data_sasol14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H29 Cl2 Cr N P2' _chemical_formula_weight 564.36 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' 'P' 'P' 0.1023 0.0942 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.181(4) _cell_length_b 17.030(5) _cell_length_c 24.820(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5571(3) _cell_formula_units_Z 8 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.723233 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31607 _diffrn_reflns_av_R_equivalents 0.1378 _diffrn_reflns_av_sigmaI/netI 0.0849 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.43 _reflns_number_total 5046 _reflns_number_gt 3244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0618P)^2^+6.0468P] 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 SHELXL _refine_ls_extinction_coef 0.00017(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5046 _refine_ls_number_parameters 312 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1185 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 0.42965(5) 0.14219(4) 0.57651(3) 0.0206(2) Uani 1 1 d . . . Cl1 Cl 0.28328(8) 0.20866(7) 0.60129(5) 0.0262(3) Uani 1 1 d . . . Cl2 Cl 0.36155(8) 0.02529(6) 0.53052(5) 0.0275(3) Uani 1 1 d . . . P1 P 0.45950(9) 0.07401(7) 0.66332(5) 0.0225(3) Uani 1 1 d . . . C2 C 0.5613(3) 0.0084(3) 0.63957(19) 0.0284(11) Uani 1 1 d . . . H2A H 0.5972 -0.0151 0.6707 0.034 Uiso 1 1 calc R . . H2B H 0.5323 -0.0346 0.6176 0.034 Uiso 1 1 calc R . . C3 C 0.6343(3) 0.0570(3) 0.60600(19) 0.0288(11) Uani 1 1 d . . . H3A H 0.6671 0.0969 0.6291 0.035 Uiso 1 1 calc R . . H3B H 0.6880 0.0225 0.5912 0.035 Uiso 1 1 calc R . . N4 N 0.5804(3) 0.0965(2) 0.56103(15) 0.0225(8) Uani 1 1 d D . . H4N H 0.563(3) 0.056(2) 0.5342(14) 0.036(14) Uiso 1 1 d D . . C5 C 0.6506(3) 0.1504(3) 0.53222(19) 0.0268(11) Uani 1 1 d . . . H5A H 0.7122 0.1214 0.5212 0.032 Uiso 1 1 calc R . . H5B H 0.6715 0.1934 0.5567 0.032 Uiso 1 1 calc R . . C6 C 0.5994(3) 0.1845(3) 0.48301(19) 0.0282(11) Uani 1 1 d . . . H6A H 0.5844 0.1422 0.4568 0.034 Uiso 1 1 calc R . . H6B H 0.6448 0.2231 0.4654 0.034 Uiso 1 1 calc R . . P2 P 0.48092(9) 0.23286(6) 0.50385(5) 0.0229(3) Uani 1 1 d . . . C7 C 0.5192(3) 0.1349(3) 0.71455(18) 0.0248(10) Uani 1 1 d . . . C8 C 0.5902(4) 0.1063(3) 0.7511(2) 0.0355(12) Uani 1 1 d . . . H8A H 0.6079 0.0522 0.7506 0.043 Uiso 1 1 calc R . . C9 C 0.6352(4) 0.1561(3) 0.7880(2) 0.0378(13) Uani 1 1 d . . . H9A H 0.6834 0.1361 0.8130 0.045 Uiso 1 1 calc R . . C10 C 0.6105(4) 0.2342(3) 0.7888(2) 0.0390(13) Uani 1 1 d . . . H10A H 0.6409 0.2681 0.8145 0.047 Uiso 1 1 calc R . . C11 C 0.5419(4) 0.2636(3) 0.7523(2) 0.0378(13) Uani 1 1 d . . . H11A H 0.5258 0.3180 0.7525 0.045 Uiso 1 1 calc R . . C12 C 0.4959(4) 0.2139(3) 0.7153(2) 0.0321(12) Uani 1 1 d . . . H12A H 0.4482 0.2344 0.6903 0.039 Uiso 1 1 calc R . . C13 C 0.3713(3) 0.0092(3) 0.69869(19) 0.0247(11) Uani 1 1 d . . . C14 C 0.3046(4) -0.0359(3) 0.6676(2) 0.0322(12) Uani 1 1 d . . . H14A H 0.3050 -0.0313 0.6294 0.039 Uiso 1 1 calc R . . C15 C 0.2375(4) -0.0878(3) 0.6927(2) 0.0369(13) Uani 1 1 d . . . H15A H 0.1932 -0.1192 0.6716 0.044 Uiso 1 1 calc R . . C16 C 0.2355(4) -0.0935(3) 0.7480(2) 0.0354(12) Uani 1 1 d . . . H16A H 0.1895 -0.1285 0.7650 0.043 Uiso 1 1 calc R . . C17 C 0.3002(4) -0.0484(3) 0.7783(2) 0.0391(13) Uani 1 1 d . . . H17A H 0.2984 -0.0525 0.8165 0.047 Uiso 1 1 calc R . . C18 C 0.3678(4) 0.0029(3) 0.7544(2) 0.0297(11) Uani 1 1 d . . . H18A H 0.4118 0.0338 0.7760 0.036 Uiso 1 1 calc R . . C19 C 0.5141(3) 0.3318(3) 0.52575(19) 0.0246(10) Uani 1 1 d . . . C20 C 0.4561(4) 0.3653(3) 0.5663(2) 0.0469(15) Uani 1 1 d . . . H20A H 0.3996 0.3374 0.5805 0.056 Uiso 1 1 calc R . . C21 C 0.4796(5) 0.4387(3) 0.5864(3) 0.0577(18) Uani 1 1 d . . . H21A H 0.4389 0.4610 0.6141 0.069 Uiso 1 1 calc R . . C22 C 0.5610(4) 0.4795(3) 0.5668(2) 0.0430(14) Uani 1 1 d . . . H22A H 0.5768 0.5299 0.5809 0.052 Uiso 1 1 calc R . . C23 C 0.6193(4) 0.4477(3) 0.5269(2) 0.0362(13) Uani 1 1 d . . . H23A H 0.6756 0.4762 0.5131 0.043 Uiso 1 1 calc R . . C24 C 0.5966(3) 0.3738(3) 0.5065(2) 0.0299(11) Uani 1 1 d . . . H24A H 0.6381 0.3518 0.4791 0.036 Uiso 1 1 calc R . . C25 C 0.4080(4) 0.2430(3) 0.44192(18) 0.0261(11) Uani 1 1 d . . . C26 C 0.4319(4) 0.2980(3) 0.4025(2) 0.0376(13) Uani 1 1 d . . . H26A H 0.4877 0.3325 0.4076 0.045 Uiso 1 1 calc R . . C27 C 0.3748(4) 0.3027(3) 0.3558(2) 0.0431(14) Uani 1 1 d . . . H27A H 0.3916 0.3404 0.3290 0.052 Uiso 1 1 calc R . . C28 C 0.2941(4) 0.2532(3) 0.3481(2) 0.0418(14) Uani 1 1 d . . . H28A H 0.2546 0.2573 0.3162 0.050 Uiso 1 1 calc R . . C29 C 0.2698(4) 0.1973(3) 0.3865(2) 0.0363(13) Uani 1 1 d . . . H29A H 0.2144 0.1626 0.3808 0.044 Uiso 1 1 calc R . . C30 C 0.3274(3) 0.1924(3) 0.4334(2) 0.0289(11) Uani 1 1 d . . . H30A H 0.3112 0.1540 0.4598 0.035 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 0.0158(4) 0.0217(4) 0.0244(4) 0.0012(3) 0.0019(3) 0.0028(3) Cl1 0.0185(6) 0.0288(6) 0.0314(7) 0.0024(5) 0.0053(5) 0.0047(4) Cl2 0.0217(6) 0.0260(6) 0.0349(7) -0.0058(5) -0.0009(5) 0.0009(5) P1 0.0213(6) 0.0202(6) 0.0259(7) -0.0007(5) -0.0020(5) 0.0026(5) C2 0.029(3) 0.028(3) 0.028(3) -0.004(2) -0.006(2) 0.009(2) C3 0.017(2) 0.033(3) 0.036(3) -0.005(2) -0.004(2) 0.007(2) N4 0.0179(19) 0.022(2) 0.028(2) -0.0042(17) -0.0005(17) 0.0017(16) C5 0.016(2) 0.020(2) 0.044(3) -0.004(2) 