data_he7-Complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Cl2 P3 Re' _chemical_formula_weight 774.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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 8.403(4) _cell_length_b 23.344(12) _cell_length_c 16.545(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.283(9) _cell_angle_gamma 90.00 _cell_volume 3226(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7191 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.08 _exptl_crystal_description 'bar' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 4.101 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14043 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6159 _reflns_number_gt 4907 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(2.70(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0130P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6159 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.184443(14) 0.583283(6) 0.244041(8) 0.01357(5) Uani 1 1 d . . . Cl1 Cl -0.04693(9) 0.58140(4) 0.32720(5) 0.02190(19) Uani 1 1 d . . . Cl2 Cl -0.02827(9) 0.61138(4) 0.12964(5) 0.0220(2) Uani 1 1 d . . . P1 P 0.10593(10) 0.48443(4) 0.22072(5) 0.0175(2) Uani 1 1 d . . . P2 P 0.21094(10) 0.68367(4) 0.28394(5) 0.0159(2) Uani 1 1 d . . . P3 P 0.35728(10) 0.59051(4) 0.13889(5) 0.0164(2) Uani 1 1 d . . . C1 C 0.3407(4) 0.56097(16) 0.3175(2) 0.0160(7) Uani 1 1 d . . . C2 C 0.4663(4) 0.54161(17) 0.3812(2) 0.0220(8) Uani 1 1 d . . . H2A H 0.5731 0.5511 0.3649 0.026 Uiso 1 1 calc R . . H2B H 0.4600 0.4995 0.3873 0.026 Uiso 1 1 calc R . . C3 C 0.4462(4) 0.57004(16) 0.4615(2) 0.0216(8) Uani 1 1 d . . . C4 C 0.3019(5) 0.56592(18) 0.4946(2) 0.0276(9) Uani 1 1 d . . . H4A H 0.2176 0.5436 0.4675 0.033 Uiso 1 1 calc R . . C5 C 0.2782(5) 0.59363(18) 0.5661(2) 0.0335(10) Uani 1 1 d . . . H5A H 0.1792 0.5899 0.5883 0.040 Uiso 1 1 calc R . . C6 C 0.3999(5) 0.62696(18) 0.6055(2) 0.0341(10) Uani 1 1 d . . . H6A H 0.3836 0.6467 0.6541 0.041 Uiso 1 1 calc R . . C7 C 0.5441(5) 0.63135(18) 0.5738(2) 0.0318(10) Uani 1 1 d . . . H7A H 0.6277 0.6539 0.6009 0.038 Uiso 1 1 calc R . . C8 C 0.5682(5) 0.60308(17) 0.5026(2) 0.0251(9) Uani 1 1 d . . . H8A H 0.6685 0.6061 0.4815 0.030 Uiso 1 1 calc R . . C11 C 0.2305(4) 0.43538(15) 0.1692(2) 0.0166(7) Uani 1 1 d . . . C12 C 0.3860(4) 0.42362(16) 0.2055(2) 0.0181(8) Uani 1 1 d . . . H12A H 0.4227 0.4402 0.2566 0.022 Uiso 1 1 calc R . . C13 C 0.4858(4) 0.38814(16) 0.1673(2) 0.0209(8) Uani 1 1 d . . . H13A H 0.5920 0.3816 0.1916 0.025 Uiso 1 1 calc R . . C14 C 0.4333(4) 0.36190(16) 0.0939(2) 0.0227(8) Uani 1 1 d . . . H14A H 0.5018 0.3369 0.0685 0.027 Uiso 1 1 calc R . . C15 C 0.2795(5) 0.37276(17) 0.0582(2) 0.0253(9) Uani 1 1 d . . . H15A H 0.2429 0.3553 0.0077 0.030 Uiso 1 1 calc R . . C16 C 0.1785(4) 0.40877(16) 0.0953(2) 0.0237(9) Uani 1 1 d . . . H16A H 0.0729 0.4155 0.0702 0.028 Uiso 1 1 calc R . . C17 C 0.0964(4) 0.44749(16) 0.3168(2) 0.0223(8) Uani 1 1 d . . . H17A H 0.0646 0.4076 0.3062 0.034 Uiso 1 1 calc R . . H17B H 0.0177 0.4664 0.3473 0.034 Uiso 1 1 calc R . . H17C H 0.2019 0.4486 0.3486 0.034 Uiso 1 1 calc R . . C18 C -0.0943(4) 0.47493(18) 0.1687(3) 0.0280(9) Uani 1 1 d . . . H18A H -0.1169 0.4340 0.1616 0.042 Uiso 1 1 calc R . . H18B H -0.1013 0.4936 0.1154 0.042 Uiso 1 1 calc R . . H18C H -0.1727 0.4921 0.2011 0.042 Uiso 1 1 calc R . . C21 C 0.4080(4) 0.71794(16) 0.2894(2) 0.0182(8) Uani 1 1 d . . . C22 C 0.5439(4) 0.68557(17) 0.3098(2) 0.0199(8) Uani 1 1 d . . . H22A H 0.5336 0.6453 0.3156 0.024 Uiso 1 1 calc R . . C23 C 0.6942(4) 0.70984(17) 0.3220(2) 0.0240(9) Uani 1 1 d . . . H23A H 0.7855 0.6866 0.3366 0.029 Uiso 1 1 calc R . . C24 C 0.7107(4) 0.76790(18) 0.3127(2) 0.0277(9) Uani 1 1 d . . . H24A H 0.8137 0.7851 0.3207 0.033 Uiso 1 1 calc R . . C25 C 0.5767(5) 0.80116(19) 0.2918(3) 0.0357(11) Uani 1 1 d . . . H25A H 0.5877 0.8414 0.2853 0.043 Uiso 1 1 calc R . . C26 C 0.4264(5) 0.77628(18) 0.2802(3) 0.0300(10) Uani 1 1 d . . . H26A H 0.3350 0.7996 0.2657 0.036 Uiso 1 1 calc R . . C27 C 0.0751(4) 0.73381(16) 0.2265(2) 0.0205(8) Uani 1 1 d . . . H27A H 0.0959 0.7727 0.2474 0.031 Uiso 1 1 calc R . . H27B H -0.0358 0.7232 0.2325 0.031 Uiso 1 1 calc R . . H27C H 0.0925 0.7324 0.1689 0.031 Uiso 1 1 calc R . . C28 C 0.1690(4) 0.69697(17) 0.3880(2) 0.0229(8) Uani 1 1 d . . . H28A H 0.1817 0.7379 0.4002 0.034 Uiso 1 1 calc R . . H28B H 0.2438 0.6749 0.4256 0.034 Uiso 1 1 calc R . . H28C H 0.0591 0.6852 0.3942 0.034 Uiso 1 1 calc R . . C31 C 0.3986(4) 0.66199(16) 0.1010(2) 0.0195(8) Uani 1 1 d . . . C32 C 0.5503(5) 0.68719(18) 0.1144(2) 0.0272(9) Uani 1 1 d . . . H32A H 0.6368 0.6663 0.1421 0.033 Uiso 1 1 calc R . . C33 C 0.5752(6) 0.74230(19) 0.0875(2) 0.0348(10) Uani 1 1 d . . . H33A H 0.6781 0.7593 0.0974 0.042 Uiso 1 1 calc R . . C34 C 0.4508(6) 0.7725(2) 0.0463(3) 0.0420(12) Uani 1 1 d . . . H34A H 0.4677 0.8106 0.0290 0.050 Uiso 1 1 calc R . . C35 C 0.3003(6) 0.7474(2) 0.0301(2) 0.0379(11) Uani 1 1 d . . . H35A H 0.2155 0.7679 0.0003 0.045 Uiso 1 1 calc R . . C36 C 0.2749(5) 0.69269(19) 0.0575(2) 0.0292(10) Uani 1 1 d . . . H36A H 0.1720 0.6757 0.0466 0.035 Uiso 1 1 calc R . . C37 C 0.5571(4) 0.55997(18) 0.1622(2) 0.0239(8) Uani 1 1 d . . . H37A H 0.6181 0.5652 0.1155 0.036 Uiso 1 1 calc R . . H37B H 0.5480 0.5190 0.1737 0.036 Uiso 1 1 calc R . . H37C H 0.6123 0.5793 0.2098 0.036 Uiso 1 1 calc R . . C38 C 0.2900(5) 0.55392(18) 0.0430(2) 0.0245(9) Uani 1 1 d . . . H38A H 0.3692 0.5596 0.0044 0.037 Uiso 1 1 calc R . . H38B H 0.1868 0.5698 0.0201 0.037 Uiso 1 1 calc R . . H38C H 0.2782 0.5129 0.0532 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.00933(6) 0.01483(9) 0.01630(7) 0.00008(6) 0.00026(4) 0.00072(6) Cl1 0.0155(4) 0.0228(5) 0.0286(4) -0.0003(4) 0.0075(3) 0.0001(4) Cl2 0.0138(4) 0.0263(6) 0.0242(4) 0.0018(4) -0.0046(3) 