# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'John Arnold' _publ_contact_author_email ARNOLD@BERKELEY.EDU _publ_section_title ; Reactivity of a Co(I) [N2P2] Complex with Azides: Evidence for a Transient Co(III) Imido Species ; loop_ _publ_author_name 'John Arnold' 'Wayne A Chomitz' # Attachment 'wac6067xs.cif' data_wac6067xs _database_code_depnum_ccdc_archive 'CCDC 677811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Co I N2 P2 Si' _chemical_formula_sum 'C22 H51 Co I N2 P2 Si' _chemical_formula_weight 619.51 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.356(2) _cell_length_b 34.812(8) _cell_length_c 9.299(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.015(4) _cell_angle_gamma 90.00 _cell_volume 2925.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 2649 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 23.3 _exptl_crystal_description block-like _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 1.804 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16609 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.36 _reflns_number_total 5914 _reflns_number_gt 4254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.631' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Towards the end of the refinement process two unusually large peak were found in the difference Fourier map near C17 and C20. These were modeled as fractional methine carbons with isotropic thermal parameters. The occupancy of C17B and C20B refined to 0.337(10). The nature of the disorder appears to be a wag around the phosphorus (P2) and a rotation around the C17-P2 and C20-P2 bonds such that the methyl groups of the two isopropyl groups are shared over both methine positions. The C17-P2, C17B-P2, C20-P2, and C20B-P2 bond distances were constrained with a loose constraint. ; _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^)+(0.0500P)^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 5914 _refine_ls_number_parameters 261 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.032 _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 I1 I 0.58770(3) 0.167573(8) 0.37479(3) 0.03488(10) Uani 1 1 d . . . Co1 Co 0.72971(6) 0.123564(15) 0.21295(6) 0.02241(14) Uani 1 1 d . A . Si1 Si 0.84795(13) 0.04770(3) 0.17225(13) 0.0281(3) Uani 1 1 d . A . P1 P 0.96500(11) 0.15480(3) 0.29272(12) 0.0274(2) Uani 1 1 d . A . P2 P 0.62389(11) 0.14144(3) -0.04159(12) 0.0301(3) Uani 1 1 d D . . N1 N 0.7176(4) 0.06827(9) 0.2447(4) 0.0260(7) Uani 1 1 d . . . N2 N 0.8979(3) 0.08725(9) 0.0739(4) 0.0267(8) Uani 1 1 d . . . C1 C 0.6366(4) 0.04853(12) 0.3407(5) 0.0294(9) Uani 1 1 d . A . C2 C 0.6395(6) 0.00428(12) 0.3219(6) 0.0467(12) Uani 1 1 d . . . H2A H 0.5946 -0.0025 0.2176 0.070 Uiso 1 1 calc R A . H2B H 0.5837 -0.0079 0.3853 0.070 Uiso 1 1 calc R . . H2C H 0.7422 -0.0048 0.3508 0.070 Uiso 1 1 calc R . . C3 C 0.7074(5) 0.05780(13) 0.5049(5) 0.0378(11) Uani 1 1 d . . . H3A H 0.7068 0.0857 0.5199 0.057 Uiso 1 1 calc R A . H3B H 0.8096 0.0484 0.5328 0.057 Uiso 1 1 calc R . . H3C H 0.6510 0.0453 0.5670 0.057 Uiso 1 1 calc R . . C4 C 0.4737(5) 0.06037(13) 0.2993(6) 0.0418(12) Uani 1 1 d . . . H4A H 0.4663 0.0883 0.3099 0.063 Uiso 1 1 calc R A . H4B H 0.4228 0.0474 0.3655 0.063 Uiso 1 1 calc R . . H4C H 0.4276 0.0530 0.1960 0.063 Uiso 1 1 calc R . . C5 C 0.7868(6) 0.00731(13) 0.0355(6) 0.0480(13) Uani 1 1 d . . . H5A H 0.6983 0.0152 -0.0410 0.072 Uiso 1 1 calc R A . H5B H 0.7641 -0.0154 0.0878 0.072 Uiso 1 1 calc R . . H5C H 0.8663 0.0011 -0.0117 0.072 Uiso 1 1 calc R . . C6 C 1.0173(5) 0.02833(13) 0.3099(5) 0.0428(12) Uani 1 1 d . . . H6A H 1.0565 0.0478 0.3858 0.064 Uiso 1 1 calc R A . H6B H 1.0927 0.0218 0.2578 0.064 Uiso 1 1 calc R . . H6C H 0.9908 0.0053 0.3575 0.064 Uiso 1 1 calc R . . C7 C 1.0521(4) 0.10167(12) 0.1108(5) 0.0313(10) Uani 1 1 d . A . H7A H 1.0611 0.1210 0.0357 0.038 Uiso 1 1 calc R . . H7B H 1.1191 0.0801 0.1046 0.038 Uiso 1 1 calc R . . C8 C 1.1022(4) 0.11974(12) 0.2656(5) 0.0316(10) Uani 1 1 d . . . H8A H 1.1988 0.1327 0.2768 0.038 Uiso 1 1 calc R A . H8B H 1.1151 0.0994 0.3424 0.038 Uiso 1 1 calc R . . C9 C 1.0282(5) 0.16982(13) 0.4894(5) 0.0377(11) Uani 1 1 d . . . H9A H 0.9581 0.1902 0.5043 0.045 Uiso 1 1 calc R A . C10 C 1.0120(5) 0.13629(15) 0.5893(5) 0.0504(13) Uani 1 1 d . A . H10A H 1.0455 0.1442 0.6938 0.076 Uiso 1 1 calc R . . H10B H 1.0721 0.1146 0.5715 0.076 Uiso 1 1 calc R . . H10C H 0.9079 0.1285 0.5670 0.076 Uiso 1 1 calc R . . C11 C 1.1830(5) 0.18731(15) 0.5364(6) 0.0487(13) Uani 1 1 d . A . H11A H 1.2062 0.1943 0.6421 0.073 Uiso 1 1 calc R . . H11B H 1.1867 0.2103 0.4768 0.073 Uiso 1 1 calc R . . H11C H 1.2556 0.1685 0.5207 0.073 Uiso 1 1 calc R . . C12 C 0.9879(5) 0.19671(12) 0.1777(5) 0.0363(11) Uani 1 1 d . . . H12A H 0.9255 0.1909 0.0753 0.044 Uiso 1 1 calc R A . C13 C 0.9172(5) 0.23246(13) 0.2279(6) 0.0480(13) Uani 1 1 d . A . H13A H 0.9296 0.2545 0.1668 0.072 Uiso 1 1 calc R . . H13B H 0.9655 0.2378 0.3327 0.072 Uiso 1 1 calc R . . H13C H 0.8115 0.2278 0.2163 0.072 Uiso 1 1 calc R . . C14 C 1.1423(5) 0.20500(15) 0.1584(6) 0.0551(15) Uani 1 1 d . A . H14A H 1.1386 0.2278 0.0956 0.083 Uiso 1 1 calc R . . H14B H 1.1766 0.1829 0.1111 0.083 Uiso 1 1 calc R . . H14C H 1.2108 0.2096 0.2561 0.083 Uiso 1 1 calc R . . C15 C 0.8296(5) 0.08880(12) -0.0874(5) 0.0339(10) Uani 1 1 d . A . H15A H 0.7503 0.0693 -0.1135 0.041 Uiso 1 1 calc R . . H15B H 0.9051 0.0822 -0.1408 0.041 Uiso 1 1 calc R . . C16 C 0.7642(4) 0.12819(13) -0.1400(5) 0.0321(10) Uani 1 1 d . A . H16A H 0.7184 0.1275 -0.2486 0.039 Uiso 1 1 calc R . . H16B H 0.8439 0.1477 -0.1203 0.039 Uiso 1 1 calc R . . C17 C 0.4733(6) 0.1033(2) -0.1180(7) 0.0271(17) Uiso 0.661(10) 1 d PD A 1 H17A H 0.5115 0.0782 -0.0707 0.033 Uiso 0.661(10) 1 calc PR A 1 C18 C 0.4401(5) 0.09778(16) -0.2822(6) 0.0579(15) Uani 1 1 d D . . H18A H 0.5313 0.0911 -0.3097 0.087 Uiso 0.661(10) 1 calc PR A 1 H18B H 0.3994 0.1216 -0.3327 0.087 Uiso 0.661(10) 1 calc PR A 1 H18C H 0.3677 0.0770 -0.3123 0.087 Uiso 0.661(10) 1 calc PR A 1 H18D H 0.5105 0.1070 -0.3362 0.087 Uiso 0.339(10) 1 d PR A 2 H18E H 0.3401 0.0977 -0.3491 0.087 Uiso 0.339(10) 1 d PR A 2 H18F H 0.4669 0.0716 -0.2460 0.087 Uiso 0.339(10) 1 d PR A 2 C19 C 0.3391(5) 0.11401(18) -0.0619(6) 0.0593(16) Uani 1 1 d D . . H19A H 0.3696 0.1173 0.0465 0.089 Uiso 0.661(10) 1 calc PR A 1 H19B H 0.2649 0.0935 -0.0874 0.089 Uiso 0.661(10) 1 calc PR A 1 H19C H 0.2964 0.1381 -0.1086 0.089 Uiso 0.661(10) 1 calc PR A 1 H19D H 0.3440 0.1322 0.0196 0.089 Uiso 0.339(10) 1 d PR A 2 H19E H 0.3635 0.0882 -0.0208 0.089 Uiso 0.339(10) 1 d PR A 2 H19F H 0.2388 0.1140 -0.1283 0.089 Uiso 0.339(10) 1 d PR A 2 C17B C 0.4425(12) 0.1243(4) -0.1506(12) 0.037(4) Uiso 0.339(10) 1 d PD A 2 H17B H 0.3970 0.1483 -0.2016 0.045 Uiso 0.339(10) 1 calc PR A 2 C20 C 0.5454(8) 0.18552(19) -0.1330(8) 0.0342(19) Uiso 0.661(10) 1 d PD A 1 H20A H 0.4612 0.1767 -0.2164 0.041 Uiso 0.661(10) 1 calc PR A 1 C21 C 0.4686(6) 0.21034(15) -0.0312(6) 0.0515(13) Uani 1 1 d D . . H21A H 0.4099 0.1935 0.0158 0.077 Uiso 0.661(10) 1 calc PR A 1 H21B H 0.4037 0.2296 -0.0924 0.077 Uiso 0.661(10) 1 calc PR A 1 H21C H 0.5446 0.2233 0.0459 0.077 Uiso 0.661(10) 1 calc PR A 1 H21D H 0.4697 0.1996 0.0665 0.077 Uiso 0.339(10) 1 d PR A 2 H21E H 0.3824 0.2005 -0.1059 0.077 Uiso 0.339(10) 1 d PR A 2 H21F H 0.4629 0.2384 -0.0273 0.077 Uiso 0.339(10) 1 d PR A 2 C22 C 0.6319(9) 0.20988(15) -0.2051(8) 0.094(3) Uani 1 1 d D . . H22A H 0.6780 0.1941 -0.2680 0.142 Uiso 0.661(10) 1 calc PR A 1 H22B H 0.7089 0.2230 -0.1293 0.142 Uiso 0.661(10) 1 calc PR A 1 H22C H 0.5671 0.2290 -0.2667 0.142 Uiso 0.661(10) 1 calc PR A 1 H22D H 0.7272 0.1989 -0.2086 0.142 Uiso 0.339(10) 1 d PR A 2 H22E H 0.6363 0.2379 -0.2121 0.142 Uiso 0.339(10) 1 d PR A 2 H22F H 0.5539 0.2000 -0.2885 0.142 Uiso 0.339(10) 1 d PR A 2 C20B C 0.6028(11) 0.1980(3) -0.0677(12) 0.017(3) Uiso 0.339(10) 1 d PD A 2 H20B H 0.6854 0.2091 0.0120 0.021 Uiso 0.339(10) 1 calc PR A 2 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 I1 0.03498(17) 0.03786(17) 0.03542(18) -0.00371(13) 0.01566(13) 0.00847(13) Co1 0.0221(3) 0.0239(3) 0.0228(3) 0.0008(2) 0.0086(2) 0.0019(2) Si1 0.0294(6) 0.0248(6) 0.0334(7) 0.0002(5) 0.0140(5) 0.0041(5) P1 0.0212(5) 0.0290(6) 0.0311(6) -0.0009(5) 0.0053(5) 0.0015(4) P2 0.0231(5) 0.0434(7) 0.0257(6) 0.0073(5) 0.0096(5) 0.0032(5) N1 0.0331(19) 0.0205(17) 0.0290(19) 0.0028(15) 0.0160(15) 0.0013(14) N2 0.0241(17) 0.0326(19) 0.0256(18) 0.0013(15) 0.0102(15) 0.0003(15) C1 0.031(2) 0.029(2) 0.032(2) 0.0076(19) 0.0155(19) 0.0013(18) C2 0.061(3) 0.029(2) 0.058(3) 0.007(2) 0.030(3) -0.006(2) C3 0.046(3) 0.044(3) 0.027(2) 0.009(2) 0.016(2) 0.002(2) C4 0.032(2) 0.046(3) 0.052(3) 0.006(2) 0.018(2) 0.000(2) C5 0.061(3) 0.037(3) 0.056(3) -0.014(2) 0.032(3) -0.005(2) C6 0.036(3) 0.041(3) 0.052(3) 0.013(2) 0.014(2) 0.012(2) C7 0.028(2) 0.033(2) 0.038(3) 0.0009(19) 0.019(2) 0.0039(18) C8 0.021(2) 0.034(2) 0.040(3) 0.002(2) 0.0083(19) 0.0049(18) C9 0.031(2) 0.042(3) 0.037(3) -0.006(2) 0.004(2) 0.006(2) C10 0.042(3) 0.074(4) 0.031(3) 0.003(3) 0.002(2) -0.002(3) C11 0.042(3) 0.048(3) 0.047(3) -0.005(2) -0.005(2) 0.000(2) C12 0.029(2) 0.035(2) 0.045(3) 0.003(2) 0.010(2) -0.0034(19) C13 0.046(3) 0.035(3) 0.062(4) 0.005(2) 0.010(3) 0.004(2) C14 0.043(3) 0.048(3) 0.083(4) 0.014(3) 0.031(3) -0.007(2) C15 0.029(2) 0.047(3) 0.029(2) -0.002(2) 0.0139(19) 0.000(2) C16 0.025(2) 0.047(3) 0.026(2) 0.004(2) 0.0101(18) -0.0021(19) C18 0.038(3) 0.071(4) 0.065(4) -0.025(3) 0.014(3) -0.002(3) C19 0.038(3) 0.091(4) 0.055(4) 0.004(3) 0.022(3) -0.015(3) C21 0.058(3) 0.047(3) 0.050(3) 0.011(3) 0.016(3) 0.005(3) C22 0.170(7) 0.031(3) 0.117(6) 0.011(3) 0.098(6) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Co1 2.7228(7) . ? Co1 N1 1.955(3) . ? Co1 P1 2.3943(13) . ? Co1 P2 2.3992(13) . ? Si1 N1 1.697(3) . ? Si1 N2 1.781(3) . ? Si1 C5 1.883(5) . ? Si1 C6 1.885(4) . ? P1 C8 1.835(4) . ? P1 C9 1.846(5) . ? P1 C12 1.854(4) . ? P2 C17B 1.836(10) . ? P2 C20 1.815(6) . ? P2 C16 1.843(4) . ? P2 C17 1.932(6) . ? P2 C20B 1.987(9) . ? N1 C1 1.481(5) . ? N2 C15 1.471(5) . ? N2 C7 1.481(5) . ? C1 C4 1.528(6) . ? C1 C3 1.534(6) . ? C1 C2 1.551(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.529(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.524(6) . ? C9 C11 1.527(6) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.529(6) . ? C12 C13 1.537(6) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.529(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.490(7) . ? C17 C19 1.527(7) . ? C17 H17A 1.0000 . ? C18 C17B 1.529(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18D 0.9799 . ? C18 H18E 0.9800 . ? C18 H18F 0.9799 . ? C19 C17B 1.470(10) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 H19D 0.9800 . ? C19 H19E 0.9799 . ? C19 H19F 0.9800 . ? C17B H17B 1.0000 . ? C20 C22 1.451(7) . ? C20 C21 1.585(7) . ? C20 H20A 1.0000 . ? C20 H22F 1.5528 . ? C21 C20B 1.449(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21 H21D 0.9801 . ? C21 H21E 0.9800 . ? C21 H21F 0.9798 . ? C22 C20B 1.434(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22 H22D 0.9799 . ? C22 H22E 0.9803 . ? C22 H22F 0.9799 . ? C20B H20B 1.0000 . ? 