Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Edwards, Peter G.' 'Baker, Robert J.' 'Gracia-Mora, Jesus' 'Ingold, Florent' 'Malik, K. M. Abdul' _publ_contact_author_name 'Prof Peter G Edwards' _publ_contact_author_address ; Prof Peter G Edwards Department of Chemistry Cardiff University P.O box 912 Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email 'EDWARDSPG@CARDIFF.AC.UK' _publ_section_title ; Manganese and rhenium triphosphorus macrocycle complexes and reactions with alkenes. ; data_s921 _database_code_CSD 153078 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H45 Cl3 P3 Re' _chemical_formula_weight 683.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.409(3) _cell_length_b 15.947(3) _cell_length_c 11.737(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2696.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all observed relections in the entire data set _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.35 _exptl_crystal_description bloc _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 4.988 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3686 _exptl_absorpt_correction_T_max 0.4353 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker-Nonius CCD area detector _diffrn_measurement_method 'theta & omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9845 _diffrn_reflns_av_R_equivalents 0.2675 _diffrn_reflns_av_sigmaI/netI 0.1586 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2556 _reflns_number_gt 2191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO' (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO' (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrigia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The C(5) and C(11) atoms were disordered and two positions for each atom were refined with occupancy 0.50. The P-C and C-C distances in the disordered groups ere refined with constraint P-C = 1.83 A and C-C = 1.53 A. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^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 The hydrogen atoms of the disordered groups were ignored; others included in the riding model _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2556 _refine_ls_number_parameters 151 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.006 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.10743(2) 0.2500 0.33525(3) 0.0194(2) Uani 1 2 d S . . Cl1 Cl 0.19270(17) 0.2500 0.15852(17) 0.0223(5) Uani 1 2 d S . . Cl2 Cl 0.20275(11) 0.35872(10) 0.41945(14) 0.0304(4) Uani 1 1 d . . . P1 P 0.01018(12) 0.14376(10) 0.25562(15) 0.0222(4) Uani 1 1 d . . . P2 P 0.02007(19) 0.2500 0.5075(2) 0.0300(6) Uani 1 2 d SD . . C1 C -0.0929(7) 0.2500 0.1108(10) 0.031(2) Uani 1 2 d S . . H1A H -0.1288 0.2500 0.0388 0.037 