Complex 1a data_sg107_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H28 Cl3 Cr N2 S2' _chemical_formula_weight 482.88 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' 'S' 'S' 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 9.0956(3) _cell_length_b 13.9065(4) _cell_length_c 17.8684(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.4240(10) _cell_angle_gamma 90.00 _cell_volume 2258.11(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3864 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8932 _exptl_absorpt_correction_T_max 0.9592 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8421 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5499 _reflns_number_gt 4432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0415P)^2^+1.0180P] 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 5499 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.24467(4) 0.74430(2) 0.247015(17) 0.02041(9) Uani 1 1 d . . . N1 N 0.22163(19) 0.88203(12) 0.20380(9) 0.0219(3) Uani 1 1 d . . . S1 S 0.49489(6) 0.79827(4) 0.28035(3) 0.02474(12) Uani 1 1 d . . . S2 S -0.01272(6) 0.72859(4) 0.20721(3) 0.02515(12) Uani 1 1 d . . . Cl1 Cl 0.34872(6) 0.69905(4) 0.13686(3) 0.03150(13) Uani 1 1 d . . . Cl2 Cl 0.27546(6) 0.59214(4) 0.29442(3) 0.03106(13) Uani 1 1 d . . . Cl3 Cl 0.13261(6) 0.79570(4) 0.35447(3) 0.03108(13) Uani 1 1 d . . . C1 C 0.3419(2) 0.93752(15) 0.19568(12) 0.0246(4) Uani 1 1 d . . . C2 C 0.3298(3) 1.03180(16) 0.17065(13) 0.0317(5) Uani 1 1 d . . . H2A H 0.4150 1.0706 0.1666 0.038 Uiso 1 1 calc R . . C3 C 0.1921(3) 1.06839(17) 0.15176(14) 0.0355(5) Uani 1 1 d . . . H3A H 0.1817 1.1328 0.1347 0.043 Uiso 1 1 calc R . . C4 C 0.0697(3) 1.01087(16) 0.15784(13) 0.0322(5) Uani 1 1 d . . . H4A H -0.0253 1.0346 0.1436 0.039 Uiso 1 1 calc R . . C5 C 0.0870(2) 0.91775(15) 0.18508(12) 0.0244(4) Uani 1 1 d . . . C6 C 0.4910(2) 0.89301(16) 0.21052(12) 0.0281(5) Uani 1 1 d . . . H6A H 0.5609 0.9441 0.2272 0.034 Uiso 1 1 calc R . . H6B H 0.5257 0.8664 0.1630 0.034 Uiso 1 1 calc R . . C7 C 0.5332(3) 0.86353(17) 0.37031(12) 0.0306(5) Uani 1 1 d . . . C8 C 0.5025(3) 0.7899(2) 0.43086(14) 0.0413(6) Uani 1 1 d . . . H8A H 0.5208 0.8190 0.4803 0.062 Uiso 1 1 calc R . . H8B H 0.5674 0.7342 0.4256 0.062 Uiso 1 1 calc R . . H8C H 0.3997 0.7690 0.4256 0.062 Uiso 1 1 calc R . . C9 C 0.6965(3) 0.8907(2) 0.37167(15) 0.0410(6) Uani 1 1 d . . . H9A H 0.7225 0.9253 0.4181 0.062 Uiso 1 1 calc R . . H9B H 0.7153 0.9319 0.3286 0.062 Uiso 1 1 calc R . . H9C H 0.7561 0.8322 0.3691 0.062 Uiso 1 1 calc R . . C10 C 0.4386(3) 0.95334(18) 0.37708(14) 0.0391(6) Uani 1 1 d . . . H10A H 0.4628 0.9852 0.4250 0.059 Uiso 1 1 calc R . . H10B H 0.3345 0.9352 0.3748 0.059 Uiso 1 1 calc R . . H10C H 0.4579 0.9974 0.3358 0.059 Uiso 1 1 calc R . . C11 C -0.0471(2) 0.85700(16) 0.19836(13) 0.0292(5) Uani 1 1 d . . . H11A H -0.1198 0.8674 0.1563 0.035 Uiso 1 1 calc R . . H11B H -0.0920 0.8798 0.2447 0.035 Uiso 1 1 calc R . . C12 C -0.0688(3) 0.67704(17) 0.11450(13) 0.0318(5) Uani 1 1 d . . . C13 C -0.0102(3) 0.57349(19) 0.11871(16) 0.0458(7) Uani 1 1 d . . . H13A H -0.0356 0.5401 0.0716 0.069 Uiso 1 1 calc R . . H13B H -0.0547 0.5397 0.1602 0.069 Uiso 1 1 calc R . . H13C H 0.0969 0.5746 0.1270 0.069 Uiso 1 1 calc R . . C14 C -0.2365(3) 0.6776(2) 0.11121(15) 0.0431(6) Uani 1 1 d . . . H14A H -0.2730 0.6507 0.0632 0.065 Uiso 1 1 calc R . . H14B H -0.2719 0.7438 0.1159 0.065 Uiso 1 1 calc R . . H14C H -0.2725 0.6386 0.1523 0.065 Uiso 1 1 calc R . . C15 C -0.0077(3) 0.7320(2) 0.04902(14) 0.0431(6) Uani 1 1 d . . . H15A H -0.0412 0.7015 0.0019 0.065 Uiso 1 1 calc R . . H15B H 0.1001 0.7313 0.0531 0.065 Uiso 1 1 calc R . . H15C H -0.0427 0.7986 0.0499 0.065 Uiso 1 1 calc R . . N2 N 0.3268(4) 0.4189(2) 0.45639(15) 0.0689(8) Uani 1 1 d . . . C16 C 0.3018(3) 0.4954(2) 0.47355(14) 0.0428(6) Uani 1 1 d . . . C17 C 0.2706(4) 0.5928(2) 0.49548(15) 0.0544(8) Uani 1 1 d . . . H17A H 0.1864 0.5932 0.5279 0.082 Uiso 1 1 calc R . . H17B H 0.2475 0.6316 0.4507 0.082 Uiso 1 1 calc R . . H17C H 0.3568 0.6199 0.5227 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01849(15) 0.02082(16) 0.02192(18) 0.00137(12) 0.00073(12) 0.00068(12) N1 0.0228(9) 0.0228(8) 0.0202(8) 0.0011(6) 0.0028(7) 0.0000(7) S1 0.0209(2) 0.0245(2) 0.0286(3) 0.00209(19) -0.0016(2) 0.0000(2) S2 0.0205(2) 0.0282(3) 0.0266(3) 0.00369(19) -0.00047(19) -0.0018(2) Cl1 0.0302(3) 0.0359(3) 0.0288(3) -0.0048(2) 0.0062(2) 0.0018(2) Cl2 0.0298(3) 0.0244(2) 0.0390(3) 0.0075(2) 0.0020(2) 0.0031(2) Cl3 0.0303(3) 0.0393(3) 0.0239(3) -0.0016(2) 0.0049(2) 0.0023(2) C1 0.0261(11) 0.0251(10) 0.0227(10) 0.0013(8) 0.0018(8) -0.0031(9) C2 0.0355(13) 0.0244(10) 0.0353(13) 0.0041(9) 0.0009(10) -0.0053(9) C3 0.0454(15) 0.0238(11) 0.0376(13) 0.0034(9) 0.0032(11) 0.0048(10) C4 0.0312(12) 0.0284(11) 0.0371(13) 0.0022(9) 0.0016(10) 0.0080(9) C5 0.0241(11) 0.0264(10) 0.0228(10) -0.0011(8) 0.0033(8) 0.0043(8) C6 0.0252(11) 0.0292(10) 0.0300(12) 0.0064(9) 0.0015(9) -0.0049(9) C7 0.0287(12) 0.0343(12) 0.0281(12) -0.0005(9) -0.0065(9) -0.0044(9) C8 0.0389(14) 0.0490(15) 0.0354(14) 0.0094(11) -0.0071(11) -0.0098(12) C9 0.0319(13) 0.0464(15) 0.0438(15) 0.0032(11) -0.0103(11) -0.0103(11) C10 0.0442(15) 0.0353(13) 0.0373(14) -0.0078(10) -0.0033(11) -0.0001(11) C11 0.0241(11) 0.0297(11) 0.0338(12) 0.0006(9) 0.0026(9) 0.0048(9) C12 0.0306(12) 0.0345(12) 0.0296(12) 0.0003(9) -0.0070(9) -0.0033(10) C13 0.0493(17) 0.0346(13) 0.0526(17) -0.0081(12) -0.0102(13) 0.0013(12) C14 0.0329(13) 0.0463(15) 0.0488(16) 0.0041(12) -0.0136(11) -0.0100(12) C15 0.0398(14) 0.0572(17) 0.0320(14) 0.0029(11) -0.0030(11) -0.0031(13) N2 0.110(3) 0.0465(15) 0.0503(16) -0.0079(12) 0.0029(15) 0.0077(16) C16 0.0591(18) 0.0388(14) 0.0305(13) -0.0001(10) 0.0023(12) -0.0037(13) C17 0.091(3) 0.0361(14) 0.0374(16) 0.0013(11) 0.0127(15) 0.0043(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.0724(17) . ? Cr1 Cl2 2.2921(6) . ? Cr1 Cl1 2.3072(6) . ? Cr1 Cl3 2.3242(6) . ? Cr1 S2 2.4277(6) . ? Cr1 S1 2.4460(6) . ? N1 C1 1.351(3) . ? N1 C5 1.350(3) . ? S1 C6 1.814(2) . ? S1 C7 1.866(2) . ? S2 C11 1.819(2) . ? S2 C12 1.857(2) . ? C1 C2 1.388(3) . ? C1 C6 1.505(3) . ? C2 C3 1.380(3) . ? C3 C4 1.379(3) . ? C4 C5 1.390(3) . ? C5 C11 1.511(3) . ? C7 C10 1.524(3) . ? C7 C8 1.524(3) . ? C7 C9 1.532(3) . ? C12 C14 1.524(3) . ? C12 C15 1.522(4) . ? C12 C13 1.536(3) . ? N2 C16 1.133(4) . ? C16 C17 1.442(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 Cl2 178.77(5) . . ? N1 Cr1 Cl1 88.45(5) . . ? Cl2 Cr1 Cl1 90.88(2) . . ? N1 Cr1 Cl3 89.01(5) . . ? Cl2 Cr1 Cl3 91.69(2) . . ? Cl1 Cr1 Cl3 177.04(2) . . ? N1 Cr1 S2 83.85(5) . . ? Cl2 Cr1 S2 97.26(2) . . ? Cl1 Cr1 S2 98.67(2) . . ? Cl3 Cr1 S2 79.55(2) . . ? N1 Cr1 S1 83.43(5) . . ? Cl2 Cr1 S1 95.47(2) . . ? Cl1 Cr1 S1 83.13(2) . . ? Cl3 Cr1 S1 98.08(2) . . ? S2 Cr1 S1 167.10(2) . . ? C1 N1 C5 119.53(18) . . ? C1 N1 Cr1 119.88(14) . . ? C5 N1 Cr1 120.58(14) . . ? C6 S1 C7 103.70(11) . . ? C6 S1 Cr1 93.71(7) . . ? C7 S1 Cr1 119.79(8) . . ? C11 S2 C12 105.18(10) . . ? C11 S2 Cr1 95.59(7) . . ? C12 S2 Cr1 121.43(8) . . ? N1 C1 C2 121.4(2) . . ? N1 C1 C6 118.30(18) . . ? C2 C1 C6 120.3(2) . . ? C1 C2 C3 119.1(2) . . ? C4 C3 C2 119.6(2) . . ? C3 C4 C5 119.2(2) . . ? N1 C5 C4 121.2(2) . . ? N1 C5 C11 119.03(18) . . ? C4 C5 C11 119.7(2) . . ? C1 C6 S1 114.27(15) . . ? C10 C7 C8 111.9(2) . . ? C10 C7 C9 110.3(2) . . ? C8 C7 C9 111.15(19) . . ? C10 C7 S1 112.43(15) . . ? C8 C7 S1 104.57(16) . . ? C9 C7 S1 106.20(17) . . ? C5 C11 S2 115.18(15) . . ? C14 C12 C15 111.4(2) . . ? C14 C12 C13 110.6(2) . . ? C15 C12 C13 111.8(2) . . ? C14 C12 S2 105.63(17) . . ? C15 C12 S2 113.35(17) . . ? C13 C12 S2 103.69(16) . . ? N2 C16 C17 179.7(4) . . ? 