr1 O3 Cr2 -6.76(10) . . . 3_657 ? Cl1 Cr1 O3 Cr2 177.51(9) . . . 3_657 ? O3 Cr1 N2 C1 91.1(9) . . . . ? O2 Cr1 N2 C1 -160.7(4) . . . . ? N3 Cr1 N2 C1 26.5(4) . . . . ? O1 Cr1 N2 C1 119.2(4) . . . . ? Cl1 Cr1 N2 C1 -64.7(4) . . . . ? O3 Cr1 N3 C4 161.2(3) . . . . ? O2 Cr1 N3 C4 -92.8(8) . . . . ? N2 Cr1 N3 C4 -26.0(3) . . . . ? O1 Cr1 N3 C4 -118.3(3) . . . . ? Cl1 Cr1 N3 C4 66.5(3) . . . . ? Cr1 N2 C1 N1 -10.2(6) . . . . ? Cr1 N2 C1 C2 171.1(3) . . . . ? C4 N1 C1 N2 -20.8(6) . . . . ? C4 N1 C1 C2 158.0(3) . . . . ? N2 C1 C2 C3 25.9(11) . . . . ? N1 C1 C2 C3 -152.9(10) . . . . ? Cr1 N3 C4 N1 10.0(5) . . . . ? Cr1 N3 C4 C5 -173.4(3) . . . . ? C1 N1 C4 N3 20.9(6) . . . . ? C1 N1 C4 C5 -156.0(4) . . . . ? N3 C4 C5 C6 -10.5(9) . . . . ? N1 C4 C5 C6 166.2(8) . . . . ? C11 C7 C8 C9 -178.1(3) 3_657 . . . ? C10 C7 C8 C9 -58.5(4) . . . . ? C12 C7 C8 C9 63.1(4) 3_657 . . . ? Cr2 O1 C10 C7 -60.7(3) 3_657 . . . ? Cr2 O1 C10 C7 59.8(3) . . . . ? Cr1 O1 C10 C7 -179.1(2) . . . . ? C11 C7 C10 O1 -61.3(3) 3_657 . . . ? C12 C7 C10 O1 62.8(4) 3_657 . . . ? C8 C7 C10 O1 -177.6(3) . . . . ? Cr2 O3 C11 C7 63.2(3) 3_657 . . 3_657 ? Cr1 O3 C11 C7 -61.4(3) . . . 3_657 ? Cr2 O2 C12 C7 -64.5(3) . . . 3_657 ? Cr1 O2 C12 C7 61.4(3) . . . 3_657 ? N4 C13 C14 C15 44(10) . . . . ? N4X C13X C14X C15X -117(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl2 0.80(2) 2.59(2) 3.352(3) 160(4) 4_565 N2 H2N Cl2 0.78(2) 2.51(3) 3.172(3) 143(3) . N3 H3N Cl3 0.80(2) 2.45(3) 3.142(3) 144(3) 3_657 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.485 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.095 # Attachment '- 7rev.cif' data_rb3 _database_code_depnum_ccdc_archive 'CCDC 810906' #TrackingRef '- 7rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cr4(tmp)2Cl6(Bz-iac)2).0.67(MeCN) _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 Cl6 Cr4 N6 O6, 0.67(MeCN)' _chemical_formula_sum 'C41.33 H50 Cl6 Cr4 N6.67 O6' _chemical_formula_weight 1156.91 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.3367(11) _cell_length_b 23.3367(11) _cell_length_c 23.501(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11084.0(17) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6123 _cell_measurement_theta_min 3.0164 _cell_measurement_theta_max 28.3892 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5316 _exptl_absorpt_coefficient_mu 1.236 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.75011 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(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_type 'Xcalibur, Sapphire2, large Be window' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14806 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5041 _reflns_number_gt 3339 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; ? ; _computing_cell_refinement ; ? ; _computing_data_reduction ; ? ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Restraints were applied to the geometry of the MeCN solvent molecule and the Cr-Cl distances of the disordered Cl atoms, Cl1 and cl3, were restrained to be the same. Also, distance restraints were applied to the N-H bond lengths. ; _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^)+(0.1042P)^2^+64.2239P] 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 5041 _refine_ls_number_parameters 334 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1995 _refine_ls_wR_factor_gt 0.1811 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.005 _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 0.91073(5) 0.50290(4) 0.06482(4) 0.0430(3) Uani 1 1 d D . . Cr2 Cr 1.00103(4) 0.44578(4) 0.04085(4) 0.0352(3) Uani 1 1 d D . . Cl1 Cl 0.7985(2) 0.4590(2) 0.0741(4) 0.0421(15) Uani 0.68(4) 1 d PD A 1 Cl2 Cl 0.98190(7) 0.33974(6) 0.02712(6) 0.0393(3) Uani 1 1 d . A . Cl3 Cl 1.0193(4) 0.4371(5) 0.1377(3) 0.029(2) Uani 0.57(8) 1 d PD A 1 O1 O 0.90825(18) 0.41850(17) 0.05262(16) 0.0413(9) Uani 1 1 d . A . O2 O 0.99115(17) 0.46293(17) -0.04371(15) 0.0361(8) Uani 1 1 d . . . O3 O 0.90637(18) 0.51235(18) -0.01842(17) 0.0418(9) Uani 1 1 d . . . N1 N 0.9288(3) 0.4996(2) 0.1474(2) 0.0489(12) Uani 1 1 d D A . H1N H 0.943(4) 0.474(4) 0.160(3) 0.10(3) Uiso 1 1 d D . . N2 N 0.9586(3) 0.6054(2) 0.1777(2) 0.0512(13) Uani 1 1 d D A . H2N H 0.971(3) 0.628(3) 0.2104(16) 0.06(2) Uiso 1 1 d D . . N3 N 0.9278(3) 0.5944(2) 0.0832(2) 0.0439(12) Uani 1 1 d D A . H3N H 0.926(4) 0.618(3) 0.055(2) 0.07(2) Uiso 1 1 d D . . C1 C 0.9539(3) 0.5449(3) 0.1862(3) 0.0479(14) Uani 1 1 d . . . C2 C 0.9787(3) 0.5336(3) 0.2396(3) 0.0489(15) Uani 1 1 d . A . C3 C 0.9416(4) 0.4742(4) 0.2681(3) 0.068(2) Uani 1 1 d . . . H3 H 0.8997 0.4437 0.2547 0.082 Uiso 1 1 calc R A . C4 C 0.9657(4) 0.4599(4) 0.3153(3) 0.075(2) Uani 1 1 d . A . H4 H 0.9403 0.4200 0.3342 0.090 Uiso 1 1 calc R . . C5 C 1.0286(4) 0.5055(4) 0.3353(4) 0.072(2) Uani 1 1 d . . . H5 H 1.0453 0.4959 0.3675 0.086 Uiso 1 1 calc R A . C6 C 1.0651(4) 0.5636(3) 0.3079(3) 0.0584(18) Uani 1 1 d . A . H6 H 1.1070 0.5941 0.3212 0.070 Uiso 1 1 calc R . . C7 C 1.0399(4) 0.5778(3) 0.2595(3) 0.0534(16) Uani 1 1 d . . . H7 H 1.0651 0.6179 0.2408 0.064 Uiso 1 1 calc R A . C8 C 0.9436(3) 0.6277(3) 0.1296(3) 0.0471(14) Uani 1 1 d . . . C9 C 0.9446(3) 0.6913(3) 0.1341(3) 0.0529(16) Uani 1 1 d . A . C10 C 0.9267(8) 0.7097(6) 0.1820(3) 0.146(6) Uani 1 1 d . . . H10 H 0.9169 0.6835 0.2143 0.176 Uiso 1 1 calc R A . C11 C 0.9222(8) 0.7671(6) 0.1845(3) 0.152(7) Uani 1 1 d . A . H11 H 0.9086 0.7779 0.2180 0.182 Uiso 1 1 calc R . . C12 C 0.9369(6) 0.8052(5) 0.1405(4) 0.097(3) Uani 1 1 d . . . H12 H 0.9336 0.8433 0.1425 0.116 Uiso 1 1 calc R A . C13 C 0.9578(6) 0.7896(5) 0.0902(5) 0.102(3) Uani 1 1 d . A . H13 H 0.9701 0.8180 0.0591 0.123 Uiso 1 1 calc R . . C14 C 0.9600(4) 0.7320(4) 0.0870(4) 0.079(3) Uani 1 1 d . . . H14 H 0.9719 0.7202 0.0530 0.095 Uiso 1 1 calc R A . C15 C 0.8599(3) 0.3710(3) 0.0136(3) 0.0486(15) Uani 1 1 d . . . H15A H 0.8160 0.3591 0.0269 0.058 Uiso 1 1 calc R A . H15B H 0.8633 0.3313 0.0138 0.058 Uiso 1 1 calc R . . H16A H 0.9351 0.4240 -0.1128 0.058 Uiso 1 1 d R . . H16B H 0.9364 0.3707 -0.0730 0.058 Uiso 1 1 d R . . H17A H 0.8140 0.4437 -0.0370 0.058 Uiso 1 1 d R . . H17B H 0.8603 0.4694 -0.0904 0.058 Uiso 1 1 d R . . C16 C 0.9337(3) 0.4108(3) -0.0736(2) 0.0429(14) Uani 1 1 d . . . C17 C 0.8578(3) 0.4563(3) -0.0512(3) 0.0490(15) Uani 1 1 d . . . C18 C 0.8681(3) 0.3965(3) -0.0475(3) 0.0482(15) Uani 1 1 d . A . C19 C 0.8188(4) 0.3419(4) -0.0896(4) 0.044(2) Uani 0.724(10) 1 d P A 1 H19A H 0.8273 0.3603 -0.1277 0.053 Uiso 0.724(10) 1 calc PR A 1 H19B H 0.8279 0.3056 -0.0896 0.053 Uiso 0.724(10) 1 calc PR A 1 C20 C 0.7483(5) 0.3154(5) -0.0763(4) 0.069(3) Uani 0.724(10) 1 d P A 1 H20A H 0.7370 0.3493 -0.0821 0.104 Uiso 0.724(10) 1 calc PR A 1 H20B H 0.7401 0.3010 -0.0374 0.104 Uiso 0.724(10) 1 calc PR A 1 H20C H 0.7218 0.2786 -0.1009 0.104 Uiso 0.724(10) 1 calc PR A 1 C19X C 0.8003(13) 0.3318(13) -0.0641(11) 0.044(2) Uani 0.276(10) 1 d P A 2 H19C H 0.8040 0.2924 -0.0609 0.053 Uiso 0.276(10) 1 calc PR A 2 H19D H 0.7642 0.3269 -0.0402 0.053 Uiso 0.276(10) 1 calc PR A 2 C20X C 0.7903(13) 0.3447(13) -0.1250(11) 0.069(3) Uani 0.276(10) 1 d P A 2 H20D H 0.7542 0.3054 -0.1411 0.104 Uiso 0.276(10) 1 calc PR A 2 H20E H 0.8299 0.3570 -0.1463 0.104 Uiso 0.276(10) 1 calc PR A 2 H20F H 0.7804 0.3800 -0.1264 0.104 Uiso 0.276(10) 1 calc PR A 2 Cl3X Cl 1.033(2) 0.4488(19) 0.1323(9) 0.060(4) Uani 0.43(8) 1 d PD A 2 Cl1X Cl 0.8053(6) 0.4608(6) 0.0958(16) 0.073(4) Uani 0.32(4) 1 d PD A 2 N1S N 0.7000(10) 0.3527(13) 0.1839(8) 0.099(8) Uiso 0.33 1 d PD B -1 C1S C 0.7411(13) 0.3826(14) 0.2168(10) 0.092(8) Uiso 0.33 1 d PD B -1 C2S C 0.7646(12) 0.4127(12) 0.2722(9) 0.076(7) Uiso 