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 N1 Co1 P1 119.01(10) . . ? N1 Co1 P2 112.29(10) . . ? P1 Co1 P2 107.41(4) . . ? N1 Co1 I1 114.50(9) . . ? P1 Co1 I1 96.57(4) . . ? P2 Co1 I1 105.29(4) . . ? N1 Si1 N2 100.91(15) . . ? N1 Si1 C5 117.4(2) . . ? N2 Si1 C5 107.72(19) . . ? N1 Si1 C6 116.5(2) . . ? N2 Si1 C6 109.80(18) . . ? C5 Si1 C6 104.3(2) . . ? C8 P1 C9 105.6(2) . . ? C8 P1 C12 104.7(2) . . ? C9 P1 C12 107.1(2) . . ? C8 P1 Co1 105.96(14) . . ? C9 P1 Co1 117.94(15) . . ? C12 P1 Co1 114.39(14) . . ? C17B P2 C20 79.1(5) . . ? C17B P2 C16 108.7(3) . . ? C20 P2 C16 103.5(2) . . ? C17B P2 C17 24.8(4) . . ? C20 P2 C17 103.9(3) . . ? C16 P2 C17 101.0(2) . . ? C17B P2 C20B 101.9(5) . . ? C20 P2 C20B 24.5(3) . . ? C16 P2 C20B 104.4(3) . . ? C17 P2 C20B 126.6(4) . . ? C17B P2 Co1 123.1(4) . . ? C20 P2 Co1 134.0(2) . . ? C16 P2 Co1 105.06(13) . . ? C17 P2 Co1 105.1(2) . . ? C20B P2 Co1 112.3(3) . . ? C1 N1 Si1 125.2(3) . . ? C1 N1 Co1 127.4(2) . . ? Si1 N1 Co1 106.23(16) . . ? C15 N2 C7 111.3(3) . . ? C15 N2 Si1 116.7(3) . . ? C7 N2 Si1 120.8(3) . . ? N1 C1 C4 110.8(3) . . ? N1 C1 C3 110.2(3) . . ? C4 C1 C3 109.8(4) . . ? N1 C1 C2 111.5(3) . . ? C4 C1 C2 106.6(4) . . ? C3 C1 C2 107.8(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 113.6(3) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 P1 110.4(3) . . ? C7 C8 H8A 109.6 . . ? P1 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? P1 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C11 111.6(4) . . ? C10 C9 P1 109.3(3) . . ? C11 C9 P1 115.7(3) . . ? C10 C9 H9A 106.6 . . ? C11 C9 H9A 106.6 . . ? P1 C9 H9A 106.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 112.1(4) . . ? C14 C12 P1 118.0(3) . . ? C13 C12 P1 109.8(3) . . ? C14 C12 H12A 105.3 . . ? C13 C12 H12A 105.3 . . ? P1 C12 H12A 105.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 113.0(3) . . ? N2 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N2 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 P2 110.1(3) . . ? C15 C16 H16A 109.6 . . ? P2 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? P2 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? C18 C17 C19 114.2(5) . . ? C18 C17 P2 113.9(4) . . ? C19 C17 P2 107.0(4) . . ? C18 C17 H17A 107.1 . . ? C19 C17 H17A 107.1 . . ? P2 C17 H17A 107.1 . . ? C17 C18 C17B 31.3(5) . . ? C17 C18 H18A 109.5 . . ? C17B C18 H18A 121.3 . . ? C17 C18 H18B 109.5 . . ? C17B C18 H18B 78.2 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17B C18 H18C 122.7 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C18 H18D 119.6 . . ? C17B C18 H18D 109.9 . . ? H18A C18 H18D 36.7 . . ? H18B C18 H18D 73.0 . . ? H18C C18 H18D 126.9 . . ? C17 C18 H18E 124.2 . . ? C17B C18 H18E 108.8 . . ? H18A C18 H18E 125.9 . . ? H18B C18 H18E 60.6 . . ? H18C C18 H18E 48.8 . . ? H18D C18 H18E 109.5 . . ? C17 C18 H18F 78.5 . . ? C17B C18 H18F 109.7 . . ? H18A C18 H18F 72.9 . . ? H18B C18 H18F 169.6 . . ? H18C C18 H18F 60.7 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? C17B C19 C17 31.5(5) . . ? C17B C19 H19A 119.3 . . ? C17 C19 H19A 109.5 . . ? C17B C19 H19B 124.7 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17B C19 H19C 78.1 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17B C19 H19D 111.7 . . ? C17 C19 H19D 123.0 . . ? H19A C19 H19D 35.6 . . ? H19B C19 H19D 123.1 . . ? H19C C19 H19D 73.8 . . ? C17B C19 H19E 108.7 . . ? C17 C19 H19E 77.3 . . ? H19A C19 H19E 74.3 . . ? H19B C19 H19E 60.4 . . ? H19C C19 H19E 169.8 . . ? H19D C19 H19E 109.5 . . ? C17B C19 H19F 107.9 . . ? C17 C19 H19F 121.5 . . ? H19A C19 H19F 128.7 . . ? H19B C19 H19F 49.1 . . ? H19C C19 H19F 60.6 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? C19 C17B C18 115.3(8) . . ? C19 C17B P2 114.7(7) . . ? C18 C17B P2 117.2(7) . . ? C19 C17B H17B 102.1 . . ? C18 C17B H17B 102.1 . . ? P2 C17B H17B 102.1 . . ? C22 C20 C21 110.5(5) . . ? C22 C20 P2 120.3(5) . . ? C21 C20 P2 111.9(4) . . ? C22 C20 H20A 104.1 . . ? C21 C20 H20A 104.1 . . ? P2 C20 H20A 104.1 . . ? C22 C20 H22F 37.9 . . ? C21 C20 H22F 121.3 . . ? P2 C20 H22F 126.7 . . ? H20A C20 H22F 66.3 . . ? C20B C21 C20 31.1(4) . . ? C20B C21 H21A 123.1 . . ? C20 C21 H21A 109.5 . . ? C20B C21 H21B 120.7 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20B C21 H21C 78.4 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20B C21 H21D 107.6 . . ? C20 C21 H21D 116.6 . . ? H21A C21 H21D 39.8 . . ? H21B C21 H21D 130.9 . . ? H21C C21 H21D 70.4 . . ? C20B C21 H21E 109.5 . . ? C20 C21 H21E 78.6 . . ? H21A C21 H21E 69.7 . . ? H21B C21 H21E 63.6 . . ? H21C C21 H21E 171.3 . . ? H21D C21 H21E 109.5 . . ? C20B C21 H21F 111.3 . . ? C20 C21 H21F 127.1 . . ? H21A C21 H21F 122.6 . . ? H21B C21 H21F 46.3 . . ? H21C C21 H21F 63.2 . . ? H21D C21 H21F 109.5 . . ? H21E C21 H21F 109.5 . . ? C20B C22 C20 33.1(4) . . ? C20B C22 H22A 125.7 . . ? C20 C22 H22A 109.5 . . ? C20B C22 H22B 76.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20B C22 H22C 119.1 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20B C22 H22D 107.5 . . ? C20 C22 H22D 114.1 . . ? H22A C22 H22D 38.2 . . ? H22B C22 H22D 72.5 . . ? H22C C22 H22D 132.7 . . ? C20B C22 H22E 111.6 . . ? C20 C22 H22E 130.7 . . ? H22A C22 H22E 119.0 . . ? H22B C22 H22E 63.2 . . ? H22C C22 H22E 46.7 . . ? H22D C22 H22E 109.5 . . ? C20B C22 H22F 109.3 . . ? C20 C22 H22F 76.7 . . ? H22A C22 H22F 71.5 . . ? H22B C22 H22F 172.4 . . ? H22C C22 H22F 63.6 . . ? H22D C22 H22F 109.5 . . ? H22E C22 H22F 109.5 . . ? C22 C20B C21 119.9(7) . . ? C22 C20B P2 111.1(6) . . ? C21 C20B P2 109.3(5) . . ? C22 C20B H20B 105.1 . . ? C21 C20B H20B 105.1 . . ? P2 C20B H20B 105.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 P1 C8 33.98(19) . . . . ? P2 Co1 P1 C8 -94.95(15) . . . . ? I1 Co1 P1 C8 156.73(15) . . . . ? N1 Co1 P1 C9 -83.9(2) . . . . ? P2 Co1 P1 C9 147.16(17) . . . . ? I1 Co1 P1 C9 38.84(17) . . . . ? N1 Co1 P1 C12 148.84(19) . . . . ? P2 Co1 P1 C12 19.91(17) . . . . ? I1 Co1 P1 C12 -88.41(16) . . . . ? N1 Co1 P2 C17B 47.4(5) . . . . ? P1 Co1 P2 C17B -180.0(5) . . . . ? I1 Co1 P2 C17B -77.9(5) . . . . ? N1 Co1 P2 C20 155.9(3) . . . . ? P1 Co1 P2 C20 -71.4(3) . . . . ? I1 Co1 P2 C20 30.7(3) . . . . ? N1 Co1 P2 C16 -77.51(18) . . . . ? P1 Co1 P2 C16 55.16(15) . . . . ? I1 Co1 P2 C16 157.28(15) . . . . ? N1 Co1 P2 C17 28.6(2) . . . . ? P1 Co1 P2 C17 161.23(19) . . . . ? I1 Co1 P2 C17 -96.7(2) . . . . ? N1 Co1 P2 C20B 169.6(3) . . . . ? P1 Co1 P2 C20B -57.7(3) . . . . ? I1 Co1 P2 C20B 44.4(3) . . . . ? N2 Si1 N1 C1 -179.3(3) . . . . ? C5 Si1 N1 C1 64.1(4) . . . . ? C6 Si1 N1 C1 -60.5(4) . . . . ? N2 Si1 N1 Co1 -11.2(2) . . . . ? C5 Si1 N1 Co1 -127.9(2) . . . . ? C6 Si1 N1 Co1 107.5(2) . . . . ? P1 Co1 N1 C1 115.8(3) . . . . ? P2 Co1 N1 C1 -117.5(3) . . . . ? I1 Co1 N1 C1 2.5(3) . . . . ? P1 Co1 N1 Si1 -51.87(19) . . . . ? P2 Co1 N1 Si1 74.78(17) . . . . ? I1 Co1 N1 Si1 -165.22(11) . . . . ? N1 Si1 N2 C15 -99.0(3) . . . . ? C5 Si1 N2 C15 24.6(3) . . . . ? C6 Si1 N2 C15 137.5(3) . . . . ? N1 Si1 N2 C7 120.2(3) . . . . ? C5 Si1 N2 C7 -116.2(3) . . . . ? C6 Si1 N2 C7 -3.2(4) . . . . ? Si1 N1 C1 C4 -139.5(3) . . . . ? Co1 N1 C1 C4 55.0(5) . . . . ? Si1 N1 C1 C3 98.7(4) . . . . ? Co1 N1 C1 C3 -66.8(4) . . . . ? Si1 N1 C1 C2 -21.0(5) . . . . ? Co1 N1 C1 C2 173.5(3) . . . . ? C15 N2 C7 C8 150.8(3) . . . . ? Si1 N2 C7 C8 -66.5(4) . . . . ? N2 C7 C8 P1 -49.7(4) . . . . ? C9 P1 C8 C7 173.5(3) . . . . ? C12 P1 C8 C7 -73.7(3) . . . . ? Co1 P1 C8 C7 47.6(3) . . . . ? C8 P1 C9 C10 -68.7(3) . . . . ? C12 P1 C9 C10 -179.9(3) . . . . ? Co1 P1 C9 C10 49.4(3) . . . . ? C8 P1 C9 C11 58.2(4) . . . . ? C12 P1 C9 C11 -53.0(4) . . . . ? Co1 P1 C9 C11 176.3(3) . . . . ? C8 P1 C12 C14 -31.7(4) . . . . ? C9 P1 C12 C14 80.1(4) . . . . ? Co1 P1 C12 C14 -147.3(3) . . . . ? C8 P1 C12 C13 -161.9(3) . . . . ? C9 P1 C12 C13 -50.1(4) . . . . ? Co1 P1 C12 C13 82.5(3) . . . . ? C7 N2 C15 C16 -84.2(4) . . . . ? Si1 N2 C15 C16 131.5(3) . . . . ? N2 C15 C16 P2 -58.3(4) . . . . ? C17B P2 C16 C15 -90.8(6) . . . . ? C20 P2 C16 C15 -173.7(4) . . . . ? C17 P2 C16 C15 -66.3(4) . . . . ? C20B P2 C16 C15 161.1(4) . . . . ? Co1 P2 C16 C15 42.8(3) . . . . ? C17B P2 C17 C18 65.6(8) . . . . ? C20 P2 C17 C18 61.8(5) . . . . ? C16 P2 C17 C18 -45.3(5) . . . . ? C20B P2 C17 C18 72.0(6) . . . . ? Co1 P2 C17 C18 -154.3(4) . . . . ? C17B P2 C17 C19 -61.6(8) . . . . ? C20 P2 C17 C19 -65.4(5) . . . . ? C16 P2 C17 C19 -172.5(4) . . . . ? C20B P2 C17 C19 -55.2(6) . . . . ? Co1 P2 C17 C19 78.5(4) . . . . ? C19 C17 C18 C17B 61.2(8) . . . . ? P2 C17 C18 C17B -62.1(8) . . . . ? C18 C17 C19 C17B -65.0(9) . . . . ? P2 C17 C19 C17B 61.9(8) . . . . ? C17 C19 C17B C18 62.9(10) . . . . ? C17 C19 C17B P2 -77.8(11) . . . . ? C17 C18 C17B C19 -66.6(11) . . . . ? C17 C18 C17B P2 73.1(10) . . . . ? C20 P2 C17B C19 -109.8(9) . . . . ? C16 P2 C17B C19 149.5(8) . . . . ? C17 P2 C17B C19 74.0(11) . . . . ? C20B P2 C17B C19 -100.7(9) . . . . ? Co1 P2 C17B C19 26.2(12) . . . . ? C20 P2 C17B C18 110.2(9) . . . . ? C16 P2 C17B C18 9.5(11) . . . . ? C17 P2 C17B C18 -65.9(10) . . . . ? C20B P2 C17B C18 119.3(9) . . . . ? Co1 P2 C17B C18 -113.7(7) . . . . ? C17B P2 C20 C22 -132.8(7) . . . . ? C16 P2 C20 C22 -26.0(7) . . . . ? C17 P2 C20 C22 -131.1(6) . . . . ? C20B P2 C20 C22 69.2(8) . . . . ? Co1 P2 C20 C22 101.2(6) . . . . ? C17B P2 C20 C21 95.0(5) . . . . ? C16 P2 C20 C21 -158.2(4) . . . . ? C17 P2 C20 C21 96.7(5) . . . . ? C20B P2 C20 C21 -63.1(8) . . . . ? Co1 P2 C20 C21 -31.1(6) . . . . ? C22 C20 C21 C20B -58.1(8) . . . . ? P2 C20 C21 C20B 78.8(8) . . . . ? C21 C20 C22 C20B 54.0(8) . . . . ? P2 C20 C22 C20B -78.7(9) . . . . ? C20 C22 C20B C21 -73.0(10) . . . . ? C20 C22 C20B P2 56.0(7) . . . . ? C20 C21 C20B C22 68.0(10) . . . . ? C20 C21 C20B P2 -61.8(7) . . . . ? C17B P2 C20B C22 -83.0(8) . . . . ? C20 P2 C20B C22 -61.0(8) . . . . ? C16 P2 C20B C22 30.0(8) . . . . ? C17 P2 C20B C22 -85.8(7) . . . . ? Co1 P2 C20B C22 143.3(6) . . . . ? C17B P2 C20B C21 51.5(7) . . . . ? C20 P2 C20B C21 73.5(9) . . . . ? C16 P2 C20B C21 164.5(6) . . . . ? C17 P2 C20B C21 48.7(8) . . . . ? Co1 P2 C20B C21 -82.