0.0029(4) P1 0.0105(4) 0.0170(6) 0.0244(4) -0.0013(4) -0.0005(3) 0.0007(4) P2 0.0129(4) 0.0165(6) 0.0184(4) -0.0002(4) 0.0022(3) 0.0007(4) P3 0.0129(4) 0.0177(6) 0.0187(4) -0.0009(4) 0.0018(3) 0.0011(4) C1 0.0127(15) 0.014(2) 0.0209(16) -0.0008(15) 0.0011(13) 0.0001(14) C2 0.0189(17) 0.021(2) 0.0253(18) 0.0035(16) -0.0010(14) 0.0007(15) C3 0.0274(19) 0.013(2) 0.0234(17) 0.0069(16) -0.0008(14) 0.0028(15) C4 0.0254(19) 0.029(3) 0.0268(19) 0.0038(18) -0.0020(15) 0.0001(17) C5 0.033(2) 0.038(3) 0.029(2) 0.010(2) 0.0054(17) 0.009(2) C6 0.050(3) 0.029(3) 0.0226(19) -0.0002(18) 0.0006(18) 0.010(2) C7 0.043(2) 0.023(3) 0.0264(19) 0.0026(18) -0.0089(17) -0.0075(19) C8 0.0266(19) 0.020(2) 0.0267(18) 0.0028(17) -0.0054(15) -0.0009(16) C11 0.0146(16) 0.013(2) 0.0224(17) 0.0016(15) 0.0009(13) 0.0025(14) C12 0.0162(16) 0.015(2) 0.0226(16) -0.0025(15) -0.0002(13) 0.0006(14) C13 0.0188(17) 0.020(2) 0.0241(18) 0.0052(16) 0.0036(14) 0.0052(16) C14 0.0259(19) 0.018(2) 0.0253(18) 0.0001(16) 0.0089(15) 0.0067(16) C15 0.031(2) 0.022(2) 0.0225(18) -0.0042(17) -0.0004(15) 0.0003(17) C16 0.0180(17) 0.024(2) 0.0276(18) -0.0017(17) -0.0062(14) 0.0027(16) C17 0.0243(18) 0.013(2) 0.0311(19) -0.0005(17) 0.0083(15) -0.0009(16) C18 0.0154(17) 0.025(2) 0.042(2) -0.0061(19) -0.0029(15) -0.0011(16) C21 0.0199(17) 0.015(2) 0.0198(17) -0.0044(15) 0.0041(13) -0.0068(15) C22 0.0200(18) 0.015(2) 0.0241(17) 0.0005(16) 0.0004(14) 0.0011(15) C23 0.0179(17) 0.021(2) 0.032(2) -0.0029(18) -0.0007(15) 0.0012(16) C24 0.0197(18) 0.024(3) 0.039(2) -0.0043(18) 0.0022(16) -0.0091(16) C25 0.032(2) 0.013(2) 0.061(3) 0.000(2) 0.003(2) -0.0063(18) C26 0.0216(19) 0.020(2) 0.048(2) 0.001(2) 0.0038(17) 0.0050(17) C27 0.0189(17) 0.017(2) 0.0255(18) 0.0009(16) 0.0012(14) 0.0069(15) C28 0.0227(18) 0.024(2) 0.0231(18) -0.0037(17) 0.0074(14) -0.0010(16) C31 0.0255(18) 0.020(2) 0.0149(15) -0.0040(15) 0.0108(13) 0.0029(16) C32 0.040(2) 0.024(3) 0.0204(18) -0.0040(17) 0.0144(16) -0.0040(18) C33 0.055(3) 0.025(3) 0.028(2) -0.0060(19) 0.0229(19) -0.013(2) C34 0.076(4) 0.017(3) 0.040(2) 0.002(2) 0.039(2) 0.001(2) C35 0.055(3) 0.031(3) 0.032(2) 0.014(2) 0.023(2) 0.021(2) C36 0.035(2) 0.031(3) 0.0242(19) 0.0043(18) 0.0143(16) 0.0098(19) C37 0.0126(16) 0.028(2) 0.0320(19) 0.0051(18) 0.0060(14) 0.0036(16) C38 0.031(2) 0.022(2) 0.0212(17) -0.0062(17) 0.0035(15) -0.0019(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.768(3) . ? Re1 P3 2.3911(13) . ? Re1 P1 2.4194(15) . ? Re1 P2 2.4383(15) . ? Re1 Cl1 2.5021(13) . ? Re1 Cl2 2.5431(12) . ? P1 C17 1.817(4) . ? P1 C18 1.818(4) . ? P1 C11 1.825(4) . ? P2 C28 1.821(4) . ? P2 C27 1.827(3) . ? P2 C21 1.832(4) . ? P3 C37 1.826(4) . ? P3 C31 1.829(4) . ? P3 C38 1.836(4) . ? C1 C2 1.478(4) . ? C2 C3 1.511(5) . ? C3 C4 1.387(5) . ? C3 C8 1.399(5) . ? C4 C5 1.382(6) . ? C5 C6 1.389(6) . ? C6 C7 1.376(6) . ? C7 C8 1.384(6) . ? C11 C16 1.399(5) . ? C11 C12 1.404(4) . ? C12 C13 1.380(5) . ? C13 C14 1.389(5) . ? C14 C15 1.383(5) . ? C15 C16 1.384(5) . ? C21 C22 1.380(5) . ? C21 C26 1.381(5) . ? C22 C23 1.378(5) . ? C23 C24 1.373(5) . ? C24 C25 1.380(6) . ? C25 C26 1.384(5) . ? C31 C36 1.396(5) . ? C31 C32 1.399(5) . ? C32 C33 1.385(5) . ? C33 C34 1.377(6) . ? C34 C35 1.393(7) . ? C35 C36 1.380(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 C1 Re1 P3 93.26(12) . . ? C1 Re1 P1 89.87(12) . . ? P3 Re1 P1 97.36(3) . . ? C1 Re1 P2 93.33(12) . . ? P3 Re1 P2 94.84(3) . . ? P1 Re1 P2 167.19(3) . . ? C1 Re1 Cl1 100.36(12) . . ? P3 Re1 Cl1 166.34(3) . . ? P1 Re1 Cl1 81.73(3) . . ? P2 Re1 Cl1 85.50(3) . . ? C1 Re1 Cl2 175.34(11) . . ? P3 Re1 Cl2 82.74(5) . . ? P1 Re1 Cl2 88.29(4) . . ? P2 Re1 Cl2 89.40(3) . . ? Cl1 Re1 Cl2 83.61(5) . . ? C17 P1 C18 103.24(19) . . ? C17 P1 C11 101.13(18) . . ? C18 P1 C11 104.54(17) . . ? C17 P1 Re1 110.52(13) . . ? C18 P1 Re1 114.46(14) . . ? C11 P1 Re1 120.84(12) . . ? C28 P2 C27 102.00(17) . . ? C28 P2 C21 98.39(16) . . ? C27 P2 C21 104.81(18) . . ? C28 P2 Re1 113.47(13) . . ? C27 P2 Re1 116.21(13) . . ? C21 P2 Re1 119.23(12) . . ? C37 P3 C31 102.94(18) . . ? C37 P3 C38 100.93(18) . . ? C31 P3 C38 100.39(17) . . ? C37 P3 Re1 115.89(13) . . ? C31 P3 Re1 117.83(11) . . ? C38 P3 Re1 116.23(13) . . ? C2 C1 Re1 177.6(3) . . ? C1 C2 C3 110.6(3) . . ? C4 C3 C8 118.2(4) . . ? C4 C3 C2 120.2(3) . . ? C8 C3 C2 121.5(3) . . ? C5 C4 C3 121.3(4) . . ? C4 C5 C6 119.8(4) . . ? C7 C6 C5 119.8(4) . . ? C6 C7 C8 120.3(4) . . ? C7 C8 C3 120.6(4) . . ? C16 C11 C12 118.3(3) . . ? C16 C11 P1 123.2(3) . . ? C12 C11 P1 118.5(3) . . ? C13 C12 C11 120.3(3) . . ? C12 C13 C14 121.0(3) . . ? C15 C14 C13 119.0(3) . . ? C14 C15 C16 120.8(3) . . ? C15 C16 C11 120.6(3) . . ? C22 C21 C26 117.8(3) . . ? C22 C21 P2 119.5(3) . . ? C26 C21 P2 122.5(3) . . ? C23 C22 C21 122.1(4) . . ? C24 C23 C22 119.5(3) . . ? C23 C24 C25 119.6(4) . . ? C24 C25 C26 120.4(4) . . ? C21 C26 C25 120.7(4) . . ? C36 C31 C32 118.7(4) . . ? C36 C31 P3 119.1(3) . . ? C32 C31 P3 122.2(3) . . ? C33 C32 C31 120.4(4) . . ? C34 C33 C32 120.1(4) . . ? C33 C34 C35 120.3(4) . . ? C36 C35 C34 119.7(4) . . ? C35 C36 C31 120.8(4) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.815 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.104 #===END data_he10-complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H42 Cl4 P3 Re' _chemical_formula_weight 859.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 23.7835(15) _cell_length_b 13.8111(9) _cell_length_c 11.2713(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3702.