# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address 'P Power' ;Department of Chemistry University of California, Davis 1 Shields Ave Davis, CA 95616 ; 'Bobby D. Ellis' ;Department of Chemistry University of California, Davis 1 Shields Ave Davis, CA 95616 ; 'James C. Fettinger' ;Department of Chemistry University of California, Davis 1 Shields Ave Davis, CA 95616 ; 'G Long' ;Department of Chemistry University of Missouri-Rolla 1870 Miner Circle Rolla, MO 65409 ; 'Chengbao Ni' ;Department of Chemistry University of California, Davis 1 Shields Ave Davis, CA 95616 ; _publ_contact_author_name 'P Power' _publ_contact_author_email PPPOWER@UCDAVIS.EDU _publ_section_title ; Reduction of Terphenyl Iron(II) or Cobalt(II) Halides in the Presence of Trimethylphosphine ; _publ_contact_author_address ; Department of Chemistry University of California, Davis 1 Shields Ave Davis, CA 95616 ; _publ_requested_journal ? # Attachment '1_S_Fe_PMe3.cif' data_p21n _database_code_depnum_ccdc_archive 'CCDC 723169' _publ_section_abstract ; ? ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H58 Fe P' _chemical_formula_sum 'C39 H58 Fe P' _chemical_formula_weight 613.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3962(13) _cell_length_b 15.737(2) _cell_length_c 22.311(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.490(2) _cell_angle_gamma 90.00 _cell_volume 3633.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7291 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.49 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_min 0.271 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_max 0.616 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9224 _exptl_absorpt_correction_T_max 0.9578 _exptl_absorpt_process_details 'SADABS 2007/4 (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39802 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8331 _reflns_number_gt 7527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SMART APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0424P)^2^+1.9979P] 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 8331 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.053 _refine_ls_shift/su_mean 0.003 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 Fe1 Fe 0.264963(18) 0.362633(12) 0.181385(9) 0.01718(6) Uani 1 1 d . . . P1 P 0.09952(4) 0.38981(2) 0.111384(18) 0.02489(9) Uani 1 1 d . . . C1 C 0.36935(12) 0.25726(8) 0.16340(6) 0.0159(2) Uani 1 1 d . . . C2 C 0.39200(12) 0.19231(8) 0.12255(6) 0.0167(2) Uani 1 1 d . . . C3 C 0.49682(13) 0.13522(8) 0.13607(6) 0.0182(3) Uani 1 1 d . . . C4 C 0.57260(13) 0.14228(8) 0.19082(6) 0.0188(3) Uani 1 1 d . . . H4A H 0.6393 0.1035 0.1996 0.023 Uiso 1 1 calc R . . C5 C 0.55238(12) 0.20535(8) 0.23313(6) 0.0164(2) Uani 1 1 d . . . C6 C 0.45188(12) 0.26105(8) 0.21730(6) 0.0157(2) Uani 1 1 d . . . C7 C 0.30825(13) 0.18154(8) 0.06447(6) 0.0184(3) Uani 1 1 d . . . C8 C 0.19981(14) 0.12766(8) 0.06190(6) 0.0198(3) Uani 1 1 d . . . C9 C 0.12646(15) 0.11537(9) 0.00676(7) 0.0250(3) Uani 1 1 d . . . H9A H 0.0538 0.0806 0.0048 0.030 Uiso 1 1 calc R . . C10 C 0.16091(16) 0.15444(10) -0.04513(7) 0.0285(3) Uani 1 1 d . . . H10A H 0.1125 0.1449 -0.0818 0.034 Uiso 1 1 calc R . . C11 C 0.26694(16) 0.20740(10) -0.04237(7) 0.0290(3) Uani 1 1 d . . . H11A H 0.2892 0.2335 -0.0773 0.035 Uiso 1 1 calc R . . C12 C 0.34171(15) 0.22254(9) 0.01215(7) 0.0242(3) Uani 1 1 d . . . C13 C 0.40509(12) 0.33919(8) 0.24816(6) 0.0164(2) Uani 1 1 d . . . C14 C 0.28263(12) 0.32914(9) 0.27304(6) 0.0185(3) Uani 1 1 d . . . C15 C 0.19255(13) 0.39620(9) 0.26595(6) 0.0218(3) Uani 1 1 d . . . H15A H 0.1019 0.3839 0.2712 0.026 Uiso 1 1 calc R . . C16 C 0.22131(14) 0.47131(9) 0.23561(7) 0.0237(3) Uani 1 1 d . . . H16A H 0.1503 0.5091 0.2209 0.028 Uiso 1 1 calc R . . C17 C 0.34347(14) 0.48309(9) 0.21441(7) 0.0227(3) Uani 1 1 d . . . H17A H 0.3536 0.5287 0.1853 0.027 Uiso 1 1 calc R . . C18 C 0.43700(13) 0.41804(9) 0.22022(6) 0.0188(3) Uani 1 1 d . . . C19 C 0.53103(14) 0.06700(9) 0.09150(7) 0.0232(3) Uani 1 1 d . . . H19A H 0.4765 0.0763 0.0538 0.028 Uiso 1 1 calc R . . C20 C 0.50320(17) -0.02238(10) 0.11362(8) 0.0320(3) Uani 1 1 d . . . H20A H 0.4135 -0.0268 0.1202 0.048 Uiso 1 1 calc R . . H20B H 0.5555 -0.0333 0.1507 0.048 Uiso 1 1 calc R . . H20C H 0.5231 -0.0632 0.0839 0.048 Uiso 1 1 calc R . . C21 C 0.67241(17) 0.07327(12) 0.07760(9) 0.0392(4) Uani 1 1 d . . . H21A H 0.6869 0.0352 0.0453 0.059 Uiso 1 1 calc R . . H21B H 0.7281 0.0581 0.1128 0.059 Uiso 1 1 calc R . . H21C H 0.6907 0.1304 0.0660 0.059 Uiso 1 1 calc R . . C22 C 0.63687(12) 0.21251(9) 0.29208(6) 0.0184(3) Uani 1 1 d . . . H22A H 0.6089 0.2627 0.3133 0.022 Uiso 1 1 calc R . . C23 C 0.62009(15) 0.13505(9) 0.33204(7) 0.0248(3) Uani 1 1 d . . . H23A H 0.5304 0.1286 0.3381 0.037 Uiso 1 1 calc R . . H23B H 0.6696 0.1429 0.3702 0.037 Uiso 1 1 calc R . . H23C H 0.6497 0.0851 0.3128 0.037 Uiso 1 1 calc R . . C24 C 0.77904(13) 0.22498(10) 0.28168(7) 0.0251(3) Uani 1 1 d . . . H24A H 0.7879 0.2753 0.2581 0.038 Uiso 1 1 calc R . . H24B H 0.8088 0.1766 0.2607 0.038 Uiso 1 1 calc R . . H24C H 0.8296 0.2308 0.3198 0.038 Uiso 1 1 calc R . . C25 C 0.16054(14) 0.08451(9) 0.11853(6) 0.0226(3) Uani 1 1 d . . . H25A H 0.2388 0.0772 0.1462 0.027 Uiso 1 1 calc R . . C26 C 0.10048(16) -0.00323(10) 0.10703(7) 0.0302(3) Uani 1 1 d . . . H26A H 0.1544 -0.0364 0.0834 0.045 Uiso 1 1 calc R . . H26B H 0.0163 0.0027 0.0857 0.045 Uiso 1 1 calc R . . H26C H 0.0930 -0.0312 0.1448 0.045 Uiso 1 1 calc R . . C27 C 0.06726(17) 0.14038(10) 0.15016(8) 0.0314(3) Uani 1 1 d . . . H27A H 0.1071 0.1943 0.1599 0.047 Uiso 1 1 calc R . . H27B H 0.0466 0.1129 0.1864 0.047 Uiso 1 1 calc R . . H27C H -0.0104 0.1490 0.1240 0.047 Uiso 1 1 calc R . . C28 C 0.45555(17) 0.28387(11) 0.01442(7) 0.0316(3) Uani 1 1 d . . . H28A H 0.5042 0.2781 0.0541 0.038 Uiso 1 1 calc R . . C29 C 0.4085(2) 0.37550(13) 0.00811(11) 0.0517(5) Uani 1 1 d . . . H29A H 0.4814 0.4129 0.0083 0.078 Uiso 1 1 calc R . . H29B H 0.3595 0.3894 0.0411 0.078 Uiso 1 1 calc R . . H29C H 0.3549 0.3819 -0.0291 0.078 Uiso 1 1 calc R . . C30 C 0.5470(2) 0.26362(17) -0.03284(11) 0.0634(7) Uani 1 1 d . . . H30A H 0.5737 0.2053 -0.0290 0.095 Uiso 1 1 calc R . . H30B H 0.6214 0.2999 -0.0271 0.095 Uiso 1 1 calc R . . H30C H 0.5036 0.2729 -0.0722 0.095 Uiso 1 1 calc R . . C31 C 0.25433(13) 0.24836(9) 0.30630(7) 0.0213(3) Uani 1 1 d . . . H31A H 0.2916 0.2005 0.2858 0.026 Uiso 1 1 calc R . . C32 C 0.11001(14) 