# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Malgorzata Holynska' _publ_contact_author_email HOLYNSKA@ETO.WCHUWR.PL _publ_section_title ; Remarkably stable dinuclear, diamagnetic rhenium(VI) salts with the [ReOCl4OReOCl4]2- anion ; loop_ _publ_author_name 'Malgorzata Holynska' 'Tadeusz Lis' # Attachment 'A.cif' data_kma1hol _database_code_depnum_ccdc_archive 'CCDC 714378' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H34 P2, Cl8 O3 Re2, 4(C H Cl3)' _chemical_formula_sum 'C42 H38 Cl20 O3 P2 Re2' _chemical_formula_weight 1734.06 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.424(4) _cell_length_b 11.516(5) _cell_length_c 12.632(5) _cell_angle_alpha 77.79(4) _cell_angle_beta 89.12(4) _cell_angle_gamma 65.00(4) _cell_volume 1466.9(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15560 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 36.82 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 5.125 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.449 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 2006)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KM4CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18674 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.1343 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 36.82 _reflns_number_total 9318 _reflns_number_gt 6289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.0 (Brandenburg & Putz, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0020P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9318 _refine_ls_number_parameters 349 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.004 _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 P1 P 0.08646(12) 0.11110(13) 0.57169(11) 0.0123(3) Uani 1 1 d . . . C1 C -0.0184(5) 0.0342(5) 0.5488(4) 0.0157(12) Uani 1 1 d . . . H1A H -0.0129 -0.0319 0.6154 0.019 Uiso 1 1 calc R . . H1B H -0.1092 0.1020 0.5348 0.019 Uiso 1 1 calc R . . C11 C 0.0798(4) 0.2270(5) 0.4509(4) 0.0131(11) Uani 1 1 d . . . C21 C 0.0038(5) 0.3624(5) 0.4378(4) 0.0166(12) Uani 1 1 d . . . H21 H -0.0444 0.3960 0.4951 0.020 Uiso 1 1 calc R . . C31 C -0.0002(5) 0.4465(5) 0.3405(4) 0.0189(12) Uani 1 1 d . . . H31 H -0.0513 0.5384 0.3315 0.023 Uiso 1 1 calc R . . C41 C 0.0687(5) 0.3996(5) 0.2563(4) 0.0189(12) Uani 1 1 d . . . H41 H 0.0643 0.4584 0.1896 0.023 Uiso 1 1 calc R . . C51 C 0.1448(5) 0.2648(5) 0.2700(4) 0.0171(12) Uani 1 1 d . . . H51 H 0.1929 0.2322 0.2124 0.021 Uiso 1 1 calc R . . C61 C 0.1513(5) 0.1785(5) 0.3658(4) 0.0135(11) Uani 1 1 d . . . H61 H 0.2036 0.0869 0.3744 0.016 Uiso 1 1 calc R . . C12 C 0.0309(5) 0.1832(5) 0.6847(4) 0.0140(11) Uani 1 1 d . . . C22 C 0.1175(5) 0.1479(5) 0.7758(4) 0.0175(12) Uani 1 1 d . . . H22 H 0.2058 0.0888 0.7754 0.021 Uiso 1 1 calc R . . C32 C 0.0749(5) 0.1984(5) 0.8655(4) 0.0208(12) Uani 1 1 d . . . H32 H 0.1341 0.1727 0.9273 0.025 Uiso 1 1 calc R . . C42 C -0.0527(5) 0.2861(5) 0.8674(5) 0.0216(13) Uani 1 1 d . . . H42 H -0.0816 0.3202 0.9300 0.026 Uiso 1 1 calc R . . C52 C -0.1386(5) 0.3238(5) 0.7754(5) 0.0212(13) Uani 1 1 d . . . H52 H -0.2259 0.3858 0.7755 0.025 Uiso 1 1 calc R . . C62 C -0.0995(5) 0.2734(5) 0.6854(4) 0.0164(12) Uani 1 1 d . . . H62 H -0.1594 0.2987 0.6243 0.020 Uiso 1 1 calc R . . C13 C 0.2490(4) -0.0078(5) 0.6060(4) 0.0120(11) Uani 1 1 d . . . C23 C 0.2779(5) -0.1370(5) 0.6616(4) 0.0179(12) Uani 1 1 d . . . H23 H 0.2112 -0.1660 0.6708 0.022 Uiso 1 1 calc R . . C33 C 0.4032(5) -0.2218(5) 0.7030(5) 0.0228(13) Uani 1 1 d . . . H33 H 0.4236 -0.3104 0.7381 0.027 Uiso 1 1 calc R . . C43 C 0.4991(5) -0.1776(5) 0.6932(5) 0.0240(13) Uani 1 1 d . . . H43 H 0.5845 -0.2350 0.7246 0.029 Uiso 1 1 calc R . . C53 C 0.4716(5) -0.0504(5) 0.6381(4) 0.0180(12) Uani 1 1 d . . . H53 H 0.5387 -0.0219 0.6297 0.022 Uiso 1 1 calc R . . C63 C 0.3483(5) 0.0340(5) 0.5959(4) 0.0171(12) Uani 1 1 d . . . H63 H 0.3295 0.1218 0.5593 0.021 Uiso 1 1 calc R . . Re1 Re 0.41120(2) 0.42906(2) 0.59613(2) 0.01342(6) Uani 1 1 d . . . Cl21 Cl 0.33452(13) 0.29820(13) 0.71685(11) 0.0206(3) Uani 1 1 d . . . Cl11 Cl 0.60002(12) 0.22142(12) 0.59111(11) 0.0183(3) Uani 1 1 d . . . Cl31 Cl 0.52918(12) 0.42447(12) 0.74989(11) 0.0178(3) Uani 1 1 d . . . Cl41 Cl 0.31022(12) 0.39215(13) 0.45634(11) 0.0189(3) Uani 1 1 d . . . O1 O 0.5000 0.5000 0.5000 0.0147(11) Uani 1 2 d S . . O21 O 0.2884(3) 0.5727(3) 0.6044(3) 0.0188(8) Uani 1 1 d . . . C3 C 0.2912(5) 0.4600(5) 0.9404(4) 0.0237(13) Uani 1 1 d D . . H3 H 0.3543 0.4059 0.8948 0.028 Uiso 1 1 calc R . . Cl13 Cl 0.21380(16) 0.62263(16) 0.86650(13) 0.0393(4) Uani 1 1 d D . . Cl23 Cl 0.17651(16) 0.39707(16) 0.97525(13) 0.0393(4) Uani 1 1 d D . . Cl33 Cl 0.37537(15) 0.45213(18) 1.05958(13) 0.0446(5) Uani 1 1 d D . . C115 C 0.6671(15) 0.0877(15) 0.8775(12) 0.038(5) Uani 0.50 1 d PD A 1 H11 H 0.6184 0.1611 0.8138 0.046 Uiso 0.50 1 calc PR A 1 Cl15 Cl 0.6446(7) 0.1497(7) 0.9946(6) 0.069(2) Uani 0.50 1 d PD A 1 Cl25 Cl 0.8314(7) 0.0135(14) 0.8526(11) 0.054(3) Uani 0.50 1 d PD A 1 Cl35 Cl 0.6046(13) -0.0325(12) 0.8929(12) 0.050(2) Uani 0.50 1 d PD A 1 C151 C 0.7148(15) 0.0884(18) 0.8758(15) 0.032(5) Uani 0.50 1 d PD B 2 H111 H 0.6768 0.1613 0.8096 0.039 Uiso 0.50 1 calc PR B 2 Cl51 Cl 0.7038(7) 0.1575(7) 0.9879(6) 0.0461(15) Uani 0.50 1 d PD B 2 Cl52 Cl 0.8786(8) -0.0069(12) 0.8588(10) 0.0352(16) Uani 0.50 1 d PD B 2 Cl53 Cl 0.6282(12) -0.0096(11) 0.8890(12) 0.0428(17) Uani 0.50 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0124(7) 0.0116(7) 0.0146(7) -0.0037(6) 0.0013(6) -0.0065(6) C1 0.017(3) 0.015(3) 0.019(3) -0.006(3) 0.006(2) -0.009(2) C11 0.012(2) 0.018(3) 0.013(3) -0.004(2) 0.000(2) -0.010(2) C21 0.013(3) 0.015(3) 0.020(3) -0.003(3) 0.001(2) -0.005(2) C31 0.019(3) 0.010(3) 0.027(3) -0.003(3) -0.003(3) -0.006(2) C41 0.018(3) 0.025(3) 0.018(3) -0.004(3) 0.003(2) -0.014(3) C51 0.016(3) 0.014(3) 0.024(3) -0.005(3) 0.002(2) -0.009(2) C61 0.018(3) 0.003(3) 0.017(3) 0.004(2) -0.006(2) -0.005(2) C12 0.021(3) 0.014(3) 0.011(3) -0.002(2) 0.000(2) -0.012(2) C22 0.017(3) 0.013(3) 0.021(3) -0.009(3) 0.006(2) -0.004(2) C32 0.033(3) 0.022(3) 0.012(3) -0.008(3) 0.003(3) -0.014(3) C42 0.026(3) 0.017(3) 0.027(3) -0.009(3) 0.011(3) -0.011(3) C52 0.016(3) 0.015(3) 0.027(3) -0.004(3) 0.000(3) -0.002(2) C62 0.014(3) 0.018(3) 0.020(3) -0.009(3) 0.002(2) -0.007(2) C13 0.015(3) 0.011(3) 0.012(3) -0.002(2) 0.001(2) -0.008(2) C23 0.014(3) 0.012(3) 0.025(3) 0.003(3) -0.002(2) -0.006(2) C33 0.024(3) 0.007(3) 0.032(4) -0.005(3) 0.002(3) 0.000(2) C43 0.011(3) 0.027(4) 0.030(3) -0.011(3) 0.001(3) -0.002(2) C53 0.013(3) 0.023(3) 0.021(3) -0.006(3) 0.007(2) -0.010(2) C63 0.018(3) 0.017(3) 0.016(3) -0.003(3) 0.001(2) -0.008(2) Re1 0.01275(10) 0.01207(11) 0.01676(11) -0.00265(9) 0.00155(8) -0.00687(8) Cl21 0.0243(7) 0.0188(8) 0.0232(7) -0.0049(6) 0.0067(6) -0.0138(6) Cl11 0.0171(6) 0.0143(7) 0.0209(7) -0.0043(6) 0.0020(6) -0.0042(6) Cl31 0.0183(7) 0.0163(7) 0.0191(7) -0.0041(6) -0.0016(6) -0.0076(6) Cl41 0.0184(7) 0.0187(7) 0.0207(7) -0.0032(6) -0.0029(6) -0.0094(6) O1 0.017(3) 0.019(3) 0.014(3) -0.003(2) 0.001(2) -0.013(2) O21 0.0095(17) 0.016(2) 0.031(2) -0.0090(18) -0.0018(17) -0.0042(15) C3 0.024(3) 0.027(4) 0.021(3) -0.012(3) 0.007(3) -0.010(3) Cl13 0.0505(10) 0.0300(10) 0.0331(9) -0.0023(8) 0.0110(8) -0.0157(8) Cl23 0.0523(10) 0.0493(11) 0.0326(9) -0.0072(9) 0.0067(8) -0.0382(9) Cl33 0.0355(10) 0.0665(13) 0.0360(10) -0.0191(10) -0.0031(8) -0.0221(9) C115 0.071(14) 0.018(9) 0.010(7) -0.003(7) -0.001(8) -0.004(9) Cl15 0.135(7) 0.028(3) 0.028(3) -0.009(2) -0.016(4) -0.017(4) Cl25 0.084(7) 0.053(6) 0.036(3) 0.004(3) -0.009(6) -0.045(6) Cl35 0.060(6) 0.037(4) 0.050(3) -0.015(3) 0.008(4) -0.017(3) C151 0.029(10) 0.028(9) 0.045(11) -0.017(8) 0.019(8) -0.013(8) Cl51 0.084(4) 0.032(3) 0.027(2) -0.0123(19) 0.008(3) -0.026(3) Cl52 0.053(4) 0.033(3) 0.028(3) -0.004(3) 0.006(4) -0.027(4) Cl53 0.037(3) 0.030(4) 0.057(3) -0.004(3) -0.003(3) -0.012(2) _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 P1 C13 1.771(5) . ? P1 C12 1.777(5) . ? P1 C11 1.781(5) . ? P1 C1 1.822(5) . ? C1 C1 1.560(9) 2_556 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C11 C21 1.401(7) . ? C11 C61 1.405(7) . ? C21 C31 1.383(7) . ? C21 H21 0.9500 . ? C31 C41 1.379(7) . ? C31 H31 0.9500 . ? C41 C51 1.394(7) . ? C41 H41 0.9500 . ? C51 C61 1.375(7) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C12 C22 1.401(7) . ? C12 C62 1.413(7) . ? C22 C32 1.372(7) . ? C22 H22 0.9500 . ? C32 C42 1.382(7) . ? C32 H32 0.9500 . ? C42 C52 1.401(7) . ? C42 H42 0.9500 . ? C52 C62 1.368(7) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C13 C63 1.402(6) . ? C13 C23 1.402(6) . ? C23 C33 1.379(7) . ? C23 H23 0.9500 . ? C33 C43 1.385(7) . ? C33 H33 0.9500 . ? C43 C53 1.383(7) . ? C43 H43 0.9500 . ? C53 C63 1.364(7) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? Re1 O21 1.680(3) . ? Re1 O1 1.8477(8) . ? Re1 Cl41 2.3289(15) . ? Re1 Cl21 2.3381(16) . ? Re1 Cl31 2.3599(16) . ? Re1 Cl11 2.465(2) . ? O1 Re1 1.8477(8) 2_666 ? C3 Cl13 1.746(5) . ? C3 Cl23 1.756(5) . ? C3 Cl33 1.764(5) . ? C3 H3 1.0000 . ? C115 Cl15 1.745(11) . ? C115 Cl25 1.758(13) . ? C115 Cl35 1.783(12) . ? C115 H11 1.0000 . ? C151 Cl51 1.744(12) . ? C151 Cl52 1.761(13) . ? C151 Cl53 1.772(13) . ? C151 H111 1.0000 . ? 