0.007(2) -0.0031(18) C6 0.028(3) 0.020(3) 0.037(3) 0.000(2) 0.011(2) -0.0011(19) P2 0.0204(6) 0.0173(6) 0.0311(7) -0.0001(5) 0.0073(5) 0.0000(5) C7 0.021(2) 0.026(3) 0.027(3) -0.002(2) 0.001(2) -0.0008(19) C8 0.031(3) 0.038(3) 0.037(3) -0.004(2) -0.006(2) 0.011(2) C9 0.026(3) 0.051(4) 0.036(3) -0.010(3) -0.010(2) 0.005(2) C10 0.034(3) 0.042(3) 0.041(3) -0.006(3) -0.006(3) -0.011(2) C11 0.045(3) 0.027(3) 0.042(3) -0.005(2) -0.002(3) -0.004(2) C12 0.032(3) 0.031(3) 0.033(3) 0.001(2) -0.003(2) 0.000(2) C13 0.025(3) 0.019(2) 0.030(3) 0.002(2) -0.001(2) 0.0057(19) C14 0.032(3) 0.030(3) 0.034(3) 0.002(2) -0.007(2) 0.000(2) C15 0.035(3) 0.028(3) 0.048(4) 0.003(2) -0.002(3) -0.003(2) C16 0.026(3) 0.025(3) 0.055(4) 0.011(3) 0.008(3) 0.001(2) C17 0.045(3) 0.033(3) 0.039(3) 0.012(3) 0.006(3) 0.009(2) C18 0.034(3) 0.024(3) 0.031(3) 0.001(2) -0.001(2) 0.003(2) C19 0.021(2) 0.019(2) 0.034(3) -0.002(2) 0.004(2) 0.0023(19) C20 0.043(3) 0.030(3) 0.067(4) -0.013(3) 0.028(3) -0.007(2) C21 0.061(4) 0.033(3) 0.079(5) -0.024(3) 0.036(4) -0.010(3) C22 0.038(3) 0.027(3) 0.064(4) -0.009(3) 0.001(3) -0.006(2) C23 0.020(3) 0.024(3) 0.065(4) -0.001(3) 0.002(3) -0.002(2) C24 0.020(3) 0.024(3) 0.045(3) 0.002(2) 0.004(2) 0.0027(19) C25 0.033(3) 0.020(2) 0.026(3) 0.002(2) 0.010(2) 0.005(2) C26 0.047(3) 0.030(3) 0.035(3) 0.002(2) 0.006(3) 0.000(2) C27 0.059(4) 0.030(3) 0.040(3) 0.005(3) 0.005(3) 0.005(3) C28 0.057(4) 0.037(3) 0.032(3) -0.006(3) -0.004(3) 0.018(3) C29 0.041(3) 0.030(3) 0.038(3) -0.009(2) -0.002(3) 0.006(2) C30 0.031(3) 0.022(3) 0.034(3) 0.003(2) 0.006(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N4 2.168(4) . ? Cr1 Cl1 2.3199(13) . ? Cr1 Cl2 2.4642(14) . ? Cr1 P2 2.4684(14) . ? Cr1 P1 2.4789(15) . ? P1 C7 1.819(5) . ? P1 C13 1.827(5) . ? P1 C2 1.842(4) . ? C2 C3 1.518(6) . ? C3 N4 1.485(6) . ? N4 C5 1.487(5) . ? C5 C6 1.512(7) . ? C6 P2 1.840(5) . ? P2 C25 1.821(5) . ? P2 C19 1.823(5) . ? C7 C12 1.380(6) . ? C7 C8 1.391(6) . ? C8 C9 1.384(7) . ? C9 C10 1.369(7) . ? C10 C11 1.374(7) . ? C11 C12 1.389(7) . ? C13 C18 1.387(7) . ? C13 C14 1.401(6) . ? C14 C15 1.396(7) . ? C15 C16 1.376(7) . ? C16 C17 1.373(7) . ? C17 C18 1.382(7) . ? C19 C20 1.387(7) . ? C19 C24 1.387(6) . ? C20 C21 1.382(7) . ? C21 C22 1.369(7) . ? C22 C23 1.365(7) . ? C23 C24 1.390(7) . ? C25 C30 1.385(7) . ? C25 C26 1.390(7) . ? C26 C27 1.385(7) . ? C27 C28 1.370(8) . ? C28 C29 1.385(7) . ? C29 C30 1.392(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cr1 Cl1 169.79(11) . . ? N4 Cr1 Cl2 87.82(10) . . ? Cl1 Cr1 Cl2 102.36(5) . . ? N4 Cr1 P2 81.02(10) . . ? Cl1 Cr1 P2 96.67(5) . . ? Cl2 Cr1 P2 105.46(5) . . ? N4 Cr1 P1 80.83(10) . . ? Cl1 Cr1 P1 97.48(5) . . ? Cl2 Cr1 P1 94.71(5) . . ? P2 Cr1 P1 152.19(5) . . ? C7 P1 C13 106.4(2) . . ? C7 P1 C2 104.7(2) . . ? C13 P1 C2 104.5(2) . . ? C7 P1 Cr1 114.16(15) . . ? C13 P1 Cr1 126.84(15) . . ? C2 P1 Cr1 96.98(16) . . ? C3 C2 P1 107.9(3) . . ? N4 C3 C2 110.9(3) . . ? C3 N4 C5 110.1(3) . . ? C3 N4 Cr1 117.9(3) . . ? C5 N4 Cr1 115.8(3) . . ? N4 C5 C6 110.3(4) . . ? C5 C6 P2 108.9(3) . . ? C25 P2 C19 106.9(2) . . ? C25 P2 C6 104.7(2) . . ? C19 P2 C6 107.1(2) . . ? C25 P2 Cr1 122.11(16) . . ? C19 P2 Cr1 115.20(16) . . ? C6 P2 Cr1 99.09(15) . . ? C12 C7 C8 118.9(4) . . ? C12 C7 P1 117.9(4) . . ? C8 C7 P1 123.1(4) . . ? C9 C8 C7 120.4(5) . . ? C10 C9 C8 120.2(5) . . ? C9 C10 C11 120.1(5) . . ? C10 C11 C12 120.1(5) . . ? C7 C12 C11 120.4(5) . . ? C18 C13 C14 119.1(4) . . ? C18 C13 P1 123.2(4) . . ? C14 C13 P1 117.8(4) . . ? C15 C14 C13 119.9(5) . . ? C16 C15 C14 120.2(5) . . ? C17 C16 C15 119.7(5) . . ? C16 C17 C18 121.2(5) . . ? C17 C18 C13 120.0(5) . . ? C20 C19 C24 118.1(4) . . ? C20 C19 P2 117.7(4) . . ? C24 C19 P2 124.2(4) . . ? C21 C20 C19 120.7(5) . . ? C22 C21 C20 120.5(5) . . ? C23 C22 C21 119.9(5) . . ? C22 C23 C24 120.2(5) . . ? C19 C24 C23 120.7(5) . . ? C30 C25 C26 119.0(5) . . ? C30 C25 P2 118.4(3) . . ? C26 C25 P2 122.6(4) . . ? C27 C26 C25 120.4(5) . . ? C28 C27 C26 120.1(5) . . ? C27 C28 C29 120.5(5) . . ? C28 C29 C30 119.4(5) . . ? C29 C30 C25 120.6(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 N4 Cr1 P1 C7 89.83(19) . . . . ? Cl1 Cr1 P1 C7 -80.00(16) . . . . ? Cl2 Cr1 P1 C7 176.86(16) . . . . ? P2 Cr1 P1 C7 40.0(2) . . . . ? N4 Cr1 P1 C13 -133.8(2) . . . . ? Cl1 Cr1 P1 C13 56.35(19) . . . . ? Cl2 Cr1 P1 C13 -46.80(19) . . . . ? P2 Cr1 P1 C13 176.34(19) . . . . ? N4 Cr1 P1 C2 -19.79(18) . . . . ? Cl1 Cr1 P1 C2 170.38(16) . . . . ? Cl2 Cr1 P1 C2 67.23(16) . . . . ? P2 Cr1 P1 C2 -69.62(19) . . . . ? C7 P1 C2 C3 -72.4(3) . . . . ? C13 P1 C2 C3 175.9(3) . . . . ? Cr1 P1 C2 C3 44.9(3) . . . . ? P1 C2 C3 N4 -56.4(4) . . . . ? C2 C3 N4 C5 173.9(4) . . . . ? C2 C3 N4 Cr1 38.1(4) . . . . ? Cl1 Cr1 N4 C3 75.0(7) . . . . ? Cl2 Cr1 N4 C3 -101.3(3) . . . . ? P2 Cr1 N4 C3 152.6(3) . . . . ? P1 Cr1 N4 C3 -6.2(3) . . . . ? Cl1 Cr1 N4 C5 -58.4(8) . . . . ? Cl2 Cr1 N4 C5 125.2(3) . . . . ? P2 Cr1 N4 C5 19.2(3) . . . . ? P1 Cr1 N4 C5 -139.6(3) . . . . ? C3 N4 C5 C6 174.2(4) . . . . ? Cr1 N4 C5 C6 -48.9(4) . . . . ? N4 C5 C6 P2 55.7(4) . . . . ? C5 C6 P2 C25 -162.4(3) . . . . ? C5 C6 P2 C19 84.4(3) . . . . ? C5 C6 P2 Cr1 -35.6(3) . . . . ? N4 Cr1 P2 C25 122.6(2) . . . . ? Cl1 Cr1 P2 C25 -67.41(18) . . . . ? Cl2 Cr1 P2 C25 37.42(18) . . . . ? P1 Cr1 P2 C25 172.41(18) . . . . ? N4 Cr1 P2 C19 -104.98(19) . . . . ? Cl1 Cr1 