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.639 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.095 # Attachment 'wac6122xs.cif' data_wac6122xs _database_code_depnum_ccdc_archive 'CCDC 677812' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H57 Co N3 P2 Si' _chemical_formula_sum 'C28 H57 Co N3 P2 Si' _chemical_formula_weight 584.73 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 13.154(5) _cell_length_b 15.801(6) _cell_length_c 16.304(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.657(5) _cell_angle_gamma 90.00 _cell_volume 3307(2) _cell_formula_units_Z 4 _cell_measurement_temperature 151(2) _cell_measurement_reflns_used 1561 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 25.1 _exptl_crystal_description blade-like _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 151(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12224 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.1372 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 22.73 _reflns_number_total 4423 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Towards the end of the refinement process an unusually large peak was found in the difference Fourier map near P2. This was modeled as a fractional phosphorus with isotropic thermal parameters. The occupancy refined to 0.062(5). The nature of the disorder appears to be a rotation and off-set around the P2-C16 bond such that the methine carbon atoms of the isopropyl groups are shared between the two phosphorus positions. The distances between P2B and C20 and C17 are reasonable and were not constrained. The angles around C20 and C17 containing P2B are meaningless because the 6% disorder in the methyl carbons was not modeled. ; _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^)+(0.0400P)^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 4423 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 0.68765(5) 0.78477(4) 0.21427(4) 0.0309(2) Uani 1 1 d . . . Si1 Si 0.76034(11) 0.79120(10) 0.07076(8) 0.0337(4) Uani 1 1 d . D . P2 P 1.13023(12) 0.83877(12) 0.26437(10) 0.0464(7) Uani 0.938(5) 1 d P . . N1 N 0.6493(3) 0.7613(3) 0.0968(2) 0.0335(11) Uani 1 1 d . D . N2 N 0.8118(3) 0.8506(2) 0.1637(2) 0.0298(10) Uani 1 1 d . D . N3 N 0.7499(3) 0.7157(2) 0.3075(2) 0.0318(10) Uani 1 1 d . D . H3A H 0.8178 0.7089 0.3158 0.038 Uiso 1 1 calc R . . C1 C 0.5606(4) 0.7112(4) 0.0510(3) 0.0410(14) Uani 1 1 d . . . C2 C 0.4682(4) 0.7218(4) 0.0936(3) 0.0477(15) Uani 1 1 d . D . H2A H 0.4487 0.7817 0.0931 0.072 Uiso 1 1 calc R . . H2B H 0.4880 0.7018 0.1518 0.072 Uiso 1 1 calc R . . H2C H 0.4088 0.6887 0.0631 0.072 Uiso 1 1 calc R . . C3 C 0.5275(4) 0.7413(4) -0.0397(3) 0.0588(18) Uani 1 1 d . D . H3B H 0.5102 0.8016 -0.0406 0.088 Uiso 1 1 calc R . . H3C H 0.4663 0.7091 -0.0685 0.088 Uiso 1 1 calc R . . H3D H 0.5848 0.7323 -0.0684 0.088 Uiso 1 1 calc R . . C4 C 0.5890(5) 0.6168(4) 0.0533(4) 0.067(2) Uani 1 1 d . D . H4A H 0.6480 0.6084 0.0265 0.100 Uiso 1 1 calc R . . H4B H 0.5290 0.5842 0.0230 0.100 Uiso 1 1 calc R . . H4C H 0.6080 0.5976 0.1118 0.100 Uiso 1 1 calc R . . C5 C 0.8521(4) 0.7053(4) 0.0572(4) 0.0537(16) Uani 1 1 d . . . H5A H 0.8232 0.6737 0.0056 0.064 Uiso 1 1 calc R D . H5B H 0.8623 0.6669 0.1055 0.064 Uiso 1 1 calc R . . H5C H 0.9192 0.7300 0.0532 0.064 Uiso 1 1 calc R . . C6 C 0.7495(4) 0.8595(4) -0.0236(3) 0.0512(16) Uani 1 1 d . . . H6A H 0.7208 0.8265 -0.0742 0.061 Uiso 1 1 calc R D . H6B H 0.8187 0.8807 -0.0264 0.061 Uiso 1 1 calc R . . H6C H 0.7034 0.9074 -0.0199 0.061 Uiso 1 1 calc R . . C7 C 0.7877(4) 0.9420(3) 0.1597(3) 0.0325(13) Uani 1 1 d . . . H7A H 0.7301 0.9525 0.1104 0.039 Uiso 1 1 calc R D . H7B H 0.8495 0.9733 0.1505 0.039 Uiso 1 1 calc R . . C8 C 0.7568(4) 0.9775(3) 0.2380(3) 0.0334(13) Uani 1 1 d . D . H8A H 0.7386 1.0380 0.2290 0.040 Uiso 1 1 calc R A 1 H8B H 0.8168 0.9732 0.2865 0.040 Uiso 1 1 calc R A 1 C9 C 0.5275(4) 0.9769(3) 0.2056(3) 0.0353(13) Uani 1 1 d . . . H9A H 0.4663 0.9446 0.2163 0.042 Uiso 1 1 calc R B 1 C10 C 0.5169(4) 1.0674(4) 0.2356(3) 0.0501(16) Uani 1 1 d . D . H10A H 0.4522 1.0923 0.2033 0.075 Uiso 1 1 calc R . . H10B H 0.5764 1.1011 0.2272 0.075 Uiso 1 1 calc R . . H10C H 0.5154 1.0668 0.2954 0.075 Uiso 1 1 calc R . . C11 C 0.5195(4) 0.9749(3) 0.1105(3) 0.0441(15) Uani 1 1 d . D . H11A H 0.4563 1.0048 0.0820 0.066 Uiso 1 1 calc R . . H11B H 0.5164 0.9161 0.0912 0.066 Uiso 1 1 calc R . . H11C H 0.5807 1.0027 0.0975 0.066 Uiso 1 1 calc R . . C12 C 0.6534(4) 0.9443(3) 0.3737(3) 0.0381(14) Uani 1 1 d . . . H12A H 0.6571 1.0071 0.3814 0.046 Uiso 1 1 calc R C 1 C13 C 0.5566(5) 0.9115(4) 0.4015(3) 0.0587(18) Uani 1 1 d . D . H13A H 0.5618 0.9257 0.4608 0.088 Uiso 1 1 calc R . . H13B H 0.5520 0.8500 0.3943 0.088 Uiso 1 1 calc R . . H13C H 0.4942 0.9380 0.3673 0.088 Uiso 1 1 calc R . . C14 C 0.7513(4) 0.9047(4) 0.4294(3) 0.0535(17) Uani 1 1 d . D . H14A H 0.7539 0.9187 0.4884 0.080 Uiso 1 1 calc R . . H14B H 0.8135 0.9271 0.4131 0.080 Uiso 1 1 calc R . . H14C H 0.7489 0.8431 0.4224 0.080 Uiso 1 1 calc R . . C23 C 0.7026(4) 0.6754(3) 0.3629(3) 0.0330(13) Uani 1 1 d . . . C24 C 0.5935(4) 0.6697(3) 0.3477(3) 0.0406(14) Uani 1 1 d . D . H24A H 0.5530 0.6935 0.2976 0.049 Uiso 1 1 calc R . . C25 C 0.5440(5) 0.6312(4) 0.4026(4) 0.0504(16) Uani 1 1 d . . . H25A H 0.4701 0.6292 0.3901 0.060 Uiso 1 1 calc R D . C26 C 0.5988(5) 0.5948(4) 0.4761(4) 0.0502(16) Uani 1 1 d . D . H26A H 0.5638 0.5673 0.5138 0.060 Uiso 1 1 calc R . . C27 C 0.7054(5) 0.5999(3) 0.4927(3) 0.0456(15) Uani 1 1 d . . . H27A H 0.7449 0.5756 0.5430 0.055 Uiso 1 1 calc R D . C28 C 0.7563(4) 0.6392(3) 0.4385(3) 0.0370(14) Uani 1 1 d . D . H28A H 0.8302 0.6420 0.4525 0.044 Uiso 1 1 calc R . . P1 P 0.64594(10) 0.92032(9) 0.26180(8) 0.0315(4) Uani 1 1 d . D 1 C15 C 0.9163(4) 0.8315(3) 0.2170(3) 0.0352(13) Uani 1 1 d . D 1 H15A H 0.9230 0.7694 0.2238 0.042 Uiso 1 1 calc R D 1 H15B H 0.9200 0.8561 0.2734 0.042 Uiso 1 1 calc R D 1 C16 C 1.0096(4) 0.8641(4) 0.1840(3) 0.0412(15) Uani 1 1 d . D 1 H16A H 1.0037 0.9260 0.1746 0.049 Uiso 1 1 calc R D 1 H16B H 1.0117 0.8363 0.1299 0.049 Uiso 1 1 calc R D 1 C17 C 1.1837(5) 0.9459(4) 0.2918(4) 0.0630(19) Uani 1 1 d . D 1 H17A H 1.2485 0.9394 0.3368 0.076 Uiso 1 1 calc R D 1 C18 C 1.1072(5) 0.9987(5) 0.3281(4) 0.086(2) Uani 1 1 d . D 1 H18A H 1.1364 1.0552 0.3424 0.128 Uiso 1 1 calc R D 1 H18B H 1.0947 0.9712 0.3789 0.128 Uiso 1 1 calc R D 1 H18C H 1.0413 1.0036 0.2865 0.128 Uiso 1 1 calc R D 1 C19 C 1.2129(5) 0.9946(4) 0.2196(4) 0.076(2) Uani 1 1 d . D 1 H19A H 1.2412 1.0500 0.2398 0.114 Uiso 1 1 calc R D 1 H19B H 1.1507 1.0024 0.1745 0.114 Uiso 1 1 calc R D 1 H19C H 1.2654 0.9627 0.1981 0.114 Uiso 1 1 calc R D 1 C20 C 1.2180(4) 0.7933(4) 0.2030(4) 0.0571(17) Uani 1 1 d . D 1 H20A H 1.2276 0.8357 0.1598 0.068 Uiso 1 1 calc R D 1 C21 C 1.3225(4) 0.7773(5) 0.2610(4) 0.075(2) Uani 1 1 d . D 1 H21A H 1.3708 0.7545 0.2286 0.112 Uiso 1 1 calc R D 1 H21B H 1.3143 0.7365 0.3044 0.112 Uiso 1 1 calc R D 1 H21C H 1.3502 0.8305 0.2877 0.112 Uiso 1 1 calc R D 1 C22 C 1.1732(5) 0.7124(4) 0.1578(5) 0.085(2) Uani 1 1 d . D 1 H22A H 1.2211 0.6908 0.1243 0.127 Uiso 1 1 calc R D 1 H22B H 1.1055 0.7248 0.1206 0.127 Uiso 1 1 calc R D 1 H22C H 1.1642 0.6698 0.1993 0.127 Uiso 1 1 calc R D 1 P2B P 1.1486(19) 0.8841(17) 0.2115(18) 0.044(10) Uiso 0.062(5) 1 d P D 2 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 0.0333(4) 0.0303(4) 0.0260(4) 0.0012(4) 0.0000(3) -0.0001(3) Si1 0.0378(9) 0.0350(9) 0.0268(8) 0.0013(7) 0.0034(6) 0.0044(7) P2 0.0315(10) 0.0675(14) 0.0381(11) 0.0153(10) 0.0034(7) 0.0082(9) N1 0.036(3) 0.035(3) 0.025(2) -0.004(2) -0.0026(19) -0.001(2) N2 0.029(2) 0.030(3) 0.028(2) 0.005(2) 0.0011(18) 0.002(2) N3 0.028(2) 0.031(2) 0.034(3) 0.004(2) 0.0017(19) 0.002(2) C1 0.044(4) 0.040(4) 0.033(3) 0.000(3) -0.003(3) -0.005(3) C2 0.041(3) 0.057(4) 0.042(3) -0.004(3) 0.002(3) -0.022(3) C3 0.048(4) 0.088(5) 0.034(4) -0.009(3) -0.006(3) -0.012(3) C4 0.072(5) 0.039(4) 0.077(5) -0.015(4) -0.009(4) -0.007(3) C5 0.050(4) 0.054(4) 0.055(4) -0.013(3) 0.007(3) 0.002(3) C6 0.061(4) 0.060(4) 0.031(3) 0.006(3) 0.006(3) -0.001(3) C7 0.035(3) 0.027(3) 0.033(3) 0.004(3) 0.002(2) -0.001(2) C8 0.033(3) 0.031(3) 0.033(3) 0.002(3) -0.002(2) 0.002(2) C9 0.031(3) 0.032(3) 0.040(3) 0.004(3) 0.002(2) 0.005(2) C10 0.047(4) 0.047(4) 0.052(4) -0.003(3) 0.002(3) 0.010(3) C11 0.039(3) 0.048(4) 0.037(4) 0.007(3) -0.007(3) 0.012(3) C12 0.044(3) 0.039(4) 0.029(3) -0.004(3) 0.002(3) -0.002(3) C13 0.067(4) 0.077(5) 0.035(4) -0.005(3) 0.018(3) -0.003(4) C14 0.074(4) 0.052(4) 0.028(3) 0.003(3) -0.005(3) 0.001(3) C23 0.036(3) 0.027(3) 0.034(3) 0.000(3) 0.004(3) -0.002(3) C24 0.046(4) 0.043(4) 0.032(3) 0.007(3) 0.008(3) -0.003(3) C25 0.050(4) 0.049(4) 0.052(4) -0.007(3) 0.011(3) 0.000(3) C26 0.071(5) 0.043(4) 