0.23188(10) 0.30757(7) 0.0280(3) Uani 1 1 d . . . H32A H 0.0688 0.2319 0.2672 0.042 Uiso 1 1 calc R . . H32B H 0.0729 0.2757 0.3305 0.042 Uiso 1 1 calc R . . H32C H 0.0974 0.1777 0.3259 0.042 Uiso 1 1 calc R . . C33 C 0.32057(15) 0.25283(10) 0.37071(7) 0.0271(3) Uani 1 1 d . . . H33A H 0.4114 0.2624 0.3694 0.041 Uiso 1 1 calc R . . H33B H 0.3076 0.2002 0.3911 0.041 Uiso 1 1 calc R . . H33C H 0.2841 0.2986 0.3919 0.041 Uiso 1 1 calc R . . C34 C 0.56992(13) 0.42950(9) 0.19857(7) 0.0218(3) Uani 1 1 d . . . H34A H 0.5978 0.3743 0.1842 0.026 Uiso 1 1 calc R . . C35 C 0.66462(14) 0.45566(10) 0.25237(7) 0.0275(3) Uani 1 1 d . . . H35A H 0.6616 0.4148 0.2841 0.041 Uiso 1 1 calc R . . H35B H 0.6409 0.5106 0.2665 0.041 Uiso 1 1 calc R . . H35C H 0.7506 0.4580 0.2401 0.041 Uiso 1 1 calc R . . C36 C 0.57343(15) 0.49303(11) 0.14702(7) 0.0303(3) Uani 1 1 d . . . H36A H 0.5066 0.4795 0.1158 0.045 Uiso 1 1 calc R . . H36B H 0.6560 0.4902 0.1312 0.045 Uiso 1 1 calc R . . H36C H 0.5599 0.5494 0.1617 0.045 Uiso 1 1 calc R . . C37 C -0.05542(16) 0.39157(13) 0.14427(9) 0.0395(4) Uani 1 1 d . . . H37A H -0.1218 0.4119 0.1149 0.059 Uiso 1 1 calc R . . H37B H -0.0491 0.4286 0.1786 0.059 Uiso 1 1 calc R . . H37C H -0.0765 0.3352 0.1565 0.059 Uiso 1 1 calc R . . C38 C 0.1077(2) 0.49745(11) 0.08076(8) 0.0382(4) Uani 1 1 d . . . H38A H 0.0258 0.5120 0.0597 0.057 Uiso 1 1 calc R . . H38B H 0.1735 0.4998 0.0534 0.057 Uiso 1 1 calc R . . H38C H 0.1280 0.5369 0.1131 0.057 Uiso 1 1 calc R . . C39 C 0.05375(18) 0.33013(11) 0.04269(8) 0.0365(4) Uani 1 1 d . . . H39A H -0.0226 0.3547 0.0220 0.055 Uiso 1 1 calc R . . H39B H 0.0368 0.2721 0.0527 0.055 Uiso 1 1 calc R . . H39C H 0.1229 0.3321 0.0171 0.055 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 Fe1 0.01601(10) 0.01529(10) 0.02007(11) -0.00206(7) 0.00085(7) 0.00193(7) P1 0.02549(19) 0.02188(19) 0.0261(2) -0.00139(14) -0.00384(15) 0.00732(14) C1 0.0139(5) 0.0144(6) 0.0197(6) 0.0002(5) 0.0023(5) -0.0010(4) C2 0.0164(6) 0.0163(6) 0.0175(6) 0.0002(5) 0.0019(5) -0.0020(5) C3 0.0194(6) 0.0160(6) 0.0198(6) -0.0019(5) 0.0042(5) -0.0004(5) C4 0.0158(6) 0.0178(6) 0.0230(7) -0.0009(5) 0.0021(5) 0.0021(5) C5 0.0135(6) 0.0166(6) 0.0192(6) -0.0004(5) 0.0019(5) -0.0017(5) C6 0.0144(5) 0.0143(6) 0.0187(6) -0.0021(5) 0.0035(5) -0.0020(4) C7 0.0217(6) 0.0159(6) 0.0173(6) -0.0017(5) 0.0006(5) 0.0025(5) C8 0.0245(7) 0.0162(6) 0.0178(6) -0.0009(5) -0.0018(5) 0.0012(5) C9 0.0304(7) 0.0212(7) 0.0220(7) -0.0014(5) -0.0055(6) -0.0030(6) C10 0.0404(9) 0.0261(7) 0.0171(7) -0.0013(6) -0.0068(6) 0.0025(6) C11 0.0412(9) 0.0289(8) 0.0170(7) 0.0038(6) 0.0032(6) 0.0025(6) C12 0.0293(7) 0.0229(7) 0.0207(7) 0.0004(5) 0.0034(6) 0.0005(6) C13 0.0144(6) 0.0167(6) 0.0178(6) -0.0030(5) 0.0005(5) -0.0001(5) C14 0.0165(6) 0.0194(6) 0.0197(6) -0.0046(5) 0.0025(5) -0.0011(5) C15 0.0177(6) 0.0239(7) 0.0238(7) -0.0066(5) 0.0034(5) 0.0016(5) C16 0.0231(7) 0.0206(7) 0.0268(7) -0.0059(5) 0.0003(5) 0.0051(5) C17 0.0265(7) 0.0161(6) 0.0250(7) -0.0028(5) 0.0008(5) -0.0001(5) C18 0.0186(6) 0.0175(6) 0.0203(6) -0.0043(5) 0.0019(5) -0.0026(5) C19 0.0260(7) 0.0220(7) 0.0219(7) -0.0052(5) 0.0040(5) 0.0042(5) C20 0.0423(9) 0.0200(7) 0.0344(9) -0.0068(6) 0.0074(7) 0.0030(6) C21 0.0351(9) 0.0408(10) 0.0445(10) -0.0137(8) 0.0183(8) 0.0018(7) C22 0.0151(6) 0.0197(6) 0.0201(6) -0.0024(5) 0.0002(5) 0.0005(5) C23 0.0252(7) 0.0242(7) 0.0244(7) 0.0021(6) -0.0010(6) -0.0001(5) C24 0.0159(6) 0.0326(8) 0.0264(7) -0.0029(6) -0.0001(5) -0.0018(6) C25 0.0247(7) 0.0224(7) 0.0195(7) 0.0010(5) -0.0039(5) -0.0068(5) C26 0.0387(9) 0.0238(7) 0.0265(8) 0.0028(6) -0.0055(6) -0.0094(6) C27 0.0357(8) 0.0304(8) 0.0290(8) -0.0012(6) 0.0081(7) -0.0081(6) C28 0.0378(9) 0.0351(9) 0.0226(7) 0.0015(6) 0.0073(6) -0.0085(7) C29 0.0608(13) 0.0327(10) 0.0609(14) 0.0013(9) 0.0018(11) -0.0164(9) C30 0.0666(14) 0.0690(15) 0.0615(14) -0.0224(12) 0.0415(12) -0.0268(12) C31 0.0197(6) 0.0189(6) 0.0265(7) -0.0022(5) 0.0085(5) -0.0015(5) C32 0.0233(7) 0.0299(8) 0.0319(8) -0.0058(6) 0.0091(6) -0.0081(6) C33 0.0252(7) 0.0288(8) 0.0280(8) 0.0051(6) 0.0060(6) -0.0010(6) C34 0.0201(6) 0.0182(6) 0.0278(7) -0.0017(5) 0.0051(5) -0.0040(5) C35 0.0216(7) 0.0279(7) 0.0327(8) 0.0003(6) 0.0017(6) -0.0062(6) C36 0.0283(7) 0.0320(8) 0.0311(8) 0.0049(6) 0.0059(6) -0.0067(6) C37 0.0216(7) 0.0470(10) 0.0489(11) -0.0035(8) -0.0016(7) 0.0092(7) C38 0.0547(11) 0.0255(8) 0.0331(9) 0.0034(7) -0.0017(8) 0.0125(7) C39 0.0420(9) 0.0320(8) 0.0321(9) -0.0059(7) -0.0144(7) 0.0115(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C13 2.0155(13) . ? Fe1 C1 2.0426(13) . ? Fe1 C18 2.1007(13) . ? Fe1 C14 2.1027(14) . ? Fe1 C15 2.1628(14) . ? Fe1 C17 2.1651(14) . ? Fe1 C16 2.1679(14) . ? Fe1 P1 2.2509(5) . ? P1 C39 1.8215(17) . ? P1 C38 1.8316(18) . ? P1 C37 1.8330(18) . ? C1 C2 1.4042(18) . ? C1 C6 1.4102(18) . ? C2 C3 1.4223(18) . ? C2 C7 1.5001(18) . ? C3 C4 1.3931(19) . ? C3 C19 1.5284(18) . ? C4 C5 1.3995(18) . ? C4 H4A 0.9300 . ? C5 C6 1.3835(18) . ? C5 C22 1.5143(18) . ? C6 C13 1.5122(17) . ? C7 C12 1.406(2) . ? C7 C8 1.4074(19) . ? C8 C9 1.3975(19) . ? C8 C25 1.5240(19) . ? C9 C10 1.388(2) . ? C9 H9A 0.9300 . ? C10 C11 1.379(2) . ? C10 H10A 0.9300 . ? C11 C12 1.400(2) . ? C11 H11A 0.9300 . ? C12 C28 1.524(2) . ? C13 C18 1.4415(19) . ? C13 C14 1.4455(18) . ? C14 C15 1.4097(19) . ? C14 C31 1.5150(19) . ? C15 C16 1.409(2) . ? C15 H15A 0.9800 . ? C16 C17 1.409(2) . ? C16 H16A 0.9800 . ? C17 C18 1.4093(19) . ? C17 H17A 0.9800 . ? C18 C34 1.5176(18) . ? C19 C20 1.528(2) . ? C19 C21 1.534(2) . ? C19 H19A 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.5301(19) . ? C22 C24 1.5305(18) . ? C22 H22A 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.527(2) . ? C25 C27 1.530(2) . ? C25 H25A 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C30 1.520(3) . ? C28 C29 1.525(3) . ? C28 H28A 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.5256(19) . ? C31 C33 1.535(2) . ? C31 H31A 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C36 1.527(2) . ? C34 C35 1.534(2) . ? C34 H34A 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? 