# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1224 data_fac-ReL1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H25 Cl3 N2 P Re' _chemical_formula_weight 737.04 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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 11.505(6) _cell_length_b 13.545(5) _cell_length_c 18.720(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.66(4) _cell_angle_gamma 90.00 _cell_volume 2891.2(25) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description Parallelopiped _exptl_crystal_colour Dark _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method ? _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 4.558 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.1998 _exptl_absorpt_correction_T_max 0.3566 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 4105 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 22.55 _reflns_number_total 3801 _reflns_number_observed 3065 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SHELXTL-PLUS P3' _computing_cell_refinement 'Siemens SHELXTL-PLUS P3' _computing_data_reduction 'Siemens SHELXTL-PLUS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson Heavy Atom' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'Ridding Model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3797 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_obs 0.0316 _refine_ls_wR_factor_all 0.0851 _refine_ls_wR_factor_obs 0.0680 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.072 _refine_ls_restrained_S_all 1.191 _refine_ls_restrained_S_obs 1.072 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.14243(2) 0.71607(2) 0.791099(14) 0.02790(11) Uani 1 d . . Cl1 Cl 0.2212(2) 0.61091(14) 0.70565(10) 0.0474(5) Uani 1 d . . Cl2 Cl -0.04667(15) 0.65655(15) 0.75036(10) 0.0456(5) Uani 1 d . . Cl3 Cl 0.1787(2) 0.59209(14) 0.88131(10) 0.0426(5) Uani 1 d . . P1 P 0.0507(2) 0.81950(13) 0.87623(10) 0.0316(4) Uani 1 d . . N1 N 0.3137(4) 0.7715(4) 0.8163(3) 0.0322(14) Uani 1 d . . N2 N 0.1510(5) 0.8306(4) 0.7178(3) 0.0310(13) Uani 1 d . . C1 C 0.3979(6) 0.7358(5) 0.8679(4) 0.041(2) Uani 1 d . . H1 H 0.3795(6) 0.6846(5) 0.8976(4) 0.049 Uiso 1 calc R . C2 C 0.5096(7) 0.7742(6) 0.8769(5) 0.057(2) Uani 1 d . . H2 H 0.5656(7) 0.7486(6) 0.9125(5) 0.068 Uiso 1 calc R . C3 C 0.5395(7) 0.8502(6) 0.8340(5) 0.057(2) Uani 1 d . . H3 H 0.6147(7) 0.8768(6) 0.8410(5) 0.068 Uiso 1 calc R . C4 C 0.4580(6) 0.8853(6) 0.7816(5) 0.051(2) Uani 1 d . . H4 H 0.4769(6) 0.9362(6) 0.7518(5) 0.061 Uiso 1 calc R . C5 C 0.3447(6) 0.8449(5) 0.7720(4) 0.036(2) Uani 1 d . . C6 C 0.2522(6) 0.8755(5) 0.7198(4) 0.039(2) Uani 1 d . . H6 H 0.2626(6) 0.9262(5) 0.6877(4) 0.047 Uiso 