0.043(4) -0.003(3) 0.025(3) -0.006(3) C27 0.068(5) 0.037(4) 0.030(3) -0.003(3) 0.005(3) 0.002(3) C28 0.046(4) 0.034(3) 0.027(3) 0.001(3) 0.002(3) -0.003(3) P1 0.0319(8) 0.0314(9) 0.0282(8) -0.0006(7) 0.0002(6) 0.0011(6) C15 0.031(3) 0.033(3) 0.038(3) 0.002(3) 0.001(2) 0.007(3) C16 0.029(3) 0.051(4) 0.040(3) 0.001(3) 0.002(3) 0.000(3) C17 0.061(4) 0.078(5) 0.040(4) -0.016(4) -0.009(3) 0.003(4) C18 0.084(5) 0.108(6) 0.065(5) -0.031(5) 0.016(4) 0.012(5) C19 0.072(5) 0.058(5) 0.095(6) -0.019(4) 0.011(4) -0.006(4) C20 0.043(4) 0.058(4) 0.064(4) 0.006(4) -0.001(3) 0.009(3) C21 0.042(4) 0.106(6) 0.077(5) 0.018(4) 0.013(3) 0.032(4) C22 0.072(5) 0.051(5) 0.129(7) -0.020(5) 0.014(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.904(4) . ? Co1 N1 1.907(4) . ? Co1 N2 2.241(4) . ? Co1 P1 2.3823(17) . ? Co1 Si1 2.7165(18) . ? Si1 N1 1.676(4) . ? Si1 N2 1.784(4) . ? Si1 C6 1.859(5) . ? Si1 C5 1.862(5) . ? P2 P2B 1.19(3) . ? P2 C20 1.831(6) . ? P2 C17 1.851(7) . ? P2 C16 1.867(5) . ? N1 C1 1.471(6) . ? N2 C7 1.477(6) . ? N2 C15 1.487(6) . ? N3 C23 1.362(6) . ? N3 H3A 0.8800 . ? C1 C3 1.524(7) . ? C1 C2 1.535(7) . ? C1 C4 1.536(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3 H3D 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.529(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 P1 1.828(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.527(7) . ? C9 C11 1.531(6) . ? C9 P1 1.855(5) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.533(7) . ? C12 C14 1.537(7) . ? C12 P1 1.845(5) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C23 C28 1.401(7) . ? C23 C24 1.404(7) . ? C24 C25 1.360(7) . ? C24 H24A 0.9500 . ? C25 C26 1.380(7) . ? C25 H25A 0.9500 . ? C26 C27 1.372(7) . ? C26 H26A 0.9500 . ? C27 C28 1.369(7) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C15 C16 1.532(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.524(8) . ? C17 C18 1.524(8) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.510(7) . ? C20 C22 1.529(8) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 N3 Co1 N1 131.50(17) . . ? N3 Co1 N2 109.83(16) . . ? N1 Co1 N2 76.96(16) . . ? N3 Co1 P1 110.20(12) . . ? N1 Co1 P1 118.21(13) . . ? N2 Co1 P1 86.62(11) . . ? N3 Co1 Si1 122.54(13) . . ? N1 Co1 Si1 37.61(12) . . ? N2 Co1 Si1 40.79(10) . . ? P1 Co1 Si1 113.34(5) . . ? N1 Si1 N2 97.08(19) . . ? N1 Si1 C6 117.4(2) . . ? N2 Si1 C6 110.1(2) . . ? N1 Si1 C5 116.6(2) . . ? N2 Si1 C5 110.4(2) . . ? C6 Si1 C5 105.0(3) . . ? N1 Si1 Co1 43.99(13) . . ? N2 Si1 Co1 55.13(13) . . ? C6 Si1 Co1 139.20(19) . . ? C5 Si1 Co1 115.78(19) . . ? P2B P2 C20 65.6(12) . . ? P2B P2 C17 59.7(12) . . ? C20 P2 C17 103.8(3) . . ? P2B P2 C16 68.7(12) . . ? C20 P2 C16 104.0(3) . . ? C17 P2 C16 101.1(3) . . ? C1 N1 Si1 131.4(3) . . ? C1 N1 Co1 128.3(3) . . ? Si1 N1 Co1 98.40(19) . . ? C7 N2 C15 112.7(4) . . ? C7 N2 Si1 116.0(3) . . ? C15 N2 Si1 121.4(3) . . ? C7 N2 Co1 107.6(3) . . ? C15 N2 Co1 110.3(3) . . ? Si1 N2 Co1 84.08(16) . . ? C23 N3 Co1 128.2(3) . . ? C23 N3 H3A 115.9 . . ? Co1 N3 H3A 115.9 . . ? N1 C1 C3 110.5(4) . . ? N1 C1 C2 109.3(4) . . ? C3 C1 C2 108.6(4) . . ? N1 C1 C4 110.4(4) . . ? C3 C1 C4 110.0(5) . . ? C2 C1 C4 107.9(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 114.5(4) . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 P1 111.5(3) . . ? C7 C8 H8A 109.3 . . ? P1 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? P1 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C11 110.6(4) . . ? C10 C9 P1 114.7(3) . . ? C11 C9 P1 110.7(3) . . ? C10 C9 H9A 106.8 . . ? C11 C9 H9A 106.8 . . ? P1 C9 H9A 106.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 109.3(5) . . ? C13 C12 P1 110.9(3) . . ? C14 C12 P1 111.0(4) . . ? C13 C12 H12A 108.6 . . ? C14 C12 H12A 108.6 . . ? P1 C12 H12A 108.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C23 C28 124.0(5) . . ? N3 C23 C24 120.7(4) . . ? C28 C23 C24 115.3(5) . . ? C25 C24 C23 122.0(5) . . ? C25 C24 H24A 119.0 . . ? C23 C24 H24A 119.0 . . ? C24 C25 C26 121.6(6) . . ? C24 C25 H25A 119.2 . . ? C26 C25 H25A 119.2 . . ? C27 C26 C25 117.6(5) . . ? C27 C26 H26A 121.2 . . ? C25 C26 H26A 121.2 . . ? C28 C27 C26 121.5(5) . . ? C28 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? C27 C28 C23 122.0(5) . . ? C27 C28 H28A 119.0 . . ? C23 C28 H28A 119.0 . . ? C8 P1 C12 103.7(2) . . ? C8 P1 C9 106.3(2) . . ? C12 P1 C9 104.3(2) . . ? C8 P1 Co1 97.11(16) . . ? C12 P1 Co1 122.70(18) . . ? C9 P1 Co1 120.06(17) . . ? N2 C15 C16 115.8(4) . . ? N2 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? N2 C15 H15B 108.3 . . ? C16 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C15 C16 P2 107.7(3) . . ? C15 C16 H16A 110.2 . . ? P2 C16 H16A 110.2 . . ? C15 C16 H16B 110.2 . . ? P2 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? C19 C17 C18 108.9(6) . . ? C19 C17 P2 114.9(4) . . ? C18 C17 P2 110.2(5) . . ? C19 C17 H17A 107.5 . . ? C18 C17 H17A 107.5 . . ? P2 C17 H17A 107.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 111.4(5) . . ? C21 C20 P2 108.7(4) . . ? C22 C20 P2 111.7(4) . . ? C21 C20 H20A 108.3 . . ? C22 C20 H20A 108.3 . . ? P2 C20 H20A 108.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.73 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.457 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.065 # Attachment 'wac6163xs.cif' data_wac6163xs _database_code_depnum_ccdc_archive 'CCDC 677813' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H62 Co N4 P2 Si' _chemical_formula_sum 'C34 H62 Co N4 P2 Si' _chemical_formula_weight 675.84 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 11.044(3) _cell_length_b 14.324(4) _cell_length_c 23.454(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.105(4) _cell_angle_gamma 90.00 _cell_volume 3704.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 167(2) _cell_measurement_reflns_used 3181 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 24.2 _exptl_crystal_description plate-like _exptl_crystal_colour 'bright green' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 167(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20702 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.39 _reflns_number_total 7547 _reflns_number_gt 5520 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.631' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0600P)^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 7547 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.004 _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 0.20374(3) 0.30588(2) 0.089562(13) 0.01904(10) Uani 1 1 d . . . Si4 Si -0.02970(6) 0.25971(5) 0.16266(3) 0.02232(17) Uani 1 1 d . . . P1 P 0.39076(6) 0.31119(4) 0.14861(3) 0.02263(16) Uani 1 1 d . . . P2 P 0.17440(6) 0.22513(4) -0.03791(3) 0.02034(15) Uani 1 1 d . . . N1 N -0.1011(2) 0.31473(14) 0.21749(9) 0.0254(5) Uani 1 1 d . . . H1A H -0.1425 0.2772 0.2389 0.031 Uiso 1 1 calc R . . N2 N 0.12146(18) 0.28186(14) 0.15957(8) 0.0208(4) Uani 1 1 d . . . N3 N 0.21227(18) 0.20246(13) 0.02830(8) 0.0199(4) Uani 1 1 d . . . N4 N 0.16991(19) 0.42033(13) 0.04428(8) 0.0207(4) Uani 1 1 d . . . C1 C -0.1040(2) 0.41374(17) 0.23420(11) 0.0257(6) Uani 1 1 d . . . C2 C 0.0160(3) 0.44297(19) 0.26481(12) 0.0337(7) Uani 1 1 d . . . H2A H 0.0822 0.4344 0.2391 0.051 Uiso 1 1 calc R . . H2B H 0.0310 0.4044 0.2990 0.051 Uiso 1 1 calc R . . H2C H 0.0116 0.5088 0.2759 0.051 Uiso 1 1 calc R . . C3 C -0.2067(3) 0.4273(2) 0.27458(13) 0.0397(7) Uani 1 1 d . . . H3A H -0.2838 0.4087 0.2552 0.060 Uiso 1 1 calc R . . H3B H -0.2108 0.4931 0.2857 0.060 Uiso 1 1 calc R . . H3C H -0.1913 0.3888 0.3087 0.060 Uiso 1 1 calc R . . C4 C -0.1281(3) 0.47433(18) 0.18151(12) 0.0342(7) Uani 1 1 d . . . H4A H -0.2049 0.4556 0.1619 0.051 Uiso 1 1 calc R . . H4B H -0.0620 0.4665 0.1557 0.051 Uiso 1 1 calc R . . H4C H -0.1329 0.5399 0.1930 0.051 Uiso 1 1 calc R . . C5 C -0.0640(3) 0.13378(19) 0.17666(14) 0.0430(8) Uani 1 1 d . . . H5A H -0.0264 0.1155 0.2138 0.064 Uiso 1 1 calc R . . H5B H -0.0315 0.0951 0.1466 0.064 Uiso 1 1 calc R . . H5C H -0.1520 0.1250 0.1769 0.064 Uiso 1 1 calc R . . C6 C -0.1025(3) 0.2921(2) 0.09190(11) 0.0351(7) Uani 1 1 d . . . H6A H -0.0856 0.3578 0.0839 0.053 Uiso 1 1 calc R . . H6B H -0.1903 0.2827 0.0925 0.053 Uiso 1 1 calc R . . H6C H -0.0698 0.2528 0.0622 0.053 Uiso 1 1 calc R . . C7 C 0.1988(2) 0.26200(18) 0.21140(10) 0.0243(5) Uani 1 1 d . . . H7A H 0.2243 0.1957 0.2111 0.029 Uiso 1 1 calc R . . H7B H 0.1516 0.2721 0.2455 0.029 Uiso 1 1 calc R . . C8 C 0.3118(2) 0.32476(18) 0.21504(10) 0.0275(6) Uani 1 1 d . . . H8A H 0.3660 0.3064 0.2482 0.033 Uiso 1 1 calc R . . H8B H 0.2878 0.3907 0.2200 0.033 Uiso 1 1 calc R . . C9 C 0.4819(2) 0.20366(17) 0.16264(11) 0.0268(6) Uani 1 1 d . . . H9A H 0.4228 0.1526 0.1697 0.032 Uiso 1 1 calc R . . C10 C 0.5686(3) 0.2082(2) 0.21561(13) 0.0392(7) Uani 1 1 d . . . H10A H 0.6128 0.1491 0.2199 0.059 Uiso 1 1 calc R . . H10B H 0.5222 0.2191 0.2494 0.059 Uiso 1 1 calc R . . H10C H 0.6263 0.2594 0.2115 0.059 Uiso 1 1 calc R . . C11 C 0.5488(3) 0.1747(2) 0.11065(13) 0.0396(7) Uani 1 1 d . . . H11A H 0.5958 0.1180 0.1194 0.059 Uiso 1 1 calc R . . H11B H 0.6036 0.2250 0.1002 0.059 Uiso 1 1 calc R . . H11C H 0.4901 0.1625 0.0787 0.059 Uiso 1 1 calc R . . C12 C 0.5097(2) 0.40306(18) 0.14483(11) 0.0298(6) Uani 1 1 d . . . H12A H 0.5889 0.3729 0.1563 0.036 Uiso 1 1 calc R . . C13 C 0.4935(3) 0.4848(2) 0.18567(14) 0.0454(8) Uani 1 1 d . . . H13A H 0.5588 0.5302 0.1815 0.068 Uiso 1 1 calc R . . H13B H 0.4963 0.4617 0.2251 0.068 Uiso 1 1 calc R . . H13C H 0.4151 0.5149 0.1767 0.068 Uiso 1 1 calc R . . C14 C 0.5185(3) 0.4367(2) 0.08370(14) 0.0503(9) Uani 1 1 d . . . H14A H 0.5813 0.4849 0.0824 0.075 Uiso 1 1 calc R . . H14B H 0.4403 0.4627 0.0698 0.075 Uiso 1 1 calc R . . H14C H 0.5396 0.3840 0.0594 0.075 Uiso 1 1 calc R . . C15 C 0.1516(2) 0.42034(16) -0.01763(10) 0.0255(6) Uani 1 1 d . . . H15A H 0.2312 0.4264 -0.0348 0.031 Uiso 1 1 calc R . . H15B H 0.1019 0.4752 -0.0296 0.031 Uiso 1 1 calc R . . C16 C 0.0888(2) 0.33168(16) -0.04031(10) 