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 C13 Fe1 C1 68.69(5) . . ? C13 Fe1 C18 40.93(5) . . ? C1 Fe1 C18 88.32(5) . . ? C13 Fe1 C14 41.03(5) . . ? C1 Fe1 C14 89.36(5) . . ? C18 Fe1 C14 73.22(5) . . ? C13 Fe1 C15 71.77(5) . . ? C1 Fe1 C15 127.26(5) . . ? C18 Fe1 C15 83.83(5) . . ? C14 Fe1 C15 38.57(5) . . ? C13 Fe1 C17 71.73(5) . . ? C1 Fe1 C17 125.99(5) . . ? C18 Fe1 C17 38.54(5) . . ? C14 Fe1 C17 83.89(5) . . ? C15 Fe1 C17 68.94(6) . . ? C13 Fe1 C16 84.66(5) . . ? C1 Fe1 C16 153.34(5) . . ? C18 Fe1 C16 69.99(5) . . ? C14 Fe1 C16 70.03(5) . . ? C15 Fe1 C16 37.96(6) . . ? C17 Fe1 C16 37.96(5) . . ? C13 Fe1 P1 176.30(4) . . ? C1 Fe1 P1 113.77(4) . . ? C18 Fe1 P1 140.46(4) . . ? C14 Fe1 P1 135.42(4) . . ? C15 Fe1 P1 104.61(4) . . ? C17 Fe1 P1 107.94(4) . . ? C16 Fe1 P1 92.89(4) . . ? C39 P1 C38 100.41(8) . . ? C39 P1 C37 100.13(9) . . ? C38 P1 C37 102.07(9) . . ? C39 P1 Fe1 127.35(6) . . ? C38 P1 Fe1 112.02(6) . . ? C37 P1 Fe1 111.57(6) . . ? C2 C1 C6 117.27(11) . . ? C2 C1 Fe1 147.53(10) . . ? C6 C1 Fe1 95.13(8) . . ? C1 C2 C3 119.65(12) . . ? C1 C2 C7 121.56(12) . . ? C3 C2 C7 118.78(12) . . ? C4 C3 C2 119.55(12) . . ? C4 C3 C19 118.63(12) . . ? C2 C3 C19 121.80(12) . . ? C3 C4 C5 122.62(12) . . ? C3 C4 H4A 118.7 . . ? C5 C4 H4A 118.7 . . ? C6 C5 C4 115.83(12) . . ? C6 C5 C22 122.39(12) . . ? C4 C5 C22 121.78(12) . . ? C5 C6 C1 125.02(12) . . ? C5 C6 C13 131.84(12) . . ? C1 C6 C13 103.10(11) . . ? C12 C7 C8 120.24(13) . . ? C12 C7 C2 119.73(12) . . ? C8 C7 C2 119.98(12) . . ? C9 C8 C7 119.12(13) . . ? C9 C8 C25 120.08(13) . . ? C7 C8 C25 120.79(12) . . ? C10 C9 C8 120.69(14) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C11 C10 C9 119.98(14) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 121.12(14) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C11 C12 C7 118.83(14) . . ? C11 C12 C28 120.10(13) . . ? C7 C12 C28 121.06(13) . . ? C18 C13 C14 120.52(12) . . ? C18 C13 C6 113.94(11) . . ? C14 C13 C6 114.80(11) . . ? C18 C13 Fe1 72.71(8) . . ? C14 C13 Fe1 72.73(8) . . ? C6 C13 Fe1 93.07(8) . . ? C15 C14 C13 118.36(12) . . ? C15 C14 C31 121.67(12) . . ? C13 C14 C31 119.96(12) . . ? C15 C14 Fe1 73.02(8) . . ? C13 C14 Fe1 66.25(7) . . ? C31 C14 Fe1 133.14(10) . . ? C16 C15 C14 120.86(13) . . ? C16 C15 Fe1 71.22(8) . . ? C14 C15 Fe1 68.41(8) . . ? C16 C15 H15A 118.3 . . ? C14 C15 H15A 118.3 . . ? Fe1 C15 H15A 118.3 . . ? C15 C16 C17 120.75(13) . . ? C15 C16 Fe1 70.82(8) . . ? C17 C16 Fe1 70.91(8) . . ? C15 C16 H16A 118.8 . . ? C17 C16 H16A 118.8 . . ? Fe1 C16 H16A 118.8 . . ? C16 C17 C18 120.64(13) . . ? C16 C17 Fe1 71.13(8) . . ? C18 C17 Fe1 68.26(8) . . ? C16 C17 H17A 118.4 . . ? C18 C17 H17A 118.4 . . ? Fe1 C17 H17A 118.4 . . ? C17 C18 C13 118.67(12) . . ? C17 C18 C34 121.71(12) . . ? C13 C18 C34 119.61(12) . . ? C17 C18 Fe1 73.20(8) . . ? C13 C18 Fe1 66.36(7) . . ? C34 C18 Fe1 133.10(10) . . ? C20 C19 C3 111.93(12) . . ? C20 C19 C21 109.84(13) . . ? C3 C19 C21 111.93(12) . . ? C20 C19 H19A 107.6 . . ? C3 C19 H19A 107.6 . . ? C21 C19 H19A 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C5 C22 C23 110.97(11) . . ? C5 C22 C24 111.49(11) . . ? C23 C22 C24 110.86(12) . . ? C5 C22 H22A 107.8 . . ? C23 C22 H22A 107.8 . . ? C24 C22 H22A 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 C26 113.65(12) . . ? C8 C25 C27 110.99(12) . . ? C26 C25 C27 109.28(13) . . ? C8 C25 H25A 107.6 . . ? C26 C25 H25A 107.6 . . ? C27 C25 H25A 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C12 112.31(15) . . ? C30 C28 C29 110.53(18) . . ? C12 C28 C29 110.76(15) . . ? C30 C28 H28A 107.7 . . ? C12 C28 H28A 107.7 . . ? C29 C28 H28A 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C14 C31 C32 112.91(12) . . ? C14 C31 C33 109.24(11) . . ? C32 C31 C33 110.15(12) . . ? C14 C31 H31A 108.1 . . ? C32 C31 H31A 108.1 . . ? C33 C31 H31A 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C18 C34 C36 113.93(12) . . ? C18 C34 C35 108.59(12) . . ? C36 C34 C35 110.72(12) . . ? C18 C34 H34A 107.8 . . ? C36 C34 H34A 107.8 . . ? C35 C34 H34A 107.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P1 C37 H37A 109.5 . . ? P1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P1 C38 H38A 109.5 . . ? P1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P1 C39 H39A 109.5 . . ? P1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.639 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.054 # Attachment '4_S_H_Co_PMe33.cif' data_cbn21fmi _database_code_depnum_ccdc_archive 'CCDC 723170' _publ_section_abstract ; ? ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H74 Co P3' _chemical_formula_sum 'C45 H74 Co P3' _chemical_formula_weight 766.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 19.466(3) _cell_length_b 14.368(3) _cell_length_c 16.471(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.466(3) _cell_angle_gamma 90.00 _cell_volume 4417.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 3327 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 23.64 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9445 _exptl_absorpt_correction_T_max 0.9742 _exptl_absorpt_process_details 'SADABS 2007/4 (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24439 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7991 _reflns_number_gt 5097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART APEX II' _computing_data_reduction 'Bruker SMART APEX II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0843P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7991 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 0.15103(3) 0.22090(4) 0.37782(3) 0.02130(16) Uani 1 1 d . . . P1 P 0.23973(5) 0.27394(7) 0.47965(6) 0.0235(3) Uani 1 1 d . . . P2 P 0.06712(6) 0.17752(7) 0.43135(7) 0.0257(3) Uani 1 1 d . . . P3 P 0.10746(5) 0.35090(7) 0.32333(7) 0.0239(3) Uani 1 1 d . . . C1 C 0.32863(19) -0.0604(2) 0.4112(2) 0.0150(8) Uani 1 1 d . . . H1 H 0.3666 -0.0272 0.4491 0.018 Uiso 1 1 calc R . . C2 C 0.30680(18) -0.1446(2) 0.4379(2) 0.0151(8) Uani 1 1 d . . . C3 C 0.24999(19) -0.1928(2) 0.3828(2) 0.0165(8) Uani 1 1 d . . . C4 C 0.22077(19) -0.1565(2) 0.3017(2) 0.0170(8) Uani 1 1 d . . . H4 H 0.1833 -0.1903 0.2636 0.020 Uiso 1 1 calc R . . C5 C 0.24316(19) -0.0739(2) 0.2733(2) 0.0160(8) Uani 1 1 d . . . C6 C 0.29707(19) -0.0228(2) 0.3311(2) 0.0154(8) Uani 1 1 d . . . C7 C 0.34519(19) -0.1848(2) 0.5239(2) 0.0161(8) Uani 1 1 d . . . C8 C 0.3269(2) -0.1567(3) 0.5960(2) 0.0199(8) Uani 1 1 d . . . C9 C 0.3626(2) -0.1991(3) 0.6742(2) 0.0250(9) Uani 1 1 d . . . H9 H 0.3503 -0.1817 0.7239 0.030 Uiso 1 1 calc R . . C10 C 0.4146(2) -0.2649(3) 0.6793(2) 0.0241(9) Uani 1 1 d . . . H10 H 0.4380 -0.2928 0.7322 0.029 Uiso 1 1 calc R . . C11 C 0.4327(2) -0.2903(3) 0.6081(3) 0.0242(9) Uani 1 1 d . . . H11 H 0.4693 -0.3353 0.6125 0.029 Uiso 1 1 calc R . . C12 C 0.3990(2) -0.2521(3) 0.5296(2) 0.0191(8) Uani 1 1 d . . . C13 C 0.31825(19) 