# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_chen135cult_cpd8 _database_code_depnum_ccdc_archive 'CCDC 919237' #TrackingRef 'chen132_134_135.cif' _audit_creation_date 2012-06-14 _audit_creation_method ; Olex2 1.2-beta (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H39 Cl2 F3 P3 Re' _chemical_formula_sum 'C33 H39 Cl2 F3 P3 Re' _chemical_formula_weight 842.65 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 '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 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 8.2020(3) _cell_length_b 14.2941(6) _cell_length_c 15.4384(5) _cell_angle_alpha 75.737(3) _cell_angle_beta 88.315(3) _cell_angle_gamma 75.493(3) _cell_volume 1697.27(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8125 _cell_measurement_temperature 172.9(3) _cell_measurement_theta_max 71.4554 _cell_measurement_theta_min 9.9167 _exptl_absorpt_coefficient_mu 10.111 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.41159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 836 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_unetI/netI 0.0382 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 10438 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.49 _diffrn_reflns_theta_min 9.93 _diffrn_ambient_temperature 172.9(3) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 38.00 72.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 150.0000 34 #__ type_ start__ end____ width___ exp.time_ 2 omega -112.00 -19.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 125.0000 -180.0000 93 #__ type_ start__ end____ width___ exp.time_ 3 omega -65.00 13.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 91.0000 -42.0000 78 #__ type_ start__ end____ width___ exp.time_ 4 omega 77.00 121.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 125.0000 60.0000 44 #__ type_ start__ end____ width___ exp.time_ 5 omega 25.00 123.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 30.0000 98 #__ type_ start__ end____ width___ exp.time_ 6 omega -13.00 71.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -38.0000 60.0000 84 #__ type_ start__ end____ width___ exp.time_ 7 omega -72.00 -20.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 25.0000 -90.0000 52 #__ type_ start__ end____ width___ exp.time_ 8 omega 38.00 72.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 120.0000 34 #__ type_ start__ end____ width___ exp.time_ 9 omega 82.00 138.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -150.0000 56 #__ type_ start__ end____ width___ exp.time_ 10 omega 138.00 178.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 25.0000 30.0000 40 #__ type_ start__ end____ width___ exp.time_ 11 omega 37.00 71.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -30.0000 34 #__ type_ start__ end____ width___ exp.time_ 12 omega 44.00 71.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 13 omega 87.00 146.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -60.0000 59 #__ type_ start__ end____ width___ exp.time_ 14 omega 41.00 148.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 120.0000 107 #__ type_ start__ end____ width___ exp.time_ 15 omega 122.00 148.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 16 omega 40.00 70.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -90.0000 30 #__ type_ start__ end____ width___ exp.time_ 17 omega 83.00 111.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 30.0000 28 #__ type_ start__ end____ width___ exp.time_ 18 omega 46.00 72.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 19 omega 38.00 69.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 30.0000 31 #__ type_ start__ end____ width___ exp.time_ 20 omega 80.00 124.