0.0239(6) Uani 1 1 d . . . H16A H 0.0609 0.3431 -0.0805 0.029 Uiso 1 1 calc R . . H16B H 0.0156 0.3218 -0.0185 0.029 Uiso 1 1 calc R . . C17 C 0.0770(2) 0.13237(17) -0.06822(10) 0.0254(6) Uani 1 1 d . . . H17A H 0.1261 0.0737 -0.0670 0.030 Uiso 1 1 calc R . . C18 C -0.0300(3) 0.11642(19) -0.03028(11) 0.0324(6) Uani 1 1 d . . . H18A H -0.0819 0.0667 -0.0467 0.049 Uiso 1 1 calc R . . H18B H -0.0771 0.1742 -0.0280 0.049 Uiso 1 1 calc R . . H18C H 0.0007 0.0983 0.0081 0.049 Uiso 1 1 calc R . . C19 C 0.0325(3) 0.1476(2) -0.13067(11) 0.0343(7) Uani 1 1 d . . . H19A H -0.0188 0.0950 -0.1435 0.051 Uiso 1 1 calc R . . H19B H 0.1024 0.1519 -0.1546 0.051 Uiso 1 1 calc R . . H19C H -0.0144 0.2056 -0.1338 0.051 Uiso 1 1 calc R . . C20 C 0.3037(2) 0.23809(18) -0.08389(10) 0.0268(6) Uani 1 1 d . . . H20A H 0.3224 0.1746 -0.0988 0.032 Uiso 1 1 calc R . . C21 C 0.4172(3) 0.2718(2) -0.04905(12) 0.0368(7) Uani 1 1 d . . . H21A H 0.4846 0.2782 -0.0743 0.055 Uiso 1 1 calc R . . H21B H 0.4388 0.2263 -0.0190 0.055 Uiso 1 1 calc R . . H21C H 0.4006 0.3323 -0.0317 0.055 Uiso 1 1 calc R . . C22 C 0.2788(3) 0.30203(18) -0.13607(11) 0.0353(7) Uani 1 1 d . . . H22A H 0.3514 0.3053 -0.1582 0.053 Uiso 1 1 calc R . . H22B H 0.2579 0.3648 -0.1231 0.053 Uiso 1 1 calc R . . H22C H 0.2112 0.2767 -0.1601 0.053 Uiso 1 1 calc R . . C23 C 0.2540(2) 0.11222(16) 0.04527(10) 0.0217(5) Uani 1 1 d . . . C24 C 0.2308(2) 0.08202(17) 0.10024(10) 0.0231(6) Uani 1 1 d . . . H24A H 0.1853 0.1206 0.1241 0.028 Uiso 1 1 calc R . . C25 C 0.2734(2) -0.00370(17) 0.12054(11) 0.0287(6) Uani 1 1 d . . . H25A H 0.2582 -0.0224 0.1584 0.034 Uiso 1 1 calc R . . C26 C 0.3378(2) -0.06224(17) 0.08613(12) 0.0308(6) Uani 1 1 d . . . H26A H 0.3670 -0.1207 0.1001 0.037 Uiso 1 1 calc R . . C27 C 0.3587(2) -0.03427(18) 0.03147(11) 0.0299(6) Uani 1 1 d . . . H27A H 0.4013 -0.0744 0.0073 0.036 Uiso 1 1 calc R . . C28 C 0.3183(2) 0.05165(17) 0.01105(11) 0.0259(6) Uani 1 1 d . . . H28A H 0.3345 0.0698 -0.0267 0.031 Uiso 1 1 calc R . . C29 C 0.1921(2) 0.50715(17) 0.06760(10) 0.0224(5) Uani 1 1 d . . . C30 C 0.2275(2) 0.58673(16) 0.03697(11) 0.0248(6) Uani 1 1 d . . . H30A H 0.2365 0.5819 -0.0030 0.030 Uiso 1 1 calc R . . C31 C 0.2493(2) 0.67142(17) 0.06392(12) 0.0299(6) Uani 1 1 d . . . H31A H 0.2738 0.7234 0.0421 0.036 Uiso 1 1 calc R . . C32 C 0.2362(3) 0.68222(17) 0.12186(12) 0.0327(7) Uani 1 1 d . . . H32A H 0.2515 0.7406 0.1400 0.039 Uiso 1 1 calc R . . C33 C 0.1999(3) 0.60532(19) 0.15272(12) 0.0337(7) Uani 1 1 d . . . H33A H 0.1901 0.6114 0.1925 0.040 Uiso 1 1 calc R . . C34 C 0.1780(2) 0.52082(17) 0.12682(11) 0.0271(6) Uani 1 1 d . . . H34A H 0.1526 0.4698 0.1492 0.033 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 0.01965(19) 0.01805(18) 0.01930(18) 0.00124(13) -0.00002(13) -0.00072(13) Si4 0.0209(4) 0.0224(4) 0.0238(4) 0.0004(3) 0.0026(3) -0.0033(3) P1 0.0189(3) 0.0241(3) 0.0245(3) 0.0000(3) -0.0024(3) -0.0020(3) P2 0.0205(3) 0.0195(3) 0.0208(3) -0.0007(3) -0.0017(3) 0.0009(3) N1 0.0262(12) 0.0249(11) 0.0257(11) 0.0029(9) 0.0053(10) -0.0039(9) N2 0.0183(11) 0.0247(11) 0.0194(10) 0.0013(9) -0.0001(8) -0.0006(9) N3 0.0199(11) 0.0193(10) 0.0202(10) -0.0011(8) -0.0013(8) 0.0015(8) N4 0.0256(11) 0.0171(10) 0.0191(10) 0.0020(8) -0.0012(9) 0.0015(9) C1 0.0231(14) 0.0272(14) 0.0269(13) -0.0017(11) 0.0017(11) -0.0001(11) C2 0.0305(15) 0.0353(16) 0.0351(15) -0.0043(12) -0.0021(13) 0.0008(13) C3 0.0371(17) 0.0397(17) 0.0434(17) -0.0054(14) 0.0128(14) 0.0017(14) C4 0.0344(16) 0.0262(14) 0.0412(17) 0.0020(12) -0.0044(13) 0.0009(12) C5 0.0410(18) 0.0273(15) 0.062(2) -0.0015(14) 0.0164(16) -0.0085(13) C6 0.0250(15) 0.0530(19) 0.0271(14) -0.0010(13) -0.0010(12) -0.0028(13) C7 0.0246(14) 0.0275(13) 0.0204(12) 0.0028(11) -0.0012(10) -0.0005(11) C8 0.0284(15) 0.0316(15) 0.0219(13) -0.0014(11) -0.0034(11) -0.0013(12) C9 0.0197(13) 0.0238(13) 0.0363(15) -0.0006(11) -0.0044(11) -0.0003(11) C10 0.0380(17) 0.0324(16) 0.0452(18) 0.0004(13) -0.0154(14) 0.0029(13) C11 0.0276(16) 0.0459(18) 0.0451(17) -0.0071(14) 0.0000(14) 0.0044(13) C12 0.0209(14) 0.0282(14) 0.0397(16) 0.0010(12) -0.0036(12) -0.0034(11) C13 0.0323(17) 0.0329(17) 0.071(2) -0.0138(15) 0.0021(16) -0.0091(14) C14 0.0426(19) 0.054(2) 0.055(2) 0.0141(16) 0.0025(16) -0.0178(16) C15 0.0296(15) 0.0196(12) 0.0272(13) 0.0017(11) 0.0002(11) 0.0019(11) C16 0.0267(14) 0.0228(13) 0.0217(12) 0.0005(10) -0.0037(11) 0.0053(11) C17 0.0229(14) 0.0222(13) 0.0305(14) -0.0051(11) -0.0047(11) 0.0025(11) C18 0.0342(16) 0.0277(14) 0.0350(15) 0.0003(12) -0.0024(13) -0.0090(12) C19 0.0324(16) 0.0424(17) 0.0276(14) -0.0124(13) -0.0034(12) -0.0038(13) C20 0.0283(15) 0.0272(14) 0.0251(13) 0.0000(11) 0.0033(11) 0.0027(11) C21 0.0259(15) 0.0416(16) 0.0432(17) 0.0056(14) 0.0039(13) -0.0017(13) C22 0.0484(19) 0.0323(15) 0.0256(14) 0.0027(12) 0.0048(13) -0.0003(14) C23 0.0183(13) 0.0183(12) 0.0277(13) -0.0013(10) -0.0056(11) -0.0005(10) C24 0.0213(13) 0.0233(13) 0.0241(13) -0.0037(10) -0.0046(11) -0.0026(10) C25 0.0307(15) 0.0242(14) 0.0299(14) 0.0049(11) -0.0096(12) -0.0050(11) C26 0.0289(15) 0.0171(13) 0.0452(17) 0.0031(12) -0.0086(13) -0.0003(11) C27 0.0269(15) 0.0232(13) 0.0392(16) -0.0037(12) -0.0024(12) 0.0033(11) C28 0.0257(14) 0.0251(13) 0.0267(14) -0.0003(11) -0.0004(11) -0.0016(11) C29 0.0176(13) 0.0228(13) 0.0268(13) 0.0022(11) -0.0006(10) 0.0024(10) C30 0.0254(14) 0.0209(13) 0.0276(13) 0.0040(11) -0.0018(11) 0.0021(11) C31 0.0240(14) 0.0195(13) 0.0458(17) 0.0038(12) -0.0023(13) -0.0002(11) C32 0.0324(16) 0.0201(13) 0.0447(17) -0.0075(12) -0.0048(13) 0.0003(12) C33 0.0400(17) 0.0331(15) 0.0277(14) -0.0059(12) -0.0016(13) 0.0031(13) C34 0.0313(15) 0.0215(13) 0.0285(14) 0.0009(11) 0.0016(12) -0.0023(11) _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 N2 1.950(2) . ? Co1 N4 1.9779(19) . ? Co1 N3 2.0694(19) . ? Co1 P1 2.4248(8) . ? Si4 N2 1.705(2) . ? Si4 N1 1.734(2) . ? Si4 C6 1.863(3) . ? Si4 C5 1.876(3) . ? P1 C8 1.836(3) . ? P1 C9 1.860(3) . ? P1 C12 1.864(3) . ? P2 N3 1.619(2) . ? P2 C16 1.795(2) . ? P2 C17 1.829(2) . ? P2 C20 1.845(3) . ? N1 C1 1.472(3) . ? N1 H1A 0.8800 . ? N2 C7 1.475(3) . ? N3 C23 1.422(3) . ? N4 C29 1.375(3) . ? N4 C15 1.455(3) . ? C1 C4 1.522(4) . ? C1 C3 1.529(4) . ? C1 C2 1.531(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.536(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.517(4) . ? C9 C10 1.528(4) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.521(4) . ? C12 C13 1.529(4) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.529(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.534(4) . ? C17 C19 1.535(3) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.536(4) . ? C20 C22 1.541(3) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.397(3) . ? C23 C28 1.401(3) . ? C24 C25 1.389(3) . ? C24 H24A 0.9500 . ? C25 C26 1.387(4) . ? C25 H25A 0.9500 . ? C26 C27 1.375(4) . ? C26 H26A 0.9500 . ? C27 C28 1.385(3) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.414(3) . ? C29 C34 1.420(4) . ? C30 C31 1.383(3) . ? C30 H30A 0.9500 . ? C31 C32 1.383(4) . ? C31 H31A 0.9500 . ? C32 C33 1.389(4) . ? C32 H32A 0.9500 . ? C33 C34 1.370(3) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N4 121.02(9) . . ? N2 Co1 N3 119.95(8) . . ? N4 Co1 N3 103.59(8) . . ? N2 Co1 P1 86.90(6) . . ? N4 Co1 P1 114.26(6) . . ? N3 Co1 P1 110.47(6) . . ? N2 Si4 N1 115.63(10) . . ? N2 Si4 C6 106.98(12) . . ? N1 Si4 C6 110.85(12) . . ? N2 Si4 C5 113.19(12) . . ? N1 Si4 C5 101.71(12) . . ? C6 Si4 C5 108.31(14) . . ? C8 P1 C9 102.41(12) . . ? C8 P1 C12 109.49(12) . . ? C9 P1 C12 102.53(12) . . ? C8 P1 Co1 93.39(9) . . ? C9 P1 Co1 120.75(8) . . ? C12 P1 Co1 125.12(9) . . ? N3 P2 C16 108.00(11) . . ? N3 P2 C17 110.06(11) . . ? C16 P2 C17 107.91(12) . . ? N3 P2 C20 114.39(11) . . ? C16 P2 C20 108.63(12) . . ? C17 P2 C20 107.68(12) . . ? C1 N1 Si4 130.75(17) . . ? C1 N1 H1A 114.6 . . ? Si4 N1 H1A 114.6 . . ? C7 N2 Si4 117.01(16) . . ? C7 N2 Co1 116.89(16) . . ? Si4 N2 Co1 124.80(11) . . ? C23 N3 P2 120.92(16) . . ? C23 N3 Co1 118.86(15) . . ? P2 N3 Co1 120.21(11) . . ? C29 N4 C15 114.13(19) . . ? C29 N4 Co1 120.78(15) . . ? C15 N4 Co1 123.22(15) . . ? N1 C1 C4 109.8(2) . . ? N1 C1 C3 108.4(2) . . ? C4 C1 C3 109.1(2) . . ? N1 C1 C2 110.9(2) . . ? C4 C1 C2 109.5(2) . . ? C3 C1 C2 109.1(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si4 C5 H5A 109.5 . . ? Si4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si4 C6 H6A 109.5 . . ? Si4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 111.4(2) . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 P1 108.20(17) . . ? C7 C8 H8A 110.1 . . ? P1 C8 H8A 110.1 . . ? C7 C8 H8B 110.1 . . ? P1 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C11 C9 C10 110.8(2) . . ? C11 C9 P1 111.50(19) . . ? C10 C9 P1 114.68(18) . . ? C11 C9 H9A 106.4 . . ? C10 C9 H9A 106.4 . . ? P1 C9 H9A 106.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 111.3(3) . . ? C14 C12 P1 110.46(19) . . ? C13 C12 P1 113.8(2) . . ? C14 C12 H12A 106.9 . . ? C13 C12 H12A 106.9 . . ? P1 C12 H12A 106.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 C16 112.5(2) . . ? N4 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N4 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 P2 117.84(18) . . ? C15 C16 H16A 107.8 . . ? P2 C16 H16A 107.8 . . ? C15 C16 H16B 107.8 . . ? P2 C16 H16B 107.8 . . ? H16A C16 H16B 107.2 . . ? C18 C17 C19 111.0(2) . . ? C18 C17 P2 109.76(17) . . ? C19 C17 P2 114.74(18) . . ? C18 C17 H17A 107.0 . . ? C19 C17 H17A 107.0 . . ? P2 C17 H17A 107.0 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 109.9(2) . . ? C21 C20 P2 110.84(18) . . ? C22 C20 P2 114.42(19) . . ? C21 C20 H20A 107.1 . . ? C22 C20 H20A 107.1 . . ? P2 C20 H20A 107.