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 Cl2 Cr1 N1 C1 -14(2) . . . . ? Cl1 Cr1 N1 C1 -70.78(15) . . . . ? Cl3 Cr1 N1 C1 110.74(15) . . . . ? S2 Cr1 N1 C1 -169.67(15) . . . . ? S1 Cr1 N1 C1 12.49(15) . . . . ? Cl2 Cr1 N1 C5 167(2) . . . . ? Cl1 Cr1 N1 C5 110.62(15) . . . . ? Cl3 Cr1 N1 C5 -67.87(15) . . . . ? S2 Cr1 N1 C5 11.73(15) . . . . ? S1 Cr1 N1 C5 -166.12(15) . . . . ? N1 Cr1 S1 C6 -22.04(9) . . . . ? Cl2 Cr1 S1 C6 157.41(8) . . . . ? Cl1 Cr1 S1 C6 67.18(8) . . . . ? Cl3 Cr1 S1 C6 -110.09(8) . . . . ? S2 Cr1 S1 C6 -31.69(13) . . . . ? N1 Cr1 S1 C7 86.05(10) . . . . ? Cl2 Cr1 S1 C7 -94.51(9) . . . . ? Cl1 Cr1 S1 C7 175.27(9) . . . . ? Cl3 Cr1 S1 C7 -2.01(9) . . . . ? S2 Cr1 S1 C7 76.40(14) . . . . ? N1 Cr1 S2 C11 -17.50(9) . . . . ? Cl2 Cr1 S2 C11 163.01(8) . . . . ? Cl1 Cr1 S2 C11 -104.98(8) . . . . ? Cl3 Cr1 S2 C11 72.62(8) . . . . ? S1 Cr1 S2 C11 -7.86(14) . . . . ? N1 Cr1 S2 C12 94.10(10) . . . . ? Cl2 Cr1 S2 C12 -85.39(9) . . . . ? Cl1 Cr1 S2 C12 6.62(9) . . . . ? Cl3 Cr1 S2 C12 -175.78(9) . . . . ? S1 Cr1 S2 C12 103.74(14) . . . . ? C5 N1 C1 C2 2.1(3) . . . . ? Cr1 N1 C1 C2 -176.56(16) . . . . ? C5 N1 C1 C6 -174.70(18) . . . . ? Cr1 N1 C1 C6 6.7(3) . . . . ? N1 C1 C2 C3 -1.8(3) . . . . ? C6 C1 C2 C3 174.9(2) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C2 C3 C4 C5 1.9(4) . . . . ? C1 N1 C5 C4 -0.3(3) . . . . ? Cr1 N1 C5 C4 178.34(16) . . . . ? C1 N1 C5 C11 -176.70(19) . . . . ? Cr1 N1 C5 C11 1.9(3) . . . . ? C3 C4 C5 N1 -1.7(3) . . . . ? C3 C4 C5 C11 174.7(2) . . . . ? N1 C1 C6 S1 -30.5(3) . . . . ? C2 C1 C6 S1 152.66(18) . . . . ? C7 S1 C6 C1 -89.25(17) . . . . ? Cr1 S1 C6 C1 32.63(16) . . . . ? C6 S1 C7 C10 45.8(2) . . . . ? Cr1 S1 C7 C10 -56.64(19) . . . . ? C6 S1 C7 C8 167.51(16) . . . . ? Cr1 S1 C7 C8 65.03(17) . . . . ? C6 S1 C7 C9 -74.86(17) . . . . ? Cr1 S1 C7 C9 -177.35(13) . . . . ? N1 C5 C11 S2 -20.7(3) . . . . ? C4 C5 C11 S2 162.80(17) . . . . ? C12 S2 C11 C5 -100.40(18) . . . . ? Cr1 S2 C11 C5 24.31(16) . . . . ? C11 S2 C12 C14 -74.59(18) . . . . ? Cr1 S2 C12 C14 178.91(13) . . . . ? C11 S2 C12 C15 47.7(2) . . . . ? Cr1 S2 C12 C15 -58.8(2) . . . . ? C11 S2 C12 C13 169.09(17) . . . . ? Cr1 S2 C12 C13 62.60(19) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.402 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.070 ===END=== data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H49 Cl3 Cr N S2' _chemical_formula_weight 610.14 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' 'S' 'S' 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.353(3) _cell_length_b 13.518(2) _cell_length_c 14.550(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.877(4) _cell_angle_gamma 90.00 _cell_volume 3147.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6013 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 29.45 _exptl_crystal_description thin_plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 '\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24797 _diffrn_reflns_av_R_equivalents 0.1092 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4510 _reflns_number_gt 2950 _reflns_threshold_expression I>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^)+(0.0499P)^2^+27.6961P] 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 4510 _refine_ls_number_parameters 516 _refine_ls_number_restraints 596 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1855 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.016 _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 0.11632(7) 0.22829(8) 0.23333(7) 0.0174(3) Uani 1 1 d . . . Cl1 Cl 0.22745(11) 0.17050(16) 0.34279(12) 0.0341(5) Uani 1 1 d . A . Cl2 Cl 0.12399(12) 0.37900(14) 0.30528(12) 0.0290(5) Uani 1 1 d . A . Cl3 Cl 0.0088(15) 0.2802(12) 0.1130(18) 0.016(2) Uani 0.50(12) 1 d P A 1 Cl3A Cl -0.008(3) 0.2752(11) 0.136(4) 0.023(6) Uani 0.50(12) 1 d P A 2 N1 N 0.1096(3) 0.0949(4) 0.1630(4) 0.0195(13) Uani 1 1 d . A . C1 C 0.1276(4) 0.0909(5) 0.0760(5) 0.0242(17) Uani 1 1 d . . . C2 C 0.1207(5) 0.0042(5) 0.0253(5) 0.0285(18) Uani 1 1 d . A . H2A H 0.1350 0.0025 -0.0348 0.034 Uiso 1 1 calc R . . C3 C 0.0927(5) -0.0811(6) 0.0631(5) 0.0285(18) Uani 1 1 d . . . H3A H 0.0864 -0.1414 0.0287 0.034 Uiso 1 1 calc R A . C4 C 0.0743(4) -0.0762(5) 0.1507(5) 0.0269(18) Uani 1 1 d . A . H4A H 0.0549 -0.1335 0.1776 0.032 Uiso 1 1 calc R . . C5 C 0.0838(4) 0.0115(5) 0.1999(5) 0.0224(17) Uani 1 1 d . . . C6 C 0.1499(5) 0.1850(6) 0.0337(5) 0.034(2) Uani 1 1 d . A . H6A H 0.0982 0.2186 0.0012 0.041 Uiso 1 1 calc R B 1 H6B H 0.1838 0.1700 -0.0136 0.041 Uiso 1 1 calc R B 1 C7 C 0.0692(5) 0.0189(5) 0.2988(5) 0.0263(17) Uani 1 1 d . A . H7A H 0.1222 0.0066 0.3442 0.032 Uiso 1 1 calc R C 1 H7B H 0.0283 -0.0320 0.3087 0.032 Uiso 1 1 calc R C 1 S1 S 0.2084(4) 0.2674(5) 0.1228(5) 0.0149(12) Uani 0.652(5) 1 d PD A 1 C8 C 0.3080(6) 0.2062(9) 0.1657(8) 0.023(2) Uani 0.652(5) 1 d PDU A 1 H8A H 0.3397 0.2437 0.2200 0.028 Uiso 0.652(5) 1 calc PR A 1 H8B H 0.2975 0.1391 0.1879 0.028 Uiso 0.652(5) 1 calc PR A 1 C9 C 0.3609(7) 0.1979(8) 0.0907(8) 0.024(2) Uani 0.652(5) 1 d PDU A 1 H9A H 0.4098 0.1554 0.1155 0.029 Uiso 0.652(5) 1 calc PR A 1 H9B H 0.3273 0.1642 0.0352 0.029 Uiso 0.652(5) 1 calc PR A 1 C10 C 0.3923(7) 0.2956(7) 0.0590(7) 0.020(2) Uani 0.652(5) 1 d PDU A 1 H10A H 0.4273 0.3294 0.1136 0.024 Uiso 0.652(5) 1 calc PR A 1 H10B H 0.3440 0.3389 0.0338 0.024 Uiso 0.652(5) 1 calc PR A 1 C11 C 0.4436(7) 0.2794(9) -0.0167(8) 0.021(2) Uani 0.652(5) 1 d PDU A 1 H11A H 0.4920 0.2367 0.0093 0.025 Uiso 0.652(5) 1 calc PR A 1 H11B H 0.4086 0.2436 -0.0701 0.025 Uiso 0.652(5) 1 calc PR A 1 C12 C 0.4754(9) 0.3739(9) -0.0532(9) 0.022(2) Uani 0.652(5) 1 d PDU A 1 H12A H 0.5128 0.4078 -0.0005 0.027 Uiso 0.652(5) 1 calc PR A 1 H12B H 0.4272 0.4182 -0.0759 0.027 Uiso 0.652(5) 1 calc PR A 1 C13 C 0.5224(12) 0.3590(9) -0.1323(11) 0.022(2) Uani 0.652(5) 1 d PDU A 1 H13A H 0.5693 0.3128 -0.1105 0.027 Uiso 0.652(5) 1 calc PR A 1 H13B H 0.4843 0.3275 -0.1860 0.027 Uiso 0.652(5) 1 calc PR A 1 C14 C 0.5565(8) 0.4531(9) -0.1659(8) 0.021(2) Uani 0.652(5) 1 d PDU A 1 H14A H 0.5995 0.4806 -0.1142 0.025 Uiso 0.652(5) 1 calc PR A 1 H14B H 0.5107 0.5021 -0.1810 0.025 Uiso 0.652(5) 1 calc PR A 1 C15 C 0.5952(9) 0.4392(10) -0.2523(10) 0.022(3) Uani 0.652(5) 1 d PDU A 1 H15A H 0.6392 0.3878 -0.2381 0.027 Uiso 0.652(5) 1 calc PR A 1 H15B H 0.5516 0.4145 -0.3048 0.027 Uiso 0.652(5) 1 calc PR A 1 C16 C 0.6328(8) 0.5313(10) -0.2836(9) 0.022(3) Uani 0.652(5) 1 d PDU A 1 H16A H 0.6806 0.5522 -0.2339 0.026 Uiso 0.652(5) 1 calc PR A 1 H16B H 0.5906 0.5849 -0.2919 0.026 Uiso 0.652(5) 1 calc PR A 1 C17 C 0.6627(9) 0.5172(14) -0.3750(11) 0.027(4) Uani 0.652(5) 1 d PDU A 1 H17A H 0.6866 0.5793 -0.3922 0.041 Uiso 0.652(5) 1 calc PR A 1 H17B H 0.6154 0.4980 -0.4248 0.041 Uiso 0.652(5) 1 calc PR A 1 H17C H 0.7054 0.4653 -0.3668 0.041 Uiso 0.652(5) 1 calc PR A 1 S1A S 0.1814(7) 0.2887(9) 0.1183(11) 0.016(2) Uani 0.348(5) 1 d PDU A 2 C8A C 0.2876(10) 0.2443(17) 0.1455(15) 0.023(3) Uani 0.348(5) 1 d PDU A 2 H8AA H 0.3170 0.2738 0.2055 0.028 Uiso 0.348(5) 1 calc PR A 2 H8AB H 0.2875 0.1716 0.1535 0.028 Uiso 0.348(5) 1 calc PR A 2 C9A C 0.3351(10) 0.2708(16) 0.0671(13) 0.023(3) Uani 0.348(5) 1 d PDU A 2 H9AA H 0.3092 0.2356 0.0087 0.028 Uiso 0.348(5) 1 calc PR A 2 H9AB H 0.3303 0.3427 0.0545 0.028 Uiso 0.348(5) 1 calc PR A 2 C10A C 0.4269(10) 0.2425(16) 0.0951(13) 0.025(3) Uani 0.348(5) 1 d PDU A 2 H10C H 0.4315 0.1762 0.1245 0.030 Uiso 0.348(5) 1 calc PR A 2 H10D H 0.4558 0.2902 0.1425 0.030 Uiso 0.348(5) 1 calc PR A 2 C11A C 0.4715(13) 0.2410(15) 0.0113(14) 0.023(3) Uani 0.348(5) 1 d PDU A 2 H11C H 0.5308 0.2234 0.0352 0.028 Uiso 0.348(5) 1 calc PR A 2 H11D H 0.4463 0.1879 -0.0323 0.028 Uiso 0.348(5) 1 calc PR A 2 C12A C 0.4684(17) 0.3360(17) -0.0437(16) 0.022(3) Uani 0.348(5) 1 d PDU A 2 H12C H 0.4905 0.3903 0.0001 0.026 Uiso 0.348(5) 1 calc PR A 2 H12D H 0.4094 0.3516 -0.0716 0.026 Uiso 0.348(5) 1 calc PR A 2 C13A C 0.518(2) 0.3327(19) -0.121(2) 0.022(3) Uani 0.348(5) 1 d PDU A 2 H13C H 0.5747 0.3083 -0.0944 0.027 Uiso 