# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peter Brueggeller' _publ_contact_author_email PETER.BRUEGGELLER@UIBK.AC.AT _publ_section_title ; Regio- and chemoselective oxidation of the bis(bidentate) phosphine cis,trans,cis-1,2,3,4-tetrakis(diphenylphosphino)cyclobutane via cobalt(II) mediated dioxygen activation ; loop_ _publ_author_name 'Peter Brueggeller' 'Christian Bachmann' 'Sylvia Eller' 'Markus Fessler' 'Rene Gutmann' ; H.Kopacka ; 'Thomas Mueller' 'Barbara Trettenbrein' # Attachment 'CIF_Filerevised2.cif' #============================================================================= data_2a _database_code_depnum_ccdc_archive 'CCDC 691862' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2Cl4(2,3-trans-dppcbO2)]' _chemical_name_common (Co2Cl4(2,3-trans-dppcbO2)) _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cl4 Co2 O2 P4, 2(C H2 Cl2)' _chemical_formula_sum 'C54 H48 Cl8 Co2 O2 P4' _chemical_formula_weight 1254.312 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' Cl Cl 0.1484 0.1585 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.0368(5) _cell_length_b 21.9990(7) _cell_length_c 13.8403(4) _cell_angle_alpha 90.00 _cell_angle_beta 120.209(1) _cell_angle_gamma 90.00 _cell_volume 5535.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 25392 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.022 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.705 _exptl_absorpt_process_details 'Otwinowski et al, 1997' _diffrn_ambient_temperature 223(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 'Kappa CCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9313 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.96 _reflns_number_total 5423 _reflns_number_gt 2251 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.0786P)^2^+31.7231P] 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 5280 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 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 0.58642(4) 0.20336(3) 0.54444(5) 0.0414(2) Uani 1 1 d . . . Cl1 Cl 0.69093(7) 0.19487(7) 0.53822(12) 0.0560(4) Uani 1 1 d . . . Cl2 Cl 0.59277(8) 0.21004(7) 0.70916(10) 0.0549(4) Uani 1 1 d . . . P1 P 0.45422(6) 0.13997(5) 0.34497(9) 0.0303(3) Uani 1 1 d . . . P2 P 0.51209(6) 0.28918(5) 0.41767(9) 0.0341(3) Uani 1 1 d . . . O1 O 0.52317(17) 0.13565(14) 0.4562(3) 0.0384(7) Uani 1 1 d . . . C1 C 0.4634(2) 0.19198(18) 0.2510(3) 0.0275(8) Uani 1 1 d . . . H1 H 0.4225 0.1843 0.1742 0.033 Uiso 1 1 calc R . . C2 C 0.4713(2) 0.26228(18) 0.2706(3) 0.0264(8) Uani 1 1 d . . . H2 H 0.4256 0.2844 0.2189 0.032 Uiso 1 1 calc R . . C11 C 0.4299(2) 0.0662(2) 0.2804(4) 0.0352(9) Uani 1 1 d . . . C12 C 0.3753(3) 0.0580(2) 0.1702(4) 0.0485(12) Uani 1 1 d . . . H12 H 0.3530 0.0918 0.1236 0.058 Uiso 1 1 calc R . . C13 C 0.3540(3) -0.0003(3) 0.1293(5) 0.0619(15) Uani 1 1 d . . . H13 H 0.3175 -0.0061 0.0541 0.074 Uiso 1 1 calc R . . C14 C 0.3857(4) -0.0501(3) 0.1975(5) 0.0640(16) Uani 1 1 d . . . H14 H 0.3694 -0.0895 0.1698 0.077 Uiso 1 1 calc R . . C15 C 0.4407(4) -0.0421(2) 0.3051(5) 0.0596(15) Uani 1 1 d . . . H15 H 0.4635 -0.0761 0.3507 0.071 Uiso 1 1 calc R . . C16 C 0.4635(3) 0.0158(2) 0.3480(4) 0.0456(11) Uani 1 1 d . . . H16 H 0.5015 0.0211 0.4224 0.055 Uiso 1 1 calc R . . C21 C 0.3782(2) 0.16627(19) 0.3572(4) 0.0329(9) Uani 1 1 d . . . C22 C 0.3854(3) 0.1703(2) 0.4632(4) 0.0393(10) Uani 1 1 d . . . H22 H 0.4303 0.1608 0.5276 0.047 Uiso 1 1 calc R . . C23 C 0.3253(3) 0.1884(2) 0.4721(4) 0.0465(12) Uani 1 1 d . . . H23 H 0.3298 0.1913 0.5430 0.056 Uiso 1 1 calc R . . C24 C 0.2602(3) 0.2020(2) 0.3796(5) 0.0491(13) Uani 1 1 d . . . H24 H 0.2200 0.2141 0.3871 0.059 Uiso 1 1 calc R . . C25 C 0.2521(3) 0.1983(2) 0.2727(5) 0.0494(12) Uani 1 1 d . . . H25 H 0.2069 0.2079 0.2089 0.059 Uiso 1 1 calc R . . C26 C 0.3109(3) 0.1805(2) 0.2625(4) 0.0438(11) Uani 1 1 d . . . H26 H 0.3059 0.1779 0.1912 0.053 Uiso 1 1 calc R . . C31 C 0.4360(3) 0.3158(2) 0.4345(4) 0.0359(9) Uani 1 1 d . . . C32 C 0.3665(3) 0.3292(3) 0.3479(5) 0.0482(12) Uani 1 1 d . . . H32 H 0.3545 0.3219 0.2737 0.058 Uiso 1 1 calc R . . C33 C 0.3141(3) 0.3537(3) 0.3699(6) 0.0593(15) Uani 1 1 d . . . H33 H 0.2670 0.3635 0.3105 0.071 Uiso 1 1 calc R . . C34 C 0.3310(4) 0.3635(3) 0.4783(6) 0.0616(16) Uani 1 1 d . . . H34 H 0.2955 0.3798 0.4932 0.074 Uiso 1 1 calc R . . C35 C 0.4000(4) 0.3492(3) 0.5650(5) 0.0630(16) Uani 1 1 d . . . H35 H 0.4115 0.3562 0.6391 0.076 Uiso 1 1 calc R . . C36 C 0.4531(3) 0.3248(2) 0.5449(4) 0.0488(12) Uani 1 1 d . . . H36 H 0.4998 0.3144 0.6046 0.059 Uiso 1 1 calc R . . C41 C 0.5580(2) 0.3598(2) 0.4196(4) 0.0366(10) Uani 1 1 d . . . C42 C 0.6314(3) 0.3578(2) 0.4470(4) 0.0469(12) Uani 1 1 d . . . H42 H 0.6569 0.3206 0.4658 0.056 Uiso 1 1 calc R . . C43 C 0.6669(3) 0.4109(3) 0.4464(5) 0.0588(15) Uani 1 1 d . . . H43 H 0.7159 0.4093 0.4622 0.071 Uiso 1 1 calc R . . C44 C 0.6318(3) 0.4646(3) 0.4234(5) 0.0638(16) Uani 1 1 d . . . H44 H 0.6570 0.5003 0.4253 0.077 Uiso 1 1 calc R . . C45 C 0.5579(4) 0.4681(3) 0.3965(6) 0.0693(17) Uani 1 1 d . . . H45 H 0.5336 0.5058 0.3805 0.083 Uiso 1 1 calc R . . C46 C 0.5217(3) 0.4156(3) 0.3942(5) 0.0569(14) Uani 1 1 d . . . H46 H 0.4721 0.4174 0.3753 0.068 Uiso 1 1 calc R . . Cl3 Cl 0.12568(18) 0.06506(16) 0.2043(2) 0.1323(10) Uani 1 1 d . . . Cl4 Cl 0.26882(19) 0.0087(3) 0.3269(3) 0.194(2) Uani 1 1 d . . . C3 C 0.1993(10) 0.0265(9) 0.2107(10) 0.207(8) Uani 1 1 d . . . H3A H 0.1799 -0.0113 0.1683 0.248 Uiso 1 1 calc R . . H3B H 0.2172 0.0510 0.1701 0.248 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 0.0459(4) 0.0442(4) 0.0394(4) -0.0124(3) 0.0254(3) -0.0115(3) Cl1 0.0465(7) 0.0702(9) 0.0538(8) -0.0157(6) 0.0270(6) -0.0054(6) Cl2 0.0653(8) 0.0641(9) 0.0370(6) -0.0091(5) 0.0271(6) -0.0119(6) P1 0.0372(6) 0.0279(5) 0.0296(5) 0.0032(4) 0.0196(5) -0.0015(4) P2 0.0357(6) 0.0404(6) 0.0324(6) -0.0099(5) 0.0217(5) -0.0039(5) O1 0.0445(17) 0.0317(16) 0.0349(16) -0.0020(13) 0.0169(14) -0.0068(13) C1 0.033(2) 0.028(2) 0.0276(19) 0.0023(16) 0.0197(17) 0.0002(16) C2 0.032(2) 0.027(2) 0.0264(19) 0.0023(15) 0.0188(17) 0.0010(16) C11 0.044(2) 0.030(2) 0.037(2) -0.0004(18) 0.025(2) -0.0049(18) C12 0.052(3) 0.042(3) 0.040(3) 0.001(2) 0.014(2) 0.002(2) C13 0.067(4) 0.049(3) 0.046(3) -0.011(2) 0.011(3) -0.010(3) C14 0.074(4) 0.038(3) 0.069(4) -0.014(3) 0.027(3) -0.011(3) C15 0.084(4) 0.029(3) 0.063(4) 0.007(2) 0.035(3) 0.003(3) C16 0.060(3) 0.036(3) 0.039(2) 0.005(2) 0.023(2) -0.004(2) C21 0.042(2) 0.028(2) 0.036(2) 0.0033(17) 0.0252(19) -0.0014(17) C22 0.051(3) 0.038(2) 0.034(2) 0.0036(19) 0.026(2) 0.000(2) C23 0.063(3) 0.047(3) 0.048(3) 0.007(2) 0.043(3) 0.004(2) C24 0.057(3) 0.048(3) 0.062(3) 0.013(2) 0.044(3) 0.011(2) C25 0.045(3) 0.057(3) 0.049(3) 0.015(2) 0.025(2) 0.013(2) C26 0.046(3) 0.055(3) 0.034(2) 0.008(2) 0.023(2) 0.002(2) C31 0.044(2) 0.032(2) 0.044(2) -0.0048(19) 0.031(2) 0.0007(19) C32 0.048(3) 0.054(3) 0.055(3) -0.004(2) 0.035(3) 0.001(2) C33 0.050(3) 0.060(4) 0.083(4) 0.002(3) 0.044(3) 0.008(3) C34 0.073(4) 0.048(3) 0.102(5) -0.012(3) 0.072(4) -0.001(3) C35 0.089(5) 0.061(4) 0.071(4) -0.015(3) 0.064(4) -0.005(3) C36 0.062(3) 0.051(3) 0.048(3) -0.006(2) 0.039(3) 0.001(2) C41 0.042(2) 0.034(2) 0.039(2) -0.0139(19) 0.024(2) -0.0112(19) C42 0.045(3) 0.049(3) 0.054(3) -0.015(2) 0.030(2) -0.011(2) C43 0.046(3) 0.061(4) 0.072(4) -0.016(3) 0.033(3) -0.017(3) C44 0.065(4) 0.056(4) 0.075(4) -0.010(3) 0.038(3) -0.024(3) C45 0.073(4) 0.043(3) 0.094(5) -0.004(3) 0.044(4) -0.007(3) C46 0.053(3) 0.052(3) 0.073(4) -0.011(3) 0.037(3) -0.012(3) Cl3 0.146(2) 0.152(3) 0.113(2) 0.0127(18) 0.0752(18) -0.014(2) Cl4 0.117(2) 0.366(7) 0.119(2) 0.024(3) 0.074(2) -0.015(3) C3 0.28(2) 0.243(19) 0.086(8) -0.014(10) 0.087(11) 0.045(16) _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 O1 1.961(3) . ? Co1 Cl2 2.2204(14) . ? Co1 Cl1 2.2509(15) . ? Co1 P2 2.5154(15) . ? P1 O1 1.495(3) . ? P1 C21 1.786(4) . ? P1 C11 1.798(4) . ? P1 C1 1.813(4) . ? P2 C41 1.822(4) . ? P2 C31 1.826(4) . ? P2 C2 1.863(4) . ? C1 C1 1.555(8) 2_655 ? C1 C2 1.564(6) . ? C1 H1 0.9900 . ? C2 C2 1.575(7) 2_655 ? C2 H2 0.9900 . ? C11 C12 1.384(7) . ? C11 C16 1.391(7) . ? C12 C13 1.383(7) . ? C12 H12 0.9400 . ? C13 C14 1.380(9) . ? C13 H13 0.9400 . ? C14 C15 1.361(8) . ? C14 H14 0.9400 . ? C15 C16 1.386(7) . ? C15 H15 0.9400 . ? C16 H16 0.9400 . ? C21 C26 1.397(6) . ? C21 C22 1.401(6) . ? C22 C23 1.388(7) . ? C22 H22 0.9400 . ? C23 C24 1.357(8) . ? C23 H23 0.9400 . ? C24 C25 1.404(7) . ? C24 H24 0.9400 . ? C25 C26 1.370(7) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? C31 C32 1.377(7) . ? C31 C36 1.396(7) . ? C32 C33 1.392(7) . ? C32 H32 0.9400 . ? C33 C34 1.373(9) . ? C33 H33 0.9400 . ? C34 C35 1.377(9) . ? C34 H34 0.9400 . ? C35 C36 1.387(8) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? C41 C42 1.394(7) . ? C41 C46 1.395(8) . ? C42 C43 1.388(8) . ? C42 H42 0.9400 . ? C43 C44 1.344(9) . ? C43 H43 0.9400 . ? C44 C45 1.408(9) . ? C44 H44 0.9400 . ? C45 C46 1.375(8) . ? C45 H45 0.9400 . ? C46 H46 0.9400 . ? Cl3 C3 1.729(17) . ? Cl4 C3 1.584(15) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 Cl2 111.19(10) . . ? O1 Co1 Cl1 106.42(11) . . ? Cl2 Co1 Cl1 119.31(7) . . ? O1 Co1 P2 98.44(10) . . ? Cl2 Co1 P2 111.20(6) . . ? Cl1 Co1 P2 108.17(6) . . ? O1 P1 C21 111.99(19) . . ? O1 P1 C11 109.9(2) . . ? C21 P1 C11 107.2(2) . . ? O1 P1 C1 112.33(18) . . ? C21 P1 C1 106.65(19) . . ? C11 P1 C1 108.63(19) . . ? C41 P2 C31 102.5(2) . . ? C41 P2 C2 103.66(19) . . ? C31 P2 C2 106.8(2) . . ? C41 P2 Co1 119.39(16) . . ? C31 P2 Co1 115.39(15) . . ? C2 P2 Co1 107.86(13) . . ? P1 O1 Co1 126.57(19) . . ? C1 C1 C2 89.1(2) 2_655 . ? C1 C1 P1 118.5(3) 2_655 . ? C2 C1 P1 122.7(3) . . ? C1 C1 H1 108.3 2_655 . ? C2 C1 H1 108.3 . . ? P1 C1 H1 108.3 . . ? C1 C2 C2 88.34(19) . 2_655 ? C1 C2 P2 117.0(3) . . ? C2 C2 P2 112.3(3) 2_655 . ? C1 C2 H2 112.4 . . ? C2 C2 H2 112.4 2_655 . ? P2 C2 H2 112.4 . . ? C12 C11 C16 119.7(4) . . ? C12 C11 P1 122.4(4) . . ? C16 C11 P1 117.6(4) . . ? C13 C12 C11 119.4(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.9(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 119.7(5) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C26 C21 C22 119.5(4) . . ? C26 C21 P1 121.1(3) . . ? C22 C21 P1 119.3(3) . . ? C23 C22 C21 119.2(4) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 120.8(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.6(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 119.3(5) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C21 120.5(4) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C32 C31 C36 119.9(4) . . ? C32 C31 P2 124.9(3) . . ? C36 C31 P2 115.2(4) . . ? C31 C32 C33 120.2(5) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 120.1(6) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.8(5) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 121.0(5) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 119.0(5) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 120.5 . . ? C42 C41 C46 119.2(4) . . ? C42 C41 P2 119.0(4) . . ? C46 C41 P2 121.9(4) . . ? C43 C42 C41 119.9(5) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C42 120.5(5) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 120.9(5) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C46 C45 C44 119.0(6) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C45 C46 C41 120.5(5) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? Cl4 C3 Cl3 121.2(8) . . ? Cl4 C3 H3A 107.0 . . ? Cl3 C3 H3A 107.0 . . ? Cl4 C3 H3B 107.0 . . ? Cl3 C3 H3B 107.0 . . ? H3A C3 H3B 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 P2 C41 -153.74(19) . . . . ? Cl2 Co1 P2 C41 89.55(17) . . . . ? Cl1 Co1 P2 C41 -43.29(17) . . . . ? O1 Co1 P2 C31 83.35(19) . . . . ? Cl2 Co1 P2 C31 -33.36(18) . . . . ? Cl1 Co1 P2 C31 -166.19(17) . . . . ? O1 Co1 P2 C2 -35.95(16) . . . . ? Cl2 Co1 P2 C2 -152.66(13) . . . . ? Cl1 Co1 P2 C2 74.51(14) . . . . ? C21 P1 O1 Co1 -76.9(3) . . . . ? C11 P1 O1 Co1 164.1(2) . . . . ? C1 P1 O1 Co1 43.1(3) . . . . ? Cl2 Co1 O1 P1 119.0(2) . . . . ? Cl1 Co1 O1 P1 -109.6(2) . . . . ? P2 Co1 O1 P1 2.3(2) . . . . ? O1 P1 C1 C1 40.4(4) . . . 2_655 ? C21 P1 C1 C1 163.4(3) . . . 2_655 ? C11 P1 C1 C1 -81.4(4) . . . 2_655 ? O1 P1 C1 C2 -68.6(4) . . . . ? C21 P1 C1 C2 54.4(4) . . . . ? C11 P1 C1 C2 169.6(3) . . . . ? C1 C1 C2 C2 17.1(4) 2_655 . . 2_655 ? P1 C1 C2 C2 140.9(3) . . . 2_655 ? C1 C1 C2 P2 -97.2(3) 2_655 . . . ? P1 C1 C2 P2 26.6(4) . . . . ? C41 P2 C2 C1 149.6(3) . . . . ? C31 P2 C2 C1 -102.5(3) . . . . ? Co1 P2 C2 C1 22.1(3) . . . . ? C41 P2 C2 C2 49.6(2) . . . 2_655 ? C31 P2 C2 C2 157.50(19) . . . 2_655 ? Co1 P2 C2 C2 -77.89(14) . . . 2_655 ? O1 P1 C11 C12 -169.8(4) . . . . ? C21 P1 C11 C12 68.4(4) . . . . ? C1 P1 C11 C12 -46.5(5) . . . . ? O1 P1 C11 C16 15.9(4) . . . . ? C21 P1 C11 C16 -106.0(4) . . . . ? C1 P1 C11 C16 139.1(4) . . . . ? C16 C11 C12 C13 1.1(8) . . . . ? P1 C11 C12 C13 -173.1(4) . . . . ? C11 C12 C13 C14 1.0(9) . . . . ? C12 C13 C14 C15 -2.7(10) . . . . ? C13 C14 C15 C16 2.2(10) . . . . ? C14 C15 C16 C11 -0.1(9) . . . . ? C12 C11 C16 C15 -1.6(8) . . . . ? P1 C11 C16 C15 172.9(4) . . . . ? O1 P1 C21 C26 172.2(4) . . . . ? C11 P1 C21 C26 -67.2(4) . . . . ? C1 P1 C21 C26 49.0(4) . . . . ? O1 P1 C21 C22 -10.5(4) . . . . ? C11 P1 C21 C22 110.1(4) . . . . ? C1 P1 C21 C22 -133.7(4) . . . . ? C26 C21 C22 C23 -0.1(7) . . . . ? P1 C21 C22 C23 -177.4(4) . . . . ? C21 C22 C23 C24 0.2(7) . . . . ? C22 C23 C24 C25 -0.2(8) . . . . ? C23 C24 C25 C26 0.2(8) . . . . ? C24 C25 C26 C21 -0.1(8) . . . . ? C22 C21 C26 C25 0.0(7) . . . . ? P1 C21 C26 C25 177.3(4) . . . . ? C41 P2 C31 C32 92.0(5) . . . . ? C2 P2 C31 C32 -16.7(5) . . . . ? Co1 P2 C31 C32 -136.5(4) . . . . ? C41 P2 C31 C36 -85.4(4) . . . . ? C2 P2 C31 C36 166.0(4) . . . . ? Co1 P2 C31 C36 46.1(4) . . . . ? C36 C31 C32 C33 2.2(8) . . . . ? P2 C31 C32 C33 -175.0(4) . . . . ? C31 C32 C33 C34 -1.2(9) . . . . ? C32 C33 C34 C35 0.3(9) . . . . ? C33 C34 C35 C36 -0.3(9) . . . . ? C34 C35 C36 C31 1.3(9) . . . . ? C32 C31 C36 C35 -2.2(8) . . . . ? P2 C31 C36 C35 175.3(4) . . . . ? C31 P2 C41 C42 158.2(4) . . . . ? C2 P2 C41 C42 -90.8(4) . . . . ? Co1 P2 C41 C42 29.2(4) . . . . ? C31 P2 C41 C46 -22.0(5) . . . . ? C2 P2 C41 C46 89.1(4) . . . . ? Co1 P2 C41 C46 -151.0(4) . . . . ? C46 C41 C42 C43 -1.3(7) . . . . ? P2 C41 C42 C43 178.5(4) . . . . ? C41 C42 C43 C44 2.3(9) . . . . ? C42 C43 C44 C45 -1.7(10) . . . . ? C43 C44 C45 C46 0.1(10) . . . . ? C44 C45 C46 C41 0.9(10) . . . . ? C42 C41 C46 C45 -0.3(8) . . . . ? P2 C41 C46 C45 179.9(5) . . . . ? _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction 0.980 _refine_diff_density_max 1.110 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.070 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 691863' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2Br4(2,3-trans-dppcbO2)]' _chemical_name_common (Co2Br4(2,3-trans-dppcbO2)) _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Br4 Co2 O2 P4, 2(C H Cl3)' _chemical_formula_sum 'C54 H46 Br4 Cl6 Co2 O2 P4' _chemical_formula_weight 1501.01 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.145(5) _cell_length_b 23.251(4) _cell_length_c 13.880(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.84(1) _cell_angle_gamma 90.00 _cell_volume 5919(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 3.679 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.130 _exptl_absorpt_correction_T_max 0.229 _exptl_absorpt_process_details 'Empirical Absorption Corrections' _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7361 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6520 _reflns_number_gt 1932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Software of the Siemens P4' _computing_data_reduction 'Software of the Siemens P4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.0835P)^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 6520 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _refine_ls_shift/su_max 0.065 _refine_ls_shift/su_mean 0.008 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 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 0.08419(8) 0.29928(7) 0.54316(11) 0.0337(4) Uani 1 1 d . . . Br1 Br 0.19541(7) 0.30628(7) 0.54082(11) 0.0665(5) Uani 1 1 d . . . Br2 Br 0.09044(7) 0.29513(7) 0.71670(9) 0.0555(4) Uani 1 1 d . . . P1 P -0.04662(18) 0.35960(13) 0.3451(2) 0.0349(8) Uani 1 1 d . . . P2 P 0.01144(16) 0.21783(12) 0.4160(2) 0.0290(7) Uani 1 1 d . . . O1 O 0.0216(4) 0.3631(3) 0.4565(6) 0.044(2) Uani 1 1 d . . . C1 C -0.0368(5) 0.3119(4) 0.2505(8) 0.029(3) Uani 1 1 d . . . H1A H -0.0775 0.3181 0.1775 0.080 Uiso 1 1 d R . . C2 C -0.0275(5) 0.2446(4) 0.2728(8) 0.024(2) Uani 1 1 d . . . H2A H -0.0756 0.2286 0.2312 0.080 Uiso 1 1 d R . . C11 C -0.0702(8) 0.4299(5) 0.2841(10) 0.051(4) Uani 1 1 d . . . C12 C -0.0363(9) 0.4779(5) 0.3506(12) 0.070(5) Uani 1 1 d . . . H12A H 0.0027 0.4726 0.4232 0.084 Uiso 1 1 calc R . . C13 C -0.0588(10) 0.5320(6) 0.3119(13) 0.081(6) Uani 1 1 d . . . H13A H -0.0344 0.5640 0.3567 0.097 Uiso 1 1 calc R . . C14 C -0.1164(13) 0.5399(8) 0.2088(19) 0.115(7) Uani 1 1 d . . . H14A H -0.1353 0.5770 0.1850 0.138 Uiso 1 1 calc R . . C15 C -0.1478(11) 0.4933(9) 0.1379(16) 0.111(7) Uani 1 1 d . . . H15A H -0.1845 0.4993 0.0639 0.134 Uiso 1 1 calc R . . C16 C -0.1248(10) 0.4382(8) 0.1764(13) 0.089(6) Uani 1 1 d . . . H16A H -0.1465 0.4065 0.1292 0.107 Uiso 1 1 calc R . . C21 C -0.1226(6) 0.3341(5) 0.3578(9) 0.032(3) Uani 1 1 d . . . C22 C -0.1904(7) 0.3206(5) 0.2589(9) 0.040(3) Uani 1 1 d . . . H22A H -0.1941 0.3228 0.1887 0.048 Uiso 1 1 calc R . . C23 C -0.2488(6) 0.3047(5) 0.2684(9) 0.038(3) Uani 1 1 d . . . H23A H -0.2939 0.2976 0.2044 0.045 Uiso 1 1 calc R . . C24 C -0.2418(7) 0.2990(5) 0.3719(10) 0.046(3) Uani 1 1 d . . . H24A H -0.2820 0.2870 0.3781 0.056 Uiso 1 1 calc R . . C25 C -0.1779(7) 0.3105(5) 0.4649(9) 0.046(3) Uani 1 1 d . . . H25A H -0.1747 0.3059 0.5344 0.056 Uiso 1 1 calc R . . C26 C -0.1168(6) 0.3290(5) 0.4609(9) 0.033(3) Uani 1 1 d . . . H26A H -0.0731 0.3377 0.5262 0.040 Uiso 1 1 calc R . . C31 C -0.0639(6) 0.1944(5) 0.4359(8) 0.032(3) Uani 1 1 d . . . C32 C -0.1340(6) 0.1825(5) 0.3509(9) 0.034(3) Uani 1 1 d . . . H32A H -0.1463 0.1900 0.2771 0.041 Uiso 1 1 calc R . . C33 C -0.1851(6) 0.1603(5) 0.3722(11) 0.043(3) Uani 1 1 d . . . H33A H -0.2318 0.1514 0.3133 0.052 Uiso 1 1 calc R . . C34 C -0.1683(8) 0.1505(6) 0.4810(13) 0.061(4) Uani 1 1 d . . . H34A H -0.2044 0.1372 0.4962 0.073 Uiso 1 1 calc R . . C35 C -0.0974(8) 0.1606(6) 0.5682(11) 0.049(3) Uani 1 1 d . . . H35A H -0.0847 0.1520 0.6418 0.059 Uiso 1 1 calc R . . C36 C -0.0464(7) 0.1835(5) 0.5441(9) 0.039(3) Uani 1 1 d . . . H36A H 0.0008 0.1917 0.6023 0.046 Uiso 1 1 calc R . . C41 C 0.0537(6) 0.1494(5) 0.4155(8) 0.034(3) Uani 1 1 d . . . C42 C 0.0158(7) 0.0982(6) 0.3890(10) 0.044(3) Uani 1 1 d . . . H42A H -0.0337 0.0984 0.3688 0.053 Uiso 1 1 calc R . . C43 C 0.0490(8) 0.0467(7) 0.3914(13) 0.074(5) Uani 1 1 d . . . H43A H 0.0231 0.0119 0.3752 0.088 Uiso 1 1 calc R . . C44 C 0.1210(8) 0.0477(6) 0.4182(11) 0.055(4) Uani 1 1 d . . . H44A H 0.1442 0.0129 0.4200 0.066 Uiso 1 1 calc R . . C45 C 0.1589(7) 0.0968(6) 0.4417(10) 0.053(4) Uani 1 1 d . . . H45A H 0.2077 0.0960 0.4580 0.063 Uiso 1 1 calc R . . C46 C 0.1270(7) 0.1488(5) 0.4424(9) 0.037(3) Uani 1 1 d . . . H46A H 0.1540 0.1831 0.4607 0.044 Uiso 1 1 calc R . . Cl1 Cl 0.1130(3) 0.0785(2) 0.7041(4) 0.1088(17) Uani 1 1 d . . . Cl2 Cl 0.1706(3) -0.02677(17) 0.6720(4) 0.0955(15) Uani 1 1 d . . . Cl3 Cl 0.2627(3) 0.04588(19) 0.8561(4) 0.1072(18) Uani 1 1 d . . . C3 C 0.1893(9) 0.0435(6) 0.7166(13) 0.070(5) Uani 1 1 d . . . H3A H 0.2046 0.0636 0.6713 0.080 Uiso 1 1 d 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 0.0328(8) 0.0320(9) 0.0353(7) 0.0091(8) 0.0162(7) 0.0012(8) Br1 0.0446(8) 0.0936(13) 0.0579(8) 0.0237(9) 0.0230(7) -0.0055(9) Br2 0.0573(9) 0.0665(10) 0.0384(6) 0.0039(7) 0.0206(6) -0.0031(8) P1 0.0460(19) 0.0234(18) 0.0382(15) -0.0073(14) 0.0232(15) 0.0007(16) P2 0.0303(16) 0.0275(18) 0.0347(14) 0.0058(13) 0.0203(13) -0.0028(14) O1 0.048(5) 0.036(5) 0.055(5) 0.001(4) 0.031(4) 0.000(4) C1 0.030(6) 0.033(7) 0.027(5) -0.002(5) 0.016(5) 0.001(5) C2 0.022(6) 0.011(6) 0.034(5) 0.003(5) 0.009(5) -0.002(5) C11 0.094(11) 0.013(7) 0.059(8) 0.002(6) 0.048(8) 0.003(7) C12 0.123(14) 0.024(8) 0.061(9) -0.008(7) 0.045(9) 0.002(9) C13 0.112(15) 0.022(9) 0.069(10) 0.009(7) 0.014(10) 0.018(9) C14 0.15(2) 0.054(13) 0.143(19) 0.021(13) 0.072(17) 0.038(14) C15 0.126(18) 0.070(14) 0.089(13) 0.007(12) 0.016(12) 0.009(13) C16 0.103(14) 0.086(14) 0.067(10) 0.024(10) 0.035(10) 0.027(11) C21 0.037(7) 0.022(6) 0.042(6) -0.007(5) 0.025(6) 0.008(6) C22 0.055(8) 0.038(8) 0.038(6) -0.001(6) 0.032(6) 0.001(7) C23 0.039(7) 0.030(7) 0.037(6) -0.009(6) 0.013(5) 0.009(7) C24 0.054(8) 0.035(8) 0.068(8) -0.018(7) 0.044(7) -0.010(7) C25 0.066(9) 0.041(8) 0.043(7) 0.007(6) 0.036(7) 0.020(8) C26 0.034(7) 0.025(7) 0.043(6) 0.000(5) 0.023(6) 0.009(6) C31 0.036(6) 0.024(7) 0.042(6) 0.004(5) 0.024(5) 0.006(6) C32 0.024(6) 0.029(7) 0.050(7) -0.011(5) 0.019(5) -0.002(6) C33 0.028(7) 0.039(8) 0.077(9) -0.011(7) 0.037(7) -0.006(6) C34 0.077(11) 0.050(10) 0.101(12) 0.000(9) 0.079(11) 0.013(8) C35 0.063(10) 0.051(9) 0.055(8) -0.007(7) 0.046(8) -0.005(8) C36 0.049(8) 0.036(8) 0.036(6) 0.003(5) 0.026(6) 0.003(6) C41 0.029(7) 0.042(8) 0.034(6) 0.016(5) 0.018(5) 0.007(6) C42 0.047(8) 0.030(8) 0.067(8) 0.011(7) 0.036(7) 0.010(7) C43 0.055(11) 0.055(11) 0.112(13) 0.015(9) 0.043(10) 0.011(9) C44 0.059(10) 0.036(9) 0.068(9) -0.006(7) 0.030(8) 0.003(8) C45 0.044(8) 0.062(10) 0.066(9) 0.014(8) 0.037(7) 0.001(8) C46 0.048(8) 0.005(6) 0.062(8) 0.005(5) 0.031(7) 0.006(6) Cl1 0.127(5) 0.068(3) 0.137(4) -0.014(3) 0.071(4) 0.002(3) Cl2 0.131(4) 0.049(3) 0.113(3) -0.014(2) 0.066(3) -0.015(3) Cl3 0.125(4) 0.070(3) 0.099(3) 0.006(3) 0.035(3) -0.038(3) C3 0.108(14) 0.043(9) 0.090(11) 0.001(8) 0.073(11) 0.005(10) _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 O1 1.953(8) . ? Co1 Br2 2.3477(19) . ? Co1 Br1 2.374(2) . ? Co1 P2 2.523(3) . ? P1 O1 1.503(8) . ? P1 C11 1.794(12) . ? P1 C1 1.809(10) . ? P1 C21 1.802(12) . ? P2 C2 1.840(9) . ? P2 C41 1.827(12) . ? P2 C31 1.829(11) . ? C1 C1 1.561(19) 2 ? C1 C2 1.588(14) . ? C1 H1A 0.9599 . ? C2 C2 1.58(2) 2 ? C2 H2A 0.9602 . ? C11 C16 1.374(18) . ? C11 C12 1.397(17) . ? C12 C13 1.359(18) . ? C12 H12A 0.9400 . ? C13 C14 1.35(2) . ? C13 H13A 0.9400 . ? C14 C15 1.39(2) . ? C14 H14A 0.9400 . ? C15 C16 1.38(2) . ? C15 H15A 0.9400 . ? C16 H16A 0.9400 . ? C21 C26 1.379(14) . ? C21 C22 1.442(15) . ? C22 C23 1.356(15) . ? C22 H22A 0.9400 . ? C23 C24 1.375(14) . ? C23 H23A 0.9400 . ? C24 C25 1.352(16) . ? C24 H24A 0.9400 . ? C25 C26 1.387(16) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C31 C36 1.380(14) . ? C31 C32 1.388(14) . ? C32 C33 1.356(15) . ? C32 H32A 0.9400 . ? C33 C34 1.387(17) . ? C33 H33A 0.9400 . ? C34 C35 1.400(17) . ? C34 H34A 0.9400 . ? C35 C36 1.384(16) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C41 C42 1.378(16) . ? C41 C46 1.401(15) . ? C42 C43 1.378(18) . ? C42 H42A 0.9400 . ? C43 C44 1.376(18) . ? C43 H43A 0.9400 . ? C44 C45 1.337(17) . ? C44 H44A 0.9400 . ? C45 C46 1.387(16) . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? Cl1 C3 1.736(15) . ? Cl2 C3 1.723(14) . ? Cl3 C3 1.781(16) . ? C3 H3A 0.9599 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 Br2 109.8(2) . . ? O1 Co1 Br1 108.2(2) . . ? Br2 Co1 Br1 117.81(7) . . ? O1 Co1 P2 98.6(2) . . ? Br2 Co1 P2 112.98(9) . . ? Br1 Co1 P2 107.77(10) . . ? O1 P1 C11 109.6(6) . . ? O1 P1 C1 112.4(5) . . ? C11 P1 C1 108.8(5) . . ? O1 P1 C21 111.3(5) . . ? C11 P1 C21 107.1(6) . . ? C1 P1 C21 107.5(5) . . ? C2 P2 C41 104.3(5) . . ? C2 P2 C31 108.0(5) . . ? C41 P2 C31 101.8(5) . . ? C2 P2 Co1 106.9(3) . . ? C41 P2 Co1 121.8(4) . . ? C31 P2 Co1 113.0(4) . . ? P1 O1 Co1 127.0(5) . . ? C1 C1 C2 88.6(5) 2 . ? C1 C1 P1 118.8(7) 2 . ? C2 C1 P1 120.7(7) . . ? C1 C1 H1A 111.4 2 . ? C2 C1 H1A 108.3 . . ? P1 C1 H1A 107.8 . . ? C2 C2 C1 88.0(5) 2 . ? C2 C2 P2 114.2(8) 2 . ? C1 C2 P2 119.3(7) . . ? C2 C2 H2A 122.0 2 . ? C1 C2 H2A 105.9 . . ? P2 C2 H2A 106.8 . . ? C16 C11 C12 118.9(13) . . ? C16 C11 P1 121.8(12) . . ? C12 C11 P1 119.0(10) . . ? C13 C12 C11 121.0(14) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C12 C13 C14 119.8(15) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C13 C14 C15 120.3(17) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 119.8(18) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C11 119.7(17) . . ? C15 C16 H16A 120.2 . . ? C11 C16 H16A 120.1 . . ? C26 C21 C22 120.1(11) . . ? C26 C21 P1 120.5(9) . . ? C22 C21 P1 119.4(8) . . ? C23 C22 C21 119.3(10) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C24 C23 C22 119.8(11) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C25 C24 C23 121.1(12) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 122.0(11) . . ? C24 C25 H25A 119.0 . . ? C26 C25 H25A 119.0 . . ? C21 C26 C25 117.7(10) . . ? C21 C26 H26A 121.2 . . ? C25 C26 H26A 121.2 . . ? C36 C31 C32 118.8(11) . . ? C36 C31 P2 116.0(8) . . ? C32 C31 P2 125.0(8) . . ? C33 C32 C31 121.4(11) . . ? C33 C32 H32A 119.3 . . ? C31 C32 H32A 119.3 . . ? C32 C33 C34 119.9(12) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C33 C34 C35 119.9(12) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C36 C35 C34 118.9(12) . . ? C36 C35 H35A 120.6 . . ? C34 C35 H35A 120.5 . . ? C35 C36 C31 121.0(11) . . ? C35 C36 H36A 119.5 . . ? C31 C36 H36A 119.5 . . ? C42 C41 C46 118.7(11) . . ? C42 C41 P2 122.2(9) . . ? C46 C41 P2 119.0(9) . . ? C43 C42 C41 121.5(12) . . ? C43 C42 H42A 119.3 . . ? C41 C42 H42A 119.3 . . ? C42 C43 C44 118.2(14) . . ? C42 C43 H43A 120.9 . . ? C44 C43 H43A 120.9 . . ? C45 C44 C43 121.9(14) . . ? C45 C44 H44A 119.1 . . ? C43 C44 H44A 119.1 . . ? C44 C45 C46 120.7(12) . . ? C44 C45 H45A 119.6 . . ? C46 C45 H45A 119.6 . . ? C45 C46 C41 118.9(11) . . ? C45 C46 H46A 120.5 . . ? C41 C46 H46A 120.5 . . ? Cl1 C3 Cl2 111.8(9) . . ? Cl1 C3 Cl3 111.0(8) . . ? Cl2 C3 Cl3 109.9(8) . . ? Cl1 C3 H3A 107.9 . . ? Cl2 C3 H3A 108.6 . . ? Cl3 C3 H3A 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 P2 C2 35.8(4) . . . . ? Br2 Co1 P2 C2 151.6(3) . . . . ? Br1 Co1 P2 C2 -76.5(3) . . . . ? O1 Co1 P2 C41 155.4(5) . . . . ? Br2 Co1 P2 C41 -88.8(4) . . . . ? Br1 Co1 P2 C41 43.1(4) . . . . ? O1 Co1 P2 C31 -82.8(4) . . . . ? Br2 Co1 P2 C31 32.9(4) . . . . ? Br1 Co1 P2 C31 164.9(4) . . . . ? C11 P1 O1 Co1 -164.5(6) . . . . ? C1 P1 O1 Co1 -43.4(7) . . . . ? C21 P1 O1 Co1 77.2(7) . . . . ? Br2 Co1 O1 P1 -120.8(5) . . . . ? Br1 Co1 O1 P1 109.4(5) . . . . ? P2 Co1 O1 P1 -2.6(6) . . . . ? O1 P1 C1 C1 -39.6(8) . . . 2 ? C11 P1 C1 C1 82.1(9) . . . 2 ? C21 P1 C1 C1 -162.4(7) . . . 2 ? O1 P1 C1 C2 67.5(9) . . . . ? C11 P1 C1 C2 -170.9(8) . . . . ? C21 P1 C1 C2 -55.3(9) . . . . ? C1 C1 C2 C2 -19.7(9) 2 . . 2 ? P1 C1 C2 C2 -142.7(8) . . . 2 ? C1 C1 C2 P2 97.2(9) 2 . . . ? P1 C1 C2 P2 -25.8(11) . . . . ? C41 P2 C2 C2 -50.4(6) . . . 2 ? C31 P2 C2 C2 -158.2(5) . . . 2 ? Co1 P2 C2 C2 79.9(4) . . . 2 ? C41 P2 C2 C1 -152.5(8) . . . . ? C31 P2 C2 C1 99.7(8) . . . . ? Co1 P2 C2 C1 -22.2(8) . . . . ? O1 P1 C11 C16 171.6(12) . . . . ? C1 P1 C11 C16 48.3(14) . . . . ? C21 P1 C11 C16 -67.6(14) . . . . ? O1 P1 C11 C12 -13.8(13) . . . . ? C1 P1 C11 C12 -137.1(11) . . . . ? C21 P1 C11 C12 107.0(12) . . . . ? C16 C11 C12 C13 3(2) . . . . ? P1 C11 C12 C13 -171.7(13) . . . . ? C11 C12 C13 C14 2(3) . . . . ? C12 C13 C14 C15 -7(3) . . . . ? C13 C14 C15 C16 6(3) . . . . ? C14 C15 C16 C11 -1(3) . . . . ? C12 C11 C16 C15 -3(3) . . . . ? P1 C11 C16 C15 171.2(15) . . . . ? O1 P1 C21 C26 9.9(10) . . . . ? C11 P1 C21 C26 -109.9(9) . . . . ? C1 P1 C21 C26 133.4(9) . . . . ? O1 P1 C21 C22 -171.8(8) . . . . ? C11 P1 C21 C22 68.5(10) . . . . ? C1 P1 C21 C22 -48.3(10) . . . . ? C26 C21 C22 C23 2.2(17) . . . . ? P1 C21 C22 C23 -176.1(9) . . . . ? C21 C22 C23 C24 -3.1(17) . . . . ? C22 C23 C24 C25 1.8(18) . . . . ? C23 C24 C25 C26 0.6(19) . . . . ? C22 C21 C26 C25 0.0(16) . . . . ? P1 C21 C26 C25 178.4(9) . . . . ? C24 C25 C26 C21 -1.5(17) . . . . ? C2 P2 C31 C36 -167.9(8) . . . . ? C41 P2 C31 C36 82.6(9) . . . . ? Co1 P2 C31 C36 -49.8(9) . . . . ? C2 P2 C31 C32 17.8(11) . . . . ? C41 P2 C31 C32 -91.7(10) . . . . ? Co1 P2 C31 C32 135.9(9) . . . . ? C36 C31 C32 C33 -0.4(17) . . . . ? P2 C31 C32 C33 173.8(9) . . . . ? C31 C32 C33 C34 1.9(18) . . . . ? C32 C33 C34 C35 -3.6(19) . . . . ? C33 C34 C35 C36 3.8(19) . . . . ? C34 C35 C36 C31 -2.3(18) . . . . ? C32 C31 C36 C35 0.6(17) . . . . ? P2 C31 C36 C35 -174.1(9) . . . . ? C2 P2 C41 C42 -88.8(10) . . . . ? C31 P2 C41 C42 23.4(10) . . . . ? Co1 P2 C41 C42 150.4(8) . . . . ? C2 P2 C41 C46 90.8(9) . . . . ? C31 P2 C41 C46 -156.9(8) . . . . ? Co1 P2 C41 C46 -30.0(10) . . . . ? C46 C41 C42 C43 1.8(18) . . . . ? P2 C41 C42 C43 -178.5(10) . . . . ? C41 C42 C43 C44 -2(2) . . . . ? C42 C43 C44 C45 0(2) . . . . ? C43 C44 C45 C46 1(2) . . . . ? C44 C45 C46 C41 -1.4(18) . . . . ? C42 C41 C46 C45 -0.2(16) . . . . ? P2 C41 C46 C45 -179.8(9) . . . . ? _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction 0.981 _refine_diff_density_max 1.430 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.110 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 691864' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2Br4(1,3-trans-dppcbO2)]' _chemical_name_common (Co2Br4(1,3-trans-dppcbO2)) _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Br4 Co2 O2 P4, C H Cl3' _chemical_formula_sum 'C53 H45 Br4 Cl3 Co2 O2 P4' _chemical_formula_weight 1381.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.930(5) _cell_length_b 13.128(6) _cell_length_c 17.295(6) _cell_angle_alpha 106.56(1) _cell_angle_beta 103.09(1) _cell_angle_gamma 92.33(1) _cell_volume 2723.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1366 _exptl_absorpt_coefficient_mu 3.849 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.129 _exptl_absorpt_correction_T_max 0.150 _exptl_absorpt_process_details 'Empirical Absorption Corrections' _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13679 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12104 _reflns_number_gt 4424 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Software of the Siemens P4' _computing_data_reduction 'Software of the Siemens P4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.0800P)^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 12104 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.2049 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.010 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 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 0.23728(12) 0.25574(12) -0.44093(9) 0.0258(4) Uani 1 1 d . . . Co2 Co 0.27810(11) 0.28533(12) -0.01669(9) 0.0241(4) Uani 1 1 d . . . Br1 Br 0.12934(12) 0.09776(11) -0.45790(8) 0.0538(4) Uani 1 1 d . . . Br2 Br 0.25429(11) 0.29021(10) -0.56410(8) 0.0407(4) Uani 1 1 d . . . Br3 Br 0.22970(10) 0.21639(10) 0.08396(7) 0.0374(3) Uani 1 1 d . . . Br4 Br 0.32225(11) 0.47340(10) 0.02177(8) 0.0421(4) Uani 1 1 d . . . P1 P 0.2318(2) 0.4357(2) -0.27429(17) 0.0203(6) Uani 1 1 d . . . P2 P 0.4050(2) 0.2605(2) -0.34580(17) 0.0217(7) Uani 1 1 d . . . P3 P 0.1474(2) 0.2248(2) -0.1510(2) 0.0295(7) Uani 1 1 d . . . P4 P 0.3960(2) 0.1435(2) -0.14082(18) 0.0220(7) Uani 1 1 d . . . O1 O 0.1896(6) 0.3772(5) -0.3656(4) 0.0284(18) Uani 1 1 d . . . O2 O 0.3976(6) 0.2284(6) -0.0614(4) 0.0312(19) Uani 1 1 d . . . C1 C 0.2843(7) 0.3444(7) -0.2169(6) 0.020(2) Uani 1 1 d . . . H1A H 0.3029 0.3827 -0.1585 0.080 Uiso 1 1 d R . . C2 C 0.3798(8) 0.2816(7) -0.2399(6) 0.020(2) Uani 1 1 d . . . H2A H 0.4447 0.3072 -0.1970 0.080 Uiso 1 1 d R . . C3 C 0.2205(8) 0.2353(8) -0.2298(6) 0.022(2) Uani 1 1 d . . . H3A H 0.1722 0.2130 -0.2841 0.080 Uiso 1 1 d R . . C4 C 0.3245(8) 0.1802(7) -0.2315(6) 0.016(2) Uani 1 1 d . . . H4A H 0.3151 0.1217 -0.2817 0.080 Uiso 1 1 d R . . C11 C 0.1268(8) 0.5049(8) -0.2373(7) 0.025(3) Uani 1 1 d . . . C12 C 0.1299(8) 0.5455(8) -0.1551(7) 0.027(3) Uani 1 1 d . . . H12A H 0.1846 0.5298 -0.1137 0.080 Uiso 1 1 d R . . C13 C 0.0512(10) 0.6117(10) -0.1321(8) 0.043(4) Uani 1 1 d . . . H13A H 0.0490 0.6382 -0.0747 0.080 Uiso 1 1 d R . . C14 C -0.0250(10) 0.6371(10) -0.1939(10) 0.050(4) Uani 1 1 d . . . H14A H -0.0757 0.6854 -0.1781 0.080 Uiso 1 1 d R . . C15 C -0.0257(11) 0.5976(11) -0.2738(9) 0.051(4) Uani 1 1 d . . . H15A H -0.0804 0.6135 -0.3151 0.080 Uiso 1 1 d R . . C16 C 0.0501(9) 0.5312(10) -0.2989(8) 0.042(3) Uani 1 1 d . . . H16A H 0.0516 0.5053 -0.3564 0.080 Uiso 1 1 d R . . C21 C 0.3374(8) 0.5406(8) -0.2520(7) 0.024(3) Uani 1 1 d . . . C22 C 0.3940(8) 0.5951(8) -0.1723(7) 0.030(3) Uani 1 1 d . . . H22A H 0.3850 0.5714 -0.1264 0.080 Uiso 1 1 d R . . C23 C 0.4652(9) 0.6819(11) -0.1591(10) 0.051(4) Uani 1 1 d . . . H23A H 0.5020 0.7245 -0.1038 0.080 Uiso 1 1 d R . . C24 C 0.4834(10) 0.7108(11) -0.2272(13) 0.067(5) Uani 1 1 d . . . H24A H 0.5385 0.7667 -0.2193 0.080 Uiso 1 1 d R . . C25 C 0.4255(11) 0.6620(10) -0.3032(10) 0.051(4) Uani 1 1 d . . . H25A H 0.4344 0.6888 -0.3477 0.080 Uiso 1 1 d R . . C26 C 0.3539(9) 0.5742(10) -0.3194(8) 0.038(3) Uani 1 1 d . . . H26A H 0.3157 0.5362 -0.3755 0.080 Uiso 1 1 d R . . C31 C 0.5048(8) 0.3679(8) -0.3369(6) 0.020(2) Uani 1 1 d . . . C32 C 0.5189(8) 0.3792(9) -0.4118(6) 0.030(3) Uani 1 1 d . . . H32A H 0.4775 0.3318 -0.4639 0.080 Uiso 1 1 d R . . C33 C 0.5929(10) 0.4608(11) -0.4100(8) 0.051(4) Uani 1 1 d . . . H33A H 0.6031 0.4694 -0.4611 0.080 Uiso 1 1 d R . . C34 C 0.6523(9) 0.5262(11) -0.3370(8) 0.046(4) Uani 1 1 d . . . H34A H 0.7038 0.5811 -0.3368 0.080 Uiso 1 1 d R . . C35 C 0.6387(8) 0.5175(8) -0.2623(7) 0.028(3) Uani 1 1 d . . . H35A H 0.6794 0.5661 -0.2104 0.080 Uiso 1 1 d R . . C36 C 0.5663(8) 0.4358(7) -0.2637(6) 0.019(2) Uani 1 1 d . . . H36A H 0.5577 0.4276 -0.2119 0.080 Uiso 1 1 d R . . C41 C 0.4786(9) 0.1438(9) -0.3608(6) 0.027(3) Uani 1 1 d . . . C42 C 0.5884(11) 0.1517(10) -0.3412(8) 0.044(3) Uani 1 1 d . . . H42A H 0.6275 0.2217 -0.3165 0.080 Uiso 1 1 d R . . C43 C 0.6428(13) 0.0628(13) -0.3565(9) 0.065(5) Uani 1 1 d . . . H43A H 0.7194 0.0682 -0.3403 0.080 Uiso 1 1 d R . . C44 C 0.5850(17) -0.0352(14) -0.3963(10) 0.079(6) Uani 1 1 d . . . H44A H 0.6211 -0.0979 -0.4099 0.080 Uiso 1 1 d R . . C45 C 0.4780(16) -0.0463(12) -0.4163(9) 0.069(5) Uani 1 1 d . . . H45A H 0.4409 -0.1172 -0.4403 0.080 Uiso 1 1 d R . . C46 C 0.4212(11) 0.0421(9) -0.4018(7) 0.036(3) Uani 1 1 d . . . H46A H 0.3447 0.0345 -0.4199 0.080 Uiso 1 1 d R . . C51 C 0.0379(10) 0.3009(9) -0.1601(8) 0.040(3) Uani 1 1 d . . . C52 C 0.0115(10) 0.3584(10) -0.0881(8) 0.045(3) Uani 1 1 d . . . H52A H 0.0594 0.3642 -0.0353 0.080 Uiso 1 1 d R . . C53 C -0.0826(10) 0.4098(11) -0.0892(9) 0.052(4) Uani 1 1 d . . . H53A H -0.1015 0.4466 -0.0387 0.080 Uiso 1 1 d R . . C54 C -0.1468(11) 0.4051(11) -0.1662(11) 0.058(4) Uani 1 1 d . . . H54A H -0.2111 0.4393 -0.1682 0.080 Uiso 1 1 d R . . C55 C -0.1223(10) 0.3529(12) -0.2374(9) 0.052(4) Uani 1 1 d . . . H55A H -0.1680 0.3538 -0.2893 0.080 Uiso 1 1 d R . . C56 C -0.0263(3) 0.2972(3) -0.2361(3) 0.041(3) Uani 1 1 d . . . H56A H -0.0088 0.2588 -0.2868 0.080 Uiso 1 1 d R . . C61 C 0.0775(3) 0.0912(3) -0.1885(3) 0.022(3) Uani 1 1 d R . . C62 C 0.0322(3) 0.0398(3) -0.2724(3) 0.036(3) Uani 1 1 d R . . H62A H 0.0465 0.0700 -0.3133 0.043 Uiso 1 1 calc R . . C63 C -0.0339(3) -0.0558(3) -0.2967(3) 0.043(3) Uani 1 1 d R . . H63A H -0.0649 -0.0909 -0.3541 0.051 Uiso 1 1 calc R . . C64 C -0.0548(3) -0.1000(3) -0.2370(3) 0.044(3) Uani 1 1 d R . . H64A H -0.0999 -0.1654 -0.2536 0.053 Uiso 1 1 calc R . . C65 C -0.0095(3) -0.0486(3) -0.1530(3) 0.042(3) Uani 1 1 d R . . H65A H -0.0238 -0.0789 -0.1122 0.050 Uiso 1 1 calc R . . C66 C 0.0566(3) 0.0470(3) -0.1287(3) 0.034(3) Uani 1 1 d R . . H66A H 0.0876 0.0821 -0.0713 0.040 Uiso 1 1 calc R . . C71 C 0.5306(3) 0.1307(3) -0.1462(3) 0.027(3) Uani 1 1 d R . . C72 C 0.6065(3) 0.2221(3) -0.1077(3) 0.036(3) Uani 1 1 d R . . H72A H 0.5834 0.2899 -0.0836 0.080 Uiso 1 1 d R . . C73 C 0.7130(10) 0.2132(12) -0.1044(9) 0.051(4) Uani 1 1 d . . . H73A H 0.7639 0.2756 -0.0772 0.080 Uiso 1 1 d R . . C74 C 0.7488(10) 0.1157(13) -0.1389(10) 0.063(5) Uani 1 1 d . . . H74A H 0.8224 0.1112 -0.1400 0.080 Uiso 1 1 d R . . C75 C 0.6740(10) 0.0253(12) -0.1749(9) 0.052(4) Uani 1 1 d . . . H75A H 0.6977 -0.0434 -0.1955 0.080 Uiso 1 1 d R . . C76 C 0.5665(3) 0.0337(3) -0.1788(2) 0.038(3) Uani 1 1 d . . . H76A H 0.5153 -0.0287 -0.2046 0.080 Uiso 1 1 d R . . C81 C 0.3341(3) 0.0173(3) -0.1456(2) 0.031(3) Uani 1 1 d R . . C82 C 0.2815(3) -0.0600(3) -0.2194(2) 0.046(4) Uani 1 1 d R . . H82A H 0.2757 -0.0464 -0.2712 0.056 Uiso 1 1 calc R . . C83 C 0.2375(3) -0.1573(3) -0.2173(2) 0.060(4) Uani 1 1 d R . . H83A H 0.2016 -0.2102 -0.2677 0.072 Uiso 1 1 calc R . . C84 C 0.2461(3) -0.1773(3) -0.1415(2) 0.065(5) Uani 1 1 d R . . H84A H 0.2160 -0.2438 -0.1401 0.078 Uiso 1 1 calc R . . C85 C 0.2986(3) -0.0999(3) -0.0677(2) 0.064(5) Uani 1 1 d R . . H85A H 0.3044 -0.1136 -0.0159 0.077 Uiso 1 1 calc R . . C86 C 0.3426(3) -0.0026(3) -0.0698(2) 0.049(4) Uani 1 1 d R . . H86A H 0.3785 0.0502 -0.0194 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.0307(3) 0.6874(3) 0.5567(2) 0.108(3) Uani 0.65 1 d PR . . Cl2 Cl 0.1746(3) 0.8099(3) 0.5022(2) 0.411(11) Uani 1 1 d R . . Cl3 Cl 0.1926(3) 0.6193(3) 0.4710(2) 0.185(8) Uani 0.50 1 d PR . . Cl4 Cl 0.1509(3) 0.5681(3) 0.4826(2) 0.108(4) Uani 0.50 1 d PR . . Cl5 Cl 0.0776(3) 0.7620(3) 0.5776(2) 0.219(15) Uani 0.35 1 d PR . . C5 C 0.0953(3) 0.6967(3) 0.4823(2) 0.109(7) Uani 1 1 d 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 0.0237(9) 0.0276(9) 0.0240(8) 0.0070(7) 0.0030(7) 0.0008(7) Co2 0.0174(8) 0.0286(9) 0.0298(9) 0.0111(7) 0.0086(7) 0.0089(7) Br1 0.0599(10) 0.0513(9) 0.0415(8) 0.0122(7) 0.0025(7) -0.0225(8) Br2 0.0449(8) 0.0450(8) 0.0330(7) 0.0169(6) 0.0054(6) 0.0012(7) Br3 0.0385(8) 0.0408(8) 0.0360(7) 0.0110(6) 0.0161(6) 0.0040(6) Br4 0.0563(9) 0.0293(7) 0.0393(8) 0.0084(6) 0.0109(7) 0.0100(6) P1 0.0166(15) 0.0181(15) 0.0268(16) 0.0094(13) 0.0025(13) 0.0066(12) P2 0.0184(16) 0.0222(16) 0.0255(16) 0.0041(13) 0.0114(13) 0.0032(13) P3 0.0247(18) 0.0217(16) 0.049(2) 0.0145(15) 0.0182(16) 0.0052(14) P4 0.0193(16) 0.0193(15) 0.0282(16) 0.0086(13) 0.0048(13) 0.0067(13) O1 0.026(4) 0.030(4) 0.026(4) 0.008(4) -0.002(4) 0.012(4) O2 0.021(4) 0.038(5) 0.036(5) 0.014(4) 0.004(4) 0.020(4) C1 0.022(5) 0.025(6) 0.012(5) 0.003(5) 0.004(4) 0.006(4) C2 0.022(6) 0.017(6) 0.023(6) 0.009(5) 0.007(5) 0.005(5) C3 0.017(6) 0.024(6) 0.030(6) 0.010(5) 0.012(5) 0.006(5) C4 0.020(6) 0.008(5) 0.029(6) 0.011(5) 0.013(5) 0.010(4) C11 0.020(6) 0.023(6) 0.026(6) -0.007(5) 0.010(5) 0.003(5) C12 0.017(6) 0.021(6) 0.050(8) 0.010(6) 0.022(6) 0.006(5) C13 0.046(9) 0.037(8) 0.057(9) 0.010(7) 0.038(8) -0.003(7) C14 0.035(8) 0.034(8) 0.099(13) 0.026(9) 0.041(9) 0.024(7) C15 0.034(9) 0.069(10) 0.056(10) 0.032(8) 0.007(8) 0.024(8) C16 0.028(7) 0.064(9) 0.046(8) 0.033(7) 0.012(6) 0.023(7) C21 0.016(6) 0.018(6) 0.048(8) 0.015(6) 0.021(6) 0.010(5) C22 0.016(6) 0.023(6) 0.042(7) 0.000(6) 0.003(6) 0.001(5) C23 0.015(7) 0.043(9) 0.092(12) 0.011(8) 0.019(8) 0.017(6) C24 0.013(8) 0.040(9) 0.148(17) 0.045(11) -0.003(10) 0.007(6) C25 0.047(9) 0.041(8) 0.091(12) 0.054(8) 0.021(9) 0.020(7) C26 0.022(7) 0.043(8) 0.061(9) 0.030(7) 0.016(7) 0.015(6) C31 0.024(6) 0.017(6) 0.016(6) -0.002(5) 0.006(5) 0.012(5) C32 0.019(6) 0.045(8) 0.015(6) -0.003(5) -0.001(5) -0.011(6) C33 0.033(8) 0.088(11) 0.033(8) 0.028(8) 0.002(7) -0.001(8) C34 0.020(7) 0.078(10) 0.055(9) 0.053(8) 0.000(6) -0.010(7) C35 0.011(6) 0.018(6) 0.044(7) 0.003(5) -0.005(5) -0.002(5) C36 0.020(6) 0.017(6) 0.022(6) 0.005(5) 0.007(5) 0.007(5) C41 0.019(6) 0.044(8) 0.026(6) 0.015(6) 0.014(5) 0.018(6) C42 0.056(10) 0.038(8) 0.057(9) 0.026(7) 0.034(8) 0.038(7) C43 0.072(12) 0.067(11) 0.067(11) 0.019(9) 0.034(9) 0.049(10) C44 0.118(17) 0.068(13) 0.066(12) 0.013(10) 0.050(12) 0.028(13) C45 0.125(16) 0.036(9) 0.060(11) 0.015(8) 0.046(12) 0.027(10) C46 0.055(9) 0.021(6) 0.030(7) 0.000(5) 0.013(6) 0.019(6) C51 0.041(8) 0.033(7) 0.054(9) 0.016(7) 0.025(7) 0.012(6) C52 0.039(9) 0.050(9) 0.053(9) 0.021(7) 0.020(7) 0.008(7) C53 0.029(8) 0.078(11) 0.070(10) 0.038(9) 0.028(8) 0.028(8) C54 0.040(9) 0.044(9) 0.110(14) 0.052(10) 0.021(10) 0.017(7) C55 0.029(8) 0.084(11) 0.049(9) 0.040(9) -0.003(7) 0.008(8) C56 0.018(7) 0.066(9) 0.042(8) 0.029(7) -0.004(6) -0.005(6) C61 0.023(6) 0.011(6) 0.033(6) 0.003(5) 0.014(5) 0.013(5) C62 0.032(7) 0.034(7) 0.038(8) 0.009(6) 0.007(6) -0.007(6) C63 0.043(9) 0.038(8) 0.035(7) -0.001(6) 0.003(7) -0.014(7) C64 0.036(8) 0.024(7) 0.061(9) 0.001(6) 0.004(7) 0.006(6) C65 0.047(9) 0.034(7) 0.051(8) 0.022(7) 0.017(7) -0.001(6) C66 0.038(8) 0.038(7) 0.027(6) 0.013(6) 0.009(6) -0.002(6) C71 0.013(6) 0.035(7) 0.041(7) 0.023(6) 0.004(5) 0.008(5) C72 0.043(8) 0.026(7) 0.046(8) 0.024(6) 0.008(7) 0.006(6) C73 0.031(8) 0.066(10) 0.063(9) 0.041(8) 0.003(7) -0.003(8) C74 0.018(8) 0.082(12) 0.104(13) 0.041(11) 0.023(8) 0.029(8) C75 0.030(8) 0.077(11) 0.066(10) 0.035(9) 0.022(8) 0.038(8) C76 0.033(8) 0.037(7) 0.050(8) 0.017(6) 0.018(7) 0.016(6) C81 0.024(6) 0.026(6) 0.046(7) 0.012(5) 0.016(5) 0.003(5) C82 0.029(8) 0.043(8) 0.065(9) 0.019(7) 0.007(7) -0.005(6) C83 0.034(9) 0.029(8) 0.110(14) 0.009(8) 0.018(9) 0.003(6) C84 0.043(9) 0.024(8) 0.148(17) 0.046(9) 0.038(10) 0.007(7) C85 0.076(12) 0.043(9) 0.107(13) 0.053(9) 0.050(10) 0.024(8) C86 0.055(9) 0.045(8) 0.068(10) 0.036(8) 0.033(8) 0.029(7) Cl1 0.105(7) 0.117(7) 0.122(7) 0.052(6) 0.044(6) 0.019(6) Cl2 0.243(13) 0.213(11) 0.75(3) 0.183(16) 0.057(16) -0.113(10) Cl3 0.153(14) 0.241(18) 0.128(12) 0.003(12) 0.028(10) 0.137(14) Cl4 0.075(7) 0.109(8) 0.088(8) -0.011(6) -0.025(6) 0.004(7) Cl5 0.29(3) 0.28(3) 0.21(3) 0.16(2) 0.17(3) 0.20(3) C5 0.088(15) 0.16(2) 0.086(14) 0.022(14) 0.053(13) 0.026(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.971(7) . ? Co1 Br2 2.355(2) . ? Co1 Br1 2.359(2) . ? Co1 P2 2.393(3) . ? Co2 O2 1.963(7) . ? Co2 Br3 2.3635(19) . ? Co2 Br4 2.375(2) . ? Co2 P3 2.438(4) . ? P1 O1 1.505(7) . ? P1 C21 1.794(10) . ? P1 C11 1.800(11) . ? P1 C1 1.822(9) . ? P2 C31 1.821(10) . ? P2 C41 1.824(11) . ? P2 C2 1.877(10) . ? P3 C51 1.769(13) . ? P3 C61 1.810 . ? P3 C3 1.856(10) . ? P4 O2 1.497(8) . ? P4 C71 1.775 . ? P4 C81 1.783 . ? P4 C4 1.832(9) . ? C1 C3 1.556(13) . ? C1 C2 1.576(13) . ? C1 H1A 0.9600 . ? C2 C4 1.545(12) . ? C2 H2A 0.9601 . ? C3 C4 1.555(13) . ? C3 H3A 0.9599 . ? C4 H4A 0.9599 . ? C11 C12 1.359(14) . ? C11 C16 1.414(15) . ? C12 C13 1.418(16) . ? C12 H12A 0.9598 . ? C13 C14 1.407(17) . ? C13 H13A 0.9601 . ? C14 C15 1.329(18) . ? C14 H14A 0.9600 . ? C15 C16 1.398(17) . ? C15 H15A 0.9601 . ? C16 H16A 0.9600 . ? C21 C22 1.373(14) . ? C21 C26 1.414(14) . ? C22 C23 1.367(16) . ? C22 H22A 0.9600 . ? C23 C24 1.40(2) . ? C23 H23A 0.9600 . ? C24 C25 1.317(19) . ? C24 H24A 0.9600 . ? C25 C26 1.369(16) . ? C25 H25A 0.9603 . ? C26 H26A 0.9600 . ? C31 C36 1.368(13) . ? C31 C32 1.395(14) . ? C32 C33 1.396(15) . ? C32 H32A 0.9600 . ? C33 C34 1.345(17) . ? C33 H33A 0.9600 . ? C34 C35 1.378(15) . ? C34 H34A 0.9599 . ? C35 C36 1.387(13) . ? C35 H35A 0.9601 . ? C36 H36A 0.9601 . ? C41 C42 1.375(15) . ? C41 C46 1.406(15) . ? C42 C43 1.379(17) . ? C42 H42A 0.9600 . ? C43 C44 1.37(2) . ? C43 H43A 0.9601 . ? C44 C45 1.34(2) . ? C44 H44A 0.9601 . ? C45 C46 1.392(18) . ? C45 H45A 0.9600 . ? C46 H46A 0.9600 . ? C51 C56 1.374(13) . ? C51 C52 1.384(17) . ? C52 C53 1.414(17) . ? C52 H52A 0.9600 . ? C53 C54 1.383(18) . ? C53 H53A 0.9602 . ? C54 C55 1.341(19) . ? C54 H54A 0.9598 . ? C55 C56 1.465(15) . ? C55 H55A 0.9600 . ? C56 H56A 0.9601 . ? C61 C62 1.3899 . ? C61 C66 1.3901 . ? C62 C63 1.3901 . ? C62 H62A 0.9500 . ? C63 C64 1.3901 . ? C63 H63A 0.9500 . ? C64 C65 1.3900 . ? C64 H64A 0.9500 . ? C65 C66 1.3899 . ? C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C76 1.384 . ? C71 C72 1.4140 . ? C72 C73 1.376 . ? C72 H72A 0.9600 . ? C73 C74 1.395(19) . ? C73 H73A 0.9599 . ? C74 C75 1.395(18) . ? C74 H74A 0.9600 . ? C75 C76 1.387(13) . ? C75 H75A 0.9600 . ? C76 H76A 0.9600 . ? C81 C86 1.3899 . ? C81 C82 1.3901 . ? C82 C83 1.3900 . ? C82 H82A 0.9500 . ? C83 C84 1.3900 . ? C83 H83A 0.9500 . ? C84 C85 1.3900 . ? C84 H84A 0.9500 . ? C85 C86 1.3900 . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? Cl1 Cl5 1.0524 . ? Cl1 C5 1.7129 . ? Cl2 C5 1.6752 . ? Cl2 Cl5 2.1938 . ? Cl2 Cl3 2.4384 . ? Cl3 Cl4 0.9376 . ? Cl3 C5 1.6610 . ? Cl4 C5 1.8624 . ? Cl5 C5 1.6984 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 Br2 112.2(2) . . ? O1 Co1 Br1 109.0(2) . . ? Br2 Co1 Br1 116.23(7) . . ? O1 Co1 P2 95.0(2) . . ? Br2 Co1 P2 113.54(10) . . ? Br1 Co1 P2 108.69(9) . . ? O2 Co2 Br3 117.6(2) . . ? O2 Co2 Br4 103.2(2) . . ? Br3 Co2 Br4 116.84(8) . . ? O2 Co2 P3 94.5(2) . . ? Br3 Co2 P3 112.66(9) . . ? Br4 Co2 P3 109.59(9) . . ? O1 P1 C21 114.0(5) . . ? O1 P1 C11 108.2(5) . . ? C21 P1 C11 103.6(5) . . ? O1 P1 C1 111.0(4) . . ? C21 P1 C1 106.6(5) . . ? C11 P1 C1 113.3(5) . . ? C31 P2 C41 102.7(5) . . ? C31 P2 C2 107.2(4) . . ? C41 P2 C2 104.1(4) . . ? C31 P2 Co1 114.3(3) . . ? C41 P2 Co1 119.8(4) . . ? C2 P2 Co1 107.7(3) . . ? C51 P3 C61 100.2 . . ? C51 P3 C3 108.2(6) . . ? C61 P3 C3 106.2 . . ? C51 P3 Co2 114.7(5) . . ? C61 P3 Co2 120.56 . . ? C3 P3 Co2 106.1(3) . . ? O2 P4 C71 107.6 . . ? O2 P4 C81 112.3 . . ? C71 P4 C81 109.0 . . ? O2 P4 C4 111.2(4) . . ? C71 P4 C4 108.8 . . ? C81 P4 C4 107.9 . . ? P1 O1 Co1 132.0(4) . . ? P4 O2 Co2 129.6(4) . . ? C3 C1 C2 88.4(7) . . ? C3 C1 P1 121.5(6) . . ? C2 C1 P1 119.1(6) . . ? C3 C1 H1A 108.2 . . ? C2 C1 H1A 109.4 . . ? P1 C1 H1A 108.6 . . ? C4 C2 C1 89.4(7) . . ? C4 C2 P2 112.5(7) . . ? C1 C2 P2 119.7(6) . . ? C4 C2 H2A 110.7 . . ? C1 C2 H2A 111.5 . . ? P2 C2 H2A 111.1 . . ? C4 C3 C1 89.8(7) . . ? C4 C3 P3 118.4(7) . . ? C1 C3 P3 118.2(7) . . ? C4 C3 H3A 110.3 . . ? C1 C3 H3A 109.1 . . ? P3 C3 H3A 109.5 . . ? C2 C4 C3 89.6(7) . . ? C2 C4 P4 112.5(7) . . ? C3 C4 P4 120.5(7) . . ? C2 C4 H4A 110.5 . . ? C3 C4 H4A 111.0 . . ? P4 C4 H4A 110.9 . . ? C12 C11 C16 121.4(11) . . ? C12 C11 P1 123.0(9) . . ? C16 C11 P1 114.7(9) . . ? C11 C12 C13 118.5(11) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 121.0 . . ? C14 C13 C12 119.7(12) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.3 . . ? C15 C14 C13 120.7(12) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 121.2(13) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.6 . . ? C15 C16 C11 118.5(12) . . ? C15 C16 H16A 121.2 . . ? C11 C16 H16A 120.4 . . ? C22 C21 C26 119.8(10) . . ? C22 C21 P1 122.5(8) . . ? C26 C21 P1 117.4(9) . . ? C23 C22 C21 119.5(12) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C24 119.6(14) . . ? C22 C23 H23A 121.2 . . ? C24 C23 H23A 119.2 . . ? C25 C24 C23 120.8(13) . . ? C25 C24 H24A 118.6 . . ? C23 C24 H24A 120.5 . . ? C24 C25 C26 121.2(13) . . ? C24 C25 H25A 118.8 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C21 118.7(12) . . ? C25 C26 H26A 120.7 . . ? C21 C26 H26A 120.6 . . ? C36 C31 C32 118.8(10) . . ? C36 C31 P2 125.3(8) . . ? C32 C31 P2 115.9(7) . . ? C31 C32 C33 119.3(10) . . ? C31 C32 H32A 120.3 . . ? C33 C32 H32A 120.4 . . ? C34 C33 C32 120.6(11) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 121.1(11) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.2 . . ? C34 C35 C36 118.5(10) . . ? C34 C35 H35A 120.8 . . ? C36 C35 H35A 120.6 . . ? C31 C36 C35 121.6(10) . . ? C31 C36 H36A 119.1 . . ? C35 C36 H36A 119.2 . . ? C42 C41 C46 118.3(11) . . ? C42 C41 P2 122.7(9) . . ? C46 C41 P2 118.6(9) . . ? C41 C42 C43 121.9(14) . . ? C41 C42 H42A 118.2 . . ? C43 C42 H42A 119.8 . . ? C44 C43 C42 118.5(15) . . ? C44 C43 H43A 119.7 . . ? C42 C43 H43A 121.8 . . ? C45 C44 C43 121.3(15) . . ? C45 C44 H44A 118.6 . . ? C43 C44 H44A 120.1 . . ? C44 C45 C46 121.2(16) . . ? C44 C45 H45A 118.4 . . ? C46 C45 H45A 120.3 . . ? C45 C46 C41 118.5(13) . . ? C45 C46 H46A 121.1 . . ? C41 C46 H46A 120.4 . . ? C56 C51 C52 119.4(11) . . ? C56 C51 P3 121.9(9) . . ? C52 C51 P3 118.5(10) . . ? C51 C52 C53 122.6(13) . . ? C51 C52 H52A 118.6 . . ? C53 C52 H52A 118.9 . . ? C54 C53 C52 117.4(14) . . ? C54 C53 H53A 121.1 . . ? C52 C53 H53A 121.5 . . ? C55 C54 C53 121.8(13) . . ? C55 C54 H54A 119.6 . . ? C53 C54 H54A 118.5 . . ? C54 C55 C56 120.7(11) . . ? C54 C55 H55A 119.0 . . ? C56 C55 H55A 120.3 . . ? C51 C56 C55 118.1(8) . . ? C51 C56 H56A 120.7 . . ? C55 C56 H56A 121.2 . . ? C62 C61 C66 120.0 . . ? C62 C61 P3 122.51 . . ? C66 C61 P3 116.83 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66A 120.0 . . ? C61 C66 H66A 120.0 . . ? C76 C71 C72 118.4 . . ? C76 C71 P4 123.0 . . ? C72 C71 P4 118.31 . . ? C73 C72 C71 119.9 . . ? C73 C72 H72A 120.5 . . ? C71 C72 H72A 119.6 . . ? C72 C73 C74 121.7 . . ? C72 C73 H73A 119.0 . . ? C74 C73 H73A 119.3 . . ? C73 C74 C75 118.2(12) . . ? C73 C74 H74A 121.2 . . ? C75 C74 H74A 120.6 . . ? C76 C75 C74 120.4(12) . . ? C76 C75 H75A 120.1 . . ? C74 C75 H75A 119.5 . . ? C71 C76 C75 121.4 . . ? C71 C76 H76A 118.7 . . ? C75 C76 H76A 119.9 . . ? C86 C81 C82 120.0 . . ? C86 C81 P4 116.06 . . ? C82 C81 P4 123.92 . . ? C83 C82 C81 120.0 . . ? C83 C82 H82A 120.0 . . ? C81 C82 H82A 120.0 . . ? C82 C83 C84 120.0 . . ? C82 C83 H83A 120.0 . . ? C84 C83 H83A 120.0 . . ? C85 C84 C83 120.0 . . ? C85 C84 H84A 120.0 . . ? C83 C84 H84A 120.0 . . ? C84 C85 C86 120.0 . . ? C84 C85 H85A 120.0 . . ? C86 C85 H85A 120.0 . . ? C81 C86 C85 120.0 . . ? C81 C86 H86A 120.0 . . ? C85 C86 H86A 120.0 . . ? Cl5 Cl1 C5 71.3 . . ? C5 Cl2 Cl5 49.9 . . ? C5 Cl2 Cl3 42.8 . . ? Cl5 Cl2 Cl3 78.5 . . ? Cl4 Cl3 C5 86.9 . . ? Cl4 Cl3 Cl2 126.5 . . ? C5 Cl3 Cl2 43.3 . . ? Cl3 Cl4 C5 62.9 . . ? Cl1 Cl5 C5 72.8 . . ? Cl1 Cl5 Cl2 121.8 . . ? C5 Cl5 Cl2 49.0 . . ? Cl3 C5 Cl2 93.9 . . ? Cl3 C5 Cl5 121.9 . . ? Cl2 C5 Cl5 81.1 . . ? Cl3 C5 Cl1 115.9 . . ? Cl2 C5 Cl1 117.1 . . ? Cl5 C5 Cl1 35.9 . . ? Cl3 C5 Cl4 30.2 . . ? Cl2 C5 Cl4 121.6 . . ? Cl5 C5 Cl4 110.7 . . ? Cl1 C5 Cl4 90.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 P2 C31 -76.1(4) . . . . ? Br2 Co1 P2 C31 40.8(4) . . . . ? Br1 Co1 P2 C31 171.8(4) . . . . ? O1 Co1 P2 C41 161.4(4) . . . . ? Br2 Co1 P2 C41 -81.7(4) . . . . ? Br1 Co1 P2 C41 49.3(4) . . . . ? O1 Co1 P2 C2 42.9(4) . . . . ? Br2 Co1 P2 C2 159.8(3) . . . . ? Br1 Co1 P2 C2 -69.1(3) . . . . ? O2 Co2 P3 C51 -153.5(5) . . . . ? Br3 Co2 P3 C51 84.1(4) . . . . ? Br4 Co2 P3 C51 -47.8(4) . . . . ? O2 Co2 P3 C61 86.6 . . . . ? Br3 Co2 P3 C61 -35.8 . . . . ? Br4 Co2 P3 C61 -167.7 . . . . ? O2 Co2 P3 C3 -33.9(4) . . . . ? Br3 Co2 P3 C3 -156.3(3) . . . . ? Br4 Co2 P3 C3 71.8(3) . . . . ? C21 P1 O1 Co1 85.3(7) . . . . ? C11 P1 O1 Co1 -160.0(6) . . . . ? C1 P1 O1 Co1 -35.1(7) . . . . ? Br2 Co1 O1 P1 -130.1(5) . . . . ? Br1 Co1 O1 P1 99.7(6) . . . . ? P2 Co1 O1 P1 -12.1(6) . . . . ? C71 P4 O2 Co2 178.8 . . . . ? C81 P4 O2 Co2 -61.2 . . . . ? C4 P4 O2 Co2 59.8(7) . . . . ? Br3 Co2 O2 P4 98.1(5) . . . . ? Br4 Co2 O2 P4 -131.7(5) . . . . ? P3 Co2 O2 P4 -20.3(5) . . . . ? O1 P1 C1 C3 -47.2(9) . . . . ? C21 P1 C1 C3 -171.9(8) . . . . ? C11 P1 C1 C3 74.8(9) . . . . ? O1 P1 C1 C2 60.4(8) . . . . ? C21 P1 C1 C2 -64.3(8) . . . . ? C11 P1 C1 C2 -177.6(7) . . . . ? C3 C1 C2 C4 -12.5(7) . . . . ? P1 C1 C2 C4 -138.2(7) . . . . ? C3 C1 C2 P2 103.3(7) . . . . ? P1 C1 C2 P2 -22.3(10) . . . . ? C31 P2 C2 C4 -162.4(7) . . . . ? C41 P2 C2 C4 -54.0(8) . . . . ? Co1 P2 C2 C4 74.1(7) . . . . ? C31 P2 C2 C1 94.6(8) . . . . ? C41 P2 C2 C1 -157.0(7) . . . . ? Co1 P2 C2 C1 -28.8(8) . . . . ? C2 C1 C3 C4 12.4(7) . . . . ? P1 C1 C3 C4 136.0(7) . . . . ? C2 C1 C3 P3 135.1(7) . . . . ? P1 C1 C3 P3 -101.3(8) . . . . ? C51 P3 C3 C4 176.7(8) . . . . ? C61 P3 C3 C4 -76.4 . . . . ? Co2 P3 C3 C4 53.0(8) . . . . ? C51 P3 C3 C1 70.0(9) . . . . ? C61 P3 C3 C1 176.9 . . . . ? Co2 P3 C3 C1 -53.6(8) . . . . ? C1 C2 C4 C3 12.5(7) . . . . ? P2 C2 C4 C3 -109.6(7) . . . . ? C1 C2 C4 P4 -110.6(7) . . . . ? P2 C2 C4 P4 127.3(6) . . . . ? C1 C3 C4 C2 -12.7(7) . . . . ? P3 C3 C4 C2 -135.1(7) . . . . ? C1 C3 C4 P4 103.4(7) . . . . ? P3 C3 C4 P4 -19.0(11) . . . . ? O2 P4 C4 C2 63.6(8) . . . . ? C71 P4 C4 C2 -54.7 . . . . ? C81 P4 C4 C2 -172.8 . . . . ? O2 P4 C4 C3 -40.1(9) . . . . ? C71 P4 C4 C3 -158.4 . . . . ? C81 P4 C4 C3 83.5 . . . . ? O1 P1 C11 C12 164.9(8) . . . . ? C21 P1 C11 C12 -73.8(10) . . . . ? C1 P1 C11 C12 41.4(10) . . . . ? O1 P1 C11 C16 -26.0(10) . . . . ? C21 P1 C11 C16 95.3(9) . . . . ? C1 P1 C11 C16 -149.5(8) . . . . ? C16 C11 C12 C13 2.6(16) . . . . ? P1 C11 C12 C13 171.1(8) . . . . ? C11 C12 C13 C14 -2.4(16) . . . . ? C12 C13 C14 C15 1.7(18) . . . . ? C13 C14 C15 C16 -1(2) . . . . ? C14 C15 C16 C11 1(2) . . . . ? C12 C11 C16 C15 -2.1(17) . . . . ? P1 C11 C16 C15 -171.4(9) . . . . ? O1 P1 C21 C22 -172.7(8) . . . . ? C11 P1 C21 C22 69.9(10) . . . . ? C1 P1 C21 C22 -49.9(10) . . . . ? O1 P1 C21 C26 13.9(10) . . . . ? C11 P1 C21 C26 -103.5(9) . . . . ? C1 P1 C21 C26 136.6(8) . . . . ? C26 C21 C22 C23 0.6(16) . . . . ? P1 C21 C22 C23 -172.7(9) . . . . ? C21 C22 C23 C24 -3.2(18) . . . . ? C22 C23 C24 C25 7(2) . . . . ? C23 C24 C25 C26 -7(2) . . . . ? C24 C25 C26 C21 4.3(19) . . . . ? C22 C21 C26 C25 -1.0(17) . . . . ? P1 C21 C26 C25 172.7(9) . . . . ? C41 P2 C31 C36 -96.1(10) . . . . ? C2 P2 C31 C36 13.2(10) . . . . ? Co1 P2 C31 C36 132.5(8) . . . . ? C41 P2 C31 C32 83.1(9) . . . . ? C2 P2 C31 C32 -167.5(8) . . . . ? Co1 P2 C31 C32 -48.2(9) . . . . ? C36 C31 C32 C33 -1.7(17) . . . . ? P2 C31 C32 C33 179.0(9) . . . . ? C31 C32 C33 C34 2(2) . . . . ? C32 C33 C34 C35 -3(2) . . . . ? C33 C34 C35 C36 3.6(19) . . . . ? C32 C31 C36 C35 2.5(16) . . . . ? P2 C31 C36 C35 -178.2(8) . . . . ? C34 C35 C36 C31 -3.4(16) . . . . ? C31 P2 C41 C42 18.2(10) . . . . ? C2 P2 C41 C42 -93.5(10) . . . . ? Co1 P2 C41 C42 146.2(8) . . . . ? C31 P2 C41 C46 -155.2(8) . . . . ? C2 P2 C41 C46 93.1(9) . . . . ? Co1 P2 C41 C46 -27.3(10) . . . . ? C46 C41 C42 C43 -3.5(18) . . . . ? P2 C41 C42 C43 -176.9(10) . . . . ? C41 C42 C43 C44 3(2) . . . . ? C42 C43 C44 C45 -4(2) . . . . ? C43 C44 C45 C46 4(3) . . . . ? C44 C45 C46 C41 -4(2) . . . . ? C42 C41 C46 C45 3.5(17) . . . . ? P2 C41 C46 C45 177.2(9) . . . . ? C61 P3 C51 C56 -67.4 . . . . ? C3 P3 C51 C56 43.6(10) . . . . ? Co2 P3 C51 C56 161.9(7) . . . . ? C61 P3 C51 C52 107.2 . . . . ? C3 P3 C51 C52 -141.9(9) . . . . ? Co2 P3 C51 C52 -23.5(11) . . . . ? C56 C51 C52 C53 3.3(18) . . . . ? P3 C51 C52 C53 -171.4(10) . . . . ? C51 C52 C53 C54 -3.0(19) . . . . ? C52 C53 C54 C55 1(2) . . . . ? C53 C54 C55 C56 1(2) . . . . ? C52 C51 C56 C55 -1.5(14) . . . . ? P3 C51 C56 C55 173.0(8) . . . . ? C54 C55 C56 C51 -0.4(16) . . . . ? C51 P3 C61 C62 75.9 . . . . ? C3 P3 C61 C62 -36.8 . . . . ? Co2 P3 C61 C62 -157.23 . . . . ? C51 P3 C61 C66 -94.8 . . . . ? C3 P3 C61 C66 152.5 . . . . ? Co2 P3 C61 C66 32.1 . . . . ? C66 C61 C62 C63 0.0 . . . . ? P3 C61 C62 C63 -170.42 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? P3 C61 C66 C65 170.96 . . . . ? O2 P4 C71 C76 143.3 . . . . ? C81 P4 C71 C76 21.2 . . . . ? C4 P4 C71 C76 -96.1 . . . . ? O2 P4 C71 C72 -30.0 . . . . ? C81 P4 C71 C72 -152.11 . . . . ? C4 P4 C71 C72 90.5 . . . . ? C76 C71 C72 C73 0.8 . . . . ? P4 C71 C72 C73 174.4 . . . . ? C71 C72 C73 C74 0.5 . . . . ? C72 C73 C74 C75 -2 . . . . ? C73 C74 C75 C76 2(2) . . . . ? C72 C71 C76 C75 -0.5 . . . . ? P4 C71 C76 C75 -173.8 . . . . ? C74 C75 C76 C71 -1.2 . . . . ? O2 P4 C81 C86 -29.9 . . . . ? C71 P4 C81 C86 89.3 . . . . ? C4 P4 C81 C86 -152.8 . . . . ? O2 P4 C81 C82 151.5 . . . . ? C71 P4 C81 C82 -89.3 . . . . ? C4 P4 C81 C82 28.7 . . . . ? C86 C81 C82 C83 0.0 . . . . ? P4 C81 C82 C83 178.51 . . . . ? C81 C82 C83 C84 0.0 . . . . ? C82 C83 C84 C85 0.0 . . . . ? C83 C84 C85 C86 0.0 . . . . ? C82 C81 C86 C85 0.0 . . . . ? P4 C81 C86 C85 -178.63 . . . . ? C84 C85 C86 C81 0.0 . . . . ? _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction 0.982 _refine_diff_density_max 0.990 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.120 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 691865' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2I4(dppcbO3)]' _chemical_name_common (Co2I4(dppcbO3)) _chemical_melting_point ? _chemical_formula_moiety '2(C52 H44 Co2 I4 O3 P4), 1.8(C H2 Cl2), H2 O' _chemical_formula_sum 'C105.80 H93.60 Cl3.60 Co4 I8 O7 P8' _chemical_formula_weight 3103.44 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' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.491(3) _cell_length_b 20.193(4) _cell_length_c 21.528(4) _cell_angle_alpha 93.74(3) _cell_angle_beta 97.49(3) _cell_angle_gamma 110.54(3) _cell_volume 5807(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2995.2 _exptl_absorpt_coefficient_mu 2.931 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.190 _exptl_absorpt_correction_T_max 0.235 _exptl_absorpt_process_details 'Empirical Absorption Corrections' _diffrn_ambient_temperature 193(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 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22104 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.1264 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.05 _reflns_number_total 20559 _reflns_number_gt 10487 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Software of the Siemens P4' _computing_data_reduction 'Software of the Siemens P4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.1506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10487 _refine_ls_number_parameters 580 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2495 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 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 0.6276(3) 0.8906(2) 0.38232(14) 0.0659(11) Uani 1 1 d . . . Co2 Co 0.1036(3) 0.64980(18) 0.29213(18) 0.0656(10) Uani 1 1 d D . . Co3 Co 0.1234(3) 0.8606(2) -0.09705(16) 0.0768(12) Uani 1 1 d . . . Co4 Co -0.3971(3) 0.63538(18) -0.23333(16) 0.0629(10) Uani 1 1 d D . . I1 I 0.81720(14) 0.93571(11) 0.40568(10) 0.0897(7) Uani 1 1 d . . . I2 I 0.55938(16) 0.98403(12) 0.42101(10) 0.0936(7) Uani 1 1 d . . . I3 I -0.08556(16) 0.60591(12) 0.28664(12) 0.1117(9) Uani 1 1 d . . . I4 I 0.17054(14) 0.56448(10) 0.23802(9) 0.0764(6) Uani 1 1 d . . . I5 I 0.31422(15) 0.91674(12) -0.07870(10) 0.0960(7) Uani 1 1 d . . . I6 I 0.05289(19) 0.93078(14) -0.02683(11) 0.1164(9) Uani 1 1 d . . . I7 I -0.58611(14) 0.59780(12) -0.24823(9) 0.0885(7) Uani 1 1 d . . . I8 I -0.33224(17) 0.56631(12) -0.30842(13) 0.1127(9) Uani 1 1 d . . . P1 P 0.5464(5) 0.7713(4) 0.4236(3) 0.064(2) Uani 1 1 d . . . P2 P 0.4861(5) 0.7826(3) 0.2640(2) 0.0461(17) Uani 1 1 d . . . P3 P 0.2311(6) 0.7038(4) 0.4232(4) 0.068(2) Uani 1 1 d D . . P4 P 0.2365(5) 0.8124(3) 0.2992(3) 0.0417(16) Uani 1 1 d . . . P5 P -0.0109(5) 0.7814(3) -0.2282(3) 0.0461(17) Uani 1 1 d . . . P6 P 0.0383(5) 0.7274(4) -0.0821(3) 0.0558(19) Uani 1 1 d . . . P7 P -0.2820(5) 0.6529(4) -0.0912(3) 0.0594(19) Uani 1 1 d . . . P8 P -0.2591(4) 0.7986(3) -0.1831(3) 0.0417(16) Uani 1 1 d . . . O1 O 0.5644(12) 0.8520(8) 0.2943(6) 0.064(5) Uani 1 1 d . . . O2 O 0.1462(15) 0.6657(13) 0.3784(8) 0.129(11) Uani 1 1 d DU . . O3 O 0.1632(11) 0.7442(7) 0.2635(6) 0.050(4) Uani 1 1 d . . . O4 O 0.0635(11) 0.8436(9) -0.1880(6) 0.066(5) Uani 1 1 d . . . O5 O -0.3379(14) 0.6251(11) -0.1501(8) 0.104(7) Uani 1 1 d D . . O6 O -0.3273(10) 0.7394(7) -0.2310(6) 0.048(4) Uani 1 1 d . . . C1 C 0.4175(15) 0.7307(12) 0.3792(9) 0.047(6) Uani 1 1 d . . . H1A H 0.3930 0.6799 0.3788 0.057 Uiso 1 1 d R . . C2 C 0.3897(16) 0.7516(11) 0.3145(8) 0.044(6) Uani 1 1 d . . . H2A H 0.3350 0.7120 0.2911 0.048 Uiso 1 1 d R . . C3 C 0.3438(14) 0.7635(10) 0.4053(9) 0.044(6) Uani 1 1 d . . . H3A H 0.3780 0.7975 0.4417 0.041 Uiso 1 1 d R . . C4 C 0.3470(14) 0.8032(10) 0.3420(8) 0.028(5) Uani 1 1 d . . . H4A H 0.3989 0.8495 0.3509 0.033 Uiso 1 1 d R . . C5 C -0.1129(16) 0.7329(11) -0.1863(9) 0.046(6) Uani 1 1 d . . . H5A H -0.1665 0.6987 -0.2159 0.055 Uiso 1 1 d R . . C6 C -0.0875(15) 0.6973(11) -0.1277(8) 0.038(6) Uani 1 1 d . . . H6A H -0.1135 0.6464 -0.1371 0.045 Uiso 1 1 d R . . C7 C -0.1638(15) 0.7212(12) -0.0955(9) 0.043(6) Uani 1 1 d . . . H7A H -0.1327 0.7459 -0.0543 0.052 Uiso 1 1 d R . . C8 C -0.1550(15) 0.7765(12) -0.1444(8) 0.038(6) Uani 1 1 d . . . H8A H -0.1014 0.8204 -0.1277 0.046 Uiso 1 1 d R . . C11B C 0.7081(11) 0.7312(6) 0.4202(7) 0.062(7) Uiso 1 1 d G . . C11C C 0.7595(8) 0.6863(9) 0.4085(7) 0.076(8) Uiso 1 1 d G . . C11D C 0.7071(12) 0.6152(8) 0.3852(8) 0.076(8) Uiso 1 1 d G . . C11E C 0.6032(12) 0.5890(6) 0.3736(7) 0.090(9) Uiso 1 1 d G . . C11F C 0.5518(8) 0.6339(8) 0.3852(7) 0.058(7) Uiso 1 1 d G . . C11A C 0.6043(11) 0.7050(8) 0.4085(7) 0.064(7) Uiso 1 1 d G . . H11A H 0.7443 0.7803 0.4363 0.077 Uiso 1 1 calc G . . H11B H 0.8312 0.7044 0.4166 0.077 Uiso 1 1 d G . . H11C H 0.7425 0.5842 0.3772 0.077 Uiso 1 1 d G . . H11D H 0.5670 0.5399 0.3575 0.077 Uiso 1 1 d G . . H11E H 0.4801 0.6158 0.3772 0.077 Uiso 1 1 d G . . C11H C 0.5328(13) 0.7115(8) 0.5346(8) 0.091(9) Uiso 1 1 d G . . C11I C 0.5230(13) 0.7107(9) 0.5979(9) 0.095(10) Uiso 1 1 d G . . C11J C 0.5149(14) 0.7692(11) 0.6313(6) 0.101(10) Uiso 1 1 d G . . C11K C 0.5165(14) 0.8284(9) 0.6012(8) 0.104(10) Uiso 1 1 d G . . C11L C 0.5263(13) 0.8291(8) 0.5379(8) 0.079(8) Uiso 1 1 d G . . C11G C 0.5345(13) 0.7707(10) 0.5045(6) 0.070(8) Uiso 1 1 d G . . H11F H 0.5385 0.6711 0.5115 0.084 Uiso 1 1 calc G . . H11G H 0.5219 0.6698 0.6186 0.084 Uiso 1 1 d G . . H11H H 0.5081 0.7687 0.6750 0.084 Uiso 1 1 d G . . H11I H 0.5109 0.8687 0.6243 0.084 Uiso 1 1 d G . . H11J H 0.5274 0.8700 0.5172 0.084 Uiso 1 1 d G . . C12B C 0.6378(11) 0.7366(7) 0.2537(7) 0.078(8) Uiso 1 1 d G . . C12C C 0.6807(9) 0.6877(10) 0.2369(8) 0.086(9) Uiso 1 1 d G . . C12D C 0.6205(13) 0.6173(9) 0.2158(8) 0.112(11) Uiso 1 1 d G . . C12E C 0.5174(13) 0.5958(7) 0.2115(8) 0.087(9) Uiso 1 1 d G . . C12F C 0.4745(9) 0.6446(9) 0.2282(7) 0.063(7) Uiso 1 1 d G . . C12A C 0.5347(12) 0.7151(8) 0.2493(7) 0.060(7) Uiso 1 1 d G . . H12A H 0.6794 0.7852 0.2682 0.072 Uiso 1 1 calc G . . H12B H 0.7519 0.7026 0.2400 0.072 Uiso 1 1 d G . . H12C H 0.6501 0.5836 0.2043 0.072 Uiso 1 1 d G . . H12D H 0.4758 0.5471 0.1969 0.072 Uiso 1 1 d G . . H12E H 0.4033 0.6297 0.2252 0.072 Uiso 1 1 d G . . C12H C 0.3421(10) 0.7416(7) 0.1574(6) 0.046(6) Uiso 1 1 d G . . C12I C 0.3045(10) 0.7486(8) 0.0965(6) 0.074(8) Uiso 1 1 d G . . C12J C 0.3524(12) 0.8088(9) 0.0685(5) 0.077(8) Uiso 1 1 d G . . C12K C 0.4379(12) 0.8620(8) 0.1016(7) 0.100(10) Uiso 1 1 d G . . C12L C 0.4755(9) 0.8549(7) 0.1626(7) 0.068(7) Uiso 1 1 d G . . C12G C 0.4276(10) 0.7948(8) 0.1905(5) 0.040(6) Uiso 1 1 d G . . H12F H 0.3090 0.7000 0.1767 0.048 Uiso 1 1 calc G . . H12G H 0.2454 0.7119 0.0736 0.048 Uiso 1 1 d G . . H12H H 0.3264 0.8136 0.0264 0.048 Uiso 1 1 d G . . H12I H 0.4710 0.9035 0.0823 0.048 Uiso 1 1 d G . . H12J H 0.5346 0.8917 0.1854 0.048 Uiso 1 1 d G . . C21B C 0.2785(14) 0.6412(9) 0.5280(8) 0.079(8) Uiso 1 1 d G . . C21C C 0.2995(16) 0.5884(12) 0.5585(7) 0.145(14) Uiso 1 1 d G . . C21D C 0.3011(17) 0.5285(10) 0.5235(11) 0.141(14) Uiso 1 1 d G . . C21E C 0.2817(16) 0.5216(9) 0.4580(11) 0.125(12) Uiso 1 1 d G . . C21F C 0.2606(15) 0.5744(11) 0.4275(7) 0.112(11) Uiso 1 1 d G . . C21A C 0.2590(14) 0.6342(9) 0.4624(9) 0.070(8) Uiso 1 1 d G . . H21A H 0.2774 0.6825 0.5521 0.084 Uiso 1 1 calc G . . H21B H 0.3130 0.5932 0.6038 0.084 Uiso 1 1 d G . . H21C H 0.3156 0.4920 0.5446 0.084 Uiso 1 1 d G . . H21D H 0.2828 0.4803 0.4338 0.084 Uiso 1 1 d G . . H21E H 0.2472 0.5696 0.3822 0.084 Uiso 1 1 d G . . C21H C 0.0755(14) 0.7104(9) 0.4784(8) 0.105(10) Uiso 1 1 d G . . C21I C 0.0323(12) 0.7333(11) 0.5253(10) 0.131(13) Uiso 1 1 d G . . C21J C 0.0902(17) 0.7902(12) 0.5704(8) 0.120(12) Uiso 1 1 d G . . C21K C 0.1913(16) 0.8242(9) 0.5686(8) 0.110(11) Uiso 1 1 d G . . C21L C 0.2346(11) 0.8013(10) 0.5218(10) 0.128(12) Uiso 1 1 d G . . C21G C 0.1767(14) 0.7444(10) 0.4766(8) 0.059(7) Uiso 1 1 d G . . H21F H 0.0356 0.6712 0.4472 0.071 Uiso 1 1 calc G . . H21G H -0.0376 0.7099 0.5265 0.071 Uiso 1 1 d G . . H21H H 0.0603 0.8060 0.6028 0.071 Uiso 1 1 d G . . H21I H 0.2313 0.8635 0.5998 0.071 Uiso 1 1 d G . . H21J H 0.3044 0.8247 0.5206 0.071 Uiso 1 1 d G . . C22B C 0.2232(10) 0.8635(7) 0.1861(7) 0.064(7) Uiso 1 1 d G . . C22C C 0.2473(12) 0.9141(9) 0.1442(6) 0.093(9) Uiso 1 1 d G . . C22D C 0.3250(13) 0.9792(8) 0.1631(7) 0.076(8) Uiso 1 1 d G . . C22E C 0.3786(11) 0.9937(7) 0.2240(8) 0.092(9) Uiso 1 1 d G . . C22F C 0.3546(11) 0.9430(8) 0.2659(6) 0.068(7) Uiso 1 1 d G . . C22A C 0.2769(11) 0.8780(7) 0.2469(6) 0.041(6) Uiso 1 1 d G . . H22A H 0.1696 0.8186 0.1730 0.049 Uiso 1 1 calc G . . H22B H 0.2102 0.9042 0.1021 0.049 Uiso 1 1 d G . . H22C H 0.3416 1.0142 0.1342 0.049 Uiso 1 1 d G . . H22D H 0.4323 1.0386 0.2371 0.049 Uiso 1 1 d G . . H22E H 0.3917 0.9530 0.3079 0.049 Uiso 1 1 d G . . C22H C 0.2395(8) 0.9034(8) 0.4013(7) 0.057(7) Uiso 1 1 d G . . C22I C 0.1936(10) 0.9342(7) 0.4411(6) 0.061(7) Uiso 1 1 d G . . C22J C 0.0900(11) 0.9100(8) 0.4341(7) 0.060(7) Uiso 1 1 d G . . C22K C 0.0323(8) 0.8549(9) 0.3873(8) 0.089(9) Uiso 1 1 d G . . C22L C 0.0782(10) 0.8240(7) 0.3476(7) 0.079(8) Uiso 1 1 d G . . C22G C 0.1818(11) 0.8482(8) 0.3546(6) 0.044(6) Uiso 1 1 d G . . H22F H 0.3111 0.9201 0.4062 0.053 Uiso 1 1 calc G . . H22G H 0.2335 0.9723 0.4733 0.053 Uiso 1 1 d G . . H22H H 0.0583 0.9313 0.4615 0.053 Uiso 1 1 d G . . H22I H -0.0393 0.8381 0.3825 0.053 Uiso 1 1 d G . . H22J H 0.0383 0.7859 0.3153 0.053 Uiso 1 1 d G . . C31B C -0.1440(11) 0.7602(6) -0.3395(7) 0.059(7) Uiso 1 1 d G . . C31C C -0.1747(10) 0.7796(8) -0.3972(6) 0.076(8) Uiso 1 1 d G . . C31D C -0.1277(12) 0.8481(9) -0.4119(6) 0.080(8) Uiso 1 1 d G . . C31E C -0.0502(12) 0.8974(7) -0.3690(7) 0.073(8) Uiso 1 1 d G . . C31F C -0.0195(10) 0.8780(7) -0.3113(7) 0.072(8) Uiso 1 1 d G . . C31A C -0.0664(11) 0.8095(8) -0.2966(5) 0.041(6) Uiso 1 1 d G . . H31A H -0.1764 0.7129 -0.3294 0.049 Uiso 1 1 calc G . . H31B H -0.2282 0.7456 -0.4269 0.049 Uiso 1 1 d G . . H31C H -0.1489 0.8615 -0.4517 0.049 Uiso 1 1 d G . . H31D H -0.0178 0.9447 -0.3792 0.049 Uiso 1 1 d G . . H31E H 0.0341 0.9121 -0.2816 0.049 Uiso 1 1 d G . . C31H C 0.1433(12) 0.7419(8) -0.2585(8) 0.089(9) Uiso 1 1 d G . . C31I C 0.1850(10) 0.6967(11) -0.2849(9) 0.100(10) Uiso 1 1 d G . . C31J C 0.1241(15) 0.6284(10) -0.3124(9) 0.126(12) Uiso 1 1 d G . . C31K C 0.0215(14) 0.6054(7) -0.3134(8) 0.095(10) Uiso 1 1 d G . . C31L C -0.0202(10) 0.6506(9) -0.2869(8) 0.077(8) Uiso 1 1 d G . . C31G C 0.0407(12) 0.7188(8) -0.2594(7) 0.052(6) Uiso 1 1 d G . . H31F H 0.1854 0.7890 -0.2395 0.063 Uiso 1 1 calc G . . H31G H 0.2558 0.7126 -0.2843 0.063 Uiso 1 1 d G . . H31H H 0.1529 0.5972 -0.3307 0.063 Uiso 1 1 d G . . H31I H -0.0205 0.5582 -0.3324 0.063 Uiso 1 1 d G . . H31J H -0.0910 0.6347 -0.2876 0.063 Uiso 1 1 d G . . C32B C 0.2033(10) 0.6984(6) -0.1057(6) 0.054(6) Uiso 1 1 d G . . C32C C 0.2554(8) 0.6567(8) -0.1251(7) 0.074(8) Uiso 1 1 d G . . C32D C 0.2037(12) 0.5872(8) -0.1532(7) 0.079(8) Uiso 1 1 d G . . C32E C 0.0999(12) 0.5593(6) -0.1618(7) 0.077(8) Uiso 1 1 d G . . C32F C 0.0479(8) 0.6009(8) -0.1424(7) 0.069(8) Uiso 1 1 d G . . C32A C 0.0996(10) 