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 C13 P1 C12 108.1(2) . . ? C13 P1 C11 108.8(2) . . ? C12 P1 C11 113.4(2) . . ? C13 P1 C1 111.0(2) . . ? C12 P1 C1 106.4(2) . . ? C11 P1 C1 109.2(2) . . ? C1 C1 P1 112.6(4) 2_556 . ? C1 C1 H1A 109.1 2_556 . ? P1 C1 H1A 109.1 . . ? C1 C1 H1B 109.1 2_556 . ? P1 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C21 C11 C61 119.9(5) . . ? C21 C11 P1 122.2(4) . . ? C61 C11 P1 117.9(4) . . ? C31 C21 C11 119.1(5) . . ? C31 C21 H21 120.4 . . ? C11 C21 H21 120.4 . . ? C41 C31 C21 121.3(5) . . ? C41 C31 H31 119.4 . . ? C21 C31 H31 119.4 . . ? C31 C41 C51 119.3(5) . . ? C31 C41 H41 120.4 . . ? C51 C41 H41 120.4 . . ? C61 C51 C41 121.0(5) . . ? C61 C51 H51 119.5 . . ? C41 C51 H51 119.5 . . ? C51 C61 C11 119.4(5) . . ? C51 C61 H61 120.3 . . ? C11 C61 H61 120.3 . . ? C22 C12 C62 119.3(5) . . ? C22 C12 P1 119.4(4) . . ? C62 C12 P1 121.2(4) . . ? C32 C22 C12 120.2(5) . . ? C32 C22 H22 119.9 . . ? C12 C22 H22 119.9 . . ? C22 C32 C42 121.0(5) . . ? C22 C32 H32 119.5 . . ? C42 C32 H32 119.5 . . ? C32 C42 C52 118.9(5) . . ? C32 C42 H42 120.6 . . ? C52 C42 H42 120.6 . . ? C62 C52 C42 121.4(5) . . ? C62 C52 H52 119.3 . . ? C42 C52 H52 119.3 . . ? C52 C62 C12 119.2(5) . . ? C52 C62 H62 120.4 . . ? C12 C62 H62 120.4 . . ? C63 C13 C23 119.1(4) . . ? C63 C13 P1 118.8(4) . . ? C23 C13 P1 121.0(3) . . ? C33 C23 C13 120.0(5) . . ? C33 C23 H23 120.0 . . ? C13 C23 H23 120.0 . . ? C23 C33 C43 119.8(5) . . ? C23 C33 H33 120.1 . . ? C43 C33 H33 120.1 . . ? C53 C43 C33 120.6(5) . . ? C53 C43 H43 119.7 . . ? C33 C43 H43 119.7 . . ? C63 C53 C43 120.1(5) . . ? C63 C53 H53 120.0 . . ? C43 C53 H53 120.0 . . ? C53 C63 C13 120.4(5) . . ? C53 C63 H63 119.8 . . ? C13 C63 H63 119.8 . . ? O21 Re1 O1 96.50(13) . . ? O21 Re1 Cl41 96.08(12) . . ? O1 Re1 Cl41 92.07(5) . . ? O21 Re1 Cl21 95.25(13) . . ? O1 Re1 Cl21 168.24(4) . . ? Cl41 Re1 Cl21 87.13(6) . . ? O21 Re1 Cl31 92.36(13) . . ? O1 Re1 Cl31 93.12(5) . . ? Cl41 Re1 Cl31 169.52(5) . . ? Cl21 Re1 Cl31 85.93(6) . . ? O21 Re1 Cl11 176.42(11) . . ? O1 Re1 Cl11 82.51(5) . . ? Cl41 Re1 Cl11 87.41(6) . . ? Cl21 Re1 Cl11 85.73(6) . . ? Cl31 Re1 Cl11 84.26(6) . . ? Re1 O1 Re1 180.000(1) . 2_666 ? Cl13 C3 Cl23 109.9(3) . . ? Cl13 C3 Cl33 110.0(3) . . ? Cl23 C3 Cl33 109.6(3) . . ? Cl13 C3 H3 109.1 . . ? Cl23 C3 H3 109.1 . . ? Cl33 C3 H3 109.1 . . ? Cl15 C115 Cl25 112.4(10) . . ? Cl15 C115 Cl35 108.8(9) . . ? Cl25 C115 Cl35 108.5(9) . . ? Cl15 C115 H11 109.0 . . ? Cl25 C115 H11 109.0 . . ? Cl35 C115 H11 109.0 . . ? Cl51 C151 Cl52 110.0(10) . . ? Cl51 C151 Cl53 111.7(10) . . ? Cl52 C151 Cl53 109.9(10) . . ? Cl51 C151 H111 108.4 . . ? Cl52 C151 H111 108.4 . . ? Cl53 C151 H111 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 P1 C1 C1 -62.6(6) . . . 2_556 ? C12 P1 C1 C1 -180.0(5) . . . 2_556 ? C11 P1 C1 C1 57.3(6) . . . 2_556 ? C13 P1 C11 C21 -138.4(4) . . . . ? C12 P1 C11 C21 -18.0(4) . . . . ? C1 P1 C11 C21 100.4(4) . . . . ? C13 P1 C11 C61 43.3(4) . . . . ? C12 P1 C11 C61 163.7(3) . . . . ? C1 P1 C11 C61 -77.9(4) . . . . ? C61 C11 C21 C31 0.4(6) . . . . ? P1 C11 C21 C31 -177.9(3) . . . . ? C11 C21 C31 C41 0.3(7) . . . . ? C21 C31 C41 C51 -0.7(7) . . . . ? C31 C41 C51 C61 0.5(7) . . . . ? C41 C51 C61 C11 0.1(7) . . . . ? C21 C11 C61 C51 -0.6(6) . . . . ? P1 C11 C61 C51 177.8(3) . . . . ? C13 P1 C12 C22 4.5(4) . . . . ? C11 P1 C12 C22 -116.3(4) . . . . ? C1 P1 C12 C22 123.7(4) . . . . ? C13 P1 C12 C62 -174.2(4) . . . . ? C11 P1 C12 C62 65.1(5) . . . . ? C1 P1 C12 C62 -55.0(5) . . . . ? C62 C12 C22 C32 1.4(7) . . . . ? P1 C12 C22 C32 -177.3(4) . . . . ? C12 C22 C32 C42 -1.0(8) . . . . ? C22 C32 C42 C52 -0.4(8) . . . . ? C32 C42 C52 C62 1.6(8) . . . . ? C42 C52 C62 C12 -1.2(8) . . . . ? C22 C12 C62 C52 -0.3(7) . . . . ? P1 C12 C62 C52 178.4(4) . . . . ? C12 P1 C13 C63 -82.0(4) . . . . ? C11 P1 C13 C63 41.6(4) . . . . ? C1 P1 C13 C63 161.7(4) . . . . ? C12 P1 C13 C23 85.9(4) . . . . ? C11 P1 C13 C23 -150.5(4) . . . . ? C1 P1 C13 C23 -30.4(5) . . . . ? C63 C13 C23 C33 -1.6(8) . . . . ? P1 C13 C23 C33 -169.5(4) . . . . ? C13 C23 C33 C43 2.5(8) . . . . ? C23 C33 C43 C53 -2.8(8) . . . . ? C33 C43 C53 C63 2.2(8) . . . . ? C43 C53 C63 C13 -1.2(8) . . . . ? C23 C13 C63 C53 1.0(7) . . . . ? P1 C13 C63 C53 169.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C115 H11 Cl11 1.00 2.74 3.58(2) 141 . C151 H111 Cl11 1.00 2.76 3.62(2) 145 . C52 H52 Cl31 0.95 2.65 3.466(6) 144 1_455 C3 H3 Cl31 1.00 2.73 3.554(6) 140 . C115 H11 Cl31 1.00 2.70 3.52(2) 140 . C33 H33 Cl31 0.95 2.74 3.614(6) 154 1_545 _diffrn_measured_fraction_theta_max 0.632 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.28 _refine_diff_density_min -1.38 _refine_diff_density_rms 0.22 # Attachment 'B.cif' data_kmcvabs _database_code_depnum_ccdc_archive 'CCDC 714379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C19 H18 P), Cl8 O3 Re2' _chemical_formula_sum 'C38 H36 Cl8 O3 P2 Re2' _chemical_formula_weight 1258.61 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.379(4) _cell_length_b 13.823(4) _cell_length_c 12.629(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.19(3) _cell_angle_gamma 90.00 _cell_volume 2160.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 13853 _cell_measurement_theta_min 2 _cell_measurement_theta_max 35 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 6.202 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.405 _exptl_absorpt_correction_T_max 0.709 _exptl_absorpt_process_details ; 'Oxford Diffraction, 2006' ; _diffrn_ambient_temperature 230(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 KM4CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13779 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.1424 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 28.51 _reflns_number_total 5050 _reflns_number_gt 2590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.0 (Brandenburg & Putz, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0050P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5050 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0618 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.58232(2) 0.91876(2) 0.58518(2) 0.03757(10) Uani 1 1 d . . . O1 O 0.5000 1.0000 0.5000 0.0342(17) Uani 1 2 d S . . O21 O 0.5276(4) 0.8149(4) 0.5450(4) 0.0571(15) Uani 1 1 d . . . Cl21 Cl 0.69963(15) 0.84466(16) 0.70634(16) 0.0663(7) Uani 1 1 d . . . Cl11 Cl 0.65764(13) 1.07124(14) 0.64977(13) 0.0467(5) Uani 1 1 d . . . Cl31 Cl 0.46070(14) 0.93362(15) 0.72496(14) 0.0552(6) Uani 1 1 d . . . Cl41 Cl 0.72424(14) 0.91771(17) 0.46459(15) 0.0603(6) Uani 1 1 d . . . P P 0.57218(15) 0.64170(16) 0.30226(16) 0.0414(6) Uani 1 1 d . . . C1 C 0.4463(5) 0.6879(5) 0.3444(5) 0.058(2) Uani 1 1 d . . . H1A H 0.4186 0.6470 0.4001 0.086 Uiso 1 1 calc R . . H1B H 0.3953 0.6888 0.2850 0.086 Uiso 1 1 calc R . . H1C H 0.4562 0.7531 0.3712 0.086 Uiso 1 1 calc R . . C11 C 0.6212(5) 0.7193(6) 0.1989(5) 0.040(2) Uani 1 1 d . . . C21 C 0.5929(5) 0.8158(6) 0.1950(6) 0.041(2) Uani 1 1 d . . . H21 H 0.5520 0.8436 0.2490 0.049 Uiso 1 1 calc R . . C31 C 0.6252(6) 0.8697(6) 0.1120(6) 0.058(2) Uani 1 1 d . . . H31 H 0.6032 0.9347 0.1079 0.069 Uiso 1 1 calc R . . C41 C 0.6889(7) 0.8332(7) 0.0332(7) 0.070(3) Uani 1 1 d . . . H41 H 0.7100 0.8722 -0.0237 0.083 Uiso 1 1 calc R . . C51 C 0.7210(6) 0.7375(7) 0.0403(6) 0.062(3) Uani 1 1 d . . . H51 H 0.7672 0.7126 -0.0111 0.074 Uiso 1 1 calc R . . C61 C 0.6875(5) 0.6777(6) 0.1203(6) 0.045(2) Uani 1 1 d . . . H61 H 0.7076 0.6121 0.1229 0.053 Uiso 1 1 calc R . . C12 C 0.5482(6) 0.5238(6) 0.2489(6) 0.041(2) Uani 1 1 d . . . C22 C 0.5962(6) 0.4404(6) 0.2948(6) 0.056(2) Uani 1 1 d . . . H22 H 0.6464 0.4467 0.3512 0.067 Uiso 1 1 calc R . . C32 C 0.5695(6) 0.3499(6) 0.2569(7) 0.056(2) Uani 1 1 d . . . H32 H 0.6025 0.2942 0.2856 0.068 Uiso 1 1 calc R . . C42 C 0.4925(7) 0.3425(7) 0.1752(7) 0.063(3) Uani 1 1 d . . . H42 H 0.4706 0.2810 0.1514 0.075 Uiso 1 1 calc R . . C52 C 0.4487(6) 0.4223(8) 0.1294(6) 0.060(2) Uani 1 1 d . . . H52 H 0.4001 0.4151 0.0717 0.072 Uiso 1 1 calc R . . C62 C 0.4739(6) 0.5143(6) 0.1659(6) 0.050(2) Uani 1 1 d . . . H62 H 0.4414 0.5692 0.1350 0.059 Uiso 1 1 calc R . . C13 C 0.6656(5) 0.6321(5) 0.4121(5) 0.038(2) Uani 1 1 d . . . C23 C 0.7733(6) 0.6559(5) 0.3998(6) 0.045(2) Uani 1 1 d . . . H23 H 0.7968 0.6801 0.3347 0.054 Uiso 1 1 calc R . . C33 C 0.8456(6) 0.6441(6) 0.4825(6) 0.064(3) Uani 1 1 d . . . H33 H 0.9181 0.6615 0.4729 0.077 Uiso 1 1 calc R . . C43 C 0.8166(7) 0.6086(6) 0.5761(6) 0.061(3) Uani 1 1 d . . . H43 H 0.8678 0.5981 0.6310 0.073 Uiso 1 1 calc R . . C53 C 0.7057(7) 0.5876(6) 0.5894(6) 0.070(2) Uani 1 1 d . . . H53 H 0.6823 0.5640 0.6549 0.084 Uiso 1 1 calc R . . C63 C 0.6319(6) 0.6011(6) 0.5080(6) 0.065(3) Uani 1 1 d . . . H63 H 0.5582 0.5890 0.5187 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.03554(16) 0.0456(2) 0.03121(15) -0.0030(2) -0.00857(11) -0.0011(2) O1 0.029(4) 0.044(5) 0.030(4) -0.010(3) -0.004(3) 0.022(3) O21 0.060(3) 0.055(4) 0.056(4) -0.010(3) -0.014(3) 0.001(3) Cl21 0.0555(14) 0.0814(18) 0.0609(15) 0.0182(13) -0.0254(11) 0.0062(12) Cl11 0.0504(11) 0.0502(13) 0.0393(10) -0.0071(11) -0.0049(8) -0.0124(11) Cl31 0.0566(12) 0.0656(17) 0.0440(12) 0.0052(12) 0.0126(9) -0.0102(11) Cl41 0.0524(12) 0.0754(16) 0.0537(13) -0.0062(14) 0.0131(10) 0.0098(13) P 0.0333(12) 0.0532(16) 0.0379(13) -0.0108(11) 0.0053(10) 0.0041(10) C1 0.040(5) 0.079(7) 0.055(5) -0.023(5) 0.008(4) 0.002(4) C11 0.032(4) 0.060(6) 0.028(4) 0.001(4) -0.011(3) 0.000(4) C21 0.051(5) 0.039(6) 0.033(5) 0.003(4) 0.009(4) 0.004(4) C31 0.045(5) 0.063(7) 0.065(6) -0.006(5) 0.006(5) 0.003(4) C41 0.080(7) 0.052(7) 0.078(7) -0.014(6) 0.034(6) -0.031(5) C51 0.052(5) 0.083(8) 0.051(6) -0.042(6) 0.016(4) -0.029(5) C61 0.048(5) 0.047(6) 0.039(5) -0.009(4) 0.006(4) -0.008(4) C12 0.034(4) 0.051(6) 0.039(5) -0.013(5) 0.015(4) -0.003(4) C22 0.043(5) 0.059(8) 0.064(6) -0.004(5) -0.007(4) 0.012(5) C32 0.065(6) 0.038(6) 0.066(7) 0.003(5) 0.006(5) 0.002(5) C42 0.077(7) 0.048(7) 0.064(7) -0.014(5) 0.003(5) -0.010(5) C52 0.053(5) 0.057(7) 0.069(6) -0.022(6) 0.011(4) -0.024(6) C62 0.042(5) 0.058(7) 0.048(5) -0.010(5) -0.001(4) -0.007(4) C13 0.020(4) 0.063(6) 0.031(4) -0.012(4) 0.003(3) -0.008(3) C23 0.045(5) 0.052(6) 0.038(5) 0.000(4) 0.004(4) 0.005(4) C33 0.034(5) 0.104(8) 0.054(6) 0.010(6) -0.009(5) -0.009(5) C43 0.070(6) 0.087(8) 0.027(5) 0.011(5) 0.013(4) 0.010(5) C53 0.066(6) 0.106(8) 0.039(5) -0.001(6) 0.012(4) 0.002(6) C63 0.050(5) 0.109(8) 0.037(5) 0.000(5) 0.012(4) -0.017(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 O21 1.662(5) . ? Re1 O1 1.8470(5) . ? Re1 Cl21 2.3253(19) . ? Re1 Cl41 2.349(2) . ? Re1 Cl31 2.3528(19) . ? Re1 Cl11 2.4384(19) . ? O1 Re1 1.8469(5) 3_676 ? P C1 1.776(6) . ? P C12 1.786(7) . ? P C13 1.793(7) . ? P C11 1.804(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C11 C21 1.380(9) . ? C11 C61 1.423(9) . ? C21 C31 1.353(9) . ? C21 H21 0.9400 . ? C31 C41 1.378(9) . ? C31 H31 0.9400 . ? C41 C51 1.383(10) . ? C41 H41 0.9400 . ? C51 C61 1.376(9) . ? C51 H51 0.9400 . ? C61 H61 0.9400 . ? C12 C62 1.386(9) . ? C12 C22 1.416(9) . ? C22 C32 1.377(10) . ? C22 H22 0.9400 . ? C32 C42 1.394(10) . ? C32 H32 0.9400 . ? C42 C52 1.353(10) . ? C42 H42 0.9400 . ? C52 C62 1.387(9) . ? C52 H52 0.9400 . ? C62 H62 0.9400 . ? C13 C63 1.358(9) . ? C13 C23 1.385(8) . ? C23 C33 1.371(8) . ? C23 H23 0.9400 . ? C33 C43 1.336(9) . ? C33 H33 0.9400 . ? C43 C53 1.417(9) . ? C43 H43 0.9400 . ? C53 C63 1.374(9) . ? C53 H53 0.9400 . ? C63 H63 0.9400 . ? 