# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1658 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[ReO(OMe){B(pz)4)}(3-SiMe3-2-Spy)]' _chemical_formula_analytical ? _chemical_formula_sum 'C21 H27 B N9 O2 Re S Si' _chemical_formula_weight 694.68 _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 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.545(3) _cell_length_b 8.2966(9) _cell_length_c 19.997(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.910(10) _cell_angle_gamma 90.00 _cell_volume 2719.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 13.0 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow-brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method ? _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 4.626 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.4863 _exptl_absorpt_correction_T_max 0.9950 _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscan' _diffrn_standards_number 3 _diffrn_standards_interval_count 'every 100 reflections' _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0.4 _diffrn_reflns_number 4418 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 23.99 _reflns_number_total 4263 _reflns_number_observed 2687 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software (Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software (Enraf-Nonius,1989)' _computing_data_reduction 'process-MOLEN (Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP(Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 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^)+(0.0329P)^2^+75.0005P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4246 _refine_ls_number_parameters 325 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_obs 0.0750 _refine_ls_wR_factor_all 0.1892 _refine_ls_wR_factor_obs 0.1358 _refine_ls_goodness_of_fit_all 1.113 _refine_ls_goodness_of_fit_obs 1.088 _refine_ls_restrained_S_all 1.190 _refine_ls_restrained_S_obs 1.091 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.24870(5) 0.06812(9) 0.22948(4) 0.0394(3) Uani 1 d . . S1 S 0.1661(3) 0.0553(7) 0.1032(3) 0.0545(14) Uani 1 d . . O1 O 0.3305(8) 0.0016(16) 0.2161(6) 0.053(4) Uani 1 d . . O2 O 0.1608(8) 0.1495(15) 0.2416(6) 0.049(3) Uani 1 d U . N1 N 0.2175(10) -0.1519(19) 0.2663(8) 0.050(4) Uani 1 d . . N2 N 0.3100(8) 0.1320(17) 0.3394(8) 0.038(4) Uani 1 d . . N3 N 0.3072(11) -0.2704(23) 0.4885(9) 0.064(5) Uani 1 d . . N4 N 0.4076(10) -0.3296(19) 0.3177(8) 0.050(4) Uani 1 d . . N5 N 0.2473(10) 0.2895(18) 0.1742(7) 0.042(4) Uani 1 d . . N11 N 0.2550(9) -0.2249(16) 0.3305(7) 0.034(3) Uani 1 d . . N21 N 0.3315(9) 0.0210(18) 0.3953(8) 0.043(4) Uani 1 d . . N31 N 0.3582(9) -0.2497(17) 0.4531(7) 0.036(4) Uani 1 d . . N41 N 0.4053(9) -0.1864(17) 0.3508(7) 0.040(4) Uani 1 d . . C1 C 0.2010(13) 0.2556(21) 0.1072(11) 0.047(5) Uani 1 d . . C2 C 0.1782(11) 0.3713(23) 0.0520(10) 0.039(5) Uani 1 d . . C3 C 0.2156(12) 0.5171(24) 0.0710(11) 0.053(6) Uani 1 d . . H3 H 0.2057(12) 0.5971(24) 0.0364(11) 0.064 Uiso 1 calc R . C4 C 0.2680(11) 0.5500(26) 0.1403(9) 0.049(5) Uani 1 d . . H4 H 0.2912(11) 0.6518(26) 0.1519(9) 0.059 Uiso 1 calc R . C5 C 0.2848(13) 0.4357(24) 0.1898(9) 0.053(5) Uani 1 d . . H5 H 0.3223(13) 0.4554(24) 0.2354(9) 0.063 Uiso 1 calc R . C6 C 0.0759(14) 0.1999(31) 0.2116(13) 0.080(7) Uani 1 d U . H6A H 0.0589(14) 0.2397(31) 0.2492(13) 0.120 Uiso 1 calc R . H6B H 0.0425(14) 0.1096(31) 0.1888(13) 0.120 Uiso 1 calc R . H6C H 0.0702(14) 0.2837(31) 0.1770(13) 0.120 Uiso 1 calc R . C7 C 0.1333(16) 0.1410(30) -0.0782(13) 0.089(8) Uani 1 d . . H7A H 0.1855(16) 0.1593(30) -0.0822(13) 0.134 Uiso 1 calc R . H7B H 0.0936(16) 0.1191(30) -0.1247(13) 0.134 Uiso 1 calc R . H7C H 0.1368(16) 0.0505(30) -0.0473(13) 0.134 Uiso 1 calc R . C8 C 0.0018(12) 0.2836(31) -0.0320(11) 0.076(8) Uani 1 d . . H8A H -0.0149(12) 0.3769(31) -0.0124(11) 0.115 Uiso 1 calc R . H8B H 0.0062(12) 0.1930(31) -0.0010(11) 0.115 Uiso 1 calc R . H8C H -0.0379(12) 0.2608(31) -0.0785(11) 0.115 Uiso 1 calc R . C9 C 0.0980(15) 0.4979(29) -0.1002(10) 0.078(8) Uani 1 d . . H9A H 0.1509(15) 0.5150(29) -0.1030(10) 0.116 Uiso 1 calc R . H9B H 0.0817(15) 