0.6705(7) -0.1143(7) 0.040(6) Uiso 1 1 d G . . H32A H 0.2391 0.7464 -0.0863 0.048 Uiso 1 1 calc G . . H32B H 0.3271 0.6760 -0.1190 0.048 Uiso 1 1 d G . . H32C H 0.2396 0.5584 -0.1666 0.048 Uiso 1 1 d G . . H32D H 0.0642 0.5112 -0.1812 0.048 Uiso 1 1 d G . . H32E H -0.0238 0.5816 -0.1485 0.048 Uiso 1 1 d G . . C32H C 0.0234(14) 0.6340(9) 0.0099(8) 0.094(9) Uiso 1 1 d G . . C32I C 0.0118(14) 0.6143(8) 0.0699(10) 0.134(13) Uiso 1 1 d G . . C32J C -0.0040(14) 0.6597(10) 0.1153(7) 0.091(9) Uiso 1 1 d G . . C32K C -0.0083(13) 0.7246(9) 0.1005(7) 0.086(9) Uiso 1 1 d G . . C32L C 0.0032(13) 0.7443(8) 0.0405(8) 0.076(8) Uiso 1 1 d G . . C32G C 0.0191(13) 0.6990(10) -0.0048(6) 0.069(8) Uiso 1 1 d G . . H32F H 0.0344 0.6027 -0.0214 0.083 Uiso 1 1 calc G . . H32G H 0.0148 0.5695 0.0801 0.083 Uiso 1 1 d G . . H32H H -0.0121 0.6461 0.1567 0.083 Uiso 1 1 d G . . H32I H -0.0193 0.7560 0.1318 0.083 Uiso 1 1 d G . . H32J H 0.0003 0.7892 0.0304 0.083 Uiso 1 1 d G . . C41B C -0.2535(12) 0.5236(9) -0.0991(6) 0.068(7) Uiso 1 1 d G . . C41C C -0.2366(13) 0.4660(8) -0.0748(8) 0.091(9) Uiso 1 1 d G . . C41D C -0.2218(14) 0.4641(8) -0.0099(9) 0.110(11) Uiso 1 1 d G . . C41E C -0.2239(13) 0.5199(10) 0.0306(6) 0.083(9) Uiso 1 1 d G . . C41F C -0.2407(12) 0.5775(8) 0.0063(7) 0.073(8) Uiso 1 1 d G . . C41A C -0.2555(12) 0.5794(7) -0.0585(7) 0.051(6) Uiso 1 1 d G . . H41A H -0.2637 0.5249 -0.1439 0.061 Uiso 1 1 calc G . . H41B H -0.2352 0.4275 -0.1028 0.061 Uiso 1 1 d G . . H41C H -0.2102 0.4244 0.0068 0.061 Uiso 1 1 d G . . H41D H -0.2137 0.5186 0.0754 0.061 Uiso 1 1 d G . . H41E H -0.2422 0.6160 0.0343 0.061 Uiso 1 1 d G . . C41H C -0.2979(10) 0.7275(9) 0.0179(8) 0.086(9) Uiso 1 1 d G . . C41I C -0.3524(14) 0.7405(9) 0.0627(7) 0.096(10) Uiso 1 1 d G . . C41J C -0.4559(14) 0.7083(11) 0.0522(8) 0.118(12) Uiso 1 1 d G . . C41K C -0.5049(10) 0.6632(10) -0.0030(10) 0.111(11) Uiso 1 1 d G . . C41L C -0.4504(13) 0.6503(9) -0.0478(7) 0.101(10) Uiso 1 1 d G . . C41G C -0.3469(12) 0.6824(9) -0.0373(7) 0.051(6) Uiso 1 1 d G . . H41F H -0.2264 0.7497 0.0251 0.061 Uiso 1 1 calc G . . H41G H -0.3185 0.7716 0.1008 0.061 Uiso 1 1 d G . . H41H H -0.4935 0.7173 0.0832 0.061 Uiso 1 1 d G . . H41I H -0.5764 0.6411 -0.0102 0.061 Uiso 1 1 d G . . H41J H -0.4843 0.6191 -0.0859 0.061 Uiso 1 1 d G . . C42B C -0.2497(11) 0.8793(8) -0.2810(7) 0.076(8) Uiso 1 1 d G . . C42C C -0.2158(14) 0.9422(10) -0.3082(6) 0.092(9) Uiso 1 1 d G . . C42D C -0.1399(15) 1.0017(8) -0.2743(9) 0.112(11) Uiso 1 1 d G . . C42E C -0.0980(12) 0.9983(8) -0.2133(9) 0.116(12) Uiso 1 1 d G . . C42F C -0.1319(12) 0.9354(10) -0.1861(6) 0.072(8) Uiso 1 1 d G . . C42A C -0.2078(12) 0.8759(7) -0.2200(7) 0.052(6) Uiso 1 1 d G . . H42A H -0.3021 0.8382 -0.3043 0.062 Uiso 1 1 calc G . . H42B H -0.2447 0.9446 -0.3503 0.062 Uiso 1 1 d G . . H42C H -0.1165 1.0451 -0.2931 0.062 Uiso 1 1 d G . . H42D H -0.0456 1.0394 -0.1900 0.062 Uiso 1 1 d G . . H42E H -0.1030 0.9330 -0.1440 0.062 Uiso 1 1 d G . . C42H C -0.2671(9) 0.8707(9) -0.0691(7) 0.062(7) Uiso 1 1 d G . . C42I C -0.3183(12) 0.8970(8) -0.0297(6) 0.085(9) Uiso 1 1 d G . . C42J C -0.4216(12) 0.8759(9) -0.0437(8) 0.079(8) Uiso 1 1 d G . . C42K C -0.4737(9) 0.8285(10) -0.0972(8) 0.106(10) Uiso 1 1 d G . . C42L C -0.4226(12) 0.8022(8) -0.1365(7) 0.078(8) Uiso 1 1 d G . . C42G C -0.3193(12) 0.8233(8) -0.1225(7) 0.057(7) Uiso 1 1 d G . . H42F H -0.1957 0.8852 -0.0593 0.068 Uiso 1 1 calc G . . H42G H -0.2823 0.9297 0.0072 0.068 Uiso 1 1 d G . . H42H H -0.4569 0.8941 -0.0166 0.068 Uiso 1 1 d G . . H42I H -0.5451 0.8140 -0.1069 0.068 Uiso 1 1 d G . . H42J H -0.4586 0.7695 -0.1735 0.068 Uiso 1 1 d G . . Cl1 Cl 0.6157(15) 0.1377(10) 0.2642(10) 0.220(8) Uani 0.80 1 d P . . Cl2 Cl 0.7305(17) 0.0487(13) 0.2737(10) 0.248(10) Uani 0.80 1 d P . . C9 C 0.616(5) 0.045(4) 0.248(3) 0.26(5) Uani 0.80 1 d P . . H9A H 0.5699 0.0128 0.2712 0.321 Uiso 0.80 1 d PR . . H9B H 0.5962 0.0295 0.2040 0.321 Uiso 0.80 1 d PR . . Cl3 Cl 0.1252(16) 0.1551(14) 0.7830(13) 0.242(11) Uani 0.70 1 d PU . . Cl3A Cl 0.129(4) 0.122(3) 0.879(3) 0.24(3) Uani 0.30 1 d PDU . . Cl4 Cl 0.224(5) 0.062(4) 0.837(3) 0.33(4) Uani 0.70 1 d PDU . . Cl4A Cl 0.245(8) 0.085(4) 0.795(6) 0.51(8) Uani 0.30 1 d PD . . C10 C 0.158(4) 0.080(3) 0.773(2) 0.107(15) Uiso 0.70 1 d PD . . H10A H 0.1045 0.0381 0.7528 0.129 Uiso 0.70 1 d PR . . H10B H 0.2094 0.0937 0.7480 0.129 Uiso 0.70 1 d PR . . C10A C 0.165(4) 0.054(3) 0.847(3) 0.038(15) Uiso 0.30 1 d PD . . H10C H 0.1093 0.0176 0.8210 0.122 Uiso 0.30 1 d PR . . H10D H 0.1903 0.0340 0.8810 0.122 Uiso 0.30 1 d PR . . O7 O -0.039(8) 0.508(5) 0.461(4) 0.47(5) Uani 1 1 d DU . . H7 H -0.035(15) 0.547(10) 0.435(7) 0.560 Uiso 1 1 d D . . H8 H -0.013(16) 0.473(8) 0.476(11) 0.560 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.058(2) 0.079(3) 0.051(2) -0.0077(19) -0.0062(17) 0.022(2) Co2 0.068(2) 0.048(2) 0.089(3) 0.021(2) 0.030(2) 0.021(2) Co3 0.075(3) 0.115(3) 0.048(2) -0.004(2) -0.0052(19) 0.052(3) Co4 0.066(2) 0.049(2) 0.076(2) 0.0129(19) 0.0172(19) 0.021(2) I1 0.0603(13) 0.0820(16) 0.1153(17) -0.0006(12) -0.0020(11) 0.0200(11) I2 0.0869(15) 0.0984(17) 0.0887(15) -0.0172(12) -0.0057(12) 0.0376(13) I3 0.0810(15) 0.0895(17) 0.158(2) -0.0131(15) 0.0560(15) 0.0150(13) I4 0.0791(13) 0.0680(14) 0.0841(13) 0.0055(10) 0.0182(10) 0.0282(11) I5 0.0767(14) 0.0972(17) 0.1095(17) 0.0063(13) -0.0145(12) 0.0376(13) I6 0.1147(19) 0.121(2) 0.1195(19) -0.0138(15) 0.0051(15) 0.0602(17) I7 0.0683(13) 0.1040(18) 0.0889(15) 0.0078(12) 0.0219(11) 0.0233(12) I8 0.0995(17) 0.0664(15) 0.170(2) -0.0132(14) 0.0541(16) 0.0209(13) P1 0.057(4) 0.102(6) 0.042(4) 0.010(4) -0.007(3) 0.045(4) P2 0.057(4) 0.054(5) 0.020(3) 0.006(3) 0.004(3) 0.011(4) P3 0.066(5) 0.074(6) 0.085(6) 0.046(5) 0.039(4) 0.037(5) P4 0.054(4) 0.033(4) 0.041(4) 0.016(3) 0.003(3) 0.018(3) P5 0.045(4) 0.050(4) 0.043(4) 0.009(3) 0.003(3) 0.017(4) P6 0.058(4) 0.082(5) 0.036(4) 0.007(3) -0.006(3) 0.041(4) P7 0.048(4) 0.072(5) 0.052(4) 0.021(4) 0.006(3) 0.012(4) P8 0.054(4) 0.035(4) 0.044(4) 0.018(3) 0.007(3) 0.024(3) O1 0.075(12) 0.061(12) 0.033(9) 0.008(8) 0.003(8) -0.002(10) O2 0.10(2) 0.10(2) 0.20(3) 0.03(2) 0.08(2) 0.030(19) O3 0.062(10) 0.032(10) 0.058(10) 0.027(8) 0.011(8) 0.013(9) O4 0.056(11) 0.102(15) 0.031(9) 0.013(9) 0.003(8) 0.020(11) O5 0.093(15) 0.094(16) 0.127(19) 0.061(14) 0.022(14) 0.024(13) O6 0.051(10) 0.045(10) 0.041(9) 0.008(8) -0.016(7) 0.017(8) C1 0.045(15) 0.055(17) 0.030(13) 0.013(11) -0.003(11) 0.006(13) C2 0.059(15) 0.053(15) 0.016(11) 0.012(10) -0.014(10) 0.020(13) C3 0.043(13) 0.054(13) 0.025(12) 0.014(10) 0.001(10) 0.005(11) C4 0.040(12) 0.007(11) 0.042(12) 0.002(9) 0.007(10) 0.011(10) C5 0.065(16) 0.029(14) 0.024(12) 0.017(11) -0.003(11) -0.004(13) C6 0.053(15) 0.043(15) 0.022(12) 0.017(10) -0.008(10) 0.027(12) C7 0.047(14) 0.061(17) 0.034(13) 0.019(12) -0.002(11) 0.036(13) C8 0.051(15) 0.047(15) 0.022(12) 0.012(11) 0.000(10) 0.025(13) Cl1 0.218(19) 0.187(18) 0.27(2) 0.019(16) 0.055(16) 0.092(15) Cl2 0.26(2) 0.30(3) 0.22(2) 0.036(18) 0.025(17) 0.15(2) C9 0.27(8) 0.47(13) 0.18(6) -0.05(7) -0.03(6) 0.33(9) Cl3 0.154(18) 0.23(3) 0.30(3) 0.07(2) 0.049(18) 0.014(17) Cl3A 0.21(5) 0.16(4) 0.26(5) -0.08(4) -0.08(4) 0.01(4) Cl4 0.33(8) 0.33(8) 0.35(6) 0.07(6) 0.02(6) 0.16(6) Cl4A 0.68(11) 0.31(7) 0.9(2) 0.39(10) 0.68(14) 0.38(8) O7 0.44(9) 0.44(8) 0.44(9) 0.05(8) 0.07(8) 0.06(7) _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 O1 1.973(13) . ? Co1 I1 2.541(4) . ? Co1 P1 2.556(8) . ? Co1 I2 2.560(4) . ? Co2 O2 1.849(16) . ? Co2 O3 1.972(14) . ? Co2 I4 2.545(4) . ? Co2 I3 2.552(3) . ? Co3 O4 1.991(14) . ? Co3 I6 2.545(4) . ? Co3 I5 2.559(4) . ? Co3 P6 2.599(7) . ? Co4 O5 1.940(15) . ? Co4 O6 1.981(14) . ? Co4 I8 2.542(4) . ? Co4 I7 2.542(3) . ? P1 C11G 1.774(15) . ? P1 C11A 1.845(13) . ? P1 C1 1.85(2) . ? P2 O1 1.499(16) . ? P2 C12A 1.769(14) . ? P2 C12G 1.769(12) . ? P2 C2 1.84(2) . ? P3 O2 1.402(15) . ? P3 C3 1.76(2) . ? P3 C21G 1.785(16) . ? P3 C21A 1.820(16) . ? P4 O3 1.495(15) . ? P4 C22G 1.764(12) . ? P4 C22A 1.786(13) . ? P4 C4 1.814(19) . ? P5 O4 1.468(16) . ? P5 C31A 1.803(12) . ? P5 C31G 1.814(14) . ? P5 C5 1.85(2) . ? P6 C32G 1.819(14) . ? P6 C32A 1.834(12) . ? P6 C6 1.826(19) . ? P7 O5 1.378(17) . ? P7 C41G 1.781(15) . ? P7 C7 1.80(2) . ? P7 C41A 1.820(14) . ? P8 O6 1.488(14) . ? P8 C42A 1.766(14) . ? P8 C42G 1.796(13) . ? P8 C8 1.834(19) . ? C1 C2 1.52(3) . ? C1 C3 1.58(3) . ? C1 H1A 0.9598 . ? C2 C4 1.51(3) . ? C2 H2A 0.9601 . ? C3 C4 1.62(3) . ? C3 H3A 0.9599 . ? C4 H4A 0.9601 . ? C5 C8 1.54(3) . ? C5 C6 1.56(3) . ? C5 H5A 0.9600 . ? C6 C7 1.57(3) . ? C6 H6A 0.9600 . ? C7 C8 1.57(3) . ? C7 H7A 0.9597 . ? C8 H8A 0.9601 . ? C11B C11C 1.3900 . ? C11B C11A 1.3900 . ? C11C C11D 1.3900 . ? C11C H11B 0.9598 . ? C11D C11E 1.3900 . ? C11D H11C 0.9601 . ? C11E C11F 1.3900 . ? C11E H11D 0.9601 . ? C11F C11A 1.3900 . ? C11F H11E 0.9599 . ? C11H C11I 1.3900 . ? C11H C11G 1.3900 . ? C11I C11J 1.3900 . ? C11I H11G 0.9598 . ? C11J C11K 1.3900 . ? C11J H11H 0.9600 . ? C11K C11L 1.3900 . ? C11K H11I 0.9597 . ? C11L C11G 1.3900 . ? C11L H11J 0.9600 . ? C12B C12C 1.3900 . ? C12B C12A 1.3900 . ? C12C C12D 1.3900 . ? C12C H12B 0.9600 . ? C12D C12E 1.3900 . ? C12D H12C 0.9600 . ? C12E C12F 1.3900 . ? C12E H12D 0.9601 . ? C12F C12A 1.3900 . ? C12F H12E 0.9600 . ? C12H C12I 1.3900 . ? C12H C12G 1.3900 . ? C12I C12J 1.3900 . ? C12I H12G 0.9600 . ? C12J C12K 1.3900 . ? C12J H12H 0.9599 . ? C12K C12L 1.3900 . ? C12K H12I 0.9601 . ? C12L C12G 1.3900 . ? C12L H12J 0.9599 . ? C21B C21C 1.3900 . ? C21B C21A 1.3900 . ? C21C C21D 1.3900 . ? C21C H21B 0.9601 . ? C21D C21E 1.3900 . ? C21D H21C 0.9600 . ? C21E C21F 1.3900 . ? C21E H21D 0.9602 . ? C21F C21A 1.3900 . ? C21F H21E 0.9602 . ? C21H C21I 1.3900 . ? C21H C21G 1.3900 . ? C21I C21J 1.3900 . ? C21I H21G 0.9601 . ? C21J C21K 1.3900 . ? C21J H21H 0.9602 . ? C21K C21L 1.3900 . ? C21K H21I 0.9601 . ? C21L C21G 1.3900 . ? C21L H21J 0.9601 . ? C22B C22C 1.3900 . ? C22B C22A 1.3900 . ? C22C C22D 1.3900 . ? C22C H22B 0.9603 . ? C22D C22E 1.3900 . ? C22D H22C 0.9601 . ? C22E C22F 1.3900 . ? C22E H22D 0.9600 . ? C22F C22A 1.3900 . ? C22F H22E 0.9599 . ? C22H C22I 1.3900 . ? C22H C22G 1.3900 . ? C22I C22J 1.3900 . ? C22I H22G 0.9602 . ? C22J C22K 1.3900 . ? C22J H22H 0.9598 . ? C22K C22L 1.3900 . ? C22K H22I 0.9601 . ? C22L C22G 1.3900 . ? C22L H22J 0.9600 . ? C31B C31C 1.3900 . ? C31B C31A 1.3900 . ? C31C C31D 1.3900 . ? C31C H31B 0.9599 . ? C31D C31E 1.3900 . ? C31D H31C 0.9601 . ? C31E C31F 1.3900 . ? C31E H31D 0.9601 . ? C31F C31A 1.3900 . ? C31F H31E 0.9601 . ? C31H C31I 1.3900 . ? C31H C31G 1.3900 . ? C31I C31J 1.3900 . ? C31I H31G 0.9599 . ? C31J C31K 1.3900 . ? C31J H31H 0.9601 . ? C31K C31L 1.3900 . ? C31K H31I 0.9601 . ? C31L C31G 1.3900 . ? C31L H31J 0.9603 . ? C32B C32C 1.3900 . ? C32B C32A 1.3900 . ? C32C C32D 1.3900 . ? C32C H32B 0.9599 . ? C32D C32E 1.3900 . ? C32D H32C 0.9598 . ? C32E C32F 1.3900 . ? C32E H32D 0.9601 . ? C32F C32A 1.3900 . ? C32F H32E 0.9601 . ? C32H C32I 1.3900 . ? C32H C32G 1.3900 . ? C32I C32J 1.3900 . ? C32I H32G 0.9600 . ? C32J C32K 1.3900 . ? C32J H32H 0.9597 . ? C32K C32L 1.3900 . ? C32K H32I 0.9601 . ? C32L C32G 1.3900 . ? C32L H32J 0.9600 . ? C41B C41C 1.3900 . ? C41B C41A 1.3900 . ? C41C C41D 1.3900 . ? C41C H41B 0.9601 . ? C41D C41E 1.3900 . ? C41D H41C 0.9598 . ? C41E C41F 1.3900 . ? C41E H41D 0.9599 . ? C41F C41A 1.3900 . ? C41F H41E 0.9601 . ? C41H C41I 1.3900 . ? C41H C41G 1.3900 . ? C41I C41J 1.3900 . ? C41I H41G 0.9601 . ? C41J C41K 1.3900 . ? C41J H41H 0.9602 . ? C41K C41L 1.3900 . ? C41K H41I 0.9600 . ? C41L C41G 1.3900 . ? C41L H41J 0.9596 . ? C42B C42C 1.3900 . ? C42B C42A 1.3900 . ? C42C C42D 1.3900 . ? C42C H42B 0.9600 . ? C42D C42E 1.3900 . ? C42D H42C 0.9599 . ? C42E C42F 1.3900 . ? C42E H42D 0.9601 . ? C42F C42A 1.3900 . ? C42F H42E 0.9598 . ? C42H C42I 1.3900 . ? C42H C42G 1.3900 . ? C42I C42J 1.3900 . ? C42I H42G 0.9600 . ? C42J C42K 1.3900 . ? C42J H42H 0.9596 . ? C42K C42L 1.3900 . ? C42K H42I 0.9598 . ? C42L C42G 1.3900 . ? C42L H42J 0.9600 . ? Cl1 C9 1.89(7) . ? Cl2 C9 1.65(5) . ? C9 H9A 0.9601 . ? C9 H9B 0.9600 . ? Cl3 C10 1.74(5) . ? Cl3 Cl3A 2.21(7) . ? Cl3A C10A 1.75(2) . ? Cl3A Cl4 2.36(8) . ? Cl4 C10A 0.89(10) . ? Cl4 Cl4A 1.06(11) . ? Cl4 C10 1.70(2) . ? Cl4 H10C 1.5695 . ? Cl4 H10D 1.2161 . ? Cl4A C10 1.26(12) . ? Cl4A C10A 1.71(3) . ? Cl4A H10B 1.1261 . ? C10 C10A 1.70(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9599 . ? C10A H10C 0.9599 . ? C10A H10D 0.9501 . ? O7 H7 0.98(11) . ? O7 H8 0.96(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 O1 Co1 I1 116.8(5) . . ? O1 Co1 P1 93.0(4) . . ? I1 Co1 P1 112.7(2) . . ? O1 Co1 I2 109.4(4) . . ? I1 Co1 I2 111.86(15) . . ? P1 Co1 I2 111.8(2) . . ? O2 Co2 O3 104.1(9) . . ? O2 Co2 I4 111.9(9) . . ? O3 Co2 I4 108.2(5) . . ? O2 Co2 I3 101.2(7) . . ? O3 Co2 I3 114.9(4) . . ? I4 Co2 I3 115.80(15) . . ? O4 Co3 I6 114.8(5) . . ? O4 Co3 I5 112.9(5) . . ? I6 Co3 I5 110.06(16) . . ? O4 Co3 P6 92.4(5) . . ? I6 Co3 P6 106.7(2) . . ? I5 Co3 P6 119.2(2) . . ? O5 Co4 O6 97.9(7) . . ? O5 Co4 I8 104.2(7) . . ? O6 Co4 I8 111.3(5) . . ? O5 Co4 I7 113.6(6) . . ? O6 Co4 I7 113.2(4) . . ? I8 Co4 I7 115.03(15) . . ? C11G P1 C11A 104.4(8) . . ? C11G P1 C1 105.8(9) . . ? C11A P1 C1 104.7(9) . . ? C11G P1 Co1 118.9(7) . . ? C11A P1 Co1 114.9(6) . . ? C1 P1 Co1 106.9(7) . . ? O1 P2 C12A 113.3(9) . . ? O1 P2 C12G 109.6(8) . . ? C12A P2 C12G 107.2(7) . . ? O1 P2 C2 109.6(9) . . ? C12A P2 C2 109.0(9) . . ? C12G P2 C2 108.0(8) . . ? O2 P3 C3 124.5(12) . . ? O2 P3 C21G 100.0(13) . . ? C3 P3 C21G 113.1(10) . . ? O2 P3 C21A 103.3(13) . . ? C3 P3 C21A 107.9(9) . . ? C21G P3 C21A 106.4(9) . . ? O3 P4 C22G 111.2(9) . . ? O3 P4 C22A 110.5(8) . . ? C22G P4 C22A 106.3(7) . . ? O3 P4 C4 113.7(8) . . ? C22G P4 C4 107.2(8) . . ? C22A P4 C4 107.6(8) . . ? O4 P5 C31A 110.0(9) . . ? O4 P5 C31G 113.9(9) . . ? C31A P5 C31G 105.2(7) . . ? O4 P5 C5 111.7(9) . . ? C31A P5 C5 107.3(8) . . ? C31G P5 C5 108.4(9) . . ? C32G P6 C32A 103.8(8) . . ? C32G P6 C6 104.2(9) . . ? C32A P6 C6 106.3(8) . . ? C32G P6 Co3 121.8(7) . . ? C32A P6 Co3 113.1(6) . . ? C6 P6 Co3 106.4(7) . . ? O5 P7 C41G 114.0(11) . . ? O5 P7 C7 112.0(11) . . ? C41G P7 C7 111.4(10) . . ? O5 P7 C41A 105.6(10) . . ? C41G P7 C41A 105.9(8) . . ? C7 P7 C41A 107.3(8) . . ? O6 P8 C42A 109.7(8) . . ? O6 P8 C42G 114.0(9) . . ? C42A P8 C42G 106.2(8) . . ? O6 P8 C8 111.4(9) . . ? C42A P8 C8 107.6(9) . . ? C42G P8 C8 107.7(8) . . ? P2 O1 Co1 133.7(9) . . ? P3 O2 Co2 140.6(15) . . ? P4 O3 Co2 130.0(8) . . ? P5 O4 Co3 133.2(10) . . ? P7 O5 Co4 152.0(14) . . ? P8 O6 Co4 136.0(8) . . ? C2 C1 C3 88.5(15) . . ? C2 C1 P1 121.1(16) . . ? C3 C1 P1 112.4(14) . . ? C2 C1 H1A 111.3 . . ? C3 C1 H1A 111.0 . . ? P1 C1 H1A 110.6 . . ? C4 C2 C1 92.6(15) . . ? C4 C2 P2 119.5(15) . . ? C1 C2 P2 119.4(15) . . ? C4 C2 H2A 107.6 . . ? C1 C2 H2A 108.3 . . ? P2 C2 H2A 108.0 . . ? C1 C3 C4 86.5(14) . . ? C1 C3 P3 117.5(14) . . ? C4 C3 P3 121.9(12) . . ? C1 C3 H3A 110.1 . . ? C4 C3 H3A 110.4 . . ? P3 C3 H3A 108.7 . . ? C2 C4 C3 87.5(13) . . ? C2 C4 P4 120.0(13) . . ? C3 C4 P4 122.0(13) . . ? C2 C4 H4A 108.5 . . ? C3 C4 H4A 108.7 . . ? P4 C4 H4A 108.4 . . ? C8 C5 C6 89.0(14) . . ? C8 C5 P5 118.3(15) . . ? C6 C5 P5 118.6(15) . . ? C8 C5 H5A 109.7 . . ? C6 C5 H5A 110.1 . . ? P5 C5 H5A 109.6 . . ? C5 C6 C7 88.2(14) . . ? C5 C6 P6 121.9(15) . . ? C7 C6 P6 114.7(13) . . ? C5 C6 H6A 110.6 . . ? C7 C6 H6A 109.3 . . ? P6 C6 H6A 110.0 . . ? C6 C7 C8 87.7(14) . . ? C6 C7 P7 116.8(15) . . ? C8 C7 P7 121.2(13) . . ? C6 C7 H7A 109.8 . . ? C8 C7 H7A 109.4 . . ? P7 C7 H7A 110.0 . . ? C5 C8 C7 88.8(14) . . ? C5 C8 P8 116.4(13) . . ? C7 C8 P8 125.1(15) . . ? C5 C8 H8A 107.5 . . ? C7 C8 H8A 109.5 . . ? P8 C8 H8A 107.7 . . ? C11C C11B C11A 120.0 . . ? C11B C11C C11D 120.0 . . ? C11B C11C H11B 120.0 . . ? C11D C11C H11B 120.0 . . ? C11C C11D C11E 120.0 . . ? C11C C11D H11C 120.0 . . ? C11E C11D H11C 120.0 . . ? C11F C11E C11D 120.0 . . ? C11F C11E H11D 120.0 . . ? C11D C11E H11D 120.0 . . ? C11E C11F C11A 120.0 . . ? C11E C11F H11E 120.0 . . ? C11A C11F H11E 120.0 . . ? C11F C11A C11B 120.0 . . ? C11F C11A P1 124.8(9) . . ? C11B C11A P1 115.2(9) . . ? C11F C11A H11A 144.0 . . ? C11B C11A H11A 24.0 . . ? P1 C11A H11A 91.3 . . ? C11I C11H C11G 120.0 . . ? C11H C11I C11J 120.0 . . ? C11H C11I H11G 120.0 . . ? C11J C11I H11G 120.0 . . ? C11I C11J C11K 120.0 . . ? C11I C11J H11H 120.0 . . ? C11K C11J H11H 120.0 . . ? C11J C11K C11L 120.0 . . ? C11J C11K H11I 120.0 . . ? C11L C11K H11I 120.0 . . ? C11G C11L C11K 120.0 . . ? C11G C11L H11J 120.0 . . ? C11K C11L H11J 120.0 . . ? C11L C11G C11H 120.0 . . ? C11L C11G P1 120.1(11) . . ? C11H C11G P1 119.9(11) . . ? C11L C11G H11F 144.0 . . ? C11H C11G H11F 24.0 . . ? P1 C11G H11F 95.9 . . ? C12C C12B C12A 120.0 . . ? C12D C12C C12B 120.0 . . ? C12D C12C H12B 120.0 . . ? C12B C12C H12B 120.0 . . ? C12E C12D C12C 120.0 . . ? C12E C12D H12C 120.0 . . ? C12C C12D H12C 120.0 . . ? C12D C12E C12F 120.0 . . ? C12D C12E H12D 120.0 . . ? C12F C12E H12D 120.0 . . ? C12A C12F C12E 120.0 . . ? C12A C12F H12E 120.0 . . ? C12E C12F H12E 120.0 . . ? C12F C12A C12B 120.0 . . ? C12F C12A P2 123.0(10) . . ? C12B C12A P2 116.7(10) . . ? C12F C12A H12A 144.0 . . ? C12B C12A H12A 24.0 . . ? P2 C12A H12A 92.9 . . ? C12I C12H C12G 120.0 . . ? C12H C12I C12J 120.0 . . ? C12H C12I H12G 120.0 . . ? C12J C12I H12G 120.0 . . ? C12I C12J C12K 120.0 . . ? C12I C12J H12H 120.0 . . ? C12K C12J H12H 120.0 . . ? C12L C12K C12J 120.0 . . ? C12L C12K H12I 120.0 . . ? C12J C12K H12I 120.0 . . ? C12K C12L C12G 120.0 . . ? C12K C12L H12J 120.0 . . ? C12G C12L H12J 120.0 . . ? C12L C12G C12H 120.0 . . ? C12L C12G P2 118.5(9) . . ? C12H C12G P2 121.0(9) . . ? C12L C12G H12F 144.0 . . ? C12H C12G H12F 24.0 . . ? P2 C12G H12F 97.2 . . ? C21C C21B C21A 120.0 . . ? C21D C21C C21B 120.0 . . ? C21D C21C H21B 120.0 . . ? C21B C21C H21B 120.0 . . ? C21C C21D C21E 120.0 . . ? C21C C21D H21C 120.0 . . ? C21E C21D H21C 120.0 . . ? C21F C21E C21D 120.0 . . ? C21F C21E H21D 120.0 . . ? C21D C21E H21D 120.0 . . ? C21E C21F C21A 120.0 . . ? C21E C21F H21E 120.0 . . ? C21A C21F H21E 120.0 . . ? C21F C21A C21B 120.0 . . ? C21F C21A P3 120.6(12) . . ? C21B C21A P3 119.4(12) . . ? C21F C21A H21A 144.0 . . ? C21B C21A H21A 24.0 . . ? P3 C21A H21A 95.4 . . ? C21I C21H C21G 120.0 . . ? C21H C21I C21J 120.0 . . ? C21H C21I H21G 120.0 . . ? C21J C21I H21G 120.0 . . ? C21I C21J C21K 120.0 . . ? C21I C21J H21H 120.0 . . ? C21K C21J H21H 120.0 . . ? C21J C21K C21L 120.0 . . ? C21J C21K H21I 120.0 . . ? C21L C21K H21I 120.0 . . ? C21G C21L C21K 120.0 . . ? C21G C21L H21J 120.0 . . ? C21K C21L H21J 120.0 . . ? C21L C21G C21H 120.0 . . ? C21L C21G P3 121.9(12) . . ? C21H C21G P3 117.4(12) . . ? C21L C21G H21F 144.0 . . ? C21H C21G H21F 24.0 . . ? P3 C21G H21F 93.7 . . ? C22C C22B C22A 120.0 . . ? C22B C22C C22D 120.0 . . ? C22B C22C H22B 120.0 . . ? C22D C22C H22B 120.0 . . ? C22E C22D C22C 120.0 . . ? C22E C22D H22C 120.0 . . ? C22C C22D H22C 120.0 . . ? C22F C22E C22D 120.0 . . ? C22F C22E H22D 120.0 . . ? C22D C22E H22D 120.0 . . ? C22E C22F C22A 120.0 . . ? C22E C22F H22E 120.0 . . ? C22A C22F H22E 120.0 . . ? C22F C22A C22B 120.0 . . ? C22F C22A P4 122.8(9) . . ? C22B C22A P4 117.1(9) . . ? C22F C22A H22A 144.0 . . ? C22B C22A H22A 24.0 . . ? P4 C22A H22A 93.2 . . ? C22I C22H C22G 120.0 . . ? C22J C22I C22H 120.0 . . ? C22J C22I H22G 120.0 . . ? C22H C22I H22G 120.0 . . ? C22K C22J C22I 120.0 . . ? C22K C22J H22H 120.0 . . ? C22I C22J H22H 120.0 . . ? C22J C22K C22L 120.0 . . ? C22J C22K H22I 120.0 . . ? C22L C22K H22I 120.0 . . ? C22G C22L C22K 120.0 . . ? C22G C22L H22J 120.0 . . ? C22K C22L H22J 120.0 . . ? C22L C22G C22H 120.0 . . ? C22L C22G P4 118.4(9) . . ? C22H C22G P4 121.4(9) . . ? C22L C22G H22F 144.0 . . ? C22H C22G H22F 24.0 . . ? P4 C22G H22F 97.6 . . ? C31C C31B C31A 120.0 . . ? C31D C31C C31B 120.0 . . ? C31D C31C H31B 120.0 . . ? C31B C31C H31B 120.0 . . ? C31C C31D C31E 120.0 . . ? C31C C31D H31C 120.0 . . ? C31E C31D H31C 120.0 . . ? C31D C31E C31F 120.0 . . ? C31D C31E H31D 120.0 . . ? C31F C31E H31D 120.0 . . ? C31A C31F C31E 120.0 . . ? C31A C31F H31E 120.0 . . ? C31E C31F H31E 120.0 . . ? C31F C31A C31B 120.0 . . ? C31F C31A P5 118.6(9) . . ? C31B C31A P5 120.4(9) . . ? C31F C31A H31A 144.0 . . ? C31B C31A H31A 24.0 . . ? P5 C31A H31A 96.9 . . ? C31I C31H C31G 120.0 . . ? C31J C31I C31H 120.0 . . ? C31J C31I H31G 120.0 . . ? C31H C31I H31G 120.0 . . ? C31K C31J C31I 120.0 . . ? C31K C31J H31H 120.0 . . ? C31I C31J H31H 120.0 . . ? C31J C31K C31L 120.0 . . ? C31J C31K H31I 120.0 . . ? C31L C31K H31I 120.0 . . ? C31G C31L C31K 120.0 . . ? C31G C31L H31J 120.0 . . ? C31K C31L H31J 120.0 . . ? C31L C31G C31H 120.0 . . ? C31L C31G P5 121.6(10) . . ? C31H C31G P5 118.3(10) . . ? C31L C31G H31F 144.0 . . ? C31H C31G H31F 24.0 . . ? P5 C31G H31F 94.4 . . ? C32C C32B C32A 120.0 . . ? C32B C32C C32D 120.0 . . ? C32B C32C H32B 120.0 . . ? C32D C32C H32B 120.0 . . ? C32C C32D C32E 120.0 . . ? C32C C32D H32C 120.0 . . ? C32E C32D H32C 120.0 . . ? C32D C32E C32F 120.0 . . ? C32D C32E H32D 120.0 . . ? C32F C32E H32D 120.0 . . ? C32E C32F C32A 120.0 . . ? C32E C32F H32E 120.0 . . ? C32A C32F H32E 120.0 . . ? C32F C32A C32B 120.0 . . ? C32F C32A P6 123.2(9) . . ? C32B C32A P6 116.6(9) . . ? C32F C32A H32A 144.0 . . ? C32B C32A H32A 24.0 . . ? P6 C32A H32A 92.7 . . ? C32I C32H C32G 120.0 . . ? C32J C32I C32H 120.0 . . ? C32J C32I H32G 120.0 . . ? C32H C32I H32G 120.0 . . ? C32K C32J C32I 120.0 . . ? C32K C32J H32H 120.0 . . ? C32I C32J H32H 120.0 . . ? C32L C32K C32J 120.0 . . ? C32L C32K H32I 120.0 . . ? C32J C32K H32I 120.0 . . ? C32K C32L C32G 120.0 . . ? C32K C32L H32J 120.0 . . ? C32G C32L H32J 120.0 . . ? C32L C32G C32H 120.0 . . ? C32L C32G P6 119.1(11) . . ? C32H C32G P6 120.9(11) . . ? C32L C32G H32F 144.0 . . ? C32H C32G H32F 24.0 . . ? P6 C32G H32F 97.0 . . ? C41C C41B C41A 120.0 . . ? C41D C41C C41B 120.0 . . ? C41D C41C H41B 120.0 . . ? C41B C41C H41B 120.0 . . ? C41E C41D C41C 120.0 . . ? C41E C41D H41C 120.0 . . ? C41C C41D H41C 120.0 . . ? C41D C41E C41F 120.0 . . ? C41D C41E H41D 120.0 . . ? C41F C41E H41D 120.0 . . ? C41E C41F C41A 120.0 . . ? C41E C41F H41E 120.0 . . ? C41A C41F H41E 120.0 . . ? C41F C41A C41B 120.0 . . ? C41F C41A P7 120.5(10) . . ? C41B C41A P7 119.4(10) . . ? C41F C41A H41A 144.0 . . ? C41B C41A H41A 24.0 . . ? P7 C41A H41A 95.5 . . ? C41I C41H C41G 120.0 . . ? C41H C41I C41J 120.0 . . ? C41H C41I H41G 120.0 . . ? C41J C41I H41G 120.0 . . ? C41K C41J C41I 120.0 . . ? C41K C41J H41H 120.0 . . ? C41I C41J H41H 120.0 . . ? C41J C41K C41L 120.0 . . ? C41J C41K H41I 120.0 . . ? C41L C41K H41I 120.0 . . ? C41G C41L C41K 120.0 . . ? C41G C41L H41J 120.0 . . ? C41K C41L H41J 120.0 . . ? C41L C41G C41H 120.0 . . ? C41L C41G P7 116.9(11) . . ? C41H C41G P7 122.4(11) . . ? C41L C41G H41F 144.0 . . ? C41H C41G H41F 24.0 . . ? P7 C41G H41F 98.7 . . ? C42C C42B C42A 120.0 . . ? C42B C42C C42D 120.0 . . ? C42B C42C H42B 120.0 . . ? C42D C42C H42B 120.0 . . ? C42E C42D C42C 120.0 . . ? C42E C42D H42C 120.0 . . ? C42C C42D H42C 120.0 . . ? C42D C42E C42F 120.0 . . ? C42D C42E H42D 120.0 . . ? C42F C42E H42D 120.0 . . ? C42A C42F C42E 120.0 . . ? C42A C42F H42E 120.0 . . ? C42E C42F H42E 120.0 . . ? C42F C42A C42B 120.0 . . ? C42F C42A P8 120.1(10) . . ? C42B C42A P8 119.7(10) . . ? C42F C42A H42A 144.0 . . ? C42B C42A H42A 24.0 . . ? P8 C42A H42A 95.8 . . ? C42I C42H C42G 120.0 . . ? C42J C42I C42H 120.0 . . ? C42J C42I H42G 120.0 . . ? C42H C42I H42G 120.0 . . ? C42K C42J C42I 120.0 . . ? C42K C42J H42H 120.0 . . ? C42I C42J H42H 120.0 . . ? C42J C42K C42L 120.0 . . ? C42J C42K H42I 120.0 . . ? C42L C42K H42I 120.0 . . ? C42K C42L C42G 120.0 . . ? C42K C42L H42J 120.0 . . ? C42G C42L H42J 120.0 . . ? C42L C42G C42H 120.0 . . ? C42L C42G P8 116.1(10) . . ? C42H C42G P8 123.1(10) . . ? C42L C42G H42F 144.0 . . ? C42H C42G H42F 24.0 . . ? P8 C42G H42F 99.5 . . ? Cl2 C9 Cl1 107(4) . . ? Cl2 C9 H9A 109.7 . . ? Cl1 C9 H9A 110.1 . . ? Cl2 C9 H9B 111.6 . . ? Cl1 C9 H9B 108.8 . . ? H9A C9 H9B 109.8 . . ? C10 Cl3 Cl3A 78(2) . . ? C10A Cl3A Cl3 85(3) . . ? C10A Cl3A Cl4 18(3) . . ? Cl3 Cl3A Cl4 80(2) . . ? C10A Cl4 Cl4A 122(10) . . ? C10A Cl4 C10 75(6) . . ? Cl4A Cl4 C10 48(7) . . ? C10A Cl4 Cl3A 38(5) . . ? Cl4A Cl4 Cl3A 107(7) . . ? C10 Cl4 Cl3A 74(3) . . ? C10A Cl4 H10C 33.2 . . ? Cl4A Cl4 H10C 106.2 . . ? C10 Cl4 H10C 62.3 . . ? Cl3A Cl4 H10C 67.7 . . ? C10A Cl4 H10D 51.5 . . ? Cl4A Cl4 H10D 172.8 . . ? C10 Cl4 H10D 125.4 . . ? Cl3A Cl4 H10D 69.6 . . ? H10C Cl4 H10D 66.7 . . ? Cl4 Cl4A C10 94(7) . . ? Cl4 Cl4A C10A 26(5) . . ? C10 Cl4A C10A 68(4) . . ? Cl4 Cl4A H10B 140.2 . . ? C10 Cl4A H10B 47.1 . . ? C10A Cl4A H10B 115.1 . . ? Cl4A C10 Cl4 39(5) . . ? Cl4A C10 C10A 69(5) . . ? Cl4 C10 C10A 30(3) . . ? Cl4A C10 Cl3 120(6) . . ? Cl4 C10 Cl3 118(4) . . ? C10A C10 Cl3 104(3) . . ? Cl4A C10 H10A 127.0 . . ? Cl4 C10 H10A 110.9 . . ? C10A C10 H10A 97.3 . . ? Cl3 C10 H10A 115.0 . . ? Cl4A C10 H10B 59.2 . . ? Cl4 C10 H10B 97.4 . . ? C10A C10 H10B 127.5 . . ? Cl3 C10 H10B 104.5 . . ? H10A C10 H10B 109.0 . . ? Cl4 C10A Cl4A 32(6) . . ? Cl4 C10A C10 75(6) . . ? Cl4A C10A C10 43(4) . . ? Cl4 C10A Cl3A 124(8) . . ? Cl4A C10A Cl3A 112(5) . . ? C10 C10A Cl3A 93(4) . . ? Cl4 C10A H10C 118.0 . . ? Cl4A C10A H10C 102.3 . . ? C10 C10A H10C 73.4 . . ? Cl3A C10A H10C 111.5 . . ? Cl4 C10A H10D 82.3 . . ? Cl4A C10A H10D 114.2 . . ? C10 C10A H10D 155.0 . . ? Cl3A C10A H10D 108.4 . . ? H10C C10A H10D 110.0 . . ? H7 O7 H8 150 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 P1 C11G -158.5(8) . . . . ? I1 Co1 P1 C11G 80.8(7) . . . . ? I2 Co1 P1 C11G -46.3(7) . . . . ? O1 Co1 P1 C11A 76.8(8) . . . . ? I1 Co1 P1 C11A -43.9(6) . . . . ? I2 Co1 P1 C11A -170.8(6) . . . . ? O1 Co1 P1 C1 -38.9(9) . . . . ? I1 Co1 P1 C1 -159.6(7) . . . . ? I2 Co1 P1 C1 73.5(8) . . . . ? O4 Co3 P6 C32G -158.8(8) . . . . ? I6 Co3 P6 C32G -42.1(7) . . . . ? I5 Co3 P6 C32G 83.2(7) . . . . ? O4 Co3 P6 C32A 76.4(7) . . . . ? I6 Co3 P6 C32A -166.8(5) . . . . ? I5 Co3 P6 C32A -41.5(6) . . . . ? O4 Co3 P6 C6 -39.9(8) . . . . ? I6 Co3 P6 C6 76.9(7) . . . . ? I5 Co3 P6 C6 -157.8(7) . . . . ? C12A P2 O1 Co1 -84.3(15) . . . . ? C12G P2 O1 Co1 156.1(12) . . . . ? C2 P2 O1 Co1 37.7(17) . . . . ? I1 Co1 O1 P2 125.5(13) . . . . ? P1 Co1 O1 P2 8.2(15) . . . . ? I2 Co1 O1 P2 -106.2(14) . . . . ? C3 P3 O2 Co2 4(4) . . . . ? C21G P3 O2 Co2 131(3) . . . . ? C21A P3 O2 Co2 -119(3) . . . . ? O3 Co2 O2 P3 -40(3) . . . . ? I4 Co2 O2 P3 77(3) . . . . ? I3 Co2 O2 P3 -159(3) . . . . ? C22G P4 O3 Co2 -69.8(13) . . . . ? C22A P4 O3 Co2 172.4(10) . . . . ? C4 P4 O3 Co2 51.3(14) . . . . ? O2 Co2 O3 P4 7.1(15) . . . . ? I4 Co2 O3 P4 -112.1(11) . . . . ? I3 Co2 O3 P4 116.8(11) . . . . ? C31A P5 O4 Co3 158.3(11) . . . . ? C31G P5 O4 Co3 -83.9(14) . . . . ? C5 P5 O4 Co3 39.2(17) . . . . ? I6 Co3 O4 P5 -102.3(13) . . . . ? I5 Co3 O4 P5 130.4(12) . . . . ? P6 Co3 O4 P5 7.3(13) . . . . ? C41G P7 O5 Co4 78(3) . . . . ? C7 P7 O5 Co4 -50(3) . . . . ? C41A P7 O5 Co4 -166(3) . . . . ? O6 Co4 O5 P7 11(3) . . . . ? I8 Co4 O5 P7 125(3) . . . . ? I7 Co4 O5 P7 -109(3) . . . . ? C42A P8 O6 Co4 169.0(11) . . . . ? C42G P8 O6 Co4 -72.2(14) . . . . ? C8 P8 O6 Co4 50.0(16) . . . . ? O5 Co4 O6 P8 -6.2(15) . . . . ? I8 Co4 O6 P8 -114.8(12) . . . . ? I7 Co4 O6 P8 113.8(12) . . . . ? C11G P1 C1 C2 150.8(17) . . . . ? C11A P1 C1 C2 -99.3(18) . . . . ? Co1 P1 C1 C2 23.1(19) . . . . ? C11G P1 C1 C3 48.3(16) . . . . ? C11A P1 C1 C3 158.2(13) . . . . ? Co1 P1 C1 C3 -79.4(14) . . . . ? C3 C1 C2 C4 17.3(16) . . . . ? P1 C1 C2 C4 -98.1(18) . . . . ? C3 C1 C2 P2 143.6(15) . . . . ? P1 C1 C2 P2 28(2) . . . . ? O1 P2 C2 C4 46.6(16) . . . . ? C12A P2 C2 C4 171.1(13) . . . . ? C12G P2 C2 C4 -72.8(15) . . . . ? O1 P2 C2 C1 -65.7(19) . . . . ? C12A P2 C2 C1 58.8(18) . . . . ? C12G P2 C2 C1 174.9(16) . . . . ? C2 C1 C3 C4 -16.1(14) . . . . ? P1 C1 C3 C4 107.1(14) . . . . ? C2 C1 C3 P3 108.2(15) . . . . ? P1 C1 C3 P3 -128.5(13) . . . . ? O2 P3 C3 C1 -79(2) . . . . ? C21G P3 C3 C1 159.1(13) . . . . ? C21A P3 C3 C1 41.6(16) . . . . ? O2 P3 C3 C4 25(2) . . . . ? C21G P3 C3 C4 -96.9(16) . . . . ? C21A P3 C3 C4 145.6(14) . . . . ? C1 C2 C4 C3 -16.9(15) . . . . ? P2 C2 C4 C3 -143.1(13) . . . . ? C1 C2 C4 P4 -142.8(15) . . . . ? P2 C2 C4 P4 91.0(17) . . . . ? C1 C3 C4 C2 16.3(14) . . . . ? P3 C3 C4 C2 -104.2(17) . . . . ? C1 C3 C4 P4 140.5(14) . . . . ? P3 C3 C4 P4 20(2) . . . . ? O3 P4 C4 C2 35.0(18) . . . . ? C22G P4 C4 C2 158.3(15) . . . . ? C22A P4 C4 C2 -87.7(16) . . . . ? O3 P4 C4 C3 -72.5(16) . . . . ? C22G P4 C4 C3 50.8(16) . . . . ? C22A P4 C4 C3 164.8(13) . . . . ? O4 P5 C5 C8 41.8(17) . . . . ? C31A P5 C5 C8 -78.8(15) . . . . ? C31G P5 C5 C8 168.0(13) . . . . ? O4 P5 C5 C6 -63.9(18) . . . . ? C31A P5 C5 C6 175.5(15) . . . . ? C31G P5 C5 C6 62.3(17) . . . . ? C8 C5 C6 C7 19.1(16) . . . . ? P5 C5 C6 C7 141.1(16) . . . . ? C8 C5 C6 P6 -99.2(18) . . . . ? P5 C5 C6 P6 23(2) . . . . ? C32G P6 C6 C5 156.5(16) . . . . ? C32A P6 C6 C5 -94.2(17) . . . . ? Co3 P6 C6 C5 26.5(18) . . . . ? C32G P6 C6 C7 52.2(16) . . . . ? C32A P6 C6 C7 161.5(13) . . . . ? Co3 P6 C6 C7 -77.7(14) . . . . ? C5 C6 C7 C8 -18.8(15) . . . . ? P6 C6 C7 C8 105.8(15) . . . . ? C5 C6 C7 P7 105.2(15) . . . . ? P6 C6 C7 P7 -130.1(13) . . . . ? O5 P7 C7 C6 -65.5(17) . . . . ? C41G P7 C7 C6 165.5(12) . . . . ? C41A P7 C7 C6 50.0(15) . . . . ? O5 P7 C7 C8 39(2) . . . . ? C41G P7 C7 C8 -89.9(17) . . . . ? C41A P7 C7 C8 154.6(15) . . . . ? C6 C5 C8 C7 -19.1(15) . . . . ? P5 C5 C8 C7 -141.4(15) . . . . ? C6 C5 C8 P8 -148.2(15) . . . . ? P5 C5 C8 P8 89.5(18) . . . . ? C6 C7 C8 C5 19.0(15) . . . . ? P7 C7 C8 C5 -101.2(17) . . . . ? C6 C7 C8 P8 140.8(16) . . . . ? P7 C7 C8 P8 21(2) . . . . ? O6 P8 C8 C5 36.5(18) . . . . ? C42A P8 C8 C5 -83.7(17) . . . . ? C42G P8 C8 C5 162.2(14) . . . . ? O6 P8 C8 C7 -72.1(18) . . . . ? C42A P8 C8 C7 167.7(16) . . . . ? C42G P8 C8 C7 53.6(19) . . . . ? C11A C11B C11C C11D 0.0 . . . . ? C11B C11C C11D C11E 0.0 . . . . ? C11C C11D C11E C11F 0.0 . . . . ? C11D C11E C11F C11A 0.0 . . . . ? C11E C11F C11A C11B 0.0 . . . . ? C11E C11F C11A P1 177.7(12) . . . . ? C11C C11B C11A C11F 0.0 . . . . ? C11C C11B C11A P1 -178.0(11) . . . . ? C11G P1 C11A C11F 94.1(11) . . . . ? C1 P1 C11A C11F -16.9(12) . . . . ? Co1 P1 C11A C11F -133.8(8) . . . . ? C11G P1 C11A C11B -88.0(10) . . . . ? C1 P1 C11A C11B 160.9(9) . . . . ? Co1 P1 C11A C11B 44.0(9) . . . . ? C11G C11H C11I C11J 0.0 . . . . ? C11H C11I C11J C11K 0.0 . . . . ? C11I C11J C11K C11L 0.0 . . . . ? C11J C11K C11L C11G 0.0 . . . . ? C11K C11L C11G C11H 0.0 . . . . ? C11K C11L C11G P1 179.7(13) . . . . ? C11I C11H C11G C11L 0.0 . . . . ? C11I C11H C11G P1 -179.7(13) . . . . ? C11A P1 C11G C11L 157.9(10) . . . . ? C1 P1 C11G C11L -91.9(12) . . . . ? Co1 P1 C11G C11L 28.2(12) . . . . ? C11A P1 C11G C11H -22.4(12) . . . . ? C1 P1 C11G C11H 87.8(12) . . . . ? Co1 P1 C11G C11H -152.1(7) . . . . ? C12A C12B C12C C12D 0.0 . . . . ? C12B C12C C12D C12E 0.0 . . . . ? C12C C12D C12E C12F 0.0 . . . . ? C12D C12E C12F C12A 0.0 . . . . ? C12E C12F C12A C12B 0.0 . . . . ? C12E C12F C12A P2 173.4(12) . . . . ? C12C C12B C12A C12F 0.0 . . . . ? C12C C12B C12A P2 -173.8(12) . . . . ? O1 P2 C12A C12F 172.5(9) . . . . ? C12G P2 C12A C12F -66.5(11) . . . . ? C2 P2 C12A C12F 50.1(12) . . . . ? O1 P2 C12A C12B -13.9(11) . . . . ? C12G P2 C12A C12B 107.2(9) . . . . ? C2 P2 C12A C12B -136.2(9) . . . . ? C12G C12H C12I C12J 0.0 . . . . ? C12H C12I C12J C12K 0.0 . . . . ? C12I C12J C12K C12L 0.0 . . . . ? C12J C12K C12L C12G 0.0 . . . . ? C12K C12L C12G C12H 0.0 . . . . ? C12K C12L C12G P2 172.2(11) . . . . ? C12I C12H C12G C12L 0.0 . . . . ? C12I C12H C12G P2 -172.0(11) . . . . ? O1 P2 C12G C12L 18.0(11) . . . . ? C12A P2 C12G C12L -105.3(10) . . . . ? C2 P2 C12G C12L 137.4(10) . . . . ? O1 P2 C12G C12H -169.8(10) . . . . ? C12A P2 C12G C12H 66.8(11) . . . . ? C2 P2 C12G C12H -50.4(11) . . . . ? C21A C21B C21C C21D 0.0 . . . . ? C21B C21C C21D C21E 0.0 . . . . ? C21C C21D C21E C21F 0.0 . . . . ? C21D C21E C21F C21A 0.0 . . . . ? C21E C21F C21A C21B 0.0 . . . . ? C21E C21F C21A P3 -179.8(15) . . . . ? C21C C21B C21A C21F 0.0 . . . . ? C21C C21B C21A P3 179.8(15) . . . . ? O2 P3 C21A C21F 47.2(15) . . . . ? C3 P3 C21A C21F -86.3(13) . . . . ? C21G P3 C21A C21F 152.0(11) . . . . ? O2 P3 C21A C21B -132.6(14) . . . . ? C3 P3 C21A C21B 93.9(13) . . . . ? C21G P3 C21A C21B -27.7(14) . . . . ? C21G C21H C21I C21J 0.0 . . . . ? C21H C21I C21J C21K 0.0 . . . . ? C21I C21J C21K C21L 0.0 . . . . ? C21J C21K C21L C21G 0.0 . . . . ? C21K C21L C21G C21H 0.0 . . . . ? C21K C21L C21G P3 -170.0(13) . . . . ? C21I C21H C21G C21L 0.0 . . . . ? C21I C21H C21G P3 170.4(13) . . . . ? O2 P3 C21G C21L -164.4(14) . . . . ? C3 P3 C21G C21L -29.9(13) . . . . ? C21A P3 C21G C21L 88.4(12) . . . . ? O2 P3 C21G C21H 25.4(15) . . . . ? C3 P3 C21G C21H 159.9(10) . . . . ? C21A P3 C21G C21H -81.8(12) . . . . ? C22A C22B C22C C22D 0.0 . . . . ? C22B C22C C22D C22E 0.0 . . . . ? C22C C22D C22E C22F 0.0 . . . . ? C22D C22E C22F C22A 0.0 . . . . ? C22E C22F C22A C22B 0.0 . . . . ? C22E C22F C22A P4 -176.2(11) . . . . ? C22C C22B C22A C22F 0.0 . . . . ? C22C C22B C22A P4 176.4(11) . . . . ? O3 P4 C22A C22F -171.2(9) . . . . ? C22G P4 C22A C22F 68.0(11) . . . . ? C4 P4 C22A C22F -46.6(11) . . . . ? O3 P4 C22A C22B 12.5(11) . . . . ? C22G P4 C22A C22B -108.3(9) . . . . ? C4 P4 C22A C22B 137.1(9) . . . . ? C22G C22H C22I C22J 0.0 . . . . ? C22H C22I C22J C22K 0.0 . . . . ? C22I C22J C22K C22L 0.0 . . . . ? C22J C22K C22L C22G 0.0 . . . . ? C22K C22L C22G C22H 0.0 . . . . ? C22K C22L C22G P4 -175.0(11) . . . . ? C22I C22H C22G C22L 0.0 . . . . ? C22I C22H C22G P4 174.9(11) . . . . ? O3 P4 C22G C22L -17.7(11) . . . . ? C22A P4 C22G C22L 102.7(9) . . . . ? C4 P4 C22G C22L -142.5(9) . . . . ? O3 P4 C22G C22H 167.4(9) . . . . ? C22A P4 C22G C22H -72.3(10) . . . . ? C4 P4 C22G C22H 42.6(11) . . . . ? C31A C31B C31C C31D 0.0 . . . . ? C31B C31C C31D C31E 0.0 . . . . ? C31C C31D C31E C31F 0.0 . . . . ? C31D C31E C31F C31A 0.0 . . . . ? C31E C31F C31A C31B 0.0 . . . . ? C31E C31F C31A P5 169.0(11) . . . . ? C31C C31B C31A C31F 0.0 . . . . ? C31C C31B C31A P5 -168.8(11) . . . . ? O4 P5 C31A C31F 15.4(11) . . . . ? C31G P5 C31A C31F -107.7(10) . . . . ? C5 P5 C31A C31F 137.0(10) . . . . ? O4 P5 C31A C31B -175.6(9) . . . . ? C31G P5 C31A C31B 61.3(11) . . . . ? C5 P5 C31A C31B -54.0(11) . . . . ? C31G C31H C31I C31J 0.0 . . . . ? C31H C31I C31J C31K 0.0 . . . . ? C31I C31J C31K C31L 0.0 . . . . ? C31J C31K C31L C31G 0.0 . . . . ? C31K C31L C31G C31H 0.0 . . . . ? C31K C31L C31G P5 176.5(12) . . . . ? C31I C31H C31G C31L 0.0 . . . . ? C31I C31H C31G P5 -176.6(12) . . . . ? O4 P5 C31G C31L 166.1(10) . . . . ? C31A P5 C31G C31L -73.4(11) . . . . ? C5 P5 C31G C31L 41.2(12) . . . . ? O4 P5 C31G C31H -17.4(12) . . . . ? C31A P5 C31G C31H 103.1(10) . . . . ? C5 P5 C31G C31H -142.3(10) . . . . ? C32A C32B C32C C32D 0.0 . . . . ? C32B C32C C32D C32E 0.0 . . . . ? C32C C32D C32E C32F 0.0 . . . . ? C32D C32E C32F C32A 0.0 . . . . ? C32E C32F C32A C32B 0.0 . . . . ? C32E C32F C32A P6 -175.5(11) . . . . ? C32C C32B C32A C32F 0.0 . . . . ? C32C C32B C32A P6 175.8(10) . . . . ? C32G P6 C32A C32F 81.0(10) . . . . ? C6 P6 C32A C32F -28.6(11) . . . . ? Co3 P6 C32A C32F -144.9(7) . . . . ? C32G P6 C32A C32B -94.6(10) . . . . ? C6 P6 C32A C32B 155.8(9) . . . . ? Co3 P6 C32A C32B 39.5(9) . . . . ? C32G C32H C32I C32J 0.0 . . . . ? C32H C32I C32J C32K 0.0 . . . . ? C32I C32J C32K C32L 0.0 . . . . ? C32J C32K C32L C32G 0.0 . . . . ? C32K C32L C32G C32H 0.0 . . . . ? C32K C32L C32G P6 -177.9(13) . . . . ? C32I C32H C32G C32L 0.0 . . . . ? C32I C32H C32G P6 177.9(13) . . . . ? C32A P6 C32G C32L 160.1(9) . . . . ? C6 P6 C32G C32L -88.8(11) . . . . ? Co3 P6 C32G C32L 31.2(11) . . . . ? C32A P6 C32G C32H -17.8(11) . . . . ? C6 P6 C32G C32H 93.3(12) . . . . ? Co3 P6 C32G C32H -146.6(8) . . . . ? C41A C41B C41C C41D 0.0 . . . . ? C41B C41C C41D C41E 0.0 . . . . ? C41C C41D C41E C41F 0.0 . . . . ? C41D C41E C41F C41A 0.0 . . . . ? C41E C41F C41A C41B 0.0 . . . . ? C41E C41F C41A P7 177.8(12) . . . . ? C41C C41B C41A C41F 0.0 . . . . ? C41C C41B C41A P7 -177.9(12) . . . . ? O5 P7 C41A C41F -151.7(12) . . . . ? C41G P7 C41A C41F -30.4(12) . . . . ? C7 P7 C41A C41F 88.7(11) . . . . ? O5 P7 C41A C41B 26.2(13) . . . . ? C41G P7 C41A C41B 147.5(10) . . . . ? C7 P7 C41A C41B -93.5(11) . . . . ? C41G C41H C41I C41J 0.0 . . . . ? C41H C41I C41J C41K 0.0 . . . . ? C41I C41J C41K C41L 0.0 . . . . ? C41J C41K C41L C41G 0.0 . . . . ? C41K C41L C41G C41H 0.0 . . . . ? C41K C41L C41G P7 171.0(12) . . . . ? C41I C41H C41G C41L 0.0 . . . . ? C41I C41H C41G P7 -170.4(13) . . . . ? O5 P7 C41G C41L 25.9(14) . . . . ? C7 P7 C41G C41L 153.8(10) . . . . ? C41A P7 C41G C41L -89.8(11) . . . . ? O5 P7 C41G C41H -163.4(12) . . . . ? C7 P7 C41G C41H -35.4(13) . . . . ? C41A P7 C41G C41H 80.9(12) . . . . ? C42A C42B C42C C42D 0.0 . . . . ? C42B C42C C42D C42E 0.0 . . . . ? C42C C42D C42E C42F 0.0 . . . . ? C42D C42E C42F C42A 0.0 . . . . ? C42E C42F C42A C42B 0.0 . . . . ? C42E C42F C42A P8 -174.0(12) . . . . ? C42C C42B C42A C42F 0.0 . . . . ? C42C C42B C42A P8 174.1(12) . . . . ? O6 P8 C42A C42F -171.6(10) . . . . ? C42G P8 C42A C42F 64.8(11) . . . . ? C8 P8 C42A C42F -50.3(12) . . . . ? O6 P8 C42A C42B 14.4(12) . . . . ? C42G P8 C42A C42B -109.2(10) . . . . ? C8 P8 C42A C42B 135.6(10) . . . . ? C42G C42H C42I C42J 0.0 . . . . ? C42H C42I C42J C42K 0.0 . . . . ? C42I C42J C42K C42L 0.0 . . . . ? C42J C42K C42L C42G 0.0 . . . . ? C42K C42L C42G C42H 0.0 . . . . ? C42K C42L C42G P8 -169.5(12) . . . . ? C42I C42H C42G C42L 0.0 . . . . ? C42I C42H C42G P8 168.8(12) . . . . ? O6 P8 C42G C42L -19.4(11) . . . . ? C42A P8 C42G C42L 101.5(10) . . . . ? C8 P8 C42G C42L -143.5(10) . . . . ? O6 P8 C42G C42H 171.4(9) . . . . ? C42A P8 C42G C42H -67.7(11) . . . . ? C8 P8 C42G C42H 47.3(13) . . . . ? _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction 0.990 _refine_diff_density_max 0.750 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.152 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 691866' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2I4(DMF)2(dppcb)]' _chemical_name_common (Co2I4(DMF)2(dppcb)) _chemical_melting_point ? _chemical_formula_moiety 'C58 H58 Co2 I4 N2 O2 P4, 2(C3 H7 N O)' _chemical_formula_sum 'C64 H72 Co2 I4 N4 O4 P4' _chemical_formula_weight 1710.638 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' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.044(2) _cell_length_b 12.524(3) _cell_length_c 14.806(3) _cell_angle_alpha 96.75(1) _cell_angle_beta 107.05(1) _cell_angle_gamma 115.21(1) _cell_volume 1700.4(7) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 2.445 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details 'Empirical Absorption Corrections' _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8876 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7826 _reflns_number_gt 5954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Software of the Siemens P4' _computing_data_reduction 'Software of the Siemens P4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.0788P)^2^+0.5115P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7684 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 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 0.32193(6) 0.35087(5) 0.25109(4) 0.02357(14) Uani 1 1 d . . . I1 I 0.12373(3) 0.38851(3) 0.30881(2) 0.03313(10) Uani 1 1 d . . . I2 I 0.27723(5) 0.39853(3) 0.08363(2) 0.05364(14) Uani 1 1 d . . . P1 P 0.51011(12) 0.53294(9) 0.32775(8) 0.0204(2) Uani 1 1 d . . . P2 P 0.42150(12) 0.29408(9) 0.37427(8) 0.0204(2) Uani 1 1 d . . . O1 O 0.1942(4) 0.1728(3) 0.1829(3) 0.0359(8) Uani 1 1 d . . . N1 N -0.0108(5) -0.0096(4) 0.1266(4) 0.0506(12) Uani 1 1 d . . . C3 C 0.0607(6) 0.1116(5) 0.1533(5) 0.0476(14) Uani 1 1 d . . . H3A H 0.0074 0.1538 0.1497 0.071 Uiso 1 1 calc R . . C4 C -0.1656(8) -0.0777(8) 0.0995(9) 0.108(4) Uani 1 1 d . . . H4A H -0.2089 -0.1412 0.0380 0.162 Uiso 1 1 calc R . . H4B H -0.2056 -0.0223 0.0916 0.162 Uiso 1 1 calc R . . H4C H -0.1861 -0.1152 0.1507 0.162 Uiso 1 1 calc R . . C5 C 0.0668(8) -0.0791(6) 0.1312(6) 0.066(2) Uani 1 1 d . . . H5A H 0.0027 -0.1607 0.0857 0.099 Uiso 1 1 calc R . . H5B H 0.1000 -0.0860 0.1975 0.099 Uiso 1 1 calc R . . H5C H 0.1494 -0.0372 0.1136 0.099 Uiso 1 1 calc R . . C1 C 0.5689(4) 0.5494(4) 0.4619(3) 0.0192(8) Uani 1 1 d D . . C2 C 0.5235(5) 0.4231(4) 0.4871(3) 0.0201(8) Uani 1 1 d . . . C11 C 0.6727(5) 0.5561(4) 0.3045(3) 0.0255(9) Uani 1 1 d . . . C12 C 0.6836(6) 0.5818(5) 0.2167(4) 0.0374(11) Uani 1 1 d . . . H12A H 0.6092 0.5884 0.1711 0.056 Uiso 1 1 calc R . . C13 C 0.8053(7) 0.5974(6) 0.1974(4) 0.0491(14) Uani 1 1 d . . . H13A H 0.8138 0.6165 0.1392 0.074 Uiso 1 1 calc R . . C14 C 0.9123(6) 0.5852(6) 0.2621(5) 0.0464(14) Uani 1 1 d . . . H14A H 0.9930 0.5946 0.2475 0.070 Uiso 1 1 calc R . . C15 C 0.9031(5) 0.5591(5) 0.3488(4) 0.0370(11) Uani 1 1 d . . . H15A H 0.9767 0.5502 0.3931 0.055 Uiso 1 1 calc R . . C16 C 0.7835(5) 0.5462(4) 0.3696(4) 0.0287(9) Uani 1 1 d . . . H16A H 0.7779 0.5304 0.4292 0.043 Uiso 1 1 calc R . . C21 C 0.5045(5) 0.6751(4) 0.3155(3) 0.0259(9) Uani 1 1 d . . . C22 C 0.3725(6) 0.6740(5) 0.2744(4) 0.0397(12) Uani 1 1 d . . . H22A H 0.2848 0.6000 0.2528 0.060 Uiso 1 1 calc R . . C23 C 0.3721(7) 0.7832(6) 0.2657(5) 0.0505(15) Uani 1 1 d . . . H23A H 0.2835 0.7831 0.2396 0.076 Uiso 1 1 calc R . . C24 C 0.5000(7) 0.8913(5) 0.2949(5) 0.0468(14) Uani 1 1 d . . . H24A H 0.4985 0.9644 0.2880 0.070 Uiso 1 1 calc R . . C25 C 0.6291(7) 0.8925(5) 0.3341(4) 0.0442(13) Uani 1 1 d . . . H25A H 0.7162 0.9667 0.3543 0.066 Uiso 1 1 calc R . . C26 C 0.6326(6) 0.7851(4) 0.3441(4) 0.0367(11) Uani 1 1 d . . . H26A H 0.7221 0.7867 0.3705 0.055 Uiso 1 1 calc R . . C31 C 0.5554(5) 0.2598(4) 0.3503(3) 0.0256(9) Uani 1 1 d . . . C32 C 0.6782(6) 0.2734(4) 0.4236(4) 0.0357(11) Uani 1 1 d . . . H32A H 0.6949 0.3013 0.4901 0.053 Uiso 1 1 calc R . . C33 C 0.7760(6) 0.2460(5) 0.3992(5) 0.0441(13) Uani 1 1 d . . . H33A H 0.8591 0.2561 0.4490 0.066 Uiso 1 1 calc R . . C34 C 0.7502(6) 0.2036(5) 0.3009(5) 0.0502(16) Uani 1 1 d . . . H34A H 0.8163 0.1850 0.2843 0.075 Uiso 1 1 calc R . . C35 C 0.6298(7) 0.1886(5) 0.2283(5) 0.0490(15) Uani 1 1 d . . . H35A H 0.6130 0.1594 0.1620 0.073 Uiso 1 1 calc R . . C36 C 0.5318(6) 0.2165(5) 0.2520(4) 0.0362(11) Uani 1 1 d . . . H36A H 0.4491 0.2061 0.2016 0.054 Uiso 1 1 calc R . . C41 C 0.3044(5) 0.1541(4) 0.3986(3) 0.0260(9) Uani 1 1 d . . . C42 C 0.3439(6) 0.0633(5) 0.4123(4) 0.0389(12) Uani 1 1 d . . . H42A H 0.4361 0.0773 0.4159 0.058 Uiso 1 1 calc R . . C43 C 0.2484(8) -0.0474(5) 0.4206(5) 0.0531(16) Uani 1 1 d . . . H43A H 0.2760 -0.1079 0.4299 0.080 Uiso 1 1 calc R . . C44 C 0.1103(7) -0.0693(5) 0.4152(5) 0.0496(15) Uani 1 1 d . . . H44A H 0.0444 -0.1448 0.4194 0.074 Uiso 1 1 calc R . . C45 C 0.0730(6) 0.0211(5) 0.4035(4) 0.0441(13) Uani 1 1 d . . . H45A H -0.0187 0.0075 0.4008 0.066 Uiso 1 1 calc R . . C46 C 0.1692(5) 0.1329(5) 0.3957(4) 0.0343(10) Uani 1 1 d . . . H46A H 0.1423 0.1942 0.3884 0.051 Uiso 1 1 calc R . . O2 O 0.3138(12) 0.9324(9) 0.0264(10) 0.175(5) Uani 1 1 d . . . N2 N 0.3351(10) 0.7613(7) 0.0082(5) 0.081(2) Uani 1 1 d . . . C6 C 0.3884(15) 0.8832(11) 0.0377(8) 0.109(4) Uani 1 1 d . . . H6A H 0.4893 0.9333 0.0689 0.163 Uiso 1 1 calc R . . C7 C 0.4336(13) 0.7182(11) 0.0144(11) 0.125(4) Uani 1 1 d . . . H7A H 0.4032 0.6605 -0.0479 0.188 Uiso 1 1 calc R . . H7B H 0.4374 0.6772 0.0660 0.188 Uiso 1 1 calc R . . H7C H 0.5287 0.7868 0.0294 0.188 Uiso 1 1 calc R . . C8 C 0.1850(13) 0.6755(15) -0.0265(9) 0.139(5) Uani 1 1 d . . . H8A H 0.1566 0.6182 -0.0885 0.209 Uiso 1 1 calc R . . H8B H 0.1296 0.7190 -0.0362 0.209 Uiso 1 1 calc R . . H8C H 0.1662 0.6307 0.0214 0.209 Uiso 1 1 calc R . . H1 H 0.670(3) 0.612(4) 0.498(4) 0.050 Uiso 1 1 d D . . H2 H 0.608(7) 0.424(6) 0.534(4) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0256(3) 0.0226(3) 0.0219(3) 0.0052(2) 0.0093(2) 0.0113(2) I1 0.02553(16) 0.03614(17) 0.04043(19) 0.00931(13) 0.01274(13) 0.01754(13) I2 0.0717(3) 0.0418(2) 0.02438(17) 0.01024(14) 0.00606(17) 0.01568(19) P1 0.0249(5) 0.0209(5) 0.0202(5) 0.0068(4) 0.0129(4) 0.0121(4) P2 0.0255(5) 0.0189(5) 0.0226(5) 0.0062(4) 0.0140(4) 0.0125(4) O1 0.0337(18) 0.0277(16) 0.0356(18) 0.0038(14) 0.0103(15) 0.0090(14) N1 0.037(2) 0.034(2) 0.061(3) -0.004(2) 0.015(2) 0.006(2) C3 0.038(3) 0.033(3) 0.053(3) -0.005(2) 0.008(3) 0.012(2) C4 0.043(4) 0.055(5) 0.169(11) -0.028(6) 0.030(5) -0.003(3) C5 0.061(4) 0.029(3) 0.083(5) -0.004(3) 0.010(4) 0.017(3) C1 0.0236(19) 0.0224(19) 0.0174(18) 0.0060(15) 0.0120(15) 0.0132(16) C2 0.027(2) 0.0213(18) 0.0184(18) 0.0041(15) 0.0137(16) 0.0144(16) C11 0.031(2) 0.024(2) 0.027(2) 0.0049(17) 0.0187(18) 0.0135(18) C12 0.050(3) 0.050(3) 0.029(2) 0.018(2) 0.025(2) 0.030(3) C13 0.058(4) 0.066(4) 0.039(3) 0.019(3) 0.038(3) 0.029(3) C14 0.044(3) 0.051(3) 0.056(3) 0.012(3) 0.037(3) 0.022(3) C15 0.032(2) 0.043(3) 0.048(3) 0.010(2) 0.023(2) 0.024(2) C16 0.035(2) 0.029(2) 0.036(2) 0.0150(19) 0.024(2) 0.0183(19) C21 0.038(2) 0.024(2) 0.025(2) 0.0115(17) 0.0193(19) 0.0174(19) C22 0.038(3) 0.035(3) 0.056(3) 0.020(2) 0.020(2) 0.023(2) C23 0.047(3) 0.050(3) 0.074(4) 0.029(3) 0.025(3) 0.036(3) C24 0.064(4) 0.029(3) 0.064(4) 0.018(3) 0.034(3) 0.030(3) C25 0.053(3) 0.027(2) 0.052(3) 0.013(2) 0.022(3) 0.018(2) C26 0.037(3) 0.029(2) 0.042(3) 0.010(2) 0.013(2) 0.016(2) C31 0.036(2) 0.0215(19) 0.031(2) 0.0101(17) 0.0219(19) 0.0171(18) C32 0.036(3) 0.031(2) 0.048(3) 0.009(2) 0.021(2) 0.020(2) C33 0.034(3) 0.039(3) 0.068(4) 0.013(3) 0.024(3) 0.023(2) C34 0.046(3) 0.036(3) 0.094(5) 0.020(3) 0.051(3) 0.024(3) C35 0.065(4) 0.044(3) 0.058(4) 0.011(3) 0.047(3) 0.028(3) C36 0.052(3) 0.036(3) 0.035(3) 0.011(2) 0.029(2) 0.025(2) C41 0.034(2) 0.0210(19) 0.027(2) 0.0080(16) 0.0186(18) 0.0122(18) C42 0.049(3) 0.036(3) 0.054(3) 0.022(2) 0.035(3) 0.028(2) C43 0.076(4) 0.033(3) 0.075(4) 0.029(3) 0.050(4) 0.031(3) C44 0.057(4) 0.030(3) 0.062(4) 0.015(3) 0.036(3) 0.012(3) C45 0.039(3) 0.039(3) 0.052(3) 0.020(2) 0.025(3) 0.010(2) C46 0.032(2) 0.038(3) 0.039(3) 0.013(2) 0.018(2) 0.018(2) O2 0.161(9) 0.131(8) 0.303(15) 0.065(9) 0.116(10) 0.112(8) N2 0.124(7) 0.063(4) 0.061(4) 0.021(3) 0.043(4) 0.044(4) C6 0.137(10) 0.091(7) 0.092(7) 0.027(6) 0.052(7) 0.045(7) C7 0.106(9) 0.094(8) 0.197(14) 0.075(9) 0.065(9) 0.054(7) C8 0.091(8) 0.223(16) 0.104(9) 0.015(9) 0.008(7) 0.104(10) _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 O1 1.985(3) . ? Co1 P1 2.1859(12) . ? Co1 P2 2.1992(12) . ? Co1 I2 2.5746(8) . ? Co1 I1 2.7614(8) . ? P1 C11 1.836(4) . ? P1 C21 1.837(4) . ? P1 C1 1.856(4) . ? P2 C31 1.820(4) . ? P2 C41 1.834(4) . ? P2 C2 1.839(4) . ? O1 C3 1.238(7) . ? N1 C3 1.318(7) . ? N1 C4 1.444(9) . ? N1 C5 1.453(8) . ? C3 H3A 0.9400 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C1 C2 1.556(5) 2_666 ? C1 C2 1.571(5) . ? C1 H1 0.98(5) . ? C2 C1 1.556(5) 2_666 ? C2 H2 0.98(6) . ? C11 C16 1.382(7) . ? C11 C12 1.401(6) . ? C12 C13 1.394(7) . ? C12 H12A 0.9400 . ? C13 C14 1.364(9) . ? C13 H13A 0.9400 . ? C14 C15 1.384(8) . ? C14 H14A 0.9400 . ? C15 C16 1.391(6) . ? C15 H15A 0.9400 . ? C16 H16A 0.9400 . ? C21 C26 1.389(7) . ? C21 C22 1.398(7) . ? C22 C23 1.390(7) . ? C22 H22A 0.9400 . ? C23 C24 1.375(9) . ? C23 H23A 0.9400 . ? C24 C25 1.365(9) . ? C24 H24A 0.9400 . ? C25 C26 1.386(7) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C31 C32 1.394(7) . ? C31 C36 1.396(6) . ? C32 C33 1.389(7) . ? C32 H32A 0.9400 . ? C33 C34 1.388(9) . ? C33 H33A 0.9400 . ? C34 C35 1.365(9) . ? C34 H34A 0.9400 . ? C35 C36 1.389(7) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C41 C46 1.386(7) . ? C41 C42 1.397(7) . ? C42 C43 1.385(7) . ? C42 H42A 0.9400 . ? C43 C44 1.404(9) . ? C43 H43A 0.9400 . ? C44 C45 1.372(8) . ? C44 H44A 0.9400 . ? C45 C46 1.395(7) . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? O2 C6 1.209(14) . ? N2 C6 1.341(13) . ? N2 C7 1.391(13) . ? N2 C8 1.421(14) . ? C6 H6A 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 P1 163.79(12) . . ? O1 Co1 P2 86.27(11) . . ? P1 Co1 P2 84.94(5) . . ? O1 Co1 I2 89.91(10) . . ? P1 Co1 I2 92.73(4) . . ? P2 Co1 I2 156.45(4) . . ? O1 Co1 I1 96.69(11) . . ? P1 Co1 I1 98.38(4) . . ? P2 Co1 I1 101.42(4) . . ? I2 Co1 I1 102.11(2) . . ? C11 P1 C21 102.3(2) . . ? C11 P1 C1 102.50(19) . . ? C21 P1 C1 104.63(19) . . ? C11 P1 Co1 114.56(14) . . ? C21 P1 Co1 122.41(16) . . ? C1 P1 Co1 108.31(13) . . ? C31 P2 C41 103.3(2) . . ? C31 P2 C2 105.4(2) . . ? C41 P2 C2 110.21(19) . . ? C31 P2 Co1 109.24(15) . . ? C41 P2 Co1 117.96(16) . . ? C2 P2 Co1 109.86(14) . . ? C3 O1 Co1 129.0(4) . . ? C3 N1 C4 122.0(6) . . ? C3 N1 C5 120.3(5) . . ? C4 N1 C5 117.6(6) . . ? O1 C3 N1 123.6(6) . . ? O1 C3 H3A 118.2 . . ? N1 C3 H3A 118.2 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C1 C2 90.5(3) 2_666 . ? C2 C1 P1 115.8(3) 2_666 . ? C2 C1 P1 113.3(3) . . ? C2 C1 H1 108(4) 2_666 . ? C2 C1 H1 115(4) . . ? P1 C1 H1 112(4) . . ? C1 C2 C1 89.5(3) 2_666 . ? C1 C2 P2 115.8(3) 2_666 . ? C1 C2 P2 110.9(3) . . ? C1 C2 H2 113(4) 2_666 . ? C1 C2 H2 110(4) . . ? P2 C2 H2 115(4) . . ? C16 C11 C12 118.7(4) . . ? C16 C11 P1 122.1(3) . . ? C12 C11 P1 119.1(4) . . ? C13 C12 C11 119.7(5) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C14 C13 C12 120.6(5) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C15 120.6(5) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C14 C15 C16 119.1(5) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C11 C16 C15 121.3(4) . . ? C11 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C26 C21 C22 119.1(4) . . ? C26 C21 P1 119.9(4) . . ? C22 C21 P1 120.9(4) . . ? C23 C22 C21 119.4(5) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C25 C24 C23 120.0(5) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.5(5) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C21 120.2(5) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C32 C31 C36 118.7(4) . . ? C32 C31 P2 124.0(4) . . ? C36 C31 P2 117.3(4) . . ? C33 C32 C31 120.5(5) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C34 C33 C32 119.6(5) . . ? C34 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C35 C34 C33 120.5(5) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 120.2(6) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C35 C36 C31 120.4(5) . . ? C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? C46 C41 C42 118.9(4) . . ? C46 C41 P2 119.8(4) . . ? C42 C41 P2 121.1(4) . . ? C43 C42 C41 120.6(5) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C42 C43 C44 120.1(5) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C45 C44 C43 119.1(5) . . ? C45 C44 H44A 120.5 . . ? C43 C44 H44A 120.5 . . ? C44 C45 C46 120.9(5) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C41 C46 C45 120.4(5) . . ? C41 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? C6 N2 C7 117.5(10) . . ? C6 N2 C8 123.3(11) . . ? C7 N2 C8 119.3(9) . . ? O2 C6 N2 123.6(13) . . ? O2 C6 H6A 118.2 . . ? N2 C6 H6A 118.2 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 P1 C11 25.4(4) . . . . ? P2 Co1 P1 C11 82.79(16) . . . . ? I2 Co1 P1 C11 -73.72(16) . . . . ? I1 Co1 P1 C11 -176.38(16) . . . . ? O1 Co1 P1 C21 150.0(4) . . . . ? P2 Co1 P1 C21 -152.60(16) . . . . ? I2 Co1 P1 C21 50.89(16) . . . . ? I1 Co1 P1 C21 -51.77(16) . . . . ? O1 Co1 P1 C1 -88.3(4) . . . . ? P2 Co1 P1 C1 -30.91(14) . . . . ? I2 Co1 P1 C1 172.59(14) . . . . ? I1 Co1 P1 C1 69.92(14) . . . . ? O1 Co1 P2 C31 82.45(19) . . . . ? P1 Co1 P2 C31 -83.92(16) . . . . ? I2 Co1 P2 C31 1.3(2) . . . . ? I1 Co1 P2 C31 178.53(15) . . . . ? O1 Co1 P2 C41 -35.00(19) . . . . ? P1 Co1 P2 C41 158.63(17) . . . . ? I2 Co1 P2 C41 -116.15(18) . . . . ? I1 Co1 P2 C41 61.08(16) . . . . ? O1 Co1 P2 C2 -162.42(18) . . . . ? P1 Co1 P2 C2 31.21(14) . . . . ? I2 Co1 P2 C2 116.43(16) . . . . ? I1 Co1 P2 C2 -66.34(14) . . . . ? P1 Co1 O1 C3 176.0(4) . . . . ? P2 Co1 O1 C3 118.8(5) . . . . ? I2 Co1 O1 C3 -84.5(5) . . . . ? I1 Co1 O1 C3 17.7(5) . . . . ? Co1 O1 C3 N1 -166.0(5) . . . . ? C4 N1 C3 O1 175.3(8) . . . . ? C5 N1 C3 O1 0.2(10) . . . . ? C11 P1 C1 C2 161.0(3) . . . 2_666 ? C21 P1 C1 C2 54.5(3) . . . 2_666 ? Co1 P1 C1 C2 -77.6(3) . . . 2_666 ? C11 P1 C1 C2 -96.5(3) . . . . ? C21 P1 C1 C2 157.0(3) . . . . ? Co1 P1 C1 C2 25.0(3) . . . . ? C2 C1 C2 C1 0.0 2_666 . . 2_666 ? P1 C1 C2 C1 -118.5(3) . . . 2_666 ? C2 C1 C2 P2 117.6(3) 2_666 . . . ? P1 C1 C2 P2 -0.9(4) . . . . ? C31 P2 C2 C1 -165.9(3) . . . 2_666 ? C41 P2 C2 C1 -55.1(4) . . . 2_666 ? Co1 P2 C2 C1 76.5(3) . . . 2_666 ? C31 P2 C2 C1 94.0(3) . . . . ? C41 P2 C2 C1 -155.2(3) . . . . ? Co1 P2 C2 C1 -23.6(3) . . . . ? C21 P1 C11 C16 126.2(4) . . . . ? C1 P1 C11 C16 17.9(4) . . . . ? Co1 P1 C11 C16 -99.2(4) . . . . ? C21 P1 C11 C12 -55.5(4) . . . . ? C1 P1 C11 C12 -163.7(4) . . . . ? Co1 P1 C11 C12 79.2(4) . . . . ? C16 C11 C12 C13 -0.4(7) . . . . ? P1 C11 C12 C13 -178.9(4) . . . . ? C11 C12 C13 C14 1.5(9) . . . . ? C12 C13 C14 C15 -1.1(9) . . . . ? C13 C14 C15 C16 -0.4(9) . . . . ? C12 C11 C16 C15 -1.1(7) . . . . ? P1 C11 C16 C15 177.3(4) . . . . ? C14 C15 C16 C11 1.5(8) . . . . ? C11 P1 C21 C26 -33.5(4) . . . . ? C1 P1 C21 C26 73.1(4) . . . . ? Co1 P1 C21 C26 -163.5(3) . . . . ? C11 P1 C21 C22 144.2(4) . . . . ? C1 P1 C21 C22 -109.2(4) . . . . ? Co1 P1 C21 C22 14.2(5) . . . . ? C26 C21 C22 C23 -1.9(8) . . . . ? P1 C21 C22 C23 -179.7(5) . . . . ? C21 C22 C23 C24 1.6(10) . . . . ? C22 C23 C24 C25 -0.8(10) . . . . ? C23 C24 C25 C26 0.4(9) . . . . ? C24 C25 C26 C21 -0.7(9) . . . . ? C22 C21 C26 C25 1.5(8) . . . . ? P1 C21 C26 C25 179.3(4) . . . . ? C41 P2 C31 C32 -82.8(4) . . . . ? C2 P2 C31 C32 32.9(4) . . . . ? Co1 P2 C31 C32 150.9(4) . . . . ? C41 P2 C31 C36 96.7(4) . . . . ? C2 P2 C31 C36 -147.6(4) . . . . ? Co1 P2 C31 C36 -29.6(4) . . . . ? C36 C31 C32 C33 0.9(7) . . . . ? P2 C31 C32 C33 -179.6(4) . . . . ? C31 C32 C33 C34 -0.6(8) . . . . ? C32 C33 C34 C35 0.0(8) . . . . ? C33 C34 C35 C36 0.4(9) . . . . ? C34 C35 C36 C31 -0.1(8) . . . . ? C32 C31 C36 C35 -0.6(7) . . . . ? P2 C31 C36 C35 179.9(4) . . . . ? C31 P2 C41 C46 -163.8(4) . . . . ? C2 P2 C41 C46 84.1(4) . . . . ? Co1 P2 C41 C46 -43.2(4) . . . . ? C31 P2 C41 C42 11.0(5) . . . . ? C2 P2 C41 C42 -101.1(4) . . . . ? Co1 P2 C41 C42 131.6(4) . . . . ? C46 C41 C42 C43 1.5(8) . . . . ? P2 C41 C42 C43 -173.4(5) . . . . ? C41 C42 C43 C44 0.1(9) . . . . ? C42 C43 C44 C45 -1.3(10) . . . . ? C43 C44 C45 C46 0.9(10) . . . . ? C42 C41 C46 C45 -1.8(8) . . . . ? P2 C41 C46 C45 173.1(4) . . . . ? C44 C45 C46 C41 0.6(9) . . . . ? C7 N2 C6 O2 171.9(13) . . . . ? C8 N2 C6 O2 -9.4(18) . . . . ? _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction 0.983 _refine_diff_density_max 0.811 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.112 #===END data_7a _database_code_depnum_ccdc_archive 'CCDC 691867' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2Cl4(dppcbO4)]' _chemical_name_common (Co2Cl4(dppcbO4)) _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cl4 Co2 O4 P4, 2(C H2 Cl2)' _chemical_formula_sum 'C54 H48 Cl8 Co2 O4 P4' _chemical_formula_weight 1286.31 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' Cl Cl 0.1484 0.1585 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.1710(4) _cell_length_b 22.5657(6) _cell_length_c 13.9413(3) _cell_angle_alpha 90.00 _cell_angle_beta 121.530(1) _cell_angle_gamma 90.00 _cell_volume 5677.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 19630 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600.0 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_process_details 'Otwinowski et al, 1997' _diffrn_ambient_temperature 223(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 'Kappa CCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25325 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6503 _reflns_number_gt 4440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6335 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 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 0.391251(18) 0.187149(16) 0.92713(3) 0.03058(12) Uani 1 1 d . . . Cl1 Cl 0.28820(4) 0.16992(4) 0.93066(7) 0.0570(3) Uani 1 1 d . . . Cl2 Cl 0.39476(5) 0.19019(4) 0.77088(6) 0.0498(2) Uani 1 1 d . . . P1 P 0.54467(4) 0.14617(3) 1.15618(5) 0.02633(17) Uani 1 1 d . . . P2 P 0.48793(3) 0.30144(3) 1.08982(5) 0.02428(16) Uani 1 1 d . . . O1 O 0.47503(9) 0.13954(8) 1.04239(15) 0.0340(4) Uani 1 1 d . . . O2 O 0.42441(9) 0.26480(8) 1.00353(14) 0.0342(4) Uani 1 1 d . . . C1 C 0.53632(14) 0.19848(11) 1.2487(2) 0.0244(5) Uani 1 1 d . . . C2 C 0.52863(14) 0.26778(11) 1.2297(2) 0.0238(5) Uani 1 1 d . . . C11 C 0.57017(14) 0.07502(12) 1.2232(2) 0.0298(6) Uani 1 1 d . . . C12 C 0.53872(17) 0.02588(14) 1.1548(3) 0.0436(8) Uani 1 1 d . . . H12A H 0.5022 0.0308 1.0784 0.052 Uiso 1 1 calc R . . C13 C 0.5611(2) -0.03056(15) 1.1989(3) 0.0590(10) Uani 1 1 d . . . H13A H 0.5398 -0.0639 1.1524 0.071 Uiso 1 1 calc R . . C14 C 0.6149(2) -0.03787(16) 1.3119(3) 0.0626(10) Uani 1 1 d . . . H14A H 0.6308 -0.0760 1.3420 0.075 Uiso 1 1 calc R . . C15 C 0.64453(19) 0.01081(16) 1.3787(3) 0.0561(9) Uani 1 1 d . . . H15A H 0.6802 0.0057 1.4555 0.067 Uiso 1 1 calc R . . C16 C 0.62354(15) 0.06719(14) 1.3366(2) 0.0428(7) Uani 1 1 d . . . H16A H 0.6450 0.1002 1.3840 0.051 Uiso 1 1 calc R . . C21 C 0.62165(14) 0.17118(12) 1.1479(2) 0.0301(6) Uani 1 1 d . . . C22 C 0.68819(14) 0.18659(13) 1.2450(2) 0.0346(7) Uani 1 1 d . . . H22A H 0.6920 0.1857 1.3153 0.042 Uiso 1 1 calc R . . C23 C 0.74890(16) 0.20328(14) 1.2379(3) 0.0431(7) Uani 1 1 d . . . H23A H 0.7941 0.2133 1.3032 0.052 Uiso 1 1 calc R . . C24 C 0.74201(18) 0.20503(14) 1.1332(3) 0.0468(8) Uani 1 1 d . . . H24A H 0.7827 0.2168 1.1280 0.056 Uiso 1 1 calc R . . C25 C 0.67679(18) 0.18991(15) 1.0375(3) 0.0469(8) Uani 1 1 d . . . H25A H 0.6733 0.1910 0.9675 0.056 Uiso 1 1 calc R . . C26 C 0.61589(16) 0.17309(13) 1.0431(2) 0.0366(7) Uani 1 1 d . . . H26A H 0.5711 0.1630 0.9772 0.044 Uiso 1 1 calc R . . C31 C 0.55807(15) 0.31536(12) 1.0579(2) 0.0299(6) Uani 1 1 d . . . C32 C 0.53598(17) 0.31562(15) 0.9440(3) 0.0428(7) Uani 1 1 d . . . H32A H 0.4880 0.3034 0.8888 0.051 Uiso 1 1 calc R . . C33 C 0.58550(18) 0.33397(18) 0.9135(3) 0.0550(9) Uani 1 1 d . . . H33A H 0.5711 0.3343 0.8373 0.066 Uiso 1 1 calc R . . C34 C 0.65574(18) 0.35167(15) 0.9946(3) 0.0501(8) Uani 1 1 d . . . H34A H 0.6887 0.3648 0.9730 0.060 Uiso 1 1 calc R . . C35 C 0.67837(17) 0.35043(15) 1.1061(3) 0.0478(8) Uani 1 1 d . . . H35A H 0.7268 0.3619 1.1608 0.057 Uiso 1 1 calc R . . C36 C 0.62954(15) 0.33217(14) 1.1382(2) 0.0365(7) Uani 1 1 d . . . H36A H 0.6451 0.3312 1.2148 0.044 Uiso 1 1 calc R . . C41 C 0.45219(14) 0.37275(12) 1.0953(2) 0.0283(6) Uani 1 1 d . . . C42 C 0.49175(16) 0.42473(13) 1.1146(3) 0.0387(7) Uani 1 1 d . . . H42A H 0.5411 0.4233 1.1325 0.046 Uiso 1 1 calc R . . C43 C 0.45892(19) 0.47898(14) 1.1078(3) 0.0530(9) Uani 1 1 d . . . H43A H 0.4857 0.5143 1.1199 0.064 Uiso 1 1 calc R . . C44 C 0.3869(2) 0.48099(16) 1.0833(3) 0.0581(10) Uani 1 1 d . . . H44A H 0.3646 0.5177 1.0790 0.070 Uiso 1 1 calc R . . C45 C 0.34765(18) 0.42970(15) 1.0653(3) 0.0499(8) Uani 1 1 d . . . H45A H 0.2990 0.4315 1.0507 0.060 Uiso 1 1 calc R . . C46 C 0.37869(14) 0.37537(14) 1.0684(2) 0.0363(7) Uani 1 1 d . . . H46A H 0.3507 0.3405 1.0526 0.044 Uiso 1 1 calc R . . Cl3 Cl 0.75497(17) -0.02140(10) 1.2124(2) 0.1451(9) Uani 0.84 1 d PU . . Cl3A Cl 0.7200(5) 0.0214(6) 1.1598(8) 0.119(3) Uani 0.16 1 d PDU . . Cl4 Cl 0.86451(8) 0.07475(8) 1.28935(13) 0.1228(6) Uani 1 1 d U . . C3 C 0.7799(4) 0.0523(4) 1.2647(7) 0.141(3) Uani 1 1 d D . . H1 H 0.5800(17) 0.1893(14) 1.327(3) 0.050 Uiso 1 1 d . . . H2 H 0.5729(17) 0.2891(15) 1.278(3) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0294(2) 0.0306(2) 0.02369(19) -0.00204(15) 0.00832(16) -0.00148(15) Cl1 0.0313(4) 0.0722(6) 0.0550(5) 0.0247(5) 0.0138(4) -0.0056(4) Cl2 0.0679(5) 0.0496(5) 0.0306(4) -0.0010(3) 0.0248(4) 0.0116(4) P1 0.0288(3) 0.0245(4) 0.0240(3) -0.0013(3) 0.0126(3) 0.0038(3) P2 0.0282(3) 0.0236(4) 0.0228(3) -0.0003(3) 0.0145(3) -0.0010(3) O1 0.0328(9) 0.0301(11) 0.0283(10) -0.0034(8) 0.0085(8) 0.0053(8) O2 0.0356(10) 0.0298(11) 0.0296(9) -0.0046(8) 0.0118(8) -0.0057(8) C1 0.0273(13) 0.0241(14) 0.0226(12) -0.0008(10) 0.0137(11) 0.0020(11) C2 0.0260(12) 0.0236(14) 0.0236(12) -0.0008(10) 0.0141(11) -0.0010(11) C11 0.0324(14) 0.0265(14) 0.0320(13) 0.0006(11) 0.0179(12) 0.0040(11) C12 0.0524(19) 0.0342(18) 0.0336(15) -0.0023(13) 0.0152(15) 0.0058(14) C13 0.078(2) 0.0276(18) 0.060(2) -0.0087(16) 0.028(2) 0.0026(16) C14 0.073(2) 0.0321(19) 0.064(2) 0.0102(17) 0.022(2) 0.0101(17) C15 0.057(2) 0.042(2) 0.0432(18) 0.0100(16) 0.0085(16) 0.0042(16) C16 0.0399(16) 0.0342(17) 0.0357(15) -0.0004(13) 0.0068(13) 0.0011(13) C21 0.0385(15) 0.0252(14) 0.0309(14) -0.0031(11) 0.0211(13) 0.0058(11) C22 0.0359(15) 0.0368(17) 0.0339(15) -0.0047(12) 0.0202(13) 0.0000(12) C23 0.0393(16) 0.0440(19) 0.0486(18) -0.0129(15) 0.0248(15) -0.0093(14) C24 0.0526(19) 0.0422(19) 0.063(2) -0.0090(16) 0.0426(18) -0.0063(15) C25 0.063(2) 0.048(2) 0.0461(18) -0.0031(15) 0.0407(18) -0.0006(16) C26 0.0443(16) 0.0389(17) 0.0305(14) -0.0014(13) 0.0222(14) 0.0012(13) C31 0.0376(15) 0.0290(15) 0.0305(14) 0.0034(11) 0.0229(13) 0.0038(12) C32 0.0423(17) 0.056(2) 0.0300(15) 0.0026(14) 0.0186(14) 0.0020(15) C33 0.065(2) 0.075(3) 0.0448(19) 0.0102(18) 0.0430(19) 0.0067(19) C34 0.054(2) 0.053(2) 0.064(2) 0.0118(18) 0.0459(19) 0.0071(16) C35 0.0351(16) 0.054(2) 0.059(2) 0.0106(17) 0.0286(16) 0.0041(14) C36 0.0338(15) 0.0439(18) 0.0352(15) 0.0037(13) 0.0204(13) 0.0016(13) C41 0.0326(14) 0.0260(14) 0.0266(13) 0.0021(11) 0.0157(12) 0.0016(11) C42 0.0435(16) 0.0275(15) 0.0486(17) -0.0003(13) 0.0267(15) -0.0036(13) C43 0.065(2) 0.0261(18) 0.072(2) -0.0033(16) 0.039(2) -0.0036(15) C44 0.070(2) 0.0340(19) 0.081(3) 0.0087(18) 0.047(2) 0.0177(17) C45 0.0453(17) 0.043(2) 0.066(2) 0.0119(17) 0.0320(17) 0.0151(15) C46 0.0337(15) 0.0375(17) 0.0397(16) 0.0063(13) 0.0205(13) 0.0021(13) Cl3 0.243(3) 0.0870(14) 0.182(2) 0.0188(14) 0.165(2) 0.0306(16) Cl3A 0.119(7) 0.130(9) 0.096(6) -0.023(6) 0.048(5) 0.030(6) Cl4 0.1063(10) 0.1564(16) 0.1050(10) -0.0082(10) 0.0548(9) 0.0409(10) C3 0.171(6) 0.122(6) 0.182(7) -0.035(6) 0.128(6) 0.010(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 O1 1.9752(19) . ? Co1 O2 1.9787(19) . ? Co1 Cl2 2.2191(10) . ? Co1 Cl1 2.2417(9) . ? P1 O1 1.505(2) . ? P1 C21 1.785(3) . ? P1 C11 1.793(3) . ? P1 C1 1.824(3) . ? P2 O2 1.4990(19) . ? P2 C31 1.787(3) . ? P2 C41 1.797(3) . ? P2 C2 1.834(3) . ? C1 C1 1.558(5) 2_657 ? C1 C2 1.580(4) . ? C1 H1 1.02(3) . ? C2 C2 1.584(5) 2_657 ? C2 H2 0.95(3) . ? C11 C12 1.385(4) . ? C11 C16 1.393(4) . ? C12 C13 1.386(4) . ? C12 H12A 0.9400 . ? C13 C14 1.389(5) . ? C13 H13A 0.9400 . ? C14 C15 1.363(5) . ? C14 H14A 0.9400 . ? C15 C16 1.374(4) . ? C15 H15A 0.9400 . ? C16 H16A 0.9400 . ? C21 C22 1.394(4) . ? C21 C26 1.402(4) . ? C22 C23 1.392(4) . ? C22 H22A 0.9400 . ? C23 C24 1.390(5) . ? C23 H23A 0.9400 . ? C24 C25 1.370(4) . ? C24 H24A 0.9400 . ? C25 C26 1.385(4) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C31 C36 1.384(4) . ? C31 C32 1.402(4) . ? C32 C33 1.384(4) . ? C32 H32A 0.9400 . ? C33 C34 1.375(5) . ? C33 H33A 0.9400 . ? C34 C35 1.367(5) . ? C34 H34A 0.9400 . ? C35 C36 1.386(4) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C41 C42 1.383(4) . ? C41 C46 1.398(4) . ? C42 C43 1.386(4) . ? C42 H42A 0.9400 . ? C43 C44 1.379(5) . ? C43 H43A 0.9400 . ? C44 C45 1.369(5) . ? C44 H44A 0.9400 . ? C45 C46 1.381(4) . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? Cl3 Cl3A 1.204(11) . ? Cl3 C3 1.782(8) . ? Cl3A C3 1.515(10) . ? Cl4 C3 1.714(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 97.40(8) . . ? O1 Co1 Cl2 109.79(6) . . ? O2 Co1 Cl2 108.44(6) . . ? O1 Co1 Cl1 110.98(7) . . ? O2 Co1 Cl1 102.54(6) . . ? Cl2 Co1 Cl1 124.02(5) . . ? O1 P1 C21 112.79(12) . . ? O1 P1 C11 108.80(12) . . ? C21 P1 C11 106.30(13) . . ? O1 P1 C1 113.94(11) . . ? C21 P1 C1 105.69(12) . . ? C11 P1 C1 108.99(12) . . ? O2 P2 C31 114.26(12) . . ? O2 P2 C41 107.89(11) . . ? C31 P2 C41 106.03(12) . . ? O2 P2 C2 110.51(12) . . ? C31 P2 C2 110.35(12) . . ? C41 P2 C2 107.46(12) . . ? P1 O1 Co1 140.46(12) . . ? P2 O2 Co1 146.85(12) . . ? C1 C1 C2 89.28(13) 2_657 . ? C1 C1 P1 118.61(17) 2_657 . ? C2 C1 P1 124.19(18) . . ? C1 C1 H1 109.1(18) 2_657 . ? C2 C1 H1 109.7(18) . . ? P1 C1 H1 105.1(18) . . ? C1 C2 C2 88.35(13) . 2_657 ? C1 C2 P2 122.53(18) . . ? C2 C2 P2 111.0(2) 2_657 . ? C1 C2 H2 114(2) . . ? C2 C2 H2 113.7(19) 2_657 . ? P2 C2 H2 106.5(19) . . ? C12 C11 C16 119.5(3) . . ? C12 C11 P1 116.9(2) . . ? C16 C11 P1 123.3(2) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 121.6(3) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.2 . . ? C15 C16 C11 119.4(3) . . ? C15 C16 H16A 120.3 . . ? C11 C16 H16A 120.3 . . ? C22 C21 C26 119.8(3) . . ? C22 C21 P1 120.6(2) . . ? C26 C21 P1 119.5(2) . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 119.3(3) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C25 C24 C23 121.0(3) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 120.5(3) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C21 119.4(3) . . ? C25 C26 H26A 120.3 . . ? C21 C26 H26A 120.3 . . ? C36 C31 C32 119.4(3) . . ? C36 C31 P2 123.2(2) . . ? C32 C31 P2 117.0(2) . . ? C33 C32 C31 119.4(3) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? C34 C33 C32 120.1(3) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C36 119.7(3) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C35 C36 C31 120.4(3) . . ? C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? C42 C41 C46 119.5(3) . . ? C42 C41 P2 122.8(2) . . ? C46 C41 P2 117.4(2) . . ? C41 C42 C43 120.3(3) . . ? C41 C42 H42A 119.8 . . ? C43 C42 H42A 119.9 . . ? C44 C43 C42 119.7(3) . . ? C44 C43 H43A 120.1 . . ? C42 C43 H43A 120.1 . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C46 C45 C44 120.8(3) . . ? C46 C45 H45A 119.6 . . ? C44 C45 H45A 119.6 . . ? C45 C46 C41 119.4(3) . . ? C45 C46 H46A 120.3 . . ? C41 C46 H46A 120.3 . . ? Cl3A Cl3 C3 57.1(5) . . ? Cl3 Cl3A C3 81.0(6) . . ? Cl3A C3 Cl3 41.9(5) . . ? Cl3A C3 Cl4 126.2(6) . . ? Cl3 C3 Cl4 114.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 P1 O1 Co1 -84.0(2) . . . . ? C11 P1 O1 Co1 158.33(18) . . . . ? C1 P1 O1 Co1 36.5(2) . . . . ? O2 Co1 O1 P1 2.3(2) . . . . ? Cl2 Co1 O1 P1 115.00(18) . . . . ? Cl1 Co1 O1 P1 -104.21(19) . . . . ? C31 P2 O2 Co1 64.4(3) . . . . ? C41 P2 O2 Co1 -177.9(2) . . . . ? C2 P2 O2 Co1 -60.7(2) . . . . ? O1 Co1 O2 P2 20.5(2) . . . . ? Cl2 Co1 O2 P2 -93.2(2) . . . . ? Cl1 Co1 O2 P2 134.0(2) . . . . ? O1 P1 C1 C1 41.2(2) . . . 2_657 ? C21 P1 C1 C1 165.56(19) . . . 2_657 ? C11 P1 C1 C1 -80.6(2) . . . 2_657 ? O1 P1 C1 C2 -69.5(2) . . . . ? C21 P1 C1 C2 54.9(2) . . . . ? C11 P1 C1 C2 168.8(2) . . . . ? C1 C1 C2 C2 16.4(3) 2_657 . . 2_657 ? P1 C1 C2 C2 141.2(2) . . . 