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 O21 Re1 O1 97.54(16) . . yes O21 Re1 Cl41 95.88(17) . . yes O1 Re1 Cl41 92.13(6) . . yes O21 Re1 Cl21 93.73(17) . . yes O1 Re1 Cl21 168.69(6) . . yes Cl21 Re1 Cl41 87.63(7) . . yes O21 Re1 Cl31 92.36(17) . . yes O1 Re1 Cl31 91.72(5) . . yes Cl41 Re1 Cl31 170.37(7) . . yes Cl21 Re1 Cl31 86.87(7) . . yes O21 Re1 Cl11 177.75(16) . . yes O1 Re1 Cl11 82.63(5) . . yes Cl41 Re1 Cl11 86.35(7) . . yes Cl21 Re1 Cl11 86.07(7) . . yes Cl31 Re1 Cl11 85.40(7) . . yes Re1 O1 Re1 179.998(16) 3_676 . ? C1 P C12 107.5(3) . . ? C1 P C13 110.5(3) . . ? C12 P C13 108.9(3) . . ? C1 P C11 108.3(3) . . ? C12 P C11 109.0(3) . . ? C13 P C11 112.5(3) . . ? P C1 H1A 109.5 . . ? P C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C21 C11 C61 121.0(7) . . ? C21 C11 P 120.8(6) . . ? C61 C11 P 118.2(6) . . ? C31 C21 C11 118.7(7) . . ? C31 C21 H21 120.6 . . ? C11 C21 H21 120.6 . . ? C21 C31 C41 122.7(8) . . ? C21 C31 H31 118.6 . . ? C41 C31 H31 118.6 . . ? C31 C41 C51 118.1(8) . . ? C31 C41 H41 121.0 . . ? C51 C41 H41 121.0 . . ? C61 C51 C41 122.1(8) . . ? C61 C51 H51 118.9 . . ? C41 C51 H51 118.9 . . ? C51 C61 C11 117.1(7) . . ? C51 C61 H61 121.4 . . ? C11 C61 H61 121.4 . . ? C62 C12 C22 119.9(7) . . ? C62 C12 P 118.3(6) . . ? C22 C12 P 121.6(6) . . ? C32 C22 C12 120.1(8) . . ? C32 C22 H22 120.0 . . ? C12 C22 H22 120.0 . . ? C22 C32 C42 118.7(8) . . ? C22 C32 H32 120.7 . . ? C42 C32 H32 120.7 . . ? C52 C42 C32 121.2(8) . . ? C52 C42 H42 119.4 . . ? C32 C42 H42 119.4 . . ? C42 C52 C62 121.3(8) . . ? C42 C52 H52 119.3 . . ? C62 C52 H52 119.3 . . ? C12 C62 C52 118.7(8) . . ? C12 C62 H62 120.7 . . ? C52 C62 H62 120.7 . . ? C63 C13 C23 119.3(7) . . ? C63 C13 P 120.5(5) . . ? C23 C13 P 120.2(6) . . ? C33 C23 C13 120.1(7) . . ? C33 C23 H23 120.0 . . ? C13 C23 H23 120.0 . . ? C43 C33 C23 122.4(8) . . ? C43 C33 H33 118.8 . . ? C23 C33 H33 118.8 . . ? C33 C43 C53 117.3(8) . . ? C33 C43 H43 121.4 . . ? C53 C43 H43 121.4 . . ? C63 C53 C43 121.0(7) . . ? C63 C53 H53 119.5 . . ? C43 C53 H53 119.5 . . ? C13 C63 C53 119.9(7) . . ? C13 C63 H63 120.1 . . ? C53 C63 H63 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 P C11 C21 27.9(6) . . . . ? C12 P C11 C21 144.6(6) . . . . ? C13 P C11 C21 -94.5(6) . . . . ? C1 P C11 C61 -150.6(5) . . . . ? C12 P C11 C61 -33.9(6) . . . . ? C13 P C11 C61 87.0(6) . . . . ? C61 C11 C21 C31 3.1(10) . . . . ? P C11 C21 C31 -175.4(5) . . . . ? C11 C21 C31 C41 -2.7(11) . . . . ? C21 C31 C41 C51 -0.2(12) . . . . ? C31 C41 C51 C61 2.9(12) . . . . ? C41 C51 C61 C11 -2.4(11) . . . . ? C21 C11 C61 C51 -0.6(10) . . . . ? P C11 C61 C51 177.9(5) . . . . ? C1 P C12 C62 57.2(6) . . . . ? C13 P C12 C62 177.0(5) . . . . ? C11 P C12 C62 -59.9(6) . . . . ? C1 P C12 C22 -117.6(6) . . . . ? C13 P C12 C22 2.2(7) . . . . ? C11 P C12 C22 125.3(6) . . . . ? C62 C12 C22 C32 0.2(11) . . . . ? P C12 C22 C32 174.9(6) . . . . ? C12 C22 C32 C42 -1.8(11) . . . . ? C22 C32 C42 C52 3.6(12) . . . . ? C32 C42 C52 C62 -3.7(12) . . . . ? C22 C12 C62 C52 -0.2(10) . . . . ? P C12 C62 C52 -175.1(5) . . . . ? C42 C52 C62 C12 2.0(11) . . . . ? C1 P C13 C63 39.8(8) . . . . ? C12 P C13 C63 -78.2(7) . . . . ? C11 P C13 C63 160.9(7) . . . . ? C1 P C13 C23 -140.5(6) . . . . ? C12 P C13 C23 101.6(6) . . . . ? C11 P C13 C23 -19.4(7) . . . . ? C63 C13 C23 C33 2.8(11) . . . . ? P C13 C23 C33 -176.9(6) . . . . ? C13 C23 C33 C43 1.0(12) . . . . ? C23 C33 C43 C53 -3.1(13) . . . . ? C33 C43 C53 C63 1.5(13) . . . . ? C23 C13 C63 C53 -4.3(12) . . . . ? P C13 C63 C53 175.4(6) . . . . ? C43 C53 C63 C13 2.2(13) . . . . ? O21 Re1 Re1 O21 180.000(5) . . 3 3 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1C O21 0.97 2.50 3.226(8) 132 . C1 H1C Cl11 0.97 2.82 3.571(8) 135 3_676 _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.73 _refine_diff_density_min -1.03 _refine_diff_density_rms 0.15 # Attachment 'C.cif' data_net1abs _database_code_depnum_ccdc_archive 'CCDC 714380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C20 H20 P), Cl8 O3 Re2' _chemical_formula_sum 'C40 H40 Cl8 O3 P2 Re2' _chemical_formula_weight 1286.66 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 16.762(5) _cell_length_b 14.459(4) _cell_length_c 18.389(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.19(3) _cell_angle_gamma 90.00 _cell_volume 4450(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25235 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 38.94 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 6.025 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.556 _exptl_absorpt_process_details ; 'Oxford Diffraction, 2006' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KM4CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75604 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.1268 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 38.94 _reflns_number_total 23590 _reflns_number_gt 12169 _reflns_threshold_expression >2sigma(I) _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^)+(0.0142P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23590 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.827 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.192943(6) 0.234087(7) 0.578893(6) 0.01808(3) Uani 1 1 d . . . O1 O 0.26152(11) 0.24387(13) 0.50425(11) 0.0236(4) Uani 1 1 d . . . O21 O 0.22848(12) 0.13456(13) 0.61452(13) 0.0341(6) Uani 1 1 d . . . Cl11 Cl 0.13435(4) 0.37924(4) 0.53041(4) 0.02068(14) Uani 1 1 d . . . Cl21 Cl 0.09461(4) 0.24415(5) 0.66576(4) 0.02679(15) Uani 1 1 d . . . Cl31 Cl 0.09593(4) 0.16351(5) 0.50011(4) 0.02456(15) Uani 1 1 d . . . Cl41 Cl 0.27207(4) 0.33189(5) 0.65422(4) 0.02504(16) Uani 1 1 d . . . Re2 Re 0.329717(6) 0.254926(7) 0.429013(6) 0.01901(3) Uani 1 1 d . . . O22 O 0.29351(12) 0.35461(13) 0.39458(14) 0.0383(6) Uani 1 1 d . . . Cl12 Cl 0.38635(4) 0.10800(4) 0.47524(4) 0.02203(15) Uani 1 1 d . . . Cl22 Cl 0.42833(4) 0.24563(6) 0.34286(4) 0.03179(16) Uani 1 1 d . . . Cl32 Cl 0.42663(4) 0.32367(5) 0.50857(4) 0.02553(16) Uani 1 1 d . . . Cl42 Cl 0.24948(4) 0.15993(5) 0.35191(4) 0.02537(16) Uani 1 1 d . . . P1 P 0.14581(4) 0.65256(4) 0.62596(4) 0.01504(14) Uani 1 1 d . . . C21 C 0.07837(16) 0.61818(17) 0.55081(15) 0.0179(6) Uani 1 1 d . . . H21A H 0.0900 0.5533 0.5379 0.022 Uiso 1 1 calc R . . H21B H 0.0230 0.6204 0.5668 0.022 Uiso 1 1 calc R . . C11 C 0.08354(17) 0.67819(18) 0.48282(16) 0.0224(6) Uani 1 1 d . . . H11A H 0.0454 0.6555 0.4445 0.034 Uiso 1 1 calc R . . H11B H 0.1378 0.6751 0.4657 0.034 Uiso 1 1 calc R . . H11C H 0.0707 0.7424 0.4946 0.034 Uiso 1 1 calc R . . C121 C 0.12081(15) 0.59598(17) 0.70857(15) 0.0154(5) Uani 1 1 d . . . C221 C 0.10967(15) 0.64812(19) 0.77123(16) 0.0197(6) Uani 1 1 d . . . H221 H 0.1118 0.7137 0.7694 0.024 Uiso 1 1 calc R . . C321 C 0.09552(16) 0.6037(2) 0.83583(16) 0.0220(6) Uani 1 1 d . . . H321 H 0.0888 0.6391 0.8786 0.026 Uiso 1 1 calc R . . C421 C 0.09101(17) 0.5086(2) 0.83890(16) 0.0239(6) Uani 1 1 d . . . H421 H 0.0805 0.4787 0.8834 0.029 Uiso 1 1 calc R . . C521 C 0.10188(18) 0.45678(19) 0.77663(17) 0.0255(7) Uani 1 1 d . . . H521 H 0.0985 0.3913 0.7787 0.031 Uiso 1 1 calc R . . C621 C 0.11758(17) 0.49949(18) 0.71132(16) 0.0211(6) Uani 1 1 d . . . H621 H 0.1260 0.4636 0.6691 0.025 Uiso 1 1 calc R . . C111 C 0.13446(15) 0.77528(17) 0.63822(14) 0.0167(5) Uani 1 1 d . . . C211 C 0.19878(16) 0.83557(18) 0.64702(16) 0.0202(6) Uani 1 1 d . . . H211 H 0.2518 0.8129 0.6448 0.024 Uiso 1 1 calc R . . C311 C 0.18560(19) 0.92947(18) 0.65907(17) 0.0266(7) Uani 1 1 d . . . H311 H 0.2296 0.9706 0.6657 0.032 Uiso 1 1 calc R . . C411 C 0.10818(18) 0.96259(18) 0.66139(17) 0.0243(6) Uani 1 1 d . . . H411 H 0.0992 1.0266 0.6693 0.029 Uiso 1 1 calc R . . C511 C 0.04394(18) 0.90293(19) 0.65233(17) 0.0249(7) Uani 1 1 d . . . H511 H -0.0090 0.9261 0.6539 0.030 Uiso 1 1 calc R . . C611 C 0.05655(17) 0.80917(18) 0.64088(17) 0.0226(6) Uani 1 1 d . . . H611 H 0.0124 0.7682 0.6349 0.027 Uiso 1 1 calc R . . C131 C 0.24740(15) 0.62265(17) 0.60958(15) 0.0160(5) Uani 1 1 d . . . C231 C 0.26704(17) 0.57835(18) 0.54550(16) 0.0200(6) Uani 1 1 d . . . H231 H 0.2267 0.5650 0.5087 0.024 Uiso 1 1 calc R . . C331 C 0.34608(17) 0.55381(19) 0.53583(18) 0.0251(7) Uani 1 1 d . . . H331 H 0.3599 0.5235 0.4925 0.030 Uiso 1 1 calc R . . C431 C 0.40433(17) 0.5738(2) 0.58962(18) 0.0273(7) Uani 1 1 d . . . H431 H 0.4585 0.5587 0.5824 0.033 Uiso 1 1 calc R . . C531 C 0.38469(17) 0.6157(2) 0.65410(17) 0.0251(6) Uani 1 1 d . . . H531 H 0.4253 0.6280 0.6909 0.030 Uiso 1 1 calc R . . C631 C 0.30633(16) 0.63983(19) 0.66526(16) 0.0222(6) Uani 1 1 d . . . H631 H 0.2927 0.6675 0.7098 0.027 Uiso 1 1 calc R . . P2 P 0.65653(4) 0.16858(4) 0.63240(4) 0.01485(14) Uani 1 1 d . . . C22 C 0.59341(16) 0.13542(18) 0.55400(15) 0.0180(6) Uani 1 1 d . . . H22A H 0.6032 0.0694 0.5431 0.022 Uiso 1 1 calc R . . H22B H 0.5369 0.1415 0.5662 0.022 Uiso 1 1 calc R . . C12 C 0.60638(17) 0.19214(18) 0.48603(15) 0.0228(6) Uani 1 1 d . . . H12A H 0.5702 0.1703 0.4460 0.034 Uiso 1 1 calc R . . H12B H 0.6618 0.1852 0.4726 0.034 Uiso 1 1 calc R . . H12C H 0.5955 0.2574 0.4957 0.034 Uiso 1 1 calc R . . C122 C 0.62913(15) 0.10818(17) 0.71281(15) 0.0160(5) Uani 1 1 d . . . C222 C 0.62829(15) 0.15667(19) 0.77829(15) 0.0185(6) Uani 1 1 d . . . H222 H 0.6383 0.2214 0.7793 0.022 Uiso 1 1 calc R . . C322 C 0.61280(17) 0.1100(2) 0.84212(17) 0.0243(6) Uani 1 1 d . . . H322 H 0.6127 0.1424 0.8871 0.029 Uiso 1 1 calc R . . C422 C 0.59761(17) 0.0164(2) 0.83965(18) 0.0280(7) Uani 1 1 d . . . H422 H 0.5865 -0.0154 0.8832 0.034 Uiso 1 1 calc R . . C522 C 0.59830(17) -0.03232(19) 0.77466(18) 0.0267(7) Uani 1 1 d . . . H522 H 0.5878 -0.0969 0.7739 0.032 Uiso 1 1 calc R . . C622 C 0.61445(16) 0.01361(18) 0.71081(17) 0.0211(6) Uani 1 1 d . . . H622 H 0.6155 -0.0193 0.6662 0.025 Uiso 1 1 calc R . . C112 C 0.75928(15) 0.14294(17) 0.61851(16) 0.0166(5) Uani 1 1 d . . . C212 C 0.81771(16) 0.16883(18) 0.67279(16) 0.0206(6) Uani 1 1 d . . . H212 H 0.8026 0.1995 0.7156 0.025 Uiso 