# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address S.Otto ; Sasol Technology Research & Development 1 Klasie Havenga Road Sasolburg 1947 South Africa and Department of Chemistry University of the Free State P.O. Box 339 Bloemfontein 9300 South Africa ; P.N.Bungu ; Sasol Technology Researh & Development 1 Klasie Havenga Road Sasolburg 1947 South Africa ; _publ_contact_author_name 'Dr Stefanus Otto' _publ_contact_author_email Fanie.Otto@sasol.com _publ_contact_author_address ;Sasol Technology Researh & Development P.O. Box 1 Sasolburg 1947 South Africa ; _publ_contact_author_phone 'Intl-27-16-960 4456' _publ_contact_author_fax 'Intl-27-11-522 3218' _publ_section_title ; Evaluation of ligand effects in the modified cobalt hydroformylation of 1-octene. Crystal structures of [CoL(CO)3]2 (L = PA-C5, PCy3 and PCp3). ; _publ_contact_letter ; Please consider this CIF file as supplementary material to our paper submitted for publication in Dalton Transactions: Evaluation of ligand effects in the modified cobalt hydroformylation of 1-octene. Crystal structures of [Co(P)(CO)3]2 (P = PA-C5, PCy3, PCyp3). Sincerely. Stefanus Otto ; # Attachment '- Bungu Otto Oxo3 cif.txt' _publ_section_exptl_refinement ; The intensity data was collected on a Bruker SMART 1K CCD diffractometer using an exposure time of 20 seconds/frame. A total of 1315 frames were collected with a frame width of 0.3\% covering up to \q = 26.36\% with 99.5% completeness accomplished. ; _publ_section_references ; Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Bruker (1998). SMART-NT (Version 5.050). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SAINT+. Version 6.02 (including XPREP). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SADABS (Version 2004/1). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. ; _publ_section_figure_captions ; See text. ; _publ_section_acknowledgements ; See text. ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #========================================================================== # 2. PROCESSING SUMMARY (Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? #===END #=================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Stefanus Otto Sasol Technology Researh & Development P.O. Box 1 Sasolburg 1947 South Africa ; _publ_requested_coeditor_name ? #========================================================================== data_pac5 _database_code_depnum_ccdc_archive 'CCDC 774590' #TrackingRef '- Bungu Otto Oxo3 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexacarbonyl-bis(1,3,5,7-tetramethyl-8-pentyl-2,4,6-trioxa-8-phosphatricyclo [3.3.1.13,7]decane)-dicobalt ; _chemical_name_common ; Hexacarbonyl-bis(1,3,5,7-tetramethyl-8-pentyl-2,4,6-trioxa-8- phosphatricyclo (3.3.1.13,7)decane)-dicobalt ; _chemical_melting_point ? _chemical_formula_moiety 'C59 H92 Co3 O18 P3' _chemical_formula_sum 'C59 H92 Co3 O18 P3' _chemical_formula_weight 1359.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.941(5) _cell_length_b 14.771(5) _cell_length_c 17.930(5) _cell_angle_alpha 74.135(5) _cell_angle_beta 87.832(5) _cell_angle_gamma 89.739(5) _cell_volume 3294.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6186 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.36 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.885 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details ; SADABS (Bruker, 2004) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART ApexII 4K CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 'First 50 frames repeated after data collection.' __diffrn_standards_interval_count 'After collection' _diffrn_standards_interval_time 'After collection' _diffrn_standards_decay_% None _diffrn_reflns_number 34064 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.30 _reflns_number_total 16295 _reflns_number_gt 10727 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^ > 2\s(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^)+(0.0548P)^2^+3.9511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16295 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.90448(3) 0.50873(3) 0.52740(3) 0.01669(11) Uani 1 1 d . . . P1 P 0.74794(6) 0.53704(6) 0.56554(5) 0.01507(17) Uani 1 1 d . . . O11 O 0.9635(2) 0.70660(19) 0.49644(19) 0.0433(8) Uani 1 1 d . . . O12 O 0.8417(2) 0.4350(2) 0.39959(17) 0.0404(7) Uani 1 1 d . . . O13 O 0.96854(19) 0.3769(2) 0.67246(16) 0.0379(7) Uani 1 1 d . . . O14 O 0.55218(16) 0.47594(16) 0.61498(13) 0.0197(5) Uani 1 1 d . . . O15 O 0.58940(17) 0.42612(16) 0.74717(13) 0.0211(5) Uani 1 1 d . . . O16 O 0.76189(16) 0.47623(16) 0.72000(13) 0.0199(5) Uani 1 1 d . . . C11 C 0.9415(3) 0.6288(3) 0.5085(2) 0.0274(8) Uani 1 1 d . . . C12 C 0.8661(2) 0.4639(3) 0.4500(2) 0.0253(8) Uani 1 1 d . . . C13 C 0.9414(2) 0.4289(3) 0.6171(2) 0.0235(8) Uani 1 1 d . . . C111 C 0.6488(2) 0.4400(2) 0.59113(19) 0.0183(7) Uani 1 1 d . . . C112 C 0.6882(2) 0.3637(2) 0.65952(19) 0.0189(7) Uani 1 1 d . . . H11A H 0.6431 0.3091 0.6701 0.023 Uiso 1 1 calc R . . H11B H 0.7569 0.3448 0.6465 0.023 Uiso 1 1 calc R . . C113 C 0.6919(2) 0.3987(2) 0.7309(2) 0.0201(7) Uani 1 1 d . . . C114 C 0.5532(2) 0.5017(2) 0.6862(2) 0.0198(7) Uani 1 1 d . . . C115 C 0.6227(2) 0.5860(2) 0.67767(19) 0.0176(7) Uani 1 1 d . . . H11C H 0.6175 0.6064 0.7247 0.021 Uiso 1 1 calc R . . H11D H 0.6004 0.6374 0.6351 0.021 Uiso 1 1 calc R . . C116 C 0.7346(2) 0.5621(2) 0.66231(19) 0.0175(7) Uani 1 1 d . . . C117 C 0.6228(3) 0.4037(3) 0.5233(2) 0.0249(8) Uani 1 1 d . . . H11E H 0.5682 0.3578 0.5387 0.037 Uiso 1 1 calc R . . H11F H 0.6828 0.3751 0.5065 0.037 Uiso 1 1 calc R . . H11G H 0.6007 0.4550 0.4815 0.037 Uiso 1 1 calc R . . C118 C 0.7250(3) 0.3251(3) 0.8017(2) 0.0279(8) Uani 1 1 d . . . H11H H 0.7946 0.3064 0.7932 0.042 Uiso 1 1 calc R . . H11I H 0.6798 0.2715 0.8114 0.042 Uiso 1 1 calc R . . H11J H 0.7218 0.3506 0.8456 0.042 Uiso 1 1 calc R . . C119 C 0.4429(3) 0.5189(3) 0.7072(2) 0.0260(8) Uani 1 1 d . . . H11K H 0.4032 0.4622 0.7140 0.039 Uiso 1 1 calc R . . H11L H 0.4149 0.5680 0.6663 0.039 Uiso 1 1 calc R . . H11M H 0.4400 0.5373 0.7545 0.039 Uiso 1 1 calc R . . C120 C 0.8093(3) 0.6360(3) 0.6715(2) 0.0255(8) Uani 1 1 d . . . H12A H 0.7994 0.6451 0.7223 0.038 Uiso 1 1 calc R . . H12B H 0.7973 0.6942 0.6330 0.038 Uiso 1 1 calc R . . H12C H 0.8789 0.6158 0.6651 0.038 Uiso 1 1 calc R . . C121 C 0.6826(2) 0.6365(2) 0.49944(19) 0.0209(7) Uani 1 1 d . . . H12D H 0.6086 0.6287 0.5101 0.025 Uiso 1 1 calc R . . H12E H 0.7029 0.6939 0.5115 0.025 Uiso 1 1 calc R . . C122 C 0.7034(3) 0.6495(3) 0.4130(2) 0.0252(8) Uani 1 1 d . . . H12F H 0.7775 0.6494 0.4023 0.030 Uiso 1 1 calc R . . H12G H 0.6734 0.5971 0.3983 0.030 Uiso 1 1 calc R . . C123 C 0.6585(3) 0.7406(3) 0.3648(2) 0.0323(9) Uani 1 1 d . . . H12H H 0.6897 0.7927 0.3792 0.039 Uiso 1 1 calc R . . H12I H 0.5849 0.7411 0.3770 0.039 Uiso 1 1 calc R . . C124 C 0.6751(3) 0.7557(3) 0.2777(2) 0.0379(10) Uani 1 1 d . . . H12J H 0.6418 0.7047 0.2631 0.046 Uiso 1 1 calc R . . H12K H 0.6417 0.8138 0.2509 0.046 Uiso 1 1 calc R . . C125 C 0.7879(4) 0.7605(3) 0.2506(3) 0.0462(12) Uani 1 1 d . . . H12L H 0.8227 0.8083 0.2675 0.069 Uiso 1 1 calc R . . H12M H 0.7926 0.7756 0.1950 0.069 Uiso 1 1 calc R . . H12N H 0.8199 0.7008 0.2722 0.069 Uiso 1 1 calc R . . Co2 Co 0.59578(3) 0.02802(3) 0.47364(3) 0.01968(11) Uani 1 1 d . . . P2 P 0.75139(6) 0.08459(6) 0.43798(5) 0.01647(18) Uani 1 1 d . . . O21 O 0.6591(2) -0.1427(2) 0.58900(17) 0.0383(7) Uani 1 1 d . . . O22 O 0.5366(2) 0.1962(2) 0.5192(2) 0.0630(11) Uani 1 1 d . . . O23 O 0.5323(2) 0.0099(3) 0.32248(18) 0.0466(8) Uani 1 1 d . . . O24 O 0.73523(18) 0.14199(18) 0.28308(14) 0.0270(6) Uani 1 1 d . . . O25 O 0.90762(19) 0.11256(19) 0.25182(15) 0.0287(6) Uani 1 1 d . . . O26 O 0.94611(17) 0.06131(18) 0.38420(15) 0.0258(6) Uani 1 1 d . . . C21 C 0.6351(2) -0.0755(3) 0.5438(2) 0.0256(8) Uani 1 1 d . . . C22 C 0.5589(3) 0.1290(3) 0.5021(3) 0.0377(10) Uani 1 1 d . . . C23 C 0.5586(3) 0.0173(3) 0.3808(2) 0.0293(9) Uani 1 1 d . . . C211 C 0.7635(3) 0.1812(2) 0.3450(2) 0.0238(8) Uani 1 1 d . . . C212 C 0.8751(3) 0.2159(3) 0.3305(2) 0.0258(8) Uani 1 1 d . . . H21A H 0.8795 0.2707 0.2859 0.031 Uiso 1 1 calc R . . H21B H 0.8981 0.2342 0.3752 0.031 Uiso 1 1 calc R . . C213 C 0.9441(3) 0.1394(3) 0.3160(2) 0.0246(8) Uani 1 1 d . . . C214 C 0.8057(3) 0.0740(3) 0.2664(2) 0.0260(8) Uani 1 1 d . . . C215 C 0.8093(3) -0.0132(2) 0.3340(2) 0.0221(7) Uani 1 1 d . . . H21C H 0.8539 -0.0593 0.3200 0.027 Uiso 1 1 calc R . . H21D H 0.7404 -0.0403 0.3457 0.027 