2_657 ? C1 C1 C2 P2 -97.6(2) 2_657 . . . ? P1 C1 C2 P2 27.2(3) . . . . ? O2 P2 C2 C1 37.2(2) . . . . ? C31 P2 C2 C1 -90.2(2) . . . . ? C41 P2 C2 C1 154.65(19) . . . . ? O2 P2 C2 C2 -64.85(14) . . . 2_657 ? C31 P2 C2 C2 167.81(13) . . . 2_657 ? C41 P2 C2 C2 52.63(15) . . . 2_657 ? O1 P1 C11 C12 17.7(3) . . . . ? C21 P1 C11 C12 -104.1(2) . . . . ? C1 P1 C11 C12 142.5(2) . . . . ? O1 P1 C11 C16 -167.7(2) . . . . ? C21 P1 C11 C16 70.6(3) . . . . ? C1 P1 C11 C16 -42.9(3) . . . . ? C16 C11 C12 C13 -0.8(5) . . . . ? P1 C11 C12 C13 174.0(3) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C12 C13 C14 C15 1.0(6) . . . . ? C13 C14 C15 C16 -1.3(6) . . . . ? C14 C15 C16 C11 0.7(6) . . . . ? C12 C11 C16 C15 0.4(5) . . . . ? P1 C11 C16 C15 -174.1(3) . . . . ? O1 P1 C21 C22 172.3(2) . . . . ? C11 P1 C21 C22 -68.6(2) . . . . ? C1 P1 C21 C22 47.2(3) . . . . ? O1 P1 C21 C26 -10.2(3) . . . . ? C11 P1 C21 C26 108.9(2) . . . . ? C1 P1 C21 C26 -135.3(2) . . . . ? C26 C21 C22 C23 -0.6(4) . . . . ? P1 C21 C22 C23 176.9(2) . . . . ? C21 C22 C23 C24 0.8(5) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C23 C24 C25 C26 0.7(5) . . . . ? C24 C25 C26 C21 -0.5(5) . . . . ? C22 C21 C26 C25 0.5(4) . . . . ? P1 C21 C26 C25 -177.1(2) . . . . ? O2 P2 C31 C36 -160.2(2) . . . . ? C41 P2 C31 C36 81.1(3) . . . . ? C2 P2 C31 C36 -35.0(3) . . . . ? O2 P2 C31 C32 27.3(3) . . . . ? C41 P2 C31 C32 -91.4(2) . . . . ? C2 P2 C31 C32 152.6(2) . . . . ? C36 C31 C32 C33 -1.4(5) . . . . ? P2 C31 C32 C33 171.3(3) . . . . ? C31 C32 C33 C34 0.1(5) . . . . ? C32 C33 C34 C35 1.3(6) . . . . ? C33 C34 C35 C36 -1.2(5) . . . . ? C34 C35 C36 C31 -0.2(5) . . . . ? C32 C31 C36 C35 1.5(4) . . . . ? P2 C31 C36 C35 -170.8(2) . . . . ? O2 P2 C41 C42 -145.0(2) . . . . ? C31 P2 C41 C42 -22.2(3) . . . . ? C2 P2 C41 C42 95.8(3) . . . . ? O2 P2 C41 C46 29.0(2) . . . . ? C31 P2 C41 C46 151.8(2) . . . . ? C2 P2 C41 C46 -90.2(2) . . . . ? C46 C41 C42 C43 0.2(4) . . . . ? P2 C41 C42 C43 174.1(2) . . . . ? C41 C42 C43 C44 1.0(5) . . . . ? C42 C43 C44 C45 -0.3(6) . . . . ? C43 C44 C45 C46 -1.7(6) . . . . ? C44 C45 C46 C41 2.9(5) . . . . ? C42 C41 C46 C45 -2.1(4) . . . . ? P2 C41 C46 C45 -176.4(2) . . . . ? _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction 0.984 _refine_diff_density_max 0.345 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.052 #===END data_7b _database_code_depnum_ccdc_archive 'CCDC 691868' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2Br4(dppcbO4)]' _chemical_name_common (Co2Br4(dppcbO4)) _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Br4 Co2 O4 P4, 2(C H2 Cl2)' _chemical_formula_sum 'C54 H48 Br4 Cl4 Co2 O4 P4' _chemical_formula_weight 1464.13 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.2304(3) _cell_length_b 22.5106(3) _cell_length_c 14.0664(3) _cell_angle_alpha 90.00 _cell_angle_beta 120.084(1) _cell_angle_gamma 90.00 _cell_volume 5816.89(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 40954 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904.0 _exptl_absorpt_coefficient_mu 3.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.130 _exptl_absorpt_correction_T_max 0.165 _exptl_absorpt_process_details 'Otwinowski et al, 1997' _diffrn_ambient_temperature 223(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 'Kappa CCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23998 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6688 _reflns_number_gt 4955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.0762P)^2^+14.3536P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6479 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 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 0.39754(3) 0.19086(3) 0.43381(5) 0.02329(17) Uani 1 1 d . . . Br1 Br 0.28689(3) 0.17299(3) 0.43312(5) 0.0527(2) Uani 1 1 d . . . Br2 Br 0.40466(3) 0.19396(2) 0.27210(4) 0.04071(18) Uani 1 1 d . . . P1 P 0.54488(6) 0.14894(5) 0.65632(9) 0.0193(2) Uani 1 1 d . . . P2 P 0.49072(6) 0.30449(5) 0.59369(9) 0.0174(2) Uani 1 1 d . . . O1 O 0.42885(18) 0.26783(14) 0.5091(3) 0.0292(7) Uani 1 1 d . . . O2 O 0.47697(18) 0.14258(14) 0.5464(3) 0.0281(7) Uani 1 1 d . . . C1 C 0.5361(2) 0.20145(17) 0.7477(3) 0.0161(8) Uani 1 1 d . . . C2 C 0.5287(2) 0.27084(17) 0.7306(3) 0.0153(8) Uani 1 1 d . . . C11 C 0.5693(3) 0.07766(19) 0.7227(4) 0.0243(9) Uani 1 1 d . . . C12 C 0.5376(3) 0.0284(2) 0.6535(5) 0.0407(13) Uani 1 1 d . . . H12A H 0.5019 0.0333 0.5793 0.049 Uiso 1 1 calc R . . C13 C 0.5606(4) -0.0278(3) 0.6981(6) 0.064(2) Uani 1 1 d . . . H13A H 0.5407 -0.0614 0.6528 0.077 Uiso 1 1 calc R . . C14 C 0.6121(4) -0.0356(3) 0.8071(6) 0.065(2) Uani 1 1 d . . . H14A H 0.6268 -0.0741 0.8357 0.078 Uiso 1 1 calc R . . C15 C 0.6422(4) 0.0136(3) 0.8747(5) 0.0568(18) Uani 1 1 d . . . H15A H 0.6769 0.0085 0.9494 0.068 Uiso 1 1 calc R . . C16 C 0.6209(3) 0.0702(2) 0.8320(4) 0.0367(12) Uani 1 1 d . . . H16A H 0.6417 0.1035 0.8775 0.044 Uiso 1 1 calc R . . C21 C 0.6211(2) 0.17357(19) 0.6466(4) 0.0233(9) Uani 1 1 d . . . C22 C 0.6864(3) 0.1888(2) 0.7405(4) 0.0292(10) Uani 1 1 d . . . H22A H 0.6892 0.1887 0.8093 0.035 Uiso 1 1 calc R . . C23 C 0.7474(3) 0.2042(2) 0.7335(5) 0.0369(12) Uani 1 1 d . . . H23A H 0.7917 0.2137 0.7968 0.044 Uiso 1 1 calc R . . C24 C 0.7412(3) 0.2051(3) 0.6305(5) 0.0420(13) Uani 1 1 d . . . H24A H 0.7818 0.2161 0.6247 0.050 Uiso 1 1 calc R . . C25 C 0.6776(3) 0.1906(2) 0.5370(5) 0.0405(13) Uani 1 1 d . . . H25A H 0.6751 0.1913 0.4683 0.049 Uiso 1 1 calc R . . C26 C 0.6166(3) 0.1748(2) 0.5448(4) 0.0337(11) Uani 1 1 d . . . H26A H 0.5726 0.1651 0.4811 0.040 Uiso 1 1 calc R . . C31 C 0.4546(2) 0.37618(19) 0.5982(4) 0.0213(9) Uani 1 1 d . . . C32 C 0.4941(3) 0.4282(2) 0.6183(5) 0.0341(11) Uani 1 1 d . . . H32A H 0.5432 0.4270 0.6369 0.041 Uiso 1 1 calc R . . C33 C 0.4606(4) 0.4822(2) 0.6109(6) 0.0529(17) Uani 1 1 d . . . H33A H 0.4869 0.5177 0.6232 0.063 Uiso 1 1 calc R . . C34 C 0.3893(4) 0.4840(3) 0.5857(6) 0.0554(17) Uani 1 1 d . . . H34A H 0.3669 0.5208 0.5806 0.067 Uiso 1 1 calc R . . C35 C 0.3507(3) 0.4326(3) 0.5681(6) 0.0459(15) Uani 1 1 d . . . H35A H 0.3024 0.4340 0.5535 0.055 Uiso 1 1 calc R . . C36 C 0.3824(3) 0.3786(2) 0.5716(4) 0.0309(11) Uani 1 1 d . . . H36A H 0.3551 0.3435 0.5560 0.037 Uiso 1 1 calc R . . C41 C 0.5612(3) 0.31890(19) 0.5620(4) 0.0239(9) Uani 1 1 d . . . C42 C 0.6309(3) 0.3342(2) 0.6404(5) 0.0341(11) Uani 1 1 d . . . H42A H 0.6452 0.3327 0.7153 0.041 Uiso 1 1 calc R . . C43 C 0.6803(3) 0.3519(3) 0.6080(6) 0.0450(14) Uani 1 1 d . . . H43A H 0.7281 0.3625 0.6612 0.054 Uiso 1 1 calc R . . C44 C 0.6593(4) 0.3539(3) 0.4987(6) 0.0468(15) Uani 1 1 d . . . H44A H 0.6926 0.3667 0.4774 0.056 Uiso 1 1 calc R . . C45 C 0.5908(4) 0.3376(3) 0.4205(5) 0.0469(15) Uani 1 1 d . . . H45A H 0.5772 0.3385 0.3458 0.056 Uiso 1 1 calc R . . C46 C 0.5406(3) 0.3196(2) 0.4516(5) 0.0374(12) Uani 1 1 d . . . H46A H 0.4933 0.3081 0.3981 0.045 Uiso 1 1 calc R . . H1 H 0.580(4) 0.199(3) 0.829(6) 0.050 Uiso 1 1 d . . . H2 H 0.573(4) 0.292(3) 0.780(5) 0.050 Uiso 1 1 d . . . Cl1 Cl 0.7508(4) -0.0180(2) 0.7050(5) 0.196(2) Uani 1 1 d DU . . Cl2 Cl 0.86491(17) 0.07475(18) 0.7944(3) 0.1303(12) Uani 1 1 d DU . . C3 C 0.7690(8) 0.0482(5) 0.744(2) 0.184(2) Uani 1 1 d D . . H3A H 0.7582 0.0541 0.8037 0.451 Uiso 1 1 calc R . . H3B H 0.7358 0.0738 0.6832 0.451 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 0.0219(3) 0.0226(3) 0.0191(3) -0.0013(2) 0.0056(2) -0.0014(2) Br1 0.0228(3) 0.0748(4) 0.0482(4) 0.0300(3) 0.0085(2) -0.0068(3) Br2 0.0588(4) 0.0394(3) 0.0244(3) -0.0010(2) 0.0212(3) 0.0088(2) P1 0.0226(5) 0.0165(5) 0.0173(5) -0.0024(4) 0.0088(4) 0.0038(4) P2 0.0221(5) 0.0153(5) 0.0184(5) 0.0003(4) 0.0129(4) -0.0017(4) O1 0.0344(18) 0.0214(16) 0.0261(17) -0.0047(13) 0.0108(15) -0.0056(13) O2 0.0271(16) 0.0264(17) 0.0206(16) -0.0034(13) 0.0042(13) 0.0044(13) C1 0.0169(19) 0.0175(19) 0.0143(19) -0.0026(14) 0.0082(16) 0.0009(15) C2 0.022(2) 0.0120(18) 0.0158(19) -0.0018(14) 0.0123(17) -0.0028(15) C11 0.031(2) 0.014(2) 0.025(2) 0.0002(16) 0.0123(19) 0.0049(17) C12 0.055(3) 0.022(2) 0.034(3) -0.008(2) 0.014(3) -0.001(2) C13 0.089(5) 0.020(3) 0.062(4) -0.007(3) 0.022(4) 0.004(3) C14 0.078(5) 0.023(3) 0.056(4) 0.010(3) 0.006(4) 0.012(3) C15 0.059(4) 0.037(3) 0.040(3) 0.012(3) -0.001(3) 0.003(3) C16 0.043(3) 0.025(2) 0.028(3) -0.0015(19) 0.007(2) 0.001(2) C21 0.027(2) 0.017(2) 0.028(2) -0.0024(17) 0.016(2) 0.0055(17) C22 0.031(3) 0.036(3) 0.026(2) -0.0098(19) 0.018(2) -0.002(2) C23 0.038(3) 0.035(3) 0.044(3) -0.013(2) 0.026(3) -0.007(2) C24 0.044(3) 0.044(3) 0.053(4) -0.011(3) 0.035(3) -0.010(2) C25 0.056(4) 0.043(3) 0.043(3) -0.001(2) 0.039(3) 0.002(3) C26 0.040(3) 0.039(3) 0.024(2) -0.002(2) 0.017(2) 0.003(2) C31 0.028(2) 0.017(2) 0.023(2) 0.0054(16) 0.0152(19) 0.0033(17) C32 0.035(3) 0.021(2) 0.048(3) -0.004(2) 0.023(2) -0.0029(19) C33 0.063(4) 0.017(3) 0.091(5) 0.002(3) 0.048(4) 0.002(3) C34 0.071(4) 0.026(3) 0.085(5) 0.012(3) 0.051(4) 0.019(3) C35 0.037(3) 0.040(3) 0.069(4) 0.014(3) 0.033(3) 0.017(2) C36 0.033(3) 0.028(2) 0.041(3) 0.008(2) 0.025(2) 0.0030(19) C41 0.032(2) 0.018(2) 0.034(3) 0.0047(17) 0.025(2) 0.0055(17) C42 0.029(2) 0.043(3) 0.038(3) 0.010(2) 0.023(2) 0.003(2) C43 0.026(3) 0.053(3) 0.064(4) 0.010(3) 0.029(3) 0.003(2) C44 0.060(4) 0.038(3) 0.076(5) 0.013(3) 0.059(4) 0.010(3) C45 0.067(4) 0.050(4) 0.043(3) 0.005(3) 0.042(3) 0.001(3) C46 0.049(3) 0.041(3) 0.034(3) -0.001(2) 0.030(3) 0.003(2) Cl1 0.303(7) 0.154(4) 0.220(5) -0.020(4) 0.197(6) -0.004(4) Cl2 0.098(2) 0.182(3) 0.109(2) -0.015(2) 0.0504(18) 0.043(2) C3 0.231(19) 0.123(11) 0.30(2) 0.022(13) 0.21(2) 0.062(12) _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 O2 1.963(3) . ? Co1 O1 1.965(3) . ? Co1 Br2 2.3551(9) . ? Co1 Br1 2.3786(9) . ? P1 O2 1.502(3) . ? P1 C21 1.780(5) . ? P1 C11 1.797(4) . ? P1 C1 1.824(4) . ? P2 O1 1.502(3) . ? P2 C41 1.792(5) . ? P2 C31 1.802(4) . ? P2 C2 1.838(4) . ? C1 C1 1.564(8) 2_656 ? C1 C2 1.576(5) . ? C1 H1 1.05(7) . ? C2 C2 1.564(8) 2_656 ? C2 H2 0.97(7) . ? C11 C16 1.380(7) . ? C11 C12 1.405(7) . ? C12 C13 1.388(8) . ? C12 H12A 0.9400 . ? C13 C14 1.377(10) . ? C13 H13A 0.9400 . ? C14 C15 1.390(9) . ? C14 H14A 0.9400 . ? C15 C16 1.384(8) . ? C15 H15A 0.9400 . ? C16 H16A 0.9400 . ? C21 C26 1.387(7) . ? C21 C22 1.396(7) . ? C22 C23 1.391(7) . ? C22 H22A 0.9400 . ? C23 C24 1.386(8) . ? C23 H23A 0.9400 . ? C24 C25 1.370(9) . ? C24 H24A 0.9400 . ? C25 C26 1.399(8) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C31 C32 1.385(6) . ? C31 C36 1.385(7) . ? C32 C33 1.383(7) . ? C32 H32A 0.9400 . ? C33 C34 1.372(9) . ? C33 H33A 0.9400 . ? C34 C35 1.368(9) . ? C34 H34A 0.9400 . ? C35 C36 1.378(7) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C41 C42 1.375(7) . ? C41 C46 1.386(7) . ? C42 C43 1.395(7) . ? C42 H42A 0.9400 . ? C43 C44 1.370(9) . ? C43 H43A 0.9400 . ? C44 C45 1.363(10) . ? C44 H44A 0.9400 . ? C45 C46 1.400(8) . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? Cl1 C3 1.570(13) . ? Cl2 C3 1.887(14) . ? C3 H3A 0.9800 . ? C3 H3B 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 O2 Co1 O1 97.57(14) . . ? O2 Co1 Br2 110.50(11) . . ? O1 Co1 Br2 109.06(10) . . ? O2 Co1 Br1 110.92(11) . . ? O1 Co1 Br1 102.58(11) . . ? Br2 Co1 Br1 122.85(4) . . ? O2 P1 C21 113.0(2) . . ? O2 P1 C11 109.1(2) . . ? C21 P1 C11 106.3(2) . . ? O2 P1 C1 113.77(19) . . ? C21 P1 C1 105.7(2) . . ? C11 P1 C1 108.5(2) . . ? O1 P2 C41 114.2(2) . . ? O1 P2 C31 107.6(2) . . ? C41 P2 C31 105.6(2) . . ? O1 P2 C2 110.73(19) . . ? C41 P2 C2 110.7(2) . . ? C31 P2 C2 107.64(19) . . ? P2 O1 Co1 146.8(2) . . ? P1 O2 Co1 140.4(2) . . ? C1 C1 C2 89.0(2) 2_656 . ? C1 C1 P1 118.5(3) 2_656 . ? C2 C1 P1 124.9(3) . . ? C1 C1 H1 108(4) 2_656 . ? C2 C1 H1 101(3) . . ? P1 C1 H1 112(3) . . ? C2 C2 C1 89.0(2) 2_656 . ? C2 C2 P2 110.9(3) 2_656 . ? C1 C2 P2 121.8(3) . . ? C2 C2 H2 113(4) 2_656 . ? C1 C2 H2 113(4) . . ? P2 C2 H2 108(4) . . ? C16 C11 C12 120.8(4) . . ? C16 C11 P1 123.3(4) . . ? C12 C11 P1 115.6(4) . . ? C13 C12 C11 118.0(5) . . ? C13 C12 H12A 121.0 . . ? C11 C12 H12A 121.0 . . ? C14 C13 C12 121.5(6) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C16 C15 C14 119.9(6) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C11 120.0(5) . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C26 C21 C22 119.6(4) . . ? C26 C21 P1 119.4(4) . . ? C22 C21 P1 120.9(4) . . ? C23 C22 C21 120.8(5) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C24 C23 C22 118.2(5) . . ? C24 C23 H23A 120.9 . . ? C22 C23 H23A 120.9 . . ? C25 C24 C23 122.1(5) . . ? C25 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? C24 C25 C26 119.3(5) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.4 . . ? C21 C26 C25 119.9(5) . . ? C21 C26 H26A 120.1 . . ? C25 C26 H26A 120.0 . . ? C32 C31 C36 119.7(4) . . ? C32 C31 P2 122.7(4) . . ? C36 C31 P2 117.3(3) . . ? C31 C32 C33 119.5(5) . . ? C31 C32 H32A 120.3 . . ? C33 C32 H32A 120.3 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C35 C34 C33 120.3(5) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 120.1(5) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C35 C36 C31 120.0(5) . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? C42 C41 C46 120.3(5) . . ? C42 C41 P2 122.9(4) . . ? C46 C41 P2 116.6(4) . . ? C41 C42 C43 119.6(5) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 C42 120.1(6) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C45 C44 C43 120.8(5) . . ? C45 C44 H44A 119.6 . . ? C43 C44 H44A 119.6 . . ? C44 C45 C46 119.8(5) . . ? C44 C45 H45A 120.1 . . ? C46 C45 H45A 120.1 . . ? C41 C46 C45 119.4(6) . . ? C41 C46 H46A 120.3 . . ? C45 C46 H46A 120.3 . . ? Cl1 C3 Cl2 117.5(6) . . ? Cl1 C3 H3A 108.1 . . ? Cl2 C3 H3A 108.1 . . ? Cl1 C3 H3B 107.6 . . ? Cl2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C41 P2 O1 Co1 64.0(4) . . . . ? C31 P2 O1 Co1 -179.1(4) . . . . ? C2 P2 O1 Co1 -61.7(4) . . . . ? O2 Co1 O1 P2 22.4(4) . . . . ? Br2 Co1 O1 P2 -92.4(4) . . . . ? Br1 Co1 O1 P2 135.9(4) . . . . ? C21 P1 O2 Co1 -81.3(4) . . . . ? C11 P1 O2 Co1 160.6(3) . . . . ? C1 P1 O2 Co1 39.3(4) . . . . ? O1 Co1 O2 P1 -1.1(4) . . . . ? Br2 Co1 O2 P1 112.5(3) . . . . ? Br1 Co1 O2 P1 -107.7(3) . . . . ? O2 P1 C1 C1 41.3(4) . . . 2_656 ? C21 P1 C1 C1 165.9(3) . . . 2_656 ? C11 P1 C1 C1 -80.4(4) . . . 2_656 ? O2 P1 C1 C2 -69.4(4) . . . . ? C21 P1 C1 C2 55.2(4) . . . . ? C11 P1 C1 C2 168.9(3) . . . . ? C1 C1 C2 C2 15.4(4) 2_656 . . 2_656 ? P1 C1 C2 C2 140.1(3) . . . 2_656 ? C1 C1 C2 P2 -98.7(4) 2_656 . . . ? P1 C1 C2 P2 26.0(5) . . . . ? O1 P2 C2 C2 -64.6(2) . . . 2_656 ? C41 P2 C2 C2 167.7(2) . . . 2_656 ? C31 P2 C2 C2 52.7(3) . . . 2_656 ? O1 P2 C2 C1 37.7(4) . . . . ? C41 P2 C2 C1 -90.0(3) . . . . ? C31 P2 C2 C1 155.0(3) . . . . ? O2 P1 C11 C16 -167.9(4) . . . . ? C21 P1 C11 C16 69.8(5) . . . . ? C1 P1 C11 C16 -43.5(5) . . . . ? O2 P1 C11 C12 18.2(5) . . . . ? C21 P1 C11 C12 -104.0(4) . . . . ? C1 P1 C11 C12 142.7(4) . . . . ? C16 C11 C12 C13 -0.9(9) . . . . ? P1 C11 C12 C13 173.1(6) . . . . ? C11 C12 C13 C14 1.0(12) . . . . ? C12 C13 C14 C15 -0.2(13) . . . . ? C13 C14 C15 C16 -0.7(13) . . . . ? C14 C15 C16 C11 0.8(11) . . . . ? C12 C11 C16 C15 0.0(9) . . . . ? P1 C11 C16 C15 -173.5(5) . . . . ? O2 P1 C21 C26 -10.9(4) . . . . ? C11 P1 C21 C26 108.8(4) . . . . ? C1 P1 C21 C26 -136.0(4) . . . . ? O2 P1 C21 C22 172.2(4) . . . . ? C11 P1 C21 C22 -68.1(4) . . . . ? C1 P1 C21 C22 47.1(4) . . . . ? C26 C21 C22 C23 -1.3(7) . . . . ? P1 C21 C22 C23 175.6(4) . . . . ? C21 C22 C23 C24 1.3(8) . . . . ? C22 C23 C24 C25 -1.0(8) . . . . ? C23 C24 C25 C26 0.6(9) . . . . ? C22 C21 C26 C25 0.8(7) . . . . ? P1 C21 C26 C25 -176.1(4) . . . . ? C24 C25 C26 C21 -0.5(8) . . . . ? O1 P2 C31 C32 -145.8(4) . . . . ? C41 P2 C31 C32 -23.4(5) . . . . ? C2 P2 C31 C32 94.9(4) . . . . ? O1 P2 C31 C36 29.0(4) . . . . ? C41 P2 C31 C36 151.4(4) . . . . ? C2 P2 C31 C36 -90.3(4) . . . . ? C36 C31 C32 C33 -0.4(8) . . . . ? P2 C31 C32 C33 174.3(5) . . . . ? C31 C32 C33 C34 1.1(10) . . . . ? C32 C33 C34 C35 0.2(11) . . . . ? C33 C34 C35 C36 -2.3(11) . . . . ? C34 C35 C36 C31 3.1(9) . . . . ? C32 C31 C36 C35 -1.7(8) . . . . ? P2 C31 C36 C35 -176.6(4) . . . . ? O1 P2 C41 C42 -158.6(4) . . . . ? C31 P2 C41 C42 83.4(4) . . . . ? C2 P2 C41 C42 -32.8(5) . . . . ? O1 P2 C41 C46 27.5(4) . . . . ? C31 P2 C41 C46 -90.5(4) . . . . ? C2 P2 C41 C46 153.3(4) . . . . ? C46 C41 C42 C43 1.6(8) . . . . ? P2 C41 C42 C43 -172.0(4) . . . . ? C41 C42 C43 C44 -0.1(8) . . . . ? C42 C43 C44 C45 -1.3(9) . . . . ? C43 C44 C45 C46 1.2(9) . . . . ? C42 C41 C46 C45 -1.7(8) . . . . ? P2 C41 C46 C45 172.3(4) . . . . ? C44 C45 C46 C41 0.4(9) . . . . ? _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction 0.981 _refine_diff_density_max 0.900 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.110 #===END data_7c _database_code_depnum_ccdc_archive 'CCDC 691869' _audit_creation_method SHELXL-97 _chemical_name_systematic '[Co2I4(dppcbO4)]' _chemical_name_common (Co2I4(dppcbO4)) _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Co2 I4 O4 P4, 2(C H2 Cl2)' _chemical_formula_sum 'C54 H48 Cl4 Co2 I4 O4 P4' _chemical_formula_weight 1652.112 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' Co Co 0.3494 0.9721 '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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 14.4421(2) _cell_length_b 20.1430(2) _cell_length_c 21.5066(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.5027(7) _cell_angle_gamma 90.00 _cell_volume 6130.77(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 70821 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.022 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 2.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.190 _exptl_absorpt_correction_T_max 0.565 _exptl_absorpt_process_details 'Otwinowski et al, 1997' _diffrn_ambient_temperature 223(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 'Kappa CCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37797 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.09 _reflns_number_total 12170 _reflns_number_gt 9466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'Denzo and Scalepack' _computing_data_reduction 'Denzo and Scalepack' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-NT V6.1' _computing_publication_material 'SHELXTL-NT V6.1' _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^)+(0.0649P)^2^+4.8538P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11879 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 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 0.65186(4) 0.32157(3) -0.02206(2) 0.03129(13) Uani 1 1 d . . . Co2 Co 0.14679(4) 0.20636(3) -0.14509(3) 0.03551(14) Uani 1 1 d . . . I1 I 0.57278(2) 0.418256(15) 0.024995(16) 0.05164(10) Uani 1 1 d . . . I2 I 0.83159(2) 0.316695(17) 0.003480(16) 0.05206(10) Uani 1 1 d . . . I3 I 0.22219(2) 0.118497(16) -0.206986(17) 0.05712(11) Uani 1 1 d . . . I4 I -0.03012(2) 0.200784(19) -0.147358(17) 0.05600(11) Uani 1 1 d . . . P1 P 0.53827(7) 0.31771(5) -0.17530(4) 0.0285(2) Uani 1 1 d . . . P2 P 0.52122(7) 0.19551(4) -0.05505(4) 0.0268(2) Uani 1 1 d . . . P3 P 0.28461(7) 0.27281(5) -0.02716(5) 0.0294(2) Uani 1 1 d . . . P4 P 0.24411(7) 0.34935(5) -0.18364(5) 0.0300(2) Uani 1 1 d . . . O1 O 0.6104(2) 0.31920(13) -0.11477(12) 0.0345(6) Uani 1 1 d . . . O2 O 0.58411(19) 0.24019(12) -0.00799(12) 0.0314(6) Uani 1 1 d . . . O3 O 0.2221(2) 0.21680(13) -0.05802(13) 0.0354(6) Uani 1 1 d . . . O4 O 0.1795(2) 0.29275(14) -0.17670(15) 0.0421(7) Uani 1 1 d . . . C1 C 0.4253(3) 0.28653(19) -0.16166(18) 0.0293(8) Uani 1 1 d . . . C2 C 0.4212(3) 0.23863(18) -0.10400(17) 0.0270(7) Uani 1 1 d . . . C3 C 0.3773(3) 0.29546(18) -0.07003(17) 0.0262(7) Uani 1 1 d D . . C4 C 0.3622(3) 0.33795(19) -0.13396(17) 0.0268(8) Uani 1 1 d . . . C11 C 0.5244(3) 0.4006(2) -0.2068(2) 0.0362(9) Uani 1 1 d . . . C12 C 0.5265(4) 0.4142(3) -0.2701(2) 0.0534(12) Uani 1 1 d . . . H12A H 0.5291 0.3793 -0.2987 0.064 Uiso 1 1 calc R . . C13 C 0.5248(5) 0.4795(3) -0.2906(3) 0.0708(17) Uani 1 1 d . . . H13A H 0.5260 0.4886 -0.3333 0.085 Uiso 1 1 calc R . . C14 C 0.5212(4) 0.5310(3) -0.2491(3) 0.0744(18) Uani 1 1 d . . . H14A H 0.5212 0.5752 -0.2632 0.089 Uiso 1 1 calc R . . C15 C 0.5179(4) 0.5178(2) -0.1874(3) 0.0635(15) Uani 1 1 d . . . H15A H 0.5131 0.5530 -0.1595 0.076 Uiso 1 1 calc R . . C16 C 0.5214(3) 0.4530(2) -0.1653(2) 0.0459(11) Uani 1 1 d . . . H16A H 0.5218 0.4446 -0.1222 0.055 Uiso 1 1 calc R . . C21 C 0.5751(3) 0.26632(19) -0.23377(17) 0.0302(8) Uani 1 1 d . . . C22 C 0.5129(3) 0.2481(2) -0.28965(19) 0.0435(10) Uani 1 1 d . . . H22A H 0.4484 0.2589 -0.2957 0.052 Uiso 1 1 calc R . . C23 C 0.5476(4) 0.2137(3) -0.3362(2) 0.0509(12) Uani 1 1 d . . . H23A H 0.5059 0.2006 -0.3735 0.061 Uiso 1 1 calc R . . C24 C 0.6409(4) 0.1988(2) -0.3285(2) 0.0523(12) Uani 1 1 d . . . H24A H 0.6635 0.1769 -0.3611 0.063 Uiso 1 1 calc R . . C25 C 0.7030(3) 0.2156(2) -0.2727(2) 0.0494(11) Uani 1 1 d . . . H25A H 0.7671 0.2038 -0.2669 0.059 Uiso 1 1 calc R . . C26 C 0.6698(3) 0.2498(2) -0.2256(2) 0.0364(9) Uani 1 1 d . . . H26A H 0.7118 0.2618 -0.1880 0.044 Uiso 1 1 calc R . . C31 C 0.4732(3) 0.13224(18) -0.01200(19) 0.0328(8) Uani 1 1 d . . . C32 C 0.3998(3) 0.0908(2) -0.0409(2) 0.0431(10) Uani 1 1 d . . . H32A H 0.3694 0.0981 -0.0832 0.052 Uiso 1 1 calc R . . C33 C 0.3719(4) 0.0387(2) -0.0065(3) 0.0546(13) Uani 1 1 d . . . H33A H 0.3228 0.0104 -0.0258 0.066 Uiso 1 1 calc R . . C34 C 0.4159(4) 0.0284(2) 0.0554(3) 0.0589(14) Uani 1 1 d . . . H34A H 0.3962 -0.0069 0.0782 0.071 Uiso 1 1 calc R . . C35 C 0.4874(4) 0.0684(3) 0.0842(2) 0.0544(13) Uani 1 1 d . . . H35A H 0.5170 0.0602 0.1265 0.065 Uiso 1 1 calc R . . C36 C 0.5175(3) 0.1216(2) 0.0512(2) 0.0416(10) Uani 1 1 d . . . H36A H 0.5665 0.1497 0.0712 0.050 Uiso 1 1 calc R . . C41 C 0.5855(3) 0.15299(18) -0.10646(18) 0.0288(8) Uani 1 1 d . . . C42 C 0.5402(3) 0.1200(2) -0.1608(2) 0.0395(9) Uani 1 1 d . . . H42A H 0.4743 0.1230 -0.1741 0.047 Uiso 1 1 calc R . . C43 C 0.5923(4) 0.0831(2) -0.1946(2) 0.0522(12) Uani 1 1 d . . . H43A H 0.5616 0.0610 -0.2315 0.063 Uiso 1 1 calc R . . C44 C 0.6878(4) 0.0776(3) -0.1759(3) 0.0573(13) Uani 1 1 d . . . H44A H 0.7223 0.0513 -0.1994 0.069 Uiso 1 1 calc R . . C45 C 0.7344(3) 0.1110(2) -0.1218(2) 0.0499(12) Uani 1 1 d . . . H45A H 0.8003 0.1077 -0.1088 0.060 Uiso 1 1 calc R . . C46 C 0.6830(3) 0.1485(2) -0.0880(2) 0.0368(9) Uani 1 1 d . . . H46A H 0.7140 0.1716 -0.0518 0.044 Uiso 1 1 calc R . . C51 C 0.3413(3) 0.2478(2) 0.05149(19) 0.0358(9) Uani 