Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Binuclear Half-Sandwich Cobalt (III) and Rhodium (III) o-Carboranedichalocogenolato Complexes with Ether Chain-bridged bis(cyclopentadienyl) Ligand ; _publ_contact_author_name 'Prof. Guo-Xin Jin' _publ_contact_author_email GXJIN@FUDAN.EDU.CN loop_ _publ_author_name 'Guo-Xin Jin' 'Yin-Qiang Cheng' 'Xiu-Feng Hou' 'Shu Liu' 'Hui Wang' # Attachment 'complex 3.CIF' data_f51207b _database_code_depnum_ccdc_archive 'CCDC 616733' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 Co2 I4 O3' _chemical_formula_weight 881.75 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' Co Co 0.3494 0.9721 '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' I I -0.4742 1.8119 '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 6.775(2) _cell_length_b 12.876(4) _cell_length_c 13.096(4) _cell_angle_alpha 86.583(5) _cell_angle_beta 85.367(4) _cell_angle_gamma 82.294(4) _cell_volume 1127.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 661 _cell_measurement_theta_min 2.289 _cell_measurement_theta_max 23.512 _exptl_crystal_description block _exptl_crystal_colour black-purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 6.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5428 _exptl_absorpt_correction_T_max 0.7222 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 4756 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3916 _reflns_number_gt 2313 _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^)+(0.0439P)^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 3916 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 0.813 _refine_ls_restrained_S_all 0.813 _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 Co1 Co -0.14608(18) 0.07026(9) 0.76495(10) 0.0409(3) Uani 1 1 d . . . Co2 Co 0.07037(18) 0.37123(9) 0.18905(10) 0.0397(3) Uani 1 1 d . . . I1 I -0.41410(10) 0.22740(5) 0.80198(6) 0.0622(2) Uani 1 1 d . . . I2 I -0.33325(11) -0.00130(6) 0.62642(6) 0.0678(3) Uani 1 1 d . . . I3 I -0.21081(10) 0.52419(5) 0.21610(6) 0.0565(2) Uani 1 1 d . . . I4 I -0.09770(10) 0.28706(5) 0.05059(5) 0.0528(2) Uani 1 1 d . . . C1 C -0.2787(16) -0.0044(8) 0.8611(10) 0.058(3) Uani 1 1 d . . . O1 O -0.3566(13) -0.0505(7) 0.9187(7) 0.090(3) Uani 1 1 d . . . C2 C -0.0607(16) 0.2966(8) 0.2850(9) 0.054(3) Uani 1 1 d . . . O2 O -0.1444(12) 0.2501(6) 0.3429(6) 0.068(2) Uani 1 1 d . . . C3 C 0.0715(14) 0.1689(8) 0.7759(8) 0.051(3) Uani 1 1 d . . . H3 H 0.0469 0.2412 0.7981 0.061 Uiso 1 1 calc R . . C4 C 0.1073(14) 0.0778(9) 0.8406(8) 0.057(3) Uani 1 1 d . . . H4 H 0.1155 0.0756 0.9151 0.068 Uiso 1 1 calc R . . C5 C 0.1382(14) -0.0070(8) 0.7793(9) 0.058(3) Uani 1 1 d . . . H5 H 0.1711 -0.0805 0.8031 0.069 Uiso 1 1 calc R . . C6 C 0.1227(13) 0.0303(7) 0.6746(8) 0.047(2) Uani 1 1 d . . . H6 H 0.1407 -0.0124 0.6142 0.057 Uiso 1 1 calc R . . C7 C 0.0721(14) 0.1388(7) 0.6753(8) 0.046(2) Uani 1 1 d . . . C8 C 0.0400(14) 0.2132(7) 0.5843(8) 0.054(3) Uani 1 1 d . . . H8A H -0.0719 0.2663 0.6006 0.065 Uiso 1 1 calc R . . H8B H 0.0072 0.1753 0.5274 0.065 Uiso 1 1 calc R . . C9 C 0.2219(15) 0.2655(8) 0.5527(7) 0.052(3) Uani 1 1 d . . . H9A H 0.2607 0.2999 0.6105 0.062 Uiso 1 1 calc R . . H9B H 0.3319 0.2133 0.5311 0.062 Uiso 1 1 calc R . . O3 O 0.1795(10) 0.3411(5) 0.4702(5) 0.0577(19) Uani 1 1 d . . . C10 C 0.3240(16) 0.4101(8) 0.4530(8) 0.061(3) Uani 1 1 d . . . H10A H 0.4553 0.3709 0.4399 0.074 Uiso 1 1 calc R . . H10B H 0.3260 0.4507 0.5129 0.074 Uiso 1 1 calc R . . C11 C 0.2711(14) 0.4815(7) 0.3621(7) 0.049(3) Uani 1 1 d . . . H11A H 0.3564 0.5367 0.3566 0.058 Uiso 1 1 calc R . . H11B H 0.1344 0.5144 0.3743 0.058 Uiso 1 1 calc R . . C12 C 0.2900(13) 0.4296(7) 0.2618(8) 0.044(2) Uani 1 1 d . . . C13 C 0.3480(13) 0.3218(8) 0.2433(9) 0.053(3) Uani 1 1 d . . . H13 H 0.3796 0.2651 0.2950 0.064 Uiso 1 1 calc R . . C14 C 0.3540(14) 0.3116(9) 0.1345(10) 0.067(4) Uani 1 1 d . . . H14 H 0.3906 0.2463 0.0987 0.081 Uiso 1 1 calc R . . C15 C 0.3044(14) 0.4097(9) 0.0892(8) 0.053(3) Uani 1 1 d . . . H15 H 0.2980 0.4259 0.0154 0.064 Uiso 1 1 calc R . . C16 C 0.2688(13) 0.4821(8) 0.1645(8) 0.047(3) Uani 1 1 d . . . H16 H 0.2309 0.5577 0.1525 0.057 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 Co1 0.0410(8) 0.0411(7) 0.0409(8) -0.0023(6) -0.0013(6) -0.0074(6) Co2 0.0390(7) 0.0424(7) 0.0389(8) -0.0011(6) -0.0024(6) -0.0105(6) I1 0.0479(4) 0.0485(4) 0.0909(6) -0.0170(4) -0.0105(4) 0.0005(3) I2 0.0536(5) 0.0898(6) 0.0657(6) -0.0322(4) -0.0045(4) -0.0172(4) I3 0.0487(4) 0.0518(4) 0.0684(5) -0.0105(4) -0.0028(4) -0.0019(3) I4 0.0591(5) 0.0566(4) 0.0462(5) -0.0083(3) -0.0076(3) -0.0154(3) C1 0.050(7) 0.057(7) 0.066(9) 0.001(6) 0.000(6) -0.001(5) O1 0.088(7) 0.082(6) 0.087(8) 0.017(5) 0.042(5) -0.008(5) C2 0.048(7) 0.054(7) 0.061(8) -0.013(6) -0.009(6) -0.006(5) O2 0.071(5) 0.082(5) 0.055(6) 0.017(4) -0.005(4) -0.032(4) C3 0.047(6) 0.054(6) 0.057(8) 0.004(5) -0.012(5) -0.021(5) C4 0.049(6) 0.084(8) 0.039(7) -0.002(6) -0.012(5) -0.011(6) C5 0.043(6) 0.056(7) 0.069(9) 0.012(6) 0.007(6) -0.003(5) C6 0.047(6) 0.050(6) 0.045(7) -0.001(5) 0.003(5) -0.010(5) C7 0.044(6) 0.048(6) 0.045(7) 0.001(5) -0.004(5) -0.007(5) C8 0.050(6) 0.059(6) 0.054(7) 0.013(5) -0.002(5) -0.021(5) C9 0.061(7) 0.066(7) 0.029(6) 0.006(5) 0.001(5) -0.017(5) O3 0.061(5) 0.071(5) 0.049(5) 0.017(4) -0.011(4) -0.040(4) C10 0.070(8) 0.076(7) 0.043(7) 0.004(6) -0.011(6) -0.028(6) C11 0.046(6) 0.055(6) 0.049(7) -0.002(5) 0.004(5) -0.029(5) C12 0.040(6) 0.051(6) 0.045(7) -0.002(5) -0.008(5) -0.020(5) C13 0.037(6) 0.052(6) 0.071(8) -0.010(6) -0.009(5) -0.003(5) C14 0.038(6) 0.075(8) 0.092(10) -0.043(8) 0.006(6) -0.008(6) C15 0.043(6) 0.076(8) 0.042(7) 0.005(6) 0.004(5) -0.023(6) C16 0.040(6) 0.049(6) 0.058(7) 0.002(5) -0.003(5) -0.022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 1.795(13) . ? Co1 C5 2.063(10) . ? Co1 C4 2.066(9) . ? Co1 C7 2.071(10) . ? Co1 C3 2.090(9) . ? Co1 C6 2.110(10) . ? Co1 I1 2.5722(15) . ? Co1 I2 2.5754(15) . ? Co2 C2 1.788(13) . ? Co2 C14 2.059(10) . ? Co2 C15 2.065(10) . ? Co2 C13 2.071(9) . ? Co2 C12 2.074(8) . ? Co2 C16 2.083(9) . ? Co2 I3 2.5693(15) . ? Co2 I4 2.5803(14) . ? C1 O1 1.080(12) . ? C2 O2 1.105(12) . ? C3 C7 1.394(14) . ? C3 C4 1.412(13) . ? C3 H3 0.9800 . ? C4 C5 1.377(13) . ? C4 H4 0.9800 . ? C5 C6 1.434(13) . ? C5 H5 0.9800 . ? C6 C7 1.393(12) . ? C6 H6 0.9800 . ? C7 C8 1.496(13) . ? C8 C9 1.499(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O3 1.431(10) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? O3 C10 1.405(11) . ? C10 C11 1.497(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.498(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C16 1.415(13) . ? C12 C13 1.422(12) . ? C13 C14 1.434(15) . ? C13 H13 0.9800 . ? C14 C15 1.375(14) . ? C14 H14 0.9800 . ? C15 C16 1.381(13) . ? C15 H15 0.9800 . ? C16 H16 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 C1 Co1 C5 98.8(4) . . ? C1 Co1 C4 98.8(5) . . ? C5 Co1 C4 39.0(4) . . ? C1 Co1 C7 164.6(4) . . ? C5 Co1 C7 66.6(4) . . ? C4 Co1 C7 66.8(4) . . ? C1 Co1 C3 131.4(5) . . ? C5 Co1 C3 65.6(4) . . ? C4 Co1 C3 39.7(4) . . ? C7 Co1 C3 39.2(4) . . ? C1 Co1 C6 131.4(4) . . ? C5 Co1 C6 40.2(4) . . ? C4 Co1 C6 66.3(4) . . ? C7 Co1 C6 38.9(3) . . ? C3 Co1 C6 65.1(4) . . ? C1 Co1 I1 87.6(3) . . ? C5 Co1 I1 150.4(3) . . ? C4 Co1 I1 111.6(3) . . ? C7 Co1 I1 102.7(3) . . ? C3 Co1 I1 88.5(3) . . ? C6 Co1 I1 140.9(3) . . ? C1 Co1 I2 89.4(4) . . ? C5 Co1 I2 113.7(3) . . ? C4 Co1 I2 152.3(3) . . ? C7 Co1 I2 101.0(3) . . ? C3 Co1 I2 139.2(3) . . ? C6 Co1 I2 88.4(3) . . ? I1 Co1 I2 95.11(5) . . ? C2 Co2 C14 119.1(5) . . ? C2 Co2 C15 158.0(4) . . ? C14 Co2 C15 38.9(4) . . ? C2 Co2 C13 94.3(4) . . ? C14 Co2 C13 40.6(4) . . ? C15 Co2 C13 66.7(4) . . ? C2 Co2 C12 106.3(4) . . ? C14 Co2 C12 67.6(4) . . ? C15 Co2 C12 66.9(4) . . ? C13 Co2 C12 40.1(3) . . ? C2 Co2 C16 144.4(4) . . ? C14 Co2 C16 65.6(4) . . ? C15 Co2 C16 38.9(4) . . ? C13 Co2 C16 66.2(4) . . ? C12 Co2 C16 39.8(4) . . ? C2 Co2 I3 88.0(3) . . ? C14 Co2 I3 151.7(4) . . ? C15 Co2 I3 113.5(3) . . ? C13 Co2 I3 137.3(3) . . ? C12 Co2 I3 98.5(3) . . ? C16 Co2 I3 87.8(3) . . ? C2 Co2 I4 88.9(3) . . ? C14 Co2 I4 93.4(3) . . ? C15 Co2 I4 93.9(3) . . ? C13 Co2 I4 127.2(3) . . ? C12 Co2 I4 159.6(3) . . ? C16 Co2 I4 126.7(3) . . ? I3 Co2 I4 95.37(5) . . ? O1 C1 Co1 178.9(11) . . ? O2 C2 Co2 178.5(10) . . ? C7 C3 C4 108.6(9) . . ? C7 C3 Co1 69.7(6) . . ? C4 C3 Co1 69.3(6) . . ? C7 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Co1 C3 H3 125.7 . . ? C5 C4 C3 107.5(9) . . ? C5 C4 Co1 70.4(6) . . ? C3 C4 Co1 71.0(5) . . ? C5 C4 H4 126.2 . . ? C3 C4 H4 126.2 . . ? Co1 C4 H4 126.2 . . ? C4 C5 C6 108.6(9) . . ? C4 C5 Co1 70.6(6) . . ? C6 C5 Co1 71.7(6) . . ? C4 C5 H5 125.7 . . ? C6 C5 H5 125.7 . . ? Co1 C5 H5 125.7 . . ? C7 C6 C5 106.8(9) . . ? C7 C6 Co1 69.0(6) . . ? C5 C6 Co1 68.2(6) . . ? C7 C6 H6 126.6 . . ? C5 C6 H6 126.6 . . ? Co1 C6 H6 126.6 . . ? C6 C7 C3 108.3(9) . . ? C6 C7 C8 126.9(9) . . ? C3 C7 C8 124.6(9) . . ? C6 C7 Co1 72.1(6) . . ? C3 C7 Co1 71.2(6) . . ? C8 C7 Co1 126.4(7) . . ? C7 C8 C9 111.6(8) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? O3 C9 C8 109.5(8) . . ? O3 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? O3 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C10 O3 C9 112.5(7) . . ? O3 C10 C11 108.0(8) . . ? O3 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? O3 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 C12 115.2(8) . . ? C10 C11 H11A 108.5 . . ? C12 C11 H11A 108.5 . . ? C10 C11 H11B 108.5 . . ? C12 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C16 C12 C13 106.3(9) . . ? C16 C12 C11 125.5(9) . . ? C13 C12 C11 128.0(9) . . ? C16 C12 Co2 70.4(5) . . ? C13 C12 Co2 69.8(5) . . ? C11 C12 Co2 128.4(7) . . ? C12 C13 C14 107.2(9) . . ? C12 C13 Co2 70.1(5) . . ? C14 C13 Co2 69.2(5) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? Co2 C13 H13 126.4 . . ? C15 C14 C13 108.1(9) . . ? C15 C14 Co2 70.8(6) . . ? C13 C14 Co2 70.1(6) . . ? C15 C14 H14 125.9 . . ? C13 C14 H14 125.9 . . ? Co2 C14 H14 125.9 . . ? C14 C15 C16 109.0(10) . . ? C14 C15 Co2 70.3(6) . . ? C16 C15 Co2 71.2(6) . . ? C14 C15 H15 125.5 . . ? C16 C15 H15 125.5 . . ? Co2 C15 H15 125.5 . . ? C15 C16 C12 109.4(9) . . ? C15 C16 Co2 69.9(5) . . ? C12 C16 Co2 69.8(5) . . ? C15 C16 H16 125.3 . . ? C12 C16 H16 125.3 . . ? Co2 C16 H16 125.3 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.106 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.164 # Attachment 'complex 5a.cif' data_f60530e _database_code_depnum_ccdc_archive 'CCDC 616734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H72 B20 Cl6 Co2 O P2 S4' _chemical_formula_weight 1510.09 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 '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' Co Co 0.3494 0.9721 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.826(4) _cell_length_b 18.124(6) _cell_length_c 33.307(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.714(6) _cell_angle_gamma 90.00 _cell_volume 7138(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 962 _cell_measurement_theta_min 2.381 _cell_measurement_theta_max 22.019 _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.90 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4694 _exptl_absorpt_correction_T_max 0.7759 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% 8.64 _diffrn_reflns_number 35152 _diffrn_reflns_av_R_equivalents 0.1111 _diffrn_reflns_av_sigmaI/netI 0.1880 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.15 _reflns_number_total 15557 _reflns_number_gt 5828 _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^)+(0.1090P)^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 15557 _refine_ls_number_parameters 849 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2023 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.2468 _refine_ls_wR_factor_gt 0.2005 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.913 _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 Co1 Co -0.16614(7) 0.29922(5) 0.21208(3) 0.0436(3) Uani 1 1 d . . . Co2 Co 0.19167(7) 0.29439(5) 0.39025(3) 0.0397(3) Uani 1 1 d . . . P1 P -0.10068(15) 0.35119(11) 0.15613(6) 0.0443(5) Uani 1 1 d . . . P2 P 0.12988(14) 0.35522(11) 0.44411(5) 0.0404(5) Uani 1 1 d . . . S1 S -0.27983(15) 0.22528(10) 0.17582(5) 0.0435(5) Uani 1 1 d . . . S2 S -0.30311(16) 0.38415(10) 0.21960(6) 0.0516(5) Uani 1 1 d . . . S3 S 0.28799(15) 0.21456(10) 0.42900(5) 0.0462(5) Uani 1 1 d . . . S4 S 0.34323(15) 0.36919(10) 0.38472(6) 0.0483(5) Uani 1 1 d . . . O1 O -0.0803(6) 0.1270(3) 0.32497(19) 0.086(2) Uani 1 1 d . . . Cl1 Cl 0.3368(5) 0.4841(3) 0.05830(18) 0.242(3) Uani 1 1 d D . . Cl2 Cl 0.1449(5) 0.4603(3) 0.01017(19) 0.252(3) Uani 1 1 d . . . Cl3 Cl 0.6146(4) 0.5357(3) 0.33550(16) 0.186(2) Uani 1 1 d . . . Cl4 Cl 0.8359(4) 0.5045(3) 0.30228(15) 0.1949(19) Uani 1 1 d . . . Cl6 Cl 0.6642(5) 0.0051(4) 0.7956(2) 0.262(3) Uani 1 1 d . . . Cl5 Cl 0.8639(6) -0.0628(5) 0.7782(3) 0.430(7) Uani 1 1 d D . . B1 B -0.4563(7) 0.2553(5) 0.2369(2) 0.047(2) Uani 1 1 d . . . H1 H -0.4014 0.2345 0.2613 0.056 Uiso 1 1 calc R . . B2 B -0.5220(7) 0.1965(5) 0.2024(3) 0.054(2) Uani 1 1 d . . . H2 H -0.5111 0.1363 0.2044 0.065 Uiso 1 1 calc R . . B3 B -0.5312(7) 0.2425(5) 0.1549(3) 0.056(2) Uani 1 1 d . . . H3 H -0.5252 0.2124 0.1264 0.067 Uiso 1 1 calc R . . B4 B -0.4737(7) 0.3315(5) 0.1607(3) 0.048(2) Uani 1 1 d . . . H4 H -0.4305 0.3597 0.1360 0.058 Uiso 1 1 calc R . . B5 B -0.5528(7) 0.3804(5) 0.1963(2) 0.053(2) Uani 1 1 d . . . H5 H -0.5613 0.4407 0.1947 0.063 Uiso 1 1 calc R . . B6 B -0.5423(7) 0.3332(5) 0.2425(3) 0.056(2) Uani 1 1 d . . . H6 H -0.5442 0.3635 0.2711 0.067 Uiso 1 1 calc R . . B7 B -0.6018(7) 0.2454(6) 0.2376(3) 0.063(3) Uani 1 1 d . . . H7 H -0.6441 0.2174 0.2626 0.075 Uiso 1 1 calc R . . B8 B -0.6521(8) 0.2373(6) 0.1865(3) 0.063(3) Uani 1 1 d . . . H8 H -0.7268 0.2043 0.1783 0.076 Uiso 1 1 calc R . . B9 B -0.6206(7) 0.3207(5) 0.1615(3) 0.057(2) Uani 1 1 d . . . H9 H -0.6753 0.3416 0.1371 0.068 Uiso 1 1 calc R . . B10 B -0.6634(7) 0.3232(6) 0.2124(3) 0.062(3) Uani 1 1 d . . . H10 H -0.7456 0.3460 0.2213 0.074 Uiso 1 1 calc R . . B11 B 0.4748(8) 0.2297(5) 0.3696(3) 0.059(3) Uani 1 1 d . . . H11 H 0.4192 0.2130 0.3444 0.070 Uiso 1 1 calc R . . B12 B 0.5226(8) 0.1629(6) 0.4042(3) 0.066(3) Uani 1 1 d . . . H12 H 0.5006 0.1041 0.4020 0.079 Uiso 1 1 calc R . . B13 B 0.5372(8) 0.2094(6) 0.4516(3) 0.066(3) Uani 1 1 d . . . H13 H 0.5230 0.1795 0.4799 0.079 Uiso 1 1 calc R . . B14 B 0.4974(7) 0.3027(5) 0.4457(2) 0.051(2) Uani 1 1 d . . . H14 H 0.4578 0.3337 0.4702 0.061 Uiso 1 1 calc R . . B15 B 0.5883(7) 0.3459(6) 0.4111(3) 0.062(3) Uani 1 1 d . . . H15 H 0.6079 0.4051 0.4129 0.074 Uiso 1 1 calc R . . B16 B 0.5733(7) 0.2998(6) 0.3645(3) 0.068(3) Uani 1 1 d . . . H16 H 0.5835 0.3294 0.3360 0.081 Uiso 1 1 calc R . . B17 B 0.6174(8) 0.2094(7) 0.3699(3) 0.079(3) Uani 1 1 d . . . H17 H 0.6577 0.1797 0.3451 0.095 Uiso 1 1 calc R . . B18 B 0.6592(9) 0.1972(7) 0.4215(3) 0.090(4) Uani 1 1 d . . . H18 H 0.7275 0.1592 0.4304 0.107 Uiso 1 1 calc R . . B19 B 0.6406(7) 0.2802(6) 0.4466(3) 0.066(3) Uani 1 1 d . . . H19 H 0.6959 0.2963 0.4720 0.079 Uiso 1 1 calc R . . B20 B 0.6878(9) 0.2795(8) 0.3969(3) 0.086(4) Uani 1 1 d . . . H20 H 0.7750 0.2953 0.3898 0.103 Uiso 1 1 calc R . . C1 C -0.4207(5) 0.2559(4) 0.18704(19) 0.0388(16) Uani 1 1 d . . . C2 C -0.4328(5) 0.3355(4) 0.2103(2) 0.0430(17) Uani 1 1 d . . . C3 C 0.4324(5) 0.2323(4) 0.41811(19) 0.0453(18) Uani 1 1 d . . . C4 C 0.4603(6) 0.3115(4) 0.3950(2) 0.0471(19) Uani 