# ic990970r.cif data_Compound_[Re(N2)2{PPh(OEt)2}4]BPh4 (2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H80 B1 N4 O8 P4 Re1' _chemical_formula_weight 1354.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 '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' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'othorhombic' _symmetry_space_group_name_H-M 'P b a a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z' 'x-1/2, -y-1/2, z' _cell_length_a 23.008(5) _cell_length_b 23.367(5) _cell_length_c 12.863(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6916(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.78 _cell_measurement_theta_max 7.41 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 1.901 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min .442 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW100 diffractometer' _diffrn_measurement_method '\q/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 25 _diffrn_reflns_number 19904 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.1235 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10103 _reflns_number_gt 3846 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10103 _refine_ls_number_parameters 406 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1629 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.2500 0.0000 0.11833(2) 0.04342(10) Uani 1 d SD . . P1 P 0.35193(7) 0.02897(7) 0.12910(14) 0.0558(4) Uani 1 d . . . P2 P 0.22042(7) 0.09992(6) 0.12565(13) 0.0522(4) Uani 1 d . . . O1 O 0.35890(18) 0.09727(16) 0.1256(4) 0.0767(14) Uani 1 d . . . O2 O 0.39758(19) 0.00595(19) 0.0457(4) 0.0737(12) Uani 1 d . . . O3 O 0.15251(17) 0.10693(15) 0.0993(3) 0.0624(12) Uani 1 d . . . O4 O 0.2508(2) 0.14684(15) 0.0530(3) 0.0676(11) Uani 1 d . . . C199 C 0.2500 0.0000 0.639(2) 0.147(14) Uani 0.50 d SP . . C200 C 0.1937(9) 0.0137(11) 0.6471(17) 0.127(8) Uani 0.50 d P . . C201 C 0.2321(11) 0.0554(8) 0.6584(16) 0.137(9) Uani 0.50 d P . . N1 N 0.2500 0.0000 0.2758(5) 0.0530(16) Uani 0.911(4) d SPDU A 1 N2 N 0.2500 0.0000 0.3553(5) 0.0565(16) Uani 0.911(4) d SPDU A 1 Cl Cl 0.2500 0.0000 0.3078(12) 0.0529(17) Uani 0.089(4) d SPDU A 2 N3 N 0.2500 0.0000 -0.0348(7) 0.070(2) Uani 1 d SU . . N4 N 0.2500 0.0000 -0.1198(9) 0.155(6) Uani 1 d SU . . B B 0.5012(6) 0.2500 0.5000 0.063(3) Uani 0.911(4) d SP . 1 C1 C 0.3911(3) 0.0082(3) 0.2449(5) 0.0613(17) Uani 1 d . . . C2 C 0.3793(3) 0.0371(3) 0.3363(6) 0.082(2) Uani 1 d . . . H2 H 0.3531 0.0674 0.3378 0.098 Uiso 1 calc R . . C3 C 0.4087(5) 0.0187(4) 0.4287(7) 0.118(3) Uani 1 d . . . H3 H 0.4026 0.0379 0.4911 0.141 Uiso 1 calc R . . C4 C 0.4465(4) -0.0279(4) 0.4248(9) 0.123(4) Uani 1 d . . . H4 H 0.4641 -0.0408 0.4856 0.147 Uiso 1 calc R . . C5 C 0.4577(4) -0.0540(4) 0.3354(8) 0.103(3) Uani 1 d . . . H5 H 0.4833 -0.0848 0.3339 0.123 Uiso 1 calc R . . C6 C 0.4317(3) -0.0359(3) 0.2449(7) 0.079(2) Uani 1 d . . . H6 H 0.4414 -0.0535 0.1824 0.094 Uiso 1 calc R . . C7 C 0.4157(3) 0.1240(3) 0.1411(9) 0.149(5) Uani 1 d . . . H7A H 0.4231 0.1277 0.2150 0.179 Uiso 1 calc R . . H7B H 0.4456 0.0995 0.1119 0.179 Uiso 1 calc R . . C8 C 0.4191(4) 0.1767(3) 0.0958(9) 0.172(6) Uani 1 d . . . H8A H 0.4277 0.1724 0.0232 0.207 Uiso 1 calc R . . H8B H 0.4494 0.1985 0.1285 0.207 Uiso 1 calc R . . H8C H 0.3827 0.1962 0.1038 0.207 Uiso 1 calc R . . C9 C 0.3870(4) 0.0074(5) -0.0624(7) 0.152(5) Uani 1 d . . . H9A H 0.3603 -0.0233 -0.0796 0.182 Uiso 1 calc R . . H9B H 0.3680 0.0432 -0.0791 0.182 Uiso 1 calc R . . C10 C 0.4353(5) 0.0021(4) -0.1235(7) 0.173(6) Uani 1 d . . . H10A H 0.4611 0.0335 -0.1105 0.208 Uiso 1 calc R . . H10B H 0.4240 0.0022 -0.1953 0.208 Uiso 1 calc R . . H10C H 0.4547 -0.0332 -0.1076 0.208 Uiso 1 calc R . . C11 C 0.2294(3) 0.1350(2) 0.2495(5) 0.0588(18) Uani 1 d . . . C12 C 0.2734(3) 0.1745(3) 0.2692(6) 0.080(2) Uani 1 d . . . H12 H 0.2990 0.1848 0.2165 0.096 Uiso 1 calc R . . C13 C 0.2792(4) 0.1985(3) 0.3671(8) 0.106(3) Uani 1 d . . . H13 H 0.3086 0.2250 0.3800 0.127 Uiso 1 calc R . . C14 C 0.2416(5) 0.1833(3) 0.4451(7) 0.119(4) Uani 1 d . . . H14 H 0.2464 0.1988 0.5112 0.143 Uiso 1 calc R . . C15 C 0.1961(4) 0.1449(3) 0.4268(7) 0.101(3) Uani 1 d . . . H15 H 0.1698 0.1357 0.4790 0.121 Uiso 1 calc R . . C16 C 0.1914(3) 0.1208(3) 0.3276(6) 0.076(2) Uani 1 d . . . H16 H 0.1619 0.0947 0.3143 0.091 Uiso 1 calc R . . C17 C 0.1236(3) 0.1622(3) 0.1064(7) 0.099(3) Uani 1 d . . . H17A H 0.1116 0.1690 0.1777 0.119 Uiso 1 calc R . . H17B H 0.1505 0.1922 0.0867 0.119 Uiso 1 calc R . . C18 C 0.0743(4) 0.1638(3) 0.0404(8) 0.146(4) Uani 1 d . . . H18A H 0.0846 0.1489 -0.0268 0.175 Uiso 1 calc R . . H18B H 0.0612 0.2026 0.0333 0.175 Uiso 1 calc R . . H18C H 0.0439 0.1409 0.0698 0.175 Uiso 1 calc R . . C19 C 0.2575(4) 0.1385(3) -0.0566(6) 0.101(3) Uani 1 d . . . H19A H 0.2239 0.1183 -0.0836 0.122 Uiso 1 calc R . . H19B H 0.2916 0.1152 -0.0695 0.122 Uiso 1 calc R . . C20 C 0.2635(4) 0.1922(4) -0.1095(6) 0.132(4) Uani 1 d . . . H20A H 0.2293 0.2149 -0.0981 0.159 Uiso 1 calc R . . H20B H 0.2682 0.1854 -0.1826 0.159 Uiso 1 calc R . . H20C H 0.2969 0.2121 -0.0832 0.159 Uiso 1 calc R . . C100 C 0.5413(4) 0.2098(3) 0.4263(6) 0.066(2) Uani 0.911(4) d P . 1 C101 C 0.5270(4) 0.1529(4) 0.3995(6) 0.085(3) Uani 0.911(4) d P . 1 H101 H 0.4944 0.1361 0.4294 0.102 Uiso 0.911(4) calc PR A 1 C102 C 0.5601(5) 0.1212(4) 0.3299(7) 0.111(4) Uani 0.911(4) d P . 1 H102 H 0.5491 0.0842 0.3122 0.133 Uiso 0.911(4) calc PR A 1 C103 C 0.6099(6) 0.1454(5) 0.2870(8) 0.129(5) Uani 0.911(4) d P . 1 H103 H 0.6327 0.1240 0.2417 0.155 Uiso 0.911(4) calc PR A 1 C104 C 0.6256(4) 0.2007(5) 0.3108(7) 0.110(4) Uani 0.911(4) d P . 1 H104 H 0.6587 0.2169 0.2815 0.132 Uiso 0.911(4) calc PR A 1 C105 C 0.5917(4) 0.2317(4) 0.3790(7) 0.093(3) Uani 0.911(4) d P . 1 H105 H 0.6027 0.2691 0.3945 0.112 Uiso 0.911(4) calc PR A 1 C106 C 0.4583(4) 0.2112(3) 0.5783(7) 0.070(2) Uani 0.911(4) d P . 1 C107 C 0.4664(4) 0.2052(3) 0.6832(7) 0.093(3) Uani 0.911(4) d P . 1 H107 H 0.4974 0.2243 0.7140 0.111 Uiso 0.911(4) calc PR A 1 C108 C 0.4304(5) 0.1717(4) 0.7464(9) 0.116(4) Uani 0.911(4) d P . 1 H108 H 0.4382 0.1691 0.8172 0.139 Uiso 0.911(4) calc PR A 1 C109 C 0.3867(6) 0.1444(5) 0.7084(10) 0.115(4) Uani 0.911(4) d P . 1 H109 H 0.3639 0.1215 0.7513 0.138 Uiso 0.911(4) calc PR A 1 C110 C 0.3739(4) 0.1490(4) 0.6061(10) 0.111(4) Uani 0.911(4) d P . 1 H110 H 0.3418 0.1298 0.5792 0.133 Uiso 0.911(4) calc PR A 1 C111 C 0.4091(4) 0.1827(3) 0.5396(8) 0.092(3) Uani 0.911(4) d P . 