0.0733(2) 0.3098(2) 0.0150(8) Uani 1 1 d . . . C14 C 0.38495(19) 0.0883(2) 0.2936(2) 0.0178(8) Uani 1 1 d . . . C15 C 0.4027(2) 0.1781(3) 0.2741(2) 0.0233(9) Uani 1 1 d . . . H15 H 0.4476 0.1888 0.2635 0.028 Uiso 1 1 calc R . . C16 C 0.3564(2) 0.2515(3) 0.2699(2) 0.0251(9) Uani 1 1 d . . . H16 H 0.3695 0.3123 0.2570 0.030 Uiso 1 1 calc R . . C17 C 0.2912(2) 0.2366(3) 0.2843(2) 0.0245(9) Uani 1 1 d . . . H17 H 0.2592 0.2875 0.2805 0.029 Uiso 1 1 calc R . . C18 C 0.2706(2) 0.1482(2) 0.3046(2) 0.0192(8) Uani 1 1 d . . . C19 C 0.21118(19) -0.0400(3) 0.1835(2) 0.0169(8) Uani 1 1 d . . . H19 H 0.2128 0.0295 0.1846 0.020 Uiso 1 1 calc R . . C20 C 0.2569(2) -0.0734(3) 0.1274(2) 0.0265(9) Uani 1 1 d . . . H20A H 0.2561 -0.1415 0.1248 0.040 Uiso 1 1 calc R . . H20B H 0.3064 -0.0519 0.1512 0.040 Uiso 1 1 calc R . . H20C H 0.2376 -0.0480 0.0702 0.040 Uiso 1 1 calc R . . C21 C 0.1331(2) -0.0691(3) 0.1445(3) 0.0312(10) Uani 1 1 d . . . H21A H 0.1304 -0.1369 0.1382 0.047 Uiso 1 1 calc R . . H21B H 0.1146 -0.0397 0.0889 0.047 Uiso 1 1 calc R . . H21C H 0.1044 -0.0492 0.1815 0.047 Uiso 1 1 calc R . . C22 C 0.2195(2) -0.2809(3) 0.4093(2) 0.0206(8) Uani 1 1 d . . . H22 H 0.2438 -0.2914 0.4707 0.025 Uiso 1 1 calc R . . C23 C 0.1385(2) -0.2723(3) 0.3982(3) 0.0288(10) Uani 1 1 d . . . H23A H 0.1290 -0.2150 0.4256 0.043 Uiso 1 1 calc R . . H23B H 0.1222 -0.3261 0.4243 0.043 Uiso 1 1 calc R . . H23C H 0.1128 -0.2702 0.3378 0.043 Uiso 1 1 calc R . . C24 C 0.2336(2) -0.3659(3) 0.3607(3) 0.0351(11) Uani 1 1 d . . . H24A H 0.2080 -0.3589 0.3005 0.053 Uiso 1 1 calc R . . H24B H 0.2167 -0.4220 0.3829 0.053 Uiso 1 1 calc R . . H24C H 0.2851 -0.3712 0.3674 0.053 Uiso 1 1 calc R . . C25 C 0.2697(2) -0.0855(3) 0.5946(2) 0.0240(9) Uani 1 1 d . . . H25 H 0.2556 -0.0557 0.5375 0.029 Uiso 1 1 calc R . . C26 C 0.2033(2) -0.1328(3) 0.6080(3) 0.0344(11) Uani 1 1 d . . . H26A H 0.1850 -0.1789 0.5632 0.052 Uiso 1 1 calc R . . H26B H 0.1663 -0.0860 0.6061 0.052 Uiso 1 1 calc R . . H26C H 0.2161 -0.1639 0.6632 0.052 Uiso 1 1 calc R . . C27 C 0.2958(2) -0.0091(3) 0.6605(3) 0.0325(10) Uani 1 1 d . . . H27A H 0.3058 -0.0359 0.7174 0.049 Uiso 1 1 calc R . . H27B H 0.2587 0.0388 0.6532 0.049 Uiso 1 1 calc R . . H27C H 0.3396 0.0188 0.6533 0.049 Uiso 1 1 calc R . . C28 C 0.4233(2) -0.2822(3) 0.4530(3) 0.0252(9) Uani 1 1 d . . . H28 H 0.3839 -0.2666 0.4010 0.030 Uiso 1 1 calc R . . C29 C 0.4373(3) -0.3865(3) 0.4514(3) 0.0428(12) Uani 1 1 d . . . H29A H 0.4399 -0.4045 0.3950 0.064 Uiso 1 1 calc R . . H29B H 0.3982 -0.4205 0.4648 0.064 Uiso 1 1 calc R . . H29C H 0.4827 -0.4015 0.4935 0.064 Uiso 1 1 calc R . . C30 C 0.4894(2) -0.2276(3) 0.4492(3) 0.0418(12) Uani 1 1 d . . . H30A H 0.4786 -0.1609 0.4463 0.063 Uiso 1 1 calc R . . H30B H 0.5033 -0.2463 0.3989 0.063 Uiso 1 1 calc R . . H30C H 0.5288 -0.2406 0.5001 0.063 Uiso 1 1 calc R . . C31 C 0.43967(19) 0.0111(3) 0.2992(2) 0.0201(9) Uani 1 1 d . . . H31 H 0.4156 -0.0499 0.3020 0.024 Uiso 1 1 calc R . . C32 C 0.5013(2) 0.0221(3) 0.3804(2) 0.0272(10) Uani 1 1 d . . . H32A H 0.5270 0.0802 0.3778 0.041 Uiso 1 1 calc R . . H32B H 0.5344 -0.0305 0.3860 0.041 Uiso 1 1 calc R . . H32C H 0.4821 0.0237 0.4293 0.041 Uiso 1 1 calc R . . C33 C 0.4693(2) 0.0091(3) 0.2225(2) 0.0279(10) Uani 1 1 d . . . H33A H 0.4297 0.0007 0.1708 0.042 Uiso 1 1 calc R . . H33B H 0.5032 -0.0426 0.2283 0.042 Uiso 1 1 calc R . . H33C H 0.4938 0.0679 0.2192 0.042 Uiso 1 1 calc R . . C34 C 0.1978(2) 0.1355(3) 0.3160(2) 0.0217(9) Uani 1 1 d . . . C35 C 0.1331(2) 0.1690(3) 0.2588(2) 0.0248(9) Uani 1 1 d . . . H35A H 0.0934 0.1238 0.2395 0.030 Uiso 1 1 calc R . . H35B H 0.1378 0.2128 0.2142 0.030 Uiso 1 1 calc R . . C36 C 0.1839(2) 0.0858(3) 0.3841(3) 0.0287(10) Uani 1 1 d . . . H36A H 0.2258 0.0686 0.4318 0.034 Uiso 1 1 calc R . . H36B H 0.1461 0.0375 0.3694 0.034 Uiso 1 1 calc R . . C37 C 0.2195(2) 0.3161(3) 0.5745(3) 0.0340(11) Uani 1 1 d . . . H37A H 0.2629 0.3427 0.6133 0.051 Uiso 1 1 calc R . . H37B H 0.2026 0.2643 0.6024 0.051 Uiso 1 1 calc R . . H37C H 0.1822 0.3640 0.5590 0.051 Uiso 1 1 calc R . . C38 C 0.2946(2) 0.3726(3) 0.4633(3) 0.0329(10) Uani 1 1 d . . . H38A H 0.2638 0.4269 0.4442 0.049 Uiso 1 1 calc R . . H38B H 0.3186 0.3560 0.4204 0.049 Uiso 1 1 calc R . . H38C H 0.3306 0.3873 0.5167 0.049 Uiso 1 1 calc R . . C39 C 0.3129(2) 0.1934(3) 0.5267(3) 0.0356(11) Uani 1 1 d . . . H39A H 0.3357 0.1737 0.4836 0.053 Uiso 1 1 calc R . . H39B H 0.2939 0.1387 0.5487 0.053 Uiso 1 1 calc R . . H39C H 0.3483 0.2245 0.5731 0.053 Uiso 1 1 calc R . . C40 C -0.0080(2) 0.1145(3) 0.3598(3) 0.0375(11) Uani 1 1 d . . . H40A H -0.0383 0.0880 0.3924 0.056 Uiso 1 1 calc R . . H40B H 0.0106 0.0644 0.3316 0.056 Uiso 1 1 calc R . . H40C H -0.0364 0.1575 0.3172 0.056 Uiso 1 1 calc R . . C41 C 0.0921(2) 0.0917(3) 0.5174(3) 0.0398(12) Uani 1 1 d . . . H41A H 0.0508 0.0789 0.5384 0.060 Uiso 1 1 calc R . . H41B H 0.1315 0.1164 0.5636 0.060 Uiso 1 1 calc R . . H41C H 0.1075 0.0340 0.4961 0.060 Uiso 1 1 calc R . . C42 C 0.0164(2) 0.2564(3) 0.4812(3) 0.0363(11) Uani 1 1 d . . . H42A H -0.0129 0.2984 0.4383 0.054 Uiso 1 1 calc R . . H42B H 0.0499 0.2930 0.5253 0.054 Uiso 1 1 calc R . . H42C H -0.0147 0.2198 0.5065 0.054 Uiso 1 1 calc R . . C43 C 0.0933(2) 0.4475(3) 0.3912(3) 0.0310(10) Uani 1 1 d . . . H43A H 0.0719 0.5006 0.3557 0.047 Uiso 1 1 calc R . . H43B H 0.1394 0.4661 0.4301 0.047 Uiso 1 1 calc R . . H43C H 0.0611 0.4269 0.4239 0.047 Uiso 1 1 calc R . . C44 C 0.1512(2) 0.4163(3) 0.2563(3) 0.0315(10) Uani 1 1 d . . . H44A H 0.1540 0.3775 0.2085 0.047 Uiso 1 1 calc R . . H44B H 0.1997 0.4340 0.2896 0.047 Uiso 1 1 calc R . . H44C H 0.1234 0.4725 0.2351 0.047 Uiso 1 1 calc R . . C45 C 0.0169(2) 0.3439(3) 0.2495(3) 0.0331(10) Uani 1 1 d . . . H45A H 0.0023 0.4055 0.2253 0.050 Uiso 1 1 calc R . . H45B H -0.0167 0.3225 0.2799 0.050 Uiso 1 1 calc R . . H45C H 0.0169 0.2999 0.2040 0.050 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 0.0174(3) 0.0201(3) 0.0269(3) 0.0001(2) 0.0071(2) -0.0003(2) P1 0.0186(5) 0.0250(6) 0.0258(6) 0.0003(5) 0.0046(5) 0.0015(5) P2 0.0204(6) 0.0247(6) 0.0338(6) 0.0036(5) 0.0107(5) 0.0011(5) P3 0.0199(6) 0.0218(6) 0.0291(6) 0.0021(4) 0.0056(5) -0.0001(4) C1 0.0111(18) 0.0157(19) 0.019(2) -0.0033(15) 0.0064(16) -0.0008(15) C2 0.0119(18) 0.0165(19) 0.0172(19) -0.0001(15) 0.0047(16) 0.0043(15) C3 0.0133(19) 0.0136(19) 0.024(2) 0.0022(15) 0.0076(17) 0.0008(15) C4 0.0139(19) 0.0170(19) 0.018(2) -0.0057(15) 0.0017(16) -0.0059(15) C5 0.0127(19) 0.019(2) 