Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Alan Welch' 'Kelly J. Dalby' 'David Ellis' 'Javier Gil-Lostes' 'Ruaraidh McIntosh' 'Georgina Rosair' _publ_contact_author_name 'Prof Alan Welch' _publ_contact_author_address ; Department of Chemistry Heriot-Watt University Riccarton EDINBURGH EH14 4AS ; _publ_contact_author_phone '0131 451-3217' _publ_contact_author_fax '0131 451 3180' _publ_contact_author_email A.J.WELCH@HW.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The synthesis and characterisation of 4,1,2-MC2B10 metallacarboranes ; data_1 _database_code_depnum_ccdc_archive 'CCDC 265425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H21 B10 Co' _chemical_formula_sum 'C10 H21 B10 Co' _chemical_formula_weight 308.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1253(19) _cell_length_b 8.692(2) _cell_length_c 12.824(4) _cell_angle_alpha 87.336(14) _cell_angle_beta 87.729(16) _cell_angle_gamma 67.391(14) _cell_volume 732.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4942 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 33.01 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 1.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6441 _exptl_absorpt_correction_T_max 0.9555 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34458 _diffrn_reflns_av_R_equivalents 0.1046 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 37.65 _reflns_number_total 7250 _reflns_number_gt 5324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.1876P] 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 7250 _refine_ls_number_parameters 220 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co4 Co 0.13454(2) 0.18586(2) 0.192499(13) 0.01219(5) Uani 1 1 d . . . C1 C 0.34464(18) 0.13176(16) 0.30723(10) 0.0137(2) Uani 1 1 d . . . C2 C 0.15593(18) 0.12716(16) 0.34912(9) 0.0136(2) Uani 1 1 d . . . B3 B 0.4632(2) 0.04314(19) 0.20353(11) 0.0144(2) Uani 1 1 d D . . H3C H 0.578(2) 0.092(2) 0.1737(14) 0.017 Uiso 1 1 d D . . B5 B 0.5005(2) -0.0897(2) 0.32204(12) 0.0166(3) Uani 1 1 d D . . H5C H 0.617(3) -0.104(3) 0.3791(13) 0.020 Uiso 1 1 d D . . B6 B 0.0267(2) 0.03172(19) 0.30198(11) 0.0142(2) Uani 1 1 d D . . H6C H -0.131(2) 0.079(2) 0.3362(14) 0.017 Uiso 1 1 d D . . B7 B 0.3266(2) -0.03971(19) 0.11708(11) 0.0155(2) Uani 1 1 d D . . H7C H 0.353(3) -0.027(2) 0.0340(11) 0.019 Uiso 1 1 d D . . B8 B 0.5294(2) -0.17180(19) 0.19522(12) 0.0164(3) Uani 1 1 d D . . H8C H 0.680(2) -0.241(2) 0.1605(14) 0.020 Uiso 1 1 d D . . B9 B 0.2456(2) -0.0957(2) 0.37945(12) 0.0159(3) Uani 1 1 d D . . H9C H 0.228(3) -0.115(3) 0.4628(11) 0.019 Uiso 1 1 d D . . B10 B 0.0943(2) -0.0449(2) 0.17027(11) 0.0158(2) Uani 1 1 d D . . H10C H -0.038(2) -0.030(3) 0.1234(14) 0.019 Uiso 1 1 d D . . B11 B 0.4149(2) -0.24916(19) 0.30061(12) 0.0174(3) Uani 1 1 d D . . H11C H 0.499(3) -0.369(2) 0.3399(14) 0.021 Uiso 1 1 d D . . B12 B 0.1479(2) -0.18288(19) 0.28138(12) 0.0166(3) Uani 1 1 d . . . H12C H 0.054(3) -0.261(3) 0.3009(15) 0.020 Uiso 1 1 d . . . B13 B 0.3193(2) -0.2274(2) 0.17237(12) 0.0176(3) Uani 1 1 d . . . H13C H 0.343(3) -0.337(3) 0.1210(15) 0.021 Uiso 1 1 d . . . C3 C 0.0776(2) 0.25006(18) 0.43621(10) 0.0169(2) Uani 1 1 d . . . H3A H 0.0993 0.1907 0.5052 0.020 Uiso 1 1 calc R . . H3B H -0.0694 0.3174 0.4289 0.020 Uiso 1 1 calc R . . C4 C 0.2012(2) 0.36206(18) 0.42478(11) 0.0188(2) Uani 1 1 d . . . H4A H 0.1249 0.4666 0.3850 0.023 Uiso 1 1 calc R . . H4B H 0.2324 0.3904 0.4942 0.023 Uiso 1 1 calc R . . C5 C 0.3977(2) 0.25817(18) 0.36532(11) 0.0183(2) Uani 1 1 d . . . H5A H 0.4404 0.3299 0.3157 0.022 Uiso 1 1 calc R . . H5B H 0.5090 0.2010 0.4144 0.022 Uiso 1 1 calc R . . C41 C 0.1593(2) 0.33939(19) 0.07168(11) 0.0213(3) Uani 1 1 d . . . H41 H 0.2783 0.3213 0.0297 0.026 Uiso 1 1 calc R . . C42 C 0.0057(3) 0.2777(2) 0.05299(12) 0.0250(3) Uani 1 1 d . . . H42 H 0.0034 0.2119 -0.0037 0.030 Uiso 1 1 calc R . . C43 C -0.1438(2) 0.3323(2) 0.13460(13) 0.0258(3) Uani 1 1 d . . . H43 H -0.2635 0.3090 0.1423 0.031 Uiso 1 1 calc R . . C44 C -0.0826(2) 0.42742(18) 0.20217(12) 0.0223(3) Uani 1 1 d . . . H44 H -0.1546 0.4794 0.2632 0.027 Uiso 1 1 calc R . . C45 C 0.1043(2) 0.43222(17) 0.16353(11) 0.0195(2) Uani 1 1 d . . . H45 H 0.1793 0.4878 0.1939 0.023 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 Co4 0.01107(8) 0.01071(8) 0.01311(8) -0.00001(5) -0.00053(5) -0.00233(6) C1 0.0125(5) 0.0122(5) 0.0156(5) -0.0013(4) -0.0006(4) -0.0036(4) C2 0.0125(5) 0.0138(5) 0.0130(5) -0.0012(4) 0.0006(4) -0.0034(4) B3 0.0118(5) 0.0136(6) 0.0164(6) -0.0011(5) 0.0013(4) -0.0034(5) B5 0.0125(5) 0.0153(6) 0.0191(6) 0.0021(5) -0.0012(5) -0.0025(5) B6 0.0121(5) 0.0136(6) 0.0164(6) -0.0013(5) 0.0014(4) -0.0044(5) B7 0.0160(6) 0.0141(6) 0.0154(6) -0.0025(5) 0.0028(5) -0.0048(5) B8 0.0137(5) 0.0124(6) 0.0207(6) -0.0014(5) 0.0030(5) -0.0024(5) B9 0.0157(6) 0.0152(6) 0.0158(6) 0.0015(5) 0.0010(5) -0.0051(5) B10 0.0151(6) 0.0160(6) 0.0160(6) -0.0021(5) 0.0004(5) -0.0055(5) B11 0.0160(6) 0.0120(6) 0.0212(7) 0.0012(5) 0.0015(5) -0.0024(5) B12 0.0169(6) 0.0139(6) 0.0192(6) -0.0007(5) 0.0022(5) -0.0066(5) B13 0.0183(6) 0.0135(6) 0.0197(6) -0.0026(5) 0.0034(5) -0.0049(5) C3 0.0183(5) 0.0175(6) 0.0152(5) -0.0043(4) 0.0029(4) -0.0071(5) C4 0.0215(6) 0.0176(6) 0.0181(6) -0.0050(5) 0.0013(5) -0.0082(5) C5 0.0178(5) 0.0199(6) 0.0197(6) -0.0054(5) 0.0002(4) -0.0095(5) C41 0.0262(6) 0.0161(6) 0.0176(6) 0.0041(5) 0.0005(5) -0.0043(5) C42 0.0328(7) 0.0189(7) 0.0202(6) 0.0026(5) -0.0114(5) -0.0058(6) C43 0.0171(6) 0.0213(7) 0.0349(8) 0.0083(6) -0.0098(5) -0.0031(5) C44 0.0203(6) 0.0140(6) 0.0237(7) 0.0019(5) 0.0017(5) 0.0028(5) C45 0.0266(6) 0.0107(5) 0.0207(6) 0.0021(4) -0.0024(5) -0.0066(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 Co4 C42 2.0284(15) . ? Co4 C41 2.0445(15) . ? Co4 C2 2.0461(13) . ? Co4 C43 2.0478(15) . ? Co4 C1 2.0484(13) . ? Co4 C44 2.0806(15) . ? Co4 C45 2.0851(15) . ? Co4 B7 2.1588(16) . ? Co4 B10 2.1651(17) . ? Co4 B3 2.1954(15) . ? Co4 B6 2.2109(15) . ? C1 C2 1.4423(17) . ? C1 C5 1.5240(19) . ? C1 B3 1.6066(19) . ? C1 B5 1.820(2) . ? C2 C3 1.5176(18) . ? C2 B6 1.606(2) . ? C2 B9 1.820(2) . ? B3 B8 1.750(2) . ? B3 B5 1.829(2) . ? B3 B7 1.842(2) . ? B3 H3C 1.111(14) . ? B5 B11 1.752(2) . ? B5 B8 1.779(2) . ? B5 B9 1.952(2) . ? B5 H5C 1.095(14) . ? B6 B12 1.756(2) . ? B6 B10 1.823(2) . ? B6 B9 1.827(2) . ? B6 H6C 1.116(13) . ? B7 B13 1.767(2) . ? B7 B8 1.773(2) . ? B7 B10 1.781(2) . ? B7 H7C 1.082(14) . ? B8 B13 1.779(2) . ? B8 B11 1.787(2) . ? B8 H8C 1.098(14) . ? B9 B11 1.746(2) . ? B9 B12 1.789(2) . ? B9 H9C 1.084(14) . ? B10 B13 1.770(2) . ? B10 B12 1.774(2) . ? B10 H10C 1.103(14) . ? B11 B13 1.779(2) . ? B11 B12 1.787(2) . ? B11 H11C 1.093(14) . ? B12 B13 1.774(2) . ? B12 H12C 1.14(2) . ? B13 H13C 1.14(2) . ? C3 C4 1.543(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.5374(19) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C41 C45 1.414(2) . ? C41 C42 1.424(2) . ? C41 H41 0.9500 . ? C42 C43 1.423(2) . ? C42 H42 0.9500 . ? C43 C44 1.414(2) . ? C43 H43 0.9500 . ? C44 C45 1.418(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 C42 Co4 C41 40.92(7) . . ? C42 Co4 C2 159.22(6) . . ? C41 Co4 C2 148.22(6) . . ? C42 Co4 C43 40.86(7) . . ? C41 Co4 C43 68.32(7) . . ? C2 Co4 C43 118.59(6) . . ? C42 Co4 C1 156.92(6) . . ? C41 Co4 C1 116.41(6) . . ? C2 Co4 C1 41.25(5) . . ? C43 Co4 C1 149.81(6) . . ? C42 Co4 C44 67.81(7) . . ? C41 Co4 C44 67.36(6) . . ? C2 Co4 C44 97.57(6) . . ? C43 Co4 C44 40.04(7) . . ? C1 Co4 C44 111.69(6) . . ? C42 Co4 C45 67.97(6) . . ? C41 Co4 C45 40.04(6) . . ? C2 Co4 C45 110.79(6) . . ? C43 Co4 C45 67.56(7) . . ? C1 Co4 C45 96.51(6) . . ? C44 Co4 C45 39.79(6) . . ? C42 Co4 B7 88.87(6) . . ? C41 Co4 B7 94.12(6) . . ? C2 Co4 B7 105.41(6) . . ? C43 Co4 B7 121.06(7) . . ? C1 Co4 B7 88.95(6) . . ? C44 Co4 B7 156.61(6) . . ? C45 Co4 B7 130.43(6) . . ? C42 Co4 B10 90.28(6) . . ? C41 Co4 B10 123.24(6) . . ? C2 Co4 B10 88.18(6) . . ? C43 Co4 B10 93.89(7) . . ? C1 Co4 B10 105.33(6) . . ? C44 Co4 B10 129.49(6) . . ? C45 Co4 B10 157.95(6) . . ? B7 Co4 B10 48.65(6) . . ? C42 Co4 B3 121.09(6) . . ? C41 Co4 B3 94.96(6) . . ? C2 Co4 B3 79.61(5) . . ? C43 Co4 B3 161.61(6) . . ? C1 Co4 B3 44.32(5) . . ? C44 Co4 B3 141.46(6) . . ? C45 Co4 B3 104.97(6) . . ? B7 Co4 B3 50.06(6) . . ? B10 Co4 B3 89.01(6) . . ? C42 Co4 B6 123.44(7) . . ? C41 Co4 B6 163.93(6) . . ? C2 Co4 B6 44.12(5) . . ? C43 Co4 B6 96.80(6) . . ? C1 Co4 B6 79.45(6) . . ? C44 Co4 B6 105.56(6) . . ? C45 Co4 B6 141.04(6) . . ? B7 Co4 B6 88.45(6) . . ? B10 Co4 B6 49.21(6) . . ? B3 Co4 B6 98.81(6) . . ? C2 C1 C5 109.43(11) . . ? C2 C1 B3 126.01(11) . . ? C5 C1 B3 123.80(11) . . ? C2 C1 B5 98.14(10) . . ? C5 C1 B5 119.96(11) . . ? B3 C1 B5 64.17(9) . . ? C2 C1 Co4 69.29(7) . . ? C5 C1 Co4 125.99(9) . . ? B3 C1 Co4 72.70(7) . . ? B5 C1 Co4 113.37(8) . . ? C1 C2 C3 109.13(11) . . ? C1 C2 B6 126.65(11) . . ? C3 C2 B6 123.58(10) . . ? C1 C2 B9 97.95(10) . . ? C3 C2 B9 119.87(10) . . ? B6 C2 B9 64.12(9) . . ? C1 C2 Co4 69.46(7) . . ? C3 C2 Co4 125.90(10) . . ? B6 C2 Co4 73.39(7) . . ? B9 C2 Co4 113.61(8) . . ? C1 B3 B8 118.09(11) . . ? C1 B3 B5 63.60(9) . . ? B8 B3 B5 59.57(9) . . ? C1 B3 B7 117.33(10) . . ? B8 B3 B7 59.09(9) . . ? B5 B3 B7 104.00(10) . . ? C1 B3 Co4 62.98(7) . . ? B8 B3 Co4 112.77(9) . . ? B5 B3 Co4 106.65(8) . . ? B7 B3 Co4 63.94(6) . . ? C1 B3 H3C 113.1(10) . . ? B8 B3 H3C 116.4(10) . . ? B5 B3 H3C 122.2(10) . . ? B7 B3 H3C 122.5(10) . . ? Co4 B3 H3C 122.9(10) . . ? B11 B5 B8 60.83(9) . . ? B11 B5 C1 124.22(10) . . ? B8 B5 C1 106.24(10) . . ? B11 B5 B3 108.69(11) . . ? B8 B5 B3 57.99(8) . . ? C1 B5 B3 52.24(7) . . ? B11 B5 B9 55.94(8) . . ? B8 B5 B9 105.66(10) . . ? C1 B5 B9 81.87(8) . . ? B3 B5 B9 112.27(10) . . ? B11 B5 H5C 122.3(11) . . ? B8 B5 H5C 129.2(10) . . ? C1 B5 H5C 107.5(11) . . ? B3 B5 H5C 123.3(10) . . ? B9 B5 H5C 115.8(10) . . ? C2 B6 B12 118.53(11) . . ? C2 B6 B10 117.36(10) . . ? B12 B6 B10 59.39(8) . . ? C2 B6 B9 63.62(9) . . ? B12 B6 B9 59.88(9) . . ? B10 B6 B9 104.30(10) . . ? C2 B6 Co4 62.48(7) . . ? B12 B6 Co4 113.06(8) . . ? B10 B6 Co4 64.09(7) . . ? B9 B6 Co4 106.19(8) . . ? C2 B6 H6C 110.3(10) . . ? B12 B6 H6C 118.3(10) . . ? B10 B6 H6C 124.6(10) . . ? B9 B6 H6C 121.6(10) . . ? Co4 B6 H6C 122.0(10) . . ? B13 B7 B8 60.35(9) . . ? B13 B7 B10 59.84(9) . . ? B8 B7 B10 108.78(11) . . ? B13 B7 B3 109.74(11) . . ? B8 B7 B3 57.85(9) . . ? B10 B7 B3 115.03(10) . . ? B13 B7 Co4 116.00(9) . . ? B8 B7 Co4 113.49(9) . . ? B10 B7 Co4 65.86(7) . . ? B3 B7 Co4 66.00(7) . . ? B13 B7 H7C 120.7(11) . . ? B8 B7 H7C 119.4(10) . . ? B10 B7 H7C 122.4(10) . . ? B3 B7 H7C 116.5(10) . . ? Co4 B7 H7C 115.6(10) . . ? B3 B8 B7 63.07(9) . . ? B3 B8 B5 62.44(9) . . ? B7 B8 B5 109.09(10) . . ? B3 B8 B13 113.57(10) . . ? B7 B8 B13 59.66(9) . . ? B5 B8 B13 108.92(10) . . ? B3 B8 B11 110.71(10) . . ? B7 B8 B11 106.03(10) . . ? B5 B8 B11 58.83(9) . . ? B13 B8 B11 59.84(9) . . ? B3 B8 H8C 115.7(11) . . ? B7 B8 H8C 121.0(10) . . ? B5 B8 H8C 121.6(10) . . ? B13 B8 H8C 120.9(11) . . ? B11 B8 H8C 124.5(10) . . ? B11 B9 B12 60.70(9) . . ? B11 B9 C2 124.40(10) . . ? B12 B9 C2 106.47(10) . . ? B11 B9 B6 108.58(11) . . ? B12 B9 B6 58.09(8) . . ? C2 B9 B6 52.26(8) . . ? B11 B9 B5 56.22(8) . . ? B12 B9 B5 106.09(10) . . ? C2 B9 B5 82.04(9) . . ? B6 B9 B5 112.55(10) . . ? B11 B9 H9C 123.0(10) . . ? B12 B9 H9C 124.6(11) . . ? C2 B9 H9C 108.7(11) . . ? B6 B9 H9C 120.3(10) . . ? B5 B9 H9C 120.0(10) . . ? B13 B10 B12 60.08(9) . . ? B13 B10 B7 59.69(9) . . ? B12 B10 B7 108.95(10) . . ? B13 B10 B6 109.87(10) . . ? B12 B10 B6 58.44(8) . . ? B7 B10 B6 115.52(11) . . ? B13 B10 Co4 115.57(9) . . ? B12 B10 Co4 114.45(9) . . ? B7 B10 Co4 65.49(7) . . ? B6 B10 Co4 66.70(7) . . ? B13 B10 H10C 123.5(11) . . ? B12 B10 H10C 118.7(10) . . ? B7 B10 H10C 124.1(10) . . ? B6 B10 H10C 113.5(10) . . ? Co4 B10 H10C 113.9(11) . . ? B9 B11 B5 67.84(9) . . ? B9 B11 B13 110.11(11) . . ? B5 B11 B13 110.18(11) . . ? B9 B11 B12 60.86(9) . . ? B5 B11 B12 115.42(11) . . ? B13 B11 B12 59.67(9) . . ? B9 B11 B8 114.68(11) . . ? B5 B11 B8 60.34(9) . . ? B13 B11 B8 59.85(9) . . ? B12 B11 B8 110.01(11) . . ? B9 B11 H11C 115.8(10) . . ? B5 B11 H11C 115.7(11) . . ? B13 B11 H11C 123.9(11) . . ? B12 B11 H11C 120.4(10) . . ? B8 B11 H11C 120.8(10) . . ? B6 B12 B13 112.81(11) . . ? B6 B12 B10 62.17(9) . . ? B13 B12 B10 59.85(9) . . ? B6 B12 B11 109.98(11) . . ? B13 B12 B11 59.95(9) . . ? B10 B12 B11 105.87(10) . . ? B6 B12 B9 62.04(9) . . ? B13 B12 B9 108.35(11) . . ? B10 B12 B9 107.95(11) . . ? B11 B12 B9 58.44(9) . . ? B6 B12 H12C 116.2(10) . . ? B13 B12 H12C 120.8(10) . . ? B10 B12 H12C 120.8(10) . . ? B11 B12 H12C 125.1(10) . . ? B9 B12 H12C 122.7(10) . . ? B7 B13 B10 60.47(9) . . ? B7 B13 B12 109.57(11) . . ? B10 B13 B12 60.07(9) . . ? B7 B13 B11 106.64(11) . . ? B10 B13 B11 106.37(11) . . ? B12 B13 B11 60.38(9) . . ? B7 B13 B8 59.99(9) . . ? B10 B13 B8 108.99(11) . . ? B12 B13 B8 110.97(11) . . ? B11 B13 B8 60.31(9) . . ? B7 B13 H13C 120.2(10) . . ? B10 B13 H13C 122.3(10) . . ? B12 B13 H13C 121.6(10) . . ? B11 B13 H13C 123.9(10) . . ? B8 B13 H13C 119.1(10) . . ? C2 C3 C4 105.43(10) . . ? C2 C3 H3A 110.7 . . ? C4 C3 H3A 110.7 . . ? C2 C3 H3B 110.7 . . ? C4 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? C5 C4 C3 105.17(11) . . ? C5 C4 H4A 110.7 . . ? C3 C4 H4A 110.7 . . ? C5 C4 H4B 110.7 . . ? C3 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? C1 C5 C4 105.13(11) . . ? C1 C5 H5A 110.7 . . ? C4 C5 H5A 110.7 . . ? C1 C5 H5B 110.7 . . ? C4 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C45 C41 C42 108.24(13) . . ? C45 C41 Co4 71.52(8) . . ? C42 C41 Co4 68.93(9) . . ? C45 C41 H41 125.9 . . ? C42 C41 H41 125.9 . . ? Co4 C41 H41 125.2 . . ? C43 C42 C41 107.65(14) . . ? C43 C42 Co4 70.30(9) . . ? C41 C42 Co4 70.15(8) . . ? C43 C42 H42 126.2 . . ? C41 C42 H42 126.2 . . ? Co4 C42 H42 125.0 . . ? C44 C43 C42 107.84(14) . . ? C44 C43 Co4 71.23(8) . . ? C42 C43 Co4 68.84(8) . . ? C44 C43 H43 126.1 . . ? C42 C43 H43 126.1 . . ? Co4 C43 H43 125.4 . . ? C43 C44 C45 108.51(13) . . ? C43 C44 Co4 68.73(8) . . ? C45 C44 Co4 70.28(8) . . ? C43 C44 H44 125.7 . . ? C45 C44 H44 125.7 . . ? Co4 C44 H44 126.8 . . ? C41 C45 C44 107.76(14) . . ? C41 C45 Co4 68.43(8) . . ? C44 C45 Co4 69.93(8) . . ? C41 C45 H45 126.1 . . ? C44 C45 H45 126.1 . . ? Co4 C45 H45 127.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C42 Co4 C1 C2 160.26(14) . . . . ? C41 Co4 C1 C2 150.83(8) . . . . ? C43 Co4 C1 C2 58.91(14) . . . . ? C44 Co4 C1 C2 76.20(9) . . . . ? C45 Co4 C1 C2 114.31(8) . . . . ? B7 Co4 C1 C2 -115.09(8) . . . . ? B10 Co4 C1 C2 -68.74(8) . . . . ? B3 Co4 C1 C2 -140.90(11) . . . . ? B6 Co4 C1 C2 -26.48(8) . . . . ? C42 Co4 C1 C5 60.76(19) . . . . ? C41 Co4 C1 C5 51.33(12) . . . . ? C2 Co4 C1 C5 -99.50(13) . . . . ? C43 Co4 C1 C5 -40.59(18) . . . . ? C44 Co4 C1 C5 -23.30(12) . . . . ? C45 Co4 C1 C5 14.81(11) . . . . ? B7 Co4 C1 C5 145.40(11) . . . . ? B10 Co4 C1 C5 -168.25(10) . . . . ? B3 Co4 C1 C5 119.60(14) . . . . ? B6 Co4 C1 C5 -125.98(11) . . . . ? C42 Co4 C1 B3 -58.84(17) . . . . ? C41 Co4 C1 B3 -68.26(9) . . . . ? C2 Co4 C1 B3 140.90(11) . . . . ? C43 Co4 C1 B3 -160.19(11) . . . . ? C44 Co4 C1 B3 -142.89(8) . . . . ? C45 Co4 C1 B3 -104.79(8) . . . . ? B7 Co4 C1 B3 25.81(8) . . . . ? B10 Co4 C1 B3 72.16(8) . . . . ? B6 Co4 C1 B3 114.42(8) . . . . ? C42 Co4 C1 B5 -109.66(16) . . . . ? C41 Co4 C1 B5 -119.08(9) . . . . ? C2 Co4 C1 B5 90.08(11) . . . . ? C43 Co4 C1 B5 148.99(11) . . . . ? C44 Co4 C1 B5 166.29(8) . . . . ? C45 Co4 C1 B5 -155.60(8) . . . . ? B7 Co4 C1 B5 -25.01(9) . . . . ? B10 Co4 C1 B5 21.34(9) . . . . ? B3 Co4 C1 B5 -50.82(9) . . . . ? B6 Co4 C1 B5 63.61(9) . . . . ? C5 C1 C2 C3 -0.01(15) . . . . ? B3 C1 C2 C3 -170.30(12) . . . . ? B5 C1 C2 C3 125.82(11) . . . . ? Co4 C1 C2 C3 -122.20(10) . . . . ? C5 C1 C2 B6 170.95(12) . . . . ? B3 C1 C2 B6 0.7(2) . . . . ? B5 C1 C2 B6 -63.22(15) . . . . ? Co4 C1 C2 B6 48.76(12) . . . . ? C5 C1 C2 B9 -125.50(11) . . . . ? B3 C1 C2 B9 64.21(14) . . . . ? B5 C1 C2 B9 0.33(10) . . . . ? Co4 C1 C2 B9 112.31(8) . . . . ? C5 C1 C2 Co4 122.19(10) . . . . ? B3 C1 C2 Co4 -48.10(12) . . . . ? B5 C1 C2 Co4 -111.98(8) . . . . ? C42 Co4 C2 C1 -158.08(16) . . . . ? C41 Co4 C2 C1 -55.98(13) . . . . ? C43 Co4 C2 C1 -150.63(8) . . . . ? C44 Co4 C2 C1 -114.45(9) . . . . ? C45 Co4 C2 C1 -75.58(9) . . . . ? B7 Co4 C2 C1 69.92(9) . . . . ? B10 Co4 C2 C1 115.94(8) . . . . ? B3 Co4 C2 C1 26.61(8) . . . . ? B6 Co4 C2 C1 140.98(11) . . . . ? C42 Co4 C2 C3 -58.8(2) . . . . ? C41 Co4 C2 C3 43.27(16) . . . . ? C43 Co4 C2 C3 -51.38(13) . . . . ? C1 Co4 C2 C3 99.25(13) . . . . ? C44 Co4 C2 C3 -15.20(12) . . . . ? C45 Co4 C2 C3 23.66(12) . . . . ? B7 Co4 C2 C3 169.17(10) . . . . ? B10 Co4 C2 C3 -144.81(11) . . . . ? B3 Co4 C2 C3 125.86(12) . . . . ? B6 Co4 C2 C3 -119.77(13) . . . . ? C42 Co4 C2 B6 60.94(19) . . . . ? C41 Co4 C2 B6 163.04(10) . . . . ? C43 Co4 C2 B6 68.39(9) . . . . ? C1 Co4 C2 B6 -140.98(11) . . . . ? C44 Co4 C2 B6 104.57(8) . . . . ? C45 Co4 C2 B6 143.44(7) . . . . ? B7 Co4 C2 B6 -71.06(8) . . . . ? B10 Co4 C2 B6 -25.04(7) . . . . ? B3 Co4 C2 B6 -114.37(8) . . . . ? C42 Co4 C2 B9 112.06(17) . . . . ? C41 Co4 C2 B9 -145.83(10) . . . . ? C43 Co4 C2 B9 119.52(9) . . . . ? C1 Co4 C2 B9 -89.85(10) . . . . ? C44 Co4 C2 B9 155.70(9) . . . . ? C45 Co4 C2 B9 -165.43(8) . . . . ? B7 Co4 C2 B9 -19.93(9) . . . . ? B10 Co4 C2 B9 26.09(9) . . . . ? B3 Co4 C2 B9 -63.24(9) . . . . ? B6 Co4 C2 B9 51.13(9) . . . . ? C2 C1 B3 B8 -55.91(17) . . . . ? C5 C1 B3 B8 135.12(13) . . . . ? B5 C1 B3 B8 25.03(11) . . . . ? Co4 C1 B3 B8 -102.73(11) . . . . ? C2 C1 B3 B5 -80.94(14) . . . . ? C5 C1 B3 B5 110.09(14) . . . . ? Co4 C1 B3 B5 -127.76(8) . . . . ? C2 C1 B3 B7 11.78(19) . . . . ? C5 C1 B3 B7 -157.19(12) . . . . ? B5 C1 B3 B7 92.72(12) . . . . ? Co4 C1 B3 B7 -35.04(10) . . . . ? C2 C1 B3 Co4 46.82(11) . . . . ? C5 C1 B3 Co4 -122.15(13) . . . . ? B5 C1 B3 Co4 127.76(8) . . . . ? C42 Co4 B3 C1 156.94(8) . . . . ? C41 Co4 B3 C1 123.38(8) . . . . ? C2 Co4 B3 C1 -25.01(7) . . . . ? C43 Co4 B3 C1 147.29(19) . . . . ? C44 Co4 B3 C1 64.12(11) . . . . ? C45 Co4 B3 C1 