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2984 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 24.71 _exptl_crystal_description 'block' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 3.722 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18749 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3677 _reflns_number_gt 3007 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3677 _refine_ls_number_parameters 203 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.633509(12) 0.2500 0.48867(3) 0.02028(13) Uani 1 2 d S . . Cl1 Cl 0.58419(9) 0.2500 0.29362(18) 0.0315(5) Uani 1 2 d S . . Cl2 Cl 0.71451(8) 0.2500 0.3510(2) 0.0356(5) Uani 1 2 d S . . P1 P 0.62850(6) 0.07491(12) 0.46671(16) 0.0291(4) Uani 1 1 d . . . P2 P 0.71428(8) 0.2500 0.6187(2) 0.0251(5) Uani 1 2 d S . . C1 C 0.5971(3) 0.2500 0.6639(7) 0.0234(17) Uani 1 2 d SU . . H1A H 0.5998 0.3085 0.7094 0.028 Uiso 1 1 d R A . C2 C 0.5606(3) 0.2500 0.5654(7) 0.0209(16) Uani 1 2 d S . . C3 C 0.5007(3) 0.2500 0.5633(7) 0.0208(16) Uani 1 2 d S . . C4 C 0.4669(4) 0.2500 0.4605(8) 0.0299(19) Uani 1 2 d S A . H4A H 0.4846 0.2500 0.3849 0.036 Uiso 1 2 calc SR . . C5 C 0.4092(4) 0.2500 0.4664(10) 0.037(2) Uani 1 2 d S . . H5A H 0.3878 0.2500 0.3952 0.045 Uiso 1 2 calc SR A . C6 C 0.3820(4) 0.2500 0.5743(9) 0.035(2) Uani 1 2 d S A . H6A H 0.3421 0.2500 0.5773 0.042 Uiso 1 2 calc SR . . C7 C 0.4131(3) 0.2500 0.6791(10) 0.037(2) Uani 1 2 d S . . H7A H 0.3944 0.2500 0.7536 0.045 Uiso 1 2 calc SR A . C8 C 0.4715(3) 0.2500 0.6746(9) 0.0305(19) Uani 1 2 d S A . H8A H 0.4924 0.2500 0.7464 0.037 Uiso 1 2 calc SR . . C11 C 0.6331(4) -0.0008(8) 0.5879(10) 0.022(3) Uiso 0.60 1 d PD A 1 C12 C 0.5877(5) -0.0001(9) 0.6670(9) 0.029(3) Uiso 0.60 1 d PD A 1 H12A H 0.5553 0.0375 0.6496 0.035 Uiso 0.60 1 calc PR A 1 C13 C 0.5899(5) -0.0541(9) 0.7708(11) 0.049(4) Uiso 0.60 1 d PD A 1 H13A H 0.5595 -0.0517 0.8255 0.059 Uiso 0.60 1 calc PR A 1 C14 C 0.6366(5) -0.1119(9) 0.7949(11) 0.049(3) Uiso 0.60 1 d PD A 1 H14A H 0.6381 -0.1494 0.8655 0.059 Uiso 0.60 1 calc PR A 1 C15 C 0.6810(5) -0.1140(9) 0.7141(11) 0.045(3) Uiso 0.60 1 d PD A 1 H15A H 0.7127 -0.1537 0.7299 0.054 Uiso 0.60 1 calc PR A 1 C16 C 0.6796(5) -0.0590(8) 0.6112(11) 0.040(3) Uiso 0.60 1 d PD A 1 H16A H 0.7102 -0.0611 0.5570 0.048 Uiso 0.60 1 calc PR A 1 C11A C 0.6248(6) 0.0060(11) 0.6237(16) 0.018(3) Uiso 0.40 1 d P A 2 C12A C 0.5776(8) 0.0183(13) 0.6903(16) 0.027(4) Uiso 0.40 1 d P A 2 H12B H 0.5494 0.0629 0.6665 0.033 Uiso 0.40 1 calc PR A 2 C13A C 0.5716(8) -0.0332(13) 0.7896(15) 0.032(4) Uiso 0.40 1 d P A 2 H13B H 0.5372 -0.0300 0.8325 0.039 Uiso 0.40 1 calc PR A 2 C14A C 0.6152(8) -0.0916(13) 0.8311(17) 0.040(4) Uiso 0.40 1 d P A 2 H14B H 0.6113 -0.1233 0.9055 0.048 Uiso 0.40 1 calc PR A 2 C15A C 0.6645(6) -0.1047(9) 0.7658(13) 0.017(3) Uiso 0.40 1 d P A 2 H15B H 0.6940 -0.1447 0.7943 0.020 Uiso 0.40 1 calc PR A 2 C16A C 0.6689(6) -0.0569(10) 0.6570(13) 0.016(3) Uiso 0.40 1 d P A 2 H16B H 0.7005 -0.0665 0.6069 0.019 Uiso 0.40 1 calc PR A 2 C17 C 0.6801(3) 0.0180(6) 0.3713(9) 0.061(2) Uani 1 1 d . A . H17A H 0.6738 -0.0521 0.3699 0.091 Uiso 1 1 calc R . . H17B H 0.7180 0.0314 0.4016 0.091 Uiso 1 1 calc R . . H17C H 0.6766 0.0440 0.2907 0.091 Uiso 1 1 calc R . . C18 C 0.5631(3) 0.0326(5) 0.3997(6) 0.0328(14) Uani 1 1 d . A . H18A H 0.5620 -0.0383 0.4015 0.049 Uiso 1 1 calc R . . H18B H 0.5611 0.0550 0.3173 0.049 Uiso 1 1 calc R . . H18C H 0.5311 0.0585 0.4443 0.049 Uiso 1 1 calc R . . C21 C 0.7048(4) 0.2617(10) 0.7798(7) 0.027(2) Uiso 0.50 1 d PD A -1 C22 C 0.7033(7) 0.1792(10) 0.8491(10) 0.038(4) Uiso 0.50 1 d PD A -1 H22A H 0.7095 0.1180 0.8127 0.045 Uiso 0.50 1 calc PR A -1 C23 C 0.6932(7) 0.1831(8) 0.9705(10) 0.044(4) Uiso 0.50 1 d PD A -1 H23A H 0.6914 0.1255 1.0164 0.053 Uiso 0.50 1 calc PR A -1 C24 C 0.6857(5) 0.2727(7) 1.0232(9) 0.041(3) Uiso 0.50 1 d PD A -1 H24A H 0.6780 0.2769 1.1057 0.049 Uiso 0.50 1 calc PR A -1 C25 C 0.6895(6) 0.3562(8) 0.9557(9) 0.039(3) Uiso 0.50 1 d PD A -1 H25A H 0.6865 0.4179 0.9925 0.046 Uiso 0.50 1 calc PR A -1 C26 C 0.6978(6) 0.3497(11) 0.8348(10) 0.030(3) Uiso 0.50 1 d PD A -1 H26A H 0.6986 0.4072 0.7886 0.037 Uiso 0.50 1 calc PR A -1 C27 C 0.7642(2) 0.1496(5) 0.6016(6) 0.0329(14) Uani 1 1 d . A . H27A H 0.7961 0.1592 0.6555 0.049 Uiso 1 1 calc R . . H27B H 0.7778 0.1476 0.5196 0.049 Uiso 1 1 calc R . . H27C H 0.7454 0.0884 0.6208 0.049 Uiso 1 1 calc R . . C1S C 0.5409(13) 0.2500 0.993(2) 0.070(7) Uiso 0.50 2 d SPD . 1 Cl11 Cl 0.5140(4) 0.1291(7) 0.9649(7) 0.121(2) Uiso 0.50 1 d PD . 1 C2S C 0.5446(14) 0.110(2) 1.004(3) 0.065(10) Uiso 0.25 1 d PD B -2 Cl21 Cl 0.5823(6) 0.0094(11) 1.0807(14) 0.118(5) Uiso 0.25 1 d PD B -2 Cl22 Cl 0.4810(5) 0.1770(9) 0.9813(10) 0.081(3) Uiso 0.25 1 d PD B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01361(19) 0.0265(2) 0.02075(19) 0.000 -0.00087(12) 0.000 Cl1 0.0276(11) 0.0451(13) 0.0218(10) 0.000 -0.0042(8) 0.000 Cl2 0.0230(11) 0.0503(14) 0.0333(12) 0.000 0.0075(8) 0.000 P1 0.0178(8) 0.0295(9) 0.0399(9) -0.0060(7) -0.0011(6) 0.0006(6) P2 0.0141(10) 0.0316(12) 0.0297(11) 0.000 -0.0034(8) 0.000 C1 0.012(3) 0.036(4) 0.023(4) 0.000 0.006(3) 0.000 C2 0.018(4) 0.018(4) 0.026(4) 0.000 0.001(3) 0.000 C3 0.016(4) 0.016(4) 0.030(4) 0.000 -0.005(3) 0.000 C4 0.026(4) 0.030(5) 0.034(5) 0.000 -0.005(4) 0.000 C5 0.023(5) 0.034(5) 0.056(6) 0.000 -0.013(4) 0.000 C6 0.019(4) 0.028(5) 0.059(7) 0.000 0.003(4) 0.000 C7 0.018(4) 0.038(5) 0.055(6) 0.000 0.010(4) 0.000 C8 0.018(4) 0.032(5) 0.042(5) 0.000 0.006(4) 0.000 C17 0.033(4) 0.047(5) 0.103(7) -0.027(5) 0.017(4) -0.004(3) C18 0.033(3) 0.030(3) 0.036(4) 0.000(3) -0.007(3) -0.003(3) C27 0.020(3) 0.030(3) 0.048(4) 0.002(3) -0.004(3) 0.002(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 Re1 C2 1.937(8) . ? Re1 C1 2.156(7) . ? Re1 P2 2.416(2) . ? Re1 P1 2.4338(17) . ? Re1 P1 2.4338(17) 8_565 ? Re1 Cl2 2.474(2) . ? Re1 Cl1 2.492(2) . ? P1 C11 1.724(10) . ? P1 C17 1.812(7) . ? P1 C18 1.825(6) . ? P1 C11A 2.011(17) . ? P2 C27 1.836(6) . ? P2 C27 1.836(6) 8_565 ? P2 C21 1.838(8) 8_565 ? P2 C21 1.838(8) . ? C1 C2 1.409(11) . ? C2 C3 1.427(10) . ? C3 C4 1.409(12) . ? C3 C8 1.434(12) . ? C4 C5 1.374(13) . ? C5 C6 1.378(15) . ? C6 C7 1.394(14) . ? C7 C8 1.389(11) . ? C11 C16 1.394(11) . ? C11 C12 1.400(11) . ? C12 C13 1.388(11) . ? C13 C14 1.395(12) . ? C14 C15 1.395(12) . ? C15 C16 1.386(11) . ? C11A C12A 1.36(2) . ? C11A C16A 1.413(19) . ? C12A C13A 1.33(2) . ? C13A C14A 1.40(2) . ? C14A C15A 1.39(2) . ? C15A C16A 1.40(2) . ? C21 C26 1.374(18) . ? C21 C22 1.382(13) . ? C22 C23 1.392(12) . ? C23 C24 1.383(12) . ? C24 C25 1.385(12) . ? C25 C26 1.379(12) . ? C1S Cl11 1.816(14) . ? C1S Cl11 1.816(14) 8_565 ? C2S Cl22 1.79(2) . ? C2S Cl21 1.87(2) . ? 