Uiso 1 1 calc R . . C216 C 0.8494(2) 0.0094(2) 0.4054(2) 0.0212(7) Uani 1 1 d . . . C217 C 0.6878(3) 0.2604(3) 0.3422(3) 0.0383(10) Uani 1 1 d . . . H21E H 0.6958 0.3069 0.2931 0.057 Uiso 1 1 calc R . . H21F H 0.7011 0.2887 0.3832 0.057 Uiso 1 1 calc R . . H21G H 0.6185 0.2358 0.3487 0.057 Uiso 1 1 calc R . . C218 C 1.0550(3) 0.1699(3) 0.2967(3) 0.0408(11) Uani 1 1 d . . . H21H H 1.0937 0.1197 0.2847 0.061 Uiso 1 1 calc R . . H21I H 1.0840 0.1850 0.3404 0.061 Uiso 1 1 calc R . . H21J H 1.0581 0.2243 0.2527 0.061 Uiso 1 1 calc R . . C219 C 0.7709(3) 0.0551(3) 0.1929(2) 0.0341(9) Uani 1 1 d . . . H21K H 0.7744 0.1123 0.1516 0.051 Uiso 1 1 calc R . . H21L H 0.7010 0.0320 0.2005 0.051 Uiso 1 1 calc R . . H21M H 0.8152 0.0089 0.1799 0.051 Uiso 1 1 calc R . . C220 C 0.8763(3) -0.0773(3) 0.4700(2) 0.0312(9) Uani 1 1 d . . . H22A H 0.9287 -0.1126 0.4512 0.047 Uiso 1 1 calc R . . H22B H 0.8156 -0.1158 0.4865 0.047 Uiso 1 1 calc R . . H22C H 0.9015 -0.0581 0.5131 0.047 Uiso 1 1 calc R . . C221 C 0.8176(3) 0.1332(3) 0.5075(2) 0.0253(8) Uani 1 1 d . . . H22D H 0.8915 0.1297 0.4976 0.030 Uiso 1 1 calc R . . H22E H 0.8002 0.1994 0.4968 0.030 Uiso 1 1 calc R . . C222 C 0.7951(3) 0.0879(3) 0.5926(2) 0.0306(9) Uani 1 1 d . . . H22F H 0.7229 0.0976 0.6047 0.037 Uiso 1 1 calc R . . H22G H 0.8061 0.0207 0.6033 0.037 Uiso 1 1 calc R . . C223 C 0.8608(3) 0.1257(3) 0.6449(2) 0.0256(8) Uani 1 1 d . . . H22H H 0.9322 0.1097 0.6361 0.031 Uiso 1 1 calc R . . H22I H 0.8561 0.1938 0.6291 0.031 Uiso 1 1 calc R . . C224 C 0.8354(4) 0.0924(4) 0.7298(3) 0.0547(14) Uani 1 1 d . . . H22J H 0.8280 0.0244 0.7440 0.066 Uiso 1 1 calc R . . H22K H 0.7690 0.1182 0.7399 0.066 Uiso 1 1 calc R . . C225 C 0.9126(3) 0.1174(3) 0.7817(2) 0.0397(10) Uani 1 1 d . . . H22L H 0.9762 0.0849 0.7779 0.060 Uiso 1 1 calc R . . H22M H 0.8858 0.0990 0.8343 0.060 Uiso 1 1 calc R . . H22N H 0.9250 0.1840 0.7658 0.060 Uiso 1 1 calc R . . Co3 Co 0.54050(3) 0.93098(3) 0.97333(3) 0.02009(11) Uani 1 1 d . . . P3 P 0.61715(6) 0.80874(6) 0.95021(5) 0.01800(18) Uani 1 1 d . . . O31 O 0.3294(2) 0.8543(2) 0.99790(19) 0.0434(8) Uani 1 1 d . . . O32 O 0.5944(3) 1.0748(2) 0.82887(19) 0.0510(9) Uani 1 1 d . . . O33 O 0.6740(2) 0.9116(2) 1.10410(17) 0.0374(7) Uani 1 1 d . . . O34 O 0.6592(2) 0.69113(19) 0.85892(15) 0.0318(6) Uani 1 1 d . . . O35 O 0.5077(2) 0.60012(18) 0.89704(15) 0.0318(6) Uani 1 1 d . . . O36 O 0.45740(18) 0.68821(18) 0.98282(15) 0.0265(6) Uani 1 1 d . . . C31 C 0.4119(3) 0.8836(3) 0.9873(2) 0.0269(8) Uani 1 1 d . . . C32 C 0.5731(3) 1.0172(3) 0.8842(2) 0.0324(9) Uani 1 1 d . . . C33 C 0.6193(3) 0.9212(3) 1.0532(2) 0.0257(8) Uani 1 1 d . . . C311 C 0.6057(3) 0.7790(3) 0.8559(2) 0.0264(8) Uani 1 1 d . . . C312 C 0.4917(3) 0.7657(3) 0.8457(2) 0.0300(9) Uani 1 1 d . . . H31A H 0.4815 0.7594 0.7941 0.036 Uiso 1 1 calc R . . H31B H 0.4541 0.8206 0.8511 0.036 Uiso 1 1 calc R . . C313 C 0.4500(3) 0.6788(3) 0.9056(2) 0.0308(9) Uani 1 1 d . . . C314 C 0.6134(3) 0.6078(3) 0.9118(2) 0.0279(8) Uani 1 1 d . . . C315 C 0.6215(3) 0.6120(2) 0.9949(2) 0.0230(7) Uani 1 1 d . . . H31C H 0.5953 0.5537 1.0299 0.028 Uiso 1 1 calc R . . H31D H 0.6936 0.6185 1.0057 0.028 Uiso 1 1 calc R . . C316 C 0.5609(2) 0.6939(2) 1.0093(2) 0.0198(7) Uani 1 1 d . . . C317 C 0.6583(3) 0.8506(3) 0.7873(2) 0.0351(9) Uani 1 1 d . . . H31E H 0.7297 0.8569 0.7977 0.053 Uiso 1 1 calc R . . H31F H 0.6247 0.9104 0.7796 0.053 Uiso 1 1 calc R . . H31G H 0.6535 0.8296 0.7414 0.053 Uiso 1 1 calc R . . C318 C 0.3376(3) 0.6605(3) 0.8956(3) 0.0418(11) Uani 1 1 d . . . H31H H 0.3282 0.6566 0.8438 0.063 Uiso 1 1 calc R . . H31I H 0.2966 0.7110 0.9048 0.063 Uiso 1 1 calc R . . H31J H 0.3163 0.6023 0.9320 0.063 Uiso 1 1 calc R . . C319 C 0.6684(4) 0.5245(3) 0.8974(2) 0.0380(10) Uani 1 1 d . . . H31K H 0.6428 0.4681 0.9339 0.057 Uiso 1 1 calc R . . H31L H 0.7412 0.5306 0.9033 0.057 Uiso 1 1 calc R . . H31M H 0.6564 0.5215 0.8456 0.057 Uiso 1 1 calc R . . C320 C 0.5487(3) 0.6883(3) 1.0945(2) 0.0265(8) Uani 1 1 d . . . H32A H 0.5068 0.7396 1.1010 0.040 Uiso 1 1 calc R . . H32B H 0.6155 0.6919 1.1150 0.040 Uiso 1 1 calc R . . H32C H 0.5159 0.6297 1.1216 0.040 Uiso 1 1 calc R . . C321 C 0.7555(2) 0.7983(3) 0.9677(2) 0.0238(8) Uani 1 1 d . A . H32D H 0.7639 0.7742 1.0232 0.029 Uiso 1 1 calc R . . H32E H 0.7839 0.7520 0.9434 0.029 Uiso 1 1 calc R . . C322 C 0.8192(3) 0.8889(3) 0.9384(3) 0.0367(10) Uani 1 1 d . . . H10A H 0.7810 0.9413 0.9485 0.044 Uiso 0.603(11) 1 calc PR A 1 H10B H 0.8326 0.9022 0.8829 0.044 Uiso 0.603(11) 1 calc PR A 1 H10C H 0.7962 0.9215 0.8872 0.044 Uiso 0.397(11) 1 calc PR A 2 H10D H 0.8026 0.9288 0.9721 0.044 Uiso 0.397(11) 1 calc PR A 2 C323 C 0.9253(6) 0.8769(6) 0.9815(6) 0.0322(19) Uani 0.603(11) 1 d P A 1 H32F H 0.9619 0.9367 0.9660 0.039 Uiso 0.603(11) 1 calc PR A 1 H32G H 0.9100 0.8627 1.0369 0.039 Uiso 0.603(11) 1 calc PR A 1 C324 C 0.9960(5) 0.8026(5) 0.9671(5) 0.038(2) Uani 0.603(11) 1 d P A 1 H32H H 1.0171 0.8192 0.9125 0.046 Uiso 0.603(11) 1 calc PR A 1 H32I H 0.9588 0.7432 0.9790 0.046 Uiso 0.603(11) 1 calc PR A 1 C325 C 1.0911(8) 0.7905(9) 1.0149(9) 0.062(4) Uani 0.603(11) 1 d P A 1 H32J H 1.1245 0.8504 1.0074 0.093 Uiso 0.603(11) 1 calc PR A 1 H32K H 1.1379 0.7481 0.9991 0.093 Uiso 0.603(11) 1 calc PR A 1 H32L H 1.0715 0.7653 1.0688 0.093 Uiso 0.603(11) 1 calc PR A 1 C326 C 0.9321(8) 0.8808(10) 0.9332(9) 0.043(4) Uani 0.397(11) 1 d P A 2 H32M H 0.9631 0.9412 0.9065 0.051 Uiso 0.397(11) 1 calc PR A 2 H32N H 0.9515 0.8357 0.9048 0.051 Uiso 0.397(11) 1 calc PR A 2 C327 C 0.9687(9) 0.8482(12) 1.0156(8) 0.051(4) Uani 0.397(11) 1 d P A 2 H32O H 0.9388 0.7870 1.0412 0.061 Uiso 0.397(11) 1 calc PR A 2 H32P H 0.9454 0.8920 1.0442 0.061 Uiso 0.397(11) 1 calc PR A 2 C328 C 1.0872(13) 0.8416(15) 1.0163(10) 0.057(5) Uani 0.397(11) 1 d P A 2 H32Q H 1.1098 0.7929 0.9934 0.085 Uiso 0.397(11) 1 calc PR A 2 H32R H 1.1090 0.8272 1.0688 0.085 Uiso 0.397(11) 1 calc PR A 2 H32S H 1.1170 0.9007 0.9871 0.085 Uiso 0.397(11) 1 calc PR A 2 C1 C 0.8195(5) 0.5274(6) 0.1866(4) 0.108(3) Uani 1 1 d . . . H1A H 0.8237 0.4963 0.2410 0.161 Uiso 1 1 calc R . . H1B H 0.8049 0.4819 0.1591 0.161 Uiso 1 1 calc R . . H1C H 0.7652 0.5732 0.1792 0.161 Uiso 1 1 calc R . . C2 C 0.9154(4) 0.5732(4) 0.1580(4) 0.0665(16) Uani 1 1 d . . . H2A H 0.9350 0.6111 0.1917 0.080 Uiso 1 1 calc R . . H2B H 0.9058 0.6154 0.1068 0.080 Uiso 1 1 calc R . . C3 C 1.0038(5) 0.5063(8) 0.1525(5) 0.142(4) Uani 1 1 d . . . H3A H 1.0215 0.4740 0.2051 0.171 Uiso 1 1 calc R . . H3B H 1.0631 0.5448 0.1287 0.171 Uiso 1 1 calc R . . C4 C 0.9910(9) 0.4279(6) 0.1073(4) 0.140(4) Uani 1 1 d . . . H4A H 1.0550 0.3935 0.1071 0.168 Uiso 1 1 calc R . . H4B H 0.9367 0.3836 0.1322 0.168 Uiso 1 1 calc R . . C5 C 0.9643(6) 0.4767(6) 0.0280(4) 0.119(3) Uani 1 1 d . . . H5A H 0.9311 0.4305 0.0073 0.142 Uiso 1 1 calc R . . H5B H 0.9118 0.5224 0.0320 0.142 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0141(2) 0.0153(2) 0.0190(2) -0.00196(18) 0.00108(17) -0.00030(16) P1 0.0148(4) 0.0133(4) 0.0163(4) -0.0028(3) -0.0005(3) -0.0010(3) O11 0.0348(15) 0.0184(15) 0.073(2) -0.0092(14) 0.0173(14) -0.0041(12) O12 0.0282(14) 0.065(2) 0.0376(18) -0.0298(16) 0.0015(12) -0.0035(14) O13 0.0277(14) 0.0432(18) 0.0308(16) 0.0095(13) 0.0029(12) 0.0071(12) O14 0.0155(11) 0.0226(13) 0.0220(13) -0.0078(10) 0.0009(9) 0.0002(9) O15 0.0231(12) 0.0180(12) 0.0191(13) -0.0006(10) 0.0039(10) 0.0037(9) O16 0.0201(11) 0.0182(12) 0.0204(13) -0.0032(10) -0.0021(9) 0.0014(9) C11 0.0199(17) 0.022(2) 0.038(2) -0.0043(16) 0.0064(15) 0.0021(14) C12 0.0155(15) 0.031(2) 0.028(2) -0.0073(16) 0.0051(14) 0.0012(14) C13 0.0173(16) 0.026(2) 0.025(2) -0.0034(16) 0.0028(14) 0.0013(14) C111 0.0162(15) 0.0176(17) 0.0213(18) -0.0063(14) 0.0030(13) -0.0013(12) C112 0.0219(16) 0.0111(16) 0.0218(18) -0.0022(13) 0.0036(13) -0.0010(12) C113 0.0202(16) 0.0156(17) 0.0229(18) -0.0030(14) 0.0036(13) 0.0034(13) C114 0.0185(15) 0.0205(18) 0.0193(18) -0.0035(14) -0.0002(13) 0.0041(13) C115 0.0228(16) 0.0151(16) 0.0152(17) -0.0048(13) 0.0002(13) 0.0015(13) C116 0.0168(15) 0.0122(16) 0.0226(18) -0.0028(13) -0.0019(13) 0.0017(12) C117 0.0228(17) 0.026(2) 0.027(2) -0.0098(16) -0.0010(14) -0.0029(14) C118 0.0308(19) 0.026(2) 0.023(2) 0.0006(15) -0.0010(15) 0.0078(15) C119 0.0227(17) 0.027(2) 0.028(2) -0.0077(16) 0.0042(15) 0.0036(14) C120 0.0271(18) 0.0220(19) 0.030(2) -0.0110(16) -0.0003(15) -0.0065(14) C121 0.0181(15) 0.0203(18) 0.0218(18) -0.0015(14) -0.0018(13) 0.0030(13) C122 0.0293(18) 0.0200(18) 0.025(2) -0.0032(15) -0.0033(15) 0.0018(14) C123 