1 1 d . . . C5 C -0.0452(7) 0.2224(5) 0.2335(3) 0.065(2) Uani 1 1 d . . . H5' H -0.0170 0.1834 0.2185 0.078 Uiso 1 1 calc R . . C6 C -0.0042(7) 0.2918(7) 0.2336(3) 0.090(3) Uani 1 1 d . . . H6' H 0.0580 0.3076 0.2190 0.108 Uiso 1 1 calc R . . C7 C -0.0682(9) 0.3363(5) 0.2584(3) 0.081(3) Uani 1 1 d . . . H7' H -0.0591 0.3864 0.2634 0.097 Uiso 1 1 calc R . . C8 C -0.1525(7) 0.2873(5) 0.2749(2) 0.061(2) Uani 1 1 d . . . H8' H -0.2083 0.3008 0.2929 0.073 Uiso 1 1 calc R . . C9 C -0.1368(6) 0.2182(4) 0.2597(2) 0.0445(18) Uani 1 1 d . . . C10 C -0.1975(7) 0.1492(4) 0.2692(2) 0.063(2) Uani 1 1 d . . . H10A H -0.2267 0.1275 0.2445 0.075 Uiso 1 1 calc R . . H10B H -0.2612 0.1605 0.2862 0.075 Uiso 1 1 calc R . . C11 C -0.1209(8) 0.0936(5) 0.2905(3) 0.078(3) Uani 1 1 d . . . H11A H -0.1631 0.0495 0.2971 0.094 Uiso 1 1 calc R . . H11B H -0.0587 0.0798 0.2733 0.094 Uiso 1 1 calc R . . C12 C 0.0097(8) 0.0918(5) 0.3439(3) 0.080(3) Uani 1 1 d . . . H12A H 0.0714 0.0856 0.3253 0.096 Uiso 1 1 calc R . . H12B H -0.0135 0.0435 0.3532 0.096 Uiso 1 1 calc R . . C13 C 0.0469(8) 0.1378(5) 0.3784(3) 0.080(3) Uani 1 1 d . . . H13A H 0.1100 0.1141 0.3921 0.096 Uiso 1 1 calc R . . H13B H -0.0145 0.1424 0.3973 0.096 Uiso 1 1 calc R . . C14 C 0.0818(6) 0.2129(4) 0.3645(2) 0.0483(19) Uani 1 1 d . . . C15 C 0.0267(6) 0.2799(4) 0.3689(2) 0.051(2) Uani 1 1 d . . . H15' H -0.0372 0.2873 0.3844 0.061 Uiso 1 1 calc R . . C16 C 0.0814(7) 0.3351(5) 0.3465(2) 0.060(2) Uani 1 1 d . . . H16' H 0.0618 0.3846 0.3444 0.072 Uiso 1 1 calc R . . C17 C 0.1720(7) 0.2988(6) 0.3283(2) 0.064(2) Uani 1 1 d . . . H17' H 0.2238 0.3210 0.3113 0.077 Uiso 1 1 calc R . . C18 C 0.1732(7) 0.2257(5) 0.3390(2) 0.059(2) Uani 1 1 d . . . H18' H 0.2256 0.1908 0.3309 0.071 Uiso 1 1 calc R . . C19 C -0.0134(6) 0.4304(4) 0.1692(2) 0.0506(19) Uani 1 1 d . . . C20 C 0.1003(7) 0.4353(5) 0.1589(3) 0.064(2) Uani 1 1 d . . . H20' H 0.1339 0.3981 0.1440 0.077 Uiso 1 1 calc R . . C21 C 0.1625(8) 0.4958(6) 0.1711(3) 0.083(3) Uani 1 1 d . . . H21 H 0.2379 0.4990 0.1637 0.100 Uiso 1 1 calc R . . C22 C 0.1187(8) 0.5500(5) 0.1929(3) 0.085(3) Uani 1 1 d . . . H22 H 0.1629 0.5901 0.2008 0.102 Uiso 1 1 calc R . . C23 C 0.0061(8) 0.5457(5) 0.2039(3) 0.081(3) Uani 1 1 d . . . H23 H -0.0259 0.5830 0.2192 0.097 Uiso 1 1 calc R . . C24 C -0.0573(7) 0.4866(5) 0.1921(2) 0.067(2) Uani 1 1 d . . . H24 H -0.1326 0.4842 0.1998 0.081 Uiso 1 1 calc R . . C25 C -0.2011(6) 0.3857(5) 0.1185(2) 0.053(2) Uani 1 1 d . . . C26 C -0.2313(7) 0.4580(5) 0.1151(3) 0.071(3) Uani 1 1 d . . . H26 H -0.2007 0.4926 0.1327 0.086 Uiso 1 1 calc R . . C27 C -0.3080(9) 0.4807(6) 0.0852(3) 0.090(3) Uani 1 1 d . . . H27 H -0.3285 0.5301 0.0833 0.108 Uiso 1 1 calc R . . C28 C -0.3521(8) 0.4315(7) 0.0592(3) 0.087(3) Uani 1 1 d . . . H28 H -0.4053 0.4466 0.0401 0.105 Uiso 1 1 calc R . . C29 C -0.3195(8) 0.3607(7) 0.0608(3) 0.086(3) Uani 1 1 d . . . H29 H -0.3470 0.3273 0.0418 0.104 Uiso 1 1 calc R . . C30 C -0.2451(6) 0.3370(5) 0.0905(2) 0.064(2) Uani 1 1 d . . . H30 H -0.2245 0.2875 0.0916 0.076 Uiso 1 1 calc R . . C31 C -0.0119(6) 0.2926(5) 0.1248(2) 0.0515(19) Uani 1 1 d . . . C32 C 0.0075(7) 0.2201(5) 0.1344(2) 0.063(2) Uani 1 1 d . . . H32 H -0.0246 0.1998 0.1572 0.076 Uiso 1 1 calc R . . C33 C 0.0753(8) 0.1767(5) 0.1099(3) 0.079(3) Uani 1 1 d . . . H33 H 0.0911 0.1279 0.1166 0.094 Uiso 1 1 calc R . . C34 C 0.1183(7) 0.2072(7) 0.0758(3) 0.087(3) Uani 1 1 d . . . H34 H 0.1629 0.1786 0.0591 0.104 Uiso 1 1 calc R . . C35 C 0.0971(8) 0.2779(7) 0.0660(3) 0.083(3) Uani 1 1 d . . . H35 H 0.1282 0.2977 0.0429 0.100 Uiso 1 1 calc R . . C36 C 0.0308(7) 0.3208(5) 0.0895(3) 0.069(2) Uani 1 1 d . . . H36 H 0.0142 0.3690 0.0818 0.082 Uiso 1 1 calc R . . C37 C 0.0498(6) 0.4359(4) 0.4273(2) 0.0484(19) Uani 1 1 d . . . C38 C -0.0660(7) 0.4433(5) 0.4335(2) 0.064(2) Uani 1 1 d . . . H38 H -0.1040 0.4079 0.4483 0.077 Uiso 1 1 calc R . . C39 C -0.1244(9) 0.5021(6) 0.4180(3) 0.087(3) Uani 1 1 d . . . H39 H -0.2014 0.5071 0.4227 0.104 Uiso 1 1 calc R . . C40 C -0.0694(9) 0.5529(6) 0.3958(3) 0.095(3) Uani 1 1 d . . . H40 H -0.1097 0.5927 0.3853 0.114 Uiso 1 1 calc R . . C41 C 0.0459(8) 0.5475(5) 0.3883(3) 0.071(3) Uani 1 1 d . . . H41 H 0.0826 0.5829 0.3731 0.085 Uiso 1 1 calc R . . C42 C 0.1036(7) 0.4886(4) 0.4040(2) 0.059(2) Uani 1 1 d . . . H42 H 0.1804 0.4837 0.3990 0.071 Uiso 1 1 calc R . . C43 C 0.2304(5) 0.3906(4) 0.48136(19) 0.0437(18) Uani 1 1 d . . . C44 C 0.2778(6) 0.4602(5) 0.4804(2) 0.057(2) Uani 1 1 d . . . H44 H 0.2564 0.4927 0.4600 0.068 Uiso 1 1 calc R . . C45 C 0.3568(7) 0.4827(5) 0.5091(3) 0.075(3) Uani 1 1 d . . . H45 H 0.3884 0.5295 0.5074 0.090 Uiso 1 1 calc R . . C46 C 0.3878(7) 0.4374(6) 0.5392(3) 0.068(3) Uani 1 1 d . . . H46 H 0.4384 0.4536 0.5589 0.082 Uiso 1 1 calc R . . C47 C 0.3451(7) 0.3680(6) 0.5407(2) 0.066(2) Uani 1 1 d . . . H47 H 0.3695 0.3360 0.5609 0.079 Uiso 1 1 calc R . . C48 C 0.2653(6) 0.3440(5) 0.5126(2) 0.054(2) Uani 1 1 d . . . H48 H 0.2350 0.2968 0.5146 0.065 Uiso 1 1 calc R . . C49 C 0.0342(5) 0.3050(4) 0.4770(2) 0.0452(18) Uani 1 1 d . . . C50 C 0.0119(6) 0.2314(5) 0.4700(2) 0.054(2) Uani 1 1 d . . . H50 H 0.0427 0.2079 0.4479 0.064 Uiso 1 1 calc R . . C51 C -0.0573(7) 0.1918(5) 0.4965(3) 0.069(3) Uani 1 1 d . . . H51 H -0.0727 0.1421 0.4922 0.083 Uiso 1 1 calc R . . C52 C -0.1020(7) 0.2281(6) 0.5292(3) 0.071(3) Uani 1 1 d . . . H52 H -0.1482 0.2026 0.5468 0.085 Uiso 1 1 calc R . . C53 C -0.0801(7) 0.2993(6) 0.5358(3) 0.071(3) Uani 1 1 d . . . H53 H -0.1121 0.3228 0.5577 0.085 Uiso 1 1 calc R . . C54 C -0.0108(6) 0.3383(5) 0.5107(2) 0.060(2) Uani 1 1 d . . . H54 H 0.0060 0.3874 0.5163 0.072 Uiso 1 1 calc R . . C55 C 0.2031(11) 0.5171(8) 0.0445(6) 0.239(10) Uani 1 1 d D . . H55A H 0.1553 0.5197 0.0679 0.287 Uiso 1 1 calc R . . H55B H 0.2097 0.5664 0.0333 0.287 Uiso 1 1 calc R . . C56 C 0.6998(19) 0.4678(12) 0.3205(7) 0.269(12) Uani 1 1 d . . . H56A H 0.6627 0.4402 0.2991 0.323 Uiso 1 1 calc R . . H56B H 0.7139 0.4344 0.3427 0.323 Uiso 1 1 calc R . . C57 C 0.8091(16) 0.0159(9) 0.7967(9) 0.364(18) Uani 1 1 d D . . H57A H 0.8311 0.0577 0.7803 0.436 Uiso 1 1 calc R . . H57B H 0.8359 0.0242 0.8240 0.436 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 Co1 0.0315(5) 0.0486(6) 0.0504(6) 0.0049(5) -0.0100(4) -0.0037(4) Co2 0.0319(5) 0.0468(6) 0.0402(5) 0.0000(5) -0.0058(4) 0.0000(4) P1 0.0325(11) 0.0498(12) 0.0503(12) 0.0051(10) -0.0060(8) -0.0040(8) P2 0.0304(10) 0.0472(12) 0.0436(11) -0.0002(9) -0.0012(8) 0.0027(8) S1 0.0379(10) 0.0428(11) 0.0495(11) -0.0061(9) -0.0047(8) 0.0050(8) S2 0.0444(12) 0.0405(12) 0.0697(13) -0.0081(10) -0.0124(9) -0.0036(8) S3 0.0376(10) 0.0496(12) 0.0513(11) 0.0060(9) -0.0044(8) 0.0002(8) S4 0.0408(11) 0.0493(12) 0.0548(12) 0.0086(9) -0.0040(9) -0.0045(8) O1 0.105(5) 0.060(4) 0.093(5) 0.007(3) -0.049(4) -0.020(3) Cl1 0.236(6) 0.212(5) 0.279(6) -0.115(5) -0.045(5) 0.057(5) Cl2 0.271(7) 0.221(6) 0.264(6) -0.003(5) -0.021(5) -0.091(5) Cl3 0.197(5) 0.134(4) 0.229(5) 0.022(3) 0.067(4) 0.037(3) Cl4 0.192(5) 0.190(5) 0.202(4) -0.036(4) -0.009(4) -0.017(4) Cl6 0.219(6) 0.267(7) 0.303(7) -0.118(6) 0.071(5) -0.052(5) Cl5 0.234(7) 0.334(9) 0.728(18) 0.281(11) 0.199(9) 0.193(7) B1 0.044(5) 0.049(6) 0.048(5) 0.011(4) -0.002(4) 0.004(4) B2 0.040(5) 0.059(6) 0.064(6) 0.013(5) -0.012(4) -0.021(4) B3 0.041(6) 0.062(6) 0.063(6) 0.002(5) -0.021(4) -0.009(4) B4 0.034(5) 0.062(6) 0.049(5) 0.005(4) -0.002(4) 0.002(4) B5 0.036(5) 0.063(6) 0.059(6) 0.004(5) -0.006(4) 0.016(4) B6 0.043(5) 0.073(7) 0.050(5) -0.008(5) -0.002(4) 0.008(5) B7 0.035(5) 0.089(8) 0.065(6) 0.017(6) 0.003(4) 0.003(5) B8 0.048(6) 0.071(7) 0.071(7) 0.012(5) -0.010(5) -0.017(5) B9 0.031(5) 0.073(7) 0.067(6) 0.008(5) -0.010(4) 0.004(4) B10 0.033(5) 0.089(8) 0.063(6) 0.009(6) -0.001(4) 0.008(5) B11 0.044(6) 0.071(7) 0.061(6) -0.016(5) -0.002(4) 0.010(5) B12 0.050(6) 0.067(7) 0.080(7) -0.018(6) -0.005(5) 0.019(5) B13 0.045(6) 0.089(8) 0.063(6) -0.007(6) -0.016(5) 0.028(5) B14 0.034(5) 0.078(7) 0.040(5) -0.007(5) -0.007(4) 0.004(4) B15 0.035(5) 0.092(8) 0.058(6) -0.008(6) -0.005(4) -0.018(5) B16 0.033(5) 0.109(9) 0.062(6) -0.001(6) 0.007(4) -0.004(5) B17 0.042(6) 0.108(9) 0.088(8) -0.025(7) 0.013(5) 0.012(6) B18 0.053(7) 0.119(11) 0.096(9) -0.027(8) -0.016(6) 0.031(7) B19 0.033(5) 0.107(9) 0.059(6) -0.008(6) -0.010(4) 0.000(5) B20 0.039(6) 0.140(12) 0.078(8) -0.027(8) 0.000(5) -0.008(6) C1 0.027(4) 0.042(4) 0.046(4) -0.002(3) -0.004(3) -0.005(3) C2 0.031(4) 0.050(5) 0.048(4) -0.004(4) -0.003(3) 0.003(3) C3 0.031(4) 0.064(5) 0.041(4) -0.007(4) -0.005(3) 0.006(3) C4 0.034(4) 0.058(5) 0.049(4) -0.007(4) 0.004(3) -0.004(3) C5 0.047(5) 0.070(6) 0.077(6) 0.028(5) -0.002(4) 0.012(4) C6 0.033(5) 0.126(10) 0.112(9) 0.046(8) -0.022(5) 0.012(6) C7 0.102(8) 0.057(6) 0.083(7) 0.023(5) -0.068(6) -0.035(6) C8 0.060(5) 0.080(7) 0.042(5) 0.008(4) -0.023(4) 0.001(5) C9 0.040(4) 0.050(5) 0.044(4) 0.007(4) -0.008(3) 0.007(3) C10 0.074(6) 0.062(6) 0.052(5) 0.003(4) -0.021(4) -0.018(4) C11 0.094(7) 0.049(6) 0.090(7) 0.009(5) -0.038(6) -0.013(5) C12 0.110(8) 0.048(6) 0.081(6) 0.011(5) -0.044(6) -0.011(5) C13 0.098(7) 0.071(7) 0.070(6) 0.011(5) -0.041(5) -0.024(5) C14 0.044(5) 0.055(5) 0.046(4) -0.009(4) -0.016(4) -0.004(4) C15 0.027(4) 0.071(6) 0.055(5) -0.005(4) -0.015(3) 0.009(4) C16 0.065(6) 0.059(6) 0.054(5) 0.006(4) -0.026(4) 0.000(4) C17 0.062(6) 0.094(7) 0.037(4) -0.002(5) -0.006(4) -0.029(5) C18 0.061(6) 0.067(6) 0.049(5) -0.023(4) -0.014(4) 0.002(4) C19 0.042(5) 0.049(5) 0.061(5) 0.016(4) -0.010(4) 0.001(4) C20 0.046(5) 0.060(6) 0.086(6) 0.005(5) -0.014(4) -0.005(4) C21 0.047(6) 0.076(7) 0.127(9) 0.014(7) -0.004(6) -0.021(5) C22 0.072(7) 0.057(7) 0.127(9) 0.004(6) -0.010(6) -0.020(5) C23 0.072(7) 0.047(6) 0.122(8) -0.012(5) -0.001(6) -0.010(5) C24 0.055(5) 0.069(6) 0.077(6) 0.002(5) -0.014(4) -0.016(5) C25 0.040(5) 0.064(6) 0.055(5) 0.013(4) -0.004(4) -0.002(4) C26 0.063(6) 0.071(7) 0.079(6) 0.014(5) -0.021(5) -0.001(5) C27 0.094(8) 0.075(7) 0.101(8) 0.033(7) -0.007(6) 0.025(6) C28 0.065(7) 0.116(10) 0.080(7) 0.011(7) -0.020(5) 0.014(7) C29 0.067(7) 0.128(10) 0.063(6) 0.004(6) -0.026(5) 0.005(6) C30 0.050(5) 0.088(7) 0.053(5) 0.007(5) -0.010(4) 0.003(5) C31 0.038(4) 0.064(6) 0.053(5) 0.000(4) -0.004(3) 0.007(4) C32 0.057(6) 0.080(7) 0.054(5) -0.010(5) -0.003(4) 0.007(5) C33 0.075(7) 0.079(7) 0.082(7) -0.009(6) -0.010(5) 0.015(5) C34 0.033(5) 0.146(11) 0.081(7) -0.029(8) 0.000(5) 0.011(6) C35 0.045(6) 0.127(10) 0.078(7) 0.000(7) 0.002(5) -0.002(6) C36 0.042(5) 0.096(7) 0.068(6) 0.002(5) 0.007(4) -0.003(5) C37 0.040(4) 0.052(5) 0.053(5) -0.002(4) -0.003(4) 0.016(3) C38 0.051(5) 0.064(6) 0.079(6) 0.001(5) -0.002(4) 0.011(4) C39 0.068(7) 0.083(8) 0.109(8) 0.024(6) -0.001(6) 0.031(6) C40 0.086(8) 0.081(8) 0.119(9) 0.006(7) -0.020(7) 0.045(6) C41 0.083(7) 0.048(5) 0.081(6) 0.012(5) -0.004(5) 0.016(5) C42 0.053(5) 0.051(5) 0.073(6) 0.007(4) 0.008(4) 0.011(4) C43 0.032(4) 0.060(5) 0.038(4) -0.001(4) -0.001(3) 0.008(3) C44 0.053(5) 0.065(6) 0.053(5) 0.006(4) -0.006(4) -0.004(4) C45 0.059(6) 0.086(7) 0.080(7) -0.019(6) -0.003(5) -0.020(5) C46 0.061(6) 0.090(7) 0.053(5) -0.020(5) -0.013(4) -0.016(5) C47 0.050(5) 0.105(8) 0.043(5) -0.009(5) -0.011(4) 0.014(5) C48 0.044(5) 0.066(6) 0.052(5) -0.003(4) -0.002(4) -0.002(4) C49 0.023(4) 0.063(5) 0.049(4) 0.002(4) -0.005(3) 0.001(3) C50 0.045(5) 0.064(6) 0.052(5) 0.005(4) 0.002(4) -0.003(4) C51 0.042(5) 0.077(6) 0.088(7) 0.024(5) -0.010(5) -0.014(4) C52 0.042(5) 0.114(9) 0.057(6) 0.028(6) 0.008(4) 0.002(5) C53 0.046(5) 0.111(9) 0.056(6) -0.002(6) 0.007(4) 0.000(5) C54 0.042(5) 0.086(7) 0.052(5) -0.005(5) -0.006(4) -0.001(4) C55 0.23(2) 0.108(13) 0.38(3) -0.134(16) 0.02(2) -0.004(13) C56 0.28(3) 0.26(3) 0.27(2) 0.06(2) 0.04(2) -0.15(2) C57 0.101(15) 0.37(4) 0.63(5) 0.03(3) 0.16(2) 0.016(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 Co1 C7 2.032(7) . ? Co1 C6 2.041(8) . ? Co1 C8 2.107(7) . ? Co1 C5 2.114(8) . ? Co1 C9 2.185(7) . ? Co1 P1 2.235(2) . ? Co1 S1 2.241(2) . ? Co1 S2 2.251(2) . ? Co2 C17 2.075(7) . ? Co2 C16 2.077(7) . ? Co2 C15 2.085(7) . ? Co2 C18 2.120(7) . ? Co2 C14 2.140(7) . ? Co2 P2 2.236(2) . ? Co2 S3 2.241(2) . ? Co2 S4 2.257(2) . ? P1 C19 1.818(8) . ? P1 C25 1.827(7) . ? P1 C31 1.828(8) . ? P2 C43 1.824(7) . ? P2 C37 1.827(7) . ? P2 C49 1.828(7) . ? S1 C1 1.799(7) . ? S2 C2 1.793(7) . ? S3 C3 1.780(7) . ? S4 C4 1.765(7) . ? O1 C11 1.379(9) . ? O1 C12 1.385(9) . ? Cl1 C55 1.746(9) . ? Cl2 C55 1.680(14) . ? Cl3 C56 1.67(3) . ? Cl4 C56 1.850(18) . ? Cl6 C57 1.725(18) . ? Cl5 C57 1.687(10) . ? B1 C1 1.718(10) . ? B1 C2 1.726(10) . ? B1 B7 1.731(12) . ? B1 B2 1.743(12) . ? B1 B6 1.752(12) . ? B2 C1 1.695(10) . ? B2 B7 1.753(13) . ? B2 B8 1.781(13) . ? B2 B3 1.790(12) . ? B3 C1 1.696(10) . ? B3 B4 1.761(12) . ? B3 B9 1.784(13) . ? B3 B8 1.788(13) . ? B4 C2 1.717(10) . ? B4 C1 1.739(11) . ? B4 B9 1.749(11) . ? B4 B5 1.758(12) . ? B5 C2 1.696(10) . ? B5 B10 1.758(13) . ? B5 B6 1.764(12) . ? B5 B9 1.768(13) . ? B6 C2 1.691(11) . ? B6 B10 1.746(12) . ? B6 B7 1.748(14) . ? B7 B10 1.790(13) . ? B7 B8 1.799(13) . ? B8 B9 1.768(13) . ? B8 B10 1.785(14) . ? B9 B10 1.776(13) . ? B11 C3 1.699(11) . ? B11 C4 1.717(11) . ? B11 B17 1.726(13) . ? B11 B16 1.734(14) . ? B11 B12 1.760(14) . ? B12 C3 1.716(11) . ? B12 B13 1.797(13) . ? B12 B17 1.818(15) . ? B12 B18 1.818(14) . ? B13 C3 1.708(11) . ? B13 B14 1.764(14) . ? B13 B18 1.782(14) . ? B13 B19 1.782(15) . ? B14 B19 1.742(12) . ? B14 C3 1.745(11) . ? B14 C4 1.748(10) . ? B14 B15 1.767(12) . ? B15 C4 1.717(11) . ? B15 B20 1.753(15) . ? B15 B16 1.770(13) . ? B15 B19 1.783(14) . ? B16 C4 1.701(11) . ? B16 B17 1.727(15) . ? B16 B20 1.759(14) . ? B17 B20 1.760(15) . ? B17 B18 1.796(16) . ? B18 B20 1.736(17) . ? B18 B19 1.737(15) . ? B19 B20 1.754(14) . ? C1 C2 1.646(9) . ? C3 C4 1.665(10) . ? C5 C6 1.348(12) . ? C5 C9 1.400(10) . ? C6 C7 1.387(13) . ? C7 C8 1.448(11) . ? C8 C9 1.365(10) . ? C9 C10 1.478(10) . ? C10 C11 1.524(11) . ? C12 C13 1.482(10) . ? C13 C14 1.499(10) . ? C14 C15 1.386(10) . ? C14 C18 1.401(10) . ? C15 C16 1.410(10) . ? C16 C17 1.402(11) . ? C17 C18 1.371(11) . ? C19 C24 1.378(10) . ? C19 C20 1.395(10) . ? C20 C21 1.378(11) . ? C21 C22 1.331(12) . ? C22 C23 1.386(11) . ? C23 C24 1.362(11) . ? C25 C26 1.363(11) . ? C25 C30 1.381(10) . ? C26 C27 1.400(11) . ? C27 C28 1.343(13) . ? C28 C29 1.341(13) . ? C29 C30 1.383(11) . ? C31 C32 1.372(11) . ? C31 C36 1.386(10) . ? C32 C33 1.394(11) . ? C33 C34 1.365(12) . ? C34 C35 1.346(13) . ? C35 C36 1.357(12) . ? C37 C42 1.388(10) . ? C37 C38 1.395(10) . ? C38 C39 1.366(11) . ? C39 C40 1.354(13) . ? C40 C41 1.392(12) . ? C41 C42 1.367(10) . ? C43 C44 1.381(10) . ? C43 C48 1.399(9) . ? C44 C45 1.390(10) . ? C45 C46 1.344(11) . ? C46 C47 1.357(11) . ? C47 C48 1.391(10) . ? C49 C50 1.378(10) . ? C49 C54 1.386(9) . ? C50 C51 1.408(10) . ? C51 C52 1.382(11) . ? C52 C53 1.333(12) . ? C53 C54 1.375(11) . ? 