83.93(8) . . . . ? B7 Co4 B3 C1 -145.41(10) . . . . ? B10 Co4 B3 C1 -113.34(8) . . . . ? B6 Co4 B3 C1 -64.93(8) . . . . ? C42 Co4 B3 B8 -92.01(11) . . . . ? C41 Co4 B3 B8 -125.57(10) . . . . ? C2 Co4 B3 B8 86.04(10) . . . . ? C43 Co4 B3 B8 -101.7(2) . . . . ? C1 Co4 B3 B8 111.05(12) . . . . ? C44 Co4 B3 B8 175.17(9) . . . . ? C45 Co4 B3 B8 -165.02(9) . . . . ? B7 Co4 B3 B8 -34.36(9) . . . . ? B10 Co4 B3 B8 -2.29(9) . . . . ? B6 Co4 B3 B8 46.12(10) . . . . ? C42 Co4 B3 B5 -155.41(9) . . . . ? C41 Co4 B3 B5 171.03(9) . . . . ? C2 Co4 B3 B5 22.65(9) . . . . ? C43 Co4 B3 B5 -165.06(18) . . . . ? C1 Co4 B3 B5 47.66(9) . . . . ? C44 Co4 B3 B5 111.77(11) . . . . ? C45 Co4 B3 B5 131.59(9) . . . . ? B7 Co4 B3 B5 -97.75(11) . . . . ? B10 Co4 B3 B5 -65.68(9) . . . . ? B6 Co4 B3 B5 -17.28(10) . . . . ? C42 Co4 B3 B7 -57.66(9) . . . . ? C41 Co4 B3 B7 -91.22(8) . . . . ? C2 Co4 B3 B7 120.40(8) . . . . ? C43 Co4 B3 B7 -67.3(2) . . . . ? C1 Co4 B3 B7 145.41(10) . . . . ? C44 Co4 B3 B7 -150.48(9) . . . . ? C45 Co4 B3 B7 -130.66(7) . . . . ? B10 Co4 B3 B7 32.07(7) . . . . ? B6 Co4 B3 B7 80.47(8) . . . . ? C2 C1 B5 B11 38.30(15) . . . . ? C5 C1 B5 B11 156.35(12) . . . . ? B3 C1 B5 B11 -87.90(13) . . . . ? Co4 C1 B5 B11 -32.59(15) . . . . ? C2 C1 B5 B8 103.72(11) . . . . ? C5 C1 B5 B8 -138.22(11) . . . . ? B3 C1 B5 B8 -22.48(10) . . . . ? Co4 C1 B5 B8 32.83(12) . . . . ? C2 C1 B5 B3 126.20(11) . . . . ? C5 C1 B5 B3 -115.74(13) . . . . ? Co4 C1 B5 B3 55.31(8) . . . . ? C2 C1 B5 B9 -0.31(10) . . . . ? C5 C1 B5 B9 117.75(12) . . . . ? B3 C1 B5 B9 -126.51(10) . . . . ? Co4 C1 B5 B9 -71.20(9) . . . . ? C1 B3 B5 B11 119.27(11) . . . . ? B8 B3 B5 B11 -35.08(10) . . . . ? B7 B3 B5 B11 5.41(12) . . . . ? Co4 B3 B5 B11 71.95(11) . . . . ? C1 B3 B5 B8 154.34(11) . . . . ? B7 B3 B5 B8 40.48(9) . . . . ? Co4 B3 B5 B8 107.03(9) . . . . ? B8 B3 B5 C1 -154.34(11) . . . . ? B7 B3 B5 C1 -113.86(10) . . . . ? Co4 B3 B5 C1 -47.31(7) . . . . ? C1 B3 B5 B9 59.30(11) . . . . ? B8 B3 B5 B9 -95.05(12) . . . . ? B7 B3 B5 B9 -54.57(13) . . . . ? Co4 B3 B5 B9 11.98(13) . . . . ? C1 C2 B6 B12 55.39(18) . . . . ? C3 C2 B6 B12 -134.88(13) . . . . ? B9 C2 B6 B12 -24.86(11) . . . . ? Co4 C2 B6 B12 102.68(11) . . . . ? C1 C2 B6 B10 -12.83(19) . . . . ? C3 C2 B6 B10 156.91(12) . . . . ? B9 C2 B6 B10 -93.08(12) . . . . ? Co4 C2 B6 B10 34.46(10) . . . . ? C1 C2 B6 B9 80.25(14) . . . . ? C3 C2 B6 B9 -110.01(13) . . . . ? Co4 C2 B6 B9 127.54(7) . . . . ? C1 C2 B6 Co4 -47.29(12) . . . . ? C3 C2 B6 Co4 122.44(13) . . . . ? B9 C2 B6 Co4 -127.54(7) . . . . ? C42 Co4 B6 C2 -158.18(8) . . . . ? C41 Co4 B6 C2 -146.29(19) . . . . ? C43 Co4 B6 C2 -124.70(8) . . . . ? C1 Co4 B6 C2 24.98(7) . . . . ? C44 Co4 B6 C2 -84.80(8) . . . . ? C45 Co4 B6 C2 -62.34(11) . . . . ? B7 Co4 B6 C2 114.20(8) . . . . ? B10 Co4 B6 C2 146.03(10) . . . . ? B3 Co4 B6 C2 65.05(8) . . . . ? C42 Co4 B6 B12 90.50(11) . . . . ? C41 Co4 B6 B12 102.4(2) . . . . ? C2 Co4 B6 B12 -111.32(12) . . . . ? C43 Co4 B6 B12 123.98(10) . . . . ? C1 Co4 B6 B12 -86.34(10) . . . . ? C44 Co4 B6 B12 163.88(9) . . . . ? C45 Co4 B6 B12 -173.66(9) . . . . ? B7 Co4 B6 B12 2.87(10) . . . . ? B10 Co4 B6 B12 34.71(9) . . . . ? B3 Co4 B6 B12 -46.27(10) . . . . ? C42 Co4 B6 B10 55.79(9) . . . . ? C41 Co4 B6 B10 67.7(2) . . . . ? C2 Co4 B6 B10 -146.03(10) . . . . ? C43 Co4 B6 B10 89.27(8) . . . . ? C1 Co4 B6 B10 -121.05(7) . . . . ? C44 Co4 B6 B10 129.17(8) . . . . ? C45 Co4 B6 B10 151.63(9) . . . . ? B7 Co4 B6 B10 -31.83(7) . . . . ? B3 Co4 B6 B10 -80.98(7) . . . . ? C42 Co4 B6 B9 154.11(9) . . . . ? C41 Co4 B6 B9 166.00(18) . . . . ? C2 Co4 B6 B9 -47.71(9) . . . . ? C43 Co4 B6 B9 -172.41(9) . . . . ? C1 Co4 B6 B9 -22.73(8) . . . . ? C44 Co4 B6 B9 -132.50(9) . . . . ? C45 Co4 B6 B9 -110.05(10) . . . . ? B7 Co4 B6 B9 66.49(9) . . . . ? B10 Co4 B6 B9 98.32(10) . . . . ? B3 Co4 B6 B9 17.35(9) . . . . ? C1 B3 B7 B13 -75.79(14) . . . . ? B8 B3 B7 B13 32.17(10) . . . . ? B5 B3 B7 B13 -8.55(12) . . . . ? Co4 B3 B7 B13 -110.49(9) . . . . ? C1 B3 B7 B8 -107.96(13) . . . . ? B5 B3 B7 B8 -40.73(9) . . . . ? Co4 B3 B7 B8 -142.66(9) . . . . ? C1 B3 B7 B10 -10.71(16) . . . . ? B8 B3 B7 B10 97.25(12) . . . . ? B5 B3 B7 B10 56.52(13) . . . . ? Co4 B3 B7 B10 -45.42(9) . . . . ? C1 B3 B7 Co4 34.70(10) . . . . ? B8 B3 B7 Co4 142.66(9) . . . . ? B5 B3 B7 Co4 101.94(8) . . . . ? C42 Co4 B7 B13 -125.15(11) . . . . ? C41 Co4 B7 B13 -165.77(10) . . . . ? C2 Co4 B7 B13 39.55(11) . . . . ? C43 Co4 B7 B13 -98.66(11) . . . . ? C1 Co4 B7 B13 77.83(10) . . . . ? C44 Co4 B7 B13 -129.48(15) . . . . ? C45 Co4 B7 B13 175.49(9) . . . . ? B10 Co4 B7 B13 -33.79(9) . . . . ? B3 Co4 B7 B13 101.20(12) . . . . ? B6 Co4 B7 B13 -1.65(10) . . . . ? C42 Co4 B7 B8 167.69(10) . . . . ? C41 Co4 B7 B8 127.08(10) . . . . ? C2 Co4 B7 B8 -27.60(11) . . . . ? C43 Co4 B7 B8 -165.81(9) . . . . ? C1 Co4 B7 B8 10.67(10) . . . . ? C44 Co4 B7 B8 163.37(13) . . . . ? C45 Co4 B7 B8 108.33(10) . . . . ? B10 Co4 B7 B8 -100.95(11) . . . . ? B3 Co4 B7 B8 34.05(9) . . . . ? B6 Co4 B7 B8 -68.81(10) . . . . ? C42 Co4 B7 B10 -91.36(8) . . . . ? C41 Co4 B7 B10 -131.97(8) . . . . ? C2 Co4 B7 B10 73.35(8) . . . . ? C43 Co4 B7 B10 -64.87(9) . . . . ? C1 Co4 B7 B10 111.62(7) . . . . ? C44 Co4 B7 B10 -95.68(16) . . . . ? C45 Co4 B7 B10 -150.72(8) . . . . ? B3 Co4 B7 B10 134.99(10) . . . . ? B6 Co4 B7 B10 32.14(7) . . . . ? C42 Co4 B7 B3 133.64(8) . . . . ? C41 Co4 B7 B3 93.03(8) . . . . ? C2 Co4 B7 B3 -61.65(8) . . . . ? C43 Co4 B7 B3 160.14(8) . . . . ? C1 Co4 B7 B3 -23.38(7) . . . . ? C44 Co4 B7 B3 129.32(15) . . . . ? C45 Co4 B7 B3 74.29(9) . . . . ? B10 Co4 B7 B3 -134.99(10) . . . . ? B6 Co4 B7 B3 -102.85(7) . . . . ? C1 B3 B8 B7 106.68(12) . . . . ? B5 B3 B8 B7 132.76(10) . . . . ? Co4 B3 B8 B7 36.22(8) . . . . ? C1 B3 B8 B5 -26.08(11) . . . . ? B7 B3 B8 B5 -132.76(10) . . . . ? Co4 B3 B8 B5 -96.54(9) . . . . ? C1 B3 B8 B13 73.79(15) . . . . ? B5 B3 B8 B13 99.87(12) . . . . ? B7 B3 B8 B13 -32.89(10) . . . . ? Co4 B3 B8 B13 3.33(14) . . . . ? C1 B3 B8 B11 8.69(16) . . . . ? B5 B3 B8 B11 34.77(10) . . . . ? B7 B3 B8 B11 -97.99(11) . . . . ? Co4 B3 B8 B11 -61.77(12) . . . . ? B13 B7 B8 B3 -144.78(10) . . . . ? B10 B7 B8 B3 -108.31(11) . . . . ? Co4 B7 B8 B3 -37.17(9) . . . . ? B13 B7 B8 B5 -101.25(11) . . . . ? B10 B7 B8 B5 -64.77(14) . . . . ? B3 B7 B8 B5 43.54(10) . . . . ? Co4 B7 B8 B5 6.37(13) . . . . ? B10 B7 B8 B13 36.47(10) . . . . ? B3 B7 B8 B13 144.78(10) . . . . ? Co4 B7 B8 B13 107.62(10) . . . . ? B13 B7 B8 B11 -39.31(10) . . . . ? B10 B7 B8 B11 -2.84(14) . . . . ? B3 B7 B8 B11 105.47(11) . . . . ? Co4 B7 B8 B11 68.31(12) . . . . ? B11 B5 B8 B3 141.43(10) . . . . ? C1 B5 B8 B3 20.88(9) . . . . ? B9 B5 B8 B3 106.79(10) . . . . ? B11 B5 B8 B7 97.59(11) . . . . ? C1 B5 B8 B7 -22.96(13) . . . . ? B3 B5 B8 B7 -43.84(10) . . . . ? B9 B5 B8 B7 62.95(13) . . . . ? B11 B5 B8 B13 34.10(10) . . . . ? C1 B5 B8 B13 -86.45(12) . . . . ? B3 B5 B8 B13 -107.33(11) . . . . ? B9 B5 B8 B13 -0.54(13) . . . . ? C1 B5 B8 B11 -120.55(11) . . . . ? B3 B5 B8 B11 -141.43(10) . . . . ? B9 B5 B8 B11 -34.64(9) . . . . ? C1 C2 B9 B11 -39.40(15) . . . . ? C3 C2 B9 B11 -156.90(12) . . . . ? B6 C2 B9 B11 87.62(14) . . . . ? Co4 C2 B9 B11 31.59(15) . . . . ? C1 C2 B9 B12 -104.81(11) . . . . ? C3 C2 B9 B12 137.69(11) . . . . ? B6 C2 B9 B12 22.21(9) . . . . ? Co4 C2 B9 B12 -33.82(11) . . . . ? C1 C2 B9 B6 -127.02(11) . . . . ? C3 C2 B9 B6 115.48(12) . . . . ? Co4 C2 B9 B6 -56.03(8) . . . . ? C1 C2 B9 B5 -0.30(10) . . . . ? C3 C2 B9 B5 -117.80(11) . . . . ? B6 C2 B9 B5 126.72(10) . . . . ? Co4 C2 B9 B5 70.69(9) . . . . ? C2 B6 B9 B11 -119.57(11) . . . . ? B12 B6 B9 B11 35.15(10) . . . . ? B10 B6 B9 B11 -5.80(13) . . . . ? Co4 B6 B9 B11 -72.50(11) . . . . ? C2 B6 B9 B12 -154.72(10) . . . . ? B10 B6 B9 B12 -40.95(9) . . . . ? Co4 B6 B9 B12 -107.65(9) . . . . ? B12 B6 B9 C2 154.72(10) . . . . ? B10 B6 B9 C2 113.77(11) . . . . ? Co4 B6 B9 C2 47.08(7) . . . . ? C2 B6 B9 B5 -59.27(11) . . . . ? B12 B6 B9 B5 95.45(11) . . . . ? B10 B6 B9 B5 54.50(13) . . . . ? Co4 B6 B9 B5 -12.20(12) . . . . ? B8 B5 B9 B11 36.81(10) . . . . ? C1 B5 B9 B11 141.48(11) . . . . ? B3 B5 B9 B11 98.12(12) . . . . ? B11 B5 B9 B12 -36.32(10) . . . . ? B8 B5 B9 B12 0.49(13) . . . . ? C1 B5 B9 B12 105.17(10) . . . . ? B3 B5 B9 B12 61.80(14) . . . . ? B11 B5 B9 C2 -141.24(11) . . . . ? B8 B5 B9 C2 -104.43(10) . . . . ? C1 B5 B9 C2 0.24(8) . . . . ? B3 B5 B9 C2 -43.12(11) . . . . ? B11 B5 B9 B6 -97.89(12) . . . . ? B8 B5 B9 B6 -61.09(13) . . . . ? C1 B5 B9 B6 43.59(11) . . . . ? B3 B5 B9 B6 0.22(15) . . . . ? B8 B7 B10 B13 -36.69(10) . . . . ? B3 B7 B10 B13 -99.20(12) . . . . ? Co4 B7 B10 B13 -144.68(9) . . . . ? B13 B7 B10 B12 35.75(11) . . . . ? B8 B7 B10 B12 -0.94(15) . . . . ? B3 B7 B10 B12 -63.45(14) . . . . ? Co4 B7 B10 B12 -108.93(10) . . . . ? B13 B7 B10 B6 99.05(12) . . . . ? B8 B7 B10 B6 62.36(14) . . . . ? B3 B7 B10 B6 -0.15(16) . . . . ? Co4 B7 B10 B6 -45.63(9) . . . . ? B13 B7 B10 Co4 144.68(9) . . . . ? B8 B7 B10 Co4 107.99(10) . . . . ? B3 B7 B10 Co4 45.48(9) . . . . ? C2 B6 B10 B13 76.20(14) . . . . ? B12 B6 B10 B13 -32.39(10) . . . . ? B9 B6 B10 B13 8.81(14) . . . . ? Co4 B6 B10 B13 110.12(10) . . . . ? C2 B6 B10 B12 108.59(13) . . . . ? B9 B6 B10 B12 41.20(10) . . . . ? Co4 B6 B10 B12 142.51(9) . . . . ? C2 B6 B10 B7 11.17(16) . . . . ? B12 B6 B10 B7 -97.42(12) . . . . ? B9 B6 B10 B7 -56.22(14) . . . . ? Co4 B6 B10 B7 45.09(9) . . . . ? C2 B6 B10 Co4 -33.92(10) . . . . ? B12 B6 B10 Co4 -142.51(9) . . . . ? B9 B6 B10 Co4 -101.31(9) . . . . ? C42 Co4 B10 B13 121.85(10) . . . . ? C41 Co4 B10 B13 96.04(11) . . . . ? C2 Co4 B10 B13 -78.88(10) . . . . ? C43 Co4 B10 B13 162.58(10) . . . . ? C1 Co4 B10 B13 -40.94(10) . . . . ? C44 Co4 B10 B13 -177.19(9) . . . . ? C45 Co4 B10 B13 130.95(14) . . . . ? B7 Co4 B10 B13 33.59(9) . . . . ? B3 Co4 B10 B13 0.76(10) . . . . ? B6 Co4 B10 B13 -101.79(11) . . . . ? C42 Co4 B10 B12 -171.10(10) . . . . ? C41 Co4 B10 B12 163.10(9) . . . . ? C2 Co4 B10 B12 -11.83(9) . . . . ? C43 Co4 B10 B12 -130.37(10) . . . . ? C1 Co4 B10 B12 26.11(10) . . . . ? C44 Co4 B10 B12 -110.14(10) . . . . ? C45 Co4 B10 B12 -162.00(13) . . . . ? B7 Co4 B10 B12 100.65(11) . . . . ? B3 Co4 B10 B12 67.81(9) . . . . ? B6 Co4 B10 B12 -34.73(9) . . . . ? C42 Co4 B10 B7 88.25(8) . . . . ? C41 Co4 B10 B7 62.45(9) . . . . ? C2 Co4 B10 B7 -112.47(7) . . . . ? C43 Co4 B10 B7 128.99(8) . . . . ? C1 Co4 B10 B7 -74.53(8) . . . . ? C44 Co4 B10 B7 149.22(8) . . . . ? C45 Co4 B10 B7 97.35(15) . . . . ? B3 Co4 B10 B7 -32.84(7) . . . . ? B6 Co4 B10 B7 -135.38(10) . . . . ? C42 Co4 B10 B6 -136.37(8) . . . . ? C41 Co4 B10 B6 -162.17(7) . . . . ? C2 Co4 B10 B6 22.91(7) . . . . ? C43 Co4 B10 B6 -95.63(8) . . . . ? C1 Co4 B10 B6 60.84(7) . . . . ? C44 Co4 B10 B6 -75.41(9) . . . . ? C45 Co4 B10 B6 -127.27(14) . . . . ? B7 Co4 B10 B6 135.38(10) . . . . ? B3 Co4 B10 B6 102.54(7) . . . . ? B12 B9 B11 B5 139.27(11) . . . . ? C2 B9 B11 B5 48.71(13) . . . . ? B6 B9 B11 B5 105.19(11) . . . . ? B12 B9 B11 B13 34.93(11) . . . . ? C2 B9 B11 B13 -55.62(16) . . . . ? B6 B9 B11 B13 0.85(14) . . . . ? B5 B9 B11 B13 -104.33(12) . . . . ? C2 B9 B11 B12 -90.55(13) . . . . ? B6 B9 B11 B12 -34.08(10) . . . . ? B5 B9 B11 B12 -139.27(11) . . . . ? B12 B9 B11 B8 100.08(13) . . . . ? C2 B9 B11 B8 9.52(18) . . . . ? B6 B9 B11 B8 66.00(14) . . . . ? B5 B9 B11 B8 -39.19(10) . . . . ? B8 B5 B11 B9 -138.64(11) . . . . ? C1 B5 B11 B9 -48.21(12) . . . . ? B3 B5 B11 B9 -104.72(11) . . . . ? B8 B5 B11 B13 -34.41(10) . . . . ? C1 B5 B11 B13 56.03(15) . . . . ? B3 B5 B11 B13 -0.49(13) . . . . ? B9 B5 B11 B13 104.23(12) . . . . ? B8 B5 B11 B12 -99.51(12) . . . . ? C1 B5 B11 B12 -9.08(17) . . . . ? B3 B5 B11 B12 -65.59(13) . . . . ? B9 B5 B11 B12 39.13(10) . . . . ? C1 B5 B11 B8 90.44(13) . . . . ? B3 B5 B11 B8 33.92(9) . . . . ? B9 B5 B11 B8 138.64(11) . . . . ? B3 B8 B11 B9 6.11(16) . . . . ? B7 B8 B11 B9 -60.61(15) . . . . ? B5 B8 B11 B9 42.33(11) . . . . ? B13 B8 B11 B9 -99.83(13) . . . . ? B3 B8 B11 B5 -36.22(10) . . . . ? B7 B8 B11 B5 -102.94(11) . . . . ? B13 B8 B11 B5 -142.16(11) . . . . ? B3 B8 B11 B13 105.94(12) . . . . ? B7 B8 B11 B13 39.22(10) . . . . ? B5 B8 B11 B13 142.16(11) . . . . ? B3 B8 B11 B12 72.35(14) . . . . ? B7 B8 B11 B12 5.63(15) . . . . ? B5 B8 B11 B12 108.57(12) . . . . ? B13 B8 B11 B12 -33.60(11) . . . . ? C2 B6 B12 B13 -73.59(15) . . . . ? B10 B6 B12 B13 33.04(11) . . . . ? B9 B6 B12 B13 -99.41(12) . . . . ? Co4 B6 B12 B13 -3.48(14) . . . . ? C2 B6 B12 B10 -106.63(12) . . . . ? B9 B6 B12 B10 -132.45(10) . . . . ? Co4 B6 B12 B10 -36.51(9) . . . . ? C2 B6 B12 B11 -8.75(16) . . . . ? B10 B6 B12 B11 97.88(11) . . . . ? B9 B6 B12 B11 -34.56(10) . . . . ? Co4 B6 B12 B11 61.37(12) . . . . ? C2 B6 B12 B9 25.82(11) . . . . ? B10 B6 B12 B9 132.45(10) . . . . ? Co4 B6 B12 B9 95.93(9) . . . . ? B13 B10 B12 B6 144.47(11) . . . . ? B7 B10 B12 B6 108.88(11) . . . . ? Co4 B10 B12 B6 37.89(9) . . . . ? B7 B10 B12 B13 -35.58(11) . . . . ? B6 B10 B12 B13 -144.47(11) . . . . ? Co4 B10 B12 B13 -106.58(10) . . . . ? B13 B10 B12 B11 39.90(10) . . . . ? B7 B10 B12 B11 4.31(14) . . . . ? B6 B10 B12 B11 -104.57(11) . . . . ? Co4 B10 B12 B11 -66.68(12) . . . . ? B13 B10 B12 B9 101.22(11) . . . . ? B7 B10 B12 B9 65.64(13) . . . . ? B6 B10 B12 B9 -43.25(9) . . . . ? Co4 B10 B12 B9 -5.36(13) . . . . ? B9 B11 B12 B6 36.02(10) . . . . ? B5 B11 B12 B6 -5.98(15) . . . . ? B13 B11 B12 B6 -105.44(12) . . . . ? B8 B11 B12 B6 -71.78(14) . . . . ? B9 B11 B12 B13 141.47(11) . . . . ? B5 B11 B12 B13 99.46(13) . . . . ? B8 B11 B12 B13 33.67(11) . . . . ? B9 B11 B12 B10 101.62(12) . . . . ? B5 B11 B12 B10 59.62(14) . . . . ? B13 B11 B12 B10 -39.85(10) . . . . ? B8 B11 B12 B10 -6.18(14) . . . . ? B5 B11 B12 B9 -42.00(11) . . . . ? B13 B11 B12 B9 -141.47(11) . . . . ? B8 B11 B12 B9 -107.80(12) . . . . ? B11 B9 B12 B6 -141.26(11) . . . . ? C2 B9 B12 B6 -20.62(9) . . . . ? B5 B9 B12 B6 -106.90(11) . . . . ? B11 B9 B12 B13 -34.62(10) . . . . ? C2 B9 B12 B13 86.02(12) . . . . ? B6 B9 B12 B13 106.64(12) . . . . ? B5 B9 B12 B13 -0.25(14) . . . . ? B11 B9 B12 B10 -97.95(11) . . . . ? C2 B9 B12 B10 22.69(12) . . . . ? B6 B9 B12 B10 43.31(9) . . . . ? B5 B9 B12 B10 -63.59(12) . . . . ? C2 B9 B12 B11 120.64(11) . . . . ? B6 B9 B12 B11 141.26(11) . . . . ? B5 B9 B12 B11 34.37(9) . . . . ? B8 B7 B13 B10 139.39(11) . . . . ? B3 B7 B13 B10 108.15(11) . . . . ? Co4 B7 B13 B10 35.95(9) . . . . ? B8 B7 B13 B12 103.49(12) . . . . ? B10 B7 B13 B12 -35.90(10) . . . . ? B3 B7 B13 B12 72.24(13) . . . . ? Co4 B7 B13 B12 0.04(14) . . . . ? B8 B7 B13 B11 39.68(10) . . . . ? B10 B7 B13 B11 -99.72(11) . . . . ? B3 B7 B13 B11 8.43(13) . . . . ? Co4 B7 B13 B11 -63.77(12) . . . . ? B10 B7 B13 B8 -139.39(11) . . . . ? B3 B7 B13 B8 -31.25(9) . . . . ? Co4 B7 B13 B8 -103.45(10) . . . . ? B12 B10 B13 B7 -140.39(11) . . . . ? B6 B10 B13 B7 -108.62(12) . . . . ? Co4 B10 B13 B7 -35.67(9) . . . . ? B7 B10 B13 B12 140.39(11) . . . . ? B6 B10 B13 B12 31.77(10) . . . . ? Co4 B10 B13 B12 104.72(10) . . . . ? B12 B10 B13 B11 -40.22(10) . . . . ? B7 B10 B13 B11 100.17(12) . . . . ? B6 B10 B13 B11 -8.45(14) . . . . ? Co4 B10 B13 B11 64.50(12) . . . . ? B12 B10 B13 B8 -103.81(12) . . . . ? B7 B10 B13 B8 36.59(10) . . . . ? B6 B10 B13 B8 -72.03(13) . . . . ? Co4 B10 B13 B8 0.91(14) . . . . ? B6 B12 B13 B7 2.18(16) . . . . ? B10 B12 B13 B7 36.07(11) . . . . ? B11 B12 B13 B7 -98.48(12) . . . . ? B9 B12 B13 B7 -64.47(14) . . . . ? B6 B12 B13 B10 -33.89(11) . . . . ? B11 B12 B13 B10 -134.54(12) . . . . ? B9 B12 B13 B10 -100.53(12) . . . . ? B6 B12 B13 B11 100.66(12) . . . . ? B10 B12 B13 B11 134.54(12) . . . . ? B9 B12 B13 B11 34.01(10) . . . . ? B6 B12 B13 B8 66.57(14) . . . . ? B10 B12 B13 B8 100.46(12) . . . . ? B11 B12 B13 B8 -34.08(11) . . . . ? B9 B12 B13 B8 -0.08(15) . . . . ? B9 B11 B13 B7 68.02(13) . . . . ? B5 B11 B13 B7 -4.92(13) . . . . ? B12 B11 B13 B7 103.43(11) . . . . ? B8 B11 B13 B7 -39.53(10) . . . . ? B9 B11 B13 B10 4.66(15) . . . . ? B5 B11 B13 B10 -68.28(13) . . . . ? B12 B11 B13 B10 40.08(10) . . . . ? B8 B11 B13 B10 -102.88(12) . . . . ? B9 B11 B13 B12 -35.41(11) . . . . ? B5 B11 B13 B12 -108.36(12) . . . . ? B8 B11 B13 B12 -142.96(11) . . . . ? B9 B11 B13 B8 107.55(12) . . . . ? B5 B11 B13 B8 34.60(10) . . . . ? B12 B11 B13 B8 142.96(11) . . . . ? B3 B8 B13 B7 34.12(10) . . . . ? B5 B8 B13 B7 101.54(11) . . . . ? B11 B8 B13 B7 135.24(11) . . . . ? B3 B8 B13 B10 -2.67(15) . . . . ? B7 B8 B13 B10 -36.79(10) . . . . ? B5 B8 B13 B10 64.75(13) . . . . ? B11 B8 B13 B10 98.44(11) . . . . ? B3 B8 B13 B12 -67.01(14) . . . . ? B7 B8 B13 B12 -101.13(12) . . . . ? B5 B8 B13 B12 0.41(15) . . . . ? B11 B8 B13 B12 34.11(11) . . . . ? B3 B8 B13 B11 -101.12(12) . . . . ? B7 B8 B13 B11 -135.24(11) . . . . ? B5 B8 B13 B11 -33.70(10) . . . . ? C1 C2 C3 C4 14.57(14) . . . . ? B6 C2 C3 C4 -156.73(12) . . . . ? B9 C2 C3 C4 126.16(12) . . . . ? Co4 C2 C3 C4 -63.46(14) . . . . ? C2 C3 C4 C5 -23.07(14) . . . . ? C2 C1 C5 C4 -14.59(15) . . . . ? B3 C1 C5 C4 155.96(12) . . . . ? B5 C1 C5 C4 -126.71(12) . . . . ? Co4 C1 C5 C4 63.45(14) . . . . ? C3 C4 C5 C1 22.97(14) . . . . ? C42 Co4 C41 C45 118.84(13) . . . . ? C2 Co4 C41 C45 -29.18(15) . . . . ? C43 Co4 C41 C45 80.47(10) . . . . ? C1 Co4 C41 C45 -66.78(10) . . . . ? C44 Co4 C41 C45 37.10(9) . . . . ? B7 Co4 C41 C45 -157.65(9) . . . . ? B10 Co4 C41 C45 160.49(8) . . . . ? B3 Co4 C41 C45 -107.43(9) . . . . ? B6 Co4 C41 C45 103.6(2) . . . . ? C2 Co4 C41 C42 -148.02(11) . . . . ? C43 Co4 C41 C42 -38.37(10) . . . . ? C1 Co4 C41 C42 174.37(9) . . . . ? C44 Co4 C41 C42 -81.75(10) . . . . ? C45 Co4 C41 C42 -118.84(13) . . . . ? B7 Co4 C41 C42 83.51(10) . . . . ? B10 Co4 C41 C42 41.65(11) . . . . ? B3 Co4 C41 C42 133.72(10) . . . . ? B6 Co4 C41 C42 -15.2(2) . . . . ? C45 C41 C42 C43 -0.41(17) . . . . ? Co4 C41 C42 C43 60.60(11) . . . . ? C45 C41 C42 Co4 -61.01(10) . . . . ? C41 Co4 C42 C43 -118.14(14) . . . . ? C2 Co4 C42 C43 10.0(2) . . . . ? C1 Co4 C42 C43 -131.08(15) . . . . ? C44 Co4 C42 C43 -37.60(10) . . . . ? C45 Co4 C42 C43 -80.70(10) . . . . ? B7 Co4 C42 C43 144.26(10) . . . . ? B10 Co4 