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 25.0000 30.0000 44 #__ type_ start__ end____ width___ exp.time_ 21 omega 38.00 67.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 60.0000 29 #__ type_ start__ end____ width___ exp.time_ 22 omega 38.00 69.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -150.0000 31 #__ type_ start__ end____ width___ exp.time_ 23 omega 41.00 69.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -150.0000 28 #__ type_ start__ end____ width___ exp.time_ 24 omega 53.00 82.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -60.0000 29 #__ type_ start__ end____ width___ exp.time_ 25 omega 87.00 173.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 64.0000 60.0000 86 #__ type_ start__ end____ width___ exp.time_ 26 omega 106.00 174.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 50.0000 -60.0000 68 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1044406000 _diffrn_orient_matrix_UB_12 0.0705740000 _diffrn_orient_matrix_UB_13 0.0155428000 _diffrn_orient_matrix_UB_21 -0.0578066000 _diffrn_orient_matrix_UB_22 0.0691523000 _diffrn_orient_matrix_UB_23 -0.0931102000 _diffrn_orient_matrix_UB_31 -0.1530901000 _diffrn_orient_matrix_UB_32 0.0586159000 _diffrn_orient_matrix_UB_33 0.0412621000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35 _diffrn_source_power 1.75 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5842 _reflns_number_total 5993 _reflns_odcompleteness_completeness 98.58 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.520 _refine_diff_density_min -2.235 _refine_diff_density_rms 0.120 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 385 _refine_ls_number_reflns 5993 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0305 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+1.1650P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.0750 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap 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 0.028263(15) 0.291077(9) 0.326793(8) 0.02130(7) Uani 1 1 d . . . Cl1 Cl -0.09328(10) 0.14354(6) 0.32892(5) 0.03084(17) Uani 1 1 d . . . Cl2 Cl -0.27173(10) 0.38958(7) 0.30785(6) 0.03605(19) Uani 1 1 d . . . P1 P 0.01436(10) 0.33040(7) 0.16314(5) 0.02675(18) Uani 1 1 d . . . P2 P 0.28700(10) 0.16584(6) 0.34730(5) 0.02112(16) Uani 1 1 d . . . P3 P -0.02321(11) 0.26640(7) 0.48596(6) 0.02641(18) Uani 1 1 d . . . F1 F -0.1422(5) 0.8784(2) 0.0896(3) 0.0857(11) Uani 1 1 d . . . F2 F 0.1130(5) 0.8804(2) 0.0565(2) 0.0789(10) Uani 1 1 d . . . F3 F 0.0127(5) 0.9199(2) 0.1750(2) 0.0749(9) Uani 1 1 d . . . C1 C 0.1401(4) 0.3806(3) 0.3279(2) 0.0294(7) Uani 1 1 d . . . C2 C 0.2527(5) 0.4476(3) 0.3298(3) 0.0345(8) Uani 1 1 d . . . H2A H 0.3645 0.4184 0.3086 0.041 Uiso 1 1 calc R . . H2B H 0.2683 0.4500 0.3925 0.041 Uiso 1 1 calc R . . C3 C 0.1880(5) 0.5532(3) 0.2734(2) 0.0318(7) Uani 1 1 d . . . C4 C 0.3007(5) 0.6089(3) 0.2375(3) 0.0351(8) Uani 1 1 d . . . H4 H 0.4183 0.5798 0.2466 0.042 Uiso 1 1 calc R . . C5 C 0.2437(5) 0.7067(3) 0.1885(3) 0.0408(9) Uani 1 1 d . . . H5 H 0.3220 0.7440 0.1635 0.049 Uiso 1 1 calc R . . C6 C 0.0725(5) 0.7499(3) 0.1761(3) 0.0398(9) Uani 1 1 d . . . C7 C -0.0418(5) 0.6946(3) 0.2125(3) 0.0393(9) Uani 1 1 d . . . H7 H -0.1594 0.7244 0.2042 0.047 Uiso 1 1 calc R . . C8 C 0.0151(5) 0.5968(3) 0.2604(3) 0.0381(8) Uani 1 1 d . . . H8 H -0.0633 0.5591 0.2846 0.046 Uiso 1 1 calc R . . C9 C 0.0124(7) 0.8562(3) 0.1244(3) 0.0496(11) Uani 1 1 d . . . C11 C 0.2061(4) 0.3290(3) 0.0994(2) 0.0290(7) Uani 1 1 d . . . C12 C 0.2418(5) 0.2833(3) 0.0293(2) 0.0381(8) Uani 1 1 d . . . H12 H 0.1697 0.2460 0.0155 0.046 Uiso 1 1 calc R . . C13 C 0.3838(5) 0.2920(4) -0.0212(3) 0.0463(10) Uani 1 1 d . . . H13 H 0.4081 0.2603 -0.0690 