0.5927(29) -0.0813(10) 0.116 Uiso 1 calc R . H9C H 0.0593(15) 0.4761(29) -0.1472(10) 0.116 Uiso 1 calc R . C11 C 0.2100(13) -0.3531(24) 0.3354(11) 0.054(6) Uani 1 d . . H11 H 0.2204(13) -0.4207(24) 0.3747(11) 0.065 Uiso 1 calc R . C12 C 0.1461(13) -0.3653(23) 0.2714(12) 0.060(6) Uani 1 d . . H12 H 0.1062(13) -0.4451(23) 0.2585(12) 0.072 Uiso 1 calc R . C13 C 0.1518(13) -0.2406(23) 0.2308(10) 0.057(6) Uani 1 d . . H13 H 0.1156(13) -0.2190(23) 0.1848(10) 0.068 Uiso 1 calc R . C21 C 0.3576(13) 0.1019(26) 0.4570(11) 0.057(6) Uani 1 d . . H21 H 0.3781(13) 0.0564(26) 0.5024(11) 0.068 Uiso 1 calc R . C22 C 0.3489(13) 0.2624(23) 0.4420(10) 0.053(6) Uani 1 d . . H22 H 0.3606(13) 0.3465(23) 0.4749(10) 0.064 Uiso 1 calc R . C23 C 0.3195(13) 0.2752(21) 0.3687(11) 0.054(6) Uani 1 d . . H23 H 0.3081(13) 0.3719(21) 0.3435(11) 0.065 Uiso 1 calc R . C31 C 0.4314(12) -0.3077(24) 0.4917(10) 0.049(5) Uani 1 d . . H31 H 0.4770(12) -0.3081(24) 0.4782(10) 0.059 Uiso 1 calc R . C32 C 0.4283(15) -0.3668(26) 0.5545(12) 0.070(7) Uani 1 d . . H32 H 0.4701(15) -0.4143(26) 0.5921(12) 0.083 Uiso 1 calc R . C33 C 0.3493(17) -0.3399(27) 0.5495(11) 0.074(8) Uani 1 d . . H33 H 0.3284(17) -0.3673(27) 0.5846(11) 0.088 Uiso 1 calc R . C41 C 0.4697(12) -0.0963(23) 0.3584(10) 0.050(5) Uani 1 d . . H41 H 0.4795(12) 0.0068(23) 0.3778(10) 0.059 Uiso 1 calc R . C42 C 0.5195(13) -0.1824(31) 0.3323(12) 0.065(6) Uani 1 d . . H42 H 0.5708(13) -0.1542(31) 0.3323(12) 0.078 Uiso 1 calc R . C43 C 0.4772(16) -0.3165(34) 0.3071(10) 0.071(7) Uani 1 d . . H43 H 0.4956(16) -0.3954(34) 0.2835(10) 0.086 Uiso 1 calc R . B1 B 0.3363(14) -0.1612(25) 0.3834(11) 0.036(5) Uani 1 d . . Si1 Si 0.1023(4) 0.3226(8) -0.0402(3) 0.0510(15) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0482(5) 0.0312(4) 0.0339(4) -0.0002(4) 0.0086(3) -0.0042(4) S1 0.073(4) 0.040(3) 0.035(3) 0.000(3) 0.000(2) -0.013(3) O1 0.049(8) 0.057(8) 0.038(7) -0.002(6) -0.001(6) 0.009(7) O2 0.060(5) 0.042(5) 0.037(5) 0.006(4) 0.005(4) -0.015(4) N1 0.067(12) 0.051(10) 0.035(9) 0.009(8) 0.022(9) -0.005(9) N2 0.019(8) 0.031(8) 0.046(9) 0.000(7) -0.009(7) -0.002(6) N3 0.075(13) 0.080(14) 0.058(11) 0.015(10) 0.047(11) 0.017(11) N4 0.057(11) 0.042(10) 0.048(10) -0.014(8) 0.016(9) -0.006(9) N5 0.057(10) 0.040(9) 0.022(8) 0.001(7) 0.005(7) -0.009(8) N11 0.043(9) 0.031(8) 0.029(8) -0.001(7) 0.015(7) 0.000(7) N21 0.041(10) 0.041(10) 0.032(9) -0.010(7) -0.004(7) 0.002(7) N31 0.039(9) 0.041(9) 0.020(8) 0.015(6) -0.001(7) 0.019(7) N41 0.048(10) 0.030(8) 0.036(8) 0.001(7) 0.007(7) -0.011(8) C1 0.065(14) 0.022(10) 0.060(14) -0.005(9) 0.029(11) -0.003(9) C2 0.029(10) 0.048(11) 0.044(11) 0.003(9) 0.017(9) 0.003(9) C3 0.050(13) 0.044(12) 0.058(13) -0.001(10) 0.010(11) -0.008(10) C4 0.042(11) 0.058(13) 0.045(11) 0.014(11) 0.011(9) -0.016(11) C5 0.088(16) 0.031(10) 0.034(10) 0.001(10) 0.017(10) -0.011(12) C6 0.078(11) 0.080(11) 0.084(11) 0.001(8) 0.032(8) 0.002(8) C7 0.112(23) 0.077(18) 0.083(18) -0.017(15) 0.039(17) 0.013(16) C8 0.046(14) 0.101(19) 0.054(14) -0.028(14) -0.017(11) -0.003(14) C9 0.106(20) 0.099(19) 0.034(12) 0.028(12) 0.033(12) 0.012(15) C11 0.071(16) 0.049(12) 0.060(14) 0.010(11) 0.046(13) -0.001(12) C12 0.056(14) 0.030(11) 0.090(17) 0.011(11) 0.022(13) -0.027(10) C13 0.056(14) 0.047(13) 0.040(12) -0.011(10) -0.016(10) -0.020(11) C21 0.056(14) 0.063(16) 0.046(13) 0.004(11) 0.012(11) 0.020(12) C22 0.082(16) 0.038(12) 0.032(11) -0.018(9) 0.011(11) 0.007(11) C23 0.077(16) 0.014(9) 0.064(15) -0.021(9) 0.015(12) 0.001(10) C31 0.060(14) 0.048(12) 0.036(11) -0.006(10) 0.012(10) 0.002(11) C32 0.073(17) 0.058(14) 0.069(16) 0.016(12) 0.015(13) 0.029(13) C33 0.123(23) 0.061(15) 0.047(14) 0.011(12) 0.043(15) 0.037(15) C41 0.047(12) 0.035(12) 0.061(13) 0.007(10) 0.013(10) 0.000(10) C42 0.044(13) 0.084(18) 0.074(16) 0.004(14) 0.031(12) -0.008(14) C43 0.084(19) 0.102(21) 0.034(12) -0.005(13) 0.030(12) 0.010(17) B1 0.050(14) 0.029(12) 0.028(11) 0.004(9) 0.014(10) -0.001(10) Si1 0.055(4) 0.061(4) 0.036(3) 0.002(3) 0.015(3) 0.006(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 O1 1.646(13) . ? Re1 O2 1.778(15) . ? Re1 N1 2.11(2) . ? Re1 N5 2.140(14) . ? Re1 N2 