C42 C43 95.63(10) . . . . ? B3 Co4 C42 C43 -175.36(9) . . . . ? B6 Co4 C42 C43 56.86(12) . . . . ? C2 Co4 C42 C41 128.18(16) . . . . ? C43 Co4 C42 C41 118.14(14) . . . . ? C1 Co4 C42 C41 -12.9(2) . . . . ? C44 Co4 C42 C41 80.55(10) . . . . ? C45 Co4 C42 C41 37.44(9) . . . . ? B7 Co4 C42 C41 -97.60(9) . . . . ? B10 Co4 C42 C41 -146.23(9) . . . . ? B3 Co4 C42 C41 -57.22(11) . . . . ? B6 Co4 C42 C41 175.01(8) . . . . ? C41 C42 C43 C44 0.35(17) . . . . ? Co4 C42 C43 C44 60.85(10) . . . . ? C41 C42 C43 Co4 -60.50(10) . . . . ? C42 Co4 C43 C44 -118.59(14) . . . . ? C41 Co4 C43 C44 -80.16(10) . . . . ? C2 Co4 C43 C44 65.45(11) . . . . ? C1 Co4 C43 C44 25.43(16) . . . . ? C45 Co4 C43 C44 -36.81(9) . . . . ? B7 Co4 C43 C44 -161.57(9) . . . . ? B10 Co4 C43 C44 155.50(9) . . . . ? B3 Co4 C43 C44 -105.9(2) . . . . ? B6 Co4 C43 C44 106.14(10) . . . . ? C41 Co4 C43 C42 38.43(10) . . . . ? C2 Co4 C43 C42 -175.96(9) . . . . ? C1 Co4 C43 C42 144.02(12) . . . . ? C44 Co4 C43 C42 118.59(14) . . . . ? C45 Co4 C43 C42 81.78(10) . . . . ? B7 Co4 C43 C42 -42.99(12) . . . . ? B10 Co4 C43 C42 -85.92(10) . . . . ? B3 Co4 C43 C42 12.7(3) . . . . ? B6 Co4 C43 C42 -135.28(10) . . . . ? C42 C43 C44 C45 -0.16(17) . . . . ? Co4 C43 C44 C45 59.19(10) . . . . ? C42 C43 C44 Co4 -59.34(10) . . . . ? C42 Co4 C44 C43 38.34(10) . . . . ? C41 Co4 C44 C43 82.78(10) . . . . ? C2 Co4 C44 C43 -126.32(9) . . . . ? C1 Co4 C44 C43 -166.56(9) . . . . ? C45 Co4 C44 C43 120.10(13) . . . . ? B7 Co4 C44 C43 43.01(19) . . . . ? B10 Co4 C44 C43 -32.43(12) . . . . ? B3 Co4 C44 C43 150.87(10) . . . . ? B6 Co4 C44 C43 -81.94(10) . . . . ? C42 Co4 C44 C45 -81.76(10) . . . . ? C41 Co4 C44 C45 -37.32(9) . . . . ? C2 Co4 C44 C45 113.58(9) . . . . ? C43 Co4 C44 C45 -120.10(13) . . . . ? C1 Co4 C44 C45 73.34(9) . . . . ? B7 Co4 C44 C45 -77.09(18) . . . . ? B10 Co4 C44 C45 -152.53(9) . . . . ? B3 Co4 C44 C45 30.77(13) . . . . ? B6 Co4 C44 C45 157.96(9) . . . . ? C42 C41 C45 C44 0.32(16) . . . . ? Co4 C41 C45 C44 -59.07(10) . . . . ? C42 C41 C45 Co4 59.39(10) . . . . ? C43 C44 C45 C41 -0.10(16) . . . . ? Co4 C44 C45 C41 58.14(10) . . . . ? C43 C44 C45 Co4 -58.24(10) . . . . ? C42 Co4 C45 C41 -38.24(9) . . . . ? C2 Co4 C45 C41 164.06(8) . . . . ? C43 Co4 C45 C41 -82.55(10) . . . . ? C1 Co4 C45 C41 124.06(9) . . . . ? C44 Co4 C45 C41 -119.57(13) . . . . ? B7 Co4 C45 C41 29.88(12) . . . . ? B10 Co4 C45 C41 -48.06(18) . . . . ? B3 Co4 C45 C41 79.69(10) . . . . ? B6 Co4 C45 C41 -154.67(9) . . . . ? C42 Co4 C45 C44 81.33(10) . . . . ? C41 Co4 C45 C44 119.57(13) . . . . ? C2 Co4 C45 C44 -76.37(10) . . . . ? C43 Co4 C45 C44 37.03(9) . . . . ? C1 Co4 C45 C44 -116.36(9) . . . . ? B7 Co4 C45 C44 149.45(9) . . . . ? B10 Co4 C45 C44 71.51(17) . . . . ? B3 Co4 C45 C44 -160.73(9) . . . . ? B6 Co4 C45 C44 -35.10(13) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.313 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.121 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 265426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H30 B10 Ru' _chemical_formula_sum 'C15 H30 B10 Ru' _chemical_formula_weight 419.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.2728(17) _cell_length_b 14.678(3) _cell_length_c 15.693(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1905.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6622 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 30.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7628 _exptl_absorpt_correction_T_max 0.8535 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26636 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 30.71 _reflns_number_total 5852 _reflns_number_gt 5596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+0.7507P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.028(17) _refine_ls_number_reflns 5852 _refine_ls_number_parameters 268 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0444 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Ru4 Ru 0.820940(14) 0.164535(8) 0.218984(7) 0.00892(3) Uani 1 1 d . . . C1 C 0.79987(19) 0.09240(10) 0.09969(9) 0.0117(3) Uani 1 1 d . . . C2 C 0.87407(19) 0.03355(10) 0.16221(10) 0.0111(3) Uani 1 1 d . . . B3 B 0.6355(2) 0.14874(12) 0.11160(11) 0.0133(3) Uani 1 1 d D . . H3 H 0.615(2) 0.2023(11) 0.0646(11) 0.016 Uiso 1 1 d D . . B5 B 0.6178(2) 0.02799(12) 0.08356(12) 0.0143(3) Uani 1 1 d D . . H5 H 0.621(2) 0.0097(14) 0.0173(10) 0.017 Uiso 1 1 d D . . B6 B 0.8069(3) 0.01196(11) 0.25582(10) 0.0125(3) Uani 1 1 d D . . H6 H 0.901(2) -0.0177(13) 0.2944(12) 0.015 Uiso 1 1 d D . . B7 B 0.54786(19) 0.15665(11) 0.21937(11) 0.0100(3) Uani 1 1 d D . . H7 H 0.484(2) 0.2183(10) 0.2370(12) 0.012 Uiso 1 1 d D . . B8 B 0.4613(2) 0.08744(13) 0.13803(11) 0.0151(3) Uani 1 1 d D . . H8 H 0.346(2) 0.1057(13) 0.1080(12) 0.018 Uiso 1 1 d D . . B9 B 0.7167(2) -0.05166(12) 0.16693(11) 0.0139(3) Uani 1 1 d D . . H9 H 0.768(2) -0.1149(11) 0.1448(12) 0.017 Uiso 1 1 d D . . B10 B 0.6409(2) 0.08221(12) 0.29573(11) 0.0140(3) Uani 1 1 d D . . H10 H 0.636(2) 0.0982(13) 0.3636(9) 0.017 Uiso 1 1 d D . . B11 B 0.5114(2) -0.02784(13) 0.16286(12) 0.0150(3) Uani 1 1 d D . . H11 H 0.435(2) -0.0840(12) 0.1380(13) 0.018 Uiso 1 1 d D . . B12 B 0.6095(2) -0.03281(12) 0.26351(11) 0.0142(3) Uani 1 1 d D . . H12 H 0.592(2) -0.0855(12) 0.3094(11) 0.017 Uiso 1 1 d D . . B13 B 0.4588(2) 0.04979(13) 0.24470(11) 0.0143(3) Uani 1 1 d D . . H13 H 0.3451(19) 0.0404(12) 0.2777(12) 0.017 Uiso 1 1 d D . . C3 C 1.0368(2) 0.00257(11) 0.12916(10) 0.0150(3) Uani 1 1 d . . . H3A H 1.0554 -0.0626 0.1420 0.018 Uiso 1 1 calc R . . H3B H 1.1254 0.0390 0.1544 0.018 Uiso 1 1 calc R . . C4 C 1.0251(2) 0.01854(12) 0.03325(11) 0.0190(3) Uani 1 1 d . . . H4A H 0.9788 -0.0354 0.0043 0.023 Uiso 1 1 calc R . . H4B H 1.1330 0.0314 0.0088 0.023 Uiso 1 1 calc R . . C5 C 0.9134(2) 0.10118(11) 0.02376(10) 0.0151(3) Uani 1 1 d . . . H5A H 0.9754 0.1588 0.0263 0.018 Uiso 1 1 calc R . . H5B H 0.8530 0.0988 -0.0306 0.018 Uiso 1 1 calc R . . C40 C 0.9596(2) 0.21584(10) 0.33412(9) 0.0119(3) Uani 1 1 d . . . C41 C 0.8187(2) 0.26869(9) 0.31809(9) 0.0126(3) Uani 1 1 d . . . H41 H 0.7294 0.2688 0.3610 0.015 Uiso 1 1 calc R . . C42 C 0.7958(2) 0.31345(10) 0.23998(9) 0.0132(3) Uani 1 1 d . . . H42 H 0.6894 0.3432 0.2282 0.016 Uiso 1 1 calc R . . C43 C 0.9073(2) 0.30309(11) 0.17289(10) 0.0137(3) Uani 1 1 d . . . C44 C 1.0441(2) 0.24738(11) 0.18778(10) 0.0132(3) Uani 1 1 d . . . H44 H 1.1124 0.2287 0.1382 0.016 Uiso 1 1 calc R . . C45 C 1.07088(19) 0.20592(11) 0.26696(10) 0.0133(3) Uani 1 1 d . . . H45 H 1.1568 0.1582 0.2717 0.016 Uiso 1 1 calc R . . C46 C 0.8799(2) 0.34831(11) 0.08917(10) 0.0184(3) Uani 1 1 d . . . H46A H 0.7700 0.3733 0.0874 0.028 Uiso 1 1 calc R . . H46B H 0.8932 0.3037 0.0433 0.028 Uiso 1 1 calc R . . H46C H 0.9582 0.3977 0.0818 0.028 Uiso 1 1 calc R . . C47 C 0.98358(19) 0.17489(11) 0.42151(9) 0.0130(3) Uani 1 1 d . . . H47 H 0.8831 0.1408 0.4369 0.016 Uiso 1 1 calc R . . C48 C 1.0059(2) 0.25186(12) 0.48627(10) 0.0183(3) Uani 1 1 d . . . H48A H 1.1108 0.2813 0.4770 0.028 Uiso 1 1 calc R . . H48B H 1.0020 0.2268 0.5441 0.028 Uiso 1 1 calc R . . H48C H 0.9194 0.2968 0.4792 0.028 Uiso 1 1 calc R . . C49 C 1.1249(2) 0.10879(12) 0.42577(10) 0.0165(3) Uani 1 1 d . . . H49A H 1.1088 0.0599 0.3841 0.025 Uiso 1 1 calc R . . H49B H 1.1314 0.0826 0.4831 0.025 Uiso 1 1 calc R . . H49C H 1.2254 0.1413 0.4129 0.025 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 Ru4 0.00799(5) 0.00861(5) 0.01016(4) 0.00019(4) 0.00036(5) -0.00005(5) C1 0.0113(8) 0.0119(6) 0.0117(6) -0.0020(5) 0.0011(6) -0.0020(6) C2 0.0101(7) 0.0082(6) 0.0152(7) -0.0010(5) 0.0006(5) -0.0003(5) B3 0.0111(8) 0.0146(8) 0.0142(7) 0.0014(6) -0.0015(6) -0.0002(6) B5 0.0126(8) 0.0155(8) 0.0148(8) -0.0002(6) -0.0011(6) -0.0023(7) B6 0.0146(9) 0.0101(7) 0.0127(6) 0.0012(5) -0.0016(6) -0.0016(7) B7 0.0074(7) 0.0115(7) 0.0113(6) -0.0006(7) 0.0003(6) -0.0016(6) B8 0.0113(8) 0.0174(9) 0.0166(8) 0.0006(6) -0.0013(6) -0.0026(7) B9 0.0152(9) 0.0111(7) 0.0153(8) -0.0001(6) 0.0005(6) -0.0022(6) B10 0.0134(9) 0.0144(8) 0.0143(8) 0.0000(6) 0.0016(6) -0.0023(6) B11 0.0135(9) 0.0160(9) 0.0154(8) 0.0015(6) -0.0004(7) -0.0026(6) B12 0.0150(9) 0.0136(8) 0.0139(8) 0.0014(6) 0.0013(6) -0.0047(7) B13 0.0100(8) 0.0173(8) 0.0157(7) -0.0007(6) 0.0024(6) -0.0025(7) C3 0.0112(7) 0.0131(7) 0.0206(7) -0.0011(6) 0.0025(6) 0.0022(6) C4 0.0180(8) 0.0193(8) 0.0196(8) -0.0033(6) 0.0082(6) 0.0009(7) C5 0.0163(8) 0.0156(7) 0.0136(7) -0.0005(6) 0.0043(6) -0.0023(6) C40 0.0131(7) 0.0100(7) 0.0126(6) -0.0018(5) -0.0020(6) -0.0019(6) C41 0.0134(7) 0.0110(6) 0.0133(6) -0.0017(5) 0.0008(6) -0.0009(7) C42 0.0140(8) 0.0087(6) 0.0168(7) -0.0007(5) -0.0013(5) -0.0001(5) C43 0.0174(8) 0.0094(6) 0.0143(7) 0.0005(5) -0.0008(6) -0.0034(6) C44 0.0128(8) 0.0126(7) 0.0142(6) -0.0008(5) 0.0006(6) -0.0036(6) C45 0.0105(7) 0.0126(7) 0.0167(7) -0.0011(5) -0.0006(5) -0.0028(5) C46 0.0266(8) 0.0136(8) 0.0151(7) 0.0044(6) 0.0005(6) -0.0011(6) C47 0.0129(7) 0.0141(7) 0.0119(6) 0.0011(5) -0.0004(5) -0.0001(6) C48 0.0216(9) 0.0194(8) 0.0141(7) -0.0015(6) -0.0020(6) 0.0014(7) C49 0.0166(8) 0.0165(7) 0.0162(7) 0.0013(6) -0.0022(6) 0.0016(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru4 C1 2.1578(14) . ? Ru4 C2 2.1642(15) . ? Ru4 C41 2.1809(14) . ? Ru4 C42 2.2203(15) . ? Ru4 B7 2.2621(16) . ? Ru4 C44 2.2643(17) . ? Ru4 B10 2.2646(18) . ? Ru4 C40 2.2690(15) . ? Ru4 C43 2.2738(16) . ? Ru4 C45 2.2828(16) . ? Ru4 B3 2.2907(18) . ? Ru4 B6 2.3159(17) . ? C1 C2 1.444(2) . ? C1 C5 1.523(2) . ? C1 B3 1.603(2) . ? C1 B5 1.796(2) . ? C2 C3 1.513(2) . ? C2 B6 1.602(2) . ? C2 B9 1.807(2) . ? B3 B8 1.749(3) . ? B3 B5 1.832(3) . ? B3 B7 1.844(3) . ? B3 H3 1.092(14) . ? B5 B11 1.731(3) . ? B5 B8 1.780(3) . ? B5 B9 1.936(3) . ? B5 H5 1.074(14) . ? B6 B12 1.765(3) . ? B6 B10 1.828(3) . ? B6 B9 1.837(2) . ? B6 H6 1.075(14) . ? B7 B13 1.778(3) . ? B7 B8 1.782(3) . ? B7 B10 1.795(2) . ? B7 H7 1.083(14) . ? B8 B13 1.763(3) . ? B8 B11 1.785(3) . ? B8 H8 1.100(15) . ? B9 B11 1.735(3) . ? B9 B12 1.778(3) . ? B9 H9 1.079(14) . ? B10 B13 1.771(3) . ? B10 B12 1.781(3) . ? B10 H10 1.091(14) . ? B11 B13 1.771(3) . ? B11 B12 1.777(3) . ? B11 H11 1.111(14) . ? B12 B13 1.764(3) . ? B12 H12 1.066(14) . ? B13 H13 1.082(14) . ? C3 C4 1.526(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.532(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C40 C45 1.407(2) . ? C40 C41 1.423(2) . ? C40 C47 1.511(2) . ? C41 C42 1.404(2) . ? C41 H41 1.0000 . ? C42 C43 1.408(2) . ? C42 H42 1.0000 . ? C43 C44 1.415(2) . ? C43 C46 1.489(2) . ? C44 C45 1.401(2) . ? C44 H44 1.0000 . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.520(2) . ? C47 C48 1.531(2) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru4 C2 39.04(6) . . ? C1 Ru4 C41 164.15(5) . . ? C2 Ru4 C41 156.64(6) . . ? C1 Ru4 C42 127.17(6) . . ? C2 Ru4 C42 162.69(6) . . ? C41 Ru4 C42 37.18(5) . . ? C1 Ru4 B7 84.06(6) . . ? C2 Ru4 B7 99.12(6) . . ? C41 Ru4 B7 91.47(7) . . ? C42 Ru4 B7 87.51(6) . . ? C1 Ru4 C44 98.15(6) . . ? C2 Ru4 C44 102.85(6) . . ? C41 Ru4 C44 77.56(6) . . ? C42 Ru4 C44 65.15(6) . . ? B7 Ru4 C44 147.39(6) . . ? C1 Ru4 B10 98.42(6) . . ? C2 Ru4 B10 83.02(6) . . ? C41 Ru4 B10 89.39(6) . . ? C42 Ru4 B10 112.63(6) . . ? B7 Ru4 B10 46.73(6) . . ? C44 Ru4 B10 159.68(6) . . ? C1 Ru4 C40 153.45(6) . . ? C2 Ru4 C40 121.33(6) . . ? C41 Ru4 C40 37.22(6) . . ? C42 Ru4 C40 66.57(5) . . ? B7 Ru4 C40 121.33(6) . . ? C44 Ru4 C40 65.27(6) . . ? B10 Ru4 C40 94.95(6) . . ? C1 Ru4 C43 100.85(6) . . ? C2 Ru4 C43 126.85(6) . . ? C41 Ru4 C43 66.58(6) . . ? C42 Ru4 C43 36.50(6) . . ? B7 Ru4 C43 111.13(6) . . ? C44 Ru4 C43 36.35(6) . . ? B10 Ru4 C43 148.56(6) . . ? C40 Ru4 C43 78.32(6) . . ? C1 Ru4 C45 119.33(6) . . ? C2 Ru4 C45 100.85(6) . . ? C41 Ru4 C45 65.53(6) . . ? C42 Ru4 C45 76.93(6) . . ? B7 Ru4 C45 156.54(6) . . ? C44 Ru4 C45 35.89(5) . . ? B10 Ru4 C45 124.21(6) . . ? C40 Ru4 C45 36.00(5) . . ? C43 Ru4 C45 65.30(6) . . ? C1 Ru4 B3 42.10(6) . . ? C2 Ru4 B3 75.12(6) . . ? C41 Ru4 B3 126.15(6) . . ? C42 Ru4 B3 98.40(6) . . ? B7 Ru4 B3 47.77(7) . . ? C44 Ru4 B3 116.19(6) . . ? B10 Ru4 B3 84.07(6) . . ? C40 Ru4 B3 163.35(6) . . ? C43 Ru4 B3 93.84(6) . . ? C45 Ru4 B3 151.19(6) . . ? C1 Ru4 B6 74.81(6) . . ? C2 Ru4 B6 41.74(6) . . ? C41 Ru4 B6 119.96(6) . . ? C42 Ru4 B6 155.55(5) . . ? B7 Ru4 B6 84.26(7) . . ? C44 Ru4 B6 127.89(7) . . ? B10 Ru4 B6 47.03(7) . . ? C40 Ru4 B6 98.48(6) . . ? C43 Ru4 B6 163.75(6) . . ? C45 Ru4 B6 102.72(6) . . ? B3 Ru4 B6 93.00(6) . . ? C2 C1 C5 108.66(14) . . ? C2 C1 B3 126.17(13) . . ? C5 C1 B3 124.83(13) . . ? C2 C1 B5 97.89(12) . . ? C5 C1 B5 116.84(12) . . ? B3 C1 B5 64.94(10) . . ? C2 C1 Ru4 70.72(8) . . ? C5 C1 Ru4 125.98(11) . . ? B3 C1 Ru4 73.39(8) . . ? B5 C1 Ru4 116.63(9) . . ? C1 C2 C3 108.98(13) . . ? C1 C2 B6 126.43(14) . . ? C3 C2 B6 124.29(14) . . ? C1 C2 B9 97.79(12) . . ? C3 C2 B9 116.57(12) . . ? B6 C2 B9 64.90(10) . . ? C1 C2 Ru4 70.24(8) . . ? C3 C2 Ru4 126.08(11) . . ? B6 C2 Ru4 74.21(8) . . ? B9 C2 Ru4 116.85(10) . . ? C1 B3 B8 117.48(13) . . ? C1 B3 B5 62.64(10) . . ? B8 B3 B5 59.57(10) . . ? C1 B3 B7 118.24(12) . . ? B8 B3 B7 59.40(10) . . ? B5 B3 B7 104.47(12) . . ? C1 B3 Ru4 64.51(8) . . ? B8 B3 Ru4 115.44(10) . . ? B5 B3 Ru4 109.15(10) . . ? B7 B3 Ru4 65.30(7) . . ? C1 B3 H3 115.3(11) . . ? B8 B3 H3 113.6(11) . . ? B5 B3 H3 121.4(10) . . ? B7 B3 H3 120.8(11) . . ? Ru4 B3 H3 122.0(10) . . ? B11 B5 B8 61.11(11) . . ? B11 B5 C1 125.05(13) . . ? B8 B5 C1 106.52(12) . . ? B11 B5 B3 109.02(13) . . ? B8 B5 B3 57.89(10) . . ? C1 B5 B3 52.41(9) . . ? B11 B5 B9 56.15(10) . . ? B8 B5 B9 106.19(12) . . ? C1 B5 B9 82.43(11) . . ? B3 B5 B9 112.84(12) . . ? B11 B5 H5 126.1(11) . . ? B8 B5 H5 127.1(11) . . ? C1 B5 H5 104.5(11) . . ? B3 B5 H5 118.2(11) . . ? B9 B5 H5 119.6(11) . . ? C2 B6 B12 117.20(13) . . ? C2 B6 B10 117.58(12) . . ? B12 B6 B10 59.41(11) . . ? C2 B6 B9 62.95(10) . . ? B12 B6 B9 59.10(10) . . ? B10 B6 B9 103.97(13) . . ? C2 B6 Ru4 64.06(7) . . ? B12 B6 Ru4 115.05(11) . . ? B10 B6 Ru4 65.01(8) . . ? B9 B6 Ru4 108.80(9) . . ? C2 B6 H6 110.3(11) . . ? B12 B6 H6 118.5(10) . . ? B10 B6 H6 125.2(11) . . ? B9 B6 H6 120.9(11) . . ? Ru4 B6 H6 119.8(11) . . ? B13 B7 B8 59.37(10) . . ? B13 B7 B10 59.43(10) . . ? B8 B7 B10 107.67(12) . . ? B13 B7 B3 108.21(12) . . ? B8 B7 B3 57.66(10) . . ? B10 B7 B3 113.92(12) . . ? B13 B7 Ru4 117.36(10) . . ? B8 B7 Ru4 115.39(10) . . ? B10 B7 Ru4 66.71(8) . . ? B3 B7 Ru4 66.93(7) . . ? B13 B7 H7 118.5(10) . . ? B8 B7 H7 117.6(10) . . ? B10 B7 H7 123.1(10) . . ? B3 B7 H7 118.6(10) . . ? Ru4 B7 H7 116.4(10) . . ? B3 B8 B13 113.32(13) . . ? B3 B8 B5 62.54(11) . . ? B13 B8 B5 108.10(13) . . ? B3 B8 B7 62.95(10) . . ? B13 B8 B7 60.21(10) . . ? B5 B8 B7 109.33(13) . . ? B3 B8 B11 110.36(13) . . ? B13 B8 B11 59.89(10) . . ? B5 B8 B11 58.08(10) . . ? B7 B8 B11 106.89(12) . . ? B3 B8 H8 119.4(11) . . ? B13 B8 H8 118.2(11) . . ? B5 B8 H8 123.2(11) . . ? B7 B8 H8 121.2(11) . . ? B11 B8 H8 121.8(11) . . ? B11 B9 B12 60.77(11) . . ? B11 B9 C2 124.35(13) . . ? B12 B9 C2 106.66(12) . . ? B11 B9 B6 108.86(13) . . ? B12 B9 B6 58.41(10) . . ? C2 B9 B6 52.16(9) . . ? B11 B9 B5 55.93(10) . . ? B12 B9 B5 105.75(12) . . ? C2 B9 B5 81.88(10) . . ? B6 B9 B5 112.21(12) . . ? B11 B9 H9 123.2(11) . . ? B12 B9 H9 127.2(11) . . ? C2 B9 H9 107.4(11) . . ? B6 B9 H9 121.4(11) . . ? B5 B9 H9 118.0(11) . . ? B13 B10 B12 59.53(10) . . ? B13 B10 B7 59.80(10) . . ? B12 B10 B7 108.95(12) . . ? B13 B10 B6 109.43(12) . . ? B12 B10 B6 58.52(10) . . ? B7 B10 B6 115.91(12) . . ? B13 B10 Ru4 117.53(10) . . ? B12 B10 Ru4 116.79(10) . . ? B7 B10 Ru4 66.56(8) . . ? B6 B10 Ru4 67.96(8) . . ? B13 B10 H10 118.0(11) . . ? B12 B10 H10 118.4(11) . . ? B7 B10 H10 120.4(11) . . ? B6 B10 H10 118.8(11) . . ? Ru4 B10 H10 115.2(11) . . ? B5 B11 B9 67.92(11) . . ? B5 B11 B13 109.99(13) . . ? B9 B11 B13 110.09(13) . . ? B5 B11 B12 115.24(13) . . ? B9 B11 B12 60.80(11) . . ? B13 B11 B12 59.61(11) . . ? B5 B11 B8 60.82(11) . . ? B9 B11 B8 115.25(13) . . ? B13 B11 B8 59.43(10) . . ? B12 B11 B8 109.82(13) . . ? B5 B11 H11 112.9(11) . . ? B9 B11 H11 114.9(11) . . ? B13 B11 H11 126.3(11) . . ? B12 B11 H11 122.8(11) . . ? B8 B11 H11 119.6(11) . . ? B13 B12 B6 112.76(13) . . ? B13 B12 B11 60.02(10) . . ? B6 B12 B11 110.28(12) . . ? B13 B12 B9 108.48(12) . . ? B6 B12 B9 62.48(10) . . ? B11 B12 B9 58.43(10) . . ? B13 B12 B10 59.95(10) . . ? B6 B12 B10 62.06(10) . . ? B11 B12 B10 106.26(13) . . ? B9 B12 B10 108.47(12) . . ? B13 B12 H12 121.1(11) . . ? B6 B12 H12 116.2(11) . . ? B11 B12 H12 124.6(11) . . ? B9 B12 H12 122.0(11) . . ? B10 B12 H12 121.0(11) . . ? B8 B13 B12 111.48(13) . . ? B8 B13 B11 60.68(10) . . ? B12 B13 B11 60.36(10) . . ? B8 B13 B10 109.59(13) . . ? B12 B13 B10 60.52(10) . . ? B11 B13 B10 106.96(13) . . ? B8 B13 B7 60.42(10) . . ? B12 B13 B7 110.55(13) . . ? B11 B13 B7 107.67(13) . . ? B10 B13 B7 60.77(10) . . ? B8 B13 H13 120.2(11) . . ? B12 B13 H13 116.6(10) . . ? B11 B13 H13 118.6(10) . . ? B10 B13 H13 123.9(11) . . ? B7 B13 H13 125.4(10) . . ? C2 C3 C4 103.62(14) . . ? C2 C3 H3A 111.0 . . ? C4 C3 H3A 111.0 . . ? C2 C3 H3B 111.0 . . ? C4 C3 H3B 111.0 . . ? H3A C3 H3B 109.0 . . ? C3 C4 C5 104.81(13) . . ? C3 C4 H4A 110.8 . . ? C5 C4 H4A 110.8 . . ? C3 C4 H4B 110.8 . . ? C5 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? C1 C5 C4 103.24(13) . . ? C1 C5 H5A 111.1 . . ? C4 C5 H5A 111.1 . . ? C1 C5 H5B 111.1 . . ? C4 C5 H5B 111.1 . . ? H5A C5 H5B 109.1 . . ? C45 C40 C41 117.39(14) . . ? C45 C40 C47 123.59(14) . . ? C41 C40 C47 119.01(14) . . ? C45 C40 Ru4 72.54(9) . . ? C41 C40 Ru4 68.02(8) . . ? C47 C40 Ru4 131.09(11) . . ? C42 C41 C40 121.36(15) . . ? C42 C41 Ru4 72.94(8) . . ? C40 C41 Ru4 74.76(8) . . ? C42 C41 H41 119.2 . . ? C40 C41 H41 119.2 . . ? Ru4 C41 H41 119.2 . . ? C41 C42 C43 120.91(15) . . ? C41 C42 Ru4 69.88(8) . . ? C43 C42 Ru4 73.82(9) . . ? C41 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? Ru4 C42 H42 119.0 . . ? C42 C43 C44 117.56(14) . . ? C42 C43 C46 120.76(15) . . ? C44 C43 C46 121.67(15) . . ? C42 C43 Ru4 69.69(9) . . ? C44 C43 Ru4 71.46(9) . . ? C46 C43 Ru4 129.14(11) . . ? C45 C44 C43 