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 C7 Co1 C6 39.8(4) . . ? C7 Co1 C8 40.9(3) . . ? C6 Co1 C8 65.5(4) . . ? C7 Co1 C5 65.4(4) . . ? C6 Co1 C5 37.8(3) . . ? C8 Co1 C5 63.5(3) . . ? C7 Co1 C9 65.6(3) . . ? C6 Co1 C9 64.0(3) . . ? C8 Co1 C9 37.0(3) . . ? C5 Co1 C9 38.0(3) . . ? C7 Co1 P1 107.1(3) . . ? C6 Co1 P1 89.2(3) . . ? C8 Co1 P1 148.0(2) . . ? C5 Co1 P1 108.6(2) . . ? C9 Co1 P1 146.6(2) . . ? C7 Co1 S1 159.9(2) . . ? C6 Co1 S1 134.7(4) . . ? C8 Co1 S1 120.8(2) . . ? C5 Co1 S1 100.8(3) . . ? C9 Co1 S1 94.5(2) . . ? P1 Co1 S1 90.82(8) . . ? C7 Co1 S2 95.4(4) . . ? C6 Co1 S2 132.8(4) . . ? C8 Co1 S2 90.3(2) . . ? C5 Co1 S2 153.8(3) . . ? C9 Co1 S2 119.1(2) . . ? P1 Co1 S2 93.54(8) . . ? S1 Co1 S2 92.36(7) . . ? C17 Co2 C16 39.5(3) . . ? C17 Co2 C15 64.7(3) . . ? C16 Co2 C15 39.6(3) . . ? C17 Co2 C18 38.1(3) . . ? C16 Co2 C18 65.6(3) . . ? C15 Co2 C18 64.2(3) . . ? C17 Co2 C14 64.4(3) . . ? C16 Co2 C14 65.8(3) . . ? C15 Co2 C14 38.3(3) . . ? C18 Co2 C14 38.4(3) . . ? C17 Co2 P2 138.2(3) . . ? C16 Co2 P2 100.3(3) . . ? C15 Co2 P2 91.3(2) . . ? C18 Co2 P2 154.6(2) . . ? C14 Co2 P2 117.3(2) . . ? C17 Co2 S3 130.4(3) . . ? C16 Co2 S3 160.6(2) . . ? C15 Co2 S3 125.6(2) . . ? C18 Co2 S3 97.5(2) . . ? C14 Co2 S3 95.0(2) . . ? P2 Co2 S3 91.44(8) . . ? C17 Co2 S4 88.6(2) . . ? C16 Co2 S4 102.8(2) . . ? C15 Co2 S4 142.1(2) . . ? C18 Co2 S4 111.2(2) . . ? C14 Co2 S4 149.4(2) . . ? P2 Co2 S4 92.12(8) . . ? S3 Co2 S4 92.08(8) . . ? C19 P1 C25 104.9(3) . . ? C19 P1 C31 105.5(4) . . ? C25 P1 C31 100.4(4) . . ? C19 P1 Co1 109.5(3) . . ? C25 P1 Co1 119.2(2) . . ? C31 P1 Co1 116.0(3) . . ? C43 P2 C37 105.0(3) . . ? C43 P2 C49 99.8(3) . . ? C37 P2 C49 105.1(3) . . ? C43 P2 Co2 120.2(2) . . ? C37 P2 Co2 108.8(2) . . ? C49 P2 Co2 116.5(3) . . ? C1 S1 Co1 104.7(2) . . ? C2 S2 Co1 105.1(2) . . ? C3 S3 Co2 104.4(2) . . ? C4 S4 Co2 104.5(2) . . ? C11 O1 C12 115.8(7) . . ? C1 B1 C2 57.1(4) . . ? C1 B1 B7 105.6(6) . . ? C2 B1 B7 105.1(6) . . ? C1 B1 B2 58.6(4) . . ? C2 B1 B2 104.5(6) . . ? B7 B1 B2 60.6(5) . . ? C1 B1 B6 104.3(6) . . ? C2 B1 B6 58.2(4) . . ? B7 B1 B6 60.2(5) . . ? B2 B1 B6 108.0(6) . . ? C1 B2 B1 60.0(4) . . ? C1 B2 B7 105.6(7) . . ? B1 B2 B7 59.4(5) . . ? C1 B2 B8 104.9(6) . . ? B1 B2 B8 108.5(7) . . ? B7 B2 B8 61.2(5) . . ? C1 B2 B3 58.2(4) . . ? B1 B2 B3 108.6(6) . . ? B7 B2 B3 109.1(7) . . ? B8 B2 B3 60.1(5) . . ? C1 B3 B4 60.4(4) . . ? C1 B3 B9 105.2(6) . . ? B4 B3 B9 59.1(5) . . ? C1 B3 B8 104.6(6) . . ? B4 B3 B8 107.1(7) . . ? B9 B3 B8 59.3(5) . . ? C1 B3 B2 58.1(4) . . ? B4 B3 B2 108.1(6) . . ? B9 B3 B2 106.9(7) . . ? B8 B3 B2 59.7(5) . . ? C2 B4 C1 56.9(4) . . ? C2 B4 B9 104.9(6) . . ? C1 B4 B9 104.8(6) . . ? C2 B4 B5 58.4(4) . . ? C1 B4 B5 104.4(6) . . ? B9 B4 B5 60.6(5) . . ? C2 B4 B3 104.4(6) . . ? C1 B4 B3 58.0(4) . . ? B9 B4 B3 61.1(5) . . ? B5 B4 B3 109.1(6) . . ? C2 B5 B4 59.6(4) . . ? C2 B5 B10 104.8(6) . . ? B4 B5 B10 108.3(7) . . ? C2 B5 B6 58.5(4) . . ? B4 B5 B6 108.1(6) . . ? B10 B5 B6 59.4(5) . . ? C2 B5 B9 105.0(6) . . ? B4 B5 B9 59.5(5) . . ? B10 B5 B9 60.5(5) . . ? B6 B5 B9 107.5(7) . . ? C2 B6 B10 105.6(6) . . ? C2 B6 B7 105.9(6) . . ? B10 B6 B7 61.6(5) . . ? C2 B6 B1 60.2(5) . . ? B10 B6 B1 109.2(7) . . ? B7 B6 B1 59.3(5) . . ? C2 B6 B5 58.8(5) . . ? B10 B6 B5 60.1(5) . . ? B7 B6 B5 109.6(7) . . ? B1 B6 B5 109.4(6) . . ? B1 B7 B6 60.5(5) . . ? B1 B7 B2 60.0(5) . . ? B6 B7 B2 107.7(6) . . ? B1 B7 B10 108.1(7) . . ? B6 B7 B10 59.1(5) . . ? B2 B7 B10 107.8(7) . . ? B1 B7 B8 108.3(6) . . ? B6 B7 B8 106.9(7) . . ? B2 B7 B8 60.2(5) . . ? B10 B7 B8 59.7(5) . . ? B9 B8 B2 108.0(6) . . ? B9 B8 B10 60.0(5) . . ? B2 B8 B10 106.8(6) . . ? B9 B8 B3 60.2(5) . . ? B2 B8 B3 60.2(5) . . ? B10 B8 B3 107.7(7) . . ? B9 B8 B7 107.9(7) . . ? B2 B8 B7 58.6(5) . . ? B10 B8 B7 59.9(5) . . ? B3 B8 B7 107.2(6) . . ? B4 B9 B8 108.5(6) . . ? B4 B9 B5 60.0(5) . . ? B8 B9 B5 108.1(6) . . ? B4 B9 B10 107.9(6) . . ? B8 B9 B10 60.5(5) . . ? B5 B9 B10 59.5(5) . . ? B4 B9 B3 59.8(5) . . ? B8 B9 B3 60.4(5) . . ? B5 B9 B3 107.6(6) . . ? B10 B9 B3 108.3(7) . . ? B6 B10 B5 60.4(5) . . ? B6 B10 B9 108.0(6) . . ? B5 B10 B9 60.0(5) . . ? B6 B10 B8 107.5(7) . . ? B5 B10 B8 107.8(6) . . ? B9 B10 B8 59.5(5) . . ? B6 B10 B7 59.2(5) . . ? B5 B10 B7 107.9(6) . . ? B9 B10 B7 107.9(7) . . ? B8 B10 B7 60.4(5) . . ? C3 B11 C4 58.4(4) . . ? C3 B11 B17 107.4(7) . . ? C4 B11 B17 106.5(7) . . ? C3 B11 B16 106.2(7) . . ? C4 B11 B16 59.1(5) . . ? B17 B11 B16 59.9(6) . . ? C3 B11 B12 59.4(5) . . ? C4 B11 B12 107.7(6) . . ? B17 B11 B12 62.8(6) . . ? B16 B11 B12 110.9(7) . . ? C3 B12 B11 58.5(5) . . ? C3 B12 B13 58.1(4) . . ? B11 B12 B13 106.3(7) . . ? C3 B12 B17 102.7(7) . . ? B11 B12 B17 57.7(5) . . ? B13 B12 B17 106.4(8) . . ? C3 B12 B18 102.5(7) . . ? B11 B12 B18 104.4(8) . . ? B13 B12 B18 59.0(6) . . ? B17 B12 B18 59.2(6) . . ? C3 B13 B14 60.3(5) . . ? C3 B13 B18 104.3(7) . . ? B14 B13 B18 105.8(8) . . ? C3 B13 B19 104.9(7) . . ? B14 B13 B19 58.8(6) . . ? B18 B13 B19 58.3(6) . . ? C3 B13 B12 58.5(5) . . ? B14 B13 B12 109.1(7) . . ? B18 B13 B12 61.1(6) . . ? B19 B13 B12 108.3(7) . . ? B19 B14 C3 105.1(6) . . ? B19 B14 C4 105.7(6) . . ? C3 B14 C4 56.9(4) . . ? B19 B14 B13 61.1(6) . . ? C3 B14 B13 58.3(5) . . ? C4 B14 B13 105.1(6) . . ? B19 B14 B15 61.1(5) . . ? C3 B14 B15 104.4(6) . . ? C4 B14 B15 58.5(4) . . ? B13 B14 B15 109.5(7) . . ? C4 B15 B20 105.0(7) . . ? C4 B15 B14 60.2(4) . . ? B20 B15 B14 106.7(8) . . ? C4 B15 B16 58.4(5) . . ? B20 B15 B16 59.9(6) . . ? B14 B15 B16 107.9(7) . . ? C4 B15 B19 105.3(7) . . ? B20 B15 B19 59.5(6) . . ? B14 B15 B19 58.8(5) . . ? B16 B15 B19 107.3(8) . . ? C4 B16 B17 107.2(7) . . ? C4 B16 B11 60.0(5) . . ? B17 B16 B11 59.8(6) . . ? C4 B16 B20 105.4(7) . . ? B17 B16 B20 60.6(7) . . ? B11 B16 B20 107.5(8) . . ? C4 B16 B15 59.3(5) . . ? B17 B16 B15 109.3(8) . . ? B11 B16 B15 108.7(7) . . ? B20 B16 B15 59.5(6) . . ? B11 B17 B16 60.3(6) . . ? B11 B17 B20 107.8(7) . . ? B16 B17 B20 60.6(6) . . ? B11 B17 B18 106.8(7) . . ? B16 B17 B18 107.2(8) . . ? B20 B17 B18 58.4(7) . . ? B11 B17 B12 59.5(5) . . ? B16 B17 B12 108.5(7) . . ? B20 B17 B12 107.7(7) . . ? B18 B17 B12 60.4(6) . . ? B20 B18 B19 60.7(7) . . ? B20 B18 B13 108.8(8) . . ? B19 B18 B13 60.9(6) . . ? B20 B18 B17 59.7(6) . . ? B19 B18 B17 108.6(9) . . ? B13 B18 B17 108.0(7) . . ? B20 B18 B12 108.7(8) . . ? B19 B18 B12 109.4(7) . . ? B13 B18 B12 59.9(6) . . ? B17 B18 B12 60.4(6) . . ? B18 B19 B14 108.8(7) . . ? B18 B19 B20 59.6(6) . . ? B14 B19 B20 107.8(7) . . ? B18 B19 B13 60.8(6) . . ? B14 B19 B13 60.1(5) . . ? B20 B19 B13 108.0(7) . . ? B18 B19 B15 107.7(7) . . ? B14 B19 B15 60.2(5) . . ? B20 B19 B15 59.4(6) . . ? B13 B19 B15 108.0(6) . . ? B18 B20 B15 109.1(8) . . ? B18 B20 B19 59.7(6) . . ? B15 B20 B19 61.1(6) . . ? B18 B20 B16 108.4(8) . . ? B15 B20 B16 60.5(6) . . ? B19 B20 B16 109.0(7) . . ? B18 B20 B17 61.8(7) . . ? B15 B20 B17 108.6(7) . . ? B19 B20 B17 109.6(8) . . ? B16 B20 B17 58.8(6) . . ? C2 C1 B2 110.4(5) . . ? C2 C1 B3 110.6(5) . . ? B2 C1 B3 63.7(5) . . ? C2 C1 B1 61.7(4) . . ? B2 C1 B1 61.4(5) . . ? B3 C1 B1 114.3(5) . . ? C2 C1 B4 60.9(4) . . ? B2 C1 B4 113.7(6) . . ? B3 C1 B4 61.7(5) . . ? B1 C1 B4 113.6(5) . . ? C2 C1 S1 117.0(4) . . ? B2 C1 S1 121.8(5) . . ? B3 C1 S1 122.2(5) . . ? B1 C1 S1 115.9(5) . . ? B4 C1 S1 117.8(4) . . ? C1 C2 B6 110.4(6) . . ? C1 C2 B5 111.6(5) . . ? B6 C2 B5 62.7(5) . . ? C1 C2 B4 62.3(4) . . ? B6 C2 B4 113.6(6) . . ? B5 C2 B4 62.0(5) . . ? C1 C2 B1 61.2(4) . . ? B6 C2 B1 61.7(5) . . ? B5 C2 B1 113.9(6) . . ? B4 C2 B1 114.4(6) . . ? C1 C2 S2 115.7(4) . . ? B6 C2 S2 124.3(5) . . ? B5 C2 S2 121.6(5) . . ? B4 C2 S2 114.6(5) . . ? B1 C2 S2 117.9(5) . . ? C4 C3 B11 61.4(5) . . ? C4 C3 B13 111.4(6) . . ? B11 C3 B13 113.3(6) . . ? C4 C3 B12 112.3(6) . . ? B11 C3 B12 62.1(5) . . ? B13 C3 B12 63.3(5) . . ? C4 C3 B14 61.6(5) . . ? B11 C3 B14 112.8(6) . . ? B13 C3 B14 61.4(5) . . ? B12 C3 B14 114.0(6) . . ? C4 C3 S3 116.5(5) . . ? B11 C3 S3 119.0(5) . . ? B13 C3 S3 120.9(5) . . ? B12 C3 S3 121.6(6) . . ? B14 C3 S3 116.2(5) . . ? C3 C4 B16 109.3(6) . . ? C3 C4 B11 60.3(5) . . ? B16 C4 B11 61.0(5) . . ? C3 C4 B15 110.3(6) . . ? B16 C4 B15 62.4(5) . . ? B11 C4 B15 112.0(6) . . ? C3 C4 B14 61.4(5) . . ? B16 C4 B14 112.0(6) . . ? B11 C4 B14 111.8(6) . . ? B15 C4 B14 61.3(5) . . ? C3 C4 S4 116.2(4) . . ? B16 C4 S4 125.4(6) . . ? B11 C4 S4 120.0(5) . . ? B15 C4 S4 122.1(6) . . ? B14 C4 S4 115.3(5) . . ? C6 C5 C9 109.4(9) . . ? C6 C5 Co1 68.2(5) . . ? C9 C5 Co1 73.8(4) . . ? C5 C6 C7 110.0(9) . . ? C5 C6 Co1 74.0(5) . . ? C7 C6 Co1 69.7(5) . . ? C6 C7 C8 104.7(9) . . ? C6 C7 Co1 70.4(5) . . ? C8 C7 Co1 72.3(4) . . ? C9 C8 C7 108.9(8) . . ? C9 C8 Co1 74.6(4) . . ? C7 C8 Co1 66.7(4) . . ? C8 C9 C5 106.9(7) . . ? C8 C9 C10 128.9(7) . . ? C5 C9 C10 124.1(8) . . ? C8 C9 Co1 68.4(4) . . ? C5 C9 Co1 68.3(4) . . ? C10 C9 Co1 130.6(5) . . ? C9 C10 C11 111.9(7) . . ? O1 C11 C10 107.2(7) . . ? O1 C12 C13 108.3(7) . . ? C12 C13 C14 110.5(7) . . ? C15 C14 C18 106.7(7) . . ? C15 C14 C13 129.1(8) . . ? C18 C14 C13 123.7(8) . . ? C15 C14 Co2 68.7(4) . . ? C18 C14 Co2 70.0(4) . . ? C13 C14 Co2 132.1(5) . . ? C14 C15 C16 110.2(7) . . ? C14 C15 Co2 73.0(4) . . ? C16 C15 Co2 69.9(4) . . ? C17 C16 C15 104.7(7) . . ? C17 C16 Co2 70.2(4) . . ? C15 C16 Co2 70.5(4) . . ? C18 C17 C16 110.2(7) . . ? C18 C17 Co2 72.7(5) . . ? C16 C17 Co2 70.3(4) . . ? C17 C18 C14 108.2(7) . . ? C17 C18 Co2 69.2(4) . . ? C14 C18 Co2 71.6(4) . . ? C24 C19 C20 117.4(7) . . ? C24 C19 P1 120.0(6) . . ? C20 C19 P1 122.5(6) . . ? C21 C20 C19 119.4(9) . . ? C22 C21 C20 122.5(9) . . ? C21 C22 C23 118.9(9) . . ? C24 C23 C22 119.8(9) . . ? C23 C24 C19 122.0(9) . . ? C26 C25 C30 117.6(8) . . ? C26 C25 P1 123.6(7) . . ? C30 C25 P1 118.8(6) . . ? C25 C26 C27 120.5(9) . . ? C28 C27 C26 120.4(10) . . ? C29 C28 C27 120.0(10) . . ? C28 C29 C30 120.4(10) . . ? C25 C30 C29 121.0(9) . . ? C32 C31 C36 119.3(8) . . ? C32 C31 P1 121.3(6) . . ? C36 C31 P1 119.2(7) . . ? C31 C32 C33 120.0(8) . . ? C34 C33 C32 118.7(9) . . ? C35 C34 C33 121.1(10) . . ? C34 C35 C36 120.9(10) . . ? C35 C36 C31 119.7(9) . . ? C42 C37 C38 118.4(7) . . ? C42 C37 P2 118.8(6) . . ? C38 C37 P2 122.5(6) . . ? C39 C38 C37 120.8(9) . . ? C40 C39 C38 119.5(9) . . ? C39 C40 C41 121.9(9) . . ? C42 C41 C40 118.2(9) . . ? C41 C42 C37 121.3(8) . . ? C44 C43 C48 117.0(7) . . ? C44 C43 P2 124.5(6) . . ? C48 C43 P2 118.6(6) . . ? C43 C44 C45 121.4(8) . . ? C46 C45 C44 120.6(9) . . ? C45 C46 C47 119.8(8) . . ? C46 C47 C48 120.9(8) . . ? C47 C48 C43 120.3(8) . . ? C50 C49 C54 118.9(7) . . ? C50 C49 P2 120.0(6) . . ? C54 C49 P2 121.0(6) . . ? C49 C50 C51 120.0(8) . . ? C52 C51 C50 118.7(9) . . ? C53 C52 C51 121.1(9) . . ? C52 C53 C54 120.8(9) . . ? C53 C54 C49 120.4(9) . . ? Cl2 C55 Cl1 109.3(7) . . ? Cl3 C56 Cl4 111.3(11) . . ? Cl5 C57 Cl6 106.4(10) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.810 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.099 # Attachment 'complex 6a.cif' data_f60406f _database_code_depnum_ccdc_archive 'CCDC 616735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 B10 Co2 O S2' _chemical_formula_weight 524.45 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' B B 0.0013 0.0007 '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' Co Co 0.3494 0.9721 '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 12.239(4) _cell_length_b 12.155(4) _cell_length_c 18.230(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.793(5) _cell_angle_gamma 90.00 _cell_volume 2708.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 688 _cell_measurement_theta_min 2.363 _cell_measurement_theta_max 21.088 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8191 _exptl_absorpt_correction_T_max 0.8972 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% 6.61 _diffrn_reflns_number 11212 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4775 _reflns_number_gt 2740 _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^)+(0.0863P)^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 4775 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.58460(7) 0.71313(7) 0.14147(4) 0.0427(3) Uani 1 1 d . . . Co2 Co 0.67210(7) 0.77063(7) 0.25627(4) 0.0429(3) Uani 1 1 d . . . S1 S 0.76471(11) 0.74571(10) 0.15393(7) 0.0222(3) Uani 1 1 d . . . S2 S 0.56171(11) 0.88031(11) 0.18713(7) 0.0232(3) Uani 1 1 d . . . O1 O 0.7621(4) 0.5129(4) 0.2073(3) 0.0690(14) Uani 1 1 d . . . C1 C 0.5428(6) 0.6321(6) 0.0443(4) 0.0558(19) Uani 1 1 d . . . H1 H 0.5772 0.6441 -0.0025 0.067 Uiso 1 1 calc R . . C2 C 0.4554(7) 0.6881(6) 0.0673(4) 0.065(2) Uani 1 1 d . . . H2 H 0.4149 0.7455 0.0397 0.078 Uiso 1 1 calc R . . C3 C 0.4307(6) 0.6473(7) 0.1377(5) 0.073(2) Uani 1 1 d . . . H3 H 0.3699 0.6706 0.1671 0.087 Uiso 1 1 calc R . . C4 C 0.5078(7) 0.5624(6) 0.1562(4) 0.065(2) Uani 1 1 d . . . H4 H 0.5108 0.5186 0.2013 0.077 Uiso 1 1 calc R . . C5 C 0.5797(6) 0.5548(6) 0.0996(4) 0.0553(19) Uani 1 1 d . . . C6 C 0.6731(7) 0.4760(6) 0.0918(4) 0.082(3) Uani 1 1 d . . . H6A H 0.7316 0.5141 0.0683 0.099 Uiso 1 1 calc R . . H6B H 0.6485 0.4166 0.0595 0.099 Uiso 1 1 calc R . . C7 C 0.7188(8) 0.4268(6) 0.1630(5) 0.091(3) Uani 1 1 d . . . H7A H 0.6614 0.3891 0.1880 0.109 Uiso 1 1 calc R . . H7B H 0.7757 0.3740 0.1533 0.109 Uiso 1 1 calc R . . C8 C 0.8006(7) 0.4795(6) 0.2785(4) 0.073(2) Uani 1 1 d . . . H8A H 0.8608 0.4281 0.2751 0.087 Uiso 1 1 calc R . . H8B H 0.7425 0.4436 0.3038 0.087 Uiso 1 1 calc R . . C9 C 0.8378(6) 0.5794(6) 0.3191(4) 0.061(2) Uani 1 1 d . . . H9A H 0.8965 0.6122 0.2928 0.073 Uiso 1 1 calc R . . H9B H 0.8686 0.5564 0.3667 0.073 Uiso 1 1 calc R . . C10 C 0.7536(6) 0.6682(6) 0.3317(3) 0.0486(17) Uani 1 1 d . . . C11 C 0.7785(6) 0.7792(6) 0.3481(3) 0.0569(19) Uani 1 1 d . . . H11 H 0.8518 0.8117 0.3495 0.068 Uiso 1 1 calc R . . C12 C 0.6813(7) 0.8359(6) 0.3616(3) 0.059(2) Uani 1 1 d . . . H12 H 0.6746 0.9136 0.3749 0.071 Uiso 1 1 calc R . . C13 C 0.5936(6) 0.7577(6) 0.3520(3) 0.058(2) Uani 1 1 d . . . H13 H 0.5159 0.7724 0.3583 0.070 Uiso 1 1 calc R . . C14 C 0.6399(6) 0.6543(6) 0.3365(3) 0.0537(18) Uani 1 1 d . . . H14 H 0.5995 0.5854 0.3284 0.064 Uiso 1 1 calc R . . C15 C 0.7699(5) 0.8893(5) 0.1195(3) 0.0424(15) Uani 1 1 d . . . C16 C 0.6626(5) 0.9625(5) 0.1370(3) 0.0401(15) Uani 1 1 d . . . B3 B 0.6773(6) 0.9216(6) 0.0470(4) 0.0448(18) Uani 1 1 d . . . H3A H 0.6247 0.8621 0.0165 0.054 Uiso 1 1 calc R . . B4 B 0.8193(7) 0.9251(7) 0.0363(4) 0.053(2) Uani 1 1 d . . . H4A H 0.8588 0.8677 -0.0008 0.063 Uiso 1 1 calc R . . B5 B 0.8855(6) 0.9681(6) 0.1217(4) 0.052(2) Uani 1 1 d . . . H5 H 0.9676 0.9381 0.1388 0.062 Uiso 1 1 calc R . . B6 B 0.7851(6) 0.9917(6) 0.1852(4) 0.049(2) Uani 1 1 d . . . H6 H 0.8023 0.9774 0.2442 0.058 Uiso 1 1 calc R . . B7 B 0.6313(7) 1.0544(6) 0.0689(4) 0.0457(19) Uani 1 1 d . . . H7 H 0.5477 1.0812 0.0529 0.055 Uiso 1 1 calc R . . B8 B 0.7329(7) 1.0367(6) 0.0049(5) 0.057(2) Uani 1 1 d . . . H8 H 0.7170 1.0534 -0.0539 0.068 Uiso 1 1 calc R . . B9 B 0.8608(7) 1.0660(7) 0.0489(5) 0.057(2) Uani 1 1 d . . . H9 H 0.9284 1.1010 0.0188 0.069 Uiso 1 1 calc R . . B10 B 0.8376(7) 1.1048(7) 0.1414(4) 0.057(2) Uani 1 1 d . . . H10 H 0.8892 1.1656 0.1713 0.068 Uiso 1 1 calc R . . B11 B 0.6959(7) 1.0962(6) 0.1530(4) 0.050(2) Uani 1 1 d . . . H11A H 0.6538 1.1497 0.1913 0.061 Uiso 1 1 calc R . . B12 B 0.7444(7) 1.1442(7) 0.0687(4) 0.054(2) Uani 1 1 d . . . H12A H 0.7358 1.2306 0.0514 0.065 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 Co1 0.0461(6) 0.0445(6) 0.0372(5) 0.0016(4) 0.0003(4) -0.0053(4) Co2 0.0484(6) 0.0456(6) 0.0346(5) 0.0008(4) 0.0012(4) 0.0011(4) S1 0.0261(7) 0.0179(7) 0.0226(6) 0.0014(5) 0.0018(5) 0.0008(5) S2 0.0247(7) 0.0244(7) 0.0210(6) 0.0003(6) 0.0058(5) 0.0038(6) O1 0.093(4) 0.050(3) 0.062(3) 0.000(3) -0.016(3) 0.004(3) C1 0.071(5) 0.057(5) 0.038(4) -0.005(4) -0.007(4) -0.009(4) C2 0.075(6) 0.060(5) 0.056(5) 0.001(4) -0.027(4) -0.007(4) C3 0.053(5) 0.081(6) 0.083(6) 0.006(5) -0.008(4) -0.024(5) C4 0.085(6) 0.049(5) 0.059(5) 0.008(4) -0.001(4) -0.028(4) C5 0.069(5) 0.048(5) 0.048(4) -0.006(4) -0.007(4) -0.012(4) C6 0.121(8) 0.051(5) 0.073(5) -0.024(4) -0.019(5) 0.014(5) C7 0.124(8) 0.037(5) 0.104(7) -0.013(5) -0.060(6) 0.008(5) C8 0.097(7) 0.052(5) 0.066(5) 0.007(4) -0.022(5) 