1 H111 H 0.3995 0.1859 0.4696 0.111 Uiso 0.911(4) calc PR A 1 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 Re 0.04668(17) 0.04133(14) 0.04225(17) 0.000 0.000 0.00085(18) P1 0.0492(9) 0.0515(8) 0.0667(12) 0.0038(8) 0.0065(9) -0.0019(7) P2 0.0525(9) 0.0483(8) 0.0558(10) 0.0028(8) -0.0039(9) 0.0032(7) O1 0.060(3) 0.050(2) 0.120(4) 0.012(3) -0.006(3) -0.008(2) O2 0.063(3) 0.092(3) 0.066(3) -0.002(3) 0.022(2) 0.002(2) O3 0.057(3) 0.052(2) 0.078(3) -0.001(2) -0.012(2) 0.009(2) O4 0.082(3) 0.054(2) 0.067(3) 0.0165(19) 0.002(3) 0.004(2) C199 0.18(4) 0.18(3) 0.08(2) 0.000 0.000 0.12(3) C200 0.096(15) 0.16(2) 0.130(17) -0.019(14) -0.081(13) 0.015(13) C201 0.16(2) 0.126(16) 0.124(16) 0.096(14) 0.011(15) 0.055(15) N1 0.042(2) 0.046(2) 0.071(5) 0.000 0.000 0.002(2) N2 0.045(2) 0.049(2) 0.075(5) 0.000 0.000 0.003(2) Cl 0.043(2) 0.046(2) 0.070(5) 0.000 0.000 0.002(3) N3 0.067(5) 0.052(4) 0.093(6) 0.000 0.000 0.000(4) N4 0.196(15) 0.154(11) 0.115(8) 0.000 0.000 0.017(8) B 0.070(7) 0.062(6) 0.059(7) 0.008(9) 0.000 0.000 C1 0.046(3) 0.070(5) 0.069(5) 0.000(4) -0.004(3) -0.008(3) C2 0.086(6) 0.086(5) 0.073(6) -0.010(5) -0.010(5) -0.012(4) C3 0.138(9) 0.150(9) 0.065(6) -0.023(6) -0.002(6) -0.062(7) C4 0.100(8) 0.101(7) 0.166(12) 0.037(8) -0.062(8) -0.018(6) C5 0.076(6) 0.085(6) 0.147(10) 0.006(6) -0.033(7) -0.005(5) C6 0.058(5) 0.075(5) 0.103(7) 0.009(5) -0.006(5) 0.001(4) C7 0.078(6) 0.076(5) 0.294(15) 0.064(7) -0.032(8) -0.033(5) C8 0.081(7) 0.095(7) 0.341(19) 0.018(9) 0.024(9) -0.039(5) C9 0.103(8) 0.276(14) 0.077(7) 0.006(9) 0.038(6) 0.040(8) C10 0.160(11) 0.262(16) 0.097(8) -0.021(10) 0.061(7) 0.008(9) C11 0.079(5) 0.040(3) 0.058(4) -0.006(3) 0.000(3) 0.005(3) C12 0.087(5) 0.064(4) 0.089(6) -0.016(4) -0.004(5) -0.001(4) C13 0.105(7) 0.080(5) 0.132(9) -0.018(6) -0.017(7) -0.017(5) C14 0.184(12) 0.081(6) 0.093(7) -0.025(5) -0.042(8) -0.009(6) C15 0.138(9) 0.089(6) 0.075(6) -0.004(5) 0.025(6) 0.016(6) C16 0.095(6) 0.067(4) 0.065(5) -0.016(4) -0.006(5) -0.001(4) C17 0.074(5) 0.068(4) 0.156(9) -0.008(5) -0.021(6) 0.021(4) C18 0.135(9) 0.103(7) 0.200(13) 0.027(7) -0.055(9) 0.039(6) C19 0.161(9) 0.065(4) 0.078(6) 0.015(4) 0.033(6) 0.004(5) C20 0.217(13) 0.104(6) 0.076(6) 0.026(5) 0.017(7) 0.019(7) C100 0.081(6) 0.069(5) 0.048(5) 0.006(4) -0.002(5) 0.015(4) C101 0.103(7) 0.086(6) 0.065(6) 0.006(4) 0.022(5) 0.008(5) C102 0.178(12) 0.081(6) 0.073(7) -0.012(5) 0.026(7) 0.021(7) C103 0.174(13) 0.141(10) 0.072(8) -0.015(8) 0.035(8) 0.063(9) C104 0.100(8) 0.166(10) 0.064(7) 0.012(7) 0.033(6) 0.027(8) C105 0.095(7) 0.096(6) 0.088(7) 0.013(5) 0.011(6) -0.010(5) C106 0.072(6) 0.057(5) 0.081(7) 0.000(5) 0.008(6) 0.016(4) C107 0.111(8) 0.093(6) 0.074(7) 0.001(5) 0.025(6) -0.018(5) C108 0.153(12) 0.107(9) 0.088(9) 0.002(6) 0.033(8) -0.005(8) C109 0.133(12) 0.100(9) 0.112(11) 0.009(8) 0.049(9) 0.013(7) C110 0.074(6) 0.081(6) 0.177(13) 0.002(7) 0.030(8) -0.007(5) C111 0.081(7) 0.090(6) 0.105(8) 0.007(5) 0.007(6) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re N3 1.970(9) . ? Re N1 2.025(7) . ? Re P2 2.4339(15) . ? Re P2 2.4340(15) 2 ? Re Cl 2.437(16) . ? Re P1 2.4448(16) 2 ? Re P1 2.4449(16) . ? P1 O2 1.595(4) . ? P1 O1 1.605(4) . ? P1 C1 1.807(7) . ? P2 O4 1.601(4) . ? P2 O3 1.607(4) . ? P2 C11 1.803(6) . ? O1 C7 1.462(8) . ? O2 C9 1.411(10) . ? O3 C17 1.455(7) . ? O4 C19 1.432(8) . ? C199 C200 1.34(2) . ? C199 C200 1.34(2) 2 ? C199 C201 1.38(2) . ? C199 C201 1.38(2) 2 ? C200 C201 1.32(2) . ? N1 N2 1.022(2) . ? N3 N4 1.092(12) . ? B C100 1.623(10) . ? B C100 1.623(10) 3_556 ? B C106 1.677(10) . ? B C106 1.677(10) 3_556 ? C1 C2 1.383(9) . ? C1 C6 1.391(9) . ? C2 C3 1.433(11) . ? C3 C4 1.395(13) . ? C4 C5 1.327(12) . ? C5 C6 1.375(10) . ? C7 C8 1.363(10) . ? C9 C10 1.366(12) . ? C11 C16 1.372(8) . ? C11 C12 1.396(9) . ? C12 C13 1.385(10) . ? C13 C14 1.372(12) . ? C14 C15 1.397(10) . ? C15 C16 1.398(9) . ? C17 C18 1.418(10) . ? C19 C20 1.432(10) . ? C100 C105 1.406(11) . ? C100 C101 1.412(10) . ? C101 C102 1.389(10) . ? C102 C103 1.390(14) . ? C103 C104 1.377(13) . ? C104 C105 1.381(11) . ? C106 C107 1.369(11) . ? C106 C111 1.406(11) . ? C107 C108 1.400(11) . ? C108 C109 1.288(14) . ? C109 C110 1.353(13) . ? C110 C111 1.416(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Re N1 180.0 . . ? N3 Re P2 92.22(4) . . ? N1 Re P2 87.78(4) . . ? N3 Re P2 92.22(4) . 2 ? N1 Re P2 87.78(4) . 2 ? P2 Re P2 175.56(8) . 2 ? N3 Re Cl 180.0 . . ? N1 Re Cl 0.0 . . ? P2 Re Cl 87.78(4) . . ? P2 Re Cl 87.78(4) 2 . ? N3 Re P1 93.25(4) . 2 ? N1 Re P1 86.75(4) . 2 ? P2 Re P1 89.72(5) . 2 ? P2 Re P1 90.02(5) 2 2 ? Cl Re P1 86.75(4) . 2 ? N3 Re P1 93.25(4) . . ? N1 Re P1 86.75(4) . . ? P2 Re P1 90.03(5) . . ? P2 Re P1 89.72(5) 2 . ? Cl Re P1 86.75(4) . . ? P1 Re P1 173.50(9) 2 . ? O2 P1 O1 104.5(2) . . ? O2 P1 C1 97.8(3) . . ? O1 P1 C1 103.9(3) . . ? O2 P1 Re 120.01(19) . . ? O1 P1 Re 111.70(17) . . ? C1 P1 Re 116.8(2) . . ? O4 P2 O3 103.4(2) . . ? O4 P2 C11 98.9(3) . . ? O3 P2 C11 104.5(3) . . ? O4 P2 Re 120.83(17) . . ? O3 P2 Re 111.19(15) . . ? C11 P2 Re 115.98(19) . . ? C7 O1 P1 120.7(4) . . ? C9 O2 P1 122.8(5) . . ? C17 O3 P2 121.4(4) . . ? C19 O4 P2 122.0(4) . . ? C200 C199 C200 171(3) . 2 ? C200 C199 C201 58.2(10) . . ? C200 C199 C201 120.1(12) 2 . ? C200 C199 C201 120.1(12) . 2 ? C200 C199 C201 58.2(10) 2 2 ? C201 C199 C201 160(3) . 2 ? C201 C200 C199 62.5(13) . . ? C200 C201 C199 59.3(13) . . ? N2 N1 Re 180.0 . . ? N4 N3 Re 180.0 . . ? C100 B C100 110.8(11) . 3_556 ? C100 B C106 111.9(3) . . ? C100 B C106 107.2(4) 3_556 . ? C100 B C106 107.2(4) . 3_556 ? C100 B C106 111.9(3) 3_556 3_556 ? C106 B C106 107.9(10) . 3_556 ? C2 C1 C6 119.6(7) . . ? C2 C1 P1 118.2(6) . . ? C6 C1 P1 122.2(6) . . ? C1 C2 C3 117.7(8) . . ? C4 C3 C2 120.0(9) . . ? C5 C4 C3 120.7(10) . . ? C4 C5 C6 120.6(10) . . ? C5 C6 C1 121.3(8) . . ? C8 C7 O1 112.3(7) . . ? C10 C9 O2 115.1(10) . . ? C16 C11 C12 119.3(6) . . ? C16 C11 P2 117.7(5) . . ? C12 C11 P2 123.0(6) . . ? C13 C12 C11 120.2(8) . . ? C14 C13 C12 119.9(8) . . ? C13 C14 C15 121.0(8) . . ? C14 C15 C16 118.0(8) . . ? C11 C16 C15 121.5(7) . . ? C18 C17 O3 110.5(7) . . ? O4 C19 C20 111.1(6) . . ? C105 C100 C101 115.5(7) . . ? C105 C100 B 120.6(8) . . ? C101 C100 B 123.8(8) . . ? C102 C101 C100 122.1(8) . . ? C101 C102 C103 119.4(9) . . ? C104 C103 C102 120.6(10) . . ? C103 C104 C105 119.1(10) . . ? C104 C105 C100 123.3(9) . . ? C107 C106 C111 114.3(9) . . ? C107 C106 B 124.5(8) . . ? C111 C106 B 121.2(8) . . ? C106 C107 C108 123.2(10) . . ? C109 C108 C107 121.3(12) . . ? C108 C109 C110 119.9(13) . . ? C109 C110 C111 120.6(11) . . ? C106 C111 C110 120.6(10) . . ? _diffrn_measured_fraction_theta_max .918 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full .918 _refine_diff_density_max 1.826 _refine_diff_density_min -1.652 _refine_diff_density_rms .098 data_Compound_[ReCl(CH3N2)(CH3NHNH2){PPh(OEt)2}3]BPh4 (1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H74 B1 Cl1 N4 O6 P3 Re1' _chemical_formula_weight 1224.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .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 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.396(5) _cell_length_b 16.986(5) _cell_length_c 11.560(5) _cell_angle_alpha 93.959(5) _cell_angle_beta 93.988(5) _cell_angle_gamma 93.087(5) _cell_volume 3003.