# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2239 ############################################################################## # # Manuscript B005693F # # # Isolation, Structural and Spectroscopc Ivestigations of Complexes with # Tridentate [O,P,O] and [O,O,O] Donor Ligands # # Rolf Siefert, Thomas Weyhermuller, and Phalguni Chaudhuri # ############################################################################## data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural 'C34 H47 O3 P' _chemical_formula_analytical ? _chemical_formula_sum 'C34 H47 O3 P' _chemical_formula_weight 534.69 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.153(10 _cell_length_b 21.418(3) _cell_length_c 14.176(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.80(2) _cell_angle_gamma 90.00 _cell_volume 3054.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6803 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block ' _exptl_crystal_colour 'yellow greenish ' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method ? _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type 'SADABS, G. Sheldrick 1994' _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.894 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD Detector' _diffrn_measurement_method '\w-scan, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10765 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.54 _reflns_number_total 4630 _reflns_number_observed 3658 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+3.0570P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4630 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all 0.1259 _refine_ls_wR_factor_obs 0.1158 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.058 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.21146(6) 0.24688(3) 0.20012(5) 0.0167(2) Uani 1 d . . O1 O 0.4767(2) 0.17576(8) 0.22262(14) 0.0234(4) Uani 1 d . . H1 H 0.4330(29) 0.1974(14) 0.1817(22) 0.030 Uiso 1 d . . O2 O 0.3673(2) 0.36794(8) 0.20410(14) 0.0239(4) Uani 1 d . . H2 H 0.3685(28) 0.3355(14) 0.1754(21) 0.031 Uiso 1 d . . O3 O 0.3098(2) 0.25624(7) 0.13010(12) 0.0201(4) Uani 1 d . . C1 C 0.2849(2) 0.20070(10) 0.3001(2) 0.0168(5) Uani 1 d . . C2 C 0.4093(2) 0.17193(11) 0.2991(2) 0.0173(6) Uani 1 d . . C3 C 0.4676(2) 0.13773(10) 0.3794(2) 0.0178(6) Uani 1 d . . C4 C 0.3940(2) 0.13133(10) 0.4547(2) 0.0183(6) Uani 1 d . . H4 H 0.4313(2) 0.10731(10) 0.5080(2) 0.022 Uiso 1 calc R . C5 C 0.2683(2) 0.15797(10) 0.4570(2) 0.0182(6) Uani 1 d . . C6 C 0.2182(2) 0.19398(11) 0.3795(2) 0.0176(6) Uani 1 d . . H6 H 0.1358(2) 0.21485(11) 0.3803(2) 0.021 Uiso 1 calc R . C7 C 0.6066(2) 0.10838(11) 0.3822(2) 0.0203(6) Uani 1 d . . C8 C 0.7101(2) 0.15899(12) 0.3686(2) 0.0263(6) Uani 1 d . . H8A H 0.6839(2) 0.18056(12) 0.3080(2) 0.039 Uiso 1 calc R . H8B H 0.7973(2) 0.13950(12) 0.3683(2) 0.039 Uiso 1 calc R . H8C H 0.7148(2) 0.18914(12) 0.4210(2) 0.039 Uiso 1 calc R . C9 C 0.6522(3) 0.07624(13) 0.4777(2) 0.0282(7) Uani 1 d . . H9A H 0.5884(3) 0.04361(13) 0.4887(2) 0.042 Uiso 1 calc R . H9B H 0.6575(3) 0.10711(13) 0.5291(2) 0.042 Uiso 1 calc R . H9C H 0.7400(3) 0.05747(13) 0.4764(2) 0.042 Uiso 1 calc R . C10 C 0.6049(3) 0.05867(12) 0.3034(2) 0.0268(6) Uani 1 d . . H10A H 0.5760(3) 0.07789(12) 0.2413(2) 0.040 Uiso 1 calc R . H10B H 0.5431(3) 0.02515(12) 0.3146(2) 0.040 Uiso 1 calc R . H10C H 0.6943(3) 0.04135(12) 0.3042(2) 0.040 Uiso 1 calc R . C11 C 0.1888(2) 0.14866(11) 0.5404(2) 0.0198(6) Uani 1 d . . C12 C 0.2489(3) 0.0987(2) 0.6098(2) 0.0469(9) Uani 1 d . . H12A H 0.2543(3) 0.0592(2) 0.5757(2) 0.070 Uiso 1 calc R . H12B H 0.1928(3) 0.0933(2) 0.6602(2) 0.070 Uiso 1 calc R . H12C H 0.3382(3) 0.1116(2) 0.6380(2) 0.070 Uiso 1 calc R . C13 C 0.0478(3) 0.1276(2) 0.5023(2) 0.0514(9) Uani 1 d . . H13A H 0.0517(3) 0.0882(2) 0.4674(2) 0.077 Uiso 1 calc R . H13B H 0.0044(3) 0.1596(2) 0.4594(2) 0.077 Uiso 1 calc R . H13C H -0.0030(3) 0.1214(2) 0.5555(2) 0.077 Uiso 1 calc R . C14 C 0.1811(3) 0.20971(14) 0.5944(2) 0.0455(9) Uani 1 d . . H14A H 0.1425(3) 0.24220(14) 0.5504(2) 0.068 Uiso 1 calc R . H14B H 0.2706(3) 0.22229(14) 0.6227(2) 0.068 Uiso 1 calc R . H14C H 0.1252(3) 0.20395(14) 0.6449(2) 0.068 Uiso 1 calc R . C15 C 0.1672(2) 0.32087(10) 0.2474(2) 0.0171(5) Uani 1 d . . C16 C 0.2557(2) 0.37136(11) 0.2477(2) 0.0170(5) Uani 1 d . . C17 C 0.2307(2) 0.42750(10) 0.2952(2) 0.0170(5) Uani 1 d . . C18 C 0.1184(2) 0.42893(10) 0.3409(2) 0.0173(5) Uani 1 d . . H18 H 0.1013(2) 0.46607(10) 0.3739(2) 0.021 Uiso 1 calc R . C19 C 0.0278(2) 0.37929(10) 0.3420(2) 0.0166(5) Uani 1 d . . C20 C 0.0534(2) 0.32598(10) 0.2927(2) 0.0174(5) Uani 1 d . . H20 H -0.0074(2) 0.29210(10) 0.2895(2) 0.021 Uiso 1 calc R . C21 C 0.3261(2) 0.48381(11) 0.2965(2) 0.0202(6) Uani 1 d . . C22 C 0.4666(2) 0.46539(12) 0.3447(2) 0.0282(7) Uani 1 d . . H22A H 0.4614(2) 0.45050(12) 0.4094(2) 0.042 Uiso 1 calc R . H22B H 0.5253(2) 0.50184(12) 0.3473(2) 0.042 Uiso 1 calc R . H22C H 0.5020(2) 0.43214(12) 0.3078(2) 0.042 Uiso 1 calc R . C23 C 0.3319(3) 0.50726(12) 0.1950(2) 0.0279(6) Uani 1 d . . H23A H 0.3618(3) 0.47337(12) 0.1566(2) 0.042 Uiso 1 calc R . H23B H 0.3944(3) 0.54226(12) 0.1968(2) 0.042 Uiso 1 calc R . H23C H 0.2433(3) 0.52115(12) 0.1667(2) 0.042 Uiso 1 calc R . C24 C 0.2790(3) 0.53829(11) 0.3537(2) 0.0259(6) Uani 1 d . . H24A H 0.2743(3) 0.52469(11) 0.4191(2) 0.039 Uiso 1 calc R . H24B H 0.1909(3) 0.55192(11) 0.3242(2) 0.039 Uiso 1 calc R . H24C H 0.3419(3) 0.57306(11) 0.3543(2) 0.039 Uiso 1 calc R . C25 C -0.0880(2) 0.38445(11) 0.4010(2) 0.0191(6) Uani 1 d . . C26 C -0.0305(3) 0.38532(13) 0.5066(2) 0.0311(7) Uani 1 d . . H26A H 0.0204(3) 0.34697(13) 0.5224(2) 0.047 Uiso 1 calc R . H26B H -0.1031(3) 0.38796(13) 0.5454(2) 0.047 Uiso 1 calc R . H26C H 0.0281(3) 0.42157(13) 0.5195(2) 0.047 Uiso 1 calc R . C27 C -0.1844(3) 0.32913(13) 0.3839(2) 0.0373(8) Uani 1 d . . H27A H -0.2223(3) 0.32784(13) 0.3166(2) 0.056 Uiso 1 calc R . H27B H -0.2560(3) 0.33407(13) 0.4232(2) 0.056 Uiso 1 calc R . H27C H -0.1364(3) 0.29017(13) 0.4010(2) 0.056 Uiso 1 calc R . C28 C -0.1674(2) 0.44454(11) 0.3770(2) 0.0235(6) Uani 1 d . . H28A H -0.2045(2) 0.44428(11) 0.3094(2) 0.035 Uiso 1 calc R . H28B H -0.1086(2) 0.48070(11) 0.3901(2) 0.035 Uiso 1 calc R . H28C H -0.2398(2) 0.44708(11) 0.4160(2) 0.035 Uiso 1 calc R . C29 C 0.0636(2) 0.20836(10) 0.1427(2) 0.0178(6) Uani 1 d . . C30 C 0.0379(2) 0.21515(11) 0.0446(2) 0.0232(6) Uani 1 d . . H30 H 0.0937(2) 0.24102(11) 0.0127(2) 0.028 Uiso 1 calc R . C31 C -0.0688(3) 0.18445(13) -0.0074(2) 0.0298(7) Uani 1 d . . H31 H -0.0853(3) 0.18883(13) -0.0747(2) 0.036 Uiso 1 calc R . C32 C -0.1508(3) 0.14746(13) 0.0395(2) 0.0307(7) Uani 1 d . . H32 H -0.2236(3) 0.12628(13) 0.0042(2) 0.037 Uiso 1 calc R . C33 C -0.1277(3) 0.14108(12) 0.1372(2) 0.0278(7) Uani 1 d . . H33 H -0.1855(3) 0.11618(12) 0.1689(2) 0.033 Uiso 1 calc R . C34 C -0.0198(2) 0.17106(11) 0.1894(2) 0.0220(6) Uani 1 d . . H34 H -0.0031(2) 0.16615(11) 0.2566(2) 0.026 Uiso 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 P1 0.0194(3) 0.0128(3) 0.0183(4) 0.0000(2) 0.0043(3) 0.0015(2) O1 0.0235(9) 0.0257(10) 0.0223(12) 0.0032(8) 0.0078(8) 0.0068(7) O2 0.0235(9) 0.0179(9) 0.0327(13) -0.0048(8) 0.0130(8) -0.0010(7) O3 0.0248(9) 0.0176(9) 0.0190(11) 0.0000(7) 0.0069(7) 0.0018(7) C1 0.0195(12) 0.0124(11) 0.018(2) -0.0017(10) 0.0017(10) 0.0003(9) C2 0.0196(12) 0.0149(12) 0.018(2) -0.0038(10) 0.0061(11) -0.0021(9) C3 0.0179(12) 0.0118(12) 0.023(2) -0.0038(10) 0.0002(11) -0.0016(9) C4 0.0209(12) 0.0138(12) 0.019(2) -0.0005(10) 0.0002(11) -0.0006(9) C5 0.0204(12) 0.0145(12) 0.019(2) -0.0027(10) 0.0011(10) -0.0020(9) C6 0.0170(12) 0.0147(12) 0.021(2) -0.0027(10) 0.0032(11) 0.0011(9) C7 0.0171(12) 0.0218(13) 0.022(2) -0.0026(10) 0.0011(11) 0.0036(10) C8 0.0178(13) 0.0273(14) 0.035(2) -0.0045(12) 0.0061(12) -0.0009(10) C9 0.0205(13) 0.0304(15) 0.033(2) -0.0005(12) 0.0015(12) 0.0078(11) C10 0.0239(14) 0.0221(14) 0.034(2) -0.0064(12) 0.0036(12) 0.0061(10) C11 0.0201(12) 0.0215(13) 0.018(2) 0.0019(10) 0.0029(11) 0.0009(10) C12 0.052(2) 0.048(2) 0.045(2) 0.016(2) 0.020(2) 0.015(2) C13 0.038(2) 0.082(3) 0.036(2) 0.002(2) 0.010(2) -0.018(2) C14 0.064(2) 0.035(2) 0.042(2) -0.0005(15) 0.023(2) 0.0031(15) C15 0.0209(12) 0.0133(12) 0.017(2) 0.0007(9) 0.0026(10) 0.0024(9) C16 0.0177(12) 0.0193(13) 0.014(2) 0.0037(10) 0.0030(10) 0.0029(9) C17 0.0175(12) 0.0133(12) 0.020(2) 0.0024(10) 0.0004(10) 0.0019(9) C18 0.0206(12) 0.0131(11) 0.018(2) -0.0009(10) 0.0004(10) 0.0021(9) C19 0.0174(12) 0.0140(12) 0.018(2) 0.0014(10) 0.0025(10) 0.0011(9) C20 0.0204(12) 0.0125(12) 0.020(2) 0.0023(10) 0.0032(10) 0.0000(9) C21 0.0215(13) 0.0177(13) 0.022(2) -0.0002(10) 0.0063(11) -0.0014(10) C22 0.0201(13) 0.0235(14) 0.040(2) -0.0007(12) 0.0009(12) -0.0034(11) C23 0.0333(15) 0.0194(13) 0.032(2) 0.0021(11) 0.0094(13) -0.0050(11) C24 0.0269(14) 0.0181(13) 0.034(2) -0.0045(11) 0.0088(12) -0.0050(10) C25 0.0207(12) 0.0160(12) 0.022(2) -0.0006(10) 0.0078(11) 0.0005(9) C26 0.032(2) 0.038(2) 0.026(2) 0.0057(12) 0.0116(13) 0.0137(12) C27 0.036(2) 0.0258(15) 0.056(2) -0.0090(14) 0.029(2) -0.0105(12) C28 0.0204(13) 0.0238(14) 0.026(2) -0.0002(11) 0.0037(11) 0.0033(10) C29 0.0217(12) 0.0101(12) 0.022(2) -0.0025(10) 0.0038(11) 0.0052(9) C30 0.0264(14) 0.0218(13) 0.021(2) 0.0011(11) 0.0022(11) 0.0042(10) C31 0.032(2) 0.035(2) 0.021(2) -0.0041(12) -0.0020(12) 0.0066(12) C32 0.0239(14) 0.032(2) 0.035(2) -0.0116(13) -0.0008(13) 0.0018(11) C33 0.0248(14) 0.0263(14) 0.033(2) -0.0047(12) 0.0054(12) -0.0010(11) C34 0.0243(13) 0.0195(13) 0.022(2) -0.0026(10) 0.0025(11) 0.0013(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O3 1.514(2) . ? P1 C15 1.801(2) . ? P1 C1 1.805(2) . ? P1 C29 1.807(2) . ? O1 C2 1.360(3) . ? O2 C16 1.364(3) . ? C1 C6 1.397(4) . ? C1 C2 1.408(3) . ? C2 C3 1.414(3) . ? C3 C4 1.390(3) . ? C3 C7 1.541(3) . ? C4 C5 1.402(3) . ? C5 C6 1.382(3) . ? C5 C11 1.532(4) . ? C7 C9 1.533(4) . ? C7 C8 1.540(3) . ? C7 C10 1.542(3) . ? C11 C14 1.522(4) . ? C11 C12 1.523(4) . ? C11 C13 1.528(4) . ? C15 C20 1.401(3) . ? C15 C16 1.406(3) . ? C16 C17 1.418(3) . ? C17 C18 1.386(3) . ? C17 C21 1.546(3) . ? C18 C19 1.407(3) . ? C19 C20 1.382(3) . ? C19 C25 1.537(3) . ? C21 C23 1.533(4) . ? C21 C24 1.534(3) . ? C21 C22 1.547(3) . ? C25 C26 1.531(4) . ? C25 C28 1.532(3) . ? C25 C27 1.535(3) . ? C29 C30 1.387(4) . ? C29 C34 1.396(3) . ? C30 C31 1.390(4) . ? C31 C32 1.384(4) . ? C32 C33 1.379(4) . ? C33 C34 1.392(4) . ? 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 O3 P1 C15 110.32(10) . . ? O3 P1 C1 110.42(10) . . ? C15 P1 C1 106.70(11) . . ? O3 P1 C29 110.27(11) . . ? C15 P1 C29 109.60(11) . . ? C1 P1 C29 109.46(11) . . ? C6 C1 C2 119.8(2) . . ? C6 C1 P1 119.7(2) . . ? C2 C1 P1 120.5(2) . . ? O1 C2 C1 122.1(2) . . ? O1 C2 C3 118.2(2) . . ? C1 C2 C3 119.7(2) . . ? C4 C3 C2 117.4(2) . . ? C4 C3 C7 121.7(2) . . ? C2 C3 C7 120.9(2) . . ? C3 C4 C5 124.3(2) . . ? C6 C5 C4 116.5(2) . . ? C6 C5 C11 120.7(2) . . ? C4 C5 C11 122.8(2) . . ? C5 C6 C1 122.1(2) . . ? C9 C7 C8 107.3(2) . . ? C9 C7 C3 111.8(2) . . ? C8 C7 C3 110.3(2) . . ? C9 C7 C10 107.6(2) . . ? C8 C7 C10 109.7(2) . . ? C3 C7 C10 110.0(2) . . ? C14 C11 C12 108.8(2) . . ? C14 C11 C13 108.8(2) . . ? C12 C11 C13 107.1(2) . . ? C14 C11 C5 110.1(2) . . ? C12 C11 C5 112.5(2) . . ? C13 C11 C5 109.4(2) . . ? C20 C15 C16 120.3(2) . . ? C20 C15 P1 120.2(2) . . ? C16 C15 P1 119.1(2) . . ? O2 C16 C15 121.8(2) . . ? O2 C16 C17 118.3(2) . . ? C15 C16 C17 119.9(2) . . ? C18 C17 C16 116.9(2) . . ? C18 C17 C21 122.1(2) . . ? C16 C17 C21 121.0(2) . . ? C17 C18 C19 124.6(2) . . ? C20 C19 C18 116.8(2) . . ? C20 C19 C25 123.0(2) . . ? C18 C19 C25 120.1(2) . . ? C19 C20 C15 121.3(2) . . ? C23 C21 C24 107.5(2) . . ? C23 C21 C17 110.4(2) . . ? C24 C21 C17 111.1(2) . . ? C23 C21 C22 110.3(2) . . ? C24 C21 C22 107.2(2) . . ? C17 C21 C22 110.2(2) . . ? C26 C25 C28 109.1(2) . . ? C26 C25 C27 108.3(2) . . ? C28 C25 C27 108.0(2) . . ? C26 C25 C19 108.3(2) . . ? C28 C25 C19 111.0(2) . . ? C27 C25 C19 112.1(2) . . ? C30 C29 C34 119.5(2) . . ? C30 C29 P1 115.9(2) . . ? C34 C29 P1 124.6(2) . . ? C29 C30 C31 120.6(3) . . ? C32 C31 C30 119.4(3) . . ? C33 C32 C31 120.6(3) . . ? C32 C33 C34 120.1(3) . . ? C33 C34 C29 119.7(3) . . ? _refine_diff_density_max 0.718 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.050 #===END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C68 H92 Ni O4 P2' _chemical_formula_weight 1094.07 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.432(1) _cell_length_b 15.174(2) _cell_length_c 17.048(2) _cell_angle_alpha 89.99(2) _cell_angle_beta 79.00(2) _cell_angle_gamma 72.07(2) _cell_volume 3238.