0.008(4) C9 0.065(5) 0.065(5) 0.052(4) -0.003(4) -0.011(4) 0.011(4) C10 0.054(5) 0.055(5) 0.037(4) 0.009(3) -0.001(3) 0.006(4) C11 0.065(5) 0.060(5) 0.045(4) -0.001(4) -0.012(4) -0.007(4) C12 0.088(6) 0.055(5) 0.034(4) -0.008(3) -0.004(4) 0.003(4) C13 0.061(5) 0.077(6) 0.038(4) 0.004(4) 0.011(4) 0.015(4) C14 0.063(5) 0.056(5) 0.042(4) 0.013(3) 0.001(4) -0.003(4) C15 0.044(4) 0.040(4) 0.043(4) -0.006(3) 0.002(3) 0.002(3) C16 0.042(4) 0.035(4) 0.043(4) -0.008(3) 0.000(3) 0.005(3) B3 0.049(5) 0.046(5) 0.039(4) 0.003(4) 0.000(4) 0.001(4) B4 0.061(5) 0.047(5) 0.052(5) 0.008(4) 0.018(4) -0.001(4) B5 0.040(5) 0.045(5) 0.070(5) 0.003(4) 0.002(4) -0.012(4) B6 0.051(5) 0.048(5) 0.046(4) -0.004(4) -0.009(4) -0.004(4) B7 0.049(5) 0.044(5) 0.044(4) -0.003(4) 0.002(4) 0.005(4) B8 0.077(6) 0.043(5) 0.053(5) 0.005(4) 0.014(5) 0.002(4) B9 0.059(6) 0.043(5) 0.071(6) 0.004(4) 0.014(5) -0.006(4) B10 0.059(6) 0.051(5) 0.059(5) -0.001(4) -0.007(4) -0.004(4) B11 0.061(5) 0.037(5) 0.053(5) -0.008(4) -0.004(4) 0.002(4) B12 0.062(5) 0.040(5) 0.060(5) 0.007(4) 0.004(4) 0.005(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 Co1 C3 2.044(7) . ? Co1 C2 2.052(7) . ? Co1 C1 2.069(6) . ? Co1 C5 2.069(7) . ? Co1 C4 2.082(7) . ? Co1 S2 2.2188(16) . ? Co1 S1 2.2402(17) . ? Co1 Co2 2.4076(13) . ? Co2 C13 2.038(6) . ? Co2 C11 2.073(7) . ? Co2 C10 2.073(6) . ? Co2 C12 2.075(6) . ? Co2 C14 2.085(6) . ? Co2 S2 2.2418(16) . ? Co2 S1 2.2500(16) . ? S1 C15 1.857(6) . ? S2 C16 1.862(6) . ? O1 C7 1.409(8) . ? O1 C8 1.419(7) . ? C1 C2 1.351(10) . ? C1 C5 1.435(9) . ? C1 H1 0.9800 . ? C2 C3 1.423(10) . ? C2 H2 0.9800 . ? C3 C4 1.427(10) . ? C3 H3 0.9800 . ? C4 C5 1.390(9) . ? C4 H4 0.9800 . ? C5 C6 1.504(10) . ? C6 C7 1.512(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.481(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.518(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C14 1.408(9) . ? C10 C11 1.412(9) . ? C11 C12 1.407(10) . ? C11 H11 0.9800 . ? C12 C13 1.438(10) . ? C12 H12 0.9800 . ? C13 C14 1.412(9) . ? C13 H13 0.9800 . ? C14 H14 0.9800 . ? C15 C16 1.632(8) . ? C15 B5 1.707(9) . ? C15 B4 1.715(9) . ? C15 B6 1.732(9) . ? C15 B3 1.744(9) . ? C16 B11 1.698(9) . ? C16 B7 1.701(9) . ? C16 B3 1.734(9) . ? C16 B6 1.737(9) . ? B3 B8 1.749(11) . ? B3 B4 1.759(11) . ? B3 B7 1.763(10) . ? B3 H3A 1.1000 . ? B4 B8 1.796(11) . ? B4 B5 1.797(11) . ? B4 B9 1.798(11) . ? B4 H4A 1.1000 . ? B5 B6 1.753(11) . ? B5 B9 1.797(11) . ? B5 B10 1.805(11) . ? B5 H5 1.1000 . ? B6 B10 1.729(11) . ? B6 B11 1.757(11) . ? B6 H6 1.1000 . ? B7 B8 1.759(11) . ? B7 B12 1.762(11) . ? B7 B11 1.766(10) . ? B7 H7 1.1000 . ? B8 B12 1.750(11) . ? B8 B9 1.760(12) . ? B8 H8 1.1000 . ? B9 B12 1.765(11) . ? B9 B10 1.788(11) . ? B9 H9 1.1000 . ? B10 B11 1.760(11) . ? B10 B12 1.772(11) . ? B10 H10 1.1000 . ? B11 B12 1.774(11) . ? B11 H11A 1.1000 . ? B12 H12A 1.1000 . ? 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 C3 Co1 C2 40.7(3) . . ? C3 Co1 C1 66.2(3) . . ? C2 Co1 C1 38.3(3) . . ? C3 Co1 C5 67.3(3) . . ? C2 Co1 C5 67.2(3) . . ? C1 Co1 C5 40.6(3) . . ? C3 Co1 C4 40.5(3) . . ? C2 Co1 C4 67.5(3) . . ? C1 Co1 C4 66.2(3) . . ? C5 Co1 C4 39.1(3) . . ? C3 Co1 S2 103.8(3) . . ? C2 Co1 S2 106.0(2) . . ? C1 Co1 S2 136.6(2) . . ? C5 Co1 S2 171.0(2) . . ? C4 Co1 S2 133.8(2) . . ? C3 Co1 S1 166.6(3) . . ? C2 Co1 S1 144.6(2) . . ? C1 Co1 S1 111.8(2) . . ? C5 Co1 S1 102.3(2) . . ? C4 Co1 S1 126.2(2) . . ? S2 Co1 S1 86.66(5) . . ? C3 Co1 Co2 120.8(2) . . ? C2 Co1 Co2 155.7(2) . . ? C1 Co1 Co2 164.4(2) . . ? C5 Co1 Co2 126.4(2) . . ? C4 Co1 Co2 109.1(2) . . ? S2 Co1 Co2 57.79(4) . . ? S1 Co1 Co2 57.77(4) . . ? C13 Co2 C11 67.5(3) . . ? C13 Co2 C10 67.5(3) . . ? C11 Co2 C10 39.8(3) . . ? C13 Co2 C12 40.9(3) . . ? C11 Co2 C12 39.7(3) . . ? C10 Co2 C12 67.3(3) . . ? C13 Co2 C14 40.0(3) . . ? C11 Co2 C14 66.5(3) . . ? C10 Co2 C14 39.6(2) . . ? C12 Co2 C14 67.3(3) . . ? C13 Co2 S2 103.3(2) . . ? C11 Co2 S2 139.6(2) . . ? C10 Co2 S2 170.72(19) . . ? C12 Co2 S2 107.3(2) . . ? C14 Co2 S2 131.9(2) . . ? C13 Co2 S1 167.6(2) . . ? C11 Co2 S1 110.8(2) . . ? C10 Co2 S1 102.91(19) . . ? C12 Co2 S1 144.3(2) . . ? C14 Co2 S1 127.6(2) . . ? S2 Co2 S1 85.87(6) . . ? C13 Co2 Co1 120.9(2) . . ? C11 Co2 Co1 162.2(2) . . ? C10 Co2 Co1 125.5(2) . . ? C12 Co2 Co1 156.5(2) . . ? C14 Co2 Co1 108.7(2) . . ? S2 Co2 Co1 56.87(5) . . ? S1 Co2 Co1 57.38(5) . . ? C15 S1 Co1 100.5(2) . . ? C15 S1 Co2 100.44(19) . . ? Co1 S1 Co2 64.85(5) . . ? C16 S2 Co1 102.04(19) . . ? C16 S2 Co2 101.48(19) . . ? Co1 S2 Co2 65.33(5) . . ? C7 O1 C8 114.3(6) . . ? C2 C1 C5 109.8(7) . . ? C2 C1 Co1 70.2(4) . . ? C5 C1 Co1 69.7(4) . . ? C2 C1 H1 125.1 . . ? C5 C1 H1 125.1 . . ? Co1 C1 H1 125.1 . . ? C1 C2 C3 108.1(7) . . ? C1 C2 Co1 71.5(4) . . ? C3 C2 Co1 69.4(4) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Co1 C2 H2 126.0 . . ? C2 C3 C4 107.3(8) . . ? C2 C3 Co1 70.0(4) . . ? C4 C3 Co1 71.2(4) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? Co1 C3 H3 126.3 . . ? C5 C4 C3 107.9(7) . . ? C5 C4 Co1 69.9(4) . . ? C3 C4 Co1 68.3(4) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Co1 C4 H4 126.0 . . ? C4 C5 C1 106.8(7) . . ? C4 C5 C6 128.6(7) . . ? C1 C5 C6 124.4(7) . . ? C4 C5 Co1 70.9(4) . . ? C1 C5 Co1 69.7(4) . . ? C6 C5 Co1 128.3(5) . . ? C5 C6 C7 114.9(7) . . ? C5 C6 H6A 108.5 . . ? C7 C6 H6A 108.5 . . ? C5 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O1 C7 C6 108.2(6) . . ? O1 C7 H7A 110.1 . . ? C6 C7 H7A 110.1 . . ? O1 C7 H7B 110.1 . . ? C6 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O1 C8 C9 107.6(6) . . ? O1 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? O1 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C8 C9 C10 117.7(6) . . ? C8 C9 H9A 107.9 . . ? C10 C9 H9A 107.9 . . ? C8 C9 H9B 107.9 . . ? C10 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? C14 C10 C11 107.8(6) . . ? C14 C10 C9 127.1(7) . . ? C11 C10 C9 124.8(7) . . ? C14 C10 Co2 70.7(4) . . ? C11 C10 Co2 70.1(4) . . ? C9 C10 Co2 129.4(5) . . ? C12 C11 C10 109.2(7) . . ? C12 C11 Co2 70.3(4) . . ? C10 C11 Co2 70.1(4) . . ? C12 C11 H11 125.4 . . ? C10 C11 H11 125.4 . . ? Co2 C11 H11 125.4 . . ? C11 C12 C13 106.7(6) . . ? C11 C12 Co2 70.1(4) . . ? C13 C12 Co2 68.2(4) . . ? C11 C12 H12 126.6 . . ? C13 C12 H12 126.6 . . ? Co2 C12 H12 126.6 . . ? C14 C13 C12 107.9(7) . . ? C14 C13 Co2 71.8(4) . . ? C12 C13 Co2 70.9(4) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? Co2 C13 H13 126.0 . . ? C10 C14 C13 108.2(7) . . ? C10 C14 Co2 69.7(4) . . ? C13 C14 Co2 68.2(4) . . ? C10 C14 H14 125.9 . . ? C13 C14 H14 125.9 . . ? Co2 C14 H14 125.9 . . ? C16 C15 B5 111.3(5) . . ? C16 C15 B4 110.9(5) . . ? B5 C15 B4 63.3(4) . . ? C16 C15 B6 62.1(4) . . ? B5 C15 B6 61.3(4) . . ? B4 C15 B6 113.5(5) . . ? C16 C15 B3 61.7(4) . . ? B5 C15 B3 113.5(5) . . ? B4 C15 B3 61.1(4) . . ? B6 C15 B3 114.0(5) . . ? C16 C15 S1 113.9(4) . . ? B5 C15 S1 124.2(4) . . ? B4 C15 S1 123.8(4) . . ? B6 C15 S1 116.5(4) . . ? B3 C15 S1 115.9(4) . . ? C15 C16 B11 111.5(5) . . ? C15 C16 B7 111.7(5) . . ? B11 C16 B7 62.6(4) . . ? C15 C16 B3 62.3(4) . . ? B11 C16 B3 113.7(5) . . ? B7 C16 B3 61.7(4) . . ? C15 C16 B6 61.8(4) . . ? B11 C16 B6 61.5(4) . . ? B7 C16 B6 113.1(5) . . ? B3 C16 B6 114.2(5) . . ? C15 C16 S2 111.3(4) . . ? B11 C16 S2 126.1(4) . . ? B7 C16 S2 125.5(4) . . ? B3 C16 S2 114.4(4) . . ? B6 C16 S2 116.0(4) . . ? C16 B3 C15 56.0(4) . . ? C16 B3 B8 104.2(5) . . ? C15 B3 B8 105.0(6) . . ? C16 B3 B4 104.3(5) . . ? C15 B3 B4 58.6(4) . . ? B8 B3 B4 61.6(5) . . ? C16 B3 B7 58.2(4) . . ? C15 B3 B7 103.7(5) . . ? B8 B3 B7 60.1(4) . . ? B4 B3 B7 109.3(6) . . ? C16 B3 H3A 125.5 . . ? C15 B3 H3A 125.3 . . ? B8 B3 H3A 122.4 . . ? B4 B3 H3A 121.2 . . ? B7 B3 H3A 122.1 . . ? C15 B4 B3 60.3(4) . . ? C15 B4 B8 104.3(5) . . ? B3 B4 B8 58.9(4) . . ? C15 B4 B5 58.1(4) . . ? B3 B4 B5 108.5(5) . . ? B8 B4 B5 106.8(6) . . ? C15 B4 B9 103.8(5) . . ? B3 B4 B9 106.5(6) . . ? B8 B4 B9 58.6(5) . . ? B5 B4 B9 60.0(4) . . ? C15 B4 H4A 124.6 . . ? B3 B4 H4A 121.3 . . ? B8 B4 H4A 123.5 . . ? B5 B4 H4A 121.6 . . ? B9 B4 H4A 123.5 . . ? C15 B5 B6 60.1(4) . . ? C15 B5 B4 58.5(4) . . ? B6 B5 B4 108.6(5) . . ? C15 B5 B9 104.2(5) . . ? B6 B5 B9 106.4(6) . . ? B4 B5 B9 60.0(4) . . ? C15 B5 B10 104.2(5) . . ? B6 B5 B10 58.1(4) . . ? B4 B5 B10 107.7(6) . . ? B9 B5 B10 59.5(4) . . ? C15 B5 H5 124.5 . . ? B6 B5 H5 121.8 . . ? B4 B5 H5 121.1 . . ? B9 B5 H5 123.1 . . ? B10 B5 H5 123.3 . . ? B10 B6 C15 106.4(5) . . ? B10 B6 C16 105.1(5) . . ? C15 B6 C16 56.1(4) . . ? B10 B6 B5 62.4(5) . . ? C15 B6 B5 58.7(4) . . ? C16 B6 B5 104.4(5) . . ? B10 B6 B11 60.6(5) . . ? C15 B6 B11 104.2(5) . . ? C16 B6 B11 58.1(4) . . ? B5 B6 B11 110.0(6) . . ? B10 B6 H6 121.3 . . ? C15 B6 H6 124.9 . . ? C16 B6 H6 125.6 . . ? B5 B6 H6 120.9 . . ? B11 B6 H6 121.8 . . ? C16 B7 B8 105.2(5) . . ? C16 B7 B12 105.1(5) . . ? B8 B7 B12 59.6(4) . . ? C16 B7 B3 60.0(4) . . ? B8 B7 B3 59.6(4) . . ? B12 B7 B3 107.9(6) . . ? C16 B7 B11 58.6(4) . . ? B8 B7 B11 108.1(6) . . ? B12 B7 B11 60.4(4) . . ? B3 B7 B11 109.0(5) . . ? C16 B7 H7 124.1 . . ? B8 B7 H7 122.6 . . ? B12 B7 H7 122.5 . . ? B3 B7 H7 120.9 . . ? B11 B7 H7 121.1 . . ? B3 B8 B12 109.1(6) . . ? B3 B8 B7 60.3(4) . . ? B12 B8 B7 60.3(4) . . ? B3 B8 B9 108.6(6) . . ? B12 B8 B9 60.4(5) . . ? B7 B8 B9 108.4(6) . . ? B3 B8 B4 59.5(4) . . ? B12 B8 B4 109.0(6) . . ? B7 B8 B4 107.8(5) . . ? B9 B8 B4 60.7(5) . . ? B3 B8 H8 121.4 . . ? B12 B8 H8 120.9 . . ? B7 B8 H8 121.8 . . ? B9 B8 H8 121.2 . . ? B4 B8 H8 121.6 . . ? B8 B9 B12 59.5(5) . . ? B8 B9 B10 107.7(6) . . ? B12 B9 B10 59.8(4) . . ? B8 B9 B5 108.4(6) . . ? B12 B9 B5 108.3(6) . . ? B10 B9 B5 60.5(4) . . ? B8 B9 B4 60.6(5) . . ? B12 B9 B4 108.2(6) . . ? B10 B9 B4 108.3(6) . . ? B5 B9 B4 60.0(4) . . ? B8 B9 H9 121.7 . . ? B12 B9 H9 121.9 . . ? B10 B9 H9 121.7 . . ? B5 B9 H9 121.4 . . ? B4 B9 H9 121.4 . . ? B6 B10 B11 60.5(5) . . ? B6 B10 B12 108.7(6) . . ? B11 B10 B12 60.3(4) . . ? B6 B10 B9 107.8(6) . . ? B11 B10 B9 107.5(6) . . ? B12 B10 B9 59.4(5) . . ? B6 B10 B5 59.4(4) . . ? B11 B10 B5 107.5(6) . . ? B12 B10 B5 107.6(6) . . ? B9 B10 B5 60.0(4) . . ? B6 B10 H10 121.5 . . ? B11 B10 H10 121.7 . . ? B12 B10 H10 121.6 . . ? B9 B10 H10 122.1 . . ? B5 B10 H10 122.2 . . ? C16 B11 B6 60.4(4) . . ? C16 B11 B10 105.4(5) . . ? B6 B11 B10 58.9(4) . . ? C16 B11 B7 58.8(4) . . ? B6 B11 B7 109.1(5) . . ? B10 B11 B7 108.3(6) . . ? C16 B11 B12 104.7(5) . . ? B6 B11 B12 107.4(6) . . ? B10 B11 B12 60.2(4) . . ? B7 B11 B12 59.7(4) . . ? C16 B11 H11A 124.0 . . ? B6 B11 H11A 121.2 . . ? B10 B11 H11A 122.4 . . ? B7 B11 H11A 121.1 . . ? B12 B11 H11A 122.8 . . ? B8 B12 B7 60.1(5) . . ? B8 B12 B9 60.1(5) . . ? B7 B12 B9 108.0(6) . . ? B8 B12 B10 108.8(6) . . ? B7 B12 B10 107.9(6) . . ? B9 B12 B10 60.7(5) . . ? B8 B12 B11 108.1(6) . . ? B7 B12 B11 59.9(4) . . ? B9 B12 B11 107.9(6) . . ? B10 B12 B11 59.5(4) . . ? B8 B12 H12A 121.3 . . ? B7 B12 H12A 121.8 . . ? B9 B12 H12A 121.5 . . ? B10 B12 H12A 121.4 . . ? B11 B12 H12A 122.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.956 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.101 # Attachment 'complex 6b.cif' data_f60614c _database_code_depnum_ccdc_archive 'CCDC 616736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 B10 Co2 O Se2' _chemical_formula_weight 618.25 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' B B 0.0013 0.0007 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 13.145(4) _cell_length_b 15.462(5) _cell_length_c 23.036(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4682(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1009 _cell_measurement_theta_min 2.693 _cell_measurement_theta_max 25.913 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 4.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4641 _exptl_absorpt_correction_T_max 0.9148 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 6.19 _diffrn_reflns_number 18710 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4130 _reflns_number_gt 2686 _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^)+(0.0505P)^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 4130 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _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 Se1 Se 0.23067(3) 0.88926(3) 0.669727(18) 0.03308(13) Uani 1 1 d . . . Se2 Se 0.04414(3) 0.88689(3) 0.58108(2) 0.03903(15) Uani 1 1 d . . . Co1 Co 0.07712(4) 0.81627(4) 0.66737(3) 0.03646(17) Uani 1 1 d . . . Co2 Co 0.08490(5) 0.97215(4) 0.65942(2) 0.03601(17) Uani 1 1 d . . . O1 O 0.1689(3) 0.9053(2) 0.79526(14) 0.0522(9) Uani 1 1 d . . . C1 C -0.0183(4) 0.7857(4) 0.7359(2) 0.0573(15) Uani 1 1 d . . . H1 H -0.0504 0.8275 0.7621 0.069 Uiso 1 1 calc R . . C2 C -0.0584(4) 0.7578(4) 0.6824(3) 0.0588(16) Uani 1 1 d . . . H2 H -0.1241 0.7746 0.6658 0.071 Uiso 1 1 calc R . . C3 C 0.0112(4) 0.6975(3) 0.6583(2) 0.0601(16) Uani 1 1 d . . . H3 H 0.0024 0.6657 0.6219 0.072 Uiso 1 1 calc R . . C4 C 0.0927(4) 0.6905(3) 0.6960(2) 0.0513(14) Uani 1 1 d . . . H4 H 0.1526 0.6538 0.6901 0.062 Uiso 1 1 calc R . . C5 C 0.0765(4) 0.7469(3) 0.7446(2) 0.0482(13) Uani 1 1 d . . . C6 C 0.1475(4) 0.7537(3) 0.7958(2) 0.0638(16) Uani 1 1 d . . . H6A H 0.1349 0.7052 0.8216 0.077 Uiso 1 1 calc R . . H6B H 0.2169 0.7487 0.7819 0.077 Uiso 1 1 calc R . . C7 C 0.1382(5) 0.8362(4) 0.8302(2) 0.0673(17) Uani 1 1 d . . . H7A H 0.0683 0.8444 0.8425 0.081 Uiso 1 1 calc R . . H7B H 0.1807 0.8331 0.8646 0.081 Uiso 1 1 calc R . . C8 C 0.1546(4) 0.9871(3) 0.8213(2) 0.0559(14) Uani 1 1 d . . . H8A H 0.2017 0.9943 0.8534 0.067 Uiso 1 1 calc R . . H8B H 0.0859 0.9916 0.8364 0.067 Uiso 1 1 calc R . . C9 C 0.1725(4) 1.0563(3) 0.7766(2) 0.0544(14) Uani 1 1 d . . . H9A H 0.1715 1.1121 0.7958 0.065 Uiso 1 1 calc R . . H9B H 0.2400 1.0483 0.7604 0.065 Uiso 1 1 calc R . . C10 C 0.0972(4) 1.0581(3) 0.7276(2) 0.0451(12) Uani 1 1 d . . . C11 C -0.0013(4) 1.0214(3) 0.7263(2) 0.0531(14) Uani 1 1 d . . . H11 H -0.0330 0.9878 0.7575 0.064 Uiso 1 1 calc R . . C12 C -0.0452(4) 1.0401(3) 0.6723(3) 0.0580(15) Uani 1 1 d . . . H12 H -0.1133 1.0226 0.6597 0.070 Uiso 1 1 calc R . . C13 C 0.0242(4) 1.0918(3) 0.6398(3) 0.0559(15) Uani 1 1 d . . . H13 H 0.0129 1.1155 0.6008 0.067 Uiso 1 1 calc R . . C14 C 0.1111(4) 1.1030(3) 0.6741(2) 0.0523(14) Uani 1 1 d . . . H14 H 0.1724 1.1349 0.6628 0.063 Uiso 1 1 calc R . . C15 C 0.2724(3) 0.8779(3) 0.58759(19) 0.0384(11) Uani 1 1 d . . . C16 C 0.1779(3) 0.8768(3) 0.54248(19) 0.0387(11) Uani 1 1 d . . . B3 B 0.2530(4) 0.9683(4) 0.5456(2) 0.0435(14) Uani 1 1 d . . . H3A H 0.2292 1.0319 0.5621 0.052 Uiso 1 1 calc R . . B4 B 0.3763(4) 0.9271(4) 0.5580(3) 0.0512(16) Uani 1 1 d . . . H4A H 0.4329 0.9645 0.5826 0.061 Uiso 1 1 calc R . . B5 B 0.3699(5) 0.8147(4) 0.5638(3) 0.0574(18) Uani 1 1 d . . . H5 H 0.4228 0.7798 0.5924 0.069 Uiso 1 1 calc R . . B6 B 0.2406(4) 0.7813(4) 0.5545(2) 0.0460(15) Uani 1 1 d . . . H6 H 0.2091 0.7244 0.5769 0.055 Uiso 1 1 calc R . . B7 B 0.2073(5) 0.9262(4) 0.4788(2) 0.0559(17) Uani 1 1 d . . . H7 H 0.1534 0.9628 0.4518 0.067 Uiso 1 1 calc R . . B8 B 0.3376(5) 0.9567(5) 0.4867(3) 0.0607(18) Uani 1 1 d . . . H8 H 0.3697 1.0131 0.4641 0.073 Uiso 1 1 calc R . . B9 B 0.4087(5) 0.8597(5) 0.4985(3) 0.067(2) Uani 1 1 d . . . H9 H 0.4878 0.8528 0.4836 0.080 Uiso 1 1 calc R . . B10 B 0.3243(5) 0.7719(5) 0.4958(3) 0.067(2) Uani 1 1 d . . . H10 H 0.3476 0.7082 0.4792 0.080 Uiso 1 1 calc R . . B11 B 0.1993(5) 0.8114(4) 0.4840(2) 0.0566(17) Uani 1 1 d . . . H11A H 0.1406 0.7748 0.4605 0.068 Uiso 1 1 calc R . . B12 B 0.3054(5) 0.8599(5) 0.4495(3) 0.067(2) Uani 1 1 d . . . H12A