0.034(2) 0.026(2) 0.028(2) 0.0082(16) 0.0044(16) 0.0086(16) C124 0.040(2) 0.033(2) 0.033(2) 0.0044(18) -0.0069(18) 0.0045(18) C125 0.058(3) 0.048(3) 0.029(2) -0.005(2) 0.006(2) 0.016(2) Co2 0.0109(2) 0.0230(3) 0.0283(3) -0.0126(2) 0.00123(18) -0.00145(17) P2 0.0121(4) 0.0164(4) 0.0213(5) -0.0057(3) -0.0010(3) -0.0003(3) O21 0.0343(15) 0.0379(18) 0.0350(17) 0.0022(14) 0.0052(12) -0.0020(13) O22 0.0322(16) 0.050(2) 0.127(3) -0.063(2) 0.0351(18) -0.0173(14) O23 0.0250(14) 0.084(3) 0.0408(19) -0.0341(18) -0.0031(13) -0.0073(15) O24 0.0290(13) 0.0277(14) 0.0253(14) -0.0083(11) -0.0069(11) 0.0028(11) O25 0.0300(13) 0.0322(15) 0.0254(14) -0.0115(11) 0.0075(11) -0.0110(11) O26 0.0144(11) 0.0280(14) 0.0324(15) -0.0041(11) 0.0026(10) -0.0053(10) C21 0.0140(15) 0.033(2) 0.031(2) -0.0125(17) 0.0077(14) -0.0057(14) C22 0.0159(17) 0.043(3) 0.063(3) -0.031(2) 0.0104(18) -0.0072(16) C23 0.0132(16) 0.038(2) 0.042(2) -0.0198(19) 0.0009(15) -0.0030(15) C211 0.0271(18) 0.0137(17) 0.030(2) -0.0047(15) -0.0034(15) 0.0007(14) C212 0.0295(18) 0.0206(19) 0.026(2) -0.0040(15) 0.0015(15) -0.0091(15) C213 0.0238(17) 0.026(2) 0.0236(19) -0.0070(15) 0.0039(14) -0.0106(14) C214 0.0255(18) 0.026(2) 0.029(2) -0.0126(16) 0.0018(15) -0.0062(15) C215 0.0197(16) 0.0181(18) 0.031(2) -0.0128(15) 0.0075(14) -0.0025(13) C216 0.0148(15) 0.0181(17) 0.029(2) -0.0045(14) 0.0028(13) 0.0009(13) C217 0.048(2) 0.021(2) 0.045(3) -0.0070(18) -0.008(2) 0.0126(18) C218 0.032(2) 0.051(3) 0.040(3) -0.016(2) 0.0141(18) -0.0235(19) C219 0.039(2) 0.040(2) 0.029(2) -0.0178(19) -0.0020(17) -0.0035(18) C220 0.0243(18) 0.024(2) 0.044(3) -0.0080(17) -0.0002(17) 0.0072(15) C221 0.0201(16) 0.027(2) 0.030(2) -0.0100(16) 0.0002(14) -0.0060(14) C222 0.0315(19) 0.035(2) 0.027(2) -0.0122(17) 0.0028(16) -0.0130(16) C223 0.0236(17) 0.026(2) 0.029(2) -0.0118(16) -0.0001(15) -0.0041(14) C224 0.071(3) 0.066(4) 0.028(2) -0.014(2) 0.009(2) -0.038(3) C225 0.048(2) 0.041(3) 0.034(2) -0.015(2) -0.0044(19) -0.002(2) Co3 0.0190(2) 0.0161(2) 0.0244(3) -0.00395(19) -0.00231(18) 0.00035(17) P3 0.0185(4) 0.0170(4) 0.0172(4) -0.0024(3) -0.0010(3) -0.0008(3) O31 0.0223(14) 0.0354(17) 0.073(2) -0.0153(16) -0.0032(14) 0.0002(12) O32 0.073(2) 0.0254(17) 0.044(2) 0.0055(14) 0.0173(16) 0.0012(15) O33 0.0465(16) 0.0322(16) 0.0363(17) -0.0124(13) -0.0186(14) 0.0094(13) O34 0.0481(16) 0.0277(15) 0.0190(14) -0.0060(11) 0.0023(12) 0.0059(12) O35 0.0486(16) 0.0210(14) 0.0254(15) -0.0039(11) -0.0148(12) -0.0028(12) O36 0.0235(12) 0.0275(14) 0.0270(14) -0.0042(11) -0.0055(10) -0.0033(10) C31 0.0245(18) 0.0213(19) 0.035(2) -0.0079(16) -0.0012(15) 0.0059(15) C32 0.036(2) 0.023(2) 0.038(2) -0.0072(18) 0.0011(18) 0.0016(16) C33 0.0283(18) 0.0200(19) 0.030(2) -0.0094(15) -0.0026(16) 0.0045(14) C311 0.042(2) 0.0202(19) 0.0158(18) -0.0029(14) -0.0022(15) -0.0008(16) C312 0.040(2) 0.024(2) 0.026(2) -0.0039(16) -0.0166(17) -0.0003(16) C313 0.039(2) 0.021(2) 0.029(2) -0.0003(16) -0.0146(17) -0.0041(16) C314 0.044(2) 0.0172(18) 0.0223(19) -0.0042(15) -0.0054(16) 0.0003(16) C315 0.0306(18) 0.0179(18) 0.0187(18) -0.0017(14) -0.0026(14) -0.0001(14) C316 0.0173(15) 0.0190(17) 0.0209(18) -0.0017(14) -0.0017(13) -0.0017(13) C317 0.049(2) 0.035(2) 0.0182(19) -0.0016(17) 0.0022(17) -0.0010(19) C318 0.045(2) 0.028(2) 0.047(3) 0.0020(19) -0.021(2) -0.0097(18) C319 0.064(3) 0.027(2) 0.025(2) -0.0099(17) -0.002(2) 0.007(2) C320 0.0310(19) 0.026(2) 0.0211(19) -0.0042(15) 0.0042(15) -0.0030(15) C321 0.0187(16) 0.0255(19) 0.026(2) -0.0062(15) 0.0025(14) -0.0008(14) C322 0.0243(19) 0.033(2) 0.049(3) -0.0064(19) 0.0011(18) -0.0101(16) C323 0.022(4) 0.040(4) 0.034(5) -0.008(4) -0.005(4) -0.006(3) C324 0.022(3) 0.044(5) 0.048(5) -0.010(4) 0.000(3) -0.003(3) C325 0.016(4) 0.063(8) 0.112(10) -0.030(7) -0.019(4) -0.004(5) C326 0.021(5) 0.063(9) 0.031(8) 0.008(6) 0.001(5) -0.005(5) C327 0.030(7) 0.089(11) 0.041(8) -0.031(8) 0.007(6) 0.000(7) C328 0.044(8) 0.089(14) 0.044(8) -0.028(10) -0.002(6) -0.018(10) C1 0.089(5) 0.131(7) 0.083(5) 0.007(5) -0.015(4) -0.048(5) C2 0.067(4) 0.058(4) 0.078(4) -0.025(3) -0.016(3) 0.000(3) C3 0.063(4) 0.289(14) 0.076(5) -0.051(7) -0.021(4) 0.072(6) C4 0.278(13) 0.070(5) 0.066(5) -0.005(4) -0.060(7) -0.028(6) C5 0.124(7) 0.119(7) 0.080(5) 0.022(5) 0.036(4) 0.066(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C11 1.776(4) . ? Co1 C12 1.780(4) . ? Co1 C13 1.795(4) . ? Co1 P1 2.1887(12) . ? Co1 Co1 2.6632(12) 2_766 ? P1 C121 1.841(3) . ? P1 C116 1.872(4) . ? P1 C111 1.877(3) . ? O11 C11 1.145(4) . ? O12 C12 1.154(5) . ? O13 C13 1.143(4) . ? O14 C114 1.430(4) . ? O14 C111 1.451(4) . ? O15 C114 1.424(4) . ? O15 C113 1.427(4) . ? O16 C113 1.430(4) . ? O16 C116 1.452(4) . ? C111 C117 1.506(5) . ? C111 C112 1.523(4) . ? C112 C113 1.508(5) . ? C112 H11A 0.9700 . ? C112 H11B 0.9700 . ? C113 C118 1.502(5) . ? C114 C119 1.501(4) . ? C114 C115 1.509(5) . ? C115 C116 1.521(4) . ? C115 H11C 0.9700 . ? C115 H11D 0.9700 . ? C116 C120 1.509(5) . ? C117 H11E 0.9600 . ? C117 H11F 0.9600 . ? C117 H11G 0.9600 . ? C118 H11H 0.9600 . ? C118 H11I 0.9600 . ? C118 H11J 0.9600 . ? C119 H11K 0.9600 . ? C119 H11L 0.9600 . ? C119 H11M 0.9600 . ? C120 H12A 0.9600 . ? C120 H12B 0.9600 . ? C120 H12C 0.9600 . ? C121 C122 1.522(5) . ? C121 H12D 0.9700 . ? C121 H12E 0.9700 . ? C122 C123 1.513(5) . ? C122 H12F 0.9700 . ? C122 H12G 0.9700 . ? C123 C124 1.524(6) . ? C123 H12H 0.9700 . ? C123 H12I 0.9700 . ? C124 C125 1.517(6) . ? C124 H12J 0.9700 . ? C124 H12K 0.9700 . ? C125 H12L 0.9600 . ? C125 H12M 0.9600 . ? C125 H12N 0.9600 . ? Co2 C22 1.761(4) . ? Co2 C21 1.781(4) . ? Co2 C23 1.799(4) . ? Co2 P2 2.1882(11) . ? Co2 Co2 2.6717(12) 2_656 ? P2 C221 1.839(4) . ? P2 C216 1.861(3) . ? P2 C211 1.877(4) . ? O21 C21 1.146(4) . ? O22 C22 1.149(5) . ? O23 C23 1.144(5) . ? O24 C214 1.436(4) . ? O24 C211 1.444(4) . ? O25 C213 1.413(4) . ? O25 C214 1.426(4) . ? O26 C213 1.434(4) . ? O26 C216 1.454(4) . ? C211 C217 1.514(5) . ? C211 C212 1.524(5) . ? C212 C213 1.508(5) . ? C212 H21A 0.9700 . ? C212 H21B 0.9700 . ? C213 C218 1.505(5) . ? C214 C219 1.505(5) . ? C214 C215 1.510(5) . ? C215 C216 1.519(5) . ? C215 H21C 0.9700 . ? C215 H21D 0.9700 . ? C216 C220 1.523(5) . ? C217 H21E 0.9600 . ? C217 H21F 0.9600 . ? C217 H21G 0.9600 . ? C218 H21H 0.9600 . ? C218 H21I 0.9600 . ? C218 H21J 0.9600 . ? C219 H21K 0.9600 . ? C219 H21L 0.9600 . ? C219 H21M 0.9600 . ? C220 H22A 0.9600 . ? C220 H22B 0.9600 . ? C220 H22C 0.9600 . ? C221 C222 1.508(5) . ? C221 H22D 0.9700 . ? C221 H22E 0.9700 . ? C222 C223 1.504(5) . ? C222 H22F 0.9700 . ? C222 H22G 0.9700 . ? C223 C224 1.491(5) . ? C223 H22H 0.9700 . ? C223 H22I 0.9700 . ? C224 C225 1.503(6) . ? C224 H22J 0.9700 . ? C224 H22K 0.9700 . ? C225 H22L 0.9600 . ? C225 H22M 0.9600 . ? C225 H22N 0.9600 . ? Co3 C33 1.763(4) . ? Co3 C32 1.787(4) . ? Co3 C31 1.791(4) . ? Co3 P3 2.1857(12) . ? Co3 Co3 2.6725(12) 2_677 ? P3 C321 1.827(3) . ? P3 C311 1.871(4) . ? P3 C316 1.871(3) . ? O31 C31 1.144(4) . ? O32 C32 1.142(5) . ? O33 C33 1.153(4) . ? O34 C314 1.447(4) . ? O34 C311 1.456(4) . ? O35 C314 1.413(5) . ? O35 C313 1.419(5) . ? O36 C313 1.435(5) . ? O36 C316 1.448(4) . ? C311 C312 1.513(5) . ? C311 C317 1.526(5) . ? C312 C313 1.517(5) . ? C312 H31A 0.9700 . ? C312 H31B 0.9700 . ? C313 C318 1.508(5) . ? C314 C319 1.497(5) . ? C314 C315 1.515(5) . ? C315 C316 1.514(5) . ? C315 H31C 0.9700 . ? C315 H31D 0.9700 . ? C316 C320 1.509(5) . ? C317 H31E 0.9600 . ? C317 H31F 0.9600 . ? C317 H31G 0.9600 . ? C318 H31H 0.9600 . ? C318 H31I 0.9600 . ? C318 H31J 0.9600 . ? C319 H31K 0.9600 . ? C319 H31L 0.9600 . ? C319 H31M 0.9600 . ? C320 H32A 0.9600 . ? C320 H32B 0.9600 . ? C320 H32C 0.9600 . ? C321 C322 1.530(5) . ? C321 H32D 0.9700 . ? C321 H32E 0.9700 . ? C322 C326 1.468(11) . ? C322 C323 1.588(9) . ? C322 H10A 0.9700 . ? C322 H10B 0.9700 . ? C322 H10C 0.9700 . ? C322 H10D 0.9700 . ? C323 C324 1.495(11) . ? C323 H32F 0.9700 . ? C323 H32G 0.9700 . ? C324 C325 1.509(12) . ? C324 H32H 0.9700 . ? C324 H32I 0.9700 . ? C325 H32J 0.9600 . ? C325 H32K 0.9600 . ? C325 H32L 0.9600 . ? C326 C327 1.517(19) . ? C326 H32M 0.9700 . ? C326 H32N 0.9700 . ? C327 C328 1.54(2) . ? C327 H32O 0.9700 . ? C327 H32P 0.9700 . ? C328 H32Q 0.9600 . ? C328 H32R 0.9600 . ? C328 H32S 0.9600 . ? C1 C2 1.426(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.525(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.598(12) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.462(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C5 1.374(13) 2_765 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Co1 C12 119.91(18) . . ? C11 Co1 C13 117.94(18) . . ? C12 Co1 C13 119.79(18) . . ? C11 Co1 P1 92.15(11) . . ? C12 Co1 P1 95.94(11) . . ? C13 Co1 P1 97.25(11) . . ? C11 Co1 Co1 82.98(11) . 