Uiso 1 2 calc SR . . H1B H -0.1381 0.2500 0.1743 0.037 Uiso 1 2 calc SR . . C2 C -0.0375(5) 0.1691(4) 0.1165(6) 0.0275(15) Uani 1 1 d . . . H2A H 0.0143 0.1727 0.0613 0.033 Uiso 1 1 calc R . . H2B H -0.0781 0.1223 0.0921 0.033 Uiso 1 1 calc R . . C3 C -0.0955(5) 0.1194(7) 0.3340(6) 0.039(2) Uani 1 1 d . A . H3A H -0.1394 0.1664 0.3226 0.047 Uiso 1 1 calc R . . H3B H -0.1238 0.0692 0.2985 0.047 Uiso 1 1 calc R . . C4 C -0.0884(6) 0.1031(5) 0.4628(7) 0.0391(19) Uani 1 1 d D . . C5 C -0.0128(9) 0.1407(4) 0.5371(10) 0.037(4) Uani 0.50 1 d PD A 1 C5' C -0.0871(6) 0.1895(6) 0.5201(11) 0.027(3) Uani 0.50 1 d PD . 2 C6 C 0.0618(5) 0.0384(4) 0.2397(7) 0.0271(15) Uani 1 1 d . . . H6A H 0.0714 0.0156 0.3172 0.033 Uiso 1 1 calc R . . H6B H 0.0150 0.0024 0.2022 0.033 Uiso 1 1 calc R . . C7 C 0.1536(6) 0.0275(5) 0.1740(6) 0.0320(18) Uani 1 1 d . . . H7 H 0.1961 0.0739 0.1976 0.038 Uiso 1 1 calc R . . C8 C 0.1425(7) 0.0321(7) 0.0468(7) 0.053(2) Uani 1 1 d . . . H8A H 0.2032 0.0253 0.0103 0.080 Uiso 1 1 calc R . . H8B H 0.1163 0.0867 0.0259 0.080 Uiso 1 1 calc R . . H8C H 0.1008 -0.0126 0.0212 0.080 Uiso 1 1 calc R . . C9 C 0.1982(7) -0.0537(6) 0.2085(9) 0.060(3) Uani 1 1 d . . . H9A H 0.2573 -0.0603 0.1679 0.090 Uiso 1 1 calc R . . H9B H 0.1569 -0.1004 0.1892 0.090 Uiso 1 1 calc R . . H9C H 0.2096 -0.0534 0.2908 0.090 Uiso 1 1 calc R . . C10 C 0.1013(7) 0.2500 0.6266(7) 0.058(4) Uani 1 2 d SD . . C11 C 0.0808(8) 0.2737(8) 0.7494(8) 0.037(4) Uani 0.50 1 d PD . . C12 C 0.1648(10) 0.2500 0.8212(11) 0.052(4) Uani 1 2 d SD . . C13 C -0.0121(9) 0.2500 0.8028(10) 0.055(4) Uani 1 2 d SD . . 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 0.0139(3) 0.0136(3) 0.0307(3) 0.000 -0.00031(14) 0.000 Cl1 0.0153(12) 0.0183(11) 0.0333(12) 0.000 0.0021(9) 0.000 Cl2 0.0268(10) 0.0240(8) 0.0404(8) -0.0045(7) -0.0056(8) -0.0088(7) P1 0.0161(8) 0.0156(8) 0.0348(8) -0.0006(7) -0.0001(7) -0.0022(7) P2 0.0261(15) 0.0317(14) 0.0321(12) 0.000 0.0023(12) 0.000 C1 0.022(5) 0.031(6) 0.039(6) 0.000 -0.008(5) 0.000 C2 0.020(3) 0.024(4) 0.038(3) -0.004(3) -0.006(3) -0.003(3) C3 0.020(4) 0.047(6) 0.050(5) -0.008(4) 0.010(3) -0.017(4) C4 0.042(5) 0.029(4) 0.046(4) 0.008(4) 0.007(4) -0.001(4) C5 0.036(9) 0.037(8) 0.039(7) 0.001(7) -0.007(7) -0.008(7) C5' 0.022(7) 0.025(7) 0.033(7) 0.001(6) 0.013(6) -0.002(6) C6 0.022(4) 0.018(3) 0.041(4) 0.002(3) 0.000(3) -0.004(3) C7 0.028(5) 0.015(3) 0.053(4) -0.006(3) -0.002(3) -0.001(3) C8 0.053(6) 0.052(6) 0.055(5) -0.016(5) -0.002(5) 0.011(5) C9 0.054(6) 0.039(5) 0.086(6) 0.011(5) 0.020(6) 0.020(5) C10 0.028(8) 0.096(14) 0.051(7) 0.000 -0.008(6) 0.000 C11 0.046(9) 0.032(10) 0.034(6) 0.000(6) -0.008(8) -0.009(7) C12 0.057(10) 0.046(8) 0.054(7) 0.000 -0.019(7) 0.000 C13 0.065(10) 0.054(8) 0.048(6) 