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5394 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Transparent Plate ' _exptl_crystal_colour 'yellow greenish' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method ? _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type 'Gaussian Face-Indexed' _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.965 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD-Detector' _diffrn_measurement_method '\w-scan, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24941 _diffrn_reflns_av_R_equivalents 0.1033 _diffrn_reflns_av_sigmaI/netI 0.1202 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11020 _reflns_number_observed 6917 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SAINT' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens ShelXTL' _computing_publication_material 'Siemens ShelXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 60 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0629P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10960 _refine_ls_number_parameters 675 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_obs 0.0589 _refine_ls_wR_factor_all 0.1412 _refine_ls_wR_factor_obs 0.1193 _refine_ls_goodness_of_fit_all 0.979 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 0.988 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.21062(4) 0.35297(3) 0.33441(3) 0.01794(14) Uani 1 d . . P1 P 0.11618(7) 0.42443(6) 0.24869(5) 0.0178(2) Uani 1 d . . O1 O 0.0629(2) 0.2399(2) 0.26305(13) 0.0236(6) Uani 1 d . . H1 H 0.0794(28) 0.2726(20) 0.2949(2) 0.035 Uiso 1 calc R . O2 O 0.3183(2) 0.3983(2) 0.28184(14) 0.0216(6) Uani 1 d . . C1 C 0.1246(3) 0.3410(2) 0.1690(2) 0.0179(8) Uani 1 d . . C2 C 0.0948(3) 0.2609(2) 0.1860(2) 0.0182(8) Uani 1 d . . C3 C 0.0940(3) 0.2011(2) 0.1237(2) 0.0219(8) Uani 1 d . . C4 C 0.1271(3) 0.2226(3) 0.0455(2) 0.0283(9) Uani 1 d . . H4 H 0.1269(3) 0.1824(3) 0.0028(2) 0.034 Uiso 1 calc R . C5 C 0.1607(3) 0.2999(3) 0.0263(2) 0.0243(9) Uani 1 d . . C6 C 0.1582(3) 0.3578(2) 0.0894(2) 0.0223(8) Uani 1 d . . H6 H 0.1801(3) 0.4112(2) 0.0783(2) 0.027 Uiso 1 calc R . C7 C 0.0551(3) 0.1161(3) 0.1410(2) 0.0285(9) Uani 1 d . . C8 C 0.0588(4) 0.0622(3) 0.0636(2) 0.0431(12) Uani 1 d . . H8A H 0.1323(4) 0.0406(3) 0.0328(2) 0.065 Uiso 1 calc R . H8B H 0.0125(4) 0.1030(3) 0.0315(2) 0.065 Uiso 1 calc R . H8C H 0.0338(4) 0.0088(3) 0.0771(2) 0.065 Uiso 1 calc R . C9 C 0.1267(4) 0.0485(3) 0.1895(3) 0.0414(11) Uani 1 d . . H9A H 0.2006(4) 0.0285(3) 0.1595(3) 0.062 Uiso 1 calc R . H9B H 0.1021(4) -0.0058(3) 0.1992(3) 0.062 Uiso 1 calc R . H9C H 0.1231(4) 0.0795(3) 0.2409(3) 0.062 Uiso 1 calc R . C10 C -0.0611(3) 0.1484(3) 0.1869(3) 0.0382(11) Uani 1 d . . H10A H -0.1057(3) 0.1915(3) 0.1552(3) 0.057 Uiso 1 calc R . H10B H -0.0654(3) 0.1798(3) 0.2382(3) 0.057 Uiso 1 calc R . H10C H -0.0864(3) 0.0945(3) 0.1965(3) 0.057 Uiso 1 calc R . C11 C 0.2021(4) 0.3201(3) -0.0603(2) 0.0363(11) Uani 1 d . . C12 C 0.3231(4) 0.2985(3) -0.0730(3) 0.0495(13) Uani 1 d . . H12A H 0.3401(4) 0.3358(3) -0.0336(3) 0.074 Uiso 1 calc R . H12B H 0.3506(4) 0.3135(3) -0.1271(3) 0.074 Uiso 1 calc R . H12C H 0.3564(4) 0.2325(3) -0.0664(3) 0.074 Uiso 1 calc R . C13 C 0.1785(5) 0.2611(3) -0.1224(2) 0.0568(15) Uani 1 d . . H13A H 0.1011(5) 0.2739(3) -0.1153(2) 0.085 Uiso 1 calc R . H13B H 0.2125(5) 0.1952(3) -0.1156(2) 0.085 Uiso 1 calc R . H13C H 0.2067(5) 0.2763(3) -0.1763(2) 0.085 Uiso 1 calc R . C14 C 0.1496(4) 0.4224(3) -0.0742(3) 0.0568(14) Uani 1 d . . H14A H 0.1636(4) 0.4619(3) -0.0350(3) 0.085 Uiso 1 calc R . H14B H 0.0724(4) 0.4350(3) -0.0682(3) 0.085 Uiso 1 calc R . H14C H 0.1793(4) 0.4356(3) -0.1284(3) 0.085 Uiso 1 calc R . C15 C -0.0231(3) 0.4934(2) 0.2753(2) 0.0189(8) Uani 1 d . . C16 C -0.0526(3) 0.5847(3) 0.3072(2) 0.0270(9) Uani 1 d . . H16 H 0.0011(3) 0.6118(3) 0.3121(2) 0.032 Uiso 1 calc R . C17 C -0.1594(3) 0.6361(3) 0.3318(2) 0.0321(10) Uani 1 d . . H17 H -0.1788(3) 0.6983(3) 0.3531(2) 0.038 Uiso 1 calc R . C18 C -0.2369(3) 0.5965(3) 0.3252(2) 0.0315(10) Uani 1 d . . H18 H -0.3101(3) 0.6319(3) 0.3414(2) 0.038 Uiso 1 calc R . C19 C -0.2097(3) 0.5061(3) 0.2953(2) 0.0293(9) Uani 1 d . . H19 H -0.2639(3) 0.4790(3) 0.2920(2) 0.035 Uiso 1 calc R . C20 C -0.1030(3) 0.4546(3) 0.2702(2) 0.0240(9) Uani 1 d . . H20 H -0.0844(3) 0.3923(3) 0.2493(2) 0.029 Uiso 1 calc R . C21 C 0.1954(3) 0.4960(2) 0.2089(2) 0.0183(8) Uani 1 d . . C22 C 0.2949(3) 0.4696(2) 0.2324(2) 0.0194(8) Uani 1 d . . C23 C 0.3684(3) 0.5177(2) 0.2043(2) 0.0205(8) Uani 1 d . . C24 C 0.3368(3) 0.5882(2) 0.1529(2) 0.0237(9) Uani 1 d . . H24 H 0.3859(3) 0.6204(2) 0.1329(2) 0.028 Uiso 1 calc R . C25 C 0.2383(3) 0.6150(2) 0.1288(2) 0.0220(8) Uani 1 d . . C26 C 0.1675(3) 0.5678(2) 0.1580(2) 0.0199(8) Uani 1 d . . H26 H 0.0996(3) 0.5842(2) 0.1435(2) 0.024 Uiso 1 calc R . C27 C 0.4773(3) 0.4976(3) 0.2291(2) 0.0237(9) Uani 1 d . . C28 C 0.5376(3) 0.5631(3) 0.1927(3) 0.0443(12) Uani 1 d . . H28A H 0.4938(3) 0.6275(3) 0.2090(3) 0.066 Uiso 1 calc R . H28B H 0.5526(3) 0.5543(3) 0.1342(3) 0.066 Uiso 1 calc R . H28C H 0.6049(3) 0.5497(3) 0.2115(3) 0.066 Uiso 1 calc R . C29 C 0.5476(4) 0.4016(3) 0.2022(5) 0.087(2) Uani 1 d . . H29A H 0.5582(4) 0.3930(3) 0.1439(5) 0.130 Uiso 1 calc R . H29B H 0.5141(4) 0.3569(3) 0.2276(5) 0.130 Uiso 1 calc R . H29C H 0.6168(4) 0.3914(3) 0.2175(5) 0.130 Uiso 1 calc R . C30 C 0.4600(4) 0.5122(6) 0.3195(3) 0.104(3) Uani 1 d . . H30A H 0.4136(4) 0.5756(6) 0.3365(3) 0.155 Uiso 1 calc R . H30B H 0.5289(4) 0.5024(6) 0.3352(3) 0.155 Uiso 1 calc R . H30C H 0.4262(4) 0.4679(6) 0.3452(3) 0.155 Uiso 1 calc R . C31 C 0.2112(3) 0.6937(3) 0.0725(2) 0.0285(9) Uani 1 d . . C32 C 0.3023(6) 0.7301(5) 0.0430(5) 0.045(2) Uiso 0.60 d P 1 H32A H 0.3280(6) 0.7478(5) 0.0888(5) 0.067 Uiso 0.60 calc PR 1 H32B H 0.2782(6) 0.7845(5) 0.0123(5) 0.067 Uiso 0.60 calc PR 1 H32C H 0.3603(6) 0.6819(5) 0.0087(5) 0.067 Uiso 0.60 calc PR 1 C33 C 0.1188(6) 0.7751(5) 0.1279(4) 0.038(2) Uiso 0.60 d P 1 H33A H 0.1468(6) 0.7945(5) 0.1717(4) 0.057 Uiso 0.60 calc PR 1 H33B H 0.0590(6) 0.7525(5) 0.1502(4) 0.057 Uiso 0.60 calc PR 1 H33C H 0.0941(6) 0.8280(5) 0.0958(4) 0.057 Uiso 0.60 calc PR 1 C34 C 0.1669(6) 0.6650(5) 0.0062(4) 0.033(2) Uiso 0.60 d P 1 H34A H 0.1077(6) 0.6418(5) 0.0289(4) 0.050 Uiso 0.60 calc PR 1 H34B H 0.2230(6) 0.6159(5) -0.0286(4) 0.050 Uiso 0.60 calc PR 1 H34C H 0.1410(6) 0.7185(5) -0.0250(4) 0.050 Uiso 0.60 calc PR 1 C32X C 0.2967(8) 0.6606(7) -0.0132(6) 0.037(3) Uiso 0.40 d P 2 H32D H 0.2916(8) 0.6026(7) -0.0347(6) 0.056 Uiso 0.40 calc PR 2 H32E H 0.3693(8) 0.6507(7) -0.0046(6) 0.056 Uiso 0.40 calc PR 2 H32F H 0.2801(8) 0.7088(7) -0.0513(6) 0.056 Uiso 0.40 calc PR 2 C33X C 0.2263(8) 0.7825(7) 0.0994(6) 0.033(2) Uiso 0.40 d P 2 H33D H 0.2957(8) 0.7685(7) 0.1152(6) 0.050 Uiso 0.40 calc PR 2 H33E H 0.1694(8) 0.8126(7) 0.1451(6) 0.050 Uiso 0.40 calc PR 2 H33F H 0.2238(8) 0.8241(7) 0.0553(6) 0.050 Uiso 0.40 calc PR 2 C34X C 0.1028(8) 0.7149(8) 0.0477(7) 0.039(3) Uiso 0.40 d P 2 H34D H 0.0935(8) 0.6570(8) 0.0302(7) 0.059 Uiso 0.40 calc PR 2 H34E H 0.1001(8) 0.7565(8) 0.0036(7) 0.059 Uiso 0.40 calc PR 2 H34F H 0.0457(8) 0.7449(8) 0.0934(7) 0.059 Uiso 0.40 calc PR 2 P2 P 0.31809(7) 0.24439(6) 0.39002(5) 0.0174(2) Uani 1 d . . O3 O 0.4654(2) 0.2315(2) 0.2295(2) 0.0338(7) Uani 1 d . . H3 H 0.4105(13) 0.2756(2) 0.2490(22) 0.051 Uiso 1 calc R . O4 O 0.0990(2) 0.3209(2) 0.39679(13) 0.0194(6) Uani 1 d . . C41 C 0.3851(3) 0.1422(2) 0.3232(2) 0.0226(8) Uani 1 d . . C42 C 0.4491(3) 0.1492(3) 0.2502(2) 0.0253(9) Uani 1 d . . C43 C 0.5013(3) 0.0714(3) 0.1961(2) 0.0318(10) Uani 1 d . . C44 C 0.4861(3) -0.0129(3) 0.2194(2) 0.0322(10) Uani 1 d . . H44 H 0.5222(3) -0.0668(3) 0.1845(2) 0.039 Uiso 1 calc R . C45 C 0.4201(3) -0.0219(3) 0.2917(2) 0.0302(10) Uani 1 d . . C46 C 0.3702(3) 0.0563(2) 0.3427(2) 0.0231(8) Uani 1 d . . H46 H 0.3250(3) 0.0522(2) 0.3918(2) 0.028 Uiso 1 calc R . C47 C 0.5721(4) 0.0791(3) 0.1151(3) 0.0408(11) Uani 1 d . . C48 C 0.5068(4) 0.1518(3) 0.0663(3) 0.0467(12) Uani 1 d . . H48A H 0.4783(4) 0.2118(3) 0.0971(3) 0.070 Uiso 1 calc R . H48B H 0.4476(4) 0.1323(3) 0.0550(3) 0.070 Uiso 1 calc R . H48C H 0.5528(4) 0.1575(3) 0.0159(3) 0.070 Uiso 1 calc R . C49 C 0.6690(3) 0.1059(3) 0.1303(3) 0.0474(12) Uani 1 d . . H49A H 0.6440(3) 0.1650(3) 0.1624(3) 0.071 Uiso 1 calc R . H49B H 0.7129(3) 0.1122(3) 0.0790(3) 0.071 Uiso 1 calc R . H49C H 0.7117(3) 0.0574(3) 0.1592(3) 0.071 Uiso 1 calc R . C50 C 0.6151(4) -0.0135(3) 0.0649(3) 0.060(2) Uani 1 d . . H50A H 0.6572(4) -0.0612(3) 0.0947(3) 0.090 Uiso 1 calc R . H50B H 0.6603(4) -0.0065(3) 0.0145(3) 0.090 Uiso 1 calc R . H50C H 0.5551(4) -0.0318(3) 0.0536(3) 0.090 Uiso 1 calc R . C51 C 0.4072(3) -0.1175(3) 0.3106(2) 0.0304(10) Uani 1 d . . C52 C 0.5141(3) -0.1863(3) 0.3195(3) 0.0375(11) Uani 1 d . . H52A H 0.5670(3) -0.1912(3) 0.2700(3) 0.056 Uiso 1 calc R . H52B H 0.5055(3) -0.2473(3) 0.3299(3) 0.056 Uiso 1 calc R . H52C H 0.5385(3) -0.1644(3) 0.3642(3) 0.056 Uiso 1 calc R . C53 C 0.3262(4) -0.1114(3) 0.3889(3) 0.0501(13) Uani 1 d . . H53A H 0.2570(4) -0.0675(3) 0.3844(3) 0.075 Uiso 1 calc R . H53B H 0.3515(4) -0.0899(3) 0.4333(3) 0.075 Uiso 1 calc R . H53C H 0.3185(4) -0.1727(3) 0.3990(3) 0.075 Uiso 1 calc R . C54 C 0.3665(4) -0.1540(3) 0.2432(3) 0.0430(12) Uani 1 d . . H54A H 0.2979(4) -0.1099(3) 0.2375(3) 0.064 Uiso 1 calc R . H54B H 0.3571(4) -0.2143(3) 0.2561(3) 0.064 Uiso 1 calc R . H54C H 0.4184(4) -0.1611(3) 0.1928(3) 0.064 Uiso 1 calc R . C55 C 0.4174(3) 0.2746(2) 0.4325(2) 0.0215(8) Uani 1 d . . C56 C 0.5261(3) 0.2259(3) 0.4113(2) 0.0286(9) Uani 1 d . . H56 H 0.5504(3) 0.1706(3) 0.3774(2) 0.034 Uiso 1 calc R . C57 C 0.5989(3) 0.2591(3) 0.4405(3) 0.0391(11) Uani 1 d . . H57 H 0.6730(3) 0.2261(3) 0.4265(3) 0.047 Uiso 1 calc R . C58 C 0.5642(3) 0.3393(3) 0.4893(2) 0.0338(10) Uani 1 d . . H58 H 0.6145(3) 0.3615(3) 0.5085(2) 0.041 Uiso 1 calc R . C59 C 0.4563(3) 0.3879(3) 0.5105(2) 0.0300(9) Uani 1 d . . H59 H 0.4325(3) 0.4430(3) 0.5445(2) 0.036 Uiso 1 calc R . C60 C 0.3834(3) 0.3557(2) 0.4818(2) 0.0231(9) Uani 1 d . . H60 H 0.3094(3) 0.3894(2) 0.4958(2) 0.028 Uiso 1 calc R . C61 C 0.2221(3) 0.2183(2) 0.4667(2) 0.0168(8) Uani 1 d . . C62 C 0.1173(3) 0.2662(2) 0.4594(2) 0.0206(8) Uani 1 d . . C63 C 0.0306(3) 0.2568(2) 0.5174(2) 0.0200(8) Uani 1 d . . C64 C 0.0568(3) 0.1928(2) 0.5746(2) 0.0206(8) Uani 1 d . . H64 H -0.0004(3) 0.1839(2) 0.6126(2) 0.025 Uiso 1 calc R . C65 C 0.1608(3) 0.1406(2) 0.5803(2) 0.0207(8) Uani 1 d . . C66 C 0.2437(3) 0.1563(2) 0.5267(2) 0.0197(8) Uani 1 d . . H66 H 0.3155(3) 0.1251(2) 0.5306(2) 0.024 Uiso 1 calc R . C67 C -0.0860(3) 0.3141(3) 0.5177(2) 0.0256(9) Uani 1 d . . C68 C -0.1626(3) 0.3020(3) 0.5931(2) 0.0361(10) Uani 1 d . . H68A H -0.2358(3) 0.3395(3) 0.5909(2) 0.054 Uiso 1 calc R . H68B H -0.1425(3) 0.3223(3) 0.6406(2) 0.054 Uiso 1 calc R . H68C H -0.1585(3) 0.2365(3) 0.5958(2) 0.054 Uiso 1 calc R . C69 C -0.0980(3) 0.4187(3) 0.5144(2) 0.0332(10) Uani 1 d . . H69A H -0.0499(3) 0.4286(3) 0.4667(2) 0.050 Uiso 1 calc R . H69B H -0.0799(3) 0.4401(3) 0.5624(2) 0.050 Uiso 1 calc R . H69C H -0.1719(3) 0.4537(3) 0.5119(2) 0.050 Uiso 1 calc R . C70 C -0.1199(3) 0.2815(3) 0.4438(2) 0.0366(11) Uani 1 d . . H70A H -0.0719(3) 0.2886(3) 0.3949(2) 0.055 Uiso 1 calc R . H70B H -0.1933(3) 0.3191(3) 0.4424(2) 0.055 Uiso 1 calc R . H70C H -0.1160(3) 0.2161(3) 0.4473(2) 0.055 Uiso 1 calc R . C71 C 0.1777(3) 0.0671(3) 0.6435(2) 0.0298(9) Uani 1 d . . C72 C 0.1165(4) 0.1096(3) 0.7267(2) 0.0402(11) Uani 1 d . . H72A H 0.1424(4) 0.1597(3) 0.7417(2) 0.060 Uiso 1 calc R . H72B H 0.1278(4) 0.0618(3) 0.7656(2) 0.060 Uiso 1 calc R . H72C H 0.0401(4) 0.1346(3) 0.7261(2) 0.060 Uiso 1 calc R . C73 C 0.1372(4) -0.0112(3) 0.6200(3) 0.0499(13) Uani 1 d . . H73A H 0.1765(4) -0.0385(3) 0.5666(3) 0.075 Uiso 1 calc R . H73B H 0.0609(4) 0.0138(3) 0.6195(3) 0.075 Uiso 1 calc R . H73C H 0.1485(4) -0.0590(3) 0.6589(3) 0.075 Uiso 1 calc R . C74 C 0.2966(3) 0.0245(3) 0.6461(3) 0.0541(14) Uani 1 d . . H74A H 0.3366(3) -0.0029(3) 0.5929(3) 0.081 Uiso 1 calc R . H74B H 0.3050(3) -0.0237(3) 0.6848(3) 0.081 Uiso 1 calc R . H74C H 0.3241(3) 0.0730(3) 0.6623(3) 0.081 Uiso 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 Ni1 0.0157(3) 0.0226(3) 0.0177(2) 0.0057(2) -0.0034(2) -0.0092(2) P1 0.0167(5) 0.0211(5) 0.0180(5) 0.0060(4) -0.0047(4) -0.0088(4) O1 0.034(2) 0.0263(15) 0.0168(13) 0.0045(11) -0.0052(12) -0.0188(12) O2 0.0147(13) 0.0270(14) 0.0270(14) 0.0122(12) -0.0058(11) -0.0112(11) C1 0.012(2) 0.023(2) 0.018(2) 0.003(2) -0.001(2) -0.005(2) C2 0.015(2) 0.023(2) 0.019(2) 0.009(2) -0.004(2) -0.008(2) C3 0.025(2) 0.023(2) 0.019(2) 0.005(2) -0.003(2) -0.011(2) C4 0.035(2) 0.031(2) 0.022(2) 0.000(2) -0.004(2) -0.015(2) C5 0.030(2) 0.026(2) 0.021(2) 0.010(2) -0.007(2) -0.012(2) C6 0.024(2) 0.022(2) 0.025(2) 0.009(2) -0.005(2) -0.013(2) C7 0.045(3) 0.025(2) 0.024(2) 0.008(2) -0.012(2) -0.020(2) C8 0.070(3) 0.039(3) 0.038(2) 0.013(2) -0.018(2) -0.038(2) C9 0.063(3) 0.024(2) 0.045(3) 0.010(2) -0.022(2) -0.017(2) C10 0.044(3) 0.043(3) 0.041(2) 0.011(2) -0.009(2) -0.033(2) C11 0.059(3) 0.036(2) 0.018(2) 0.004(2) 0.001(2) -0.027(2) C12 0.061(3) 0.059(3) 0.029(2) 0.006(2) 0.012(2) -0.032(3) C13 0.101(4) 0.067(3) 0.016(2) 0.004(2) -0.004(3) -0.050(3) C14 0.095(4) 0.045(3) 0.026(2) 0.011(2) -0.010(3) -0.018(3) C15 0.019(2) 0.027(2) 0.013(2) 0.006(2) -0.003(2) -0.010(2) C16 0.027(2) 0.031(2) 0.026(2) -0.001(2) -0.004(2) -0.014(2) C17 0.030(3) 0.031(2) 0.029(2) -0.010(2) 0.002(2) -0.006(2) C18 0.017(2) 0.036(3) 0.030(2) 0.001(2) 0.003(2) 0.002(2) C19 0.019(2) 0.040(3) 0.032(2) 0.010(2) -0.007(2) -0.011(2) C20 0.021(2) 0.024(2) 0.026(2) 0.004(2) -0.005(2) -0.006(2) C21 0.021(2) 0.022(2) 0.015(2) 0.002(2) -0.004(2) -0.010(2) C22 0.022(2) 0.020(2) 0.017(2) 0.003(2) 0.000(2) -0.010(2) C23 0.021(2) 0.022(2) 0.021(2) -0.001(2) -0.003(2) -0.011(2) C24 0.026(2) 0.023(2) 0.026(2) 0.003(2) -0.003(2) -0.015(2) C25 0.023(2) 0.018(2) 0.024(2) 0.001(2) -0.002(2) -0.007(2) C26 0.016(2) 0.023(2) 0.021(2) 0.000(2) -0.003(2) -0.007(2) C27 0.018(2) 0.034(2) 0.025(2) 0.008(2) -0.005(2) -0.016(2) C28 0.034(3) 0.040(3) 0.073(3) 0.022(2) -0.020(2) -0.025(2) C29 0.024(3) 0.039(3) 0.203(8) 0.010(4) -0.038(4) -0.009(2) C30 0.054(4) 0.269(9) 0.029(3) 0.029(4) -0.019(3) -0.104(5) C31 0.030(2) 0.024(2) 0.039(2) 0.016(2) -0.012(2) -0.016(2) P2 0.0150(5) 0.0170(5) 0.0205(5) 0.0027(4) -0.0011(4) -0.0069(4) O3 0.034(2) 0.0193(14) 0.040(2) -0.0026(13) 0.0161(14) -0.0115(13) O4 0.0130(13) 0.0269(14) 0.0210(13) 0.0080(11) -0.0052(11) -0.0089(11) C41 0.018(2) 0.022(2) 0.028(2) -0.001(2) -0.003(2) -0.009(2) C42 0.022(2) 0.023(2) 0.030(2) 0.001(2) 0.003(2) -0.009(2) C43 0.029(2) 0.028(2) 0.034(2) -0.002(2) 0.009(2) -0.010(2) C44 0.031(2) 0.022(2) 0.036(2) -0.010(2) 0.011(2) -0.008(2) C45 0.027(2) 0.026(2) 0.038(2) 0.000(2) 0.002(2) -0.014(2) C46 0.021(2) 0.018(2) 0.027(2) -0.001(2) 0.003(2) -0.007(2) C47 0.046(3) 0.027(2) 0.038(2) -0.001(2) 0.017(2) -0.011(2) C48 0.058(3) 0.046(3) 0.034(2) -0.003(2) 0.009(2) -0.023(2) C49 0.037(3) 0.047(3) 0.047(3) 0.006(2) 0.020(2) -0.013(2) C50 0.076(4) 0.042(3) 0.046(3) -0.013(2) 0.034(3) -0.021(3) C51 0.030(2) 0.019(2) 0.039(2) -0.002(2) 0.005(2) -0.010(2) C52 0.040(3) 0.026(2) 0.048(3) 0.005(2) -0.004(2) -0.016(2) C53 0.056(3) 0.028(2) 0.064(3) -0.002(2) 0.012(3) -0.024(2) C54 0.048(3) 0.019(2) 0.066(3) 0.006(2) -0.015(3) -0.014(2) C55 0.017(2) 0.025(2) 0.024(2) 0.005(2) -0.003(2) -0.010(2) C56 0.021(2) 0.023(2) 0.040(2) -0.001(2) -0.007(2) -0.004(2) C57 0.021(2) 0.035(3) 0.061(3) 0.002(2) -0.016(2) -0.005(2) C58 0.026(2) 0.041(3) 