0.017(2) -0.0013(15) 0.0050(16) 0.0025(15) C6 0.0143(19) 0.0158(19) 0.018(2) -0.0009(15) 0.0072(16) 0.0001(15) C7 0.0123(19) 0.0163(19) 0.018(2) 0.0013(15) 0.0018(16) -0.0057(15) C8 0.019(2) 0.019(2) 0.021(2) -0.0001(16) 0.0046(17) -0.0061(16) C9 0.025(2) 0.032(2) 0.018(2) 0.0000(17) 0.0053(18) -0.0093(19) C10 0.020(2) 0.025(2) 0.022(2) 0.0094(17) -0.0033(18) -0.0063(18) C11 0.019(2) 0.017(2) 0.033(2) 0.0057(17) 0.0022(18) 0.0004(17) C12 0.0143(19) 0.0163(19) 0.025(2) 0.0019(16) 0.0030(17) -0.0030(15) C13 0.020(2) 0.0154(19) 0.0078(18) -0.0026(14) 0.0013(16) -0.0027(16) C14 0.018(2) 0.021(2) 0.0137(19) -0.0012(15) 0.0028(16) -0.0046(16) C15 0.018(2) 0.030(2) 0.021(2) 0.0005(17) 0.0036(18) -0.0071(18) C16 0.026(2) 0.019(2) 0.029(2) 0.0049(17) 0.0060(19) -0.0090(17) C17 0.027(2) 0.021(2) 0.024(2) 0.0011(17) 0.0055(18) 0.0038(18) C18 0.020(2) 0.017(2) 0.020(2) -0.0016(16) 0.0050(17) -0.0014(16) C19 0.019(2) 0.0178(19) 0.0128(19) 0.0010(15) 0.0023(16) -0.0015(16) C20 0.030(2) 0.029(2) 0.018(2) 0.0007(17) 0.0026(19) 0.0066(19) C21 0.020(2) 0.040(3) 0.026(2) 0.0074(19) -0.0065(19) -0.008(2) C22 0.021(2) 0.022(2) 0.017(2) 0.0036(16) 0.0036(17) -0.0036(17) C23 0.021(2) 0.031(2) 0.035(2) 0.0039(19) 0.0103(19) -0.0093(19) C24 0.035(3) 0.018(2) 0.054(3) -0.001(2) 0.017(2) -0.0064(19) C25 0.021(2) 0.032(2) 0.021(2) 0.0024(18) 0.0092(18) 0.0023(18) C26 0.026(2) 0.039(3) 0.040(3) 0.001(2) 0.012(2) 0.001(2) C27 0.035(3) 0.030(2) 0.038(3) -0.0020(19) 0.019(2) 0.004(2) C28 0.022(2) 0.024(2) 0.028(2) -0.0003(18) 0.0052(18) 0.0043(18) C29 0.060(3) 0.032(3) 0.038(3) 0.001(2) 0.017(3) 0.020(2) C30 0.028(3) 0.056(3) 0.046(3) 0.006(2) 0.017(2) 0.002(2) C31 0.014(2) 0.022(2) 0.025(2) -0.0021(16) 0.0053(17) -0.0052(16) C32 0.020(2) 0.031(2) 0.030(2) 0.0049(18) 0.0078(19) -0.0005(18) C33 0.024(2) 0.032(2) 0.028(2) -0.0066(18) 0.0092(19) -0.0052(19) C34 0.020(2) 0.019(2) 0.027(2) -0.0081(17) 0.0088(18) -0.0005(17) C35 0.024(2) 0.025(2) 0.024(2) -0.0063(17) 0.0047(18) -0.0024(18) C36 0.029(2) 0.016(2) 0.046(3) 0.0017(18) 0.019(2) 0.0007(18) C37 0.031(2) 0.035(3) 0.033(3) -0.006(2) 0.004(2) 0.000(2) C38 0.026(2) 0.034(3) 0.037(3) 0.001(2) 0.006(2) -0.004(2) C39 0.024(2) 0.039(3) 0.039(3) 0.005(2) 0.002(2) 0.007(2) C40 0.025(2) 0.038(3) 0.051(3) 0.002(2) 0.014(2) -0.009(2) C41 0.034(3) 0.040(3) 0.049(3) 0.016(2) 0.019(2) 0.005(2) C42 0.028(2) 0.038(3) 0.049(3) 0.003(2) 0.022(2) 0.004(2) C43 0.028(2) 0.020(2) 0.044(3) -0.0033(19) 0.010(2) 0.0030(19) C44 0.029(2) 0.026(2) 0.039(3) 0.0057(19) 0.009(2) -0.0006(19) C45 0.024(2) 0.035(3) 0.037(3) 0.002(2) 0.004(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C34 1.974(4) . ? Co1 C35 2.034(4) . ? Co1 C36 2.037(4) . ? Co1 P3 2.1405(12) . ? Co1 P2 2.1564(12) . ? Co1 P1 2.1756(12) . ? P1 C37 1.820(4) . ? P1 C39 1.829(4) . ? P1 C38 1.839(4) . ? P2 C40 1.836(4) . ? P2 C41 1.837(4) . ? P2 C42 1.841(4) . ? P3 C44 1.833(4) . ? P3 C45 1.838(4) . ? P3 C43 1.851(4) . ? C1 C2 1.394(5) . ? C1 C6 1.397(5) . ? C1 H1 0.9500 . ? C2 C3 1.399(5) . ? C2 C7 1.516(5) . ? C3 C4 1.396(5) . ? C3 C22 1.514(5) . ? C4 C5 1.390(5) . ? C4 H4 0.9500 . ? C5 C6 1.408(5) . ? C5 C19 1.513(5) . ? C6 C13 1.510(5) . ? C7 C8 1.392(5) . ? C7 C12 1.409(5) . ? C8 C9 1.417(5) . ? C8 C25 1.507(5) . ? C9 C10 1.370(6) . ? C9 H9 0.9500 . ? C10 C11 1.367(6) . ? C10 H10 0.9500 . ? C11 C12 1.386(5) . ? C11 H11 0.9500 . ? C12 C28 1.531(5) . ? C13 C18 1.407(5) . ? C13 C14 1.414(5) . ? C14 C15 1.397(5) . ? C14 C31 1.523(5) . ? C15 C16 1.376(6) . ? C15 H15 0.9500 . ? C16 C17 1.374(5) . ? C16 H16 0.9500 . ? C17 C18 1.400(5) . ? C17 H17 0.9500 . ? C18 C34 1.492(5) . ? C19 C21 1.531(5) . ? C19 C20 1.531(5) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.526(5) . ? C22 C23 1.540(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.526(6) . ? C25 C26 1.530(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.522(6) . ? C28 C29 1.525(6) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.531(5) . ? C31 C32 1.531(5) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.420(5) . ? C34 C35 1.426(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 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 C34 Co1 C35 41.65(15) . . ? C34 Co1 C36 41.42(15) . . ? C35 Co1 C36 70.44(16) . . ? C34 Co1 P3 120.78(12) . . ? C35 Co1 P3 88.66(12) . . ? C36 Co1 P3 159.09(13) . . ? C34 Co1 P2 123.03(12) . . ? C35 Co1 P2 110.19(12) . . ? C36 Co1 P2 88.12(12) . . ? P3 Co1 P2 99.65(5) . . ? C34 Co1 P1 103.53(12) . . ? C35 Co1 P1 138.92(12) . . ? C36 Co1 P1 97.19(13) . . ? P3 Co1 P1 98.70(5) . . ? P2 Co1 P1 108.28(5) . . ? C37 P1 C39 100.3(2) . . ? C37 P1 C38 98.3(2) . . ? C39 P1 C38 97.7(2) . . ? C37 P1 Co1 117.46(15) . . ? C39 P1 Co1 117.25(16) . . ? C38 P1 Co1 121.60(15) . . ? C40 P2 C41 98.8(2) . . ? C40 P2 C42 99.2(2) . . ? C41 P2 C42 97.3(2) . . ? C40 P2 Co1 115.96(15) . . ? C41 P2 Co1 116.34(15) . . ? C42 P2 Co1 124.61(15) . . ? C44 P3 C45 98.8(2) . . ? C44 P3 C43 98.8(2) . . ? C45 P3 C43 99.3(2) . . ? C44 P3 Co1 120.22(14) . . ? C45 P3 Co1 114.90(15) . . ? C43 P3 Co1 120.66(14) . . ? C2 C1 C6 122.9(3) . . ? C2 C1 H1 118.6 . . ? C6 C1 H1 118.6 . . ? C1 C2 C3 118.7(3) . . ? C1 C2 C7 120.8(3) . . ? C3 C2 C7 120.5(3) . . ? C4 C3 C2 118.0(3) . . ? C4 C3 C22 120.1(3) . . ? C2 C3 C22 121.9(3) . . ? C5 C4 C3 124.0(3) . . ? C5 C4 H4 118.0 . . ? C3 C4 H4 118.0 . . ? C4 C5 C6 117.6(3) . . ? C4 C5 C19 121.5(3) . . ? C6 C5 C19 121.0(3) . . ? C1 C6 C5 118.7(3) . . ? C1 C6 C13 119.8(3) . . ? C5 C6 C13 121.4(3) . . ? C8 C7 C12 120.5(3) . . ? C8 C7 C2 120.6(3) . . ? C12 C7 C2 118.9(3) . . ? C7 C8 C9 118.2(4) . . ? C7 C8 C25 123.4(3) . . ? C9 C8 C25 118.3(3) . . ? C10 C9 C8 121.1(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 121.7(4) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 118.7(3) . . ? C11 C12 C28 118.8(3) . . ? C7 C12 C28 122.4(3) . . ? C18 C13 C14 119.7(3) . . ? C18 C13 C6 119.6(3) . . ? C14 C13 C6 120.6(3) . . ? C15 C14 C13 119.0(3) . . ? C15 C14 C31 118.2(3) . . ? C13 C14 C31 122.7(3) . . ? C16 C15 C14 121.2(4) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 119.7(4) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.6(4) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C13 118.7(3) . . ? C17 C18 C34 119.1(3) . . ? C13 C18 C34 122.1(3) . . ? C5 C19 C21 114.0(3) . . ? C5 C19 C20 109.9(3) . . ? C21 C19 C20 109.9(3) . . ? C5 C19 H19 107.6 . . ? C21 C19 H19 107.6 . . ? C20 C19 H19 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C22 C24 112.0(3) . . ? C3 C22 C23 111.7(3) . . ? C24 C22 C23 109.4(3) . . ? C3 C22 H22 107.8 . . ? C24 C22 H22 107.8 . . ? C23 C22 H22 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C8 C25 C27 112.5(3) . . ? C8 C25 C26 110.3(3) . . ? C27 C25 C26 110.0(3) . . ? C8 C25 H25 108.0 . . ? C27 C25 H25 108.0 . . ? C26 C25 H25 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 110.4(4) . . ? C30 C28 C12 110.5(3) . . ? C29 C28 C12 113.0(3) . . ? C30 C28 H28 107.6 . . ? C29 C28 H28 107.6 . . ? C12 C28 H28 107.