1 1 d . . . C52 C 0.3073(4) 0.1919(2) 0.0773(2) 0.0503(12) Uani 1 1 d . . . H52A H 0.2593 0.1660 0.0528 0.060 Uiso 1 1 calc R . . C53 C 0.3449(5) 0.1747(3) 0.1396(3) 0.0647(15) Uani 1 1 d . . . H53A H 0.3228 0.1366 0.1573 0.078 Uiso 1 1 calc R . . C54 C 0.4136(5) 0.2126(3) 0.1754(2) 0.0702(17) Uani 1 1 d . . . H54A H 0.4373 0.2010 0.2179 0.084 Uiso 1 1 calc R . . C55 C 0.4476(5) 0.2660(3) 0.1510(2) 0.0700(17) Uani 1 1 d . . . H55A H 0.4960 0.2910 0.1761 0.084 Uiso 1 1 calc R . . C56 C 0.4117(4) 0.2851(3) 0.0883(2) 0.0554(13) Uani 1 1 d . . . H56A H 0.4353 0.3230 0.0714 0.066 Uiso 1 1 calc R . . C61 C 0.2201(3) 0.3469(2) -0.01848(18) 0.0332(8) Uani 1 1 d . . . C62 C 0.2651(3) 0.4083(2) -0.0093(2) 0.0390(9) Uani 1 1 d . . . H62A H 0.3299 0.4117 -0.0098 0.047 Uiso 1 1 calc R . . C63 C 0.2147(3) 0.4643(2) 0.0004(2) 0.0455(11) Uani 1 1 d . . . H63A H 0.2453 0.5056 0.0072 0.055 Uiso 1 1 calc R . . C64 C 0.1207(4) 0.4593(2) 0.0001(3) 0.0554(13) Uani 1 1 d . . . H64A H 0.0860 0.4977 0.0051 0.066 Uiso 1 1 calc R . . C65 C 0.0757(4) 0.3985(3) -0.0074(3) 0.0613(14) Uani 1 1 d . . . H65A H 0.0113 0.3955 -0.0055 0.074 Uiso 1 1 calc R . . C66 C 0.1248(3) 0.3419(2) -0.0178(2) 0.0449(10) Uani 1 1 d . . . H66A H 0.0938 0.3007 -0.0242 0.054 Uiso 1 1 calc R . . C71 C 0.2596(3) 0.3539(2) -0.26419(19) 0.0404(10) Uani 1 1 d . . . C72 C 0.2435(4) 0.2963(3) -0.3007(2) 0.0537(13) Uani 1 1 d . . . H72A H 0.2256 0.2569 -0.2830 0.064 Uiso 1 1 calc R . . C73 C 0.2542(5) 0.2978(4) -0.3634(3) 0.077(2) Uani 1 1 d . . . H73A H 0.2440 0.2591 -0.3882 0.092 Uiso 1 1 calc R . . C74 C 0.2794(5) 0.3548(5) -0.3890(3) 0.090(2) Uani 1 1 d . . . H74A H 0.2857 0.3552 -0.4316 0.109 Uiso 1 1 calc R . . C75 C 0.2959(5) 0.4121(4) -0.3540(3) 0.080(2) Uani 1 1 d . . . H75A H 0.3143 0.4510 -0.3724 0.096 Uiso 1 1 calc R . . C76 C 0.2853(4) 0.4124(3) -0.2908(2) 0.0556(13) Uani 1 1 d . . . H76A H 0.2954 0.4515 -0.2665 0.067 Uiso 1 1 calc R . . C81 C 0.1939(3) 0.4266(2) -0.16640(19) 0.0351(9) Uani 1 1 d . . . C82 C 0.2468(4) 0.4854(2) -0.1559(2) 0.0421(10) Uani 1 1 d . . . H82A H 0.3124 0.4846 -0.1540 0.051 Uiso 1 1 calc R . . C83 C 0.2013(4) 0.5444(2) -0.1483(2) 0.0565(13) Uani 1 1 d . . . H83A H 0.2363 0.5840 -0.1408 0.068 Uiso 1 1 calc R . . C84 C 0.1058(4) 0.5457(3) -0.1515(3) 0.0657(16) Uani 1 1 d . . . H84A H 0.0756 0.5861 -0.1464 0.079 Uiso 1 1 calc R . . C85 C 0.0539(4) 0.4883(3) -0.1620(3) 0.0665(15) Uani 1 1 d . . . H85A H -0.0117 0.4896 -0.1644 0.080 Uiso 1 1 calc R . . C86 C 0.0975(3) 0.4285(2) -0.1693(2) 0.0475(11) Uani 1 1 d . . . H86A H 0.0617 0.3892 -0.1762 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.78702(16) 0.52624(12) -0.16580(9) 0.1021(6) Uani 1 1 d . . . Cl2 Cl 0.8208(3) 0.39390(17) -0.2039(2) 0.198(2) Uani 1 1 d . . . C5 C 0.7769(6) 0.4432(5) -0.1526(4) 0.112(3) Uani 1 1 d . . . H5A H 0.8101 0.4331 -0.1093 0.134 Uiso 1 1 calc R . . H5B H 0.7100 0.4325 -0.1554 0.134 Uiso 1 1 calc R . . Cl3 Cl 0.1354(2) 0.0314(2) 0.0412(2) 0.206(2) Uani 1 1 d . . . Cl4 Cl 0.0255(4) 0.1434(3) 0.0529(2) 0.233(2) Uani 1 1 d . . . C6 C 0.0706(9) 0.0933(6) -0.0011(6) 0.165(6) Uani 1 1 d . . . H6A H 0.0188 0.0744 -0.0326 0.199 Uiso 1 1 calc R . . H6B H 0.1106 0.1198 -0.0235 0.199 Uiso 1 1 calc R . . H1 H 0.393(4) 0.269(2) -0.198(2) 0.050 Uiso 1 1 d . . . H2 H 0.373(4) 0.206(3) -0.118(2) 0.050 Uiso 1 1 d . . . H3 H 0.430(2) 0.317(2) -0.0429(19) 0.050 Uiso 1 1 d D . . H4 H 0.388(4) 0.379(3) -0.127(2) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0309(3) 0.0278(3) 0.0314(3) -0.0005(2) -0.0030(2) -0.0047(2) Co2 0.0335(3) 0.0296(3) 0.0412(3) -0.0068(2) 0.0019(2) -0.0068(2) I1 0.04667(19) 0.03820(17) 0.0683(2) -0.01683(14) 0.00732(15) -0.00479(12) I2 0.03114(16) 0.0646(2) 0.05592(19) 0.00671(15) -0.00213(14) -0.00707(13) I3 0.0541(2) 0.04547(19) 0.0677(2) -0.02607(15) 0.00240(16) 0.00173(14) I4 0.03457(17) 0.0713(2) 0.0611(2) -0.00804(16) 0.00704(15) -0.01157(14) P1 0.0283(5) 0.0278(5) 0.0275(5) 0.0038(4) 0.0015(4) 0.0014(4) P2 0.0272(5) 0.0220(5) 0.0294(5) 0.0030(4) 0.0010(4) -0.0015(4) P3 0.0289(5) 0.0289(5) 0.0296(5) -0.0027(4) 0.0038(4) -0.0010(4) P4 0.0275(5) 0.0269(5) 0.0328(5) 0.0002(4) -0.0009(4) 0.0011(4) O1 0.0348(15) 0.0356(15) 0.0287(13) 0.0017(11) -0.0044(12) -0.0036(11) O2 0.0347(15) 0.0277(13) 0.0288(13) 0.0031(11) -0.0005(11) -0.0045(11) O3 0.0359(15) 0.0303(14) 0.0388(15) -0.0023(11) 0.0044(12) -0.0047(11) O4 0.0379(16) 0.0344(15) 0.0514(17) -0.0003(13) 0.0024(14) -0.0067(12) C1 0.032(2) 0.0268(19) 0.0265(18) 0.0016(15) -0.0013(16) 0.0022(15) C2 0.0234(18) 0.0251(18) 0.0308(18) 0.0006(15) 0.0011(15) -0.0013(15) C3 0.0196(17) 0.0256(18) 0.0307(18) 0.0002(14) -0.0015(15) 0.0002(14) C4 0.0227(18) 0.0238(18) 0.0321(19) 0.0026(15) 0.0014(15) -0.0009(14) C11 0.027(2) 0.036(2) 0.044(2) 0.0140(18) 0.0031(17) 0.0026(16) C12 0.065(3) 0.050(3) 0.042(3) 0.019(2) 0.003(2) 0.000(2) C13 0.081(4) 0.063(4) 0.066(4) 0.033(3) 0.011(3) 0.006(3) C14 0.068(4) 0.048(3) 0.106(5) 0.041(4) 0.015(3) 0.009(3) C15 0.060(3) 0.031(2) 0.100(5) 0.009(3) 0.017(3) 0.003(2) C16 0.048(3) 0.036(2) 0.054(3) 0.003(2) 0.011(2) 0.000(2) C21 0.030(2) 0.034(2) 0.0276(18) 0.0051(15) 0.0059(15) -0.0008(16) C22 0.037(2) 0.061(3) 0.032(2) -0.005(2) 0.0069(18) -0.003(2) C23 0.062(3) 0.058(3) 0.031(2) -0.004(2) 0.005(2) -0.004(2) C24 0.071(4) 0.049(3) 0.044(3) -0.002(2) 0.026(3) 0.004(2) C25 0.041(3) 0.054(3) 0.057(3) 0.007(2) 0.020(2) 0.007(2) C26 0.032(2) 0.037(2) 0.039(2) 0.0084(17) 0.0057(17) -0.0011(17) C31 0.034(2) 0.0211(18) 0.043(2) 0.0042(16) 0.0078(17) 0.0018(15) C32 0.046(3) 0.032(2) 0.051(3) 0.0016(19) 0.008(2) -0.0065(18) C33 0.054(3) 0.035(2) 0.079(4) -0.003(2) 0.021(3) -0.011(2) C34 0.074(4) 0.038(3) 0.073(4) 0.021(2) 0.036(3) 0.002(2) C35 0.062(3) 0.049(3) 0.053(3) 0.024(2) 0.016(2) 0.008(2) C36 0.046(3) 0.037(2) 0.043(2) 0.0111(18) 0.011(2) 0.0025(18) C41 0.0281(19) 0.0235(18) 0.0349(19) 0.0057(15) 0.0065(16) 0.0019(14) C42 0.040(2) 0.039(2) 0.037(2) 0.0000(18) 0.0033(18) -0.0005(18) C43 0.067(3) 0.049(3) 0.040(2) -0.006(2) 0.010(2) 0.003(2) C44 0.072(4) 0.050(3) 0.060(3) 0.008(2) 0.035(3) 0.017(3) C45 0.042(3) 0.050(3) 0.064(3) 0.013(2) 0.025(2) 0.014(2) C46 0.032(2) 0.034(2) 0.044(2) 0.0073(17) 0.0065(18) 0.0000(16) C51 0.032(2) 0.041(2) 0.035(2) -0.0006(17) 0.0084(17) 0.0013(17) C52 0.064(3) 0.047(3) 0.040(2) 0.004(2) 0.010(2) 0.005(2) C53 0.092(4) 0.057(3) 0.049(3) 0.017(2) 0.023(3) 0.006(3) C54 0.092(5) 0.078(4) 0.034(3) 0.010(3) -0.003(3) 0.009(3) C55 0.085(4) 0.079(4) 0.035(3) -0.003(3) -0.015(3) 0.007(3) C56 0.070(3) 0.057(3) 0.032(2) 0.001(2) -0.006(2) -0.012(3) C61 0.030(2) 0.036(2) 0.033(2) -0.0012(16) 0.0041(16) 0.0001(16) C62 0.033(2) 0.038(2) 0.046(2) -0.0066(18) 0.0069(19) -0.0017(17) C63 0.048(3) 0.033(2) 0.057(3) -0.009(2) 0.015(2) -0.0083(19) C64 0.045(3) 0.038(3) 0.086(4) -0.011(2) 0.020(3) 0.005(2) C65 0.035(3) 0.051(3) 0.100(4) -0.007(3) 0.018(3) 0.006(2) C66 0.035(2) 0.038(2) 0.062(3) -0.002(2) 0.010(2) -0.0046(18) C71 0.033(2) 0.052(3) 0.031(2) 0.0003(18) -0.0055(17) 0.0093(18) C72 0.049(3) 0.065(3) 0.040(2) -0.010(2) -0.011(2) 0.012(2) C73 0.064(4) 0.115(6) 0.041(3) -0.028(3) -0.012(3) 0.014(4) C74 0.064(4) 0.171(8) 0.032(3) -0.006(4) -0.001(3) 0.009(5) C75 0.077(4) 0.116(6) 0.041(3) 0.020(3) 0.002(3) -0.012(4) C76 0.054(3) 0.067(3) 0.040(3) 0.008(2) -0.004(2) -0.009(2) C81 0.034(2) 0.036(2) 0.031(2) -0.0010(16) -0.0048(16) 0.0053(17) C82 0.052(3) 0.030(2) 0.042(2) -0.0014(18) 0.003(2) -0.0004(19) C83 0.076(4) 0.029(2) 0.059(3) -0.004(2) -0.001(3) 0.006(2) C84 0.074(4) 0.039(3) 0.078(4) -0.006(3) -0.001(3) 0.027(3) C85 0.044(3) 0.064(4) 0.087(4) 0.002(3) 0.003(3) 0.025(3) C86 0.037(2) 0.050(3) 0.054(3) 0.001(2) 0.003(2) 0.011(2) Cl1 0.1090(15) 0.1195(16) 0.0799(11) 0.0180(11) 0.0241(11) 0.0112(12) Cl2 0.246(4) 0.142(2) 0.246(4) -0.109(3) 0.149(3) -0.102(3) C5 0.090(6) 0.144(8) 0.111(6) 0.013(6) 0.041(5) -0.030(5) Cl3 0.115(2) 0.190(3) 0.320(5) 0.137(4) 0.061(3) 0.023(2) Cl4 0.334(7) 0.224(5) 0.167(3) 0.011(3) 0.111(4) 0.086(5) C6 0.154(10) 0.164(11) 0.155(10) 0.084(9) -0.026(8) -0.052(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.963(3) . ? Co1 O1 1.965(3) . ? Co1 I2 2.5456(8) . ? Co1 I1 2.5657(7) . ? Co2 O4 1.960(3) . ? Co2 O3 1.980(3) . ? Co2 I4 2.5481(8) . ? Co2 I3 2.5823(8) . ? P1 O1 1.497(3) . ? P1 C21 1.789(4) . ? P1 C11 1.798(4) . ? P1 C1 1.826(4) . ? P2 O2 1.514(3) . ? P2 C31 1.794(4) . ? P2 C41 1.796(4) . ? P2 C2 1.828(4) . ? P3 O3 1.513(3) . ? P3 C61 1.788(4) . ? P3 C51 1.798(4) . ? P3 C3 1.828(4) . ? P4 O4 1.499(3) . ? P4 C81 1.786(4) . ? P4 C71 1.793(4) . ? P4 C4 1.837(4) . ? C1 C4 1.573(5) . ? C1 C2 1.582(5) . ? C1 H1 0.90(5) . ? C2 C3 1.559(5) . ? C2 H2 0.96(5) . ? C3 C4 1.597(5) . ? C3 H3 0.97(4) . ? C4 H4 0.90(5) . ? C11 C16 1.389(7) . ? C11 C12 1.394(6) . ? C12 C13 1.384(8) . ? C12 H12A 0.9400 . ? C13 C14 1.377(10) . ? C13 H13A 0.9400 . ? C14 C15 1.363(9) . ? C14 H14A 0.9400 . ? C15 C16 1.386(7) . ? C15 H15A 0.9400 . ? C16 H16A 0.9400 . ? C21 C26 1.385(6) . ? C21 C22 1.399(6) . ? C22 C23 1.390(7) . ? C22 H22A 0.9400 . ? C23 C24 1.358(7) . ? C23 H23A 0.9400 . ? C24 C25 1.389(7) . ? C24 H24A 0.9400 . ? C25 C26 1.388(6) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C31 C32 1.394(6) . ? C31 C36 1.399(6) . ? C32 C33 1.389(7) . ? C32 H32A 0.9400 . ? C33 C34 1.372(8) . ? C33 H33A 0.9400 . ? C34 C35 1.358(8) . ? C34 H34A 0.9400 . ? C35 C36 1.402(6) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C41 C46 1.387(6) . ? C41 C42 1.389(6) . ? C42 C43 1.366(7) . ? C42 H42A 0.9400 . ? C43 C44 1.362(8) . ? C43 H43A 0.9400 . ? C44 C45 1.395(8) . ? C44 H44A 0.9400 . ? C45 C46 1.366(6) . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? C51 C56 1.380(6) . ? C51 C52 1.388(7) . ? C52 C53 1.386(7) . ? C52 H52A 0.9400 . ? C53 C54 1.363(9) . ? C53 H53A 0.9400 . ? C54 C55 1.332(9) . ? C54 H54A 0.9400 . ? C55 C56 1.398(7) . ? C55 H55A 0.9400 . ? C56 H56A 0.9400 . ? C61 C66 1.384(6) . ? C61 C62 1.393(6) . ? C62 C63 1.380(6) . ? C62 H62A 0.9400 . ? C63 C64 1.361(7) . ? C63 H63A 0.9400 . ? C64 C65 1.382(7) . ? C64 H64A 0.9400 . ? C65 C66 1.383(7) . ? C65 H65A 0.9400 . ? C66 H66A 0.9400 . ? C71 C76 1.391(7) . ? C71 C72 1.394(7) . ? C72 C73 1.388(8) . ? C72 H72A 0.9400 . ? C73 C74 1.354(11) . ? C73 H73A 0.9400 . ? C74 C75 1.372(11) . ? C74 H74A 0.9400 . ? C75 C76 1.399(8) . ? C75 H75A 0.9400 . ? C76 H76A 0.9400 . ? C81 C86 1.381(6) . ? C81 C82 1.403(6) . ? C82 C83 1.385(7) . ? C82 H82A 0.9400 . ? C83 C84 1.367(8) . ? C83 H83A 0.9400 . ? C84 C85 1.372(8) . ? C84 H84A 0.9400 . ? C85 C86 1.382(7) . ? C85 H85A 0.9400 . ? C86 H86A 0.9400 . ? Cl1 C5 1.707(10) . ? Cl2 C5 1.699(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? Cl3 C6 1.709(11) . ? Cl4 C6 1.759(16) . ? C6 H6A 0.9800 . ? C6 H6B 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 O2 Co1 O1 94.34(11) . . ? O2 Co1 I2 116.91(8) . . ? O1 Co1 I2 108.02(9) . . ? O2 Co1 I1 107.35(9) . . ? O1 Co1 I1 110.43(9) . . ? I2 Co1 I1 117.33(2) . . ? O4 Co2 O3 96.23(12) . . ? O4 Co2 I4 110.05(9) . . ? O3 Co2 I4 112.49(9) . . ? O4 Co2 I3 105.89(10) . . ? O3 Co2 I3 110.59(9) . . ? I4 Co2 I3 118.96(3) . . ? O1 P1 C21 111.72(17) . . ? O1 P1 C11 108.37(18) . . ? C21 P1 C11 107.38(19) . . ? O1 P1 C1 110.89(17) . . ? C21 P1 C1 108.30(18) . . ? C11 P1 C1 110.12(18) . . ? O2 P2 C31 108.62(17) . . ? O2 P2 C41 112.35(17) . . ? C31 P2 C41 106.21(18) . . ? O2 P2 C2 113.72(16) . . ? C31 P2 C2 107.01(18) . . ? C41 P2 C2 108.54(17) . . ? O3 P3 C61 112.99(18) . . ? O3 P3 C51 108.89(18) . . ? C61 P3 C51 106.54(19) . . ? O3 P3 C3 113.42(17) . . ? C61 P3 C3 107.05(18) . . ? C51 P3 C3 107.60(18) . . ? O4 P4 C81 110.79(19) . . ? O4 P4 C71 109.6(2) . . ? C81 P4 C71 106.8(2) . . ? O4 P4 C4 111.75(17) . . ? C81 P4 C4 110.89(18) . . ? C71 P4 C4 106.77(19) . . ? P1 O1 Co1 154.4(2) . . ? P2 O2 Co1 130.10(16) . . ? P3 O3 Co2 131.39(17) . . ? P4 O4 Co2 155.2(2) . . ? C4 C1 C2 89.4(3) . . ? C4 C1 P1 116.0(3) . . ? C2 C1 P1 120.6(3) . . ? C4 C1 H1 111(3) . . ? C2 C1 H1 111(3) . . ? P1 C1 H1 108(3) . . ? C3 C2 C1 90.1(3) . . ? C3 C2 P2 115.3(2) . . ? C1 C2 P2 126.4(3) . . ? C3 C2 H2 109(3) . . ? C1 C2 H2 108(3) . . ? P2 C2 H2 107(3) . . ? C2 C3 C4 89.3(3) . . ? C2 C3 P3 117.4(3) . . ? C4 C3 P3 125.5(2) . . ? C2 C3 H3 106(3) . . ? C4 C3 H3 104(3) . . ? P3 C3 H3 112(3) . . ? C1 C4 C3 89.1(3) . . ? C1 C4 P4 113.7(3) . . ? C3 C4 P4 121.3(3) . . ? C1 C4 H4 114(3) . . ? C3 C4 H4 112(3) . . ? P4 C4 H4 107(3) . . ? C16 C11 C12 119.2(4) . . ? C16 C11 P1 118.6(3) . . ? C12 C11 P1 121.9(4) . . ? C13 C12 C11 119.7(5) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C15 C14 C13 119.8(5) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 120.7(6) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C15 C16 C11 119.9(5) . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C26 C21 C22 119.7(4) . . ? C26 C21 P1 118.3(3) . . ? C22 C21 P1 121.7(3) . . ? C23 C22 C21 119.2(4) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C23 C24 C25 120.4(4) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 119.6(4) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C21 C26 C25 120.2(4) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C32 C31 C36 120.1(4) . . ? C32 C31 P2 122.2(3) . . ? C36 C31 P2 117.5(3) . . ? C33 C32 C31 119.4(5) . . ? C33 C32 H32A 120.3 . . ? C31 C32 H32A 120.3 . . ? C34 C33 C32 120.2(5) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C35 C34 C33 121.1(4) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C36 120.5(5) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C31 C36 C35 118.7(4) . . ? C31 C36 H36A 120.6 . . ? C35 C36 H36A 120.6 . . ? C46 C41 C42 119.3(4) . . ? C46 C41 P2 118.3(3) . . ? C42 C41 P2 122.1(3) . . ? C43 C42 C41 119.5(4) . . ? C43 C42 H42A 120.3 . . ? C41 C42 H42A 120.3 . . ? C44 C43 C42 121.3(5) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C43 C44 C45 119.9(5) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C46 C45 C44 119.2(5) . . ? C46 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? C45 C46 C41 120.8(4) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? C56 C51 C52 119.4(4) . . ? C56 C51 P3 122.2(3) . . ? C52 C51 P3 118.2(3) . . ? C53 C52 C51 119.2(5) . . ? C53 C52 H52A 120.4 . . ? C51 C52 H52A 120.4 . . ? C54 C53 C52 120.4(5) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C55 C54 C53 121.0(5) . . ? C55 C54 H54A 119.5 . . ? C53 C54 H54A 119.5 . . ? C54 C55 C56 120.4(6) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C51 C56 C55 119.6(5) . . ? C51 C56 H56A 120.2 . . ? C55 C56 H56A 120.2 . . ? C66 C61 C62 120.0(4) . . ? C66 C61 P3 118.7(3) . . ? C62 C61 P3 121.2(3) . . ? C63 C62 C61 120.1(4) . . ? C63 C62 H62A 119.9 . . ? C61 C62 H62A 119.9 . . ? C64 C63 C62 119.7(4) . . ? C64 C63 H63A 120.2 . . ? C62 C63 H63A 120.2 . . ? C63 C64 C65 120.8(4) . . ? C63 C64 H64A 119.6 . . ? C65 C64 H64A 119.6 . . ? C64 C65 C66 120.3(5) . . ? C64 C65 H65A 119.8 . . ? C66 C65 H65A 119.8 . . ? C65 C66 C61 119.0(4) . . ? C65 C66 H66A 120.5 . . ? C61 C66 H66A 120.5 . . ? C76 C71 C72 120.0(5) . . ? C76 C71 P4 122.4(4) . . ? C72 C71 P4 117.6(4) . . ? C73 C72 C71 119.4(6) . . ? C73 C72 H72A 120.3 . . ? C71 C72 H72A 120.3 . . ? C74 C73 C72 120.2(6) . . ? C74 C73 H73A 119.9 . . ? C72 C73 H73A 119.9 . . ? C73 C74 C75 121.5(6) . . ? C73 C74 H74A 119.2 . . ? C75 C74 H74A 119.2 . . ? C74 C75 C76 119.6(7) . . ? C74 C75 H75A 120.2 . . ? C76 C75 H75A 120.2 . . ? C71 C76 C75 119.1(6) . . ? C71 C76 H76A 120.4 . . ? C75 C76 H76A 120.4 . . ? C86 C81 C82 119.7(4) . . ? C86 C81 P4 117.5(3) . . ? C82 C81 P4 122.5(3) . . ? C83 C82 C81 119.2(5) . . ? C83 C82 H82A 120.4 . . ? C81 C82 H82A 120.4 . . ? C84 C83 C82 120.5(5) . . ? C84 C83 H83A 119.7 . . ? C82 C83 H83A 119.7 . . ? C83 C84 C85 120.3(5) . . ? C83 C84 H84A 119.8 . . ? C85 C84 H84A 119.8 . . ? C84 C85 C86 120.5(5) . . ? C84 C85 H85A 119.8 . . ? C86 C85 H85A 119.8 . . ? C81 C86 C85 119.8(5) . . ? C81 C86 H86A 120.1 . . ? C85 C86 H86A 120.1 . . ? Cl2 C5 Cl1 114.2(5) . . ? Cl2 C5 H5A 108.7 . . ? Cl1 C5 H5A 108.7 . . ? Cl2 C5 H5B 108.7 . . ? Cl1 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? Cl3 C6 Cl4 107.5(7) . . ? Cl3 C6 H6A 110.2 . . ? Cl4 C6 H6A 110.2 . . ? Cl3 C6 H6B 110.2 . . ? Cl4 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 P1 O1 Co1 -142.9(4) . . . . ? C11 P1 O1 Co1 99.0(4) . . . . ? C1 P1 O1 Co1 -22.0(5) . . . . ? O2 Co1 O1 P1 57.3(4) . . . . ? I2 Co1 O1 P1 177.5(4) . . . . ? I1 Co1 O1 P1 -53.0(4) . . . . ? C31 P2 O2 Co1 -175.8(2) . . . . ? C41 P2 O2 Co1 67.0(3) . . . . ? C2 P2 O2 Co1 -56.8(3) . . . . ? O1 Co1 O2 P2 -1.5(2) . . . . ? I2 Co1 O2 P2 -114.2(2) . . . . ? I1 Co1 O2 P2 111.5(2) . . . . ? C61 P3 O3 Co2 67.0(3) . . . . ? C51 P3 O3 Co2 -174.9(2) . . . . ? C3 P3 O3 Co2 -55.1(3) . . . . ? O4 Co2 O3 P3 -0.6(3) . . . . ? I4 Co2 O3 P3 -115.3(2) . . . . ? I3 Co2 O3 P3 109.0(2) . . . . ? C81 P4 O4 Co2 -128.2(5) . . . . ? C71 P4 O4 Co2 114.2(5) . . . . ? C4 P4 O4 Co2 -4.0(6) . . . . ? O3 Co2 O4 P4 39.8(5) . . . . ? I4 Co2 O4 P4 156.5(5) . . . . ? I3 Co2 O4 P4 -73.7(5) . . . . ? O1 P1 C1 C4 80.2(3) . . . . ? C21 P1 C1 C4 -156.9(3) . . . . ? C11 P1 C1 C4 -39.8(3) . . . . ? O1 P1 C1 C2 -25.8(3) . . . . ? C21 P1 C1 C2 97.1(3) . . . . ? C11 P1 C1 C2 -145.8(3) . . . . ? C4 C1 C2 C3 -11.1(3) . . . . ? P1 C1 C2 C3 109.2(3) . . . . ? C4 C1 C2 P2 -133.2(3) . . . . ? P1 C1 C2 P2 -13.0(5) . . . . ? O2 P2 C2 C3 -35.3(3) . . . . ? C31 P2 C2 C3 84.6(3) . . . . ? C41 P2 C2 C3 -161.1(3) . . . . ? O2 P2 C2 C1 75.2(3) . . . . ? C31 P2 C2 C1 -164.8(3) . . . . ? C41 P2 C2 C1 -50.6(4) . . . . ? C1 C2 C3 C4 10.9(3) . . . . ? P2 C2 C3 C4 141.9(3) . . . . ? C1 C2 C3 P3 141.3(3) . . . . ? P2 C2 C3 P3 -87.7(3) . . . . ? O3 P3 C3 C2 -34.3(3) . . . . ? C61 P3 C3 C2 -159.6(3) . . . . ? C51 P3 C3 C2 86.2(3) . . . . ? O3 P3 C3 C4 76.4(3) . . . . ? C61 P3 C3 C4 -48.9(3) . . . . ? C51 P3 C3 C4 -163.1(3) . . . . ? C2 C1 C4 C3 10.8(3) . . . . ? P1 C1 C4 C3 -113.4(3) . . . . ? C2 C1 C4 P4 -113.2(3) . . . . ? P1 C1 C4 P4 122.6(2) . . . . ? C2 C3 C4 C1 -10.9(3) . . . . ? P3 C3 C4 C1 -134.8(3) . . . . ? C2 C3 C4 P4 106.5(3) . . . . ? P3 C3 C4 P4 -17.4(4) . . . . ? O4 P4 C4 C1 76.8(3) . . . . ? C81 P4 C4 C1 -159.0(3) . . . . ? C71 P4 C4 C1 -43.0(3) . . . . ? O4 P4 C4 C3 -27.4(3) . . . . ? C81 P4 C4 C3 96.8(3) . . . . ? C71 P4 C4 C3 -147.2(3) . . . . ? O1 P1 C11 C16 -41.9(4) . . . . ? C21 P1 C11 C16 -162.7(3) . . . . ? C1 P1 C11 C16 79.5(4) . . . . ? O1 P1 C11 C12 131.3(4) . . . . ? C21 P1 C11 C12 10.4(4) . . . . ? C1 P1 C11 C12 -107.3(4) . . . . ? C16 C11 C12 C13 -0.6(7) . . . . ? P1 C11 C12 C13 -173.7(4) . . . . ? C11 C12 C13 C14 0.2(9) . . . . ? C12 C13 C14 C15 -1.1(10) . . . . ? C13 C14 C15 C16 2.4(9) . . . . ? C14 C15 C16 C11 -2.8(8) . . . . ? C12 C11 C16 C15 1.8(7) . . . . ? P1 C11 C16 C15 175.2(4) . . . . ? O1 P1 C21 C26 -17.6(4) . . . . ? C11 P1 C21 C26 101.1(3) . . . . ? C1 P1 C21 C26 -140.0(3) . . . . ? O1 P1 C21 C22 168.6(3) . . . . ? C11 P1 C21 C22 -72.7(4) . . . . ? C1 P1 C21 C22 46.2(4) . . . . ? C26 C21 C22 C23 -0.2(6) . . . . ? P1 C21 C22 C23 173.6(4) . . . . ? C21 C22 C23 C24 -1.1(7) . . . . ? C22 C23 C24 C25 2.3(8) . . . . ? C23 C24 C25 C26 -2.2(7) . . . . ? C22 C21 C26 C25 0.3(6) . . . . ? P1 C21 C26 C25 -173.7(3) . . . . ? C24 C25 C26 C21 0.9(7) . . . . ? O2 P2 C31 C32 168.2(3) . . . . ? C41 P2 C31 C32 -70.7(4) . . . . ? C2 P2 C31 C32 45.0(4) . . . . ? O2 P2 C31 C36 -17.2(4) . . . . ? C41 P2 C31 C36 103.9(3) . . . . ? C2 P2 C31 C36 -140.3(3) . . . . ? C36 C31 C32 C33 -0.7(7) . . . . ? P2 C31 C32 C33 173.8(4) . . . . ? C31 C32 C33 C34 0.4(7) . . . . ? C32 C33 C34 C35 -0.3(8) . . . . ? C33 C34 C35 C36 0.5(8) . . . . ? C32 C31 C36 C35 0.9(6) . . . . ? P2 C31 C36 C35 -173.9(4) . . . . ? C34 C35 C36 C31 -0.8(7) . . . . ? O2 P2 C41 C46 18.5(3) . . . . ? C31 P2 C41 C46 -100.1(3) . . . . ? C2 P2 C41 C46 145.1(3) . . . . ? O2 P2 C41 C42 -167.1(3) . . . . ? C31 P2 C41 C42 74.3(4) . . . . ? C2 P2 C41 C42 -40.4(4) . . . . ? C46 C41 C42 C43 0.8(6) . . . . ? P2 C41 C42 C43 -173.6(3) . . . . ? C41 C42 C43 C44 0.5(7) . . . . ? C42 C43 C44 C45 -1.1(8) . . . . ? C43 C44 C45 C46 0.5(7) . . . . ? C44 C45 C46 C41 0.8(7) . . . . ? C42 C41 C46 C45 -1.4(6) . . . . ? P2 C41 C46 C45 173.2(3) . . . . ? O3 P3 C51 C56 171.6(4) . . . . ? C61 P3 C51 C56 -66.2(4) . . . . ? C3 P3 C51 C56 48.3(4) . . . . ? O3 P3 C51 C52 -13.7(4) . . . . ? C61 P3 C51 C52 108.4(4) . . . . ? C3 P3 C51 C52 -137.0(3) . . . . ? C56 C51 C52 C53 -0.1(7) . . . . ? P3 C51 C52 C53 -174.9(4) . . . . ? C51 C52 C53 C54 0.8(9) . . . . ? C52 C53 C54 C55 -1.6(10) . . . . ? C53 C54 C55 C56 1.5(10) . . . . ? C52 C51 C56 C55 0.0(8) . . . . ? P3 C51 C56 C55 174.6(4) . . . . ? C54 C55 C56 C51 -0.7(9) . . . . ? O3 P3 C61 C66 22.7(4) . . . . ? C51 P3 C61 C66 -96.8(4) . . . . ? C3 P3 C61 C66 148.3(3) . . . . ? O3 P3 C61 C62 -160.5(3) . . . . ? C51 P3 C61 C62 79.9(4) . . . . ? C3 P3 C61 C62 -35.0(4) . . . . ? C66 C61 C62 C63 -0.1(7) . . . . ? P3 C61 C62 C63 -176.8(3) . . . . ? C61 C62 C63 C64 -0.9(7) . . . . ? C62 C63 C64 C65 2.5(8) . . . . ? C63 C64 C65 C66 -3.0(9) . . . . ? C64 C65 C66 C61 2.0(8) . . . . ? C62 C61 C66 C65 -0.4(7) . . . . ? P3 C61 C66 C65 176.3(4) . . . . ? O4 P4 C71 C76 156.1(4) . . . . ? C81 P4 C71 C76 36.0(4) . . . . ? C4 P4 C71 C76 -82.7(4) . . . . ? O4 P4 C71 C72 -23.0(4) . . . . ? C81 P4 C71 C72 -143.1(4) . . . . ? C4 P4 C71 C72 98.2(4) . . . . ? C76 C71 C72 C73 0.5(7) . . . . ? P4 C71 C72 C73 179.7(4) . . . . ? C71 C72 C73 C74 -0.5(9) . . . . ? C72 C73 C74 C75 0.7(10) . . . . ? C73 C74 C75 C76 -1.0(10) . . . . ? C72 C71 C76 C75 -0.8(7) . . . . ? P4 C71 C76 C75 -179.9(4) . . . . ? C74 C75 C76 C71 1.0(9) . . . . ? O4 P4 C81 C86 -19.8(4) . . . . ? C71 P4 C81 C86 99.5(4) . . . . ? C4 P4 C81 C86 -144.5(3) . . . . ? O4 P4 C81 C82 165.9(3) . . . . ? C71 P4 C81 C82 -74.8(4) . . . . ? C4 P4 C81 C82 41.2(4) . . . . ? C86 C81 C82 C83 0.3(6) . . . . ? P4 C81 C82 C83 174.4(4) . . . . ? C81 C82 C83 C84 -0.5(7) . . . . ? C82 C83 C84 C85 0.3(9) . . . . ? C83 C84 C85 C86 0.3(9) . . . . ? C82 C81 C86 C85 0.3(7) . . . . ? P4 C81 C86 C85 -174.1(4) . . . . ? C84 C85 C86 C81 -0.6(9) . . . . ? _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction 0.982 _refine_diff_density_max 0.670 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.100 #============================================================================= # END of CIF #=============================================================================