0.348(5) 1 calc PR A 2 H13D H 0.4910 0.2836 -0.1688 0.027 Uiso 0.348(5) 1 calc PR A 2 C14A C 0.5255(15) 0.4292(17) -0.1713(16) 0.022(3) Uani 0.348(5) 1 d PDU A 2 H14C H 0.5547 0.4779 -0.1252 0.026 Uiso 0.348(5) 1 calc PR A 2 H14D H 0.4689 0.4552 -0.1973 0.026 Uiso 0.348(5) 1 calc PR A 2 C15A C 0.5730(18) 0.419(2) -0.2509(19) 0.023(3) Uani 0.348(5) 1 d PDU A 2 H15C H 0.6233 0.3780 -0.2289 0.028 Uiso 0.348(5) 1 calc PR A 2 H15D H 0.5371 0.3842 -0.3040 0.028 Uiso 0.348(5) 1 calc PR A 2 C16A C 0.5996(16) 0.516(2) -0.2856(18) 0.024(3) Uani 0.348(5) 1 d PDU A 2 H16C H 0.6426 0.5470 -0.2358 0.029 Uiso 0.348(5) 1 calc PR A 2 H16D H 0.5509 0.5617 -0.2989 0.029 Uiso 0.348(5) 1 calc PR A 2 C17A C 0.635(2) 0.504(3) -0.374(2) 0.029(5) Uani 0.348(5) 1 d PDU A 2 H17D H 0.6527 0.5680 -0.3937 0.044 Uiso 0.348(5) 1 calc PR A 2 H17E H 0.5912 0.4763 -0.4244 0.044 Uiso 0.348(5) 1 calc PR A 2 H17F H 0.6824 0.4584 -0.3613 0.044 Uiso 0.348(5) 1 calc PR A 2 S2 S 0.0295(5) 0.1420(9) 0.3190(5) 0.0231(15) Uani 0.652(5) 1 d PDU A 1 C18 C -0.0773(6) 0.1348(8) 0.2558(8) 0.017(2) Uani 0.652(5) 1 d PDU A 1 H18A H -0.0981 0.2023 0.2378 0.021 Uiso 0.652(5) 1 calc PR A 1 H18B H -0.0797 0.0962 0.1974 0.021 Uiso 0.652(5) 1 calc PR A 1 C19 C -0.1340(6) 0.0857(8) 0.3149(7) 0.0212(19) Uani 0.652(5) 1 d PDU A 1 H19A H -0.1877 0.0671 0.2735 0.025 Uiso 0.652(5) 1 calc PR A 1 H19B H -0.1070 0.0246 0.3439 0.025 Uiso 0.652(5) 1 calc PR A 1 C20 C -0.1507(7) 0.1549(8) 0.3915(7) 0.022(2) Uani 0.652(5) 1 d PDU A 1 H20A H -0.0968 0.1760 0.4310 0.026 Uiso 0.652(5) 1 calc PR A 1 H20B H -0.1800 0.2146 0.3623 0.026 Uiso 0.652(5) 1 calc PR A 1 C21 C -0.2033(7) 0.1050(9) 0.4529(7) 0.025(2) Uani 0.652(5) 1 d PDU A 1 H21A H -0.2538 0.0765 0.4121 0.030 Uiso 0.652(5) 1 calc PR A 1 H21B H -0.1709 0.0498 0.4875 0.030 Uiso 0.652(5) 1 calc PR A 1 C22 C -0.2302(9) 0.1741(10) 0.5229(9) 0.030(2) Uani 0.652(5) 1 d PDU A 1 H22A H -0.2636 0.2288 0.4889 0.036 Uiso 0.652(5) 1 calc PR A 1 H22B H -0.1801 0.2029 0.5641 0.036 Uiso 0.652(5) 1 calc PR A 1 C23 C -0.283(2) 0.1179(13) 0.5843(19) 0.035(2) Uani 0.652(5) 1 d PDU A 1 H23A H -0.3396 0.1032 0.5466 0.042 Uiso 0.652(5) 1 calc PR A 1 H23B H -0.2560 0.0547 0.6071 0.042 Uiso 0.652(5) 1 calc PR A 1 C24 C -0.2901(9) 0.1829(11) 0.6655(9) 0.040(2) Uani 0.652(5) 1 d PDU A 1 H24A H -0.2329 0.1905 0.7037 0.047 Uiso 0.652(5) 1 calc PR A 1 H24B H -0.3075 0.2490 0.6393 0.047 Uiso 0.652(5) 1 calc PR A 1 C25 C -0.3447(9) 0.1585(15) 0.7312(10) 0.039(2) Uani 0.652(5) 1 d PDU A 1 H25A H -0.4021 0.1468 0.6950 0.047 Uiso 0.652(5) 1 calc PR A 1 H25B H -0.3467 0.2158 0.7731 0.047 Uiso 0.652(5) 1 calc PR A 1 C26 C -0.3167(10) 0.0703(12) 0.7893(10) 0.047(3) Uani 0.652(5) 1 d PDU A 1 H26A H -0.2560 0.0756 0.8153 0.056 Uiso 0.652(5) 1 calc PR A 1 H26B H -0.3263 0.0105 0.7493 0.056 Uiso 0.652(5) 1 calc PR A 1 C27 C -0.3648(18) 0.059(2) 0.8728(16) 0.049(5) Uani 0.652(5) 1 d PDU A 1 H27A H -0.3462 -0.0012 0.9082 0.074 Uiso 0.652(5) 1 calc PR A 1 H27B H -0.4251 0.0553 0.8473 0.074 Uiso 0.652(5) 1 calc PR A 1 H27C H -0.3529 0.1166 0.9146 0.074 Uiso 0.652(5) 1 calc PR A 1 S2A S 0.0479(8) 0.1345(15) 0.3458(10) 0.021(3) Uani 0.348(5) 1 d PDU A 2 C18A C -0.0642(10) 0.1311(15) 0.3120(14) 0.019(3) Uani 0.348(5) 1 d PDU A 2 H18C H -0.0860 0.1992 0.2993 0.023 Uiso 0.348(5) 1 calc PR A 2 H18D H -0.0809 0.0921 0.2535 0.023 Uiso 0.348(5) 1 calc PR A 2 C19A C -0.1020(10) 0.0844(16) 0.3903(13) 0.023(3) Uani 0.348(5) 1 d PDU A 2 H19C H -0.0816 0.0156 0.4017 0.028 Uiso 0.348(5) 1 calc PR A 2 H19D H -0.0840 0.1223 0.4493 0.028 Uiso 0.348(5) 1 calc PR A 2 C20A C -0.1968(10) 0.0846(17) 0.3624(12) 0.027(2) Uani 0.348(5) 1 d PDU A 2 H20C H -0.2150 0.0381 0.3096 0.032 Uiso 0.348(5) 1 calc PR A 2 H20D H -0.2165 0.1516 0.3409 0.032 Uiso 0.348(5) 1 calc PR A 2 C21A C -0.2354(13) 0.0544(16) 0.4448(12) 0.027(3) Uani 0.348(5) 1 d PDU A 2 H21C H -0.2935 0.0320 0.4203 0.033 Uiso 0.348(5) 1 calc PR A 2 H21D H -0.2038 -0.0026 0.4769 0.033 Uiso 0.348(5) 1 calc PR A 2 C22A C -0.2367(18) 0.1360(18) 0.5164(16) 0.029(3) Uani 0.348(5) 1 d PDU A 2 H22C H -0.2596 0.1961 0.4815 0.034 Uiso 0.348(5) 1 calc PR A 2 H22D H -0.1780 0.1507 0.5465 0.034 Uiso 0.348(5) 1 calc PR A 2 C23A C -0.285(4) 0.120(2) 0.595(4) 0.033(3) Uani 0.348(5) 1 d PDU A 2 H23C H -0.3302 0.0720 0.5699 0.040 Uiso 0.348(5) 1 calc PR A 2 H23D H -0.2463 0.0851 0.6461 0.040 Uiso 0.348(5) 1 calc PR A 2 C24A C -0.3253(16) 0.2021(17) 0.6409(16) 0.031(3) Uani 0.348(5) 1 d PDU A 2 H24B H -0.2819 0.2496 0.6709 0.037 Uiso 0.348(5) 1 calc PR A 2 H24C H -0.3660 0.2379 0.5925 0.037 Uiso 0.348(5) 1 calc PR A 2 C25A C -0.3697(15) 0.161(3) 0.7143(17) 0.035(3) Uani 0.348(5) 1 d PDU A 2 H25C H -0.4021 0.2138 0.7371 0.042 Uiso 0.348(5) 1 calc PR A 2 H25D H -0.4092 0.1083 0.6858 0.042 Uiso 0.348(5) 1 calc PR A 2 C26A C -0.3078(17) 0.118(2) 0.7954(17) 0.037(3) Uani 0.348(5) 1 d PDU A 2 H26C H -0.2678 0.1709 0.8226 0.045 Uiso 0.348(5) 1 calc PR A 2 H26D H -0.2758 0.0652 0.7721 0.045 Uiso 0.348(5) 1 calc PR A 2 C27A C -0.350(3) 0.075(4) 0.875(3) 0.041(6) Uani 0.348(5) 1 d PDU A 2 H27D H -0.3072 0.0483 0.9256 0.062 Uiso 0.348(5) 1 calc PR A 2 H27E H -0.3894 0.0227 0.8487 0.062 Uiso 0.348(5) 1 calc PR A 2 H27F H -0.3806 0.1282 0.8997 0.062 Uiso 0.348(5) 1 calc PR A 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 0.0147(6) 0.0224(6) 0.0140(6) 0.0054(5) 0.0006(5) -0.0015(5) Cl1 0.0238(10) 0.0573(13) 0.0177(9) 0.0137(9) -0.0037(8) 0.0050(9) Cl2 0.0271(10) 0.0349(11) 0.0241(10) -0.0093(8) 0.0030(8) -0.0058(8) Cl3 0.014(4) 0.025(3) 0.011(5) 0.004(3) 0.007(3) 0.004(2) Cl3A 0.023(7) 0.015(3) 0.026(10) -0.003(4) -0.008(7) 0.001(3) N1 0.018(3) 0.025(3) 0.014(3) 0.006(3) 0.001(3) 0.001(3) C1 0.025(4) 0.029(4) 0.021(4) 0.000(3) 0.009(3) -0.005(3) C2 0.038(5) 0.031(4) 0.018(4) 0.004(3) 0.008(3) -0.003(4) C3 0.030(4) 0.025(4) 0.031(4) -0.001(3) 0.009(4) 0.000(3) C4 0.027(4) 0.018(4) 0.039(5) 0.010(3) 0.013(4) 0.003(3) C5 0.017(4) 0.019(4) 0.033(4) 0.011(3) 0.009(3) 0.003(3) C6 0.054(5) 0.034(5) 0.014(4) 0.002(3) 0.007(4) -0.018(4) C7 0.029(4) 0.022(4) 0.030(4) 0.010(3) 0.011(4) -0.001(3) S1 0.018(3) 0.017(3) 0.0118(19) 0.0054(19) 0.008(3) 0.003(2) C8 0.020(5) 0.029(6) 0.024(5) 0.011(4) 0.012(5) 0.008(4) C9 0.022(4) 0.026(4) 0.027(4) 0.010(4) 0.013(4) 0.007(4) C10 0.022(5) 0.021(5) 0.020(4) 0.007(4) 0.010(4) 0.002(4) C11 0.020(5) 0.019(5) 0.026(5) 0.011(4) 0.008(4) 0.000(4) C12 0.025(4) 0.021(6) 0.024(4) 0.005(4) 0.010(4) -0.004(5) C13 0.025(4) 0.022(6) 0.024(4) -0.001(4) 0.014(4) -0.005(5) C14 0.022(5) 0.022(5) 0.024(4) 0.005(4) 0.017(4) -0.004(4) C15 0.021(6) 0.025(6) 0.023(4) 0.001(4) 0.010(4) -0.008(5) C16 0.017(6) 0.026(5) 0.024(4) 0.004(4) 0.009(5) -0.010(5) C17 0.020(9) 0.038(8) 0.026(6) 0.009(5) 0.011(6) -0.004(7) S1A 0.013(6) 0.014(6) 0.018(3) 0.006(3) 0.002(5) 0.002(4) C8A 0.019(6) 0.025(7) 0.028(6) 0.010(6) 0.012(5) 0.000(6) C9A 0.023(5) 0.023(6) 0.025(5) 0.010(5) 0.010(5) 0.002(5) C10A 0.023(5) 0.026(6) 0.027(5) 0.006(5) 0.010(5) 0.001(5) C11A 0.024(6) 0.022(7) 0.025(6) 0.011(6) 0.011(5) -0.003(6) C12A 0.024(5) 0.021(7) 0.024(5) 0.011(6) 0.010(5) -0.004(6) C13A 0.025(5) 0.021(7) 0.022(5) 0.007(5) 0.009(5) -0.005(6) C14A 0.022(6) 0.023(7) 0.023(5) 0.005(5) 0.013(5) -0.004(6) C15A 0.022(7) 0.026(6) 0.025(5) 0.004(5) 0.013(5) -0.005(6) C16A 0.022(8) 0.030(7) 0.023(5) 0.005(5) 0.011(6) -0.006(7) C17A 0.021(12) 0.041(10) 0.030(9) 0.013(8) 0.014(9) -0.004(10) S2 0.024(3) 0.032(3) 0.015(4) 0.004(3) 0.010(2) 0.000(3) C18 0.015(5) 0.024(5) 0.016(5) -0.006(4) 0.009(4) -0.004(4) C19 0.019(4) 0.031(4) 0.016(4) 0.001(4) 0.009(4) -0.004(4) C20 0.022(4) 0.033(4) 0.013(4) 0.000(4) 0.008(4) -0.001(4) C21 0.020(4) 0.037(5) 0.021(4) 0.000(4) 0.012(4) -0.004(4) C22 0.022(4) 0.052(5) 0.019(4) 0.000(4) 0.011(4) -0.004(5) C23 0.029(4) 0.053(5) 0.025(5) 0.004(4) 0.013(4) 0.001(4) C24 0.042(5) 0.052(5) 0.028(5) 0.000(4) 0.015(4) -0.013(5) C25 