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C14 C31 C33 112.6(3) . . ? C14 C31 C32 109.8(3) . . ? C33 C31 C32 109.8(3) . . ? C14 C31 H31 108.2 . . ? C33 C31 H31 108.2 . . ? C32 C31 H31 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C34 C35 111.2(3) . . ? C36 C34 C18 124.1(4) . . ? C35 C34 C18 124.7(3) . . ? C36 C34 Co1 71.7(2) . . ? C35 C34 Co1 71.4(2) . . ? C18 C34 Co1 125.6(3) . . ? C34 C35 Co1 66.9(2) . . ? C34 C35 H35A 117.0 . . ? Co1 C35 H35A 117.0 . . ? C34 C35 H35B 117.0 . . ? Co1 C35 H35B 117.0 . . ? H35A C35 H35B 114.0 . . ? C34 C36 Co1 66.9(2) . . ? C34 C36 H36A 117.0 . . ? Co1 C36 H36A 117.0 . . ? C34 C36 H36B 117.0 . . ? Co1 C36 H36B 117.0 . . ? H36A C36 H36B 114.0 . . ? P1 C37 H37A 109.5 . . ? P1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P1 C38 H38A 109.5 . . ? P1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P1 C39 H39A 109.5 . . ? P1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P2 C40 H40A 109.5 . . ? P2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? P2 C41 H41A 109.5 . . ? P2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P2 C42 H42A 109.5 . . ? P2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P3 C43 H43A 109.5 . . ? P3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? P3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? P3 C44 H44A 109.5 . . ? P3 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? P3 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? P3 C45 H45A 109.5 . . ? P3 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? P3 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.976 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.089 # Attachment '5_D_H_CoPMe33.cif' data_final _database_code_depnum_ccdc_archive 'CCDC 723171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H62 Co P3' _chemical_formula_sum 'C39 H62 Co P3' _chemical_formula_weight 682.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.347(5) _cell_length_b 12.992(3) _cell_length_c 26.446(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8021(3) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8041 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 27.39 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type 'Empirical, SADabs (multi-scan)' _exptl_absorpt_correction_T_min 0.8895 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details 'SADABS 2007/3 (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 SMART APEXII CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 98145 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9193 _reflns_number_gt 7608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.1-4) (Bruker, 2007)' _computing_cell_refinement 'SAINT (7.46A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.46A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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^)+(0.0352P)^2^+3.8133P] 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 9193 _refine_ls_number_parameters 414 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.381162(8) 0.776706(14) 0.200513(7) 0.01556(5) Uani 1 1 d . . . P1 P 0.362416(15) 0.94058(3) 0.201105(13) 0.01782(8) Uani 1 1 d . . . P2 P 0.469493(15) 0.76108(3) 0.176963(14) 0.02044(8) Uani 1 1 d . . . P3 P 0.390289(17) 0.75189(3) 0.280667(14) 0.02457(9) Uani 1 1 d . . . C1 C 0.25254(6) 0.82643(10) 0.03718(5) 0.0170(3) Uani 1 1 d . . . H1A H 0.2441 0.8956 0.0461 0.020 Uiso 1 1 calc R . . C2 C 0.27355(6) 0.80532(11) -0.01110(5) 0.0175(3) Uani 1 1 d . . . C3 C 0.28546(6) 0.70364(11) -0.02394(6) 0.0230(3) Uani 1 1 d . . . H3A H 0.2997 0.6878 -0.0567 0.028 Uiso 1 1 calc R . . C4 C 0.27669(7) 0.62522(11) 0.01086(6) 0.0257(3) Uani 1 1 d . . . H4A H 0.2847 0.5560 0.0017 0.031 Uiso 1 1 calc R . . C5 C 0.25626(6) 0.64752(11) 0.05892(6) 0.0212(3) Uani 1 1 d . . . H5A H 0.2509 0.5934 0.0826 0.025 Uiso 1 1 calc R . . C6 C 0.24359(5) 0.74840(10) 0.07271(5) 0.0161(3) Uani 1 1 d . . . C7 C 0.28234(6) 0.88869(11) -0.04947(5) 0.0204(3) Uani 1 1 d . . . C8 C 0.33438(7) 0.94294(11) -0.05135(5) 0.0246(3) Uani 1 1 d . . . C9 C 0.34218(8) 1.01582(13) -0.08963(6) 0.0370(4) Uani 1 1 d . . . H9A H 0.3775 1.0519 -0.0919 0.044 Uiso 1 1 calc R . . C10 C 0.29928(9) 1.03604(14) -0.12415(7) 0.0435(5) Uani 1 1 d . . . H10A H 0.3052 1.0855 -0.1501 0.052 Uiso 1 1 calc R . . C11 C 0.24794(8) 0.98466(14) -0.12109(6) 0.0381(4) Uani 1 1 d . . . H11A H 0.2183 1.0006 -0.1445 0.046 Uiso 1 1 calc R . . C12 C 0.23850(7) 0.90979(13) -0.08446(6) 0.0285(3) Uani 1 1 d . B . C13 C 0.22064(6) 0.77164(10) 0.12446(5) 0.0170(3) Uani 1 1 d . . . C14 C 0.16362(6) 0.80674(11) 0.12999(5) 0.0198(3) Uani 1 1 d . . . C15 C 0.14215(6) 0.82447(12) 0.17851(6) 0.0246(3) Uani 1 1 d . . . H15A H 0.1043 0.8499 0.1825 0.029 Uiso 1 1 calc R . . C16 C 0.17527(6) 0.80559(12) 0.22095(6) 0.0254(3) Uani 1 1 d . . . H16A H 0.1599 0.8169 0.2537 0.030 Uiso 1 1 calc R . . C17 C 0.23073(6) 0.77028(11) 0.21547(6) 0.0220(3) Uani 1 1 d . . . H17A H 0.2530 0.7568 0.2448 0.026 Uiso 1 1 calc R . . C18 C 0.25500(6) 0.75384(10) 0.16767(5) 0.0177(3) Uani 1 1 d . . . C19 C 0.38237(7) 0.92202(13) -0.01379(6) 0.0280(3) Uani 1 1 d . . . H19A H 0.3657 0.8819 0.0149 0.034 Uiso 1 1 calc R . . C20 C 0.42921(9) 0.85658(18) -0.03743(8) 0.0487(5) Uani 1 1 d . . . H20A H 0.4129 0.7910 -0.0488 0.073 Uiso 1 1 calc R . . H20B H 0.4592 0.8435 -0.0124 0.073 Uiso 1 1 calc R . . H20C H 0.4457 0.8931 -0.0664 0.073 Uiso 1 1 calc R . . C21 C 0.40700(9) 1.02158(15) 0.00803(7) 0.0427(5) Uani 1 1 d . . . H21A H 0.3759 1.0637 0.0218 0.064 Uiso 1 1 calc R . . H21B H 0.4267 1.0599 -0.0188 0.064 Uiso 1 1 calc R . . H21C H 0.4342 1.0050 0.0350 0.064 Uiso 1 1 calc R . . C22 C 0.18151(7) 0.85236(17) -0.08338(7) 0.0415(5) Uani 1 1 d D . . H22A H 0.1902 0.7896 -0.0629 0.050 Uiso 1 1 calc R A 1 C23 C 0.16539(8) 0.80904(15) -0.13455(8) 0.0427(4) Uani 1 1 d . B . H23A H 0.1984 0.7730 -0.1491 0.064 Uiso 1 1 calc R . . H23B H 0.1539 0.8653 -0.1571 0.064 Uiso 1 1 calc R . . H23C H 0.1334 