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 C2 Re1 C1 39.8(3) . . ? C2 Re1 P2 116.2(2) . . ? C1 Re1 P2 76.3(2) . . ? C2 Re1 P1 90.09(5) . . ? C1 Re1 P1 94.21(5) . . ? P2 Re1 P1 95.77(4) . . ? C2 Re1 P1 90.09(5) . 8_565 ? C1 Re1 P1 94.21(5) . 8_565 ? P2 Re1 P1 95.77(4) . 8_565 ? P1 Re1 P1 167.04(8) . 8_565 ? C2 Re1 Cl2 167.6(2) . . ? C1 Re1 Cl2 152.5(2) . . ? P2 Re1 Cl2 76.20(8) . . ? P1 Re1 Cl2 88.53(4) . . ? P1 Re1 Cl2 88.53(4) 8_565 . ? C2 Re1 Cl1 88.4(2) . . ? C1 Re1 Cl1 128.3(2) . . ? P2 Re1 Cl1 155.42(7) . . ? P1 Re1 Cl1 83.53(4) . . ? P1 Re1 Cl1 83.53(4) 8_565 . ? Cl2 Re1 Cl1 79.22(7) . . ? C11 P1 C17 99.5(5) . . ? C11 P1 C18 100.9(4) . . ? C17 P1 C18 101.1(3) . . ? C11 P1 C11A 11.0(5) . . ? C17 P1 C11A 110.3(6) . . ? C18 P1 C11A 100.1(5) . . ? C11 P1 Re1 121.2(4) . . ? C17 P1 Re1 117.3(3) . . ? C18 P1 Re1 113.7(2) . . ? C11A P1 Re1 112.5(5) . . ? C27 P2 C27 98.1(4) . 8_565 ? C27 P2 C21 96.7(4) . 8_565 ? C27 P2 C21 104.5(4) 8_565 8_565 ? C27 P2 C21 104.5(4) . . ? C27 P2 C21 96.7(4) 8_565 . ? C21 P2 C21 10.1(9) 8_565 . ? C27 P2 Re1 116.8(2) . . ? C27 P2 Re1 116.8(2) 8_565 . ? C21 P2 Re1 120.1(3) 8_565 . ? C21 P2 Re1 120.1(3) . . ? C2 C1 Re1 61.7(4) . . ? C1 C2 C3 129.0(7) . . ? C1 C2 Re1 78.5(4) . . ? C3 C2 Re1 152.6(6) . . ? C4 C3 C2 125.6(8) . . ? C4 C3 C8 116.4(7) . . ? C2 C3 C8 118.0(7) . . ? C5 C4 C3 121.9(9) . . ? C4 C5 C6 120.8(9) . . ? C5 C6 C7 120.0(8) . . ? C8 C7 C6 119.9(9) . . ? C7 C8 C3 121.0(9) . . ? C16 C11 C12 119.8(9) . . ? C16 C11 P1 123.3(8) . . ? C12 C11 P1 116.9(7) . . ? C13 C12 C11 120.3(9) . . ? C12 C13 C14 120.1(9) . . ? C13 C14 C15 119.2(8) . . ? C16 C15 C14 121.2(9) . . ? C15 C16 C11 119.5(10) . . ? C12A C11A C16A 122.8(15) . . ? C12A C11A P1 117.6(11) . . ? C16A C11A P1 119.5(12) . . ? C13A C12A C11A 119.1(17) . . ? C12A C13A C14A 120.6(18) . . ? C15A C14A C13A 121.5(16) . . ? C14A C15A C16A 117.7(13) . . ? C15A C16A C11A 118.0(14) . . ? C26 C21 C22 118.2(9) . . ? C26 C21 P2 122.6(9) . . ? C22 C21 P2 119.2(10) . . ? C21 C22 C23 121.8(10) . . ? C24 C23 C22 118.7(9) . . ? C23 C24 C25 120.1(8) . . ? C26 C25 C24 119.8(9) . . ? C21 C26 C25 121.3(11) . . ? Cl11 C1S Cl11 133.7(18) . 8_565 ? Cl22 C2S Cl21 149(2) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.801 _refine_diff_density_min -1.527 _refine_diff_density_rms 0.146 #===END data_he25-complex8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H45 Cl5 P3 Re' _chemical_formula_weight 982.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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 10.1416(4) _cell_length_b 19.4068(8) _cell_length_c 20.9570(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.468(2) _cell_angle_gamma 90.00 _cell_volume 4112.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5059 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.30 _exptl_crystal_description 'bar' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 3.425 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22835 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7955 _reflns_number_gt 6853 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7955 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0478 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.290808(10) 0.275191(5) 0.457087(4) 0.01130(4) Uani 1 1 d . . . Cl1 Cl 0.48136(7) 0.29371(4) 0.54137(3) 0.02039(15) Uani 1 1 d . . . Cl2 Cl 0.17993(6) 0.22671(3) 0.54670(3) 0.01770(14) Uani 1 1 d . . . P1 P 0.19022(7) 0.38164(4) 0.49081(3) 0.01561(15) Uani 1 1 d . . . P2 P 0.45068(7) 0.32593(4) 0.39419(3) 0.01376(14) Uani 1 1 d . . . P3 P 0.36495(7) 0.15680(4) 0.44171(3) 0.01552(15) Uani 1 1 d . . . C1 C 0.1708(3) 0.27056(13) 0.39135(12) 0.0135(5) Uani 1 1 d . . . C2 C 0.0832(3) 0.27258(13) 0.33464(12) 0.0143(5) Uani 1 1 d . . . H2A H 0.0992 0.3076 0.3046 0.017 Uiso 1 1 calc R . . C3 C -0.0204(3) 0.23001(14) 0.31894(12) 0.0142(5) Uani 1 1 d . . . C11 C 0.1769(3) 0.45658(13) 0.43766(12) 0.0152(6) Uani 1 1 d . . . C12 C 0.0859(3) 0.45690(14) 0.38460(12) 0.0196(6) Uani 1 1 d . . . H12A H 0.0297 0.4182 0.3765 0.024 Uiso 1 1 calc R . . C13 C 0.0757(3) 0.51234(15) 0.34352(13) 0.0226(6) Uani 1 1 d . . . H13A H 0.0112 0.5121 0.3081 0.027 Uiso 1 1 calc R . . C14 C 0.1594(3) 0.56859(14) 0.35366(13) 0.0213(6) Uani 1 1 d . . . H14A H 0.1538 0.6063 0.3247 0.026 Uiso 1 1 calc R . . C15 C 0.2507(3) 0.56937(14) 0.40601(13) 0.0207(6) Uani 1 1 d . . . H15A H 0.3077 0.6079 0.4134 0.025 Uiso 1 1 calc R . . C16 C 0.2593(3) 0.51391(14) 0.44780(12) 0.0188(6) Uani 1 1 d . . . H16A H 0.3222 0.5149 0.4839 0.023 Uiso 1 1 calc R . . C17 C 0.0168(3) 0.37189(16) 0.50620(14) 0.0260(7) Uani 1 1 d . . . H17A H -0.0180 0.4163 0.5196 0.039 Uiso 1 1 calc R . . H17B H 0.0089 0.3378 0.5402 0.039 Uiso 1 1 calc R . . H17C H -0.0338 0.3563 0.4671 0.039 Uiso 1 1 calc R . . C18 C 0.2609(3) 0.41618(16) 0.56666(13) 0.0289(7) Uani 1 1 d . . . H18A H 0.2148 0.4588 0.5765 0.043 Uiso 1 1 calc R . . H18B H 0.3550 0.4259 0.5636 0.043 Uiso 1 1 calc R . . H18C H 0.2509 0.3824 0.6007 0.043 Uiso 1 1 calc R . . C21 C 0.3948(3) 0.34263(13) 0.31080(12) 0.0148(6) Uani 1 1 d . . . C22 C 0.4030(3) 0.29198(14) 0.26373(13) 0.0184(6) Uani 1 1 d . . . H22A H 0.4454 0.2494 0.2744 0.022 Uiso 1 1 calc R . . C23 C 0.3502(3) 0.30320(16) 0.20202(13) 