1 calc R . C7 C 0.0621(6) 0.8618(5) 0.6617(4) 0.033(2) Uani 1 d . . C8 C 0.0364(6) 0.9610(6) 0.6523(4) 0.043(2) Uani 1 d . . H8 H 0.0748(6) 1.0075(6) 0.6835(4) 0.052 Uiso 1 calc R . C9 C -0.0464(7) 0.9908(7) 0.5962(4) 0.060(2) Uani 1 d . . H9 H -0.0644(7) 1.0575(7) 0.5906(4) 0.072 Uiso 1 calc R . C10 C -0.1021(7) 0.9243(8) 0.5490(4) 0.063(3) Uani 1 d . . H10 H -0.1578(7) 0.9450(8) 0.5114(4) 0.075 Uiso 1 calc R . C11 C -0.0744(8) 0.8251(7) 0.5580(4) 0.061(2) Uani 1 d . . H11 H -0.1115(8) 0.7792(7) 0.5257(4) 0.073 Uiso 1 calc R . C12 C 0.0063(7) 0.7936(6) 0.6134(4) 0.049(2) Uani 1 d . . H12 H 0.0239(7) 0.7267(6) 0.6187(4) 0.059 Uiso 1 calc R . C13 C 0.1607(6) 0.8689(5) 0.9465(4) 0.034(2) Uani 1 d . . C14 C 0.2488(6) 0.9298(5) 0.9271(4) 0.043(2) Uani 1 d . . H14 H 0.2477(6) 0.9471(5) 0.8790(4) 0.051 Uiso 1 calc R . C15 C 0.3373(7) 0.9652(6) 0.9771(5) 0.053(2) Uani 1 d . . H15 H 0.3951(7) 1.0060(6) 0.9629(5) 0.063 Uiso 1 calc R . C16 C 0.3397(7) 0.9394(7) 1.0490(5) 0.061(2) Uani 1 d . . H16 H 0.3994(7) 0.9622(7) 1.0834(5) 0.073 Uiso 1 calc R . C17 C 0.2523(8) 0.8793(7) 1.0688(4) 0.067(3) Uani 1 d . . H17 H 0.2534(8) 0.8618(7) 1.1169(4) 0.080 Uiso 1 calc R . C18 C 0.1633(6) 0.8450(6) 1.0181(4) 0.050(2) Uani 1 d . . H18 H 0.1046(6) 0.8054(6) 1.0324(4) 0.060 Uiso 1 calc R . C19 C -0.0284(6) 0.9254(5) 0.8321(4) 0.036(2) Uani 1 d . . C20 C 0.0081(7) 1.0214(6) 0.8412(4) 0.048(2) Uani 1 d . . H20 H 0.0750(7) 1.0360(6) 0.8731(4) 0.058 Uiso 1 calc R . C21 C -0.0539(8) 1.0974(7) 0.8030(5) 0.065(3) Uani 1 d . . H21 H -0.0268(8) 1.1620(7) 0.8085(5) 0.078 Uiso 1 calc R . C22 C -0.1542(8) 1.0776(8) 0.7576(5) 0.075(3) Uani 1 d . . H22 H -0.1954(8) 1.1284(8) 0.7321(5) 0.090 Uiso 1 calc R . C23 C -0.1946(8) 0.9796(8) 0.7498(5) 0.067(3) Uani 1 d . . H23 H -0.2638(8) 0.9655(8) 0.7200(5) 0.081 Uiso 1 calc R . C24 C -0.1320(6) 0.9053(7) 0.7862(4) 0.053(2) Uani 1 d . . H24 H -0.1585(6) 0.8405(7) 0.7804(4) 0.064 Uiso 1 calc R . C25 C -0.0605(6) 0.7662(5) 0.9276(4) 0.037(2) Uani 1 d . . C26 C -0.0768(7) 0.6661(6) 0.9316(5) 0.057(2) Uani 1 d . . H26 H -0.0365(7) 0.6234(6) 0.9048(5) 0.069 Uiso 1 calc R . C27 C -0.1547(8) 0.6285(7) 0.9764(5) 0.070(3) Uani 1 d . . H27 H -0.1651(8) 0.5606(7) 0.9797(5) 0.084 Uiso 1 calc R . C28 C -0.2151(7) 0.6907(8) 1.0150(5) 0.067(3) Uani 1 d . . H28 H -0.2668(7) 0.6654(8) 1.0445(5) 0.080 Uiso 1 calc R . C29 C -0.1997(7) 0.7909(7) 1.0104(5) 0.063(2) Uani 1 d . . H29 H -0.2411(7) 0.8334(7) 1.0368(5) 0.076 Uiso 1 calc R . C30 C -0.1241(6) 0.8282(6) 0.9674(4) 0.049(2) Uani 1 d . . H30 H -0.1146(6) 0.8962(6) 0.9645(4) 0.058 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0295(2) 0.0282(2) 0.0264(2) -0.00191(14) 