0.045(3) 0.005(2) -0.016(2) -0.020(2) C59 0.033(3) 0.030(2) 0.034(2) 0.003(2) -0.011(2) -0.016(2) C60 0.017(2) 0.024(2) 0.029(2) -0.001(2) -0.003(2) -0.007(2) C61 0.016(2) 0.016(2) 0.018(2) 0.000(2) 0.000(2) -0.007(2) C62 0.021(2) 0.023(2) 0.020(2) 0.001(2) -0.002(2) -0.011(2) C63 0.015(2) 0.024(2) 0.021(2) -0.001(2) -0.001(2) -0.007(2) C64 0.019(2) 0.025(2) 0.018(2) 0.000(2) 0.003(2) -0.013(2) C65 0.027(2) 0.017(2) 0.019(2) 0.000(2) -0.001(2) -0.010(2) C66 0.015(2) 0.021(2) 0.023(2) 0.003(2) -0.003(2) -0.006(2) C67 0.017(2) 0.034(2) 0.022(2) 0.003(2) 0.001(2) -0.006(2) C68 0.019(2) 0.055(3) 0.031(2) 0.007(2) -0.001(2) -0.009(2) C69 0.021(2) 0.041(3) 0.030(2) 0.007(2) -0.003(2) 0.000(2) C70 0.019(2) 0.066(3) 0.029(2) 0.007(2) -0.005(2) -0.020(2) C71 0.035(2) 0.022(2) 0.031(2) 0.009(2) -0.004(2) -0.009(2) C72 0.056(3) 0.034(2) 0.031(2) 0.012(2) -0.011(2) -0.013(2) C73 0.084(4) 0.032(3) 0.035(3) 0.010(2) 0.000(3) -0.027(3) C74 0.035(3) 0.049(3) 0.067(3) 0.041(3) -0.004(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O4 1.859(2) . ? Ni1 O2 1.866(2) . ? Ni1 P2 2.1804(11) . ? Ni1 P1 2.1864(11) . ? P1 C21 1.791(3) . ? P1 C15 1.809(4) . ? P1 C1 1.822(4) . ? O1 C2 1.372(4) . ? O2 C22 1.368(4) . ? C1 C6 1.396(5) . ? C1 C2 1.405(5) . ? C2 C3 1.401(5) . ? C3 C4 1.394(5) . ? C3 C7 1.543(5) . ? C4 C5 1.399(5) . ? C5 C6 1.377(5) . ? C5 C11 1.541(5) . ? C7 C10 1.534(6) . ? C7 C9 1.535(5) . ? C7 C8 1.538(5) . ? C11 C13 1.526(6) . ? C11 C12 1.528(6) . ? C11 C14 1.534(6) . ? C15 C20 1.390(5) . ? C15 C16 1.396(5) . ? C16 C17 1.388(5) . ? C17 C18 1.374(5) . ? C18 C19 1.376(5) . ? C19 C20 1.387(5) . ? C21 C26 1.398(5) . ? C21 C22 1.408(5) . ? C22 C23 1.415(5) . ? C23 C24 1.397(5) . ? C23 C27 1.541(5) . ? C24 C25 1.401(5) . ? C25 C26 1.380(5) . ? C25 C31 1.531(5) . ? C27 C29 1.488(6) . ? C27 C30 1.520(6) . ? C27 C28 1.528(5) . ? C31 C34 1.495(7) . ? C31 C32 1.496(8) . ? C31 C33X 1.506(10) . ? C31 C34X 1.532(11) . ? C31 C33 1.602(8) . ? C31 C32X 1.647(11) . ? P2 C61 1.789(3) . ? P2 C55 1.805(4) . ? P2 C41 1.807(4) . ? O3 C42 1.367(4) . ? O4 C62 1.365(4) . ? C41 C42 1.395(5) . ? C41 C46 1.409(5) . ? C42 C43 1.407(5) . ? C43 C44 1.402(5) . ? C43 C47 1.546(5) . ? C44 C45 1.408(5) . ? C45 C46 1.379(5) . ? C45 C51 1.541(5) . ? C47 C50 1.534(6) . ? C47 C48 1.536(6) . ? C47 C49 1.543(6) . ? C51 C52 1.528(5) . ? C51 C53 1.534(6) . ? C51 C54 1.534(6) . ? C55 C60 1.392(5) . ? C55 C56 1.395(5) . ? C56 C57 1.395(5) . ? C57 C58 1.376(6) . ? C58 C59 1.385(6) . ? C59 C60 1.384(5) . ? C61 C66 1.400(5) . ? C61 C62 1.400(5) . ? C62 C63 1.420(5) . ? C63 C64 1.392(5) . ? C63 C67 1.538(5) . ? C64 C65 1.400(5) . ? C65 C66 1.381(5) . ? C65 C71 1.546(5) . ? C67 C68 1.535(5) . ? C67 C69 1.547(5) . ? C67 C70 1.548(5) . ? C71 C72 1.527(6) . ? C71 C73 1.533(6) . ? C71 C74 1.538(6) . ? 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 O4 Ni1 O2 172.39(11) . . ? O4 Ni1 P2 87.00(8) . . ? O2 Ni1 P2 94.34(8) . . ? O4 Ni1 P1 94.66(8) . . ? O2 Ni1 P1 86.51(8) . . ? P2 Ni1 P1 161.06(4) . . ? C21 P1 C15 110.1(2) . . ? C21 P1 C1 107.9(2) . . ? C15 P1 C1 105.7(2) . . ? C21 P1 Ni1 99.04(12) . . ? C15 P1 Ni1 124.21(11) . . ? C1 P1 Ni1 109.05(11) . . ? C22 O2 Ni1 120.1(2) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 P1 119.7(3) . . ? C2 C1 P1 121.1(3) . . ? O1 C2 C3 117.8(3) . . ? O1 C2 C1 121.8(3) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 117.6(3) . . ? C4 C3 C7 121.3(3) . . ? C2 C3 C7 121.1(3) . . ? C3 C4 C5 123.7(4) . . ? C6 C5 C4 116.8(3) . . ? C6 C5 C11 120.1(3) . . ? C4 C5 C11 123.0(3) . . ? C5 C6 C1 122.3(3) . . ? C10 C7 C9 110.4(3) . . ? C10 C7 C8 107.5(3) . . ? C9 C7 C8 107.2(3) . . ? C10 C7 C3 109.5(3) . . ? C9 C7 C3 110.3(3) . . ? C8 C7 C3 111.9(3) . . ? C13 C11 C12 108.1(4) . . ? C13 C11 C14 107.8(4) . . ? C12 C11 C14 109.9(4) . . ? C13 C11 C5 112.7(3) . . ? C12 C11 C5 108.3(3) . . ? C14 C11 C5 109.9(3) . . ? C20 C15 C16 118.6(3) . . ? C20 C15 P1 120.7(3) . . ? C16 C15 P1 120.5(3) . . ? C17 C16 C15 120.7(3) . . ? C18 C17 C16 119.5(4) . . ? C17 C18 C19 120.8(4) . . ? C18 C19 C20 119.9(4) . . ? C19 C20 C15 120.5(4) . . ? C26 C21 C22 121.9(3) . . ? C26 C21 P1 126.1(3) . . ? C22 C21 P1 111.9(3) . . ? O2 C22 C21 119.4(3) . . ? O2 C22 C23 121.6(3) . . ? C21 C22 C23 119.0(3) . . ? C24 C23 C22 116.7(3) . . ? C24 C23 C27 120.0(3) . . ? C22 C23 C27 123.3(3) . . ? C23 C24 C25 125.0(3) . . ? C26 C25 C24 117.2(3) . . ? C26 C25 C31 121.9(3) . . ? C24 C25 C31 120.9(3) . . ? C25 C26 C21 120.3(3) . . ? C29 C27 C30 110.2(5) . . ? C29 C27 C28 106.8(4) . . ? C30 C27 C28 106.9(4) . . ? C29 C27 C23 111.4(3) . . ? C30 C27 C23 109.4(3) . . ? C28 C27 C23 112.0(3) . . ? C34 C31 C32 112.9(5) . . ? C33X C31 C34X 109.9(6) . . ? C34 C31 C25 110.4(4) . . ? C32 C31 C25 113.0(4) . . ? C33X C31 C25 114.3(5) . . ? C34X C31 C25 116.5(5) . . ? C34 C31 C33 108.7(4) . . ? C32 C31 C33 107.4(4) . . ? C25 C31 C33 103.8(4) . . ? C33X C31 C32X 104.6(6) . . ? C34X C31 C32X 102.9(6) . . ? C25 C31 C32X 107.4(4) . . ? C61 P2 C55 110.8(2) . . ? C61 P2 C41 108.5(2) . . ? C55 P2 C41 108.0(2) . . ? C61 P2 Ni1 99.37(12) . . ? C55 P2 Ni1 117.62(12) . . ? C41 P2 Ni1 112.04(12) . . ? C62 O4 Ni1 119.8(2) . . ? C42 C41 C46 119.7(3) . . ? C42 C41 P2 119.6(3) . . ? C46 C41 P2 120.6(3) . . ? O3 C42 C41 121.2(3) . . ? O3 C42 C43 117.6(3) . . ? C41 C42 C43 121.2(3) . . ? C44 C43 C42 116.8(3) . . ? C44 C43 C47 122.0(3) . . ? C42 C43 C47 121.3(3) . . ? C43 C44 C45 123.4(4) . . ? C46 C45 C44 117.8(3) . . ? C46 C45 C51 123.1(3) . . ? C44 C45 C51 119.2(3) . . ? C45 C46 C41 121.1(3) . . ? C50 C47 C48 107.7(4) . . ? C50 C47 C49 107.6(4) . . ? C48 C47 C49 110.5(3) . . ? C50 C47 C43 111.5(3) . . ? C48 C47 C43 110.1(3) . . ? C49 C47 C43 109.5(4) . . ? C52 C51 C53 108.2(4) . . ? C52 C51 C54 109.5(3) . . ? C53 C51 C54 107.9(3) . . ? C52 C51 C45 110.1(3) . . ? C53 C51 C45 111.1(3) . . ? C54 C51 C45 109.9(3) . . ? C60 C55 C56 119.6(3) . . ? C60 C55 P2 117.4(3) . . ? C56 C55 P2 122.7(3) . . ? C55 C56 C57 119.2(4) . . ? C58 C57 C56 120.6(4) . . ? C57 C58 C59 120.4(4) . . ? C60 C59 C58 119.6(4) . . ? C59 C60 C55 120.7(3) . . ? C66 C61 C62 121.7(3) . . ? C66 C61 P2 126.6(3) . . ? C62 C61 P2 111.7(3) . . ? O4 C62 C61 120.2(3) . . ? O4 C62 C63 120.5(3) . . ? C61 C62 C63 119.4(3) . . ? C64 C63 C62 116.3(3) . . ? C64 C63 C67 121.5(3) . . ? C62 C63 C67 122.3(3) . . ? C63 C64 C65 125.0(3) . . ? C66 C65 C64 117.2(3) . . ? C66 C65 C71 123.3(3) . . ? C64 C65 C71 119.4(3) . . ? C65 C66 C61 120.1(3) . . ? C68 C67 C63 112.1(3) . . ? C68 C67 C69 107.6(3) . . ? C63 C67 C69 110.7(3) . . ? C68 C67 C70 108.1(3) . . ? C63 C67 C70 108.8(3) . . ? C69 C67 C70 109.4(3) . . ? C72 C71 C73 109.4(3) . . ? C72 C71 C74 108.9(4) . . ? C73 C71 C74 107.8(4) . . ? C72 C71 C65 110.9(3) . . ? C73 C71 C65 108.3(3) . . ? C74 C71 C65 111.4(3) . . ? _refine_diff_density_max 0.490 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.071 #===END data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C68 H93 Co O5 P2], 1.25 C4 H8 O' _chemical_formula_analytical ? _chemical_formula_sum 'C73 H103 Co O6.25 P2' _chemical_formula_weight 1201.42 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.428(2) _cell_length_b 17.910(3) _cell_length_c 27.350(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.61(2) _cell_angle_gamma 90.00 _cell_volume 7033(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16621 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_method ? _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa-CCD' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36148 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12361 _reflns_number_observed 7002 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 26 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12335 _refine_ls_number_parameters 764 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1306 _refine_ls_R_factor_obs 0.0663 _refine_ls_wR_factor_all 0.1907 _refine_ls_wR_factor_obs 0.1626 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_goodness_of_fit_obs 1.202 _refine_ls_restrained_S_all 1.044 _refine_ls_restrained_S_obs 1.205 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 1.30532(3) -0.19423(3) 0.68946(2) 0.02959(14) Uani 1 d . . P1 P 1.26275(6) -0.07717(5) 0.68976(3) 0.0276(2) Uani 1 d . . O1 O 1.25337(15) -0.19565(13) 0.62295(9) 0.0380(7) Uani 1 d . . O2 O 1.2195(2) -0.12240(13) 0.79565(9) 0.0320(6) Uani 1 d . . H2 H 1.2617(25) -0.1443(21) 0.7799(13) 0.048 Uiso 1 d . . O10 O 1.1877(2) -0.2363(2) 0.71561(11) 0.0593(9) Uani 1 d D . H10D H 1.1435(15) -0.2850(15) 0.7273(15) 0.089 Uiso 1 d D . H10E H 1.1382(26) -0.2149(24) 0.6833(12) 0.089 Uiso 1 d D . C1 C 1.2322(2) -0.1321(2) 0.59919(14) 0.0366(10) Uani 1 d . . C2 C 1.2347(2) -0.0634(2) 0.62520(13) 0.0311(9) Uani 1 d . . C3 C 1.2179(2) 0.0042(2) 0.60085(13) 0.0353(10) Uani 1 d . . H3 H 1.2203(2) 0.0485(2) 0.61874(13) 0.042 Uiso 1 calc R . C4 C 1.1974(2) 0.0064(2) 0.55014(14) 0.0428(11) Uani 1 d . . C5 C 1.1922(2) -0.0627(3) 0.52601(15) 0.0482(12) Uani 1 d . . H5 H 1.1769(2) -0.0619(3) 0.49218(15) 0.058 Uiso 1 calc R . C6 C 1.2076(2) -0.1322(2) 0.54769(14) 0.0415(11) Uani 1 d . . C7 C 1.1990(3) -0.2048(3) 0.5180(2) 0.0544(13) Uani 1 d . . C8 C 1.1241(3) -0.2542(2) 0.5372(2) 0.0665(15) Uani 1 d . . H8A H 1.1187(3) -0.2997(2) 0.5186(2) 0.100 Uiso 1 calc R . H8B H 1.0656(3) -0.2284(2) 0.5338(2) 0.100 Uiso 1 calc R . H8C H 1.1412(3) -0.2655(2) 0.5712(2) 0.100 Uiso 1 calc R . C9 C 1.2928(3) -0.2465(2) 0.5215(2) 0.0621(14) Uani 1 d . . H9A H 1.3393(3) -0.2150(2) 0.5094(2) 0.093 Uiso 1 calc R . H9B H 1.2863(3) -0.2912(2) 0.5022(2) 0.093 Uiso 1 calc R . H9C H 1.3111(3) -0.2591(2) 0.5552(2) 0.093 Uiso 1 calc R . C10 C 1.1711(3) -0.1894(3) 0.4628(2) 0.075(2) Uani 1 d . . H10A H 1.2174(3) -0.1584(3) 0.4500(2) 0.113 Uiso 1 calc R . H10B H 1.1119(3) -0.1644(3) 0.4589(2) 0.113 Uiso 1 calc R . H10C H 1.1667(3) -0.2358(3) 0.4451(2) 0.113 Uiso 1 calc R . C11 C 1.1806(2) 0.0799(2) 0.52212(12) 0.0601(13) Uani 1 d D . C12 C 1.1907(7) 0.1510(3) 0.5536(3) 0.071(3) Uani 0.55 d PD 1 H12A H 1.1790(7) 0.1940(3) 0.5330(3) 0.107 Uiso 0.55 calc PR 1 H12B H 1.2527(7) 0.1537(3) 0.5698(3) 0.107 Uiso 0.55 calc PR 1 H12C H 1.1467(7) 0.1497(3) 0.5778(3) 0.107 Uiso 0.55 calc PR 1 C13 C 1.2493(5) 0.0838(5) 0.4822(2) 0.067(3) Uani 0.55 d PD 1 H13A H 1.2399(5) 0.1296(5) 0.4641(2) 0.100 Uiso 0.55 calc PR 1 H13B H 1.2386(5) 0.0423(5) 0.4601(2) 0.100 Uiso 0.55 calc PR 1 H13C H 1.3121(5) 0.0819(5) 0.4974(2) 0.100 Uiso 0.55 calc PR 1 C14 C 1.0827(4) 0.0780(5) 0.4933(3) 0.065(3) Uani 0.55 d PD 1 H14A H 1.0718(4) 0.1240(5) 0.4756(3) 0.098 Uiso 0.55 calc PR 1 H14B H 1.0363(4) 0.0718(5) 0.5159(3) 0.098 Uiso 0.55 calc PR 1 H14C H 1.0792(4) 0.0371(5) 0.4705(3) 0.098 Uiso 0.55 calc PR 1 C12X C 1.1075(5) 0.1259(5) 0.5472(3) 0.061(3) Uani 0.45 d PD 2 H12D H 1.0962(5) 0.1723(5) 0.5300(3) 0.092 Uiso 0.45 calc PR 2 H12E H 1.1305(5) 0.1359(5) 0.5807(3) 0.092 Uiso 0.45 calc PR 2 H12F H 1.0504(5) 0.0981(5) 0.5464(3) 0.092 Uiso 0.45 calc PR 2 C13X C 1.2704(5) 0.1265(5) 0.5332(4) 0.086(4) Uani 0.45 d PD 2 H13D H 1.2634(5) 0.1735(5) 0.5164(4) 0.129 Uiso 0.45 calc PR 2 H13E H 1.3222(5) 0.0999(5) 0.5222(4) 0.129 Uiso 0.45 calc PR 2 H13F H 1.2813(5) 0.1351(5) 0.5679(4) 0.129 Uiso 0.45 calc PR 2 C14X C 1.1561(12) 0.0721(8) 0.4664(2) 0.109(5) Uani 0.45 d PD 2 H14D H 1.1468(12) 0.1208(8) 0.4520(2) 0.164 Uiso 0.45 calc PR 2 H14E H 1.1000(12) 0.0434(8) 0.4602(2) 0.164 Uiso 0.45 calc PR 2 H14F H 1.2060(12) 0.0474(8) 0.4522(2) 0.164 Uiso 0.45 calc PR 2 C15 C 1.1578(2) -0.0596(2) 0.72052(13) 0.0286(9) Uani 1 d . . C16 C 1.1500(2) -0.0832(2) 0.76864(13) 0.0258(9) Uani 1 d . . C17 C 1.0723(2) -0.0650(2) 0.79343(13) 0.0288(9) Uani 1 d . . C18 C 1.0019(2) -0.0238(2) 0.76625(14) 0.0344(10) Uani 1 d . . H18 H 0.9491(2) -0.0114(2) 0.78155(14) 0.041 Uiso 1 calc R . C19 C 1.0060(2) -0.0005(2) 0.71839(14) 0.0343(9) Uani 1 d . . C20 C 1.0849(2) -0.0191(2) 0.69605(14) 0.0348(10) Uani 1 d . . H20 H 1.0894(2) -0.0042(2) 0.66380(14) 0.042 Uiso 1 calc R . C21 C 1.0644(2) -0.0891(2) 0.84639(14) 0.0347(10) Uani 1 d . . C22 C 1.0665(2) -0.1746(2) 0.85075(15) 0.0417(11) Uani 1 d . . H22A H 1.1224(2) -0.1933(2) 0.83884(15) 0.063 Uiso 1 calc R . H22B H 1.0133(2) -0.1952(2) 0.83158(15) 0.063 Uiso 1 calc R . H22C H 1.0650(2) -0.1886(2) 0.88454(15) 0.063 Uiso 1 calc R . C23 C 0.9747(2) -0.0621(2) 0.86564(14) 0.0430(11) Uani 1 d . . H23A H 0.9729(2) -0.0785(2) 0.89894(14) 0.065 Uiso 1 calc R . H23B H 0.9222(2) -0.0821(2) 0.84562(14) 0.065 Uiso 1 calc R . H23C H 0.9724(2) -0.0085(2) 0.86449(14) 0.065 Uiso 1 calc R . C24 C 1.1446(2) -0.0542(2) 0.88049(14) 0.0471(11) Uani 1 d . . H24A H 1.2032(2) -0.0695(2) 0.86994(14) 0.071 Uiso 1 calc R . H24B H 1.1405(2) -0.0707(2) 0.91360(14) 0.071 Uiso 1 calc R . H24C H 1.1399(2) -0.0008(2) 0.87910(14) 0.071 Uiso 1 calc R . C25 C 0.9278(2) 0.0456(2) 0.68993(11) 0.0470(11) Uani 1 d D . C26 C 0.8917(4) 0.0016(3) 0.6440(2) 0.057(2) Uiso 0.72 d PD 1 H26A H 0.8681(4) -0.0458(3) 0.6535(2) 0.086 Uiso 0.72 calc PR 1 H26B H 0.9416(4) -0.0062(3) 0.6238(2) 0.086 Uiso 0.72 calc PR 1 H26C H 0.8428(4) 0.0293(3) 0.6258(2) 0.086 Uiso 0.72 calc PR 1 C27 C 0.9655(4) 0.1208(3) 0.6755(2) 0.056(2) Uiso 0.72 d PD 1 H27A H 1.0183(4) 0.1134(3) 0.6573(2) 0.084 Uiso 0.72 calc PR 1 H27B H 0.9841(4) 0.1493(3) 0.7046(2) 0.084 Uiso 0.72 calc PR 1 H27C H 0.9180(4) 0.1474(3) 0.6556(2) 0.084 Uiso 0.72 calc PR 1 C28 C 0.8435(3) 0.0547(3) 0.7191(2) 0.0457(15) Uiso 0.72 d PD 1 H28A H 0.8213(3) 0.0064(3) 0.7277(2) 0.069 Uiso 0.72 calc PR 1 H28B H 0.7950(3) 0.0808(3) 0.6995(2) 0.069 Uiso 0.72 calc PR 1 H28C H 0.8611(3) 0.0827(3) 0.7485(2) 0.069 Uiso 0.72 calc PR 1 C26X C 0.9118(11) 0.1140(5) 0.7217(5) 0.072(5) Uiso 0.28 d PD 2 H26D H 0.9686(11) 0.1421(5) 0.7272(5) 0.108 Uiso 0.28 calc PR 2 H26E H 0.8929(11) 0.0979(5) 0.7527(5) 0.108 Uiso 0.28 calc PR 2 H26F H 0.8641(11) 0.1448(5) 0.7052(5) 0.108 Uiso 0.28 calc PR 2 C27X C 0.9600(7) 0.0896(6) 0.6467(3) 0.022(3) Uiso 0.28 d PD 2 H27D H 1.0180(7) 0.1139(6) 0.6568(3) 0.033 Uiso 0.28 calc PR 2 H27E H 0.9139(7) 0.1264(6) 0.6361(3) 0.033 Uiso 0.28 calc PR 2 H27F H 0.9681(7) 0.0561(6) 0.6201(3) 0.033 Uiso 