0.056 Uiso 1 1 calc R . . C14 C 0.4889(5) 0.3465(4) -0.0020(3) 0.0457(10) Uani 1 1 d . . . H14 H 0.5844 0.3531 -0.0371 0.055 Uiso 1 1 calc R . . C15 C 0.4548(5) 0.3914(3) 0.0681(3) 0.0413(9) Uani 1 1 d . . . H15 H 0.5278 0.4282 0.0820 0.050 Uiso 1 1 calc R . . C16 C 0.3145(5) 0.3830(3) 0.1184(2) 0.0345(8) Uani 1 1 d . . . H16 H 0.2916 0.4145 0.1664 0.041 Uiso 1 1 calc R . . C17 C -0.0974(5) 0.2592(3) 0.1148(3) 0.0376(8) Uani 1 1 d . . . H17A H -0.0343 0.1891 0.1289 0.056 Uiso 1 1 calc R . . H17B H -0.1084 0.2857 0.0498 0.056 Uiso 1 1 calc R . . H17C H -0.2097 0.2646 0.1397 0.056 Uiso 1 1 calc R . . C18 C -0.1022(5) 0.4583(3) 0.1134(3) 0.0389(8) Uani 1 1 d . . . H18A H -0.2134 0.4713 0.1395 0.058 Uiso 1 1 calc R . . H18B H -0.1155 0.4679 0.0486 0.058 Uiso 1 1 calc R . . H18C H -0.0402 0.5044 0.1252 0.058 Uiso 1 1 calc R . . C21 C 0.3751(4) 0.1192(2) 0.2507(2) 0.0252(6) Uani 1 1 d . . . C22 C 0.2875(4) 0.0669(3) 0.2121(2) 0.0304(7) Uani 1 1 d . . . H22 H 0.1815 0.0583 0.2341 0.036 Uiso 1 1 calc R . . C23 C 0.3553(5) 0.0274(3) 0.1413(3) 0.0394(9) Uani 1 1 d . . . H23 H 0.2953 -0.0080 0.1149 0.047 Uiso 1 1 calc R . . C24 C 0.5106(5) 0.0394(4) 0.1090(3) 0.0453(10) Uani 1 1 d . . . H24 H 0.5576 0.0116 0.0612 0.054 Uiso 1 1 calc R . . C25 C 0.5963(5) 0.0920(4) 0.1468(3) 0.0422(9) Uani 1 1 d . . . H25 H 0.7019 0.1008 0.1244 0.051 Uiso 1 1 calc R . . C26 C 0.5299(5) 0.1322(3) 0.2172(2) 0.0324(7) Uani 1 1 d . . . H26 H 0.5898 0.1686 0.2425 0.039 Uiso 1 1 calc R . . C27 C 0.2876(5) 0.0471(3) 0.4260(2) 0.0331(7) Uani 1 1 d . . . H27A H 0.2658 0.0577 0.4861 0.050 Uiso 1 1 calc R . . H27B H 0.3977 0.0001 0.4265 0.050 Uiso 1 1 calc R . . H27C H 0.1996 0.0198 0.4077 0.050 Uiso 1 1 calc R . . C28 C 0.4640(4) 0.1969(3) 0.3921(2) 0.0301(7) Uani 1 1 d . . . H28A H 0.4916 0.2535 0.3495 0.045 Uiso 1 1 calc R . . H28B H 0.5619 0.1393 0.4020 0.045 Uiso 1 1 calc R . . H28C H 0.4337 0.2146 0.4489 0.045 Uiso 1 1 calc R . . C31 C 0.1555(4) 0.2479(3) 0.5614(2) 0.0290(7) Uani 1 1 d . . . C32 C 0.2291(6) 0.1565(3) 0.6194(3) 0.0411(9) Uani 1 1 d . . . H32 H 0.1822 0.1011 0.6238 0.049 Uiso 1 1 calc R . . C33 C 0.3726(6) 0.1464(4) 0.6712(3) 0.0598(14) Uani 1 1 d . . . H33 H 0.4236 0.0838 0.7105 0.072 Uiso 1 1 calc R . . C34 C 0.4394(7) 0.2255(6) 0.6657(4) 0.0684(17) Uani 1 1 d . . . H34 H 0.5383 0.2171 0.7003 0.082 Uiso 1 1 calc R . . C35 C 0.3661(7) 0.3177(5) 0.6108(3) 0.0639(15) Uani 1 1 d . . . H35 H 0.4118 0.3731 0.6082 0.077 Uiso 1 1 calc R . . C36 C 0.2252(6) 0.3275(3) 0.5599(3) 0.0426(9) Uani 1 1 d . . . H36 H 0.1736 0.3910 0.5223 0.051 Uiso 1 1 calc R . . C37 C -0.1202(6) 0.1663(4) 0.5381(3) 0.0479(11) Uani 1 1 d . . . H37A H -0.2304 0.1778 0.5090 0.072 Uiso 1 1 calc R . . H37B H -0.1346 0.1644 0.6017 0.072 Uiso 1 1 calc R . . H37C H -0.0479 0.1025 0.5319 0.072 Uiso 1 1 calc R . . C38 C -0.1695(6) 0.3727(4) 0.5143(3) 0.0566(13) Uani 1 1 d . . . H38A H -0.1260 0.4321 0.4940 0.085 Uiso 1 1 calc R . . H38B H -0.1818 0.3588 0.5792 0.085 Uiso 1 1 calc R . . H38C H -0.2795 0.3843 0.4848 0.085 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 0.01856(10) 0.02208(9) 0.02130(10) -0.00254(6) 0.00081(6) -0.00434(6) Cl1 0.0252(4) 0.0353(4) 0.0352(4) -0.0085(3) 0.0008(3) -0.0137(3) Cl2 0.0217(4) 0.0408(5) 0.0359(4) -0.0011(3) 0.0013(3) 0.0016(3) P1 0.0224(4) 0.0336(4) 0.0218(4) -0.0015(3) -0.0014(3) -0.0074(3) P2 0.0182(4) 0.0230(4) 0.0217(4) -0.0054(3) -0.0008(3) -0.0042(3) P3 0.0252(4) 0.0294(4) 0.0242(4) -0.0070(3) 0.0038(3) -0.0062(3) F1 0.082(2) 0.0396(15) 0.118(3) 0.0041(17) -0.036(2) -0.0034(15) F2 0.110(3) 0.0483(16) 0.0660(19) 0.0036(14) 0.0182(19) -0.0163(17) F3 0.106(3) 0.0386(14) 0.085(2) -0.0269(15) 0.0075(19) -0.0170(16) C1 0.0293(17) 0.0322(17) 