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 117.5(2) . . ? C24 C23 N3 117.8(2) . . ? C28 C23 N3 124.7(2) . . ? C25 C24 C23 121.0(2) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C26 C25 C24 120.6(2) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C27 C26 C25 118.9(2) . . ? C27 C26 H26A 120.5 . . ? C25 C26 H26A 120.5 . . ? C26 C27 C28 121.0(3) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? C27 C28 C23 121.0(2) . . ? C27 C28 H28A 119.5 . . ? C23 C28 H28A 119.5 . . ? N4 C29 C30 125.1(2) . . ? N4 C29 C34 119.2(2) . . ? C30 C29 C34 115.7(2) . . ? C31 C30 C29 121.4(2) . . ? C31 C30 H30A 119.3 . . ? C29 C30 H30A 119.3 . . ? C30 C31 C32 121.5(2) . . ? C30 C31 H31A 119.3 . . ? C32 C31 H31A 119.3 . . ? C31 C32 C33 118.2(2) . . ? C31 C32 H32A 120.9 . . ? C33 C32 H32A 120.9 . . ? C34 C33 C32 121.2(3) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C33 C34 C29 122.0(2) . . ? C33 C34 H34A 119.0 . . ? C29 C34 H34A 119.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Co1 P1 C8 -16.26(10) . . . . ? N4 Co1 P1 C8 106.53(11) . . . . ? N3 Co1 P1 C8 -137.16(10) . . . . ? N2 Co1 P1 C9 90.34(12) . . . . ? N4 Co1 P1 C9 -146.86(12) . . . . ? N3 Co1 P1 C9 -30.55(12) . . . . ? N2 Co1 P1 C12 -133.02(13) . . . . ? N4 Co1 P1 C12 -10.22(13) . . . . ? N3 Co1 P1 C12 106.09(13) . . . . ? N2 Si4 N1 C1 52.6(2) . . . . ? C6 Si4 N1 C1 -69.3(2) . . . . ? C5 Si4 N1 C1 175.7(2) . . . . ? N1 Si4 N2 C7 55.6(2) . . . . ? C6 Si4 N2 C7 179.63(18) . . . . ? C5 Si4 N2 C7 -61.2(2) . . . . ? N1 Si4 N2 Co1 -137.85(12) . . . . ? C6 Si4 N2 Co1 -13.85(17) . . . . ? C5 Si4 N2 Co1 105.37(16) . . . . ? N4 Co1 N2 C7 -126.38(16) . . . . ? N3 Co1 N2 C7 102.11(17) . . . . ? P1 Co1 N2 C7 -9.78(16) . . . . ? N4 Co1 N2 Si4 67.09(16) . . . . ? N3 Co1 N2 Si4 -64.42(15) . . . . ? P1 Co1 N2 Si4 -176.32(13) . . . . ? C16 P2 N3 C23 164.27(18) . . . . ? C17 P2 N3 C23 46.7(2) . . . . ? C20 P2 N3 C23 -74.7(2) . . . . ? C16 P2 N3 Co1 -16.96(16) . . . . ? C17 P2 N3 Co1 -134.53(13) . . . . ? C20 P2 N3 Co1 104.11(14) . . . . ? N2 Co1 N3 C23 -50.9(2) . . . . ? N4 Co1 N3 C23 170.38(17) . . . . ? P1 Co1 N3 C23 47.59(18) . . . . ? N2 Co1 N3 P2 130.26(12) . . . . ? N4 Co1 N3 P2 -8.42(15) . . . . ? P1 Co1 N3 P2 -131.20(11) . . . . ? N2 Co1 N4 C29 60.9(2) . . . . ? N3 Co1 N4 C29 -160.97(18) . . . . ? P1 Co1 N4 C29 -40.7(2) . . . . ? N2 Co1 N4 C15 -135.58(19) . . . . ? N3 Co1 N4 C15 2.5(2) . . . . ? P1 Co1 N4 C15 122.78(18) . . . . ? Si4 N1 C1 C4 45.7(3) . . . . ? Si4 N1 C1 C3 164.8(2) . . . . ? Si4 N1 C1 C2 -75.4(3) . . . . ? Si4 N2 C7 C8 -152.38(18) . . . . ? Co1 N2 C7 C8 40.0(3) . . . . ? N2 C7 C8 P1 -54.6(2) . . . . ? C9 P1 C8 C7 -83.10(19) . . . . ? C12 P1 C8 C7 168.63(17) . . . . ? Co1 P1 C8 C7 39.42(17) . . . . ? C8 P1 C9 C11 175.76(19) . . . . ? C12 P1 C9 C11 -70.7(2) . . . . ? Co1 P1 C9 C11 74.1(2) . . . . ? C8 P1 C9 C10 -57.3(2) . . . . ? C12 P1 C9 C10 56.2(2) . . . . ? Co1 P1 C9 C10 -158.95(17) . . . . ? C8 P1 C12 C14 -143.2(2) . . . . ? C9 P1 C12 C14 108.6(2) . . . . ? Co1 P1 C12 C14 -34.2(3) . . . . ? C8 P1 C12 C13 -17.1(2) . . . . ? C9 P1 C12 C13 -125.3(2) . . . . ? Co1 P1 C12 C13 91.9(2) . . . . ? C29 N4 C15 C16 -161.8(2) . . . . ? Co1 N4 C15 C16 33.7(3) . . . . ? N4 C15 C16 P2 -71.8(3) . . . . ? N3 P2 C16 C15 61.6(2) . . . . ? C17 P2 C16 C15 -179.47(19) . . . . ? C20 P2 C16 C15 -63.0(2) . . . . ? N3 P2 C17 C18 52.8(2) . . . . ? C16 P2 C17 C18 -64.9(2) . . . . ? C20 P2 C17 C18 178.04(17) . . . . ? N3 P2 C17 C19 178.53(18) . . . . ? C16 P2 C17 C19 60.9(2) . . . . ? C20 P2 C17 C19 -56.2(2) . . . . ? N3 P2 C20 C21 -27.5(2) . . . . ? C16 P2 C20 C21 93.2(2) . . . . ? C17 P2 C20 C21 -150.20(19) . . . . ? N3 P2 C20 C22 -152.52(18) . . . . ? C16 P2 C20 C22 -31.8(2) . . . . ? C17 P2 C20 C22 84.8(2) . . . . ? P2 N3 C23 C24 -149.97(19) . . . . ? Co1 N3 C23 C24 31.2(3) . . . . ? P2 N3 C23 C28 30.9(3) . . . . ? Co1 N3 C23 C28 -147.9(2) . . . . ? C28 C23 C24 C25 1.9(3) . . . . ? N3 C23 C24 C25 -177.3(2) . . . . ? C23 C24 C25 C26 -1.4(4) . . . . ? C24 C25 C26 C27 -0.2(4) . . . . ? C25 C26 C27 C28 1.2(4) . . . . ? C26 C27 C28 C23 -0.7(4) . . . . ? C24 C23 C28 C27 -0.9(4) . . . . ? N3 C23 C28 C27 178.2(2) . . . . ? C15 N4 C29 C30 -16.7(3) . . . . ? Co1 N4 C29 C30 148.2(2) . . . . ? C15 N4 C29 C34 162.6(2) . . . . ? Co1 N4 C29 C34 -32.5(3) . . . . ? N4 C29 C30 C31 -179.3(2) . . . . ? C34 C29 C30 C31 1.4(4) . . . . ? C29 C30 C31 C32 -0.7(4) . . . . ? C30 C31 C32 C33 -0.2(4) . . . . ? C31 C32 C33 C34 0.2(4) . . . . ? C32 C33 C34 C29 0.6(4) . . . . ? N4 C29 C34 C33 179.3(2) . . . . ? C30 C29 C34 C33 -1.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.410 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.067 # Attachment 'wac6167cxs.cif' data_wac6167cxs _database_code_depnum_ccdc_archive 'CCDC 677814' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H51 Co N2 P2 Si' _chemical_formula_sum 'C22 H51 Co N2 P2 Si' _chemical_formula_weight 492.61 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.742(4) _cell_length_b 17.148(5) _cell_length_c 11.265(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2847.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 244(2) _cell_measurement_reflns_used 3150 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 25.3 _exptl_crystal_description 'hexangonal rods' _exptl_crystal_colour blue _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 244(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 'SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14951 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 26.53 _reflns_number_total 2931 _reflns_number_gt 1747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054d' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2931 _refine_ls_number_parameters 141 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 0.16502(4) 0.2500 0.61148(6) 0.0533(3) Uani 1 2 d S . . P1 P 0.11834(7) 0.35248(5) 0.71398(10) 0.0696(3) Uani 1 1 d . . . Si1 Si 0.10410(12) 0.2500 0.38802(15) 0.1034(8) Uani 1 2 d S . . N1 N 0.2069(3) 0.2500 0.4503(4) 0.0748(13) Uani 1 2 d S . . N2 N 0.0341(3) 0.2500 0.5165(4) 0.0735(12) Uani 1 2 d S . . C1 C 0.2975(4) 0.2500 0.4008(5) 0.101(2) Uani 1 2 d S . . C2 C 0.3655(5) 0.2500 0.4907(7) 0.133(3) Uani 1 2 d SD . . H2A H 0.4298(10) 0.2500 0.478(6) 0.180 Uiso 1 2 d SD . . H2B H 0.350(3) 0.285(3) 0.554(4) 0.180 Uiso 1 1 d D . . C3 C 0.3103(5) 0.3200(7) 0.3242(9) 0.337(9) Uani 1 1 d . . . H3A H 0.3713 0.3199 0.2918 0.505 Uiso 1 1 calc R . . H3B H 0.3014 0.3668 0.3711 0.505 Uiso 1 1 calc R . . H3C H 0.2667 0.3189 0.2598 0.505 Uiso 1 1 calc R . . C4 C 0.0749(4) 0.3359(5) 0.2908(5) 0.176(3) Uani 1 1 d . . . H4A H 0.0543 0.3174 0.2140 0.264 Uiso 1 1 calc R . . H4B H 0.1282 0.3684 0.2804 0.264 Uiso 1 1 calc R . . H4C H 0.0271 0.3662 0.3280 0.264 Uiso 1 1 calc R . . C5 C -0.0161(3) 0.3226(3) 0.5489(5) 0.0951(15) Uani 1 1 d . . . H5A H -0.0810 0.3131 0.5374 0.114 Uiso 1 1 calc R . . H5B H 0.0018 0.3639 0.4935 0.114 Uiso 1 1 calc R . . C6 C -0.0020(3) 0.3518(3) 0.6727(5) 0.0929(14) Uani 1 1 d . . . H6A H -0.0355 0.3186 0.7282 0.112 Uiso 1 1 calc R . . H6B H -0.0263 0.4048 0.6792 0.112 Uiso 1 1 calc R . . C7 C 0.1619(4) 0.4509(3) 0.6768(6) 0.1153(19) Uani 1 1 d . . . H7A H 0.1382 0.4859 0.7395 0.138 Uiso 1 1 calc R . . C8 C 0.2631(4) 0.4535(3) 0.6890(7) 0.153(2) Uani 1 1 d . . . H8A H 0.2846 0.5057 0.6710 0.230 Uiso 1 1 calc R . . H8B H 0.2903 0.4166 0.6344 0.230 Uiso 1 1 calc R . . H8C H 0.2799 0.4400 0.7697 0.230 Uiso 1 1 calc R . . C9 C 0.1317(6) 0.4826(5) 0.5699(10) 0.280(7) Uani 1 1 d . . . H9A H 0.1571 0.5344 0.5600 0.420 Uiso 1 1 calc R . . H9B H 0.0660 0.4860 0.5708 0.420 Uiso 1 1 calc R . . H9C H 0.1509 0.4496 0.5047 0.420 Uiso 1 1 calc R . . C10 C 0.1081(4) 0.3579(3) 0.8817(5) 0.1062(18) Uani 1 1 d . . . H10A H 0.0761 0.3097 0.9060 0.127 Uiso 1 1 calc R . . C11 C 0.0525(5) 0.4241(4) 0.9289(6) 0.154(3) Uani 1 1 d . . . H11A H 0.0507 0.4214 1.0149 0.231 Uiso 1 1 calc R . . H11B H -0.0087 0.4206 0.8978 0.231 Uiso 1 1 calc R . . H11C H 0.0794 0.4732 0.9046 0.231 Uiso 1 1 calc R . . C12 C 0.2013(5) 0.3539(4) 0.9399(6) 0.149(2) Uani 1 1 d . . . H12A H 0.1946 0.3562 1.0255 0.223 Uiso 1 1 calc R . . H12B H 0.2378 0.3976 0.9133 0.223 Uiso 1 1 calc R . . H12C H 0.2309 0.3055 0.9179 0.223 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 0.0415(4) 0.0647(4) 0.0537(4) 0.000 0.0019(3) 0.000 P1 0.0598(6) 0.0591(6) 0.0900(8) -0.0056(5) 0.0114(5) 0.0008(5) Si1 0.0567(10) 0.200(2) 0.0538(10) 0.000 -0.0071(7) 0.000 N1 0.049(2) 0.123(4) 0.053(3) 0.000 0.002(2) 0.000 N2 0.040(2) 0.105(3) 0.075(3) 0.000 -0.002(2) 0.000 C1 0.055(3) 0.190(8) 0.058(4) 0.000 0.014(3) 0.000 C2 0.048(3) 0.232(11) 0.120(7) 0.000 0.012(4) 0.000 C3 0.094(5) 0.56(2) 0.356(13) 0.339(15) 0.089(7) 0.051(8) C4 0.083(4) 0.338(10) 0.107(4) 0.101(6) 0.000(3) 0.025(5) C5 0.051(2) 0.122(4) 0.112(4) 0.032(3) -0.004(2) 0.015(2) C6 0.067(3) 0.088(3) 0.124(4) -0.003(3) 0.013(3) 0.014(2) C7 0.105(4) 0.065(3) 0.176(6) 0.017(3) 0.020(4) 0.004(3) C8 0.114(5) 0.108(4) 0.238(7) 0.026(5) 0.005(5) -0.046(4) C9 0.172(8) 0.222(10) 0.445(15) 0.237(11) -0.106(10) -0.071(7) C10 0.125(5) 0.090(3) 0.103(4) -0.024(3) 0.039(3) -0.010(3) C11 0.183(7) 0.125(5) 0.154(6) -0.054(4) 0.063(5) 0.004(5) C12 0.160(6) 0.182(7) 0.104(4) -0.024(4) -0.021(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.917(4) . ? Co1 N2 2.207(4) . ? Co1 P1 2.2124(11) 7_565 ? Co1 P1 2.2124(11) . ? Co1 Si1 2.6726(19) . ? P1 C6 1.833(5) . ? P1 C7 1.854(5) . ? P1 C10 1.897(5) . ? Si1 N1 1.669(5) . ? Si1 N2 1.777(5) . ? Si1 C4 1.886(6) 7_565 ? Si1 C4 1.886(6) . ? N1 C1 1.448(7) . ? N2 C5 1.492(5) . ? N2 C5 1.492(5) 7_565 ? C1 C2 1.424(9) . ? C1 C3 1.491(8) . ? C1 C3 1.491(8) 7_565 ? C2 H2A 0.959(5) . ? C2 H2B 0.960(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.497(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C9 1.393(10) . ? C7 C8 1.499(7) . ? C7 H7A 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.498(7) . ? C10 C12 1.524(9) . ? C10 H10A 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 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 N1 Co1 N2 79.76(18) . . ? N1 Co1 P1 126.46(4) . 7_565 ? N2 Co1 P1 88.91(8) . 