0.00510(11) -0.00160(14) Cl1 0.0599(12) 0.0390(11) 0.0467(12) -0.0111(9) 0.0202(10) 0.0031(9) Cl2 0.0382(10) 0.0560(12) 0.0411(11) -0.0069(10) -0.0004(8) -0.0131(9) Cl3 0.0501(11) 0.0398(11) 0.0374(11) 0.0080(9) 0.0037(9) 0.0038(9) P1 0.0320(10) 0.0338(10) 0.0298(10) -0.0007(8) 0.0068(8) 0.0002(8) N1 0.031(3) 0.030(3) 0.035(3) -0.010(3) 0.003(3) 0.005(3) N2 0.035(3) 0.029(3) 0.029(3) -0.004(3) 0.004(3) 0.000(3) C1 0.041(5) 0.040(5) 0.040(4) -0.003(4) -0.002(4) 0.008(4) C2 0.038(5) 0.052(5) 0.075(6) -0.005(5) -0.014(4) -0.006(4) C3 0.037(5) 0.050(5) 0.081(7) -0.007(5) 0.001(5) -0.002(4) C4 0.042(5) 0.043(5) 0.068(6) 0.004(4) 0.008(4) -0.006(4) C5 0.035(4) 0.029(4) 0.045(5) -0.001(4) 0.007(4) -0.001(3) C6 0.048(5) 0.029(4) 0.040(5) -0.001(3) 0.011(4) 0.000(4) C7 0.031(4) 0.041(5) 0.028(4) -0.001(4) 0.006(3) -0.001(3) C8 0.048(5) 0.049(5) 0.032(4) -0.006(4) 0.005(4) 0.003(4) C9 0.068(6) 0.061(6) 0.048(6) 0.014(5) -0.004(5) 0.005(5) C10 0.051(5) 0.095(8) 0.039(5) 0.017(5) -0.005(4) 0.009(5) C11 0.071(6) 0.071(6) 0.037(5) 0.009(5) -0.010(4) -0.016(5) C12 0.065(5) 0.047(5) 0.035(4) 0.001(4) 0.004(4) -0.005(4) C13 0.030(4) 0.042(4) 0.032(4) -0.002(4) 0.006(3) 0.004(3) C14 0.049(5) 0.041(5) 0.039(5) 0.000(4) 0.008(4) -0.001(4) C15 0.038(5) 0.048(5) 0.070(6) -0.016(5) 0.000(4) -0.001(4) C16 0.045(5) 0.071(6) 0.063(6) -0.026(5) -0.003(5) 0.006(5) C17 0.058(6) 0.109(8) 0.032(5) -0.010(5) 0.000(4) 0.009(6) C18 0.039(4) 0.069(6) 0.041(5) 0.000(5) 0.004(4) 0.003(4) C19 0.035(4) 0.042(5) 0.034(4) -0.002(4) 0.012(3) 0.006(4) C20 0.051(5) 0.045(5) 0.051(5) 0.005(4) 0.012(4) 0.010(4) C21 0.073(7) 0.049(6) 0.078(7) 0.015(5) 0.032(6) 0.014(5) C22 0.065(7) 0.098(9) 0.069(7) 0.044(6) 0.031(6) 0.046(6) C23 0.044(5) 0.090(8) 0.066(6) 0.015(6) 0.003(4) 0.026(5) C24 0.040(5) 0.065(6) 0.054(5) 0.007(5) 0.007(4) 0.003(4) C25 0.039(4) 0.040(5) 0.033(4) 0.002(4) 0.007(3) -0.002(4) C26 0.061(5) 0.051(6) 0.067(6) -0.002(5) 0.031(5) -0.008(5) C27 0.080(7) 0.051(6) 0.088(7) 0.014(5) 0.043(6) -0.013(5) C28 0.047(5) 0.095(8) 0.065(6) 0.014(6) 0.032(5) -0.008(5) C29 0.057(5) 0.080(7) 0.061(6) -0.001(5) 0.035(5) 0.003(5) C30 0.038(4) 0.054(5) 0.056(5) -0.005(4) 0.018(4) -0.002(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 N2 2.083(5) . y Re N1 2.103(5) . y Re Cl2 2.350(2) . y Re Cl3 2.379(2) . y Re Cl1 2.407(2) . y Re P1 2.463(2) . y P1 C13 1.827(7) . ? P1 C19 1.835(7) . ? P1 C25 1.846(7) . ? N1 C1 1.363(8) . ? N1 C5 1.371(8) . y N2 C6 1.309(8) . y N2 C7 1.430(8) . ? C1 C2 1.376(10) . ? C2 C3 1.377(11) . ? C3 C4 1.351(10) . ? C4 C5 1.402(9) . ? C5 C6 1.408(9) . y C7 C8 1.382(10) . ? C7 C12 1.389(10) . ? C8 C9 1.380(10) . ? C9 C10 1.361(12) . ? C10 C11 