0.045(6) 0.045(5) 0.034(5) 0.004(4) 0.020(4) -0.002(5) C26 0.045(6) 0.057(7) 0.043(5) 0.010(6) 0.018(5) 0.009(7) C27 0.061(11) 0.053(11) 0.036(7) 0.020(7) 0.013(7) 0.006(10) S2A 0.022(5) 0.019(4) 0.023(7) 0.008(5) 0.010(4) -0.004(4) C18A 0.022(5) 0.024(5) 0.013(5) -0.001(5) 0.008(5) -0.001(5) C19A 0.026(5) 0.030(5) 0.017(5) 0.002(5) 0.011(5) -0.002(5) C20A 0.025(5) 0.038(5) 0.020(5) 0.002(5) 0.011(4) -0.003(4) C21A 0.026(6) 0.041(6) 0.019(5) 0.005(6) 0.013(5) -0.001(6) C22A 0.025(5) 0.042(6) 0.021(5) 0.006(5) 0.011(4) -0.002(5) C23A 0.029(5) 0.051(5) 0.024(5) 0.003(5) 0.014(5) -0.001(5) C24A 0.031(6) 0.043(5) 0.023(5) 0.005(5) 0.015(5) -0.002(5) C25A 0.039(6) 0.041(6) 0.030(6) 0.004(5) 0.017(5) -0.003(6) C26A 0.042(6) 0.038(7) 0.037(6) 0.012(6) 0.019(5) -0.001(7) C27A 0.046(11) 0.046(12) 0.037(9) 0.013(9) 0.023(9) 0.005(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.066(6) . ? Cr1 Cl2 2.282(2) . ? Cr1 Cl1 2.293(2) . ? Cr1 S1A 2.310(14) . ? Cr1 Cl3A 2.314(14) . ? Cr1 Cl3 2.319(14) . ? Cr1 S2 2.379(9) . ? Cr1 S1 2.476(7) . ? Cr1 S2A 2.508(15) . ? N1 C5 1.353(8) . ? N1 C1 1.359(9) . ? C1 C2 1.377(10) . ? C1 C6 1.491(10) . ? C2 C3 1.396(10) . ? C3 C4 1.371(10) . ? C4 C5 1.378(10) . ? C5 C7 1.510(10) . ? C6 S1 1.824(11) . ? C6 S1A 1.866(16) . ? C7 S2A 1.77(2) . ? C7 S2 1.830(14) . ? S1 C8 1.818(10) . ? C8 C9 1.530(12) . ? C9 C10 1.523(12) . ? C10 C11 1.532(12) . ? C11 C12 1.517(14) . ? C12 C13 1.522(12) . ? C13 C14 1.510(14) . ? C14 C15 1.531(13) . ? C15 C16 1.501(14) . ? C16 C17 1.520(14) . ? S1A C8A 1.804(14) . ? C8A C9A 1.547(17) . ? C9A C10A 1.522(17) . ? C10A C11A 1.543(17) . ? C11A C12A 1.508(19) . ? C12A C13A 1.520(17) . ? C13A C14A 1.511(18) . ? C14A C15A 1.527(17) . ? C15A C16A 1.504(19) . ? C16A C17A 1.524(18) . ? S2 C18 1.802(10) . ? C18 C19 1.539(13) . ? C19 C20 1.521(13) . ? C20 C21 1.520(13) . ? C21 C22 1.511(14) . ? C22 C23 1.565(14) . ? C23 C24 1.495(17) . ? C24 C25 1.474(13) . ? C25 C26 1.477(17) . ? C26 C27 1.586(17) . ? S2A C18A 1.798(14) . ? C18A C19A 1.540(18) . ? C19A C20A 1.521(18) . ? C20A C21A 1.522(18) . ? C21A C22A 1.520(19) . ? C22A C23A 1.533(16) . ? C23A C24A 1.52(2) . ? C24A C25A 1.516(17) . ? C25A C26A 1.50(2) . ? C26A C27A 1.579(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 Cl2 177.59(16) . . ? N1 Cr1 Cl1 90.03(16) . . ? Cl2 Cr1 Cl1 91.41(8) . . ? N1 Cr1 S1A 86.3(4) . . ? Cl2 Cr1 S1A 91.5(3) . . ? Cl1 Cr1 S1A 101.9(3) . . ? N1 Cr1 Cl3A 89.1(6) . . ? Cl2 Cr1 Cl3A 89.8(5) . . ? Cl1 Cr1 Cl3A 171.8(17) . . ? S1A Cr1 Cl3A 86.2(18) . . ? N1 Cr1 Cl3 86.3(4) . . ? Cl2 Cr1 Cl3 92.2(4) . . ? Cl1 Cr1 Cl3 175.2(7) . . ? S1A Cr1 Cl3 74.7(9) . . ? Cl3A Cr1 Cl3 11.6(10) . . ? N1 Cr1 S2 81.6(3) . . ? Cl2 Cr1 S2 100.4(3) . . ? Cl1 Cr1 S2 86.67(17) . . ? S1A Cr1 S2 165.2(4) . . ? Cl3A Cr1 S2 85.1(16) . . ? Cl3 Cr1 S2 95.9(9) . . ? N1 Cr1 S1 80.9(2) . . ? Cl2 Cr1 S1 97.11(19) . . ? Cl1 Cr1 S1 91.30(16) . . ? S1A Cr1 S1 11.8(3) . . ? Cl3A Cr1 S1 96.6(18) . . ? Cl3 Cr1 S1 85.0(9) . . ? S2 Cr1 S1 162.4(3) . . ? N1 Cr1 S2A 84.1(5) . . ? Cl2 Cr1 S2A 98.2(5) . . ? Cl1 Cr1 S2A 76.8(3) . . ? S1A Cr1 S2A 170.2(6) . . ? Cl3A Cr1 S2A 95.0(17) . . ? Cl3 Cr1 S2A 105.9(9) . . ? S2 Cr1 S2A 10.2(4) . . ? S1 Cr1 S2A 160.8(5) . . ? C5 N1 C1 118.9(6) . . ? C5 N1 Cr1 121.3(5) . . ? C1 N1 Cr1 119.8(5) . . ? N1 C1 C2 121.5(6) . . ? N1 C1 C6 118.0(6) . . ? C2 C1 C6 120.4(6) . . ? C1 C2 C3 119.3(7) . . ? C4 C3 C2 118.6(7) . . ? C3 C4 C5 120.1(7) . . ? N1 C5 C4 121.5(6) . . ? N1 C5 C7 116.6(6) . . ? C4 C5 C7 121.9(6) . . ? C1 C6 S1 111.4(5) . . ? C1 C6 S1A 115.3(6) . . ? S1 C6 S1A 16.2(3) . . ? C5 C7 S2A 120.6(7) . . ? C5 C7 S2 110.1(5) . . ? S2A C7 S2 14.3(5) . . ? C8 S1 C6 105.6(6) . . ? C8 S1 Cr1 107.5(4) . . ? C6 S1 Cr1 91.8(4) . . ? C9 C8 S1 112.8(8) . . ? C10 C9 C8 115.3(9) . . ? C9 C10 C11 111.3(8) . . ? C12 C11 C10 114.1(9) . . ? C11 C12 C13 114.5(9) . . ? C14 C13 C12 114.2(9) . . ? C13 C14 C15 113.9(9) . . ? C16 C15 C14 114.3(9) . . ? C15 C16 C17 112.8(9) . . ? C8A S1A C6 91.0(10) . . ? C8A S1A Cr1 106.8(8) . . ? C6 S1A Cr1 96.1(6) . . ? C9A C8A S1A 111.6(13) . . ? C10A C9A C8A 111.2(13) . . ? C9A C10A C11A 113.1(14) . . ? C12A C11A C10A 116.0(16) . . ? C11A C12A C13A 113.9(16) . . ? C14A C13A C12A 116.2(17) . . ? C13A C14A C15A 113.2(16) . . ? C16A C15A C14A 113.8(16) . . ? C15A C16A C17A 111.6(17) . . ? C18 S2 C7 102.0(7) . . ? C18 S2 Cr1 112.3(5) . . ? C7 S2 Cr1 95.3(4) . . ? C19 C18 S2 111.7(8) . . ? C20 C19 C18 111.4(8) . . ? C21 C20 C19 111.5(9) . . ? C22 C21 C20 113.6(10) . . ? C21 C22 C23 110.9(10) . . ? C24 C23 C22 107.9(13) . . ? C25 C24 C23 122.3(12) . . ? C24 C25 C26 113.2(12) . . ? C25 C26 C27 111.8(13) . . ? C7 S2A C18A 98.2(11) . . ? C7 S2A Cr1 92.6(7) . . ? C18A S2A Cr1 113.6(8) . . ? C19A C18A S2A 110.5(13) . . ? C20A C19A C18A 110.1(13) . . ? C19A C20A C21A 110.7(14) . . ? C22A C21A C20A 114.3(17) . . ? C21A C22A C23A 119.2(18) . . ? C24A C23A C22A 124(2) . . ? C25A C24A C23A 110.7(18) . . ? C26A C25A C24A 110.6(18) . . ? C25A C26A C27A 113(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.572 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.116 ===END=== data_07116 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H33 Cl2 Cr N O S2' _chemical_formula_weight 478.48 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' 'S' 'S' 0.1246 0.1234 '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' 'Cl' 'Cl' 0.1484 0.1585 '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 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 11.9048(14) _cell_length_b 12.2321(14) _cell_length_c 17.021(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.792(2) _cell_angle_gamma 90.00 _cell_volume 2360.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2299 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.63 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8069 _exptl_absorpt_correction_T_max 0.9565 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 6488 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.70 _reflns_number_total 4137 _reflns_number_gt 2454 _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^)+(0.0631P)^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 4137 _refine_ls_number_parameters 287 _refine_ls_number_restraints 166 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.959 _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 0.71288(6) 0.73618(6) 0.23812(4) 0.03229(19) Uani 1 1 d . . . Cl1 Cl 0.84229(10) 0.83423(9) 0.17832(6) 0.0407(3) Uani 1 1 d . A . Cl2 Cl 0.57534(10) 0.64075(10) 0.28993(8) 0.0513(3) Uani 1 1 d . A . S1 S 0.69430(10) 0.88737(9) 0.35243(7) 0.0365(3) Uani 1 1 d . A . S2 S 0.79946(9) 0.55727(9) 0.17574(6) 0.0313(3) Uani 1 1 d . A . N1 N 0.8585(3) 0.6876(3) 0.34329(18) 0.0268(8) Uani 1 1 d . A . C1 C 0.7930(4) 1.0069(3) 0.3735(3) 0.0374(11) Uani 1 1 d . . . C2 C 0.7750(4) 1.0699(4) 0.4459(3) 0.0535(14) Uani 1 1 d . A . H2A H 0.8244 1.1346 0.4563 0.080 Uiso 1 1 calc R . . H2B H 0.7962 1.0238 0.4946 0.080 Uiso 1 1 calc R . . H2C H 0.6929 1.0913 0.4328 0.080 Uiso 1 1 calc R . . C3 C 0.9208(4) 0.9734(3) 0.3908(3) 0.0377(11) Uani 1 1 d . A . H3A H 0.9701 1.0381 0.3999 0.056 Uiso 1 1 calc R . . H3B H 0.9296 0.9330 0.3440 0.056 Uiso 1 1 calc R . . H3C H 0.9443 0.9275 0.4396 0.056 Uiso 1 1 calc R . . C4 C 0.7525(4) 1.0738(4) 0.2951(3) 0.0481(13) Uani 1 1 d . A . H4A H 0.7980 1.1408 0.3021 0.072 Uiso 1 1 calc R . . H4B H 0.6695 1.0915 0.2833 0.072 Uiso 1 1 calc R . . H4C H 0.7638 1.0321 0.2497 0.072 Uiso 1 1 calc R . . C5 C 0.7638(4) 0.7903(3) 0.4320(2) 0.0361(11) Uani 1 1 d . . . H5A H 0.7932 0.8303 0.4842 0.043 Uiso 1 1 calc R A . H5B H 0.7030 0.7396 0.4376 0.043 Uiso 1 1 calc R . . C6 C 0.8651(4) 0.7230(3) 0.4206(2) 0.0324(10) Uani 1 1 d . A . C7 C 0.9560(4) 0.6933(4) 0.4879(3) 0.0409(12) Uani 1 1 d . . . H7A H 0.9585 0.7183 0.5407 0.049 Uiso 1 1 calc R A . C8 C 1.0445(4) 0.6264(4) 0.4784(3) 