0.28 calc PR 2 C28X C 0.8370(6) 0.0026(8) 0.6821(7) 0.075(5) Uiso 0.28 d PD 2 H28D H 0.8255(6) -0.0222(8) 0.7120(7) 0.112 Uiso 0.28 calc PR 2 H28E H 0.8411(6) -0.0338(8) 0.6566(7) 0.112 Uiso 0.28 calc PR 2 H28F H 0.7869(6) 0.0365(8) 0.6727(7) 0.112 Uiso 0.28 calc PR 2 C29 C 1.3421(2) -0.0038(2) 0.71331(13) 0.0272(9) Uani 1 d . . C30 C 1.3521(2) 0.0132(2) 0.76364(14) 0.0360(10) Uani 1 d . . H30 H 1.3174(2) -0.0126(2) 0.78508(14) 0.043 Uiso 1 calc R . C31 C 1.4131(3) 0.0681(2) 0.78126(15) 0.0427(11) Uani 1 d . . H31 H 1.4192(3) 0.0794(2) 0.81461(15) 0.051 Uiso 1 calc R . C32 C 1.4655(3) 0.1067(2) 0.74983(15) 0.0431(11) Uani 1 d . . H32 H 1.5071(3) 0.1434(2) 0.76208(15) 0.052 Uiso 1 calc R . C33 C 1.4560(2) 0.0907(2) 0.70064(15) 0.0393(10) Uani 1 d . . H33 H 1.4905(2) 0.1170(2) 0.67943(15) 0.047 Uiso 1 calc R . C34 C 1.3946(2) 0.0349(2) 0.68220(14) 0.0314(9) Uani 1 d . . H34 H 1.3891(2) 0.0238(2) 0.64883(14) 0.038 Uiso 1 calc R . P2 P 1.44540(6) -0.18317(5) 0.67078(3) 0.0254(2) Uani 1 d . . O3 O 1.3330(2) -0.30039(12) 0.68286(9) 0.0389(7) Uani 1 d . . O4 O 1.35513(14) -0.19486(12) 0.75726(8) 0.0287(6) Uani 1 d . . C35 C 1.4571(2) -0.2679(2) 0.63749(13) 0.0260(9) Uani 1 d . . C36 C 1.3908(2) -0.3202(2) 0.65016(14) 0.0338(10) Uani 1 d . . C37 C 1.3906(2) -0.3917(2) 0.62786(14) 0.0338(10) Uani 1 d . . C38 C 1.4572(2) -0.4053(2) 0.59594(13) 0.0315(9) Uani 1 d . . H38 H 1.4577(2) -0.4523(2) 0.58157(13) 0.038 Uiso 1 calc R . C39 C 1.5245(2) -0.3536(2) 0.58344(12) 0.0270(9) Uani 1 d . . C40 C 1.5227(2) -0.2842(2) 0.60515(12) 0.0243(8) Uani 1 d . . H40 H 1.5658(2) -0.2481(2) 0.59809(12) 0.029 Uiso 1 calc R . C41 C 1.3160(3) -0.4497(2) 0.6377(2) 0.0527(12) Uani 1 d . . C42 C 1.3240(3) -0.5213(2) 0.6077(2) 0.0669(15) Uani 1 d . . H42A H 1.3180(3) -0.5094(2) 0.5734(2) 0.100 Uiso 1 calc R . H42B H 1.2754(3) -0.5553(2) 0.6145(2) 0.100 Uiso 1 calc R . H42C H 1.3834(3) -0.5441(2) 0.6166(2) 0.100 Uiso 1 calc R . C43 C 1.2196(3) -0.4165(2) 0.6221(2) 0.081(2) Uani 1 d . . H43A H 1.2153(3) -0.4037(2) 0.5879(2) 0.122 Uiso 1 calc R . H43B H 1.2108(3) -0.3725(2) 0.6412(2) 0.122 Uiso 1 calc R . H43C H 1.1725(3) -0.4525(2) 0.6276(2) 0.122 Uiso 1 calc R . C44 C 1.3257(3) -0.4709(2) 0.6921(2) 0.079(2) Uani 1 d . . H44A H 1.3209(3) -0.4268(2) 0.7116(2) 0.119 Uiso 1 calc R . H44B H 1.3852(3) -0.4940(2) 0.7004(2) 0.119 Uiso 1 calc R . H44C H 1.2771(3) -0.5052(2) 0.6983(2) 0.119 Uiso 1 calc R . C45 C 1.5927(2) -0.3752(2) 0.54675(14) 0.0344(10) Uani 1 d . . C46 C 1.6587(3) -0.3116(2) 0.5374(2) 0.0538(12) Uani 1 d . . H46A H 1.7004(3) -0.3274(2) 0.5141(2) 0.081 Uiso 1 calc R . H46B H 1.6940(3) -0.2979(2) 0.5676(2) 0.081 Uiso 1 calc R . H46C H 1.6234(3) -0.2693(2) 0.5245(2) 0.081 Uiso 1 calc R . C47 C 1.5371(3) -0.3934(2) 0.49726(14) 0.0519(12) Uani 1 d . . H47A H 1.5793(3) -0.4071(2) 0.47373(14) 0.078 Uiso 1 calc R . H47B H 1.5019(3) -0.3503(2) 0.48567(14) 0.078 Uiso 1 calc R . H47C H 1.4953(3) -0.4341(2) 0.50151(14) 0.078 Uiso 1 calc R . C48 C 1.6487(3) -0.4438(2) 0.5648(2) 0.0519(12) Uani 1 d . . H48A H 1.6914(3) -0.4568(2) 0.5414(2) 0.078 Uiso 1 calc R . H48B H 1.6071(3) -0.4848(2) 0.5685(2) 0.078 Uiso 1 calc R . H48C H 1.6828(3) -0.4330(2) 0.5959(2) 0.078 Uiso 1 calc R . C49 C 1.5063(2) -0.1927(2) 0.73038(12) 0.0246(8) Uani 1 d . . C50 C 1.4478(2) -0.2011(2) 0.76819(13) 0.0285(9) Uani 1 d . . C51 C 1.4895(2) -0.2179(2) 0.81628(13) 0.0299(9) Uani 1 d . . C52 C 1.5863(2) -0.2244(2) 0.82201(14) 0.0332(9) Uani 1 d . . H52 H 1.6140(2) -0.2342(2) 0.85350(14) 0.040 Uiso 1 calc R . C53 C 1.6454(2) -0.2176(2) 0.78465(13) 0.0297(9) Uani 1 d . . C54 C 1.6036(2) -0.2028(2) 0.73843(13) 0.0288(9) Uani 1 d . . H54 H 1.6397(2) -0.1993(2) 0.71217(13) 0.035 Uiso 1 calc R . C55 C 1.4320(2) -0.2275(2) 0.86045(13) 0.0347(10) Uani 1 d . . C56 C 1.3472(2) -0.2784(2) 0.84786(14) 0.0410(10) Uani 1 d . . H56A H 1.3678(2) -0.3266(2) 0.83812(14) 0.061 Uiso 1 calc R . H56B H 1.3074(2) -0.2568(2) 0.82142(14) 0.061 Uiso 1 calc R . H56C H 1.3133(2) -0.2836(2) 0.87619(14) 0.061 Uiso 1 calc R . C57 C 1.4001(3) -0.1500(2) 0.87614(14) 0.0431(11) Uani 1 d . . H57A H 1.4536(3) -0.1187(2) 0.88390(14) 0.065 Uiso 1 calc R . H57B H 1.3664(3) -0.1548(2) 0.90455(14) 0.065 Uiso 1 calc R . H57C H 1.3605(3) -0.1280(2) 0.84978(14) 0.065 Uiso 1 calc R . C58 C 1.4901(3) -0.2632(2) 0.90523(14) 0.0472(11) Uani 1 d . . H58A H 1.5109(3) -0.3119(2) 0.89640(14) 0.071 Uiso 1 calc R . H58B H 1.4523(3) -0.2676(2) 0.93207(14) 0.071 Uiso 1 calc R . H58C H 1.5431(3) -0.2323(2) 0.91490(14) 0.071 Uiso 1 calc R . C59 C 1.7509(2) -0.2317(2) 0.79239(14) 0.0369(10) Uani 1 d . . C60 C 1.8017(3) -0.1725(2) 0.7655(2) 0.0510(12) Uani 1 d . . H60A H 1.7894(3) -0.1242(2) 0.7786(2) 0.077 Uiso 1 calc R . H60B H 1.7804(3) -0.1738(2) 0.7312(2) 0.077 Uiso 1 calc R . H60C H 1.8675(3) -0.1821(2) 0.7698(2) 0.077 Uiso 1 calc R . C61 C 1.7873(3) -0.2290(3) 0.8468(2) 0.070(2) Uani 1 d . . H61A H 1.7560(3) -0.2661(3) 0.8645(2) 0.105 Uiso 1 calc R . H61B H 1.7758(3) -0.1805(3) 0.8598(2) 0.105 Uiso 1 calc R . H61C H 1.8531(3) -0.2388(3) 0.8503(2) 0.105 Uiso 1 calc R . C62 C 1.7714(3) -0.3078(2) 0.7710(2) 0.080(2) Uani 1 d . . H62A H 1.7397(3) -0.3458(2) 0.7876(2) 0.121 Uiso 1 calc R . H62B H 1.8373(3) -0.3169(2) 0.7753(2) 0.121 Uiso 1 calc R . H62C H 1.7502(3) -0.3085(2) 0.7366(2) 0.121 Uiso 1 calc R . C63 C 1.4966(2) -0.1102(2) 0.63693(12) 0.0249(8) Uani 1 d . . C64 C 1.5661(2) -0.0627(2) 0.65784(14) 0.0304(9) Uani 1 d . . H64 H 1.5891(2) -0.0686(2) 0.69058(14) 0.036 Uiso 1 calc R . C65 C 1.6008(2) -0.0070(2) 0.62997(15) 0.0394(10) Uani 1 d . . H65 H 1.6489(2) 0.0234(2) 0.64358(15) 0.047 Uiso 1 calc R . C66 C 1.5648(3) 0.0037(2) 0.5824(2) 0.0579(13) Uani 1 d . . H66 H 1.5872(3) 0.0422(2) 0.5640(2) 0.069 Uiso 1 calc R . C67 C 1.4954(3) -0.0423(3) 0.5618(2) 0.0618(14) Uani 1 d . . H67 H 1.4707(3) -0.0344(3) 0.5295(2) 0.074 Uiso 1 calc R . C68 C 1.4625(3) -0.0994(2) 0.58811(14) 0.0406(10) Uani 1 d . . H68 H 1.4171(3) -0.1313(2) 0.57340(14) 0.049 Uiso 1 calc R . O70X O 1.0158(6) -0.2577(5) 0.6837(3) 0.093(3) Uiso 0.46 d PD 1 C71X C 0.9825(17) -0.3221(10) 0.6544(10) 0.535(38) Uiso 0.46 d PD 1 H71A H 0.9614(17) -0.3594(10) 0.6765(10) 0.642 Uiso 0.46 calc PR 1 H71B H 1.0349(17) -0.3432(10) 0.6396(10) 0.642 Uiso 0.46 calc PR 1 C72X C 0.9025(9) -0.3083(7) 0.6128(5) 0.096(4) Uiso 0.46 d PD 1 H72A H 0.9244(9) -0.3079(7) 0.5804(5) 0.115 Uiso 0.46 calc PR 1 H72B H 0.8518(9) -0.3437(7) 0.6137(5) 0.115 Uiso 0.46 calc PR 1 O70Y O 1.0332(4) -0.2585(3) 0.6577(2) 0.051(2) Uiso 0.54 d P 2 C71Y C 0.9860(4) -0.3291(4) 0.6498(3) 0.036(2) Uiso 0.54 d P 2 H71C H 1.0008(4) -0.3617(4) 0.6778(3) 0.044 Uiso 0.54 calc PR 2 H71D H 1.0053(4) -0.3533(4) 0.6207(3) 0.044 Uiso 0.54 calc PR 2 C72Y C 0.8833(8) -0.3129(7) 0.6433(5) 0.103(4) Uiso 0.54 d P 2 H72C H 0.8523(8) -0.3437(7) 0.6174(5) 0.123 Uiso 0.54 calc PR 2 H72D H 0.8551(8) -0.3220(7) 0.6735(5) 0.123 Uiso 0.54 calc PR 2 C73 C 0.8774(4) -0.2319(3) 0.6296(3) 0.115(2) Uani 1 d . . H73A H 0.8324(4) -0.2348(3) 0.6536(3) 0.138 Uiso 1 calc R 1 H73B H 0.8516(4) -0.2018(3) 0.6021(3) 0.138 Uiso 1 calc R 1 C74 C 0.9703(3) -0.1989(3) 0.6526(2) 0.102(2) Uani 1 d . . H74A H 1.0092(3) -0.1844(3) 0.6272(2) 0.123 Uiso 1 calc R 1 H74B H 0.9591(3) -0.1552(3) 0.6722(2) 0.123 Uiso 1 calc R 1 C80 C 0.9605(3) 0.0264(3) 0.9896(2) 0.080(6) Uiso 0.25 d PR . C81 C 0.9978(3) -0.4326(3) 0.5397(2) 0.109(8) Uiso 0.25 d PR . C82 C 0.9180(3) -0.4157(3) 0.5088(2) 0.178(14) Uiso 0.25 d PR . C83 C 0.9058(3) -0.0097(3) 0.9891(2) 0.120(9) Uiso 0.25 d PR . 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 0.0215(2) 0.0242(3) 0.0439(3) -0.0057(2) 0.0077(2) -0.0018(2) P1 0.0221(5) 0.0268(5) 0.0334(6) -0.0053(5) 0.0000(4) 0.0016(4) O1 0.0262(13) 0.0347(15) 0.052(2) -0.0170(13) -0.0043(12) 0.0017(11) O2 0.0260(13) 0.0291(14) 0.041(2) 0.0007(12) 0.0052(11) 0.0073(10) O10 0.042(2) 0.059(2) 0.082(2) -0.034(2) 0.0323(15) -0.0179(14) C1 0.018(2) 0.046(3) 0.045(3) -0.013(2) -0.002(2) 0.001(2) C2 0.020(2) 0.036(2) 0.037(2) -0.009(2) 0.000(2) 0.0058(15) C3 0.032(2) 0.039(2) 0.035(2) -0.008(2) 0.003(2) 0.005(2) C4 0.034(2) 0.059(3) 0.034(3) -0.001(2) -0.003(2) 0.012(2) C5 0.030(2) 0.082(3) 0.031(2) -0.015(2) -0.003(2) 0.010(2) C6 0.026(2) 0.055(3) 0.042(3) -0.015(2) -0.004(2) 0.008(2) C7 0.038(2) 0.073(3) 0.048(3) -0.034(2) -0.013(2) 0.013(2) C8 0.044(3) 0.066(3) 0.086(4) -0.046(3) -0.011(2) 0.001(2) C9 0.046(3) 0.072(3) 0.065(3) -0.041(3) -0.010(2) 0.015(2) C10 0.049(3) 0.114(4) 0.059(3) -0.052(3) -0.015(2) 0.020(3) C11 0.058(3) 0.077(4) 0.046(3) 0.011(3) 0.007(2) 0.008(2) C12 0.106(8) 0.058(6) 0.049(6) 0.009(5) 0.012(5) 0.015(5) C13 0.077(6) 0.082(7) 0.041(5) 0.001(5) 0.006(5) 0.007(5) C14 0.078(6) 0.077(6) 0.039(5) 0.022(5) -0.011(4) 0.026(5) C12X 0.066(7) 0.052(7) 0.063(7) 0.020(6) -0.006(6) 0.010(5) C13X 0.113(10) 0.074(9) 0.079(9) 0.037(7) 0.042(8) 0.023(7) C14X 0.183(15) 0.109(11) 0.033(7) 0.034(7) -0.006(8) 0.017(11) C15 0.024(2) 0.026(2) 0.035(2) -0.006(2) 0.002(2) 0.0010(15) C16 0.020(2) 0.022(2) 0.035(2) -0.006(2) -0.001(2) 0.0009(14) C17 0.024(2) 0.024(2) 0.038(2) -0.006(2) 0.000(2) 0.0014(14) C18 0.023(2) 0.034(2) 0.046(3) -0.006(2) 0.004(2) 0.006(2) C19 0.026(2) 0.036(2) 0.041(2) -0.001(2) 0.002(2) 0.005(2) C20 0.032(2) 0.035(2) 0.036(2) 0.000(2) -0.002(2) 0.003(2) C21 0.024(2) 0.039(2) 0.042(2) -0.004(2) 0.003(2) 0.005(2) C22 0.031(2) 0.048(3) 0.047(3) 0.012(2) 0.009(2) 0.009(2) C23 0.032(2) 0.056(3) 0.041(2) 0.004(2) 0.005(2) 0.008(2) C24 0.034(2) 0.063(3) 0.043(3) -0.015(2) 0.002(2) 0.012(2) C25 0.029(2) 0.057(3) 0.055(3) 0.011(2) 0.002(2) 0.015(2) C29 0.028(2) 0.022(2) 0.031(2) -0.001(2) 0.002(2) 0.0031(14) C30 0.042(2) 0.029(2) 0.037(2) 0.000(2) 0.006(2) -0.006(2) C31 0.050(2) 0.041(2) 0.037(2) -0.004(2) 0.000(2) -0.013(2) C32 0.048(2) 0.034(2) 0.048(3) -0.008(2) 0.004(2) -0.012(2) C33 0.044(2) 0.027(2) 0.048(3) 0.001(2) 0.010(2) -0.003(2) C34 0.034(2) 0.027(2) 0.033(2) -0.008(2) 0.002(2) 0.001(2) P2 0.0211(5) 0.0230(5) 0.0326(6) -0.0008(4) 0.0056(4) -0.0005(4) O3 0.0373(14) 0.0220(13) 0.062(2) -0.0087(13) 0.0279(13) -0.0053(11) O4 0.0253(12) 0.0281(13) 0.0340(15) 0.0025(11) 0.0090(10) 0.0049(10) C35 0.025(2) 0.019(2) 0.034(2) -0.002(2) 0.005(2) -0.0011(14) C36 0.026(2) 0.031(2) 0.046(3) -0.001(2) 0.011(2) 0.003(2) C37 0.028(2) 0.022(2) 0.052(3) -0.003(2) 0.008(2) -0.0009(15) C38 0.031(2) 0.022(2) 0.042(2) -0.008(2) 0.004(2) 0.0001(15) C39 0.023(2) 0.030(2) 0.029(2) -0.004(2) 0.003(2) -0.0013(15) C40 0.020(2) 0.027(2) 0.025(2) 0.001(2) -0.0025(15) -0.0024(14) C41 0.047(2) 0.026(2) 0.091(4) -0.016(2) 0.035(2) -0.013(2) C42 0.056(3) 0.034(3) 0.116(4) -0.020(3) 0.038(3) -0.016(2) C43 0.039(2) 0.042(3) 0.169(5) -0.042(3) 0.040(3) -0.016(2) C44 0.108(4) 0.036(3) 0.107(4) -0.003(3) 0.077(3) -0.021(3) C45 0.031(2) 0.031(2) 0.042(2) -0.004(2) 0.008(2) 0.000(2) C46 0.051(3) 0.053(3) 0.063(3) -0.010(2) 0.031(2) -0.001(2) C47 0.070(3) 0.045(3) 0.040(3) -0.007(2) 0.006(2) -0.002(2) C48 0.044(2) 0.056(3) 0.057(3) -0.002(2) 0.014(2) 0.012(2) C49 0.028(2) 0.019(2) 0.028(2) 0.001(2) 0.007(2) 0.0003(14) C50 0.026(2) 0.019(2) 0.041(2) 0.001(2) 0.005(2) 0.0064(14) C51 0.035(2) 0.020(2) 0.036(2) 0.002(2) 0.005(2) 0.0060(15) C52 0.040(2) 0.025(2) 0.034(2) 0.001(2) 0.000(2) 0.007(2) C53 0.032(2) 0.023(2) 0.034(2) 0.001(2) 0.004(2) 0.0034(15) C54 0.030(2) 0.023(2) 0.035(2) 0.000(2) 0.013(2) -0.0005(15) C55 0.040(2) 0.035(2) 0.030(2) 0.003(2) 0.004(2) 0.009(2) C56 0.047(2) 0.036(2) 0.043(3) 0.008(2) 0.017(2) 0.006(2) C57 0.048(2) 0.043(3) 0.039(2) -0.004(2) 0.009(2) 0.015(2) C58 0.058(3) 0.051(3) 0.035(3) 0.009(2) 0.015(2) 0.018(2) C59 0.033(2) 0.029(2) 0.048(3) 0.004(2) 0.002(2) 0.004(2) C60 0.029(2) 0.058(3) 0.065(3) 0.012(2) 0.001(2) -0.001(2) C61 0.037(3) 0.115(4) 0.057(3) 0.024(3) -0.002(2) 0.001(3) C62 0.027(2) 0.045(3) 0.168(6) -0.021(3) 0.003(3) 0.009(2) C63 0.023(2) 0.025(2) 0.028(2) 0.003(2) 0.004(2) -0.0028(14) C64 0.027(2) 0.029(2) 0.035(2) -0.002(2) 0.003(2) 0.003(2) C65 0.033(2) 0.033(2) 0.052(3) 0.001(2) 0.003(2) -0.013(2) C66 0.069(3) 0.054(3) 0.052(3) 0.017(2) 0.008(2) -0.033(2) C67 0.082(3) 0.066(3) 0.035(3) 0.021(2) -0.005(2) -0.026(3) C68 0.040(2) 0.039(2) 0.042(3) 0.004(2) -0.002(2) -0.012(2) C73 0.074(4) 0.091(5) 0.172(7) 0.020(5) -0.034(4) -0.015(3) C74 0.075(4) 0.081(4) 0.150(6) -0.020(4) 0.005(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.898(2) . ? Co1 O4 1.922(2) . ? Co1 O3 1.955(2) . ? Co1 O10 2.049(3) . ? Co1 P2 2.1416(10) . ? Co1 P1 2.1849(11) . ? P1 C2 1.789(4) . ? P1 C29 1.819(3) . ? P1 C15 1.830(4) . ? O1 C1 1.332(4) . ? O2 C16 1.378(4) . ? C1 C6 1.419(5) . ? C1 C2 1.419(5) . ? C2 C3 1.392(5) . ? C3 C4 1.390(5) . ? C4 C5 1.401(5) . ? C4 C11 1.530(6) . ? C5 C6 1.388(6) . ? C6 C7 1.532(5) . ? C7 C8 1.529(6) . ? C7 C9 1.540(5) . ? C7 C10 1.549(6) . ? C11 C12 1.536(5) . ? C11 C14X 1.537(5) . ? C11 C13X 1.546(5) . ? C11 C13 1.547(5) . ? C11 C14 1.550(4) . ? C11 C12X 1.550(5) . ? C15 C20 1.394(4) . ? C15 C16 1.397(5) . ? C16 C17 1.404(5) . ? C17 C18 1.408(5) . ? C17 C21 1.526(5) . ? C18 C19 1.381(5) . ? C19 C20 1.385(5) . ? C19 C25 1.545(5) . ? C21 C23 1.523(5) . ? C21 C22 1.536(5) . ? C21 C24 1.546(5) . ? C25 C28X 1.518(5) . ? C25 C27 1.519(4) . ? C25 C28 1.528(4) . ? C25 C27X 1.530(5) . ? C25 C26 1.531(4) . ? C25 C26X 1.532(5) . ? C29 C34 1.380(5) . ? C29 C30 1.403(5) . ? C30 C31 1.376(5) . ? C31 C32 1.384(5) . ? C32 C33 1.369(5) . ? C33 C34 1.395(5) . ? P2 C49 1.783(3) . ? P2 C35 1.786(3) . ? P2 C63 1.801(3) . ? O3 C36 1.329(4) . ? O4 C50 1.346(4) . ? C35 C40 1.388(5) . ? C35 C36 1.406(5) . ? C36 C37 1.420(5) . ? C37 C38 1.382(5) . ? C37 C41 1.538(5) . ? C38 C39 1.407(5) . ? C39 C40 1.379(5) . ? C39 C45 1.523(5) . ? C41 C44 1.528(6) . ? C41 C42 1.531(5) . ? C41 C43 1.533(6) . ? C45 C46 1.524(5) . ? C45 C48 1.526(5) . ? C45 C47 1.539(5) . ? C49 C50 1.405(5) . ? C49 C54 1.410(4) . ? C50 C51 1.424(5) . ? C51 C52 1.395(5) . ? C51 C55 1.540(5) . ? C52 C53 1.399(5) . ? C53 C54 1.372(5) . ? C53 C59 1.537(5) . ? C55 C57 1.537(5) . ? C55 C56 1.538(5) . ? C55 C58 1.553(5) . ? C59 C60 1.520(5) . ? C59 C62 1.523(5) . ? C59 C61 1.530(5) . ? C63 C68 1.391(5) . ? C63 