2_766 ? C12 Co1 Co1 84.39(11) . 2_766 ? C13 Co1 Co1 87.29(11) . 2_766 ? P1 Co1 Co1 174.52(4) . 2_766 ? C121 P1 C116 104.11(15) . . ? C121 P1 C111 104.69(15) . . ? C116 P1 C111 93.82(15) . . ? C121 P1 Co1 115.11(11) . . ? C116 P1 Co1 116.33(10) . . ? C111 P1 Co1 119.77(11) . . ? C114 O14 C111 115.7(2) . . ? C114 O15 C113 112.1(2) . . ? C113 O16 C116 116.1(2) . . ? O11 C11 Co1 178.7(3) . . ? O12 C12 Co1 179.6(3) . . ? O13 C13 Co1 176.9(3) . . ? O14 C111 C117 105.1(3) . . ? O14 C111 C112 108.7(3) . . ? C117 C111 C112 113.2(3) . . ? O14 C111 P1 109.3(2) . . ? C117 C111 P1 113.1(2) . . ? C112 C111 P1 107.4(2) . . ? C113 C112 C111 110.9(3) . . ? C113 C112 H11A 109.5 . . ? C111 C112 H11A 109.5 . . ? C113 C112 H11B 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 108.0 . . ? O15 C113 O16 110.4(3) . . ? O15 C113 C118 107.3(3) . . ? O16 C113 C118 106.5(3) . . ? O15 C113 C112 107.2(3) . . ? O16 C113 C112 111.8(3) . . ? C118 C113 C112 113.6(3) . . ? O15 C114 O14 110.9(3) . . ? O15 C114 C119 107.0(3) . . ? O14 C114 C119 106.6(3) . . ? O15 C114 C115 108.6(3) . . ? O14 C114 C115 110.5(3) . . ? C119 C114 C115 113.3(3) . . ? C114 C115 C116 110.8(3) . . ? C114 C115 H11C 109.5 . . ? C116 C115 H11C 109.5 . . ? C114 C115 H11D 109.5 . . ? C116 C115 H11D 109.5 . . ? H11C C115 H11D 108.1 . . ? O16 C116 C120 105.5(3) . . ? O16 C116 C115 108.9(2) . . ? C120 C116 C115 112.4(3) . . ? O16 C116 P1 106.8(2) . . ? C120 C116 P1 113.4(2) . . ? C115 C116 P1 109.6(2) . . ? C111 C117 H11E 109.5 . . ? C111 C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? C111 C117 H11G 109.5 . . ? H11E C117 H11G 109.5 . . ? H11F C117 H11G 109.5 . . ? C113 C118 H11H 109.5 . . ? C113 C118 H11I 109.5 . . ? H11H C118 H11I 109.5 . . ? C113 C118 H11J 109.5 . . ? H11H C118 H11J 109.5 . . ? H11I C118 H11J 109.5 . . ? C114 C119 H11K 109.5 . . ? C114 C119 H11L 109.5 . . ? H11K C119 H11L 109.5 . . ? C114 C119 H11M 109.5 . . ? H11K C119 H11M 109.5 . . ? H11L C119 H11M 109.5 . . ? C116 C120 H12A 109.5 . . ? C116 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C116 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C122 C121 P1 116.4(2) . . ? C122 C121 H12D 108.2 . . ? P1 C121 H12D 108.2 . . ? C122 C121 H12E 108.2 . . ? P1 C121 H12E 108.2 . . ? H12D C121 H12E 107.4 . . ? C123 C122 C121 111.7(3) . . ? C123 C122 H12F 109.3 . . ? C121 C122 H12F 109.3 . . ? C123 C122 H12G 109.3 . . ? C121 C122 H12G 109.3 . . ? H12F C122 H12G 107.9 . . ? C122 C123 C124 113.7(3) . . ? C122 C123 H12H 108.8 . . ? C124 C123 H12H 108.8 . . ? C122 C123 H12I 108.8 . . ? C124 C123 H12I 108.8 . . ? H12H C123 H12I 107.7 . . ? C125 C124 C123 114.0(3) . . ? C125 C124 H12J 108.8 . . ? C123 C124 H12J 108.8 . . ? C125 C124 H12K 108.8 . . ? C123 C124 H12K 108.8 . . ? H12J C124 H12K 107.7 . . ? C124 C125 H12L 109.5 . . ? C124 C125 H12M 109.5 . . ? H12L C125 H12M 109.5 . . ? C124 C125 H12N 109.5 . . ? H12L C125 H12N 109.5 . . ? H12M C125 H12N 109.5 . . ? C22 Co2 C21 120.4(2) . . ? C22 Co2 C23 119.1(2) . . ? C21 Co2 C23 118.10(18) . . ? C22 Co2 P2 91.81(12) . . ? C21 Co2 P2 96.36(11) . . ? C23 Co2 P2 97.42(11) . . ? C22 Co2 Co2 82.43(12) . 2_656 ? C21 Co2 Co2 84.82(10) . 2_656 ? C23 Co2 Co2 87.27(11) . 2_656 ? P2 Co2 Co2 173.87(4) . 2_656 ? C221 P2 C216 105.08(16) . . ? C221 P2 C211 103.42(17) . . ? C216 P2 C211 93.47(16) . . ? C221 P2 Co2 116.14(12) . . ? C216 P2 Co2 119.06(11) . . ? C211 P2 Co2 116.40(11) . . ? C214 O24 C211 115.6(3) . . ? C213 O25 C214 112.0(3) . . ? C213 O26 C216 115.3(2) . . ? O21 C21 Co2 179.1(3) . . ? O22 C22 Co2 178.2(4) . . ? O23 C23 Co2 178.2(3) . . ? O24 C211 C217 105.1(3) . . ? O24 C211 C212 108.9(3) . . ? C217 C211 C212 112.5(3) . . ? O24 C211 P2 107.4(2) . . ? C217 C211 P2 112.8(3) . . ? C212 C211 P2 109.9(2) . . ? C213 C212 C211 110.2(3) . . ? C213 C212 H21A 109.6 . . ? C211 C212 H21A 109.6 . . ? C213 C212 H21B 109.6 . . ? C211 C212 H21B 109.6 . . ? H21A C212 H21B 108.1 . . ? O25 C213 O26 111.8(3) . . ? O25 C213 C218 107.0(3) . . ? O26 C213 C218 105.8(3) . . ? O25 C213 C212 108.5(3) . . ? O26 C213 C212 110.2(3) . . ? C218 C213 C212 113.6(3) . . ? O25 C214 O24 110.2(3) . . ? O25 C214 C219 107.8(3) . . ? O24 C214 C219 106.4(3) . . ? O25 C214 C215 107.7(3) . . ? O24 C214 C215 111.1(3) . . ? C219 C214 C215 113.5(3) . . ? C214 C215 C216 111.2(3) . . ? C214 C215 H21C 109.4 . . ? C216 C215 H21C 109.4 . . ? C214 C215 H21D 109.4 . . ? C216 C215 H21D 109.4 . . ? H21C C215 H21D 108.0 . . ? O26 C216 C215 108.7(3) . . ? O26 C216 C220 104.8(3) . . ? C215 C216 C220 113.8(3) . . ? O26 C216 P2 109.5(2) . . ? C215 C216 P2 107.6(2) . . ? C220 C216 P2 112.4(2) . . ? C211 C217 H21E 109.5 . . ? C211 C217 H21F 109.5 . . ? H21E C217 H21F 109.5 . . ? C211 C217 H21G 109.5 . . ? H21E C217 H21G 109.5 . . ? H21F C217 H21G 109.5 . . ? C213 C218 H21H 109.5 . . ? C213 C218 H21I 109.5 . . ? H21H C218 H21I 109.5 . . ? C213 C218 H21J 109.5 . . ? H21H C218 H21J 109.5 . . ? H21I C218 H21J 109.5 . . ? C214 C219 H21K 109.5 . . ? C214 C219 H21L 109.5 . . ? H21K C219 H21L 109.5 . . ? C214 C219 H21M 109.5 . . ? H21K C219 H21M 109.5 . . ? H21L C219 H21M 109.5 . . ? C216 C220 H22A 109.5 . . ? C216 C220 H22B 109.5 . . ? H22A C220 H22B 109.5 . . ? C216 C220 H22C 109.5 . . ? H22A C220 H22C 109.5 . . ? H22B C220 H22C 109.5 . . ? C222 C221 P2 117.4(2) . . ? C222 C221 H22D 107.9 . . ? P2 C221 H22D 107.9 . . ? C222 C221 H22E 107.9 . . ? P2 C221 H22E 107.9 . . ? H22D C221 H22E 107.2 . . ? C223 C222 C221 113.5(3) . . ? C223 C222 H22F 108.9 . . ? C221 C222 H22F 108.9 . . ? C223 C222 H22G 108.9 . . ? C221 C222 H22G 108.9 . . ? H22F C222 H22G 107.7 . . ? C224 C223 C222 116.8(3) . . ? C224 C223 H22H 108.1 . . ? C222 C223 H22H 108.1 . . ? C224 C223 H22I 108.1 . . ? C222 C223 H22I 108.1 . . ? H22H C223 H22I 107.3 . . ? C223 C224 C225 115.9(4) . . ? C223 C224 H22J 108.3 . . ? C225 C224 H22J 108.3 . . ? C223 C224 H22K 108.3 . . ? C225 C224 H22K 108.3 . . ? H22J C224 H22K 107.4 . . ? C224 C225 H22L 109.5 . . ? C224 C225 H22M 109.5 . . ? H22L C225 H22M 109.5 . . ? C224 C225 H22N 109.5 . . ? H22L C225 H22N 109.5 . . ? H22M C225 H22N 109.5 . . ? C33 Co3 C32 118.72(18) . . ? C33 Co3 C31 120.54(17) . . ? C32 Co3 C31 118.09(18) . . ? C33 Co3 P3 89.77(12) . . ? C32 Co3 P3 99.40(13) . . ? C31 Co3 P3 97.17(12) . . ? C33 Co3 Co3 80.74(12) . 2_677 ? C32 Co3 Co3 88.27(13) . 2_677 ? C31 Co3 Co3 84.84(12) . 2_677 ? P3 Co3 Co3 169.90(4) . 2_677 ? C321 P3 C311 103.79(17) . . ? C321 P3 C316 104.40(15) . . ? C311 P3 C316 93.89(16) . . ? C321 P3 Co3 116.05(13) . . ? C311 P3 Co3 122.05(12) . . ? C316 P3 Co3 113.34(12) . . ? C314 O34 C311 115.5(3) . . ? C314 O35 C313 112.0(3) . . ? C313 O36 C316 116.3(3) . . ? O31 C31 Co3 178.1(4) . . ? O32 C32 Co3 177.3(4) . . ? O33 C33 Co3 176.4(3) . . ? O34 C311 C312 108.9(3) . . ? O34 C311 C317 104.3(3) . . ? C312 C311 C317 113.4(3) . . ? O34 C311 P3 109.8(2) . . ? C312 C311 P3 106.9(3) . . ? C317 C311 P3 113.4(3) . . ? C311 C312 C313 110.7(3) . . ? C311 C312 H31A 109.5 . . ? C313 C312 H31A 109.5 . . ? C311 C312 H31B 109.5 . . ? C313 C312 H31B 109.5 . . ? H31A C312 H31B 108.1 . . ? O35 C313 O36 110.4(3) . . ? O35 C313 C318 108.2(3) . . ? O36 C313 C318 106.4(3) . . ? O35 C313 C312 108.1(3) . . ? O36 C313 C312 111.2(3) . . ? C318 C313 C312 112.6(3) . . ? O35 C314 O34 110.7(3) . . ? O35 C314 C319 108.0(3) . . ? O34 C314 C319 107.3(3) . . ? O35 C314 C315 108.4(3) . . ? O34 C314 C315 110.3(3) . . ? C319 C314 C315 112.1(3) . . ? C316 C315 C314 111.2(3) . . ? C316 C315 H31C 109.4 . . ? C314 C315 H31C 109.4 . . ? C316 C315 H31D 109.4 . . ? C314 C315 H31D 109.4 . . ? H31C C315 H31D 108.0 . . ? O36 C316 C320 106.1(3) . . ? O36 C316 C315 107.5(3) . . ? C320 C316 C315 112.4(3) . . ? O36 C316 P3 106.7(2) . . ? C320 C316 P3 112.8(2) . . ? C315 C316 P3 110.9(2) . . ? C311 C317 H31E 109.5 . . ? C311 C317 H31F 109.5 . . ? H31E C317 H31F 109.5 . . ? C311 C317 H31G 109.5 . . ? H31E C317 H31G 109.5 . . ? H31F C317 H31G 109.5 . . ? C313 C318 H31H 109.5 . . ? C313 C318 H31I 109.5 . . ? H31H C318 H31I 109.5 . . ? C313 C318 H31J 109.5 . . ? H31H C318 H31J 109.5 . . ? H31I C318 H31J 109.5 . . ? C314 C319 H31K 109.5 . . ? C314 C319 H31L 109.5 . . ? H31K C319 H31L 109.5 . . ? C314 C319 H31M 109.5 . . ? H31K C319 H31M 109.5 . . ? H31L C319 H31M 109.5 . . ? C316 C320 H32A 109.5 . . ? C316 C320 H32B 109.5 . . ? H32A C320 H32B 109.5 . . ? C316 C320 H32C 