0.0446(13) Uani 1 1 d . A . H8 H 1.1076 0.6055 0.5244 0.053 Uiso 1 1 calc R . . C9 C 1.0390(4) 0.5911(4) 0.4013(3) 0.0363(11) Uani 1 1 d . . . H9A H 1.0989 0.5463 0.3934 0.044 Uiso 1 1 calc R A . C10 C 0.9444(4) 0.6217(3) 0.3347(2) 0.0281(10) Uani 1 1 d . A . C11 C 0.9408(3) 0.5846(3) 0.2497(2) 0.0322(10) Uani 1 1 d . . . H11A H 0.9882 0.5179 0.2557 0.039 Uiso 1 1 calc R A . H11B H 0.9799 0.6407 0.2262 0.039 Uiso 1 1 calc R . . C12 C 0.7579(4) 0.4195(3) 0.2009(2) 0.0333(11) Uani 1 1 d . . . C13 C 0.7797(4) 0.4058(4) 0.2940(3) 0.0437(12) Uani 1 1 d . A . H13A H 0.7457 0.3373 0.3044 0.066 Uiso 1 1 calc R . . H13B H 0.7433 0.4660 0.3144 0.066 Uiso 1 1 calc R . . H13C H 0.8639 0.4055 0.3222 0.066 Uiso 1 1 calc R . . C14 C 0.8283(4) 0.3331(3) 0.1709(2) 0.0390(12) Uani 1 1 d . A . H14A H 0.8067 0.2609 0.1849 0.058 Uiso 1 1 calc R . . H14B H 0.9120 0.3449 0.1972 0.058 Uiso 1 1 calc R . . H14C H 0.8109 0.3388 0.1115 0.058 Uiso 1 1 calc R . . C15 C 0.6266(4) 0.4104(4) 0.1539(3) 0.0500(13) Uani 1 1 d . A . H15A H 0.5986 0.3380 0.1618 0.075 Uiso 1 1 calc R . . H15B H 0.6144 0.4228 0.0956 0.075 Uiso 1 1 calc R . . H15C H 0.5833 0.4648 0.1745 0.075 Uiso 1 1 calc R . . O1 O 0.5735(10) 0.7850(10) 0.1381(5) 0.0533(18) Uani 0.50 1 d PDU A 1 C21 C 0.5308(9) 0.7370(9) 0.0583(7) 0.061(2) Uani 0.50 1 d PDU A 1 H21A H 0.4999 0.6637 0.0626 0.073 Uiso 0.50 1 calc PR A 1 H21B H 0.5955 0.7299 0.0342 0.073 Uiso 0.50 1 calc PR A 1 C22 C 0.4363(9) 0.8064(9) 0.0045(6) 0.062(2) Uani 0.50 1 d PDU A 1 H22A H 0.4674 0.8547 -0.0298 0.074 Uiso 0.50 1 calc PR A 1 H22B H 0.3728 0.7617 -0.0312 0.074 Uiso 0.50 1 calc PR A 1 C23 C 0.3952(10) 0.8684(11) 0.0623(6) 0.061(2) Uani 0.50 1 d PDU A 1 H23A H 0.3147 0.8463 0.0590 0.073 Uiso 0.50 1 calc PR A 1 H23B H 0.3947 0.9466 0.0497 0.073 Uiso 0.50 1 calc PR A 1 C24 C 0.4758(8) 0.8468(10) 0.1455(6) 0.056(2) Uani 0.50 1 d PDU A 1 H24A H 0.5035 0.9159 0.1739 0.068 Uiso 0.50 1 calc PR A 1 H24B H 0.4346 0.8059 0.1779 0.068 Uiso 0.50 1 calc PR A 1 O1A O 0.5735(11) 0.7850(10) 0.1381(5) 0.0533(18) Uani 0.50 1 d PDU A 2 C21A C 0.5707(9) 0.7674(10) 0.0553(6) 0.057(2) Uani 0.50 1 d PDU A 2 H21C H 0.5543 0.6904 0.0402 0.068 Uiso 0.50 1 calc PR A 2 H21D H 0.6465 0.7872 0.0478 0.068 Uiso 0.50 1 calc PR A 2 C22A C 0.4792(9) 0.8351(10) 0.0059(7) 0.063(2) Uani 0.50 1 d PDU A 2 H22C H 0.4214 0.7904 -0.0349 0.075 Uiso 0.50 1 calc PR A 2 H22D H 0.5121 0.8888 -0.0237 0.075 Uiso 0.50 1 calc PR A 2 C23A C 0.4224(10) 0.8905(12) 0.0583(6) 0.061(2) Uani 0.50 1 d PDU A 2 H23C H 0.3532 0.8501 0.0623 0.074 Uiso 0.50 1 calc PR A 2 H23D H 0.3987 0.9649 0.0388 0.074 Uiso 0.50 1 calc PR A 2 C24A C 0.5167(9) 0.8911(10) 0.1366(6) 0.063(2) Uani 0.50 1 d PDU A 2 H24C H 0.4849 0.8985 0.1831 0.076 Uiso 0.50 1 calc PR A 2 H24D H 0.5722 0.9509 0.1386 0.076 Uiso 0.50 1 calc PR A 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 0.0278(4) 0.0342(4) 0.0349(4) -0.0056(3) 0.0096(3) -0.0016(3) Cl1 0.0476(7) 0.0387(6) 0.0391(6) -0.0002(5) 0.0179(5) -0.0055(6) Cl2 0.0422(7) 0.0464(7) 0.0742(8) -0.0140(6) 0.0309(6) -0.0141(6) S1 0.0311(6) 0.0374(6) 0.0434(6) -0.0098(5) 0.0149(5) -0.0016(5) S2 0.0349(6) 0.0299(6) 0.0297(5) -0.0030(4) 0.0105(5) 0.0003(5) N1 0.0249(19) 0.0273(19) 0.0302(17) -0.0032(15) 0.0112(15) -0.0082(16) C1 0.040(3) 0.032(3) 0.041(2) -0.009(2) 0.013(2) 0.002(2) C2 0.062(3) 0.043(3) 0.063(3) -0.020(2) 0.031(3) -0.006(3) C3 0.041(3) 0.035(3) 0.040(2) -0.005(2) 0.015(2) -0.005(2) C4 0.041(3) 0.046(3) 0.052(3) 0.000(2) 0.007(2) 0.004(3) C5 0.050(3) 0.033(2) 0.030(2) -0.0076(19) 0.021(2) -0.008(2) C6 0.042(3) 0.024(2) 0.037(2) -0.0015(18) 0.019(2) -0.007(2) C7 0.056(3) 0.037(3) 0.030(2) -0.005(2) 0.014(2) -0.006(2) C8 0.040(3) 0.040(3) 0.043(3) 0.003(2) -0.004(2) -0.003(2) C9 0.036(3) 0.035(3) 0.036(2) 0.003(2) 0.010(2) 0.001(2) C10 0.029(2) 0.022(2) 0.034(2) -0.0019(17) 0.0101(19) -0.003(2) C11 0.029(2) 0.032(2) 0.038(2) -0.0051(19) 0.0144(19) -0.001(2) C12 0.034(3) 0.030(2) 0.035(2) -0.0052(18) 0.009(2) -0.006(2) C13 0.059(3) 0.036(3) 0.044(2) -0.004(2) 0.028(2) -0.009(2) C14 0.052(3) 0.028(2) 0.037(2) -0.0053(19) 0.014(2) 0.000(2) C15 0.052(3) 0.037(3) 0.067(3) -0.014(2) 0.027(3) -0.009(2) O1 0.035(3) 0.078(3) 0.041(3) -0.010(3) 0.004(3) 0.014(3) C21 0.044(4) 0.083(4) 0.048(3) -0.015(3) 0.003(3) 0.006(4) C22 0.045(4) 0.082(4) 0.050(3) -0.009(3) 0.004(3) 0.001(4) C23 0.042(4) 0.084(4) 0.054(3) 0.000(3) 0.011(3) 0.009(4) C24 0.038(4) 0.083(4) 0.048(3) -0.008(3) 0.012(3) 0.016(3) O1A 0.035(3) 0.078(3) 0.041(3) -0.010(3) 0.004(3) 0.014(3) C21A 0.035(4) 0.089(4) 0.045(3) -0.017(3) 0.010(3) 0.005(4) C22A 0.051(4) 0.085(4) 0.050(3) -0.001(3) 0.013(3) 0.004(4) C23A 0.046(4) 0.079(4) 0.054(4) -0.003(3) 0.007(3) 0.014(4) C24A 0.046(4) 0.078(4) 0.055(4) -0.013(4) -0.001(3) 0.019(4) _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 O1A 2.069(10) . ? Cr1 O1 2.069(9) . ? Cr1 N1 2.160(3) . ? Cr1 Cl2 2.3882(14) . ? Cr1 Cl1 2.4096(13) . ? Cr1 S1 2.7420(13) . ? Cr1 S2 2.7654(13) . ? S1 C5 1.800(4) . ? S1 C1 1.842(4) . ? S2 C11 1.798(4) . ? S2 C12 1.843(4) . ? N1 C10 1.344(5) . ? N1 C6 1.366(5) . ? C1 C4 1.514(6) . ? C1 C3 1.514(6) . ? C1 C2 1.522(6) . ? C5 C6 1.520(6) . ? C6 C7 1.363(6) . ? C7 C8 1.383(6) . ? C8 C9 1.365(6) . ? C9 C10 1.383(5) . ? C10 C11 1.504(5) . ? C12 C15 1.527(6) . ? C12 C14 1.530(6) . ? C12 C13 1.535(6) . ? O1 C21 1.424(13) . ? O1 C24 1.425(15) . ? C21 C22 1.482(10) . ? C22 C23 1.442(11) . ? C23 C24 1.472(10) . ? O1A C21A 1.416(14) . ? O1A C24A 1.461(17) . ? C21A C22A 1.421(10) . ? C22A C23A 1.443(11) . ? C23A C24A 1.457(10) . ? 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 O1A Cr1 O1 0.0(10) . . ? O1A Cr1 N1 179.2(3) . . ? O1 Cr1 N1 179.2(3) . . ? O1A Cr1 Cl2 88.7(4) . . ? O1 Cr1 Cl2 88.7(4) . . ? N1 Cr1 Cl2 91.53(9) . . ? O1A Cr1 Cl1 88.0(4) . . ? O1 Cr1 Cl1 88.0(4) . . ? N1 Cr1 Cl1 91.85(9) . . ? Cl2 Cr1 Cl1 176.59(5) . . ? O1A Cr1 S1 99.9(3) . . ? O1 Cr1 S1 99.9(3) . . ? N1 Cr1 S1 79.40(9) . . ? Cl2 Cr1 S1 81.64(4) . . ? Cl1 Cr1 S1 99.48(4) . . ? O1A Cr1 S2 102.2(3) . . ? O1 Cr1 S2 102.2(3) . . ? N1 Cr1 S2 78.54(9) . . ? Cl2 Cr1 S2 97.64(4) . . ? Cl1 Cr1 S2 82.55(4) . . ? S1 Cr1 S2 157.90(4) . . ? C5 S1 C1 104.9(2) . . ? C5 S1 Cr1 88.33(13) . . ? C1 S1 Cr1 119.27(14) . . ? C11 S2 C12 105.53(19) . . ? C11 S2 Cr1 87.86(13) . . ? C12 S2 Cr1 118.46(14) . . ? C10 N1 C6 118.3(3) . . ? C10 N1 Cr1 121.3(2) . . ? C6 N1 Cr1 120.4(3) . . ? C4 C1 C3 110.4(4) . . ? C4 C1 C2 110.7(4) . . ? C3 C1 C2 111.2(4) . . ? C4 C1 S1 104.2(3) . . ? C3 C1 S1 111.5(3) . . ? C2 C1 S1 108.7(3) . . ? C6 C5 S1 117.5(3) . . ? C7 C6 N1 121.5(4) . . ? C7 C6 C5 119.6(4) . . ? N1 C6 C5 118.7(3) . . ? C6 C7 C8 119.8(4) . . ? C9 C8 C7 119.1(4) . . ? C8 C9 C10 119.4(4) . . ? N1 C10 C9 121.9(4) . . ? N1 C10 C11 119.1(3) . . ? C9 C10 C11 118.9(4) . . ? C10 C11 S2 118.4(3) . . ? C15 C12 C14 110.7(3) . . ? C15 C12 C13 110.8(4) . . ? C14 C12 C13 109.4(3) . . ? C15 C12 S2 104.4(3) . . ? C14 C12 S2 109.9(3) . . ? C13 C12 S2 111.5(3) . . ? C21 O1 C24 103.9(8) . . ? C21 O1 Cr1 129.0(8) . . ? C24 O1 Cr1 123.4(6) . . ? O1 C21 C22 109.6(9) . . ? C23 C22 C21 103.5(9) . . ? C22 C23 C24 107.7(9) . . ? O1 C24 C23 108.7(8) . . ? C21A O1A C24A 104.3(10) . . ? C21A O1A Cr1 123.0(9) . . ? C24A O1A Cr1 121.4(6) . . ? O1A C21A C22A 106.4(10) . . ? C21A C22A C23A 109.1(9) . . ? C22A C23A C24A 101.1(9) . . ? C23A C24A O1A 103.6(9) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.410 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.080 ===END=== data_sg3967 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H92 Al4 Cl4 Cr2 N2 S4' _chemical_formula_weight 1131.16 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2413(11) _cell_length_b 18.245(2) _cell_length_c 21.310(3) _cell_angle_alpha 112.897(2) _cell_angle_beta 100.925(2) _cell_angle_gamma 90.513(2) _cell_volume 3236.