0.33 1 d PD B -1 H2S1 H 0.7277 0.4063 0.2950 0.113 Uiso 0.33 1 calc P C -1 H2S2 H 0.7949 0.4592 0.2677 0.113 Uiso 0.33 1 calc P D -1 H2S3 H 0.7867 0.3924 0.2907 0.113 Uiso 0.33 1 calc P E -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0414(5) 0.0374(5) 0.0564(6) -0.0110(4) -0.0078(4) 0.0243(4) Cr2 0.0325(5) 0.0315(5) 0.0457(5) -0.0160(4) -0.0185(4) 0.0189(4) Cl1 0.032(2) 0.0530(16) 0.042(3) 0.0050(16) 0.0030(13) 0.0222(16) Cl2 0.0440(7) 0.0333(7) 0.0459(8) -0.0132(6) -0.0150(6) 0.0233(6) Cl3 0.023(3) 0.023(2) 0.031(3) -0.0084(13) -0.002(3) 0.004(2) O1 0.037(2) 0.0303(19) 0.057(2) -0.0116(17) -0.0148(18) 0.0172(17) O2 0.0363(19) 0.0302(18) 0.045(2) -0.0181(16) -0.0197(16) 0.0191(16) O3 0.033(2) 0.039(2) 0.058(2) -0.0143(18) -0.0176(17) 0.0221(17) N1 0.067(3) 0.038(3) 0.050(3) -0.004(2) 0.002(3) 0.033(3) N2 0.069(4) 0.042(3) 0.055(3) -0.016(2) -0.012(3) 0.037(3) N3 0.055(3) 0.040(3) 0.047(3) -0.004(2) -0.001(2) 0.032(2) C1 0.058(4) 0.042(3) 0.055(4) -0.009(3) -0.006(3) 0.034(3) C2 0.062(4) 0.038(3) 0.056(4) -0.010(3) -0.006(3) 0.032(3) C3 0.072(5) 0.055(4) 0.075(5) 0.002(4) -0.016(4) 0.030(4) C4 0.083(6) 0.049(4) 0.080(5) 0.010(4) -0.016(4) 0.024(4) C5 0.096(6) 0.052(4) 0.085(5) -0.002(4) -0.023(5) 0.051(4) C6 0.065(4) 0.037(3) 0.083(5) -0.020(3) -0.020(4) 0.033(3) C7 0.070(4) 0.040(3) 0.063(4) -0.006(3) 0.000(3) 0.036(3) C8 0.053(4) 0.049(3) 0.052(4) -0.010(3) -0.010(3) 0.035(3) C9 0.065(4) 0.051(4) 0.061(4) -0.017(3) -0.016(3) 0.042(3) C10 0.36(2) 0.161(10) 0.037(4) -0.020(5) -0.033(7) 0.221(13) C11 0.38(2) 0.165(11) 0.038(4) -0.016(5) -0.023(7) 0.231(14) C12 0.161(10) 0.077(6) 0.098(7) -0.020(5) -0.017(6) 0.094(7) C13 0.144(9) 0.071(6) 0.118(8) 0.027(5) 0.052(7) 0.074(6) C14 0.097(6) 0.060(5) 0.098(6) 0.013(4) 0.044(5) 0.051(5) C15 0.030(3) 0.032(3) 0.074(4) -0.014(3) -0.017(3) 0.008(2) C16 0.045(3) 0.032(3) 0.047(3) -0.021(2) -0.029(3) 0.016(3) C17 0.032(3) 0.043(3) 0.065(4) -0.013(3) -0.025(3) 0.014(3) C18 0.040(3) 0.032(3) 0.063(4) -0.012(3) -0.026(3) 0.011(3) C19 0.034(5) 0.035(4) 0.034(6) 0.003(4) -0.012(4) -0.005(4) C20 0.044(5) 0.056(6) 0.068(6) -0.006(5) -0.012(4) -0.004(4) C19X 0.034(5) 0.035(4) 0.034(6) 0.003(4) -0.012(4) -0.005(4) C20X 0.044(5) 0.056(6) 0.068(6) -0.006(5) -0.012(4) -0.004(4) Cl3X 0.074(9) 0.044(7) 0.069(5) -0.018(4) -0.044(5) 0.035(8) Cl1X 0.087(6) 0.078(5) 0.086(11) -0.017(6) -0.027(7) 0.066(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 O1 1.963(4) . ? Cr1 O3 1.977(4) . ? Cr1 N1 1.996(5) . ? Cr1 N3 2.013(5) . ? Cr1 O2 2.073(4) 10_765 ? Cr1 Cl1X 