0.7608 -0.1307 0.064 Uiso 1 1 calc R . . C24 C 0.1338(4) 0.9003(8) -0.0557(4) 0.042(2) Uani 0.38(3) 1 d PD B 1 H24A H 0.1238 0.9660 -0.0717 0.062 Uiso 0.38(3) 1 calc PR B 1 H24B H 0.1452 0.9125 -0.0206 0.062 Uiso 0.38(3) 1 calc PR B 1 H24C H 0.1005 0.8544 -0.0565 0.062 Uiso 0.38(3) 1 calc PR B 1 C24A C 0.1338(3) 0.9336(14) -0.0707(7) 0.091(4) Uani 0.62(3) 1 d PD B 2 H24D H 0.0965 0.8992 -0.0692 0.137 Uiso 0.62(3) 1 calc PR B 2 H24E H 0.1330 0.9865 -0.0971 0.137 Uiso 0.62(3) 1 calc PR B 2 H24F H 0.1421 0.9656 -0.0380 0.137 Uiso 0.62(3) 1 calc PR B 2 C25 C 0.12346(6) 0.82184(12) 0.08527(6) 0.0246(3) Uani 1 1 d . . . H25A H 0.1444 0.8012 0.0539 0.030 Uiso 1 1 calc R . . C26 C 0.10616(8) 0.93514(14) 0.08000(8) 0.0403(4) Uani 1 1 d . . . H26A H 0.1406 0.9775 0.0761 0.060 Uiso 1 1 calc R . . H26B H 0.0852 0.9569 0.1103 0.060 Uiso 1 1 calc R . . H26C H 0.0816 0.9435 0.0502 0.060 Uiso 1 1 calc R . . C27 C 0.07012(7) 0.75388(15) 0.09005(7) 0.0359(4) Uani 1 1 d . . . H27A H 0.0818 0.6820 0.0947 0.054 Uiso 1 1 calc R . . H27B H 0.0470 0.7599 0.0593 0.054 Uiso 1 1 calc R . . H27C H 0.0474 0.7762 0.1192 0.054 Uiso 1 1 calc R . . C28 C 0.31524(6) 0.71590(10) 0.16393(5) 0.0179(3) Uani 1 1 d . . . C29 C 0.35664(6) 0.75040(11) 0.12767(5) 0.0192(3) Uani 1 1 d . . . H29A H 0.3463 0.8113 0.1071 0.023 Uiso 1 1 calc R . . H29B H 0.3778 0.6967 0.1088 0.023 Uiso 1 1 calc R . . C30 C 0.33928(6) 0.63801(11) 0.19597(6) 0.0229(3) Uani 1 1 d . . . H30A H 0.3598 0.5808 0.1792 0.028 Uiso 1 1 calc R . . H30B H 0.3164 0.6168 0.2257 0.028 Uiso 1 1 calc R . . C31 C 0.31196(8) 0.99093(13) 0.24811(7) 0.0333(4) Uani 1 1 d . . . H31A H 0.3082 1.0656 0.2439 0.050 Uiso 1 1 calc R . . H31B H 0.3262 0.9758 0.2822 0.050 Uiso 1 1 calc R . . H31C H 0.2745 0.9583 0.2434 0.050 Uiso 1 1 calc R . . C32 C 0.33034(7) 0.99681(12) 0.14455(6) 0.0300(4) Uani 1 1 d . . . H32A H 0.3238 1.0705 0.1501 0.045 Uiso 1 1 calc R . . H32B H 0.2938 0.9627 0.1375 0.045 Uiso 1 1 calc R . . H32C H 0.3563 0.9875 0.1158 0.045 Uiso 1 1 calc R . . C33 C 0.42084(7) 1.03363(13) 0.21065(7) 0.0316(4) Uani 1 1 d . . . H33A H 0.4053 1.1037 0.2099 0.047 Uiso 1 1 calc R . . H33B H 0.4493 1.0258 0.1837 0.047 Uiso 1 1 calc R . . H33C H 0.4391 1.0210 0.2435 0.047 Uiso 1 1 calc R . . C34 C 0.53082(7) 0.80192(15) 0.21604(6) 0.0323(4) Uani 1 1 d . . . H34A H 0.5665 0.7909 0.1972 0.048 Uiso 1 1 calc R . . H34B H 0.5316 0.7615 0.2473 0.048 Uiso 1 1 calc R . . H34C H 0.5270 0.8751 0.2243 0.048 Uiso 1 1 calc R . . C35 C 0.49350(7) 0.63052(13) 0.16075(6) 0.0299(3) Uani 1 1 d . . . H35A H 0.5339 0.6324 0.1508 0.045 Uiso 1 1 calc R . . H35B H 0.4704 0.6040 0.1327 0.045 Uiso 1 1 calc R . . H35C H 0.4890 0.5854 0.1902 0.045 Uiso 1 1 calc R . . C36 C 0.48983(7) 0.82776(14) 0.11825(6) 0.0302(3) Uani 1 1 d . . . H36A H 0.5294 0.8099 0.1094 0.045 Uiso 1 1 calc R . . H36B H 0.4868 0.9023 0.1232 0.045 Uiso 1 1 calc R . . H36C H 0.4641 0.8066 0.0909 0.045 Uiso 1 1 calc R . . C37 C 0.32750(8) 0.73714(14) 0.32231(6) 0.0332(4) Uani 1 1 d . . . H37A H 0.3404 0.7228 0.3569 0.050 Uiso 1 1 calc R . . H37B H 0.3038 0.6800 0.3102 0.050 Uiso 1 1 calc R . . H37C H 0.3050 0.8008 0.3220 0.050 Uiso 1 1 calc R . . C38 C 0.42760(8) 0.63253(15) 0.29772(6) 0.0389(4) Uani 1 1 d . . . H38A H 0.4292 0.6263 0.3346 0.058 Uiso 1 1 calc R . . H38B H 0.4666 0.6341 0.2840 0.058 Uiso 1 1 calc R . . H38C H 0.4069 0.5735 0.2836 0.058 Uiso 1 1 calc R . . C39 C 0.43078(8) 0.84445(16) 0.31965(6) 0.0383(4) Uani 1 1 d . . . H39A H 0.4338 0.8183 0.3543 0.057 Uiso 1 1 calc R . . H39B H 0.4108 0.9108 0.3199 0.057 Uiso 1 1 calc R . . H39C H 0.4692 0.8534 0.3055 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01502(9) 0.01827(10) 0.01340(9) 0.00125(7) -0.00051(7) 0.00199(7) P1 0.01724(17) 0.01798(17) 0.01824(17) -0.00112(13) -0.00205(13) 0.00008(13) P2 0.01493(17) 0.02744(19) 0.01896(18) -0.00097(14) -0.00061(13) 0.00209(14) P3 0.0247(2) 0.0336(2) 0.01545(18) 0.00416(15) 0.00067(14) 0.00978(16) C1 0.0150(6) 0.0168(6) 0.0192(6) -0.0018(5) -0.0034(5) 0.0010(5) C2 0.0143(6) 0.0208(7) 0.0176(6) -0.0003(5) -0.0031(5) -0.0014(5) C3 0.0257(7) 0.0235(7) 0.0197(7) -0.0046(6) 0.0043(6) -0.0032(6) C4 0.0328(8) 0.0165(7) 0.0276(8) -0.0050(6) 0.0094(6) -0.0021(6) C5 0.0239(7) 0.0164(6) 0.0234(7) -0.0001(5) 0.0054(6) -0.0026(5) C6 0.0108(6) 0.0191(6) 0.0183(6) -0.0027(5) -0.0005(5) -0.0006(5) C7 0.0258(7) 0.0196(7) 0.0156(6) -0.0016(5) -0.0010(5) 0.0001(6) C8 0.0319(8) 0.0233(7) 0.0185(7) -0.0001(6) -0.0023(6) -0.0061(6) C9 0.0501(11) 0.0332(9) 0.0278(8) 0.0060(7) -0.0056(8) -0.0198(8) C10 0.0729(14) 0.0309(9) 0.0269(9) 0.0122(7) -0.0116(9) -0.0140(9) C11 0.0518(11) 0.0360(9) 0.0265(8) 0.0084(7) -0.0160(8) -0.0015(8) C12 0.0308(8) 0.0329(8) 0.0219(7) 0.0025(6) -0.0056(6) 0.0001(7) C13 0.0173(6) 0.0145(6) 0.0193(7) -0.0013(5) 0.0031(5) -0.0024(5) C14 0.0161(7) 0.0191(7) 0.0242(7) -0.0022(5) 0.0015(5) -0.0005(5) C15 0.0170(7) 0.0265(7) 0.0302(8) -0.0050(6) 0.0055(6) 0.0006(6) C16 0.0213(7) 0.0325(8) 0.0224(7) -0.0052(6) 0.0085(6) -0.0028(6) C17 0.0203(7) 0.0263(7) 0.0194(7) -0.0014(6) 0.0022(5) -0.0023(6) C18 0.0164(6) 0.0158(6) 0.0210(7) -0.0014(5) 0.0032(5) -0.0028(5) C19 0.0258(8) 0.0361(9) 0.0219(7) 0.0022(6) -0.0018(6) -0.0106(7) C20 0.0376(11) 0.0683(14) 0.0402(11) -0.0102(10) -0.0085(9) 0.0083(10) C21 0.0466(11) 0.0470(11) 0.0345(10) -0.0029(8) -0.0110(8) -0.0188(9) C22 0.0276(9) 0.0649(13) 0.0320(9) 0.0143(9) -0.0115(7) -0.0050(8) C23 0.0365(10) 0.0354(10) 0.0562(12) -0.0110(9) 0.0028(9) -0.0059(8) C24 0.048(4) 0.054(5) 0.023(3) -0.005(3) 0.014(3) -0.019(3) C24A 0.035(3) 0.158(9) 0.081(6) -0.083(6) 0.000(3) -0.013(4) C25 0.0169(7) 0.0299(8) 0.0272(8) -0.0044(6) -0.0005(6) 0.0042(6) C26 0.0396(10) 0.0340(9) 0.0474(11) 0.0003(8) -0.0114(8) 0.0107(8) C27 0.0217(8) 0.0461(10) 0.0398(10) -0.0129(8) -0.0017(7) -0.0045(7) C28 0.0175(7) 0.0177(6) 0.0185(6) -0.0031(5) 0.0007(5) -0.0013(5) C29 0.0170(6) 0.0235(7) 0.0171(6) -0.0033(5) -0.0002(5) -0.0003(5) C30 0.0235(7) 0.0187(7) 0.0266(8) 0.0011(6) 0.0032(6) 0.0012(6) C31 0.0369(9) 0.0259(8) 0.0371(9) -0.0048(7) 0.0100(8) 0.0050(7) C32 0.0372(9) 0.0209(7) 0.0317(8) 0.0049(6) -0.0128(7) 0.0013(6) C33 0.0270(8) 0.0262(8) 0.0417(10) -0.0044(7) -0.0073(7) -0.0061(6) C34 0.0187(7) 0.0467(10) 0.0315(8) -0.0073(7) -0.0058(6) 0.0018(7) C35 0.0214(8) 0.0342(9) 0.0340(9) -0.0036(7) 0.0020(6) 0.0070(6) C36 0.0203(7) 0.0429(9) 0.0275(8) 0.0038(7) 0.0041(6) -0.0025(7) C37 0.0356(9) 0.0458(10) 0.0181(7) 0.0086(7) 0.0066(6) 0.0129(8) C38 