2.141(14) . ? Re1 S1 2.424(5) . ? S1 C1 1.76(2) . ? O2 C6 1.45(2) . ? N1 C13 1.34(2) . ? N1 N11 1.36(2) . ? N2 C23 1.31(2) . ? N2 N21 1.39(2) . ? N3 C33 1.31(3) . ? N3 N31 1.34(2) . ? N4 C43 1.32(3) . ? N4 N41 1.37(2) . ? N5 C1 1.33(2) . ? N5 C5 1.36(2) . ? N11 C11 1.35(2) . ? N11 B1 1.54(2) . ? N21 C21 1.33(2) . ? N21 B1 1.54(2) . ? N31 C31 1.33(2) . ? N31 B1 1.50(2) . ? N41 C41 1.32(2) . ? N41 B1 1.58(3) . ? C1 C2 1.41(2) . ? C2 C3 1.36(2) . ? C2 Si1 1.89(2) . ? C3 C4 1.39(2) . ? C4 C5 1.33(2) . ? C7 Si1 1.85(2) . ? C8 Si1 1.86(2) . ? C9 Si1 1.87(2) . ? C11 C12 1.37(3) . ? C12 C13 1.34(3) . ? C21 C22 1.36(3) . ? C22 C23 1.37(3) . ? C31 C32 1.37(3) . ? C32 C33 1.37(3) . ? C41 C42 1.37(3) . ? C42 C43 1.33(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 O2 177.0(6) . . ? O1 Re1 N1 96.7(6) . . ? O2 Re1 N1 86.3(6) . . ? O1 Re1 N5 93.1(6) . . ? O2 Re1 N5 83.9(6) . . ? N1 Re1 N5 164.9(6) . . ? O1 Re1 N2 95.9(6) . . ? O2 Re1 N2 84.7(5) . . ? N1 Re1 N2 87.3(6) . . ? N5 Re1 N2 103.1(5) . . ? O1 Re1 S1 92.7(4) . . ? O2 Re1 S1 86.2(4) . . ? N1 Re1 S1 101.1(4) . . ? N5 Re1 S1 66.9(4) . . ? N2 Re1 S1 167.2(4) . . ? C1 S1 Re1 80.9(7) . . ? C6 O2 Re1 149.7(13) . . ? C13 N1 N11 106.9(15) . . ? C13 N1 Re1 124.8(13) . . ? N11 N1 Re1 128.1(12) . . ? C23 N2 N21 106.7(15) . . ? C23 N2 Re1 128.4(13) . . ? N21 N2 Re1 123.6(10) . . ? C33 N3 N31 106.6(18) . . ? C43 N4 N41 101.2(17) . . ? C1 N5 C5 119.5(15) . . ? C1 N5 Re1 103.3(12) . . ? C5 N5 Re1 137.0(12) . . ? C11 N11 N1 108.8(15) . . ? C11 N11 B1 130.2(16) . . ? N1 N11 B1 121.0(14) . . ? C21 N21 N2 108.4(15) . . ? C21 N21 B1 128.1(17) . . ? N2 N21 B1 122.7(15) . . ? N3 N31 C31 109.7(15) . . ? N3 N31 B1 123.9(16) . . ? C31 N31 B1 126.2(17) . . ? C41 N41 N4 112.2(16) . . ? C41 N41 B1 129.0(16) . . ? N4 N41 B1 118.2(15) . . ? N5 C1 C2 123.2(17) . . ? N5 C1 S1 108.9(14) . . ? C2 C1 S1 127.6(16) . . ? C3 C2 C1 114.3(17) . . ? C3 C2 Si1 124.2(15) . . ? C1 C2 Si1 121.5(14) . . ? C2 C3 C4 122.3(19) . . ? C5 C4 C3 119.6(20) . . ? C4 C5 N5 120.4(17) . . ? N11 C11 C12 107.2(17) . . ? C13 C12 C11 107.1(17) . . ? N1 C13 C12 109.9(17) . . ? N21 C21 C22 108.3(18) . . ? C21 C22 C23 106.3(17) . . ? N2 C23 C22 110.2(18) . . ? N31 C31 C32 108.4(19) . . ? C33 C32 C31 104.2(20) . . ? N3 C33 C32 111.1(21) . . ? N41 C41 C42 107.3(18) . . ? C43 C42 C41 103.6(20) . . ? N4 C43 C42 115.6(22) . . ? N31 B1 N11 109.8(15) . . ? N31 B1 N21 110.4(16) . . ? N11 B1 N21 110.8(16) . . ? N31 B1 N41 109.8(16) . . ? N11 B1 N41 109.3(15) . . ? N21 B1 N41 106.6(16) . . ? C8 Si1 C7 108.7(12) . . ? C8 Si1 C9 111.7(11) . . ? C7 Si1 C9 108.7(11) . . ? C8 Si1 C2 108.1(8) . . ? C7 Si1 C2 111.4(10) . . ? C9 Si1 C2 108.2(10) . . ? _refine_diff_density_max 2.984 _refine_diff_density_min -1.238 _refine_diff_density_rms 0.215 data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [ReO{B(pz)4}(Spy)2}].pySH _chemical_formula_analytical ? _chemical_formula_sum 'C27 H25 B N11 O Re S3' _chemical_formula_weight 812.77 _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 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 10.4190(10) _cell_length_b 25.297(2) _cell_length_c 11.5820(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.35(2) _cell_angle_gamma 90.00 _cell_volume 3043.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.9 _cell_measurement_theta_max 29.3 _exptl_crystal_description 'irregular' _exptl_crystal_colour 'brownish' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method ? _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 4.242 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.8258 _exptl_absorpt_correction_T_max 1.0000 _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscan' _diffrn_standards_number 3 _diffrn_standards_interval_count 'every 100 reflections' _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 6704 _diffrn_reflns_av_R_equivalents 0.1148 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.97 _reflns_number_total 6366 _reflns_number_observed 4286 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software (Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software (Enraf-Nonius,1989)' _computing_data_reduction 