H 0.3170 0.8541 0.4024 0.080 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 Se1 0.0282(2) 0.0436(3) 0.0275(3) 0.0014(2) -0.00017(18) -0.0023(2) Se2 0.0283(3) 0.0524(3) 0.0365(3) -0.0040(2) -0.0042(2) -0.0001(2) Co1 0.0311(4) 0.0407(4) 0.0376(4) 0.0012(3) 0.0027(3) -0.0062(3) Co2 0.0313(4) 0.0397(4) 0.0370(4) -0.0049(3) 0.0003(3) 0.0029(3) O1 0.069(3) 0.052(2) 0.035(2) -0.0008(16) 0.0062(18) -0.0093(19) C1 0.053(4) 0.058(4) 0.062(4) 0.001(3) 0.024(3) -0.014(3) C2 0.040(3) 0.065(4) 0.072(4) 0.014(3) -0.003(3) -0.018(3) C3 0.068(4) 0.052(4) 0.061(4) -0.002(3) -0.001(3) -0.025(3) C4 0.050(3) 0.038(3) 0.066(4) 0.010(3) 0.005(3) -0.006(3) C5 0.049(3) 0.050(3) 0.046(3) 0.010(3) 0.004(3) -0.015(3) C6 0.077(4) 0.063(4) 0.051(4) 0.017(3) -0.010(3) -0.016(3) C7 0.082(4) 0.081(4) 0.039(3) 0.012(3) -0.004(3) -0.024(4) C8 0.063(4) 0.068(4) 0.036(3) -0.015(3) -0.001(3) -0.003(3) C9 0.065(4) 0.049(3) 0.049(3) -0.016(3) -0.002(3) -0.004(3) C10 0.043(3) 0.041(3) 0.051(3) -0.014(2) -0.002(3) 0.003(2) C11 0.049(3) 0.053(3) 0.057(4) -0.017(3) 0.015(3) 0.011(3) C12 0.037(3) 0.061(4) 0.076(4) -0.018(3) -0.008(3) 0.018(3) C13 0.055(4) 0.046(3) 0.067(4) -0.002(3) -0.012(3) 0.014(3) C14 0.053(3) 0.038(3) 0.066(4) 0.002(3) -0.006(3) 0.001(2) C15 0.029(3) 0.053(3) 0.032(3) 0.001(2) 0.002(2) 0.002(2) C16 0.034(3) 0.053(3) 0.029(3) 0.002(2) -0.002(2) -0.001(2) B3 0.040(3) 0.055(4) 0.036(3) 0.010(3) -0.001(3) -0.006(3) B4 0.030(3) 0.082(5) 0.041(4) 0.009(3) 0.002(3) -0.007(3) B5 0.052(4) 0.066(4) 0.054(4) 0.003(3) 0.010(3) 0.016(3) B6 0.045(4) 0.047(4) 0.046(4) -0.002(3) 0.002(3) 0.006(3) B7 0.056(4) 0.078(5) 0.034(4) 0.008(3) -0.001(3) 0.002(3) B8 0.055(4) 0.085(5) 0.042(4) 0.015(3) 0.011(3) -0.013(4) B9 0.048(4) 0.104(6) 0.048(4) 0.001(4) 0.017(3) 0.004(4) B10 0.067(5) 0.080(5) 0.053(4) -0.014(4) 0.016(4) 0.021(4) B11 0.061(4) 0.074(5) 0.035(3) -0.013(3) 0.004(3) -0.003(3) B12 0.069(5) 0.097(6) 0.034(4) 0.000(3) 0.018(3) 0.007(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 Se1 C15 1.978(5) . ? Se1 Co1 2.3132(9) . ? Se1 Co2 2.3175(9) . ? Se2 C16 1.976(5) . ? Se2 Co2 2.2982(9) . ? Se2 Co1 2.3090(9) . ? Co1 C2 2.027(5) . ? Co1 C3 2.042(5) . ? Co1 C4 2.064(5) . ? Co1 C1 2.071(5) . ? Co1 C5 2.078(5) . ? Co1 Co2 2.4193(11) . ? Co2 C12 2.029(5) . ? Co2 C11 2.059(5) . ? Co2 C10 2.063(5) . ? Co2 C13 2.065(5) . ? Co2 C14 2.080(5) . ? O1 C7 1.398(6) . ? O1 C8 1.412(5) . ? C1 C5 1.397(7) . ? C1 C2 1.409(7) . ? C1 H1 0.9800 . ? C2 C3 1.419(7) . ? C2 H2 0.9800 . ? C3 C4 1.384(7) . ? C3 H3 0.9800 . ? C4 C5 1.435(7) . ? C4 H4 0.9800 . ? C5 C6 1.508(7) . ? C6 C7 1.507(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.504(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.502(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.414(7) . ? C10 C14 1.425(7) . ? C11 C12 1.401(7) . ? C11 H11 0.9800 . ? C12 C13 1.426(7) . ? C12 H12 0.9800 . ? C13 C14 1.401(7) . ? C13 H13 0.9800 . ? C14 H14 0.9800 . ? C15 C16 1.620(6) . ? C15 B5 1.703(7) . ? C15 B4 1.705(7) . ? C15 B3 1.719(7) . ? C15 B6 1.728(7) . ? C16 B7 1.698(7) . ? C16 B11 1.707(7) . ? C16 B6 1.715(7) . ? C16 B3 1.726(7) . ? B3 B8 1.762(8) . ? B3 B4 1.764(8) . ? B3 B7 1.775(8) . ? B3 H3A 1.1000 . ? B4 B5 1.744(9) . ? B4 B9 1.773(9) . ? B4 B8 1.779(8) . ? B4 H4A 1.1000 . ? B5 B9 1.733(9) . ? B5 B6 1.790(9) . ? B5 B10 1.802(9) . ? B5 H5 1.1000 . ? B6 B10 1.748(8) . ? B6 B11 1.774(8) . ? B6 H6 1.1000 . ? B7 B12 1.779(9) . ? B7 B11 1.781(9) . ? B7 B8 1.786(9) . ? B7 H7 1.1000 . ? B8 B12 1.776(10) . ? B8 B9 1.789(10) . ? B8 H8 1.1000 . ? B9 B10 1.754(10) . ? B9 B12 1.767(10) . ? B9 H9 1.1000 . ? B10 B12 1.747(9) . ? B10 B11 1.773(9) . ? B10 H10 1.1000 . ? B11 B12 1.771(9) . ? B11 H11A 1.1000 . ? B12 H12A 1.1000 . ? 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 C15 Se1 Co1 100.13(13) . . ? C15 Se1 Co2 100.40(13) . . ? Co1 Se1 Co2 62.99(3) . . ? C16 Se2 Co2 101.02(13) . . ? C16 Se2 Co1 100.55(13) . . ? Co2 Se2 Co1 63.35(3) . . ? C2 Co1 C3 40.8(2) . . ? C2 Co1 C4 67.2(2) . . ? C3 Co1 C4 39.4(2) . . ? C2 Co1 C1 40.2(2) . . ? C3 Co1 C1 67.4(2) . . ? C4 Co1 C1 66.5(2) . . ? C2 Co1 C5 67.7(2) . . ? C3 Co1 C5 67.7(2) . . ? C4 Co1 C5 40.55(19) . . ? C1 Co1 C5 39.34(19) . . ? C2 Co1 Se2 101.12(16) . . ? C3 Co1 Se2 104.94(16) . . ? C4 Co1 Se2 137.69(16) . . ? C1 Co1 Se2 130.59(17) . . ? C5 Co1 Se2 168.71(14) . . ? C2 Co1 Se1 168.59(17) . . ? C3 Co1 Se1 144.28(18) . . ? C4 Co1 Se1 111.44(15) . . ? C1 Co1 Se1 128.44(16) . . ? C5 Co1 Se1 103.61(14) . . ? Se2 Co1 Se1 87.32(3) . . ? C2 Co1 Co2 119.63(17) . . ? C3 Co1 Co2 155.01(18) . . ? C4 Co1 Co2 163.48(16) . . ? C1 Co1 Co2 108.09(16) . . ? C5 Co1 Co2 125.40(15) . . ? Se2 Co1 Co2 58.11(2) . . ? Se1 Co1 Co2 58.59(2) . . ? C12 Co2 C11 40.06(19) . . ? C12 Co2 C10 67.7(2) . . ? C11 Co2 C10 40.12(19) . . ? C12 Co2 C13 40.8(2) . . ? C11 Co2 C13 67.7(2) . . ? C10 Co2 C13 67.7(2) . . ? C12 Co2 C14 67.2(2) . . ? C11 Co2 C14 67.0(2) . . ? C10 Co2 C14 40.22(19) . . ? C13 Co2 C14 39.51(19) . . ? C12 Co2 Se2 102.46(16) . . ? C11 Co2 Se2 132.19(16) . . ? C10 Co2 Se2 170.13(14) . . ? C13 Co2 Se2 104.56(16) . . ? C14 Co2 Se2 136.43(15) . . ? C12 Co2 Se1 165.52(17) . . ? C11 Co2 Se1 125.67(16) . . ? C10 Co2 Se1 102.34(14) . . ? C13 Co2 Se1 146.88(17) . . ? C14 Co2 Se1 112.60(15) . . ? Se2 Co2 Se1 87.48(3) . . ? C12 Co2 Co1 117.98(17) . . ? C11 Co2 Co1 106.78(16) . . ? C10 Co2 Co1 125.98(15) . . ? C13 Co2 Co1 153.21(16) . . ? C14 Co2 Co1 164.50(15) . . ? Se2 Co2 Co1 58.54(3) . . ? Se1 Co2 Co1 58.42(2) . . ? C7 O1 C8 113.6(4) . . ? C5 C1 C2 109.1(5) . . ? C5 C1 Co1 70.6(3) . . ? C2 C1 Co1 68.2(3) . . ? C5 C1 H1 125.4 . . ? C2 C1 H1 125.4 . . ? Co1 C1 H1 125.4 . . ? C1 C2 C3 107.6(5) . . ? C1 C2 Co1 71.6(3) . . ? C3 C2 Co1 70.1(3) . . ? C1 C2 H2 126.2 . . ? C3 C2 H2 126.2 . . ? Co1 C2 H2 126.2 . . ? C4 C3 C2 107.8(5) . . ? C4 C3 Co1 71.2(3) . . ? C2 C3 Co1 69.1(3) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Co1 C3 H3 126.1 . . ? C3 C4 C5 109.1(5) . . ? C3 C4 Co1 69.4(3) . . ? C5 C4 Co1 70.3(3) . . ? C3 C4 H4 125.5 . . ? C5 C4 H4 125.5 . . ? Co1 C4 H4 125.5 . . ? C1 C5 C4 106.4(5) . . ? C1 C5 C6 129.4(5) . . ? C4 C5 C6 124.1(5) . . ? C1 C5 Co1 70.1(3) . . ? C4 C5 Co1 69.2(3) . . ? C6 C5 Co1 129.1(3) . . ? C7 C6 C5 114.9(5) . . ? C7 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? O1 C7 C6 108.7(4) . . ? O1 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? O1 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O1 C8 C9 108.9(4) . . ? O1 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? O1 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C10 C9 C8 115.2(4) . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C14 107.2(5) . . ? C11 C10 C9 127.7(5) . . ? C14 C10 C9 125.0(5) . . ? C11 C10 Co2 69.8(3) . . ? C14 C10 Co2 70.5(3) . . ? C9 C10 Co2 127.7(4) . . ? C12 C11 C10 108.2(5) . . ? C12 C11 Co2 68.8(3) . . ? C10 C11 Co2 70.1(3) . . ? C12 C11 H11 125.9 . . ? C10 C11 H11 125.9 . . ? Co2 C11 H11 125.9 . . ? C11 C12 C13 108.6(5) . . ? C11 C12 Co2 71.1(3) . . ? C13 C12 Co2 71.0(3) . . ? C11 C12 H12 125.7 . . ? C13 C12 H12 125.7 . . ? Co2 C12 H12 125.7 . . ? C14 C13 C12 107.1(5) . . ? C14 C13 Co2 70.8(3) . . ? C12 C13 Co2 68.3(3) . . ? C14 C13 H13 126.5 . . ? C12 C13 H13 126.5 . . ? Co2 C13 H13 126.5 . . ? C13 C14 C10 108.8(5) . . ? C13 C14 Co2 69.6(3) . . ? C10 C14 Co2 69.2(3) . . ? C13 C14 H14 125.6 . . ? C10 C14 H14 125.6 . . ? Co2 C14 H14 125.6 . . ? C16 C15 B5 111.4(4) . . ? C16 C15 B4 111.2(4) . . ? B5 C15 B4 61.6(3) . . ? C16 C15 B3 62.2(3) . . ? B5 C15 B3 113.3(4) . . ? B4 C15 B3 62.0(3) . . ? C16 C15 B6 61.5(3) . . ? B5 C15 B6 62.9(3) . . ? B4 C15 B6 113.8(4) . . ? B3 C15 B6 114.8(4) . . ? C16 C15 Se1 113.7(3) . . ? B5 C15 Se1 124.6(3) . . ? B4 C15 Se1 124.3(3) . . ? B3 C15 Se1 115.2(3) . . ? B6 C15 Se1 115.6(3) . . ? C15 C16 B7 112.0(4) . . ? C15 C16 B11 112.7(4) . . ? B7 C16 B11 63.1(3) . . ? C15 C16 B6 62.3(3) . . ? B7 C16 B6 114.7(4) . . ? B11 C16 B6 62.5(3) . . ? C15 C16 B3 61.7(3) . . ? B7 C16 B3 62.5(3) . . ? B11 C16 B3 115.0(4) . . ? B6 C16 B3 115.1(4) . . ? C15 C16 Se2 113.1(3) . . ? B7 C16 Se2 123.8(3) . . ? B11 C16 Se2 123.3(3) . . ? B6 C16 Se2 115.0(3) . . ? B3 C16 Se2 115.2(3) . . ? C15 B3 C16 56.1(3) . . ? C15 B3 B8 104.9(4) . . ? C16 B3 B8 104.3(4) . . ? C15 B3 B4 58.6(3) . . ? C16 B3 B4 103.7(4) . . ? B8 B3 B4 60.6(3) . . ? C15 B3 B7 103.9(4) . . ? C16 B3 B7 58.0(3) . . ? B8 B3 B7 60.6(3) . . ? B4 B3 B7 108.6(4) . . ? C15 B3 H3A 125.1 . . ? C16 B3 H3A 125.7 . . ? B8 B3 H3A 122.4 . . ? B4 B3 H3A 121.9 . . ? B7 B3 H3A 122.1 . . ? C15 B4 B5 59.1(3) . . ? C15 B4 B3 59.4(3) . . ? B5 B4 B3 109.2(4) . . ? C15 B4 B9 103.8(4) . . ? B5 B4 B9 59.0(4) . . ? B3 B4 B9 107.9(4) . . ? C15 B4 B8 104.7(4) . . ? B5 B4 B8 108.3(5) . . ? B3 B4 B8 59.6(3) . . ? B9 B4 B8 60.5(4) . . ? C15 B4 H4A 124.8 . . ? B5 B4 H4A 121.1 . . ? B3 B4 H4A 121.0 . . ? B9 B4 H4A 123.0 . . ? B8 B4 H4A 122.3 . . ? C15 B5 B9 105.7(4) . . ? C15 B5 B4 59.3(3) . . ? B9 B5 B4 61.3(4) . . ? C15 B5 B6 59.2(3) . . ? B9 B5 B6 107.0(5) . . ? B4 B5 B6 108.9(4) . . ? C15 B5 B10 103.8(4) . . ? B9 B5 B10 59.5(4) . . ? B4 B5 B10 108.4(5) . . ? B6 B5 B10 58.3(3) . . ? C15 B5 H5 124.3 . . ? B9 B5 H5 122.1 . . ? B4 B5 H5 120.3 . . ? B6 B5 H5 122.0 . . ? B10 B5 H5 123.5 . . ? C16 B6 C15 56.1(3) . . ? C16 B6 B10 104.4(4) . . ? C15 B6 B10 105.1(4) . . ? C16 B6 B11 58.6(3) . . ? C15 B6 B11 104.5(4) . . ? B10 B6 B11 60.5(3) . . ? C16 B6 B5 103.1(4) . . ? C15 B6 B5 57.9(3) . . ? B10 B6 B5 61.2(4) . . ? B11 B6 B5 108.9(4) . . ? C16 B6 H6 125.7 . . ? C15 B6 H6 125.1 . . ? B10 B6 H6 122.2 . . ? B11 B6 H6 121.6 . . ? B5 B6 H6 122.2 . . ? C16 B7 B3 59.6(3) . . ? C16 B7 B12 103.5(4) . . ? B3 B7 B12 107.1(5) . . ? C16 B7 B11 58.7(3) . . ? B3 B7 B11 109.1(4) . . ? B12 B7 B11 59.7(4) . . ? C16 B7 B8 104.4(4) . . ? B3 B7 B8 59.3(3) . . ? B12 B7 B8 59.8(4) . . ? B11 B7 B8 108.3(4) . . ? C16 B7 H7 124.9 . . ? B3 B7 H7 121.2 . . ? B12 B7 H7 123.3 . . ? B11 B7 H7 120.9 . . ? B8 B7 H7 122.6 . . ? B3 B8 B12 107.8(4) . . ? B3 B8 B4 59.8(3) . . ? B12 B8 B4 107.2(5) . . ? B3 B8 B7 60.1(3) . . ? B12 B8 B7 59.9(4) . . ? B4 B8 B7 107.5(4) . . ? B3 B8 B9 107.3(4) . . ? B12 B8 B9 59.4(4) . . ? B4 B8 B9 59.6(4) . . ? B7 B8 B9 107.2(5) . . ? B3 B8 H8 121.8 . . ? B12 B8 H8 122.0 . . ? B4 B8 H8 122.2 . . ? B7 B8 H8 122.0 . . ? B9 B8 H8 122.4 . . ? B5 B9 B10 62.2(4) . . ? B5 B9 B12 109.2(5) . . ? B10 B9 B12 59.5(4) . . ? B5 B9 B4 59.7(3) . . ? B10 B9 B4 109.2(4) . . ? B12 B9 B4 107.9(5) . . ? B5 B9 B8 108.3(4) . . ? B10 B9 B8 108.2(5) . . ? B12 B9 B8 59.9(4) . . ? B4 B9 B8 59.9(3) . . ? B5 B9 H9 120.7 . . ? B10 B9 H9 120.8 . . ? B12 B9 H9 121.8 . . ? B4 B9 H9 121.7 . . ? B8 B9 H9 121.9 . . ? B12 B10 B6 108.5(5) . . ? B12 B10 B9 60.6(4) . . ? B6 B10 B9 107.9(5) . . ? B12 B10 B11 60.4(4) . . ? B6 B10 B11 60.5(3) . . ? B9 B10 B11 109.0(5) . . ? B12 B10 B5 107.0(5) . . ? B6 B10 B5 60.5(3) . . ? B9 B10 B5 58.3(4) . . ? B11 B10 B5 108.4(4) . . ? B12 B10 H10 121.6 . . ? B6 B10 H10 121.2 . . ? B9 B10 H10 121.9 . . ? B11 B10 H10 120.9 . . ? B5 B10 H10 122.5 . . ? C16 B11 B12 103.5(4) . . ? C16 B11 B10 103.6(4) . . ? B12 B11 B10 59.1(4) . . ? C16 B11 B6 59.0(3) . . ? B12 B11 B6 106.3(5) . . ? B10 B11 B6 59.0(3) . . ? C16 B11 B7 58.2(3) . . ? B12 B11 B7 60.1(4) . . ? B10 B11 B7 107.4(5) . . ? B6 B11 B7 107.8(4) . . ? C16 B11 H11A 125.3 . . ? B12 B11 H11A 123.3 . . ? B10 B11 H11A 123.2 . . ? B6 B11 H11A 122.0 . . ? B7 B11 H11A 121.4 . . ? B10 B12 B9 59.9(4) . . ? B10 B12 B11 60.5(4) . . ? B9 B12 B11 108.5(5) . . ? B10 B12 B8 109.1(5) . . ? B9 B12 B8 60.7(4) . . ? B11 B12 B8 109.1(4) . . ? B10 B12 B7 108.7(4) . . ? B9 B12 B7 108.5(5) . . ? B11 B12 B7 60.2(4) . . ? B8 B12 B7 60.3(4) . . ? B10 B12 H12A 121.2 . . ? B9 B12 H12A 121.5 . . ? B11 B12 H12A 121.2 . . ? B8 B12 H12A 120.8 . . ? B7 B12 H12A 121.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.975 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.113 # Attachment 'complex 10b.cif' data_f60412d _database_code_depnum_ccdc_archive 'CCDC 616737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H70 B20 Cl4 O P2 Rh2 Se4' _chemical_formula_weight 1700.72 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.047(3) _cell_length_b 18.278(5) _cell_length_c 33.285(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.573(5) _cell_angle_gamma 90.00 _cell_volume 7329(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 857 _cell_measurement_theta_min 2.311 _cell_measurement_theta_max 20.448 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 2.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6907 _exptl_absorpt_correction_T_max 0.7765 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% 3.88 _diffrn_reflns_number 30475 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.1612 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12901 _reflns_number_gt 5064 _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^)+(0.0610P)^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 12901 _refine_ls_number_parameters 812 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1553 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 0.943 _refine_ls_shift/su_mean 0.124 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 Rh1 Rh 0.80129(5) 0.29437(4) 0.39297(2) 0.0481(2) Uani 1 1 d . . . Rh2 Rh 1.16422(6) 0.29596(5) 0.21477(2) 0.0523(2) Uani 1 1 d . . . Se1 Se 0.63506(8) 0.37180(6) 0.38777(3) 0.0594(3) Uani 1 1 d . . . Se2 Se 0.70233(8) 0.21045(6) 0.43759(3) 0.0580(3) Uani 1 1 d . . . Se3 Se 1.27962(7) 0.21239(6) 0.17522(3) 0.0550(3) Uani 1 1 d . . . Se4 Se 1.31728(8) 0.38381(6) 0.22047(3) 0.0668(3) Uani 1 1 d . . . P1 P 0.86377(19) 0.35925(14) 0.44749(7) 0.0484(7) Uani 1 1 d . . . P2 P 1.1003(2) 0.34577(15) 0.15584(8) 0.0537(7) Uani 1 1 d . . . O1 O 1.0498(11) 0.1182(5) 0.3233(3) 0.188(6) Uani 1 1 d . . . B3 B 0.5110(10) 0.2225(7) 0.3723(4) 0.070(4) Uani 1 1 d . . . H3 H 0.5682 0.2077 0.3481 0.083 Uiso 1 1 calc R . . B4 B 0.4078(9) 0.2893(8) 0.3656(4) 0.072(4) Uani 1 1 d . . . H4 H 0.3965 0.3187 0.3370 0.087 Uiso 1 1 calc R . . B5 B 0.3880(9) 0.3343(8) 0.4118(4) 0.072(4) Uani 1 1 d . . . H5 H 0.3643 0.3923 0.4133 0.087 Uiso 1 1 calc R . . B6 B 0.4792(9) 0.2952(7) 0.4479(3) 0.068(4) Uani 1 1 d . . . H6 H 0.5153 0.3280 0.4725 0.081 Uiso 1 1 calc R . . B7 B 0.4653(11) 0.1567(8) 0.4072(4) 0.086(5) Uani 1 1 d . . . H7 H 0.4918 0.0992 0.4057 0.103 Uiso 1 1 calc R . . B8 B 0.3731(11) 0.1980(10) 0.3707(5) 0.110(6) Uani 1 1 d . . . H8 H 0.3378 0.1668 0.3453 0.132 Uiso 1 1 calc R . . B9 B 0.2976(11) 0.2659(10) 0.3955(5) 0.104(6) Uani 1 1 d . . . H9 H 0.2118 0.2792 0.3864 0.125 Uiso 1 1 calc R . . B10 B 0.3396(10) 0.2677(9) 0.4461(4) 0.093(5) Uani 1 1 d . . . H10 H 0.2811 0.2818 0.4701 0.111 Uiso 1 1 calc R . . B11 B 0.4432(10) 0.2035(9) 0.4541(4) 0.089(5) Uani 1 1 d . . . H11 H 0.4553 0.1763 0.4833 0.107 Uiso 1 1 calc R . . B12 B 0.3308(10) 0.1832(10) 0.4218(5) 0.106(6) Uani 1 1 d . . . H12 H 0.2683 0.1419 0.4297 0.127 Uiso 1 1 calc R . . B13 B 1.4840(9) 0.3174(6) 0.1610(3) 0.053(3) Uani 1 1 d . . . H13 H 1.4425 0.3447 0.1355 0.063 Uiso 1 1 calc R . . B14 B 1.5361(9) 0.2280(7) 0.1566(4) 0.066(4) Uani 1 1 d . . . H14 H 1.5277 0.1969 0.1285 0.079 Uiso 1 1 calc R . . B15 B 1.5271(9) 0.1837(7) 0.2037(3) 0.063(4) Uani 1 1 d . . . H15 H 1.5124 0.1244 0.2057 0.076 Uiso 1 1 calc R . . B16 B 1.4677(9) 0.2470(7) 0.2376(3) 0.057(3) Uani 1 1 d . . . H16 H 1.4134 0.2296 0.2622 0.069 Uiso 1 1 calc R . . B17 B 1.5660(9) 0.3646(7) 0.1971(3) 0.062(3) Uani 1 1 d . . . H17 H 1.5763 0.4244 0.1955 0.075 Uiso 1 1 calc R . . B18 B 1.6275(9) 