0.0216(6) Uani 1 1 d . . . H23A H 0.3576 0.2688 0.1703 0.026 Uiso 1 1 calc R . . C24 C 0.2862(3) 0.36491(15) 0.18618(13) 0.0226(6) Uani 1 1 d . . . H24A H 0.2483 0.3724 0.1439 0.027 Uiso 1 1 calc R . . C25 C 0.2779(3) 0.41528(16) 0.23224(13) 0.0248(7) Uani 1 1 d . . . H25A H 0.2344 0.4576 0.2215 0.030 Uiso 1 1 calc R . . C26 C 0.3327(3) 0.40444(14) 0.29409(12) 0.0199(6) Uani 1 1 d . . . H26A H 0.3277 0.4397 0.3253 0.024 Uiso 1 1 calc R . . C27 C 0.5206(3) 0.40843(14) 0.42096(13) 0.0188(6) Uani 1 1 d . . . H27A H 0.5847 0.4238 0.3913 0.028 Uiso 1 1 calc R . . H27B H 0.5651 0.4033 0.4639 0.028 Uiso 1 1 calc R . . H27C H 0.4497 0.4426 0.4221 0.028 Uiso 1 1 calc R . . C28 C 0.6052(3) 0.27907(14) 0.38983(13) 0.0192(6) Uani 1 1 d . . . H28A H 0.6631 0.3046 0.3629 0.029 Uiso 1 1 calc R . . H28B H 0.5867 0.2334 0.3713 0.029 Uiso 1 1 calc R . . H28C H 0.6489 0.2740 0.4329 0.029 Uiso 1 1 calc R . . C31 C 0.3981(3) 0.12971(13) 0.36113(12) 0.0168(6) Uani 1 1 d . . . C32 C 0.2932(3) 0.12959(14) 0.31358(13) 0.0197(6) Uani 1 1 d . . . H32A H 0.2075 0.1427 0.3243 0.024 Uiso 1 1 calc R . . C33 C 0.3119(3) 0.11071(15) 0.25104(13) 0.0245(7) Uani 1 1 d . . . H33A H 0.2394 0.1107 0.2195 0.029 Uiso 1 1 calc R . . C34 C 0.4364(3) 0.09202(15) 0.23490(14) 0.0261(7) Uani 1 1 d . . . H34A H 0.4502 0.0801 0.1920 0.031 Uiso 1 1 calc R . . C35 C 0.5409(3) 0.09065(15) 0.28125(14) 0.0241(7) Uani 1 1 d . . . H35A H 0.6261 0.0770 0.2700 0.029 Uiso 1 1 calc R . . C36 C 0.5230(3) 0.10889(14) 0.34393(13) 0.0187(6) Uani 1 1 d . . . H36A H 0.5956 0.1073 0.3754 0.022 Uiso 1 1 calc R . . C37 C 0.2447(3) 0.09100(14) 0.46003(13) 0.0225(6) Uani 1 1 d . . . H37A H 0.2814 0.0452 0.4528 0.034 Uiso 1 1 calc R . . H37B H 0.1633 0.0973 0.4323 0.034 Uiso 1 1 calc R . . H37C H 0.2249 0.0952 0.5049 0.034 Uiso 1 1 calc R . . C38 C 0.5093(3) 0.12937(15) 0.49174(13) 0.0242(7) Uani 1 1 d . . . H38A H 0.5302 0.0815 0.4817 0.036 Uiso 1 1 calc R . . H38B H 0.4911 0.1329 0.5369 0.036 Uiso 1 1 calc R . . H38C H 0.5846 0.1589 0.4837 0.036 Uiso 1 1 calc R . . C41 C -0.0636(2) 0.17663(14) 0.36409(12) 0.0139(5) Uani 1 1 d . . . C42 C -0.0913(3) 0.10938(14) 0.34292(12) 0.0164(6) Uani 1 1 d . . . H42A H -0.0859 0.0982 0.2991 0.020 Uiso 1 1 calc R . . C43 C -0.1264(3) 0.05887(15) 0.38534(13) 0.0201(6) Uani 1 1 d . . . H43A H -0.1441 0.0133 0.3705 0.024 Uiso 1 1 calc R . . C44 C -0.1359(3) 0.07475(15) 0.44929(13) 0.0210(6) Uani 1 1 d . . . H44A H -0.1598 0.0402 0.4783 0.025 Uiso 1 1 calc R . . C45 C -0.1104(3) 0.14130(15) 0.47056(13) 0.0215(6) Uani 1 1 d . . . H45A H -0.1186 0.1525 0.5142 0.026 Uiso 1 1 calc R . . C46 C -0.0732(3) 0.19168(14) 0.42878(12) 0.0161(6) Uani 1 1 d . . . H46A H -0.0539 0.2369 0.4442 0.019 Uiso 1 1 calc R . . C51 C -0.0907(3) 0.23471(13) 0.25457(12) 0.0132(5) Uani 1 1 d . . . C52 C -0.0236(3) 0.25173(14) 0.20117(13) 0.0159(6) Uani 1 1 d . . . H52A H 0.0694 0.2587 0.2059 0.019 Uiso 1 1 calc R . . C53 C -0.0904(3) 0.25864(14) 0.14116(13) 0.0172(6) Uani 1 1 d . . . H53A H -0.0430 0.2703 0.1053 0.021 Uiso 1 1 calc R . . C54 C -0.2266(3) 0.24862(14) 0.13311(13) 0.0168(6) Uani 1 1 d . . . H54A H -0.2727 0.2541 0.0922 0.020 Uiso 1 1 calc R . . C55 C -0.2943(3) 0.23047(13) 0.18579(12) 0.0160(6) Uani 1 1 d . . . H55A H -0.3871 0.2230 0.1808 0.019 Uiso 1 1 calc R . . C56 C -0.2275(3) 0.22322(13) 0.24527(12) 0.0143(5) Uani 1 1 d . . . H56A H -0.2750 0.2102 0.2807 0.017 Uiso 1 1 calc R . . C1S C 0.2319(3) 0.90907(15) 0.29334(14) 0.0253(7) Uani 1 1 d . . . H1SA H 0.2137 0.8591 0.3003 0.030 Uiso 1 1 calc R . . Cl1S Cl 0.10888(8) 0.95757(5) 0.32714(4) 0.0390(2) Uani 1 1 d . . . Cl2S Cl 0.22808(9) 0.92421(4) 0.21016(4) 0.03655(19) Uani 1 1 d . . . Cl3S Cl 0.38767(8) 0.92832(5) 0.32987(4) 0.0439(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01071(6) 0.01417(6) 0.00885(5) 0.00045(4) -0.00031(4) -0.00060(4) Cl1 0.0164(3) 0.0296(4) 0.0143(3) -0.0002(3) -0.0049(2) -0.0014(3) Cl2 0.0185(3) 0.0220(4) 0.0129(3) 0.0036(3) 0.0035(2) 0.0006(3) P1 0.0184(4) 0.0158(4) 0.0126(3) -0.0006(3) 0.0013(3) 0.0004(3) P2 0.0129(3) 0.0163(4) 0.0119(3) -0.0008(3) 0.0005(3) -0.0018(3) P3 0.0159(4) 0.0158(4) 0.0149(3) 0.0018(3) 0.0018(3) 0.0009(3) C1 0.0129(13) 0.0110(13) 0.0173(13) 0.0013(11) 0.0061(10) -0.0015(10) C2 0.0145(13) 0.0134(13) 0.0149(13) 0.0041(11) 0.0012(10) 0.0007(11) C3 0.0127(13) 0.0178(14) 0.0123(12) -0.0016(11) 0.0025(10) 0.0023(11) C11 0.0173(14) 0.0147(14) 0.0140(12) -0.0022(11) 0.0044(10) 0.0020(11) C12 0.0222(15) 0.0157(15) 0.0207(14) -0.0025(12) -0.0001(11) -0.0023(12) C13 0.0248(16) 0.0245(16) 0.0177(14) -0.0008(12) -0.0036(12) 0.0013(12) C14 0.0267(16) 0.0153(15) 0.0222(14) 0.0025(12) 0.0041(12) 0.0020(12) C15 0.0225(16) 0.0154(15) 0.0246(14) -0.0038(12) 0.0042(12) -0.0030(12) C16 0.0193(15) 0.0182(15) 0.0183(13) -0.0047(11) -0.0020(11) 0.0009(11) C17 0.0234(16) 0.0226(16) 0.0336(16) 0.0050(13) 0.0130(13) 0.0074(13) C18 0.047(2) 0.0272(18) 0.0122(13) -0.0059(13) -0.0028(13) 0.0049(15) C21 0.0132(13) 0.0179(14) 0.0135(12) 0.0000(11) 0.0024(10) -0.0063(11) C22 0.0142(14) 0.0198(15) 0.0215(14) -0.0020(12) 0.0027(11) -0.0024(11) C23 0.0201(15) 0.0272(16) 0.0178(14) -0.0060(12) 0.0038(11) -0.0065(12) C24 0.0244(16) 0.0293(17) 0.0136(13) 0.0026(12) -0.0025(11) -0.0061(13) C25 0.0310(17) 0.0214(16) 0.0213(14) 0.0045(12) -0.0026(12) 0.0024(13) C26 0.0276(16) 0.0174(15) 0.0146(13) -0.0029(11) 0.0021(12) -0.0025(12) C27 0.0159(14) 0.0203(15) 0.0205(14) -0.0058(12) 0.0024(11) -0.0054(11) C28 0.0145(14) 0.0222(15) 0.0209(14) -0.0006(12) 0.0018(11) -0.0018(11) C31 0.0205(15) 0.0110(13) 0.0194(14) -0.0015(11) 0.0048(11) 0.0007(11) C32 0.0181(15) 0.0181(15) 0.0229(14) -0.0003(12) 0.0015(11) 0.0018(11) C33 0.0294(17) 0.0241(17) 0.0195(14) -0.0027(12) -0.0016(12) -0.0025(13) C34 0.0329(18) 0.0236(17) 0.0227(15) -0.0067(13) 0.0083(13) -0.0051(13) C35 0.0234(16) 