7_565 ? N1 Co1 P1 126.46(4) . . ? N2 Co1 P1 88.91(8) . . ? P1 Co1 P1 105.17(6) 7_565 . ? N1 Co1 Si1 38.40(14) . . ? N2 Co1 Si1 41.36(12) . . ? P1 Co1 Si1 112.77(4) 7_565 . ? P1 Co1 Si1 112.77(4) . . ? C6 P1 C7 106.4(2) . . ? C6 P1 C10 100.1(3) . . ? C7 P1 C10 102.0(3) . . ? C6 P1 Co1 99.42(16) . . ? C7 P1 Co1 119.8(2) . . ? C10 P1 Co1 125.67(17) . . ? N1 Si1 N2 100.7(2) . . ? N1 Si1 C4 116.8(2) . 7_565 ? N2 Si1 C4 109.9(2) . 7_565 ? N1 Si1 C4 116.8(2) . . ? N2 Si1 C4 109.9(2) . . ? C4 Si1 C4 102.8(5) 7_565 . ? N1 Si1 Co1 45.51(15) . . ? N2 Si1 Co1 55.14(14) . . ? C4 Si1 Co1 128.6(2) 7_565 . ? C4 Si1 Co1 128.6(2) . . ? C1 N1 Si1 132.5(4) . . ? C1 N1 Co1 131.4(4) . . ? Si1 N1 Co1 96.1(2) . . ? C5 N2 C5 113.0(4) . 7_565 ? C5 N2 Si1 119.1(3) . . ? C5 N2 Si1 119.1(3) 7_565 . ? C5 N2 Co1 108.3(3) . . ? C5 N2 Co1 108.3(3) 7_565 . ? Si1 N2 Co1 83.49(16) . . ? C2 C1 N1 112.1(5) . . ? C2 C1 C3 108.8(6) . . ? N1 C1 C3 109.9(4) . . ? C2 C1 C3 108.8(6) . 7_565 ? N1 C1 C3 109.9(4) . 7_565 ? C3 C1 C3 107.3(11) . 7_565 ? C1 C2 H2A 126(4) . . ? C1 C2 H2B 111(3) . . ? H2A C2 H2B 109.6(12) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 116.0(4) . . ? N2 C5 H5A 108.3 . . ? C6 C5 H5A 108.3 . . ? N2 C5 H5B 108.3 . . ? C6 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 P1 111.9(3) . . ? C5 C6 H6A 109.2 . . ? P1 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? P1 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C9 C7 C8 112.7(6) . . ? C9 C7 P1 116.1(5) . . ? C8 C7 P1 110.5(4) . . ? C9 C7 H7A 105.5 . . ? C8 C7 H7A 105.5 . . ? P1 C7 H7A 105.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 112.0(5) . . ? C11 C10 P1 115.7(5) . . ? C12 C10 P1 110.7(4) . . ? C11 C10 H10A 105.9 . . ? C12 C10 H10A 105.9 . . ? P1 C10 H10A 105.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 P1 C6 88.1(2) . . . . ? N2 Co1 P1 C6 11.7(2) . . . . ? P1 Co1 P1 C6 -76.87(18) 7_565 . . . ? Si1 Co1 P1 C6 46.41(18) . . . . ? N1 Co1 P1 C7 -27.1(3) . . . . ? N2 Co1 P1 C7 -103.5(2) . . . . ? P1 Co1 P1 C7 167.9(2) 7_565 . . . ? Si1 Co1 P1 C7 -68.8(2) . . . . ? N1 Co1 P1 C10 -162.1(3) . . . . ? N2 Co1 P1 C10 121.5(3) . . . . ? P1 Co1 P1 C10 32.9(2) 7_565 . . . ? Si1 Co1 P1 C10 156.2(2) . . . . ? N2 Co1 Si1 N1 180.0 . . . . ? P1 Co1 Si1 N1 -120.52(4) 7_565 . . . ? P1 Co1 Si1 N1 120.52(4) . . . . ? N1 Co1 Si1 N2 180.0 . . . . ? P1 Co1 Si1 N2 59.48(4) 7_565 . . . ? P1 Co1 Si1 N2 -59.48(4) . . . . ? N1 Co1 Si1 C4 91.5(3) . . . 7_565 ? N2 Co1 Si1 C4 -88.5(3) . . . 7_565 ? P1 Co1 Si1 C4 -29.1(3) 7_565 . . 7_565 ? P1 Co1 Si1 C4 -148.0(3) . . . 7_565 ? N1 Co1 Si1 C4 -91.5(3) . . . . ? N2 Co1 Si1 C4 88.5(3) . . . . ? P1 Co1 Si1 C4 148.0(3) 7_565 . . . ? P1 Co1 Si1 C4 29.1(3) . . . . ? N2 Si1 N1 C1 180.0 . . . . ? C4 Si1 N1 C1 61.1(3) 7_565 . . . ? C4 Si1 N1 C1 -61.1(3) . . . . ? Co1 Si1 N1 C1 180.0 . . . . ? N2 Si1 N1 Co1 0.0 . . . . ? C4 Si1 N1 Co1 -118.9(3) 7_565 . . . ? C4 Si1 N1 Co1 118.9(3) . . . . ? N2 Co1 N1 C1 180.0 . . . . ? P1 Co1 N1 C1 -99.06(10) 7_565 . . . ? P1 Co1 N1 C1 99.06(10) . . . . ? Si1 Co1 N1 C1 180.0 . . . . ? N2 Co1 N1 Si1 0.0 . . . . ? P1 Co1 N1 Si1 80.94(10) 7_565 . . . ? P1 Co1 N1 Si1 -80.94(10) . . . . ? N1 Si1 N2 C5 107.4(3) . . . . ? C4 Si1 N2 C5 -128.8(4) 7_565 . . . ? C4 Si1 N2 C5 -16.4(4) . . . . ? Co1 Si1 N2 C5 107.4(3) . . . . ? N1 Si1 N2 C5 -107.4(3) . . . 7_565 ? C4 Si1 N2 C5 16.4(4) 7_565 . . 7_565 ? C4 Si1 N2 C5 128.8(4) . . . 7_565 ? Co1 Si1 N2 C5 -107.4(3) . . . 7_565 ? N1 Si1 N2 Co1 0.0 . . . . ? C4 Si1 N2 Co1 123.8(3) 7_565 . . . ? C4 Si1 N2 Co1 -123.8(3) . . . . ? N1 Co1 N2 C5 -118.6(3) . . . . ? P1 Co1 N2 C5 114.0(3) 7_565 . . . ? P1 Co1 N2 C5 8.8(3) . . . . ? Si1 Co1 N2 C5 -118.6(3) . . . . ? N1 Co1 N2 C5 118.6(3) . . . 7_565 ? P1 Co1 N2 C5 -8.8(3) 7_565 . . 7_565 ? P1 Co1 N2 C5 -114.0(3) . . . 7_565 ? Si1 Co1 N2 C5 118.6(3) . . . 7_565 ? N1 Co1 N2 Si1 0.0 . . . . ? P1 Co1 N2 Si1 -127.40(3) 7_565 . . . ? P1 Co1 N2 Si1 127.40(3) . . . . ? Si1 N1 C1 C2 180.0 . . . . ? Co1 N1 C1 C2 0.0 . . . . ? Si1 N1 C1 C3 58.9(6) . . . . ? Co1 N1 C1 C3 -121.1(6) . . . . ? Si1 N1 C1 C3 -58.9(6) . . . 7_565 ? Co1 N1 C1 C3 121.1(6) . . . 7_565 ? C5 N2 C5 C6 86.5(5) 7_565 . . . ? Si1 N2 C5 C6 -126.3(4) . . . . ? Co1 N2 C5 C6 -33.5(4) . . . . ? N2 C5 C6 P1 46.4(5) . . . . ? C7 P1 C6 C5 92.4(4) . . . . ? C10 P1 C6 C5 -161.7(3) . . . . ? Co1 P1 C6 C5 -32.7(4) . . . . ? C6 P1 C7 C9 -41.0(7) . . . . ? C10 P1 C7 C9 -145.5(7) . . . . ? Co1 P1 C7 C9 70.5(7) . . . . ? C6 P1 C7 C8 -171.0(5) . . . . ? C10 P1 C7 C8 84.5(6) . . . . ? Co1 P1 C7 C8 -59.5(6) . . . . ? C6 P1 C10 C11 -54.8(5) . . . . ? C7 P1 C10 C11 54.5(5) . . . . ? Co1 P1 C10 C11 -164.3(4) . . . . ? C6 P1 C10 C12 176.4(4) . . . . ? C7 P1 C10 C12 -74.3(4) . . . . ? Co1 P1 C10 C12 66.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.53 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.408 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.056 # Attachment 'wac6204xs.cif' data_wac6204xs _database_code_depnum_ccdc_archive 'CCDC 677815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H51 Co N2 O3 P2 Si' _chemical_formula_sum 'C25 H51 Co N2 O3 P2 Si' _chemical_formula_weight 576.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.3023(11) _cell_length_b 12.2795(17) _cell_length_c 15.354(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.718(2) _cell_angle_gamma 90.00 _cell_volume 1562.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 2011 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 23.5 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8958 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5638 _reflns_number_gt 4739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.631' _computing_cell_refinement 'Bruker SAINT v7.07' _computing_data_reduction 'Bruker SAINT v7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0400P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(14) _refine_ls_number_reflns 5638 _refine_ls_number_parameters 307 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 0.28384(5) 0.94732(4) 0.74695(3) 0.02037(12) Uani 1 1 d . . . Si1 Si 0.35427(11) 1.08745(8) 0.59406(6) 0.0217(2) Uani 1 1 d . . . P1 P 0.50245(11) 0.90280(7) 0.83247(6) 0.0214(2) Uani 1 1 d . . . P2 P 0.20666(13) 1.33618(8) 0.84022(7) 0.0297(2) Uani 1 1 d . . . N1 N 0.1487(3) 1.0576(2) 0.59391(18) 0.0226(6) Uani 1 1 d . . . N2 N 0.4222(3) 1.0810(2) 0.70753(17) 0.0202(6) Uani 1 1 d . . . O1 O -0.0382(3) 0.9774(2) 0.67689(16) 0.0337(7) Uani 1 1 d . . . O2 O 0.0572(3) 0.9479(3) 0.88290(16) 0.0432(7) Uani 1 1 d . . . O3 O 0.2651(4) 0.7463(3) 0.64898(19) 0.0498(8) Uani 1 1 d . . . C1 C 0.0209(4) 1.0823(3) 0.5218(2) 0.0276(8) Uani 1 1 d . . . C2 C 0.0988(5) 1.1356(4) 0.4445(2) 0.0435(11) Uani 1 1 d . . . H2A H 0.1780 1.0856 0.4219 0.065 Uiso 1 1 calc R . . H2B H 0.1529 1.2031 0.4639 0.065 Uiso 1 1 calc R . . H2C H 0.0152 1.1521 0.3984 0.065 Uiso 1 1 calc R . . C3 C -0.1022(5) 1.1629(3) 0.5547(2) 0.0335(9) Uani 1 1 d . . . H3A H -0.1546 1.1308 0.6040 0.050 Uiso 1 1 calc R . . H3B H -0.1838 1.1793 0.5075 0.050 Uiso 1 1 calc R . . H3C H -0.0470 1.2302 0.5736 0.050 Uiso 1 1 calc R . . C4 C -0.0585(5) 0.9766(3) 0.4890(3) 0.0449(12) Uani 1 1 d . . . H4A H 0.0242 0.9272 0.4691 0.067 Uiso 1 1 calc R . . H4B H -0.1372 0.9926 0.4403 0.067 Uiso 1 1 calc R . . H4C H -0.1135 0.9421 0.5364 0.067 Uiso 1 1 calc R . . C5 C 0.4629(5) 0.9861(3) 0.5289(2) 0.0339(9) Uani 1 1 d . . . H5A H 0.4372 0.9123 0.5481 0.051 Uiso 1 1 calc R . . H5B H 0.5795 0.9983 0.5375 0.051 Uiso 1 1 calc R . . H5C H 0.4291 0.9944 0.4669 0.051 Uiso 1 1 calc R . . C6 C 0.4087(5) 1.2256(3) 0.5536(2) 0.0332(9) Uani 1 1 d . . . H6A H 0.3540 1.2814 0.5865 0.050 Uiso 1 1 calc R . . H6B H 0.3747 1.2318 0.4915 0.050 Uiso 1 1 calc R . . H6C H 0.5258 1.2358 0.5617 0.050 Uiso 1 1 calc R . . C7 C 0.5989(4) 1.0550(3) 0.7181(2) 0.0257(8) Uani 1 1 d . . . H7A H 0.6618 1.1218 0.7082 0.031 Uiso 1 1 calc R . . H7B H 0.6254 1.0009 0.6734 0.031 Uiso 1 1 calc R . . C8 C 0.6477(4) 1.0101(3) 0.8080(2) 0.0259(8) Uani 1 1 d . . . H8A H 0.6464 1.0687 0.8522 0.031 Uiso 1 1 calc R . . H8B H 0.7582 0.9795 0.8090 0.031 Uiso 1 1 calc R . . C9 C 0.6057(4) 0.7715(3) 0.8122(2) 0.0281(8) Uani 1 1 d . . . H9A H 0.5225 0.7128 0.8143 0.034 Uiso 1 1 calc R . . C10 C 0.6696(5) 0.7687(4) 0.7206(3) 0.0399(10) Uani 1 1 d . . . H10A H 0.7233 0.6989 0.7118 0.060 Uiso 1 1 calc R . . H10B H 0.7468 0.8282 0.7149 0.060 Uiso 1 1 calc R . . H10C H 0.5794 0.7773 0.6767 0.060 Uiso 1 1 calc R . . C11 C 0.7425(5) 0.7424(4) 0.8805(3) 0.0401(10) Uani 1 1 d . . . H11A H 0.7906 0.6727 0.8651 0.060 Uiso 1 1 calc R . . H11B H 0.6990 0.7366 0.9381 0.060 Uiso 1 1 calc R . . H11C H 0.8252 0.7995 0.8817 0.060 Uiso 1 1 calc R . . C12 C 0.4967(4) 0.9065(3) 0.9529(2) 0.0282(8) Uani 1 1 d . . . H12A H 0.6095 0.8954 0.9782 0.034 Uiso 1 1 calc R . . C13 C 0.4376(5) 1.0163(4) 0.9865(3) 0.0379(10) Uani 1 1 d . . . H13A H 0.4370 1.0139 1.0503 0.057 Uiso 1 1 calc R . . H13B H 0.3282 1.0306 0.9614 0.057 Uiso 1 1 calc R . . H13C H 0.5101 1.0743 0.9694 0.057 Uiso 1 1 calc R . . C14 C 0.3940(5) 0.8131(3) 0.9849(3) 0.0367(10) Uani 1 1 d . . . H14A H 0.3923 0.8165 1.0486 0.055 Uiso 1 1 calc R . . H14B H 0.4402 0.7434 0.9679 0.055 Uiso 1 1 calc R . . H14C H 0.2836 0.8196 0.9586 0.055 Uiso 1 1 calc R . . C15 C 0.3938(4) 1.1824(3) 0.7602(2) 0.0232(8) Uani 1 1 d . . . H15A H 0.4675 1.2397 0.7412 0.028 Uiso 1 1 calc R . . H15B H 0.4254 1.1662 0.8221 0.028 Uiso 1 1 calc R . . C16 C 0.2237(4) 1.2292(3) 0.7556(2) 0.0271(8) Uani 1 1 d . . . H16A H 0.1451 1.1703 0.7648 0.033 Uiso 1 1 calc R . . H16B H 0.1979 1.2608 0.6970 0.033 Uiso 1 1 calc R . . C17 C 0.2115(5) 1.4640(4) 0.7760(2) 0.0378(10) Uani 1 1 d . . . H17A H 0.1285 1.4591 0.7259 0.045 Uiso 1 1 calc R . . C18 C 0.1708(6) 1.5614(4) 0.8330(3) 0.0532(13) Uani 1 1 d . . . H18A H 0.1724 1.6283 0.7984 0.080 Uiso 1 1 calc R . . H18B H 0.2508 1.5667 0.8827 0.080 Uiso 1 1 calc R . . H18C H 0.0632 1.5513 0.8545 0.080 Uiso 1 1 calc R . . C19 C 0.3776(6) 1.4795(3) 0.7398(3) 0.0472(12) Uani 1 1 d . . . H19A H 0.3783 1.5471 0.7060 0.071 Uiso 1 1 calc R . . H19B H 0.4007 1.4178 0.7021 0.071 Uiso 1 1 calc R . . H19C H 0.4602 1.4834 0.7883 0.071 Uiso 1 1 