0.000 0.022(7) 0.000 _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 P2 2.381(3) . ? Re1 P1 2.3891(17) . ? Re1 P1 2.3891(17) 7_565 ? Re1 Cl1 2.411(2) . ? Re1 Cl2 2.4226(16) . ? Re1 Cl2 2.4226(16) 7_565 ? P1 C2 1.817(7) . ? P1 C3 1.821(7) . ? P1 C6 1.847(7) . ? P2 C10 1.823(5) . ? P2 C5' 1.826(5) . ? P2 C5' 1.826(5) 7_565 ? P2 C5 1.840(5) . ? P2 C5 1.840(5) 7_565 ? C1 C2 1.519(8) 7_565 ? C1 C2 1.519(8) . ? C3 C4 1.538(10) . ? C4 C5 1.520(5) . ? C4 C5' 1.535(5) . ? C5' C5' 1.928(18) 7_565 ? C6 C7 1.541(10) . ? C7 C9 1.500(11) . ? C7 C8 1.504(10) . ? C10 C11 1.520(5) . ? C10 C11 1.520(5) 7_565 ? C11 C11 0.76(3) 7_565 ? C11 C12 1.523(5) . ? C11 C13 1.525(5) . ? C12 C11 1.523(5) 7_565 ? C13 C11 1.525(5) 7_565 ? 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 P2 Re1 P1 91.26(6) . . ? P2 Re1 P1 91.26(6) . 7_565 ? P1 Re1 P1 90.33(8) . 7_565 ? P2 Re1 Cl1 178.73(9) . . ? P1 Re1 Cl1 87.84(6) . . ? P1 Re1 Cl1 87.84(6) 7_565 . ? P2 Re1 Cl2 87.33(6) . . ? P1 Re1 Cl2 178.47(6) . . ? P1 Re1 Cl2 89.12(6) 7_565 . ? Cl1 Re1 Cl2 93.56(6) . . ? P2 Re1 Cl2 87.33(6) . 7_565 ? P1 Re1 Cl2 89.12(6) . 7_565 ? P1 Re1 Cl2 178.47(6) 7_565 7_565 ? Cl1 Re1 Cl2 93.56(6) . 7_565 ? Cl2 Re1 Cl2 91.40(8) . 7_565 ? C2 P1 C3 100.7(4) . . ? C2 P1 C6 105.3(3) . . ? C3 P1 C6 101.2(4) . . ? C2 P1 Re1 114.6(2) . . ? C3 P1 Re1 116.4(3) . . ? C6 P1 Re1 116.6(2) . . ? C10 P2 C5' 118.7(5) . . ? C10 P2 C5' 118.7(5) . 7_565 ? C5' P2 C5' 63.7(7) . 7_565 ? C10 P2 C5 91.1(3) . . ? C5' P2 C5 42.8(6) . . ? C5' P2 C5 105.5(5) 7_565 . ? C10 P2 C5 91.1(3) . 7_565 ? C5' P2 C5 105.5(5) . 7_565 ? C5' P2 C5 42.8(6) 7_565 7_565 ? C5 P2 C5 142.8(10) . 7_565 ? C10 P2 Re1 108.2(4) . . ? C5' P2 Re1 121.1(4) . . ? C5' P2 Re1 121.1(4) 7_565 . ? C5 P2 Re1 107.2(5) . . ? C5 P2 Re1 107.2(5) 7_565 . ? C2 C1 C2 116.3(8) 7_565 . ? C1 C2 P1 115.3(6) . . ? C4 C3 P1 118.5(6) . . ? C5 C4 C5' 52.0(7) . . ? C5 C4 C3 123.0(8) . . ? C5' C4 C3 106.2(8) . . ? C4 C5 P2 116.8(6) . . ? C4 C5' P2 116.7(6) . . ? C4 C5' C5' 154.0(6) . 7_565 ? P2 C5' C5' 58.1(3) . 7_565 ? C7 C6 P1 120.0(5) . . ? C9 C7 C8 110.8(8) . . ? C9 C7 C6 109.3(7) . . ? C8 C7 C6 113.5(7) . . ? C11 C10 C11 28.8(10) . 7_565 ? C11 C10 P2 127.1(7) . . ? C11 C10 P2 127.1(7) 7_565 . ? C11 C11 C10 75.6(5) 7_565 . ? C11 C11 C12 75.6(5) 7_565 . ? C10 C11 C12 108.0(8) . . ? C11 C11 C13 75.7(5) 7_565 . ? C10 C11 C13 119.9(10) . . ? C12 C11 C13 114.2(11) . . ? C11 C12 C11 28.7(10) 7_565 . ? C11 C13 C11 28.7(10) 7_565 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.555 _refine_diff_density_min -4.258 _refine_diff_density_rms 0.307 data_s922 _database_code_CSD 187745 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H33 Br Mn O2 P3' _chemical_formula_weight 497.