2.265(11) . ? Cr1 Cl1 2.297(4) . ? Cr2 O1 1.947(4) . ? Cr2 O3 1.947(4) 10_765 ? Cr2 O2 2.046(3) 10_765 ? Cr2 O2 2.063(4) . ? Cr2 Cl3X 2.262(12) . ? Cr2 Cl2 2.3070(14) . ? Cr2 Cl3 2.342(7) . ? O1 C15 1.447(6) . ? O2 C16 1.463(6) . ? O2 Cr2 2.046(3) 10_765 ? O2 Cr1 2.073(4) 10_765 ? O3 C17 1.451(6) . ? O3 Cr2 1.947(4) 10_765 ? N1 C1 1.292(8) . ? N1 H1N 0.89(2) . ? N2 C8 1.361(8) . ? N2 C1 1.378(7) . ? N2 H2N 0.89(2) . ? N3 C8 1.282(7) . ? N3 H3N 0.88(2) . ? C1 C2 1.458(9) . ? C2 C7 1.360(9) . ? C2 C3 1.385(10) . ? C3 C4 1.359(10) . ? C3 H3 0.9300 . ? C4 C5 1.395(11) . ? C4 H4 0.9300 . ? C5 C6 1.351(10) . ? C5 H5 0.9300 . ? C6 C7 1.394(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.476(8) . ? C9 C10 1.343(11) . ? C9 C14 1.383(10) . ? C10 C11 1.393(10) . ? C10 H10 0.9300 . ? C11 C12 1.294(13) . ? C11 H11 0.9300 . ? C12 C13 1.395(13) . ? C12 H12 0.9300 . ? C13 C14 1.375(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C18 1.529(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C18 1.523(9) . ? C16 H16A 0.9662 . ? C16 H16B 0.9678 . ? C17 C18 1.532(8) . ? C17 H17A 0.9711 . ? C17 H17B 0.9648 . ? C18 C19 1.566(9) . ? C18 C19X 1.60(2) . ? C19 C20 1.474(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C19X C20X 1.50(4) . ? C19X H19C 0.9700 . ? C19X H19D 0.9700 . ? C20X H20D 0.9600 . ? C20X H20E 0.9600 . ? C20X H20F 0.9600 . ? N1S C1S 1.156(16) . ? C1S C2S 1.450(16) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? 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 O1 Cr1 O3 89.43(16) . . ? O1 Cr1 N1 90.25(18) . . ? O3 Cr1 N1 172.0(2) . . ? O1 Cr1 N3 170.62(19) . . ? O3 Cr1 N3 95.02(18) . . ? N1 Cr1 N3 84.2(2) . . ? O1 Cr1 O2 79.84(15) . 10_765 ? O3 Cr1 O2 80.15(15) . 10_765 ? N1 Cr1 O2 91.9(2) . 10_765 ? N3 Cr1 O2 92.77(18) . 10_765 ? O1 Cr1 Cl1X 97.5(3) . . ? O3 Cr1 Cl1X 105.1(10) . . ? N1 Cr1 Cl1X 82.9(10) . . ? N3 Cr1 Cl1X 89.3(4) . . ? O2 Cr1 Cl1X 174.2(8) 10_765 . ? O1 Cr1 Cl1 96.42(17) . . ? O3 Cr1 Cl1 91.9(3) . . ? N1 Cr1 Cl1 96.1(3) . . ? N3 Cr1 Cl1 91.7(2) . . ? O2 Cr1 Cl1 171.2(3) 10_765 . ? Cl1X Cr1 Cl1 13.3(7) . . ? O1 Cr2 O3 167.48(17) . 10_765 ? O1 Cr2 O2 80.88(15) . 10_765 ? O3 Cr2 O2 89.28(15) 10_765 10_765 ? O1 Cr2 O2 89.22(15) . . ? O3 Cr2 O2 81.11(16) 10_765 . ? O2 Cr2 O2 77.88(14) 10_765 . ? O1 Cr2 Cl3X 99.6(12) . . ? O3 Cr2 Cl3X 88.8(13) 10_765 . ? O2 Cr2 Cl3X 94.5(6) 10_765 . ? O2 Cr2 Cl3X 167.4(13) . . ? O1 Cr2 Cl2 94.70(11) . . ? O3 Cr2 Cl2 94.10(12) 10_765 . ? O2 Cr2 Cl2 171.88(10) 10_765 . ? O2 Cr2 Cl2 95.34(10) . . ? Cl3X Cr2 Cl2 92.9(6) . . ? O1 Cr2 Cl3 93.1(2) . . ? O3 Cr2 Cl3 95.8(2) 10_765 . ? O2 Cr2 Cl3 97.6(2) 10_765 . ? O2 Cr2 Cl3 174.5(2) . . ? Cl3X Cr2 Cl3 7.7(13) . . ? Cl2 Cr2 Cl3 89.4(2) . . ? C15 O1 Cr2 118.3(3) . . ? C15 O1 Cr1 118.8(3) . . ? Cr2 O1 Cr1 102.87(17) . . ? C16 O2 Cr2 116.7(3) . 