121.58(15) . . ? C45 C44 Ru4 72.77(9) . . ? C43 C44 Ru4 72.19(9) . . ? C45 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? Ru4 C44 H44 118.8 . . ? C44 C45 C40 121.06(15) . . ? C44 C45 Ru4 71.33(9) . . ? C40 C45 Ru4 71.46(9) . . ? C44 C45 H45 118.8 . . ? C40 C45 H45 118.8 . . ? Ru4 C45 H45 118.8 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C40 C47 C49 113.24(13) . . ? C40 C47 C48 108.96(13) . . ? C49 C47 C48 110.42(13) . . ? C40 C47 H47 108.0 . . ? C49 C47 H47 108.0 . . ? C48 C47 H47 108.0 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 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 C41 Ru4 C1 C2 173.4(2) . . . . ? C42 Ru4 C1 C2 165.28(9) . . . . ? B7 Ru4 C1 C2 -112.41(10) . . . . ? C44 Ru4 C1 C2 100.38(9) . . . . ? B10 Ru4 C1 C2 -67.82(10) . . . . ? C40 Ru4 C1 C2 51.61(16) . . . . ? C43 Ru4 C1 C2 137.15(9) . . . . ? C45 Ru4 C1 C2 69.50(10) . . . . ? B3 Ru4 C1 C2 -139.18(13) . . . . ? B6 Ru4 C1 C2 -26.77(9) . . . . ? C2 Ru4 C1 C5 -99.49(16) . . . . ? C41 Ru4 C1 C5 73.9(3) . . . . ? C42 Ru4 C1 C5 65.79(15) . . . . ? B7 Ru4 C1 C5 148.10(14) . . . . ? C44 Ru4 C1 C5 0.89(14) . . . . ? B10 Ru4 C1 C5 -167.31(13) . . . . ? C40 Ru4 C1 C5 -47.9(2) . . . . ? C43 Ru4 C1 C5 37.66(14) . . . . ? C45 Ru4 C1 C5 -29.99(15) . . . . ? B3 Ru4 C1 C5 121.33(16) . . . . ? B6 Ru4 C1 C5 -126.26(14) . . . . ? C2 Ru4 C1 B3 139.18(13) . . . . ? C41 Ru4 C1 B3 -47.4(3) . . . . ? C42 Ru4 C1 B3 -55.54(11) . . . . ? B7 Ru4 C1 B3 26.77(9) . . . . ? C44 Ru4 C1 B3 -120.44(9) . . . . ? B10 Ru4 C1 B3 71.37(9) . . . . ? C40 Ru4 C1 B3 -169.21(11) . . . . ? C43 Ru4 C1 B3 -83.67(9) . . . . ? C45 Ru4 C1 B3 -151.32(8) . . . . ? B6 Ru4 C1 B3 112.41(10) . . . . ? C2 Ru4 C1 B5 89.28(13) . . . . ? C41 Ru4 C1 B5 -97.4(2) . . . . ? C42 Ru4 C1 B5 -105.45(11) . . . . ? B7 Ru4 C1 B5 -23.14(11) . . . . ? C44 Ru4 C1 B5 -170.34(10) . . . . ? B10 Ru4 C1 B5 21.46(11) . . . . ? C40 Ru4 C1 B5 140.88(12) . . . . ? C43 Ru4 C1 B5 -133.57(11) . . . . ? C45 Ru4 C1 B5 158.78(10) . . . . ? B3 Ru4 C1 B5 -49.91(11) . . . . ? B6 Ru4 C1 B5 62.50(11) . . . . ? C5 C1 C2 C3 0.05(17) . . . . ? B3 C1 C2 C3 -173.45(14) . . . . ? B5 C1 C2 C3 121.91(13) . . . . ? Ru4 C1 C2 C3 -122.56(12) . . . . ? C5 C1 C2 B6 173.95(14) . . . . ? B3 C1 C2 B6 0.5(2) . . . . ? B5 C1 C2 B6 -64.18(17) . . . . ? Ru4 C1 C2 B6 51.34(14) . . . . ? C5 C1 C2 B9 -121.59(13) . . . . ? B3 C1 C2 B9 64.91(17) . . . . ? B5 C1 C2 B9 0.27(12) . . . . ? Ru4 C1 C2 B9 115.80(9) . . . . ? C5 C1 C2 Ru4 122.61(11) . . . . ? B3 C1 C2 Ru4 -50.89(14) . . . . ? B5 C1 C2 Ru4 -115.53(9) . . . . ? C41 Ru4 C2 C1 -175.44(14) . . . . ? C42 Ru4 C2 C1 -42.9(2) . . . . ? B7 Ru4 C2 C1 68.63(10) . . . . ? C44 Ru4 C2 C1 -87.11(9) . . . . ? B10 Ru4 C2 C1 112.66(10) . . . . ? C40 Ru4 C2 C1 -155.79(9) . . . . ? C43 Ru4 C2 C1 -56.58(11) . . . . ? C45 Ru4 C2 C1 -123.75(9) . . . . ? B3 Ru4 C2 C1 26.96(9) . . . . ? B6 Ru4 C2 C1 139.24(13) . . . . ? C1 Ru4 C2 C3 99.55(16) . . . . ? C41 Ru4 C2 C3 -75.9(2) . . . . ? C42 Ru4 C2 C3 56.7(3) . . . . ? B7 Ru4 C2 C3 168.18(13) . . . . ? C44 Ru4 C2 C3 12.44(14) . . . . ? B10 Ru4 C2 C3 -147.80(14) . . . . ? C40 Ru4 C2 C3 -56.24(15) . . . . ? C43 Ru4 C2 C3 42.97(16) . . . . ? C45 Ru4 C2 C3 -24.20(14) . . . . ? B3 Ru4 C2 C3 126.51(14) . . . . ? B6 Ru4 C2 C3 -121.22(18) . . . . ? C1 Ru4 C2 B6 -139.24(13) . . . . ? C41 Ru4 C2 B6 45.32(19) . . . . ? C42 Ru4 C2 B6 177.87(18) . . . . ? B7 Ru4 C2 B6 -70.60(10) . . . . ? C44 Ru4 C2 B6 133.66(9) . . . . ? B10 Ru4 C2 B6 -26.58(9) . . . . ? C40 Ru4 C2 B6 64.98(10) . . . . ? C43 Ru4 C2 B6 164.18(9) . . . . ? C45 Ru4 C2 B6 97.01(10) . . . . ? B3 Ru4 C2 B6 -112.27(10) . . . . ? C1 Ru4 C2 B9 -88.83(13) . . . . ? C41 Ru4 C2 B9 95.73(18) . . . . ? C42 Ru4 C2 B9 -131.73(18) . . . . ? B7 Ru4 C2 B9 -20.20(12) . . . . ? C44 Ru4 C2 B9 -175.94(10) . . . . ? B10 Ru4 C2 B9 23.82(11) . . . . ? C40 Ru4 C2 B9 115.38(11) . . . . ? C43 Ru4 C2 B9 -145.42(10) . . . . ? C45 Ru4 C2 B9 147.41(10) . . . . ? B3 Ru4 C2 B9 -61.87(11) . . . . ? B6 Ru4 C2 B9 50.40(11) . . . . ? C2 C1 B3 B8 -56.9(2) . . . . ? C5 C1 B3 B8 130.59(15) . . . . ? B5 C1 B3 B8 24.22(13) . . . . ? Ru4 C1 B3 B8 -106.77(13) . . . . ? C2 C1 B3 B5 -81.14(16) . . . . ? C5 C1 B3 B5 106.37(16) . . . . ? Ru4 C1 B3 B5 -130.99(9) . . . . ? C2 C1 B3 B7 11.2(2) . . . . ? C5 C1 B3 B7 -161.25(14) . . . . ? B5 C1 B3 B7 92.38(14) . . . . ? Ru4 C1 B3 B7 -38.61(11) . . . . ? C2 C1 B3 Ru4 49.84(14) . . . . ? C5 C1 B3 Ru4 -122.64(15) . . . . ? B5 C1 B3 Ru4 130.99(9) . . . . ? C2 Ru4 B3 C1 -25.21(8) . . . . ? C41 Ru4 B3 C1 165.57(8) . . . . ? C42 Ru4 B3 C1 138.39(8) . . . . ? B7 Ru4 B3 C1 -142.77(12) . . . . ? C44 Ru4 B3 C1 72.02(9) . . . . ? B10 Ru4 B3 C1 -109.54(9) . . . . ? C40 Ru4 B3 C1 163.02(18) . . . . ? C43 Ru4 B3 C1 101.95(9) . . . . ? C45 Ru4 B3 C1 60.26(15) . . . . ? B6 Ru4 B3 C1 -63.30(9) . . . . ? C1 Ru4 B3 B8 109.83(14) . . . . ? C2 Ru4 B3 B8 84.62(12) . . . . ? C41 Ru4 B3 B8 -84.59(13) . . . . ? C42 Ru4 B3 B8 -111.78(12) . . . . ? B7 Ru4 B3 B8 -32.93(11) . . . . ? C44 Ru4 B3 B8 -178.15(10) . . . . ? B10 Ru4 B3 B8 0.29(12) . . . . ? C40 Ru4 B3 B8 -87.1(2) . . . . ? C43 Ru4 B3 B8 -148.21(12) . . . . ? C45 Ru4 B3 B8 170.09(11) . . . . ? B6 Ru4 B3 B8 46.53(12) . . . . ? C1 Ru4 B3 B5 45.21(10) . . . . ? C2 Ru4 B3 B5 20.00(10) . . . . ? C41 Ru4 B3 B5 -149.21(9) . . . . ? C42 Ru4 B3 B5 -176.40(10) . . . . ? B7 Ru4 B3 B5 -97.55(12) . . . . ? C44 Ru4 B3 B5 117.23(10) . . . . ? B10 Ru4 B3 B5 -64.33(11) . . . . ? C40 Ru4 B3 B5 -151.77(18) . . . . ? C43 Ru4 B3 B5 147.16(10) . . . . ? C45 Ru4 B3 B5 105.47(14) . . . . ? B6 Ru4 B3 B5 -18.09(11) . . . . ? C1 Ru4 B3 B7 142.77(12) . . . . ? C2 Ru4 B3 B7 117.55(9) . . . . ? C41 Ru4 B3 B7 -51.66(10) . . . . ? C42 Ru4 B3 B7 -78.85(8) . . . . ? C44 Ru4 B3 B7 -145.22(8) . . . . ? B10 Ru4 B3 B7 33.23(8) . . . . ? C40 Ru4 B3 B7 -54.2(2) . . . . ? C43 Ru4 B3 B7 -115.28(8) . . . . ? C45 Ru4 B3 B7 -156.97(11) . . . . ? B6 Ru4 B3 B7 79.46(9) . . . . ? C2 C1 B5 B11 38.51(18) . . . . ? C5 C1 B5 B11 154.12(15) . . . . ? B3 C1 B5 B11 -87.85(17) . . . . ? Ru4 C1 B5 B11 -33.82(19) . . . . ? C2 C1 B5 B8 104.46(13) . . . . ? C5 C1 B5 B8 -139.93(14) . . . . ? B3 C1 B5 B8 -21.90(12) . . . . ? Ru4 C1 B5 B8 32.12(15) . . . . ? C2 C1 B5 B3 126.36(13) . . . . ? C5 C1 B5 B3 -118.03(15) . . . . ? Ru4 C1 B5 B3 54.02(10) . . . . ? C2 C1 B5 B9 -0.25(12) . . . . ? C5 C1 B5 B9 115.35(14) . . . . ? B3 C1 B5 B9 -126.61(12) . . . . ? Ru4 C1 B5 B9 -72.59(11) . . . . ? C1 B3 B5 B11 120.08(14) . . . . ? B8 B3 B5 B11 -34.95(12) . . . . ? B7 B3 B5 B11 5.46(16) . . . . ? Ru4 B3 B5 B11 73.92(14) . . . . ? C1 B3 B5 B8 155.03(13) . . . . ? B7 B3 B5 B8 40.41(11) . . . . ? Ru4 B3 B5 B8 108.87(11) . . . . ? B8 B3 B5 C1 -155.03(13) . . . . ? B7 B3 B5 C1 -114.62(12) . . . . ? Ru4 B3 B5 C1 -46.16(9) . . . . ? C1 B3 B5 B9 59.70(13) . . . . ? B8 B3 B5 B9 -95.33(14) . . . . ? B7 B3 B5 B9 -54.92(15) . . . . ? Ru4 B3 B5 B9 13.53(15) . . . . ? C1 C2 B6 B12 56.4(2) . . . . ? C3 C2 B6 B12 -130.56(16) . . . . ? B9 C2 B6 B12 -24.39(12) . . . . ? Ru4 C2 B6 B12 106.22(13) . . . . ? C1 C2 B6 B10 -11.4(2) . . . . ? C3 C2 B6 B10 161.59(14) . . . . ? B9 C2 B6 B10 -92.24(15) . . . . ? Ru4 C2 B6 B10 38.37(11) . . . . ? C1 C2 B6 B9 80.81(16) . . . . ? C3 C2 B6 B9 -106.17(16) . . . . ? Ru4 C2 B6 B9 130.61(10) . . . . ? C1 C2 B6 Ru4 -49.80(14) . . . . ? C3 C2 B6 Ru4 123.22(15) . . . . ? B9 C2 B6 Ru4 -130.61(10) . . . . ? C1 Ru4 B6 C2 25.22(9) . . . . ? C41 Ru4 B6 C2 -161.01(9) . . . . ? C42 Ru4 B6 C2 -178.47(13) . . . . ? B7 Ru4 B6 C2 110.61(9) . . . . ? C44 Ru4 B6 C2 -63.34(11) . . . . ? B10 Ru4 B6 C2 142.63(12) . . . . ? C40 Ru4 B6 C2 -128.51(9) . . . . ? C43 Ru4 B6 C2 -51.2(2) . . . . ? C45 Ru4 B6 C2 -92.10(9) . . . . ? B3 Ru4 B6 C2 63.59(9) . . . . ? C1 Ru4 B6 B12 -84.27(11) . . . . ? C2 Ru4 B6 B12 -109.49(14) . . . . ? C41 Ru4 B6 B12 89.50(12) . . . . ? C42 Ru4 B6 B12 72.03(18) . . . . ? B7 Ru4 B6 B12 1.11(11) . . . . ? C44 Ru4 B6 B12 -172.84(9) . . . . ? B10 Ru4 B6 B12 33.13(10) . . . . ? C40 Ru4 B6 B12 122.00(11) . . . . ? C43 Ru4 B6 B12 -160.73(18) . . . . ? C45 Ru4 B6 B12 158.40(10) . . . . ? B3 Ru4 B6 B12 -45.91(11) . . . . ? C1 Ru4 B6 B10 -117.40(9) . . . . ? C2 Ru4 B6 B10 -142.63(12) . . . . ? C41 Ru4 B6 B10 56.36(10) . . . . ? C42 Ru4 B6 B10 38.90(17) . . . . ? B7 Ru4 B6 B10 -32.02(8) . . . . ? C44 Ru4 B6 B10 154.03(8) . . . . ? C40 Ru4 B6 B10 88.87(9) . . . . ? C43 Ru4 B6 B10 166.14(19) . . . . ? C45 Ru4 B6 B10 125.27(8) . . . . ? B3 Ru4 B6 B10 -79.04(9) . . . . ? C1 Ru4 B6 B9 -20.35(10) . . . . ? C2 Ru4 B6 B9 -45.58(10) . . . . ? C41 Ru4 B6 B9 153.41(10) . . . . ? C42 Ru4 B6 B9 135.95(13) . . . . ? B7 Ru4 B6 B9 65.03(11) . . . . ? C44 Ru4 B6 B9 -108.92(11) . . . . ? B10 Ru4 B6 B9 97.05(13) . . . . ? C40 Ru4 B6 B9 -174.08(10) . . . . ? C43 Ru4 B6 B9 -96.8(2) . . . . ? C45 Ru4 B6 B9 -137.68(10) . . . . ? B3 Ru4 B6 B9 18.01(11) . . . . ? C1 B3 B7 B13 -74.38(16) . . . . ? B8 B3 B7 B13 32.53(12) . . . . ? B5 B3 B7 B13 -7.96(15) . . . . ? Ru4 B3 B7 B13 -112.69(11) . . . . ? C1 B3 B7 B8 -106.91(15) . . . . ? B5 B3 B7 B8 -40.49(11) . . . . ? Ru4 B3 B7 B8 -145.22(10) . . . . ? C1 B3 B7 B10 -10.46(18) . . . . ? B8 B3 B7 B10 96.45(14) . . . . ? B5 B3 B7 B10 55.95(15) . . . . ? Ru4 B3 B7 B10 -48.78(10) . . . . ? C1 B3 B7 Ru4 38.31(11) . . . . ? B8 B3 B7 Ru4 145.22(10) . . . . ? B5 B3 B7 Ru4 104.73(10) . . . . ? C1 Ru4 B7 B13 75.26(12) . . . . ? C2 Ru4 B7 B13 39.12(12) . . . . ? C41 Ru4 B7 B13 -119.99(12) . . . . ? C42 Ru4 B7 B13 -156.96(12) . . . . ? C44 Ru4 B7 B13 171.10(10) . . . . ? B10 Ru4 B7 B13 -32.21(11) . . . . ? C40 Ru4 B7 B13 -96.46(12) . . . . ? C43 Ru4 B7 B13 174.62(10) . . . . ? C45 Ru4 B7 B13 -108.94(16) . . . . ? B3 Ru4 B7 B13 99.33(14) . . . . ? B6 Ru4 B7 B13 -0.01(12) . . . . ? C1 Ru4 B7 B8 8.17(11) . . . . ? C2 Ru4 B7 B8 -27.97(12) . . . . ? C41 Ru4 B7 B8 172.93(11) . . . . ? C42 Ru4 B7 B8 135.95(11) . . . . ? C44 Ru4 B7 B8 104.02(14) . . . . ? B10 Ru4 B7 B8 -99.30(13) . . . . ? C40 Ru4 B7 B8 -163.55(10) . . . . ? C43 Ru4 B7 B8 107.53(11) . . . . ? C45 Ru4 B7 B8 -176.02(12) . . . . ? B3 Ru4 B7 B8 32.24(10) . . . . ? B6 Ru4 B7 B8 -67.10(11) . . . . ? C1 Ru4 B7 B10 107.47(8) . . . . ? C2 Ru4 B7 B10 71.33(9) . . . . ? C41 Ru4 B7 B10 -87.78(8) . . . . ? C42 Ru4 B7 B10 -124.75(8) . . . . ? C44 Ru4 B7 B10 -156.69(10) . . . . ? C40 Ru4 B7 B10 -64.25(9) . . . . ? C43 Ru4 B7 B10 -153.17(8) . . . . ? C45 Ru4 B7 B10 -76.73(17) . . . . ? B3 Ru4 B7 B10 131.53(11) . . . . ? B6 Ru4 B7 B10 32.19(8) . . . . ? C1 Ru4 B7 B3 -24.07(8) . . . . ? C2 Ru4 B7 B3 -60.21(9) . . . . ? C41 Ru4 B7 B3 140.69(8) . . . . ? C42 Ru4 B7 B3 103.71(8) . . . . ? C44 Ru4 B7 B3 71.78(13) . . . . ? B10 Ru4 B7 B3 -131.53(11) . . . . ? C40 Ru4 B7 B3 164.21(7) . . . . ? C43 Ru4 B7 B3 75.30(9) . . . . ? C45 Ru4 B7 B3 151.74(14) . . . . ? B6 Ru4 B7 B3 -99.34(8) . . . . ? C1 B3 B8 B13 74.05(18) . . . . ? B5 B3 B8 B13 99.05(15) . . . . ? B7 B3 B8 B13 -34.13(13) . . . . ? Ru4 B3 B8 B13 0.89(18) . . . . ? C1 B3 B8 B5 -25.00(13) . . . . ? B7 B3 B8 B5 -133.18(12) . . . . ? Ru4 B3 B8 B5 -98.16(12) . . . . ? C1 B3 B8 B7 108.18(14) . . . . ? B5 B3 B8 B7 133.18(12) . . . . ? Ru4 B3 B8 B7 35.02(10) . . . . ? C1 B3 B8 B11 9.06(19) . . . . ? B5 B3 B8 B11 34.06(12) . . . . ? B7 B3 B8 B11 -99.12(13) . . . . ? Ru4 B3 B8 B11 -64.10(15) . . . . ? B11 B5 B8 B3 141.79(13) . . . . ? C1 B5 B8 B3 20.42(11) . . . . ? B9 B5 B8 B3 107.15(13) . . . . ? B11 B5 B8 B13 34.36(12) . . . . ? C1 B5 B8 B13 -87.01(14) . . . . ? B3 B5 B8 B13 -107.43(14) . . . . ? B9 B5 B8 B13 -0.28(16) . . . . ? B11 B5 B8 B7 98.30(14) . . . . ? C1 B5 B8 B7 -23.07(16) . . . . ? B3 B5 B8 B7 -43.49(12) . . . . ? B9 B5 B8 B7 63.66(15) . . . . ? C1 B5 B8 B11 -121.37(14) . . . . ? B3 B5 B8 B11 -141.79(13) . . . . ? B9 B5 B8 B11 -34.63(11) . . . . ? B13 B7 B8 B3 -143.58(13) . . . . ? B10 B7 B8 B3 -107.57(13) . . . . ? Ru4 B7 B8 B3 -35.51(10) . . . . ? B10 B7 B8 B13 36.01(12) . . . . ? B3 B7 B8 B13 143.58(13) . . . . ? Ru4 B7 B8 B13 108.07(12) . . . . ? B13 B7 B8 B5 -100.29(14) . . . . ? B10 B7 B8 B5 -64.27(15) . . . . ? B3 B7 B8 B5 43.29(12) . . . . ? Ru4 B7 B8 B5 7.78(16) . . . . ? B13 B7 B8 B11 -38.91(12) . . . . ? B10 B7 B8 B11 -2.90(16) . . . . ? B3 B7 B8 B11 104.67(14) . . . . ? Ru4 B7 B8 B11 69.15(14) . . . . ? C1 C2 B9 B11 -38.72(18) . . . . ? C3 C2 B9 B11 -154.54(15) . . . . ? B6 C2 B9 B11 87.99(16) . . . . ? Ru4 C2 B9 B11 33.02(19) . . . . ? C1 C2 B9 B12 -104.34(14) . . . . ? C3 C2 B9 B12 139.84(14) . . . . ? B6 C2 B9 B12 22.37(12) . . . . ? Ru4 C2 B9 B12 -32.59(15) . . . . ? C1 C2 B9 B6 -126.71(13) . . . . ? C3 C2 B9 B6 117.47(16) . . . . ? Ru4 C2 B9 B6 -54.96(11) . . . . ? C1 C2 B9 B5 -0.25(11) . . . . ? C3 C2 B9 B5 -116.07(14) . . . . ? B6 C2 B9 B5 126.46(12) . . . . ? Ru4 C2 B9 B5 71.50(11) . . . . ? C2 B6 B9 B11 -119.32(14) . . . . ? B12 B6 B9 B11 35.34(12) . . . . ? B10 B6 B9 B11 -5.20(15) . . . . ? Ru4 B6 B9 B11 -73.17(13) . . . . ? C2 B6 B9 B12 -154.66(13) . . . . ? B10 B6 B9 B12 -40.54(12) . . . . ? Ru4 B6 B9 B12 -108.51(12) . . . . ? B12 B6 B9 C2 154.66(13) . . . . ? B10 B6 B9 C2 114.12(12) . . . . ? Ru4 B6 B9 C2 46.15(9) . . . . ? C2 B6 B9 B5 -59.32(13) . . . . ? B12 B6 B9 B5 95.34(13) . . . . ? B10 B6 B9 B5 54.80(15) . . . . ? Ru4 B6 B9 B5 -13.17(15) . . . . ? B8 B5 B9 B11 36.81(12) . . . . ? C1 B5 B9 B11 141.88(13) . . . . ? B3 B5 B9 B11 98.24(14) . . . . ? B11 B5 B9 B12 -36.57(12) . . . . ? B8 B5 B9 B12 0.24(16) . . . . ? C1 B5 B9 B12 105.31(12) . . . . ? B3 B5 B9 B12 61.66(16) . . . . ? B11 B5 B9 C2 -141.68(13) . . . . ? B8 B5 B9 C2 -104.87(12) . . . . ? C1 B5 B9 C2 0.20(9) . . . . ? B3 B5 B9 C2 -43.44(13) . . . . ? B11 B5 B9 B6 -98.36(14) . . . . ? B8 B5 B9 B6 -61.55(16) . . . . ? C1 B5 B9 B6 43.52(13) . . . . ? B3 B5 B9 B6 -0.13(18) . . . . ? B8 B7 B10 B13 -35.99(12) . . . . ? B3 B7 B10 B13 -97.76(14) . . . . ? Ru4 B7 B10 B13 -146.65(10) . . . . ? B13 B7 B10 B12 34.90(12) . . . . ? B8 B7 B10 B12 -1.09(16) . . . . ? B3 B7 B10 B12 -62.87(16) . . . . ? Ru4 B7 B10 B12 -111.75(11) . . . . ? B13 B7 B10 B6 98.35(14) . . . . ? B8 B7 B10 B6 62.36(16) . . . . ? B3 B7 B10 B6 0.58(18) . . . . ? Ru4 B7 B10 B6 -48.30(11) . . . . ? B13 B7 B10 Ru4 146.65(10) . . . . ? B8 B7 B10 Ru4 110.66(11) . . . . ? B3 B7 B10 Ru4 48.88(10) . . . . ? C2 B6 B10 B13 74.70(17) . . . . ? B12 B6 B10 B13 -32.18(11) . . . . ? B9 B6 B10 B13 8.20(15) . . . . ? Ru4 B6 B10 B13 112.71(11) . . . . ? C2 B6 B10 B12 106.88(15) . . . . ? B9 B6 B10 B12 40.38(11) . . . . ? Ru4 B6 B10 B12 144.89(10) . . . . ? C2 B6 B10 B7 9.64(19) . . . . ? B12 B6 B10 B7 -97.24(14) . . . . ? B9 B6 B10 B7 -56.86(15) . . . . ? Ru4 B6 B10 B7 47.65(10) . . . . ? C2 B6 B10 Ru4 -38.01(12) . . . . ? B12 B6 B10 Ru4 -144.89(10) . . . . ? B9 B6 B10 Ru4 -104.50(10) . . . . ? C1 Ru4 B10 B13 -41.16(13) . . . . ? C2 Ru4 B10 B13 -77.14(12) . . . . ? C41 Ru4 B10 B13 125.00(12) . . . . ? C42 Ru4 B10 B13 95.19(12) . . . . ? B7 Ru4 B10 B13 32.40(11) . . . . ? C44 Ru4 B10 B13 174.51(14) . . . . ? C40 Ru4 B10 B13 161.84(12) . . . . ? C43 Ru4 B10 B13 86.21(16) . . . . ? C45 Ru4 B10 B13 -175.54(10) . . . . ? B3 Ru4 B10 B13 -1.46(12) . . . . ? B6 Ru4 B10 B13 -101.17(14) . . . . ? C1 Ru4 B10 B12 26.67(12) . . . . ? C2 Ru4 B10 B12 -9.31(11) . . . . ? C41 Ru4 B10 B12 -167.17(12) . . . . ? C42 Ru4 B10 B12 163.02(11) . . . . ? B7 Ru4 B10 B12 100.23(14) . . . . ? C44 Ru4 B10 B12 -117.66(18) . . . . ? C40 Ru4 B10 B12 -130.33(12) . . . . ? C43 Ru4 B10 B12 154.04(11) . . . . ? C45 Ru4 B10 B12 -107.71(12) . . . . ? B3 Ru4 B10 B12 66.37(12) . . . . ? B6 Ru4 B10 B12 -33.34(11) . . . . ? C1 Ru4 B10 B7 -73.56(9) . . . . ? C2 Ru4 B10 B7 -109.55(9) . . . . ? C41 Ru4 B10 B7 92.60(9) . . . . ? C42 Ru4 B10 B7 62.79(9) . . . . ? C44 Ru4 B10 B7 142.11(17) . . . . ? C40 Ru4 B10 B7 129.44(8) . . . . ? C43 Ru4 B10 B7 53.81(14) . . . . ? C45 Ru4 B10 B7 152.06(8) . . . . ? B3 Ru4 B10 B7 -33.86(8) . . . . ? B6 Ru4 B10 B7 -133.57(11) . . . . ? C1 Ru4 B10 B6 60.01(9) . . . . ? C2 Ru4 B10 B6 24.02(8) . . . . ? C41 Ru4 B10 B6 -133.84(8) . . . . ? C42 Ru4 B10 B6 -163.64(7) . . . . ? B7 Ru4 B10 B6 133.57(11) . . . . ? C44 Ru4 B10 B6 -84.32(19) . . . . ? C40 Ru4 B10 B6 -96.99(8) . . . . ? C43 Ru4 B10 B6 -172.62(10) . . . . ? C45 Ru4 B10 B6 -74.37(9) . . . . ? B3 Ru4 B10 B6 99.70(8) . . . . ? B8 B5 B11 B9 -138.91(13) . . . . ? C1 B5 B11 B9 -48.37(16) . . . . ? B3 B5 B11 B9 -105.26(13) . . . . ? B8 B5 B11 B13 -34.62(13) . . . . ? C1 B5 B11 B13 55.9(2) . . . . ? B3 B5 B11 B13 -0.96(17) . . . . ? B9 B5 B11 B13 104.29(14) . . . . ? B8 B5 B11 B12 -99.55(15) . . . . ? C1 B5 B11 B12 -9.0(2) . . . . ? B3 B5 B11 B12 -65.90(17) . . . . ? B9 B5 B11 B12 39.36(13) . . . . ? C1 B5 B11 B8 90.55(16) . . . . ? B3 B5 B11 B8 33.66(12) . . . . ? B9 B5 B11 B8 138.91(13) . . . . ? B12 B9 B11 B5 138.92(13) . . . . ? C2 B9 B11 B5 48.03(15) . . . . ? B6 B9 B11 B5 104.54(13) . . . . ? B12 B9 B11 B13 34.77(12) . . . . ? C2 B9 B11 B13 -56.11(19) . . . . ? B6 B9 B11 B13 0.40(17) . . . . ? B5 B9 B11 B13 -104.15(14) . . . . ? C2 B9 B11 B12 -90.89(16) . . . . ? B6 B9 B11 B12 -34.37(11) . . . . ? B5 B9 B11 B12 -138.92(13) . . . . ? B12 B9 B11 B8 99.54(15) . . . . ? C2 B9 B11 B8 8.7(2) . . . . ? B6 B9 B11 B8 65.17(17) . . . . ? B5 B9 B11 B8 -39.37(12) . . . . ? B3 B8 B11 B5 -35.84(13) . . . . ? B13 B8 B11 B5 -141.68(14) . . . . ? B7 B8 B11 B5 -102.62(14) . . . . ? B3 B8 B11 B9 6.49(19) . . . . ? B13 B8 B11 B9 -99.35(15) . . . . ? B5 B8 B11 B9 42.32(13) . . . . ? B7 B8 B11 B9 -60.29(17) . . . . ? B3 B8 B11 B13 105.84(14) . . . . ? B5 B8 B11 B13 141.68(14) . . . . ? B7 B8 B11 B13 39.06(12) . . . . ? B3 B8 B11 B12 72.70(16) . . . . ? B13 B8 B11 B12 -33.14(13) . . . . ? B5 B8 B11 B12 108.53(14) . . . . ? B7 B8 B11 B12 5.92(17) . . . . ? C2 B6 B12 B13 -74.35(17) . . . . ? B10 B6 B12 B13 33.16(12) . . . . ? B9 B6 B12 B13 -99.73(14) . . . . ? Ru4 B6 B12 B13 -1.97(15) . . . . ? C2 B6 B12 B11 -9.35(18) . . . . ? B10 B6 B12 B11 98.16(14) . . . . ? B9 B6 B12 B11 -34.73(12) . . . . ? Ru4 B6 B12 B11 63.03(14) . . . . ? C2 B6 B12 B9 25.38(13) . . . . ? B10 B6 B12 B9 132.89(12) . . . . ? Ru4 B6 B12 B9 97.75(11) . . . . ? C2 B6 B12 B10 -107.51(15) . . . . ? B9 B6 B12 B10 -132.89(12) . . . . ? Ru4 B6 B12 B10 -35.13(10) . . . . ? B5 B11 