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.42 _cell_measurement_theta_max 7.46 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'orange' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 2.196 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 1. _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW100 diffractometer' _diffrn_measurement_method '\q/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 28 _diffrn_reflns_number 17456 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 30.00 _reflns_number_total 17456 _reflns_number_gt 12407 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17456 _refine_ls_number_parameters 679 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 3.883 _refine_ls_shift/su_mean 0.050 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.190096(8) 0.237020(7) 0.125439(11) 0.03252(4) Uani 1 d . . . Cl1 Cl -0.13623(5) 0.17058(5) -0.04678(7) 0.04733(19) Uani 1 d . . . P1 P -0.08059(5) 0.18925(5) 0.25110(7) 0.03681(18) Uani 1 d . . . P2 P -0.28640(5) 0.12292(4) 0.14380(7) 0.03909(18) Uani 1 d . . . P3 P -0.10341(5) 0.35228(4) 0.08164(7) 0.03630(18) Uani 1 d . . . O1 O -0.06436(15) 0.09679(12) 0.24323(19) 0.0543(6) Uani 1 d . . . O2 O 0.01299(13) 0.23319(14) 0.24127(19) 0.0534(6) Uani 1 d . . . O3 O -0.37862(14) 0.14330(13) 0.0821(2) 0.0581(6) Uani 1 d . . . O4 O -0.30760(15) 0.09511(13) 0.2681(2) 0.0569(6) Uani 1 d . . . O5 O -0.14891(15) 0.38323(12) -0.03497(19) 0.0517(6) Uani 1 d . . . O6 O -0.00145(13) 0.35580(12) 0.0615(2) 0.0498(6) Uani 1 d . . . N1 N -0.23411(16) 0.29167(14) 0.2466(2) 0.0400(6) Uani 1 d . . . N2 N -0.2549(2) 0.32729(18) 0.3326(3) 0.0664(9) Uani 1 d . . . N3 N -0.28795(17) 0.27343(16) -0.0096(2) 0.0410(6) Uani 1 d . . . N4 N -0.3533(2) 0.3238(2) 0.0329(3) 0.0674(9) Uani 1 d D . . B1 B -0.6109(2) 0.2751(2) -0.3795(3) 0.0462(9) Uani 1 d . . . C32 C -0.3333(3) 0.3682(3) 0.3406(4) 0.1008(17) Uani 1 d . . . H01A H -0.3524 0.3840 0.2653 0.151 Uiso 1 calc R . . H01B H -0.3224 0.4142 0.3938 0.151 Uiso 1 calc R . . H01C H -0.3778 0.3339 0.3681 0.151 Uiso 1 calc R . . C1 C -0.4151(3) 0.3391(3) -0.0658(4) 0.0924(16) Uani 1 d . . . H1A H -0.3859 0.3715 -0.1178 0.139 Uiso 1 calc R . . H1B H -0.4634 0.3659 -0.0371 0.139 Uiso 1 calc R . . H1C H -0.4359 0.2898 -0.1066 0.139 Uiso 1 calc R . . C2 C -0.0260(2) 0.0550(2) 0.1481(3) 0.0616(10) Uani 1 d . . . H2A H 0.0179 0.0889 0.1168 0.074 Uiso 1 calc R . . H2B H -0.0704 0.0380 0.0864 0.074 Uiso 1 calc R . . C3 C 0.0145(3) -0.0152(2) 0.1967(4) 0.0979(16) Uani 1 d . . . H3A H 0.0580 0.0025 0.2578 0.147 Uiso 1 calc R . . H3B H 0.0411 -0.0447 0.1362 0.147 Uiso 1 calc R . . H3C H -0.0297 -0.0482 0.2271 0.147 Uiso 1 calc R . . C4 C 0.0903(2) 0.2132(3) 0.3108(4) 0.0865(14) Uani 1 d . . . H4A H 0.0746 0.2027 0.3884 0.104 Uiso 1 calc R . . H4B H 0.1128 0.1656 0.2760 0.104 Uiso 1 calc R . . C5 C 0.1563(3) 0.2761(3) 0.3183(5) 0.123(2) Uani 1 d . . . H5A H 0.1675 0.2902 0.2415 0.185 Uiso 1 calc R . . H5B H 0.2088 0.2593 0.3564 0.185 Uiso 1 calc R . . H5C H 0.1369 0.3211 0.3621 0.185 Uiso 1 calc R . . C6 C -0.09731(19) 0.19982(18) 0.4053(3) 0.0411(7) Uani 1 d . . . C7 C -0.0875(2) 0.2743(2) 0.4630(3) 0.0594(10) Uani 1 d . . . H7 H -0.0746 0.3183 0.4222 0.071 Uiso 1 calc R . . C8 C -0.0970(3) 0.2835(3) 0.5820(3) 0.0770(12) Uani 1 d . . . H8 H -0.0889 0.3335 0.6208 0.092 Uiso 1 calc R . . C9 C -0.1181(3) 0.2200(3) 0.6418(3) 0.0761(13) Uani 1 d . . . H9 H -0.1248 0.2267 0.7212 0.091 Uiso 1 calc R . . C10 C -0.1295(3) 0.1465(3) 0.5861(3) 0.0723(12) Uani 1 d . . . H10 H -0.1445 0.1033 0.6274 0.087 Uiso 1 calc R . . C11 C -0.1189(2) 0.1358(2) 0.4684(3) 0.0564(9) Uani 1 d . . . H11 H -0.1262 0.0853 0.4312 0.068 Uiso 1 calc R . . C12 C -0.4543(2) 0.0897(2) 0.0663(4) 0.0857(14) Uani 1 d . . . H12A H -0.4607 0.0615 0.1357 0.103 Uiso 1 calc R . . H12B H -0.4488 0.0514 0.0015 0.103 Uiso 1 calc R . . C13 C -0.5314(3) 0.1364(3) 0.0432(6) 0.140(3) Uani 1 d . . . H13A H -0.5469 0.1622 0.1147 0.210 Uiso 1 calc R . . H13B H -0.5794 0.1019 0.0099 0.210 Uiso 1 calc R . . H13C H -0.5178 0.1754 -0.0101 0.210 Uiso 1 calc R . . C14 C -0.3499(3) 0.1413(2) 0.3556(4) 0.0800(13) Uani 1 d . . . H14A H -0.3808 0.1828 0.3203 0.096 Uiso 1 calc R . . H14B H -0.3068 0.1655 0.4144 0.096 Uiso 1 calc R . . C15 C -0.4126(3) 0.0865(3) 0.4096(4) 0.1080(18) Uani 1 d . . . H15A H -0.4555 0.0635 0.3510 0.162 Uiso 1 calc R . . H15B H -0.4410 0.1156 0.4688 0.162 Uiso 1 calc R . . H15C H -0.3814 0.0453 0.4437 0.162 Uiso 1 calc R . . C16 C -0.2643(2) 0.02721(17) 0.0769(3) 0.0452(8) Uani 1 d . . . C17 C -0.2689(2) 0.0155(2) -0.0443(3) 0.0584(9) Uani 1 d . . . H17 H -0.2854 0.0560 -0.0898 0.070 Uiso 1 calc R . . C18 C -0.2488(3) -0.0569(2) -0.0968(4) 0.0756(12) Uani 1 d . . . H18 H -0.2514 -0.0643 -0.1775 0.091 Uiso 1 calc R . . C19 C -0.2253(3) -0.1168(3) -0.0309(5) 0.0885(15) Uani 1 d . . . H19 H -0.2126 -0.1651 -0.0666 0.106 Uiso 1 calc R . . C20 C -0.2205(3) -0.1060(2) 0.0883(5) 0.0844(14) Uani 1 d . . . H20 H -0.2038 -0.1469 0.1329 0.101 Uiso 1 calc R . . C21 C -0.2401(2) -0.03466(19) 0.1425(4) 0.0623(10) Uani 1 d . . . H21 H -0.2372 -0.0281 0.2232 0.075 Uiso 1 calc R . . C22 C -0.1171(3) 0.4534(2) -0.0889(4) 0.0733(12) Uani 1 d . . . H22A H -0.0664 0.4417 -0.1309 0.088 Uiso 1 calc R . . H22B H -0.1004 0.4958 -0.0297 0.088 Uiso 1 calc R . . C23 C -0.1870(3) 0.4774(3) -0.1688(4) 0.1008(17) Uani 1 d . . . H23A H -0.2027 0.4353 -0.2275 0.151 Uiso 1 calc R . . H23B H -0.1672 0.5237 -0.2048 0.151 Uiso 1 calc R . . H23C H -0.2368 0.4889 -0.1265 0.151 Uiso 1 calc R . . C24 C 0.0433(3) 0.2971(2) -0.0057(4) 0.0855(14) Uani 1 d . . . H24A H 0.0498 0.2513 0.0391 0.103 Uiso 1 calc R A 1 H24B H 0.0071 0.2803 -0.0761 0.103 Uiso 1 calc R A 1 C25 C 0.1235(6) 0.3228(6) -0.0358(11) 0.098(4) Uani 0.50 d P B 1 H25A H 0.1202 0.3744 -0.0644 0.147 Uiso 0.50 calc PR B 1 H25B H 0.1423 0.2867 -0.0954 0.147 Uiso 0.50 calc PR B 1 H25C H 0.1644 0.3253 0.0311 0.147 Uiso 0.50 calc PR B 1 C25 C 0.0621(9) 0.3129(6) -0.1109(9) 0.103(4) Uani 0.50 d P B 2 H25A H 0.0092 0.3195 -0.1574 0.155 Uiso 0.50 calc PR B 2 H25B H 0.0920 0.2701 -0.1453 0.155 Uiso 0.50 calc PR B 2 H25C H 0.0987 0.3607 -0.1070 0.155 Uiso 0.50 calc PR B 2 C26 C -0.10269(19) 0.43539(16) 0.1888(3) 0.0395(7) Uani 1 d . . . C27 C -0.1766(2) 0.47861(19) 0.1944(3) 0.0574(9) Uani 1 d . . . H27 H -0.2245 0.4653 0.1420 0.069 Uiso 1 calc R . . C28 C -0.1796(3) 0.5402(2) 0.2758(4) 0.0771(13) Uani 1 d . . . H28 H -0.2291 0.5693 0.2779 0.093 Uiso 1 calc R . . C29 C -0.1100(4) 0.5591(2) 0.3538(4) 0.0838(14) Uani 1 d . . . H29 H -0.1123 0.6011 0.4092 0.101 Uiso 1 calc R . . C30 C -0.0359(3) 0.5165(2) 0.3517(3) 0.0729(12) Uani 1 d . . . H30 H 0.0111 0.5298 0.4057 0.088 Uiso 1 calc R . . C31 C -0.0321(2) 0.45379(19) 0.2685(3) 0.0529(9) Uani 1 d . . . H31 H 0.0172 0.4246 0.2666 0.063 Uiso 1 calc R . . C100 C -0.6948(2) 0.2111(2) -0.4009(3) 0.0492(8) Uani 1 d . . . C101 C -0.7783(2) 0.2267(2) -0.3671(3) 0.0574(9) Uani 1 d . . . H101 H -0.7856 0.2746 -0.3259 0.069 Uiso 1 calc R . . C102 C -0.8508(3) 0.1744(3) -0.3918(4) 0.0739(12) Uani 1 d . . . H102 H -0.9045 0.1877 -0.3668 0.089 Uiso 1 calc R . . C103 C -0.8434(3) 0.1031(3) -0.4530(4) 0.0845(14) Uani 1 d . . . H103 H -0.8915 0.0676 -0.4687 0.101 Uiso 1 calc R . . C104 C -0.7634(3) 0.0852(3) -0.4908(4) 0.0867(14) Uani 1 d . . . H104 H -0.7576 0.0379 -0.5344 0.104 Uiso 1 calc R . . C105 C -0.6908(3) 0.1380(2) -0.4638(4) 0.0723(12) Uani 1 d . . . H105 H -0.6373 0.1239 -0.4889 0.087 Uiso 1 calc R . . C106 C -0.6160(2) 0.33586(19) -0.2628(3) 0.0461(8) Uani 1 d . . . C107 C -0.5801(2) 0.4137(2) -0.2520(3) 0.0564(9) Uani 1 d . . . H107 H -0.5540 0.4328 -0.3154 0.068 Uiso 1 calc R . . C108 C -0.5812(3) 0.4642(2) -0.1520(4) 0.0667(11) Uani 1 d . . . H108 H -0.5570 0.5156 -0.1499 0.080 Uiso 1 calc R . . C109 C -0.6187(3) 0.4371(3) -0.0560(4) 0.0751(12) Uani 1 d . . . H109 H -0.6213 0.4705 0.0107 0.090 Uiso 1 calc R . . C110 C -0.6519(3) 0.3602(3) -0.0601(3) 0.0724(11) Uani 1 d . . . H110 H -0.6756 0.3410 0.0050 0.087 Uiso 1 calc R . . C111 C -0.6505(2) 0.3109(2) -0.1611(3) 0.0596(9) Uani 1 d . . . H111 H -0.6733 0.2591 -0.1613 0.072 Uiso 1 calc R . . C112 C -0.5177(2) 0.2335(2) -0.3550(3) 0.0524(9) Uani 1 d . . . C113 C -0.5118(2) 0.1632(2) -0.3007(3) 0.0613(10) Uani 1 d . . . H113 H -0.5630 0.1362 -0.2839 0.074 Uiso 1 calc R . . C114 C -0.4317(3) 0.1314(3) -0.2702(4) 0.0806(13) Uani 1 d . . . H114 H -0.4304 0.0839 -0.2349 0.097 Uiso 1 calc R . . C115 C -0.3551(3) 0.1711(3) -0.2930(4) 0.0872(15) Uani 1 d . . . H115 H -0.3017 0.1509 -0.2725 0.105 Uiso 1 calc R . . C116 C -0.3583(3) 0.2407(3) -0.3462(4) 0.0812(13) Uani 1 d . . . H116 H -0.3062 0.2662 -0.3630 0.097 Uiso 1 calc R . . C117 C -0.43652(19) 0.2750(2) -0.3762(3) 0.0485(8) Uani 1 d . . . H117 H -0.4363 0.3234 -0.4092 0.058 Uiso 1 calc R . . C118 C -0.6115(2) 0.3221(2) -0.4998(3) 0.0516(8) Uani 1 d . . . C119 C -0.6544(3) 0.3910(2) -0.5145(3) 0.0716(11) Uani 1 d . . . H119 H -0.6821 0.4131 -0.4521 0.086 Uiso 1 calc R . . C120 C -0.6581(3) 0.4287(3) -0.6175(4) 0.0991(16) Uani 1 d . . . H120 H -0.6866 0.4755 -0.6216 0.119 Uiso 1 calc R . . C121 C -0.6208(4) 0.3982(4) -0.7119(4) 0.1079(18) Uani 1 d . . . H121 H -0.6229 0.4238 -0.7805 0.130 Uiso 1 calc R . . C122 C -0.5800(3) 0.3292(4) -0.7047(4) 0.1062(18) Uani 1 d . . . H122 H -0.5558 0.3064 -0.7696 0.127 Uiso 1 calc R . . C123 C -0.5747(3) 0.2928(3) -0.5997(4) 0.0816(13) Uani 1 d . . . H123 H -0.5450 0.2466 -0.5963 0.098 Uiso 1 calc R . . H3NB H -0.255(2) 0.3071(19) -0.066(4) 0.103(15) Uiso 1 d D . . H3NA H -0.313(2) 0.2247(18) -0.060(3) 0.061(10) Uiso 1 d D . . H4N H -0.386(5) 0.282(3) 0.072(6) 0.28(4) 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 Re1 0.03081(6) 0.03340(6) 0.03466(7) 0.00621(4) 0.00370(4) 0.00760(4) Cl1 0.0564(5) 0.0478(4) 0.0402(4) 0.0037(4) 0.0127(4) 0.0131(4) P1 0.0336(4) 0.0426(4) 0.0367(4) 0.0118(3) 0.0047(3) 0.0102(3) P2 0.0367(4) 0.0352(4) 0.0465(5) 0.0063(4) 0.0067(4) 0.0035(3) P3 0.0348(4) 0.0354(4) 0.0402(5) 0.0093(3) 0.0056(3) 0.0041(3) O1 0.0665(15) 0.0483(13) 0.0540(15) 0.0134(11) 0.0171(12) 0.0290(11) O2 0.0323(12) 0.0805(16) 0.0506(14) 0.0292(12) -0.0002(10) 0.0046(11) O3 0.0347(12) 0.0561(14) 0.0825(18) 0.0082(13) -0.0035(12) 0.0002(10) O4 0.0656(16) 0.0540(14) 0.0555(15) 0.0086(12) 0.0266(12) 0.0094(12) O5 0.0589(14) 0.0481(13) 0.0484(14) 0.0216(11) -0.0052(11) -0.0045(11) O6 0.0405(12) 0.0498(13) 0.0624(15) 0.0086(11) 0.0207(11) 0.0061(10) N1 0.0408(14) 0.0350(13) 0.0453(16) 0.0037(12) 0.0068(12) 0.0068(11) N2 0.069(2) 0.066(2) 0.067(2) -0.0018(17) 0.0229(18) 0.0167(17) N3 0.0391(14) 0.0379(14) 0.0459(16) 0.0086(13) -0.0077(13) 0.0081(11) N4 0.0510(18) 0.070(2) 0.079(2) -0.0110(18) -0.0164(17) 0.0333(16) B1 0.042(2) 0.056(2) 0.041(2) 0.0032(18) -0.0001(17) 0.0088(17) C32 0.097(4) 0.096(3) 0.118(4) 0.000(3) 0.049(3) 0.042(3) C1 0.072(3) 0.089(3) 0.111(4) -0.008(3) -0.040(3) 0.039(2) C2 0.065(2) 0.063(2) 0.062(2) 0.0066(19) 0.0161(19) 0.0308(19) C3 0.122(4) 0.086(3) 0.097(4) 0.016(3) 0.027(3) 0.073(3) C4 0.037(2) 0.139(4) 0.088(3) 0.049(3) -0.010(2) 0.012(2) C5 0.067(3) 0.159(5) 0.137(5) 0.041(4) -0.045(3) -0.028(3) C6 0.0349(16) 0.0526(19) 0.0370(18) 0.0125(15) 0.0005(13) 0.0042(14) C7 0.069(2) 0.062(2) 0.047(2) 0.0046(18) 0.0093(19) -0.0092(19) C8 0.084(3) 0.094(3) 0.048(2) -0.016(2) 0.007(2) -0.017(2) C9 0.058(2) 0.136(4) 0.036(2) 0.017(3) 0.0075(18) -0.003(3) C10 0.075(3) 0.096(3) 0.052(3) 0.036(2) 0.016(2) 0.011(2) C11 0.060(2) 0.059(2) 0.054(2) 0.0212(18) 0.0125(18) 0.0112(17) C12 0.053(2) 0.078(3) 0.123(4) 0.005(3) -0.001(3) -0.016(2) C13 0.034(2) 0.116(4) 0.268(8) 0.003(5) 0.004(4) 0.003(3) C14 0.091(3) 0.077(3) 0.075(3) -0.004(2) 0.034(3) 0.002(2) C15 0.118(4) 0.105(4) 0.108(4) 0.001(3) 0.073(3) -0.010(3) C16 0.0451(18) 0.0358(16) 0.056(2) 0.0047(15) 0.0100(16) 0.0007(14) C17 0.059(2) 0.050(2) 0.066(3) 0.0014(18) 0.0112(19) 0.0012(17) C18 0.081(3) 0.067(3) 0.078(3) -0.016(2) 0.028(2) -0.005(2) C19 0.089(3) 0.053(3) 0.125(5) -0.015(3) 0.035(3) 0.010(2) C20 0.095(3) 0.045(2) 0.117(4) 0.014(3) 0.018(3) 0.019(2) C21 0.074(3) 0.0412(19) 0.074(3) 0.0077(18) 0.012(2) 0.0082(18) C22 0.077(3) 0.070(3) 0.075(3) 0.044(2) -0.001(2) -0.008(2) C23 0.076(3) 0.112(4) 0.124(4) 0.085(3) -0.003(3) 0.012(3) C24 0.085(3) 0.069(3) 0.111(4) 0.010(3) 0.056(3) 0.015(2) C25 0.057(6) 0.074(7) 0.168(12) -0.007(7) 0.056(7) 0.006(5) C25 0.137(11) 0.101(8) 0.076(8) 0.012(6) 0.043(7) -0.012(8) C26 0.0379(16) 0.0348(15) 0.0467(19) 0.0088(14) 0.0051(14) 0.0010(13) C27 0.048(2) 0.0459(19) 0.079(3) 0.0008(18) 0.0113(19) 0.0091(16) C28 0.075(3) 0.059(3) 0.098(4) -0.011(2) 0.022(3) 0.015(2) C29 0.118(4) 0.060(3) 0.072(3) -0.017(2) 0.027(3) 0.000(3) C30 0.088(3) 0.073(3) 0.053(3) 0.001(2) -0.008(2) -0.019(2) C31 0.053(2) 0.052(2) 0.054(2) 0.0091(17) 0.0022(17) -0.0015(16) C100 0.051(2) 0.0513(19) 0.046(2) 0.0102(16) -0.0031(16) 0.0083(16) C101 0.048(2) 0.066(2) 0.057(2) 0.0082(19) -0.0028(18) 0.0034(18) C102 0.054(2) 0.090(3) 0.078(3) 0.026(3) -0.005(2) -0.003(2) C103 0.072(3) 0.078(3) 0.101(4) 0.037(3) -0.029(3) -0.019(2) C104 0.097(4) 0.060(3) 0.098(4) -0.001(2) -0.022(3) 0.001(3) C105 0.066(3) 0.062(2) 0.086(3) -0.004(2) -0.007(2) 0.011(2) C106 0.0387(17) 0.054(2) 0.046(2) 0.0052(16) -0.0011(15) 0.0133(15) C107 0.049(2) 0.065(2) 0.057(2) 0.0086(19) 0.0000(17) 0.0131(17) C108 0.067(3) 0.059(2) 0.071(3) -0.008(2) -0.015(2) 0.0173(19) C109 0.070(3) 0.094(3) 0.059(3) -0.020(2) -0.004(2) 0.029(2) C110 0.068(3) 0.104(3) 0.046(2) 0.000(2) 0.009(2) 0.008(2) C111 0.056(2) 0.073(2) 0.050(2) 0.0033(19) 0.0072(18) -0.0003(19) C112 0.052(2) 0.062(2) 0.044(2) -0.0027(17) 0.0034(16) 0.0156(17) C113 0.048(2) 0.074(3) 0.063(3) 0.005(2) 0.0040(18) 0.0169(18) C114 0.079(3) 0.095(3) 0.072(3) 0.013(2) 0.000(2) 0.040(3) C115 0.053(3) 0.128(4) 0.081(3) -0.006(3) -0.003(2) 0.042(3) C116 0.046(2) 0.108(4) 0.090(3) -0.003(3) 0.008(2) 0.018(2) C117 