calc R . . C20 C -0.0106(5) 1.3240(4) 0.8626(3) 0.0438(11) Uani 1 1 d . . . H20A H -0.0329 1.3829 0.9051 0.053 Uiso 1 1 calc R . . C21 C -0.1310(6) 1.3385(5) 0.7854(3) 0.0663(16) Uani 1 1 d . . . H21A H -0.2407 1.3304 0.8046 0.099 Uiso 1 1 calc R . . H21B H -0.1120 1.2833 0.7412 0.099 Uiso 1 1 calc R . . H21C H -0.1186 1.4112 0.7604 0.099 Uiso 1 1 calc R . . C22 C -0.0363(6) 1.2159(4) 0.9091(3) 0.0571(13) Uani 1 1 d . . . H22A H -0.1503 1.2086 0.9211 0.086 Uiso 1 1 calc R . . H22B H 0.0303 1.2142 0.9641 0.086 Uiso 1 1 calc R . . H22C H -0.0054 1.1556 0.8718 0.086 Uiso 1 1 calc R . . C23 C 0.1029(4) 0.9982(3) 0.6665(2) 0.0246(8) Uani 1 1 d . . . C24 C 0.1525(4) 0.9553(4) 0.8326(2) 0.0283(8) Uani 1 1 d . . . C25 C 0.2799(5) 0.8284(3) 0.6852(2) 0.0312(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0184(2) 0.0203(2) 0.0224(2) 0.0030(2) 0.00100(16) -0.0027(2) Si1 0.0196(5) 0.0215(5) 0.0244(5) 0.0028(4) 0.0048(4) -0.0003(4) P1 0.0205(5) 0.0201(5) 0.0234(4) 0.0017(3) 0.0003(4) 0.0003(4) P2 0.0295(6) 0.0288(6) 0.0303(5) -0.0074(4) -0.0009(4) 0.0026(4) N1 0.0202(16) 0.0270(18) 0.0205(14) 0.0047(11) -0.0003(12) 0.0017(12) N2 0.0159(15) 0.0204(16) 0.0245(14) 0.0029(12) 0.0023(11) -0.0007(12) O1 0.0202(14) 0.045(2) 0.0356(15) 0.0137(12) -0.0002(11) -0.0054(11) O2 0.0276(14) 0.064(2) 0.0386(14) 0.0101(17) 0.0090(11) 0.0025(17) O3 0.065(2) 0.0298(19) 0.0523(19) -0.0110(15) -0.0134(16) -0.0004(15) C1 0.025(2) 0.036(2) 0.0216(18) 0.0059(16) 0.0018(15) 0.0036(17) C2 0.034(2) 0.070(3) 0.027(2) 0.014(2) 0.0026(18) 0.005(2) C3 0.031(2) 0.040(3) 0.029(2) 0.0104(17) 0.0052(17) 0.0097(18) C4 0.043(3) 0.047(3) 0.043(2) -0.0060(19) -0.0140(19) -0.0003(19) C5 0.033(2) 0.034(2) 0.035(2) -0.0037(16) 0.0090(17) 0.0075(17) C6 0.039(2) 0.032(2) 0.029(2) 0.0102(17) 0.0061(17) -0.0024(18) C7 0.0209(19) 0.025(2) 0.0311(19) 0.0021(15) 0.0028(15) -0.0029(15) C8 0.0180(19) 0.026(2) 0.033(2) -0.0014(16) 0.0004(15) -0.0010(15) C9 0.026(2) 0.021(2) 0.037(2) 0.0020(16) 0.0079(16) -0.0005(16) C10 0.040(3) 0.034(3) 0.047(3) -0.0088(19) 0.010(2) 0.0083(19) C11 0.029(2) 0.036(3) 0.056(3) 0.011(2) 0.0022(19) 0.0107(19) C12 0.029(2) 0.032(2) 0.0231(17) 0.0054(15) -0.0041(15) -0.0007(16) C13 0.042(3) 0.043(3) 0.029(2) -0.0094(18) 0.0036(18) -0.005(2) C14 0.039(3) 0.041(3) 0.030(2) 0.0138(18) 0.0041(18) -0.0026(19) C15 0.0195(19) 0.022(2) 0.0274(18) -0.0013(14) 0.0011(14) 0.0020(15) C16 0.0223(19) 0.024(2) 0.035(2) -0.0048(16) 0.0027(15) -0.0033(16) C17 0.045(2) 0.030(3) 0.037(2) 0.0005(18) -0.0084(18) 0.0043(19) C18 0.063(3) 0.029(3) 0.068(3) -0.010(2) 0.008(3) 0.007(2) C19 0.059(3) 0.027(3) 0.055(3) 0.0032(18) 0.002(2) -0.0049(19) C20 0.034(2) 0.049(3) 0.049(3) -0.021(2) 0.009(2) 0.000(2) C21 0.032(3) 0.090(4) 0.077(4) -0.018(3) 0.001(3) 0.008(3) C22 0.044(3) 0.060(4) 0.071(3) -0.017(3) 0.027(2) -0.010(2) C23 0.0223(19) 0.024(2) 0.0276(19) -0.0005(15) 0.0011(15) -0.0041(15) C24 0.0217(17) 0.033(2) 0.0299(18) 0.0094(18) -0.0024(14) -0.0016(18) C25 0.032(2) 0.030(2) 0.031(2) 0.0080(18) -0.0047(16) -0.0011(17) _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 C25 1.740(4) . ? Co1 C24 1.765(4) . ? Co1 C23 1.983(4) . ? Co1 N2 2.114(3) . ? Co1 P1 2.2379(10) . ? Si1 N1 1.746(3) . ? Si1 N2 1.798(3) . ? Si1 C5 1.866(4) . ? Si1 C6 1.872(4) . ? P1 C8 1.841(4) . ? P1 C12 1.853(3) . ? P1 C9 1.862(4) . ? P2 C17 1.855(5) . ? P2 C16 1.860(4) . ? P2 C20 1.863(4) . ? N1 C23 1.404(4) . ? N1 C1 1.513(4) . ? N2 C7 1.500(4) . ? N2 C15 1.510(4) . ? O1 C23 1.219(4) . ? O2 C24 1.145(4) . ? O3 C25 1.154(5) . ? C1 C4 1.527(6) . ? C1 C3 1.531(5) . ? C1 C2 1.535(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.518(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.536(5) . ? C9 C10 1.535(5) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.529(5) . ? C12 C13 1.535(5) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.522(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C19 1.532(6) . ? C17 C18 1.533(6) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.511(6) . ? C20 C22 1.529(7) . ? C20 H20A 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 C25 Co1 C24 117.5(2) . . ? C25 Co1 C23 86.45(16) . . ? C24 Co1 C23 88.13(15) . . ? C25 Co1 N2 119.16(15) . . ? C24 Co1 N2 122.92(17) . . ? C23 Co1 N2 88.88(13) . . ? C25 Co1 P1 95.78(13) . . ? C24 Co1 P1 95.34(11) . . ? C23 Co1 P1 174.42(11) . . ? N2 Co1 P1 85.57(8) . . ? N1 Si1 N2 103.72(13) . . ? N1 Si1 C5 111.47(17) . . ? N2 Si1 C5 111.00(16) . . ? N1 Si1 C6 116.54(16) . . ? N2 Si1 C6 107.10(16) . . ? C5 Si1 C6 106.93(18) . . ? C8 P1 C12 104.20(17) . . ? C8 P1 C9 105.72(17) . . ? C12 P1 C9 103.29(17) . . ? C8 P1 Co1 102.87(12) . . ? C12 P1 Co1 120.46(12) . . ? C9 P1 Co1 118.57(13) . . ? C17 P2 C16 102.77(18) . . ? C17 P2 C20 102.7(2) . . ? C16 P2 C20 100.97(18) . . ? C23 N1 C1 118.1(3) . . ? C23 N1 Si1 115.0(2) . . ? C1 N1 Si1 126.7(2) . . ? C7 N2 C15 107.7(3) . . ? C7 N2 Si1 110.9(2) . . ? C15 N2 Si1 115.6(2) . . ? C7 N2 Co1 110.4(2) . . ? C15 N2 Co1 112.33(19) . . ? Si1 N2 Co1 99.76(13) . . ? N1 C1 C4 109.8(3) . . ? N1 C1 C3 109.9(3) . . ? C4 C1 C3 112.0(3) . . ? N1 C1 C2 109.9(3) . . ? C4 C1 C2 107.5(3) . . ? C3 C1 C2 107.6(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 112.2(3) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 P1 107.8(2) . . ? C7 C8 H8A 110.1 . . ? P1 C8 H8A 110.1 . . ? C7 C8 H8B 110.1 . . ? P1 C8 H8B 110.1 . . ? H8A C8 H8B 108.5 . . ? C11 C9 C10 109.6(3) . . ? C11 C9 P1 114.5(3) . . ? C10 C9 P1 111.2(3) . . ? C11 C9 H9A 107.0 . . ? C10 C9 H9A 107.0 . . ? P1 C9 H9A 107.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 110.7(3) . . ? C14 C12 P1 110.7(3) . . ? C13 C12 P1 112.8(2) . . ? C14 C12 H12A 107.5 . . ? C13 C12 H12A 107.5 . . ? P1 C12 H12A 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 117.6(3) . . ? N2 C15 H15A 107.9 . . ? C16 C15 H15A 107.9 . . ? N2 C15 H15B 107.9 . . ? C16 C15 H15B 107.9 . . ? H15A C15 H15B 107.2 . . ? C15 C16 P2 110.3(2) . . ? C15 C16 H16A 109.6 . . ? P2 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? P2 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C19 C17 C18 110.3(4) . . ? C19 C17 P2 110.4(3) . . ? C18 C17 P2 110.1(3) . . ? C19 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? P2 C17 H17A 108.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 111.3(4) . . ? C21 C20 P2 116.5(3) . . ? C22 C20 P2 108.8(3) . . ? C21 C20 H20A 106.6 . . ? C22 C20 H20A 106.6 . . ? P2 C20 H20A 106.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C23 N1 121.6(3) . . ? O1 C23 Co1 123.2(3) . . ? N1 C23 Co1 115.2(2) . . ? O2 C24 Co1 170.4(4) . . ? O3 C25 Co1 173.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 Co1 P1 C8 118.07(18) . . . . ? C24 Co1 P1 C8 -123.53(19) . . . . ? C23 Co1 P1 C8 4.8(12) . . . . ? N2 Co1 P1 C8 -0.83(14) . . . . ? C25 Co1 P1 C12 -126.69(19) . . . . ? C24 Co1 P1 C12 -8.3(2) . . . . ? C23 Co1 P1 C12 120.0(12) . . . . ? N2 Co1 P1 C12 114.41(17) . . . . ? C25 Co1 P1 C9 1.91(19) . . . . ? C24 Co1 P1 C9 120.3(2) . . . . ? C23 Co1 P1 C9 -111.4(12) . . . . ? N2 Co1 P1 C9 -116.99(16) . . . . ? N2 Si1 N1 C23 -23.4(3) . . . . ? C5 Si1 N1 C23 96.1(3) . . . . ? C6 Si1 N1 C23 -140.8(3) . . . . ? N2 Si1 N1 C1 161.1(3) . . . . ? C5 Si1 N1 C1 -79.4(3) . . . . ? C6 Si1 N1 C1 43.7(3) . . . . ? N1 Si1 N2 C7 154.7(2) . . . . ? C5 Si1 N2 C7 34.8(3) . . . . ? C6 Si1 N2 C7 -81.5(3) . . . . ? N1 Si1 N2 C15 -82.4(2) . . . . ? C5 Si1 N2 C15 157.8(2) . . . . ? C6 Si1 N2 C15 41.4(3) . . . . ? N1 Si1 N2 Co1 38.25(15) . . . . ? C5 Si1 N2 Co1 -81.57(17) . . . . ? C6 Si1 N2 Co1 162.04(15) . . . . ? C25 Co1 N2 C7 -68.0(3) . . . . ? C24 Co1 N2 C7 119.6(2) . . . . ? C23 Co1 N2 C7 -153.3(2) . . . . ? P1 Co1 N2 C7 26.1(2) . . . . ? C25 Co1 N2 C15 171.8(2) . . . . ? C24 Co1 N2 C15 -0.6(3) . . . . ? C23 Co1 N2 C15 86.5(2) . . . . ? P1 Co1 N2 C15 -94.1(2) . . . . ? C25 Co1 N2 Si1 48.8(2) . . . . ? C24 Co1 N2 Si1 -123.60(16) . . . . ? C23 Co1 N2 Si1 -36.55(15) . . . . ? P1 Co1 N2 Si1 142.91(12) . . . . ? C23 N1 C1 C4 -55.3(4) . . . . ? Si1 N1 C1 C4 120.0(3) . . . . ? C23 N1 C1 C3 68.3(4) . . . . ? Si1 N1 C1 C3 -116.3(3) . . . . ? C23 N1 C1 C2 -173.4(3) . . . . ? Si1 N1 C1 C2 1.9(5) . . . . ? C15 N2 C7 C8 72.8(3) . . . . ? Si1 N2 C7 C8 -159.8(2) . . . . ? Co1 N2 C7 C8 -50.1(3) . . . . ? N2 C7 C8 P1 48.0(3) . . . . ? C12 P1 C8 C7 -150.2(2) . . . . ? C9 P1 C8 C7 101.2(3) . . . . ? Co1 P1 C8 C7 -23.8(3) . . . . ? C8 P1 C9 C11 71.9(3) . . . . ? C12 P1 C9 C11 -37.3(3) . . . . ? Co1 P1 C9 C11 -173.5(2) . . . . ? C8 P1 C9 C10 -53.1(3) . . . . ? C12 P1 C9 C10 -162.3(3) . . . . ? Co1 P1 C9 C10 61.5(3) . . . . ? C8 P1 C12 C14 -173.9(3) . . . . ? C9 P1 C12 C14 -63.6(3) . . . . ? Co1 P1 C12 C14 71.6(3) . . . . ? C8 P1 C12 C13 61.5(3) . . . . ? C9 P1 C12 C13 171.8(3) . . . . ? Co1 P1 C12 C13 -53.0(3) . . . . ? C7 N2 C15 C16 176.5(3) . . . . ? Si1 N2 C15 C16 51.9(4) . . . . ? Co1 N2 C15 C16 -61.7(3) . . . . ? N2 C15 C16 P2 169.3(2) . . . . ? C17 P2 C16 C15 103.6(3) . . . . ? C20 P2 C16 C15 -150.5(3) . . . . ? C16 P2 C17 C19 -67.2(3) . . . . ? C20 P2 C17 C19 -171.8(3) . . . . ? C16 P2 C17 C18 170.7(3) . . . . ? C20 P2 C17 C18 66.2(3) . . . . ? C17 P2 C20 C21 48.5(4) . . . . ? C16 P2 C20 C21 -57.4(4) . . . . ? C17 P2 C20 C22 175.2(3) . . . . ? C16 P2 C20 C22 69.2(3) . . . . ? C1 N1 C23 O1 -8.4(5) . . . . ? Si1 N1 C23 O1 175.7(3) . . . . ? C1 N1 C23 Co1 169.6(2) . . . . ? Si1 N1 C23 Co1 -6.3(3) . . . . ? C25 Co1 C23 O1 86.3(3) . . . . ? C24 Co1 C23 O1 -31.5(3) . . . . ? N2 Co1 C23 O1 -154.4(3) . . . . ? P1 Co1 C23 O1 -160.0(9) . . . . ? C25 Co1 C23 N1 -91.7(3) . . . . ? C24 Co1 C23 N1 150.6(3) . . . . ? N2 Co1 C23 N1 27.6(3) . . . . ? P1 Co1 C23 N1 22.0(14) . . . . ? C25 Co1 C24 O2 -13(2) . . . . ? C23 Co1 C24 O2 72(2) . . . . ? N2 Co1 C24 O2 160(2) . . . . ? P1 Co1 C24 O2 -112(2) . . . . ? C24 Co1 C25 O3 4(3) . . . . ? C23 Co1 C25 O3 -82(3) . . . . ? N2 Co1 C25 O3 -169(3) . . . . ? P1 Co1 C25 O3 103(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.474 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.064