B12 B13 99.30(15) . . . . ? B9 B11 B12 B13 141.62(13) . . . . ? B8 B11 B12 B13 33.08(13) . . . . ? B5 B11 B12 B6 -5.95(19) . . . . ? B9 B11 B12 B6 36.37(12) . . . . ? B13 B11 B12 B6 -105.25(14) . . . . ? B8 B11 B12 B6 -72.17(16) . . . . ? B5 B11 B12 B9 -42.32(13) . . . . ? B13 B11 B12 B9 -141.62(13) . . . . ? B8 B11 B12 B9 -108.54(14) . . . . ? B5 B11 B12 B10 59.69(17) . . . . ? B9 B11 B12 B10 102.01(13) . . . . ? B13 B11 B12 B10 -39.61(12) . . . . ? B8 B11 B12 B10 -6.53(17) . . . . ? B11 B9 B12 B13 -34.55(12) . . . . ? C2 B9 B12 B13 85.95(15) . . . . ? B6 B9 B12 B13 106.61(14) . . . . ? B5 B9 B12 B13 -0.10(16) . . . . ? B11 B9 B12 B6 -141.16(13) . . . . ? C2 B9 B12 B6 -20.66(11) . . . . ? B5 B9 B12 B6 -106.71(12) . . . . ? C2 B9 B12 B11 120.50(14) . . . . ? B6 B9 B12 B11 141.16(13) . . . . ? B5 B9 B12 B11 34.44(11) . . . . ? B11 B9 B12 B10 -98.12(14) . . . . ? C2 B9 B12 B10 22.38(16) . . . . ? B6 B9 B12 B10 43.04(12) . . . . ? B5 B9 B12 B10 -63.68(15) . . . . ? B7 B10 B12 B13 -35.01(12) . . . . ? B6 B10 B12 B13 -144.36(12) . . . . ? Ru4 B10 B12 B13 -107.68(12) . . . . ? B13 B10 B12 B6 144.36(12) . . . . ? B7 B10 B12 B6 109.35(13) . . . . ? Ru4 B10 B12 B6 36.68(10) . . . . ? B13 B10 B12 B11 39.65(12) . . . . ? B7 B10 B12 B11 4.64(16) . . . . ? B6 B10 B12 B11 -104.71(13) . . . . ? Ru4 B10 B12 B11 -68.04(15) . . . . ? B13 B10 B12 B9 101.12(14) . . . . ? B7 B10 B12 B9 66.11(16) . . . . ? B6 B10 B12 B9 -43.24(12) . . . . ? Ru4 B10 B12 B9 -6.57(16) . . . . ? B3 B8 B13 B12 -66.99(17) . . . . ? B5 B8 B13 B12 0.23(18) . . . . ? B7 B8 B13 B12 -102.14(14) . . . . ? B11 B8 B13 B12 33.85(13) . . . . ? B3 B8 B13 B11 -100.83(15) . . . . ? B5 B8 B13 B11 -33.62(12) . . . . ? B7 B8 B13 B11 -135.99(13) . . . . ? B3 B8 B13 B10 -1.91(19) . . . . ? B5 B8 B13 B10 65.31(16) . . . . ? B7 B8 B13 B10 -37.06(12) . . . . ? B11 B8 B13 B10 98.93(14) . . . . ? B3 B8 B13 B7 35.15(13) . . . . ? B5 B8 B13 B7 102.37(14) . . . . ? B11 B8 B13 B7 135.99(13) . . . . ? B6 B12 B13 B8 67.10(16) . . . . ? B11 B12 B13 B8 -33.97(13) . . . . ? B9 B12 B13 B8 -0.07(17) . . . . ? B10 B12 B13 B8 101.03(14) . . . . ? B6 B12 B13 B11 101.07(13) . . . . ? B9 B12 B13 B11 33.90(12) . . . . ? B10 B12 B13 B11 135.00(13) . . . . ? B6 B12 B13 B10 -33.94(12) . . . . ? B11 B12 B13 B10 -135.00(13) . . . . ? B9 B12 B13 B10 -101.10(13) . . . . ? B6 B12 B13 B7 1.87(17) . . . . ? B11 B12 B13 B7 -99.19(14) . . . . ? B9 B12 B13 B7 -65.30(16) . . . . ? B10 B12 B13 B7 35.81(12) . . . . ? B5 B11 B13 B8 35.17(13) . . . . ? B9 B11 B13 B8 108.15(15) . . . . ? B12 B11 B13 B8 143.39(14) . . . . ? B5 B11 B13 B12 -108.22(14) . . . . ? B9 B11 B13 B12 -35.25(12) . . . . ? B8 B11 B13 B12 -143.39(14) . . . . ? B5 B11 B13 B10 -68.17(16) . . . . ? B9 B11 B13 B10 4.80(17) . . . . ? B12 B11 B13 B10 40.05(12) . . . . ? B8 B11 B13 B10 -103.34(14) . . . . ? B5 B11 B13 B7 -4.19(17) . . . . ? B9 B11 B13 B7 68.79(16) . . . . ? B12 B11 B13 B7 104.03(14) . . . . ? B8 B11 B13 B7 -39.36(12) . . . . ? B12 B10 B13 B8 -104.20(14) . . . . ? B7 B10 B13 B8 36.91(12) . . . . ? B6 B10 B13 B8 -72.40(16) . . . . ? Ru4 B10 B13 B8 2.24(17) . . . . ? B7 B10 B13 B12 141.11(13) . . . . ? B6 B10 B13 B12 31.80(11) . . . . ? Ru4 B10 B13 B12 106.44(12) . . . . ? B12 B10 B13 B11 -39.98(12) . . . . ? B7 B10 B13 B11 101.13(14) . . . . ? B6 B10 B13 B11 -8.18(16) . . . . ? Ru4 B10 B13 B11 66.46(15) . . . . ? B12 B10 B13 B7 -141.11(13) . . . . ? B6 B10 B13 B7 -109.31(13) . . . . ? Ru4 B10 B13 B7 -34.67(11) . . . . ? B10 B7 B13 B8 -139.41(13) . . . . ? B3 B7 B13 B8 -31.87(12) . . . . ? Ru4 B7 B13 B8 -104.76(13) . . . . ? B8 B7 B13 B12 103.71(14) . . . . ? B10 B7 B13 B12 -35.70(12) . . . . ? B3 B7 B13 B12 71.84(15) . . . . ? Ru4 B7 B13 B12 -1.05(17) . . . . ? B8 B7 B13 B11 39.48(12) . . . . ? B10 B7 B13 B11 -99.93(14) . . . . ? B3 B7 B13 B11 7.61(16) . . . . ? Ru4 B7 B13 B11 -65.28(15) . . . . ? B8 B7 B13 B10 139.41(13) . . . . ? B3 B7 B13 B10 107.54(12) . . . . ? Ru4 B7 B13 B10 34.65(11) . . . . ? C1 C2 C3 C4 -19.70(17) . . . . ? B6 C2 C3 C4 166.24(14) . . . . ? B9 C2 C3 C4 89.72(16) . . . . ? Ru4 C2 C3 C4 -98.64(14) . . . . ? C2 C3 C4 C5 31.43(17) . . . . ? C2 C1 C5 C4 19.51(17) . . . . ? B3 C1 C5 C4 -166.89(14) . . . . ? B5 C1 C5 C4 -89.96(16) . . . . ? Ru4 C1 C5 C4 98.82(14) . . . . ? C3 C4 C5 C1 -31.30(17) . . . . ? C1 Ru4 C40 C45 27.11(17) . . . . ? C2 Ru4 C40 C45 62.42(11) . . . . ? C41 Ru4 C40 C45 -130.32(13) . . . . ? C42 Ru4 C40 C45 -100.21(10) . . . . ? B7 Ru4 C40 C45 -171.59(9) . . . . ? C44 Ru4 C40 C45 -27.94(9) . . . . ? B10 Ru4 C40 C45 147.24(10) . . . . ? C43 Ru4 C40 C45 -63.82(9) . . . . ? B3 Ru4 C40 C45 -126.9(2) . . . . ? B6 Ru4 C40 C45 100.00(10) . . . . ? C1 Ru4 C40 C41 157.43(12) . . . . ? C2 Ru4 C40 C41 -167.27(9) . . . . ? C42 Ru4 C40 C41 30.11(9) . . . . ? B7 Ru4 C40 C41 -41.27(11) . . . . ? C44 Ru4 C40 C41 102.37(10) . . . . ? B10 Ru4 C40 C41 -82.44(10) . . . . ? C43 Ru4 C40 C41 66.50(10) . . . . ? C45 Ru4 C40 C41 130.32(13) . . . . ? B3 Ru4 C40 C41 3.4(3) . . . . ? B6 Ru4 C40 C41 -129.68(10) . . . . ? C1 Ru4 C40 C47 -92.58(18) . . . . ? C2 Ru4 C40 C47 -57.27(16) . . . . ? C41 Ru4 C40 C47 110.00(18) . . . . ? C42 Ru4 C40 C47 140.11(16) . . . . ? B7 Ru4 C40 C47 68.73(16) . . . . ? C44 Ru4 C40 C47 -147.63(16) . . . . ? B10 Ru4 C40 C47 27.56(15) . . . . ? C43 Ru4 C40 C47 176.50(15) . . . . ? C45 Ru4 C40 C47 -119.68(18) . . . . ? B3 Ru4 C40 C47 113.4(2) . . . . ? B6 Ru4 C40 C47 -19.68(15) . . . . ? C45 C40 C41 C42 -3.5(2) . . . . ? C47 C40 C41 C42 175.57(14) . . . . ? Ru4 C40 C41 C42 -58.51(13) . . . . ? C45 C40 C41 Ru4 55.00(13) . . . . ? C47 C40 C41 Ru4 -125.92(13) . . . . ? C1 Ru4 C41 C42 -10.7(3) . . . . ? C2 Ru4 C41 C42 158.74(13) . . . . ? B7 Ru4 C41 C42 -83.92(11) . . . . ? C44 Ru4 C41 C42 65.09(11) . . . . ? B10 Ru4 C41 C42 -130.61(11) . . . . ? C40 Ru4 C41 C42 130.38(15) . . . . ? C43 Ru4 C41 C42 28.53(10) . . . . ? C45 Ru4 C41 C42 100.89(11) . . . . ? B3 Ru4 C41 C42 -48.41(13) . . . . ? B6 Ru4 C41 C42 -168.14(9) . . . . ? C1 Ru4 C41 C40 -141.1(2) . . . . ? C2 Ru4 C41 C40 28.4(2) . . . . ? C42 Ru4 C41 C40 -130.38(15) . . . . ? B7 Ru4 C41 C40 145.69(10) . . . . ? C44 Ru4 C41 C40 -65.30(10) . . . . ? B10 Ru4 C41 C40 99.01(10) . . . . ? C43 Ru4 C41 C40 -101.85(10) . . . . ? C45 Ru4 C41 C40 -29.50(9) . . . . ? B3 Ru4 C41 C40 -178.79(9) . . . . ? B6 Ru4 C41 C40 61.48(12) . . . . ? C40 C41 C42 C43 3.8(2) . . . . ? Ru4 C41 C42 C43 -55.58(14) . . . . ? C40 C41 C42 Ru4 59.39(13) . . . . ? C1 Ru4 C42 C41 176.35(10) . . . . ? C2 Ru4 C42 C41 -151.10(18) . . . . ? B7 Ru4 C42 C41 95.74(11) . . . . ? C44 Ru4 C42 C41 -102.57(12) . . . . ? B10 Ru4 C42 C41 55.33(12) . . . . ? C40 Ru4 C42 C41 -30.14(11) . . . . ? C43 Ru4 C42 C41 -132.53(15) . . . . ? C45 Ru4 C42 C41 -66.58(11) . . . . ? B3 Ru4 C42 C41 142.38(11) . . . . ? B6 Ru4 C42 C41 25.5(2) . . . . ? C1 Ru4 C42 C43 -51.12(12) . . . . ? C2 Ru4 C42 C43 -18.6(2) . . . . ? C41 Ru4 C42 C43 132.53(15) . . . . ? B7 Ru4 C42 C43 -131.73(10) . . . . ? C44 Ru4 C42 C43 29.96(9) . . . . ? B10 Ru4 C42 C43 -172.13(9) . . . . ? C40 Ru4 C42 C43 102.39(10) . . . . ? C45 Ru4 C42 C43 65.96(10) . . . . ? B3 Ru4 C42 C43 -85.09(10) . . . . ? B6 Ru4 C42 C43 158.01(14) . . . . ? C41 C42 C43 C44 -1.1(2) . . . . ? Ru4 C42 C43 C44 -54.85(13) . . . . ? C41 C42 C43 C46 178.02(15) . . . . ? Ru4 C42 C43 C46 124.26(15) . . . . ? C41 C42 C43 Ru4 53.76(13) . . . . ? C1 Ru4 C43 C42 140.84(10) . . . . ? C2 Ru4 C43 C42 173.20(9) . . . . ? C41 Ru4 C43 C42 -29.04(10) . . . . ? B7 Ru4 C43 C42 53.06(11) . . . . ? C44 Ru4 C43 C42 -130.13(14) . . . . ? B10 Ru4 C43 C42 14.01(16) . . . . ? C40 Ru4 C43 C42 -66.23(10) . . . . ? C45 Ru4 C43 C42 -101.72(10) . . . . ? B3 Ru4 C43 C42 98.94(10) . . . . ? B6 Ru4 C43 C42 -146.36(19) . . . . ? C1 Ru4 C43 C44 -89.03(10) . . . . ? C2 Ru4 C43 C44 -56.67(11) . . . . ? C41 Ru4 C43 C44 101.10(10) . . . . ? C42 Ru4 C43 C44 130.13(14) . . . . ? B7 Ru4 C43 C44 -176.80(9) . . . . ? B10 Ru4 C43 C44 144.15(12) . . . . ? C40 Ru4 C43 C44 63.90(9) . . . . ? C45 Ru4 C43 C44 28.41(9) . . . . ? B3 Ru4 C43 C44 -130.93(10) . . . . ? B6 Ru4 C43 C44 -16.2(3) . . . . ? C1 Ru4 C43 C46 27.15(16) . . . . ? C2 Ru4 C43 C46 59.51(18) . . . . ? C41 Ru4 C43 C46 -142.72(17) . . . . ? C42 Ru4 C43 C46 -113.69(19) . . . . ? B7 Ru4 C43 C46 -60.63(17) . . . . ? C44 Ru4 C43 C46 116.18(19) . . . . ? B10 Ru4 C43 C46 -99.68(18) . . . . ? C40 Ru4 C43 C46 -179.92(16) . . . . ? C45 Ru4 C43 C46 144.59(17) . . . . ? B3 Ru4 C43 C46 -14.75(16) . . . . ? B6 Ru4 C43 C46 100.0(2) . . . . ? C42 C43 C44 C45 -1.8(2) . . . . ? C46 C43 C44 C45 179.11(15) . . . . ? Ru4 C43 C44 C45 -55.76(14) . . . . ? C42 C43 C44 Ru4 53.98(13) . . . . ? C46 C43 C44 Ru4 -125.13(15) . . . . ? C1 Ru4 C44 C45 -130.25(9) . . . . ? C2 Ru4 C44 C45 -90.80(10) . . . . ? C41 Ru4 C44 C45 65.26(9) . . . . ? C42 Ru4 C44 C45 102.42(10) . . . . ? B7 Ru4 C44 C45 138.03(12) . . . . ? B10 Ru4 C44 C45 14.1(2) . . . . ? C40 Ru4 C44 C45 28.03(9) . . . . ? C43 Ru4 C44 C45 132.49(14) . . . . ? B3 Ru4 C44 C45 -170.36(9) . . . . ? B6 Ru4 C44 C45 -53.19(11) . . . . ? C1 Ru4 C44 C43 97.25(9) . . . . ? C2 Ru4 C44 C43 136.71(9) . . . . ? C41 Ru4 C44 C43 -67.24(9) . . . . ? C42 Ru4 C44 C43 -30.07(9) . . . . ? B7 Ru4 C44 C43 5.54(16) . . . . ? B10 Ru4 C44 C43 -118.39(18) . . . . ? C40 Ru4 C44 C43 -104.47(10) . . . . ? C45 Ru4 C44 C43 -132.49(14) . . . . ? B3 Ru4 C44 C43 57.15(11) . . . . ? B6 Ru4 C44 C43 174.32(9) . . . . ? C43 C44 C45 C40 2.0(2) . . . . ? Ru4 C44 C45 C40 -53.47(13) . . . . ? C43 C44 C45 Ru4 55.49(14) . . . . ? C41 C40 C45 C44 0.6(2) . . . . ? C47 C40 C45 C44 -178.41(14) . . . . ? Ru4 C40 C45 C44 53.41(13) . . . . ? C41 C40 C45 Ru4 -52.78(12) . . . . ? C47 C40 C45 Ru4 128.18(15) . . . . ? C1 Ru4 C45 C44 60.06(11) . . . . ? C2 Ru4 C45 C44 96.98(10) . . . . ? C41 Ru4 C45 C44 -103.00(10) . . . . ? C42 Ru4 C45 C44 -65.47(9) . . . . ? B7 Ru4 C45 C44 -115.15(16) . . . . ? B10 Ru4 C45 C44 -174.13(9) . . . . ? C40 Ru4 C45 C44 -133.45(14) . . . . ? C43 Ru4 C45 C44 -28.75(9) . . . . ? B3 Ru4 C45 C44 18.17(17) . . . . ? B6 Ru4 C45 C44 139.62(9) . . . . ? C1 Ru4 C45 C40 -166.49(9) . . . . ? C2 Ru4 C45 C40 -129.57(9) . . . . ? C41 Ru4 C45 C40 30.44(9) . . . . ? C42 Ru4 C45 C40 67.98(9) . . . . ? B7 Ru4 C45 C40 18.29(19) . . . . ? C44 Ru4 C45 C40 133.45(14) . . . . ? B10 Ru4 C45 C40 -40.68(12) . . . . ? C43 Ru4 C45 C40 104.70(10) . . . . ? B3 Ru4 C45 C40 151.62(11) . . . . ? B6 Ru4 C45 C40 -86.93(10) . . . . ? C45 C40 C47 C49 -9.7(2) . . . . ? C41 C40 C47 C49 171.25(14) . . . . ? Ru4 C40 C47 C49 86.08(18) . . . . ? C45 C40 C47 C48 113.56(16) . . . . ? C41 C40 C47 C48 -65.46(18) . . . . ? Ru4 C40 C47 C48 -150.63(13) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.893 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.062 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 265427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H38 B10 P2 Pt, C5 H12' _chemical_formula_sum 'C26 H50 B10 P2 Pt' _chemical_formula_weight 727.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.063(4) _cell_length_b 18.802(6) _cell_length_c 9.882(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.350(9) _cell_angle_gamma 90.00 _cell_volume 2936.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2465 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 21.32 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 4.907 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27428 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7047 _reflns_number_gt 4908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^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 7047 _refine_ls_number_parameters 364 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt4 Pt 0.214392(14) 0.535076(12) 0.66997(2) 0.02104(9) Uani 1 1 d . . . P1 P 0.14057(11) 0.45471(8) 0.77908(18) 0.0248(4) Uani 1 1 d . . . P2 P 0.20784(10) 0.62744(8) 0.82030(17) 0.0228(3) Uani 1 1 d . . . B3 B 0.3098(5) 0.6006(5) 0.5697(8) 0.0308(17) Uani 1 1 d . . . H3 H 0.3284 0.6520 0.6239 0.037 Uiso 1 1 calc R . . B5 B 0.3789(5) 0.5381(4) 0.4763(8) 0.0266(16) Uani 1 1 d D . . H5 H 0.4447(18) 0.550(3) 0.468(7) 0.032 Uiso 1 1 d D . . B6 B 0.2450(5) 0.4390(4) 0.5418(7) 0.0259(16) Uani 1 1 d . . . H6 H 0.2233 0.3901 0.5901 0.031 Uiso 1 1 calc R . . B7 B 0.2034(4) 0.5926(4) 0.4615(7) 0.0262(16) Uani 1 1 d . . . H7 H 0.1584 0.6385 0.4542 0.031 Uiso 1 1 calc R . . B8 B 0.2958(4) 0.5947(4) 0.3868(7) 0.0259(15) Uani 1 1 d . . . H8 H 0.3129 0.6437 0.3335 0.031 Uiso 1 1 calc R . . B9 B 0.3375(5) 0.4455(4) 0.4538(9) 0.0334(19) Uani 1 1 d . . . H9 H 0.3805 0.4004 0.4392 0.040 Uiso 1 1 calc R . . B10 B 0.1670(5) 0.5022(4) 0.4491(7) 0.0273(16) Uani 1 1 d . . . H10 H 0.0976 0.4905 0.4360 0.033 Uiso 1 1 calc R . . B11 B 0.3137(5) 0.5093(4) 0.3243(8) 0.0242(15) Uani 1 1 d . . . H11 H 0.3424 0.5032 0.2298 0.029 Uiso 1 1 calc R . . B12 B 0.2328(5) 0.4517(4) 0.3605(8) 0.0272(16) Uani 1 1 d . . . H12 H 0.2061 0.4070 0.2909 0.033 Uiso 1 1 calc R . . B13 B 0.2079(5) 0.5413(4) 0.3133(8) 0.0278(17) Uani 1 1 d . . . H13 H 0.1666 0.5549 0.2128 0.033 Uiso 1 1 calc R . . C1 C 0.3601(5) 0.5381(4) 0.6510(8) 0.047(2) Uani 1 1 d . . . C2 C 0.3475(5) 0.4669(4) 0.6166(8) 0.050(2) Uani 1 1 d . . . C3 C 0.4065(6) 0.4206(5) 0.7202(9) 0.074(3) Uani 1 1 d U . . H3A H 0.3759 0.3790 0.7483 0.088 Uiso 1 1 calc R . . H3B H 0.4553 0.4036 0.6804 0.088 Uiso 1 1 calc R . . C4 C 0.4356(4) 0.4693(4) 0.8408(7) 0.0352(17) Uani 1 1 d U . . H4A H 0.4935 0.4570 0.8880 0.042 Uiso 1 1 calc R . . H4B H 0.3967 0.4671 0.9079 0.042 Uiso 1 1 calc R . . C5 C 0.4334(5) 0.5440(5) 0.7724(9) 0.059(3) Uani 1 1 d . . . H5A H 0.4228 0.5818 0.8369 0.070 Uiso 1 1 calc R . . H5B H 0.4873 0.5542 0.7406 0.070 Uiso 1 1 calc R . . C101 C 0.0800(5) 0.4846(4) 0.9048(7) 0.0361(17) Uani 1 1 d . . . H10D H 0.0531 0.4437 0.9408 0.054 Uiso 1 1 calc R . . H10E H 0.0364 0.5180 0.8617 0.054 Uiso 1 1 calc R . . H10F H 0.1176 0.5084 0.9804 0.054 Uiso 1 1 calc R . . C102 C 0.0592(4) 0.4075(3) 0.6631(6) 0.0297(15) Uani 1 1 d . . . H10A H 0.0305 0.3742 0.7156 0.045 Uiso 1 1 calc R . . H10B H 0.0850 0.3810 0.5958 0.045 Uiso 1 1 calc R . . H10C H 0.0181 0.4415 0.6150 0.045 Uiso 1 1 calc R . . C111 C 0.2039(4) 0.3842(3) 0.8747(6) 0.0275(14) Uani 1 1 d . . . C112 C 0.2556(4) 0.4007(3) 1.0001(6) 0.0292(15) Uani 1 1 d . . . H11A H 0.2575 0.4480 1.0343 0.035 Uiso 1 1 calc R . . C113 C 0.3045(4) 0.3475(4) 1.0752(7) 0.0352(16) Uani 1 1 d . . . H11C H 0.3402 0.3590 1.1598 0.042 Uiso 1 1 calc R . . C114 C 0.3011(4) 0.2792(3) 1.0276(7) 0.0328(16) Uani 1 1 d . . . H11B H 0.3331 0.2429 1.0803 0.039 Uiso 1 1 calc R . . C115 C 0.2506(4) 0.2628(3) 0.9017(7) 0.0332(16) Uani 1 1 d . . . H11E H 0.2486 0.2153 0.8684 0.040 Uiso 1 1 calc R . . C116 C 0.2042(4) 0.3140(3) 0.8258(7) 0.0321(16) Uani 1 1 d . . . H11D H 0.1715 0.3022 0.7387 0.039 Uiso 1 1 calc R . . C201 C 0.2717(4) 0.6187(4) 0.9915(7) 0.0363(17) Uani 1 1 d . . . H20D H 0.2638 0.6608 1.0463 0.054 Uiso 1 1 calc R . . H20E H 0.3315 0.6144 0.9840 0.054 Uiso 1 1 calc R . . H20F H 0.2541 0.5762 1.0363 0.054 Uiso 1 1 calc R . . C202 C 0.2402(5) 0.7144(3) 0.7692(8) 0.0387(18) Uani 1 1 d . . . H20A H 0.2348 0.7492 0.8409 0.058 Uiso 1 1 calc R . . H20B H 0.2042 0.7285 0.6827 0.058 Uiso 1 1 calc R . . H20C H 0.2993 0.7123 0.7566 0.058 Uiso 1 1 calc R . . C211 C 0.1018(4) 0.6493(3) 0.8459(6) 0.0233(13) Uani 1 1 d . . . C212 C 0.0846(4) 0.6712(3) 0.9724(7) 0.0296(15) Uani 1 1 d . . . H21D H 0.1291 0.6735 1.0498 0.036 Uiso 1 1 calc R . . C213 C 0.0025(4) 0.6901(3) 0.9865(7) 0.0318(15) Uani 1 1 d . . . H21A H -0.0091 0.7051 1.0730 0.038 Uiso 1 1 calc R . . C214 C -0.0611(4) 0.6864(3) 0.8734(8) 0.0364(17) Uani 1 1 d . . . H21E H -0.1172 0.6990 0.8823 0.044 Uiso 1 1 calc R . . C215 C -0.0452(4) 0.6650(4) 0.7483(8) 0.0370(17) Uani 1 1 d . . . H21C H -0.0902 0.6624 0.6716 0.044 Uiso 1 1 calc R . . C216 C 0.0361(4) 0.6471(3) 0.7326(7) 0.0274(14) Uani 1 1 d . . . H21B H 0.0471 0.6333 0.6450 0.033 Uiso 1 1 calc R . . C1S C 0.4811(5) 0.7463(5) -0.2077(14) 0.053(3) Uani 1 1 d DU . . C2S C 0.4806(6) 0.7559(9) -0.066(2) 0.150(7) Uani 1 1 d DU . . C3S C 0.4834(10) 0.6908(12) -0.075(2) 0.089(8) Uani 0.50 1 d PDU . . C4S C 0.4734(5) 0.7090(4) 0.0502(10) 0.0411(19) Uani 1 1 d DU . . C5S C 0.4583(10) 0.7231(10) 0.192(2) 0.167(8) Uani 1 1 d DU . . C6S C 0.5079(9) 0.7696(8) 0.161(3) 0.069(6) Uani 0.50 1 d PDU . . 