0.0289(16) 0.062(2) 0.054(2) -0.0025(17) -0.0027(15) 0.0101(15) C118 0.0425(19) 0.065(2) 0.047(2) 0.0042(17) 0.0031(16) 0.0051(16) C119 0.076(3) 0.086(3) 0.054(3) 0.013(2) -0.004(2) 0.020(2) C120 0.117(4) 0.106(4) 0.076(4) 0.033(3) -0.017(3) 0.020(3) C121 0.119(5) 0.149(5) 0.060(3) 0.041(3) 0.002(3) 0.010(4) C122 0.101(4) 0.174(6) 0.050(3) 0.015(3) 0.023(3) 0.028(4) C123 0.085(3) 0.112(4) 0.052(3) 0.007(2) 0.012(2) 0.029(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 N1 1.817(3) . ? Re1 N3 2.235(2) . ? Re1 P1 2.3623(9) . ? Re1 P2 2.4064(9) . ? Re1 P3 2.4125(9) . ? Re1 Cl1 2.4383(11) . ? P1 O1 1.601(2) . ? P1 O2 1.601(2) . ? P1 C6 1.817(3) . ? P2 O4 1.593(2) . ? P2 O3 1.610(2) . ? P2 C16 1.811(3) . ? P3 O6 1.602(2) . ? P3 O5 1.609(2) . ? P3 C26 1.812(3) . ? O1 C2 1.446(4) . ? O2 C4 1.458(4) . ? O3 C12 1.433(4) . ? O4 C14 1.448(4) . ? O5 C22 1.459(4) . ? O6 C24 1.454(4) . ? N1 N2 1.200(4) . ? N2 C32 1.431(5) . ? N3 N4 1.445(4) . ? N4 C1 1.480(5) . ? B1 C100 1.636(5) . ? B1 C118 1.651(5) . ? B1 C112 1.650(5) . ? B1 C106 1.650(5) . ? C2 C3 1.499(5) . ? C4 C5 1.428(6) . ? C6 C7 1.385(4) . ? C6 C11 1.389(4) . ? C7 C8 1.392(5) . ? C8 C9 1.358(5) . ? C9 C10 1.361(5) . ? C10 C11 1.383(5) . ? C12 C13 1.481(6) . ? C14 C15 1.503(5) . ? C16 C21 1.389(4) . ? C16 C17 1.398(5) . ? C17 C18 1.393(5) . ? C18 C19 1.362(6) . ? C19 C20 1.374(6) . ? C20 C21 1.383(5) . ? C22 C23 1.461(5) . ? C24 C25 1.311(10) . ? C24 C25 1.363(9) . ? C26 C31 1.383(4) . ? C26 C27 1.389(4) . ? C27 C28 1.363(5) . ? C28 C29 1.362(6) . ? C29 C30 1.383(6) . ? C30 C31 1.392(5) . ? C100 C101 1.403(5) . ? C100 C105 1.402(5) . ? C101 C102 1.389(5) . ? C102 C103 1.374(6) . ? C103 C104 1.378(6) . ? C104 C105 1.398(5) . ? C106 C107 1.399(5) . ? C106 C111 1.405(5) . ? C107 C108 1.393(5) . ? C108 C109 1.381(5) . ? C109 C110 1.374(6) . ? C110 C111 1.391(5) . ? C112 C113 1.390(5) . ? C112 C117 1.446(5) . ? C113 C114 1.406(5) . ? C114 C115 1.377(6) . ? C115 C116 1.372(6) . ? C116 C117 1.399(5) . ? C118 C119 1.389(5) . ? C118 C123 1.394(5) . ? C119 C120 1.390(6) . ? C120 C121 1.353(7) . ? C121 C122 1.364(7) . ? C122 C123 1.400(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 N1 Re1 N3 95.36(11) . . ? N1 Re1 P1 91.14(8) . . ? N3 Re1 P1 173.48(7) . . ? N1 Re1 P2 92.17(8) . . ? N3 Re1 P2 87.45(8) . . ? P1 Re1 P2 91.78(3) . . ? N1 Re1 P3 91.34(8) . . ? N3 Re1 P3 85.43(8) . . ? P1 Re1 P3 94.97(3) . . ? P2 Re1 P3 172.33(3) . . ? N1 Re1 Cl1 175.66(8) . . ? N3 Re1 Cl1 80.65(8) . . ? P1 Re1 Cl1 92.87(4) . . ? P2 Re1 Cl1 89.38(3) . . ? P3 Re1 Cl1 86.66(3) . . ? O1 P1 O2 105.54(12) . . ? O1 P1 C6 97.32(13) . . ? O2 P1 C6 104.21(13) . . ? O1 P1 Re1 119.37(9) . . ? O2 P1 Re1 112.38(8) . . ? C6 P1 Re1 116.00(10) . . ? O4 P2 O3 105.56(13) . . ? O4 P2 C16 97.75(14) . . ? O3 P2 C16 104.84(14) . . ? O4 P2 Re1 121.19(10) . . ? O3 P2 Re1 105.10(9) . . ? C16 P2 Re1 120.67(11) . . ? O6 P3 O5 104.52(12) . . ? O6 P3 C26 98.40(13) . . ? O5 P3 C26 104.59(13) . . ? O6 P3 Re1 126.00(8) . . ? O5 P3 Re1 106.67(8) . . ? C26 P3 Re1 114.55(10) . . ? C2 O1 P1 124.8(2) . . ? C4 O2 P1 121.9(2) . . ? C12 O3 P2 124.5(2) . . ? C14 O4 P2 125.4(2) . . ? C22 O5 P3 123.7(2) . . ? C24 O6 P3 126.0(2) . . ? N2 N1 Re1 173.3(3) . . ? N1 N2 C32 125.0(4) . . ? N4 N3 Re1 115.6(2) . . ? N3 N4 C1 108.8(3) . . ? C100 B1 C118 104.5(3) . . ? C100 B1 C112 113.1(3) . . ? C118 B1 C112 111.0(3) . . ? C100 B1 C106 112.9(3) . . ? C118 B1 C106 112.2(3) . . ? C112 B1 C106 103.3(3) . . ? O1 C2 C3 106.6(3) . . ? C5 C4 O2 110.9(4) . . ? C7 C6 C11 118.4(3) . . ? C7 C6 P1 119.1(2) . . ? C11 C6 P1 122.5(3) . . ? C6 C7 C8 120.1(4) . . ? C9 C8 C7 120.5(4) . . ? C8 C9 C10 120.2(4) . . ? C9 C10 C11 120.3(4) . . ? C10 C11 C6 120.5(4) . . ? O3 C12 C13 108.0(3) . . ? O4 C14 C15 107.8(3) . . ? C21 C16 C17 118.6(3) . . ? C21 C16 P2 122.0(3) . . ? C17 C16 P2 119.3(3) . . ? C18 C17 C16 119.9(4) . . ? C19 C18 C17 120.5(4) . . ? C18 C19 C20 120.1(4) . . ? C19 C20 C21 120.4(4) . . ? C20 C21 C16 120.4(4) . . ? O5 C22 C23 108.3(3) . . ? C25 C24 C25 55.0(6) . . ? C25 C24 O6 117.7(6) . . ? C25 C24 O6 114.4(5) . . ? C31 C26 C27 119.6(3) . . ? C31 C26 P3 121.3(2) . . ? C27 C26 P3 119.0(3) . . ? C28 C27 C26 120.9(4) . . ? C29 C28 C27 119.7(4) . . ? C28 C29 C30 120.9(4) . . ? C29 C30 C31 119.7(4) . . ? C26 C31 C30 119.1(3) . . ? C101 C100 C105 113.9(3) . . ? C101 C100 B1 123.5(3) . . ? C105 C100 B1 122.4(3) . . ? C102 C101 C100 123.5(4) . . ? C103 C102 C101 120.3(4) . . ? C102 C103 C104 118.8(4) . . ? C103 C104 C105 120.1(4) . . ? C104 C105 C100 123.3(4) . . ? C107 C106 C111 114.0(3) . . ? C107 C106 B1 123.7(3) . . ? C111 C106 B1 122.0(3) . . ? C108 C107 C106 123.9(4) . . ? C109 C108 C107 119.4(4) . . ? C110 C109 C108 119.2(4) . . ? C109 C110 C111 120.4(4) . . ? C110 C111 C106 123.0(4) . . ? C113 C112 C117 116.9(3) . . ? C113 C112 B1 122.6(3) . . ? C117 C112 B1 120.0(3) . . ? C112 C113 C114 122.7(4) . . ? C115 C114 C113 119.5(4) . . ? C116 C115 C114 119.4(4) . . ? C115 C116 C117 122.9(4) . . ? C116 C117 C112 118.5(4) . . ? C119 C118 C123 113.6(4) . . ? C119 C118 B1 123.4(3) . . ? C123 C118 B1 122.8(3) . . ? C120 C119 C118 123.4(4) . . ? C121 C120 C119 120.8(5) . . ? C120 C121 C122 118.9(5) . . ? C121 C122 C123 119.9(5) . . ? C118 C123 C122 123.4(4) . . ? _diffrn_measured_fraction_theta_max .996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full .996 _refine_diff_density_max 1.471 _refine_diff_density_min -1.880 _refine_diff_density_rms .084 data_Compound_[ReCl(PhN2){PPh(OEt)2}4]BPh4 (7) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H85 B Cl N2 O8 P4 Re' _chemical_formula_weight 1254.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'P21/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 19.613(5) _cell_length_b 20.101(5) _cell_length_c 19.918(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.12(2) _cell_angle_gamma 90.00 _cell_volume 7110(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.57 _cell_measurement_theta_max 7.23 _exptl_crystal_description 'prisms' _exptl_crystal_colour 'red' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 1.889 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min .796 _exptl_absorpt_correction_T_max 1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW100 diffractometer' _diffrn_measurement_method '\q/2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16450 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1798 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 28.01 _reflns_number_total 16450 _reflns_number_gt 7496 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16450 _refine_ls_number_parameters 800 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1902 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.772785(15) 0.095274(15) 0.452892(15) 0.03246(9) Uani 1 d . . . P1 P 0.77675(10) 0.00877(10) 0.36857(11) 0.0369(5) Uani 1 d . . . P2 P 0.74570(11) 0.00480(10) 0.52023(10) 0.0375(5) Uani 1 d . . . P3 P 0.79542(11) 0.17828(10) 0.54943(10) 0.0394(5) Uani 1 d . . . P4 P 0.79554(11) 0.18457(10) 0.38029(11) 0.0414(5) Uani 1 d . . . Cl Cl 0.90824(9) 0.07710(10) 0.51703(10) 0.0486(5) Uani 1 d . . . O1 O 0.8275(2) 0.0305(2) 0.3275(3) 0.0453(13) Uani 1 d . . . O2 O 0.8082(3) -0.0621(2) 0.4032(3) 0.0497(14) Uani 1 d . . . O3 O 0.7036(3) 0.0347(2) 0.5670(2) 0.0458(13) Uani 1 d . . . O4 O 0.8113(3) -0.0419(2) 0.5755(2) 0.0490(14) Uani 1 d . . . O5 O 0.8562(3) 0.2306(3) 0.5486(3) 0.0592(16) Uani 1 d . . . O6 O 0.7180(3) 0.2155(2) 0.5323(2) 0.0484(13) Uani 1 d . . . O7 O 0.7444(3) 0.1669(2) 0.2951(2) 0.0543(14) Uani 1 d . . . O8 O 0.8779(3) 0.2012(3) 0.3874(3) 0.0600(15) Uani 1 d . . . N1 N 0.6744(3) 0.1152(3) 0.4040(3) 0.0366(15) Uani 1 d . . . N2 N 0.6103(3) 0.1316(3) 0.3629(3) 0.0432(16) Uani 1 d . . . C1 C 0.5521(4) 0.1488(3) 0.3856(4) 0.0388(18) Uani 1 d . . . C2 C 0.4919(4) 0.1821(4) 0.3332(4) 0.058(2) Uani 1 d . . . H2 H 0.4910 0.1928 0.2874 0.070 Uiso 1 calc R . . C3 C 0.4323(5) 0.1995(4) 0.3499(6) 0.078(3) Uani 1 d . . . H3 H 0.3910 0.2221 0.3152 0.093 Uiso 1 calc R . . C4 C 0.4345(5) 0.1832(5) 0.4185(6) 0.076(3) Uani 1 d . . . H4 H 0.3947 0.1946 0.4299 0.092 Uiso 1 calc R . . C5 C 0.4950(5) 0.1504(5) 0.4687(5) 0.073(3) Uani 1 d . . . H5 H 0.4960 0.1395 0.5145 0.087 Uiso 1 calc R . . C6 C 0.5554(4) 0.1326(4) 0.4539(4) 0.053(2) Uani 1 d . . . H6 H 0.5968 0.1103 0.4890 0.064 Uiso 1 calc R . . C7 C 0.8304(4) -0.0077(5) 0.2671(5) 0.073(3) Uani 1 d . . . H7A H 0.7992 0.0136 0.2204 0.087 Uiso 1 calc R . . H7B H 0.8105 -0.0519 0.2668 0.087 Uiso 1 calc R . . C8 C 0.9083(5) -0.0129(5) 0.2745(5) 0.100(4) Uani 1 d . . . H8A H 0.9307 0.0305 0.2823 0.150 Uiso 1 calc R . . H8B H 0.9079 -0.0318 0.2300 0.150 Uiso 1 calc R . . H8C H 0.9371 -0.0410 0.3159 0.150 Uiso 1 calc R . . C9 C 0.8867(4) -0.0797(4) 0.4476(4) 0.065(3) Uani 1 d . . . H9A H 0.8990 -0.0747 0.5000 0.078 Uiso 1 calc R . . H9B H 0.9195 -0.0509 0.4355 0.078 Uiso 1 calc R . . C10 C 0.8970(5) -0.1501(4) 0.4309(6) 0.120(4) Uani 1 d . . . H10A H 0.8690 -0.1787 0.4486 0.179 Uiso 1 calc R . . H10B H 0.9495 -0.1615 0.4550 0.179 Uiso 1 calc R . . H10C H 0.8793 -0.1556 0.3783 0.179 Uiso 1 calc R . . C11 C 0.6888(4) -0.0186(4) 0.2950(4) 0.0359(18) Uani 1 d . . . C12 C 0.6372(4) 0.0287(4) 0.2527(4) 0.044(2) Uani 1 d . . . H12 H 0.6477 0.0737 0.2625 0.053 Uiso 1 calc R . . C13 C 0.5698(4) 0.0087(5) 0.1956(4) 0.060(2) Uani 1 d . . . H13 H 0.5350 0.0407 0.1679 0.071 Uiso 1 calc R . . C14 C 0.5537(5) -0.0572(5) 0.1794(4) 0.062(3) Uani 1 d . . . H14 H 0.5085 -0.0701 0.1408 0.075 Uiso 1 calc R . . C15 C 0.6051(5) -0.1036(5) 0.2206(5) 0.067(3) Uani 1 d . . . H15 H 0.5949 -0.1485 0.2098 0.080 Uiso 1 calc R . . C16 C 0.6725(4) -0.0848(4) 0.2786(4) 0.051(2) Uani 1 d . . . H16 H 0.7067 -0.1170 0.3065 0.061 Uiso 1 calc R . . C17 C 0.6787(5) -0.0075(4) 0.6123(4) 0.066(3) Uani 1 d . . . H17A H 0.6707 -0.0524 0.5927 0.079 Uiso 1 calc R . . H17B H 0.7180 -0.0091 0.6626 0.079 Uiso 1 calc R . . C18 C 0.6104(5) 0.0166(5) 0.6137(5) 0.100(4) Uani 1 d . . . H18A H 0.6169 0.0622 0.6294 0.149 Uiso 1 calc R . . H18B H 0.5987 -0.0097 0.6477 0.149 Uiso 1 calc R . . H18C H 0.5700 0.0133 0.5650 0.149 Uiso 1 calc R . . C19 C 0.8733(5) -0.0163(5) 0.6404(5) 0.088(3) Uani 1 d . . . H19A H 0.9159 -0.0084 0.6288 0.106 Uiso 1 calc R . . H19B H 0.8589 0.0260 0.6540 0.106 Uiso 1 calc R . . C20 C 0.8956(5) -0.0607(5) 0.7021(5) 0.108(4) Uani 1 d . . . H20A H 0.8530 -0.0705 0.7123 0.163 Uiso 1 calc R . . H20B H 0.9344 -0.0404 0.7448 0.163 Uiso 1 calc R . . H20C H 0.9143 -0.1012 0.6906 0.163 Uiso 1 calc R . . C21 C 0.6828(4) -0.0611(4) 0.4658(4) 0.0387(19) Uani 1 d . . . C22 C 0.6090(4) -0.0441(4) 0.4135(4) 0.047(2) Uani 1 d . . . H22 H 0.5938 0.0001 0.4073 0.057 Uiso 1 calc R . . C23 C 0.5603(4) -0.0923(5) 0.3724(4) 0.057(2) Uani 1 d . . . H23 H 0.5122 -0.0808 0.3382 0.069 Uiso 1 calc R . . C24 C 0.5822(5) -0.1585(5) 0.3813(5) 0.061(2) Uani 1 d . . . H24 H 0.5486 -0.1911 0.3530 0.073 Uiso 1 calc R . . C25 C 0.6531(5) -0.1765(4) 0.4314(4) 0.062(2) Uani 1 d . . . H25 H 0.6678 -0.2209 0.4373 0.074 Uiso 1 calc R . . C26 C 0.7019(4) -0.1277(4) 0.4728(4) 0.053(2) Uani 1 d . . . H26 H 0.7498 -0.1401 0.5070 0.063 Uiso 1 calc R . . C27 C 0.8886(5) 0.2860(4) 0.5997(4) 0.073(3) Uani 1 d . . . H27A H 0.8795 0.2798 0.6435 0.088 Uiso 1 calc R . . H27B H 0.8647 0.3273 0.5761 0.088 Uiso 1 calc R . . C28 C 0.9726(6) 0.2899(5) 0.6219(5) 0.122(5) Uani 1 d . . . H28A H 0.9968 0.2512 0.6501 0.183 Uiso 1 calc R . . H28B H 0.9927 0.3290 0.6514 0.183 Uiso 1 calc R . . H28C H 0.9815 0.2921 0.5781 0.183 Uiso 1 calc R . . C29 C 0.7111(5) 0.2782(4) 0.5662(5) 0.070(3) Uani 1 d . . . H29A H 0.7325 0.3144 0.5492 0.084 Uiso 1 calc R . . H29B H 0.7376 0.2753 0.6198 0.084 Uiso 1 calc R . . C30 C 0.6299(5) 0.2897(4) 0.5437(5) 0.082(3) Uani 1 d . . . H30A H 0.6035 0.2873 0.4907 0.123 Uiso 1 calc R . . H30B H 0.6228 0.3329 0.5603 0.123 Uiso 1 calc R . . H30C H 0.6107 0.2564 0.5657 0.123 Uiso 1 calc R . . C31 C 0.8331(4) 0.1563(4) 0.6470(4) 0.0386(19) Uani 1 d . . . C32 C 0.9102(4) 0.1451(4) 0.6870(4) 0.054(2) Uani 1 d . . . H32 H 0.9425 0.1502 0.6642 0.065 Uiso 1 calc R . . C33 C 0.9380(5) 0.1267(4) 0.7599(5) 0.063(2) Uani 1 d . . . H33 H 0.9893 0.1192 0.7864 0.076 Uiso 1 calc R . . C34 C 0.8910(6) 0.1192(5) 0.7945(5) 0.076(3) Uani 1 d . . . H34 H 0.9107 0.1070 0.8442 0.091 Uiso 1 calc R . . C35 C 0.8148(5) 0.1298(5) 0.7557(5) 0.075(3) Uani 1 d . . . H35 H 0.7828 0.1244 0.7789 0.090 Uiso 1 calc R . . C36 C 0.7866(4) 0.1482(4) 0.6829(4) 0.050(2) Uani 1 d . . . H36 H 0.7352 0.1555 0.6568 0.060 Uiso 1 calc R . . C37 C 0.7350(6) 0.2128(5) 0.2348(4) 0.098(4) Uani 1 d . . . H37A H 0.6965 0.2450 0.2303 0.118 Uiso 1 calc R . . H37B H 0.7818 0.2368 0.2478 0.118 Uiso 1 calc R . . C38 C 0.7160(8) 0.1837(6) 0.1692(6) 0.175(7) Uani 1 d . . . H38A H 0.7472 0.1454 0.1751 0.263 Uiso 1 calc R . . H38B H 0.7229 0.2145 0.1358 0.263 Uiso 1 calc R . . H38C H 0.6642 0.1702 0.1494 0.263 Uiso 1 calc R . . C39 C 0.9255(5) 0.1581(4) 0.3677(5) 0.079(3) Uani 1 d . . . H39A H 0.8945 0.1270 0.3299 0.095 Uiso 1 calc R . . H39B H 0.9582 0.1328 0.4109 0.095 Uiso 1 calc R . . C40 C 0.9707(5) 0.1967(5) 0.3402(6) 0.113(4) Uani 1 d . . . H40A H 0.9384 0.2185 0.2950 0.170 Uiso 1 calc R . . H40B H 1.0048 0.1677 0.3311 0.170 Uiso 1 calc R . . H40C H 0.9990 0.2295 0.3765 0.170 Uiso 1 calc R . . C41 C 0.7675(4) 0.2698(4) 0.3884(4) 0.0435(19) Uani 1 d . . . C42 C 0.8173(5) 0.3214(4) 0.4075(5) 0.066(3) Uani 1 d . . . H42 H 0.8671 0.3131 0.4165 0.079 Uiso 1 calc R . . C43 C 0.7957(6) 0.3851(5) 0.4136(5) 0.086(3) Uani 1 d . . . H43 H 0.8299 0.4201 0.4253 0.103 Uiso 1 calc R . . C44 C 0.7217(7) 0.3962(5) 0.4019(5) 0.087(3) Uani 1 d . . . H44 H 0.7065 0.4390 0.4069 0.104 Uiso 1 calc R . . C45 C 0.6719(5) 0.3463(5) 0.3835(5) 0.081(3) Uani 1 d . . . H45 H 0.6223 0.3544 0.3755 0.098 Uiso 1 calc R . . C46 C 0.6946(5) 0.2828(4) 