'process-MOLEN (Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP(Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 723 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^)+(0.0216P)^2^+7.6152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5643 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_obs 0.0507 _refine_ls_wR_factor_all 0.1148 _refine_ls_wR_factor_obs 0.0747 _refine_ls_goodness_of_fit_all 1.104 _refine_ls_goodness_of_fit_obs 1.118 _refine_ls_restrained_S_all 1.389 _refine_ls_restrained_S_obs 1.118 _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 Re1 Re 0.21698(3) 0.120175(13) 0.39144(3) 0.02550(9) Uani 1 d . . S1 S 0.2006(2) 0.17617(9) 0.5471(2) 0.0330(5) Uani 1 d . . S2 S 0.1080(2) 0.05719(9) 0.4908(2) 0.0405(6) Uani 1 d . . O1 O 0.1061(5) 0.1428(2) 0.2893(5) 0.0387(15) Uani 1 d . . N1 N 0.3592(6) 0.1681(2) 0.3125(5) 0.0260(14) Uani 1 d . . N2 N 0.4000(6) 0.0898(2) 0.4773(5) 0.0278(15) Uani 1 d . . N3 N 0.2653(6) 0.0559(3) 0.2812(6) 0.029(2) Uani 1 d . . N4 N 0.7218(6) 0.1047(3) 0.2515(6) 0.038(2) Uani 1 d . . N5 N 0.2635(6) 0.2764(3) 0.5192(6) 0.034(2) Uani 1 d . . N6 N 0.0322(8) 0.0814(3) 0.7000(7) 0.053(2) Uani 1 d . . N11 N 0.4617(5) 0.1470(3) 0.2626(5) 0.0233(14) Uani 1 d . . N21 N 0.4998(6) 0.0771(3) 0.4128(5) 0.0261(15) Uani 1 d . . N31 N 0.3767(6) 0.0567(3) 0.2257(5) 0.0269(15) Uani 1 d . . N41 N 0.6180(6) 0.0710(3) 0.2357(5) 0.030(2) Uani 1 d . . C1 C 0.3132(7) 0.2292(3) 0.5451(7) 0.031(2) Uani 1 d . . C2 C 0.0058(8) 0.0889(4) 0.5872(7) 0.036(2) Uani 1 d . . C3 C 0.4443(8) 0.2210(4) 0.5755(8) 0.046(2) Uani 1 d . . H3 H 0.4759(8) 0.1873(4) 0.5930(8) 0.055 Uiso 1 calc R . C4 C 0.5248(9) 0.2638(4) 0.5788(9) 0.056(3) Uani 1 d . . H4 H 0.6126(9) 0.2594(4) 0.5968(9) 0.067 Uiso 1 calc R . C5 C 0.4742(9) 0.3138(4) 0.5551(8) 0.048(3) Uani 1 d . . H5 H 0.5266(9) 0.3436(4) 0.5600(8) 0.058 Uiso 1 calc R . C6 C 0.3451(9) 0.3181(4) 0.5244(8) 0.042(2) Uani 1 d . . H6 H 0.3117(9) 0.3514(4) 0.5061(8) 0.051 Uiso 1 calc R . C7 C -0.0980(7) 0.1173(4) 0.5407(8) 0.048(2) Uani 1 d . . H7 H -0.1128(7) 0.1215(4) 0.4611(8) 0.058 Uiso 1 calc R . C8 C -0.1796(8) 0.1395(4) 0.6157(10) 0.056(3) Uani 1 d . . H8 H -0.2500(8) 0.1595(4) 0.5873(10) 0.067 Uiso 1 calc R . C9 C -0.1558(11) 0.1318(4) 0.7312(11) 0.066(3) Uani 1 d . . H9 H -0.2109(11) 0.1454(4) 0.7832(11) 0.080 Uiso 1 calc R . C10 C -0.0510(13) 0.1040(4) 0.7688(9) 0.073(4) Uani 1 d . . H10 H -0.0345(13) 0.1001(4) 0.8483(9) 0.088 Uiso 1 calc R . C11 C 0.5142(8) 0.1840(3) 0.1971(7) 0.036(2) Uani 1 d . . H11 H 0.5858(8) 0.1794(3) 0.1548(7) 0.043 Uiso 1 calc R . C12 C 0.4430(8) 0.2299(3) 0.2035(7) 0.039(2) Uani 1 d . . H12 H 0.4560(8) 0.2620(3) 0.1668(7) 0.046 Uiso 1 calc R . C13 C 0.3486(8) 0.2178(3) 0.2764(7) 0.035(2) Uani 1 d . . H13 H 0.2859(8) 0.2413(3) 0.2975(7) 0.041 Uiso 1 calc R . C21 C 0.5962(7) 0.0579(3) 0.4842(7) 0.029(2) Uani 1 d . . H21 H 0.6752(7) 0.0462(3) 0.4618(7) 0.035 Uiso 1 calc R . C22 C 0.5596(8) 0.0585(4) 0.5957(7) 0.039(2) Uani 1 d . . H22 H 0.6080(8) 0.0480(4) 0.6625(7) 0.047 Uiso 1 calc R . C23 C 0.4349(7) 0.0780(3) 0.5868(7) 0.031(2) Uani 1 d . . H23 H 0.3835(7) 0.0822(3) 0.6484(7) 0.037 Uiso 1 calc R . C31 C 0.3572(8) 0.0283(4) 0.1287(7) 0.041(2) Uani 1 d . . H31 H 0.4175(8) 0.0237(4) 0.0743(7) 0.049 Uiso 1 calc R . C32 C 0.2367(8) 0.0071(4) 0.1206(8) 0.048(3) Uani 1 d . . H32 H 0.2000(8) -0.0152(4) 0.0633(8) 0.058 Uiso 1 calc R . C33 C 0.1810(8) 0.0262(3) 0.2177(8) 0.039(2) Uani 1 d . . H33 H 0.0972(8) 0.0193(3) 0.2357(8) 0.047 Uiso 1 calc R . C41 C 0.6571(8) 0.0234(4) 0.2054(7) 0.041(2) Uani 1 d . . H41 H 0.6045(8) -0.0059(4) 0.1904(7) 0.049 Uiso 1 calc R . C42 C 0.7879(8) 0.0247(4) 0.2000(8) 0.050(3) Uani 1 d . . H42 H 0.8418(8) -0.0028(4) 0.1814(8) 0.060 Uiso 1 calc R . C43 C 0.8213(8) 0.0760(4) 0.2282(8) 0.045(2) Uani 1 d . . H43 H 0.9051(8) 0.0889(4) 0.2304(8) 0.054 Uiso 1 calc R . B1 B 0.4934(8) 0.0878(4) 0.2822(8) 0.026(2) Uani 1 d . . S1A S 0.5447(3) 0.10582(10) 0.9153(2) 0.0535(7) Uani 1 d . . C1A C 0.4486(8) 0.1589(4) 0.8955(7) 0.036(2) Uani 1 d . . N1A N 0.4982(8) 0.2082(3) 0.9111(6) 0.040(2) Uani 1 d . . C2A C 0.3137(9) 0.1575(4) 0.8620(8) 