0.0203(16) 0.0301(16) -0.0040(13) 0.0123(13) -0.0004(12) C36 0.0166(15) 0.0150(14) 0.0242(14) -0.0001(12) 0.0005(11) -0.0009(11) C37 0.0255(16) 0.0145(15) 0.0286(16) 0.0020(12) 0.0087(13) -0.0024(12) C38 0.0261(17) 0.0240(16) 0.0220(15) 0.0050(13) -0.0025(12) 0.0096(13) C41 0.0072(12) 0.0188(14) 0.0155(12) 0.0004(11) 0.0000(10) 0.0015(10) C42 0.0124(13) 0.0218(15) 0.0146(13) -0.0025(11) -0.0018(10) -0.0007(11) C43 0.0195(15) 0.0164(15) 0.0240(15) -0.0006(12) -0.0014(12) -0.0006(12) C44 0.0174(15) 0.0229(16) 0.0226(14) 0.0083(12) 0.0009(11) -0.0027(12) C45 0.0205(15) 0.0301(17) 0.0139(13) 0.0014(12) 0.0012(11) -0.0049(12) C46 0.0128(14) 0.0186(15) 0.0165(13) -0.0029(11) -0.0009(10) -0.0030(11) C51 0.0127(13) 0.0111(14) 0.0159(13) -0.0014(10) 0.0014(10) 0.0009(10) C52 0.0097(13) 0.0185(14) 0.0196(14) -0.0026(11) 0.0011(11) -0.0009(11) C53 0.0188(15) 0.0165(15) 0.0168(13) 0.0003(11) 0.0048(11) -0.0014(11) C54 0.0183(15) 0.0176(14) 0.0139(13) -0.0020(11) -0.0026(11) 0.0011(11) C55 0.0099(13) 0.0180(15) 0.0198(13) -0.0021(12) 0.0000(10) 0.0002(11) C56 0.0150(13) 0.0135(14) 0.0148(13) -0.0008(11) 0.0039(10) -0.0020(11) C1S 0.0247(17) 0.0212(16) 0.0302(16) 0.0011(13) 0.0033(13) 0.0024(12) Cl1S 0.0328(5) 0.0435(5) 0.0420(5) -0.0065(4) 0.0120(4) 0.0098(4) Cl2S 0.0417(5) 0.0395(5) 0.0287(4) -0.0028(4) 0.0047(3) 0.0088(4) Cl3S 0.0279(5) 0.0505(6) 0.0510(5) 0.0083(5) -0.0102(4) -0.0017(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 Re1 C1 1.768(3) . ? Re1 P2 2.3810(7) . ? Re1 P1 2.4332(7) . ? Re1 P3 2.4467(7) . ? Re1 Cl2 2.4507(6) . ? Re1 Cl1 2.5400(6) . ? P1 C18 1.820(3) . ? P1 C17 1.823(3) . ? P1 C11 1.830(3) . ? P2 C28 1.820(3) . ? P2 C27 1.822(3) . ? P2 C21 1.824(3) . ? P3 C38 1.813(3) . ? P3 C31 1.825(3) . ? P3 C37 1.827(3) . ? C1 C2 1.428(4) . ? C2 C3 1.357(4) . ? C3 C51 1.479(4) . ? C3 C41 1.492(3) . ? C11 C12 1.389(4) . ? C11 C16 1.398(4) . ? C12 C13 1.377(4) . ? C13 C14 1.389(4) . ? C14 C15 1.380(4) . ? C15 C16 1.386(4) . ? C21 C26 1.387(4) . ? C21 C22 1.400(4) . ? C22 C23 1.378(4) . ? C23 C24 1.390(4) . ? C24 C25 1.381(4) . ? C25 C26 1.386(4) . ? C31 C32 1.400(4) . ? C31 C36 1.403(4) . ? C32 C33 1.388(4) . ? C33 C34 1.381(4) . ? C34 C35 1.381(4) . ? C35 C36 1.386(4) . ? C41 C46 1.398(3) . ? C41 C42 1.400(4) . ? C42 C43 1.388(4) . ? C43 C44 1.386(4) . ? C44 C45 1.384(4) . ? C45 C46 1.384(4) . ? C51 C52 1.394(4) . ? C51 C56 1.404(4) . ? C52 C53 1.388(4) . ? C53 C54 1.392(4) . ? C54 C55 1.390(4) . ? C55 C56 1.379(4) . ? C1S Cl3S 1.741(3) . ? C1S Cl1S 1.756(3) . ? C1S Cl2S 1.765(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 C1 Re1 P2 92.69(8) . . ? C1 Re1 P1 89.46(8) . . ? P2 Re1 P1 97.39(2) . . ? C1 Re1 P3 92.85(8) . . ? P2 Re1 P3 94.93(2) . . ? P1 Re1 P3 167.34(2) . . ? C1 Re1 Cl2 104.38(8) . . ? P2 Re1 Cl2 162.93(2) . . ? P1 Re1 Cl2 82.86(2) . . ? P3 Re1 Cl2 84.52(2) . . ? C1 Re1 Cl1 171.61(8) . . ? P2 Re1 Cl1 79.19(2) . . ? P1 Re1 Cl1 89.51(2) . . ? P3 Re1 Cl1 89.97(2) . . ? Cl2 Re1 Cl1 83.75(2) . . ? C18 P1 C17 101.74(15) . . ? C18 P1 C11 104.14(13) . . ? C17 P1 C11 99.42(13) . . ? C18 P1 Re1 114.89(11) . . ? C17 P1 Re1 113.29(10) . . ? C11 P1 Re1 120.70(8) . . ? C28 P2 C27 97.95(13) . . ? C28 P2 C21 104.19(12) . . ? C27 P2 C21 102.91(12) . . ? C28 P2 Re1 116.56(9) . . ? C27 P2 Re1 117.29(9) . . ? C21 P2 Re1 115.46(8) . . ? C38 P3 C31 104.59(13) . . ? C38 P3 C37 101.27(14) . . ? C31 P3 C37 99.63(13) . . ? C38 P3 Re1 116.24(10) . . ? C31 P3 Re1 118.24(9) . . ? C37 P3 Re1 114.30(10) . . ? C2 C1 Re1 173.2(2) . . ? C3 C2 C1 127.2(2) . . ? C2 C3 C51 119.5(2) . . ? C2 C3 C41 121.9(2) . . ? C51 C3 C41 118.5(2) . . ? C12 C11 C16 118.1(2) . . ? C12 C11 P1 120.2(2) . . ? C16 C11 P1 121.7(2) . . ? C13 C12 C11 121.1(3) . . ? C12 C13 C14 120.2(3) . . ? C15 C14 C13 119.6(3) . . ? C14 C15 C16 119.9(3) . . ? C15 C16 C11 121.0(2) . . ? C26 C21 C22 118.7(2) . . ? C26 C21 P2 119.79(19) . . ? C22 C21 P2 121.3(2) . . ? C23 C22 C21 120.7(3) . . ? C22 C23 C24 120.0(3) . . ? C25 C24 C23 119.7(3) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 120.6(3) . . ? C32 C31 C36 117.9(2) . . ? C32 C31 P3 118.3(2) . . ? C36 C31 P3 123.8(2) . . ? C33 C32 C31 121.3(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C35 119.9(3) . . ? C34 C35 C36 120.8(3) . . ? C35 C36 C31 120.3(3) . . ? C46 C41 C42 118.4(2) . . ? C46 C41 C3 121.1(2) . . ? C42 C41 C3 120.5(2) . . ? C43 C42 C41 120.7(2) . . ? C44 C43 C42 120.2(3) . . ? C45 C44 C43 119.6(3) . . ? C44 C45 C46 120.6(2) . . ? C45 C46 C41 120.6(3) . . ? C52 C51 C56 117.7(2) . . ? C52 C51 C3 121.1(2) . . ? C56 C51 C3 121.2(2) . . ? C53 C52 C51 121.0(2) . . ? C52 C53 C54 120.4(2) . . ? C55 C54 C53 119.1(2) . . ? C56 C55 C54 120.4(2) . . ? C55 C56 C51 121.3(2) . . ? Cl3S C1S Cl1S 110.89(16) . . ? Cl3S C1S Cl2S 110.36(16) . . ? Cl1S C1S Cl2S 110.33(16) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.972 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.088 #===END data_chen21-complex9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H46 Cl2 O P3 Re' _chemical_formula_weight 880.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 '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 8.1451(10) _cell_length_b 12.1004(10) _cell_length_c 21.0248(13) _cell_angle_alpha 102.461(7) _cell_angle_beta 97.347(7) _cell_angle_gamma 104.028(7) _cell_volume 1927.