0.3766(5) 0.069(3) Uani 1 d . . . H46 H 0.6599 0.2482 0.3636 0.083 Uiso 1 calc R . . C47 C 0.8463(4) -0.3916(4) 0.5453(3) 0.0375(19) Uani 1 d . . . C48 C 0.8902(4) -0.3377(4) 0.5464(4) 0.047(2) Uani 1 d . . . H48 H 0.8847 -0.2984 0.5683 0.056 Uiso 1 calc R . . C49 C 0.9427(4) -0.3393(4) 0.5161(4) 0.059(2) Uani 1 d . . . H49 H 0.9713 -0.3018 0.5183 0.071 Uiso 1 calc R . . C50 C 0.9520(4) -0.3963(5) 0.4833(4) 0.058(2) Uani 1 d . . . H50 H 0.9867 -0.3977 0.4629 0.070 Uiso 1 calc R . . C51 C 0.9097(5) -0.4512(4) 0.4808(4) 0.065(3) Uani 1 d . . . H51 H 0.9157 -0.4903 0.4589 0.077 Uiso 1 calc R . . C52 C 0.8579(4) -0.4483(4) 0.5110(4) 0.053(2) Uani 1 d . . . H52 H 0.8294 -0.4860 0.5083 0.064 Uiso 1 calc R . . C53 C 0.7832(4) -0.4614(4) 0.6197(4) 0.0427(19) Uani 1 d . . . C54 C 0.8480(5) -0.4974(4) 0.6599(4) 0.062(2) Uani 1 d . . . H54 H 0.8931 -0.4814 0.6613 0.074 Uiso 1 calc R . . C55 C 0.8503(6) -0.5562(5) 0.6985(5) 0.080(3) Uani 1 d . . . H55 H 0.8960 -0.5778 0.7245 0.096 Uiso 1 calc R . . C56 C 0.7862(7) -0.5815(5) 0.6980(5) 0.085(3) Uani 1 d . . . H56 H 0.7872 -0.6202 0.7240 0.102 Uiso 1 calc R . . C57 C 0.7206(6) -0.5492(5) 0.6588(5) 0.076(3) Uani 1 d . . . H57 H 0.6757 -0.5661 0.6571 0.091 Uiso 1 calc R . . C58 C 0.7202(5) -0.4905(4) 0.6210(4) 0.058(2) Uani 1 d . . . H58 H 0.6741 -0.4696 0.5948 0.069 Uiso 1 calc R . . C59 C 0.8050(4) -0.3307(4) 0.6424(4) 0.0380(19) Uani 1 d . . . C60 C 0.8536(4) -0.3397(4) 0.7166(4) 0.051(2) Uani 1 d . . . H60 H 0.8751 -0.3815 0.7313 0.062 Uiso 1 calc R . . C61 C 0.8719(4) -0.2905(5) 0.7698(4) 0.060(2) Uani 1 d . . . H61 H 0.9046 -0.2997 0.8188 0.072 Uiso 1 calc R . . C62 C 0.8418(5) -0.2281(5) 0.7501(5) 0.068(3) Uani 1 d . . . H62 H 0.8529 -0.1947 0.7855 0.081 Uiso 1 calc R . . C63 C 0.7951(5) -0.2161(4) 0.6775(5) 0.068(3) Uani 1 d . . . H63 H 0.7743 -0.1740 0.6633 0.082 Uiso 1 calc R . . C64 C 0.7784(4) -0.2654(4) 0.6252(4) 0.055(2) Uani 1 d . . . H64 H 0.7480 -0.2550 0.5760 0.066 Uiso 1 calc R . . C65 C 0.7006(4) -0.3747(4) 0.5124(4) 0.0426(19) Uani 1 d . . . C66 C 0.6405(4) -0.3487(4) 0.5244(5) 0.059(2) Uani 1 d . . . H66 H 0.6483 -0.3397 0.5729 0.071 Uiso 1 calc R . . C67 C 0.5702(5) -0.3356(4) 0.4682(6) 0.075(3) Uani 1 d . . . H67 H 0.5321 -0.3189 0.4796 0.090 Uiso 1 calc R . . C68 C 0.5563(5) -0.3471(5) 0.3955(6) 0.088(4) Uani 1 d . . . H68 H 0.5091 -0.3382 0.3576 0.106 Uiso 1 calc R . . C69 C 0.6122(6) -0.3717(5) 0.3795(5) 0.091(4) Uani 1 d . . . H69 H 0.6036 -0.3794 0.3306 0.110 Uiso 1 calc R . . C70 C 0.6827(4) -0.3853(4) 0.4368(4) 0.062(3) Uani 1 d . . . H70 H 0.7199 -0.4024 0.4244 0.075 Uiso 1 calc R . . B B 0.7835(4) -0.3900(4) 0.5800(4) 0.040(2) Uani 1 d . . . C101 C 0.0478(9) 0.0421(9) 0.9495(9) 0.072(5) Uiso 0.50 d P . . C102 C 0.0073(9) 0.0113(8) 0.9760(8) 0.056(5) Uiso 0.50 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 Re 0.03514(15) 0.03165(15) 0.03070(14) -0.00347(17) 0.01409(11) -0.00652(17) P1 0.0378(11) 0.0343(13) 0.0414(12) -0.0093(10) 0.0196(9) -0.0078(10) P2 0.0399(12) 0.0321(12) 0.0394(11) 0.0030(10) 0.0159(9) -0.0050(10) P3 0.0473(13) 0.0375(13) 0.0349(11) -0.0048(9) 0.0188(10) -0.0080(10) P4 0.0510(13) 0.0386(13) 0.0388(12) -0.0042(10) 0.0231(10) -0.0142(10) Cl 0.0364(10) 0.0572(15) 0.0463(11) -0.0041(10) 0.0119(8) -0.0068(9) O1 0.047(3) 0.048(3) 0.052(3) -0.020(3) 0.030(3) -0.014(3) O2 0.040(3) 0.036(3) 0.068(4) 0.000(3) 0.017(3) 0.001(3) O3 0.054(3) 0.046(4) 0.044(3) 0.001(3) 0.028(3) -0.007(3) O4 0.042(3) 0.042(3) 0.047(3) 0.008(3) 0.003(3) -0.002(3) O5 0.088(4) 0.051(4) 0.049(3) -0.022(3) 0.040(3) -0.034(3) O6 0.052(3) 0.038(3) 0.046(3) -0.009(3) 0.013(3) 0.010(3) O7 0.078(4) 0.048(4) 0.033(3) 0.000(3) 0.020(3) -0.016(3) O8 0.067(4) 0.056(4) 0.075(4) -0.015(3) 0.047(3) -0.021(3) N1 0.047(4) 0.038(4) 0.027(3) 0.001(3) 0.018(3) -0.004(3) N2 0.038(4) 0.043(4) 0.042(4) 0.003(3) 0.011(3) -0.001(3) C1 0.032(4) 0.027(4) 0.055(5) -0.003(4) 0.016(4) -0.003(3) C2 0.052(5) 0.060(6) 0.059(6) 0.003(5) 0.020(5) 0.012(5) C3 0.055(6) 0.062(7) 0.102(8) -0.005(6) 0.019(6) 0.019(5) C4 0.062(7) 0.071(8) 0.113(9) -0.014(7) 0.053(7) 0.002(6) C5 0.070(7) 0.083(8) 0.085(7) 0.009(6) 0.052(6) 0.011(6) C6 0.053(5) 0.059(6) 0.052(5) 0.010(5) 0.027(4) 0.011(4) C7 0.064(6) 0.095(8) 0.079(6) -0.047(6) 0.050(5) -0.025(5) C8 0.093(8) 0.126(10) 0.110(8) -0.044(7) 0.072(7) -0.013(7) C9 0.045(5) 0.052(7) 0.080(6) -0.009(5) 0.009(4) 0.003(4) C10 0.079(8) 0.047(7) 0.198(12) -0.022(8) 0.024(8) 0.020(6) C11 0.038(4) 0.035(5) 0.038(4) -0.014(4) 0.020(4) -0.013(4) C12 0.043(5) 0.045(5) 0.037(4) -0.010(4) 0.010(4) -0.011(4) C13 0.050(5) 0.074(7) 0.044(5) -0.008(5) 0.010(4) -0.002(5) C14 0.047(5) 0.082(8) 0.050(5) -0.028(5) 0.013(4) -0.024(5) C15 0.069(6) 0.062(7) 0.070(6) -0.029(5) 0.031(5) -0.032(5) C16 0.051(5) 0.044(6) 0.050(5) -0.015(4) 0.014(4) -0.010(4) C17 0.089(7) 0.059(6) 0.071(6) 0.017(5) 0.056(6) 0.000(5) C18 0.100(8) 0.104(9) 0.132(9) 0.041(7) 0.085(7) 0.021(7) C19 0.083(7) 0.073(8) 0.060(6) 0.014(6) -0.016(5) -0.029(6) C20 0.082(8) 0.112(10) 0.087(8) 0.032(7) -0.008(6) -0.005(7) C21 0.043(5) 0.026(5) 0.052(5) 0.006(4) 0.025(4) -0.005(4) C22 0.046(5) 0.048(6) 0.053(5) 0.000(4) 0.025(4) -0.005(4) C23 0.032(4) 0.081(7) 0.055(5) -0.010(6) 0.014(4) -0.020(5) C24 0.061(6) 0.056(7) 0.066(6) -0.016(5) 0.028(5) -0.032(5) C25 0.073(7) 0.046(6) 0.065(6) -0.002(5) 0.027(5) -0.020(5) C26 0.049(5) 0.052(6) 0.054(5) 0.008(5) 0.020(4) -0.011(5) C27 0.109(8) 0.059(6) 0.059(6) -0.023(5) 0.043(6) -0.045(6) C28 0.142(10) 0.147(11) 0.111(9) -0.055(8) 0.088(8) -0.103(9) C29 0.083(7) 0.041(6) 0.074(6) -0.012(5) 0.022(5) 0.021(5) C30 0.085(7) 0.071(7) 0.086(7) -0.014(6) 0.033(6) 0.023(6) C31 0.042(5) 0.045(5) 0.031(4) -0.004(4) 0.017(4) -0.004(4) C32 0.045(5) 0.066(6) 0.053(5) -0.014(5) 0.022(4) -0.011(4) C33 0.050(5) 0.076(7) 0.050(6) -0.003(5) 0.008(5) 0.003(5) C34 0.094(8) 0.093(8) 0.039(5) 0.012(5) 0.026(5) 0.015(6) C35 0.078(7) 0.106(9) 0.053(6) 0.012(6) 0.040(5) 0.006(6) C36 0.044(5) 0.063(6) 0.046(5) -0.002(4) 0.023(4) -0.001(4) C37 0.173(11) 0.080(8) 0.032(5) 0.013(5) 0.035(6) -0.027(7) C38 0.321(19) 0.125(12) 0.056(8) 0.017(8) 0.057(10) 0.013(12) C39 0.074(7) 0.068(7) 0.120(8) 0.004(6) 0.064(6) -0.006(6) C40 0.135(10) 0.092(9) 0.181(11) -0.045(8) 0.133(9) -0.042(7) C41 0.055(5) 0.034(5) 0.044(5) -0.001(4) 0.023(4) -0.003(4) C42 0.075(6) 0.049(6) 0.083(7) -0.009(5) 0.041(5) -0.013(5) C43 0.114(9) 0.040(7) 0.116(9) -0.019(6) 0.061(8) -0.019(6) C44 0.145(10) 0.030(6) 0.090(7) 0.012(6) 0.054(8) 0.017(7) C45 0.073(7) 0.059(7) 0.104(8) 0.025(6) 0.030(6) 0.015(6) C46 0.071(7) 0.031(6) 0.099(7) 0.014(5) 0.030(6) -0.005(5) C47 0.032(4) 0.045(6) 0.031(4) -0.002(4) 0.010(3) -0.002(4) C48 0.051(5) 0.042(5) 0.054(5) 0.002(4) 0.029(4) 0.006(4) C49 0.067(6) 0.055(6) 0.070(6) 0.007(5) 0.044(5) -0.013(5) C50 0.067(6) 0.061(7) 0.060(5) -0.002(5) 0.041(5) -0.001(5) C51 0.083(7) 0.053(6) 0.077(6) -0.021(5) 0.052(6) -0.009(5) C52 0.050(5) 