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.962(2) _cell_length_b 15.473(3) _cell_length_c 17.228(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2122.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 24.90 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 2.739 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6385 _exptl_absorpt_correction_T_max 0.7346 _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf Nonius FAST area detector _diffrn_measurement_method 'Darr, Drake, Hursthouse & Malik, 1993)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9181 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.90 _reflns_number_total 3279 _reflns_number_gt 2770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MADNES (Enraf Nonius software, 1989)' _computing_cell_refinement 'REFINE in MADNES' _computing_data_reduction 'ABSMAD (Karaulov, 1991)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The C9 and C9' atoms of the disordered CH2CH2CH2 group are partially occupied, refined with site occupancies 0.70 and 0.30 respectively. The C1, C9 and C9' atoms were refined with ISOR constraint 0.005. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^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 The hydrogen atoms on the C8, C9, C10 atoms were ignored; others included in the riding model _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.478(15) _refine_ls_number_reflns 3279 _refine_ls_number_parameters 230 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.00556(8) 0.47532(4) 0.24895(3) 0.02342(17) Uani 1 1 d . . . Mn1 Mn 0.04839(10) 0.49636(6) 0.10237(4) 0.0107(2) Uani 1 1 d . . . P1 P 0.0928(2) 0.51593(12) -0.02500(8) 0.0198(4) Uani 1 1 d . A . P2 P 0.2470(2) 0.59890(11) 0.13897(7) 0.0137(4) Uani 1 1 d . . . P3 P 0.2393(2) 0.38301(10) 0.11478(8) 0.0151(4) Uani 1 1 d . A . O1 O -0.2067(6) 0.3685(3) 0.0595(2) 0.0218(11) Uani 1 1 d . . . O2 O -0.2088(6) 0.6323(3) 0.1155(2) 0.0226(11) Uani 1 1 d . . . C1 C -0.1106(9) 0.4168(4) 0.0767(3) 0.0164(15) Uani 1 1 d U . . C2 C -0.1070(8) 0.5800(4) 0.1082(3) 0.0165(15) Uani 1 1 d . . . C3 C -0.0960(8) 0.5101(5) -0.0888(3) 0.0390(19) Uani 1 1 d . . . H3A H -0.0596 0.5202 -0.1430 0.047 Uiso 1 1 calc R . . H3B H -0.1413 0.4506 -0.0861 0.047 Uiso 1 1 calc R . . C4 C -0.2369(10) 0.5721(6) -0.0707(4) 0.055(3) Uani 1 1 d . . . H4A H -0.2861 0.5575 -0.0203 0.082 Uiso 1 1 calc R . . H4B H -0.3232 0.5680 -0.1111 0.082 Uiso 1 1 calc R . . H4C H -0.1927 0.6312 -0.0691 0.082 Uiso 1 1 calc R . . C5 C 0.1898(10) 0.6143(5) -0.0628(3) 0.043(2) Uani 1 1 d . . . H5A H 0.2947 0.5980 -0.0899 0.051 Uiso 1 1 calc R . . H5B H 0.1133 0.6397 -0.1019 0.051 Uiso 1 1 calc R . . C6 C 0.2323(10) 0.6847(5) -0.0029(3) 0.042(2) Uani 1 1 d . . . H6A H 0.2822 0.7344 -0.0308 0.051 Uiso 1 