1 1 calc R . . C312 C 0.89707(16) 0.1492(2) 0.66320(17) 0.0241(6) Uani 1 1 d . . . H312 H 0.9369 0.1680 0.6989 0.029 Uiso 1 1 calc R . . C412 C 0.91891(17) 0.10196(19) 0.60160(17) 0.0255(7) Uani 1 1 d . . . H412 H 0.9737 0.0897 0.5951 0.031 Uiso 1 1 calc R . . C512 C 0.86170(17) 0.07252(19) 0.54959(17) 0.0240(6) Uani 1 1 d . . . H512 H 0.8769 0.0385 0.5084 0.029 Uiso 1 1 calc R . . C612 C 0.78150(17) 0.09320(17) 0.55825(17) 0.0211(6) Uani 1 1 d . . . H612 H 0.7419 0.0732 0.5228 0.025 Uiso 1 1 calc R . . C132 C 0.64158(16) 0.29058(17) 0.64811(15) 0.0177(6) Uani 1 1 d . . . C232 C 0.56234(17) 0.31813(19) 0.65761(17) 0.0229(6) Uani 1 1 d . . . H23A H 0.5202 0.2741 0.6541 0.028 Uiso 1 1 calc R . . C332 C 0.54642(18) 0.4099(2) 0.67205(16) 0.0254(7) Uani 1 1 d . . . H332 H 0.4930 0.4291 0.6782 0.031 Uiso 1 1 calc R . . C432 C 0.60780(19) 0.47392(19) 0.67767(17) 0.0264(7) Uani 1 1 d . . . H432 H 0.5964 0.5368 0.6878 0.032 Uiso 1 1 calc R . . C532 C 0.68562(19) 0.44656(18) 0.66855(17) 0.0263(7) Uani 1 1 d . . . H532 H 0.7275 0.4908 0.6726 0.032 Uiso 1 1 calc R . . C632 C 0.70308(17) 0.35479(18) 0.65356(16) 0.0207(6) Uani 1 1 d . . . H632 H 0.7566 0.3362 0.6471 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01705(5) 0.01348(4) 0.02367(6) 0.00051(4) 0.00059(4) 0.00007(4) O1 0.0219(8) 0.0196(9) 0.0292(10) -0.0098(8) -0.0005(8) -0.0050(8) O21 0.0282(12) 0.0204(10) 0.0530(17) 0.0049(10) -0.0047(11) -0.0014(9) Cl11 0.0292(4) 0.0150(3) 0.0175(4) 0.0004(2) -0.0014(3) 0.0030(3) Cl21 0.0279(3) 0.0324(4) 0.0206(3) 0.0018(3) 0.0052(3) -0.0068(3) Cl31 0.0216(3) 0.0227(3) 0.0296(4) -0.0094(3) 0.0034(3) -0.0053(3) Cl41 0.0245(4) 0.0242(3) 0.0256(4) -0.0019(3) -0.0055(3) -0.0014(3) Re2 0.01737(5) 0.01483(5) 0.02483(6) 0.00275(4) 0.00122(4) 0.00102(4) O22 0.0282(12) 0.0195(10) 0.0661(19) 0.0127(11) -0.0067(12) -0.0004(9) Cl12 0.0323(4) 0.0149(3) 0.0184(4) -0.0008(3) -0.0031(3) 0.0044(3) Cl22 0.0274(3) 0.0467(4) 0.0217(3) 0.0062(4) 0.0053(3) -0.0047(4) Cl32 0.0214(3) 0.0206(3) 0.0348(4) -0.0066(3) 0.0027(3) -0.0027(3) Cl42 0.0245(4) 0.0271(3) 0.0239(4) -0.0017(3) -0.0041(3) 0.0015(3) P1 0.0148(3) 0.0143(3) 0.0162(4) -0.0007(3) 0.0022(3) 0.0013(2) C21 0.0169(13) 0.0177(12) 0.0191(15) -0.0008(11) 0.0003(11) 0.0032(10) C11 0.0251(15) 0.0204(13) 0.0217(16) -0.0001(11) 0.0003(12) 0.0052(11) C121 0.0116(12) 0.0204(12) 0.0142(14) 0.0012(10) 0.0004(10) 0.0008(10) C221 0.0168(13) 0.0214(13) 0.0208(16) -0.0017(11) 0.0010(12) 0.0008(11) C321 0.0167(14) 0.0318(15) 0.0178(16) -0.0049(12) 0.0026(11) 0.0026(11) C421 0.0220(15) 0.0322(16) 0.0177(16) 0.0076(12) 0.0020(12) 0.0021(12) C521 0.0332(17) 0.0191(13) 0.0239(17) 0.0044(12) -0.0009(14) -0.0003(12) C621 0.0247(15) 0.0197(13) 0.0188(16) -0.0025(11) 0.0012(12) 0.0016(11) C111 0.0222(13) 0.0167(12) 0.0114(12) -0.0006(10) 0.0019(10) 0.0031(10) C211 0.0166(14) 0.0211(13) 0.0227(16) 0.0001(11) -0.0015(12) -0.0011(10) C311 0.0343(17) 0.0159(13) 0.0291(18) 0.0017(12) -0.0027(14) -0.0050(12) C411 0.0340(17) 0.0162(12) 0.0225(16) 0.0002(11) -0.0006(13) 0.0040(12) C511 0.0249(15) 0.0222(14) 0.0275(17) -0.0027(12) 0.0005(13) 0.0079(12) C611 0.0243(15) 0.0162(12) 0.0273(17) -0.0004(12) 0.0008(12) 0.0017(11) C131 0.0154(13) 0.0151(11) 0.0176(15) 0.0053(10) 0.0021(11) 0.0001(10) C231 0.0224(14) 0.0177(12) 0.0203(16) -0.0003(11) 0.0046(12) 0.0005(11) C331 0.0271(16) 0.0221(14) 0.0272(17) 0.0039(12) 0.0111(13) 0.0073(12) C431 0.0193(15) 0.0314(16) 0.0317(19) 0.0130(14) 0.0071(13) 0.0066(12) C531 0.0188(14) 0.0325(15) 0.0236(17) 0.0078(13) -0.0017(12) 0.0020(12) C631 0.0220(14) 0.0249(14) 0.0199(16) 0.0033(12) 0.0021(12) 0.0023(11) P2 0.0147(3) 0.0141(3) 0.0158(4) -0.0009(3) 0.0009(3) 0.0008(2) C22 0.0175(13) 0.0185(12) 0.0177(15) -0.0019(11) -0.0031(11) 0.0000(10) C12 0.0275(15) 0.0245(14) 0.0160(15) 0.0003(11) -0.0004(12) 0.0035(12) C122 0.0124(12) 0.0197(12) 0.0155(14) 0.0012(10) -0.0015(11) 0.0027(10) C222 0.0150(13) 0.0240(13) 0.0165(15) -0.0014(11) 0.0016(11) 0.0000(10) C322 0.0205(15) 0.0352(16) 0.0168(16) 0.0012(12) -0.0020(12) 0.0029(12) C422 0.0241(16) 0.0356(17) 0.0246(18) 0.0121(14) 0.0046(13) 0.0017(13) C522 0.0276(16) 0.0207(14) 0.0320(19) 0.0084(13) 0.0027(14) 0.0006(12) C622 0.0226(15) 0.0178(12) 0.0227(17) -0.0002(11) 0.0007(12) -0.0001(11) C112 0.0133(12) 0.0155(12) 0.0213(15) 0.0033(11) 0.0021(11) 0.0018(10) C212 0.0206(14) 0.0245(14) 0.0171(15) 0.0038(11) 0.0037(11) -0.0001(11) C312 0.0164(14) 0.0322(15) 0.0239(17) 0.0091(13) 0.0017(12) 0.0006(12) C412 0.0169(14) 0.0252(14) 0.0350(19) 0.0115(13) 0.0077(13) 0.0067(11) C512 0.0261(16) 0.0227(14) 0.0237(17) 0.0029(12) 0.0076(13) 0.0066(12) C612 0.0232(15) 0.0168(12) 0.0234(16) 0.0007(11) 0.0014(12) 0.0020(11) C132 0.0196(14) 0.0176(12) 0.0155(14) -0.0013(10) -0.0020(11) 0.0021(10) C232 0.0218(15) 0.0213(14) 0.0255(16) -0.0025(12) -0.0004(12) 0.0037(11) C332 0.0273(16) 0.0235(15) 0.0255(18) -0.0023(12) 0.0013(13) 0.0109(12) C432 0.0385(18) 0.0165(13) 0.0242(17) -0.0027(12) 0.0024(14) 0.0056(12) C532 0.0343(17) 0.0162(13) 0.0279(18) 0.0003(12) -0.0021(14) -0.0028(12) C632 0.0211(14) 0.0199(13) 0.0211(16) 0.0029(11) 0.0010(12) 0.0016(11) 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 O21 1.677(2) . ? Re1 O1 1.844(2) . ? Re1 Cl41 2.3395(9) . ? Re1 Cl31 2.3500(10) . ? Re1 Cl21 2.3628(11) . ? Re1 Cl11 2.4631(8) . ? O1 Re2 1.850(2) . ? Re2 O22 1.6745(19) . ? Re2 Cl42 2.3439(9) . ? Re2 Cl32 2.3457(10) . ? Re2 Cl22 2.3562(11) . ? Re2 Cl12 2.4591(8) . ? P1 C121 1.795(3) . ? P1 C131 1.798(3) . ? P1 C111 1.800(3) . ? P1 C21 1.806(3) . ? C21 C11 1.528(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C121 C621 1.397(4) . ? C121 C221 1.398(4) . ? C221 C321 1.383(4) . ? C221 H221 0.9500 . ? C321 C421 1.378(4) . ? C321 H321 0.9500 . ? C421 C521 1.389(4) . ? C421 H421 0.9500 . ? C521 C621 1.389(4) . ? C521 H521 0.9500 . ? C621 H621 0.9500 . ? C111 C211 1.389(4) . ? C111 C611 1.398(4) . ? C211 C311 1.395(4) . ? C211 H211 0.9500 . ? C311 C411 1.386(4) . ? C311 H311 0.9500 . ? C411 C511 1.382(4) . ? C411 H411 0.9500 . ? C511 C611 1.390(4) . ? C511 H511 0.9500 . ? C611 H611 0.9500 . ? C131 C231 1.397(4) . ? C131 C631 1.405(4) . ? C231 C331 1.393(4) . ? C231 H231 0.9500 . ? C331 C431 1.381(4) . ? C331 H331 0.9500 . ? C431 C531 1.387(4) . ? C431 H431 0.9500 . ? C531 C631 1.385(4) . ? C531 H531 0.9500 . ? C631 H631 0.9500 . ? P2 C112 1.794(3) . ? P2 C122 1.799(3) . ? P2 C22 1.805(3) . ? P2 C132 1.807(3) . ? C22 C12 1.521(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C122 C622 1.389(4) . ? C122 C222 1.394(4) . ? C222 C322 1.391(4) . ? C222 H222 0.9500 . ? C322 C422 1.377(4) . ? C322 H322 0.9500 . ? C422 C522 1.388(4) . ? C422 H422 0.9500 . ? C522 C622 1.389(4) . ? C522 H522 0.9500 . ? C622 H622 0.9500 . ? C112 C612 1.389(4) . ? C112 C212 1.410(4) . ? C212 C312 1.381(4) . ? C212 H212 0.9500 . ? C312 C412 1.389(4) . ? C312 H312 0.9500 . ? C412 C512 1.383(4) . ? C412 H412 0.9500 . ? C512 C612 1.395(4) . ? C512 H512 0.9500 . ? C612 H612 0.9500 . ? C132 C632 1.387(4) . ? C132 C232 1.407(4) . ? C232 C332 1.382(4) . ? C232 H23A 0.9500 . ? C332 C432 1.384(4) . ? C332 H332 0.9500 . ? C432 C532 1.382(4) . ? C432 H432 0.9500 . ? C532 C632 1.390(4) . ? C532 H532 0.9500 . ? C632 H632 0.9500 . ? 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 O21 Re1 O1 97.71(11) . . ? O21 Re1 Cl41 96.32(8) . . ? O1 Re1 Cl41 92.18(6) . . ? O21 Re1 Cl31 94.98(7) . . ? O1 Re1 Cl31 90.74(6) . . ? Cl41 Re1 Cl31 167.84(2) . . ? O21 Re1 Cl21 91.99(9) . . ? O1 Re1 Cl21 170.28(6) . . ? Cl41 Re1 Cl21 87.50(3) . . ? Cl31 Re1 Cl21 87.63(3) . . ? O21 Re1 Cl11 176.92(8) . . ? O1 Re1 Cl11 85.28(6) . . ? Cl41 Re1 Cl11 84.31(3) . . ? Cl31 Re1 Cl11 84.18(3) . . ? Cl21 Re1 Cl11 85.02(3) . . ? Re1 O1 Re2 179.34(13) . . ? O22 Re2 O1 97.53(11) . . ? O22 Re2 Cl42 95.28(8) . . ? O1 Re2 Cl42 92.53(6) . . ? O22 Re2 Cl32 95.45(8) . . ? O1 Re2 Cl32 90.32(6) . . ? Cl42 Re2 Cl32 168.44(2) . . ? O22 Re2 Cl22 92.75(9) . . ? O1 Re2 Cl22 169.65(6) . . ? Cl42 Re2 Cl22 87.72(3) . . ? Cl32 Re2 Cl22 87.49(3) . . ? O22 Re2 Cl12 177.63(9) . . ? O1 Re2 Cl12 84.81(6) . . ? Cl42 Re2 Cl12 84.28(3) . . ? Cl32 Re2 Cl12 84.83(3) . . ? Cl22 Re2 Cl12 84.92(3) . . ? C121 P1 C131 107.46(12) . . ? C121 P1 C111 108.17(13) . . ? C131 P1 C111 111.45(12) . . ? C121 P1 C21 110.88(13) . . ? C131 P1 C21 111.34(13) . . ? C111 P1 C21 107.52(12) . . ? C11 C21 P1 114.09(19) . . ? C11 C21 H21A 108.7 . . ? P1 C21 H21A 108.7 . . ? C11 C21 H21B 108.7 . . ? P1 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C21 C11 H11A 109.5 . . ? C21 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C21 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C621 C121 C221 120.1(3) . . ? C621 C121 P1 119.8(2) . . ? C221 C121 P1 120.0(2) . . ? C321 C221 C121 119.7(3) . . ? C321 C221 H221 120.2 . . ? C121 C221 H221 120.2 . . ? C421 C321 C221 120.7(3) . . ? C421 C321 H321 119.6 . . ? C221 C321 H321 119.6 . . ? C321 C421 C521 119.6(3) . . ? C321 C421 H421 120.2 . . ? C521 C421 H421 120.2 . . ? C621 C521 C421 120.9(3) . . ? C621 C521 H521 119.6 . . ? C421 C521 H521 119.6 . . ? C521 C621 C121 119.0(3) . . ? C521 C621 H621 120.5 . . ? C121 C621 H621 120.5 . . ? C211 C111 C611 119.8(2) . . ? C211 C111 P1 123.1(2) . . ? C611 C111 P1 117.1(2) . . ? C111 C211 C311 120.0(3) . . ? C111 C211 H211 120.0 . . ? C311 C211 H211 120.0 . . ? C411 C311 C211 119.9(3) . . ? C411 C311 H311 120.1 . . ? C211 C311 H311 120.1 . . ? C511 C411 C311 120.3(3) . . ? C511 C411 H411 119.8 . . ? C311 C411 H411 119.8 . . ? C411 C511 C611 120.2(3) . . ? C411 C511 H511 119.9 . . ? C611 C511 H511 119.9 . . ? C511 C611 C111 119.8(3) . . ? C511 C611 H611 120.1 . . ? C111 C611 H611 120.1 . . ? C231 C131 C631 120.5(3) . . ? C231 C131 P1 121.4(2) . . ? C631 C131 P1 118.0(2) . . ? C331 C231 C131 119.7(3) . . ? C331 C231 H231 120.2 . . ? C131 C231 H231 120.2 . . ? C431 C331 C231 119.7(3) . . ? C431 C331 H331 120.2 . . ? C231 C331 H331 120.2 . . ? C331 C431 C531 120.8(3) . . ? C331 C431 H431 119.6 . . ? C531 C431 H431 119.6 . . ? C631 C531 C431 120.6(3) . . ? C631 C531 H531 119.7 . . ? C431 C531 H531 119.7 . . ? C531 C631 C131 118.8(3) . . ? C531 C631 H631 120.6 . . ? C131 C631 H631 120.6 . . ? C112 P2 C122 107.93(12) . . ? C112 P2 C22 110.87(14) . . ? C122 P2 C22 