P2 C19 64.99(17) . . . . ? Cl2 Cr1 P2 C19 169.82(16) . . . . ? P1 Cr1 P2 C19 -55.2(2) . . . . ? N4 Cr1 P2 C6 8.86(19) . . . . ? Cl1 Cr1 P2 C6 178.82(16) . . . . ? Cl2 Cr1 P2 C6 -76.35(16) . . . . ? P1 Cr1 P2 C6 58.65(19) . . . . ? C13 P1 C7 C12 -111.4(4) . . . . ? C2 P1 C7 C12 138.3(4) . . . . ? Cr1 P1 C7 C12 33.5(4) . . . . ? C13 P1 C7 C8 71.8(4) . . . . ? C2 P1 C7 C8 -38.6(4) . . . . ? Cr1 P1 C7 C8 -143.4(4) . . . . ? C12 C7 C8 C9 1.2(7) . . . . ? P1 C7 C8 C9 178.0(4) . . . . ? C7 C8 C9 C10 -0.4(8) . . . . ? C8 C9 C10 C11 -0.8(8) . . . . ? C9 C10 C11 C12 1.2(8) . . . . ? C8 C7 C12 C11 -0.8(7) . . . . ? P1 C7 C12 C11 -177.8(4) . . . . ? C10 C11 C12 C7 -0.4(8) . . . . ? C7 P1 C13 C18 -9.2(4) . . . . ? C2 P1 C13 C18 101.3(4) . . . . ? Cr1 P1 C13 C18 -148.1(3) . . . . ? C7 P1 C13 C14 170.9(3) . . . . ? C2 P1 C13 C14 -78.6(4) . . . . ? Cr1 P1 C13 C14 31.9(4) . . . . ? C18 C13 C14 C15 -1.5(7) . . . . ? P1 C13 C14 C15 178.4(4) . . . . ? C13 C14 C15 C16 1.2(7) . . . . ? C14 C15 C16 C17 -0.4(7) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? C16 C17 C18 C13 -0.2(7) . . . . ? C14 C13 C18 C17 1.0(7) . . . . ? P1 C13 C18 C17 -178.9(4) . . . . ? C25 P2 C19 C20 100.1(4) . . . . ? C6 P2 C19 C20 -148.2(4) . . . . ? Cr1 P2 C19 C20 -39.1(5) . . . . ? C25 P2 C19 C24 -83.6(4) . . . . ? C6 P2 C19 C24 28.1(5) . . . . ? Cr1 P2 C19 C24 137.3(4) . . . . ? C24 C19 C20 C21 0.7(8) . . . . ? P2 C19 C20 C21 177.3(5) . . . . ? C19 C20 C21 C22 -0.4(10) . . . . ? C20 C21 C22 C23 0.2(10) . . . . ? C21 C22 C23 C24 -0.4(8) . . . . ? C20 C19 C24 C23 -0.9(7) . . . . ? P2 C19 C24 C23 -177.3(4) . . . . ? C22 C23 C24 C19 0.8(8) . . . . ? C19 P2 C25 C30 -142.4(4) . . . . ? C6 P2 C25 C30 104.3(4) . . . . ? Cr1 P2 C25 C30 -6.6(4) . . . . ? C19 P2 C25 C26 39.4(5) . . . . ? C6 P2 C25 C26 -74.0(4) . . . . ? Cr1 P2 C25 C26 175.1(3) . . . . ? C30 C25 C26 C27 1.0(7) . . . . ? P2 C25 C26 C27 179.2(4) . . . . ? C25 C26 C27 C28 0.1(8) . . . . ? C26 C27 C28 C29 -0.9(8) . . . . ? C27 C28 C29 C30 0.8(7) . . . . ? C28 C29 C30 C25 0.3(7) . . . . ? C26 C25 C30 C29 -1.1(7) . . . . ? P2 C25 C30 C29 -179.4(4) . . . . ? 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 N4 H4N Cl2 0.9799(11) 2.34(3) 3.171(4) 141(4) 5_656 N4 H4N Cl2 0.9799(11) 2.71(4) 3.220(4) 113(3) . _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.43 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.775 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.096 #===END data_sasol24 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H52 Cl2 Cr2 N2 S4' _chemical_formula_weight 671.82 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.291(2) _cell_length_b 9.907(3) _cell_length_c 11.420(3) _cell_angle_alpha 88.901(5) _cell_angle_beta 70.838(5) _cell_angle_gamma 68.979(5) _cell_volume 822.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max .13 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4216 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5276 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.39 _reflns_number_total 2925 _reflns_number_gt 2108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0513P)^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 SHELXL _refine_ls_extinction_coef 0.0060(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2925 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.002 _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 0.40488(7) 0.44509(6) 0.11136(5) 0.01486(17) Uani 1 1 d . . . Cl1 Cl 0.13081(11) 0.39969(9) 0.19312(7) 0.0230(2) Uani 1 1 d . . . S1 S 0.58565(11) 0.25341(9) 0.22258(7) 0.0169(2) Uani 1 1 d . . . C2 C 0.8088(4) 0.2664(4) 0.1418(3) 0.0187(7) Uani 1 1 d . . . H2A H 0.8372 0.3222 0.1980 0.022 Uiso 1 1 calc R . . H2B H 0.9057 0.1675 0.1196 0.022 Uiso 1 1 calc R . . C3 C 0.8088(4) 0.3411(3) 0.0237(3) 0.0182(7) Uani 1 1 d . . . H3A H 0.9242 0.3596 -0.0114 0.022 Uiso 1 1 calc R . . H3B H 0.8059 0.2753 -0.0391 0.022 Uiso 1 1 calc R . . N4 N 0.6500(3) 0.4803(3) 0.0474(2) 0.0146(6) Uani 1 1 d . . . C5 C 0.6703(5) 0.5928(3) 0.1191(3) 0.0182(7) Uani 1 1 d . . . H5A H 0.6387 0.6844 0.0802 0.022 Uiso 1 1 calc R . . H5B H 0.8011 0.5617 0.1117 0.022 Uiso 1 1 calc R . . C6 C 0.5542(5) 0.6239(4) 0.2557(3) 0.0207(8) Uani 1 1 d . . . H6A H 0.5733 0.7016 0.2960 0.025 Uiso 1 1 calc R . . H6B H 0.5885 0.5354 0.2981 0.025 Uiso 1 1 calc R . . S7 S 0.31459(11) 0.68132(9) 0.26657(7) 0.0182(2) Uani 1 1 d . . . C8 C 0.1825(5) 0.6868(4) 0.4338(3) 0.0208(8) Uani 1 1 d . . . C9 C 0.2364(5) 0.5358(4) 0.4768(3) 0.0260(8) Uani 1 1 d . . . H9A H 0.1648 0.5416 0.5653 0.039 Uiso 1 1 calc R . . H9B H 0.3679 0.4977 0.4652 0.039 Uiso 1 1 calc R . . H9C H 0.2112 0.4708 0.4276 0.039 Uiso 1 1 calc R . . C10 C -0.0158(5) 0.7421(4) 0.4387(3) 0.0295(9) Uani 1 1 d . . . H10A H -0.0971 0.7487 0.5248 0.044 Uiso 1 1 calc R . . H10B H -0.0310 0.6748 0.3852 0.044 Uiso 1 1 calc R . . H10C H -0.0476 0.8386 0.4094 0.044 Uiso 1 1 calc R . . C11 C 0.2116(5) 0.7935(4) 0.5110(3) 0.0318(9) Uani 1 1 d . . . H11A H 0.1418 0.7964 0.5994 0.048 Uiso 1 1 calc R . . H11B H 0.1688 0.8907 0.4843 0.048 Uiso 1 1 calc R . . H11C H 0.3428 0.7623 0.4990 0.048 Uiso 1 1 calc R . . C12 C 0.6224(5) 0.0621(3) 0.1775(3) 0.0201(8) Uani 1 1 d . . . C13 C 0.6897(5) 0.0292(4) 0.0363(3) 0.0277(8) Uani 1 1 d . . . H13A H 0.7080 -0.0717 0.0147 0.042 Uiso 1 1 calc R . . H13B H 0.8065 0.0432 -0.0006 0.042 