0.3041(7) 0.1633(4) 0.071(4) Uani 1 1 d . . . H18 H 1.6810 0.3237 0.1390 0.085 Uiso 1 1 calc R . . B19 B 1.6569(9) 0.2221(8) 0.1890(4) 0.085(5) Uani 1 1 d . . . H19 H 1.7291 0.1882 0.1814 0.102 Uiso 1 1 calc R . . B20 B 1.6133(9) 0.2312(8) 0.2385(4) 0.072(4) Uani 1 1 d . . . H20 H 1.6555 0.2024 0.2633 0.086 Uiso 1 1 calc R . . B21 B 1.5597(9) 0.3195(8) 0.2426(4) 0.071(4) Uani 1 1 d . . . H21 H 1.5671 0.3499 0.2710 0.085 Uiso 1 1 calc R . . B22 B 1.6710(10) 0.3047(8) 0.2134(4) 0.074(4) Uani 1 1 d . . . H22 H 1.7536 0.3253 0.2221 0.089 Uiso 1 1 calc R . . C1 C 0.5176(7) 0.3025(5) 0.3982(3) 0.057(3) Uani 1 1 d . . . C2 C 0.5469(7) 0.2269(5) 0.4230(3) 0.058(3) Uani 1 1 d . . . C19 C 0.9457(7) 0.4350(5) 0.4277(3) 0.054(3) Uani 1 1 d . . . C20 C 1.0606(8) 0.4400(6) 0.4337(3) 0.077(3) Uani 1 1 d . . . H20A H 1.0982 0.4078 0.4506 0.092 Uiso 1 1 calc R . . C21 C 1.1159(9) 0.4944(8) 0.4135(4) 0.096(4) Uani 1 1 d . . . H21A H 1.1920 0.4992 0.4179 0.115 Uiso 1 1 calc R . . C22 C 1.0671(12) 0.5397(7) 0.3885(4) 0.102(4) Uani 1 1 d . . . H22A H 1.1090 0.5743 0.3748 0.123 Uiso 1 1 calc R . . C23 C 0.9551(11) 0.5364(6) 0.3823(4) 0.095(4) Uani 1 1 d . . . H23A H 0.9204 0.5698 0.3653 0.114 Uiso 1 1 calc R . . C24 C 0.8933(8) 0.4834(6) 0.4013(3) 0.066(3) Uani 1 1 d . . . H24A H 0.8173 0.4801 0.3965 0.079 Uiso 1 1 calc R . . C25 C 0.7665(7) 0.3996(6) 0.4840(3) 0.053(3) Uani 1 1 d . . . C26 C 0.7303(9) 0.4705(7) 0.4809(3) 0.081(4) Uani 1 1 d . . . H26A H 0.7563 0.5005 0.4605 0.098 Uiso 1 1 calc R . . C27 C 0.6560(11) 0.4970(8) 0.5079(4) 0.109(5) Uani 1 1 d . . . H27A H 0.6327 0.5454 0.5062 0.131 Uiso 1 1 calc R . . C28 C 0.6149(10) 0.4522(10) 0.5379(4) 0.105(5) Uani 1 1 d . . . H28A H 0.5637 0.4704 0.5561 0.126 Uiso 1 1 calc R . . C29 C 0.6499(9) 0.3817(8) 0.5405(4) 0.087(4) Uani 1 1 d . . . H29A H 0.6230 0.3514 0.5606 0.104 Uiso 1 1 calc R . . C30 C 0.7246(8) 0.3550(6) 0.5134(3) 0.066(3) Uani 1 1 d . . . H30A H 0.7472 0.3064 0.5150 0.079 Uiso 1 1 calc R . . C31 C 0.9589(6) 0.3093(6) 0.4806(3) 0.051(3) Uani 1 1 d . . . C32 C 1.0029(8) 0.3439(6) 0.5148(3) 0.067(3) Uani 1 1 d . . . H32A H 0.9864 0.3926 0.5203 0.080 Uiso 1 1 calc R . . C33 C 1.0721(8) 0.3035(8) 0.5403(3) 0.086(4) Uani 1 1 d . . . H33A H 1.1025 0.3258 0.5630 0.103 Uiso 1 1 calc R . . C34 C 1.0958(9) 0.2322(8) 0.5326(4) 0.082(4) Uani 1 1 d . . . H34A H 1.1406 0.2062 0.5505 0.098 Uiso 1 1 calc R . . C35 C 1.0543(8) 0.1977(7) 0.4987(3) 0.074(3) Uani 1 1 d . . . H35A H 1.0726 0.1494 0.4930 0.088 Uiso 1 1 calc R . . C36 C 0.9852(7) 0.2370(6) 0.4733(3) 0.058(3) Uani 1 1 d . . . H36A H 0.9555 0.2142 0.4507 0.069 Uiso 1 1 calc R . . C9 C 0.9049(11) 0.2087(7) 0.3623(4) 0.075(3) Uani 1 1 d . . . C5 C 0.9634(8) 0.2710(8) 0.3664(3) 0.070(3) Uani 1 1 d . . . H5A H 1.0354 0.2758 0.3801 0.083 Uiso 1 1 calc R . . C6 C 0.9055(14) 0.3292(7) 0.3443(4) 0.095(5) Uani 1 1 d . . . H6A H 0.9322 0.3787 0.3386 0.114 Uiso 1 1 calc R . . C7 C 0.8147(11) 0.2926(10) 0.3267(3) 0.091(4) Uani 1 1 d . . . H7A H 0.7611 0.3149 0.3081 0.109 Uiso 1 1 calc R . . C8 C 0.8140(11) 0.2212(10) 0.3382(4) 0.098(5) Uani 1 1 d . . . H8A H 0.7594 0.1845 0.3297 0.118 Uiso 1 1 calc R . . C10 C 0.9372(12) 0.1321(7) 0.3786(4) 0.126(5) Uani 1 1 d . . . H10A H 0.9962 0.1369 0.3984 0.151 Uiso 1 1 calc R . . H10B H 0.8737 0.1100 0.3915 0.151 Uiso 1 1 calc R . . C11 C 0.9743(11) 0.0851(7) 0.3455(4) 0.122(5) Uani 1 1 d . . . H11A H 1.0054 0.0403 0.3565 0.146 Uiso 1 1 calc R . . H11B H 0.9110 0.0721 0.3287 0.146 Uiso 1 1 calc R . . C12 C 1.1104(12) 0.0926(8) 0.2973(5) 0.134(6) Uani 1 1 d . . . H12A H 1.0640 0.0629 0.2798 0.160 Uiso 1 1 calc R . . H12B H 1.1617 0.0595 0.3107 0.160 Uiso 1 1 calc R . . C13 C 1.1761(11) 0.1399(7) 0.2717(4) 0.103(4) Uani 1 1 d . . . H13A H 1.1863 0.1159 0.2460 0.123 Uiso 1 1 calc R . . H13B H 1.2489 0.1465 0.2839 0.123 Uiso 1 1 calc R . . C14 C 1.1249(9) 0.2132(7) 0.2647(3) 0.060(3) Uani 1 1 d . . . C15 C 1.1618(9) 0.2782(7) 0.2817(3) 0.068(3) Uani 1 1 d . . . H15A H 1.2270 0.2825 0.2994 0.081 Uiso 1 1 calc R . . C16 C 1.0942(14) 0.3359(9) 0.2708(4) 0.109(5) Uani 1 1 d . . . H16A H 1.0981 0.3861 0.2812 0.130 Uiso 1 1 calc R . . C17 C 1.0100(10) 0.3063(10) 0.2467(4) 0.105(6) Uani 1 1 d . . . H17A H 0.9439 0.3324 0.2371 0.126 Uiso 1 1 calc R . . C18 C 1.0305(10) 0.2289(8) 0.2421(3) 0.083(4) Uani 1 1 d . . . H18A H 0.9826 0.1935 0.2282 0.099 Uiso 1 1 calc R . . C37 C 1.0138(9) 0.4237(6) 0.1683(3) 0.063(3) Uani 1 1 d . . . C38 C 1.0557(10) 0.4792(7) 0.1915(4) 0.092(4) Uani 1 1 d . . . H38A H 1.1307 0.4782 0.1985 0.110 Uiso 1 1 calc R . . C39 C 0.9924(12) 0.5360(7) 0.2048(4) 0.102(4) Uani 1 1 d . . . H39A H 1.0250 0.5728 0.2202 0.123 Uiso 1 1 calc R . . C40 C 0.8823(13) 0.5393(7) 0.1958(4) 0.105(5) Uani 1 1 d . . . H40A H 0.8386 0.5774 0.2053 0.126 Uiso 1 1 calc R . . C41 C 0.8379(10) 0.4857(9) 0.1726(4) 0.112(5) Uani 1 1 d . . . H41A H 0.7628 0.4881 0.1659 0.134 Uiso 1 1 calc R . . C42 C 0.9008(9) 0.4263(6) 0.1583(3) 0.082(4) Uani 1 1 d . . . H42A H 0.8682 0.3900 0.1426 0.098 Uiso 1 1 calc R . . C43 C 1.0130(7) 0.2855(7) 0.1254(3) 0.057(3) Uani 1 1 d . . . C44 C 0.9890(8) 0.2158(7) 0.1364(3) 0.068(3) Uani 1 1 d . . . H44A H 1.0189 0.1979 0.1604 0.081 Uiso 1 1 calc R . . C45 C 0.9211(9) 0.1700(7) 0.1133(4) 0.082(4) Uani 1 1 d . . . H45A H 0.9060 0.1226 0.1219 0.098 Uiso 1 1 calc R . . C46 C 0.8774(9) 0.1953(8) 0.0782(4) 0.093(4) Uani 1 1 d . . . H46A H 0.8309 0.1655 0.0629 0.111 Uiso 1 1 calc R . . C47 C 0.9012(9) 0.2637(9) 0.0654(4) 0.091(4) Uani 1 1 d . . . H47A H 0.8734 0.2801 0.0408 0.109 Uiso 1 1 calc R . . C48 C 0.9685(8) 0.3106(7) 0.0892(3) 0.080(4) Uani 1 1 d . . . H48A H 0.9828 0.3581 0.0807 0.096 Uiso 1 1 calc R . . C49 C 1.1965(8) 0.3792(7) 0.1176(3) 0.062(3) Uani 1 1 d . . . C50 C 1.2288(9) 0.4515(7) 0.1156(3) 0.089(4) Uani 1 1 d . . . H50A H 1.1999 0.4858 0.1332 0.107 Uiso 1 1 calc R . . C51 C 1.3068(11) 0.4727(8) 0.0861(4) 0.109(5) Uani 1 1 d . . . H51A H 1.3313 0.5209 0.0848 0.131 Uiso 1 1 calc R . . C52 C 1.3454(12) 0.4226(11) 0.0598(5) 0.121(6) Uani 1 1 d . . . H52A H 1.3958 0.4365 0.0403 0.145 Uiso 1 1 calc R . . C53 C 1.3112(10) 0.3523(9) 0.0619(4) 0.094(4) Uani 1 1 d . . . H53A H 1.3383 0.3188 0.0434 0.113 Uiso 1 1 calc R . . C54 C 1.2379(8) 0.3290(7) 0.0902(3) 0.075(3) Uani 1 1 d . . . H54A H 1.2160 0.2802 0.0912 0.090 Uiso 1 1 calc R . . C3 C 1.4289(7) 0.2475(5) 0.1884(2) 0.048(2) Uani 1 1 d . . . C4 C 1.4483(7) 0.3238(5) 0.2105(3) 0.049(3) Uani 1 1 d . . . Cl3 Cl 0.8426(9) 0.9803(6) 0.4420(3) 0.434(7) Uani 1 1 d . . . Cl4 Cl 0.6466(11) 0.9609(6) 0.4824(3) 0.467(8) Uani 1 1 d . . . Cl1 Cl -0.1143(7) 1.0340(4) 0.2042(2) 0.302(4) Uani 1 1 d . . . Cl2 Cl 0.1176(6) 1.0319(4) 0.1661(2) 0.257(3) Uani 1 1 d . . . C55 C 0.0232(18) 0.9883(13) 0.1901(6) 0.242(10) Uiso 1 1 d . . . H55A H 0.0571 0.9709 0.2149 0.290 Uiso 1 1 calc R . . H55B H 0.0048 0.9453 0.1743 0.290 Uiso 1 1 calc R . . C56 C 0.714(2) 1.0048(14) 0.4580(7) 0.259(12) Uiso 1 1 d . . . H56A H 0.7236 1.0509 0.4721 0.311 Uiso 1 1 calc R . . H56B H 0.6709 1.0156 0.4340 0.311 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 Rh1 0.0361(4) 0.0635(6) 0.0450(5) -0.0003(4) 0.0034(3) 0.0023(4) Rh2 0.0373(4) 0.0642(6) 0.0556(5) -0.0009(5) 0.0088(3) 0.0062(4) Se1 0.0425(6) 0.0662(8) 0.0695(7) 0.0062(6) -0.0031(5) 0.0061(5) Se2 0.0481(6) 0.0627(7) 0.0632(7) 0.0073(6) 0.0033(5) -0.0001(5) Se3 0.0448(6) 0.0604(7) 0.0599(7) -0.0132(6) 0.0069(5) -0.0040(5) Se4 0.0507(7) 0.0576(8) 0.0923(9) -0.0186(6) 0.0050(6) 0.0031(5) P1 0.0370(14) 0.0608(19) 0.0476(16) 0.0041(13) 0.0035(11) -0.0029(13) P2 0.0400(15) 0.064(2) 0.0576(17) 0.0021(14) 0.0062(12) 0.0028(13) O1 0.280(15) 0.090(8) 0.197(11) 0.042(7) 0.192(11) 0.067(8) B3 0.060(8) 0.090(11) 0.058(8) -0.021(8) 0.003(6) -0.007(7) B4 0.035(7) 0.119(13) 0.062(8) -0.020(9) -0.008(6) 0.016(8) B5 0.036(7) 0.097(11) 0.084(9) -0.016(8) -0.001(6) 0.010(7) B6 0.055(8) 0.088(10) 0.059(8) -0.026(8) 0.017(6) -0.004(8) B7 0.074(10) 0.075(11) 0.107(12) -0.033(9) 0.010(8) -0.034(8) B8 0.051(9) 0.163(18) 0.116(14) -0.057(13) -0.003(8) -0.018(10) B9 0.034(8) 0.156(17) 0.121(13) -0.020(12) -0.012(8) -0.015(9) B10 0.041(8) 0.148(16) 0.089(11) -0.007(10) 0.020(7) -0.007(9) B11 0.055(9) 0.132(14) 0.081(10) 0.001(10) 0.017(7) -0.029(9) B12 0.047(9) 0.147(18) 0.124(14) -0.012(13) 0.019(9) -0.035(9) B13 0.051(8) 0.064(9) 0.044(7) 0.002(6) 0.010(6) -0.012(6) B14 0.057(8) 0.086(11) 0.055(8) -0.004(7) 0.019(6) 0.002(7) B15 0.062(8) 0.062(9) 0.067(9) 0.003(7) 0.007(6) 0.021(7) B16 0.055(8) 0.075(9) 0.043(7) -0.005(6) 0.000(6) 0.006(7) B17 0.044(7) 0.062(9) 0.081(9) -0.004(7) 0.008(6) -0.014(6) B18 0.039(7) 0.098(11) 0.076(9) 0.012(8) 0.021(6) 0.004(7) B19 0.028(7) 0.127(14) 0.100(11) 0.017(10) 0.013(6) 0.024(8) B20 0.052(8) 0.103(12) 0.060(8) -0.004(8) -0.015(6) 0.026(7) B21 0.050(8) 0.105(12) 0.058(8) -0.008(8) -0.012(6) -0.008(7) B22 0.041(7) 0.095(12) 0.087(10) -0.001(9) 0.001(6) -0.009(7) C1 0.043(6) 0.068(8) 0.060(6) -0.002(6) 0.000(5) 0.014(5) C2 0.050(6) 0.067(8) 0.057(7) 0.001(6) 0.004(5) -0.016(5) C19 0.043(6) 0.063(7) 0.055(7) 0.004(6) 0.003(5) -0.008(5) C20 0.050(7) 0.099(10) 0.080(8) 0.009(7) -0.004(6) -0.030(7) C21 0.051(8) 0.109(12) 0.128(12) 0.023(9) -0.011(8) -0.021(8) C22 0.097(12) 0.093(11) 0.118(12) 0.028(9) 0.016(9) -0.034(9) C23 0.103(11) 0.072(10) 0.110(11) 0.035(8) -0.015(8) -0.029(8) C24 0.047(6) 0.068(8) 0.083(8) 0.011(6) 0.007(6) -0.010(6) C25 0.044(6) 0.068(8) 0.047(6) -0.015(6) -0.002(5) 0.002(5) C26 0.094(9) 0.092(10) 0.059(7) -0.021(7) 0.006(6) 0.027(8) C27 0.118(12) 0.117(13) 0.092(11) -0.024(10) 0.004(9) 0.049(10) C28 0.052(8) 0.173(17) 0.090(11) -0.047(11) -0.004(7) 0.023(10) C29 0.059(8) 0.116(12) 0.085(9) -0.030(9) 0.008(7) -0.015(8) C30 0.056(7) 0.080(9) 0.063(7) -0.010(6) 0.023(6) -0.002(6) C31 0.025(5) 0.083(9) 0.046(6) 0.011(6) 0.011(4) -0.006(5) C32 0.047(6) 0.100(9) 0.054(7) 0.000(7) 0.001(5) -0.006(6) C33 0.045(7) 0.162(15) 0.050(7) 0.019(9) -0.004(5) -0.018(8) C34 0.049(7) 0.119(13) 0.077(9) 0.029(9) 0.009(6) 0.026(8) C35 0.048(7) 0.101(10) 0.072(8) 0.024(8) 0.011(6) 0.016(7) C36 0.041(6) 0.072(8) 0.060(7) 0.014(6) 0.006(5) 0.008(5) C9 0.062(8) 0.070(9) 0.093(9) 0.003(8) 0.039(7) 0.019(8) C5 0.026(6) 0.119(12) 0.063(7) -0.005(8) 0.005(5) -0.004(7) C6 0.154(14) 0.059(9) 0.073(9) 0.002(7) 0.085(9) -0.016(9) C7 0.081(10) 0.142(15) 0.050(8) -0.004(10) 0.009(6) 0.029(11) C8 0.073(10) 0.142(15) 0.080(10) -0.040(10) 0.007(7) -0.003(10) C10 0.168(14) 0.081(11) 0.131(12) 0.001(9) 0.074(10) 0.020(10) C11 0.138(13) 0.091(11) 0.137(13) 0.016(10) 0.076(10) 0.036(9) C12 0.139(14) 0.115(14) 0.148(15) 0.056(11) 0.054(11) 0.014(10) C13 0.130(12) 0.082(10) 0.097(10) 0.006(8) 0.038(8) 0.037(9) C14 0.061(7) 0.076(9) 0.044(6) 0.009(7) 0.021(5) 0.004(7) C15 0.057(7) 0.085(10) 0.062(7) -0.017(7) 0.006(5) 0.014(7) C16 0.130(14) 0.106(13) 0.091(11) -0.016(9) 0.069(10) 0.000(11) C17 0.056(9) 0.143(15) 0.118(12) 0.078(11) 0.061(8) 0.052(9) C18 0.063(8) 0.126(13) 0.060(8) 0.022(8) 0.003(6) -0.030(8) C37 0.054(7) 0.068(9) 0.067(7) 0.012(6) 0.012(5) 0.007(6) C38 0.079(9) 0.074(10) 0.122(11) -0.002(8) 0.002(8) 0.019(8) C39 0.094(11) 0.085(11) 0.129(12) -0.012(8) 0.019(9) 0.009(9) C40 0.096(12) 0.075(11) 0.144(14) -0.018(9) 0.020(10) 0.019(9) C41 0.059(9) 0.112(13) 0.164(15) 0.004(11) 0.009(9) 0.032(9) C42 0.059(8) 0.065(9) 0.121(10) 0.011(7) 0.001(7) 0.013(6) C43 0.036(6) 0.082(9) 0.054(7) -0.002(7) 0.005(5) 0.005(6) C44 0.065(7) 0.082(9) 0.056(7) -0.006(7) 0.005(6) 0.003(7) C45 0.077(9) 0.085(10) 0.084(10) -0.015(8) 0.012(7) -0.005(7) C46 0.061(8) 0.126(14) 0.091(11) -0.026(9) 0.003(7) -0.015(8) C47 0.059(8) 0.143(14) 0.070(9) 0.005(9) -0.009(6) -0.006(8) C48 0.053(7) 0.105(11) 0.082(9) 0.010(8) 0.013(6) -0.003(7) C49 0.050(6) 0.075(9) 0.061(7) 0.006(6) 0.012(5) -0.005(6) C50 0.076(9) 0.091(11) 0.102(10) 0.008(8) 0.026(7) 0.005(7) C51 0.099(11) 0.100(12) 0.129(13) 0.045(10) 0.046(9) -0.009(9) C52 0.082(11) 0.165(18) 0.117(14) 0.033(13) 0.035(9) -0.014(11) C53 0.077(10) 0.130(14) 0.075(9) -0.007(9) 0.019(7) 0.001(9) C54 0.049(7) 0.110(10) 0.066(8) 0.014(7) 0.016(6) 0.003(6) C3 0.035(5) 0.070(7) 0.038(6) -0.006(5) 0.007(4) 0.006(5) C4 0.048(6) 0.048(6) 0.051(6) -0.018(5) 0.009(5) -0.012(5) Cl3 0.436(14) 0.403(14) 0.467(14) 0.236(12) 0.133(11) 0.180(11) Cl4 0.67(2) 0.366(14) 0.363(12) 0.022(10) 0.043(13) -0.280(15) Cl1 0.326(9) 0.215(8) 0.365(10) 0.056(7) -0.058(7) -0.016(7) Cl2 0.270(7) 0.180(6) 0.322(8) 0.034(6) -0.005(6) -0.043(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C6 2.155(9) . ? Rh1 C5 2.194(9) . ? Rh1 C7 2.212(11) . ? Rh1 C9 2.253(11) . ? Rh1 C8 2.268(12) . ? Rh1 P1 2.289(3) . ? Rh1 Se2 2.4526(13) . ? Rh1 Se1 2.4568(13) . ? Rh2 C17 2.158(10) . ? Rh2 C16 2.181(11) . ? Rh2 C18 2.226(10) . ? Rh2 C15 2.252(10) . ? Rh2 P2 2.289(3) . ? Rh2 C14 2.300(10) . ? Rh2 Se4 2.4508(14) . ? Rh2 Se3 2.4566(13) . ? Se1 C1 1.933(10) . ? Se2 C2 1.953(9) . ? Se3 C3 1.955(8) . ? Se4 C4 1.954(9) . ? P1 C31 1.827(9) . ? P1 C19 1.827(9) . ? P1 C25 1.849(9) . ? P2 C37 1.815(11) . ? P2 C43 1.824(10) . ? P2 C49 1.834(9) . ? O1 C12 1.231(13) . ? O1 C11 1.325(13) . ? B3 C1 1.699(15) . ? B3 B8 1.721(17) . ? B3 C2 1.739(14) . ? B3 B4 1.756(17) . ? B3 B7 1.762(18) . ? B4 C1 1.720(13) . ? B4 B9 1.722(17) . ? B4 B8 1.73(2) . ? B4 B5 1.763(16) . ? B5 C1 1.730(13) . ? B5 B9 1.740(19) . ? B5 B10 1.772(19) . ? B5 B6 1.772(17) . ? B6 C2 1.709(14) . ? B6 C1 1.729(14) . ? B6 B10 1.756(16) . ? B6 B11 1.743(18) . ? B7 C2 1.697(14) . ? B7 B12 1.765(18) . ? B7 B11 1.803(18) . ? B7 B8 1.80(2) . ? B8 B9 1.75(2) . ? B8 B12 1.80(2) . ? B9 B10 1.755(19) . ? B9 B12 1.79(2) . ? B10 B12 1.75(2) . ? B10 B11 1.73(2) . ? B11 C2 1.685(14) . ? B11 B12 1.761(18) . ? B13 C3 1.707(13) . ? B13 C4 1.710(13) . ? B13 B18 1.746(14) . ? B13 B14 1.757(16) . ? B13 B17 1.773(15) . ? B14 C3 1.715(13) . ? B14 B15 1.768(15) . ? B14 B18 1.786(17) . ? B14 B19 1.805(17) . ? B15 C3 1.735(14) . ? B15 B20 1.774(16) . ? B15 B16 1.772(15) . ? B15 B19 1.787(16) . ? B16 C4 1.684(14) . ? B16 C3 1.699(13) . ? B16 B21 1.734(17) . ? B16 B20 1.778(15) . ? B17 C4 1.666(13) . ? B17 B21 1.726(16) . ? B17 B22 1.755(17) . ? B17 B18 1.748(16) . ? B18 B22 1.742(16) . ? B18 B19 1.759(18) . ? B19 B22 1.721(18) . ? B19 B20 1.742(16) . ? B20 B22 1.732(18) . ? B20 B21 1.745(18) . ? B21 B22 1.687(16) . ? B21 C4 1.709(14) . ? C1 C2 1.647(13) . ? C19 C24 1.394(12) . ? C19 C20 1.399(11) . ? C20 C21 1.375(14) . ? C21 C22 1.311(15) . ? C22 C23 1.364(14) . ? C23 C24 1.378(13) . ? C25 C26 1.372(13) . ? C25 C30 1.374(12) . ? C26 C27 1.363(13) . ? C27 C28 1.385(17) . ? C28 C29 1.359(16) . ? C29 C30 1.369(13) . ? C31 C36 1.381(12) . ? C31 C32 1.400(12) . ? C32 C33 1.395(13) . ? C33 C34 1.359(15) . ? C34 C35 1.383(14) . ? C35 C36 1.381(12) . ? C9 C5 1.346(14) . ? C9 C8 1.371(15) . ? C9 C10 1.548(15) . ? C5 C6 1.464(15) . ? C6 C7 1.405(16) . ? C7 C8 1.359(16) . ? C10 C11 1.469(14) . ? C12 C13 1.454(15) . ? C13 C14 1.493(14) . ? C14 C15 1.387(13) . ? C14 C18 1.388(13) . ? C15 C16 1.380(16) . ? C16 C17 1.397(17) . ? C17 C18 1.444(17) . ? C37 C38 1.369(14) . ? C37 C42 1.399(12) . ? C38 C39 1.365(14) . ? C39 C40 1.358(15) . ? C40 C41 1.356(16) . ? C41 C42 1.409(15) . ? C43 C44 1.357(13) . ? C43 C48 1.390(13) . ? C44 C45 1.397(14) . ? C45 C46 1.359(14) . ? C46 C47 1.353(15) . ? C47 C48 1.417(15) . ? C49 C50 1.380(14) . ? C49 C54 1.390(13) . ? C50 C51 1.419(14) . ? C51 C52 1.351(17) . ? C52 C53 1.351(17) . ? C53 C54 1.367(14) . ? C3 C4 1.592(12) . ? Cl3 C56 1.70(2) . ? Cl4 C56 1.41(2) . ? Cl1 C55 1.92(2) . ? Cl2 C55 1.61(2) . ? 