111.25(13) . . ? C112 P2 C132 111.55(12) . . ? C122 P2 C132 107.36(13) . . ? C22 P2 C132 107.85(12) . . ? C12 C22 P2 114.14(19) . . ? C12 C22 H22A 108.7 . . ? P2 C22 H22A 108.7 . . ? C12 C22 H22B 108.7 . . ? P2 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C22 C12 H12A 109.5 . . ? C22 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C22 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C622 C122 C222 120.5(3) . . ? C622 C122 P2 120.6(2) . . ? C222 C122 P2 118.8(2) . . ? C322 C222 C122 119.7(3) . . ? C322 C222 H222 120.1 . . ? C122 C222 H222 120.1 . . ? C422 C322 C222 119.5(3) . . ? C422 C322 H322 120.3 . . ? C222 C322 H322 120.3 . . ? C322 C422 C522 121.1(3) . . ? C322 C422 H422 119.4 . . ? C522 C422 H422 119.4 . . ? C422 C522 C622 119.8(3) . . ? C422 C522 H522 120.1 . . ? C622 C522 H522 120.1 . . ? C522 C622 C122 119.4(3) . . ? C522 C622 H622 120.3 . . ? C122 C622 H622 120.3 . . ? C612 C112 C212 119.7(3) . . ? C612 C112 P2 121.5(2) . . ? C212 C112 P2 118.6(2) . . ? C312 C212 C112 119.4(3) . . ? C312 C212 H212 120.3 . . ? C112 C212 H212 120.3 . . ? C212 C312 C412 120.3(3) . . ? C212 C312 H312 119.8 . . ? C412 C312 H312 119.8 . . ? C512 C412 C312 120.7(3) . . ? C512 C412 H412 119.6 . . ? C312 C412 H412 119.6 . . ? C412 C512 C612 119.4(3) . . ? C412 C512 H512 120.3 . . ? C612 C512 H512 120.3 . . ? C112 C612 C512 120.3(3) . . ? C112 C612 H612 119.8 . . ? C512 C612 H612 119.8 . . ? C632 C132 C232 120.3(2) . . ? C632 C132 P2 123.8(2) . . ? C232 C132 P2 115.9(2) . . ? C332 C232 C132 119.3(3) . . ? C332 C232 H23A 120.3 . . ? C132 C232 H23A 120.3 . . ? C232 C332 C432 120.4(3) . . ? C232 C332 H332 119.8 . . ? C432 C332 H332 119.8 . . ? C532 C432 C332 120.1(3) . . ? C532 C432 H432 119.9 . . ? C332 C432 H432 119.9 . . ? C432 C532 C632 120.5(3) . . ? C432 C532 H532 119.7 . . ? C632 C532 H532 119.7 . . ? C132 C632 C532 119.3(3) . . ? C132 C632 H632 120.3 . . ? C532 C632 H632 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C121 P1 C21 C11 167.26(19) . . . . ? C131 P1 C21 C11 -73.2(2) . . . . ? C111 P1 C21 C11 49.2(2) . . . . ? C131 P1 C121 C621 -65.4(2) . . . . ? C111 P1 C121 C621 174.1(2) . . . . ? C21 P1 C121 C621 56.5(2) . . . . ? C131 P1 C121 C221 110.5(2) . . . . ? C111 P1 C121 C221 -10.0(2) . . . . ? C21 P1 C121 C221 -127.7(2) . . . . ? C621 C121 C221 C321 0.0(4) . . . . ? P1 C121 C221 C321 -175.8(2) . . . . ? C121 C221 C321 C421 -1.0(4) . . . . ? C221 C321 C421 C521 0.9(4) . . . . ? C321 C421 C521 C621 0.3(4) . . . . ? C421 C521 C621 C121 -1.2(4) . . . . ? C221 C121 C621 C521 1.1(4) . . . . ? P1 C121 C621 C521 177.0(2) . . . . ? C121 P1 C111 C211 107.0(2) . . . . ? C131 P1 C111 C211 -10.9(3) . . . . ? C21 P1 C111 C211 -133.2(2) . . . . ? C121 P1 C111 C611 -71.1(2) . . . . ? C131 P1 C111 C611 171.0(2) . . . . ? C21 P1 C111 C611 48.7(3) . . . . ? C611 C111 C211 C311 0.5(4) . . . . ? P1 C111 C211 C311 -177.5(2) . . . . ? C111 C211 C311 C411 -0.7(5) . . . . ? C211 C311 C411 C511 0.4(5) . . . . ? C311 C411 C511 C611 0.1(5) . . . . ? C411 C511 C611 C111 -0.3(5) . . . . ? C211 C111 C611 C511 0.0(4) . . . . ? P1 C111 C611 C511 178.2(2) . . . . ? C121 P1 C131 C231 121.5(2) . . . . ? C111 P1 C131 C231 -120.1(2) . . . . ? C21 P1 C131 C231 -0.1(3) . . . . ? C121 P1 C131 C631 -54.5(2) . . . . ? C111 P1 C131 C631 63.9(2) . . . . ? C21 P1 C131 C631 -176.1(2) . . . . ? C631 C131 C231 C331 -2.1(4) . . . . ? P1 C131 C231 C331 -178.0(2) . . . . ? C131 C231 C331 C431 -0.2(4) . . . . ? C231 C331 C431 C531 1.8(4) . . . . ? C331 C431 C531 C631 -1.1(4) . . . . ? C431 C531 C631 C131 -1.2(4) . . . . ? C231 C131 C631 C531 2.8(4) . . . . ? P1 C131 C631 C531 178.9(2) . . . . ? C112 P2 C22 C12 -67.0(2) . . . . ? C122 P2 C22 C12 172.91(19) . . . . ? C132 P2 C22 C12 55.4(2) . . . . ? C112 P2 C122 C622 -76.3(2) . . . . ? C22 P2 C122 C622 45.5(3) . . . . ? C132 P2 C122 C622 163.3(2) . . . . ? C112 P2 C122 C222 99.3(2) . . . . ? C22 P2 C122 C222 -138.9(2) . . . . ? C132 P2 C122 C222 -21.1(2) . . . . ? C622 C122 C222 C322 0.1(4) . . . . ? P2 C122 C222 C322 -175.5(2) . . . . ? C122 C222 C322 C422 -0.7(4) . . . . ? C222 C322 C422 C522 0.7(4) . . . . ? C322 C422 C522 C622 -0.1(4) . . . . ? C422 C522 C622 C122 -0.5(4) . . . . ? C222 C122 C622 C522 0.5(4) . . . . ? P2 C122 C622 C522 176.0(2) . . . . ? C122 P2 C112 C612 114.4(2) . . . . ? C22 P2 C112 C612 -7.6(3) . . . . ? C132 P2 C112 C612 -127.9(2) . . . . ? C122 P2 C112 C212 -61.3(2) . . . . ? C22 P2 C112 C212 176.7(2) . . . . ? C132 P2 C112 C212 56.4(2) . . . . ? C612 C112 C212 C312 3.9(4) . . . . ? P2 C112 C212 C312 179.6(2) . . . . ? C112 C212 C312 C412 -1.8(4) . . . . ? C212 C312 C412 C512 -1.1(4) . . . . ? C312 C412 C512 C612 2.0(4) . . . . ? C212 C112 C612 C512 -3.0(4) . . . . ? P2 C112 C612 C512 -178.6(2) . . . . ? C412 C512 C612 C112 0.0(4) . . . . ? C112 P2 C132 C632 -4.1(3) . . . . ? C122 P2 C132 C632 114.0(3) . . . . ? C22 P2 C132 C632 -126.0(3) . . . . ? C112 P2 C132 C232 178.3(2) . . . . ? C122 P2 C132 C232 -63.7(2) . . . . ? C22 P2 C132 C232 56.3(3) . . . . ? C632 C132 C232 C332 0.3(4) . . . . ? P2 C132 C232 C332 178.1(2) . . . . ? C132 C232 C332 C432 -0.5(5) . . . . ? C232 C332 C432 C532 0.3(5) . . . . ? C332 C432 C532 C632 0.1(5) . . . . ? C232 C132 C632 C532 0.0(4) . . . . ? P2 C132 C632 C532 -177.5(2) . . . . ? C432 C532 C632 C132 -0.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C311 H311 O21 0.95 2.55 3.170(3) 123 1_565 C21 H21A Cl11 0.99 2.63 3.605(3) 168 . C321 H321 Cl12 0.95 2.73 3.471(3) 135 2_556 _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.34 _refine_diff_density_min -1.19 _refine_diff_density_rms 0.17 # Attachment 'D.cif' data_res45abs _database_code_depnum_ccdc_archive 'CCDC 714381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H34 P2, Cl8 O3 Re2' _chemical_formula_sum 'C38 H34 Cl8 O3 P2 Re2' _chemical_formula_weight 1256.59 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.102(3) _cell_length_b 10.762(3) _cell_length_c 11.888(3) _cell_angle_alpha 100.65(3) _cell_angle_beta 111.63(3) _cell_angle_gamma 90.37(3) _cell_volume 1060.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7357 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 37.90 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 602 _exptl_absorpt_coefficient_mu 6.319 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.408 _exptl_absorpt_correction_T_max 0.804 _exptl_absorpt_process_details 'CrysAlis RED (Oxford Diffraction, 2006)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KM4CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20192 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.3231 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 37.90 _reflns_number_total 9391 _reflns_number_gt 4036 _reflns_threshold_expression >2sigma(I) _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^)+(0.0091P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9391 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 0.709 _refine_ls_restrained_S_all 0.709 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.34702(3) 0.42060(2) 0.35136(3) 0.01478(6) Uani 1 1 d . . . Cl41 Cl 0.53463(17) 0.31501(13) 0.28266(13) 0.0193(3) Uani 1 1 d . . . P1 P 0.43028(17) 0.10985(13) -0.14989(13) 0.0128(3) Uani 1 1 d . . . C1 C 0.4591(7) 0.0622(5) -0.0050(5) 0.0176(13) Uani 1 1 d . . . H1A H 0.5244 0.1302 0.0645 0.021 Uiso 1 1 calc R . . H1B H 0.3549 0.0510 0.0019 0.021 Uiso 1 1 calc R . . Cl11 Cl 0.35911(17) 0.24206(12) 0.45380(13) 0.0197(3) Uani 1 1 d . . . Cl31 Cl 0.14747(17) 0.48702(13) 0.42168(13) 0.0220(3) Uani 1 1 d . . . Cl21 Cl 0.14654(17) 0.29282(13) 0.17953(13) 0.0218(3) Uani 1 1 d . . . O1 O 0.5000 0.5000 0.5000 0.0221(14) Uani 1 2 d S . . C11 C 0.6175(6) 0.1247(5) -0.1633(5) 0.0123(11) Uani 1 1 d . . . C41 C 0.9177(7) 0.1500(6) -0.1669(5) 0.0270(15) Uani 1 1 d . . . H41 H 1.0214 0.1577 -0.1676 0.032 Uiso 1 1 calc R . . C42 C 0.2037(6) 0.4874(5) -0.1559(5) 0.0174(13) Uani 1 1 d . . . H42 H 0.1542 0.5648 -0.1590 0.021 Uiso 1 1 calc R . . C21 C 0.7043(6) 0.2438(5) -0.1224(5) 0.0186(13) Uani 1 1 d . . . H21 H 0.6602 0.3163 -0.0925 0.022 Uiso 1 1 calc R . . C12 C 0.3470(6) 0.2587(4) -0.1468(5) 0.0108(11) Uani 1 1 d . . . O21 O 0.3426(5) 0.5364(4) 0.2732(4) 0.0278(10) Uani 1 1 d . . . C13 C 0.3012(6) -0.0081(5) -0.2751(5) 0.0132(11) Uani 1 1 d . . . C62 C 0.3112(6) 0.3157(5) -0.2507(5) 0.0159(12) Uani 1 1 d . . . H62 H 0.3368 0.2761 -0.3187 0.019 Uiso 1 1 calc R . . C32 C 0.2399(6) 0.4337(5) -0.0508(5) 0.0165(12) Uani 1 1 d . . . H32 H 0.2162 0.4753 0.0175 0.020 Uiso 1 1 calc R . . C22 C 0.3106(6) 0.3195(5) -0.0466(5) 0.0179(12) Uani 1 1 d . . . H22 H 0.3342 0.2828 0.0243 0.021 Uiso 1 1 calc R . . C52 C 0.2398(7) 0.4282(5) -0.2546(5) 0.0196(13) Uani 1 1 d . . . H52 H 0.2153 0.4650 -0.3255 0.024 Uiso 1 1 calc R . . C23 C 0.1889(7) -0.0837(5) -0.2578(6) 0.0253(15) Uani 1 1 d . . . H23 H 0.1842 -0.0746 -0.1782 0.030 Uiso 1 1 calc R . . C31 C 0.8559(7) 0.2555(5) -0.1257(6) 0.0267(15) Uani 1 1 d . . . H31 H 0.9147 0.3359 -0.0995 0.032 Uiso 1 1 calc R . . C61 C 0.6839(7) 0.0201(5) -0.2052(5) 0.0189(13) Uani 1 1 d . . . H61 H 0.6263 -0.0608 -0.2324 0.023 Uiso 1 1 calc R . . C63 C 0.3097(7) -0.0230(5) -0.3908(5) 0.0246(14) Uani 1 1 d . . . H63 H 0.3867 0.0271 -0.4030 0.029 Uiso 1 1 calc R . . C33 C 0.0851(7) -0.1711(5) -0.3549(7) 0.0323(17) Uani 1 1 d . . . H33 H 0.0077 -0.2216 -0.3435 0.039 Uiso 1 1 calc R . . C51 C 0.8349(7) 0.0326(5) -0.2078(6) 0.0281(15) Uani 1 1 d . . . H51 H 0.8802 -0.0392 -0.2375 0.034 Uiso 1 1 calc R . . C43 C 0.0958(8) -0.1838(6) -0.4683(7) 0.042(2) Uani 1 1 d . . . H43 H 0.0251 -0.2448 -0.5353 0.050 Uiso 1 1 calc R . . C53 C 0.2051(8) -0.1115(6) -0.4888(6) 0.0385(18) Uani 1 1 d . . . H53 H 0.2090 -0.1219 -0.5688 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01598(11) 0.01312(11) 0.01401(13) 0.00096(8) 0.00509(9) 0.00015(8) Cl41 0.0196(7) 0.0195(7) 0.0187(8) -0.0021(6) 0.0100(6) -0.0007(6) P1 0.0167(8) 0.0106(7) 0.0122(8) 0.0024(6) 0.0066(6) 0.0013(6) C1 0.026(3) 0.013(3) 0.017(3) 0.000(2) 0.013(3) 0.004(2) Cl11 0.0269(8) 0.0158(7) 0.0175(8) 0.0039(6) 0.0095(6) 0.0022(6) Cl31 0.0186(8) 0.0240(8) 0.0206(9) -0.0029(6) 0.0075(7) 0.0023(6) Cl21 0.0210(8) 0.0264(8) 0.0153(8) 0.0016(6) 0.0048(6) 0.0009(6) O1 0.029(3) 0.010(3) 0.035(4) 0.000(3) 