Uiso 1 1 calc R . . H13C H 0.5980 0.0950 0.0038 0.042 Uiso 1 1 calc R . . C14 C 0.4349(5) 0.0515(4) 0.2399(3) 0.0257(8) Uani 1 1 d . . . H14A H 0.4431 -0.0472 0.2204 0.038 Uiso 1 1 calc R . . H14B H 0.3445 0.1216 0.2089 0.038 Uiso 1 1 calc R . . H14C H 0.3967 0.0733 0.3304 0.038 Uiso 1 1 calc R . . C15 C 0.7613(5) -0.0398(4) 0.2318(4) 0.0317(9) Uani 1 1 d . . . H15A H 0.7818 -0.1410 0.2089 0.047 Uiso 1 1 calc R . . H15B H 0.7131 -0.0189 0.3229 0.047 Uiso 1 1 calc R . . H15C H 0.8779 -0.0248 0.1984 0.047 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 0.0134(3) 0.0197(3) 0.0149(3) 0.0046(2) -0.0059(2) -0.0092(2) Cl1 0.0190(4) 0.0343(5) 0.0221(5) 0.0091(4) -0.0077(4) -0.0171(4) S1 0.0173(4) 0.0172(4) 0.0186(4) 0.0037(3) -0.0074(3) -0.0080(4) C2 0.0152(17) 0.0195(18) 0.0252(18) 0.0040(15) -0.0099(15) -0.0082(15) C3 0.0124(17) 0.0201(18) 0.0236(18) 0.0041(15) -0.0045(14) -0.0095(14) N4 0.0137(14) 0.0163(14) 0.0179(14) 0.0038(11) -0.0074(12) -0.0087(12) C5 0.0215(18) 0.0205(19) 0.0179(17) 0.0040(14) -0.0082(15) -0.0128(15) C6 0.026(2) 0.0238(19) 0.0211(18) 0.0039(15) -0.0129(16) -0.0147(16) S7 0.0204(5) 0.0190(5) 0.0161(4) 0.0028(3) -0.0074(4) -0.0074(4) C8 0.0192(19) 0.0243(19) 0.0159(17) -0.0013(15) -0.0034(15) -0.0070(15) C9 0.023(2) 0.028(2) 0.0213(19) 0.0043(16) -0.0035(15) -0.0073(17) C10 0.025(2) 0.031(2) 0.025(2) 0.0032(17) -0.0036(17) -0.0066(17) C11 0.037(2) 0.034(2) 0.022(2) -0.0043(17) -0.0091(18) -0.0115(19) C12 0.0214(19) 0.0149(18) 0.0233(18) 0.0027(15) -0.0085(15) -0.0053(15) C13 0.029(2) 0.024(2) 0.027(2) -0.0006(16) -0.0063(17) -0.0107(17) C14 0.0210(19) 0.0217(19) 0.032(2) 0.0058(16) -0.0059(16) -0.0091(16) C15 0.032(2) 0.021(2) 0.044(2) 0.0074(18) -0.0201(19) -0.0052(17) _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 N4 2.071(2) 2_665 ? Cr1 N4 2.076(3) . ? Cr1 Cl1 2.3584(11) . ? Cr1 S1 2.5655(10) . ? Cr1 S7 2.6854(12) . ? Cr1 Cr1 2.9381(11) 2_665 ? S1 C2 1.826(3) . ? S1 C12 1.863(3) . ? C2 C3 1.526(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.478(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C5 1.484(4) . ? N4 Cr1 2.071(2) 2_665 ? C5 C6 1.508(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 S7 1.821(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? S7 C8 1.854(3) . ? C8 C10 1.517(5) . ? C8 C11 1.520(5) . ? C8 C9 1.521(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.523(5) . ? C12 C14 1.524(5) . ? C12 C15 1.530(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 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 N4 Cr1 N4 89.79(10) 2_665 . ? N4 Cr1 Cl1 93.27(8) 2_665 . ? N4 Cr1 Cl1 176.94(7) . . ? N4 Cr1 S1 151.73(8) 2_665 . ? N4 Cr1 S1 81.55(7) . . ? Cl1 Cr1 S1 95.62(4) . . ? N4 Cr1 S7 106.70(8) 2_665 . ? N4 Cr1 S7 80.16(8) . . ? Cl1 Cr1 S7 99.16(4) . . ? S1 Cr1 S7 98.30(4) . . ? N4 Cr1 Cr1 44.96(7) 2_665 2_665 ? N4 Cr1 Cr1 44.82(7) . 2_665 ? Cl1 Cr1 Cr1 138.23(3) . 2_665 ? S1 Cr1 Cr1 121.13(4) . 2_665 ? S7 Cr1 Cr1 94.69(4) . 2_665 ? C2 S1 C12 103.97(15) . . ? C2 S1 Cr1 96.38(10) . . ? C12 S1 Cr1 115.03(10) . . ? C3 C2 S1 110.9(2) . . ? C3 C2 H2A 109.5 . . ? S1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? N4 C3 C2 112.3(3) . . ? N4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? N4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C3 N4 C5 110.9(2) . . ? C3 N4 Cr1 114.14(19) . 2_665 ? C5 N4 Cr1 111.44(19) . 2_665 ? C3 N4 Cr1 110.47(19) . . ? C5 N4 Cr1 118.3(2) . . ? Cr1 N4 Cr1 90.21(10) 2_665 . ? N4 C5 C6 115.3(3) . . ? N4 C5 H5A 108.4 . . ? C6 C5 H5A 108.4 . . ? N4 C5 H5B 108.4 . . ? C6 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C5 C6 S7 107.5(2) . . ? C5 C6 H6A 110.2 . . ? S7 C6 H6A 110.2 . . ? C5 C6 H6B 110.2 . . ? S7 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 S7 C8 105.68(15) . . ? C6 S7 Cr1 89.32(11) . . ? C8 S7 Cr1 118.54(11) . . ? C10 C8 C11 110.4(3) . . ? C10 C8 C9 110.5(3) . . ? C11 C8 C9 111.5(3) . . ? C10 C8 S7 103.6(2) . . ? C11 C8 S7 109.5(2) . . ? C9 C8 S7 111.1(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 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 112.0(3) . . ? C13 C12 C15 111.0(3) . . ? C14 C12 C15 109.7(3) . . ? C13 C12 S1 110.8(2) . . ? C14 C12 S1 104.6(2) . . ? C15 C12 S1 108.6(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 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 N4 Cr1 S1 C2 63.86(19) 2_665 . . . ? N4 Cr1 S1 C2 -9.62(13) . . . . ? Cl1 Cr1 S1 C2 171.56(11) . . . . ? S7 Cr1 S1 C2 -88.30(11) . . . . ? Cr1 Cr1 S1 C2 12.34(11) 2_665 . . . ? N4 Cr1 S1 C12 -44.8(2) 2_665 . . . ? N4 Cr1 S1 C12 -118.30(14) . . . . ? Cl1 Cr1 S1 C12 62.89(12) . . . . ? S7 Cr1 S1 C12 163.03(12) . . . . ? Cr1 Cr1 S1 C12 -96.34(13) 2_665 . . . ? C12 S1 C2 C3 100.7(2) . . . . ? Cr1 S1 C2 C3 -17.2(2) . . . . ? S1 C2 C3 N4 50.6(3) . . . . ? C2 C3 N4 C5 71.1(3) . . . . ? C2 C3 N4 Cr1 -162.0(2) . . . 2_665 ? C2 C3 N4 Cr1 -62.1(3) . . . . ? N4 Cr1 N4 C3 -116.0(2) 2_665 . . . ? Cl1 Cr1 N4 C3 59.7(16) . . . . ? S1 Cr1 N4 C3 37.02(18) . . . . ? S7 Cr1 N4 C3 137.03(19) . . . . ? Cr1 Cr1 N4 C3 -116.0(2) 2_665 . . . ? N4 Cr1 N4 C5 114.7(2) 2_665 . . . ? Cl1 Cr1 N4 C5 -69.7(16) . . . . ? S1 Cr1 N4 C5 -92.3(2) . . . . ? S7 Cr1 N4 C5 7.66(19) . . . . ? Cr1 Cr1 N4 C5 114.7(2) 2_665 . . . ? N4 Cr1 N4 Cr1 0.0 2_665 . . 2_665 ? Cl1 Cr1 N4 Cr1 175.7(14) . . . 2_665 ? S1 Cr1 N4 Cr1 152.99(9) . . . 2_665 ? S7 Cr1 N4 Cr1 -107.00(8) . . . 