109.5 . . ? H32A C320 H32C 109.5 . . ? H32B C320 H32C 109.5 . . ? C322 C321 P3 116.0(3) . . ? C322 C321 H32D 108.3 . . ? P3 C321 H32D 108.3 . . ? C322 C321 H32E 108.3 . . ? P3 C321 H32E 108.3 . . ? H32D C321 H32E 107.4 . . ? C326 C322 C321 118.0(6) . . ? C326 C322 C323 32.1(5) . . ? C321 C322 C323 109.3(4) . . ? C326 C322 H10A 126.2 . . ? C321 C322 H10A 109.8 . . ? C323 C322 H10A 109.8 . . ? C326 C322 H10B 78.0 . . ? C321 C322 H10B 109.8 . . ? C323 C322 H10B 109.8 . . ? H10A C322 H10B 108.3 . . ? C326 C322 H10C 107.8 . . ? C321 C322 H10C 107.8 . . ? C323 C322 H10C 136.2 . . ? H10A C322 H10C 78.0 . . ? H10B C322 H10C 33.8 . . ? C326 C322 H10D 107.8 . . ? C321 C322 H10D 107.8 . . ? C323 C322 H10D 82.8 . . ? H10A C322 H10D 30.4 . . ? H10B C322 H10D 132.8 . . ? H10C C322 H10D 107.1 . . ? C324 C323 C322 115.9(6) . . ? C324 C323 H32F 108.3 . . ? C322 C323 H32F 108.3 . . ? C324 C323 H32G 108.3 . . ? C322 C323 H32G 108.3 . . ? H32F C323 H32G 107.4 . . ? C323 C324 C325 112.6(8) . . ? C323 C324 H32H 109.1 . . ? C325 C324 H32H 109.1 . . ? C323 C324 H32I 109.1 . . ? C325 C324 H32I 109.1 . . ? H32H C324 H32I 107.8 . . ? C322 C326 C327 107.1(10) . . ? C322 C326 H32M 110.3 . . ? C327 C326 H32M 110.3 . . ? C322 C326 H32N 110.3 . . ? C327 C326 H32N 110.3 . . ? H32M C326 H32N 108.6 . . ? C326 C327 C328 110.9(11) . . ? C326 C327 H32O 109.5 . . ? C328 C327 H32O 109.5 . . ? C326 C327 H32P 109.5 . . ? C328 C327 H32P 109.5 . . ? H32O C327 H32P 108.0 . . ? C327 C328 H32Q 109.5 . . ? C327 C328 H32R 109.5 . . ? H32Q C328 H32R 109.5 . . ? C327 C328 H32S 109.5 . . ? H32Q C328 H32S 109.5 . . ? H32R C328 H32S 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 114.3(7) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 C4 120.7(7) . . ? C2 C3 H3A 107.1 . . ? C4 C3 H3A 107.1 . . ? C2 C3 H3B 107.1 . . ? C4 C3 H3B 107.1 . . ? H3A C3 H3B 106.8 . . ? C5 C4 C3 107.1(7) . . ? C5 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? C5 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.6 . . ? C5 C5 C4 123.3(11) 2_765 . ? C5 C5 H5A 106.5 2_765 . ? C4 C5 H5A 106.5 . . ? C5 C5 H5B 106.5 2_765 . ? C4 C5 H5B 106.5 . . ? H5A C5 H5B 106.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.472 _refine_diff_density_min -0.966 _refine_diff_density_rms 0.094 #========================================================================== # 4. TEXT _publ_section_abstract ; See text. ; _publ_section_comment ; See text. ; _publ_section_exptl_prep ; See text. ; _publ_section_exptl_refinement ; The intensity data was collected on a Bruker SMART 1K CCD diffractometer using an exposure time of 20 seconds/frame. A total of 1315 frames were collected with a frame width of 0.3\% covering up to \q = 26.36\% with 99.5% completeness accomplished. ; _publ_section_references ; Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Bruker (1998). SMART-NT (Version 5.050). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SAINT+. Version 6.02 (including XPREP). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SADABS (Version 2004/1). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. ; _publ_section_figure_captions ; See text. ; _publ_section_acknowledgements ; See text. ; #=========================================================================== # data_pcy3dim _database_code_depnum_ccdc_archive 'CCDC 774591' #TrackingRef '- Bungu Otto Oxo3 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexacarbonyl-bis(tricyclohexylphosphine)-dicobalt ; _chemical_name_common Hexacarbonyl-bis(tricyclohexylphosphine)-dicobalt _chemical_melting_point ? _chemical_formula_moiety 'C42 H66 Co2 O6 P2' _chemical_formula_sum 'C42 H66 Co2 O6 P2' _chemical_formula_weight 846.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 14.7630(5) _cell_length_b 10.6770(3) _cell_length_c 14.8800(4) _cell_angle_alpha 90.00 _cell_angle_beta 119.2980(10) _cell_angle_gamma 90.00 _cell_volume 2045.44(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7462 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.30 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.887 _exptl_absorpt_process_details ; SADABS (Bruker, 2004) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART ApexII 4K CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 'First 50 frames repeated after data collection.' __diffrn_standards_interval_count 'After collection' _diffrn_standards_interval_time 'After collection' _diffrn_standards_decay_% None _diffrn_reflns_number 34166 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5100 _reflns_number_gt 4548 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^ > 2\s(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^)+(0.0274P)^2^+0.9093P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5100 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Co Co 0.580074(12) 0.454871(14) -0.006593(11) 0.00920(5) Uani 1 1 d . . . P P 0.71724(2) 0.37484(3) -0.00615(2) 0.00866(6) Uani 1 1 d . . . O1 O 0.42464(7) 0.29775(9) -0.17123(7) 0.01996(19) Uani 1 1 d . . . O2 O 0.61014(7) 0.71295(8) -0.05371(7) 0.0206(2) Uani 1 1 d . . . O3 O 0.64640(7) 0.35978(9) 0.20073(7) 0.01932(19) Uani 1 1 d . . . C1 C 0.48586(9) 0.36029(11) -0.10807(9) 0.0132(2) Uani 1 1 d . . . C2 C 0.59998(9) 0.61182(11) -0.03430(9) 0.0139(2) Uani 1 1 d . . . C3 C 0.62063(9) 0.40061(11) 0.12052(9) 0.0132(2) Uani 1 1 d . . . C11 C 0.74715(9) 0.21490(10) 0.05100(9) 0.0103(2) Uani 1 1 d . . . H11 H 0.7745 0.2274 0.1251 0.012 Uiso 1 1 calc R . . C12 C 0.65026(9) 0.13186(11) 0.01573(9) 0.0119(2) Uani 1 1 d . . . H12A H 0.6004 0.1746 0.0295 0.014 Uiso 1 1 calc R . . H12B H 0.6181 0.1181 -0.0580 0.014 Uiso 1 1 calc R . . C13 C 0.67804(10) 0.00566(11) 0.07129(10) 0.0148(2) Uani 1 1 d . . . H13A H 0.7030 0.0188 0.1442 0.018 Uiso 1 1 calc R . . H13B H 0.6163 -0.0462 0.0445 0.018 Uiso 1 1 calc R . . C14 C 0.76123(10) -0.06190(11) 0.05727(10) 0.0147(2) Uani 1 1 d . . . H14A H 0.7785 -0.1406 0.0946 0.018 Uiso 1 1 calc R . . H14B H 0.7349 -0.0802 -0.0152 0.018 Uiso 1 1 calc R . . C15 C 0.85815(9) 0.01900(11) 0.09696(9) 0.0140(2) Uani 1 1 d . . . H15A H 0.9099 -0.0244 0.0864 0.017 Uiso 1 1 calc R . . H15B H 0.8869 0.0326 0.1704 0.017 Uiso 1 1 calc R . . C16 C 0.83359(9) 0.14549(11) 0.04165(10) 0.0139(2) Uani 1 1 d . . . H16A H 0.8119 0.1324 -0.0306 0.017 Uiso 1 1 calc R . . H16B H 0.8958 0.1967 0.0712 0.017 Uiso 1 1 calc R . . C21 C 0.71178(9) 0.36659(11) -0.13370(8) 0.0107(2) Uani 1 1 d . . . H21 H 0.7833 0.3579 -0.1205 0.013 Uiso 1 1 calc R . . C22 C 0.64927(9) 0.25655(11) -0.20316(9) 0.0130(2) Uani 1 1 d . . . H22A H 0.6744 0.1785 -0.1657 0.016 Uiso 1 1 calc R . . H22B H 0.5766 0.2655 -0.2224 0.016 Uiso 1 1 calc R . . C23 C 0.66015(10) 0.25334(11) -0.30040(9) 0.0153(2) Uani 1 1 d . . . H23A H 0.7321 0.2369 -0.2809 0.018 Uiso 1 1 calc R . . H23B H 0.6186 0.1851 -0.3442 0.018 Uiso 1 1 calc R . . C24 C 0.62619(10) 0.37509(12) -0.36117(9) 0.0150(2) Uani 1 1 d . . . H24A H 0.5516 0.3844 -0.3913 0.018 Uiso 1 1 calc R . . H24B H 0.6425 0.3720 -0.4169 0.018 Uiso 1 1 calc R . . C25 C 0.68003(10) 0.48750(12) -0.29272(9) 0.0148(2) Uani 1 1 d . . . H25A H 0.6508 0.5639 -0.3315 0.018 Uiso 1 1 calc R . . H25B H 0.7533 0.4855 -0.2721 0.018 Uiso 1 1 calc R . . C26 C 0.66757(9) 0.48803(11) -0.19634(9) 0.0127(2) Uani 1 1 d . . . H26A H 0.5946 0.4955 -0.2166 0.015 Uiso 1 1 calc R . . H26B H 0.7037 0.5597 -0.1538 0.015 Uiso 1 1 calc R . . C31 C 0.84343(9) 0.45610(11) 0.07712(9) 0.0113(2) Uani 1 1 d . . . H31 H 0.8979 0.3941 0.0920 0.014 Uiso 1 1 calc R . . C32 C 0.85517(10) 0.49421(12) 0.18200(9) 0.0150(2) Uani 1 1 d . . . H32A H 0.8034 0.5570 0.1716 0.018 Uiso 1 1 calc R . . H32B H 0.8431 0.4218 0.2141 0.018 Uiso 1 1 calc R . . C33 C 0.96373(10) 0.54681(12) 0.25358(10) 0.0183(3) Uani 1 1 d . . . H33A H 0.9674 0.5740 0.3175 0.022 Uiso 1 1 calc R . . H33B H 1.0148 0.4811 0.2699 0.022 Uiso 1 1 calc R . . C34 C 0.98996(10) 0.65674(12) 0.20505(10) 0.0185(3) Uani 1 1 d . . . H34A H 0.9446 0.7267 0.1968 0.022 Uiso 1 1 calc R . . H34B H 1.0610 0.6830 0.2502 0.022 Uiso 1 1 calc R . . C35 C 0.97701(10) 0.62007(13) 0.10056(10) 0.0185(3) Uani 1 1 d . . . H35A H 1.0282 0.5570 0.1101 0.022 Uiso 1 1 calc R . . H35B H 0.9894 0.6928 0.0690 0.022 Uiso 1 1 calc R . . C36 C 0.86809(9) 0.56870(11) 0.02849(9) 0.0146(2) Uani 1 1 d . . . H36A H 0.8636 0.5434 -0.0362 0.017 Uiso 1 1 calc R . . H36B H 0.8171 0.6341 0.0139 0.017 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 Co 0.00953(8) 0.00909(8) 0.00940(8) 0.00012(5) 0.00496(6) 0.00122(5) P 0.00961(13) 0.00827(13) 0.00841(13) 