1.386(12) . ? C11 C12 1.365(11) . ? C13 C18 1.375(9) . ? C13 C14 1.392(9) . ? C14 C15 1.374(10) . ? C15 C16 1.387(11) . ? C16 C17 1.382(12) . ? C17 C18 1.381(11) . ? C19 C20 1.370(10) . ? C19 C24 1.400(10) . ? C20 C21 1.394(11) . ? C21 C22 1.365(12) . ? C22 C23 1.408(13) . ? C23 C24 1.366(11) . ? C25 C26 1.373(10) . ? C25 C30 1.393(10) . ? C26 C27 1.402(10) . ? C27 C28 1.359(12) . ? C28 C29 1.373(12) . ? C29 C30 1.359(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Re N1 75.9(2) . . y N2 Re Cl2 99.5(2) . . y N1 Re Cl2 174.1(2) . . y N2 Re Cl3 167.0(2) . . y N1 Re Cl3 91.3(2) . . y Cl2 Re Cl3 93.18(7) . . y N2 Re Cl1 87.0(2) . . y N1 Re Cl1 86.32(15) . . y Cl2 Re Cl1 89.74(7) . . y Cl3 Re Cl1 90.46(8) . . y N2 Re P1 93.7(2) . . y N1 Re P1 96.98(15) . . y Cl2 Re P1 86.97(7) . . y Cl3 Re P1 89.55(7) . . y Cl1 Re P1 176.70(6) . . y C13 P1 C19 107.0(3) . . ? C13 P1 C25 103.3(3) . . ? C19 P1 C25 101.7(3) . . ? C13 P1 Re 111.0(2) . . ? C19 P1 Re 112.5(2) . . ? C25 P1 Re 120.1(2) . . ? C1 N1 C5 117.9(6) . . ? C1 N1 Re 126.0(5) . . ? C5 N1 Re 115.8(4) . . y C6 N2 C7 115.5(6) . . ? C6 N2 Re 116.6(5) . . y C7 N2 Re 127.7(4) . . ? N1 C1 C2 121.1(7) . . ? C1 C2 C3 120.9(8) . . ? C4 C3 C2 118.9(8) . . ? C3 C4 C5 119.9(8) . . ? N1 C5 C4 121.2(7) . . ? N1 C5 C6 113.5(6) . . y C4 C5 C6 125.2(7) . . ? N2 C6 C5 118.0(6) . . y C8 C7 C12 119.5(7) . . ? C8 C7 N2 120.0(6) . . ? C12 C7 N2 120.3(6) . . ? C9 C8 C7 119.7(8) . . ? C10 C9 C8 121.2(8) . . ? C9 C10 C11 118.8(8) . . ? C12 C11 C10 121.2(9) . . ? C11 C12 C7 119.6(8) . . ? C18 C13 C14 118.1(7) . . ? C18 C13 P1 122.6(6) . . ? C14 C13 P1 119.2(5) . . ? C15 C14 C13 121.9(7) . . ? C14 C15 C16 119.3(8) . . ? C17 C16 C15 119.2(8) . . ? C18 C17 C16 120.8(8) . . ? C13 C18 C17 120.6(8) . . ? C20 C19 C24 118.9(7) . . ? C20 C19 P1 124.1(6) . . ? C24 C19 P1 117.0(6) . . ? C19 C20 C21 120.7(8) . . ? C22 C21 C20 120.4(9) . . ? C21 C22 C23 119.3(8) . . ? C24 C23 C22 119.9(9) . . ? C23 C24 C19 120.8(9) . . ? C26 C25 C30 118.7(7) . . ? C26 C25 P1 121.6(6) . . ? C30 C25 P1 119.5(6) . . ? C25 C26 C27 119.7(8) . . ? C28 C27 C26 120.3(8) . . ? C27 C28 C29 120.0(8) . . ? C30 C29 C28 120.1(8) . . ? C29 C30 C25 121.1(8) . . ? _refine_diff_density_max 0.672 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.110 #===END data_fac-ReL4' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H25 Cl4 N2 O2 P Re' _chemical_formula_weight 804.49 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.994(6) _cell_length_b 11.617(6) _cell_length_c 15.135(9) _cell_angle_alpha 76.26(4) _cell_angle_beta 88.11(5) _cell_angle_gamma 67.40(4) _cell_volume 1572.5(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 14 _exptl_crystal_description Parallelopiped _exptl_crystal_colour Orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method ? _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 4.285 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.227 _exptl_absorpt_correction_T_max 0.427 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 4733 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.55 _reflns_number_total 4663 _reflns_number_observed 4054 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SHELXTL PLUS' _computing_cell_refinement 'Siemens SHELXTL PLUS' _computing_data_reduction 'Siemens SHELXTL PLUS' _computing_structure_solution 'SHELXTL V 5.03 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL V 5.03 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V 5.03' _computing_publication_material 'Siemens SHELXTL V 5.03' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+3.1243P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Patterson Heavey atom Method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4652 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_obs 0.0506 _refine_ls_wR_factor_all 0.1554 _refine_ls_wR_factor_obs 0.1319 _refine_ls_goodness_of_fit_all 1.153 _refine_ls_goodness_of_fit_obs 1.177 _refine_ls_restrained_S_all 1.288 _refine_ls_restrained_S_obs 1.177 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.15241(4) 0.23317(3) 0.34727(3) 0.0351(2) Uani 1 d . . N1 N 0.3461(8) 0.2674(7) 0.3249(6) 0.040(2) Uani 1 d . . N2 N 0.0904(8) 0.3853(7) 0.2337(5) 0.038(2) Uani 1 d . . P P 0.2372(3) 0.0644(2) 0.2543(2) 0.0374(6) Uani 1 d . . O1 O 0.1716(8) 0.5238(7) 0.1344(5) 0.051(2) Uani 1 d . . Cl1 Cl 0.0965(3) 0.3758(3) 0.4412(2) 0.0541(7) Uani 1 d . . Cl2 Cl -0.0691(3) 0.2150(3) 0.3561(2) 0.0533(7) Uani 1 d . . Cl3 Cl 0.2637(3) 0.0594(2) 0.4724(2) 0.0468(6) Uani 1 d . . Cl4 Cl -0.5040(3) 0.6975(4) 0.0611(3) 0.0894(12) Uani 1 d . . C1 C 0.4736(12) 0.1989(12) 0.3741(9) 0.064(3) Uani 1 d . . H1A H 0.4832(12) 0.1303(12) 0.4233(9) 0.077 Uiso 1 calc R . C2 C 0.5859(14) 0.2325(15) 0.3501(12) 0.105(6) Uani 1 d . . H2A H 0.6732(14) 0.1866(15) 0.3851(12) 0.127 Uiso 1 calc R . C3 C 0.5801(13) 0.3325(13) 0.2756(11) 0.083(5) Uani 1 d . . H3A H 0.6592(13) 0.3554(13) 0.2619(11) 0.099 Uiso 1 calc R . C4 C 0.4525(12) 0.3942(12) 0.2244(9) 0.067(4) Uani 1 d . . H4A H 0.4431(12) 0.4585(12) 0.1721(9) 0.081 Uiso 1 calc R . C5 C 0.3380(10) 0.3603(9) 0.2511(7) 0.041(2) Uani 1 d . . C6 C 0.1899(10) 0.4329(9) 0.1991(7) 0.039(2) Uani 1 d . . C7 C -0.0545(10) 0.4590(9) 0.1932(6) 0.039(2) Uani 1 d . . C8 C -0.0889(11) 0.4606(10) 0.1055(7) 0.050(3) Uani 1 d . . H8A H -0.0181(11) 0.4123(10) 0.0728(7) 0.060 Uiso 1 calc R . C9 C -0.2279(12) 0.5335(12) 0.0652(8) 0.060(3) Uani 1 d . . H9A H -0.2507(12) 0.5334(12) 0.0061(8) 0.072 Uiso 1 calc R . C10 C -0.3302(10) 0.6049(11) 0.1129(8) 0.053(3) Uani 1 d . . C11 C -0.2995(12) 0.6051(11) 0.2010(8) 0.057(3) Uani 1 d . . H11A H -0.3701(12) 0.6545(11) 0.2333(8) 0.068 Uiso 1 calc R . C12 C -0.1621(12) 0.5306(11) 0.2396(8) 0.055(3) Uani 1 d . . H12A H -0.1410(12) 0.5286(11) 0.2995(8) 0.066 Uiso 1 calc R . C13 C 0.4343(12) 0.0081(10) 0.2513(8) 0.052(3) Uani 1 d . . C14 C 0.4993(14) 0.0850(14) 0.1918(9) 0.071(3) Uani 1 d . . H14A H 0.4404(14) 0.1607(14) 0.1513(9) 0.085 Uiso 1 calc R . C15 C 0.6437(16) 0.0493(19) 0.1935(13) 0.101(5) Uani 1 d . . H15A H 0.6849(16) 0.0979(19) 0.1527(13) 0.121 Uiso 1 calc R . C16 C 0.7319(17) -0.0609(23) 0.2567(15) 0.115(7) Uani 1 d . . H16A H 0.8320(17) -0.0847(23) 0.2582(15) 0.137 Uiso 1 calc R . C17 C 0.6726(15) -0.1371(15) 0.3184(11) 0.079(4) Uani 1 d . . H17A H 0.7315(15) -0.2115(15) 0.3600(11) 0.095 Uiso 1 calc R . C18 C 0.5199(12) -0.0957(11) 0.3144(9) 0.060(3) Uani 1 d . . H18A H 0.4773(12) -0.1414(11) 0.3565(9) 0.073 Uiso 1 calc R . C19 C 0.1569(13) 0.1153(10) 0.1386(7) 0.054(3) Uani 1 d . . C20 C 0.2372(23) 0.1125(19) 0.0614(10) 0.108(6) Uani 1 d . . H20A H 0.3372(23) 0.0890(19) 0.0667(10) 0.130 Uiso 1 calc R . C21 C 0.1649(32) 0.1457(21) -0.0240(11) 0.127(8) Uani 1 d . . H21A H 0.2180(32) 0.1442(21) -0.0757(11) 0.152 Uiso 1 calc R . C22 C 0.0212(30) 0.1797(17) -0.0334(13) 0.116(8) Uani 1 d . . H22A H -0.0255(30) 0.2026(17) -0.0908(13) 0.140 Uiso 1 calc R . C23 C -0.0547(24) 0.1802(21) 0.0418(16) 0.134(8) Uani 1 d . . H23A H -0.1538(24) 0.1991(21) 0.0360(16) 0.160 Uiso 1 calc R . C24 C 0.0110(16) 0.1534(15) 0.1273(10) 0.089(5) Uani 1 d . . H24A H -0.0453(16) 0.1616(15) 0.1773(10) 0.106 Uiso 1 calc R . C25 C 0.2030(10) -0.0837(8) 0.2953(6) 0.037(2) Uani 1 d . . C26 C 0.1296(12) -0.1063(10) 0.3713(7) 0.050(3) Uani 1 d . . H26A H 0.1001(12) -0.0488(10) 0.4085(7) 0.060 Uiso 1 calc R . C27 C 0.1003(15) -0.2166(12) 0.3916(9) 0.071(4) Uani 1 d . . H27A H 0.0497(15) -0.2330(12) 0.4425(9) 0.085 Uiso 1 calc R . C28 C 0.1443(16) -0.3007(12) 0.3381(9) 0.073(4) Uani 1 d . . H28A H 0.1246(16) -0.3747(12) 0.3530(9) 0.087 Uiso 1 calc R . C29 C 0.2177(15) -0.2781(11) 0.2623(9) 0.068(3) Uani 1 d . . H29A H 0.2462(15) -0.3353(11) 0.2249(9) 0.082 Uiso 1 calc R . C30 C 0.2480(13) -0.1715(10) 0.2426(8) 0.053(3) Uani 1 d . . H30A H 0.3006(13) -0.1571(10) 0.1923(8) 0.064 Uiso 1 calc R . O2 O 0.5834(14) -0.4369(13) 0.4517(10) 0.128(4) Uiso 1 d . . H2C H 0.5906(14) -0.4551(13) 0.5171(10) 0.153 Uiso 1 d R . H2B H 0.6293(14) -0.5084(13) 0.4248(10) 0.153 Uiso 1 d 