2_665 ? C3 N4 C5 C6 -103.4(3) . . . . ? Cr1 N4 C5 C6 128.3(2) 2_665 . . . ? Cr1 N4 C5 C6 25.8(3) . . . . ? N4 C5 C6 S7 -58.4(3) . . . . ? C5 C6 S7 C8 170.4(2) . . . . ? C5 C6 S7 Cr1 50.9(2) . . . . ? N4 Cr1 S7 C6 -116.97(13) 2_665 . . . ? N4 Cr1 S7 C6 -30.18(13) . . . . ? Cl1 Cr1 S7 C6 146.79(11) . . . . ? S1 Cr1 S7 C6 49.68(11) . . . . ? Cr1 Cr1 S7 C6 -72.74(11) 2_665 . . . ? N4 Cr1 S7 C8 135.49(14) 2_665 . . . ? N4 Cr1 S7 C8 -137.72(13) . . . . ? Cl1 Cr1 S7 C8 39.26(12) . . . . ? S1 Cr1 S7 C8 -57.86(12) . . . . ? Cr1 Cr1 S7 C8 179.72(12) 2_665 . . . ? C6 S7 C8 C10 177.3(2) . . . . ? Cr1 S7 C8 C10 -84.7(2) . . . . ? C6 S7 C8 C11 59.6(3) . . . . ? Cr1 S7 C8 C11 157.53(19) . . . . ? C6 S7 C8 C9 -64.0(3) . . . . ? Cr1 S7 C8 C9 33.9(3) . . . . ? C2 S1 C12 C13 -56.8(2) . . . . ? Cr1 S1 C12 C13 47.2(3) . . . . ? C2 S1 C12 C14 -177.7(2) . . . . ? Cr1 S1 C12 C14 -73.6(2) . . . . ? C2 S1 C12 C15 65.3(3) . . . . ? Cr1 S1 C12 C15 169.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.395 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.083 #===END data_sasol30 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H32 Cl4 Cr Li O4' _chemical_formula_weight 489.16 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' '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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.954(4) _cell_length_b 10.2303(12) _cell_length_c 19.885(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.807(2) _cell_angle_gamma 90.00 _cell_volume 6649.3(13) _cell_formula_units_Z 12 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 81 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max .05 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3060 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.666666 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18443 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.37 _reflns_number_total 6041 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0455P)^2^+9.0834P] 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 6041 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.169930(15) 0.33071(6) 0.58633(3) 0.01618(15) Uani 1 1 d . . . Cl1 Cl 0.17722(3) 0.49252(9) 0.67243(5) 0.0240(2) Uani 1 1 d . . . Cl2 Cl 0.16569(3) 0.48132(9) 0.49677(5) 0.0249(2) Uani 1 1 d . . . Cl3 Cl 0.17428(2) 0.16643(9) 0.67398(5) 0.0225(2) Uani 1 1 d . . . Cl4 Cl 0.16180(2) 0.16010(9) 0.49975(5) 0.0211(2) Uani 1 1 d . . . O1 O 0.10802(6) 0.3334(2) 0.54448(13) 0.0223(5) Uani 1 1 d . . . C2 C 0.08758(10) 0.3620(4) 0.5901(2) 0.0275(9) Uani 1 1 d . . . H2A H 0.0919 0.4542 0.6071 0.033 Uiso 1 1 calc R . . H2B H 0.0978 0.3045 0.6353 0.033 Uiso 1 1 calc R . . C3 C 0.04303(11) 0.3358(5) 0.5374(2) 0.0393(11) Uani 1 1 d . . . H3A H 0.0363 0.2424 0.5385 0.047 Uiso 1 1 calc R . . H3B H 0.0252 0.3897 0.5512 0.047 Uiso 1 1 calc R . . C4 C 0.03836(11) 0.3737(5) 0.4606(2) 0.0382(11) Uani 1 1 d . . . H4A H 0.0151 0.3269 0.4195 0.046 Uiso 1 1 calc R . . H4B H 0.0339 0.4690 0.4522 0.046 Uiso 1 1 calc R . . C5 C 0.07815(10) 0.3338(4) 0.4638(2) 0.0297(9) Uani 1 1 d . . . H5A H 0.0759 0.2458 0.4415 0.036 Uiso 1 1 calc R . . H5B H 0.0863 0.3967 0.4354 0.036 Uiso 1 1 calc R . . O6 O 0.23137(6) 0.3191(2) 0.62997(13) 0.0228(6) Uani 1 1 d . . . C7 C 0.25363(11) 0.3302(4) 0.5862(2) 0.0310(9) Uani 1 1 d . . . H7A H 0.2491 0.4174 0.5620 0.037 Uiso 1 1 calc R . . H7B H 0.2442 0.2628 0.5459 0.037 Uiso 1 1 calc R . . C8 C 0.29696(12) 0.3119(6) 0.6390(2) 0.0625(17) Uani 1 1 d . . . H8A H 0.3136 0.3793 0.6304 0.075 Uiso 1 1 calc R . . H8B H 0.3062 0.2247 0.6316 0.075 Uiso 1 1 calc R . . C9 C 0.30141(11) 0.3235(5) 0.7161(2) 0.0363(10) Uani 1 1 d . . . H9A H 0.3179 0.2498 0.7479 0.044 Uiso 1 1 calc R . . H9B H 0.3156 0.4062 0.7398 0.044 Uiso 1 1 calc R . . C10 C 0.26063(11) 0.3218(6) 0.7110(2) 0.0519(14) Uani 1 1 d . . . H10A H 0.2564 0.4007 0.7353 0.062 Uiso 1 1 calc R . . H10B H 0.2573 0.2435 0.7369 0.062 Uiso 1 1 calc R . . Li1 Li 0.16768(17) -0.0034(6) 0.5879(3) 0.0236(14) Uani 1 1 d . . . O11 O 0.11822(7) -0.0989(2) 0.56202(15) 0.0288(6) Uani 1 1 d . . . C12 C 0.08342(11) -0.0220(4) 0.5530(2) 0.0348(10) Uani 1 1 d . . . H12A H 0.0755 0.0402 0.5103 0.042 Uiso 1 1 calc R . . H12B H 0.0902 0.0283 0.6000 0.042 Uiso 1 1 calc R . . C13 C 0.04920(11) -0.1152(4) 0.5373(2) 0.0328(9) Uani 1 1 d . . . H13A H 0.0311 -0.1246 0.4820 0.039 Uiso 1 1 calc R . . H13B H 0.0327 -0.0860 0.5619 0.039 Uiso 1 1 calc R . . C14 C 0.07135(12) -0.2426(4) 0.5719(3) 0.0410(11) Uani 1 1 d . . . H14A H 0.0799 -0.2467 0.6270 0.049 Uiso 1 1 calc R . . H14B H 0.0540 -0.3192 0.5464 0.049 Uiso 1 1 calc R . . C15 C 0.10780(11) -0.2358(4) 0.5573(2) 0.0336(10) Uani 1 1 d . . . H15A H 0.1309 -0.2867 0.5960 0.040 Uiso 1 1 calc R . . H15B H 0.1009 -0.2709 0.5064 0.040 Uiso 1 1 calc R . . O16 O 0.21521(7) -0.1068(2) 0.60897(14) 0.0264(6) Uani 1 1 d . . . C17 C 0.21476(11) -0.2383(4) 0.5831(2) 0.0345(10) Uani 1 1 d . . . H17A H 0.1990 -0.2428 0.5270 0.041 Uiso 1 1 calc R . . H17B H 0.2020 -0.2981 0.6051 0.041 Uiso 1 1 calc R . . C18 C 0.25858(11) -0.2758(4) 0.6092(3) 0.0390(10) Uani 1 1 d . . . H18A H 0.2614 -0.3234 0.5686 0.047 Uiso 1 1 calc R . . H18B H 0.2687 -0.3324 0.6548 0.047 Uiso 1 1 calc R . . C19 C 0.28215(12) -0.1482(4) 0.6276(3) 0.0401(11) Uani 1 1 d . . . H19A H 0.3031 -0.1456 0.6817 0.048 Uiso 1 1 calc R . . H19B