C64 1.395(4) . ? C64 C65 1.379(5) . ? C65 C66 1.366(5) . ? C66 C67 1.375(5) . ? C67 C68 1.363(5) . ? O70X C71X 1.458(10) . ? O70X C74 1.468(9) . ? C71X C72X 1.560(10) . ? C72X C73 1.499(14) . ? O70Y C74 1.399(7) . ? O70Y C71Y 1.443(8) . ? C71Y C72Y 1.504(12) . ? C72Y C73 1.499(12) . ? C73 C74 1.542(7) . ? C80 C83 1.02 . ? C80 C81 1.279(10) 2_756 ? C80 C80 1.545(10) 3_757 ? C80 C83 1.982(10) 3_757 ? C80 C82 2.033(9) 2_756 ? C81 C80 1.279(10) 2_746 ? C81 C82 1.39 . ? C82 C83 1.445(10) 4 ? C82 C80 2.033(9) 2_746 ? C83 C82 1.445(10) 4_556 ? C83 C80 1.982(10) 3_757 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O4 178.30(10) . . ? O1 Co1 O3 87.91(11) . . ? O4 Co1 O3 91.32(10) . . ? O1 Co1 O10 93.82(11) . . ? O4 Co1 O10 84.57(11) . . ? O3 Co1 O10 81.83(10) . . ? O1 Co1 P2 93.79(8) . . ? O4 Co1 P2 87.60(7) . . ? O3 Co1 P2 82.07(7) . . ? O10 Co1 P2 161.90(9) . . ? O1 Co1 P1 86.08(8) . . ? O4 Co1 P1 94.63(7) . . ? O3 Co1 P1 173.56(8) . . ? O10 Co1 P1 96.26(8) . . ? P2 Co1 P1 100.62(4) . . ? C2 P1 C29 108.9(2) . . ? C2 P1 C15 108.2(2) . . ? C29 P1 C15 103.5(2) . . ? C2 P1 Co1 99.49(12) . . ? C29 P1 Co1 121.80(11) . . ? C15 P1 Co1 114.35(12) . . ? C1 O1 Co1 120.4(2) . . ? O1 C1 C6 120.4(3) . . ? O1 C1 C2 120.2(3) . . ? C6 C1 C2 119.4(4) . . ? C3 C2 C1 121.3(3) . . ? C3 C2 P1 127.1(3) . . ? C1 C2 P1 111.6(3) . . ? C4 C3 C2 120.8(4) . . ? C3 C4 C5 116.2(4) . . ? C3 C4 C11 122.1(3) . . ? C5 C4 C11 121.7(3) . . ? C6 C5 C4 126.3(4) . . ? C5 C6 C1 115.9(4) . . ? C5 C6 C7 122.2(4) . . ? C1 C6 C7 121.9(4) . . ? C8 C7 C6 109.4(3) . . ? C8 C7 C9 110.1(4) . . ? C6 C7 C9 110.7(3) . . ? C8 C7 C10 108.2(3) . . ? C6 C7 C10 111.5(4) . . ? C9 C7 C10 106.9(4) . . ? C4 C11 C12 115.5(4) . . ? C4 C11 C14X 115.4(6) . . ? C4 C11 C13X 106.1(5) . . ? C14X C11 C13X 110.5(8) . . ? C4 C11 C13 108.1(4) . . ? C12 C11 C13 109.1(5) . . ? C4 C11 C14 109.1(4) . . ? C12 C11 C14 109.6(5) . . ? C13 C11 C14 104.9(5) . . ? C4 C11 C12X 108.5(4) . . ? C14X C11 C12X 112.7(7) . . ? C13X C11 C12X 102.7(6) . . ? C20 C15 C16 118.9(3) . . ? C20 C15 P1 119.2(3) . . ? C16 C15 P1 121.9(2) . . ? O2 C16 C15 122.5(3) . . ? O2 C16 C17 115.6(3) . . ? C15 C16 C17 121.8(3) . . ? C16 C17 C18 115.8(3) . . ? C16 C17 C21 122.0(3) . . ? C18 C17 C21 122.1(3) . . ? C19 C18 C17 124.3(3) . . ? C18 C19 C20 117.3(3) . . ? C18 C19 C25 122.9(3) . . ? C20 C19 C25 119.8(3) . . ? C19 C20 C15 121.9(4) . . ? C23 C21 C17 112.6(3) . . ? C23 C21 C22 107.5(3) . . ? C17 C21 C22 110.6(3) . . ? C23 C21 C24 106.0(3) . . ? C17 C21 C24 109.7(3) . . ? C22 C21 C24 110.4(3) . . ? C27 C25 C28 111.4(4) . . ? C28X C25 C27X 118.4(8) . . ? C27 C25 C26 110.2(4) . . ? C28 C25 C26 105.0(3) . . ? C28X C25 C26X 108.1(9) . . ? C27X C25 C26X 95.8(7) . . ? C28X C25 C19 112.2(6) . . ? C27 C25 C19 110.1(3) . . ? C28 C25 C19 111.9(3) . . ? C27X C25 C19 113.8(4) . . ? C26 C25 C19 108.1(3) . . ? C26X C25 C19 106.5(6) . . ? C34 C29 C30 119.0(3) . . ? C34 C29 P1 120.6(3) . . ? C30 C29 P1 120.3(3) . . ? C31 C30 C29 120.0(4) . . ? C30 C31 C32 120.6(4) . . ? C33 C32 C31 119.8(4) . . ? C32 C33 C34 120.3(4) . . ? C29 C34 C33 120.3(3) . . ? C49 P2 C35 108.8(2) . . ? C49 P2 C63 110.4(2) . . ? C35 P2 C63 106.9(2) . . ? C49 P2 Co1 99.52(12) . . ? C35 P2 Co1 100.46(11) . . ? C63 P2 Co1 129.34(11) . . ? C36 O3 Co1 117.9(2) . . ? C50 O4 Co1 119.0(2) . . ? C40 C35 C36 122.7(3) . . ? C40 C35 P2 127.4(3) . . ? C36 C35 P2 109.8(3) . . ? O3 C36 C35 118.4(3) . . ? O3 C36 C37 123.7(3) . . ? C35 C36 C37 117.9(3) . . ? C38 C37 C36 117.2(3) . . ? C38 C37 C41 122.3(3) . . ? C36 C37 C41 120.4(3) . . ? C37 C38 C39 125.2(3) . . ? C40 C39 C38 116.5(3) . . ? C40 C39 C45 123.6(3) . . ? C38 C39 C45 119.9(3) . . ? C39 C40 C35 120.4(3) . . ? C44 C41 C42 107.9(4) . . ? C44 C41 C43 111.1(4) . . ? C42 C41 C43 106.9(3) . . ? C44 C41 C37 109.8(3) . . ? C42 C41 C37 112.4(3) . . ? C43 C41 C37 108.7(3) . . ? C39 C45 C46 112.1(3) . . ? C39 C45 C48 110.3(3) . . ? C46 C45 C48 109.7(3) . . ? C39 C45 C47 108.6(3) . . ? C46 C45 C47 106.9(3) . . ? C48 C45 C47 109.1(3) . . ? C50 C49 C54 122.1(3) . . ? C50 C49 P2 113.9(2) . . ? C54 C49 P2 123.3(3) . . ? O4 C50 C49 118.9(3) . . ? O4 C50 C51 122.9(3) . . ? C49 C50 C51 118.2(3) . . ? C52 C51 C50 116.7(3) . . ? C52 C51 C55 120.8(3) . . ? C50 C51 C55 122.5(3) . . ? C51 C52 C53 125.8(3) . . ? C54 C53 C52 116.5(3) . . ? C54 C53 C59 119.9(3) . . ? C52 C53 C59 123.4(3) . . ? C53 C54 C49 120.6(3) . . ? C57 C55 C56 110.2(3) . . ? C57 C55 C51 108.5(3) . . ? C56 C55 C51 111.6(3) . . ? C57 C55 C58 107.8(3) . . ? C56 C55 C58 106.8(3) . . ? C51 C55 C58 112.0(3) . . ? C60 C59 C62 108.5(4) . . ? C60 C59 C61 108.2(3) . . ? C62 C59 C61 109.9(4) . . ? C60 C59 C53 109.7(3) . . ? C62 C59 C53 108.8(3) . . ? C61 C59 C53 111.7(3) . . ? C68 C63 C64 118.8(3) . . ? C68 C63 P2 118.0(3) . . ? C64 C63 P2 123.1(3) . . ? C65 C64 C63 120.0(3) . . ? C66 C65 C64 120.2(3) . . ? C65 C66 C67 120.1(4) . . ? C68 C67 C66 120.6(4) . . ? C67 C68 C63 120.2(3) . . ? C71X O70X C74 98.3(10) . . ? O70X C71X C72X 117.2(13) . . ? C73 C72X C71X 95.9(10) . . ? C74 O70Y C71Y 111.2(5) . . ? O70Y C71Y C72Y 107.1(7) . . ? C73 C72Y C71Y 104.3(8) . . ? C72Y C73 C74 104.1(6) . . ? C72X C73 C74 104.4(6) . . ? O70Y C74 C73 106.1(5) . . ? O70X C74 C73 106.4(5) . . ? C83 C80 C81 140.1(5) . 2_756 ? C83 C80 C80 99.2(4) . 3_757 ? C81 C80 C80 102.0(7) 2_756 3_757 ? C83 C80 C83 129.7(3) . 3_757 ? C81 C80 C83 76.5(5) 2_756 3_757 ? C80 C80 C83 30.5(2) 3_757 3_757 ? C83 C80 C82 171.41(14) . 2_756 ? C81 C80 C82 42.6(3) 2_756 2_756 ? C80 C80 C82 72.6(5) 3_757 2_756 ? C83 C80 C82 42.2(3) 3_757 2_756 ? C80 C81 C82 99.0(5) 2_746 . ? C81 C82 C83 95.09(12) . 4 ? C81 C82 C80 38.4(3) . 2_746 ? C83 C82 C80 67.1(2) 4 2_746 ? C80 C83 C82 120.93(8) . 4_556 ? C80 C83 C80 50.3(3) . 3_757 ? C82 C83 C80 70.8(3) 4_556 3_757 ? _refine_diff_density_max 0.962 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.074 #===END data_5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C68 H92 Cl O4 P2 Rh], H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C68 H94 Cl O5 P2 Rh' _chemical_formula_weight 1191.73 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4953(9) _cell_length_b 19.8157(12) _cell_length_c 24.397(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.23(2) _cell_angle_gamma 90.00 _cell_volume 6519.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15479 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped ' _exptl_crystal_colour 'orange yellow ' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method ? _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa-CCD' _diffrn_measurement_method '263 frames a 20 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39050 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.53 _reflns_number_total 14777 _reflns_number_observed 10344 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 21 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0419P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14756 _refine_ls_number_parameters 704 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_obs 0.0378 _refine_ls_wR_factor_all 0.0890 _refine_ls_wR_factor_obs 0.0813 _refine_ls_goodness_of_fit_all 0.963 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 0.972 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh1 Rh 0.557826(12) 0.763294(8) 0.798234(7) 0.01386(5) Uani 1 d . . Cl1 Cl 0.59162(4) 0.83512(3) 0.72339(2) 0.02040(12) Uani 1 d . . P1 P 0.71385(4) 0.75403(3) 0.82398(2) 0.01461(12) Uani 1 d . . P2 P 0.52531(4) 0.66571(3) 0.75063(2) 0.01453(12) Uani 1 d . . O1 O 0.56395(10) 0.84804(7) 0.84672(6) 0.0177(3) Uani 1 d . . O2 O 0.52989(10) 0.71068(7) 0.86640(5) 0.0159(3) Uani 1 d . . O3 O 0.67057(10) 0.70624(7) 0.67070(6) 0.0200(3) Uani 1 d . . H3 H 0.6735(6) 0.7429(5) 0.6880(8) 0.030 Uiso 1 calc R . O4 O 0.39240(11) 0.76872(7) 0.78327(6) 0.0166(3) Uani 1 d . . H4 H 0.3819(17) 0.7805(12) 0.7550(9) 0.022 Uiso 1 d . . C1 C 0.65222(15) 0.87347(10) 0.85962(8) 0.0157(5) Uani 1 d . . C2 C 0.7395(2) 0.83721(10) 0.84961(8) 0.0157(5) Uani 1 d . . C3 C 0.83418(15) 0.86258(10) 0.86221(8) 0.0160(5) Uani 1 d . . H3A H 0.89087(15) 0.83612(10) 0.85492(8) 0.019 Uiso 1 calc R . C4 C 0.8460(2) 0.92615(10) 0.88529(8) 0.0164(5) Uani 1 d . . C5 C 0.7588(2) 0.96154(10) 0.89622(8) 0.0174(5) Uani 1 d . . H5 H 0.7658(2) 1.00477(10) 0.91277(8) 0.021 Uiso 1 calc R . C6 C 0.6632(2) 0.93827(10) 0.88471(8) 0.0161(5) Uani 1 d . . C7 C 0.5707(2) 0.97902(10) 0.89824(9) 0.0214(5) Uani 1 d . . C8 C 0.5121(2) 0.94004(11) 0.94094(9) 0.0280(6) Uani 1 d . . H8A H 0.4948(2) 0.89521(11) 0.92654(9) 0.042 Uiso 1 calc R . H8B H 0.4513(2) 0.96481(11) 0.94860(9) 0.042 Uiso 1 calc R . H8C H 0.5528(2) 0.93528(11) 0.97486(9) 0.042 Uiso 1 calc R . C9 C 0.5041(2) 0.98931(11) 0.84625(10) 0.0289(6) Uani 1 d . . H9A H 0.4858(2) 0.94529(11) 0.83059(10) 0.043 Uiso 1 calc R . H9B H 0.5401(2) 1.01545(11) 0.81934(10) 0.043 Uiso 1 calc R . H9C H 0.4440(2) 1.01374(11) 0.85571(10) 0.043 Uiso 1 calc R . C10 C 0.5973(2) 1.04897(11) 0.92118(10) 0.0295(6) Uani 1 d . . H10A H 0.5364(2) 1.07334(11) 0.92929(10) 0.044 Uiso 1 calc R . H10B H 0.6339(2) 1.07428(11) 0.89404(10) 0.044 Uiso 1 calc R . H10C H 0.6385(2) 1.04402(11) 0.95490(10) 0.044 Uiso 1 calc R . C11 C 0.9512(2) 0.95373(11) 0.89759(9) 0.0203(5) Uani 1 d . . C12 C 1.0056(2) 0.90656(11) 0.93878(9) 0.0254(5) Uani 1 d . . H12A H 1.0079(2) 0.86089(11) 0.92346(9) 0.038 Uiso 1 calc R . H12B H 0.9703(2) 0.90568(11) 0.97312(9) 0.038 Uiso 1 calc R . H12C H 1.0734(2) 0.92306(11) 0.94600(9) 0.038 Uiso 1 calc R . C13 C 0.9488(2) 1.02450(11) 0.92264(10) 0.0254(5) Uani 1 d . . H13A H 0.9116(2) 1.02337(11) 0.95633(10) 0.038 Uiso 1 calc R . H13B H 0.9166(2) 1.05573(11) 0.89640(10) 0.038 Uiso 1 calc R . H13C H 1.0167(2) 1.03971(11) 0.93123(10) 0.038 Uiso 1 calc R . C14 C 1.0097(2) 0.95657(11) 0.84495(9) 0.0243(5) Uani 1 d . . H14A H 1.0118(2) 0.91150(11) 0.82848(9) 0.037 Uiso 1 calc R . H14B H 1.0774(2) 0.97200(11) 0.85378(9) 0.037 Uiso 1 calc R . H14C H 0.9772(2) 0.98801(11) 0.81895(9) 0.037 Uiso 1 calc R . C15 C 0.70479(15) 0.69471(10) 0.87877(8) 0.0153(5) Uani 1 d . . C16 C 0.60771(15) 0.68683(10) 0.89586(9) 0.0157(5) Uani 1 d . . C17 C 0.5915(2) 0.65068(10) 0.94580(9) 0.0184(5) Uani 1 d . . C18 C 0.6732(2) 0.61698(10) 0.96884(9) 0.0214(5) Uani 1 d . . H18 H 0.6635(2) 0.59104(10) 1.00094(9) 0.026 Uiso 1 calc R . C19 C 0.7688(2) 0.61825(11) 0.94846(9) 0.0214(5) Uani 1 d . . C20 C 0.7851(2) 0.66034(10) 0.90479(9) 0.0191(5) Uani 1 d . . H20 H 0.8503(2) 0.66619(10) 0.89223(9) 0.023 Uiso 1 calc R . C21 C 0.4900(2) 0.64965(11) 0.97147(9) 0.0231(5) Uani 1 d . . C22 C 0.4557(2) 0.72292(12) 0.98105(10) 0.0327(6) Uani 1 d . . H22A H 0.3907(2) 0.72255(12) 0.99751(10) 0.049 Uiso 1 calc R . H22B H 0.4510(2) 0.74691(12) 0.94592(10) 0.049 Uiso 1 calc R . H22C H 0.5038(2) 0.74580(12) 1.00580(10) 0.049 Uiso 1 calc R . C23 C 0.4923(2) 0.61360(13) 1.02733(9) 0.0343(6) Uani 1 d . . H23A H 0.4259(2) 0.61421(13) 1.04214(9) 0.051 Uiso 1 calc R . H23B H 0.5388(2) 0.63685(13) 1.05277(9) 0.051 Uiso 1 calc R . H23C H 0.5138(2) 0.56677(13) 1.02269(9) 0.051 Uiso 1 calc R . C24 C 0.4130(2) 0.61290(12) 0.93400(10) 0.0298(6) Uani 1 d . . H24A H 0.3486(2) 0.61289(12) 0.95130(10) 0.045 Uiso 1 calc R . H24B H 0.4345(2) 0.56627(12) 0.92829(10) 0.045 Uiso 1 calc R . H24C H 0.4068(2) 0.63614(12) 0.89858(10) 0.045 Uiso 1 calc R . C25 C 0.8506(2) 0.57348(11) 0.97476(10) 0.0261(5) Uani 1 d . . C26 C 0.9431(2) 0.57306(13) 0.94066(10) 0.0348(6) Uani 1 d . . H26A H 0.9258(2) 0.55655(13) 0.90365(10) 0.052 Uiso 1 calc R . H26B H 0.9932(2) 0.54340(13) 0.95801(10) 0.052 Uiso 1 calc R . H26C H 0.9696(2) 0.61898(13) 0.93843(10) 0.052 Uiso 1 calc R . C27 C 0.8775(2) 0.59930(12) 1.03265(9) 0.0305(6) Uani 1 d . . H27A H 0.8181(2) 0.59956(12) 1.05452(9) 0.046 Uiso 1 calc R . H27B H 0.9041(2) 0.64522(12) 1.03044(9) 0.046 Uiso 1 calc R . H27C H 0.9277(2) 0.56964(12) 1.05002(9) 0.046 Uiso 1 calc R . C28 C 0.8117(2) 0.50062(11) 0.97813(12) 0.0418(7) Uani 1 d . . H28A H 0.7522(2) 0.49975(11) 0.99990(12) 0.063 Uiso 1 calc R . H28B H 0.8629(2) 0.47183(11) 0.99556(12) 0.063 Uiso 1 calc R . H28C H 0.7953(2) 0.48388(11) 0.94108(12) 0.063 Uiso 1 calc R . C29 C 0.80959(14) 0.73115(10) 0.77786(9) 0.0175(5) Uani 1 d . . C30 C 0.8472(2) 0.78053(12) 0.74315(9) 0.0239(5) Uani 1 d . . H30 H 0.8268(2) 0.82619(12) 0.74648(9) 0.029 Uiso 1 calc R . C31 C 0.9139(2) 0.76269(14) 0.70406(10) 0.0351(6) Uani 1 d . . H31 H 0.9389(2) 0.79609(14) 0.68034(10) 0.042 Uiso 1 calc R . C32 C 0.9442(2) 0.6966(2) 0.69941(11) 0.0413(7) Uani 1 d . . H32 H 0.9900(2) 0.6846(2) 0.67247(11) 0.050 Uiso 1 calc R . C33 C 0.9082(2) 0.64787(13) 0.73379(11) 0.0360(7) Uani 1 d . . H33 H 0.9300(2) 0.60251(13) 0.73060(11) 0.043 Uiso 1 calc R . C34 C 0.8406(2) 0.66437(11) 0.77286(9) 0.0241(5) Uani 1 d . . H34 H 0.8156(2) 0.63047(11) 0.79612(9) 0.029 Uiso 1 calc R . C35 C 0.5025(2) 0.67346(10) 0.67639(8) 0.0152(4) Uani 1 d . . C36 C 0.57730(15) 0.69941(10) 0.64510(9) 0.0158(5) Uani 1 d . . C37 C 0.5617(2) 0.71596(10) 0.58985(9) 0.0166(5) Uani 1 d . . C38 C 0.4653(2) 0.70519(10) 0.56753(9) 0.0179(5) Uani 1 d . . H38 H 0.4520(2) 0.71691(10) 0.53021(9) 0.022 Uiso 1 calc R . C39 C 0.3879(2) 0.67824(10) 0.59711(9) 0.0178(5) Uani 1 d . . C40 C 0.4082(2) 0.66225(10) 0.65226(9) 0.0178(5) Uani 1 d . . H40 H 0.3575(2) 0.64360(10) 0.67353(9) 0.021 Uiso 1 calc R . C41 C 0.6458(2) 0.74349(10) 0.55537(9) 0.0201(5) Uani 1 d . . C42 C 0.6093(2) 0.76161(12) 0.49704(9) 0.0287(6) Uani 1 d . . H42A H 0.5584(2) 0.79680(12) 0.49852(9) 0.043 Uiso 1 calc R . H42B H 0.5810(2) 0.72145(12) 0.47898(9) 0.043 Uiso 1 calc R . H42C H 0.6651(2) 0.77819(12) 0.47628(9) 0.043 Uiso 1 calc R . C43 C 0.6912(2) 0.80805(11) 0.58091(9) 0.0267(5) Uani 1 d . . H43A H 0.7157(2) 0.79857(11) 0.61848(9) 0.040 Uiso 1 calc R . H43B H 0.6406(2) 0.84345(11) 0.58147(9) 0.040 Uiso 1 calc R . H43C H 0.7464(2) 0.82320(11) 0.55903(9) 0.040 Uiso 1 calc R . C44 C 0.7252(2) 0.68832(11) 0.55153(10) 0.0292(6) Uani 1 d . . H44A H 0.7497(2) 0.67591(11) 0.58851(10) 0.044 Uiso 1 calc R . H44B H 0.7804(2) 0.70529(11) 0.53047(10) 0.044 Uiso 1 calc R . H44C H 0.6963(2) 