1 calc R . . H6B H 0.1262 0.7049 0.0209 0.051 Uiso 1 1 calc R . . C7 C 0.3528(8) 0.6583(4) 0.0626(3) 0.0236(17) Uani 1 1 d . . . H7A H 0.4048 0.7108 0.0849 0.028 Uiso 1 1 calc R . . H7B H 0.4437 0.6220 0.0407 0.028 Uiso 1 1 calc R . . C8 C 0.2198(12) 0.4327(6) -0.0763(3) 0.055(3) Uani 1 1 d . . . C9 C 0.3797(12) 0.4064(6) -0.0379(5) 0.027(2) Uani 0.70 1 d PU A 1 C9' C 0.255(3) 0.3573(14) -0.0486(11) 0.025(5) Uani 0.30 1 d PU A 2 C10 C 0.3531(9) 0.3408(4) 0.0275(3) 0.0262(18) Uani 1 1 d . . . C11 C 0.1584(8) 0.6886(4) 0.1952(3) 0.0212(16) Uani 1 1 d . . . H11A H 0.0880 0.7237 0.1599 0.025 Uiso 1 1 calc R . . H11B H 0.0830 0.6639 0.2352 0.025 Uiso 1 1 calc R . . C12 C 0.2818(9) 0.7493(4) 0.2359(3) 0.0286(18) Uani 1 1 d . . . H12A H 0.3414 0.7177 0.2767 0.043 Uiso 1 1 calc R . . H12B H 0.2201 0.7977 0.2589 0.043 Uiso 1 1 calc R . . H12C H 0.3630 0.7714 0.1980 0.043 Uiso 1 1 calc R . . C13 C 0.4261(8) 0.5656(4) 0.1991(3) 0.0175(15) Uani 1 1 d . . . H13A H 0.5094 0.6130 0.1999 0.021 Uiso 1 1 calc R . . H13B H 0.3865 0.5567 0.2530 0.021 Uiso 1 1 calc R . . C14 C 0.5145(8) 0.4816(4) 0.1709(3) 0.0174(13) Uani 1 1 d . A . H14A H 0.5389 0.4873 0.1148 0.021 Uiso 1 1 calc R . . H14B H 0.6233 0.4761 0.1983 0.021 Uiso 1 1 calc R . . C15 C 0.4159(8) 0.4006(4) 0.1835(3) 0.0214(16) Uani 1 1 d . . . H15A H 0.3702 0.4016 0.2369 0.026 Uiso 1 1 calc R A . H15B H 0.4934 0.3508 0.1798 0.026 Uiso 1 1 calc R . . C16 C 0.1390(9) 0.2835(4) 0.1510(3) 0.0260(17) Uani 1 1 d . . . H16A H 0.0695 0.2990 0.1966 0.031 Uiso 1 1 calc R A . H16B H 0.0618 0.2621 0.1102 0.031 Uiso 1 1 calc R . . C17 C 0.2558(10) 0.2082(4) 0.1748(4) 0.042(2) Uani 1 1 d . A . H17A H 0.3364 0.1969 0.1330 0.063 Uiso 1 1 calc R . . H17B H 0.1885 0.1562 0.1842 0.063 Uiso 1 1 calc R . . H17C H 0.3166 0.2237 0.2222 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0241(3) 0.0303(3) 0.0159(3) 0.0027(3) 0.0028(3) -0.0017(3) Mn1 0.0103(5) 0.0118(5) 0.0101(4) 0.0002(4) -0.0006(3) -0.0001(4) P1 0.0241(10) 0.0243(10) 0.0109(7) 0.0015(7) 0.0012(6) 0.0036(9) P2 0.0135(10) 0.0140(9) 0.0136(8) 0.0000(7) -0.0005(7) -0.0008(8) P3 0.0128(10) 0.0120(9) 0.0205(8) 0.0012(7) 0.0004(7) 0.0007(8) O1 0.023(3) 0.014(3) 0.029(2) -0.007(2) -0.004(2) 0.001(2) O2 0.020(3) 0.022(3) 0.025(2) 0.001(2) -0.004(2) 0.002(2) C1 0.015(3) 0.023(3) 0.011(3) 0.007(2) 0.005(2) 0.015(3) C2 0.020(4) 0.022(4) 0.008(3) 0.001(3) 0.001(3) -0.011(3) C3 0.046(5) 0.055(5) 0.015(3) -0.006(4) -0.010(3) 0.001(5) C4 0.025(5) 0.104(8) 0.035(4) -0.012(4) -0.022(4) 0.016(6) C5 0.038(6) 0.066(7) 0.024(4) 0.015(4) -0.007(3) -0.019(5) C6 0.046(6) 0.037(5) 0.044(4) 0.021(4) 0.011(4) -0.002(5) C7 0.016(4) 0.029(4) 0.025(3) 0.004(3) -0.002(3) -0.006(4) C8 0.073(7) 0.072(7) 0.020(4) -0.002(4) 0.020(4) 0.042(6) C9 