H 0.2958 -0.1368 0.5955 0.048 Uiso 1 1 calc R . . C20 C 0.25024(11) -0.0435(4) 0.6108(3) 0.0385(10) Uani 1 1 d . . . H20A H 0.2607 0.0245 0.6508 0.046 Uiso 1 1 calc R . . H20B H 0.2430 -0.0017 0.5612 0.046 Uiso 1 1 calc R . . Cr21 Cr 0.0000 -0.11033(8) 0.2500 0.01567(19) Uani 1 2 d S . . Cl21 Cl 0.00677(2) 0.04693(8) 0.33828(5) 0.0226(2) Uani 1 1 d . . . Cl23 Cl -0.00783(2) -0.27763(9) 0.16138(5) 0.0212(2) Uani 1 1 d . . . O21 O 0.06149(6) -0.1165(2) 0.28940(12) 0.0210(5) Uani 1 1 d . . . C22 C 0.08197(10) -0.1007(4) 0.2426(2) 0.0260(8) Uani 1 1 d . . . H22A H 0.0784 -0.0106 0.2223 0.031 Uiso 1 1 calc R . . H22B H 0.0708 -0.1628 0.1994 0.031 Uiso 1 1 calc R . . C23 C 0.12631(11) -0.1286(6) 0.2940(2) 0.0528(14) Uani 1 1 d . . . H23A H 0.1436 -0.0575 0.2907 0.063 Uiso 1 1 calc R . . H23B H 0.1345 -0.2119 0.2795 0.063 Uiso 1 1 calc R . . C24 C 0.13119(10) -0.1376(4) 0.3743(2) 0.0308(9) Uani 1 1 d . . . H24A H 0.1354 -0.2293 0.3922 0.037 Uiso 1 1 calc R . . H24B H 0.1547 -0.0843 0.4101 0.037 Uiso 1 1 calc R . . C25 C 0.09147(10) -0.0845(4) 0.3673(2) 0.0299(9) Uani 1 1 d . . . H25A H 0.0844 -0.1270 0.4044 0.036 Uiso 1 1 calc R . . H25B H 0.0932 0.0111 0.3758 0.036 Uiso 1 1 calc R . . Li21 Li 0.0000 -0.4427(9) 0.2500 0.026(2) Uani 1 2 d S . . O31 O 0.04841(7) -0.5444(2) 0.27845(15) 0.0304(6) Uani 1 1 d . . . C32 C 0.05330(11) -0.6796(4) 0.2625(2) 0.0285(9) Uani 1 1 d . . . H32A H 0.0391 -0.6965 0.2070 0.034 Uiso 1 1 calc R . . H32B H 0.0422 -0.7393 0.2875 0.034 Uiso 1 1 calc R . . C33 C 0.09879(10) -0.6981(4) 0.2942(2) 0.0286(9) Uani 1 1 d . . . H33A H 0.1051 -0.7675 0.2665 0.034 Uiso 1 1 calc R . . H33B H 0.1117 -0.7206 0.3490 0.034 Uiso 1 1 calc R . . C34 C 0.11304(12) -0.5656(4) 0.2818(2) 0.0374(10) Uani 1 1 d . . . H34A H 0.1421 -0.5501 0.3186 0.045 Uiso 1 1 calc R . . H34B H 0.1096 -0.5576 0.2295 0.045 Uiso 1 1 calc R . . C35 C 0.08515(11) -0.4719(4) 0.2947(3) 0.0372(10) Uani 1 1 d . . . H35A H 0.0984 -0.4405 0.3479 0.045 Uiso 1 1 calc R . . H35B H 0.0786 -0.3955 0.2604 0.045 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 0.0160(3) 0.0165(3) 0.0146(3) -0.0012(2) 0.0060(2) -0.0011(2) Cl1 0.0260(5) 0.0210(5) 0.0223(5) -0.0041(4) 0.0089(4) 0.0009(4) Cl2 0.0279(5) 0.0217(5) 0.0213(5) 0.0032(4) 0.0082(4) -0.0032(4) Cl3 0.0255(4) 0.0231(5) 0.0186(5) 0.0014(4) 0.0100(4) -0.0011(4) Cl4 0.0247(4) 0.0187(5) 0.0187(4) -0.0018(4) 0.0093(4) 0.0004(4) O1 0.0185(12) 0.0301(15) 0.0177(13) 0.0001(11) 0.0078(10) 0.0016(11) C2 0.0235(18) 0.037(2) 0.026(2) -0.0013(17) 0.0142(16) 0.0056(16) C3 0.0230(19) 0.057(3) 0.039(2) -0.006(2) 0.0151(18) -0.004(2) C4 0.0217(19) 0.058(3) 0.026(2) -0.004(2) 0.0045(17) 0.0078(19) C5 0.0220(18) 0.043(3) 0.0169(19) -0.0011(18) 0.0034(15) -0.0029(18) O6 0.0181(12) 0.0341(16) 0.0154(12) -0.0035(11) 0.0071(10) -0.0030(11) C7 0.029(2) 0.045(3) 0.026(2) -0.0012(19) 0.0190(17) -0.0026(18) C8 0.025(2) 0.128(5) 0.040(3) -0.008(3) 0.020(2) 0.002(3) C9 0.0215(19) 0.054(3) 0.030(2) 0.006(2) 0.0083(17) -0.0055(19) C10 0.021(2) 0.106(4) 0.021(2) -0.008(2) 0.0032(17) 0.003(2) Li1 0.023(3) 0.017(3) 0.028(3) 0.002(3) 0.009(3) 0.003(2) O11 0.0250(13) 0.0172(14) 0.0453(16) -0.0021(12) 0.0172(12) -0.0025(11) C12 0.029(2) 0.028(2) 0.051(3) -0.004(2) 0.021(2) 0.0035(18) C13 0.029(2) 0.036(2) 0.034(2) -0.003(2) 0.0147(18) -0.0030(18) C14 0.038(2) 0.032(2) 0.052(3) 0.016(2) 0.020(2) -0.001(2) C15 0.030(2) 0.021(2) 0.044(2) 0.0064(19) 0.0128(19) 0.0019(17) O16 0.0264(13) 0.0183(14) 0.0350(15) -0.0008(12) 0.0147(12) 0.0003(11) C17 0.034(2) 0.020(2) 0.045(2) -0.0028(19) 0.015(2) -0.0021(18) C18 0.036(2) 0.028(2) 0.048(3) 0.003(2) 0.016(2) 0.0116(19) C19 0.028(2) 0.044(3) 0.049(3) -0.007(2) 0.018(2) -0.0006(19) C20 0.026(2) 0.027(2) 0.059(3) 0.000(2) 0.017(2) -0.0055(18) Cr21 0.0168(4) 0.0145(4) 0.0157(4) 0.000 0.0075(3) 0.000 Cl21 0.0283(4) 0.0192(5) 0.0207(4) -0.0038(4) 0.0117(4) 0.0006(4) Cl23 0.0241(4) 0.0197(5) 0.0186(4) -0.0019(4) 0.0091(4) 0.0001(4) O21 0.0188(12) 0.0275(14) 0.0160(12) -0.0037(11) 0.0076(10) -0.0024(10) C22 0.0269(19) 0.032(2) 0.027(2) -0.0015(18) 0.0192(17) -0.0016(17) C23 0.021(2) 0.101(4) 0.040(3) 0.001(3) 0.0166(19) -0.002(2) C24 0.0212(18) 0.034(2) 0.032(2) -0.0072(18) 0.0080(17) -0.0031(17) C25 0.0201(18) 0.042(3) 0.023(2) -0.0077(18) 0.0055(16) -0.0052(17) Li21 0.035(5) 0.018(5) 0.027(5) 0.000 0.016(4) 0.000 O31 0.0251(13) 0.0149(14) 0.0462(16) -0.0024(13) 0.0124(12) -0.0023(11) C32 0.0281(19) 0.019(2) 0.035(2) -0.0044(18) 0.0121(17) 0.0002(16) C33 0.0246(19) 0.034(2) 0.025(2) 0.0004(18) 0.0098(16) 0.0042(17) C34 0.032(2) 0.043(3) 0.040(2) 0.003(2) 0.0193(19) -0.0069(19) C35 0.028(2) 0.022(2) 0.051(3) 0.007(2) 0.0099(19) -0.0057(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 Cr1 O6 2.021(2) . ? Cr1 O1 2.037(2) . ? Cr1 Cl2 2.3043(11) . ? Cr1 Cl1 2.3052(11) . ? Cr1 Cl4 2.3702(11) . ? Cr1 Cl3 2.3720(11) . ? Cl3 Li1 2.370(6) . ? Cl4 Li1 2.359(6) . ? O1 C2 1.456(4) . ? O1 C5 1.463(4) . ? C2 C3 1.507(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.505(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.499(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? O6 C7 1.454(4) . ? O6 C10 1.463(4) . ? C7 C8 1.460(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.469(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.463(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? Li1 O11 