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 C6 Rh1 C5 39.3(4) . . ? C6 Rh1 C7 37.5(4) . . ? C5 Rh1 C7 61.4(4) . . ? C6 Rh1 C9 62.3(4) . . ? C5 Rh1 C9 35.2(4) . . ? C7 Rh1 C9 59.5(5) . . ? C6 Rh1 C8 61.6(5) . . ? C5 Rh1 C8 59.6(4) . . ? C7 Rh1 C8 35.3(4) . . ? C9 Rh1 C8 35.3(4) . . ? C6 Rh1 P1 104.7(4) . . ? C5 Rh1 P1 97.7(3) . . ? C7 Rh1 P1 140.4(5) . . ? C9 Rh1 P1 122.7(4) . . ? C8 Rh1 P1 156.7(4) . . ? C6 Rh1 Se2 158.4(3) . . ? C5 Rh1 Se2 124.2(4) . . ? C7 Rh1 Se2 129.4(5) . . ? C9 Rh1 Se2 96.6(3) . . ? C8 Rh1 Se2 99.0(4) . . ? P1 Rh1 Se2 90.11(7) . . ? C6 Rh1 Se1 104.9(4) . . ? C5 Rh1 Se1 144.3(4) . . ? C7 Rh1 Se1 90.3(4) . . ? C9 Rh1 Se1 145.4(4) . . ? C8 Rh1 Se1 110.2(4) . . ? P1 Rh1 Se1 91.08(7) . . ? Se2 Rh1 Se1 90.12(4) . . ? C17 Rh2 C16 37.5(4) . . ? C17 Rh2 C18 38.4(4) . . ? C16 Rh2 C18 63.1(5) . . ? C17 Rh2 C15 60.4(4) . . ? C16 Rh2 C15 36.2(4) . . ? C18 Rh2 C15 60.0(4) . . ? C17 Rh2 P2 95.9(3) . . ? C16 Rh2 P2 118.0(5) . . ? C18 Rh2 P2 109.3(3) . . ? C15 Rh2 P2 153.8(3) . . ? C17 Rh2 C14 61.1(4) . . ? C16 Rh2 C14 61.2(5) . . ? C18 Rh2 C14 35.7(3) . . ? C15 Rh2 C14 35.5(3) . . ? P2 Rh2 C14 144.2(3) . . ? C17 Rh2 Se4 123.7(6) . . ? C16 Rh2 Se4 90.6(4) . . ? C18 Rh2 Se4 151.2(3) . . ? C15 Rh2 Se4 92.0(3) . . ? P2 Rh2 Se4 92.99(8) . . ? C14 Rh2 Se4 122.3(3) . . ? C17 Rh2 Se3 144.4(5) . . ? C16 Rh2 Se3 153.2(5) . . ? C18 Rh2 Se3 107.0(4) . . ? C15 Rh2 Se3 117.0(3) . . ? P2 Rh2 Se3 88.60(7) . . ? C14 Rh2 Se3 95.7(3) . . ? Se4 Rh2 Se3 91.12(4) . . ? C1 Se1 Rh1 102.0(3) . . ? C2 Se2 Rh1 103.0(3) . . ? C3 Se3 Rh2 101.5(3) . . ? C4 Se4 Rh2 103.2(3) . . ? C31 P1 C19 105.0(4) . . ? C31 P1 C25 101.5(4) . . ? C19 P1 C25 106.5(5) . . ? C31 P1 Rh1 114.8(4) . . ? C19 P1 Rh1 106.3(3) . . ? C25 P1 Rh1 121.4(3) . . ? C37 P2 C43 105.8(5) . . ? C37 P2 C49 105.4(5) . . ? C43 P2 C49 100.4(5) . . ? C37 P2 Rh2 107.8(3) . . ? C43 P2 Rh2 115.0(4) . . ? C49 P2 Rh2 121.2(3) . . ? C12 O1 C11 129.4(13) . . ? C1 B3 B8 106.3(9) . . ? C1 B3 C2 57.2(6) . . ? B8 B3 C2 105.9(9) . . ? C1 B3 B4 59.7(7) . . ? B8 B3 B4 59.7(8) . . ? C2 B3 B4 105.2(8) . . ? C1 B3 B7 105.5(8) . . ? B8 B3 B7 62.3(8) . . ? C2 B3 B7 58.0(6) . . ? B4 B3 B7 109.5(9) . . ? C1 B4 B3 58.5(6) . . ? C1 B4 B9 105.2(9) . . ? B3 B4 B9 107.6(11) . . ? C1 B4 B8 105.0(9) . . ? B3 B4 B8 59.1(8) . . ? B9 B4 B8 61.0(9) . . ? C1 B4 B5 59.6(6) . . ? B3 B4 B5 108.3(9) . . ? B9 B4 B5 59.9(7) . . ? B8 B4 B5 109.2(10) . . ? C1 B5 B9 104.0(9) . . ? C1 B5 B10 104.0(9) . . ? B9 B5 B10 60.0(8) . . ? C1 B5 B6 59.1(6) . . ? B9 B5 B6 107.7(11) . . ? B10 B5 B6 59.4(7) . . ? C1 B5 B4 59.0(6) . . ? B9 B5 B4 58.9(7) . . ? B10 B5 B4 107.0(10) . . ? B6 B5 B4 108.4(9) . . ? C2 B6 C1 57.3(5) . . ? C2 B6 B10 103.7(9) . . ? C1 B6 B10 104.8(8) . . ? C2 B6 B11 58.4(7) . . ? C1 B6 B11 104.9(9) . . ? B10 B6 B11 59.3(8) . . ? C2 B6 B5 105.1(8) . . ? C1 B6 B5 59.2(6) . . ? B10 B6 B5 60.3(7) . . ? B11 B6 B5 108.3(10) . . ? C2 B7 B3 60.3(6) . . ? C2 B7 B12 103.7(10) . . ? B3 B7 B12 106.7(11) . . ? C2 B7 B11 57.4(6) . . ? B3 B7 B11 107.2(10) . . ? B12 B7 B11 59.2(8) . . ? C2 B7 B8 104.2(10) . . ? B3 B7 B8 57.7(8) . . ? B12 B7 B8 60.6(8) . . ? B11 B7 B8 106.9(11) . . ? B3 B8 B4 61.2(8) . . ? B3 B8 B9 107.8(11) . . ? B4 B8 B9 59.3(9) . . ? B3 B8 B12 106.9(10) . . ? B4 B8 B12 108.0(11) . . ? B9 B8 B12 60.5(8) . . ? B3 B8 B7 60.0(7) . . ? B4 B8 B7 108.8(9) . . ? B9 B8 B7 107.4(11) . . ? B12 B8 B7 58.6(8) . . ? B10 B9 B4 109.5(9) . . ? B10 B9 B5 60.9(8) . . ? B4 B9 B5 61.2(7) . . ? B10 B9 B8 108.7(12) . . ? B4 B9 B8 59.7(8) . . ? B5 B9 B8 109.2(9) . . ? B10 B9 B12 59.0(9) . . ? B4 B9 B12 108.8(11) . . ? B5 B9 B12 108.5(10) . . ? B8 B9 B12 61.1(10) . . ? B9 B10 B12 61.5(9) . . ? B9 B10 B6 107.7(9) . . ? B12 B10 B6 108.8(10) . . ? B9 B10 B11 109.6(11) . . ? B12 B10 B11 60.8(9) . . ? B6 B10 B11 59.9(7) . . ? B9 B10 B5 59.1(8) . . ? B12 B10 B5 109.0(10) . . ? B6 B10 B5 60.3(7) . . ? B11 B10 B5 108.8(9) . . ? C2 B11 B10 105.8(11) . . ? C2 B11 B12 104.4(9) . . ? B10 B11 B12 60.0(8) . . ? C2 B11 B6 59.8(7) . . ? B10 B11 B6 60.7(8) . . ? B12 B11 B6 108.8(11) . . ? C2 B11 B7 58.1(6) . . ? B10 B11 B7 107.5(10) . . ? B12 B11 B7 59.3(8) . . ? B6 B11 B7 108.4(9) . . ? B10 B12 B11 59.2(8) . . ? B10 B12 B7 108.6(9) . . ? B11 B12 B7 61.5(7) . . ? B10 B12 B9 59.5(9) . . ? B11 B12 B9 106.7(11) . . ? B7 B12 B9 107.4(10) . . ? B10 B12 B8 106.8(12) . . ? B11 B12 B8 108.8(9) . . ? B7 B12 B8 60.7(8) . . ? B9 B12 B8 58.4(9) . . ? C3 B13 C4 55.5(5) . . ? C3 B13 B18 105.2(8) . . ? C4 B13 B18 103.0(8) . . ? C3 B13 B14 59.3(6) . . ? C4 B13 B14 103.7(8) . . ? B18 B13 B14 61.3(7) . . ? C3 B13 B17 102.7(8) . . ? C4 B13 B17 57.1(5) . . ? B18 B13 B17 59.6(6) . . ? B14 B13 B17 108.2(9) . . ? C3 B14 B13 58.9(6) . . ? C3 B14 B15 59.7(6) . . ? B13 B14 B15 109.1(8) . . ? C3 B14 B18 103.2(8) . . ? B13 B14 B18 59.0(6) . . ? B15 B14 B18 106.8(9) . . ? C3 B14 B19 104.6(8) . . ? B13 B14 B19 107.0(9) . . ? B15 B14 B19 60.0(7) . . ? B18 B14 B19 58.6(7) . . ? C3 B15 B20 104.8(8) . . ? C3 B15 B16 57.9(6) . . ? B20 B15 B16 60.2(6) . . ? C3 B15 B14 58.6(6) . . ? B20 B15 B14 108.3(9) . . ? B16 B15 B14 107.1(9) . . ? C3 B15 B19 104.5(9) . . ? B20 B15 B19 58.6(7) . . ? B16 B15 B19 106.1(9) . . ? B14 B15 B19 61.0(7) . . ? C4 B16 C3 56.1(5) . . ? C4 B16 B21 60.0(7) . . ? C3 B16 B21 104.9(8) . . ? C4 B16 B20 106.0(9) . . ? C3 B16 B20 106.2(7) . . ? B21 B16 B20 59.6(7) . . ? C4 B16 B15 104.9(8) . . ? C3 B16 B15 59.9(6) . . ? B21 B16 B15 107.4(9) . . ? B20 B16 B15 60.0(6) . . ? C4 B17 B21 60.5(6) . . ? C4 B17 B22 104.5(9) . . ? B21 B17 B22 57.9(7) . . ? C4 B17 B18 104.8(8) . . ? B21 B17 B18 106.5(9) . . ? B22 B17 B18 59.6(7) . . ? C4 B17 B13 59.6(6) . . ? B21 B17 B13 109.4(9) . . ? B22 B17 B13 107.5(9) . . ? B18 B17 B13 59.4(6) . . ? B22 B18 B13 109.3(8) . . ? B22 B18 B17 60.4(7) . . ? B13 B18 B17 61.0(6) . . ? B22 B18 B19 58.9(7) . . ? B13 B18 B19 109.6(8) . . ? B17 B18 B19 108.1(9) . . ? B22 B18 B14 107.7(9) . . ? B13 B18 B14 59.6(6) . . ? B17 B18 B14 108.0(8) . . ? B19 B18 B14 61.2(7) . . ? B22 B19 B20 60.0(8) . . ? B22 B19 B18 60.1(8) . . ? B20 B19 B18 108.5(10) . . ? B22 B19 B15 107.4(9) . . ? B20 B19 B15 60.3(7) . . ? B18 B19 B15 107.2(8) . . ? B22 B19 B14 107.8(9) . . ? B20 B19 B14 108.1(8) . . ? B18 B19 B14 60.1(7) . . ? B15 B19 B14 59.0(6) . . ? B22 B20 B19 59.4(7) . . ? B22 B20 B21 58.0(7) . . ? B19 B20 B21 106.1(10) . . ? B22 B20 B16 105.4(9) . . ? B19 B20 B16 107.8(8) . . ? B21 B20 B16 59.0(6) . . ? B22 B20 B15 107.5(9) . . ? B19 B20 B15 61.1(7) . . ? B21 B20 B15 106.8(8) . . ? B16 B20 B15 59.9(6) . . ? B22 B21 C4 105.7(9) . . ? B22 B21 B17 61.9(7) . . ? C4 B21 B17 58.0(6) . . ? B22 B21 B16 109.5(10) . . ? C4 B21 B16 58.6(6) . . ? B17 B21 B16 108.3(8) . . ? B22 B21 B20 60.6(7) . . ? C4 B21 B20 106.4(9) . . ? B17 B21 B20 110.7(9) . . ? B16 B21 B20 61.5(7) . . ? B21 B22 B19 109.7(9) . . ? B21 B22 B20 61.4(7) . . ? B19 B22 B20 60.6(7) . . ? B21 B22 B18 108.6(8) . . ? B19 B22 B18 61.0(7) . . ? B20 B22 B18 109.7(9) . . ? B21 B22 B17 60.2(7) . . ? B19 B22 B17 109.5(9) . . ? B20 B22 B17 110.0(8) . . ? B18 B22 B17 60.0(7) . . ? C2 C1 B3 62.6(6) . . ? C2 C1 B4 111.0(8) . . ? B3 C1 B4 61.8(7) . . ? C2 C1 B6 60.8(6) . . ? B3 C1 B6 114.0(9) . . ? B4 C1 B6 112.5(8) . . ? C2 C1 B5 109.8(8) . . ? B3 C1 B5 112.5(8) . . ? B4 C1 B5 61.4(6) . . ? B6 C1 B5 61.6(6) . . ? C2 C1 Se1 119.1(6) . . ? B3 C1 Se1 120.3(6) . . ? B4 C1 Se1 122.6(7) . . ? B6 C1 Se1 115.2(7) . . ? B5 C1 Se1 119.5(7) . . ? C1 C2 B11 111.4(9) . . ? C1 C2 B7 111.0(8) . . ? B11 C2 B7 64.4(7) . . ? C1 C2 B6 62.0(6) . . ? B11 C2 B6 61.8(7) . . ? B7 C2 B6 115.1(8) . . ? C1 C2 B3 60.1(6) . . ? B11 C2 B3 113.9(8) . . ? B7 C2 B3 61.7(7) . . ? B6 C2 B3 112.9(8) . . ? C1 C2 Se2 117.0(6) . . ? B11 C2 Se2 121.6(7) . . ? B7 C2 Se2 120.8(8) . . ? B6 C2 Se2 116.9(6) . . ? B3 C2 Se2 117.5(6) . . ? C24 C19 C20 119.3(9) . . ? C24 C19 P1 117.8(7) . . ? C20 C19 P1 122.4(8) . . ? C21 C20 C19 117.5(11) . . ? C22 C21 C20 123.4(12) . . ? C21 C22 C23 120.3(12) . . ? C24 C23 C22 120.1(12) . . ? C23 C24 C19 119.4(10) . . ? C26 C25 C30 119.6(10) . . ? C26 C25 P1 122.1(8) . . ? C30 C25 P1 118.1(8) . . ? C25 C26 C27 119.8(12) . . ? C28 C27 C26 120.4(14) . . ? C29 C28 C27 119.6(13) . . ? C28 C29 C30 120.1(13) . . ? C29 C30 C25 120.4(11) . . ? C36 C31 C32 119.3(9) . . ? C36 C31 P1 121.0(8) . . ? C32 C31 P1 119.6(9) . . ? C33 C32 C31 118.3(11) . . ? C34 C33 C32 121.3(12) . . ? C33 C34 C35 121.0(12) . . ? C36 C35 C34 118.3(12) . . ? C35 C36 C31 121.8(11) . . ? C5 C9 C8 109.4(12) . . ? C5 C9 C10 126.9(14) . . ? C8 C9 C10 123.5(15) . . ? C5 C9 Rh1 70.0(7) . . ? C8 C9 Rh1 73.0(7) . . ? C10 C9 Rh1 127.5(7) . . ? C9 C5 C6 108.5(10) . . ? C9 C5 Rh1 74.8(6) . . ? C6 C5 Rh1 68.9(5) . . ? C7 C6 C5 103.2(11) . . ? C7 C6 Rh1 73.5(6) . . ? C5 C6 Rh1 71.7(5) . . ? C8 C7 C6 110.3(13) . . ? C8 C7 Rh1 74.6(8) . . ? C6 C7 Rh1 69.0(6) . . ? C7 C8 C9 108.5(14) . . ? C7 C8 Rh1 70.1(8) . . ? C9 C8 Rh1 71.7(7) . . ? C11 C10 C9 110.2(11) . . ? O1 C11 C10 111.5(12) . . ? O1 C12 C13 121.1(14) . . ? C12 C13 C14 113.5(10) . . ? C15 C14 C18 107.6(11) . . ? C15 C14 C13 125.1(11) . . ? C18 C14 C13 127.3(13) . . ? C15 C14 Rh2 70.4(6) . . ? C18 C14 Rh2 69.2(6) . . ? C13 C14 Rh2 128.0(7) . . ? C14 C15 C16 111.2(11) . . ? C14 C15 Rh2 74.2(6) . . ? C16 C15 Rh2 69.1(7) . . ? C17 C16 C15 106.1(13) . . ? C17 C16 Rh2 70.4(7) . . ? C15 C16 Rh2 74.7(7) . . ? C16 C17 C18 108.5(12) . . ? C16 C17 Rh2 72.1(7) . . ? C18 C17 Rh2 73.3(6) . . ? C14 C18 C17 106.6(11) . . ? C14 C18 Rh2 75.1(6) . . ? C17 C18 Rh2 68.3(6) . . ? C38 C37 C42 117.5(10) . . ? C38 C37 P2 120.1(9) . . ? C42 C37 P2 122.1(10) . . ? C39 C38 C37 122.8(12) . . ? C38 C39 C40 120.7(13) . . ? C41 C40 C39 118.2(13) . . ? C40 C41 C42 122.6(12) . . ? C37 C42 C41 118.1(12) . . ? C44 C43 C48 117.6(10) . . ? C44 C43 P2 122.7(9) . . ? C48 C43 P2 119.8(10) . . ? C43 C44 C45 122.6(11) . . ? C46 C45 C44 119.4(13) . . ? C47 C46 C45 120.2(13) . . ? C46 C47 C48 120.3(12) . . ? C43 C48 C47 119.9(12) . . ? C50 C49 C54 119.8(10) . . ? C50 C49 P2 122.3(9) . . ? C54 C49 P2 117.9(9) . . ? C49 C50 C51 119.0(12) . . ? C52 C51 C50 119.8(14) . . ? C51 C52 C53 120.3(14) . . ? C52 C53 C54 122.1(14) . . ? C53 C54 C49 119.0(12) . . ? C4 C3 B16 61.4(6) . . ? C4 C3 B13 62.3(6) . . ? B16 C3 B13 114.5(8) . . ? C4 C3 B14 111.0(7) . . ? B16 C3 B14 113.0(7) . . ? B13 C3 B14 61.8(6) . . ? C4 C3 B15 110.9(7) . . ? B16 C3 B15 62.1(6) . . ? B13 C3 B15 113.1(7) . . ? B14 C3 B15 61.7(6) . . ? C4 C3 Se3 121.4(6) . . ? B16 C3 Se3 117.2(6) . . ? B13 C3 Se3 119.2(6) . . ? B14 C3 Se3 119.4(6) . . ? B15 C3 Se3 117.9(7) . . ? C3 C4 B17 113.0(7) . . ? C3 C4 B16 62.4(6) . . ? B17 C4 B16 113.8(8) . . ? C3 C4 B21 111.1(8) . . ? B17 C4 B21 61.5(6) . . ? B16 C4 B21 61.5(6) . . ? C3 C4 B13 62.1(5) . . ? B17 C4 B13 63.3(6) . . ? B16 C4 B13 115.1(7) . . ? B21 C4 B13 113.4(8) . . ? C3 C4 Se4 117.1(6) . . ? B17 C4 Se4 119.0(7) . . ? B16 C4 Se4 119.0(6) . . ? B21 C4 Se4 123.3(7) . . ? B13 C4 Se4 114.5(6) . . ? Cl2 C55 Cl1 121.4(15) . . ? Cl4 C56 Cl3 124.3(19) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.516 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.102 # Attachment 'complex 9.cif' data_f51210a _database_code_depnum_ccdc_archive 'CCDC 616738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H46 I4 O P2 Rh2' _chemical_formula_weight 1438.23 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 8.080(3) _cell_length_b 17.147(6) _cell_length_c 17.467(6) _cell_angle_alpha 90.537(5) _cell_angle_beta 94.058(5) _cell_angle_gamma 93.095(5) _cell_volume 2410.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2.531 _cell_measurement_theta_max 23.776 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 3.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7306 _exptl_absorpt_correction_T_max 0.8504 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 5.97 _diffrn_reflns_number 10148 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8386 _reflns_number_gt 4584 _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^)+(0.0739P)^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 8386 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 Rh1 Rh 0.49496(11) 0.22556(6) 0.18869(5) 0.0516(3) Uani 1 1 d . . . Rh2 Rh -0.14717(10) -0.19390(5) 0.24357(5) 0.0456(3) Uani 1 1 d . . . P1 P 0.6442(4) 0.34413(17) 0.18901(17) 0.0490(8) Uani 1 1 d . . . P2 P -0.2757(4) -0.19653(17) 0.35713(16) 0.0441(7) Uani 1 1 d . . . O1 O 0.1632(14) -0.0271(7) 0.0673(6) 0.107(3) Uani 1 1 d . . . I1 I 0.77592(10) 0.14814(5) 0.19915(5) 0.0598(3) Uani 1 1 d . . . I2 I 0.46591(11) 0.23943(5) 0.33963(5) 0.0654(3) Uani 1 1 d . . . I3 I -0.13191(12) -0.34890(5) 0.24149(5) 0.0739(3) Uani 1 1 d . . . I4 I -0.43512(10) -0.19801(6) 0.15584(5) 0.0706(3) Uani 1 1 d . . . C5 C 0.352(2) 0.1247(9) 0.1261(11) 0.084(5) Uani 1 1 d . . . C1 C 0.4048(17) 0.1811(9) 0.0758(8) 0.074(4) Uani 1 1 d . . . H1 H 0.4748 0.1719 0.0334 0.088 Uiso 1 1 calc R . . C2 C 0.3304(19) 0.2511(9) 0.0897(9) 0.082(5) Uani 1 1 d . . . H2 H 0.3358 0.2982 0.0585 0.098 Uiso 1 1 calc R . . C3 C 0.2365(17) 0.2390(10) 0.1549(10) 0.083(5) Uani 1 1 d . . . H3 H 0.1639 0.2760 0.1769 0.099 Uiso 1 1 calc R . . C4 C 0.2525(18) 0.1583(13) 0.1762(9) 0.097(6) Uani 1 1 d . . . H4 H 0.1971 0.1316 0.2175 0.116 Uiso 1 1 calc R . . C6 C 0.398(2) 0.0376(9) 0.1296(10) 0.122(7) Uani 1 1 d . . . H6A H 0.5178 0.0353 0.1346 0.146 Uiso 1 1 calc R . . H6B H 0.3539 0.0137 0.1746 0.146 Uiso 1 1 calc R . . C7 C 0.3299(19) -0.0077(10) 0.0590(11) 0.117(7) Uani 1 1 d . . . H7A H 0.3419 0.0238 0.0137 0.140 Uiso 1 1 calc R . . H7B H 0.3900 -0.0546 0.0535 0.140 Uiso 1 1 calc R . . C10 C -0.0055(14) -0.1335(8) 0.1551(7) 0.058(3) Uani 1 1 d . . . C11 C 0.0947(14) -0.1832(8) 0.1935(7) 0.064(3) Uani 1 1 d . . . H11 H 0.1500 -0.2260 0.1701 0.077 Uiso 1 1 calc R . . C12 C 0.1078(14) -0.1629(9) 0.2728(6) 0.063(4) Uani 1 1 d . . . H12 H 0.1790 -0.1866 0.3129 0.076 Uiso 1 1 calc R . . C13 C 0.0223(17) -0.0965(8) 0.2804(8) 0.067(4) Uani 1 1 d . . . H13 H 0.0181 -0.0662 0.3280 0.081 Uiso 1 1 calc R . . C14 C -0.0534(16) -0.0792(7) 0.2123(8) 0.064(4) Uani 1 1 d . . . H14 H -0.1207 -0.0340 0.2021 0.077 Uiso 1 1 calc R . . C9 C -0.0485(16) -0.1288(8) 0.0695(8) 0.077(4) Uani 1 1 d . . . H9A H -0.0879 -0.1800 0.0497 0.093 Uiso 1 1 calc R . . H9B H -0.1371 -0.0934 0.0600 0.093 Uiso 1 1 calc R . . C8 C 0.099(2) -0.1007(10) 0.0288(9) 0.111(6) Uani 1 1 d . . . H8A H 0.1833 -0.1391 0.0320 0.133 Uiso 1 1 calc R . . H8B H 0.0676 -0.0918 -0.0248 0.133 Uiso 1 1 calc R . . C15 C 0.7851(16) 0.3541(7) 0.1121(6) 0.056(3) Uani 1 1 d . . . C16 C 0.752(2) 0.3129(8) 0.0453(7) 0.079(4) Uani 1 1 d . . . H16 H 0.6595 0.2782 0.0395 0.095 Uiso 1 1 calc R . . C17 C 0.856(2) 0.3222(9) -0.0140(8) 0.091(5) Uani 1 1 d . . . H17 H 0.8319 0.2934 -0.0592 0.109 Uiso 1 1 calc R . . C18 C 0.990(2) 0.3722(10) -0.0074(9) 0.090(5) Uani 1 1 d . . . H18 H 1.0588 0.3772 -0.0478 0.108 Uiso 1 1 calc R . . C19 C 1.0252(19) 0.4144(11) 0.0560(10) 0.098(5) Uani 1 1 d . . . H19 H 1.1170 0.4497 0.0601 0.118 Uiso 1 1 calc R . . C20 C 0.9223(18) 0.4051(9) 0.1170(8) 0.080(4) Uani 1 1 d . . . H20 H 0.9476 0.4343 0.1618 0.095 Uiso 1 1 calc R . . C21 C 0.7754(14) 0.3759(7) 0.2740(6) 0.049(3) Uani 1 1 d . . . C22 C 0.9129(16) 0.3362(7) 0.2994(7) 0.065(4) Uani 1 1 d . . . H22 H 0.9327 0.2901 0.2740 0.078 Uiso 1 1 calc R . . C23 C 1.0233(16) 0.3608(8) 0.3605(7) 0.068(4) Uani 1 1 d . . . H23 H 1.1164 0.3333 0.3748 0.082 Uiso 1 1 calc R . . C24 C 0.9890(19) 0.4270(8) 0.3985(7) 0.078(4) Uani 1 1 d . . . H24 H 1.0600 0.4447 0.4400 0.094 Uiso 1 1 calc R . . C25 C 0.854(2) 0.4682(8) 0.3777(8) 0.091(5) Uani 