0.00010(10) 0.00465(11) 0.00044(10) O1 0.0181(4) 0.0209(5) 0.0166(4) -0.0051(4) 0.0052(4) -0.0011(4) O2 0.0209(5) 0.0138(4) 0.0276(5) 0.0015(4) 0.0122(4) -0.0015(4) O3 0.0197(5) 0.0256(5) 0.0126(4) 0.0027(4) 0.0078(4) 0.0019(4) C1 0.0140(5) 0.0147(6) 0.0132(5) 0.0025(4) 0.0085(5) 0.0040(4) C2 0.0113(5) 0.0160(6) 0.0145(6) -0.0015(4) 0.0064(5) 0.0011(4) C3 0.0114(5) 0.0135(5) 0.0159(6) -0.0028(4) 0.0077(5) 0.0009(4) C11 0.0116(5) 0.0089(5) 0.0103(5) 0.0011(4) 0.0053(4) 0.0009(4) C12 0.0123(5) 0.0109(5) 0.0129(5) 0.0005(4) 0.0066(4) -0.0002(4) C13 0.0176(6) 0.0114(5) 0.0168(6) 0.0013(4) 0.0096(5) -0.0009(4) C14 0.0177(6) 0.0099(5) 0.0157(6) -0.0002(4) 0.0075(5) 0.0005(4) C15 0.0143(6) 0.0113(5) 0.0145(6) 0.0004(4) 0.0057(5) 0.0028(4) C16 0.0133(5) 0.0119(5) 0.0181(6) 0.0016(4) 0.0090(5) 0.0023(4) C21 0.0120(5) 0.0118(5) 0.0098(5) -0.0003(4) 0.0064(4) -0.0002(4) C22 0.0172(6) 0.0118(5) 0.0113(5) -0.0011(4) 0.0078(5) -0.0010(4) C23 0.0205(6) 0.0149(6) 0.0129(5) -0.0024(4) 0.0101(5) -0.0012(5) C24 0.0166(6) 0.0181(6) 0.0112(5) -0.0001(4) 0.0075(5) -0.0015(5) C25 0.0176(6) 0.0159(6) 0.0119(5) 0.0016(4) 0.0080(5) -0.0027(5) C26 0.0152(6) 0.0118(5) 0.0108(5) 0.0007(4) 0.0062(5) -0.0008(4) C31 0.0097(5) 0.0116(5) 0.0113(5) -0.0001(4) 0.0041(4) 0.0001(4) C32 0.0167(6) 0.0166(6) 0.0109(5) -0.0010(4) 0.0061(5) -0.0029(5) C33 0.0173(6) 0.0206(6) 0.0120(6) -0.0014(5) 0.0032(5) -0.0023(5) C34 0.0151(6) 0.0181(6) 0.0182(6) -0.0045(5) 0.0050(5) -0.0039(5) C35 0.0148(6) 0.0212(6) 0.0188(6) -0.0023(5) 0.0075(5) -0.0057(5) C36 0.0146(6) 0.0159(6) 0.0133(5) -0.0005(4) 0.0068(5) -0.0039(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Co C1 1.7830(12) . ? Co C2 1.7841(13) . ? Co C3 1.7787(12) . ? Co P 2.1949(3) . ? Co Co 2.6478(3) 3_665 ? P C11 1.8619(11) . ? P C21 1.8619(11) . ? P C31 1.8707(12) . ? O1 C1 1.1466(15) . ? O2 C2 1.1463(15) . ? O3 C3 1.1466(15) . ? C11 C16 1.5398(16) . ? C11 C12 1.5403(16) . ? C11 H11 0.9800 . ? C12 C13 1.5282(16) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.5242(17) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.5215(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.5300(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C21 C22 1.5384(16) . ? C21 C26 1.5429(16) . ? C21 H21 0.9800 . ? C22 C23 1.5324(16) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.5215(17) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.5222(17) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.5327(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C31 C36 1.5361(16) . ? C31 C32 1.5383(16) . ? C31 H31 0.9800 . ? C32 C33 1.5322(17) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.5240(18) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.5220(18) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.5325(17) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Co C1 115.68(5) . . ? C3 Co C2 122.95(5) . . ? C1 Co C2 118.99(5) . . ? C3 Co P 92.29(4) . . ? C1 Co P 96.79(4) . . ? C2 Co P 96.33(4) . . ? C3 Co Co 83.56(4) . 3_665 ? C1 Co Co 85.07(4) . 3_665 ? C2 Co Co 85.95(4) . 3_665 ? P Co Co 175.855(13) . 3_665 ? C11 P C21 107.73(5) . . ? C11 P C31 100.73(5) . . ? C21 P C31 103.27(5) . . ? C11 P Co 111.76(4) . . ? C21 P Co 115.83(4) . . ? C31 P Co 116.08(4) . . ? O1 C1 Co 177.94(11) . . ? O2 C2 Co 178.28(12) . . ? O3 C3 Co 176.66(11) . . ? C16 C11 C12 111.39(9) . . ? C16 C11 P 114.95(8) . . ? C12 C11 P 113.53(8) . . ? C16 C11 H11 105.3 . . ? C12 C11 H11 105.3 . . ? P C11 H11 105.3 . . ? C13 C12 C11 111.38(9) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 111.35(10) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 110.24(10) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 111.22(10) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C11 111.40(10) . . ? C15 C16 H16A 109.3 . . ? C11 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C11 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C22 C21 C26 107.38(9) . . ? C22 C21 P 115.69(8) . . ? C26 C21 P 111.75(8) . . ? C22 C21 H21 107.2 . . ? C26 C21 H21 107.2 . . ? P C21 H21 107.2 . . ? C23 C22 C21 110.23(10) . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 112.69(10) . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23B 109.1 . . ? C22 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C23 C24 C25 111.32(10) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 111.50(10) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C21 110.68(10) . . ? C25 C26 H26A 109.5 . . ? C21 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C36 C31 C32 109.63(9) . . ? C36 C31 P 116.09(8) . . ? C32 C31 P 112.09(8) . . ? C36 C31 H31 106.1 . . ? C32 C31 H31 106.1 . . ? P C31 H31 106.1 . . ? C33 C32 C31 111.25(10) . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 112.01(10) . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 110.60(10) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.79(10) . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C31 111.10(10) . . ? C35 C36 H36A 109.4 . . ? C31 C36 H36A 109.4 . . ? C35 C36 H36B 109.4 . . ? C31 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.396 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.052 #========================================================================== # 4. TEXT _publ_section_abstract ; See text. ; _publ_section_comment ; See text. ; _publ_section_exptl_prep ; See text. ; _publ_section_exptl_refinement ; The intensity data was collected on a Bruker SMART 1K CCD diffractometer using an exposure time of 20 seconds/frame. A total of 1315 frames were collected with a frame width of 0.3\% covering up to \q = 26.36\% with 99.5% completeness accomplished. ; _publ_section_references ; Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Bruker (1998). SMART-NT (Version 5.050). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SAINT+. Version 6.02 (including XPREP). Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2004). SADABS (Version 2004/1). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. ; _publ_section_figure_captions ; See text. ; _publ_section_acknowledgements ; See text. ; #========================================================================== data_9lfo5_all _database_code_depnum_ccdc_archive 'CCDC 774592' #TrackingRef '- Bungu Otto Oxo3 cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexacarbonyl-bis(tricyclopentylphosphine)-dicobalt ; _chemical_name_common Hexacarbonyl-bis(tricyclopentylphosphine)-dicobalt _chemical_melting_point ? _chemical_formula_moiety 'C36 H54 Co2 O6 P2' _chemical_formula_sum 'C36 H54 Co2 O6 P2' _chemical_formula_weight 762.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.0823(7) _cell_length_b 11.8940(9) _cell_length_c 15.1109(11) _cell_angle_alpha 86.804(2) _cell_angle_beta 88.797(3) _cell_angle_gamma 83.983(2) _cell_volume 1799.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6712 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.45 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details ; SADABS (Bruker, 2004) ; _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 'Bruker X8 ApexII 4K Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number 'First 50 frames repeated after data collection.' __diffrn_standards_interval_count 'After collection' _diffrn_standards_interval_time 'After collection' _diffrn_standards_decay_% None _diffrn_reflns_number 25423 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8748 _reflns_number_gt 6880 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^ > 2\s(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^)+(0.1040P)^2^+2.9500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8748 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1717 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.56543(4) 0.91572(4) 0.45770(3) 0.01222(13) Uani 1 1 d . . . P1 P 0.65070(8) 0.76966(7) 0.38413(6) 0.01118(19) Uani 1 1 d . . . O11 O 0.3564(3) 0.7873(2) 0.53514(19) 0.0250(6) Uani 1 1 d . . . O12 O 0.5172(3) 1.0562(2) 0.29393(18) 0.0267(6) Uani 1 1 d . . . O13 O 0.7910(3) 0.9533(3) 0.5674(2) 0.0331(7) Uani 1 1 d . . . C11 C 0.4365(4) 0.8397(3) 0.5054(2) 0.0167(7) Uani 1 1 d . . . C12 C 0.5367(4) 1.0032(3) 0.3590(2) 0.0169(7) Uani 1 1 d . . . C13 C 0.7048(4) 0.9363(3) 0.5243(2) 0.0196(7) Uani 1 1 d . . . C111 C 0.6407(3) 0.6337(3) 0.4472(2) 0.0140(7) Uani 1 1 d . . . H111 H 0.5460 0.6216 0.4505 0.017 Uiso 1 1 calc R . . C112 C 0.7160(4) 0.5235(3) 0.4105(2) 0.0177(7) Uani 1 1 d . . . H11A H 0.6534 0.4767 0.3869 0.021 Uiso 1 1 calc R . . H11B H 0.7790 0.5422 0.3640 0.021 