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 Re 0.0338(2) 0.0346(2) 0.0355(2) -0.0020(2) 0.00174(15) -0.0156(2) N1 0.033(4) 0.038(4) 0.052(5) -0.004(4) 0.010(4) -0.023(4) N2 0.037(4) 0.028(4) 0.039(4) -0.001(3) 0.004(3) -0.007(3) P 0.0422(13) 0.0323(13) 0.0362(13) -0.0028(10) 0.0035(10) -0.0161(11) O1 0.060(4) 0.041(4) 0.048(4) 0.006(3) 0.003(3) -0.023(3) Cl1 0.075(2) 0.0453(14) 0.049(2) -0.0193(12) 0.0109(13) -0.0265(13) Cl2 0.0361(12) 0.065(2) 0.060(2) -0.0053(13) 0.0047(11) -0.0270(12) Cl3 0.0550(14) 0.0420(13) 0.0399(13) 0.0006(11) -0.0062(11) -0.0206(11) Cl4 0.046(2) 0.104(3) 0.073(2) 0.006(2) -0.0110(15) 0.004(2) C1 0.048(6) 0.068(8) 0.068(8) 0.015(6) -0.015(6) -0.031(6) C2 0.048(7) 0.104(12) 0.141(15) 0.046(10) -0.033(8) -0.046(8) C3 0.044(7) 0.067(8) 0.123(12) 0.023(8) -0.004(7) -0.032(6) C4 0.047(6) 0.056(7) 0.087(9) 0.016(6) 0.004(6) -0.026(6) C5 0.040(5) 0.044(6) 0.040(5) -0.008(5) 0.008(4) -0.019(4) C6 0.042(5) 0.032(5) 0.042(6) -0.013(5) 0.008(4) -0.012(4) C7 0.037(5) 0.035(5) 0.040(5) -0.001(4) 0.001(4) -0.014(4) C8 0.052(6) 0.045(6) 0.046(6) -0.015(5) 0.008(5) -0.011(5) C9 0.056(7) 0.076(8) 0.038(6) -0.004(6) -0.006(5) -0.020(6) C10 0.032(5) 0.057(7) 0.055(7) -0.003(5) 0.006(5) -0.009(5) C11 0.048(6) 0.055(7) 0.053(7) -0.014(5) 0.006(5) -0.005(5) C12 0.055(7) 0.064(7) 0.043(6) -0.019(5) 0.001(5) -0.017(6) C13 0.053(6) 0.045(6) 0.055(7) -0.015(5) 0.007(5) -0.013(5) C14 0.062(8) 0.085(9) 0.066(8) -0.014(7) 0.021(6) -0.034(7) C15 0.057(9) 0.128(15) 0.114(14) -0.025(12) 0.025(9) -0.036(10) C16 0.048(8) 0.166(19) 0.140(17) -0.087(16) 0.012(10) -0.024(11) C17 0.059(8) 0.089(10) 0.086(10) -0.033(8) -0.012(7) -0.017(7) C18 0.057(7) 0.056(7) 0.065(8) -0.028(6) -0.003(6) -0.010(6) C19 0.075(8) 0.040(6) 0.044(6) -0.004(5) -0.009(6) -0.023(5) C20 0.153(16) 0.149(16) 0.050(9) -0.022(10) 0.013(10) -0.090(14) C21 0.227(26) 0.142(18) 0.041(9) -0.017(10) 0.007(12) -0.108(19) C22 0.187(23) 0.078(11) 0.071(12) 0.001(9) -0.065(14) -0.044(13) C23 0.121(16) 0.149(19) 0.116(17) -0.043(15) -0.065(14) -0.025(14) C24 0.080(10) 0.111(12) 0.064(9) -0.017(8) -0.024(7) -0.025(9) C25 0.041(5) 0.029(5) 0.041(5) -0.003(4) -0.001(4) -0.015(4) C26 0.064(7) 0.046(6) 0.048(6) -0.010(5) 0.013(5) -0.030(5) C27 0.092(9) 0.068(8) 0.071(9) -0.010(7) 0.018(7) -0.056(8) C28 0.107(11) 0.044(7) 0.070(9) 0.001(6) 0.000(8) -0.040(7) C29 0.102(10) 0.034(6) 0.070(8) -0.011(6) -0.001(7) -0.030(6) C30 0.078(8) 0.041(6) 0.053(7) -0.023(5) 0.009(6) -0.028(6) _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 N2 2.061(7) . y Re N1 2.123(7) . y Re Cl2 2.300(3) . y Re Cl1 2.331(3) . y Re Cl3 2.345(3) . y Re P 2.549(3) . y N1 C5 1.336(12) . y N1 C1 1.346(13) . ? N2 C6 