1 1 d . . . H25 H 0.8331 0.5128 0.4053 0.109 Uiso 1 1 calc R . . C26 C 0.7487(16) 0.4437(7) 0.3157(7) 0.072(4) Uani 1 1 d . . . H26 H 0.6580 0.4727 0.3012 0.086 Uiso 1 1 calc R . . C27 C 0.5070(16) 0.4243(7) 0.1750(7) 0.058(3) Uani 1 1 d . . . C28 C 0.5346(17) 0.4834(8) 0.1244(8) 0.071(4) Uani 1 1 d . . . H28 H 0.6210 0.4806 0.0922 0.085 Uiso 1 1 calc R . . C29 C 0.437(2) 0.5467(8) 0.1203(9) 0.084(4) Uani 1 1 d . . . H29 H 0.4557 0.5864 0.0855 0.101 Uiso 1 1 calc R . . C30 C 0.311(2) 0.5496(9) 0.1690(10) 0.086(5) Uani 1 1 d . . . H30 H 0.2463 0.5929 0.1683 0.103 Uiso 1 1 calc R . . C31 C 0.2787(19) 0.4914(8) 0.2173(8) 0.078(4) Uani 1 1 d . . . H31 H 0.1901 0.4944 0.2482 0.094 Uiso 1 1 calc R . . C32 C 0.3726(16) 0.4282(8) 0.2223(7) 0.067(4) Uani 1 1 d . . . H32 H 0.3492 0.3883 0.2562 0.080 Uiso 1 1 calc R . . C33 C -0.1182(13) -0.1832(7) 0.4375(6) 0.045(3) Uani 1 1 d . . . C34 C 0.0055(15) -0.2366(7) 0.4481(6) 0.056(3) Uani 1 1 d . . . H34 H 0.0081 -0.2777 0.4132 0.067 Uiso 1 1 calc R . . C35 C 0.1212(15) -0.2300(8) 0.5073(7) 0.063(3) Uani 1 1 d . . . H35 H 0.2036 -0.2658 0.5130 0.075 Uiso 1 1 calc R . . C36 C 0.1159(17) -0.1699(10) 0.5592(8) 0.083(4) Uani 1 1 d . . . H36 H 0.1941 -0.1660 0.6010 0.099 Uiso 1 1 calc R . . C37 C -0.0024(17) -0.1151(9) 0.5510(7) 0.079(4) Uani 1 1 d . . . H37 H -0.0032 -0.0739 0.5859 0.095 Uiso 1 1 calc R . . C38 C -0.1210(15) -0.1231(8) 0.4891(7) 0.065(4) Uani 1 1 d . . . H38 H -0.2027 -0.0870 0.4828 0.078 Uiso 1 1 calc R . . C39 C -0.4164(13) -0.1179(6) 0.3677(6) 0.040(3) Uani 1 1 d . . . C40 C -0.3987(15) -0.0513(7) 0.3271(7) 0.058(3) Uani 1 1 d . . . H40 H -0.3203 -0.0485 0.2906 0.070 Uiso 1 1 calc R . . C41 C -0.4917(17) 0.0120(7) 0.3375(7) 0.068(4) Uani 1 1 d . . . H41 H -0.4749 0.0575 0.3099 0.081 Uiso 1 1 calc R . . C42 C -0.6121(15) 0.0062(8) 0.3910(8) 0.066(4) Uani 1 1 d . . . H42 H -0.6784 0.0479 0.3986 0.079 Uiso 1 1 calc R . . C43 C -0.6324(15) -0.0592(8) 0.4314(7) 0.061(3) Uani 1 1 d . . . H43 H -0.7138 -0.0627 0.4664 0.073 Uiso 1 1 calc R . . C44 C -0.5344(15) -0.1215(7) 0.4218(7) 0.059(3) Uani 1 1 d . . . H44 H -0.5473 -0.1658 0.4515 0.071 Uiso 1 1 calc R . . C45 C -0.4013(14) -0.2803(6) 0.3855(6) 0.043(3) Uani 1 1 d . . . C46 C -0.3738(17) -0.3184(8) 0.4558(7) 0.069(4) Uani 1 1 d . . . H46 H -0.2829 -0.3020 0.4888 0.083 Uiso 1 1 calc R . . C47 C -0.478(2) -0.3793(9) 0.4772(9) 0.098(5) Uani 1 1 d . . . H47 H -0.4529 -0.4049 0.5229 0.117 Uiso 1 1 calc R . . C48 C -0.618(2) -0.4030(9) 0.4326(9) 0.095(5) Uani 1 1 d . . . H48 H -0.6912 -0.4427 0.4477 0.113 Uiso 1 1 calc R . . C49 C -0.6433(19) -0.3666(9) 0.3670(10) 0.091(5) Uani 1 1 d . . . H49 H -0.7369 -0.3824 0.3355 0.109 Uiso 1 1 calc R . . C50 C -0.5425(19) -0.3075(8) 0.3423(8) 0.079(4) Uani 1 1 d . . . H50 H -0.5693 -0.2849 0.2952 0.095 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 Rh1 0.0431(6) 0.0574(6) 0.0534(6) -0.0051(5) -0.0050(4) 0.0057(4) Rh2 0.0390(5) 0.0580(6) 0.0397(5) -0.0082(4) 0.0014(4) 0.0058(4) P1 0.0485(19) 0.0492(18) 0.0487(19) -0.0050(15) -0.0057(14) 0.0100(14) P2 0.0452(18) 0.0504(18) 0.0370(17) -0.0036(14) 0.0029(13) 0.0061(14) O1 0.090(9) 0.107(8) 0.124(9) -0.015(7) 0.017(7) -0.014(7) I1 0.0481(5) 0.0588(5) 0.0727(6) -0.0053(4) 0.0026(4) 0.0088(4) I2 0.0682(6) 0.0714(6) 0.0584(6) 0.0004(4) 0.0084(4) 0.0157(4) I3 0.0819(7) 0.0615(6) 0.0795(7) -0.0172(5) 0.0070(5) 0.0157(5) I4 0.0487(5) 0.1053(7) 0.0558(5) 0.0035(5) -0.0091(4) 0.0019(5) C5 0.068(11) 0.078(11) 0.100(13) -0.010(10) -0.038(9) -0.011(9) C1 0.072(10) 0.086(11) 0.060(9) -0.021(9) -0.024(7) 0.011(9) C2 0.077(11) 0.084(11) 0.077(11) -0.014(9) -0.045(9) 0.012(9) C3 0.045(9) 0.095(13) 0.108(14) -0.017(10) -0.012(8) 0.019(8) C4 0.036(9) 0.161(19) 0.085(12) -0.008(13) -0.017(8) -0.038(10) C6 0.136(16) 0.071(11) 0.142(16) -0.031(11) -0.087(13) 0.002(10) C7 0.056(11) 0.097(13) 0.20(2) 0.030(13) -0.008(11) -0.002(9) C10 0.040(7) 0.086(10) 0.047(8) 0.005(7) 0.009(6) -0.001(7) C11 0.038(7) 0.088(10) 0.068(9) -0.005(8) 0.011(6) 0.005(7) C12 0.034(7) 0.111(12) 0.041(8) -0.004(7) -0.008(5) -0.004(7) C13 0.067(10) 0.075(10) 0.057(9) -0.019(8) 0.004(7) -0.022(8) C14 0.055(9) 0.051(8) 0.088(11) -0.001(7) 0.028(8) -0.001(6) C9 0.045(8) 0.091(11) 0.095(11) -0.001(9) 0.015(7) -0.022(7) C8 0.139(17) 0.105(13) 0.084(12) -0.033(10) 0.010(11) -0.038(12) C15 0.078(10) 0.050(7) 0.040(7) 0.000(6) 0.007(6) 0.003(7) C16 0.122(13) 0.060(9) 0.056(9) -0.001(7) 0.012(9) -0.002(8) C17 0.146(17) 0.070(10) 0.061(10) -0.008(8) 0.043(10) -0.005(10) C18 0.091(13) 0.105(13) 0.078(12) 0.009(10) 0.014(9) 0.022(10) C19 0.062(11) 0.144(16) 0.085(12) -0.011(12) -0.013(9) -0.005(10) C20 0.075(11) 0.106(12) 0.054(9) 0.000(8) -0.008(8) -0.014(9) C21 0.047(7) 0.064(8) 0.036(7) -0.007(6) 0.000(5) -0.001(6) C22 0.070(10) 0.059(8) 0.066(9) -0.005(7) -0.002(7) 0.002(7) C23 0.060(9) 0.085(10) 0.055(8) 0.007(8) -0.015(7) -0.010(7) C24 0.106(13) 0.069(10) 0.053(9) -0.014(8) -0.020(8) -0.016(9) C25 0.124(14) 0.066(10) 0.077(10) -0.034(8) -0.034(10) 0.016(9) C26 0.072(10) 0.064(9) 0.078(10) -0.010(8) -0.014(7) 0.020(7) C27 0.079(10) 0.049(8) 0.046(8) -0.007(6) -0.010(6) 0.009(7) C28 0.076(10) 0.063(9) 0.075(10) -0.008(8) 0.001(7) 0.012(7) C29 0.108(14) 0.062(10) 0.084(11) 0.013(8) -0.003(10) 0.017(9) C30 0.086(12) 0.061(10) 0.110(14) -0.037(10) -0.023(10) 0.034(8) C31 0.099(12) 0.051(9) 0.083(11) -0.011(8) 0.000(8) 0.008(8) C32 0.066(9) 0.067(9) 0.070(9) -0.006(7) 0.002(7) 0.025(7) C33 0.035(6) 0.068(8) 0.032(6) -0.005(6) 0.006(5) 0.006(6) C34 0.063(8) 0.064(8) 0.041(7) -0.008(6) -0.004(6) 0.013(6) C35 0.050(8) 0.090(10) 0.048(8) 0.002(7) -0.004(6) 0.015(7) C36 0.047(9) 0.131(14) 0.069(10) 0.006(10) -0.009(7) 0.003(9) C37 0.070(10) 0.114(12) 0.052(9) -0.035(8) -0.005(7) 0.008(9) C38 0.049(8) 0.087(10) 0.060(8) -0.019(7) 0.006(6) 0.021(7) C39 0.045(7) 0.046(7) 0.030(6) -0.001(5) -0.001(5) 0.003(5) C40 0.061(8) 0.060(8) 0.057(8) -0.009(7) 0.015(6) 0.018(6) C41 0.087(10) 0.048(8) 0.072(9) 0.014(7) 0.022(8) 0.017(7) C42 0.055(9) 0.063(9) 0.080(10) -0.021(8) 0.009(7) 0.017(7) C43 0.057(9) 0.064(9) 0.066(9) -0.005(7) 0.025(6) 0.008(7) C44 0.056(8) 0.062(8) 0.058(8) -0.009(7) 0.002(6) -0.001(6) C45 0.053(7) 0.043(6) 0.032(6) -0.013(5) 0.000(5) -0.004(5) C46 0.066(9) 0.072(9) 0.066(10) 0.011(8) -0.005(7) -0.006(7) C47 0.120(15) 0.081(11) 0.087(12) 0.035(10) -0.004(11) -0.027(10) C48 0.146(18) 0.077(11) 0.062(11) -0.003(9) 0.029(11) -0.016(11) C49 0.074(11) 0.088(12) 0.105(14) -0.023(10) 0.010(9) -0.043(9) C50 0.088(12) 0.082(11) 0.069(10) -0.005(8) 0.006(8) 0.016(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C3 2.155(13) . ? Rh1 C2 2.168(12) . ? Rh1 C1 2.170(12) . ? Rh1 C4 2.214(13) . ? Rh1 C5 2.258(14) . ? Rh1 P1 2.307(3) . ? Rh1 I2 2.6730(16) . ? Rh1 I1 2.6872(14) . ? Rh2 C12 2.125(11) . ? Rh2 C14 2.158(12) . ? Rh2 C13 2.164(12) . ? Rh2 C11 2.197(12) . ? Rh2 C10 2.218(12) . ? Rh2 P2 2.303(3) . ? Rh2 I3 2.6672(16) . ? Rh2 I4 2.6912(14) . ? P1 C27 1.820(12) . ? P1 C21 1.824(11) . ? P1 C15 1.824(12) . ? P2 C45 1.808(11) . ? P2 C39 1.826(11) . ? P2 C33 1.831(10) . ? O1 C7 1.388(16) . ? O1 C8 1.476(16) . ? C5 C4 1.37(2) . ? C5 C1 1.384(19) . ? C5 C6 1.56(2) . ? C1 C2 1.397(18) . ? C1 H1 0.9800 . ? C2 C3 1.42(2) . ? C2 H2 0.9800 . ? C3 C4 1.45(2) . ? C3 H3 0.9800 . ? C4 H4 0.9800 . ? C6 C7 1.50(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C10 C11 1.355(16) . ? C10 C14 1.447(16) . ? C10 C9 1.514(17) . ? C11 C12 1.420(16) . ? C11 H11 0.9800 . ? C12 C13 1.373(17) . ? C12 H12 0.9800 . ? C13 C14 1.342(17) . ? C13 H13 0.9800 . ? C14 H14 0.9800 . ? C9 C8 1.492(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C15 C16 1.361(16) . ? C15 C20 1.372(17) . ? C16 C17 1.381(18) . ? C16 H16 0.9300 . ? C17 C18 1.34(2) . ? C17 H17 0.9300 . ? C18 C19 1.322(19) . ? C18 H18 0.9300 . ? C19 C20 1.402(19) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.383(15) . ? C21 C26 1.400(15) . ? C22 C23 1.389(16) . ? C22 H22 0.9300 . ? C23 C24 1.361(17) . ? C23 H23 0.9300 . ? C24 C25 1.360(19) . ? C24 H24 0.9300 . ? C25 C26 1.377(16) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.370(16) . ? C27 C32 1.414(17) . ? C28 C29 1.376(18) . ? C28 H28 0.9300 . ? C29 C30 1.38(2) . ? C29 H29 0.9300 . ? C30 C31 1.339(19) . ? C30 H30 0.9300 . ? C31 C32 1.356(17) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.366(15) . ? C33 C34 1.395(15) . ? C34 C35 1.344(15) . ? C34 H34 0.9300 . ? C35 C36 1.372(18) . ? C35 H35 0.9300 . ? C36 C37 1.377(18) . ? C36 H36 0.9300 . ? C37 C38 1.394(16) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.356(15) . ? C39 C44 1.389(15) . ? C40 C41 1.371(15) . ? C40 H40 0.9300 . ? C41 C42 1.395(17) . ? C41 H41 0.9300 . ? C42 C43 1.339(16) . ? C42 H42 0.9300 . ? C43 C44 1.379(15) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C50 1.380(17) . ? C45 C46 1.405(15) . ? C46 C47 1.378(18) . ? C46 H46 0.9300 . ? C47 C48 1.37(2) . ? C47 H47 0.9300 . ? C48 C49 1.32(2) . ? C48 H48 0.9300 . ? C49 C50 1.358(19) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? 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 C3 Rh1 C2 38.5(5) . . ? C3 Rh1 C1 63.2(6) . . ? C2 Rh1 C1 37.6(5) . . ? C3 Rh1 C4 38.6(6) . . ? C2 Rh1 C4 63.2(6) . . ? C1 Rh1 C4 61.4(6) . . ? C3 Rh1 C5 62.2(6) . . ? C2 Rh1 C5 61.8(5) . . ? C1 Rh1 C5 36.4(5) . . ? C4 Rh1 C5 35.7(5) . . ? C3 Rh1 P1 111.0(5) . . ? C2 Rh1 P1 94.9(4) . . ? C1 Rh1 P1 114.8(5) . . ? C4 Rh1 P1 149.3(6) . . ? C5 Rh1 P1 151.2(5) . . ? C3 Rh1 I2 96.0(5) . . ? C2 Rh1 I2 132.4(5) . . ? C1 Rh1 I2 151.2(5) . . ? C4 Rh1 I2 89.9(4) . . ? C5 Rh1 I2 117.5(5) . . ? P1 Rh1 I2 90.46(8) . . ? C3 Rh1 I1 154.3(4) . . ? C2 Rh1 I1 130.6(5) . . ? C1 Rh1 I1 96.5(4) . . ? C4 Rh1 I1 119.1(6) . . ? C5 Rh1 I1 92.1(4) . . ? P1 Rh1 I1 91.32(8) . . ? I2 Rh1 I1 96.40(4) . . ? C12 Rh2 C14 62.3(5) . . ? C12 Rh2 C13 37.3(5) . . ? C14 Rh2 C13 36.2(4) . . ? C12 Rh2 C11 38.3(4) . . ? C14 Rh2 C11 61.7(5) . . ? C13 Rh2 C11 61.9(5) . . ? C12 Rh2 C10 62.7(4) . . ? C14 Rh2 C10 38.6(4) . . ? C13 Rh2 C10 62.2(5) . . ? C11 Rh2 C10 35.7(4) . . ? C12 Rh2 P2 106.4(3) . . ? C14 Rh2 P2 114.1(4) . . ? C13 Rh2 P2 93.4(4) . . ? C11 Rh2 P2 144.2(3) . . ? C10 Rh2 P2 152.5(3) . . ? C12 Rh2 I3 98.8(4) . . ? C14 Rh2 I3 150.8(3) . . ? C13 Rh2 I3 135.1(4) . . ? C11 Rh2 I3 89.5(4) . . ? C10 Rh2 I3 114.1(3) . . ? P2 Rh2 I3 91.86(8) . . ? C12 Rh2 I4 156.0(3) . . ? C14 Rh2 I4 97.9(4) . . ? C13 Rh2 I4 130.7(4) . . ? C11 Rh2 I4 121.8(3) . . ? C10 Rh2 I4 93.4(3) . . ? P2 Rh2 I4 93.84(8) . . ? I3 Rh2 I4 93.26(4) . . ? C27 P1 C21 102.5(5) . . ? C27 P1 C15 104.7(6) . . ? C21 P1 C15 103.1(6) . . ? C27 P1 Rh1 111.2(4) . . ? C21 P1 Rh1 119.8(4) . . ? C15 P1 Rh1 114.0(4) . . ? C45 P2 C39 101.5(5) . . ? C45 P2 C33 102.9(5) . . ? C39 P2 C33 105.3(5) . . ? C45 P2 Rh2 122.3(3) . . ? C39 P2 Rh2 113.9(4) . . ? C33 P2 Rh2 109.3(3) . . ? C7 O1 C8 114.8(13) . . ? C4 C5 C1 108.6(15) . . ? C4 C5 C6 124(2) . . ? C1 C5 C6 127.5(18) . . ? C4 C5 Rh1 70.4(8) . . ? C1 C5 Rh1 68.3(8) . . ? C6 C5 Rh1 125.5(9) . . ? C5 C1 C2 109.8(15) . . ? C5 C1 Rh1 75.3(8) . . ? C2 C1 Rh1 71.1(7) . . ? C5 C1 H1 125.0 . . ? C2 C1 H1 125.0 . . ? Rh1 C1 H1 125.0 . . ? C1 C2 C3 106.9(14) . . ? C1 C2 Rh1 71.3(7) . . ? C3 C2 Rh1 70.3(8) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? Rh1 C2 H2 126.5 . . ? C2 C3 C4 106.4(14) . . ? C2 C3 Rh1 71.3(8) . . ? C4 C3 Rh1 72.9(8) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? Rh1 C3 H3 126.6 . . ? C5 C4 C3 108.1(16) . . ? C5 C4 Rh1 73.9(8) . . ? C3 C4 Rh1 68.5(8) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? Rh1 C4 H4 125.9 . . ? C7 C6 C5 111.7(13) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? O1 C7 C6 107.8(16) . . ? O1 C7 H7A 110.1 . . ? C6 C7 H7A 110.1 . . ? O1 C7 H7B 110.1 . . ? C6 C7 H7B 110.1 . . ? H7A C7 H7B 108.5 . . ? C11 C10 C14 105.8(11) . . ? C11 C10 C9 128.6(12) . . ? C14 C10 C9 125.4(12) . . ? C11 C10 Rh2 71.3(7) . . ? C14 C10 Rh2 68.5(6) . . ? C9 C10 Rh2 128.9(8) . . ? C10 C11 C12 109.2(12) . . ? C10 C11 Rh2 73.0(7) . . ? C12 C11 Rh2 68.1(6) . . ? C10 C11 H11 125.4 . . ? C12 C11 H11 125.4 . . ? Rh2 C11 H11 125.4 . . ? C13 C12 C11 106.8(11) . . ? C13 C12 Rh2 72.9(7) . . ? C11 C12 Rh2 73.6(6) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? Rh2 C12 H12 126.2 . . ? C14 C13 C12 109.4(12) . . ? C14 C13 Rh2 71.7(7) . . ? C12 C13 Rh2 69.8(7) . . ? C14 C13 H13 125.3 . . ? C12 C13 H13 125.3 . . ? Rh2 C13 H13 125.3 . . ? C13 C14 C10 108.6(12) . . ? C13 C14 Rh2 72.2(8) . . ? C10 C14 Rh2 73.0(7) . . ? C13 C14 H14 125.6 . . ? C10 C14 H14 125.6 . . ? Rh2 C14 H14 125.6 . . ? C8 C9 C10 110.9(11) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.0 . . ? O1 C8 C9 106.6(12) . . ? O1 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? O1 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? C16 C15 C20 117.2(12) . . ? C16 C15 P1 120.3(11) . . ? C20 C15 P1 122.4(10) . . ? C15 C16 C17 120.5(14) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 121.0(15) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 120.6(16) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.1(16) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C15 C20 C19 121.7(13) . . ? C15 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C26 115.6(10) . . ? C22 C21 P1 121.7(9) . . ? C26 C21 P1 122.6(9) . . ? C21 C22 C23 124.1(12) . . ? C21 C22 H22 118.0 . . ? C23 C22 H22 118.0 . . ? C24 C23 C22 117.0(13) . . ? C24 C23 H23 121.5 . . ? C22 C23 H23 121.5 . . ? C25 C24 C23 122.1(12) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 119.9(13) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 121.3(12) . . ? C25 C26 H26 119.3 . . ? C21 C26 H26 119.3 . . ? C28 C27 C32 118.9(12) . . ? C28 C27 P1 122.9(10) . . ? C32 C27 P1 118.1(10) . . ? C27 C28 C29 121.2(14) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 118.2(15) . . ? C30 C29 H29 120.9 . . ? C28 C29 H29 120.9 . . ? C31 C30 C29 121.5(14) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 121.5(15) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C31 C32 C27 118.7(14) . . ? C31 C32 H32 120.7 . . ? C27 C32 H32 120.7 . . ? C38 C33 C34 118.7(10) . . ? C38 C33 P2 121.5(9) . . ? C34 C33 P2 119.8(8) . . ? C35 C34 C33 121.7(11) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C34 C35 C36 119.0(12) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C35 C36 C37 121.6(12) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C36 C37 C38 118.3(12) . . ? C36 C37 H37 120.8 . . ? C38 C37 H37 120.8 . . ? C33 C38 C37 120.6(12) . . ? C33 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C40 C39 C44 118.0(10) . . ? C40 C39 P2 120.4(8) . . ? C44 C39 P2 121.3(9) . . ? C39 C40 C41 122.8(11) . . ? C39 C40 H40 118.6 . . ? C41 C40 H40 118.6 . . ? C40 C41 C42 118.1(12) . . ? C40 C41 H41 121.0 . . ? C42 C41 H41 121.0 . . ? C43 C42 C41 120.2(12) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 121.0(12) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C43 C44 C39 119.9(12) . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? C50 C45 C46 114.4(11) . . ? C50 C45 P2 121.8(10) . . ? C46 C45 P2 123.5(9) . . ? C47 C46 C45 121.7(13) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C48 C47 C46 121.4(15) . . ? C48 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C49 C48 C47 116.4(15) . . ? C49 C48 H48 121.8 . . ? C47 C48 H48 121.8 . . ? C48 C49 C50 124.7(16) . . ? C48 C49 H49 117.7 . . ? C50 C49 H49 117.7 . . ? C49 C50 C45 121.4(14) . . ? C49 C50 H50 119.3 . . ? C45 C50 H50 119.3 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.195 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.171