0.64856(11) 0.53317(10) 0.044 Uiso 1 calc R . C45 C 0.2822(2) 0.66706(11) 0.57202(9) 0.0226(5) Uani 1 d . . C46 C 0.2716(2) 0.69064(12) 0.51237(9) 0.0300(6) Uani 1 d . . H46A H 0.3192(2) 0.66639(12) 0.49031(9) 0.045 Uiso 1 calc R . H46B H 0.2846(2) 0.73922(12) 0.51052(9) 0.045 Uiso 1 calc R . H46C H 0.2041(2) 0.68141(12) 0.49807(9) 0.045 Uiso 1 calc R . C47 C 0.2582(2) 0.59127(12) 0.57313(11) 0.0390(7) Uani 1 d . . H47A H 0.3063(2) 0.56663(12) 0.55166(11) 0.058 Uiso 1 calc R . H47B H 0.1913(2) 0.58375(12) 0.55731(11) 0.058 Uiso 1 calc R . H47C H 0.2618(2) 0.57511(12) 0.61112(11) 0.058 Uiso 1 calc R . C48 C 0.2073(2) 0.7056(2) 0.60548(10) 0.0434(7) Uani 1 d . . H48A H 0.2132(2) 0.6910(2) 0.64387(10) 0.065 Uiso 1 calc R . H48B H 0.1401(2) 0.6963(2) 0.59080(10) 0.065 Uiso 1 calc R . H48C H 0.2207(2) 0.7541(2) 0.60325(10) 0.065 Uiso 1 calc R . C49 C 0.40189(14) 0.64901(10) 0.77450(8) 0.0141(4) Uani 1 d . . C50 C 0.34586(15) 0.70528(10) 0.78801(8) 0.0148(4) Uani 1 d . . C51 C 0.24979(15) 0.70006(10) 0.80647(8) 0.0156(5) Uani 1 d . . C52 C 0.21282(15) 0.63433(10) 0.81083(8) 0.0188(5) Uani 1 d . . H52 H 0.14774(15) 0.62883(10) 0.82365(8) 0.023 Uiso 1 calc R . C53 C 0.2656(2) 0.57639(10) 0.79753(9) 0.0179(5) Uani 1 d . . C54 C 0.36112(15) 0.58483(10) 0.77884(8) 0.0172(5) Uani 1 d . . H54 H 0.39868(15) 0.54645(10) 0.76898(8) 0.021 Uiso 1 calc R . C55 C 0.1866(2) 0.76191(10) 0.82029(9) 0.0194(5) Uani 1 d . . C56 C 0.1651(2) 0.80256(11) 0.76739(10) 0.0285(6) Uani 1 d . . H56A H 0.2278(2) 0.81685(11) 0.75206(10) 0.043 Uiso 1 calc R . H56B H 0.1255(2) 0.84242(11) 0.77578(10) 0.043 Uiso 1 calc R . H56C H 0.1283(2) 0.77430(11) 0.74064(10) 0.043 Uiso 1 calc R . C57 C 0.2409(2) 0.80579(11) 0.86389(10) 0.0282(6) Uani 1 d . . H57A H 0.3053(2) 0.81972(11) 0.85049(10) 0.042 Uiso 1 calc R . H57B H 0.2510(2) 0.77975(11) 0.89780(10) 0.042 Uiso 1 calc R . H57C H 0.2010(2) 0.84588(11) 0.87118(10) 0.042 Uiso 1 calc R . C58 C 0.0863(2) 0.74094(11) 0.84240(9) 0.0228(5) Uani 1 d . . H58A H 0.0505(2) 0.71287(11) 0.81512(9) 0.034 Uiso 1 calc R . H58B H 0.0471(2) 0.78134(11) 0.84978(9) 0.034 Uiso 1 calc R . H58C H 0.0972(2) 0.71522(11) 0.87641(9) 0.034 Uiso 1 calc R . C59 C 0.2224(2) 0.50485(10) 0.80214(9) 0.0217(5) Uani 1 d . . C60 C 0.2909(2) 0.46172(11) 0.83974(10) 0.0317(6) Uani 1 d . . H60A H 0.2950(2) 0.48171(11) 0.87650(10) 0.048 Uiso 1 calc R . H60B H 0.3572(2) 0.46007(11) 0.82480(10) 0.048 Uiso 1 calc R . H60C H 0.2641(2) 0.41587(11) 0.84190(10) 0.048 Uiso 1 calc R . C61 C 0.2161(2) 0.47368(12) 0.74502(10) 0.0332(6) Uani 1 d . . H61A H 0.2822(2) 0.47308(12) 0.72974(10) 0.050 Uiso 1 calc R . H61B H 0.1711(2) 0.50049(12) 0.72122(10) 0.050 Uiso 1 calc R . H61C H 0.1909(2) 0.42742(12) 0.74735(10) 0.050 Uiso 1 calc R . C62 C 0.1188(2) 0.50553(12) 0.82561(13) 0.0431(7) Uani 1 d . . H62A H 0.1223(2) 0.52553(12) 0.86238(13) 0.065 Uiso 1 calc R . H62B H 0.0938(2) 0.45922(12) 0.82780(13) 0.065 Uiso 1 calc R . H62C H 0.0739(2) 0.53229(12) 0.80168(13) 0.065 Uiso 1 calc R . C63 C 0.59766(15) 0.59004(10) 0.76588(8) 0.0159(5) Uani 1 d . . C64 C 0.5895(2) 0.56003(10) 0.81746(9) 0.0191(5) Uani 1 d . . H64 H 0.5443(2) 0.57783(10) 0.84263(9) 0.023 Uiso 1 calc R . C65 C 0.6469(2) 0.50456(11) 0.83189(10) 0.0244(5) Uani 1 d . . H65 H 0.6415(2) 0.48465(11) 0.86706(10) 0.029 Uiso 1 calc R . C66 C 0.7129(2) 0.47769(11) 0.79506(9) 0.0247(5) Uani 1 d . . H66 H 0.7521(2) 0.43948(11) 0.80502(9) 0.030 Uiso 1 calc R . C67 C 0.7208(2) 0.50673(11) 0.74436(9) 0.0228(5) Uani 1 d . . H67 H 0.7655(2) 0.48826(11) 0.71927(9) 0.027 Uiso 1 calc R . C68 C 0.6641(2) 0.56284(10) 0.72921(9) 0.0195(5) Uani 1 d . . H68 H 0.6706(2) 0.58263(10) 0.69406(9) 0.023 Uiso 1 calc R . O5 O 0.37477(12) 0.81948(8) 0.68210(7) 0.0262(4) Uani 1 d D . H5A H 0.4364(12) 0.8294(12) 0.6840(10) 0.039 Uiso 1 d D . H5B H 0.3653(19) 0.7929(11) 0.6550(8) 0.039 Uiso 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01174(8) 0.01183(8) 0.01789(10) -0.00086(7) -0.00086(6) -0.00049(7) Cl1 0.0214(3) 0.0165(3) 0.0233(3) 0.0020(2) 0.0002(2) -0.0030(2) P1 0.0110(3) 0.0140(3) 0.0187(3) -0.0027(2) -0.0009(2) 0.0000(2) P2 0.0122(3) 0.0132(3) 0.0181(3) -0.0002(2) -0.0004(2) -0.0002(2) O1 0.0147(8) 0.0145(7) 0.0238(8) -0.0037(6) -0.0024(6) 0.0006(6) O2 0.0139(7) 0.0154(7) 0.0184(8) 0.0014(6) -0.0010(6) 0.0015(6) O3 0.0167(8) 0.0221(8) 0.0210(9) -0.0016(7) -0.0033(6) -0.0041(7) O4 0.0150(7) 0.0139(8) 0.0205(8) 0.0034(7) -0.0028(7) -0.0017(6) C1 0.0156(11) 0.0161(11) 0.0152(11) 0.0006(9) -0.0007(9) -0.0010(9) C2 0.0197(11) 0.0112(10) 0.0162(11) -0.0006(9) -0.0006(9) -0.0024(9) C3 0.0145(11) 0.0142(10) 0.0192(12) 0.0005(9) -0.0015(9) 0.0023(9) C4 0.0172(11) 0.0157(11) 0.0161(11) 0.0003(9) -0.0015(9) -0.0016(9) C5 0.0211(12) 0.0122(10) 0.0187(12) -0.0024(9) -0.0011(9) -0.0013(9) C6 0.0163(11) 0.0146(10) 0.0173(12) 0.0003(9) 0.0004(9) 0.0011(9) C7 0.0188(12) 0.0149(11) 0.0306(13) -0.0057(10) 0.0013(10) -0.0003(9) C8 0.0249(13) 0.0275(13) 0.0321(14) -0.0099(11) 0.0082(11) -0.0022(10) C9 0.0229(13) 0.0196(12) 0.044(2) 0.0020(11) -0.0044(11) 0.0040(10) C10 0.0213(13) 0.0192(12) 0.048(2) -0.0100(12) 0.0022(11) 0.0020(10) C11 0.0171(11) 0.0179(11) 0.0255(13) -0.0020(10) -0.0050(10) -0.0006(9) C12 0.0245(13) 0.0209(12) 0.0301(14) -0.0018(10) -0.0069(11) -0.0020(10) C13 0.0203(12) 0.0212(12) 0.0343(14) -0.0047(11) -0.0038(11) -0.0043(10) C14 0.0192(12) 0.0219(12) 0.0316(14) 0.0003(11) -0.0020(10) -0.0026(10) C15 0.0151(11) 0.0106(10) 0.0201(12) -0.0029(9) -0.0009(9) -0.0006(8) C16 0.0168(11) 0.0102(10) 0.0200(12) -0.0044(9) -0.0010(9) 0.0010(9) C17 0.0186(11) 0.0142(11) 0.0225(12) -0.0014(10) -0.0001(9) 0.0005(9) C18 0.0258(13) 0.0183(12) 0.0199(12) 0.0032(10) -0.0016(10) -0.0001(10) C19 0.0212(12) 0.0176(11) 0.0248(13) -0.0004(10) -0.0060(10) 0.0038(9) C20 0.0139(11) 0.0169(11) 0.0262(13) -0.0043(10) -0.0025(9) -0.0010(9) C21 0.0205(12) 0.0279(13) 0.0210(12) 0.0021(10) 0.0030(10) 0.0034(10) C22 0.0308(14) 0.0363(15) 0.0318(14) -0.0007(12) 0.0101(12) 0.0082(12) C23 0.0299(14) 0.044(2) 0.0294(14) 0.0115(12) 0.0079(11) 0.0039(12) C24 0.0204(13) 0.0369(14) 0.0321(14) 0.0076(12) 0.0030(11) -0.0068(11) C25 0.0226(13) 0.0226(12) 0.0325(14) 0.0039(11) -0.0064(11) 0.0056(10) C26 0.0257(14) 0.0382(15) 0.040(2) 0.0048(13) -0.0048(12) 0.0169(12) C27 0.0262(14) 0.0317(14) 0.0330(15) 0.0081(12) -0.0074(11) 0.0036(11) C28 0.035(2) 0.0230(13) 0.066(2) 0.0046(13) -0.0199(14) 0.0064(12) C29 0.0076(10) 0.0235(12) 0.0214(12) -0.0066(10) -0.0007(9) -0.0013(9) C30 0.0168(11) 0.0318(14) 0.0231(13) -0.0047(11) -0.0015(10) -0.0055(10) C31 0.0224(13) 0.057(2) 0.0259(14) -0.0070(13) 0.0022(11) -0.0139(13) C32 0.0208(13) 0.067(2) 0.036(2) -0.028(2) 0.0060(12) -0.0022(14) C33 0.0198(13) 0.040(2) 0.048(2) -0.0233(14) -0.0021(12) 0.0046(12) C34 0.0150(11) 0.0255(12) 0.0314(14) -0.0118(11) -0.0038(10) 0.0006(10) C35 0.0178(11) 0.0106(10) 0.0173(11) -0.0013(9) -0.0006(9) 0.0003(9) C36 0.0146(11) 0.0099(10) 0.0228(12) -0.0024(9) -0.0018(9) 0.0020(8) C37 0.0173(11) 0.0126(10) 0.0199(12) -0.0024(9) 0.0017(9) 0.0018(9) C38 0.0201(12) 0.0146(11) 0.0189(12) 0.0013(9) -0.0016(9) 0.0027(9) C39 0.0164(11) 0.0161(11) 0.0206(12) -0.0041(9) -0.0017(9) 0.0027(9) C40 0.0161(11) 0.0139(11) 0.0237(12) -0.0025(10) 0.0026(9) -0.0014(9) C41 0.0197(11) 0.0202(11) 0.0206(12) 0.0013(10) 0.0024(9) -0.0017(9) C42 0.0285(13) 0.0325(13) 0.0251(13) 0.0041(11) 0.0026(11) -0.0074(11) C43 0.0303(14) 0.0224(12) 0.0279(14) 0.0023(11) 0.0057(11) -0.0072(11) C44 0.0265(13) 0.0267(13) 0.0355(14) 0.0027(11) 0.0141(11) 0.0037(11) C45 0.0150(11) 0.0276(13) 0.0249(13) -0.0004(10) -0.0030(10) -0.0012(10) C46 0.0239(13) 0.0380(15) 0.0271(14) 0.0023(12) -0.0091(11) 0.0003(11) C47 0.0264(14) 0.038(2) 0.051(2) 0.0107(14) -0.0169(13) -0.0144(12) C48 0.0170(13) 0.076(2) 0.037(2) -0.0092(15) -0.0044(12) 0.0103(13) C49 0.0114(10) 0.0165(11) 0.0144(11) 0.0014(9) -0.0005(8) 0.0001(8) C50 0.0150(11) 0.0145(10) 0.0147(11) 0.0011(9) -0.0038(9) -0.0027(9) C51 0.0136(11) 0.0174(11) 0.0154(11) -0.0017(9) -0.0038(9) -0.0004(9) C52 0.0115(11) 0.0232(12) 0.0217(12) 0.0004(10) 0.0014(9) -0.0009(9) C53 0.0162(11) 0.0156(11) 0.0216(12) -0.0012(9) -0.0009(9) -0.0028(9) C54 0.0171(11) 0.0152(11) 0.0191(12) -0.0005(9) -0.0008(9) 0.0006(9) C55 0.0147(11) 0.0180(11) 0.0255(12) -0.0024(10) 0.0007(9) 0.0019(9) C56 0.0190(12) 0.0250(13) 0.042(2) 0.0051(11) 0.0026(11) 0.0080(10) C57 0.0216(13) 0.0255(13) 0.0377(15) -0.0114(11) 0.0036(11) 0.0011(10) C58 0.0164(11) 0.0221(12) 0.0300(13) -0.0061(11) 0.0021(10) 0.0014(10) C59 0.0167(12) 0.0168(11) 0.0317(14) 0.0006(10) 0.0025(10) -0.0033(9) C60 0.0331(14) 0.0230(13) 0.039(2) 0.0100(12) -0.0029(12) -0.0063(11) C61 0.0362(15) 0.0208(12) 0.042(2) -0.0024(12) -0.0040(12) -0.0098(11) C62 0.0302(15) 0.0199(13) 0.081(2) 0.0029(14) 0.0213(15) -0.0080(11) C63 0.0143(11) 0.0133(10) 0.0197(12) -0.0036(9) -0.0047(9) -0.0013(9) C64 0.0172(11) 0.0178(11) 0.0221(12) -0.0061(10) -0.0016(9) -0.0021(9) C65 0.0292(13) 0.0196(12) 0.0239(13) 0.0019(10) -0.0045(10) 0.0017(10) C66 0.0237(13) 0.0179(12) 0.0321(14) -0.0034(11) -0.0062(11) 0.0068(10) C67 0.0180(12) 0.0211(12) 0.0291(14) -0.0082(10) -0.0031(10) 0.0039(9) C68 0.0175(11) 0.0199(11) 0.0208(12) -0.0021(10) -0.0029(9) -0.0016(9) O5 0.0263(9) 0.0221(9) 0.0297(10) 0.0007(7) -0.0046(8) 0.0014(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O2 2.0108(14) . ? Rh1 O1 2.0540(13) . ? Rh1 P1 2.1814(6) . ? Rh1 O4 2.2506(14) . ? Rh1 P2 2.2893(6) . ? Rh1 Cl1 2.3733(6) . ? P1 C15 1.788(2) . ? P1 C2 1.792(2) . ? P1 C29 1.804(2) . ? P2 C49 1.816(2) . ? P2 C63 1.820(2) . ? P2 C35 1.832(2) . ? O1 C1 1.320(2) . ? O2 C16 1.336(2) . ? O3 C36 1.390(2) . ? O4 C50 1.412(2) . ? C1 C2 1.409(3) . ? C1 C6 1.428(3) . ? C2 C3 1.396(3) . ? C3 C4 1.386(3) . ? C4 C5 1.404(3) . ? C4 C11 1.540(3) . ? C5 C6 1.389(3) . ? C6 C7 1.533(3) . ? C7 C10 1.532(3) . ? C7 C9 1.539(3) . ? C7 C8 1.540(3) . ? C11 C13 1.531(3) . ? C11 C14 1.535(3) . ? C11 C12 1.538(3) . ? C15 C16 1.399(3) . ? C15 C20 1.410(3) . ? C16 C17 1.437(3) . ? C17 C18 1.389(3) . ? C17 C21 1.528(3) . ? C18 C19 1.401(3) . ? C19 C20 1.377(3) . ? C19 C25 1.537(3) . ? C21 C23 1.538(3) . ? C21 C24 1.540(3) . ? C21 C22 1.544(3) . ? C25 C26 1.527(3) . ? C25 C27 1.533(3) . ? C25 C28 1.539(3) . ? C29 C34 1.395(3) . ? C29 C30 1.402(3) . ? C30 C31 1.383(3) . ? C31 C32 1.378(4) . ? C32 C33 1.380(4) . ? C33 C34 1.383(3) . ? C35 C36 1.388(3) . ? C35 C40 1.398(3) . ? C36 C37 1.395(3) . ? C37 C38 1.407(3) . ? C37 C41 1.539(3) . ? C38 C39 1.398(3) . ? C39 C40 1.399(3) . ? C39 C45 1.546(3) . ? C41 C42 1.531(3) . ? C41 C44 1.537(3) . ? C41 C43 1.540(3) . ? C45 C48 1.528(3) . ? C45 C46 1.530(3) . ? C45 C47 1.537(3) . ? C49 C54 1.391(3) . ? C49 C50 1.394(3) . ? C50 C51 1.393(3) . ? C51 C52 1.400(3) . ? C51 C55 1.538(3) . ? C52 C53 1.396(3) . ? C53 C54 1.394(3) . ? C53 C59 1.538(3) . ? C55 C58 1.534(3) . ? C55 C57 1.537(3) . ? C55 C56 1.539(3) . ? C59 C61 1.524(3) . ? C59 C62 1.532(3) . ? C59 C60 1.536(3) . ? C63 C68 1.399(3) . ? C63 C64 1.400(3) . ? C64 C65 1.383(3) . ? C65 C66 1.394(3) . ? C66 C67 1.372(3) . ? C67 C68 1.391(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Rh1 O1 87.27(5) . . ? O2 Rh1 P1 85.88(4) . . ? O1 Rh1 P1 83.47(4) . . ? O2 Rh1 O4 86.69(6) . . ? O1 Rh1 O4 94.12(5) . . ? P1 Rh1 O4 172.29(4) . . ? O2 Rh1 P2 86.74(4) . . ? O1 Rh1 P2 170.20(4) . . ? P1 Rh1 P2 103.82(2) . . ? O4 Rh1 P2 77.80(4) . . ? O2 Rh1 Cl1 174.29(4) . . ? O1 Rh1 Cl1 87.03(4) . . ? P1 Rh1 Cl1 93.42(2) . . ? O4 Rh1 Cl1 93.76(4) . . ? P2 Rh1 Cl1 98.92(2) . . ? C15 P1 C2 111.20(9) . . ? C15 P1 C29 111.87(10) . . ? C2 P1 C29 108.40(10) . . ? C15 P1 Rh1 100.21(7) . . ? C2 P1 Rh1 101.20(7) . . ? C29 P1 Rh1 123.25(7) . . ? C49 P2 C63 106.00(9) . . ? C49 P2 C35 102.20(10) . . ? C63 P2 C35 109.85(9) . . ? C49 P2 Rh1 98.70(7) . . ? C63 P2 Rh1 120.09(7) . . ? C35 P2 Rh1 116.90(6) . . ? C1 O1 Rh1 117.72(13) . . ? C16 O2 Rh1 117.36(13) . . ? C50 O4 Rh1 112.69(11) . . ? O1 C1 C2 121.1(2) . . ? O1 C1 C6 121.5(2) . . ? C2 C1 C6 117.4(2) . . ? C3 C2 C1 122.8(2) . . ? C3 C2 P1 124.8(2) . . ? C1 C2 P1 112.23(15) . . ? C4 C3 C2 120.4(2) . . ? C3 C4 C5 116.6(2) . . ? C3 C4 C11 119.5(2) . . ? C5 C4 C11 124.0(2) . . ? C6 C5 C4 125.1(2) . . ? C5 C6 C1 117.7(2) . . ? C5 C6 C7 122.7(2) . . ? C1 C6 C7 119.6(2) . . ? C10 C7 C6 112.0(2) . . ? C10 C7 C9 107.6(2) . . ? C6 C7 C9 110.3(2) . . ? C10 C7 C8 109.0(2) . . ? C6 C7 C8 109.0(2) . . ? C9 C7 C8 109.0(2) . . ? C13 C11 C14 108.7(2) . . ? C13 C11 C12 108.2(2) . . ? C14 C11 C12 108.7(2) . . ? C13 C11 C4 111.7(2) . . ? C14 C11 C4 110.5(2) . . ? C12 C11 C4 109.0(2) . . ? C16 C15 C20 121.6(2) . . ? C16 C15 P1 112.85(15) . . ? C20 C15 P1 125.5(2) . . ? O2 C16 C15 121.7(2) . . ? O2 C16 C17 119.3(2) . . ? C15 C16 C17 118.9(2) . . ? C18 C17 C16 116.0(2) . . ? C18 C17 C21 122.5(2) . . ? C16 C17 C21 121.5(2) . . ? C17 C18 C19 125.1(2) . . ? C20 C19 C18 117.5(2) . . ? C20 C19 C25 122.6(2) . . ? C18 C19 C25 119.8(2) . . ? C19 C20 C15 119.9(2) . . ? C17 C21 C23 112.4(2) . . ? C17 C21 C24 111.0(2) . . ? C23 C21 C24 107.2(2) . . ? C17 C21 C22 109.1(2) . . ? C23 C21 C22 107.4(2) . . ? C24 C21 C22 109.6(2) . . ? C26 C25 C27 109.5(2) . . ? C26 C25 C19 111.4(2) . . ? C27 C25 C19 109.5(2) . . ? C26 C25 C28 108.1(2) . . ? C27 C25 C28 109.5(2) . . ? C19 C25 C28 108.9(2) . . ? C34 C29 C30 119.5(2) . . ? C34 C29 P1 121.2(2) . . ? C30 C29 P1 119.1(2) . . ? C31 C30 C29 119.9(2) . . ? C32 C31 C30 120.2(2) . . ? C31 C32 C33 120.2(2) . . ? C32 C33 C34 120.7(2) . . ? C33 C34 C29 119.5(2) . . ? C36 C35 C40 119.8(2) . . ? C36 C35 P2 118.5(2) . . ? C40 C35 P2 121.2(2) . . ? C35 C36 O3 117.0(2) . . ? C35 C36 C37 122.2(2) . . ? O3 C36 C37 120.7(2) . . ? C36 C37 C38 116.1(2) . . ? C36 C37 C41 121.7(2) . . ? C38 C37 C41 122.2(2) . . ? C39 C38 C37 123.8(2) . . ? C38 C39 C40 117.4(2) . . ? C38 C39 C45 123.1(2) . . ? C40 C39 C45 119.4(2) . . ? C35 C40 C39 120.7(2) . . ? C42 C41 C44 108.1(2) . . ? C42 C41 C37 112.0(2) . . ? C44 C41 C37 108.2(2) . . ? C42 C41 C43 106.9(2) . . ? C44 C41 C43 110.4(2) . . ? C37 C41 C43 111.3(2) . . ? C48 C45 C46 108.4(2) . . ? C48 C45 C47 109.5(2) . . ? C46 C45 C47 107.6(2) . . ? C48 C45 C39 109.6(2) . . ? C46 C45 C39 112.6(2) . . ? C47 C45 C39 109.0(2) . . ? C54 C49 C50 119.6(2) . . ? C54 C49 P2 124.1(2) . . ? C50 C49 P2 116.3(2) . . ? C51 C50 C49 122.5(2) . . ? C51 C50 O4 121.0(2) . . ? C49 C50 O4 116.5(2) . . ? C50 C51 C52 115.6(2) . . ? C50 C51 C55 122.9(2) . . ? C52 C51 C55 121.5(2) . . ? C53 C52 C51 124.1(2) . . ? C54 C53 C52 117.6(2) . . ? C54 C53 C59 119.5(2) . . ? C52 C53 C59 122.9(2) . . ? C49 C54 C53 120.5(2) . . ? C58 C55 C57 108.2(2) . . ? C58 C55 C51 111.4(2) . . ? C57 C55 C51 110.4(2) . . ? C58 C55 C56 107.2(2) . . ? C57 C55 C56 110.7(2) . . ? C51 C55 C56 108.7(2) . . ? C61 C59 C62 109.0(2) . . ? C61 C59 C60 109.4(2) . . ? C62 C59 C60 108.6(2) . . ? C61 C59 C53 108.3(2) . . ? C62 C59 C53 111.9(2) . . ? C60 C59 C53 109.6(2) . . ? C68 C63 C64 119.1(2) . . ? C68 C63 P2 122.6(2) . . ? C64 C63 P2 118.3(2) . . ? C65 C64 C63 120.2(2) . . ? C64 C65 C66 120.3(2) . . ? C67 C66 C65 119.6(2) . . ? C66 C67 C68 120.9(2) . . ? C67 C68 C63 119.8(2) . . ? _refine_diff_density_max 0.628 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.072 #===END data_7 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C74 H108 Co2 O9 P2], 2 EtOH, 0.5 H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C78 H121 Co2 O11.50 P2' _chemical_formula_weight 1422.55 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.036(2) _cell_length_b 16.294(3) _cell_length_c 18.969(3) _cell_angle_alpha 99.19(2) _cell_angle_beta 102.99(2) _cell_angle_gamma 108.59(2) _cell_volume 4155.