0.024(3) 0.005(2) C11 0.014(3) 0.010(3) 0.014(3) 0.004(2) 0.006(2) 0.002(2) C41 0.015(3) 0.034(4) 0.026(4) 0.001(3) 0.004(3) -0.007(3) C42 0.019(3) 0.005(3) 0.022(4) 0.000(2) 0.002(3) 0.003(2) C21 0.016(3) 0.016(3) 0.022(3) -0.005(2) 0.010(3) 0.001(2) C12 0.010(3) 0.008(2) 0.018(3) 0.005(2) 0.008(2) 0.000(2) O21 0.033(3) 0.024(2) 0.023(3) 0.0074(19) 0.004(2) -0.0010(19) C13 0.019(3) 0.008(3) 0.009(3) 0.001(2) 0.002(2) 0.004(2) C62 0.017(3) 0.021(3) 0.009(3) 0.002(2) 0.005(2) 0.001(2) C32 0.020(3) 0.013(3) 0.011(3) -0.006(2) 0.004(2) -0.002(2) C22 0.020(3) 0.022(3) 0.010(3) 0.000(2) 0.004(2) -0.002(2) C52 0.023(3) 0.021(3) 0.013(3) 0.010(2) 0.003(3) -0.001(2) C23 0.019(3) 0.019(3) 0.035(4) -0.004(3) 0.010(3) 0.000(3) C31 0.016(3) 0.016(3) 0.040(4) 0.000(3) 0.004(3) 0.000(2) C61 0.021(3) 0.014(3) 0.027(4) 0.000(2) 0.016(3) -0.001(2) C63 0.034(4) 0.018(3) 0.021(4) 0.005(3) 0.009(3) 0.002(3) C33 0.018(3) 0.020(3) 0.059(5) -0.002(3) 0.021(3) 0.001(3) C51 0.026(4) 0.021(3) 0.039(4) 0.000(3) 0.017(3) 0.004(3) C43 0.022(4) 0.024(4) 0.050(5) -0.016(3) -0.010(3) 0.000(3) C53 0.050(5) 0.027(4) 0.020(4) -0.005(3) -0.002(3) -0.004(3) 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 O21 1.678(4) . ? Re1 O1 1.8450(10) . ? Re1 Cl31 2.3289(16) . ? Re1 Cl21 2.3611(19) . ? Re1 Cl41 2.3632(16) . ? Re1 Cl11 2.4404(15) . ? P1 C12 1.776(5) . ? P1 C11 1.778(5) . ? P1 C13 1.789(5) . ? P1 C1 1.815(5) . ? C1 C1 1.538(10) 2_655 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O1 Re1 1.8450(9) 2_666 ? C11 C61 1.380(7) . ? C11 C21 1.406(7) . ? C41 C31 1.361(8) . ? C41 C51 1.376(8) . ? C41 H41 0.9500 . ? C42 C52 1.379(7) . ? C42 C32 1.403(7) . ? C42 H42 0.9500 . ? C21 C31 1.400(8) . ? C21 H21 0.9500 . ? C12 C22 1.401(7) . ? C12 C62 1.413(7) . ? C13 C63 1.385(7) . ? C13 C23 1.398(8) . ? C62 C52 1.378(7) . ? C62 H62 0.9500 . ? C32 C22 1.392(7) . ? C32 H32 0.9500 . ? C22 H22 0.9500 . ? C52 H52 0.9500 . ? C23 C33 1.376(8) . ? C23 H23 0.9500 . ? C31 H31 0.9500 . ? C61 C51 1.392(8) . ? C61 H61 0.9500 . ? C63 C53 1.390(8) . ? C63 H63 0.9500 . ? C33 C43 1.368(9) . ? C33 H33 0.9500 . ? C51 H51 0.9500 . ? C43 C53 1.376(10) . ? C43 H43 0.9500 . ? C53 H53 0.9500 . ? 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 O21 Re1 O1 97.44(14) . . ? O21 Re1 Cl31 97.00(15) . . ? O1 Re1 Cl31 90.65(5) . . ? O21 Re1 Cl21 92.15(14) . . ? O1 Re1 Cl21 170.33(4) . . ? Cl31 Re1 Cl21 86.95(6) . . ? O21 Re1 Cl41 92.53(15) . . ? O1 Re1 Cl41 93.01(5) . . ? Cl31 Re1 Cl41 169.27(5) . . ? Cl21 Re1 Cl41 87.77(6) . . ? O21 Re1 Cl11 175.80(14) . . ? O1 Re1 Cl11 84.67(5) . . ? Cl31 Re1 Cl11 86.58(6) . . ? Cl21 Re1 Cl11 85.84(6) . . ? Cl41 Re1 Cl11 83.72(5) . . ? C12 P1 C11 110.0(2) . . ? C12 P1 C13 111.1(2) . . ? C11 P1 C13 109.8(3) . . ? C12 P1 C1 107.9(2) . . ? C11 P1 C1 108.8(3) . . ? C13 P1 C1 109.2(3) . . ? C1 C1 P1 112.0(5) 2_655 . ? C1 C1 H1A 109.2 2_655 . ? P1 C1 H1A 109.2 . . ? C1 C1 H1B 109.2 2_655 . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? Re1 O1 Re1 179.999(15) 2_666 . ? C61 C11 C21 119.3(5) . . ? C61 C11 P1 121.2(4) . . ? C21 C11 P1 119.3(4) . . ? C31 C41 C51 122.2(6) . . ? C31 C41 H41 118.9 . . ? C51 C41 H41 118.9 . . ? C52 C42 C32 120.3(5) . . ? C52 C42 H42 119.9 . . ? C32 C42 H42 119.9 . . ? C31 C21 C11 120.0(5) . . ? C31 C21 H21 120.0 . . ? C11 C21 H21 120.0 . . ? C22 C12 C62 118.8(5) . . ? C22 C12 P1 122.3(4) . . ? C62 C12 P1 118.9(4) . . ? C63 C13 C23 119.6(5) . . ? C63 C13 P1 120.0(4) . . ? C23 C13 P1 120.4(4) . . ? C52 C62 C12 120.8(5) . . ? C52 C62 H62 119.6 . . ? C12 C62 H62 119.6 . . ? C22 C32 C42 120.0(5) . . ? C22 C32 H32 120.0 . . ? C42 C32 H32 120.0 . . ? C32 C22 C12 120.0(5) . . ? C32 C22 H22 120.0 . . ? C12 C22 H22 120.0 . . ? C62 C52 C42 120.1(5) . . ? C62 C52 H52 119.9 . . ? C42 C52 H52 119.9 . . ? C33 C23 C13 120.7(6) . . ? C33 C23 H23 119.7 . . ? C13 C23 H23 119.7 . . ? C41 C31 C21 118.9(5) . . ? C41 C31 H31 120.5 . . ? C21 C31 H31 120.5 . . ? C11 C61 C51 120.3(5) . . ? C11 C61 H61 119.9 . . ? C51 C61 H61 119.9 . . ? C13 C63 C53 119.7(6) . . ? C13 C63 H63 120.1 . . ? C53 C63 H63 120.1 . . ? C43 C33 C23 118.6(6) . . ? C43 C33 H33 120.7 . . ? C23 C33 H33 120.7 . . ? C41 C51 C61 119.3(5) . . ? C41 C51 H51 120.4 . . ? C61 C51 H51 120.4 . . ? C33 C43 C53 122.5(6) . . ? C33 C43 H43 118.8 . . ? C53 C43 H43 118.8 . . ? C43 C53 C63 119.0(7) . . ? C43 C53 H53 120.5 . . ? C63 C53 H53 120.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 P1 C1 C1 -176.4(5) . . . 2_655 ? C11 P1 C1 C1 -57.1(6) . . . 2_655 ? C13 P1 C1 C1 62.8(6) . . . 2_655 ? C12 P1 C11 C61 -159.8(5) . . . . ? C13 P1 C11 C61 -37.3(5) . . . . ? C1 P1 C11 C61 82.2(5) . . . . ? C12 P1 C11 C21 24.7(5) . . . . ? C13 P1 C11 C21 147.2(4) . . . . ? C1 P1 C11 C21 -93.3(5) . . . . ? C61 C11 C21 C31 0.7(8) . . . . ? P1 C11 C21 C31 176.3(4) . . . . ? C11 P1 C12 C22 -119.9(4) . . . . ? C13 P1 C12 C22 118.3(5) . . . . ? C1 P1 C12 C22 -1.4(5) . . . . ? C11 P1 C12 C62 62.3(5) . . . . ? C13 P1 C12 C62 -59.5(5) . . . . ? C1 P1 C12 C62 -179.2(4) . . . . ? C12 P1 C13 C63 87.2(5) . . . . ? C11 P1 C13 C63 -34.7(5) . . . . ? C1 P1 C13 C63 -153.9(4) . . . . ? C12 P1 C13 C23 -91.3(5) . . . . ? C11 P1 C13 C23 146.8(5) . . . . ? C1 P1 C13 C23 27.6(5) . . . . ? C22 C12 C62 C52 -0.9(8) . . . . ? P1 C12 C62 C52 177.0(4) . . . . ? C52 C42 C32 C22 -0.8(8) . . . . ? C42 C32 C22 C12 0.6(8) . . . . ? C62 C12 C22 C32 0.3(8) . . . . ? P1 C12 C22 C32 -177.5(4) . . . . ? C12 C62 C52 C42 0.7(8) . . . . ? C32 C42 C52 C62 0.2(8) . . . . ? C63 C13 C23 C33 -1.1(8) . . . . ? P1 C13 C23 C33 177.4(4) . . . . ? C51 C41 C31 C21 1.3(10) . . . . ? C11 C21 C31 C41 -1.0(9) . . . . ? C21 C11 C61 C51 -0.5(8) . . . . ? P1 C11 C61 C51 -176.0(5) . . . . ? C23 C13 C63 C53 0.9(8) . . . . ? P1 C13 C63 C53 -177.6(5) . . . . ? C13 C23 C33 C43 1.0(9) . . . . ? C31 C41 C51 C61 -1.1(10) . . . . ? C11 C61 C51 C41 0.7(9) . . . . ? C23 C33 C43 C53 -0.7(10) . . . . ? C33 C43 C53 C63 0.6(10) . . . . ? C13 C63 C53 C43 -0.7(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C62 H62 Cl11 0.95 2.74 3.642(6) 158 1_554 _diffrn_measured_fraction_theta_max 0.818 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.91 _refine_diff_density_min -1.58 _refine_diff_density_rms 0.24 # Attachment 'E.cif' data_recl4pac _database_code_depnum_ccdc_archive 'CCDC 714382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C20 H20 P), Cl8 O3 Re2, 3(C H Cl3)' _chemical_formula_sum 'C43 H43 Cl17 O3 P2 Re2' _chemical_formula_weight 1644.76 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.961(5) _cell_length_b 12.910(5) _cell_length_c 19.574(8) _cell_angle_alpha 83.68(3) _cell_angle_beta 75.51(3) _cell_angle_gamma 78.86(3) _cell_volume 2865(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23702 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 36.80 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 5.107 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.499 _exptl_absorpt_correction_T_max 0.658 _exptl_absorpt_process_details ; (ABSPACK and analytical correction; Oxford Diffraction, 2006) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KM4CCD _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49739 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 35.00 _reflns_number_total 21042 _reflns_number_gt 14239 _reflns_threshold_expression >2sigma(I) _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^)+(0.0220P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21042 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.555016(10) 0.388435(9) 0.215645(6) 0.01484(3) Uani 1 1 d . . . O21 O 0.5622(2) 0.40516(17) 0.12871(11) 0.0225(5) Uani 1 1 d . . . Cl11 Cl 0.54121(7) 0.35022(6) 0.34343(4) 0.02092(15) Uani 1 1 d . . . Cl21 Cl 0.72630(7) 0.25994(6) 0.20200(4) 0.02295(16) Uani 1 1 d . . . Cl31 Cl 0.44661(7) 0.24861(6) 0.22881(4) 0.02130(16) Uani 1 1 d . . . Cl41 Cl 0.67155(7) 0.51053(6) 0.22177(4) 0.02172(15) Uani 1 1 d . . . Re2 Re 0.291515(10) 0.582345(9) 0.285111(6) 0.01559(3) Uani 1 1 d . . . O22 O 0.3165(2) 0.57355(17) 0.36621(12) 0.0242(5) Uani 1 1 d . . . Cl12 Cl 0.25792(7) 0.58827(6) 0.16464(4) 0.02081(15) Uani 1 1 d . . . Cl22 Cl 0.12045(7) 0.70851(6) 0.30938(4) 0.02102(15) Uani 1 1 d . . . Cl42 Cl 0.17150(7) 0.45253(6) 0.31409(4) 0.02232(16) Uani 1 1 d . . . Cl32 Cl 0.39311(7) 0.72431(6) 0.24149(4) 0.02141(15) Uani 1 1 d . . . O1 O 0.42179(19) 0.48583(16) 0.24622(12) 0.0188(4) Uani 1 1 d . . . P1 P 0.73303(7) 0.60798(6) 0.40464(4) 0.02039(17) Uani 1 1 d . . . C121 C 0.8061(3) 0.4774(2) 0.42552(17) 0.0236(7) Uani 1 1 d . . . C221 C 0.8705(3) 0.4581(3) 0.47713(19) 0.0319(8) Uani 1 1 d . . . H221 H 0.8808 0.5149 0.5006 0.038 Uiso 1 1 calc R . . C321 C 0.9197(4) 0.3544(3) 0.4940(2) 0.0379(9) Uani 1 1 d . . . H321 H 0.9647 0.3403 0.5287 0.046 Uiso 1 1 calc R . . C421 C 0.9029(4) 0.2723(3) 0.4603(2) 0.0368(9) Uani 1 1 d . . . H421 H 0.9359 0.2017 0.4722 0.044 Uiso 1 1 calc R . . C521 C 0.8386(3) 0.2918(3) 0.4092(2) 0.0329(8) Uani 1 1 d . . . H521 H 0.8276 0.2346 0.3864 0.040 Uiso 1 1 calc R . . C621 C 0.7902(3) 0.3943(3) 0.39113(19) 0.0290(8) Uani 1 1 d . . . H621 H 0.7467 0.4078 0.3557 0.035 Uiso 1 1 calc R . . C111 C 0.7558(3) 0.7010(2) 0.45887(16) 0.0203(6) Uani 1 1 d . . . C211 C 0.8228(3) 0.7797(2) 0.43030(17) 0.0229(7) Uani 1 1 d . . . H211 H 0.8570 0.7852 0.3810 0.027 Uiso 1 1 calc R . . C311 C 0.8391(3) 0.8494(3) 0.47423(18) 0.0314(8) Uani 1 1 d . . . H311 H 0.8842 0.9033 0.4550 0.038 Uiso 1 1 calc R . . C411 C 0.7900(3) 0.8411(3) 0.54614(18) 0.0307(8) Uani 1 1 d . . . H411 H 0.8023 0.8890 0.5760 0.037 Uiso 1 1 calc R . . C511 C 0.7234(3) 0.7638(3) 0.57485(18) 0.0290(8) Uani 1 1 d . . . H511 H 0.6894 0.7591 0.6242 0.035 Uiso 1 1 calc R . . C611 C 0.7061(3) 0.6931(3) 0.53152(17) 0.0271(7) Uani 1 1 d . . . H611 H 0.6607 0.6396 0.5511 0.033 Uiso 1 1 calc R . . C131 C 0.7896(3) 0.6487(2) 0.31373(16) 0.0190(6) Uani 1 1 d . . . C231 C 0.8948(3) 0.5947(2) 0.27599(17) 0.0210(6) Uani 1 1 d . . . H231 H 0.9347 0.5335 0.2971 0.025 Uiso 1 1 calc R . . C331 C 0.9416(3) 0.6306(3) 0.20708(17) 0.0268(7) Uani 1 1 d . . . H331 H 1.0138 0.5941 0.1811 0.032 Uiso 1 1 calc R . . C431 C 0.8835(3) 0.7187(3) 0.17648(19) 0.0322(8) Uani 1 1 d . . . H431 H 0.9157 0.7428 0.1293 0.039 Uiso 1 1 calc R . . C531 C 0.7777(4) 