0.053(3) Uani 1 d . . H2A H 0.2721(9) 0.1251(4) 0.8522(8) 0.063 Uiso 1 calc R . C3A C 0.2470(9) 0.2020(5) 0.8447(9) 0.060(3) Uani 1 d . . H3A H 0.1596(9) 0.1995(5) 0.8221(9) 0.072 Uiso 1 calc R . C4A C 0.3015(9) 0.2518(5) 0.8587(8) 0.057(3) Uani 1 d . . H4A H 0.2532(9) 0.2824(5) 0.8454(8) 0.068 Uiso 1 calc R . C5A C 0.4293(9) 0.2536(4) 0.8930(8) 0.048(2) Uani 1 d . . H5A H 0.4700(9) 0.2861(4) 0.9041(8) 0.058 Uiso 1 calc R . H1A H 0.5749(89) 0.2085(39) 0.9419(82) 0.065(35) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02138(13) 0.02731(15) 0.02838(15) -0.0006(2) 0.00568(10) 0.0001(2) S1 0.0303(10) 0.0358(12) 0.0343(12) -0.0063(10) 0.0110(9) -0.0027(9) S2 0.0362(12) 0.0336(13) 0.0543(15) -0.0001(11) 0.0210(11) -0.0037(10) O1 0.032(3) 0.048(4) 0.035(3) -0.002(3) -0.004(3) 0.003(3) N1 0.028(3) 0.024(4) 0.027(4) 0.001(3) 0.008(3) 0.000(3) N2 0.026(3) 0.031(4) 0.027(4) -0.001(3) 0.010(3) 0.004(3) N3 0.024(3) 0.029(4) 0.036(4) -0.010(3) 0.008(3) -0.007(3) N4 0.025(3) 0.039(5) 0.050(5) 0.004(3) 0.011(3) -0.003(3) N5 0.035(4) 0.031(4) 0.035(4) -0.003(3) 0.008(3) -0.007(3) N6 0.064(5) 0.046(5) 0.049(5) 0.002(4) 0.010(4) 0.000(4) N11 0.018(3) 0.029(4) 0.024(3) 0.004(3) 0.010(3) 0.003(3) N21 0.025(3) 0.028(4) 0.025(4) 0.006(3) -0.003(3) 0.000(3) N31 0.023(3) 0.031(4) 0.028(4) 0.000(3) 0.009(3) 0.004(3) N41 0.023(3) 0.033(4) 0.033(4) -0.005(3) 0.006(3) 0.004(3) C1 0.033(4) 0.039(5) 0.023(4) -0.004(4) 0.007(3) -0.003(4) C2 0.040(5) 0.040(6) 0.031(5) -0.003(4) 0.014(4) -0.013(4) C3 0.037(5) 0.046(6) 0.055(6) -0.005(5) -0.006(4) 0.010(4) C4 0.034(5) 0.069(8) 0.062(7) -0.018(6) -0.009(5) -0.009(5) C5 0.045(6) 0.057(7) 0.042(6) -0.002(5) 0.006(5) -0.024(5) C6 0.050(6) 0.037(5) 0.041(5) -0.007(4) 0.007(4) -0.002(4) C7 0.031(4) 0.065(6) 0.048(5) -0.013(6) 0.001(4) 0.001(5) C8 0.031(5) 0.054(7) 0.085(8) -0.012(6) 0.008(6) -0.001(4) C9 0.070(7) 0.049(8) 0.087(9) -0.018(6) 0.046(7) -0.013(6) C10 0.115(10) 0.065(8) 0.044(6) -0.004(6) 0.029(7) -0.008(7) C11 0.044(5) 0.032(5) 0.032(5) 0.001(4) 0.013(4) -0.004(4) C12 0.050(5) 0.030(5) 0.037(5) 0.007(4) 0.011(4) -0.007(4) C13 0.041(5) 0.030(5) 0.032(5) 0.001(4) 0.000(4) 0.003(4) C21 0.019(4) 0.028(5) 0.040(5) 0.008(4) -0.002(3) 0.000(3) C22 0.038(5) 0.049(6) 0.030(5) 0.007(4) -0.007(4) 0.000(4) C23 0.036(4) 0.020(4) 0.037(5) 0.006(4) 0.005(4) -0.003(4) C31 0.046(5) 0.050(6) 0.026(5) -0.015(4) 0.004(4) -0.009(5) C32 0.042(5) 0.052(6) 0.049(6) -0.021(5) 0.000(5) -0.011(5) C33 0.026(4) 0.038(5) 0.053(6) -0.012(5) 0.005(4) -0.005(4) C41 0.041(5) 0.041(6) 0.041(5) 0.000(4) 0.011(4) -0.003(4) C42 0.035(5) 0.060(7) 0.054(6) 0.003(5) 0.002(5) 0.018(5) C43 0.018(4) 0.066(7) 0.050(6) 0.008(5) 0.004(4) 0.002(4) B1 0.021(4) 0.023(5) 0.035(5) -0.001(4) 0.004(4) -0.001(4) S1A 0.058(2) 0.044(2) 0.061(2) -0.0072(12) 0.0132(13) -0.0008(12) C1A 0.036(5) 0.042(6) 0.030(5) -0.010(4) 0.007(4) -0.006(4) N1A 0.039(5) 0.043(5) 0.037(5) 0.001(4) 0.000(4) -0.006(4) C2A 0.045(6) 0.062(7) 0.052(6) -0.026(5) 0.007(5) -0.009(5) C3A 0.039(6) 0.078(8) 0.060(7) -0.018(6) -0.008(5) 0.003(6) C4A 0.048(6) 0.066(7) 0.052(7) -0.010(6) -0.014(5) 0.015(6) C5A 0.050(6) 0.046(6) 0.050(6) -0.001(5) 0.007(5) 0.005(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 Re1 O1 1.690(5) . ? Re1 N3 2.150(6) . ? Re1 N1 2.169(6) . ? Re1 N2 2.220(6) . ? Re1 S1 2.309(2) . ? Re1 S2 2.313(2) . ? S1 C1 1.782(8) . ? S2 C2 1.790(9) . ? N1 C13 1.326(10) . ? N1 N11 1.362(8) . ? N2 C23 1.327(9) . ? N2 N21 1.364(8) . ? N3 C33 1.334(9) . ? N3 N31 1.368(8) . ? N4 C43 1.310(10) . ? N4 N41 1.379(8) . ? N5 C1 1.328(10) . ? N5 C6 1.353(10) . ? N6 C2 1.328(11) . ? N6 C10 1.349(13) . ? N11 C11 1.345(9) . ? N11 B1 1.549(10) . ? N21 C21 1.342(9) . ? N21 B1 1.534(11) . ? N31 C31 1.334(10) . ? N31 B1 1.551(10) . ? N41 C41 1.326(10) . ? N41 B1 1.503(10) . ? C1 C3 1.400(11) . ? C2 C7 1.375(12) . ? C3 C4 1.368(12) . ? C4 C5 1.391(13) . ? C5 C6 1.369(12) . ? C7 C8 1.379(12) . ? C8 C9 1.356(14) . ? C9 C10 1.343(15) . ? C11 C12 1.385(11) . ? C12 C13 1.379(11) . ? C21 C22 1.374(11) . ? C22 C23 1.387(11) . ? C31 C32 1.363(11) . ? C32 C33 1.390(12) . ? C41 C42 1.369(11) . ? C42 C43 1.377(13) . ? S1A