Uiso 1 1 calc R . . C113 C 0.7895(4) 0.4615(3) 0.4907(3) 0.0215(8) Uani 1 1 d . . . H11C H 0.7831 0.3806 0.4908 0.026 Uiso 1 1 calc R . . H11D H 0.8829 0.4744 0.4890 0.026 Uiso 1 1 calc R . . C114 C 0.7198(4) 0.5110(3) 0.5721(3) 0.0215(8) Uani 1 1 d . . . H11E H 0.7782 0.5019 0.6227 0.026 Uiso 1 1 calc R . . H11F H 0.6393 0.4755 0.5869 0.026 Uiso 1 1 calc R . . C115 C 0.6871(4) 0.6355(3) 0.5438(2) 0.0172(7) Uani 1 1 d . . . H11G H 0.7652 0.6762 0.5469 0.021 Uiso 1 1 calc R . . H11H H 0.6168 0.6707 0.5811 0.021 Uiso 1 1 calc R . . C121 C 0.5587(3) 0.7621(3) 0.2812(2) 0.0135(6) Uani 1 1 d . . . H121 H 0.5740 0.8303 0.2446 0.016 Uiso 1 1 calc R . . C122 C 0.4047(3) 0.7652(3) 0.2946(2) 0.0168(7) Uani 1 1 d . . . H12A H 0.3833 0.7248 0.3497 0.020 Uiso 1 1 calc R . . H12B H 0.3640 0.8427 0.2959 0.020 Uiso 1 1 calc R . . C123 C 0.3552(4) 0.7071(4) 0.2150(3) 0.0248(8) Uani 1 1 d . . . H12C H 0.3149 0.6394 0.2348 0.030 Uiso 1 1 calc R . . H12D H 0.2895 0.7579 0.1825 0.030 Uiso 1 1 calc R . . C124 C 0.4778(4) 0.6770(3) 0.1564(2) 0.0201(8) Uani 1 1 d . . . H12E H 0.4899 0.7373 0.1121 0.024 Uiso 1 1 calc R . . H12F H 0.4704 0.6075 0.1270 0.024 Uiso 1 1 calc R . . C125 C 0.5934(4) 0.6620(3) 0.2222(2) 0.0184(7) Uani 1 1 d . . . H12G H 0.5955 0.5902 0.2562 0.022 Uiso 1 1 calc R . . H12H H 0.6787 0.6667 0.1920 0.022 Uiso 1 1 calc R . . C131 C 0.8242(3) 0.7697(3) 0.3434(2) 0.0142(7) Uani 1 1 d . . . H131 H 0.8386 0.7134 0.2983 0.017 Uiso 1 1 calc R . . C132 C 0.8575(3) 0.8836(3) 0.3006(2) 0.0166(7) Uani 1 1 d . . . H13A H 0.8313 0.9450 0.3391 0.020 Uiso 1 1 calc R . . H13B H 0.8136 0.8998 0.2441 0.020 Uiso 1 1 calc R . . C133 C 1.0103(4) 0.8661(3) 0.2882(3) 0.0228(8) Uani 1 1 d . . . H13C H 1.0340 0.8358 0.2310 0.027 Uiso 1 1 calc R . . H13D H 1.0486 0.9371 0.2919 0.027 Uiso 1 1 calc R . . C134 C 1.0601(4) 0.7818(4) 0.3635(3) 0.0269(9) Uani 1 1 d . . . H13E H 1.1139 0.8177 0.4038 0.032 Uiso 1 1 calc R . . H13F H 1.1138 0.7175 0.3399 0.032 Uiso 1 1 calc R . . C135 C 0.9353(3) 0.7433(3) 0.4119(3) 0.0189(7) Uani 1 1 d . . . H13G H 0.9476 0.6630 0.4285 0.023 Uiso 1 1 calc R . . H13H H 0.9149 0.7850 0.4647 0.023 Uiso 1 1 calc R . . Co2 Co 0.05845(4) 0.40852(4) 0.04587(3) 0.01306(14) Uani 1 1 d . . . P2 P 0.14989(8) 0.25104(7) 0.11422(6) 0.01187(19) Uani 1 1 d . . . O21 O 0.3035(3) 0.4830(3) -0.0343(2) 0.0307(7) Uani 1 1 d . . . O22 O -0.1095(3) 0.2830(2) -0.0596(2) 0.0307(7) Uani 1 1 d . . . O23 O -0.0435(4) 0.5268(3) 0.2026(2) 0.0403(8) Uani 1 1 d . . . C21 C 0.2082(4) 0.4523(3) -0.0033(2) 0.0196(7) Uani 1 1 d . . . C22 C -0.0452(4) 0.3333(3) -0.0178(2) 0.0200(7) Uani 1 1 d . . . C23 C -0.0031(4) 0.4791(3) 0.1418(3) 0.0231(8) Uani 1 1 d . . . C211 C 0.3182(3) 0.2509(3) 0.1583(2) 0.0141(7) Uani 1 1 d . . . H211 H 0.3320 0.1873 0.2023 0.017 Uiso 1 1 calc R . . C212 C 0.4358(3) 0.2401(3) 0.0914(2) 0.0174(7) Uani 1 1 d . . . H21A H 0.4553 0.1623 0.0752 0.021 Uiso 1 1 calc R . . H21B H 0.4152 0.2876 0.0382 0.021 Uiso 1 1 calc R . . C213 C 0.5534(4) 0.2789(4) 0.1384(3) 0.0281(9) Uani 1 1 d . . . H21C H 0.6028 0.3264 0.0984 0.034 Uiso 1 1 calc R . . H21D H 0.6132 0.2142 0.1596 0.034 Uiso 1 1 calc R . . C214 C 0.4946(4) 0.3461(3) 0.2167(3) 0.0225(8) Uani 1 1 d . . . H21E H 0.5174 0.3052 0.2726 0.027 Uiso 1 1 calc R . . H21F H 0.5285 0.4195 0.2161 0.027 Uiso 1 1 calc R . . C215 C 0.3434(4) 0.3597(3) 0.2042(2) 0.0188(7) Uani 1 1 d . . . H21G H 0.3156 0.4269 0.1671 0.023 Uiso 1 1 calc R . . H21H H 0.2963 0.3642 0.2608 0.023 Uiso 1 1 calc R . . C221 C 0.0593(3) 0.1944(3) 0.2110(2) 0.0145(7) Uani 1 1 d . . . H221 H 0.1009 0.1172 0.2240 0.017 Uiso 1 1 calc R . . C222 C 0.0607(4) 0.2559(3) 0.2978(2) 0.0181(7) Uani 1 1 d . . . H22A H 0.1437 0.2357 0.3289 0.022 Uiso 1 1 calc R . . H22B H 0.0477 0.3374 0.2868 0.022 Uiso 1 1 calc R . . C223 C -0.0566(4) 0.2131(4) 0.3499(2) 0.0242(8) Uani 1 1 d . . . H22C H -0.0344 0.1363 0.3741 0.029 Uiso 1 1 calc R . . H22D H -0.0844 0.2616 0.3979 0.029 Uiso 1 1 calc R . . C224 C -0.1645(4) 0.2180(4) 0.2805(3) 0.0272(9) Uani 1 1 d . . . H22E H -0.2102 0.2938 0.2733 0.033 Uiso 1 1 calc R . . H22F H -0.2294 0.1657 0.2973 0.033 Uiso 1 1 calc R . . C225 C -0.0906(4) 0.1841(3) 0.1942(2) 0.0206(8) Uani 1 1 d . . . H22G H -0.1224 0.2344 0.1447 0.025 Uiso 1 1 calc R . . H22H H -0.1040 0.1071 0.1814 0.025 Uiso 1 1 calc R . . C231 C 0.1582(3) 0.1270(3) 0.0445(2) 0.0141(7) Uani 1 1 d . . . H231 H 0.0655 0.1134 0.0349 0.017 Uiso 1 1 calc R . . C232 C 0.2218(4) 0.1440(3) -0.0498(2) 0.0181(7) Uani 1 1 d . . . H23A H 0.1536 0.1527 -0.0947 0.022 Uiso 1 1 calc R . . H23B H 0.2700 0.2106 -0.0534 0.022 Uiso 1 1 calc R . . C233 C 0.3180(4) 0.0360(3) -0.0627(2) 0.0181(7) Uani 1 1 d . . . H23C H 0.3150 0.0126 -0.1230 0.022 Uiso 1 1 calc R . . H23D H 0.4089 0.0488 -0.0497 0.022 Uiso 1 1 calc R . . C234 C 0.2679(4) -0.0530(3) 0.0026(2) 0.0191(7) Uani 1 1 d . . . H23E H 0.3378 -0.1134 0.0166 0.023 Uiso 1 1 calc R . . H23F H 0.1921 -0.0850 -0.0207 0.023 Uiso 1 1 calc R . . C235 C 0.2277(4) 0.0145(3) 0.0842(2) 0.0174(7) Uani 1 1 d . . . H23G H 0.3054 0.0271 0.1177 0.021 Uiso 1 1 calc R . . H23H H 0.1672 -0.0246 0.1227 0.021 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0111(2) 0.0098(2) 0.0154(2) -0.00149(17) 0.00009(17) 0.00089(17) P1 0.0096(4) 0.0103(4) 0.0134(4) -0.0005(3) -0.0007(3) 0.0003(3) O11 0.0241(15) 0.0236(14) 0.0285(15) -0.0051(11) 0.0094(12) -0.0078(12) O12 0.0332(17) 0.0214(14) 0.0240(15) 0.0045(11) -0.0050(12) 0.0017(12) O13 0.0231(16) 0.0310(17) 0.0448(19) -0.0123(14) -0.0173(14) 0.0078(13) C11 0.0142(17) 0.0142(16) 0.0212(18) -0.0065(13) -0.0005(13) 0.0039(13) C12 0.0174(18) 0.0106(16) 0.0221(18) -0.0035(13) -0.0012(14) 0.0024(13) C13 0.0194(18) 0.0144(17) 0.0237(19) -0.0024(14) -0.0022(15) 0.0055(14) C111 0.0145(16) 0.0100(15) 0.0175(17) -0.0019(12) 0.0002(13) -0.0007(13) C112 0.0185(18) 0.0123(16) 0.0224(18) -0.0020(13) -0.0015(14) -0.0013(13) C113 0.024(2) 0.0142(17) 0.026(2) -0.0008(14) -0.0050(15) 0.0004(15) C114 0.026(2) 0.0140(17) 0.0242(19) 0.0045(14) -0.0054(15) -0.0015(15) C115 0.0222(19) 0.0133(17) 0.0157(17) 0.0015(13) -0.0013(14) -0.0002(14) C121 0.0151(16) 0.0106(15) 0.0145(16) -0.0001(12) -0.0016(12) -0.0001(13) C122 0.0111(16) 0.0216(18) 0.0181(17) -0.0024(14) -0.0028(13) -0.0015(14) C123 0.0161(18) 0.039(2) 0.0211(19) -0.0077(16) -0.0031(14) -0.0077(17) C124 0.0201(19) 0.0244(19) 0.0166(17) -0.0035(14) -0.0034(14) -0.0038(15) C125 0.0192(18) 0.0203(18) 0.0159(17) -0.0037(14) -0.0024(13) -0.0014(14) C131 0.0130(16) 0.0115(16) 0.0180(17) -0.0004(12) 0.0011(13) -0.0016(13) C132 0.0126(16) 0.0162(17) 0.0204(17) 0.0039(13) 0.0009(13) -0.0016(13) C133 0.0171(18) 0.0209(19) 0.030(2) 0.0069(15) 0.0039(15) -0.0035(15) C134 0.0123(18) 0.029(2) 0.038(2) 0.0077(17) 0.0022(16) -0.0024(16) C135 0.0127(17) 0.0182(18) 0.0250(19) 0.0048(14) -0.0026(14) 0.0003(14) Co2 0.0120(2) 0.0107(2) 0.0157(3) 0.00055(17) -0.00197(17) 0.00195(17) P2 0.0101(4) 0.0119(4) 0.0134(4) -0.0006(3) -0.0017(3) 0.0004(3) O21 0.0163(14) 0.0291(16) 0.0443(18) 0.0102(13) 0.0059(12) 0.0009(12) O22 0.0348(17) 0.0189(14) 0.0389(17) 0.0013(12) -0.0196(14) -0.0033(12) O23 0.061(2) 0.0300(17) 0.0250(16) -0.0021(13) 0.0065(15) 0.0198(16) C21 0.0223(19) 0.0124(17) 0.0222(18) 0.0049(13) -0.0041(14) 0.0046(14) C22 0.0217(19) 0.0147(17) 0.0220(18) 0.0063(14) -0.0062(15) 0.0030(14) C23 0.026(2) 0.0180(18) 0.0225(19) 0.0034(15) -0.0017(15) 0.0074(15) C211 0.0113(16) 0.0176(17) 0.0137(16) -0.0012(13) -0.0019(12) -0.0022(13) C212 0.0115(16) 0.0187(18) 0.0212(18) -0.0012(14) 0.0011(13) 0.0030(13) C213 0.022(2) 0.036(2) 0.029(2) -0.0038(18) 0.0007(16) -0.0159(18) C214 0.0195(19) 0.0195(19) 0.029(2) -0.0033(15) -0.0073(15) -0.0018(15) C215 0.0188(18) 0.0175(18) 0.0209(18) -0.0022(14) -0.0063(14) -0.0035(14) C221 0.0133(16) 0.0155(16) 0.0146(16) 0.0006(13) -0.0025(12) -0.0024(13) C222 0.0165(17) 0.0203(18) 0.0174(17) -0.0019(14) -0.0007(13) -0.0010(14) C223 0.0188(19) 0.037(2) 0.0162(18) -0.0026(16) 0.0032(14) 0.0008(16) C224 0.0157(19) 0.040(2) 0.025(2) -0.0010(17) 0.0024(15) 0.0012(17) C225 0.0144(17) 0.030(2) 0.0190(18) -0.0015(15) -0.0022(14) -0.0064(15) C231 0.0147(16) 0.0128(16) 0.0147(16) -0.0007(12) -0.0007(12) -0.0007(13) C232 0.0212(18) 0.0159(17) 0.0161(17) -0.0012(13) -0.0024(14) 0.0037(14) C233 0.0194(18) 0.0172(17) 0.0170(17) -0.0012(13) -0.0002(13) 0.0020(14) C234 0.0208(18) 0.0131(17) 0.0232(19) -0.0035(14) 0.0007(14) 0.0005(14) C235 0.0204(18) 0.0118(16) 0.0191(17) -0.0015(13) 0.0004(14) 0.0022(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C11 