0.0266(16) -0.0063(13) 0.0044(13) -0.0090(14) C2 0.0357(19) 0.0318(18) 0.0367(19) -0.0047(15) -0.0008(15) -0.0130(15) C3 0.040(2) 0.0327(18) 0.0264(16) -0.0110(14) 0.0035(14) -0.0117(15) C4 0.0356(19) 0.0329(18) 0.0394(19) -0.0112(15) 0.0063(16) -0.0116(15) C5 0.046(2) 0.036(2) 0.044(2) -0.0110(17) 0.0091(18) -0.0171(18) C6 0.046(2) 0.0344(19) 0.041(2) -0.0159(16) 0.0025(17) -0.0076(17) C7 0.036(2) 0.037(2) 0.046(2) -0.0176(17) 0.0025(17) -0.0047(16) C8 0.039(2) 0.037(2) 0.039(2) -0.0124(16) 0.0096(16) -0.0097(16) C9 0.062(3) 0.031(2) 0.055(3) -0.0121(19) 0.000(2) -0.009(2) C11 0.0237(16) 0.0368(18) 0.0205(15) 0.0009(13) -0.0001(12) -0.0043(14) C12 0.0333(19) 0.051(2) 0.0304(18) -0.0091(16) 0.0003(15) -0.0130(17) C13 0.039(2) 0.067(3) 0.0314(19) -0.0141(19) 0.0043(17) -0.008(2) C14 0.030(2) 0.067(3) 0.0334(19) -0.0016(18) 0.0064(16) -0.0119(19) C15 0.033(2) 0.053(2) 0.0364(19) -0.0014(17) 0.0014(16) -0.0191(18) C16 0.0294(18) 0.042(2) 0.0300(17) -0.0038(15) 0.0001(14) -0.0103(15) C17 0.0304(19) 0.053(2) 0.0317(18) -0.0070(16) -0.0042(15) -0.0181(17) C18 0.0311(19) 0.041(2) 0.0339(18) 0.0041(15) 0.0006(15) -0.0024(16) C21 0.0251(16) 0.0266(15) 0.0221(14) -0.0071(12) -0.0025(12) -0.0020(13) C22 0.0277(17) 0.0334(18) 0.0307(17) -0.0104(14) -0.0027(14) -0.0060(14) C23 0.042(2) 0.048(2) 0.0339(19) -0.0199(17) -0.0076(16) -0.0101(18) C24 0.043(2) 0.063(3) 0.0340(19) -0.0263(19) 0.0018(17) -0.006(2) C25 0.0303(19) 0.063(3) 0.037(2) -0.0209(19) 0.0087(16) -0.0103(18) C26 0.0276(17) 0.043(2) 0.0292(17) -0.0137(15) 0.0010(14) -0.0090(15) C27 0.0376(19) 0.0273(17) 0.0300(17) -0.0014(13) 0.0013(15) -0.0059(14) C28 0.0236(16) 0.0402(19) 0.0296(17) -0.0157(14) -0.0015(13) -0.0064(14) C31 0.0316(18) 0.0336(18) 0.0224(15) -0.0090(13) 0.0068(13) -0.0081(14) C32 0.049(2) 0.040(2) 0.0294(18) -0.0108(15) -0.0016(16) 0.0018(17) C33 0.054(3) 0.078(3) 0.034(2) -0.022(2) -0.013(2) 0.019(3) C34 0.039(2) 0.124(5) 0.054(3) -0.049(3) -0.003(2) -0.014(3) C35 0.064(3) 0.105(5) 0.047(3) -0.034(3) 0.013(2) -0.052(3) C36 0.054(2) 0.051(2) 0.0316(19) -0.0121(17) 0.0071(17) -0.027(2) C37 0.050(3) 0.071(3) 0.036(2) -0.013(2) 0.0120(18) -0.039(2) C38 0.055(3) 0.062(3) 0.043(2) -0.026(2) -0.005(2) 0.017(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 Re1 Cl1 2.5415(8) . ? Re1 Cl2 2.4952(8) . ? Re1 P1 2.4489(8) . ? Re1 P2 2.3802(8) . ? Re1 P3 2.4347(8) . ? Re1 C1 1.755(3) . ? P1 C11 1.829(3) . ? P1 C17 1.820(4) . ? P1 C18 1.822(4) . ? P2 C21 1.837(3) . ? P2 C27 1.827(3) . ? P2 C28 1.821(3) . ? P3 C31 1.825(4) . ? P3 C37 1.815(4) . ? P3 C38 1.822(4) . ? F1 C9 1.323(6) . ? F2 C9 1.346(6) . ? F3 C9 1.339(5) . ? C1 C2 1.493(5) . ? C2 C3 1.515(5) . ? C3 C4 1.384(5) . ? C3 C8 1.397(6) . ? C4 C5 1.384(6) . ? C5 C6 1.383(6) . ? C6 C7 1.393(6) . ? C6 C9 1.496(6) . ? C7 C8 1.381(6) . ? C11 C12 1.385(5) . ? C11 C16 1.394(5) . ? C12 C13 1.396(6) . ? C13 C14 1.379(7) . ? C14 C15 1.377(6) . ? C15 C16 1.382(5) . ? C21 C22 1.395(5) . ? C21 C26 1.396(5) . ? C22 C23 1.391(5) . ? C23 C24 1.389(6) . ? C24 C25 1.380(6) . ? C25 C26 1.386(5) . ? C31 C32 1.391(5) . ? C31 C36 1.390(5) . ? C32 C33 1.401(7) . ? C33 C34 1.358(9) . ? C34 C35 1.378(9) . ? C35 C36 1.375(7) . ? 