1.349(12) . y N2 C7 1.436(12) . ? P C19 1.816(11) . ? P C13 1.825(11) . ? P C25 1.841(9) . ? O1 C6 1.217(11) . y Cl4 C10 1.744(10) . ? C1 C2 1.34(2) . ? C2 C3 1.40(2) . ? C3 C4 1.36(2) . ? C4 C5 1.367(14) . ? C5 C6 1.524(13) . ? C7 C12 1.372(14) . ? C7 C8 1.377(14) . ? C8 C9 1.387(15) . ? C9 C10 1.36(2) . ? C10 C11 1.38(2) . ? C11 C12 1.369(15) . ? C13 C18 1.35(2) . ? C13 C14 1.43(2) . ? C14 C15 1.34(2) . ? C15 C16 1.39(3) . ? C16 C17 1.41(3) . ? C17 C18 1.41(2) . ? C19 C24 1.35(2) . ? C19 C20 1.40(2) . ? C20 C21 1.40(2) . ? C21 C22 1.34(3) . ? C22 C23 1.35(3) . ? C23 C24 1.38(2) . ? C25 C26 1.371(14) . ? C25 C30 1.375(13) . ? C26 C27 1.39(2) . ? C27 C28 1.35(2) . ? C28 C29 1.37(2) . ? C29 C30 1.35(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 N2 Re N1 78.2(3) . . y N2 Re Cl2 95.1(2) . . y N1 Re Cl2 173.2(2) . . y N2 Re Cl1 90.2(2) . . y N1 Re Cl1 86.0(2) . . y Cl2 Re Cl1 94.42(11) . . y N2 Re Cl3 170.1(2) . . y N1 Re Cl3 92.0(2) . . y Cl2 Re Cl3 94.77(11) . . y Cl1 Re Cl3 90.53(11) . . y N2 Re P 93.7(2) . . y N1 Re P 90.7(2) . . y Cl2 Re P 89.37(10) . . y Cl1 Re P 174.29(9) . . y Cl3 Re P 84.89(10) . . y C5 N1 C1 119.6(8) . . ? C5 N1 Re 114.5(6) . . y C1 N1 Re 125.7(7) . . ? C6 N2 C7 114.6(7) . . ? C6 N2 Re 118.2(6) . . y C7 N2 Re 126.6(6) . . ? C19 P C13 109.2(5) . . ? C19 P C25 99.8(5) . . ? C13 P C25 104.3(5) . . ? C19 P Re 116.0(4) . . ? C13 P Re 108.3(4) . . ? C25 P Re 118.3(3) . . ? C2 C1 N1 118.1(11) . . ? C1 C2 C3 123.9(12) . . ? C4 C3 C2 116.3(11) . . ? C3 C4 C5 118.9(11) . . ? N1 C5 C4 123.1(9) . . ? N1 C5 C6 116.3(8) . . y C4 C5 C6 120.6(9) . . ? O1 C6 N2 127.1(9) . . y O1 C6 C5 120.2(9) . . y N2 C6 C5 112.7(8) . . y C12 C7 C8 117.9(9) . . ? C12 C7 N2 121.6(9) . . ? C8 C7 N2 120.5(9) . . ? C7 C8 C9 120.9(10) . . ? C10 C9 C8 119.2(10) . . ? C9 C10 C11 121.4(10) . . ? C9 C10 Cl4 118.8(9) . . ? C11 C10 Cl4 119.8(8) . . ? C12 C11 C10 118.1(10) . . ? C11 C12 C7 122.4(10) . . ? C18 C13 C14 118.9(11) . . ? C18 C13 P 120.0(9) . . ? C14 C13 P 120.3(9) . . ? C15 C14 C13 120.9(14) . . ? C14 C15 C16 119.6(16) . . ? C15 C16 C17 121.4(14) . . ? C16 C17 C18 117.1(14) . . ? C13 C18 C17 121.8(14) . . ? C24 C19 C20 118.5(13) . . ? C24 C19 P 117.7(10) . . ? C20 C19 P 123.8(11) . . ? C19 C20 C21 118.9(19) . . ? C22 C21 C20 121.7(20) . . ? C21 C22 C23 118.8(17) . . ? C22 C23 C24 121.6(20) . . ? C19 C24 C23 120.4(17) . . ? C26 C25 C30 119.6(9) . . ? C26 C25 P 123.7(8) . . ? C30 C25 P 116.6(8) . . ? C25 C26 C27 118.5(11) . . ? C28 C27 C26 120.7(12) . . ? C27 C28 C29 120.7(12) . . ? C30 C29 C28 118.9(12) . . ? C29 C30 C25 121.5(11) . . ? _refine_diff_density_max 3.087 _refine_diff_density_min -1.727 _refine_diff_density_rms 0.189