0.054(6) 0.067(6) -0.014(5) 0.035(4) -0.012(4) C53 0.048(5) 0.037(5) 0.047(5) -0.008(4) 0.023(4) -0.003(4) C54 0.071(6) 0.048(6) 0.072(6) 0.012(5) 0.036(5) 0.011(5) C55 0.112(9) 0.051(7) 0.081(7) 0.020(6) 0.044(7) 0.025(6) C56 0.145(11) 0.046(7) 0.072(7) 0.015(5) 0.053(8) 0.001(7) C57 0.091(8) 0.066(7) 0.081(7) 0.006(6) 0.045(6) -0.025(6) C58 0.071(6) 0.051(6) 0.057(6) -0.004(5) 0.033(5) -0.004(5) C59 0.031(4) 0.035(5) 0.051(5) 0.002(4) 0.021(4) -0.003(4) C60 0.045(5) 0.047(6) 0.052(5) -0.003(4) 0.011(4) 0.005(4) C61 0.046(5) 0.092(8) 0.034(5) -0.013(5) 0.009(4) -0.008(5) C62 0.073(7) 0.053(7) 0.071(7) -0.017(5) 0.025(5) -0.006(5) C63 0.075(7) 0.048(6) 0.068(6) 0.002(5) 0.016(5) 0.012(5) C64 0.067(6) 0.041(6) 0.046(5) -0.003(4) 0.013(4) 0.002(5) C65 0.041(5) 0.036(5) 0.053(5) -0.005(4) 0.022(4) -0.007(4) C66 0.046(5) 0.058(6) 0.070(6) 0.000(5) 0.021(5) 0.002(5) C67 0.038(6) 0.065(7) 0.111(8) -0.001(7) 0.019(6) 0.005(5) C68 0.045(6) 0.076(8) 0.103(9) 0.004(7) -0.007(6) 0.001(6) C69 0.079(8) 0.114(10) 0.051(6) -0.001(6) -0.002(6) 0.010(7) C70 0.052(5) 0.073(7) 0.054(5) -0.007(5) 0.014(4) 0.004(5) B 0.030(5) 0.048(7) 0.041(5) 0.003(4) 0.014(4) -0.003(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 Re N1 1.799(6) . ? Re Cl 2.4376(19) . ? Re P3 2.440(2) . ? Re P1 2.442(2) . ? Re P2 2.448(2) . ? Re P4 2.462(2) . ? P1 O2 1.589(5) . ? P1 O1 1.594(5) . ? P1 C11 1.812(7) . ? P2 O4 1.596(5) . ? P2 O3 1.601(5) . ? P2 C21 1.822(7) . ? P3 O5 1.594(5) . ? P3 O6 1.594(5) . ? P3 C31 1.817(7) . ? P4 O8 1.596(5) . ? P4 O7 1.602(5) . ? P4 C41 1.827(8) . ? O1 C7 1.449(8) . ? O2 C9 1.457(8) . ? O3 C17 1.465(8) . ? O4 C19 1.443(8) . ? O5 C27 1.460(8) . ? O6 C29 1.462(8) . ? O7 C37 1.462(8) . ? O8 C39 1.443(8) . ? N1 N2 1.220(7) . ? N2 C1 1.436(8) . ? C1 C2 1.373(9) . ? C1 C6 1.374(9) . ? C2 C3 1.388(10) . ? C3 C4 1.389(11) . ? C4 C5 1.355(11) . ? C5 C6 1.384(9) . ? C7 C8 1.475(10) . ? C9 C10 1.488(10) . ? C11 C16 1.374(9) . ? C11 C12 1.382(9) . ? C12 C13 1.387(9) . ? C13 C14 1.370(10) . ? C14 C15 1.363(11) . ? C15 C16 1.388(9) . ? C17 C18 1.436(10) . ? C19 C20 1.429(10) . ? C21 C26 1.382(9) . ? C21 C22 1.420(9) . ? C22 C23 1.362(9) . ? C23 C24 1.386(10) . ? C24 C25 1.371(10) . ? C25 C26 1.373(9) . ? C27 C28 1.517(11) . ? C29 C30 1.479(10) . ? C31 C36 1.385(9) . ? C31 C32 1.396(9) . ? C32 C33 1.367(10) . ? C33 C34 1.372(10) . ? C34 C35 1.376(10) . ? C35 C36 1.366(9) . ? C37 C38 1.333(11) . ? C39 C40 1.450(10) . ? C41 C42 1.364(10) . ? C41 C46 1.372(10) . ? C42 C43 1.371(11) . ? C43 C44 1.386(12) . ? C44 C45 1.339(11) . ? C45 C46 1.377(11) . ? C47 C48 1.378(9) . ? C47 C52 1.397(9) . ? C47 B 1.647(10) . ? C48 C49 1.397(9) . ? C49 C50 1.369(10) . ? C50 C51 1.369(10) . ? C51 C52 1.384(9) . ? C53 C58 1.378(9) . ? C53 C54 1.383(9) . ? C53 B 1.641(11) . ? C54 C55 1.400(11) . ? C55 C56 1.352(12) . ? C56 C57 1.354(12) . ? C57 C58 1.399(11) . ? C59 C60 1.388(9) . ? C59 C64 1.400(9) . ? C59 B 1.643(10) . ? C60 C61 1.381(10) . ? C61 C62 1.371(10) . ? C62 C63 1.366(10) . ? C63 C64 1.374(10) . ? C65 C66 1.398(9) . ? C65 C70 1.410(9) . ? C65 B 1.641(10) . ? C66 C67 1.384(10) . ? C67 C68 1.375(12) . ? C68 C69 1.357(12) . ? C69 C70 1.396(10) . ? C101 C102 1.283(19) . ? C102 C102 1.20(3) 3_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Re Cl 175.52(17) . . ? N1 Re P3 93.95(17) . . ? Cl Re P3 84.05(7) . . ? N1 Re P1 97.25(17) . . ? Cl Re P1 84.71(7) . . ? P3 Re P1 168.76(6) . . ? N1 Re P2 91.68(17) . . ? Cl Re P2 92.48(7) . . ? P3 Re P2 94.90(7) . . ? P1 Re P2 85.73(7) . . ? N1 Re P4 86.57(17) . . ? Cl Re P4 89.32(7) . . ? P3 Re P4 86.94(7) . . ? P1 Re P4 92.78(7) . . ? P2 Re P4 177.55(6) . . ? O2 P1 O1 104.9(3) . . ? O2 P1 C11 98.0(3) . . ? O1 P1 C11 104.8(3) . . ? O2 P1 Re 117.4(2) . . ? O1 P1 Re 111.50(19) . . ? C11 P1 Re 118.4(2) . . ? O4 P2 O3 106.4(3) . . ? O4 P2 C21 97.3(3) . . ? O3 P2 C21 103.5(3) . . ? O4 P2 Re 121.1(2) . . ? O3 P2 Re 109.01(19) . . ? C21 P2 Re 117.6(2) . . ? O5 P3 O6 109.6(3) . . ? O5 P3 C31 101.8(3) . . ? O6 P3 C31 105.1(3) . . ? O5 P3 Re 109.26(19) . . ? O6 P3 Re 108.32(19) . . ? C31 P3 Re 122.2(2) . . ? O8 P4 O7 107.2(3) . . ? O8 P4 C41 97.3(3) . . ? O7 P4 C41 103.0(3) . . ? O8 P4 Re 122.0(2) . . ? O7 P4 Re 105.8(2) . . ? C41 P4 Re 119.7(2) . . ? C7 O1 P1 122.3(5) . . ? C9 O2 P1 126.6(5) . . ? C17 O3 P2 122.0(5) . . ? C19 O4 P2 122.2(5) . . ? C27 O5 P3 127.0(5) . . ? C29 O6 P3 124.9(5) . . ? C37 O7 P4 122.3(5) . . ? C39 O8 P4 126.7(5) . . ? N2 N1 Re 170.9(5) . . ? N1 N2 C1 125.8(6) . . ? C2 C1 C6 122.2(7) . . ? C2 C1 N2 114.9(7) . . ? C6 C1 N2 123.0(7) . . ? C1 C2 C3 118.7(8) . . ? C2 C3 C4 119.9(8) . . ? C5 C4 C3 119.5(8) . . ? C4 C5 C6 122.0(9) . . ? C1 C6 C5 117.7(8) . . ? O1 C7 C8 111.2(6) . . ? O2 C9 C10 107.7(6) . . ? C16 C11 C12 119.0(7) . . ? C16 C11 P1 122.1(6) . . ? C12 C11 P1 118.9(5) . . ? C11 C12 C13 119.8(7) . . ? C14 C13 C12 121.1(8) . . ? C15 C14 C13 118.9(8) . . ? C14 C15 C16 120.9(8) . . ? C11 C16 C15 120.3(8) . . ? C18 C17 O3 112.0(7) . . ? C20 C19 O4 112.3(7) . . ? C26 C21 C22 117.1(7) . . ? C26 C21 P2 123.9(6) . . ? C22 C21 P2 118.9(6) . . ? C23 C22 C21 120.4(8) . . ? C22 C23 C24 120.4(8) . . ? C25 C24 C23 120.6(8) . . ? C24 C25 C26 118.8(8) . . ? C25 C26 C21 122.7(8) . . ? O5 C27 C28 109.9(7) . . ? O6 C29 C30 107.2(7) . . ? C36 C31 C32 118.5(7) . . ? C36 C31 P3 121.5(6) . . ? C32 C31 P3 120.0(5) . . ? C33 C32 C31 119.8(7) . . ? C32 C33 C34 120.8(8) . . ? C33 C34 C35 120.1(8) . . ? C36 C35 C34 119.5(8) . . ? C35 C36 C31 121.4(7) . . ? C38 C37 O7 114.5(9) . . ? O8 C39 C40 110.6(7) . . ? C42 C41 C46 118.3(8) . . ? C42 C41 P4 122.1(7) . . ? C46 C41 P4 119.7(6) . . ? C41 C42 C43 121.6(9) . . ? C42 C43 C44 118.4(9) . . ? C45 C44 C43 121.1(10) . . ? C44 C45 C46 119.5(9) . . ? C41 C46 C45 121.1(8) . . ? C48 C47 C52 114.7(6) . . ? C48 C47 B 123.5(7) . . ? C52 C47 B 121.8(7) . . ? C47 C48 C49 123.0(7) . . ? C50 C49 C48 119.9(8) . . ? C49 C50 C51 119.4(7) . . ? C50 C51 C52 119.7(8) . . ? C51 C52 C47 123.4(7) . . ? C58 C53 C54 112.3(8) . . ? C58 C53 B 124.5(7) . . ? C54 C53 B 123.1(7) . . ? C53 C54 C55 124.6(9) . . ? C56 C55 C54 120.0(10) . . ? C55 C56 C57 118.6(10) . . ? C56 C57 C58 120.1(9) . . ? C53 C58 C57 124.6(8) . . ? C60 C59 C64 113.5(7) . . ? C60 C59 B 123.4(7) . . ? C64 C59 B 123.0(7) . . ? C61 C60 C59 124.2(8) . . ? C62 C61 C60 119.7(8) . . ? C63 C62 C61 118.6(8) . . ? C62 C63 C64 120.8(8) . . ? C63 C64 C59 123.2(8) . . ? C66 C65 C70 113.1(7) . . ? C66 C65 B 122.9(7) . . ? C70 C65 B 124.0(7) . . ? C67 C66 C65 123.8(8) . . ? C68 C67 C66 120.2(9) . . ? C69 C68 C67 119.3(9) . . ? C68 C69 C70 119.9(9) . . ? C69 C70 C65 123.7(8) . . ? C53 B C65 110.7(6) . . ? C53 B C59 108.7(6) . . ? C65 B C59 109.3(6) . . ? C53 B C47 110.0(6) . . ? C65 B C47 108.5(6) . . ? C59 B C47 109.5(6) . . ? C102 C102 C101 156(2) 3_557 . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 3.135 _refine_diff_density_min -1.393 _refine_diff_density_rms 0.140