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 211(2) _cell_measurement_reflns_used 9181 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 24.70 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8534 _exptl_absorpt_correction_T_max 0.9258 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 211(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_% <1 _diffrn_reflns_number 31841 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 24.85 _reflns_number_total 10940 _reflns_number_gt 7620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2003)' _computing_cell_refinement 'SMART, Bruker (2003)' _computing_data_reduction 'XPREP, Bruker (2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.1056P)^2^+7.2898P] 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 10940 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2055 _refine_ls_wR_factor_gt 0.1847 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.52021(9) 0.36633(5) 0.27737(4) 0.0321(2) Uani 1 1 d . . . Cr2 Cr 0.25607(9) 0.85706(5) 0.28352(4) 0.0331(2) Uani 1 1 d . . . Al1 Al 0.5464(2) 0.46080(12) 0.09894(10) 0.0491(5) Uani 1 1 d . . . Al2 Al 0.8815(2) 0.31136(14) 0.39487(12) 0.0589(6) Uani 1 1 d . . . Al3 Al 0.1032(3) 0.92446(14) 0.09483(11) 0.0615(6) Uani 1 1 d . . . Al4 Al 0.0310(2) 0.82871(12) 0.42747(10) 0.0480(5) Uani 1 1 d . . . Cl1 Cl 0.58653(16) 0.42745(8) 0.19672(7) 0.0396(3) Uani 1 1 d . . . Cl2 Cl 0.77094(15) 0.34622(10) 0.29996(8) 0.0472(4) Uani 1 1 d . . . Cl4 Cl 0.09742(16) 0.89920(9) 0.19470(7) 0.0425(3) Uani 1 1 d . . . Cl5 Cl 0.04107(15) 0.85578(9) 0.32681(8) 0.0437(4) Uani 1 1 d . . . N1 N 0.3032(5) 0.3891(3) 0.2532(2) 0.0361(10) Uani 1 1 d . . . N2 N 0.4369(5) 0.8598(3) 0.2396(3) 0.0422(12) Uani 1 1 d . . . S1 S 0.41951(18) 0.23907(9) 0.18234(9) 0.0488(4) Uani 1 1 d . . . S2 S 0.53005(16) 0.48996(9) 0.37972(7) 0.0407(3) Uani 1 1 d . . . S3 S 0.24146(17) 0.71739(9) 0.20233(8) 0.0429(4) Uani 1 1 d . . . S4 S 0.36492(17) 0.98711(9) 0.36846(8) 0.0442(4) Uani 1 1 d . . . C1 C 0.2211(6) 0.3471(4) 0.1885(3) 0.0468(15) Uani 1 1 d . . . C2 C 0.0730(7) 0.3622(4) 0.1715(4) 0.0577(18) Uani 1 1 d . . . H2A H 0.0153 0.3324 0.1269 0.069 Uiso 1 1 calc R . . C3 C 0.0125(7) 0.4210(5) 0.2203(4) 0.0625(19) Uani 1 1 d . . . H3A H -0.0853 0.4329 0.2090 0.075 Uiso 1 1 calc R . . C4 C 0.0974(7) 0.4612(4) 0.2853(4) 0.0556(17) Uani 1 1 d . . . H4A H 0.0570 0.5004 0.3195 0.067 Uiso 1 1 calc R . . C5 C 0.2415(6) 0.4450(3) 0.3012(3) 0.0400(13) Uani 1 1 d . . . C6 C 0.2925(7) 0.2865(4) 0.1371(3) 0.0551(17) Uani 1 1 d . . . H6A H 0.3463 0.3120 0.1145 0.066 Uiso 1 1 calc R . . H6B H 0.2171 0.2463 0.1012 0.066 Uiso 1 1 calc R . . C7 C 0.5290(9) 0.1796(4) 0.1169(4) 0.0634(19) Uani 1 1 d . . . C8 C 0.6266(11) 0.2316(5) 0.0985(5) 0.084(3) Uani 1 1 d . . . H8A H 0.6810 0.1981 0.0649 0.126 Uiso 1 1 calc R . . H8B H 0.6958 0.2665 0.1402 0.126 Uiso 1 1 calc R . . H8C H 0.5660 0.2636 0.0787 0.126 Uiso 1 1 calc R . . C9 C 0.4178(11) 0.1246(5) 0.0526(4) 0.084(3) Uani 1 1 d . . . H9A H 0.4701 0.0924 0.0174 0.127 Uiso 1 1 calc R . . H9B H 0.3529 0.1564 0.0343 0.127 Uiso 1 1 calc R . . H9C H 0.3595 0.0899 0.0651 0.127 Uiso 1 1 calc R . . C10 C 0.6195(10) 0.1333(5) 0.1540(5) 0.089(3) Uani 1 1 d . . . H10A H 0.6813 0.1000 0.1243 0.133 Uiso 1 1 calc R . . H10B H 0.5533 0.0999 0.1643 0.133 Uiso 1 1 calc R . . H10C H 0.6815 0.1705 0.1971 0.133 Uiso 1 1 calc R . . C11 C 0.3332(7) 0.4840(4) 0.3741(3) 0.0493(15) Uani 1 1 d . . . H11A H 0.3101 0.4541 0.4010 0.059 Uiso 1 1 calc R . . H11B H 0.3041 0.5382 0.3959 0.059 Uiso 1 1 calc R . . C12 C 0.5716(7) 0.5884(4) 0.3762(3) 0.0475(15) Uani 1 1 d . . . C13 C 0.7323(8) 0.5861(4) 0.3669(4) 0.0634(19) Uani 1 1 d . . . H13A H 0.7641 0.6353 0.3640 0.095 Uiso 1 1 calc R . . H13B H 0.7391 0.5412 0.3245 0.095 Uiso 1 1 calc R . . H13C H 0.7954 0.5805 0.4064 0.095 Uiso 1 1 calc R . . C14 C 0.5602(10) 0.6516(4) 0.4467(4) 0.073(2) Uani 1 1 d . . . H14A H 0.5807 0.7042 0.4475 0.110 Uiso 1 1 calc R . . H14B H 0.6315 0.6443 0.4830 0.110 Uiso 1 1 calc R . . H14C H 0.4611 0.6466 0.4544 0.110 Uiso 1 1 calc R . . C15 C 0.4685(8) 0.6003(4) 0.3181(4) 0.0586(18) Uani 1 1 d . . . H15A H 0.4953 0.6518 0.3181 0.088 Uiso 1 1 calc R . . H15B H 0.3677 0.5983 0.3246 0.088 Uiso 1 1 calc R . . H15C H 0.4759 0.5583 0.2739 0.088 Uiso 1 1 calc R . . C16 C 0.4711(7) 0.3137(4) 0.3420(4) 0.0492(15) Uani 1 1 d . . . H16A H 0.5136 0.3481 0.3901 0.074 Uiso 1 1 calc R . . H16B H 0.5121 0.2625 0.3303 0.074 Uiso 1 1 calc R . . H16C H 0.3645 0.3059 0.3360 0.074 Uiso 1 1 calc R . . C17 C 0.3513(9) 0.4056(5) 0.0414(4) 0.072(2) Uani 1 1 d . . . H17A H 0.3291 0.4176 0.0002 0.108 Uiso 1 1 calc R . . H17B H 0.2754 0.4239 0.0683 0.108 Uiso 1 1 calc R . . H17C H 0.3541 0.3484 0.0275 0.108 Uiso 1 1 calc R . . C18 C 0.7182(9) 0.4165(5) 0.0561(4) 0.0613(19) Uani 1 1 d . . . H18A H 0.7142 0.4266 0.0144 0.092 Uiso 1 1 calc R . . H18B H 0.7139 0.3594 0.0440 0.092 Uiso 1 1 calc R . . H18C H 0.8099 0.4420 0.0891 0.092 Uiso 1 1 calc R . . C19 C 0.5580(9) 0.5771(4) 0.1406(4) 0.067(2) Uani 1 1 d . . . H19A H 0.5422 0.5972 0.1041 0.100 Uiso 1 1 calc R . . H19B H 0.6549 0.5979 0.1704 0.100 Uiso 1 1 calc R . . H19C H 0.4825 0.5941 0.1680 0.100 Uiso 1 1 calc R . . C20 C 0.7953(8) 0.2013(5) 0.3679(6) 0.086(3) Uani 1 1 d . . . H20A H 0.8349 0.1825 0.4040 0.130 Uiso 1 1 calc R . . H20B H 0.8202 0.1666 0.3244 0.130 Uiso 1 1 calc R . . H20C H 0.6886 0.2006 0.3622 0.130 Uiso 1 1 calc R . . C21 C 1.0868(8) 0.3201(6) 0.3870(5) 0.085(3) Uani 1 1 d . . . H21A H 1.1499 0.3074 0.4225 0.127 Uiso 1 1 calc R . . H21B H 1.1149 0.3743 0.3932 0.127 Uiso 1 1 calc R . . H21C H 1.0977 0.2832 0.3413 0.127 Uiso 1 1 calc R . . C22 C 0.8304(12) 0.3981(7) 0.4759(5) 0.100(3) Uani 1 1 d . . . H22A H 0.8701 0.3898 0.5179 0.150 Uiso 1 1 calc R . . H22B H 0.7236 0.3979 0.4696 0.150 Uiso 1 1 calc R . . H22C H 0.8724 0.4490 0.4800 0.150 Uiso 1 1 calc R . . C23 C 0.4437(7) 0.8040(3) 0.1764(3) 0.0452(14) Uani 1 1 d . . . C24 C 0.5634(9) 0.8029(5) 0.1467(5) 0.072(2) Uani 1 1 d . . . H24A H 0.5673 0.7626 0.1032 0.086 Uiso 1 1 calc R . . C25 C 0.6785(9) 0.8625(6) 0.1825(6) 0.087(3) Uani 1 1 d . . . H25A H 0.7611 0.8638 0.1630 0.105 Uiso 1 1 calc R . . C26 C 0.6710(8) 0.9197(5) 0.2463(5) 0.070(2) Uani 1 1 d . . . H26A H 0.7475 0.9610 0.2704 0.084 Uiso 1 1 calc R . . C27 C 0.5514(7) 0.9163(4) 0.2752(4) 0.0521(16) Uani 1 1 d . . . C28 C 0.3111(8) 0.7429(4) 0.1388(3) 0.0515(16) Uani 1 1 d . . . H28A H 0.3401 0.6951 0.1040 0.062 Uiso 1 1 calc R . . H28B H 0.2340 0.7651 0.1148 0.062 Uiso 1 1 calc R . . C29 C 0.0621(8) 0.6560(4) 0.1555(3) 0.0547(17) Uani 1 1 d . . . C30 C 0.0890(12) 0.5862(6) 0.0930(5) 0.115(4) Uani 1 1 d . . . H30A H -0.0033 0.5533 0.0680 0.172 Uiso 1 1 calc R . . H30B H 0.1602 0.5546 0.1082 0.172 Uiso 1 1 calc R . . H30C H 0.1274 0.6056 0.0624 0.172 Uiso 1 1 calc R . . C31 C 0.0166(9) 0.6285(5) 0.2077(4) 0.073(2) Uani 1 1 d . . . H31A H -0.0770 0.5958 0.1870 0.110 Uiso 1 1 calc R . . H31B H 0.0059 0.6747 0.2486 0.110 Uiso 1 1 calc R . . H31C H 0.0917 0.5975 0.2210 0.110 Uiso 1 1 calc R . . C32 C -0.0562(8) 0.7046(5) 0.1353(5) 0.076(2) Uani 1 1 d . . . H32A H -0.1476 0.6706 0.1113 0.114 Uiso 1 1 calc R . . H32B H -0.0242 0.7264 0.1047 0.114 Uiso 1 1 calc R . . H32C H -0.0723 0.7480 0.1769 0.114 Uiso 1 1 calc R . . C33 C 0.5484(7) 0.9729(4) 0.3486(4) 0.0566(17) Uani 1 1 d . . . H33A H 0.5963 1.0250 0.3571 0.068 Uiso 1 1 calc R . . H33B H 0.6074 0.9530 0.3810 0.068 Uiso 1 1 calc R . . C34 C 0.3156(7) 1.0801(3) 0.3560(3) 0.0472(15) Uani 1 1 d . . . C35 C 0.3471(9) 1.0801(4) 0.2881(4) 0.0600(18) Uani 1 1 d . . . H35A H 0.3198 1.1295 0.2840 0.090 Uiso 1 1 calc R . . H35B H 0.2898 1.0352 0.2490 0.090 Uiso 1 1 calc R . . H35C H 0.4517 1.0757 0.2883 0.090 Uiso 1 1 calc R . . C36 C 0.1503(8) 1.0819(4) 0.3574(4) 0.0633(19) Uani 1 1 d . . . H36A H 0.1146 1.1291 0.3514 0.095 Uiso 1 1 calc R . . H36B H 0.1359 1.0833 0.4018 0.095 Uiso 1 1 calc R . . H36C H 