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 Pt4 0.02623(13) 0.01920(13) 0.01810(14) -0.00134(10) 0.00508(9) 0.00188(10) P1 0.0335(9) 0.0185(8) 0.0229(9) -0.0004(6) 0.0066(7) 0.0007(6) P2 0.0281(8) 0.0192(8) 0.0221(9) -0.0027(6) 0.0074(7) -0.0009(6) B3 0.036(4) 0.036(4) 0.024(4) -0.006(3) 0.014(3) -0.001(3) B5 0.035(4) 0.023(4) 0.021(4) 0.005(3) 0.004(3) 0.001(3) B6 0.032(4) 0.026(4) 0.019(4) -0.007(3) 0.003(3) 0.006(3) B7 0.028(4) 0.025(4) 0.026(4) 0.002(3) 0.006(3) 0.009(3) B8 0.034(4) 0.024(4) 0.020(4) 0.003(3) 0.006(3) 0.000(3) B9 0.037(4) 0.032(4) 0.033(5) 0.008(3) 0.013(4) 0.010(3) B10 0.028(4) 0.029(4) 0.025(4) -0.003(3) 0.004(3) 0.006(3) B11 0.034(4) 0.018(3) 0.021(4) 0.000(3) 0.007(3) -0.002(3) B12 0.037(4) 0.026(4) 0.020(4) 0.001(3) 0.010(3) 0.003(3) B13 0.032(4) 0.032(4) 0.019(4) 0.008(3) 0.002(3) 0.003(3) C1 0.035(4) 0.063(6) 0.040(5) 0.015(4) 0.002(3) -0.021(4) C2 0.046(4) 0.054(5) 0.037(4) -0.017(4) -0.023(4) 0.028(4) C3 0.092(7) 0.057(6) 0.052(6) -0.020(4) -0.043(5) 0.045(5) C4 0.034(4) 0.043(4) 0.023(4) -0.004(3) -0.009(3) 0.004(3) C5 0.046(5) 0.076(7) 0.047(5) 0.021(4) -0.010(4) -0.024(4) C101 0.055(5) 0.022(3) 0.034(4) 0.007(3) 0.016(4) 0.000(3) C102 0.034(3) 0.027(4) 0.026(4) 0.005(3) 0.001(3) 0.001(3) C111 0.045(4) 0.018(3) 0.019(3) 0.001(3) 0.005(3) 0.005(3) C112 0.050(4) 0.016(3) 0.021(3) -0.001(3) 0.005(3) 0.000(3) C113 0.047(4) 0.031(4) 0.026(4) -0.002(3) 0.000(3) 0.000(3) C114 0.047(4) 0.022(3) 0.029(4) 0.007(3) 0.005(3) 0.004(3) C115 0.051(4) 0.014(3) 0.033(4) 0.000(3) 0.003(3) 0.004(3) C116 0.042(4) 0.020(3) 0.032(4) -0.002(3) -0.001(3) 0.003(3) C201 0.036(4) 0.040(4) 0.031(4) -0.007(3) 0.003(3) 0.008(3) C202 0.048(4) 0.023(4) 0.051(5) -0.008(3) 0.024(4) -0.006(3) C211 0.031(3) 0.014(3) 0.027(3) 0.001(2) 0.009(3) 0.000(2) C212 0.041(4) 0.016(3) 0.033(4) -0.003(3) 0.009(3) 0.000(3) C213 0.035(4) 0.024(4) 0.041(4) 0.000(3) 0.019(3) -0.002(3) C214 0.035(4) 0.022(3) 0.056(5) 0.011(3) 0.019(3) 0.008(3) C215 0.029(4) 0.038(4) 0.044(5) 0.014(3) 0.006(3) 0.008(3) C216 0.034(3) 0.022(3) 0.027(4) 0.001(3) 0.009(3) 0.000(3) C1S 0.014(4) 0.027(4) 0.109(9) -0.004(5) -0.012(5) -0.013(3) C2S 0.020(5) 0.129(13) 0.29(2) 0.076(15) 0.003(10) 0.017(6) C3S 0.026(9) 0.094(16) 0.15(2) -0.077(16) 0.014(11) -0.015(10) C4S 0.035(4) 0.022(4) 0.063(6) -0.002(4) 0.001(4) -0.008(3) C5S 0.104(12) 0.144(16) 0.28(2) 0.133(15) 0.094(14) 0.103(11) C6S 0.020(7) 0.024(8) 0.16(2) -0.034(10) 0.007(10) -0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt4 B10 2.265(7) . ? Pt4 P2 2.3001(17) . ? Pt4 P1 2.3046(18) . ? Pt4 B7 2.305(7) . ? Pt4 B6 2.310(7) . ? Pt4 B3 2.322(8) . ? Pt4 C1 2.381(8) . ? Pt4 C2 2.626(8) . ? P1 C101 1.800(7) . ? P1 C102 1.809(6) . ? P1 C111 1.827(6) . ? P2 C211 1.813(6) . ? P2 C202 1.814(7) . ? P2 C201 1.821(6) . ? B3 C1 1.563(11) . ? B3 B8 1.784(10) . ? B3 B7 1.852(10) . ? B3 B5 1.958(11) . ? B3 H3 1.1200 . ? B5 B11 1.755(10) . ? B5 C1 1.806(12) . ? B5 B8 1.810(10) . ? B5 B9 1.862(11) . ? B5 C2 2.055(12) . ? B5 H5 1.10(2) . ? B6 C2 1.758(10) . ? B6 B12 1.783(10) . ? B6 B10 1.847(10) . ? B6 B9 1.856(11) . ? B6 H6 1.1200 . ? B7 B13 1.766(11) . ? B7 B8 1.773(10) . ? B7 B10 1.794(11) . ? B7 H7 1.1200 . ? B8 B11 1.762(10) . ? B8 B13 1.777(10) . ? B8 H8 1.1200 . ? B9 C2 1.638(11) . ? B9 B11 1.746(10) . ? B9 B12 1.772(11) . ? B9 H9 1.1200 . ? B10 B13 1.759(11) . ? B10 B12 1.765(10) . ? B10 H10 1.1200 . ? B11 B12 1.778(11) . ? B11 B13 1.787(10) . ? B11 H11 1.1200 . ? B12 B13 1.776(10) . ? B12 H12 1.1200 . ? B13 H13 1.1200 . ? C1 C2 1.387(10) . ? C1 C5 1.527(10) . ? C2 C3 1.535(9) . ? C3 C4 1.508(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.557(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? C101 H10F 0.9800 . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C111 C112 1.396(8) . ? C111 C116 1.407(8) . ? C112 C113 1.400(9) . ? C112 H11A 0.9500 . ? C113 C114 1.365(9) . ? C113 H11C 0.9500 . ? C114 C115 1.393(9) . ? C114 H11B 0.9500 . ? C115 C116 1.357(8) . ? C115 H11E 0.9500 . ? C116 H11D 0.9500 . ? C201 H20D 0.9800 . ? C201 H20E 0.9800 . ? C201 H20F 0.9800 . ? C202 H20A 0.9800 . ? C202 H20B 0.9800 . ? C202 H20C 0.9800 . ? C211 C212 1.390(9) . ? C211 C216 1.394(8) . ? C212 C213 1.396(9) . ? C212 H21D 0.9500 . ? C213 C214 1.375(9) . ? C213 H21A 0.9500 . ? C214 C215 1.367(10) . ? C214 H21E 0.9500 . ? C215 C216 1.384(9) . ? C215 H21C 0.9500 . ? C216 H21B 0.9500 . ? C1S C2S 1.408(19) . ? C1S C6S 1.47(3) 4_575 ? C2S C3S 1.23(2) . ? C2S C4S 1.473(17) . ? C3S C4S 1.317(19) . ? C4S C5S 1.49(2) . ? C4S C6S 1.607(17) . ? C5S C6S 1.26(2) . ? C6S C1S 1.47(3) 4_576 ? 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 B10 Pt4 P2 141.46(19) . . ? B10 Pt4 P1 99.2(2) . . ? P2 Pt4 P1 96.07(6) . . ? B10 Pt4 B7 46.2(3) . . ? P2 Pt4 B7 102.60(19) . . ? P1 Pt4 B7 139.68(19) . . ? B10 Pt4 B6 47.6(2) . . ? P2 Pt4 B6 169.67(18) . . ? P1 Pt4 B6 85.5(2) . . ? B7 Pt4 B6 82.3(3) . . ? B10 Pt4 B3 82.3(3) . . ? P2 Pt4 B3 89.2(2) . . ? P1 Pt4 B3 169.0(2) . . ? B7 Pt4 B3 47.2(3) . . ? B6 Pt4 B3 87.6(3) . . ? B10 Pt4 C1 95.5(3) . . ? P2 Pt4 C1 101.1(2) . . ? P1 Pt4 C1 130.38(19) . . ? B7 Pt4 C1 80.6(3) . . ? B6 Pt4 C1 70.5(3) . . ? B3 Pt4 C1 38.8(3) . . ? B10 Pt4 C2 79.5(2) . . ? P2 Pt4 C2 129.17(17) . . ? P1 Pt4 C2 106.2(2) . . ? B7 Pt4 C2 89.1(3) . . ? B6 Pt4 C2 41.1(2) . . ? B3 Pt4 C2 63.2(3) . . ? C1 Pt4 C2 31.7(3) . . ? C101 P1 C102 99.9(3) . . ? C101 P1 C111 100.9(3) . . ? C102 P1 C111 104.1(3) . . ? C101 P1 Pt4 120.4(2) . . ? C102 P1 Pt4 113.5(2) . . ? C111 P1 Pt4 115.6(2) . . ? C211 P2 C202 99.1(3) . . ? C211 P2 C201 106.1(3) . . ? C202 P2 C201 101.4(4) . . ? C211 P2 Pt4 114.5(2) . . ? C202 P2 Pt4 116.9(2) . . ? C201 P2 Pt4 116.6(2) . . ? C1 B3 B8 115.7(6) . . ? C1 B3 B7 125.0(6) . . ? B8 B3 B7 58.3(4) . . ? C1 B3 B5 60.5(5) . . ? B8 B3 B5 57.6(4) . . ? B7 B3 B5 102.8(5) . . ? C1 B3 Pt4 72.6(4) . . ? B8 B3 Pt4 115.3(4) . . ? B7 B3 Pt4 65.9(3) . . ? B5 B3 Pt4 110.9(4) . . ? C1 B3 H3 109.5 . . ? B8 B3 H3 120.8 . . ? B7 B3 H3 119.0 . . ? B5 B3 H3 128.2 . . ? Pt4 B3 H3 113.2 . . ? B11 B5 C1 129.9(6) . . ? B11 B5 B8 59.2(4) . . ? C1 B5 B8 103.4(5) . . ? B11 B5 B9 57.6(4) . . ? C1 B5 B9 89.8(5) . . ? B8 B5 B9 106.0(5) . . ? B11 B5 B3 106.6(5) . . ? C1 B5 B3 48.9(4) . . ? B8 B5 B3 56.4(4) . . ? B9 B5 B3 113.4(5) . . ? B11 B5 C2 101.3(5) . . ? C1 B5 C2 41.5(3) . . ? B8 B5 C2 117.6(5) . . ? B9 B5 C2 49.2(4) . . ? B3 B5 C2 81.0(4) . . ? B11 B5 H5 116(4) . . ? C1 B5 H5 113(4) . . ? B8 B5 H5 118(3) . . ? B9 B5 H5 121(3) . . ? B3 B5 H5 123(3) . . ? C2 B5 H5 123(3) . . ? C2 B6 B12 108.0(6) . . ? C2 B6 B10 121.1(6) . . ? B12 B6 B10 58.2(4) . . ? C2 B6 B9 53.8(4) . . ? B12 B6 B9 58.2(4) . . ? B10 B6 B9 104.7(5) . . ? C2 B6 Pt4 79.1(4) . . ? B12 B6 Pt4 116.8(4) . . ? B10 B6 Pt4 64.9(3) . . ? B9 B6 Pt4 118.2(5) . . ? C2 B6 H6 113.9 . . ? B12 B6 H6 123.5 . . ? B10 B6 H6 120.2 . . ? B9 B6 H6 126.3 . . ? Pt4 B6 H6 107.1 . . ? B13 B7 B8 60.3(4) . . ? B13 B7 B10 59.2(4) . . ? B8 B7 B10 106.2(5) . . ? B13 B7 B3 110.6(5) . . ? B8 B7 B3 58.9(4) . . ? B10 B7 B3 111.8(5) . . ? B13 B7 Pt4 118.5(4) . . ? B8 B7 Pt4 116.6(4) . . ? B10 B7 Pt4 65.7(3) . . ? B3 B7 Pt4 66.9(3) . . ? B13 B7 H7 119.3 . . ? B8 B7 H7 122.2 . . ? B10 B7 H7 121.9 . . ? B3 B7 H7 119.5 . . ? Pt4 B7 H7 111.4 . . ? B11 B8 B7 109.1(5) . . ? B11 B8 B13 60.6(4) . . ? B7 B8 B13 59.7(4) . . ? B11 B8 B3 114.4(5) . . ? B7 B8 B3 62.8(4) . . ? B13 B8 B3 113.3(5) . . ? B11 B8 B5 58.9(4) . . ? B7 B8 B5 112.5(5) . . ? B13 B8 B5 109.3(5) . . ? B3 B8 B5 66.0(4) . . ? B11 B8 H8 121.0 . . ? B7 B8 H8 120.6 . . ? B13 B8 H8 121.1 . . ? B3 B8 H8 115.4 . . ? B5 B8 H8 119.5 . . ? C2 B9 B11 121.4(6) . . ? C2 B9 B12 114.3(6) . . ? B11 B9 B12 60.7(4) . . ? C2 B9 B6 60.1(5) . . ? B11 B9 B6 107.5(5) . . ? B12 B9 B6 58.8(4) . . ? C2 B9 B5 71.6(5) . . ? B11 B9 B5 58.1(4) . . ? B12 B9 B5 106.7(5) . . ? B6 B9 B5 107.7(5) . . ? C2 B9 H9 111.0 . . ? B11 B9 H9 119.1 . . ? B12 B9 H9 122.2 . . ? B6 B9 H9 125.0 . . ? B5 B9 H9 120.6 . . ? B13 B10 B12 60.5(4) . . ? B13 B10 B7 59.6(4) . . ? B12 B10 B7 109.1(5) . . ? B13 B10 B6 109.5(5) . . ? B12 B10 B6 59.1(4) . . ? B7 B10 B6 113.1(5) . . ? B13 B10 Pt4 120.9(5) . . ? B12 B10 Pt4 119.8(4) . . ? B7 B10 Pt4 68.1(3) . . ? B6 B10 Pt4 67.5(3) . . ? B13 B10 H10 119.6 . . ? B12 B10 H10 120.5 . . ? B7 B10 H10 120.0 . . ? B6 B10 H10 120.2 . . ? Pt4 B10 H10 108.7 . . ? B9 B11 B5 64.2(4) . . ? B9 B11 B8 113.4(6) . . ? B5 B11 B8 61.9(4) . . ? B9 B11 B12 60.4(4) . . ? B5 B11 B12 111.2(5) . . ? B8 B11 B12 108.3(5) . . ? B9 B11 B13 110.9(5) . . ? B5 B11 B13 111.3(5) . . ? B8 B11 B13 60.1(4) . . ? B12 B11 B13 59.8(4) . . ? B9 B11 H11 118.1 . . ? B5 B11 H11 118.3 . . ? B8 B11 H11 120.3 . . ? B12 B11 H11 122.0 . . ? B13 B11 H11 120.9 . . ? B10 B12 B9 112.0(5) . . ? B10 B12 B13 59.6(4) . . ? B9 B12 B13 110.3(5) . . ? B10 B12 B11 107.2(5) . . ? B9 B12 B11 58.9(4) . . ? B13 B12 B11 60.4(4) . . ? B10 B12 B6 62.7(4) . . ? B9 B12 B6 62.9(4) . . ? B13 B12 B6 111.7(5) . . ? B11 B12 B6 109.3(5) . . ? B10 B12 H12 120.7 . . ? B9 B12 H12 119.6 . . ? B13 B12 H12 120.4 . . ? B11 B12 H12 123.1 . . ? B6 B12 H12 118.6 . . ? B10 B13 B7 61.2(4) . . ? B10 B13 B12 59.9(4) . . ? B7 B13 B12 109.9(5) . . ? B10 B13 B8 107.6(5) . . ? B7 B13 B8 60.0(4) . . ? B12 B13 B8 107.7(5) . . ? B10 B13 B11 107.1(5) . . ? B7 B13 B11 108.3(5) . . ? B12 B13 B11 59.9(4) . . ? B8 B13 B11 59.3(4) . . ? B10 B13 H13 121.9 . . ? B7 B13 H13 120.4 . . ? B12 B13 H13 121.2 . . ? B8 B13 H13 122.4 . . ? B11 B13 H13 122.4 . . ? C2 C1 C5 108.7(7) . . ? C2 C1 B3 124.1(7) . . ? C5 C1 B3 127.1(7) . . ? C2 C1 B5 78.9(6) . . ? C5 C1 B5 120.8(6) . . ? B3 C1 B5 70.6(5) . . ? C2 C1 Pt4 83.9(5) . . ? C5 C1 Pt4 124.8(6) . . ? B3 C1 Pt4 68.6(4) . . ? B5 C1 Pt4 114.3(4) . . ? C1 C2 C3 109.7(6) . . ? C1 C2 B9 117.5(8) . . ? C3 C2 B9 117.1(6) . . ? C1 C2 B6 118.4(6) . . ? C3 C2 B6 122.1(8) . . ? B9 C2 B6 66.1(5) . . ? C1 C2 B5 59.6(5) . . ? C3 C2 B5 128.5(7) . . ? B9 C2 B5 59.3(5) . . ? B6 C2 B5 103.6(5) . . ? C1 C2 Pt4 64.4(4) . . ? C3 C2 Pt4 124.8(6) . . ? B9 C2 Pt4 112.2(4) . . ? B6 C2 Pt4 59.7(3) . . ? B5 C2 Pt4 97.2(3) . . ? C4 C3 C2 104.5(6) . . ? C4 C3 H3A 110.9 . . ? C2 C3 H3A 110.9 . . ? C4 C3 H3B 110.9 . . ? C2 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? C3 C4 C5 103.0(6) . . ? C3 C4 H4A 111.2 . . ? C5 C4 H4A 111.2 . . ? C3 C4 H4B 111.2 . . ? C5 C4 H4B 111.2 . . ? H4A C4 H4B 109.1 . . ? C1 C5 C4 103.2(6) . . ? C1 C5 H5A 111.1 . . ? C4 C5 H5A 111.1 . . ? C1 C5 H5B 111.1 . . ? C4 C5 H5B 111.1 . . ? H5A C5 H5B 109.1 . . ? P1 C101 H10D 109.5 . . ? P1 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? P1 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? P1 C102 H10A 109.5 . . ? P1 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? P1 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? C112 C111 C116 118.3(6) . . ? C112 C111 P1 119.0(5) . . ? C116 C111 P1 122.6(5) . . ? C111 C112 C113 120.0(6) . . ? C111 C112 H11A 120.0 . . ? C113 C112 H11A 120.0 . . ? C114 C113 C112 120.4(6) . . ? C114 C113 H11C 119.8 . . ? C112 C113 H11C 119.8 . . ? C113 C114 C115 119.7(6) . . ? C113 C114 H11B 120.1 . . ? C115 C114 H11B 120.1 . . ? C116 C115 C114 120.8(6) . . ? C116 C115 H11E 119.6 . . ? C114 C115 H11E 119.6 . . ? C115 C116 C111 120.7(6) . . ? C115 C116 H11D 119.6 . . ? C111 C116 H11D 119.6 . . ? P2 C201 H20D 109.5 . . ? P2 C201 H20E 109.5 . . ? H20D C201 H20E 109.5 . . ? P2 C201 H20F 109.5 . . ? H20D C201 H20F 109.5 . . ? H20E C201 H20F 109.5 . . ? P2 C202 H20A 109.5 . . ? P2 C202 H20B 109.5 . . ? H20A C202 H20B 109.5 . . ? P2 C202 H20C 109.5 . . ? H20A C202 H20C 109.5 . . ? H20B C202 H20C 109.5 . . ? C212 C211 C216 119.1(6) . . ? C212 C211 P2 122.4(5) . . ? C216 C211 P2 118.4(5) . . ? C211 C212 C213 120.6(6) . . ? C211 C212 H21D 119.7 . . ? C213 C212 H21D 119.7 . . ? C214 C213 C212 118.9(6) . . ? C214 C213 H21A 120.5 . . ? C212 C213 H21A 120.5 . . ? C215 C214 C213 121.1(6) . . ? C215 C214 H21E 119.4 . . ? C213 C214 H21E 119.4 . . ? C214 C215 C216 120.4(7) . . ? C214 C215 H21C 119.8 . . ? C216 C215 H21C 119.8 . . ? C215 C216 C211 119.8(6) . . ? C215 C216 H21B 120.1 . . ? C211 C216 H21B 120.1 . . ? C5S C1S C2S 137.1(15) 4_575 . ? C2S C1S C6S 162.9(10) . 4_575 ? C5S C1S C3S 161.8(12) 4_575 . ? C6S C1S C3S 126.8(11) 4_575 . ? C3S C2S C1S 78.5(17) . . ? C1S C2S C4S 135.5(15) . . ? C2S C3S C4S 70.6(14) . . ? C4S C3S C1S 125.8(16) . . ? C3S C4S C5S 174.8(14) . . ? C2S C4S C5S 132.8(12) . . ? C3S C4S C6S 137.3(14) . . ? C2S C4S C6S 92.4(12) . . ? C1S C5S C6S 75(2) 4_576 . ? C1S C5S C4S 145.2(19) 4_576 . ? C6S C5S C4S 71.0(14) . . ? C1S C6S C4S 109.8(12) 4_576 . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.816 _refine_diff_density_min -2.041 _refine_diff_density_rms 0.211 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 265428' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 B10 Ni P2, C H2 Cl2' _chemical_formula_sum 'C32 H42 B10 Cl2 Ni P2' _chemical_formula_weight 726.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4030(12) _cell_length_b 16.4829(12) _cell_length_c 20.251(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.788(4) _cell_angle_gamma 90.00 _cell_volume 3468.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1892 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 20.49 _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8022 _exptl_absorpt_correction_T_max 0.8659 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33869 _diffrn_reflns_av_R_equivalents 0.1126 _diffrn_reflns_av_sigmaI/netI 0.1110 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.91 _reflns_number_total 6670 _reflns_number_gt 4239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2671P] 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 6670 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni4 Ni 0.26712(5) 0.29913(3) 0.10996(2) 0.01772(17) Uani 1 1 d . . . P1 P 0.06872(10) 0.27551(7) 0.13615(5) 0.0190(3) Uani 1 1 d . . . P2 P 0.18743(10) 0.40508(6) 0.05476(5) 0.0182(3) Uani 1 1 d . . . C1 C 0.3284(4) 0.1841(2) 0.0761(2) 0.0207(9) Uani 1 1 d . . . C2 C 0.4231(4) 0.2294(2) 0.0420(2) 0.0204(9) Uani 1 1 d . . . B3 B 0.3234(5) 0.1808(3) 0.1522(2) 0.0215(11) Uani 1 1 d . . . H3C H 0.259(4) 0.133(3) 0.171(2) 0.028(12) Uiso 1 1 d . . . B5 B 0.4898(5) 0.1568(3) 0.1097(2) 0.0214(11) Uani 1 1 d . . . H5C H 0.513(4) 0.096(3) 0.091(2) 0.031(12) Uiso 1 1 d . . . B6 B 0.4549(5) 0.3272(3) 0.0733(2) 0.0206(11) Uani 1 1 d . . . H6C H 0.459(4) 0.374(2) 0.0307(19) 0.019(10) Uiso 1 1 d . . . B7 B 0.3681(5) 0.2684(3) 0.2038(2) 0.0210(11) Uani 1 1 d . . . H7C H 0.316(4) 0.272(2) 0.2487(19) 0.019(10) Uiso 1 1 d . . . B8 B 0.4764(5) 0.1868(3) 0.1991(2) 0.0234(11) Uani 1 1 d . . . H8C H 0.488(4) 0.134(3) 0.233(2) 0.040(13) Uiso 1 1 d . . . B9 B 0.5728(5) 0.2460(3) 0.0719(2) 0.0231(11) Uani 1 1 d . . . H9C H 0.645(4) 0.237(2) 0.0381(19) 0.018(10) Uiso 1 1 d . . . B10 B 0.4320(5) 0.3506(3) 0.1602(2) 0.0205(11) Uani 1 1 d . . . H10C H 0.423(5) 0.413(3) 0.178(2) 0.044(14) Uiso 1 1 d . . . B11 B 0.6075(5) 0.2176(3) 0.1549(3) 0.0240(11) Uani 1 1 d . . . H11C H 0.708(4) 0.192(2) 0.1619(17) 0.011(10) Uiso 1 1 d . . . B12 B 0.5864(5) 0.3224(3) 0.1328(2) 0.0219(11) Uani 1 1 d . . . H12C H 0.674(4) 0.362(2) 0.1253(18) 0.013(10) Uiso 1 1 d . . . B13 B 0.5366(5) 0.2855(3) 0.2097(2) 0.0211(11) Uani 1 1 d . . . H13C H 0.590(3) 0.309(2) 0.2560(17) 0.008(9) Uiso 1 1 d . . . C3 C 0.4109(4) 0.2082(3) -0.0314(2) 0.0259(10) Uani 1 1 d . . . H3A H 0.4968 0.2015 -0.0496 0.031 Uiso 1 1 calc R . . H3B H 0.3633 0.2510 -0.0566 0.031 Uiso 1 1 calc R . . C4 C 0.3359(5) 0.1276(3) -0.0341(2) 0.0324(11) Uani 1 1 d . . . H14C H 0.2795 0.1245 -0.0748 0.039 Uiso 1 1 calc R . . H4B H 0.3957 0.0809 -0.0331 0.039 Uiso 1 1 calc R . . C5 C 0.2557(4) 0.1281(3) 0.0275(2) 0.0258(10) Uani 1 1 d . . . H5A H 0.1679 0.1490 0.0167 0.031 Uiso 1 1 calc R . . H5B H 0.2490 0.0727 0.0460 0.031 Uiso 1 1 calc R . . C101 C -0.0378(4) 0.3170(2) 0.06981(19) 0.0207(9) Uani 1 1 d . . . H10A H -0.0324 0.2843 0.0290 0.025 Uiso 1 1 calc R . . H10B H -0.1282 0.3172 0.0830 0.025 Uiso 1 1 calc R . . C102 C 0.0087(4) 0.4029(2) 0.0586(2) 0.0210(9) Uani 1 1 d . . . H10E H -0.0178 0.4383 0.0950 0.025 Uiso 1 1 calc R . . H10D H -0.0311 0.4242 0.0167 0.025 Uiso 1 1 calc R . . C111 C 0.0243(4) 0.3372(2) 0.20649(19) 0.0195(9) Uani 1 1 d . . . C112 C -0.0940(4) 0.3259(3) 0.2340(2) 0.0248(10) Uani 1 1 d . . . H112 H -0.1474 0.2819 0.2198 0.030 Uiso 1 1 calc R . . C113 C -0.1344(4) 0.3785(3) 0.2821(2) 0.0260(10) Uani 1 1 d . . . H113 H -0.2151 0.3702 0.3011 0.031 Uiso 1 1 calc R . . C114 C -0.0572(4) 0.4430(3) 0.3026(2) 0.0300(11) Uani 1 1 d . . . H114 H -0.0859 0.4796 0.3350 0.036 Uiso 1 1 calc R . . C115 C 0.0622(4) 0.4548(3) 0.2759(2) 0.0251(10) Uani 1 1 d . . . H115 H 0.1153 0.4988 0.2904 0.030 Uiso 1 1 calc R . . C116 C 0.1026(4) 0.4019(2) 0.22851(19) 0.0212(9) Uani 1 1 d . . . H116 H 0.1845 0.4094 0.2105 0.025 Uiso 1 1 calc R . . C121 C 0.0061(4) 0.1752(2) 0.1529(2) 0.0199(9) Uani 1 1 d . . . C122 C 0.0281(4) 0.1418(3) 0.2155(2) 0.0249(10) Uani 1 1 d . . . H122 H 0.0732 0.1720 0.2492 0.030 Uiso 1 1 calc R . . C123 C -0.0164(4) 0.0638(3) 0.2289(2) 0.0328(11) Uani 1 1 d . . . H123 H -0.0018 0.0411 0.2718 0.039 Uiso 1 1 calc R . . C124 C -0.0814(5) 0.0197(3) 0.1802(3) 0.0398(13) Uani 1 1 d . . . H124 H -0.1109 -0.0334 0.1896 0.048 Uiso 1 1 calc R . . C125 C -0.1042(5) 0.0518(3) 0.1177(3) 0.0351(12) Uani 1 1 d . . . H125 H -0.1495 0.0211 0.0844 0.042 Uiso 1 1 calc R . . C126 C -0.0604(4) 0.1296(3) 0.1038(2) 0.0270(10) Uani 1 1 d . . . H126 H -0.0757 0.1519 0.0609 0.032 Uiso 1 1 calc R . . C211 C 0.2349(4) 0.5074(2) 0.08235(19) 0.0212(9) Uani 1 1 d . . . C212 C 0.3626(4) 0.5330(3) 0.0763(2) 0.0236(10) Uani 1 1 d . . . H212 H 0.4235 0.4969 0.0588 0.028 Uiso 1 1 calc R . . C213 C 0.4008(4) 0.6102(2) 0.0954(2) 0.0222(10) Uani 1 1 d . . . H213 H 0.4872 0.6268 0.0903 0.027 Uiso 1 1 calc R . . C214 C 0.3139(4) 0.6638(3) 0.1221(2) 0.0265(10) Uani 1 1 d . . . H214 H 0.3399 0.7172 0.1344 0.032 Uiso 1 1 calc R . . C215 C 0.1885(4) 0.6382(3) 0.1305(2) 0.0278(11) Uani 1 1 d . . . H215 H 0.1290 0.6733 0.1503 0.033 Uiso 1 1 calc R . . C216 C 0.1504(4) 0.5612(2) 0.1100(2) 0.0237(10) Uani 1 1 d . . . H216 H 0.0639 0.5448 0.1150 0.028 Uiso 1 1 calc R . . C221 C 0.2066(4) 0.4050(2) -0.03430(19) 0.0182(9) Uani 1 1 d . . . C222 C 0.2565(4) 0.4690(3) -0.0700(2) 0.0237(10) Uani 1 1 d . . . H222 H 0.2876 0.5163 -0.0477 0.028 Uiso 1 1 calc R . . C223 C 0.2608(4) 0.4634(3) -0.1388(2) 0.0249(10) Uani 1 1 d . . . H223 H 0.2959 0.5070 -0.1628 0.030 Uiso 1 1 calc R . . C224 C 0.2151(4) 0.3958(3) -0.1723(2) 0.0232(10) Uani 1 1 d . . . H224 H 0.2187 0.3930 -0.2190 0.028 Uiso 1 1 calc R . . C225 C 0.1639(4) 0.3321(3) -0.1378(2) 0.0264(10) Uani 1 1 d . . . H225 H 0.1307 0.2858 -0.1607 0.032 Uiso 1 1 calc R . . C226 C 0.1615(4) 0.3365(3) -0.0692(2) 0.0228(10) Uani 1 1 d . . . H226 H 0.1284 0.2920 -0.0455 0.027 Uiso 1 1 calc R . . C1S C 0.1662(5) 0.8970(3) 0.1222(2) 0.0390(13) Uani 1 1 d . . . H1S1 H 0.2032 0.8682 0.1616 0.047 Uiso 1 1 calc R . . H1S2 H 0.1441 0.9528 0.1357 0.047 Uiso 1 1 calc R . . Cl1 Cl 0.02564(12) 0.84668(7) 0.09277(6) 0.0397(3) Uani 1 1 d . . . Cl2 Cl 0.28168(12) 0.90119(8) 0.06128(7) 0.0427(3) Uani 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 Ni4 0.0180(3) 0.0158(3) 0.0194(3) 0.0009(2) 0.0012(2) 0.0000(2) P1 0.0196(6) 0.0179(6) 0.0197(6) 0.0003(4) 0.0013(4) -0.0006(5) P2 0.0199(6) 0.0159(6) 0.0188(5) 0.0015(4) 0.0016(4) 0.0002(5) C1 0.021(2) 0.015(2) 0.026(2) 0.0004(17) -0.0018(18) 0.0026(18) C2 0.021(2) 0.018(2) 0.023(2) 0.0006(17) 0.0026(17) 0.0030(18) B3 0.018(3) 0.017(3) 0.029(3) 0.001(2) 0.000(2) 0.000(2) B5 0.025(3) 0.013(3) 0.026(3) 0.004(2) 0.002(2) 0.001(2) B6 0.023(3) 0.021(3) 0.018(2) 0.002(2) 0.004(2) -0.002(2) B7 0.021(3) 0.016(3) 0.025(3) 0.001(2) -0.004(2) 0.001(2) B8 0.025(3) 0.021(3) 0.024(3) -0.001(2) -0.001(2) -0.001(2) B9 0.021(3) 0.019(3) 0.029(3) 0.001(2) 0.002(2) 0.000(2) B10 0.023(3) 0.020(3) 