1.919(6) . ? Li1 O16 1.921(6) . ? O11 C15 1.443(4) . ? O11 C12 1.446(4) . ? C12 C13 1.496(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.522(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.506(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O16 C20 1.433(4) . ? O16 C17 1.438(4) . ? C17 C18 1.502(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.516(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.511(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? Cr21 O21 2.030(2) 2 ? Cr21 O21 2.030(2) . ? Cr21 Cl21 2.3070(10) . ? Cr21 Cl21 2.3070(10) 2 ? Cr21 Cl23 2.3754(11) 2 ? Cr21 Cl23 2.3754(11) . ? Cl23 Li21 2.359(6) . ? O21 C22 1.457(4) . ? O21 C25 1.461(4) . ? C22 C23 1.499(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.524(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.509(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? Li21 O31 1.913(5) 2 ? Li21 O31 1.913(5) . ? Li21 Cl23 2.359(6) 2 ? O31 C35 1.445(4) . ? O31 C32 1.450(4) . ? C32 C33 1.507(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.516(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.515(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? 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 O6 Cr1 O1 177.13(11) . . ? O6 Cr1 Cl2 91.66(7) . . ? O1 Cr1 Cl2 90.97(7) . . ? O6 Cr1 Cl1 90.27(7) . . ? O1 Cr1 Cl1 90.78(7) . . ? Cl2 Cr1 Cl1 92.07(4) . . ? O6 Cr1 Cl4 90.28(7) . . ? O1 Cr1 Cl4 88.60(7) . . ? Cl2 Cr1 Cl4 89.49(4) . . ? Cl1 Cr1 Cl4 178.33(4) . . ? O6 Cr1 Cl3 88.00(7) . . ? O1 Cr1 Cl3 89.31(7) . . ? Cl2 Cr1 Cl3 176.85(4) . . ? Cl1 Cr1 Cl3 91.07(4) . . ? Cl4 Cr1 Cl3 87.37(4) . . ? Li1 Cl3 Cr1 92.29(15) . . ? Li1 Cl4 Cr1 92.62(15) . . ? C2 O1 C5 109.7(2) . . ? C2 O1 Cr1 124.0(2) . . ? C5 O1 Cr1 125.2(2) . . ? O1 C2 C3 104.3(3) . . ? O1 C2 H2A 110.9 . . ? C3 C2 H2A 110.9 . . ? O1 C2 H2B 110.9 . . ? C3 C2 H2B 110.9 . . ? H2A C2 H2B 108.9 . . ? C4 C3 C2 103.3(3) . . ? C4 C3 H3A 111.1 . . ? C2 C3 H3A 111.1 . . ? C4 C3 H3B 111.1 . . ? C2 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? C5 C4 C3 104.0(3) . . ? C5 C4 H4A 111.0 . . ? C3 C4 H4A 111.0 . . ? C5 C4 H4B 111.0 . . ? C3 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? O1 C5 C4 105.7(3) . . ? O1 C5 H5A 110.6 . . ? C4 C5 H5A 110.6 . . ? O1 C5 H5B 110.6 . . ? C4 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C7 O6 C10 108.9(3) . . ? C7 O6 Cr1 125.1(2) . . ? C10 O6 Cr1 125.2(2) . . ? O6 C7 C8 107.3(3) . . ? O6 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O6 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? C7 C8 C9 106.9(3) . . ? C7 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? C7 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.6 . . ? C10 C9 C8 108.5(3) . . ? C10 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C9 C10 O6 106.5(3) . . ? C9 C10 H10A 110.4 . . ? O6 C10 H10A 110.4 . . ? C9 C10 H10B 110.4 . . ? O6 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? O11 Li1 O16 115.9(3) . . ? O11 Li1 Cl4 114.6(3) . . ? O16 Li1 Cl4 108.1(3) . . ? O11 Li1 Cl3 109.4(3) . . ? O16 Li1 Cl3 118.1(3) . . ? Cl4 Li1 Cl3 87.7(2) . . ? C15 O11 C12 109.0(3) . . ? C15 O11 Li1 134.7(3) . . ? C12 O11 Li1 115.9(3) . . ? O11 C12 C13 107.2(3) . . ? O11 C12 H12A 110.3 . . ? C13 C12 H12A 110.3 . . ? O11 C12 H12B 110.3 . . ? C13 C12 H12B 110.3 . . ? H12A C12 H12B 108.5 . . ? C12 C13 C14 103.1(3) . . ? C12 C13 H13A 111.1 . . ? C14 C13 H13A 111.1 . . ? C12 C13 H13B 111.1 . . ? C14 C13 H13B 111.1 . . ? H13A C13 H13B 109.1 . . ? C15 C14 C13 102.4(3) . . ? C15 C14 H14A 111.3 . . ? C13 C14 H14A 111.3 . . ? C15 C14 H14B 111.3 . . ? C13 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? O11 C15 C14 105.6(3) . . ? O11 C15 H15A 110.6 . . ? C14 C15 H15A 110.6 . . ? O11 C15 H15B 110.6 . . ? C14 C15 H15B 110.6 . . ? H15A C15 H15B 108.8 . . ? C20 O16 C17 106.9(3) . . ? C20 O16 Li1 118.7(3) . . ? C17 O16 Li1 125.5(3) . . ? O16 C17 C18 106.6(3) . . ? O16 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O16 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 C19 105.6(3) . . ? C17 C18 H18A 110.6 . . ? C19 C18 H18A 110.6 . . ? C17 C18 H18B 110.6 . . ? C19 C18 H18B 110.6 . . ? H18A C18 H18B 108.8 . . ? C20 C19 C18 104.8(3) . . ? C20 C19 H19A 110.8 . . ? C18 C19 H19A 110.8 . . ? C20 C19 H19B 110.8 . . ? C18 C19 H19B 110.8 . . ? H19A C19 H19B 108.9 . . ? O16 C20 C19 106.7(3) . . ? O16 C20 H20A 110.4 . . ? C19 C20 H20A 110.4 . . ? O16 C20 H20B 110.4 . . ? C19 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? O21 Cr21 O21 176.42(15) 2 . ? O21 Cr21 Cl21 91.14(7) 2 . ? O21 Cr21 Cl21 91.35(7) . . ? O21 Cr21 Cl21 91.35(7) 2 2 ? O21 Cr21 Cl21 91.14(7) . 2 ? Cl21 Cr21 Cl21 91.57(5) . 2 ? O21 Cr21 Cl23 89.47(7) 2 2 ? O21 Cr21 Cl23 87.95(7) . 2 ? Cl21 Cr21 Cl23 90.32(3) . 2 ? Cl21 Cr21 Cl23 177.92(4) 2 2 ? O21 Cr21 Cl23 87.95(7) 2 . ? O21 Cr21 Cl23 89.47(7) . . ? Cl21 Cr21 Cl23 177.92(4) . . ? Cl21 Cr21 Cl23 90.32(3) 2 . ? Cl23 Cr21 Cl23 87.80(5) 2 . ? Li21 Cl23 Cr21 91.81(15) . . ? C22 O21 C25 106.9(2) . . ? C22 O21 Cr21 124.85(19) . . ? C25 O21 Cr21 124.11(19) . . ? O21 C22 C23 105.7(3) . . ? O21 C22 H22A 110.6 . . ? C23 C22 H22A 110.6 . . ? O21 C22 H22B 110.6 . . ? C23 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? C22 C23 C24 106.5(3) . . ? C22 C23 H23A 110.4 . . ? C24 C23 H23A 110.4 . . ? C22 C23 H23B 110.4 . . ? C24 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? C25 C24 C23 104.3(3) . . ? C25 C24 H24A 110.9 . . ? C23 C24 H24A 110.9 . . ? C25 C24 H24B 110.9 . . ? C23 C24 H24B 110.9 . . ? H24A C24 H24B 108.9 . . ? O21 C25 C24 103.9(3) . . ? O21 C25 H25A 111.0 . . ? C24 C25 H25A 111.0 . . ? O21 C25 H25B 111.0 . . ? C24 C25 H25B 111.0 . . ? H25A C25 H25B 109.0 . . ? O31 Li21 O31 114.1(5) 2 . ? O31 Li21 Cl23 112.47(11) 2 2 ? O31 Li21 Cl23 113.36(11) . 