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5739 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.74 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method ? _exptl_crystal_F_000 1530 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33548 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15582 _reflns_number_observed 9657 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1522 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14060 _refine_ls_number_parameters 847 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_obs 0.0691 _refine_ls_wR_factor_all 0.1984 _refine_ls_wR_factor_obs 0.1642 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.112 _refine_ls_shift/esd_max -0.046 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.69209(4) 0.23019(4) 0.22919(3) 0.0180(2) Uani 1 d . . Co2 Co 0.51619(4) 0.28735(4) 0.23232(3) 0.0166(2) Uani 1 d . . P1 P 0.62177(8) 0.33347(8) 0.10798(6) 0.0169(3) Uani 1 d . . P2 P 0.54418(8) 0.13499(8) 0.31208(6) 0.0152(2) Uani 1 d . . O1 O 0.5867(2) 0.2628(2) 0.15065(14) 0.0165(6) Uani 1 d . . O2 O 0.7952(2) 0.3195(2) 0.20366(15) 0.0215(7) Uani 1 d . . O3 O 0.5114(2) 0.3983(2) 0.2003(2) 0.0191(7) Uani 1 d . . O4 O 0.5520(2) 0.1717(2) 0.24323(15) 0.0170(6) Uani 1 d . . O5 O 0.7509(2) 0.1835(2) 0.31336(15) 0.0196(7) Uani 1 d . . O6 O 0.4859(2) 0.2883(2) 0.3285(2) 0.0188(7) Uani 1 d . . C1 C 0.7240(3) 0.3240(3) 0.0798(2) 0.0196(10) Uani 1 d . . C2 C 0.8028(3) 0.3202(3) 0.1349(2) 0.0178(9) Uani 1 d . . C3 C 0.8874(3) 0.3179(3) 0.1142(2) 0.0234(10) Uani 1 d . . C4 C 0.8876(3) 0.3210(3) 0.0411(2) 0.0237(10) Uani 1 d . . H4 H 0.9448(3) 0.3210(3) 0.0277(2) 0.028 Uiso 1 calc R . C5 C 0.8106(3) 0.3240(3) -0.0136(2) 0.0233(10) Uani 1 d . . C6 C 0.7287(3) 0.3263(3) 0.0064(2) 0.0199(10) Uani 1 d . . H6 H 0.6751(3) 0.3294(3) -0.0293(2) 0.024 Uiso 1 calc R . C7 C 0.9766(3) 0.3155(4) 0.1711(3) 0.0316(12) Uani 1 d . . C8 C 0.9469(4) 0.2318(4) 0.2009(3) 0.0359(13) Uani 1 d . . H8A H 1.0044(4) 0.2312(4) 0.2371(3) 0.054 Uiso 1 calc R . H8B H 0.9212(4) 0.1783(4) 0.1593(3) 0.054 Uiso 1 calc R . H8C H 0.8961(4) 0.2325(4) 0.2253(3) 0.054 Uiso 1 calc R . C9 C 1.0197(4) 0.4025(4) 0.2358(3) 0.0399(14) Uani 1 d . . H9A H 1.0381(4) 0.4548(4) 0.2153(3) 0.060 Uiso 1 calc R . H9B H 1.0779(4) 0.4024(4) 0.2716(3) 0.060 Uiso 1 calc R . H9C H 0.9703(4) 0.4049(4) 0.2612(3) 0.060 Uiso 1 calc R . C10 C 1.0596(4) 0.3140(5) 0.1363(3) 0.049(2) Uani 1 d . . H10A H 1.0800(4) 0.3669(5) 0.1168(3) 0.073 Uiso 1 calc R . H10B H 1.0358(4) 0.2599(5) 0.0954(3) 0.073 Uiso 1 calc R . H10C H 1.1157(4) 0.3141(5) 0.1745(3) 0.073 Uiso 1 calc R . C11 C 0.8199(4) 0.3251(3) -0.0930(2) 0.0277(11) Uani 1 d . . C12 C 0.7316(4) 0.3342(4) -0.1437(2) 0.0354(13) Uani 1 d . . H12A H 0.7242(4) 0.3894(4) -0.1218(2) 0.053 Uiso 1 calc R . H12B H 0.6723(4) 0.2828(4) -0.1491(2) 0.053 Uiso 1 calc R . H12C H 0.7412(4) 0.3361(4) -0.1929(2) 0.053 Uiso 1 calc R . C13 C 0.9108(4) 0.4058(4) -0.0881(3) 0.0377(13) Uani 1 d . . H13A H 0.9694(4) 0.4019(4) -0.0557(3) 0.056 Uiso 1 calc R . H13B H 0.9030(4) 0.4612(4) -0.0673(3) 0.056 Uiso 1 calc R . H13C H 0.9182(4) 0.4056(4) -0.1381(3) 0.056 Uiso 1 calc R . C14 C 0.8301(4) 0.2385(4) -0.1280(3) 0.0428(14) Uani 1 d . . H14A H 0.8870(4) 0.2320(4) -0.0958(3) 0.064 Uiso 1 calc R . H14B H 0.8393(4) 0.2406(4) -0.1773(3) 0.064 Uiso 1 calc R . H14C H 0.7706(4) 0.1875(4) -0.1333(3) 0.064 Uiso 1 calc R . C15 C 0.6563(3) 0.4456(3) 0.1620(2) 0.0176(9) Uani 1 d . . C16 C 0.5940(3) 0.4646(3) 0.2032(2) 0.0185(10) Uani 1 d . . C17 C 0.6237(3) 0.5531(3) 0.2466(2) 0.0193(10) Uani 1 d . . C18 C 0.7129(3) 0.6153(3) 0.2469(2) 0.0189(10) Uani 1 d . . H18 H 0.7324(3) 0.6746(3) 0.2763(2) 0.023 Uiso 1 calc R . C19 C 0.7756(3) 0.5977(3) 0.2079(2) 0.0197(10) Uani 1 d . . C20 C 0.7449(3) 0.5112(3) 0.1644(2) 0.0193(10) Uani 1 d . . H20 H 0.7845(3) 0.4962(3) 0.1358(2) 0.023 Uiso 1 calc R . C21 C 0.5619(3) 0.5810(3) 0.2938(2) 0.0223(10) Uani 1 d . . C22 C 0.5532(4) 0.5272(3) 0.3524(3) 0.0288(11) Uani 1 d . . H22A H 0.6189(4) 0.5381(3) 0.3844(3) 0.043 Uiso 1 calc R . H22B H 0.5200(4) 0.4634(3) 0.3275(3) 0.043 Uiso 1 calc R . H22C H 0.5150(4) 0.5457(3) 0.3830(3) 0.043 Uiso 1 calc R . C23 C 0.4593(3) 0.5640(3) 0.2437(3) 0.0291(11) Uani 1 d . . H23A H 0.4650(3) 0.5986(3) 0.2060(3) 0.044 Uiso 1 calc R . H23B H 0.4210(3) 0.5824(3) 0.2742(3) 0.044 Uiso 1 calc R . H23C H 0.4262(3) 0.5002(3) 0.2187(3) 0.044 Uiso 1 calc R . C24 C 0.6090(4) 0.6804(3) 0.3361(3) 0.0318(12) Uani 1 d . . H24A H 0.6159(4) 0.7174(3) 0.3002(3) 0.048 Uiso 1 calc R . H24B H 0.6739(4) 0.6923(3) 0.3700(3) 0.048 Uiso 1 calc R . H24C H 0.5672(4) 0.6949(3) 0.3650(3) 0.048 Uiso 1 calc R . C25 C 0.8761(3) 0.6666(3) 0.2136(3) 0.0245(11) Uani 1 d . . C26 C 0.8948(4) 0.7589(3) 0.2626(3) 0.0392(14) Uani 1 d . . H26A H 0.8434(4) 0.7803(3) 0.2412(3) 0.059 Uiso 1 calc R . H26B H 0.9590(4) 0.8012(3) 0.2645(3) 0.059 Uiso 1 calc R . H26C H 0.8939(4) 0.7539(3) 0.3132(3) 0.059 Uiso 1 calc R . C27 C 0.9571(4) 0.6346(4) 0.2480(3) 0.0380(13) Uani 1 d . . H27A H 0.9541(4) 0.6274(4) 0.2978(3) 0.057 Uiso 1 calc R . H27B H 1.0213(4) 0.6788(4) 0.2521(3) 0.057 Uiso 1 calc R . H27C H 0.9479(4) 0.5771(4) 0.2161(3) 0.057 Uiso 1 calc R . C28 C 0.8809(4) 0.6778(4) 0.1354(3) 0.0382(13) Uani 1 d . . H28A H 0.8292(4) 0.6985(4) 0.1134(3) 0.057 Uiso 1 calc R . H28B H 0.8715(4) 0.6202(4) 0.1036(3) 0.057 Uiso 1 calc R . H28C H 0.9452(4) 0.7218(4) 0.1395(3) 0.057 Uiso 1 calc R . C29 C 0.5235(3) 0.3124(3) 0.0247(2) 0.0184(10) Uani 1 d . . C30 C 0.4599(4) 0.2243(3) -0.0089(2) 0.0295(12) Uani 1 d . . H30 H 0.4654(4) 0.1776(3) 0.0139(2) 0.035 Uiso 1 calc R . C31 C 0.3878(4) 0.2052(4) -0.0766(3) 0.0364(13) Uani 1 d . . H31 H 0.3445(4) 0.1452(4) -0.1000(3) 0.044 Uiso 1 calc R . C32 C 0.3790(4) 0.2721(4) -0.1094(2) 0.0311(12) Uani 1 d . . H32 H 0.3304(4) 0.2580(4) -0.1559(2) 0.037 Uiso 1 calc R . C33 C 0.4401(4) 0.3601(4) -0.0756(2) 0.0290(12) Uani 1 d . . H33 H 0.4325(4) 0.4065(4) -0.0981(2) 0.035 Uiso 1 calc R . C34 C 0.5125(3) 0.3801(3) -0.0089(2) 0.0238(10) Uani 1 d . . H34 H 0.5549(3) 0.4405(3) 0.0143(2) 0.029 Uiso 1 calc R . C35 C 0.6485(3) 0.1939(3) 0.3915(2) 0.0167(9) Uani 1 d . . C36 C 0.7437(3) 0.2088(3) 0.3823(2) 0.0179(9) Uani 1 d . . C37 C 0.8264(3) 0.2493(3) 0.4481(2) 0.0194(10) Uani 1 d . . C38 C 0.8094(3) 0.2807(3) 0.5142(2) 0.0184(10) Uani 1 d . . H38 H 0.8647(3) 0.3092(3) 0.5573(2) 0.022 Uiso 1 calc R . C39 C 0.7170(3) 0.2739(3) 0.5227(2) 0.0181(9) Uani 1 d . . C40 C 0.6369(3) 0.2277(3) 0.4598(2) 0.0180(9) Uani 1 d . . H40 H 0.5726(3) 0.2190(3) 0.4634(2) 0.022 Uiso 1 calc R . C41 C 0.9318(3) 0.2650(3) 0.4444(2) 0.0254(11) Uani 1 d . . C42 C 0.9396(4) 0.1800(4) 0.4049(3) 0.0372(13) Uani 1 d . . H42A H 0.9203(4) 0.1335(4) 0.4314(3) 0.056 Uiso 1 calc R . H42B H 1.0075(4) 0.1920(4) 0.4042(3) 0.056 Uiso 1 calc R . H42C H 0.8961(4) 0.1597(4) 0.3535(3) 0.056 Uiso 1 calc R . C43 C 0.9621(3) 0.3382(4) 0.4028(3) 0.0318(12) Uani 1 d . . H43A H 0.9571(3) 0.3930(4) 0.4284(3) 0.048 Uiso 1 calc R . H43B H 0.9186(3) 0.3180(4) 0.3514(3) 0.048 Uiso 1 calc R . H43C H 1.0300(3) 0.3502(4) 0.4021(3) 0.048 Uiso 1 calc R . C44 C 1.0053(3) 0.2954(4) 0.5232(3) 0.0372(13) Uani 1 d . . H44A H 1.0027(3) 0.3504(4) 0.5509(3) 0.056 Uiso 1 calc R . H44B H 1.0717(3) 0.3066(4) 0.5192(3) 0.056 Uiso 1 calc R . H44C H 0.9880(3) 0.2484(4) 0.5498(3) 0.056 Uiso 1 calc R . C45 C 0.7026(3) 0.3194(3) 0.5943(2) 0.0222(10) Uani 1 d . . C46 C 0.6248(4) 0.2518(4) 0.6179(3) 0.0358(13) Uani 1 d . . H46A H 0.5633(4) 0.2258(4) 0.5769(3) 0.054 Uiso 1 calc R . H46B H 0.6137(4) 0.2822(4) 0.6621(3) 0.054 Uiso 1 calc R . H46C H 0.6477(4) 0.2042(4) 0.6296(3) 0.054 Uiso 1 calc R . C47 C 0.7971(4) 0.3581(4) 0.6591(3) 0.0380(14) Uani 1 d . . H47A H 0.8480(4) 0.4016(4) 0.6452(3) 0.057 Uiso 1 calc R . H47B H 0.8189(4) 0.3098(4) 0.6704(3) 0.057 Uiso 1 calc R . H47C H 0.7852(4) 0.3878(4) 0.7032(3) 0.057 Uiso 1 calc R . C48 C 0.6674(4) 0.3951(4) 0.5779(3) 0.0406(14) Uani 1 d . . H48A H 0.6067(4) 0.3704(4) 0.5362(3) 0.061 Uiso 1 calc R . H48B H 0.7180(4) 0.4396(4) 0.5646(3) 0.061 Uiso 1 calc R . H48C H 0.6552(4) 0.4236(4) 0.6223(3) 0.061 Uiso 1 calc R . C49 C 0.4371(3) 0.1376(3) 0.3363(2) 0.0164(9) Uani 1 d . . C50 C 0.4218(3) 0.2193(3) 0.3418(2) 0.0162(9) Uani 1 d . . C51 C 0.3396(3) 0.2242(3) 0.3648(2) 0.0192(10) Uani 1 d . . C52 C 0.2780(3) 0.1477(3) 0.3785(2) 0.0239(11) Uani 1 d . . H52 H 0.2228(3) 0.1514(3) 0.3934(2) 0.029 Uiso 1 calc R . C53 C 0.2917(3) 0.0663(3) 0.3721(2) 0.0215(10) Uani 1 d . . C54 C 0.3733(3) 0.0631(3) 0.3510(2) 0.0190(10) Uani 1 d . . H54 H 0.3861(3) 0.0093(3) 0.3464(2) 0.023 Uiso 1 calc R . C55 C 0.3200(3) 0.3120(3) 0.3765(3) 0.0258(11) Uani 1 d . . C56 C 0.4070(3) 0.3832(3) 0.4390(2) 0.0274(11) Uani 1 d . . H56A H 0.4678(3) 0.3911(3) 0.4254(2) 0.041 Uiso 1 calc R . H56B H 0.4121(3) 0.3639(3) 0.4857(2) 0.041 Uiso 1 calc R . H56C H 0.3968(3) 0.4400(3) 0.4459(2) 0.041 Uiso 1 calc R . C57 C 0.3067(4) 0.3425(3) 0.3032(3) 0.0308(12) Uani 1 d . . H57A H 0.2509(4) 0.2961(3) 0.2641(3) 0.046 Uiso 1 calc R . H57B H 0.3664(4) 0.3524(3) 0.2876(3) 0.046 Uiso 1 calc R . H57C H 0.2942(4) 0.3982(3) 0.3111(3) 0.046 Uiso 1 calc R . C58 C 0.2262(4) 0.3015(4) 0.3998(3) 0.0436(15) Uani 1 d . . H58A H 0.1696(4) 0.2562(4) 0.3606(3) 0.065 Uiso 1 calc R . H58B H 0.2169(4) 0.3588(4) 0.4069(3) 0.065 Uiso 1 calc R . H58C H 0.2322(4) 0.2827(4) 0.4466(3) 0.065 Uiso 1 calc R . C59 C 0.2240(3) -0.0156(4) 0.3900(3) 0.0312(12) Uani 1 d . . C60 C 0.1930(4) -0.0996(4) 0.3266(3) 0.0446(15) Uani 1 d . . H60A H 0.1565(4) -0.0913(4) 0.2803(3) 0.067 Uiso 1 calc R . H60B H 0.1511(4) -0.1513(4) 0.3394(3) 0.067 Uiso 1 calc R . H60C H 0.2515(4) -0.1100(4) 0.3197(3) 0.067 Uiso 1 calc R . C61 C 0.1300(4) -0.0040(4) 0.3998(4) 0.057(2) Uani 1 d . . H61A H 0.0942(4) 0.0056(4) 0.3539(4) 0.086 Uiso 1 calc R . H61B H 0.1471(4) 0.0477(4) 0.4415(4) 0.086 Uiso 1 calc R . H61C H 0.0887(4) -0.0579(4) 0.4103(4) 0.086 Uiso 1 calc R . C62 C 0.2810(5) -0.0306(4) 0.4617(3) 0.054(2) Uani 1 d . . H62A H 0.3408(5) -0.0381(4) 0.4549(3) 0.082 Uiso 1 calc R . H62B H 0.2399(5) -0.0844(4) 0.4724(3) 0.082 Uiso 1 calc R . H62C H 0.2985(5) 0.0213(4) 0.5034(3) 0.082 Uiso 1 calc R . C63 C 0.5351(3) 0.0208(3) 0.2884(2) 0.0204(10) Uani 1 d . . C64 C 0.4941(3) -0.0269(3) 0.2130(2) 0.0251(11) Uani 1 d . . H64 H 0.4723(3) 0.0012(3) 0.1762(2) 0.030 Uiso 1 calc R . C65 C 0.4855(4) -0.1147(3) 0.1927(3) 0.0335(12) Uani 1 d . . H65 H 0.4581(4) -0.1470(3) 0.1417(3) 0.040 Uiso 1 calc R . C66 C 0.5166(4) -0.1558(3) 0.2461(3) 0.0329(12) Uani 1 d . . H66 H 0.5103(4) -0.2165(3) 0.2319(3) 0.040 Uiso 1 calc R . C67 C 0.5570(4) -0.1091(3) 0.3202(3) 0.0318(12) Uani 1 d . . H67 H 0.5788(4) -0.1376(3) 0.3568(3) 0.038 Uiso 1 calc R . C68 C 0.5656(3) -0.0216(3) 0.3414(2) 0.0247(11) Uani 1 d . . H68 H 0.5927(3) 0.0099(3) 0.3926(2) 0.030 Uiso 1 calc R . O70 O 0.3722(2) 0.2093(2) 0.1652(2) 0.0273(8) Uani 1 d D . H70 H 0.3472(34) 0.2428(28) 0.1396(24) 0.035 Uiso 1 d D . C70 C 0.3319(5) 0.1197(4) 0.1251(4) 0.057(2) Uani 1 d . . H70A H 0.3836(5) 0.0939(4) 0.1318(4) 0.069 Uiso 1 calc R . H70B H 0.3076(5) 0.1162(4) 0.0713(4) 0.069 Uiso 1 calc R . C71 C 0.2473(7) 0.0650(6) 0.1506(4) 0.119(4) Uani 1 d . . H71A H 0.2211(7) 0.0027(6) 0.1213(4) 0.179 Uiso 1 calc R . H71B H 0.1953(7) 0.0896(6) 0.1430(4) 0.179 Uiso 1 calc R . H71C H 0.2713(7) 0.0675(6) 0.2037(4) 0.179 Uiso 1 calc R . O80 O 0.6852(2) 0.1199(2) 0.1500(2) 0.0295(8) Uani 1 d D . H80 H 0.7256(30) 0.0966(32) 0.1736(25) 0.038 Uiso 1 d D . C80 C 0.6215(4) 0.0764(4) 0.0773(3) 0.0379(13) Uani 1 d . . H80A H 0.5754(4) 0.1073(4) 0.0645(3) 0.045 Uiso 1 calc R . H80B H 0.5825(4) 0.0142(4) 0.0762(3) 0.045 Uiso 1 calc R . C81 C 0.6762(5) 0.0746(5) 0.0185(3) 0.062(2) Uani 1 d . . H81A H 0.6288(5) 0.0437(5) -0.0309(3) 0.093 Uiso 1 calc R . H81B H 0.7210(5) 0.0429(5) 0.0302(3) 0.093 Uiso 1 calc R . H81C H 0.7139(5) 0.1360(5) 0.0185(3) 0.093 Uiso 1 calc R . O9 O 0.6828(2) 0.3521(2) 0.3060(2) 0.0240(7) Uani 1 d . . C90 C 0.7619(7) 0.4350(6) 0.3399(5) 0.031(2) Uiso 0.55 d P 1 H90A H 0.7473(7) 0.4816(6) 0.3172(5) 0.037 Uiso 0.55 calc PR 1 H90B H 0.8219(7) 0.4302(6) 0.3293(5) 0.037 Uiso 0.55 calc PR 1 C91 C 0.7823(8) 0.4644(7) 0.4254(5) 0.041(2) Uiso 0.55 d P 1 H91A H 0.8376(8) 0.5218(7) 0.4456(5) 0.062 Uiso 0.55 calc PR 1 H91B H 0.7984(8) 0.4192(7) 0.4484(5) 0.062 Uiso 0.55 calc PR 1 H91C H 0.7238(8) 0.4707(7) 0.4363(5) 0.062 Uiso 0.55 calc PR 1 O100 O 0.6860(4) 0.6651(4) -0.1275(3) 0.0244(14) Uiso 0.50 d P 1 C100 C 0.7251(5) 0.6449(6) -0.0678(5) 0.090(3) Uani 1 d . 