0.018(2) 0.002(2) -0.003(2) 0.004(2) B11 0.019(3) 0.020(3) 0.032(3) 0.000(2) 0.000(2) -0.003(2) B12 0.021(3) 0.014(3) 0.030(3) 0.004(2) -0.001(2) -0.004(2) B13 0.017(2) 0.021(3) 0.025(3) 0.000(2) -0.002(2) 0.000(2) C3 0.027(2) 0.030(3) 0.021(2) -0.0024(19) 0.0035(18) -0.002(2) C4 0.034(3) 0.031(3) 0.033(3) -0.009(2) 0.003(2) -0.005(2) C5 0.027(2) 0.021(2) 0.029(2) -0.0048(19) -0.0009(19) -0.002(2) C101 0.021(2) 0.020(2) 0.021(2) -0.0032(17) 0.0036(17) 0.0029(18) C102 0.019(2) 0.022(2) 0.023(2) 0.0036(18) 0.0026(17) -0.0014(18) C111 0.020(2) 0.015(2) 0.023(2) 0.0019(17) -0.0029(17) 0.0054(18) C112 0.025(2) 0.024(2) 0.026(2) -0.0011(19) 0.0009(19) -0.004(2) C113 0.022(2) 0.029(3) 0.028(2) -0.001(2) 0.0078(19) 0.002(2) C114 0.027(3) 0.037(3) 0.027(2) -0.007(2) 0.0029(19) 0.005(2) C115 0.027(3) 0.023(3) 0.025(2) -0.0038(19) -0.0027(19) 0.000(2) C116 0.022(2) 0.019(2) 0.022(2) 0.0023(17) -0.0017(18) -0.0011(19) C121 0.017(2) 0.018(2) 0.025(2) -0.0006(17) 0.0059(17) 0.0003(18) C122 0.026(2) 0.023(3) 0.026(2) 0.0022(18) 0.0070(19) 0.002(2) C123 0.034(3) 0.025(3) 0.041(3) 0.007(2) 0.013(2) 0.003(2) C124 0.041(3) 0.024(3) 0.057(4) -0.003(2) 0.022(3) -0.006(2) C125 0.032(3) 0.024(3) 0.050(3) -0.008(2) 0.007(2) -0.006(2) C126 0.026(2) 0.021(2) 0.034(3) -0.0028(19) 0.003(2) 0.001(2) C211 0.027(2) 0.020(2) 0.016(2) -0.0001(17) -0.0051(18) 0.0005(19) C212 0.026(2) 0.021(2) 0.024(2) -0.0013(18) 0.0033(18) 0.0040(19) C213 0.025(2) 0.017(2) 0.024(2) -0.0020(18) 0.0022(18) -0.0050(19) C214 0.035(3) 0.015(2) 0.029(2) -0.0017(18) 0.002(2) -0.003(2) C215 0.031(3) 0.021(3) 0.031(3) -0.0059(19) 0.003(2) 0.004(2) C216 0.028(2) 0.018(2) 0.026(2) 0.0023(18) 0.0018(18) 0.000(2) C221 0.017(2) 0.018(2) 0.020(2) 0.0022(17) 0.0008(16) 0.0026(18) C222 0.022(2) 0.020(2) 0.029(2) -0.0035(19) 0.0033(18) 0.0004(19) C223 0.029(3) 0.024(3) 0.022(2) 0.0046(18) 0.0058(19) -0.003(2) C224 0.025(2) 0.027(3) 0.018(2) 0.0017(18) -0.0004(18) -0.001(2) C225 0.028(3) 0.024(3) 0.027(2) -0.0047(19) 0.0013(19) -0.002(2) C226 0.021(2) 0.020(2) 0.028(2) -0.0012(18) 0.0016(18) -0.0031(19) C1S 0.039(3) 0.038(3) 0.039(3) -0.002(2) -0.002(2) -0.002(2) Cl1 0.0441(8) 0.0365(8) 0.0381(7) -0.0061(5) -0.0014(6) -0.0084(6) Cl2 0.0379(7) 0.0393(8) 0.0513(8) -0.0064(6) 0.0064(6) 0.0058(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni4 C1 2.125(4) . ? Ni4 B10 2.128(5) . ? Ni4 B6 2.173(5) . ? Ni4 B7 2.186(5) . ? Ni4 P1 2.1907(12) . ? Ni4 B3 2.197(5) . ? Ni4 P2 2.2128(12) . ? Ni4 C2 2.463(4) . ? P1 C121 1.815(4) . ? P1 C111 1.828(4) . ? P1 C101 1.832(4) . ? P2 C221 1.824(4) . ? P2 C211 1.836(4) . ? P2 C102 1.865(4) . ? C1 C2 1.439(6) . ? C1 C5 1.524(6) . ? C1 B3 1.545(6) . ? C1 B5 1.837(6) . ? C2 C3 1.526(5) . ? C2 B9 1.665(6) . ? C2 B6 1.757(6) . ? C2 B5 1.923(6) . ? B3 B8 1.816(7) . ? B3 B7 1.829(7) . ? B3 B5 2.009(7) . ? B3 H3C 1.11(4) . ? B5 B11 1.798(7) . ? B5 B9 1.886(7) . ? B5 B8 1.887(7) . ? B5 H5C 1.10(4) . ? B6 B12 1.780(7) . ? B6 B9 1.816(7) . ? B6 B10 1.828(7) . ? B6 H6C 1.16(4) . ? B7 B8 1.760(7) . ? B7 B10 1.765(7) . ? B7 B13 1.773(7) . ? B7 H7C 1.08(4) . ? B8 B11 1.741(7) . ? B8 B13 1.752(7) . ? B8 H8C 1.11(5) . ? B9 B12 1.763(7) . ? B9 B11 1.766(7) . ? B9 H9C 1.05(4) . ? B10 B12 1.785(7) . ? B10 B13 1.800(6) . ? B10 H10C 1.10(5) . ? B11 B13 1.763(7) . ? B11 B12 1.796(7) . ? B11 H11C 1.13(4) . ? B12 B13 1.774(7) . ? B12 H12C 1.14(4) . ? B13 H13C 1.13(3) . ? C3 C4 1.539(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.533(6) . ? C4 H14C 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C101 C102 1.517(5) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10E 0.9900 . ? C102 H10D 0.9900 . ? C111 C112 1.389(6) . ? C111 C116 1.402(6) . ? C112 C113 1.384(6) . ? C112 H112 0.9500 . ? C113 C114 1.384(6) . ? C113 H113 0.9500 . ? C114 C115 1.391(6) . ? C114 H114 0.9500 . ? C115 C116 1.377(6) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.392(6) . ? C121 C126 1.401(6) . ? C122 C123 1.398(6) . ? C122 H122 0.9500 . ? C123 C124 1.376(7) . ? C123 H123 0.9500 . ? C124 C125 1.380(7) . ? C124 H124 0.9500 . ? C125 C126 1.394(6) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C211 C216 1.385(6) . ? C211 C212 1.406(6) . ? C212 C213 1.382(6) . ? C212 H212 0.9500 . ? C213 C214 1.393(6) . ? C213 H213 0.9500 . ? C214 C215 1.389(6) . ? C214 H214 0.9500 . ? C215 C216 1.388(6) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.394(6) . ? C221 C226 1.400(5) . ? C222 C223 1.399(6) . ? C222 H222 0.9500 . ? C223 C224 1.377(6) . ? C223 H223 0.9500 . ? C224 C225 1.381(6) . ? C224 H224 0.9500 . ? C225 C226 1.394(6) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C1S Cl1 1.759(5) . ? C1S Cl2 1.765(5) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni4 B10 105.23(18) . . ? C1 Ni4 B6 77.91(18) . . ? B10 Ni4 B6 50.29(18) . . ? C1 Ni4 B7 86.27(17) . . ? B10 Ni4 B7 48.29(18) . . ? B6 Ni4 B7 86.79(18) . . ? C1 Ni4 P1 102.75(12) . . ? B10 Ni4 P1 134.62(14) . . ? B6 Ni4 P1 173.58(13) . . ? B7 Ni4 P1 99.62(14) . . ? C1 Ni4 B3 41.86(17) . . ? B10 Ni4 B3 88.55(18) . . ? B6 Ni4 B3 95.42(19) . . ? B7 Ni4 B3 49.34(18) . . ? P1 Ni4 B3 89.12(14) . . ? C1 Ni4 P2 130.69(12) . . ? B10 Ni4 P2 101.54(13) . . ? B6 Ni4 P2 88.88(13) . . ? B7 Ni4 P2 140.76(13) . . ? P1 Ni4 P2 85.89(4) . . ? B3 Ni4 P2 169.48(13) . . ? C1 Ni4 C2 35.59(14) . . ? B10 Ni4 C2 85.14(17) . . ? B6 Ni4 C2 44.00(16) . . ? B7 Ni4 C2 94.34(16) . . ? P1 Ni4 C2 134.95(10) . . ? B3 Ni4 C2 68.45(16) . . ? P2 Ni4 C2 109.08(10) . . ? C121 P1 C111 104.77(19) . . ? C121 P1 C101 105.50(19) . . ? C111 P1 C101 101.34(18) . . ? C121 P1 Ni4 123.93(14) . . ? C111 P1 Ni4 111.50(14) . . ? C101 P1 Ni4 107.43(14) . . ? C221 P2 C211 105.13(18) . . ? C221 P2 C102 101.44(18) . . ? C211 P2 C102 104.97(19) . . ? C221 P2 Ni4 116.26(13) . . ? C211 P2 Ni4 118.85(13) . . ? C102 P2 Ni4 108.29(13) . . ? C2 C1 C5 109.6(4) . . ? C2 C1 B3 123.6(4) . . ? C5 C1 B3 125.7(4) . . ? C2 C1 B5 70.7(3) . . ? C5 C1 B5 120.5(3) . . ? B3 C1 B5 72.3(3) . . ? C2 C1 Ni4 85.1(2) . . ? C5 C1 Ni4 127.0(3) . . ? B3 C1 Ni4 71.6(2) . . ? B5 C1 Ni4 112.5(3) . . ? C1 C2 C3 108.7(4) . . ? C1 C2 B9 124.1(4) . . ? C3 C2 B9 115.1(3) . . ? C1 C2 B6 115.1(3) . . ? C3 C2 B6 124.5(3) . . ? B9 C2 B6 64.0(3) . . ? C1 C2 B5 64.3(3) . . ? C3 C2 B5 124.2(3) . . ? B9 C2 B5 62.9(3) . . ? B6 C2 B5 105.0(3) . . ? C1 C2 Ni4 59.3(2) . . ? C3 C2 Ni4 128.7(3) . . ? B9 C2 Ni4 110.5(3) . . ? B6 C2 Ni4 59.21(19) . . ? B5 C2 Ni4 96.7(2) . . ? C1 B3 B8 116.6(4) . . ? C1 B3 B7 121.5(4) . . ? B8 B3 B7 57.7(3) . . ? C1 B3 B5 60.6(3) . . ? B8 B3 B5 58.9(3) . . ? B7 B3 B5 101.5(3) . . ? C1 B3 Ni4 66.6(2) . . ? B8 B3 Ni4 111.4(3) . . ? B7 B3 Ni4 65.0(2) . . ? B5 B3 Ni4 103.1(3) . . ? C1 B3 H3C 115(2) . . ? B8 B3 H3C 112(2) . . ? B7 B3 H3C 120(2) . . ? B5 B3 H3C 124(2) . . ? Ni4 B3 H3C 127(2) . . ? B11 B5 C1 129.8(4) . . ? B11 B5 B9 57.2(3) . . ? C1 B5 B9 95.0(3) . . ? B11 B5 B8 56.3(3) . . ? C1 B5 B8 100.5(3) . . ? B9 B5 B8 104.0(3) . . ? B11 B5 C2 103.3(3) . . ? C1 B5 C2 44.9(2) . . ? B9 B5 C2 51.8(2) . . ? B8 B5 C2 118.7(3) . . ? B11 B5 B3 104.6(3) . . ? C1 B5 B3 47.1(2) . . ? B9 B5 B3 116.2(3) . . ? B8 B5 B3 55.5(3) . . ? C2 B5 B3 83.9(3) . . ? B11 B5 H5C 122(2) . . ? C1 B5 H5C 108(2) . . ? B9 B5 H5C 117(2) . . ? B8 B5 H5C 127(2) . . ? C2 B5 H5C 113(2) . . ? B3 B5 H5C 122(2) . . ? C2 B6 B12 109.2(3) . . ? C2 B6 B9 55.5(3) . . ? B12 B6 B9 58.7(3) . . ? C2 B6 B10 120.7(3) . . ? B12 B6 B10 59.3(3) . . ? B9 B6 B10 106.9(3) . . ? C2 B6 Ni4 76.8(2) . . ? B12 B6 Ni4 115.7(3) . . ? B9 B6 Ni4 117.9(3) . . ? B10 B6 Ni4 63.6(2) . . ? C2 B6 H6C 110.7(19) . . ? B12 B6 H6C 119(2) . . ? B9 B6 H6C 116(2) . . ? B10 B6 H6C 125.9(19) . . ? Ni4 B6 H6C 117(2) . . ? B8 B7 B10 107.6(4) . . ? B8 B7 B13 59.4(3) . . ? B10 B7 B13 61.1(3) . . ? B8 B7 B3 60.8(3) . . ? B10 B7 B3 114.3(3) . . ? B13 B7 B3 112.8(3) . . ? B8 B7 Ni4 114.3(3) . . ? B10 B7 Ni4 64.1(2) . . ? B13 B7 Ni4 117.0(3) . . ? B3 B7 Ni4 65.7(2) . . ? B8 B7 H7C 116(2) . . ? B10 B7 H7C 127(2) . . ? B13 B7 H7C 118(2) . . ? B3 B7 H7C 114(2) . . ? Ni4 B7 H7C 119(2) . . ? B11 B8 B13 60.6(3) . . ? B11 B8 B7 108.9(4) . . ? B13 B8 B7 60.7(3) . . ? B11 B8 B3 115.8(4) . . ? B13 B8 B3 114.4(4) . . ? B7 B8 B3 61.5(3) . . ? B11 B8 B5 59.2(3) . . ? B13 B8 B5 108.6(3) . . ? B7 B8 B5 109.2(3) . . ? B3 B8 B5 65.7(3) . . ? B11 B8 H8C 119(2) . . ? B13 B8 H8C 129(2) . . ? B7 B8 H8C 128(2) . . ? B3 B8 H8C 110(2) . . ? B5 B8 H8C 112(2) . . ? C2 B9 B12 114.4(4) . . ? C2 B9 B11 116.5(4) . . ? B12 B9 B11 61.2(3) . . ? C2 B9 B6 60.5(3) . . ? B12 B9 B6 59.6(3) . . ? B11 B9 B6 106.7(3) . . ? C2 B9 B5 65.2(3) . . ? B12 B9 B5 107.2(3) . . ? B11 B9 B5 58.9(3) . . ? B6 B9 B5 104.2(3) . . ? C2 B9 H9C 115(2) . . ? B12 B9 H9C 121(2) . . ? B11 B9 H9C 118(2) . . ? B6 B9 H9C 128(2) . . ? B5 B9 H9C 121(2) . . ? B7 B10 B12 108.8(3) . . ? B7 B10 B13 59.6(3) . . ? B12 B10 B13 59.3(3) . . ? B7 B10 B6 112.9(3) . . ? B12 B10 B6 59.0(3) . . ? B13 B10 B6 107.9(3) . . ? B7 B10 Ni4 67.6(2) . . ? B12 B10 Ni4 117.6(3) . . ? B13 B10 Ni4 118.7(3) . . ? B6 B10 Ni4 66.1(2) . . ? B7 B10 H10C 121(2) . . ? B12 B10 H10C 116(3) . . ? B13 B10 H10C 116(2) . . ? B6 B10 H10C 122(2) . . ? Ni4 B10 H10C 117(3) . . ? B8 B11 B13 60.0(3) . . ? B8 B11 B9 115.9(4) . . ? B13 B11 B9 111.0(4) . . ? B8 B11 B12 108.6(4) . . ? B13 B11 B12 59.8(3) . . ? B9 B11 B12 59.3(3) . . ? B8 B11 B5 64.4(3) . . ? B13 B11 B5 112.3(4) . . ? B9 B11 B5 63.9(3) . . ? B12 B11 B5 109.7(3) . . ? B8 B11 H11C 124.7(19) . . ? B13 B11 H11C 125.0(19) . . ? B9 B11 H11C 111.3(19) . . ? B12 B11 H11C 119.6(18) . . ? B5 B11 H11C 117.1(18) . . ? B9 B12 B13 110.6(3) . . ? B9 B12 B6 61.7(3) . . ? B13 B12 B6 111.2(3) . . ? B9 B12 B10 111.1(3) . . ? B13 B12 B10 60.8(3) . . ? B6 B12 B10 61.7(3) . . ? B9 B12 B11 59.5(3) . . ? B13 B12 B11 59.2(3) . . ? B6 B12 B11 107.0(3) . . ? B10 B12 B11 105.9(3) . . ? B9 B12 H12C 110.9(19) . . ? B13 B12 H12C 125.8(19) . . ? B6 B12 H12C 118.5(19) . . ? B10 B12 H12C 128.9(19) . . ? B11 B12 H12C 120.0(19) . . ? B8 B13 B11 59.4(3) . . ? B8 B13 B7 59.9(3) . . ? B11 B13 B7 107.4(3) . . ? B8 B13 B12 109.1(3) . . ? B11 B13 B12 61.0(3) . . ? B7 B13 B12 108.9(3) . . ? B8 B13 B10 106.4(3) . . ? B11 B13 B10 106.7(3) . . ? B7 B13 B10 59.2(3) . . ? B12 B13 B10 59.9(3) . . ? B8 B13 H13C 125.2(18) . . ? B11 B13 H13C 122.3(18) . . ? B7 B13 H13C 123.6(19) . . ? B12 B13 H13C 117.2(18) . . ? B10 B13 H13C 121.0(18) . . ? C2 C3 C4 104.5(3) . . ? C2 C3 H3A 110.8 . . ? C4 C3 H3A 110.8 . . ? C2 C3 H3B 110.8 . . ? C4 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? C5 C4 C3 105.2(3) . . ? C5 C4 H14C 110.7 . . ? C3 C4 H14C 110.7 . . ? C5 C4 H4B 110.7 . . ? C3 C4 H4B 110.7 . . ? H14C C4 H4B 108.8 . . ? C1 C5 C4 104.8(4) . . ? C1 C5 H5A 110.8 . . ? C4 C5 H5A 110.8 . . ? C1 C5 H5B 110.8 . . ? C4 C5 H5B 110.8 . . ? H5A C5 H5B 108.9 . . ? C102 C101 P1 105.8(3) . . ? C102 C101 H10A 110.6 . . ? P1 C101 H10A 110.6 . . ? C102 C101 H10B 110.6 . . ? P1 C101 H10B 110.6 . . ? H10A C101 H10B 108.7 . . ? C101 C102 P2 110.5(3) . . ? C101 C102 H10E 109.6 . . ? P2 C102 H10E 109.6 . . ? C101 C102 H10D 109.6 . . ? P2 C102 H10D 109.6 . . ? H10E C102 H10D 108.1 . . ? C112 C111 C116 119.2(4) . . ? C112 C111 P1 120.0(3) . . ? C116 C111 P1 120.4(3) . . ? C113 C112 C111 120.3(4) . . ? C113 C112 H112 119.9 . . ? C111 C112 H112 119.9 . . ? C114 C113 C112 120.0(4) . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C113 C114 C115 120.5(4) . . ? C113 C114 H114 119.8 . . ? C115 C114 H114 119.8 . . ? C116 C115 C114 119.4(4) . . ? C116 C115 H115 120.3 . . ? C114 C115 H115 120.3 . . ? C115 C116 C111 120.7(4) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C122 C121 C126 119.2(4) . . ? C122 C121 P1 119.1(3) . . ? C126 C121 P1 121.7(3) . . ? C121 C122 C123 120.0(4) . . ? C121 C122 H122 120.0 . . ? C123 C122 H122 120.0 . . ? C124 C123 C122 120.1(5) . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C123 C124 C125 120.8(5) . . ? C123 C124 H124 119.6 . . ? C125 C124 H124 119.6 . . ? C124 C125 C126 119.6(5) . . ? C124 C125 H125 120.2 . . ? C126 C125 H125 120.2 . . ? C125 C126 C121 120.3(4) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? C216 C211 C212 117.6(4) . . ? C216 C211 P2 123.0(3) . . ? C212 C211 P2 119.4(3) . . ? C213 C212 C211 120.8(4) . . ? C213 C212 H212 119.6 . . ? C211 C212 H212 119.6 . . ? C212 C213 C214 120.6(4) . . ? C212 C213 H213 119.7 . . ? C214 C213 H213 119.7 . . ? C215 C214 C213 119.1(4) . . ? C215 C214 H214 120.5 . . ? C213 C214 H214 120.5 . . ? C216 C215 C214 119.8(4) . . ? C216 C215 H215 120.1 . . ? C214 C215 H215 120.1 . . ? C211 C216 C215 122.0(4) . . ? C211 C216 H216 119.0 . . ? C215 C216 H216 119.0 . . ? C222 C221 C226 118.2(4) . . ? C222 C221 P2 125.0(3) . . ? C226 C221 P2 116.7(3) . . ? C221 C222 C223 119.9(4) . . ? C221 C222 H222 120.0 . . ? C223 C222 H222 120.0 . . ? C224 C223 C222 121.0(4) . . ? C224 C223 H223 119.5 . . ? C222 C223 H223 119.5 . . ? C223 C224 C225 120.0(4) . . ? C223 C224 H224 120.0 . . ? C225 C224 H224 120.0 . . ? C224 C225 C226 119.3(4) . . ? C224 C225 H225 120.3 . . ? C226 C225 H225 120.3 . . ? C225 C226 C221 121.6(4) . . ? C225 C226 H226 119.2 . . ? C221 C226 H226 119.2 . . ? Cl1 C1S Cl2 111.4(3) . . ? Cl1 C1S H1S1 109.3 . . ? Cl2 C1S H1S1 109.3 . . ? Cl1 C1S H1S2 109.3 . . ? Cl2 C1S H1S2 109.3 . . ? H1S1 C1S H1S2 108.0 . . ? 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 C1 Ni4 P1 C121 20.2(2) . . . . ? B10 Ni4 P1 C121 -106.8(2) . . . . ? B7 Ni4 P1 C121 -68.1(2) . . . . ? B3 Ni4 P1 C121 -19.7(2) . . . . ? P2 Ni4 P1 C121 151.03(17) . . . . ? C2 Ni4 P1 C121 38.0(2) . . . . ? C1 Ni4 P1 C111 146.72(18) . . . . ? B10 Ni4 P1 C111 19.7(2) . . . . ? B7 Ni4 P1 C111 58.40(19) . . . . ? B3 Ni4 P1 C111 106.83(19) . . . . ? P2 Ni4 P1 C111 -82.44(14) . . . . ? C2 Ni4 P1 C111 164.52(19) . . . . ? C1 Ni4 P1 C101 -103.09(18) . . . . ? B10 Ni4 P1 C101 129.9(2) . . . . ? B7 Ni4 P1 C101 168.59(19) . . . . ? B3 Ni4 P1 C101 -142.98(19) . . . . ? P2 Ni4 P1 C101 27.75(14) . . . . ? C2 Ni4 P1 C101 -85.3(2) . . . . ? C1 Ni4 P2 C221 -14.7(2) . . . . ? B10 Ni4 P2 C221 107.2(2) . . . . ? B6 Ni4 P2 C221 58.2(2) . . . . ? B7 Ni4 P2 C221 141.8(3) . . . . ? P1 Ni4 P2 C221 -118.04(15) . . . . ? B3 Ni4 P2 C221 -56.2(8) . . . . ? C2 Ni4 P2 C221 18.40(18) . . . . ? C1 Ni4 P2 C211 -141.9(2) . . . . ? B10 Ni4 P2 C211 -20.0(2) . . . . ? B6 Ni4 P2 C211 -68.9(2) . . . . ? B7 Ni4 P2 C211 14.6(3) . . . . ? P1 Ni4 P2 C211 114.80(17) . . . . ? B3 Ni4 P2 C211 176.7(8) . . . . ? C2 Ni4 P2 C211 -108.76(19) . . . . ? C1 Ni4 P2 C102 98.6(2) . . . . ? B10 Ni4 P2 C102 -139.5(2) . . . . ? B6 Ni4 P2 C102 171.54(19) . . . . ? B7 Ni4 P2 C102 -104.9(3) . . . . ? P1 Ni4 P2 C102 -4.72(14) . . . . ? B3 Ni4 P2 C102 57.1(8) . . . . ? C2 Ni4 P2 C102 131.72(17) . . . . ? B10 Ni4 C1 C2 -57.9(3) . . . . ? B6 Ni4 C1 C2 -15.3(2) . . . . ? B7 Ni4 C1 C2 -102.8(3) . . . . ? P1 Ni4 C1 C2 158.2(2) . . . . ? B3 Ni4 C1 C2 -127.9(4) . . . . ? P2 Ni4 C1 C2 62.6(3) . . . . ? B10 Ni4 C1 C5 -168.8(4) . . . . ? B6 Ni4 C1 C5 -126.2(4) . . . . ? B7 Ni4 C1 C5 146.3(4) . . . . ? P1 Ni4 C1 C5 47.3(4) . . . . ? B3 Ni4 C1 C5 121.2(5) . . . . ? P2 Ni4 C1 C5 -48.3(4) . . . . ? C2 Ni4 C1 C5 -110.9(5) . . . . ? B10 Ni4 C1 B3 69.9(3) . . . . ? B6 Ni4 C1 B3 112.6(3) . . . . ? B7 Ni4 C1 B3 25.1(3) . . . . ? P1 Ni4 C1 B3 -74.0(2) . . . . ? P2 Ni4 C1 B3 -169.6(2) . . . . ? C2 Ni4 C1 B3 127.9(4) . . . . ? B10 Ni4 C1 B5 8.9(3) . . . . ? B6 Ni4 C1 B5 51.6(3) . . . . ? B7 Ni4 C1 B5 -35.9(3) . . . . ? P1 Ni4 C1 B5 -135.0(2) . . . . ? B3 Ni4 C1 B5 -61.0(3) . . . . ? P2 Ni4 C1 B5 129.4(2) . . . . ? C2 Ni4 C1 B5 66.8(3) . . . . ? C5 C1 C2 C3 3.2(5) . . . . ? B3 C1 C2 C3 171.4(4) . . . . ? B5 C1 C2 C3 119.7(4) . . . . ? Ni4 C1 C2 C3 -124.5(3) . . . . ? C5 C1 C2 B9 -137.2(4) . . . . ? B3 C1 C2 B9 31.0(6) . . . . ? B5 C1 C2 B9 -20.7(4) . . . . ? Ni4 C1 C2 B9 95.1(4) . . . . ? C5 C1 C2 B6 148.3(3) . . . . ? B3 C1 C2 B6 -43.5(5) . . . . ? B5 C1 C2 B6 -95.3(4) . . . . ? Ni4 C1 C2 B6 20.6(3) . . . . ? C5 C1 C2 B5 -116.5(4) . . . . ? B3 C1 C2 B5 51.8(4) . . . . ? Ni4 C1 C2 B5 115.8(2) . . . . ? C5 C1 C2 Ni4 127.7(3) . . . . ? B3 C1 C2 Ni4 -64.1(4) . . . . ? B5 C1 C2 Ni4 -115.8(2) . . . . ? B10 Ni4 C2 C1 124.9(3) . . . . ? B6 Ni4 C2 C1 158.2(3) . . . . ? B7 Ni4 C2 C1 77.4(3) . . . . ? P1 Ni4 C2 C1 -30.8(3) . . . . ? B3 Ni4 C2 C1 34.5(3) . . . . ? P2 Ni4 C2 C1 -134.6(2) . . . . ? C1 Ni4 C2 C3 90.1(4) . . . . ? B10 Ni4 C2 C3 -145.0(4) . . . . ? B6 Ni4 C2 C3 -111.6(4) . . . . ? B7 Ni4 C2 C3 167.6(4) . . . . ? P1 Ni4 C2 C3 59.3(4) . . . . ? B3 Ni4 C2 C3 124.7(4) . . . . ? P2 Ni4 C2 C3 -44.4(4) . . . . ? C1 Ni4 C2 B9 -118.3(4) . . . . ? B10 Ni4 C2 B9 6.5(3) . . . . ? B6 Ni4 C2 B9 39.9(3) . . . . ? B7 Ni4 C2 B9 -40.9(3) . . . . ? P1 Ni4 C2 B9 -149.1(2) . . . . ? B3 Ni4 C2 B9 -83.8(3) . . . . ? P2 Ni4 C2 B9 107.1(3) . . . . ? C1 Ni4 C2 B6 -158.2(3) . . . . ? B10 Ni4 C2 B6 -33.4(2) . . . . ? B7 Ni4 C2 B6 -80.8(2) . . . . ? P1 Ni4 C2 B6 170.96(19) . . . . ? B3 Ni4 C2 B6 -123.7(3) . . . . ? P2 Ni4 C2 B6 67.2(2) . . . . ? C1 Ni4 C2 B5 -54.8(3) . . . . ? B10 Ni4 C2 B5 70.1(2) . . . . ? B6 Ni4 C2 B5 103.5(3) . . . . ? B7 Ni4 C2 B5 22.6(2) . . . . ? P1 Ni4 C2 B5 -85.6(2) . . . . ? B3 Ni4 C2 B5 -20.3(2) . . . . ? P2 Ni4 C2 B5 170.65(19) . . . . ? C2 C1 B3 B8 -32.4(6) . . . . ? C5 C1 B3 B8 134.0(4) . . . . ? B5 C1 B3 B8 18.8(4) . . . . ? Ni4 C1 B3 B8 -103.2(4) . . . . ? C2 C1 B3 B7 34.5(6) . . . . ? C5 C1 B3 B7 -159.2(4) . . . . ? B5 C1 B3 B7 85.6(4) . . . . ? Ni4 C1 B3 B7 -36.3(3) . . . . ? C2 C1 B3 B5 -51.1(4) . . . . ? C5 C1 B3 B5 115.2(4) . . . . ? Ni4 C1 B3 B5 -121.9(2) . . . . ? C2 C1 B3 Ni4 70.8(4) . . . . ? C5 C1 B3 Ni4 -122.8(4) . . . . ? B5 C1 B3 Ni4 121.9(2) . . . . ? B10 Ni4 B3 C1 -115.0(3) . . . . ? B6 Ni4 B3 C1 -65.1(3) . . . . ? B7 Ni4 B3 C1 -146.1(3) . . . . ? P1 Ni4 B3 C1 110.4(2) . . . . ? P2 Ni4 B3 C1 48.8(9) . . . . ? C2 Ni4 B3 C1 -29.6(2) . . . . ? C1 Ni4 B3 B8 110.8(4) . . . . ? B10 Ni4 B3 B8 -4.2(3) . . . . ? B6 Ni4 B3 B8 45.7(3) . . . . ? B7 Ni4 B3 B8 -35.3(3) . . . . ? P1 Ni4 B3 B8 -138.9(3) . . . . ? P2 Ni4 B3 B8 159.5(6) . . . . ? C2 Ni4 B3 B8 81.2(3) . . . . ? C1 Ni4 B3 B7 146.1(3) . . . . ? B10 Ni4 B3 B7 31.2(2) . . . . ? B6 Ni4 B3 B7 81.0(2) . . . . ? P1 Ni4 B3 B7 -103.5(2) . . . . ? P2 Ni4 B3 B7 -165.1(7) . . . . ? C2 Ni4 B3 B7 116.5(2) . . . . ? C1 Ni4 B3 B5 49.4(3) . . . . ? B10 Ni4 B3 B5 -65.6(3) . . . . ? B6 Ni4 B3 B5 -15.7(3) . . . . ? B7 Ni4 B3 B5 -96.8(3) . . . . ? P1 Ni4 B3 B5 159.7(2) . . . . ? P2 Ni4 B3 B5 98.1(8) . . . . ? C2 Ni4 B3 B5 19.8(2) . . . . ? C2 C1 B5 B11 65.6(5) . . . . ? C5 C1 B5 B11 167.5(4) . . . . ? B3 C1 B5 B11 -71.0(5) . . . . ? Ni4 C1 B5 B11 -10.4(5) . . . . ? C2 C1 B5 B9 15.1(3) . . . . ? C5 C1 B5 B9 117.0(4) . . . . ? B3 C1 B5 B9 -121.6(3) . . . . ? Ni4 C1 B5 B9 -61.0(3) . . . . ? C2 C1 B5 B8 120.3(3) . . . . ? C5 C1 B5 B8 -137.8(4) . . . . ? B3 C1 B5 B8 -16.3(3) . . . . ? Ni4 C1 B5 B8 44.3(3) . . . . ? C5 C1 B5 C2 101.9(4) . . . . ? B3 C1 B5 C2 -136.6(4) . . . . ? Ni4 C1 B5 C2 -76.0(3) . . . . ? C2 C1 B5 B3 136.6(4) . . . . ? C5 C1 B5 B3 -121.5(4) . . . . ? Ni4 C1 B5 B3 60.6(3) . . . . ? C1 C2 B5 B11 -134.0(4) . . . . ? C3 C2 B5 B11 130.0(4) . . . . ? B9 C2 B5 B11 26.8(3) . . . . ? B6 C2 B5 B11 -23.0(4) . . . . ? Ni4 C2 B5 B11 -82.9(3) . . . . ? C3 C2 B5 C1 -96.0(4) . . . . ? B9 C2 B5 C1 160.8(4) . . . . ? B6 C2 B5 C1 111.0(4) . . . . ? Ni4 C2 B5 C1 51.2(2) . . . . ? C1 C2 B5 B9 -160.8(4) . . . . ? C3 C2 B5 B9 103.2(4) . . . . ? B6 C2 B5 B9 -49.8(3) . . . . ? Ni4 C2 B5 B9 -109.6(3) . . . . ? C1 C2 B5 B8 -75.4(4) . . . . ? C3 C2 B5 B8 -171.4(4) . . . . ? B9 C2 B5 B8 85.4(4) . . . . ? B6 C2 B5 B8 35.7(4) . . . . ? Ni4 C2 B5 B8 -24.2(4) . . . . ? C1 C2 B5 B3 -30.4(3) . . . . ? C3 C2 B5 B3 -126.4(4) . . . . ? B9 C2 B5 B3 130.4(3) . . . . ? B6 C2 B5 B3 80.6(3) . . . . ? Ni4 C2 B5 B3 20.7(2) . . . . ? C1 B3 B5 B11 131.4(4) . . . . ? B8 B3 B5 B11 -29.0(3) . . . . ? B7 B3 B5 B11 11.6(4) . . . . ? Ni4 B3 B5 B11 78.3(3) . . . . ? B8 B3 B5 C1 -160.4(4) . . . . ? B7 B3 B5 C1 -119.8(4) . . . . ? Ni4 B3 B5 C1 -53.1(2) . . . . ? C1 B3 B5 B9 71.1(4) . . . . ? B8 B3 B5 B9 -89.3(4) . . . . ? B7 B3 B5 B9 -48.7(4) . . . . ? Ni4 B3 B5 B9 18.0(4) . . . . ? C1 B3 B5 B8 160.4(4) . . . . ? B7 B3 B5 B8 40.6(3) . . . . ? Ni4 B3 B5 B8 107.3(3) . . . . ? C1 B3 B5 C2 29.2(3) . . . . ? B8 B3 B5 C2 -131.2(3) . . . . ? B7 B3 B5 C2 -90.6(3) . . . . ? Ni4 B3 B5 C2 -23.9(3) . . . . ? C1 C2 B6 B12 92.3(4) . . . . ? C3 C2 B6 B12 -128.8(4) . . . . ? B9 C2 B6 B12 -25.1(3) . . . . ? B5 C2 B6 B12 24.0(4) . . . . ? Ni4 C2 B6 B12 112.9(3) . . . . ? C1 C2 B6 B9 117.4(4) . . . . ? C3 C2 B6 B9 -103.7(4) . . . . ? B5 C2 B6 B9 49.1(3) . . . . ? Ni4 C2 B6 B9 138.0(3) . . . . ? C1 C2 B6 B10 27.3(5) . . . . ? C3 C2 B6 B10 166.1(4) . . . . ? B9 C2 B6 B10 -90.2(4) . . . . ? B5 C2 B6 B10 -41.0(5) . . . . ? Ni4 C2 B6 B10 47.9(3) . . . . ? C1 C2 B6 Ni4 -20.6(3) . . . . ? C3 C2 B6 Ni4 118.2(4) . . . . ? B9 C2 B6 Ni4 -138.0(3) . . . . ? B5 C2 B6 Ni4 -88.9(3) . . . . ? C1 Ni4 B6 C2 12.7(2) . . . . ? B10 Ni4 B6 C2 134.6(3) . . . . ? B7 Ni4 B6 C2 99.6(2) . . . . ? B3 Ni4 B6 C2 51.0(2) . . . . ? P2 Ni4 B6 C2 -119.40(19) . . . . ? C1 Ni4 B6 B12 -92.4(3) . . . . ? B10 Ni4 B6 B12 29.4(3) . . . . ? B7 Ni4 B6 B12 -5.6(3) . . . . ? B3 Ni4 B6 B12 -54.2(3) . . . . ? P2 Ni4 B6 B12 135.4(3) . . . . ? C2 Ni4 B6 B12 -105.2(4) . . . . ? C1 Ni4 B6 B9 -25.8(3) . . . . ? B10 Ni4 B6 B9 96.0(4) . . . . ? B7 Ni4 B6 B9 61.0(3) . . . . ? B3 Ni4 B6 B9 12.4(3) . . . . ? P2 Ni4 B6 B9 -158.0(3) . . . . ? C2 Ni4 B6 B9 -38.6(3) . . . . ? C1 Ni4 B6 B10 -121.8(2) . . . . ? B7 Ni4 B6 B10 -34.9(2) . . . . ? B3 Ni4 B6 B10 -83.6(2) . . . . ? P2 Ni4 B6 B10 106.0(2) . . . . ? C2 Ni4 B6 B10 -134.6(3) . . . . ? C1 B3 B7 B8 -103.6(4) . . . . ? B5 B3 B7 B8 -41.2(3) . . . . ? Ni4 B3 B7 B8 -140.4(3) . . . . ? C1 B3 B7 B10 -6.3(6) . . . . ? B8 B3 B7 B10 97.3(4) . . . . ? B5 B3 B7 B10 56.1(4) . . . . ? Ni4 B3 B7 B10 -43.2(3) . . . . ? C1 B3 B7 B13 -73.7(5) . . . . ? B8 B3 B7 B13 29.9(3) . . . . ? B5 B3 B7 B13 -11.3(4) . . . . ? Ni4 B3 B7 B13 -110.5(3) . . . . ? C1 B3 B7 Ni4 36.8(3) . . . . ? B8 B3 B7 Ni4 140.4(3) . . . . ? B5 B3 B7 Ni4 99.3(3) . . . . ? C1 Ni4 B7 B8 15.7(3) . . . . ? B10 Ni4 B7 B8 -98.6(4) . . . . ? B6 Ni4 B7 B8 -62.4(3) . . . . ? P1 Ni4 B7 B8 118.0(3) . . . . ? B3 Ni4 B7 B8 37.6(3) . . . . ? P2 Ni4 B7 B8 -146.7(2) . . . . ? C2 Ni4 B7 B8 -19.0(3) . . . . ? C1 Ni4 B7 B10 114.2(2) . . . . ? B6 Ni4 B7 B10 36.2(3) . . . . ? P1 Ni4 B7 B10 -143.4(2) . . . . ? B3 Ni4 B7 B10 136.1(3) . . . . ? P2 Ni4 B7 B10 -48.1(3) . . . . ? C2 Ni4 B7 B10 79.5(2) . . . . ? C1 Ni4 B7 B13 82.4(3) . . . . ? B10 Ni4 B7 B13 -31.9(3) . . . . ? B6 Ni4 B7 B13 4.3(3) . . . . ? P1 Ni4 B7 B13 -175.3(3) . . . . ? B3 Ni4 B7 B13 104.2(4) . . . . ? P2 Ni4 B7 B13 -80.0(4) . . . . ? C2 Ni4 B7 B13 47.7(3) . . . . ? C1 Ni4 B7 B3 -21.9(2) . . . . ? B10 Ni4 B7 B3 -136.1(3) . . . . ? B6 Ni4 B7 B3 -100.0(2) . . . . ? P1 Ni4 B7 B3 80.4(2) . . . . ? P2 Ni4 B7 B3 175.75(19) . . . . ? C2 Ni4 B7 B3 -56.6(2) . . . . ? B10 B7 B8 B11 1.2(4) . . . . ? B13 B7 B8 B11 -38.0(3) . . . . ? B3 B7 B8 B11 109.7(4) . . . . ? Ni4 B7 B8 B11 70.2(4) . . . . ? B10 B7 B8 B13 39.2(3) . . . . ? B3 B7 B8 B13 147.7(4) . . . . ? Ni4 B7 B8 B13 108.2(3) . . . . ? B10 B7 B8 B3 -108.5(4) . . . . ? B13 B7 B8 B3 -147.7(4) . . . . ? Ni4 B7 B8 B3 -39.5(3) . . . . ? B10 B7 B8 B5 -61.8(4) . . . . ? B13 B7 B8 B5 -101.1(4) . . . . ? B3 B7 B8 B5 46.7(3) . . . . ? Ni4 B7 B8 B5 7.1(4) . . . . ? C1 B3 B8 B11 13.5(6) . . . . ? B7 B3 B8 B11 -98.5(4) . . . . ? B5 B3 B8 B11 32.6(3) . . . . ? Ni4 B3 B8 B11 -60.2(4) . . . . ? C1 B3 B8 B13 81.2(5) . . . . ? B7 B3 B8 B13 -30.8(3) . . . . ? B5 B3 B8 B13 100.3(4) . . . . ? Ni4 B3 B8 B13 7.6(5) . . . . ? C1 B3 B8 B7 112.0(4) . . . . ? B5 B3 B8 B7 131.1(3) . . . . ? Ni4 B3 B8 B7 38.3(3) . . . . ? C1 B3 B8 B5 -19.1(4) . . . . ? B7 B3 B8 B5 -131.1(3) . . . . ? Ni4 B3 B8 B5 -92.8(3) . . . . ? C1 B5 B8 B11 -131.2(4) . . . . ? B9 B5 B8 B11 -33.3(3) . . . . ? C2 B5 B8 B11 -87.1(4) . . . . ? B3 B5 B8 B11 -145.7(4) . . . . ? B11 B5 B8 B13 36.6(3) . . . . ? C1 B5 B8 B13 -94.6(4) . . . . ? B9 B5 B8 B13 3.3(4) . . . . ? C2 B5 B8 B13 -50.6(5) . . . . ? B3 B5 B8 B13 -109.1(4) . . . . ? B11 B5 B8 B7 101.1(4) . . . . ? C1 B5 B8 B7 -30.1(4) . . . . ? B9 B5 B8 B7 67.8(4) . . . . ? C2 B5 B8 B7 14.0(5) . . . . ? B3 B5 B8 B7 -44.6(3) . . . . ? B11 B5 B8 B3 145.7(4) . . . . ? C1 B5 B8 B3 14.5(3) . . . . ? B9 B5 B8 B3 112.4(3) . . . . ? C2 B5 B8 B3 58.5(4) . . . . ? C1 C2 B9 B12 -77.5(5) . . . . ? C3 C2 B9 B12 144.3(4) . . . . ? B6 C2 B9 B12 26.4(3) . . . . ? B5 C2 B9 B12 -98.5(4) . . . . ? Ni4 C2 B9 B12 -11.4(4) . . . . ? C1 C2 B9 B11 -8.9(6) . . . . ? C3 C2 B9 B11 -147.1(4) . . . . ? B6 C2 B9 B11 95.0(4) . . . . ? B5 C2 B9 B11 -29.9(3) . . . . ? Ni4 C2 B9 B11 57.2(4) . . . . ? C1 C2 B9 B6 -103.9(4) . . . . ? C3 C2 B9 B6 117.9(4) . . . . ? B5 C2 B9 B6 -124.9(3) . . . . ? Ni4 C2 B9 B6 -37.8(2) . . . . ? C1 C2 B9 B5 21.0(4) . . . . ? C3 C2 B9 B5 -117.2(4) . . . . ? B6 C2 B9 B5 124.9(3) . . . . ? Ni4 C2 B9 B5 87.1(3) . . . . ? B12 B6 B9 C2 152.0(4) . . . . ? B10 B6 B9 C2 116.0(4) . . . . ? Ni4 B6 B9 C2 47.4(3) . . . . ? C2 B6 B9 B12 -152.0(4) . . . . ? B10 B6 B9 B12 -36.0(3) . . . . ? Ni4 B6 B9 B12 -104.6(3) . . . . ? C2 B6 B9 B11 -111.5(4) . . . . ? B12 B6 B9 B11 40.6(3) . . . . ? B10 B6 B9 B11 4.5(4) . . . . ? Ni4 B6 B9 B11 -64.0(4) . . . . ? C2 B6 B9 B5 -50.2(3) . . . . ? B12 B6 B9 B5 101.8(4) . . . . ? B10 B6 B9 B5 65.8(4) . . . . ? Ni4 B6 B9 B5 -2.8(4) . . . . ? B11 B5 B9 C2 -148.6(4) . . . . ? C1 B5 B9 C2 -13.5(3) . . . . ? B8 B5 B9 C2 -115.7(3) . . . . ? B3 B5 B9 C2 -57.6(3) . . . . ? B11 B5 B9 B12 -39.1(3) . . . . ? C1 B5 B9 B12 96.0(4) . . . . ? B8 B5 B9 B12 -6.2(4) . . . . ? C2 B5 B9 B12 109.5(4) . . . . ? B3 B5 B9 B12 51.9(4) . . . . ? C1 B5 B9 B11 135.1(4) . . . . ? B8 B5 B9 B11 32.9(3) . . . . ? C2 B5 B9 B11 148.6(4) . . . . ? B3 B5 B9 B11 91.0(4) . . . . ? B11 B5 B9 B6 -101.2(4) . . . . ? C1 B5 B9 B6 33.9(4) . . . . ? B8 B5 B9 B6 -68.3(4) . . . . ? C2 B5 B9 B6 47.4(3) . . . . ? B3 B5 B9 B6 -10.2(4) . . . . ? B8 B7 B10 B12 -3.9(4) . . . . ? B13 B7 B10 B12 34.5(3) . . . . ? B3 B7 B10 B12 -69.1(4) . . . . ? Ni4 B7 B10 B12 -112.9(3) . . . . ? B8 B7 B10 B13 -38.4(3) . . . . ? B3 B7 B10 B13 -103.6(4) . . . . ? Ni4 B7 B10 B13 -147.5(3) . . . . ? B8 B7 B10 B6 59.6(4) . . . . ? B13 B7 B10 B6 98.0(4) . . . . ? B3 B7 B10 B6 -5.6(5) . . . . ? Ni4 B7 B10 B6 -49.5(3) . . . . ? B8 B7 B10 Ni4 109.1(3) . . . . ? B13 B7 B10 Ni4 147.5(3) . . . . ? B3 B7 B10 Ni4 43.9(3) . . . . ? C2 B6 B10 B7 -3.5(5) . . . . ? B12 B6 B10 B7 -98.8(4) . . . . ? B9 B6 B10 B7 -63.0(4) . . . . ? Ni4 B6 B10 B7 50.2(3) . . . . ? C2 B6 B10 B12 95.3(4) . . . . ? B9 B6 B10 B12 35.8(3) . . . . ? Ni4 B6 B10 B12 149.1(3) . . . . ? C2 B6 B10 B13 60.4(5) . . . . ? B12 B6 B10 B13 -34.9(3) . . . . ? B9 B6 B10 B13 0.9(4) . . . . ? Ni4 B6 B10 B13 114.1(3) . . . . ? C2 B6 B10 Ni4 -53.8(3) . . . . ? B12 B6 B10 Ni4 -149.1(3) . . . . ? B9 B6 B10 Ni4 -113.3(3) . . . . ? C1 Ni4 B10 B7 -70.6(3) . . . . ? B6 Ni4 B10 B7 -130.0(3) . . . . ? P1 Ni4 B10 B7 55.6(3) . . . . ? B3 Ni4 B10 B7 -31.7(2) . . . . ? P2 Ni4 B10 B7 151.3(2) . . . . ? C2 Ni4 B10 B7 -100.2(2) . . . . ? C1 Ni4 B10 B12 29.6(3) . . . . ? B6 Ni4 B10 B12 -29.8(3) . . . . ? B7 Ni4 B10 B12 100.2(4) . . . . ? P1 Ni4 B10 B12 155.8(2) . . . . ? B3 Ni4 B10 B12 68.4(3) . . . . ? P2 Ni4 B10 B12 -108.6(3) . . . . ? C2 Ni4 B10 B12 -0.1(3) . . . . ? C1 Ni4 B10 B13 -38.7(3) . . . . ? B6 Ni4 B10 B13 -98.1(4) . . . . ? B7 Ni4 B10 B13 31.9(3) . . . . ? P1 Ni4 B10 B13 87.5(3) . . . . ? B3 Ni4 B10 B13 0.2(3) . . . . ? P2 Ni4 B10 B13 -176.8(3) . . . . ? C2 Ni4 B10 B13 -68.3(3) . . . . ? C1 Ni4 B10 B6 59.4(2) . . . . ? B7 Ni4 B10 B6 130.0(3) . . . . ? P1 Ni4 B10 B6 -174.40(18) . . . . ? B3 Ni4 B10 B6 98.3(2) . . . . ? P2 Ni4 B10 B6 -78.7(2) . . . . ? C2 Ni4 B10 B6 29.8(2) . . . . ? B7 B8 B11 B13 38.0(3) . . . . ? B3 B8 B11 B13 104.8(4) . . . . ? B5 B8 B11 B13 139.6(3) . . . . ? B13 B8 B11 B9 -100.4(4) . . . . ? B7 B8 B11 B9 -62.4(5) . . . . ? B3 B8 B11 B9 4.4(6) . . . . ? B5 B8 B11 B9 39.2(4) . . . . ? B13 B8 B11 B12 -36.1(3) . . . . ? B7 B8 B11 B12 1.9(5) . . . . ? B3 B8 B11 B12 68.7(5) . . . . ? B5 B8 B11 B12 103.5(4) . . . . ? B13 B8 B11 B5 -139.6(3) . . . . ? B7 B8 B11 B5 -101.6(4) . . . . ? B3 B8 B11 B5 -34.8(4) . . . . ? C2 B9 B11 B8 -7.5(6) . . . . ? B12 B9 B11 B8 97.1(4) . . . . ? B6 B9 B11 B8 57.3(5) . . . . ? B5 B9 B11 B8 -39.4(4) . . . . ? C2 B9 B11 B13 -73.4(5) . . . . ? B12 B9 B11 B13 31.3(3) . . . . ? B6 B9 B11 B13 -8.5(5) . . . . ? B5 B9 B11 B13 -105.3(4) . . . . ? C2 B9 B11 B12 -104.6(4) . . . . ? B6 B9 B11 B12 -39.8(3) . . . . ? B5 B9 B11 B12 -136.6(4) . . . . ? C2 B9 B11 B5 31.9(4) . . . . ? B12 B9 B11 B5 136.6(4) . . . . ? B6 B9 B11 B5 96.8(4) . . . . ? C1 B5 B11 B8 74.4(5) . . . . ? B9 B5 B11 B8 140.7(4) . . . . ? C2 B5 B11 B8 115.8(3) . . . . ? B3 B5 B11 B8 28.7(3) . . . . ? C1 B5 B11 B13 37.1(6) . . . . ? B9 B5 B11 B13 103.3(4) . . . . ? B8 B5 B11 B13 -37.3(3) . . . . ? C2 B5 B11 B13 78.4(4) . . . . ? B3 B5 B11 B13 -8.6(4) . . . . ? C1 B5 B11 B9 -66.3(4) . . . . ? B8 B5 B11 B9 -140.7(4) . . . . ? C2 B5 B11 B9 -24.9(3) . . . . ? B3 B5 B11 B9 -112.0(3) . . . . ? C1 B5 B11 B12 -27.4(6) . . . . ? B9 B5 B11 B12 38.9(3) . . . . ? B8 B5 B11 B12 -101.8(4) . . . . ? C2 B5 B11 B12 14.0(4) . . . . ? B3 B5 B11 B12 -73.1(4) . . . . ? C2 B9 B12 B13 77.1(4) . . . . ? B11 B9 B12 B13 -31.0(3) . . . . ? B6 B9 B12 B13 103.7(4) . . . . ? B5 B9 B12 B13 7.0(5) . . . . ? C2 B9 B12 B6 -26.6(3) . . . . ? B11 B9 B12 B6 -134.7(4) . . . . ? B5 B9 B12 B6 -96.7(4) . . . . ? C2 B9 B12 B10 11.6(5) . . . . ? B11 B9 B12 B10 -96.5(4) . . . . ? B6 B9 B12 B10 38.2(3) . . . . ? B5 B9 B12 B10 -58.5(4) . . . . ? C2 B9 B12 B11 108.1(4) . . . . ? B6 B9 B12 B11 134.7(4) . . . . ? B5 B9 B12 B11 38.0(3) . . . . ? C2 B6 B12 B9 24.2(3) . . . . ? B10 B6 B12 B9 139.1(4) . . . . ? Ni4 B6 B12 B9 108.4(3) . . . . ? C2 B6 B12 B13 -78.5(4) . . . . ? B9 B6 B12 B13 -102.7(4) . . . . ? B10 B6 B12 B13 36.4(3) . . . . ? Ni4 B6 B12 B13 5.7(5) . . . . ? C2 B6 B12 B10 -114.9(4) . . . . ? B9 B6 B12 B10 -139.1(4) . . . . ? Ni4 B6 B12 B10 -30.7(3) . . . . ? C2 B6 B12 B11 -15.7(4) . . . . ? B9 B6 B12 B11 -39.8(3) . . . . ? B10 B6 B12 B11 99.3(4) . . . . ? Ni4 B6 B12 B11 68.5(4) . . . . ? B7 B10 B12 B9 67.8(4) . . . . ? B13 B10 B12 B9 102.5(4) . . . . ? B6 B10 B12 B9 -38.2(3) . . . . ? Ni4 B10 B12 B9 -6.1(5) . . . . ? B7 B10 B12 B13 -34.7(3) . . . . ? B6 B10 B12 B13 -140.7(4) . . . . ? Ni4 B10 B12 B13 -108.6(3) . . . . ? B7 B10 B12 B6 106.0(4) . . . . ? B13 B10 B12 B6 140.7(4) . . . . ? Ni4 B10 B12 B6 32.1(3) . . . . ? B7 B10 B12 B11 4.9(4) . . . . ? B13 B10 B12 B11 39.6(3) . . . . ? B6 B10 B12 B11 -101.0(4) . . . . ? Ni4 B10 B12 B11 -69.0(4) . . . . ? B8 B11 B12 B9 -109.7(4) . . . . ? B13 B11 B12 B9 -145.9(4) . . . . ? B5 B11 B12 B9 -41.0(3) . . . . ? B8 B11 B12 B13 36.2(3) . . . . ? B9 B11 B12 B13 145.9(4) . . . . ? B5 B11 B12 B13 104.9(4) . . . . ? B8 B11 B12 B6 -68.8(4) . . . . ? B13 B11 B12 B6 -105.0(4) . . . . ? B9 B11 B12 B6 40.9(3) . . . . ? B5 B11 B12 B6 -0.1(5) . . . . ? B8 B11 B12 B10 -4.2(4) . . . . ? B13 B11 B12 B10 -40.4(3) . . . . ? B9 B11 B12 B10 105.5(4) . . . . ? B5 B11 B12 B10 64.5(4) . . . . ? B7 B8 B13 B11 -138.1(4) . . . . ? B3 B8 B13 B11 -107.1(4) . . . . ? B5 B8 B13 B11 -36.0(3) . . . . ? B11 B8 B13 B7 138.1(4) . . . . ? B3 B8 B13 B7 31.0(3) . . . . ? B5 B8 B13 B7 102.1(4) . . . . ? B11 B8 B13 B12 36.8(3) . . . . ? B7 B8 B13 B12 -101.3(4) . . . . ? B3 B8 B13 B12 -70.3(4) . . . . ? B5 B8 B13 B12 0.8(5) . . . . ? B11 B8 B13 B10 100.0(4) . . . . ? B7 B8 B13 B10 -38.1(3) . . . . ? B3 B8 B13 B10 -7.0(5) . . . . ? B5 B8 B13 B10 64.0(4) . . . . ? B9 B11 B13 B8 108.6(4) . . . . ? B12 B11 B13 B8 139.7(4) . . . . ? B5 B11 B13 B8 39.2(3) . . . . ? B8 B11 B13 B7 -37.3(3) . . . . ? B9 B11 B13 B7 71.3(4) . . . . ? B12 B11 B13 B7 102.4(4) . . . . ? B5 B11 B13 B7 1.9(5) . . . . ? B8 B11 B13 B12 -139.7(4) . . . . ? B9 B11 B13 B12 -31.1(3) . . . . ? B5 B11 B13 B12 -100.5(4) . . . . ? B8 B11 B13 B10 -99.5(4) . . . . ? B9 B11 B13 B10 9.1(5) . . . . ? B12 B11 B13 B10 40.2(3) . . . . ? B5 B11 B13 B10 -60.3(4) . . . . ? B10 B7 B13 B8 -136.5(4) . . . . ? B3 B7 B13 B8 -30.4(3) . . . . ? Ni4 B7 B13 B8 -103.6(3) . . . . ? B8 B7 B13 B11 37.0(3) . . . . ? B10 B7 B13 B11 -99.5(4) . . . . ? B3 B7 B13 B11 6.7(5) . . . . ? Ni4 B7 B13 B11 -66.6(4) . . . . ? B8 B7 B13 B12 101.7(4) . . . . ? B10 B7 B13 B12 -34.8(3) . . . . ? B3 B7 B13 B12 71.3(4) . . . . ? Ni4 B7 B13 B12 -2.0(4) . . . . ? B8 B7 B13 B10 136.5(4) . . . . ? B3 B7 B13 B10 106.2(4) . . . . ? Ni4 B7 B13 B10 32.9(3) . . . . ? B9 B12 B13 B8 -5.0(5) . . . . ? B6 B12 B13 B8 61.5(4) . . . . ? B10 B12 B13 B8 98.3(4) . . . . ? B11 B12 B13 B8 -36.1(3) . . . . ? B9 B12 B13 B11 31.1(3) . . . . ? B6 B12 B13 B11 97.6(4) . . . . ? B10 B12 B13 B11 134.4(3) . . . . ? B9 B12 B13 B7 -68.8(4) . . . . ? B6 B12 B13 B7 -2.2(5) . . . . ? B10 B12 B13 B7 34.5(3) . . . . ? B11 B12 B13 B7 -99.9(4) . . . . ? B9 B12 B13 B10 -103.3(4) . . . . ? B6 B12 B13 B10 -36.8(3) . . . . ? B11 B12 B13 B10 -134.4(3) . . . . ? B7 B10 B13 B8 38.4(3) . . . . ? B12 B10 B13 B8 -103.0(4) . . . . ? B6 B10 B13 B8 -68.2(4) . . . . ? Ni4 B10 B13 B8 3.9(4) . . . . ? B7 B10 B13 B11 100.6(4) . . . . ? B12 B10 B13 B11 -40.7(3) . . . . ? B6 B10 B13 B11 -5.9(4) . . . . ? Ni4 B10 B13 B11 66.1(4) . . . . ? B12 B10 B13 B7 -141.4(4) . . . . ? B6 B10 B13 B7 -106.5(4) . . . . ? Ni4 B10 B13 B7 -34.5(3) . . . . ? B7 B10 B13 B12 141.4(4) . . . . ? B6 B10 B13 B12 34.8(3) . . . . ? Ni4 B10 B13 B12 106.9(3) . . . . ? C1 C2 C3 C4 -18.7(5) . . . . ? B9 C2 C3 C4 125.7(4) . . . . ? B6 C2 C3 C4 -159.7(4) . . . . ? B5 C2 C3 C4 52.5(5) . . . . ? Ni4 C2 C3 C4 -83.8(4) . . . . ? C2 C3 C4 C5 26.6(5) . . . . ? C2 C1 C5 C4 13.7(5) . . . . ? B3 C1 C5 C4 -154.3(4) . . . . ? B5 C1 C5 C4 -65.0(5) . . . . ? Ni4 C1 C5 C4 112.6(4) . . . . ? C3 C4 C5 C1 -24.7(5) . . . . ? C121 P1 C101 C102 176.4(3) . . . . ? C111 P1 C101 C102 67.5(3) . . . . ? Ni4 P1 C101 C102 -49.6(3) . . . . ? P1 C101 C102 P2 46.0(3) . . . . ? C221 P2 C102 C101 98.1(3) . . . . ? C211 P2 C102 C101 -152.7(3) . . . . ? Ni4 P2 C102 C101 -24.8(3) . . . . ? C121 P1 C111 C112 -38.1(4) . . . . ? C101 P1 C111 C112 71.5(4) . . . . ? Ni4 P1 C111 C112 -174.5(3) . . . . ? C121 P1 C111 C116 148.8(3) . . . . ? C101 P1 C111 C116 -101.7(3) . . . . ? Ni4 P1 C111 C116 12.4(4) . . . . ? C116 C111 C112 C113 0.7(6) . . . . ? P1 C111 C112 C113 -172.5(3) . . . . ? C111 C112 C113 C114 0.5(7) . . . . ? C112 C113 C114 C115 -1.2(7) . . . . ? C113 C114 C115 C116 0.6(6) . . . . ? C114 C115 C116 C111 0.6(6) . . . . ? C112 C111 C116 C115 -1.3(6) . . . . ? P1 C111 C116 C115 171.9(3) . . . . ? C111 P1 C121 C122 -46.9(4) . . . . ? C101 P1 C121 C122 -153.4(3) . . . . ? Ni4 P1 C121 C122 82.5(4) . . . . ? C111 P1 C121 C126 135.0(3) . . . . ? C101 P1 C121 C126 28.5(4) . . . . ? Ni4 P1 C121 C126 -95.6(4) . . . . ? C126 C121 C122 C123 -0.2(6) . . . . ? P1 C121 C122 C123 -178.3(3) . . . . ? C121 C122 C123 C124 0.3(7) . . . . ? C122 C123 C124 C125 -0.4(7) . . . . ? C123 C124 C125 C126 0.3(7) . . . . ? C124 C125 C126 C121 -0.2(7) . . . . ? C122 C121 C126 C125 0.1(6) . . . . ? P1 C121 C126 C125 178.2(3) . . . . ? C221 P2 C211 C216 116.4(4) . . . . ? C102 P2 C211 C216 9.8(4) . . . . ? Ni4 P2 C211 C216 -111.4(3) . . . . ? C221 P2 C211 C212 -64.4(4) . . . . ? C102 P2 C211 C212 -170.9(3) . . . . ? Ni4 P2 C211 C212 67.9(3) . . . . ? C216 C211 C212 C213 -1.9(6) . . . . ? P2 C211 C212 C213 178.8(3) . . . . ? C211 C212 C213 C214 1.0(6) . . . . ? C212 C213 C214 C215 1.3(6) . . . . ? C213 C214 C215 C216 -2.5(6) . . . . ? C212 C211 C216 C215 0.7(6) . . . . ? P2 C211 C216 C215 179.9(3) . . . . ? C214 C215 C216 C211 1.6(6) . . . . ? C211 P2 C221 C222 4.3(4) . . . . ? C102 P2 C221 C222 113.5(4) . . . . ? Ni4 P2 C221 C222 -129.4(3) . . . . ? C211 P2 C221 C226 -172.4(3) . . . . ? C102 P2 C221 C226 -63.3(3) . . . . ? Ni4 P2 C221 C226 53.9(3) . . . . ? C226 C221 C222 C223 -0.2(6) . . . . ? P2 C221 C222 C223 -176.9(3) . . . . ? C221 C222 C223 C224 0.7(7) . . . . ? C222 C223 C224 C225 0.0(7) . . . . ? C223 C224 C225 C226 -1.2(7) . . . . ? C224 C225 C226 C221 1.7(7) . . . . ? C222 C221 C226 C225 -1.0(6) . . . . ? P2 C221 C226 C225 176.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.467 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.133