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 Cl2 Re1 Cl1 84.65(3) . . ? P1 Re1 Cl1 88.56(3) . . ? P1 Re1 Cl2 83.51(3) . . ? P2 Re1 Cl1 82.31(3) . . ? P2 Re1 Cl2 166.93(3) . . ? P2 Re1 P1 96.88(3) . . ? P2 Re1 P3 94.42(3) . . ? P3 Re1 Cl1 88.11(3) . . ? P3 Re1 Cl2 84.37(3) . . ? P3 Re1 P1 167.68(3) . . ? C1 Re1 Cl1 171.86(12) . . ? C1 Re1 Cl2 103.48(12) . . ? C1 Re1 P1 92.62(11) . . ? C1 Re1 P2 89.56(12) . . ? C1 Re1 P3 92.35(11) . . ? C11 P1 Re1 120.61(11) . . ? C17 P1 Re1 115.50(13) . . ? C17 P1 C11 104.62(18) . . ? C17 P1 C18 102.0(2) . . ? C18 P1 Re1 112.68(14) . . ? C18 P1 C11 98.73(17) . . ? C21 P2 Re1 118.65(11) . . ? C27 P2 Re1 116.44(13) . . ? C27 P2 C21 99.20(16) . . ? C28 P2 Re1 115.64(12) . . ? C28 P2 C21 103.23(15) . . ? C28 P2 C27 100.85(18) . . ? C31 P3 Re1 117.71(11) . . ? C37 P3 Re1 117.46(14) . . ? C37 P3 C31 103.59(19) . . ? C37 P3 C38 101.0(3) . . ? C38 P3 Re1 113.64(16) . . ? C38 P3 C31 100.9(2) . . ? C2 C1 Re1 173.6(3) . . ? C1 C2 C3 114.3(3) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 C8 119.4(4) . . ? C8 C3 C2 120.6(3) . . ? C5 C4 C3 120.7(4) . . ? C6 C5 C4 119.9(4) . . ? C5 C6 C7 119.8(4) . . ? C5 C6 C9 119.4(4) . . ? C7 C6 C9 120.8(4) . . ? C8 C7 C6 120.3(4) . . ? C7 C8 C3 119.9(4) . . ? F1 C9 F2 107.0(4) . . ? F1 C9 F3 106.8(4) . . ? F1 C9 C6 113.5(4) . . ? F2 C9 C6 112.3(4) . . ? F3 C9 F2 104.8(4) . . ? F3 C9 C6 111.9(4) . . ? C12 C11 P1 123.2(3) . . ? C12 C11 C16 118.7(3) . . ? C16 C11 P1 117.9(3) . . ? C11 C12 C13 120.2(4) . . ? C14 C13 C12 120.4(4) . . ? C15 C14 C13 119.7(4) . . ? C14 C15 C16 120.1(4) . . ? C15 C16 C11 120.9(4) . . ? C22 C21 P2 119.0(3) . . ? C22 C21 C26 119.4(3) . . ? C26 C21 P2 121.5(3) . . ? C23 C22 C21 120.0(3) . . ? C24 C23 C22 120.2(4) . . ? C25 C24 C23 119.6(4) . . ? C24 C25 C26 120.8(4) . . ? C25 C26 C21 119.9(3) . . ? C32 C31 P3 122.9(3) . . ? C36 C31 P3 119.2(3) . . ? C36 C31 C32 117.9(4) . . ? C31 C32 C33 119.7(4) . . ? C34 C33 C32 120.4(5) . . ? C33 C34 C35 121.1(5) . . ? C36 C35 C34 118.4(5) . . ? C35 C36 C31 122.4(5) . . ? data_chen132cult_cpd9 _database_code_depnum_ccdc_archive 'CCDC 919238' #TrackingRef 'chen132_134_135.cif' _audit_creation_date 2012-05-21 _audit_creation_method ; Olex2 1.2-beta (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H39 Cl2 F3 P3 Re' _chemical_formula_sum 'C33 H39 Cl2 F3 P3 Re' _chemical_formula_weight 842.65 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 '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 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.4371(2) _cell_length_b 13.1854(4) _cell_length_c 13.7827(5) _cell_angle_alpha 103.898(3) _cell_angle_beta 93.937(2) _cell_angle_gamma 95.447(2) _cell_volume 1649.84(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9006 _cell_measurement_temperature 173.00(14) _cell_measurement_theta_max 71.4071 _cell_measurement_theta_min 7.6209 _exptl_absorpt_coefficient_mu 10.402 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.30450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 836 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_special_details ; 'There is a rotational disorder of CF3 group which has been split into three sets of disorder CF3 groups with F(1), F(2) and F(3) as PART 1; F(1A), F(2A) and F(3A) as PART 2; and F(1B), F(2B) and F(3B) as PART 3. Their occupancies are 0.40, 0.30 and 0.30 respectively.' ; _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_unetI/netI 0.0255 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9611 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.49 _diffrn_reflns_theta_min 7.63 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 39.00 76.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -111.0000 150.0000 37 #__ type_ start__ end____ width___ exp.time_ 2 omega 32.00 77.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -178.0000 -60.0000 45 #__ type_ start__ end____ width___ exp.time_ 3 omega -16.00 72.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -99.0000 150.0000 88 #__ type_ start__ end____ width___ exp.time_ 4 omega 29.00 127.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 38.0000 0.0000 98 #__ type_ start__ end____ width___ exp.time_ 5 omega 34.00 124.