0.0959 1.0345 0.3200 0.095 Uiso 1 1 calc R . . C37 C 0.4055(9) 1.1488(4) 0.4189(4) 0.0627(19) Uani 1 1 d . . . H37A H 0.3836 1.1990 0.4151 0.094 Uiso 1 1 calc R . . H37B H 0.5101 1.1425 0.4208 0.094 Uiso 1 1 calc R . . H37C H 0.3800 1.1487 0.4610 0.094 Uiso 1 1 calc R . . C38 C 0.3822(7) 0.8195(4) 0.3558(4) 0.0517(16) Uani 1 1 d . . . H38A H 0.4822 0.8139 0.3478 0.078 Uiso 1 1 calc R . . H38B H 0.3383 0.7685 0.3507 0.078 Uiso 1 1 calc R . . H38C H 0.3848 0.8588 0.4026 0.078 Uiso 1 1 calc R . . C39 C 0.3145(11) 0.9383(6) 0.0937(4) 0.093(3) Uani 1 1 d . . . H39A H 0.3238 0.9490 0.0534 0.139 Uiso 1 1 calc R . . H39B H 0.3604 0.8899 0.0914 0.139 Uiso 1 1 calc R . . H39C H 0.3633 0.9828 0.1359 0.139 Uiso 1 1 calc R . . C40 C 0.0095(11) 0.8213(6) 0.0161(4) 0.092(3) Uani 1 1 d . . . H40A H 0.0065 0.8256 -0.0281 0.138 Uiso 1 1 calc R . . H40B H -0.0904 0.8107 0.0204 0.138 Uiso 1 1 calc R . . H40C H 0.0674 0.7778 0.0180 0.138 Uiso 1 1 calc R . . C41 C -0.004(2) 1.0177(9) 0.1106(7) 0.184(8) Uani 1 1 d . . . H41A H -0.0088 1.0337 0.0719 0.276 Uiso 1 1 calc R . . H41B H 0.0466 1.0609 0.1533 0.276 Uiso 1 1 calc R . . H41C H -0.1033 1.0057 0.1146 0.276 Uiso 1 1 calc R . . C42 C -0.1847(8) 0.8306(5) 0.4201(4) 0.069(2) Uani 1 1 d . . . H42A H -0.2117 0.8206 0.4581 0.104 Uiso 1 1 calc R . . H42B H -0.2353 0.7896 0.3761 0.104 Uiso 1 1 calc R . . H42C H -0.2134 0.8825 0.4226 0.104 Uiso 1 1 calc R . . C43 C 0.1541(9) 0.9188(5) 0.5030(4) 0.073(2) Uani 1 1 d . . . H43A H 0.1572 0.9136 0.5468 0.110 Uiso 1 1 calc R . . H43B H 0.1127 0.9682 0.5052 0.110 Uiso 1 1 calc R . . H43C H 0.2536 0.9196 0.4946 0.110 Uiso 1 1 calc R . . C44 C 0.0999(9) 0.7215(5) 0.4097(4) 0.071(2) Uani 1 1 d . . . H44A H 0.0974 0.7084 0.4495 0.106 Uiso 1 1 calc R . . H44B H 0.2003 0.7213 0.4024 0.106 Uiso 1 1 calc R . . H44C H 0.0356 0.6822 0.3686 0.106 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0231(4) 0.0326(5) 0.0417(5) 0.0153(4) 0.0081(4) 0.0034(3) Cr2 0.0256(5) 0.0305(5) 0.0397(5) 0.0116(4) 0.0035(4) 0.0011(4) Al1 0.0506(11) 0.0598(12) 0.0431(10) 0.0272(9) 0.0095(8) 0.0085(9) Al2 0.0417(11) 0.0745(15) 0.0794(15) 0.0496(12) 0.0143(10) 0.0109(10) Al3 0.0735(15) 0.0644(14) 0.0476(12) 0.0277(11) 0.0038(10) 0.0026(11) Al4 0.0451(11) 0.0512(11) 0.0497(11) 0.0232(9) 0.0079(8) -0.0002(9) Cl1 0.0416(8) 0.0409(8) 0.0377(7) 0.0173(6) 0.0080(6) 0.0031(6) Cl2 0.0285(7) 0.0648(10) 0.0628(10) 0.0384(8) 0.0146(6) 0.0111(7) Cl4 0.0366(8) 0.0454(8) 0.0439(8) 0.0185(7) 0.0033(6) 0.0022(6) Cl5 0.0340(7) 0.0530(9) 0.0488(8) 0.0244(7) 0.0100(6) 0.0069(6) N1 0.026(2) 0.038(3) 0.047(3) 0.021(2) 0.007(2) 0.001(2) N2 0.026(2) 0.038(3) 0.063(3) 0.021(3) 0.007(2) 0.004(2) S1 0.0454(9) 0.0340(8) 0.0606(10) 0.0115(7) 0.0129(7) -0.0020(7) S2 0.0383(8) 0.0423(8) 0.0374(8) 0.0120(6) 0.0066(6) 0.0019(6) S3 0.0412(8) 0.0310(7) 0.0505(9) 0.0101(7) 0.0092(7) 0.0017(6) S4 0.0456(9) 0.0357(8) 0.0425(8) 0.0102(7) 0.0007(7) -0.0046(6) C1 0.032(3) 0.051(4) 0.055(4) 0.021(3) 0.003(3) -0.006(3) C2 0.035(4) 0.064(5) 0.068(5) 0.028(4) -0.004(3) -0.002(3) C3 0.033(4) 0.076(5) 0.091(6) 0.047(5) 0.009(4) 0.007(3) C4 0.040(4) 0.062(4) 0.075(5) 0.033(4) 0.023(3) 0.014(3) C5 0.031(3) 0.040(3) 0.056(4) 0.021(3) 0.018(3) 0.006(2) C6 0.049(4) 0.052(4) 0.049(4) 0.011(3) -0.003(3) -0.003(3) C7 0.076(5) 0.032(3) 0.073(5) 0.004(3) 0.027(4) 0.011(3) C8 0.101(7) 0.056(5) 0.087(6) 0.005(4) 0.056(5) 0.002(5) C9 0.094(7) 0.057(5) 0.078(6) 0.003(4) 0.015(5) -0.007(5) C10 0.071(6) 0.066(5) 0.117(7) 0.019(5) 0.029(5) 0.024(4) C11 0.051(4) 0.049(4) 0.055(4) 0.021(3) 0.028(3) 0.014(3) C12 0.049(4) 0.034(3) 0.054(4) 0.010(3) 0.012(3) -0.001(3) C13 0.054(4) 0.046(4) 0.076(5) 0.012(4) 0.011(4) -0.016(3) C14 0.084(6) 0.048(4) 0.064(5) -0.004(4) 0.018(4) -0.010(4) C15 0.071(5) 0.046(4) 0.065(4) 0.024(3) 0.023(4) 0.016(3) C16 0.036(3) 0.055(4) 0.070(4) 0.036(3) 0.016(3) 0.000(3) C17 0.066(5) 0.086(6) 0.061(5) 0.039(4) -0.016(4) -0.006(4) C18 0.073(5) 0.071(5) 0.051(4) 0.028(4) 0.030(4) 0.016(4) C19 0.066(5) 0.066(5) 0.088(5) 0.047(4) 0.026(4) 0.022(4) C20 0.045(4) 0.094(6) 0.160(9) 0.094(7) 0.018(5) 0.009(4) C21 0.040(4) 0.095(6) 0.141(8) 0.073(6) 0.011(5) 0.009(4) C22 0.112(8) 0.127(9) 0.077(6) 0.056(6) 0.019(5) 0.039(7) C23 0.038(3) 0.034(3) 0.065(4) 0.016(3) 0.022(3) 0.010(3) C24 0.058(5) 0.059(5) 0.101(6) 0.022(4) 0.042(4) 0.011(4) C25 0.054(5) 0.088(6) 0.140(9) 0.050(6) 0.054(5) 0.011(5) C26 0.032(4) 0.053(4) 0.120(7) 0.028(5) 0.021(4) -0.002(3) C27 0.030(3) 0.044(4) 0.078(5) 0.024(3) 0.003(3) 0.003(3) C28 0.055(4) 0.039(3) 0.056(4) 0.010(3) 0.018(3) 0.005(3) C29 0.056(4) 0.042(4) 0.055(4) 0.009(3) 0.007(3) -0.012(3) C30 0.115(8) 0.075(6) 0.096(7) -0.037(5) 0.045(6) -0.043(6) C31 0.064(5) 0.057(5) 0.096(6) 0.031(4) 0.008(4) -0.020(4) C32 0.047(4) 0.074(5) 0.093(6) 0.033(5) -0.013(4) -0.020(4) C33 0.032(3) 0.047(4) 0.075(5) 0.014(3) -0.005(3) -0.007(3) C34 0.054(4) 0.030(3) 0.050(4) 0.005(3) 0.013(3) 0.002(3) C35 0.077(5) 0.037(4) 0.061(4) 0.017(3) 0.009(4) -0.009(3) C36 0.058(4) 0.040(4) 0.083(5) 0.011(4) 0.022(4) 0.009(3) C37 0.079(5) 0.036(4) 0.055(4) -0.001(3) 0.015(4) -0.009(3) C38 0.035(3) 0.058(4) 0.065(4) 0.035(3) -0.002(3) 0.006(3) C39 0.116(8) 0.096(7) 0.066(5) 0.029(5) 0.028(5) -0.028(6) C40 0.103(7) 0.111(7) 0.040(4) 0.026(4) -0.024(4) -0.041(6) C41 0.31(2) 0.192(15) 0.134(11) 0.119(11) 0.103(12) 0.182(15) C42 0.061(5) 0.063(5) 0.084(5) 0.025(4) 0.026(4) -0.004(4) C43 0.073(5) 0.078(6) 0.054(4) 0.019(4) -0.002(4) -0.011(4) C44 0.076(5) 0.063(5) 0.089(6) 0.046(4) 0.021(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 2.061(4) . ? Cr1 C16 2.070(6) . ? Cr1 Cl2 2.3378(16) . ? Cr1 S1 2.4385(18) . ? Cr1 S2 2.4386(17) . ? Cr1 Cl1 2.5399(16) . ? Cr2 N2 2.072(5) . ? Cr2 C38 2.087(6) . ? Cr2 Cl5 2.3473(17) . ? Cr2 S4 2.4174(17) . ? Cr2 S3 2.4453(17) . ? Cr2 Cl4 2.5346(16) . ? Al1 C19 1.948(8) . ? Al1 C17 1.984(7) . ? Al1 C18 2.002(7) . ? Al1 Cl1 2.355(2) . ? Al2 C21 1.947(8) . ? Al2 C22 1.976(10) . ? Al2 C20 1.974(8) . ? Al2 Cl2 2.402(2) . ? Al3 C41 1.923(11) . ? Al3 C39 1.973(10) . ? Al3 C40 2.018(8) . ? Al3 Cl4 2.356(2) . ? Al4 C43 1.950(8) . ? Al4 C44 1.978(8) . ? Al4 C42 1.972(8) . ? Al4 Cl5 2.399(2) . ? N1 C1 1.354(7) . ? N1 C5 1.354(7) . ? N2 C23 1.349(8) . ? N2 C27 1.352(8) . ? S1 C6 1.814(7) . ? S1 C7 1.877(7) . ? S2 C11 1.800(6) . ? S2 C12 1.866(6) . ? S3 C28 1.811(7) . ? S3 C29 1.862(7) . ? S4 C33 1.821(7) . ? S4 C34 1.865(6) . ? C1 C2 1.406(9) . ? C1 C6 1.484(9) . ? C2 C3 1.381(10) . ? C3 C4 1.364(10) . ? C4 C5 1.375(9) . ? C5 C11 1.506(9) . ? C7 C10 1.523(12) . ? C7 C9 1.523(11) . ? C7 C8 1.508(11) . ? C12 C15 1.501(9) . ? C12 C13 1.534(9) . ? C12 C14 1.520(9) . ? C23 C24 1.371(9) . ? C23 C28 1.515(9) . ? C24 C25 1.386(12) . ? C25 C26 1.370(12) . ? C26 C27 1.375(10) . ? C27 C33 1.508(10) . ? C29 C30 1.507(11) . ? C29 C31 1.508(10) . ? C29 C32 1.517(11) . ? C34 C35 1.529(9) . ? C34 C37 1.520(9) . ? C34 C36 1.534(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 C16 92.0(2) . . ? N1 Cr1 Cl2 175.56(13) . . ? C16 Cr1 Cl2 92.43(18) . . ? N1 Cr1 S1 79.59(14) . . ? C16 Cr1 S1 85.5(2) . . ? Cl2 Cr1 S1 101.27(7) . . ? N1 Cr1 S2 83.04(14) . . ? C16 Cr1 S2 83.4(2) . . ? Cl2 Cr1 S2 96.96(6) . . ? S1 Cr1 S2 158.99(6) . . ? N1 Cr1 Cl1 89.53(13) . . ? C16 Cr1 Cl1 178.10(19) . . ? Cl2 Cr1 Cl1 86.07(5) . . ? S1 Cr1 Cl1 93.69(6) . . ? S2 Cr1 Cl1 97.91(6) . . ? N2 Cr2 C38 91.0(2) . . ? N2 Cr2 Cl5 175.96(14) . . ? C38 Cr2 Cl5 92.98(19) . . ? N2 Cr2 S4 84.23(14) . . ? C38 Cr2 S4 82.2(2) . . ? Cl5 Cr2 S4 96.79(6) . . ? N2 Cr2 S3 79.38(14) . . ? C38 Cr2 S3 85.1(2) . . ? Cl5 Cr2 S3 100.47(6) . . ? S4 Cr2 S3 159.04(7) . . ? N2 Cr2 Cl4 89.96(14) . . ? C38 Cr2 Cl4 178.34(19) . . ? Cl5 Cr2 Cl4 86.02(6) . . ? S4 Cr2 Cl4 99.23(6) . . ? S3 Cr2 Cl4 93.77(6) . . ? C19 Al1 C17 116.0(4) . . ? C19 Al1 C18 114.2(3) . . ? C17 Al1 C18 114.0(4) . . ? C19 Al1 Cl1 102.9(2) . . ? C17 Al1 Cl1 106.1(2) . . ? C18 