C1A 1.680(9) . ? C1A N1A 1.356(11) . ? C1A C2A 1.430(12) . ? N1A C5A 1.362(11) . ? C2A C3A 1.329(13) . ? C3A C4A 1.387(14) . ? C4A C5A 1.361(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 N3 91.1(3) . . ? O1 Re1 N1 88.2(2) . . ? N3 Re1 N1 88.5(2) . . ? O1 Re1 N2 161.7(2) . . ? N3 Re1 N2 76.9(2) . . ? N1 Re1 N2 78.0(2) . . ? O1 Re1 S1 104.6(2) . . ? N3 Re1 S1 164.1(2) . . ? N1 Re1 S1 94.5(2) . . ? N2 Re1 S1 88.5(2) . . ? O1 Re1 S2 104.3(2) . . ? N3 Re1 S2 85.5(2) . . ? N1 Re1 S2 166.2(2) . . ? N2 Re1 S2 88.6(2) . . ? S1 Re1 S2 88.06(8) . . ? C1 S1 Re1 111.3(3) . . ? C2 S2 Re1 109.9(3) . . ? C13 N1 N11 106.6(6) . . ? C13 N1 Re1 128.3(5) . . ? N11 N1 Re1 122.9(5) . . ? C23 N2 N21 107.8(6) . . ? C23 N2 Re1 132.1(5) . . ? N21 N2 Re1 120.1(5) . . ? C33 N3 N31 107.2(6) . . ? C33 N3 Re1 125.4(5) . . ? N31 N3 Re1 120.9(5) . . ? C43 N4 N41 104.8(7) . . ? C1 N5 C6 117.3(7) . . ? C2 N6 C10 115.2(9) . . ? C11 N11 N1 109.5(6) . . ? C11 N11 B1 131.6(7) . . ? N1 N11 B1 118.8(6) . . ? C21 N21 N2 108.3(6) . . ? C21 N21 B1 130.2(7) . . ? N2 N21 B1 121.4(6) . . ? C31 N31 N3 107.9(6) . . ? C31 N31 B1 133.7(7) . . ? N3 N31 B1 118.3(6) . . ? C41 N41 N4 110.0(6) . . ? C41 N41 B1 130.0(7) . . ? N4 N41 B1 117.8(6) . . ? N5 C1 C3 123.1(8) . . ? N5 C1 S1 115.8(6) . . ? C3 C1 S1 121.1(7) . . ? N6 C2 C7 123.9(8) . . ? N6 C2 S2 117.5(7) . . ? C7 C2 S2 118.5(7) . . ? C4 C3 C1 118.3(9) . . ? C3 C4 C5 119.5(9) . . ? C6 C5 C4 118.3(9) . . ? N5 C6 C5 123.5(9) . . ? C2 C7 C8 118.1(9) . . ? C9 C8 C7 119.2(10) . . ? C10 C9 C8 118.6(10) . . ? C9 C10 N6 125.0(11) . . ? N11 C11 C12 108.1(7) . . ? C13 C12 C11 104.8(7) . . ? N1 C13 C12 111.0(8) . . ? N21 C21 C22 109.1(7) . . ? C21 C22 C23 105.0(7) . . ? N2 C23 C22 109.8(7) . . ? N31 C31 C32 110.5(8) . . ? C31 C32 C33 104.2(8) . . ? N3 C33 C32 110.1(7) . . ? N41 C41 C42 108.5(8) . . ? C41 C42 C43 104.3(8) . . ? N4 C43 C42 112.4(8) . . ? N41 B1 N21 109.2(6) . . ? N41 B1 N11 113.7(7) . . ? N21 B1 N11 108.0(7) . . ? N41 B1 N31 112.1(7) . . ? N21 B1 N31 107.5(6) . . ? N11 B1 N31 106.1(6) . . ? N1A C1A C2A 114.5(9) . . ? N1A C1A S1A 119.9(7) . . ? C2A C1A S1A 125.5(7) . . ? C1A N1A C5A 124.3(8) . . ? C3A C2A C1A 120.8(9) . . ? C2A C3A C4A 123.1(9) . . ? C5A C4A C3A 116.5(10) . . ? C4A C5A N1A 120.7(10) . . ? _refine_diff_density_max 0.700 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.168 #===END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [ReO{B(pz)4}Cl(Spy)].HCl _chemical_formula_analytical ? _chemical_formula_sum 'C18 H19 B Cl4 N9 O Re S' _chemical_formula_weight 748.29 _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 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'B' 'B' 0.0013 0.0007 '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' 'S' 'S' 0.1246 0.1234 '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 8.5130(6) _cell_length_b 9.1937(8) _cell_length_c 16.678(2) _cell_angle_alpha 80.472(9) _cell_angle_beta 81.748(9) _cell_angle_gamma 89.193(6) _cell_volume 1273.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 25.9 _exptl_crystal_description 'plates' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method ? _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 5.303 _exptl_absorpt_correction_type 'empirical via\y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.5279 _exptl_absorpt_correction_T_max 1.0000 _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscan' _diffrn_standards_number 3 _diffrn_standards_interval_count 'every 100 reflections ' _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 1.1 _diffrn_reflns_number 4612 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 24.96 _reflns_number_total 4446 _reflns_number_observed 3670 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software (Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software (Enraf-Nonius,1989)' _computing_data_reduction 'process-MOLEN (Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0371P)^2^+6.5775P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4445 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_obs 0.0481 _refine_ls_wR_factor_all 0.1080 _refine_ls_wR_factor_obs 0.0937 _refine_ls_goodness_of_fit_all 1.143 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.144 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.05936(4) 0.12344(4) 0.22136(3) 0.03030(13) Uani 1 d . . S1 S -0.0224(3) 0.0832(3) 0.3632(2) 0.0457(7) Uani 1 d . . Cl1 Cl 0.1275(3) -0.1246(3) 0.2272(2) 0.0484(7) Uani 1 d . . O1 O 0.2329(7) 0.2114(8) 0.2134(4) 0.044(2) Uani 1 d . . N1 N 0.0719(8) 0.1331(8) 0.0956(5) 0.031(2) Uani 1 d . . N2 N -0.0607(8) 0.3252(9) 0.2117(5) 0.033(2) Uani 1 d . . N3 N -0.1893(8) 0.0567(8) 0.2110(5) 0.029(2) Uani 1 d . . N4 N -0.3760(9) 0.2454(9) -0.0039(5) 0.043(2) Uani 1 d . . N5 N 0.0571(11) -0.1907(11) 0.4351(6) 0.051(2) Uani 1 d . . N11 N -0.0339(8) 0.2133(8) 0.0508(4) 0.027(2) Uani 1 d . . N21 N -0.1554(8) 0.3721(8) 0.1533(4) 0.028(2) Uani 1 d . . N31 N -0.2738(8) 0.1298(8) 0.1528(5) 0.027(2) Uani 1 d . . N41 N -0.2871(8) 0.3345(8) 0.0310(5) 0.032(2) Uani 1 d . . C1 C 0.1091(12) -0.0496(12) 0.4050(6) 0.044(3) Uani 1 d . . C2 C 0.2642(13) -0.0160(16) 0.4098(8) 0.067(4) Uani 1 d . . H2 H 0.3035(13) 0.0794(16) 0.3911(8) 0.080 Uiso 1 calc R . C3 C 0.3601(14) -0.1242(16) 0.4422(8) 0.066(4) Uani 1 d . . H3 H 0.4667(14) -0.1034(16) 0.4423(8) 0.079 Uiso 1 calc R . C4 C 0.3021(16) -0.2607(16) 0.4741(8) 0.067(4) Uani 1 d . . H4 H 0.3666(16) -0.3317(16) 0.4989(8) 0.080 Uiso 1 calc R . C5 C 0.1514(15) -0.2930(12) 0.4697(7) 0.054(3) Uani 1 d . . H5 H 0.1116(15) -0.3874(12) 0.4908(7) 0.065 Uiso 1 calc R . C11 C 0.0131(11) 0.2142(10) -0.0281(6) 0.033(2) Uani 1 d . . H11 H -0.0413(11) 0.2583(10) -0.0702(6) 0.040 Uiso 1 calc R . C12 C 0.1542(11) 0.1404(10) -0.0391(6) 0.035(2) Uani 1 d . . H12 H 0.2146(11) 0.1267(10) -0.0883(6) 0.042 Uiso 1 calc R . C13 C 0.1852(10) 0.0918(10) 0.0390(6) 0.037(2) Uani 1 d . . H13 H 0.2737(10) 0.0370(10) 0.0515(6) 0.044 Uiso 1 calc R . C21 C -0.2149(11) 0.5039(10) 0.1652(6) 0.039(2) Uani 1 d . . H21 H -0.2845(11) 0.5587(10) 0.1342(6) 0.047 Uiso 1 calc R . C22 C -0.1566(13) 0.5444(10) 0.2305(7) 0.047(3) Uani 1 d . . H22 H -0.1762(13) 0.6315(10) 0.2515(7) 0.057 Uiso 1 calc R . C23 C -0.0635(12) 0.4306(11) 0.2584(6) 0.041(2) Uani 1 d . . H23 H -0.0097(12) 0.4269(11) 0.3035(6) 0.049 Uiso 1 calc R . C31 C -0.4181(10) 0.0708(10) 0.1621(6) 0.034(2) Uani 1 d . . H31 H -0.4978(10) 0.1025(10) 0.1307(6) 0.040 Uiso 1 calc R . C32 C -0.4289(11) -0.0457(12) 0.2264(6) 0.042(3) Uani 1 d . . H32 H -0.5151(11) -0.1092(12) 0.2459(6) 0.051 Uiso 1 calc R . C33 C -0.2874(10) -0.0486(10) 0.2553(6) 0.032(2) Uani 1 d . . H33 H -0.2622(10) -0.1150(10) 0.3000(6) 0.039 Uiso 1 calc R . C41 C -0.2638(12) 0.4669(12) -0.0180(6) 0.045(3) Uani 1 d . . H41 H -0.2062(12) 0.5454(12) -0.0078(6) 0.053 Uiso 1 calc R . C42 C -0.3376(13) 0.4666(12) -0.0842(7) 0.050(3) Uani 1 d . . H42 H -0.3411(13) 0.5429(12) -0.1281(7) 0.060 Uiso 1 calc R . C43 C -0.4075(13) 0.3277(13) -0.0725(7) 0.052(3) Uani 1 d . . H43 H -0.4687(13) 0.2964(13) -0.1085(7) 0.062 Uiso 1 calc R . B1 B -0.1924(11) 0.2649(11) 0.0954(7) 0.030(2) Uani 1 d . . Cl1S Cl 0.5441(4) -0.7204(4) 0.3263(2) 0.0803(11) Uani 1 d . . Cl2S Cl 0.3595(6) -0.4532(5) 0.2945(3) 0.1007(14) Uani 1 d . . C1S C 0.4708(15) -0.5587(15) 0.3624(8) 0.065(3) Uani 1 d . . H1S1 H 0.4052(15) -0.5858(15) 0.4152(8) 0.078 Uiso 1 calc R . H1S2 H 0.5593(15) -0.4999(15) 0.3702(8) 0.078 Uiso 1 calc R . Cl2 Cl -0.2552(3) -0.3337(3) 0.4380(2) 0.0594(8) Uani 1 d . . H1 H -0.0557(227) -0.2223(215) 0.4362(117) 0.172(81) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0283(2) 0.0300(2) 0.0329(2) -0.00374(15) -0.00706(14) 0.00088(13) S1 0.052(2) 0.052(2) 0.0333(15) -0.0032(13) -0.0090(12) 0.0029(13) Cl1 0.0512(15) 0.0358(14) 0.059(2) -0.0022(13) -0.0181(13) 0.0111(11) O1 0.024(3) 0.053(4) 0.058(5) -0.013(4) -0.012(3) 0.001(3) N1 0.017(3) 0.040(5) 0.036(5) -0.004(4) -0.005(3) 0.007(3) N2 0.028(4) 0.045(5) 0.027(4) -0.010(4) -0.002(3) 0.000(3) N3 0.024(4) 0.029(4) 0.034(5) -0.006(3) -0.009(3) 0.001(3) N4 0.039(5) 0.045(5) 0.048(6) -0.010(4) -0.016(4) 0.001(4) N5 0.049(6) 0.054(6) 0.048(6) 0.005(5) -0.009(5) -0.008(5) N11 0.024(4) 0.025(4) 0.031(5) -0.004(3) -0.002(3) -0.008(3) N21 0.034(4) 0.025(4) 0.026(4) -0.005(3) -0.005(3) 