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7271 _cell_measurement_theta_min 3.89 _cell_measurement_theta_max 71.49 _exptl_crystal_description 'bar' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 8.838 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13102 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 67.50 _reflns_number_total 6576 _reflns_number_gt 5599 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+3.2000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6576 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.23235(4) 0.55210(3) 0.208836(16) 0.02370(13) Uani 1 1 d . . . Cl2 Cl 0.0205(3) 0.61598(18) 0.27312(10) 0.0358(4) Uani 1 1 d . . . Cl1 Cl -0.0306(2) 0.42245(16) 0.12228(9) 0.0300(4) Uani 1 1 d . . . P1 P 0.1998(2) 0.39816(17) 0.26920(9) 0.0257(4) Uani 1 1 d . . . P3 P 0.2146(2) 0.71100(17) 0.15622(9) 0.0264(4) Uani 1 1 d . . . P2 P 0.3828(2) 0.46610(16) 0.13111(9) 0.0228(4) Uani 1 1 d . . . O1 O 0.4636(8) 0.8552(5) 0.3411(3) 0.0374(13) Uani 1 1 d . . . H1 H 0.3782 0.7973 0.3200 0.045 Uiso 1 1 d R . . C1 C 0.4287(10) 0.6353(6) 0.2593(4) 0.0269(15) Uani 1 1 d . . . C2 C 0.6062(9) 0.7129(6) 0.2946(4) 0.0258(15) Uani 1 1 d . . . H2A H 0.6605 0.7549 0.2637 0.031 Uiso 1 1 calc R . . H2B H 0.6781 0.6625 0.3065 0.031 Uiso 1 1 calc R . . C3 C 0.6035(10) 0.8039(7) 0.3577(4) 0.0300(16) Uani 1 1 d . . . C4 C 0.5711(11) 0.7478(7) 0.4144(4) 0.0328(17) Uani 1 1 d . . . C5 C 0.6749(11) 0.6775(8) 0.4324(5) 0.0385(19) Uani 1 1 d . . . H5A H 0.7588 0.6612 0.4070 0.046 Uiso 1 1 calc R . . C6 C 0.6548(13) 0.6319(9) 0.4869(5) 0.045(2) Uani 1 1 d . . . H6A H 0.7245 0.5841 0.4986 0.054 Uiso 1 1 calc R . . C7 C 0.5334(14) 0.6558(9) 0.5245(5) 0.053(3) Uani 1 1 d . . . H7A H 0.5197 0.6241 0.5617 0.063 Uiso 1 1 calc R . . C8 C 0.4348(14) 0.7241(10) 0.5083(5) 0.049(2) Uani 1 1 d . . . H8A H 0.3512 0.7396 0.5339 0.059 Uiso 1 1 calc R . . C9 C 0.4545(12) 0.7725(8) 0.4539(4) 0.0398(19) Uani 1 1 d . . . H9A H 0.3870 0.8229 0.4441 0.048 Uiso 1 1 calc R . . C10 C 0.7692(12) 0.9034(8) 0.3782(4) 0.0381(19) Uani 1 1 d . . . C11 C 0.7694(13) 1.0104(8) 0.4152(6) 0.052(3) Uani 1 1 d . . . H11A H 0.6641 1.0231 0.4254 0.063 Uiso 1 1 calc R . . C12 C 0.9223(16) 1.1028(9) 0.4386(7) 0.069(3) Uani 1 1 d . . . H12A H 0.9201 1.1767 0.4648 0.083 Uiso 1 1 calc R . . C13 C 1.0785(15) 1.0856(10) 0.4231(7) 0.065(3) Uani 1 1 d . . . H13A H 1.1831 1.1471 0.4388 0.078 Uiso 1 1 calc R . . C14 C 1.0764(14) 0.9785(10) 0.3847(6) 0.057(3) Uani 1 1 d . . . H14A H 1.1805 0.9662 0.3728 0.068 Uiso 1 1 calc R . . C15 C 0.9247(12) 0.8870(8) 0.3628(5) 0.046(2) Uani 1 1 d . . . H15A H 0.9270 0.8127 0.3371 0.055 Uiso 1 1 calc R . . C21 C 0.3699(10) 0.3241(7) 0.2823(4) 0.0311(17) Uani 1 1 d . . . C22 C 0.3326(12) 0.2067(8) 0.2799(5) 0.041(2) Uani 1 1 d . . . H22A H 0.2174 0.1579 0.2653 0.050 Uiso 1 1 calc R . . C23 C 0.4650(13) 0.1592(8) 0.2991(5) 0.045(2) Uani 1 1 d . . . H23A H 0.4388 0.0777 0.2977 0.054 Uiso 1 1 calc R . . C24 C 0.6331(12) 0.2281(8) 0.3200(4) 0.0388(19) Uani 1 1 d . . . H24A H 0.7223 0.1947 0.3327 0.047 Uiso 1 1 calc R . . C25 C 0.6703(11) 0.3487(8) 0.3222(5) 0.0381(19) Uani 1 1 d . . . H25A H 0.7853 0.3977 0.3370 0.046 Uiso 1 1 calc R . . C26 C 0.5389(11) 0.3963(7) 0.3029(4) 0.0347(18) Uani 1 1 d . . . H26A H 0.5640 0.4775 0.3037 0.042 Uiso 1 1 calc R . . C27 C 0.0027(10) 0.2779(8) 0.2389(4) 0.0348(18) Uani 1 1 d . . . H27A H 0.0006 0.2210 0.2658 0.052 Uiso 1 1 calc R . . H27B H -0.0016 0.2389 0.1925 0.052 Uiso 1 1 calc R . . H27C H -0.0971 0.3092 0.2421 0.052 Uiso 1 1 calc R . . C28 C 0.1862(10) 0.4533(8) 0.3564(4) 0.0333(17) Uani 1 1 d . . . H28A H 0.1731 0.3886 0.3782 0.050 Uiso 1 1 calc R . . H28B H 0.0866 0.4850 0.3585 0.050 Uiso 1 1 calc R . . H28C H 0.2917 0.5157 0.3791 0.050 Uiso 1 1 calc R . . C31 C 0.3804(10) 0.3110(6) 0.1235(4) 0.0265(15) Uani 1 1 d . . . C32 C 0.2237(11) 0.2239(7) 0.0993(4) 0.0334(17) Uani 1 1 d . . . H32A H 0.1205 0.2456 0.0898 0.040 Uiso 1 1 calc R . . C33 C 0.2182(13) 0.1066(8) 0.0892(5) 0.044(2) Uani 1 1 d . . . H33A H 0.1122 0.0471 0.0716 0.052 Uiso 1 1 calc R . . C34 C 0.3710(14) 0.0761(9) 0.1051(5) 0.050(2) Uani 1 1 d . . . H34A H 0.3686 -0.0044 0.0993 0.061 Uiso 1 1 calc R . . C35 C 0.5250(13) 0.1633(9) 0.1293(5) 0.045(2) Uani 1 1 d . . . H35A H 0.6283 0.1423 0.1399 0.054 Uiso 1 1 calc R . . C36 C 0.5298(12) 0.2772(8) 0.1379(4) 0.0371(18) Uani 1 1 d . . . H36A H 0.6371 0.3359 0.1541 0.045 Uiso 1 1 calc R . . C37 C 0.6093(10) 0.5429(7) 0.1413(4) 0.0292(16) Uani 1 1 d . . . H37A H 0.6598 0.5010 0.1072 0.044 Uiso 1 1 calc R . . H37B H 0.6697 0.5458 0.1853 0.044 Uiso 1 1 calc R . . H37C H 0.6208 0.6233 0.1370 0.044 Uiso 1 1 calc R . . C38 C 0.3097(11) 0.4559(7) 0.0440(4) 0.0342(17) Uani 1 1 d . . . H38A H 0.3813 0.4189 0.0172 0.051 Uiso 1 1 calc R . . H38B H 0.3193 0.5352 0.0379 0.051 Uiso 1 1 calc R . . H38C H 0.1893 0.4083 0.0300 0.051 Uiso 1 1 calc R . . C41 C 0.4135(10) 0.7887(7) 0.1333(4) 0.0280(16) Uani 1 1 d . . . C42 C 0.4369(13) 0.7727(7) 0.0681(5) 0.041(2) Uani 1 1 d . . . H42A H 0.3470 0.7229 0.0329 0.049 Uiso 1 1 calc R . . C43 C 0.5930(15) 0.8303(8) 0.0550(6) 0.053(3) Uani 1 1 d . . . H43A H 0.6101 0.8177 0.0104 0.064 Uiso 1 1 calc R . . C44 C 0.7244(14) 0.9055(9) 0.1051(6) 0.054(3) Uani 1 1 d . . . H44A H 0.8306 0.9435 0.0949 0.064 Uiso 1 1 calc R . . C45 C 0.7005(12) 0.9254(8) 0.1707(6) 0.050(3) Uani 1 1 d . . . H45A H 0.7897 0.9771 0.2056 0.060 Uiso 1 1 calc R . . C46 C 0.5427(10) 0.8678(7) 0.1843(5) 0.0333(18) Uani 1 1 d . . . H46A H 0.5234 0.8826 0.2286 0.040 Uiso 1 1 calc R . . C47 C 0.0543(11) 0.6747(9) 0.0810(5) 0.041(2) Uani 1 1 d . . . H47A H 0.0599 0.7453 0.0647 0.062 Uiso 1 1 calc R . . H47B H -0.0607 0.6455 0.0905 0.062 Uiso 1 1 calc R . . H47C H 0.0771 0.6137 0.0471 0.062 Uiso 1 1 calc R . . C48 C 0.1552(11) 0.8350(8) 0.2054(4) 0.0354(18) Uani 1 1 d . . . H48A H 0.1515 0.8934 0.1798 0.053 Uiso 1 1 calc R . . H48B H 0.2407 0.8714 0.2465 0.053 Uiso 1 1 calc R . . H48C H 0.0415 0.8064 0.2161 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01646(19) 0.03185(19) 0.02090(19) 0.00400(12) -0.00086(12) 0.00795(12) Cl2 0.0347(10) 0.0474(10) 0.0324(10) 0.0095(8) 0.0105(9) 0.0231(9) Cl1 0.0153(8) 0.0402(9) 0.0281(9) 0.0029(7) -0.0019(7) 0.0044(7) P1 0.0199(9) 0.0339(9) 0.0238(9) 0.0086(8) 0.0018(8) 0.0087(7) P3 0.0212(9) 0.0345(9) 