2 ? O31 Li21 Cl23 113.36(11) 2 . ? O31 Li21 Cl23 112.47(11) . . ? Cl23 Li21 Cl23 88.6(3) 2 . ? C35 O31 C32 109.8(3) . . ? C35 O31 Li21 116.0(3) . . ? C32 O31 Li21 130.5(3) . . ? O31 C32 C33 104.9(3) . . ? O31 C32 H32A 110.8 . . ? C33 C32 H32A 110.8 . . ? O31 C32 H32B 110.8 . . ? C33 C32 H32B 110.8 . . ? H32A C32 H32B 108.8 . . ? C32 C33 C34 103.0(3) . . ? C32 C33 H33A 111.2 . . ? C34 C33 H33A 111.2 . . ? C32 C33 H33B 111.2 . . ? C34 C33 H33B 111.2 . . ? H33A C33 H33B 109.1 . . ? C35 C34 C33 102.9(3) . . ? C35 C34 H34A 111.2 . . ? C33 C34 H34A 111.2 . . ? C35 C34 H34B 111.2 . . ? C33 C34 H34B 111.2 . . ? H34A C34 H34B 109.1 . . ? O31 C35 C34 106.3(3) . . ? O31 C35 H35A 110.5 . . ? C34 C35 H35A 110.5 . . ? O31 C35 H35B 110.5 . . ? C34 C35 H35B 110.5 . . ? H35A C35 H35B 108.7 . . ? 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 O6 Cr1 Cl3 Li1 -89.13(15) . . . . ? O1 Cr1 Cl3 Li1 89.86(15) . . . . ? Cl2 Cr1 Cl3 Li1 -5.2(7) . . . . ? Cl1 Cr1 Cl3 Li1 -179.37(14) . . . . ? Cl4 Cr1 Cl3 Li1 1.23(14) . . . . ? O6 Cr1 Cl4 Li1 86.75(15) . . . . ? O1 Cr1 Cl4 Li1 -90.61(15) . . . . ? Cl2 Cr1 Cl4 Li1 178.41(14) . . . . ? Cl1 Cr1 Cl4 Li1 -22.4(15) . . . . ? Cl3 Cr1 Cl4 Li1 -1.24(14) . . . . ? O6 Cr1 O1 C2 79(2) . . . . ? Cl2 Cr1 O1 C2 -124.5(3) . . . . ? Cl1 Cr1 O1 C2 -32.4(3) . . . . ? Cl4 Cr1 O1 C2 146.0(3) . . . . ? Cl3 Cr1 O1 C2 58.6(3) . . . . ? O6 Cr1 O1 C5 -114.1(19) . . . . ? Cl2 Cr1 O1 C5 42.3(3) . . . . ? Cl1 Cr1 O1 C5 134.4(3) . . . . ? Cl4 Cr1 O1 C5 -47.1(3) . . . . ? Cl3 Cr1 O1 C5 -134.5(3) . . . . ? C5 O1 C2 C3 18.3(4) . . . . ? Cr1 O1 C2 C3 -173.1(2) . . . . ? O1 C2 C3 C4 -33.1(4) . . . . ? C2 C3 C4 C5 35.5(4) . . . . ? C2 O1 C5 C4 4.0(4) . . . . ? Cr1 O1 C5 C4 -164.4(3) . . . . ? C3 C4 C5 O1 -24.7(4) . . . . ? O1 Cr1 O6 C7 122.4(19) . . . . ? Cl2 Cr1 O6 C7 -34.0(3) . . . . ? Cl1 Cr1 O6 C7 -126.1(3) . . . . ? Cl4 Cr1 O6 C7 55.5(3) . . . . ? Cl3 Cr1 O6 C7 142.8(3) . . . . ? O1 Cr1 O6 C10 -69(2) . . . . ? Cl2 Cr1 O6 C10 134.3(3) . . . . ? Cl1 Cr1 O6 C10 42.3(3) . . . . ? Cl4 Cr1 O6 C10 -136.2(3) . . . . ? Cl3 Cr1 O6 C10 -48.8(3) . . . . ? C10 O6 C7 C8 11.9(5) . . . . ? Cr1 O6 C7 C8 -178.2(3) . . . . ? O6 C7 C8 C9 -14.2(6) . . . . ? C7 C8 C9 C10 11.4(6) . . . . ? C8 C9 C10 O6 -4.2(6) . . . . ? C7 O6 C10 C9 -4.7(5) . . . . ? Cr1 O6 C10 C9 -174.7(3) . . . . ? Cr1 Cl4 Li1 O11 111.5(3) . . . . ? Cr1 Cl4 Li1 O16 -117.6(2) . . . . ? Cr1 Cl4 Li1 Cl3 1.24(14) . . . . ? Cr1 Cl3 Li1 O11 -116.5(2) . . . . ? Cr1 Cl3 Li1 O16 108.0(3) . . . . ? Cr1 Cl3 Li1 Cl4 -1.24(14) . . . . ? O16 Li1 O11 C15 3.3(6) . . . . ? Cl4 Li1 O11 C15 130.3(4) . . . . ? Cl3 Li1 O11 C15 -133.2(4) . . . . ? O16 Li1 O11 C12 174.5(3) . . . . ? Cl4 Li1 O11 C12 -58.5(4) . . . . ? Cl3 Li1 O11 C12 38.0(4) . . . . ? C15 O11 C12 C13 -3.6(4) . . . . ? Li1 O11 C12 C13 -177.0(3) . . . . ? O11 C12 C13 C14 24.1(4) . . . . ? C12 C13 C14 C15 -34.6(4) . . . . ? C12 O11 C15 C14 -18.9(4) . . . . ? Li1 O11 C15 C14 152.8(4) . . . . ? C13 C14 C15 O11 33.1(4) . . . . ? O11 Li1 O16 C20 165.3(3) . . . . ? Cl4 Li1 O16 C20 35.2(4) . . . . ? Cl3 Li1 O16 C20 -62.1(4) . . . . ? O11 Li1 O16 C17 22.4(5) . . . . ? Cl4 Li1 O16 C17 -107.8(4) . . . . ? Cl3 Li1 O16 C17 155.0(3) . . . . ? C20 O16 C17 C18 30.2(4) . . . . ? Li1 O16 C17 C18 176.6(3) . . . . ? O16 C17 C18 C19 -18.0(4) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C17 O16 C20 C19 -30.3(4) . . . . ? Li1 O16 C20 C19 -179.4(3) . . . . ? C18 C19 C20 O16 18.2(5) . . . . ? O21 Cr21 Cl23 Li21 -89.55(7) 2 . . . ? O21 Cr21 Cl23 Li21 87.97(7) . . . . ? Cl21 Cr21 Cl23 Li21 -25.4(9) . . . . ? Cl21 Cr21 Cl23 Li21 179.11(3) 2 . . . ? Cl23 Cr21 Cl23 Li21 0.0 2 . . . ? O21 Cr21 O21 C22 99.0(3) 2 . . . ? Cl21 Cr21 O21 C22 -126.8(3) . . . . ? Cl21 Cr21 O21 C22 -35.2(3) 2 . . . ? Cl23 Cr21 O21 C22 143.0(3) 2 . . . ? Cl23 Cr21 O21 C22 55.1(3) . . . . ? O21 Cr21 O21 C25 -107.0(3) 2 . . . ? Cl21 Cr21 O21 C25 27.2(3) . . . . ? Cl21 Cr21 O21 C25 118.8(3) 2 . . . ? Cl23 Cr21 O21 C25 -63.0(3) 2 . . . ? Cl23 Cr21 O21 C25 -150.9(3) . . . . ? C25 O21 C22 C23 28.9(4) . . . . ? Cr21 O21 C22 C23 -173.4(3) . . . . ? O21 C22 C23 C24 -9.5(5) . . . . ? C22 C23 C24 C25 -12.4(5) . . . . ? C22 O21 C25 C24 -36.8(4) . . . . ? Cr21 O21 C25 C24 165.3(2) . . . . ? C23 C24 C25 O21 29.6(4) . . . . ? Cr21 Cl23 Li21 O31 113.9(3) . . . 2 ? Cr21 Cl23 Li21 O31 -114.8(3) . . . . ? Cr21 Cl23 Li21 Cl23 0.0 . . . 2 ? O31 Li21 O31 C35 175.3(3) 2 . . . ? Cl23 Li21 O31 C35 -54.2(3) 2 . . . ? Cl23 Li21 O31 C35 44.4(4) . . . . ? O31 Li21 O31 C32 19.6(3) 2 . . . ? Cl23 Li21 O31 C32 150.1(3) 2 . . . ? Cl23 Li21 O31 C32 -111.3(4) . . . . ? C35 O31 C32 C33 18.1(4) . . . . ? Li21 O31 C32 C33 175.0(3) . . . . ? O31 C32 C33 C34 -33.4(4) . . . . ? C32 C33 C34 C35 35.6(4) . . . . ? C32 O31 C35 C34 4.7(4) . . . . ? Li21 O31 C35 C34 -155.9(2) . . . . ? C33 C34 C35 O31 -25.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.371 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.075 #===END