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 57.0000 -120.0000 90 #__ type_ start__ end____ width___ exp.time_ 6 omega -111.00 -7.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 111.0000 30.0000 104 #__ type_ start__ end____ width___ exp.time_ 7 omega -70.00 -20.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 38.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 8 omega 47.00 72.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 9 omega 37.00 69.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 90.0000 32 #__ type_ start__ end____ width___ exp.time_ 10 omega 40.00 71.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 0.0000 31 #__ type_ start__ end____ width___ exp.time_ 11 omega 44.00 70.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 12 omega 39.00 71.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -90.0000 32 #__ type_ start__ end____ width___ exp.time_ 13 omega 45.00 146.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -90.0000 101 #__ type_ start__ end____ width___ exp.time_ 14 omega 40.00 71.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -120.0000 31 #__ type_ start__ end____ width___ exp.time_ 15 omega 105.00 131.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -64.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 16 omega 122.00 147.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 17 omega 38.00 107.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 -180.0000 69 #__ type_ start__ end____ width___ exp.time_ 18 omega 46.00 122.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 60.0000 76 #__ type_ start__ end____ width___ exp.time_ 19 omega 38.00 102.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 12.0000 -180.0000 64 #__ type_ start__ end____ width___ exp.time_ 20 omega 119.00 174.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 12.0000 -180.0000 55 #__ type_ start__ end____ width___ exp.time_ 21 omega 43.00 75.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -64.0000 -30.0000 32 #__ type_ start__ end____ width___ exp.time_ 22 omega 52.00 103.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -159.0000 -65.0000 51 #__ type_ start__ end____ width___ exp.time_ 23 omega 87.00 173.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 64.0000 30.0000 86 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0174420000 _diffrn_orient_matrix_UB_12 -0.1092082000 _diffrn_orient_matrix_UB_13 -0.0743215000 _diffrn_orient_matrix_UB_21 -0.0339710000 _diffrn_orient_matrix_UB_22 0.0507972000 _diffrn_orient_matrix_UB_23 -0.0872807000 _diffrn_orient_matrix_UB_31 0.1602425000 _diffrn_orient_matrix_UB_32 0.0132040000 _diffrn_orient_matrix_UB_33 -0.0153452000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35 _diffrn_source_power 1.75 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5731 _reflns_number_total 5800 _reflns_odcompleteness_completeness 98.07 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.038 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 394 _refine_ls_number_reflns 5800 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0270 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+1.1565P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.0702 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap 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 0.663682(12) 0.802851(9) 0.696815(8) 0.01719(7) Uani 1 1 d . . . Cl1 Cl 0.41513(8) 0.72105(6) 0.70076(6) 0.02781(16) Uani 1 1 d . . . Cl2 Cl 0.56550(8) 0.78213(6) 0.52110(5) 0.02601(16) Uani 1 1 d . . . P1 P 0.85480(8) 0.89590(6) 0.63211(5) 0.01902(15) Uani 1 1 d . . . P2 P 0.72930(8) 0.62321(6) 0.63690(6) 0.02096(16) Uani 1 1 d . . . P3 P 0.55376(8) 0.96327(6) 0.75580(6) 0.02259(16) Uani 1 1 d . . . F1 F 