0.0218(9) 0.0053(7) -0.0036(8) 0.0102(8) P2 0.0174(9) 0.0288(8) 0.0220(9) 0.0062(7) 0.0015(7) 0.0076(7) O1 0.034(3) 0.044(3) 0.036(3) 0.009(3) 0.000(3) 0.019(3) C1 0.032(4) 0.026(3) 0.023(4) 0.008(3) -0.004(3) 0.014(3) C2 0.022(4) 0.028(3) 0.022(4) 0.003(3) -0.006(3) 0.007(3) C3 0.018(4) 0.039(4) 0.026(4) 0.000(3) -0.007(3) 0.007(3) C4 0.036(4) 0.031(4) 0.023(4) 0.003(3) -0.003(3) 0.002(3) C5 0.029(4) 0.047(5) 0.035(5) 0.005(4) -0.003(4) 0.014(4) C6 0.047(6) 0.054(5) 0.028(5) 0.008(4) -0.008(4) 0.013(4) C7 0.059(7) 0.050(5) 0.044(6) 0.016(5) 0.011(5) 0.003(5) C8 0.048(6) 0.063(6) 0.033(5) 0.010(4) 0.012(5) 0.008(5) C9 0.036(5) 0.052(5) 0.030(4) 0.005(4) 0.004(4) 0.016(4) C10 0.035(5) 0.037(4) 0.030(4) 0.002(3) -0.009(4) 0.003(4) C11 0.039(5) 0.040(5) 0.064(7) -0.002(5) 0.000(5) 0.004(4) C12 0.063(7) 0.039(5) 0.082(9) -0.014(5) -0.001(7) 0.004(5) C13 0.046(6) 0.053(6) 0.070(8) -0.008(6) 0.000(6) -0.006(5) C14 0.038(5) 0.058(6) 0.058(7) -0.003(5) 0.010(5) -0.002(5) C15 0.032(5) 0.047(5) 0.044(5) -0.006(4) 0.005(4) 0.002(4) C21 0.030(4) 0.038(4) 0.025(4) 0.011(3) 0.007(3) 0.005(3) C22 0.039(5) 0.037(4) 0.049(5) 0.012(4) 0.011(4) 0.011(4) C23 0.055(6) 0.039(4) 0.048(6) 0.015(4) 0.015(5) 0.017(4) C24 0.039(5) 0.049(5) 0.037(5) 0.014(4) 0.009(4) 0.024(4) C25 0.025(4) 0.049(5) 0.042(5) 0.012(4) 0.002(4) 0.017(4) C26 0.037(5) 0.033(4) 0.033(4) 0.008(3) 0.001(4) 0.012(3) C27 0.022(4) 0.045(4) 0.035(4) 0.013(4) 0.006(4) 0.002(3) C28 0.023(4) 0.048(4) 0.027(4) 0.006(4) 0.005(3) 0.010(3) C31 0.022(4) 0.031(4) 0.022(4) 0.003(3) 0.002(3) 0.003(3) C32 0.031(4) 0.031(4) 0.038(5) 0.008(3) 0.008(4) 0.007(3) C33 0.045(5) 0.034(4) 0.052(6) 0.011(4) 0.022(5) 0.005(4) C34 0.064(7) 0.041(5) 0.059(6) 0.021(5) 0.029(6) 0.023(5) C35 0.051(6) 0.049(5) 0.052(6) 0.021(4) 0.021(5) 0.029(5) C36 0.036(5) 0.043(4) 0.035(5) 0.010(4) 0.004(4) 0.016(4) C37 0.024(4) 0.031(4) 0.030(4) 0.003(3) 0.002(3) 0.009(3) C38 0.031(4) 0.039(4) 0.035(4) 0.010(4) 0.007(4) 0.015(3) C41 0.030(4) 0.030(4) 0.025(4) 0.007(3) -0.005(3) 0.016(3) C42 0.056(6) 0.033(4) 0.036(5) 0.008(4) 0.014(4) 0.013(4) C43 0.074(7) 0.042(5) 0.060(7) 0.022(5) 0.039(6) 0.029(5) C44 0.046(6) 0.043(5) 0.087(8) 0.029(5) 0.033(6) 0.018(4) C45 0.031(5) 0.042(5) 0.080(8) 0.027(5) 0.002(5) 0.008(4) C46 0.032(4) 0.032(4) 0.046(5) 0.017(4) 0.008(4) 0.020(3) C47 0.029(4) 0.054(5) 0.034(5) 0.005(4) -0.011(4) 0.011(4) C48 0.030(4) 0.048(5) 0.031(4) 0.005(4) 0.003(4) 0.021(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 Re1 C1 1.738(8) . ? Re1 P2 2.3774(18) . ? Re1 P3 2.4399(19) . ? Re1 P1 2.4530(18) . ? Re1 Cl2 2.4886(18) . ? Re1 Cl1 2.5498(18) . ? P1 C27 1.818(8) . ? P1 C28 1.838(8) . ? P1 C21 1.846(8) . ? P3 C47 1.815(9) . ? P3 C48 1.834(8) . ? P3 C41 1.842(8) . ? P2 C37 1.815(8) . ? P2 C38 1.820(9) . ? P2 C31 1.844(8) . ? O1 C3 1.463(9) . ? C1 C2 1.512(11) . ? C2 C3 1.538(10) . ? C3 C4 1.514(11) . ? C3 C10 1.516(11) . ? C4 C9 1.384(12) . ? C4 C5 1.410(12) . ? C5 C6 1.387(13) . ? C6 C7 1.388(15) . ? C7 C8 1.348(15) . ? C8 C9 1.402(13) . ? C10 C11 1.358(13) . ? C10 C15 1.396(13) . ? C11 C12 1.405(15) . ? C12 C13 1.404(17) . ? C13 C14 1.366(16) . ? C14 C15 1.391(13) . ? C21 C22 1.367(12) . ? C21 C26 1.395(12) . ? C22 C23 1.395(13) . ? C23 C24 1.377(14) . ? C24 C25 1.405(13) . ? C25 C26 1.390(11) . ? C31 C36 1.393(11) . ? C31 C32 1.396(11) . ? C32 C33 1.378(12) . ? C33 C34 1.402(14) . ? C34 C35 1.381(15) . ? C35 C36 1.341(13) . ? C41 C42 1.387(12) . ? C41 C46 1.398(12) . ? C42 C43 1.386(14) . ? C43 C44 1.381(17) . ? C44 C45 1.396(16) . ? C45 C46 1.402(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 P2 89.4(3) . . ? C1 Re1 P3 91.8(2) . . ? P2 Re1 P3 94.00(6) . . ? C1 Re1 P1 93.2(2) . . ? P2 Re1 P1 95.91(6) . . ? P3 Re1 P1 168.94(6) . . ? C1 Re1 Cl2 102.5(3) . . ? P2 Re1 Cl2 168.07(7) . . ? P3 Re1 Cl2 85.51(6) . . ? P1 Re1 Cl2 83.78(6) . . ? C1 Re1 Cl1 171.9(3) . . ? P2 Re1 Cl1 82.57(6) . . ? P3 Re1 Cl1 87.30(6) . . ? P1 Re1 Cl1 89.11(6) . . ? Cl2 Re1 Cl1 85.50(7) . . ? C27 P1 C28 102.2(4) . . ? C27 P1 C21 104.2(4) . . ? C28 P1 C21 98.5(4) . . ? C27 P1 Re1 115.1(3) . . ? C28 P1 Re1 112.7(3) . . ? C21 P1 Re1 121.4(2) . . ? C47 P3 C48 99.6(4) . . ? C47 P3 C41 103.4(4) . . ? C48 P3 C41 101.0(4) . . ? C47 P3 Re1 117.2(3) . . ? C48 P3 Re1 116.1(3) . . ? C41 P3 Re1 116.8(2) . . ? C37 P2 C38 100.4(4) . . ? C37 P2 C31 104.1(3) . . ? C38 P2 C31 98.6(4) . . ? C37 P2 Re1 115.5(3) . . ? C38 P2 Re1 117.3(3) . . ? C31 P2 Re1 118.1(2) . . ? C2 C1 Re1 171.8(6) . . ? C1 C2 C3 113.2(6) . . ? O1 C3 C4 109.3(6) . . ? O1 C3 C10 107.2(7) . . ? C4 C3 C10 110.4(7) . . ? O1 C3 C2 106.8(6) . . ? C4 C3 C2 111.9(7) . . ? C10 C3 C2 111.1(7) . . ? C9 C4 C5 118.0(8) . . ? C9 C4 C3 122.3(8) . . ? C5 C4 C3 119.4(8) . . ? C6 C5 C4 120.2(9) . . ? C5 C6 C7 120.3(9) . . ? C8 C7 C6 120.1(9) . . ? C7 C8 C9 120.7(10) . . ? C4 C9 C8 120.7(9) . . ? C11 C10 C15 118.6(9) . . ? C11 C10 C3 119.6(9) . . ? C15 C10 C3 121.8(8) . . ? C10 C11 C12 121.3(10) . . ? C13 C12 C11 119.9(10) . . ? C14 C13 C12 118.4(10) . . ? C13 C14 C15 121.2(10) . . ? C14 C15 C10 120.6(9) . . ? C22 C21 C26 120.7(8) . . ? C22 C21 P1 122.2(7) . . ? C26 C21 P1 116.7(6) . . ? C21 C22 C23 119.5(9) . . ? C24 C23 C22 121.2(8) . . ? C23 C24 C25 118.9(8) . . ? C26 C25 C24 120.0(8) . . ? C25 C26 C21 119.6(8) . . ? C36 C31 C32 118.9(7) . . ? C36 C31 P2 122.5(6) . . ? C32 C31 P2 118.5(6) . . ? C33 C32 C31 120.2(8) . . ? C32 C33 C34 119.2(9) . . ? C35 C34 C33 119.9(8) . . ? C36 C35 C34 120.6(9) . . ? C35 C36 C31 121.2(9) . . ? C42 C41 C46 119.8(8) . . ? C42 C41 P3 122.5(7) . . ? C46 C41 P3 117.7(6) . . ? C43 C42 C41 119.2(10) . . ? C44 C43 C42 121.6(10) . . ? C43 C44 C45 119.8(9) . . ? C44 C45 C46 118.9(10) . . ? C41 C46 C45 120.6(9) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 2.815 _refine_diff_density_min -1.709 _refine_diff_density_rms 0.181