1 H10D H 0.7188(5) 0.6856(6) -0.0262(5) 0.109 Uiso 1 calc R 1 H10E H 0.7961(5) 0.6653(6) -0.0633(5) 0.109 Uiso 1 calc R 1 C101 C 0.7025(5) 0.5591(4) -0.0482(3) 0.057(2) Uani 1 d . 1 H10F H 0.7458(5) 0.5669(4) 0.0015(3) 0.085 Uiso 1 calc R 1 H10G H 0.7126(5) 0.5162(4) -0.0851(3) 0.085 Uiso 1 calc R 1 H10H H 0.6340(5) 0.5366(4) -0.0478(3) 0.085 Uiso 1 calc R 1 C90X C 0.7199(8) 0.4045(8) 0.3776(6) 0.035(3) Uiso 0.45 d P 2 H90C H 0.7464(8) 0.3709(8) 0.4103(6) 0.042 Uiso 0.45 calc PR 2 H90D H 0.6650(8) 0.4143(8) 0.3936(6) 0.042 Uiso 0.45 calc PR 2 C91X C 0.7995(9) 0.4947(9) 0.3907(7) 0.040(3) Uiso 0.45 d P 2 H91D H 0.8206(9) 0.5262(9) 0.4436(7) 0.060 Uiso 0.45 calc PR 2 H91E H 0.7740(9) 0.5301(9) 0.3602(7) 0.060 Uiso 0.45 calc PR 2 H91F H 0.8556(9) 0.4864(9) 0.3767(7) 0.060 Uiso 0.45 calc PR 2 O101 O 0.6588(5) 0.6728(5) -0.0902(4) 0.037(2) Uiso 0.50 d P 2 O200 O 0.7433(3) 0.0215(3) 0.2358(2) 0.0422(10) Uani 1 d . . H200 H 0.7421(34) 0.0537(34) 0.2746(5) 0.063 Uiso 1 calc R . C201 C 0.8089(7) -0.0573(6) 0.3201(5) 0.096(3) Uani 1 d . . H20A H 0.8597(7) -0.0830(6) 0.3299(5) 0.144 Uiso 1 calc R . H20B H 0.7441(7) -0.1042(6) 0.3093(5) 0.144 Uiso 1 calc R . H20C H 0.8198(7) -0.0105(6) 0.3641(5) 0.144 Uiso 1 calc R . C200 C 0.8134(5) -0.0181(5) 0.2552(4) 0.064(2) Uani 1 d . . H20D H 0.8798(5) 0.0278(5) 0.2662(4) 0.077 Uiso 1 calc R . H20E H 0.8040(5) -0.0657(5) 0.2115(4) 0.077 Uiso 1 calc R . O300 O 0.0000 0.0000 0.0000 0.159(9) Uiso 0.50 d SP . O301 O 0.9161(25) -0.0811(23) 0.0708(18) 0.154(12) Uiso 0.25 d P . 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 0.0221(3) 0.0201(4) 0.0137(3) 0.0052(3) 0.0062(2) 0.0093(3) Co2 0.0213(3) 0.0144(4) 0.0156(3) 0.0043(2) 0.0068(2) 0.0072(3) P1 0.0224(6) 0.0172(7) 0.0122(5) 0.0043(5) 0.0048(5) 0.0087(5) P2 0.0181(6) 0.0128(6) 0.0147(5) 0.0033(4) 0.0048(5) 0.0057(5) O1 0.023(2) 0.012(2) 0.0134(14) 0.0024(12) 0.0041(12) 0.0062(13) O2 0.028(2) 0.022(2) 0.0137(14) 0.0055(13) 0.0068(13) 0.0072(14) O3 0.021(2) 0.017(2) 0.021(2) 0.0072(13) 0.0065(13) 0.0081(14) O4 0.021(2) 0.015(2) 0.0158(14) 0.0051(12) 0.0057(12) 0.0064(13) O5 0.027(2) 0.023(2) 0.0137(14) 0.0042(13) 0.0059(13) 0.0150(14) O6 0.021(2) 0.017(2) 0.0177(15) 0.0043(13) 0.0072(13) 0.0044(13) C1 0.027(2) 0.019(3) 0.017(2) 0.003(2) 0.011(2) 0.011(2) C2 0.026(2) 0.015(3) 0.014(2) 0.003(2) 0.008(2) 0.007(2) C3 0.027(2) 0.022(3) 0.021(2) 0.005(2) 0.007(2) 0.009(2) C4 0.023(2) 0.025(3) 0.022(2) 0.004(2) 0.010(2) 0.008(2) C5 0.032(3) 0.022(3) 0.016(2) 0.003(2) 0.012(2) 0.007(2) C6 0.026(2) 0.019(3) 0.016(2) 0.005(2) 0.006(2) 0.010(2) C7 0.027(3) 0.046(4) 0.026(3) 0.011(2) 0.009(2) 0.018(2) C8 0.039(3) 0.046(4) 0.033(3) 0.018(3) 0.010(2) 0.025(3) C9 0.028(3) 0.053(4) 0.031(3) 0.015(3) 0.004(2) 0.006(3) C10 0.034(3) 0.092(5) 0.036(3) 0.031(3) 0.013(3) 0.034(3) C11 0.034(3) 0.030(3) 0.017(2) 0.001(2) 0.011(2) 0.009(2) C12 0.039(3) 0.050(4) 0.016(2) 0.009(2) 0.011(2) 0.011(3) C13 0.043(3) 0.042(4) 0.025(3) 0.008(2) 0.016(2) 0.007(3) C14 0.051(3) 0.046(4) 0.031(3) -0.001(3) 0.023(3) 0.015(3) C15 0.021(2) 0.019(3) 0.010(2) 0.003(2) -0.001(2) 0.007(2) C16 0.025(2) 0.018(3) 0.014(2) 0.004(2) 0.003(2) 0.011(2) C17 0.028(2) 0.016(3) 0.016(2) 0.006(2) 0.006(2) 0.011(2) C18 0.026(2) 0.014(3) 0.014(2) 0.001(2) 0.001(2) 0.008(2) C19 0.019(2) 0.021(3) 0.015(2) 0.006(2) -0.002(2) 0.005(2) C20 0.022(2) 0.024(3) 0.016(2) 0.008(2) 0.006(2) 0.012(2) C21 0.032(3) 0.018(3) 0.024(2) 0.006(2) 0.015(2) 0.014(2) C22 0.045(3) 0.015(3) 0.025(2) 0.001(2) 0.014(2) 0.008(2) C23 0.033(3) 0.028(3) 0.033(3) 0.008(2) 0.017(2) 0.015(2) C24 0.045(3) 0.018(3) 0.036(3) 0.005(2) 0.021(2) 0.011(2) C25 0.020(2) 0.022(3) 0.029(2) 0.006(2) 0.006(2) 0.007(2) C26 0.025(3) 0.027(3) 0.053(3) 0.002(3) 0.003(3) 0.003(2) C27 0.029(3) 0.042(4) 0.043(3) 0.015(3) 0.007(2) 0.014(3) C28 0.028(3) 0.039(4) 0.044(3) 0.017(3) 0.012(2) 0.003(2) C29 0.021(2) 0.025(3) 0.010(2) 0.004(2) 0.006(2) 0.010(2) C30 0.036(3) 0.026(3) 0.024(2) 0.007(2) 0.003(2) 0.011(2) C31 0.037(3) 0.030(3) 0.027(3) -0.002(2) -0.004(2) 0.005(3) C32 0.033(3) 0.046(4) 0.016(2) 0.011(2) 0.001(2) 0.019(3) C33 0.036(3) 0.035(3) 0.023(2) 0.015(2) 0.007(2) 0.019(3) C34 0.031(3) 0.021(3) 0.020(2) 0.009(2) 0.007(2) 0.009(2) C35 0.022(2) 0.012(2) 0.015(2) 0.002(2) 0.003(2) 0.008(2) C36 0.028(2) 0.013(2) 0.015(2) 0.006(2) 0.006(2) 0.010(2) C37 0.021(2) 0.018(3) 0.019(2) 0.008(2) 0.005(2) 0.007(2) C38 0.019(2) 0.018(3) 0.015(2) 0.004(2) 0.001(2) 0.006(2) C39 0.020(2) 0.021(3) 0.016(2) 0.006(2) 0.005(2) 0.009(2) C40 0.022(2) 0.019(3) 0.018(2) 0.007(2) 0.009(2) 0.010(2) C41 0.023(2) 0.036(3) 0.022(2) 0.011(2) 0.008(2) 0.015(2) C42 0.035(3) 0.046(4) 0.039(3) 0.012(3) 0.014(2) 0.023(3) C43 0.020(2) 0.039(3) 0.031(3) 0.010(2) 0.008(2) 0.004(2) C44 0.025(3) 0.060(4) 0.026(3) 0.011(3) 0.004(2) 0.017(3) C45 0.027(2) 0.023(3) 0.017(2) 0.004(2) 0.007(2) 0.010(2) C46 0.038(3) 0.042(4) 0.027(3) 0.002(2) 0.020(2) 0.010(3) C47 0.034(3) 0.051(4) 0.022(2) 0.000(2) 0.009(2) 0.011(3) C48 0.065(4) 0.041(4) 0.029(3) 0.008(2) 0.019(3) 0.034(3) C49 0.017(2) 0.019(3) 0.014(2) 0.003(2) 0.006(2) 0.008(2) C50 0.018(2) 0.018(3) 0.012(2) 0.003(2) 0.000(2) 0.008(2) C51 0.018(2) 0.024(3) 0.017(2) 0.004(2) 0.003(2) 0.010(2) C52 0.020(2) 0.028(3) 0.023(2) 0.007(2) 0.008(2) 0.007(2) C53 0.021(2) 0.017(3) 0.022(2) 0.004(2) 0.007(2) 0.001(2) C54 0.019(2) 0.020(3) 0.013(2) 0.001(2) -0.003(2) 0.007(2) C55 0.028(3) 0.026(3) 0.032(3) 0.009(2) 0.015(2) 0.015(2) C56 0.038(3) 0.028(3) 0.021(2) 0.005(2) 0.016(2) 0.015(2) C57 0.033(3) 0.025(3) 0.035(3) 0.007(2) 0.002(2) 0.018(2) C58 0.042(3) 0.036(4) 0.069(4) 0.017(3) 0.032(3) 0.023(3) C59 0.024(3) 0.029(3) 0.037(3) 0.011(2) 0.010(2) 0.003(2) C60 0.037(3) 0.025(3) 0.065(4) 0.010(3) 0.018(3) 0.001(3) C61 0.046(4) 0.040(4) 0.102(5) 0.034(4) 0.047(4) 0.014(3) C62 0.066(4) 0.054(4) 0.046(3) 0.032(3) 0.017(3) 0.015(3) C63 0.024(2) 0.014(3) 0.023(2) 0.004(2) 0.009(2) 0.007(2) C64 0.033(3) 0.017(3) 0.021(2) 0.001(2) 0.006(2) 0.007(2) C65 0.045(3) 0.018(3) 0.033(3) -0.003(2) 0.007(2) 0.013(2) C66 0.042(3) 0.012(3) 0.039(3) -0.001(2) 0.008(2) 0.009(2) C67 0.038(3) 0.023(3) 0.037(3) 0.011(2) 0.010(2) 0.014(2) C68 0.028(3) 0.023(3) 0.023(2) 0.004(2) 0.006(2) 0.011(2) O70 0.025(2) 0.020(2) 0.029(2) 0.0020(15) -0.0007(15) 0.0066(15) C70 0.061(4) 0.033(4) 0.056(4) -0.002(3) -0.015(3) 0.017(3) C71 0.119(7) 0.075(7) 0.071(5) 0.033(5) -0.030(5) -0.054(6) O80 0.040(2) 0.030(2) 0.019(2) 0.0018(14) 0.004(2) 0.020(2) C80 0.044(3) 0.039(4) 0.026(3) -0.003(2) 0.003(2) 0.021(3) C81 0.096(5) 0.054(5) 0.028(3) -0.006(3) 0.018(3) 0.024(4) O9 0.027(2) 0.014(2) 0.023(2) -0.0015(13) 0.0006(14) 0.0048(14) C100 0.029(3) 0.094(6) 0.131(7) 0.081(6) -0.012(4) 0.000(4) C101 0.065(4) 0.037(4) 0.051(4) 0.012(3) -0.007(3) 0.011(3) O200 0.059(2) 0.038(3) 0.035(2) 0.004(2) 0.008(2) 0.031(2) C201 0.096(6) 0.085(7) 0.111(7) 0.031(6) 0.014(6) 0.049(6) C200 0.084(5) 0.059(5) 0.051(4) 0.005(3) 0.004(4) 0.045(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 O2 1.969(3) . ? Co1 O5 2.023(3) . ? Co1 O80 2.109(3) . ? Co1 O4 2.115(3) . ? Co1 O1 2.178(3) . ? Co1 O9 2.332(3) . ? Co2 O6 1.977(3) . ? Co2 O3 2.015(3) . ? Co2 O70 2.101(3) . ? Co2 O1 2.120(3) . ? Co2 O4 2.146(3) . ? Co2 O9 2.369(3) . ? P1 O1 1.536(3) . ? P1 C1 1.780(4) . ? P1 C15 1.792(5) . ? P1 C29 1.803(4) . ? P2 O4 1.533(3) . ? P2 C35 1.780(4) . ? P2 C49 1.782(4) . ? P2 C63 1.795(5) . ? O2 C2 1.337(5) . ? O3 C16 1.344(5) . ? O5 C36 1.347(5) . ? O6 C50 1.328(5) . ? C1 C2 1.416(6) . ? C1 C6 1.417(6) . ? C2 C3 1.423(6) . ? C3 C4 1.397(6) . ? C3 C7 1.537(6) . ? C4 C5 1.391(6) . ? C5 C6 1.377(6) . ? C5 C11 1.545(6) . ? C7 C8 1.533(7) . ? C7 C10 1.543(7) . ? C7 C9 1.561(7) . ? C11 C12 1.518(7) . ? C11 C14 1.530(7) . ? C11 C13 1.537(7) . ? C15 C20 1.404(6) . ? C15 C16 1.423(6) . ? C16 C17 1.414(6) . ? C17 C18 1.399(6) . ? C17 C21 1.543(6) . ? C18 C19 1.391(6) . ? C19 C20 1.386(6) . ? C19 C25 1.538(6) . ? C21 C22 1.525(6) . ? C21 C23 1.532(6) . ? C21 C24 1.539(7) . ? C25 C27 1.529(7) . ? C25 C28 1.538(7) . ? C25 C26 1.539(7) . ? C29 C30 1.393(7) . ? C29 C34 1.394(6) . ? C30 C31 1.397(7) . ? C31 C32 1.366(7) . ? C32 C33 1.383(7) . ? C33 C34 1.384(6) . ? C35 C40 1.396(6) . ? C35 C36 1.429(6) . ? C36 C37 1.433(6) . ? C37 C38 1.386(6) . ? C37 C41 1.543(6) . ? C38 C39 1.405(6) . ? C39 C40 1.390(6) . ? C39 C45 1.535(6) . ? C41 C42 1.518(7) . ? C41 C43 1.539(7) . ? C41 C44 1.541(6) . ? C45 C47 1.524(6) . ? C45 C46 1.532(7) . ? C45 C48 1.538(7) . ? C49 C54 1.398(6) . ? C49 C50 1.415(6) . ? C50 C51 1.420(6) . ? C51 C52 1.399(6) . ? C51 C55 1.542(6) . ? C52 C53 1.397(7) . ? C53 C54 1.388(6) . ? C53 C59 1.539(6) . ? C55 C56 1.536(7) . ? C55 C58 1.538(6) . ? C55 C57 1.543(7) . ? C59 C62 1.534(7) . ? C59 C61 1.531(7) . ? C59 C60 1.534(7) . ? C63 C68 1.384(6) . ? C63 C64 1.405(6) . ? C64 C65 1.377(7) . ? C65 C66 1.377(7) . ? C66 C67 1.381(7) . ? C67 C68 1.373(7) . ? O70 C70 1.396(7) . ? C70 C71 1.528(10) . ? O80 C80 1.408(6) . ? C80 C81 1.529(8) . ? O9 C90X 1.367(11) . ? O9 C90 1.417(10) . ? C90 C91 1.546(13) . ? O100 C100 1.296(9) . ? C100 C101 1.459(9) . ? C90X C91X 1.51(2) . ? O200 C200 1.413(7) . ? C201 C200 1.480(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O5 111.07(12) . . ? O2 Co1 O80 95.37(13) . . ? O5 Co1 O80 90.41(12) . . ? O2 Co1 O4 155.56(12) . . ? O5 Co1 O4 89.70(11) . . ? O80 Co1 O4 97.28(13) . . ? O2 Co1 O1 86.73(12) . . ? O5 Co1 O1 161.23(11) . . ? O80 Co1 O1 93.90(11) . . ? O4 Co1 O1 71.64(11) . . ? O2 Co1 O9 85.73(12) . . ? O5 Co1 O9 95.76(11) . . ? O80 Co1 O9 172.90(11) . . ? O4 Co1 O9 79.27(11) . . ? O1 Co1 O9 79.14(10) . . ? O6 Co2 O3 109.70(12) . . ? O6 Co2 O70 95.50(13) . . ? O3 Co2 O70 93.04(13) . . ? O6 Co2 O1 156.84(12) . . ? O3 Co2 O1 89.34(11) . . ? O70 Co2 O1 96.54(12) . . ? O6 Co2 O4 87.61(11) . . ? O3 Co2 O4 161.18(11) . . ? O70 Co2 O4 92.52(12) . . ? O1 Co2 O4 72.17(11) . . ? O6 Co2 O9 85.44(11) . . ? O3 Co2 O9 95.75(12) . . ? O70 Co2 O9 170.28(12) . . ? O1 Co2 O9 79.45(10) . . ? O4 Co2 O9 77.84(11) . . ? O1 P1 C1 110.3(2) . . ? O1 P1 C15 112.9(2) . . ? C1 P1 C15 108.5(2) . . ? O1 P1 C29 108.3(2) . . ? C1 P1 C29 107.8(2) . . ? C15 P1 C29 109.0(2) . . ? O4 P2 C35 113.1(2) . . ? O4 P2 C49 111.0(2) . . ? C35 P2 C49 108.7(2) . . ? O4 P2 C63 107.3(2) . . ? C35 P2 C63 107.9(2) . . ? C49 P2 C63 108.7(2) . . ? P1 O1 Co2 120.3(2) . . ? P1 O1 Co1 120.6(2) . . ? Co2 O1 Co1 91.56(10) . . ? C2 O2 Co1 125.8(3) . . ? C16 O3 Co2 121.1(2) . . ? P2 O4 Co1 119.1(2) . . ? P2 O4 Co2 119.6(2) . . ? Co1 O4 Co2 92.61(11) . . ? C36 O5 Co1 120.1(3) . . ? C50 O6 Co2 124.1(3) . . ? C2 C1 C6 121.6(4) . . ? C2 C1 P1 117.5(3) . . ? C6 C1 P1 120.8(3) . . ? O2 C2 C1 119.3(4) . . ? O2 C2 C3 122.7(4) . . ? C1 C2 C3 118.0(4) . . ? C4 C3 C2 117.5(4) . . ? C4 C3 C7 121.4(4) . . ? C2 C3 C7 121.1(4) . . ? C5 C4 C3 125.1(4) . . ? C6 C5 C4 117.4(4) . . ? C6 C5 C11 123.0(4) . . ? C4 C5 C11 119.6(4) . . ? C5 C6 C1 120.3(4) . . ? C8 C7 C3 110.3(4) . . ? C8 C7 C10 107.8(5) . . ? C3 C7 C10 111.9(4) . . ? C8 C7 C9 111.2(4) . . ? C3 C7 C9 108.9(4) . . ? C10 C7 C9 106.6(4) . . ? C12 C11 C14 108.7(4) . . ? C12 C11 C13 107.4(4) . . ? C14 C11 C13 109.7(4) . . ? C12 C11 C5 112.2(4) . . ? C14 C11 C5 109.6(4) . . ? C13 C11 C5 109.2(4) . . ? C20 C15 C16 121.8(4) . . ? C20 C15 P1 119.5(3) . . ? C16 C15 P1 118.6(3) . . ? O3 C16 C17 123.2(4) . . ? O3 C16 C15 119.1(4) . . ? C17 C16 C15 117.7(4) . . ? C18 C17 C16 117.7(4) . . ? C18 C17 C21 120.3(4) . . ? C16 C17 C21 122.0(4) . . ? C19 C18 C17 125.5(4) . . ? C20 C19 C18 116.3(4) . . ? C20 C19 C25 119.9(4) . . ? C18 C19 C25 123.8(4) . . ? C19 C20 C15 121.0(4) . . ? C22 C21 C23 109.5(4) . . ? C22 C21 C24 106.9(4) . . ? C23 C21 C24 108.1(4) . . ? C22 C21 C17 109.4(4) . . ? C23 C21 C17 110.3(3) . . ? C24 C21 C17 112.5(4) . . ? C27 C25 C28 109.4(4) . . ? C27 C25 C26 108.6(4) . . ? C28 C25 C26 107.9(4) . . ? C27 C25 C19 109.4(4) . . ? C28 C25 C19 109.9(4) . . ? C26 C25 C19 111.7(4) . . ? C30 C29 C34 119.4(4) . . ? C30 C29 P1 118.1(3) . . ? C34 C29 P1 122.4(3) . . ? C29 C30 C31 119.3(5) . . ? C32 C31 C30 120.6(5) . . ? C31 C32 C33 120.6(4) . . ? C32 C33 C34 119.6(5) . . ? C33 C34 C29 120.4(4) . . ? C40 C35 C36 121.4(4) . . ? C40 C35 P2 120.4(3) . . ? C36 C35 P2 118.2(3) . . ? O5 C36 C35 118.8(4) . . ? O5 C36 C37 123.8(4) . . ? C35 C36 C37 117.4(4) . . ? C38 C37 C36 117.6(4) . . ? C38 C37 C41 120.8(4) . . ? C36 C37 C41 121.3(4) . . ? C37 C38 C39 125.4(4) . . ? C40 C39 C38 116.1(4) . . ? C40 C39 C45 120.1(4) . . ? C38 C39 C45 123.7(4) . . ? C39 C40 C35 121.5(4) . . ? C42 C41 C43 109.6(4) . . ? C42 C41 C44 106.7(4) . . ? C43 C41 C44 108.7(4) . . ? C42 C41 C37 111.5(4) . . ? C43 C41 C37 109.1(4) . . ? C44 C41 C37 111.3(4) . . ? C47 C45 C46 108.0(4) . . ? C47 C45 C39 112.1(4) . . ? C46 C45 C39 110.1(4) . . ? C47 C45 C48 109.3(4) . . ? C46 C45 C48 109.3(4) . . ? C39 C45 C48 108.0(4) . . ? C54 C49 C50 122.1(4) . . ? C54 C49 P2 121.4(3) . . ? C50 C49 P2 116.5(3) . . ? O6 C50 C49 119.3(4) . . ? O6 C50 C51 123.2(4) . . ? C49 C50 C51 117.4(4) . . ? C52 C51 C50 118.2(4) . . ? C52 C51 C55 120.6(4) . . ? C50 C51 C55 121.2(4) . . ? C51 C52 C53 124.7(4) . . ? C54 C53 C52 116.4(4) . . ? C54 C53 C59 120.3(4) . . ? C52 C53 C59 123.2(4) . . ? C53 C54 C49 121.1(4) . . ? C56 C55 C58 108.0(4) . . ? C56 C55 C51 108.5(4) . . ? C58 C55 C51 112.3(4) . . ? C56 C55 C57 110.9(4) . . ? C58 C55 C57 107.1(4) . . ? C51 C55 C57 110.0(4) . . ? C62 C59 C61 110.0(5) . . ? C62 C59 C60 108.3(5) . . ? C61 C59 C60 107.3(4) . . ? C62 C59 C53 108.5(4) . . ? C61 C59 C53 112.2(4) . . ? C60 C59 C53 110.6(4) . . ? C68 C63 C64 119.3(4) . . ? C68 C63 P2 122.6(3) . . ? C64 C63 P2 118.1(4) . . ? C65 C64 C63 119.8(5) . . ? C66 C65 C64 120.2(5) . . ? C65 C66 C67 120.1(5) . . ? C68 C67 C66 120.3(5) . . ? C67 C68 C63 120.3(4) . . ? C70 O70 Co2 130.1(3) . . ? O70 C70 C71 111.9(6) . . ? C80 O80 Co1 131.1(3) . . ? O80 C80 C81 112.7(5) . . ? C90X O9 Co1 142.0(6) . . ? C90 O9 Co1 124.5(4) . . ? C90X O9 Co2 127.5(5) . . ? C90 O9 Co2 143.0(4) . . ? Co1 O9 Co2 81.90(10) . . ? O9 C90 C91 113.2(7) . . ? O100 C100 C101 130.1(7) . . ? O9 C90X C91X 116.6(9) . . ? O200 C200 C201 114.6(6) . . ? _refine_diff_density_max 0.966 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.100 #===END