10_765 ? C16 O2 Cr2 116.5(3) . . ? Cr2 O2 Cr2 102.12(14) 10_765 . ? C16 O2 Cr1 125.5(3) . 10_765 ? Cr2 O2 Cr1 95.80(15) 10_765 10_765 ? Cr2 O2 Cr1 95.52(14) . 10_765 ? C17 O3 Cr2 118.6(3) . 10_765 ? C17 O3 Cr1 119.0(4) . . ? Cr2 O3 Cr1 102.58(16) 10_765 . ? C1 N1 Cr1 132.3(4) . . ? C1 N1 H1N 98(6) . . ? Cr1 N1 H1N 122(6) . . ? C8 N2 C1 127.6(5) . . ? C8 N2 H2N 124(5) . . ? C1 N2 H2N 108(5) . . ? C8 N3 Cr1 132.1(4) . . ? C8 N3 H3N 109(5) . . ? Cr1 N3 H3N 118(5) . . ? N1 C1 N2 120.4(6) . . ? N1 C1 C2 121.2(5) . . ? N2 C1 C2 118.4(5) . . ? C7 C2 C3 119.0(6) . . ? C7 C2 C1 121.4(6) . . ? C3 C2 C1 119.4(6) . . ? C4 C3 C2 120.8(7) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.6(7) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.0(7) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 119.8(7) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C2 C7 C6 120.6(6) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? N3 C8 N2 121.7(5) . . ? N3 C8 C9 121.8(6) . . ? N2 C8 C9 116.5(5) . . ? C10 C9 C14 117.8(6) . . ? C10 C9 C8 122.1(7) . . ? C14 C9 C8 120.0(6) . . ? C9 C10 C11 121.8(8) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 120.4(8) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.3(8) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.4(8) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C9 120.2(7) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? O1 C15 C18 113.6(5) . . ? O1 C15 H15A 108.8 . . ? C18 C15 H15A 108.8 . . ? O1 C15 H15B 108.8 . . ? C18 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? O2 C16 C18 113.1(4) . . ? O2 C16 H16A 108.9 . . ? C18 C16 H16A 108.9 . . ? O2 C16 H16B 108.7 . . ? C18 C16 H16B 108.9 . . ? H16A C16 H16B 108.2 . . ? O3 C17 C18 112.7(4) . . ? O3 C17 H17A 108.7 . . ? C18 C17 H17A 109.1 . . ? O3 C17 H17B 109.0 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.1 . . ? C16 C18 C15 112.4(5) . . ? C16 C18 C17 112.0(5) . . ? C15 C18 C17 111.1(5) . . ? C16 C18 C19 100.0(6) . . ? C15 C18 C19 112.2(5) . . ? C17 C18 C19 108.7(5) . . ? C16 C18 C19X 121.5(12) . . ? C15 C18 C19X 89.4(10) . . ? C17 C18 C19X 108.4(12) . . ? C19 C18 C19X 25.8(8) . . ? C20 C19 C18 114.8(8) . . ? C20 C19 H19A 108.6 . . ? C18 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? C18 C19 H19B 108.6 . . ? H19A C19 H19B 107.5 . . ? C20X C19X C18 102.9(17) . . ? C20X C19X H19C 111.2 . . ? C18 C19X H19C 111.2 . . ? C20X C19X H19D 111.2 . . ? C18 C19X H19D 111.2 . . ? H19C C19X H19D 109.1 . . ? C19X C20X H20D 109.5 . . ? C19X C20X H20E 109.5 . . ? H20D C20X H20E 109.5 . . ? C19X C20X H20F 109.5 . . ? H20D C20X H20F 109.5 . . ? H20E C20X H20F 109.5 . . ? N1S C1S C2S 153(3) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cr2 O1 C15 88.3(8) 10_765 . . . ? O2 Cr2 O1 C15 126.9(4) 10_765 . . . ? O2 Cr2 O1 C15 49.1(4) . . . . ? Cl3X Cr2 O1 C15 -140.0(8) . . . . ? Cl2 Cr2 O1 C15 -46.2(4) . . . . ? Cl3 Cr2 O1 C15 -135.8(4) . . . . ? O3 Cr2 O1 Cr1 -44.8(8) 10_765 . . . ? O2 Cr2 O1 Cr1 -6.21(16) 10_765 . . . ? O2 Cr2 O1 Cr1 -84.06(17) . . . . ? Cl3X Cr2 O1 Cr1 86.9(8) . . . . ? Cl2 Cr2 O1 Cr1 -179.35(14) . . . . ? Cl3 Cr2 O1 Cr1 91.0(3) . . . . ? O3 Cr1 O1 C15 -46.7(4) . . . . ? N1 Cr1 O1 C15 141.4(4) . . . . ? N3 Cr1 O1 C15 -165.1(11) . . . . ? O2 Cr1 O1 C15 -126.7(4) 10_765 . . . ? Cl1X Cr1 O1 C15 58.5(10) . . . . ? Cl1 Cr1 O1 C15 45.2(5) . . . . ? O3 Cr1 O1 Cr2 86.24(18) . . . . ? N1 Cr1 O1 Cr2 -85.7(2) . . . . ? N3 Cr1 O1 Cr2 -32.2(13) . . . . ? O2 Cr1 O1 Cr2 6.14(16) 10_765 . . . ? Cl1X Cr1 O1 Cr2 -168.6(10) . . . . ? Cl1 Cr1 O1 Cr2 178.1(3) . . . . ? O1 Cr2 O2 C16 -47.5(3) . . . . ? O3 Cr2 O2 C16 140.5(4) 10_765 . . . ? O2 Cr2 O2 C16 -128.3(4) 10_765 . . . ? Cl3X Cr2 O2 C16 178(2) . . . . ? Cl2 Cr2 O2 C16 47.1(3) . . . . ? Cl3 Cr2 O2 C16 -163(2) . . . . ? O1 Cr2 O2 Cr2 80.84(16) . . . 10_765 ? O3 Cr2 O2 Cr2 -91.19(17) 10_765 . . 10_765 ? O2 Cr2 O2 Cr2 0.0 10_765 . . 10_765 ? Cl3X Cr2 O2 Cr2 -54(2) . . . 10_765 ? Cl2 Cr2 O2 Cr2 175.49(13) . . . 10_765 ? Cl3 Cr2 O2 Cr2 -35(2) . . . 10_765 ? O1 Cr2 O2 Cr1 178.00(14) . . . 10_765 ? O3 Cr2 O2 Cr1 5.97(14) 10_765 . . 10_765 ? O2 Cr2 O2 Cr1 97.16(17) 10_765 . . 10_765 ? Cl3X Cr2 O2 Cr1 43(2) . . . 10_765 ? Cl2 Cr2 O2 Cr1 -87.35(11) . . . 10_765 ? Cl3 Cr2 O2 Cr1 62(2) . . . 10_765 ? O1 Cr1 O3 C17 47.1(4) . . . . ? N1 Cr1 O3 C17 134.8(12) . . . . ? N3 Cr1 O3 C17 -141.2(4) . . . . ? O2 Cr1 O3 C17 126.8(4) 10_765 . . . ? Cl1X Cr1 O3 C17 -50.6(5) . . . . ? Cl1 Cr1 O3 C17 -49.4(4) . . . . ? O1 Cr1 O3 Cr2 -86.16(18) . . . 10_765 ? N1 Cr1 O3 Cr2 1.6(13) . . . 10_765 ? N3 Cr1 O3 Cr2 85.6(2) . . . 10_765 ? O2 Cr1 O3 Cr2 -6.37(15) 10_765 . . 10_765 ? Cl1X Cr1 O3 Cr2 176.2(3) . . . 10_765 ? Cl1 Cr1 O3 Cr2 177.44(18) . . . 