0.024(4) 0.033(4) 0.023(4) -0.002(4) 0.005(3) 0.008(4) C9' 0.029(7) 0.023(7) 0.023(6) -0.005(5) 0.001(5) 0.006(5) C10 0.035(5) 0.030(4) 0.014(3) -0.002(3) 0.008(3) 0.009(4) C11 0.023(4) 0.013(4) 0.028(4) -0.009(3) -0.002(3) -0.003(3) C12 0.028(5) 0.022(4) 0.035(4) -0.015(3) -0.002(3) -0.002(3) C13 0.020(4) 0.017(4) 0.016(3) 0.000(3) 0.003(3) -0.005(3) C14 0.013(3) 0.022(4) 0.017(3) 0.006(3) -0.008(2) -0.004(4) C15 0.018(4) 0.021(4) 0.025(3) 0.004(3) -0.006(3) 0.009(3) C16 0.025(4) 0.011(4) 0.042(4) 0.001(3) 0.000(3) 0.001(4) C17 0.022(5) 0.016(4) 0.089(5) 0.022(4) 0.006(4) -0.001(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 Br1 Mn1 2.5689(9) . ? Mn1 C2 1.793(7) . ? Mn1 C1 1.821(8) . ? Mn1 P1 2.2431(15) . ? Mn1 P2 2.3272(19) . ? Mn1 P3 2.3308(19) . ? P1 C5 1.827(7) . ? P1 C8 1.861(8) . ? P1 C3 1.865(6) . ? P2 C7 1.813(6) . ? P2 C11 1.834(6) . ? P2 C13 1.836(6) . ? P3 C16 1.843(7) . ? P3 C15 1.858(6) . ? P3 C10 1.874(6) . ? O1 C1 1.109(7) . ? O2 C2 1.152(7) . ? C3 C4 1.509(10) . ? C5 C6 1.538(9) . ? C6 C7 1.536(8) . ? C8 C9' 1.29(2) . ? C8 C9 1.491(12) . ? C9 C10 1.532(11) . ? C9' C10 1.55(2) . ? C11 C12 1.529(8) . ? C13 C14 1.556(8) . ? C14 C15 1.494(8) . ? C16 C17 1.547(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mn1 C1 91.2(3) . . ? C2 Mn1 P1 93.79(18) . . ? C1 Mn1 P1 87.87(16) . . ? C2 Mn1 P2 87.8(2) . . ? C1 Mn1 P2 178.15(18) . . ? P1 Mn1 P2 93.78(6) . . ? C2 Mn1 P3 171.08(18) . . ? C1 Mn1 P3 88.1(2) . . ? P1 Mn1 P3 95.08(6) . . ? P2 Mn1 P3 92.57(7) . . ? C2 Mn1 Br1 86.84(17) . . ? C1 Mn1 Br1 93.51(16) . . ? P1 Mn1 Br1 178.47(6) . . ? P2 Mn1 Br1 84.85(4) . . ? P3 Mn1 Br1 84.32(4) . . ? C5 P1 C8 100.3(4) . . ? C5 P1 C3 99.9(3) . . ? C8 P1 C3 97.1(3) . . ? C5 P1 Mn1 121.8(2) . . ? C8 P1 Mn1 117.2(2) . . ? C3 P1 Mn1 116.3(2) . . ? C7 P2 C11 100.3(3) . . ? C7 P2 C13 101.0(3) . . ? C11 P2 C13 102.3(3) . . ? C7 P2 Mn1 117.7(2) . . ? C11 P2 Mn1 113.4(2) . . ? C13 P2 Mn1 119.3(2) . . ? C16 P3 C15 103.6(3) . . ? C16 P3 C10 100.9(3) . . ? C15 P3 C10 101.3(3) . . ? C16 P3 Mn1 112.1(2) . . ? C15 P3 Mn1 116.2(2) . . ? C10 P3 Mn1 120.3(2) . . ? O1 C1 Mn1 178.7(5) . . ? O2 C2 Mn1 176.6(5) . . ? C4 C3 P1 116.5(5) . . ? C6 C5 P1 116.4(4) . . ? C7 C6 C5 116.2(6) . . ? C6 C7 P2 112.2(5) . . ? C9' C8 C9 53.4(12) . . ? C9' C8 P1 124.7(10) . . ? C9 C8 P1 116.2(6) . . ? C8 C9 C10 112.9(8) . . ? C8 C9' C10 124.9(17) . . ? C9 C10 C9' 48.4(9) . . ? C9 C10 P3 115.2(5) . . ? C9' C10 P3 112.3(9) . . ? C12 C11 P2 117.3(5) . . ? C14 C13 P2 114.2(4) . . ? C15 C14 C13 114.6(5) . . ? C14 C15 P3 115.4(4) . . ? C17 C16 P3 117.3(5) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 24.90 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.409 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.103