0.001(3) N31 0.024(4) 0.023(4) 0.033(4) -0.004(3) 0.000(3) -0.002(3) N41 0.024(4) 0.033(4) 0.039(5) -0.001(4) -0.012(3) 0.000(3) C1 0.053(6) 0.042(6) 0.037(6) 0.004(5) -0.013(5) -0.008(5) C2 0.047(7) 0.088(10) 0.057(8) 0.026(7) -0.019(6) -0.023(6) C3 0.042(6) 0.091(11) 0.063(9) 0.003(8) -0.016(6) -0.004(7) C4 0.070(9) 0.073(9) 0.057(8) 0.004(7) -0.028(7) 0.014(7) C5 0.075(8) 0.031(6) 0.056(8) 0.000(5) -0.016(6) 0.007(6) C11 0.046(6) 0.024(5) 0.027(5) 0.003(4) -0.002(4) -0.012(4) C12 0.038(5) 0.038(6) 0.029(6) -0.014(4) 0.007(4) -0.001(4) C13 0.025(5) 0.034(5) 0.054(7) -0.015(5) -0.004(4) 0.004(4) C21 0.042(5) 0.025(5) 0.049(7) -0.003(5) -0.006(5) 0.007(4) C22 0.064(7) 0.014(5) 0.064(8) -0.017(5) 0.003(6) -0.004(5) C23 0.047(6) 0.037(6) 0.039(6) -0.012(5) -0.002(5) -0.003(5) C31 0.024(4) 0.030(5) 0.049(6) -0.012(5) -0.003(4) -0.004(4) C32 0.028(5) 0.049(6) 0.050(7) -0.013(5) 0.004(4) -0.014(4) C33 0.033(5) 0.025(5) 0.035(6) 0.003(4) 0.000(4) -0.005(4) C41 0.053(6) 0.039(6) 0.039(6) 0.006(5) -0.010(5) -0.004(5) C42 0.063(7) 0.041(6) 0.040(7) 0.016(5) -0.013(5) -0.004(5) C43 0.054(7) 0.055(7) 0.048(7) -0.004(6) -0.021(6) 0.015(6) B1 0.025(5) 0.031(6) 0.033(6) -0.003(5) -0.007(4) -0.003(4) Cl1S 0.077(2) 0.066(2) 0.094(3) -0.025(2) 0.017(2) -0.015(2) Cl2S 0.125(3) 0.107(3) 0.078(3) -0.016(2) -0.043(3) 0.018(3) C1S 0.068(8) 0.080(9) 0.053(8) -0.027(7) -0.012(6) -0.008(7) Cl2 0.052(2) 0.062(2) 0.060(2) 0.006(2) -0.0113(14) -0.0181(14) _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 O1 1.673(6) . ? Re1 N1 2.073(8) . ? Re1 N2 2.099(8) . ? Re1 N3 2.250(7) . ? Re1 Cl1 2.335(3) . ? Re1 S1 2.337(3) . ? S1 C1 1.771(10) . ? N1 C13 1.346(11) . ? N1 N11 1.380(10) . ? N2 C23 1.339(12) . ? N2 N21 1.364(10) . ? N3 C33 1.338(11) . ? N3 N31 1.372(10) . ? N4 C43 1.324(13) . ? N4 N41 1.373(11) . ? N5 C5 1.339(14) . ? N5 C1 1.366(13) . ? N11 C11 1.318(11) . ? N11 B1 1.552(12) . ? N21 C21 1.342(11) . ? N21 B1 1.553(13) . ? N31 C31 1.328(11) . ? N31 B1 1.543(12) . ? N41 C41 1.349(12) . ? N41 B1 1.490(12) . ? C1 C2 1.377(14) . ? C2 C3 1.37(2) . ? C3 C4 1.35(2) . ? C4 C5 1.34(2) . ? C11 C12 1.376(13) . ? C12 C13 1.367(13) . ? C21 C22 1.366(14) . ? C22 C23 1.364(14) . ? C31 C32 1.379(14) . ? C32 C33 1.359(13) . ? C41 C42 1.347(14) . ? C42 C43 1.39(2) . ? Cl1S C1S 1.767(13) . ? Cl2S C1S 1.742(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 N1 93.6(3) . . ? O1 Re1 N2 90.6(3) . . ? N1 Re1 N2 89.3(3) . . ? O1 Re1 N3 165.5(3) . . ? N1 Re1 N3 78.6(3) . . ? N2 Re1 N3 77.2(3) . . ? O1 Re1 Cl1 104.4(2) . . ? N1 Re1 Cl1 86.8(2) . . ? N2 Re1 Cl1 164.7(2) . . ? N3 Re1 Cl1 87.5(2) . . ? O1 Re1 S1 102.1(3) . . ? N1 Re1 S1 164.3(2) . . ? N2 Re1 S1 89.6(2) . . ? N3 Re1 S1 85.9(2) . . ? Cl1 Re1 S1 90.22(10) . . ? C1 S1 Re1 105.7(4) . . ? C13 N1 N11 105.0(7) . . ? C13 N1 Re1 131.9(6) . . ? N11 N1 Re1 122.3(5) . . ? C23 N2 N21 106.6(8) . . ? C23 N2 Re1 129.3(7) . . ? N21 N2 Re1 124.1(6) . . ? C33 N3 N31 105.4(7) . . ? C33 N3 Re1 132.2(6) . . ? N31 N3 Re1 122.4(5) . . ? C43 N4 N41 105.1(9) . . ? C5 N5 C1 121.8(10) . . ? C11 N11 N1 109.2(7) . . ? C11 N11 B1 130.1(8) . . ? N1 N11 B1 120.0(7) . . ? C21 N21 N2 108.7(8) . . ? C21 N21 B1 131.8(8) . . ? N2 N21 B1 118.9(7) . . ? C31 N31 N3 110.0(7) . . ? C31 N31 B1 133.0(8) . . ? N3 N31 B1 116.8(7) . . ? C41 N41 N4 109.6(8) . . ? C41 N41 B1 128.3(8) . . ? N4 N41 B1 118.7(7) . . ? N5 C1 C2 117.7(10) . . ? N5 C1 S1 120.0(8) . . ? C2 C1 S1 122.3(9) . . ? C3 C2 C1 119.4(12) . . ? C4 C3 C2 120.9(11) . . ? C5 C4 C3 119.5(11) . . ? C4 C5 N5 120.6(11) . . ? N11 C11 C12 110.1(8) . . ? C13 C12 C11 104.0(8) . . ? N1 C13 C12 111.7(8) . . ? N21 C21 C22 108.7(9) . . ? C23 C22 C21 105.8(9) . . ? N2 C23 C22 110.2(9) . . ? N31 C31 C32 107.9(8) . . ? C33 C32 C31 105.7(8) . . ? N3 C33 C32 111.0(8) . . ? C42 C41 N41 108.7(10) . . ? C41 C42 C43 105.0(9) . . ? N4 C43 C42 111.5(10) . . ? N41 B1 N31 114.1(7) . . ? N41 B1 N11 107.4(8) . . ? N31 B1 N11 108.0(7) . . ? N41 B1 N21 112.9(8) . . ? N31 B1 N21 105.2(7) . . ? N11 B1 N21 109.0(7) . . ? Cl2S C1S Cl1S 112.2(7) . . ? _refine_diff_density_max 1.913 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.175 #===END