1.777(4) . ? Co1 C12 1.781(4) . ? Co1 C13 1.791(4) . ? Co1 P1 2.2034(9) . ? Co1 Co1 2.6561(9) 2_676 ? P1 C121 1.839(3) . ? P1 C111 1.842(3) . ? P1 C131 1.842(3) . ? O11 C11 1.142(4) . ? O12 C12 1.147(5) . ? O13 C13 1.138(5) . ? C111 C115 1.545(5) . ? C111 C112 1.567(5) . ? C111 H111 0.9800 . ? C112 C113 1.544(5) . ? C112 H11A 0.9700 . ? C112 H11B 0.9700 . ? C113 C114 1.521(5) . ? C113 H11C 0.9700 . ? C113 H11D 0.9700 . ? C114 C115 1.521(5) . ? C114 H11E 0.9700 . ? C114 H11F 0.9700 . ? C115 H11G 0.9700 . ? C115 H11H 0.9700 . ? C121 C125 1.534(5) . ? C121 C122 1.559(5) . ? C121 H121 0.9800 . ? C122 C123 1.537(5) . ? C122 H12A 0.9700 . ? C122 H12B 0.9700 . ? C123 C124 1.529(5) . ? C123 H12C 0.9700 . ? C123 H12D 0.9700 . ? C124 C125 1.537(5) . ? C124 H12E 0.9700 . ? C124 H12F 0.9700 . ? C125 H12G 0.9700 . ? C125 H12H 0.9700 . ? C131 C132 1.535(5) . ? C131 C135 1.537(5) . ? C131 H131 0.9800 . ? C132 C133 1.541(5) . ? C132 H13A 0.9700 . ? C132 H13B 0.9700 . ? C133 C134 1.531(6) . ? C133 H13C 0.9700 . ? C133 H13D 0.9700 . ? C134 C135 1.541(5) . ? C134 H13E 0.9700 . ? C134 H13F 0.9700 . ? C135 H13G 0.9700 . ? C135 H13H 0.9700 . ? Co2 C22 1.776(4) . ? Co2 C21 1.783(4) . ? Co2 C23 1.783(4) . ? Co2 P2 2.2108(10) . ? Co2 Co2 2.6908(9) 2_565 ? P2 C211 1.836(3) . ? P2 C221 1.841(3) . ? P2 C231 1.854(3) . ? O21 C21 1.145(5) . ? O22 C22 1.148(5) . ? O23 C23 1.151(5) . ? C211 C212 1.541(5) . ? C211 C215 1.548(5) . ? C211 H211 0.9800 . ? C212 C213 1.520(5) . ? C212 H21A 0.9700 . ? C212 H21B 0.9700 . ? C213 C214 1.538(6) . ? C213 H21C 0.9700 . ? C213 H21D 0.9700 . ? C214 C215 1.531(5) . ? C214 H21E 0.9700 . ? C214 H21F 0.9700 . ? C215 H21G 0.9700 . ? C215 H21H 0.9700 . ? C221 C222 1.539(5) . ? C221 C225 1.556(5) . ? C221 H221 0.9800 . ? C222 C223 1.523(5) . ? C222 H22A 0.9700 . ? C222 H22B 0.9700 . ? C223 C224 1.522(5) . ? C223 H22C 0.9700 . ? C223 H22D 0.9700 . ? C224 C225 1.540(5) . ? C224 H22E 0.9700 . ? C224 H22F 0.9700 . ? C225 H22G 0.9700 . ? C225 H22H 0.9700 . ? C231 C235 1.541(5) . ? C231 C232 1.562(5) . ? C231 H231 0.9800 . ? C232 C233 1.545(5) . ? C232 H23A 0.9700 . ? C232 H23B 0.9700 . ? C233 C234 1.524(5) . ? C233 H23C 0.9700 . ? C233 H23D 0.9700 . ? C234 C235 1.533(5) . ? C234 H23E 0.9700 . ? C234 H23F 0.9700 . ? C235 H23G 0.9700 . ? C235 H23H 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Co1 C12 120.34(17) . . ? C11 Co1 C13 118.88(17) . . ? C12 Co1 C13 118.43(17) . . ? C11 Co1 P1 92.38(11) . . ? C12 Co1 P1 92.81(11) . . ? C13 Co1 P1 100.17(12) . . ? C11 Co1 Co1 82.26(11) . 2_676 ? C12 Co1 Co1 86.39(11) . 2_676 ? C13 Co1 Co1 86.09(12) . 2_676 ? P1 Co1 Co1 173.23(4) . 2_676 ? C121 P1 C111 106.55(15) . . ? C121 P1 C131 102.32(15) . . ? C111 P1 C131 106.60(16) . . ? C121 P1 Co1 110.20(11) . . ? C111 P1 Co1 112.67(11) . . ? C131 P1 Co1 117.53(11) . . ? O11 C11 Co1 177.5(3) . . ? O12 C12 Co1 177.6(3) . . ? O13 C13 Co1 177.4(3) . . ? C115 C111 C112 105.2(3) . . ? C115 C111 P1 112.9(2) . . ? C112 C111 P1 119.0(2) . . ? C115 C111 H111 106.3 . . ? C112 C111 H111 106.3 . . ? P1 C111 H111 106.3 . . ? C113 C112 C111 105.4(3) . . ? C113 C112 H11A 110.7 . . ? C111 C112 H11A 110.7 . . ? C113 C112 H11B 110.7 . . ? C111 C112 H11B 110.7 . . ? H11A C112 H11B 108.8 . . ? C114 C113 C112 105.4(3) . . ? C114 C113 H11C 110.7 . . ? C112 C113 H11C 110.7 . . ? C114 C113 H11D 110.7 . . ? C112 C113 H11D 110.7 . . ? H11C C113 H11D 108.8 . . ? C113 C114 C115 103.4(3) . . ? C113 C114 H11E 111.1 . . ? C115 C114 H11E 111.1 . . ? C113 C114 H11F 111.1 . . ? C115 C114 H11F 111.1 . . ? H11E C114 H11F 109.0 . . ? C114 C115 C111 104.0(3) . . ? C114 C115 H11G 111.0 . . ? C111 C115 H11G 111.0 . . ? C114 C115 H11H 111.0 . . ? C111 C115 H11H 111.0 . . ? H11G C115 H11H 109.0 . . ? C125 C121 C122 103.5(3) . . ? C125 C121 P1 119.6(2) . . ? C122 C121 P1 114.2(2) . . ? C125 C121 H121 106.2 . . ? C122 C121 H121 106.2 . . ? P1 C121 H121 106.2 . . ? C123 C122 C121 105.6(3) . . ? C123 C122 H12A 110.6 . . ? C121 C122 H12A 110.6 . . ? C123 C122 H12B 110.6 . . ? C121 C122 H12B 110.6 . . ? H12A C122 H12B 108.8 . . ? C124 C123 C122 106.3(3) . . ? C124 C123 H12C 110.5 . . ? C122 C123 H12C 110.5 . . ? C124 C123 H12D 110.5 . . ? C122 C123 H12D 110.5 . . ? H12C C123 H12D 108.7 . . ? C123 C124 C125 103.6(3) . . ? C123 C124 H12E 111.0 . . ? C125 C124 H12E 111.0 . . ? C123 C124 H12F 111.0 . . ? C125 C124 H12F 111.0 . . ? H12E C124 H12F 109.0 . . ? C121 C125 C124 102.0(3) . . ? C121 C125 H12G 111.4 . . ? C124 C125 H12G 111.4 . . ? C121 C125 H12H 111.4 . . ? C124 C125 H12H 111.4 . . ? H12G C125 H12H 109.2 . . ? C132 C131 C135 102.0(3) . . ? C132 C131 P1 114.2(2) . . ? C135 C131 P1 117.3(2) . . ? C132 C131 H131 107.6 . . ? C135 C131 H131 107.6 . . ? P1 C131 H131 107.6 . . ? C131 C132 C133 103.2(3) . . ? C131 C132 H13A 111.1 . . ? C133 C132 H13A 111.1 . . ? C131 C132 H13B 111.1 . . ? C133 C132 H13B 111.1 . . ? H13A C132 H13B 109.1 . . ? C134 C133 C132 105.5(3) . . ? C134 C133 H13C 110.6 . . ? C132 C133 H13C 110.6 . . ? C134 C133 H13D 110.6 . . ? C132 C133 H13D 110.6 . . ? H13C C133 H13D 108.8 . . ? C133 C134 C135 106.6(3) . . ? C133 C134 H13E 110.4 . . ? C135 C134 H13E 110.4 . . ? C133 C134 H13F 110.4 . . ? C135 C134 H13F 110.4 . . ? H13E C134 H13F 108.6 . . ? C131 C135 C134 103.9(3) . . ? C131 C135 H13G 111.0 . . ? C134 C135 H13G 111.0 . . ? C131 C135 H13H 111.0 . . ? C134 C135 H13H 111.0 . . ? H13G C135 H13H 109.0 . . ? C22 Co2 C21 118.96(17) . . ? C22 Co2 C23 121.80(19) . . ? C21 Co2 C23 116.42(18) . . ? C22 Co2 P2 92.26(12) . . ? C21 Co2 P2 96.85(12) . . ? C23 Co2 P2 97.78(13) . . ? C22 Co2 Co2 84.03(12) . 2_565 ? C21 Co2 Co2 83.93(12) . 2_565 ? C23 Co2 Co2 85.26(12) . 2_565 ? P2 Co2 Co2 176.09(4) . 2_565 ? C211 P2 C221 101.63(15) . . ? C211 P2 C231 105.52(16) . . ? C221 P2 C231 99.19(15) . . ? C211 P2 Co2 117.94(12) . . ? C221 P2 Co2 117.21(12) . . ? C231 P2 Co2 112.98(12) . . ? O21 C21 Co2 178.3(3) . . ? O22 C22 Co2 178.3(4) . . ? O23 C23 Co2 178.5(4) . . ? C212 C211 C215 101.5(3) . . ? C212 C211 P2 117.2(2) . . ? C215 C211 P2 114.9(2) . . ? C212 C211 H211 107.6 . . ? C215 C211 H211 107.6 . . ? P2 C211 H211 107.6 . . ? C213 C212 C211 105.7(3) . . ? C213 C212 H21A 110.6 . . ? C211 C212 H21A 110.6 . . ? C213 C212 H21B 110.6 . . ? C211 C212 H21B 110.6 . . ? H21A C212 H21B 108.7 . . ? C212 C213 C214 106.4(3) . . ? C212 C213 H21C 110.5 . . ? C214 C213 H21C 110.5 . . ? C212 C213 H21D 110.5 . . ? C214 C213 H21D 110.5 . . ? H21C C213 H21D 108.6 . . ? C215 C214 C213 105.7(3) . . ? C215 C214 H21E 110.6 . . ? C213 C214 H21E 110.6 . . ? C215 C214 H21F 110.6 . . ? C213 C214 H21F 110.6 . . ? H21E C214 H21F 108.7 . . ? C214 C215 C211 103.2(3) . . ? C214 C215 H21G 111.1 . . ? C211 C215 H21G 111.1 . . ? C214 C215 H21H 111.1 . . ? C211 C215 H21H 111.1 . . ? H21G C215 H21H 109.1 . . ? C222 C221 C225 105.0(3) . . ? C222 C221 P2 117.9(2) . . ? C225 C221 P2 114.1(2) . . ? C222 C221 H221 106.3 . . ? C225 C221 H221 106.3 . . ? P2 C221 H221 106.3 . . ? C223 C222 C221 102.7(3) . . ? C223 C222 H22A 111.2 . . ? C221 C222 H22A 111.2 . . ? C223 C222 H22B 111.2 . . ? C221 C222 H22B 111.2 . . ? H22A C222 H22B 109.1 . . ? C224 C223 C222 103.0(3) . . ? C224 C223 H22C 111.2 . . ? C222 C223 H22C 111.2 . . ? C224 C223 H22D 111.2 . . ? C222 C223 H22D 111.2 . . ? H22C C223 H22D 109.1 . . ? C223 C224 C225 105.3(3) . . ? C223 C224 H22E 110.7 . . ? C225 C224 H22E 110.7 . . ? C223 C224 H22F 110.7 . . ? C225 C224 H22F 110.7 . . ? H22E C224 H22F 108.8 . . ? C224 C225 C221 105.5(3) . . ? C224 C225 H22G 110.6 . . ? C221 C225 H22G 110.6 . . ? C224 C225 H22H 110.6 . . ? C221 C225 H22H 110.6 . . ? H22G C225 H22H 108.8 . . ? C235 C231 C232 105.7(3) . . ? C235 C231 P2 117.0(2) . . ? C232 C231 P2 115.5(2) . . ? C235 C231 H231 105.9 . . ? C232 C231 H231 105.9 . . ? P2 C231 H231 105.9 . . ? C233 C232 C231 105.5(3) . . ? C233 C232 H23A 110.6 . . ? C231 C232 H23A 110.6 . . ? C233 C232 H23B 110.6 . . ? C231 C232 H23B 110.6 . . ? H23A C232 H23B 108.8 . . ? C234 C233 C232 104.8(3) . . ? C234 C233 H23C 110.8 . . ? C232 C233 H23C 110.8 . . ? C234 C233 H23D 110.8 . . ? C232 C233 H23D 110.8 . . ? H23C C233 H23D 108.9 . . ? C233 C234 C235 103.0(3) . . ? C233 C234 H23E 111.2 . . ? C235 C234 H23E 111.2 . . ? C233 C234 H23F 111.2 . . ? C235 C234 H23F 111.2 . . ? H23E C234 H23F 109.1 . . ? C234 C235 C231 103.6(3) . . ? C234 C235 H23G 111.0 . . ? C231 C235 H23G 111.0 . . ? C234 C235 H23H 111.0 . . ? C231 C235 H23H 111.0 . . ? H23G C235 H23H 109.0 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.366 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.154