0.7730(3) 0.21434(19) 0.0341(9) Uani 1 1 d . . . H531 H 0.7375 0.8335 0.1928 0.041 Uiso 1 1 calc R . . C631 C 0.7319(3) 0.7391(3) 0.28229(19) 0.0304(8) Uani 1 1 d . . . H631 H 0.6606 0.7769 0.3084 0.036 Uiso 1 1 calc R . . P2 P 0.13449(7) 0.25233(6) 0.10212(4) 0.01586(15) Uani 1 1 d . . . C122 C 0.2615(3) 0.2866(2) 0.03861(15) 0.0165(6) Uani 1 1 d . . . C222 C 0.3335(3) 0.3471(2) 0.05628(17) 0.0209(6) Uani 1 1 d . . . H222 H 0.3185 0.3687 0.1031 0.025 Uiso 1 1 calc R . . C322 C 0.4281(3) 0.3757(2) 0.00440(17) 0.0229(7) Uani 1 1 d . . . H322 H 0.4782 0.4160 0.0163 0.028 Uiso 1 1 calc R . . C422 C 0.4494(3) 0.3462(2) -0.06380(18) 0.0230(7) Uani 1 1 d . . . H422 H 0.5134 0.3670 -0.0988 0.028 Uiso 1 1 calc R . . C522 C 0.3771(3) 0.2856(2) -0.08156(17) 0.0229(7) Uani 1 1 d . . . H522 H 0.3920 0.2650 -0.1286 0.027 Uiso 1 1 calc R . . C622 C 0.2836(3) 0.2556(2) -0.03048(16) 0.0206(6) Uani 1 1 d . . . H622 H 0.2347 0.2139 -0.0424 0.025 Uiso 1 1 calc R . . C112 C 0.1486(3) 0.1106(2) 0.11615(15) 0.0174(6) Uani 1 1 d . . . C212 C 0.2586(3) 0.0473(2) 0.10200(16) 0.0213(6) Uani 1 1 d . . . H212 H 0.3265 0.0779 0.0815 0.026 Uiso 1 1 calc R . . C312 C 0.2687(3) -0.0607(2) 0.11789(17) 0.0261(7) Uani 1 1 d . . . H312 H 0.3440 -0.1040 0.1083 0.031 Uiso 1 1 calc R . . C412 C 0.1705(3) -0.1065(2) 0.14754(17) 0.0276(8) Uani 1 1 d . . . H412 H 0.1786 -0.1808 0.1583 0.033 Uiso 1 1 calc R . . C512 C 0.0595(3) -0.0432(2) 0.16165(17) 0.0256(7) Uani 1 1 d . . . H512 H -0.0080 -0.0745 0.1819 0.031 Uiso 1 1 calc R . . C612 C 0.0478(3) 0.0652(2) 0.14612(16) 0.0222(7) Uani 1 1 d . . . H612 H -0.0274 0.1085 0.1556 0.027 Uiso 1 1 calc R . . C132 C 0.0063(3) 0.3032(2) 0.06795(15) 0.0167(6) Uani 1 1 d . . . C232 C -0.0292(3) 0.2426(2) 0.02503(16) 0.0214(6) Uani 1 1 d . . . H232 H 0.0107 0.1724 0.0163 0.026 Uiso 1 1 calc R . . C332 C -0.1231(3) 0.2854(3) -0.00483(17) 0.0266(7) Uani 1 1 d . . . H332 H -0.1469 0.2445 -0.0344 0.032 Uiso 1 1 calc R . . C432 C -0.1824(3) 0.3870(3) 0.00805(18) 0.0277(7) Uani 1 1 d . . . H432 H -0.2470 0.4157 -0.0123 0.033 Uiso 1 1 calc R . . C532 C -0.1472(3) 0.4469(3) 0.05086(17) 0.0253(7) Uani 1 1 d . . . H532 H -0.1882 0.5167 0.0598 0.030 Uiso 1 1 calc R . . C632 C -0.0531(3) 0.4064(2) 0.08070(17) 0.0223(7) Uani 1 1 d . . . H632 H -0.0291 0.4482 0.1096 0.027 Uiso 1 1 calc R . . C5 C 0.6494(3) 0.0737(2) 0.11264(19) 0.0271(7) Uani 1 1 d . . . H5 H 0.6460 0.1120 0.1550 0.033 Uiso 1 1 calc R . . Cl15 Cl 0.79697(8) 0.01293(7) 0.07928(5) 0.0345(2) Uani 1 1 d . . . Cl25 Cl 0.59995(9) 0.16564(8) 0.04912(5) 0.0422(2) Uani 1 1 d . . . Cl35 Cl 0.55813(9) -0.02224(8) 0.13877(7) 0.0475(3) Uani 1 1 d . . . Cl23 Cl 0.77679(9) 0.02102(8) 0.31125(6) 0.0483(3) Uani 1 1 d . . . C22 C 0.1252(3) 0.3091(2) 0.18397(16) 0.0208(6) Uani 1 1 d . . . H22A H 0.1977 0.2804 0.2004 0.025 Uiso 1 1 calc R . . H22B H 0.1210 0.3865 0.1751 0.025 Uiso 1 1 calc R . . C12 C 0.0190(3) 0.2869(3) 0.24289(17) 0.0266(7) Uani 1 1 d . . . H12A H 0.0193 0.3193 0.2858 0.040 Uiso 1 1 calc R . . H12B H 0.0232 0.2103 0.2527 0.040 Uiso 1 1 calc R . . H12C H -0.0533 0.3169 0.2277 0.040 Uiso 1 1 calc R . . Cl13 Cl 0.62881(12) 0.08290(10) 0.44572(6) 0.0579(3) Uani 1 1 d . . . Cl33 Cl 0.53297(11) -0.00360(9) 0.34903(9) 0.0689(4) Uani 1 1 d . . . C3 C 0.6334(3) 0.0742(3) 0.35624(19) 0.0304(8) Uani 1 1 d . . . H3 H 0.6111 0.1469 0.3349 0.036 Uiso 1 1 calc R . . C21 C 0.5789(3) 0.5980(3) 0.4259(2) 0.0324(8) Uani 1 1 d . . . H21A H 0.5674 0.5504 0.3928 0.039 Uiso 1 1 calc R . . H21B H 0.5594 0.5634 0.4740 0.039 Uiso 1 1 calc R . . C11 C 0.4918(3) 0.6989(3) 0.4235(2) 0.0437(10) Uani 1 1 d . . . H11A H 0.4122 0.6827 0.4362 0.065 Uiso 1 1 calc R . . H11B H 0.5071 0.7332 0.3756 0.065 Uiso 1 1 calc R . . H11C H 0.4996 0.7466 0.4570 0.065 Uiso 1 1 calc R . . Cl14 Cl 0.24877(9) -0.11246(7) 0.39717(5) 0.0341(2) Uani 1 1 d . . . Cl24 Cl 0.28239(8) 0.04486(7) 0.27945(4) 0.03062(19) Uani 1 1 d . . . Cl34 Cl 0.04977(8) 0.00241(7) 0.34550(5) 0.0360(2) Uani 1 1 d . . . C4 C 0.2003(3) -0.0534(2) 0.32191(17) 0.0236(7) Uani 1 1 d . . . H4 H 0.2110 -0.1092 0.2881 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01428(6) 0.01347(5) 0.01690(6) -0.00115(4) -0.00409(5) -0.00206(4) O21 0.0246(12) 0.0239(11) 0.0220(11) -0.0011(9) -0.0105(10) -0.0046(9) Cl11 0.0226(4) 0.0216(3) 0.0183(3) -0.0005(3) -0.0042(3) -0.0045(3) Cl21 0.0171(4) 0.0197(3) 0.0285(4) -0.0028(3) -0.0020(3) 0.0016(3) Cl31 0.0214(4) 0.0175(3) 0.0254(4) -0.0039(3) -0.0026(3) -0.0069(3) Cl41 0.0220(4) 0.0212(3) 0.0249(4) -0.0007(3) -0.0066(3) -0.0097(3) Re2 0.01545(6) 0.01472(5) 0.01702(6) -0.00250(4) -0.00465(5) -0.00165(4) O22 0.0270(13) 0.0246(11) 0.0234(12) -0.0030(9) -0.0086(10) -0.0062(10) Cl12 0.0202(4) 0.0241(3) 0.0182(3) -0.0047(3) -0.0057(3) -0.0007(3) Cl22 0.0178(4) 0.0189(3) 0.0251(4) -0.0068(3) -0.0025(3) -0.0005(3) Cl42 0.0203(4) 0.0178(3) 0.0299(4) 0.0015(3) -0.0070(3) -0.0061(3) Cl32 0.0213(4) 0.0172(3) 0.0251(4) -0.0040(3) -0.0021(3) -0.0047(3) O1 0.0137(10) 0.0162(9) 0.0271(11) -0.0033(8) -0.0051(9) -0.0021(7) P1 0.0197(4) 0.0218(4) 0.0193(4) -0.0052(3) -0.0009(3) -0.0055(3) C121 0.0273(17) 0.0213(15) 0.0207(15) -0.0009(12) -0.0005(14) -0.0078(13) C221 0.042(2) 0.0287(18) 0.0264(18) -0.0029(14) -0.0106(17) -0.0046(16) C321 0.052(3) 0.035(2) 0.0253(18) 0.0037(15) -0.0159(18) 0.0019(18) C421 0.045(2) 0.0270(18) 0.031(2) 0.0062(14) 0.0019(18) -0.0058(16) C521 0.033(2) 0.0272(17) 0.038(2) -0.0059(15) -0.0011(17) -0.0113(15) C621 0.0305(19) 0.0274(17) 0.0289(18) -0.0048(14) -0.0041(16) -0.0068(14) C111 0.0207(16) 0.0201(14) 0.0197(15) -0.0050(11) -0.0027(13) -0.0036(12) C211 0.0262(17) 0.0238(15) 0.0182(15) -0.0006(12) -0.0032(14) -0.0062(13) C311 0.047(2) 0.0214(16) 0.0263(18) -0.0014(13) -0.0063(17) -0.0115(15) C411 0.044(2) 0.0231(16) 0.0271(18) -0.0084(13) -0.0101(17) -0.0061(15) C511 0.037(2) 0.0276(17) 0.0192(16) -0.0079(13) -0.0022(15) 0.0010(15) C611 0.0296(18) 0.0264(16) 0.0229(17) -0.0018(13) 0.0019(15) -0.0096(14) C131 0.0192(15) 0.0204(14) 0.0193(15) -0.0043(11) -0.0058(13) -0.0047(12) C231 0.0151(15) 0.0254(15) 0.0227(16) -0.0033(12) -0.0049(13) -0.0025(12) C331 0.0206(16) 0.0392(19) 0.0214(16) -0.0084(14) 0.0003(14) -0.0105(14) C431 0.040(2) 0.042(2) 0.0206(17) 0.0030(14) -0.0112(16) -0.0196(17) C531 0.044(2) 0.0307(19) 0.0306(19) 0.0070(15) -0.0183(18) -0.0061(17) C631 0.032(2) 0.0259(17) 0.0291(18) -0.0043(14) -0.0076(16) 0.0073(14) P2 0.0175(4) 0.0147(3) 0.0151(4) -0.0023(3) -0.0035(3) -0.0019(3) C122 0.0146(14) 0.0160(13) 0.0182(14) 0.0004(10) -0.0034(12) -0.0025(11) C222 0.0256(17) 0.0160(13) 0.0218(15) 0.0009(11) -0.0082(14) -0.0032(12) C322 0.0256(17) 0.0186(14) 0.0272(17) 0.0028(12) -0.0100(14) -0.0074(13) C422 0.0203(16) 0.0193(14) 0.0280(17) 0.0050(12) -0.0053(14) -0.0042(12) C522 0.0216(16) 0.0232(15) 0.0218(16) -0.0029(12) -0.0003(13) -0.0046(12) C622 0.0216(16) 0.0197(14) 0.0212(15) -0.0038(11) -0.0050(13) -0.0037(12) C112 0.0222(15) 0.0168(13) 0.0137(13) -0.0020(10) -0.0053(12) -0.0027(11) C212 0.0249(17) 0.0215(14) 0.0176(14) -0.0016(11) -0.0061(13) -0.0024(12) C312 0.0329(19) 0.0211(15) 0.0248(17) -0.0019(12) -0.0135(15) 0.0035(14) C412 0.046(2) 0.0165(14) 0.0237(16) -0.0004(12) -0.0160(16) -0.0047(14) C512 0.036(2) 0.0185(14) 0.0249(17) 0.0018(12) -0.0068(15) -0.0121(14) C612 0.0252(17) 0.0195(14) 0.0225(16) -0.0018(11) -0.0059(14) -0.0049(12) C132 0.0163(14) 0.0177(13) 0.0146(13) 0.0007(10) -0.0019(12) -0.0021(11) C232 0.0198(16) 0.0243(15) 0.0193(15) -0.0036(12) -0.0043(13) -0.0009(12) C332 0.0228(17) 0.0389(19) 0.0201(16) -0.0042(13) -0.0099(14) -0.0026(14) C432 0.0216(17) 0.0335(18) 0.0249(17) 0.0055(14) -0.0083(14) 0.0022(14) C532 0.0245(17) 0.0229(15) 0.0220(16) 0.0048(12) -0.0014(14) 0.0026(13) C632 0.0245(17) 0.0184(14) 0.0233(16) -0.0028(12) -0.0040(14) -0.0035(12) C5 0.0304(19) 0.0203(15) 0.0321(18) -0.0078(13) -0.0109(16) -0.0001(13) Cl15 0.0235(4) 0.0282(4) 0.0497(6) -0.0036(4) -0.0079(4) 0.0002(3) Cl25 0.0450(6) 0.0392(5) 0.0332(5) 0.0006(4) -0.0091(4) 0.0133(4) Cl35 0.0271(5) 0.0306(5) 0.0807(8) 0.0004(5) -0.0076(5) -0.0039(4) Cl23 0.0399(6) 0.0388(5) 0.0491(6) 0.0117(4) 0.0042(5) 0.0070(4) C22 0.0217(16) 0.0214(14) 0.0210(15) -0.0039(11) -0.0077(13) -0.0030(12) C12 0.0320(19) 0.0286(17) 0.0198(16) -0.0056(12) -0.0018(15) -0.0102(14) Cl13 0.0746(9) 0.0572(7) 0.0379(6) -0.0091(5) -0.0164(6) 0.0060(6) Cl33 0.0461(7) 0.0433(6) 0.1329(13) -0.0273(7) -0.0468(8) 0.0009(5) C3 0.032(2) 0.0257(17) 0.0338(19) -0.0018(14) -0.0107(16) -0.0004(14) C21 0.0249(18) 0.0317(18) 0.042(2) -0.0114(16) -0.0029(17) -0.0098(15) C11 0.028(2) 0.042(2) 0.062(3) -0.016(2) -0.013(2) 0.0006(17) Cl14 0.0480(6) 0.0264(4) 0.0298(4) 0.0016(3) -0.0148(4) -0.0056(4) Cl24 0.0337(5) 0.0389(5) 0.0216(4) 0.0000(3) -0.0032(4) -0.0174(4) Cl34 0.0252(4) 0.0374(5) 0.0410(5) 0.0005(4) -0.0019(4) -0.0039(4) C4 0.0237(17) 0.0235(15) 0.0234(16) -0.0036(12) -0.0051(14) -0.0032(13) _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 O21 1.674(2) . ? Re1 O1 1.842(2) . ? Re1 Cl41 2.3272(11) . ? Re1 Cl21 2.3519(13) . ? Re1 Cl31 2.3750(11) . ? Re1 Cl11 2.4659(13) . ? Re2 O22 1.675(2) . ? Re2 O1 1.851(2) . ? Re2 Cl22 2.3369(13) . ? Re2 Cl42 2.3460(11) . ? Re2 Cl32 2.3583(12) . ? Re2 Cl12 2.4801(12) . ? P1 C111 1.788(3) . ? P1 C131 1.797(3) . ? P1 C121 1.797(3) . ? P1 C21 1.813(4) . ? C121 C221 1.391(5) . ? C121 C621 1.394(5) . ? C221 C321 1.393(5) . ? C221 H221 0.9500 . ? C321 C421 1.379(5) . ? C321 H321 0.9500 . ? C421 C521 1.381(6) . ? C421 H421 0.9500 . ? C521 C621 1.384(5) . ? C521 H521 0.9500 . ? C621 H621 0.9500 . ? C111 C211 1.397(4) . ? C111 C611 1.398(4) . ? C211 C311 1.382(5) . ? C211 H211 0.9500 . ? C311 C411 1.384(5) . ? C311 H311 0.9500 . ? C411 C511 1.381(5) . ? C411 H411 0.9500 . ? C511 C611 1.388(5) . ? C511 H511 0.9500 . ? C611 H611 0.9500 . ? C131 C231 1.388(4) . ? C131 C631 1.400(5) . ? C231 C331 1.390(4) . ? C231 H231 0.9500 . ? C331 C431 1.374(5) . ? C331 H331 0.9500 . ? C431 C531 1.395(5) . ? C431 H431 0.9500 . ? C531 C631 1.364(5) . ? C531 H531 0.9500 . ? C631 H631 0.9500 . ? P2 C122 1.800(3) . ? P2 C112 1.801(3) . ? P2 C22 1.804(3) . ? P2 C132 1.804(3) . ? C122 C222 1.393(4) . ? C122 C622 1.400(4) . ? C222 C322 1.397(4) . ? C222 H222 0.9500 . ? C322 C422 1.377(5) . ? C322 H322 0.9500 . ? C422 C522 1.398(5) . ? C422 H422 0.9500 . ? C522 C622 1.387(4) . ? C522 H522 0.9500 . ? C622 H622 0.9500 . ? C112 C212 1.389(4) . ? C112 C612 1.408(4) . ? C212 C312 1.383(4) . ? C212 H212 0.9500 . ? C312 C412 1.385(5) . ? C312 H312 0.9500 . ? C412 C512 1.398(5) . ? C412 H412 0.9500 . ? C512 C612 1.387(4) . ? C512 H512 0.9500 . ? C612 H612 0.9500 . ? C132 C232 1.397(4) . ? C132 C632 1.400(4) . ? C232 C332 1.388(5) . ? C232 H232 0.9500 . ? C332 C432 1.383(5) . ? C332 H332 0.9500 . ? C432 C532 1.387(5) . ? C432 H432 0.9500 . ? C532 C632 1.385(5) . ? C532 H532 0.9500 . ? C632 H632 0.9500 . ? C5 Cl25 1.754(4) . ? C5 Cl35 1.758(4) . ? C5 Cl15 1.777(4) . ? C5 H5 1.0000 . ? Cl23 C3 1.764(4) . ? C22 C12 1.537(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Cl13 C3 1.754(4) . ? Cl33 C3 1.748(4) . ? C3 H3 1.0000 . ? C21 C11 1.507(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? Cl14 C4 1.760(4) . ? Cl24 C4 1.762(3) . ? Cl34 C4 1.769(3) . ? C4 H4 1.0000 . ? 