0.0396(10) 0.0499(11) 0.0273(8) 0.0153(8) 0.0036(7) 0.0223(8) C39 0.0373(10) 0.0584(12) 0.0193(8) -0.0061(8) -0.0090(7) 0.0071(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. PLATON/SQUEEZE was run to analyze the potential void space but nothing was found. See end of this file for output results. ; 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 C28 1.9820(14) . ? Co1 C29 2.0384(14) . ? Co1 C30 2.0537(15) . ? Co1 P3 2.1547(6) . ? Co1 P2 2.1638(6) . ? Co1 P1 2.1735(6) . ? P1 C32 1.8252(16) . ? P1 C31 1.8333(16) . ? P1 C33 1.8400(16) . ? P2 C35 1.8371(16) . ? P2 C36 1.8405(16) . ? P2 C34 1.8438(16) . ? P3 C38 1.8347(17) . ? P3 C37 1.8434(17) . ? P3 C39 1.8447(19) . ? C1 C2 1.3950(19) . ? C1 C6 1.3979(19) . ? C1 H1A 0.9500 . ? C2 C3 1.392(2) . ? C2 C7 1.4982(19) . ? C3 C4 1.388(2) . ? C3 H3A 0.9500 . ? C4 C5 1.388(2) . ? C4 H4A 0.9500 . ? C5 C6 1.3921(19) . ? C5 H5A 0.9500 . ? C6 C13 1.5004(19) . ? C7 C8 1.405(2) . ? C7 C12 1.407(2) . ? C8 C9 1.398(2) . ? C8 C19 1.522(2) . ? C9 C10 1.381(3) . ? C9 H9A 0.9500 . ? C10 C11 1.374(3) . ? C10 H10A 0.9500 . ? C11 C12 1.390(2) . ? C11 H11A 0.9500 . ? C12 C22 1.526(2) . ? C13 C14 1.4147(19) . ? C13 C18 1.415(2) . ? C14 C15 1.396(2) . ? C14 C25 1.522(2) . ? C15 C16 1.385(2) . ? C15 H15A 0.9500 . ? C16 C17 1.381(2) . ? C16 H16A 0.9500 . ? C17 C18 1.402(2) . ? C17 H17A 0.9500 . ? C18 C28 1.4936(19) . ? C19 C20 1.520(3) . ? C19 C21 1.528(2) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.471(8) . ? C22 C23 1.513(3) . ? C22 C24A 1.570(8) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25 C27 1.532(2) . ? C25 C26 1.533(2) . ? C25 H25A 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.4333(19) . ? C28 C30 1.434(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 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 C28 Co1 C29 41.74(5) . . ? C28 Co1 C30 41.58(6) . . ? C29 Co1 C30 70.36(6) . . ? C28 Co1 P3 119.82(4) . . ? C29 Co1 P3 158.80(4) . . ? C30 Co1 P3 88.47(4) . . ? C28 Co1 P2 124.20(4) . . ? C29 Co1 P2 88.85(4) . . ? C30 Co1 P2 110.77(4) . . ? P3 Co1 P2 100.071(17) . . ? C28 Co1 P1 103.74(4) . . ? C29 Co1 P1 96.57(4) . . ? C30 Co1 P1 139.81(4) . . ? P3 Co1 P1 99.173(17) . . ? P2 Co1 P1 106.613(16) . . ? C32 P1 C31 98.58(8) . . ? C32 P1 C33 98.83(8) . . ? C31 P1 C33 98.56(8) . . ? C32 P1 Co1 117.96(5) . . ? C31 P1 Co1 118.93(6) . . ? C33 P1 Co1 119.69(6) . . ? C35 P2 C36 99.15(8) . . ? C35 P2 C34 99.18(8) . . ? C36 P2 C34 97.88(8) . . ? C35 P2 Co1 116.40(6) . . ? C36 P2 Co1 116.40(5) . . ? C34 P2 Co1 123.49(6) . . ? C38 P3 C37 98.21(8) . . ? C38 P3 C39 99.80(9) . . ? C37 P3 C39 98.13(9) . . ? C38 P3 Co1 114.53(6) . . ? C37 P3 Co1 121.64(6) . . ? C39 P3 Co1 120.20(6) . . ? C2 C1 C6 121.68(12) . . ? C2 C1 H1A 119.2 . . ? C6 C1 H1A 119.2 . . ? C3 C2 C1 118.69(13) . . ? C3 C2 C7 119.57(12) . . ? C1 C2 C7 121.73(12) . . ? C4 C3 C2 120.35(13) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 120.31(13) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 120.61(13) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 118.35(12) . . ? C5 C6 C13 120.28(12) . . ? C1 C6 C13 121.37(12) . . ? C8 C7 C12 120.52(14) . . ? C8 C7 C2 120.33(13) . . ? C12 C7 C2 119.12(13) . . ? C9 C8 C7 118.56(15) . . ? C9 C8 C19 119.84(14) . . ? C7 C8 C19 121.58(13) . . ? C10 C9 C8 120.88(16) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C11 C10 C9 120.09(16) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 121.27(16) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C11 C12 C7 118.64(15) . . ? C11 C12 C22 119.56(15) . . ? C7 C12 C22 121.79(14) . . ? C14 C13 C18 120.17(13) . . ? C14 C13 C6 119.69(12) . . ? C18 C13 C6 120.08(12) . . ? C15 C14 C13 119.08(13) . . ? C15 C14 C25 118.13(13) . . ? C13 C14 C25 122.74(13) . . ? C16 C15 C14 121.00(14) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C17 C16 C15 119.80(14) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 121.62(14) . . ? C16 C17 H17A 119.2 . . ? C18 C17 H17A 119.2 . . ? C17 C18 C13 118.30(13) . . ? C17 C18 C28 119.39(13) . . ? C13 C18 C28 122.30(12) . . ? C20 C19 C8 111.17(14) . . ? C20 C19 C21 110.98(15) . . ? C8 C19 C21 111.85(14) . . ? C20 C19 H19A 107.5 . . ? C8 C19 H19A 107.5 . . ? C21 C19 H19A 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C23 114.4(5) . . ? C24 C22 C12 117.6(5) . . ? C23 C22 C12 112.45(15) . . ? C23 C22 C24A 105.3(4) . . ? C12 C22 C24A 107.1(6) . . ? C24 C22 H22A 103.4 . . ? C23 C22 H22A 103.4 . . ? C12 C22 H22A 103.4 . . ? C24A C22 H22A 125.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? C22 C24A H24D 109.5 . . ? C22 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C14 C25 C27 111.25(13) . . ? C14 C25 C26 110.91(13) . . ? C27 C25 C26 110.29(14) . . ? C14 C25 H25A 108.1 . . ? C27 C25 H25A 108.1 . . ? C26 C25 H25A 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 110.62(12) . . ? C29 C28 C18 125.17(13) . . ? C30 C28 C18 124.21(13) . . ? C29 C28 Co1 71.24(8) . . ? C30 C28 Co1 71.89(8) . . ? C18 C28 Co1 124.56(10) . . ? C28 C29 Co1 67.02(8) . . ? C28 C29 H29A 117.0 . . ? Co1 C29 H29A 117.0 . . ? C28 C29 H29B 117.0 . . ? Co1 C29 H29B 117.0 . . ? H29A C29 H29B 114.0 . . ? C28 C30 Co1 66.53(8) . . ? C28 C30 H30A 117.1 . . ? Co1 C30 H30A 117.1 . . ? C28 C30 H30B 117.1 . . ? Co1 C30 H30B 117.1 . . ? H30A C30 H30B 114.1 . . ? P1 C31 H31A 109.5 . . ? P1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P1 C32 H32A 109.5 . . ? P1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P1 C33 H33A 109.5 . . ? P1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P2 C34 H34A 109.5 . . ? P2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? P2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? P2 C35 H35A 109.5 . . ? P2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P2 C36 H36A 109.5 . . ? P2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? P2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P3 C37 H37A 109.5 . . ? P3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P3 C38 H38A 109.5 . . ? P3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.474 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.048 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 108 2 ' ' 2 0.500 0.000 0.500 108 2 ' ' 3 0.000 0.500 0.500 108 2 ' ' 4 0.500 0.500 1.000 108 2 ' ' _platon_squeeze_details ; ; # TITL final P b c a R = 0.03 # CELL 23.3470 12.9920 26.4460 90.00 90.00 90.00 # SPGR Pbca # Note: Atoms in Void as Cxxx and Qxxx all others # Q101 0.618 0.284 0.296 ! 0.56 eA-3