0.4274(6) 0.6216(7) 1.1871(6) 0.0202(14) Uiso 0.40 1 d PD A 1 F1A F 0.4416(9) 0.6531(8) 1.2120(7) 0.038(2) Uiso 0.30 1 d PD A 3 F1B F 0.4390(11) 0.5950(9) 1.1725(9) 0.052(4) Uiso 0.30 1 d PD A 2 F2 F 0.6330(8) 0.5631(6) 1.1809(6) 0.0279(12) Uiso 0.40 1 d PD A 1 F2A F 0.5843(12) 0.5393(7) 1.1578(7) 0.044(2) Uiso 0.30 1 d PD A 3 F2B F 0.6657(10) 0.5954(8) 1.2079(8) 0.044(2) Uiso 0.30 1 d PD A 2 F3 F 0.6172(10) 0.7226(6) 1.2705(4) 0.0318(15) Uiso 0.40 1 d PD A 1 F3A F 0.6597(10) 0.6865(9) 1.2635(7) 0.050(2) Uiso 0.30 1 d PD A 3 F3B F 0.5723(13) 0.7300(7) 1.2676(6) 0.043(3) Uiso 0.30 1 d PD A 2 C1 C 0.8367(4) 0.8373(3) 0.8172(2) 0.0228(6) Uani 1 1 d . . . H1A H 0.9149 0.7918 0.8098 0.027 Uiso 1 1 calc R . . H1B H 0.8670 0.9121 0.8514 0.027 Uiso 1 1 calc R . . C2 C 0.7024(3) 0.7933(2) 0.8337(2) 0.0240(6) Uani 1 1 d . . . C3 C 0.6575(3) 0.7611(3) 0.9225(2) 0.0235(6) Uani 1 1 d . . . C4 C 0.7562(4) 0.7837(3) 1.0072(3) 0.0313(7) Uani 1 1 d . . . H4 H 0.8454 0.8234 1.0066 0.038 Uiso 1 1 calc R . . C5 C 0.7273(4) 0.7496(3) 1.0921(3) 0.0361(8) Uani 1 1 d . . . H5 H 0.7964 0.7653 1.1486 0.043 Uiso 1 1 calc R . . C6 C 0.5971(4) 0.6926(3) 1.0942(3) 0.0287(7) Uani 1 1 d . A . C7 C 0.4957(4) 0.6721(3) 1.0121(3) 0.0366(8) Uani 1 1 d . . . H7 H 0.4055 0.6345 1.0142 0.044 Uiso 1 1 calc R . . C8 C 0.5246(4) 0.7059(3) 0.9271(3) 0.0369(8) Uani 1 1 d . . . H8 H 0.4540 0.6915 0.8715 0.044 Uiso 1 1 calc R . . C9 C 0.5694(4) 0.6494(3) 1.1827(3) 0.0335(8) Uani 1 1 d D . . C11 C 0.9585(3) 0.8206(2) 0.5387(2) 0.0215(6) Uani 1 1 d . . . C12 C 1.0907(3) 0.7906(2) 0.5664(2) 0.0247(6) Uani 1 1 d . . . H12 H 1.1277 0.8095 0.6350 0.030 Uiso 1 1 calc R . . C13 C 1.1685(4) 0.7332(3) 0.4943(3) 0.0293(7) Uani 1 1 d . . . H13 H 1.2588 0.7142 0.5137 0.035 Uiso 1 1 calc R . . C14 C 1.1148(4) 0.7041(3) 0.3951(3) 0.0314(7) Uani 1 1 d . . . H14 H 1.1674 0.6641 0.3463 0.038 Uiso 1 1 calc R . . C15 C 0.9843(4) 0.7331(3) 0.3663(3) 0.0305(7) Uani 1 1 d . . . H15 H 0.9475 0.7129 0.2977 0.037 Uiso 1 1 calc R . . C16 C 0.9073(3) 0.7912(3) 0.4369(2) 0.0238(6) Uani 1 1 d . . . H16 H 0.8184 0.8116 0.4162 0.029 Uiso 1 1 calc R . . C17 C 0.9981(3) 0.9819(3) 0.7177(2) 0.0277(7) Uani 1 1 d . . . H17A H 0.9565 1.0347 0.7669 0.042 Uiso 1 1 calc R . . H17B H 1.0612 1.0172 0.6793 0.042 Uiso 1 1 calc R . . H17C H 1.0533 0.9399 0.7527 0.042 Uiso 1 1 calc R . . C18 C 0.7976(4) 0.9916(3) 0.5648(3) 0.0269(6) Uani 1 1 d . . . H18A H 0.7166 0.9586 0.5155 0.040 Uiso 1 1 calc R . . H18B H 0.8770 1.0152 0.5303 0.040 Uiso 1 1 calc R . . H18C H 0.7688 1.0521 0.6128 0.040 Uiso 1 1 calc R . . C21 C 0.8676(4) 0.5865(2) 0.7181(3) 0.0246(6) Uani 1 1 d . . . C22 C 0.8294(4) 0.5559(3) 0.8039(3) 0.0275(7) Uani 1 1 d . . . H22 H 0.7330 0.5551 0.8198 0.033 Uiso 1 1 calc R . . C23 C 0.9314(4) 0.5268(3) 0.8660(3) 0.0332(7) Uani 1 1 d . . . H23 H 0.9041 0.5061 0.9242 0.040 Uiso 1 1 calc R . . C24 C 1.0719(4) 0.5273(3) 0.8444(3) 0.0348(8) Uani 1 1 d . . . H24 H 1.1407 0.5061 0.8868 0.042 Uiso 1 1 calc R . . C25 C 1.1119(4) 0.5592(3) 0.7603(3) 0.0377(8) Uani 1 1 d . . . H25 H 1.2089 0.5611 0.7457 0.045 Uiso 1 1 calc R . . C26 C 1.0104(4) 0.5882(3) 0.6976(3) 0.0318(7) Uani 1 1 d . . . H26 H 1.0385 0.6095 0.6400 0.038 Uiso 1 1 calc R . . C27 C 0.5815(4) 0.5221(3) 0.6330(3) 0.0303(7) Uani 1 1 d . . . H27A H 0.5414 0.5354 0.6980 0.045 Uiso 1 1 calc R . . H27B H 0.6165 0.4529 0.6188 0.045 Uiso 1 1 calc R . . H27C H 0.5074 0.5236 0.5802 0.045 Uiso 1 1 calc R . . C28 C 0.7869(4) 0.5776(3) 0.5114(3) 0.0300(7) Uani 1 1 d . . . H28A H 0.7213 0.5965 0.4621 0.045 Uiso 1 1 calc R . . H28B H 0.7866 0.5010 0.4953 0.045 Uiso 1 1 calc R . . H28C H 0.8837 0.6108 0.5095 0.045 Uiso 1 1 calc R . . C31 C 0.6734(4) 1.0764(3) 0.8302(2) 