Al1 Cl1 101.4(2) . . ? C21 Al2 C22 114.6(5) . . ? C21 Al2 C20 114.8(4) . . ? C22 Al2 C20 118.8(5) . . ? C21 Al2 Cl2 97.9(3) . . ? C22 Al2 Cl2 102.4(3) . . ? C20 Al2 Cl2 104.3(3) . . ? C41 Al3 C39 116.3(7) . . ? C41 Al3 C40 117.9(6) . . ? C39 Al3 C40 109.5(4) . . ? C41 Al3 Cl4 102.3(4) . . ? C39 Al3 Cl4 105.8(3) . . ? C40 Al3 Cl4 103.0(3) . . ? C43 Al4 C44 116.8(4) . . ? C43 Al4 C42 116.5(4) . . ? C44 Al4 C42 113.4(3) . . ? C43 Al4 Cl5 102.9(3) . . ? C44 Al4 Cl5 107.1(2) . . ? C42 Al4 Cl5 97.0(2) . . ? Al1 Cl1 Cr1 155.99(8) . . ? Cr1 Cl2 Al2 122.50(8) . . ? Al3 Cl4 Cr2 142.13(9) . . ? Cr2 Cl5 Al4 124.48(8) . . ? C1 N1 C5 119.6(5) . . ? C1 N1 Cr1 119.5(4) . . ? C5 N1 Cr1 121.0(4) . . ? C23 N2 C27 119.3(5) . . ? C23 N2 Cr2 120.6(4) . . ? C27 N2 Cr2 120.1(4) . . ? C6 S1 C7 104.7(3) . . ? C6 S1 Cr1 92.7(2) . . ? C7 S1 Cr1 122.2(2) . . ? C11 S2 C12 103.6(3) . . ? C11 S2 Cr1 94.1(2) . . ? C12 S2 Cr1 120.3(2) . . ? C28 S3 C29 106.1(3) . . ? C28 S3 Cr2 93.0(2) . . ? C29 S3 Cr2 122.6(2) . . ? C33 S4 C34 104.1(3) . . ? C33 S4 Cr2 94.7(2) . . ? C34 S4 Cr2 121.2(2) . . ? N1 C1 C2 119.9(6) . . ? N1 C1 C6 118.2(5) . . ? C2 C1 C6 121.9(6) . . ? C3 C2 C1 119.9(6) . . ? C4 C3 C2 118.6(6) . . ? C3 C4 C5 120.5(7) . . ? N1 C5 C4 121.3(6) . . ? N1 C5 C11 117.2(5) . . ? C4 C5 C11 121.3(6) . . ? C1 C6 S1 108.7(5) . . ? C10 C7 C9 111.9(7) . . ? C10 C7 C8 111.7(8) . . ? C9 C7 C8 110.8(7) . . ? C10 C7 S1 102.5(6) . . ? C9 C7 S1 106.8(6) . . ? C8 C7 S1 112.7(5) . . ? C5 C11 S2 114.8(4) . . ? C15 C12 C13 112.3(6) . . ? C15 C12 C14 111.2(6) . . ? C13 C12 C14 110.8(6) . . ? C15 C12 S2 112.7(4) . . ? C13 C12 S2 103.3(4) . . ? C14 C12 S2 106.1(5) . . ? N2 C23 C24 122.1(6) . . ? N2 C23 C28 116.8(5) . . ? C24 C23 C28 121.1(6) . . ? C23 C24 C25 118.4(8) . . ? C26 C25 C24 119.6(7) . . ? C27 C26 C25 119.8(7) . . ? N2 C27 C26 120.7(7) . . ? N2 C27 C33 118.4(6) . . ? C26 C27 C33 120.8(6) . . ? C23 C28 S3 108.5(4) . . ? C30 C29 C31 111.1(7) . . ? C30 C29 C32 111.9(8) . . ? C31 C29 C32 108.8(7) . . ? C30 C29 S3 108.3(6) . . ? C31 C29 S3 104.3(5) . . ? C32 C29 S3 112.2(5) . . ? C27 C33 S4 115.2(4) . . ? C35 C34 C37 111.3(5) . . ? C35 C34 C36 112.3(6) . . ? C37 C34 C36 110.5(5) . . ? C35 C34 S4 112.5(4) . . ? C37 C34 S4 106.1(5) . . ? C36 C34 S4 103.7(4) . . ? 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 C19 Al1 Cl1 Cr1 115.7(3) . . . . ? C17 Al1 Cl1 Cr1 -6.6(4) . . . . ? C18 Al1 Cl1 Cr1 -125.9(3) . . . . ? N1 Cr1 Cl1 Al1 -32.0(2) . . . . ? C16 Cr1 Cl1 Al1 111(6) . . . . ? Cl2 Cr1 Cl1 Al1 148.6(2) . . . . ? S1 Cr1 Cl1 Al1 47.5(2) . . . . ? S2 Cr1 Cl1 Al1 -114.9(2) . . . . ? N1 Cr1 Cl2 Al2 158.9(19) . . . . ? C16 Cr1 Cl2 Al2 -14.4(2) . . . . ? S1 Cr1 Cl2 Al2 -100.27(11) . . . . ? S2 Cr1 Cl2 Al2 69.23(11) . . . . ? Cl1 Cr1 Cl2 Al2 166.74(11) . . . . ? C21 Al2 Cl2 Cr1 -172.6(3) . . . . ? C22 Al2 Cl2 Cr1 -55.2(4) . . . . ? C20 Al2 Cl2 Cr1 69.2(3) . . . . ? C41 Al3 Cl4 Cr2 -139.5(6) . . . . ? C39 Al3 Cl4 Cr2 -17.2(4) . . . . ? C40 Al3 Cl4 Cr2 97.7(3) . . . . ? N2 Cr2 Cl4 Al3 5.2(2) . . . . ? C38 Cr2 Cl4 Al3 -121(7) . . . . ? Cl5 Cr2 Cl4 Al3 -174.38(14) . . . . ? S4 Cr2 Cl4 Al3 89.37(15) . . . . ? S3 Cr2 Cl4 Al3 -74.13(15) . . . . ? N2 Cr2 Cl5 Al4 178(74) . . . . ? C38 Cr2 Cl5 Al4 4.7(2) . . . . ? S4 Cr2 Cl5 Al4 -77.81(10) . . . . ? S3 Cr2 Cl5 Al4 90.25(10) . . . . ? Cl4 Cr2 Cl5 Al4 -176.64(10) . . . . ? C43 Al4 Cl5 Cr2 65.4(3) . . . . ? C44 Al4 Cl5 Cr2 -58.2(3) . . . . ? C42 Al4 Cl5 Cr2 -175.3(2) . . . . ? C16 Cr1 N1 C1 -109.4(5) . . . . ? Cl2 Cr1 N1 C1 77(2) . . . . ? S1 Cr1 N1 C1 -24.3(4) . . . . ? S2 Cr1 N1 C1 167.5(4) . . . . ? Cl1 Cr1 N1 C1 69.5(4) . . . . ? C16 Cr1 N1 C5 70.3(4) . . . . ? Cl2 Cr1 N1 C5 -103.0(19) . . . . ? S1 Cr1 N1 C5 155.3(4) . . . . ? S2 Cr1 N1 C5 -12.8(4) . . . . ? Cl1 Cr1 N1 C5 -110.8(4) . . . . ? C38 Cr2 N2 C23 107.7(5) . . . . ? Cl5 Cr2 N2 C23 -65(2) . . . . ? S4 Cr2 N2 C23 -170.2(4) . . . . ? S3 Cr2 N2 C23 22.9(4) . . . . ? Cl4 Cr2 N2 C23 -70.9(4) . . . . ? C38 Cr2 N2 C27 -70.3(5) . . . . ? Cl5 Cr2 N2 C27 117(2) . . . . ? S4 Cr2 N2 C27 11.8(4) . . . . ? S3 Cr2 N2 C27 -155.1(4) . . . . ? Cl4 Cr2 N2 C27 111.1(4) . . . . ? N1 Cr1 S1 C6 34.0(3) . . . . ? C16 Cr1 S1 C6 126.9(3) . . . . ? Cl2 Cr1 S1 C6 -141.5(2) . . . . ? S2 Cr1 S1 C6 68.8(3) . . . . ? Cl1 Cr1 S1 C6 -54.8(2) . . . . ? N1 Cr1 S1 C7 143.3(3) . . . . ? C16 Cr1 S1 C7 -123.8(3) . . . . ? Cl2 Cr1 S1 C7 -32.3(3) . . . . ? S2 Cr1 S1 C7 178.0(3) . . . . ? Cl1 Cr1 S1 C7 54.5(3) . . . . ? N1 Cr1 S2 C11 21.7(2) . . . . ? C16 Cr1 S2 C11 -71.1(3) . . . . ? Cl2 Cr1 S2 C11 -162.7(2) . . . . ? S1 Cr1 S2 C11 -12.6(3) . . . . ? Cl1 Cr1 S2 C11 110.3(2) . . . . ? N1 Cr1 S2 C12 -86.7(3) . . . . ? C16 Cr1 S2 C12 -179.5(3) . . . . ? Cl2 Cr1 S2 C12 88.8(2) . . . . ? S1 Cr1 S2 C12 -121.1(3) . . . . ? Cl1 Cr1 S2 C12 1.9(2) . . . . ? N2 Cr2 S3 C28 -33.9(3) . . . . ? C38 Cr2 S3 C28 -125.8(3) . . . . ? Cl5 Cr2 S3 C28 142.0(2) . . . . ? S4 Cr2 S3 C28 -73.0(3) . . . . ? Cl4 Cr2 S3 C28 55.4(2) . . . . ? N2 Cr2 S3 C29 -145.1(3) . . . . ? C38 Cr2 S3 C29 122.9(3) . . . . ? Cl5 Cr2 S3 C29 30.8(3) . . . . ? S4 Cr2 S3 C29 175.7(3) . . . . ? Cl4 Cr2 S3 C29 -55.9(3) . . . . ? N2 Cr2 S4 C33 -19.1(3) . . . . ? C38 Cr2 S4 C33 72.7(3) . . . . ? Cl5 Cr2 S4 C33 164.8(2) . . . . ? S3 Cr2 S4 C33 19.5(3) . . . . ? Cl4 Cr2 S4 C33 -108.1(2) . . . . ? N2 Cr2 S4 C34 90.5(3) . . . . ? C38 Cr2 S4 C34 -177.7(3) . . . . ? Cl5 Cr2 S4 C34 -85.6(3) . . . . ? S3 Cr2 S4 C34 129.1(3) . . . . ? Cl4 Cr2 S4 C34 1.5(3) . . . . ? C5 N1 C1 C2 0.4(8) . . . . ? Cr1 N1 C1 C2 -179.9(5) . . . . ? C5 N1 C1 C6 179.8(5) . . . . ? Cr1 N1 C1 C6 -0.5(7) . . . . ? N1 C1 C2 C3 1.3(10) . . . . ? C6 C1 C2 C3 -178.0(6) . . . . ? C1 C2 C3 C4 -2.3(10) . . . . ? C2 C3 C4 C5 1.6(10) . . . . ? C1 N1 C5 C4 -1.1(8) . . . . ? Cr1 N1 C5 C4 179.2(5) . . . . ? C1 N1 C5 C11 174.2(5) . . . . ? Cr1 N1 C5 C11 -5.5(7) . . . . ? C3 C4 C5 N1 0.1(10) . . . . ? C3 C4 C5 C11 -175.0(6) . . . . ? N1 C1 C6 S1 36.1(7) . . . . ? C2 C1 C6 S1 -144.6(6) . . . . ? C7 S1 C6 C1 -169.1(5) . . . . ? Cr1 S1 C6 C1 -44.8(4) . . . . ? C6 S1 C7 C10 -173.3(5) . . . . ? Cr1 S1 C7 C10 83.9(5) . . . . ? C6 S1 C7 C9 -55.4(6) . . . . ? Cr1 S1 C7 C9 -158.3(5) . . . . ? C6 S1 C7 C8 66.5(7) . . . . ? Cr1 S1 C7 C8 -36.4(8) . . . . ? N1 C5 C11 S2 29.1(7) . . . . ? C4 C5 C11 S2 -155.6(5) . . . . ? C12 S2 C11 C5 90.6(5) . . . . ? Cr1 S2 C11 C5 -32.0(5) . . . . ? C11 S2 C12 C15 -48.2(5) . . . . ? Cr1 S2 C12 C15 55.0(5) . . . . ? C11 S2 C12 C13 -169.6(4) . . . . ? Cr1 S2 C12 C13 -66.4(5) . . . . ? C11 S2 C12 C14 73.7(5) . . . . ? Cr1 S2 C12 C14 176.9(4) . . . . ? C27 N2 C23 C24 -0.3(9) . . . . ? Cr2 N2 C23 C24 -178.3(5) . . . . ? C27 N2 C23 C28 -179.3(5) . . . . ? Cr2 N2 C23 C28 2.7(7) . . . . ? N2 C23 C24 C25 -1.8(11) . . . . ? C28 C23 C24 C25 177.2(7) . . . . ? C23 C24 C25 C26 1.1(13) . . . . ? C24 C25 C26 C27 1.6(13) . . . . ? C23 N2 C27 C26 3.0(9) . . . . ? Cr2 N2 C27 C26 -178.9(5) . . . . ? C23 N2 C27 C33 -174.0(6) . . . . ? Cr2 N2 C27 C33 4.1(8) . . . . ? C25 C26 C27 N2 -3.7(11) . . . . ? C25 C26 C27 C33 173.2(8) . . . . ? N2 C23 C28 S3 -37.9(7) . . . . ? C24 C23 C28 S3 143.1(6) . . . . ? C29 S3 C28 C23 170.7(4) . . . . ? Cr2 S3 C28 C23 45.5(4) . . . . ? C28 S3 C29 C30 55.5(7) . . . . ? Cr2 S3 C29 C30 159.9(6) . . . . ? C28 S3 C29 C31 173.9(5) . . . . ? Cr2 S3 C29 C31 -81.7(5) . . . . ? C28 S3 C29 C32 -68.5(6) . . . . ? Cr2 S3 C29 C32 35.9(6) . . . . ? N2 C27 C33 S4 -24.6(8) . . . . ? C26 C27 C33 S4 158.4(6) . . . . ? C34 S4 C33 C27 -96.3(5) . . . . ? Cr2 S4 C33 C27 27.6(5) . . . . ? C33 S4 C34 C35 46.8(5) . . . . ? Cr2 S4 C34 C35 -57.8(5) . . . . ? C33 S4 C34 C37 -75.1(5) . . . . ? Cr2 S4 C34 C37 -179.7(4) . . . . ? C33 S4 C34 C36 168.4(4) . . . . ? Cr2 S4 C34 C36 63.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.85 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.133 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.098 ===END===