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 O21 Re1 O1 98.57(11) . . ? O21 Re1 Cl41 98.00(8) . . ? O1 Re1 Cl41 90.44(8) . . ? O21 Re1 Cl21 93.54(9) . . ? O1 Re1 Cl21 167.86(7) . . ? Cl41 Re1 Cl21 87.00(4) . . ? O21 Re1 Cl31 91.76(8) . . ? O1 Re1 Cl31 92.47(7) . . ? Cl41 Re1 Cl31 169.28(3) . . ? Cl21 Re1 Cl31 88.00(4) . . ? O21 Re1 Cl11 175.64(7) . . ? O1 Re1 Cl11 83.13(8) . . ? Cl41 Re1 Cl11 85.97(4) . . ? Cl21 Re1 Cl11 84.85(4) . . ? Cl31 Re1 Cl11 84.14(4) . . ? O22 Re2 O1 96.54(11) . . ? O22 Re2 Cl22 95.90(9) . . ? O1 Re2 Cl22 167.54(7) . . ? O22 Re2 Cl42 93.39(8) . . ? O1 Re2 Cl42 92.40(7) . . ? Cl22 Re2 Cl42 87.48(4) . . ? O22 Re2 Cl32 95.38(8) . . ? O1 Re2 Cl32 91.07(8) . . ? Cl22 Re2 Cl32 87.14(4) . . ? Cl42 Re2 Cl32 170.14(3) . . ? O22 Re2 Cl12 177.85(8) . . ? O1 Re2 Cl12 81.64(8) . . ? Cl22 Re2 Cl12 85.94(4) . . ? Cl42 Re2 Cl12 85.57(4) . . ? Cl32 Re2 Cl12 85.81(4) . . ? Re1 O1 Re2 174.61(14) . . ? C111 P1 C131 108.22(15) . . ? C111 P1 C121 110.42(16) . . ? C131 P1 C121 110.28(15) . . ? C111 P1 C21 109.32(16) . . ? C131 P1 C21 113.86(18) . . ? C121 P1 C21 104.72(17) . . ? C221 C121 C621 120.6(3) . . ? C221 C121 P1 121.8(2) . . ? C621 C121 P1 117.5(3) . . ? C121 C221 C321 119.3(3) . . ? C121 C221 H221 120.4 . . ? C321 C221 H221 120.4 . . ? C421 C321 C221 119.9(4) . . ? C421 C321 H321 120.0 . . ? C221 C321 H321 120.0 . . ? C321 C421 C521 120.6(3) . . ? C321 C421 H421 119.7 . . ? C521 C421 H421 119.7 . . ? C421 C521 C621 120.3(3) . . ? C421 C521 H521 119.8 . . ? C621 C521 H521 119.8 . . ? C521 C621 C121 119.2(4) . . ? C521 C621 H621 120.4 . . ? C121 C621 H621 120.4 . . ? C211 C111 C611 119.9(3) . . ? C211 C111 P1 121.5(2) . . ? C611 C111 P1 118.6(2) . . ? C311 C211 C111 119.6(3) . . ? C311 C211 H211 120.2 . . ? C111 C211 H211 120.2 . . ? C211 C311 C411 120.3(3) . . ? C211 C311 H311 119.9 . . ? C411 C311 H311 119.9 . . ? C511 C411 C311 120.6(3) . . ? C511 C411 H411 119.7 . . ? C311 C411 H411 119.7 . . ? C411 C511 C611 119.9(3) . . ? C411 C511 H511 120.0 . . ? C611 C511 H511 120.0 . . ? C511 C611 C111 119.7(3) . . ? C511 C611 H611 120.2 . . ? C111 C611 H611 120.2 . . ? C231 C131 C631 119.8(3) . . ? C231 C131 P1 119.9(2) . . ? C631 C131 P1 120.1(2) . . ? C131 C231 C331 119.6(3) . . ? C131 C231 H231 120.2 . . ? C331 C231 H231 120.2 . . ? C431 C331 C231 120.1(3) . . ? C431 C331 H331 119.9 . . ? C231 C331 H331 119.9 . . ? C331 C431 C531 120.3(3) . . ? C331 C431 H431 119.8 . . ? C531 C431 H431 119.8 . . ? C631 C531 C431 119.9(3) . . ? C631 C531 H531 120.0 . . ? C431 C531 H531 120.0 . . ? C531 C631 C131 120.2(3) . . ? C531 C631 H631 119.9 . . ? C131 C631 H631 119.9 . . ? C122 P2 C112 109.88(14) . . ? C122 P2 C22 108.10(15) . . ? C112 P2 C22 109.71(14) . . ? C122 P2 C132 108.74(14) . . ? C112 P2 C132 109.03(14) . . ? C22 P2 C132 111.37(15) . . ? C222 C122 C622 120.2(3) . . ? C222 C122 P2 121.2(2) . . ? C622 C122 P2 118.5(2) . . ? C122 C222 C322 119.2(3) . . ? C122 C222 H222 120.4 . . ? C322 C222 H222 120.4 . . ? C422 C322 C222 120.8(3) . . ? C422 C322 H322 119.6 . . ? C222 C322 H322 119.6 . . ? C322 C422 C522 120.0(3) . . ? C322 C422 H422 120.0 . . ? C522 C422 H422 120.0 . . ? C622 C522 C422 119.9(3) . . ? C622 C522 H522 120.0 . . ? C422 C522 H522 120.0 . . ? C522 C622 C122 119.9(3) . . ? C522 C622 H622 120.0 . . ? C122 C622 H622 120.0 . . ? C212 C112 C612 120.3(3) . . ? C212 C112 P2 120.2(2) . . ? C612 C112 P2 119.4(2) . . ? C312 C212 C112 119.6(3) . . ? C312 C212 H212 120.2 . . ? C112 C212 H212 120.2 . . ? C212 C312 C412 120.8(3) . . ? C212 C312 H312 119.6 . . ? C412 C312 H312 119.6 . . ? C312 C412 C512 119.8(3) . . ? C312 C412 H412 120.1 . . ? C512 C412 H412 120.1 . . ? C612 C512 C412 120.0(3) . . ? C612 C512 H512 120.0 . . ? C412 C512 H512 120.0 . . ? C512 C612 C112 119.4(3) . . ? C512 C612 H612 120.3 . . ? C112 C612 H612 120.3 . . ? C232 C132 C632 119.9(3) . . ? C232 C132 P2 120.2(2) . . ? C632 C132 P2 119.8(2) . . ? C332 C232 C132 119.6(3) . . ? C332 C232 H232 120.2 . . ? C132 C232 H232 120.2 . . ? C432 C332 C232 120.7(3) . . ? C432 C332 H332 119.7 . . ? C232 C332 H332 119.7 . . ? C332 C432 C532 119.6(3) . . ? C332 C432 H432 120.2 . . ? C532 C432 H432 120.2 . . ? C632 C532 C432 120.8(3) . . ? C632 C532 H532 119.6 . . ? C432 C532 H532 119.6 . . ? C532 C632 C132 119.4(3) . . ? C532 C632 H632 120.3 . . ? C132 C632 H632 120.3 . . ? Cl25 C5 Cl35 110.3(2) . . ? Cl25 C5 Cl15 110.6(2) . . ? Cl35 C5 Cl15 110.58(18) . . ? Cl25 C5 H5 108.4 . . ? Cl35 C5 H5 108.4 . . ? Cl15 C5 H5 108.4 . . ? C12 C22 P2 113.5(2) . . ? C12 C22 H22A 108.9 . . ? P2 C22 H22A 108.9 . . ? C12 C22 H22B 108.9 . . ? P2 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C22 C12 H12A 109.5 . . ? C22 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C22 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Cl33 C3 Cl13 109.6(2) . . ? Cl33 C3 Cl23 111.0(2) . . ? Cl13 C3 Cl23 109.8(2) . . ? Cl33 C3 H3 108.8 . . ? Cl13 C3 H3 108.8 . . ? Cl23 C3 H3 108.8 . . ? C11 C21 P1 117.7(3) . . ? C11 C21 H21A 107.9 . . ? P1 C21 H21A 107.9 . . ? C11 C21 H21B 107.9 . . ? P1 C21 H21B 107.9 . . ? H21A C21 H21B 107.2 . . ? C21 C11 H11A 109.5 . . ? C21 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C21 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Cl14 C4 Cl24 110.94(19) . . ? Cl14 C4 Cl34 110.41(18) . . ? Cl24 C4 Cl34 109.82(18) . . ? Cl14 C4 H4 108.5 . . ? Cl24 C4 H4 108.5 . . ? Cl34 C4 H4 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C111 P1 C121 C221 -0.4(3) . . . . ? C131 P1 C121 C221 119.1(3) . . . . ? C21 P1 C121 C221 -118.0(3) . . . . ? C111 P1 C121 C621 175.7(2) . . . . ? C131 P1 C121 C621 -64.7(3) . . . . ? C21 P1 C121 C621 58.1(3) . . . . ? C621 C121 C221 C321 0.3(5) . . . . ? P1 C121 C221 C321 176.3(3) . . . . ? C121 C221 C321 C421 -0.8(6) . . . . ? C221 C321 C421 C521 0.6(6) . . . . ? C321 C421 C521 C621 0.1(6) . . . . ? C421 C521 C621 C121 -0.7(5) . . . . ? C221 C121 C621 C521 0.4(5) . . . . ? P1 C121 C621 C521 -175.7(3) . . . . ? C131 P1 C111 C211 -8.5(3) . . . . ? C121 P1 C111 C211 112.3(3) . . . . ? C21 P1 C111 C211 -133.0(3) . . . . ? C131 P1 C111 C611 172.3(3) . . . . ? C121 P1 C111 C611 -66.9(3) . . . . ? C21 P1 C111 C611 47.8(3) . . . . ? C611 C111 C211 C311 -0.2(5) . . . . ? P1 C111 C211 C311 -179.4(3) . . . . ? C111 C211 C311 C411 0.4(6) . . . . ? C211 C311 C411 C511 -0.6(6) . . . . ? C311 C411 C511 C611 0.6(6) . . . . ? C411 C511 C611 C111 -0.4(5) . . . . ? C211 C111 C611 C511 0.2(5) . . . . ? P1 C111 C611 C511 179.4(3) . . . . ? C111 P1 C131 C231 105.1(3) . . . . ? C121 P1 C131 C231 -15.8(3) . . . . ? C21 P1 C131 C231 -133.2(3) . . . . ? C111 P1 C131 C631 -70.6(3) . . . . ? C121 P1 C131 C631 168.5(3) . . . . ? C21 P1 C131 C631 51.2(3) . . . . ? C631 C131 C231 C331 -0.4(5) . . . . ? P1 C131 C231 C331 -176.1(2) . . . . ? C131 C231 C331 C431 -0.3(5) . . . . ? C231 C331 C431 C531 0.3(5) . . . . ? C331 C431 C531 C631 0.6(6) . . . . ? C431 C531 C631 C131 -1.3(6) . . . . ? C231 C131 C631 C531 1.2(5) . . . . ? P1 C131 C631 C531 176.9(3) . . . . ? C112 P2 C122 C222 -119.6(3) . . . . ? C22 P2 C122 C222 0.1(3) . . . . ? C132 P2 C122 C222 121.1(3) . . . . ? C112 P2 C122 C622 63.4(3) . . . . ? C22 P2 C122 C622 -176.9(2) . . . . ? C132 P2 C122 C622 -55.8(3) . . . . ? C622 C122 C222 C322 -0.3(4) . . . . ? P2 C122 C222 C322 -177.2(2) . . . . ? C122 C222 C322 C422 1.0(5) . . . . ? C222 C322 C422 C522 -0.9(5) . . . . ? C322 C422 C522 C622 0.2(5) . . . . ? C422 C522 C622 C122 0.4(5) . . . . ? C222 C122 C622 C522 -0.4(5) . . . . ? P2 C122 C622 C522 176.6(2) . . . . ? C122 P2 C112 C212 23.4(3) . . . . ? C22 P2 C112 C212 -95.4(3) . . . . ? C132 P2 C112 C212 142.4(2) . . . . ? C122 P2 C112 C612 -161.0(2) . . . . ? C22 P2 C112 C612 80.3(3) . . . . ? C132 P2 C112 C612 -41.9(3) . . . . ? C612 C112 C212 C312 -0.4(5) . . . . ? P2 C112 C212 C312 175.3(2) . . . . ? C112 C212 C312 C412 0.2(5) . . . . ? C212 C312 C412 C512 0.1(5) . . . . ? C312 C412 C512 C612 -0.2(5) . . . . ? C412 C512 C612 C112 0.0(5) . . . . ? C212 C112 C612 C512 0.3(5) . . . . ? P2 C112 C612 C512 -175.4(2) . . . . ? C122 P2 C132 C232 88.0(3) . . . . ? C112 P2 C132 C232 -31.8(3) . . . . ? C22 P2 C132 C232 -153.0(2) . . . . ? C122 P2 C132 C632 -87.8(3) . . . . ? C112 P2 C132 C632 152.4(2) . . . . ? C22 P2 C132 C632 31.2(3) . . . . ? C632 C132 C232 C332 0.2(4) . . . . ? P2 C132 C232 C332 -175.6(2) . . . . ? C132 C232 C332 C432 -0.6(5) . . . . ? C232 C332 C432 C532 0.4(5) . . . . ? C332 C432 C532 C632 0.2(5) . . . . ? C432 C532 C632 C132 -0.6(5) . . . . ? C232 C132 C632 C532 0.4(4) . . . . ? P2 C132 C632 C532 176.3(2) . . . . ? C122 P2 C22 C12 179.2(2) . . . . ? C112 P2 C22 C12 -61.0(3) . . . . ? C132 P2 C22 C12 59.8(3) . . . . ? C111 P1 C21 C11 53.5(4) . . . . ? C131 P1 C21 C11 -67.6(3) . . . . ? C121 P1 C21 C11 171.8(3) . . . . ? O21 Re1 Re2 O22 -168.17(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C621 H621 Cl11 0.95 2.77 3.497(4) 134 . C611 H611 Cl11 0.95 2.75 3.430(4) 129 2_666 C3 H3 Cl11 1.00 2.61 3.521(4) 152 . C5 H5 Cl21 1.00 2.64 3.503(4) 145 . C4 H4 Cl22 1.00 2.73 3.441(4) 129 1_545 C4 H4 Cl32 1.00 2.80 3.557(4) 133 1_545 _diffrn_measured_fraction_theta_max 0.834 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.66 _refine_diff_density_min -1.94 _refine_diff_density_rms 0.17