10_765 ? O1 Cr1 N1 C1 159.7(6) . . . . ? O3 Cr1 N1 C1 72.1(15) . . . . ? N3 Cr1 N1 C1 -12.7(6) . . . . ? O2 Cr1 N1 C1 79.9(6) 10_765 . . . ? Cl1X Cr1 N1 C1 -102.7(7) . . . . ? Cl1 Cr1 N1 C1 -103.8(6) . . . . ? O1 Cr1 N3 C8 -53.1(15) . . . . ? O3 Cr1 N3 C8 -171.2(6) . . . . ? N1 Cr1 N3 C8 0.8(6) . . . . ? O2 Cr1 N3 C8 -90.8(6) 10_765 . . . ? Cl1X Cr1 N3 C8 83.7(11) . . . . ? Cl1 Cr1 N3 C8 96.8(6) . . . . ? Cr1 N1 C1 N2 16.2(10) . . . . ? Cr1 N1 C1 C2 -162.9(5) . . . . ? C8 N2 C1 N1 -5.1(11) . . . . ? C8 N2 C1 C2 174.1(6) . . . . ? N1 C1 C2 C7 129.9(7) . . . . ? N2 C1 C2 C7 -49.3(9) . . . . ? N1 C1 C2 C3 -44.6(9) . . . . ? N2 C1 C2 C3 136.2(7) . . . . ? C7 C2 C3 C4 0.0(11) . . . . ? C1 C2 C3 C4 174.6(7) . . . . ? C2 C3 C4 C5 -0.2(13) . . . . ? C3 C4 C5 C6 0.3(13) . . . . ? C4 C5 C6 C7 -0.1(11) . . . . ? C3 C2 C7 C6 0.2(10) . . . . ? C1 C2 C7 C6 -174.3(6) . . . . ? C5 C6 C7 C2 -0.1(10) . . . . ? Cr1 N3 C8 N2 6.8(10) . . . . ? Cr1 N3 C8 C9 -171.4(5) . . . . ? C1 N2 C8 N3 -6.1(11) . . . . ? C1 N2 C8 C9 172.1(6) . . . . ? N3 C8 C9 C10 144.4(10) . . . . ? N2 C8 C9 C10 -33.9(12) . . . . ? N3 C8 C9 C14 -31.1(11) . . . . ? N2 C8 C9 C14 150.6(7) . . . . ? C14 C9 C10 C11 1.2(19) . . . . ? C8 C9 C10 C11 -174.4(12) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? C10 C11 C12 C13 0(2) . . . . ? C11 C12 C13 C14 2.6(19) . . . . ? C12 C13 C14 C9 -2.9(16) . . . . ? C10 C9 C14 C13 1.0(15) . . . . ? C8 C9 C14 C13 176.7(9) . . . . ? Cr2 O1 C15 C18 -64.0(6) . . . . ? Cr1 O1 C15 C18 61.7(6) . . . . ? Cr2 O2 C16 C18 -60.6(5) 10_765 . . . ? Cr2 O2 C16 C18 60.3(5) . . . . ? Cr1 O2 C16 C18 179.5(3) 10_765 . . . ? Cr2 O3 C17 C18 64.2(6) 10_765 . . . ? Cr1 O3 C17 C18 -61.6(6) . . . . ? O2 C16 C18 C15 -62.5(6) . . . . ? O2 C16 C18 C17 63.4(6) . . . . ? O2 C16 C18 C19 178.3(5) . . . . ? O2 C16 C18 C19X -166.3(12) . . . . ? O1 C15 C18 C16 63.4(6) . . . . ? O1 C15 C18 C17 -63.0(6) . . . . ? O1 C15 C18 C19 175.2(6) . . . . ? O1 C15 C18 C19X -172.5(12) . . . . ? O3 C17 C18 C16 -64.0(7) . . . . ? O3 C17 C18 C15 62.6(6) . . . . ? O3 C17 C18 C19 -173.5(6) . . . . ? O3 C17 C18 C19X 159.3(11) . . . . ? C16 C18 C19 C20 179.6(8) . . . . ? C15 C18 C19 C20 60.3(9) . . . . ? C17 C18 C19 C20 -62.9(9) . . . . ? C19X C18 C19 C20 31(3) . . . . ? C16 C18 C19X C20X -69(2) . . . . ? C15 C18 C19X C20X 175(2) . . . . ? C17 C18 C19X C20X 63(2) . . . . ? C19 C18 C19X C20X -32(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N Cl2 0.88(2) 2.70(7) 3.206(5) 118(6) 10_765 N2 H2N Cl2 0.89(2) 2.59(2) 3.484(5) 179(6) 14_565 N1 H1N Cl3X 0.89(2) 2.51(7) 3.21(2) 136(7) . N1 H1N Cl3 0.89(2) 2.38(6) 3.118(10) 141(7) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.440 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.108