0.0269(7) Uani 1 1 d . . . C32 C 0.7296(4) 1.0715(3) 0.9254(3) 0.0320(7) Uani 1 1 d . . . H32 H 0.7009 1.0125 0.9506 0.038 Uiso 1 1 calc R . . C33 C 0.8266(5) 1.1522(4) 0.9830(3) 0.0449(10) Uani 1 1 d . . . H33 H 0.8641 1.1486 1.0477 0.054 Uiso 1 1 calc R . . C34 C 0.8693(4) 1.2381(3) 0.9468(4) 0.0481(11) Uani 1 1 d . . . H34 H 0.9372 1.2929 0.9861 0.058 Uiso 1 1 calc R . . C35 C 0.8135(4) 1.2443(3) 0.8536(3) 0.0418(9) Uani 1 1 d . . . H35 H 0.8427 1.3036 0.8289 0.050 Uiso 1 1 calc R . . C36 C 0.7146(4) 1.1641(3) 0.7958(3) 0.0333(7) Uani 1 1 d . . . H36 H 0.6750 1.1695 0.7322 0.040 Uiso 1 1 calc R . . C37 C 0.4190(4) 0.9543(3) 0.8437(3) 0.0360(8) Uani 1 1 d . . . H37A H 0.3357 0.9061 0.8086 0.054 Uiso 1 1 calc R . . H37B H 0.3896 1.0241 0.8705 0.054 Uiso 1 1 calc R . . H37C H 0.4594 0.9279 0.8989 0.054 Uiso 1 1 calc R . . C38 C 0.4530(4) 1.0111(3) 0.6619(3) 0.0336(8) Uani 1 1 d . . . H38A H 0.5177 1.0304 0.6149 0.050 Uiso 1 1 calc R . . H38B H 0.4086 1.0728 0.6951 0.050 Uiso 1 1 calc R . . H38C H 0.3785 0.9557 0.6251 0.050 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 0.01483(9) 0.02236(9) 0.01528(9) 0.00829(6) -0.00015(5) -0.00149(6) Cl1 0.0185(3) 0.0408(4) 0.0255(4) 0.0153(3) -0.0013(3) -0.0061(3) Cl2 0.0239(4) 0.0354(4) 0.0186(3) 0.0104(3) -0.0024(3) -0.0035(3) P1 0.0179(3) 0.0221(3) 0.0175(3) 0.0078(3) 0.0004(3) -0.0024(3) P2 0.0223(4) 0.0210(4) 0.0197(3) 0.0079(3) -0.0001(3) -0.0027(3) P3 0.0200(4) 0.0278(4) 0.0215(4) 0.0088(3) 0.0017(3) 0.0039(3) C1 0.0257(16) 0.0264(15) 0.0163(14) 0.0084(12) -0.0024(12) -0.0016(12) C2 0.0229(15) 0.0244(15) 0.0275(16) 0.0117(12) -0.0015(12) 0.0062(12) C3 0.0253(16) 0.0277(15) 0.0191(14) 0.0081(12) 0.0021(12) 0.0051(12) C4 0.0253(16) 0.0419(19) 0.0282(17) 0.0152(15) -0.0015(13) -0.0022(14) C5 0.0323(18) 0.054(2) 0.0252(17) 0.0196(16) -0.0031(14) -0.0020(16) C6 0.0313(17) 0.0328(17) 0.0255(16) 0.0116(13) 0.0061(13) 0.0070(14) C7 0.0299(18) 0.054(2) 0.0274(17) 0.0177(16) 0.0020(14) -0.0067(16) C8 0.0288(18) 0.057(2) 0.0268(17) 0.0198(16) -0.0028(14) -0.0074(16) C9 0.0347(19) 0.043(2) 0.0287(17) 0.0187(15) 0.0048(14) 0.0092(16) C11 0.0226(15) 0.0223(14) 0.0205(14) 0.0095(11) 0.0020(12) -0.0027(11) C12 0.0253(15) 0.0255(15) 0.0239(15) 0.0102(12) -0.0023(12) -0.0014(12) C13 0.0219(16) 0.0333(17) 0.0361(18) 0.0144(14) 0.0044(13) 0.0044(13) C14 0.0360(19) 0.0322(17) 0.0312(18) 0.0130(14) 0.0131(15) 0.0091(15) C15 0.0363(19) 0.0338(17) 0.0220(15) 0.0090(13) 0.0028(14) 0.0020(14) C16 0.0202(14) 0.0300(15) 0.0231(15) 0.0116(12) 0.0011(12) 0.0005(12) C17 0.0232(15) 0.0324(17) 0.0237(15) 0.0052(13) -0.0007(12) -0.0100(13) C18 0.0267(16) 0.0284(16) 0.0288(16) 0.0134(13) 0.0047(13) 0.0019(13) C21 0.0319(17) 0.0173(14) 0.0252(16) 0.0080(12) 0.0011(13) -0.0003(12) C22 0.0308(17) 0.0266(16) 0.0242(16) 0.0054(13) 0.0022(13) 0.0012(13) C23 0.044(2) 0.0298(17) 0.0248(16) 0.0087(13) -0.0021(15) 0.0012(15) C24 0.038(2) 0.0323(17) 0.0354(18) 0.0110(15) -0.0059(15) 0.0088(15) C25 0.0273(18) 0.041(2) 0.048(2) 0.0178(17) 0.0023(16) 0.0031(15) C26 0.0307(18) 0.0314(17) 0.0390(19) 0.0198(15) 0.0032(15) 0.0029(14) C27 0.0285(17) 0.0286(16) 0.0323(17) 0.0104(13) -0.0012(13) -0.0086(13) C28 0.0366(18) 0.0277(16) 0.0247(16) 0.0049(13) 0.0057(14) 0.0006(14) C31 0.0245(16) 0.0286(16) 0.0262(16) 0.0026(13) 0.0045(13) 0.0059(13) C32 0.0297(17) 0.0384(18) 0.0266(17) 0.0043(14) 0.0028(14) 0.0064(14) C33 0.037(2) 0.056(3) 0.0325(19) -0.0060(18) -0.0038(16) 0.0079(19) C34 0.035(2) 0.041(2) 0.054(3) -0.0134(19) 0.0021(18) -0.0018(17) C35 0.043(2) 0.0282(18) 0.050(2) -0.0007(16) 0.0139(18) 0.0013(16) C36 0.0368(19) 0.0289(17) 0.0347(18) 0.0061(14) 0.0089(15) 0.0075(14) C37 0.0269(17) 0.044(2) 0.039(2) 0.0114(16) 0.0124(15) 0.0039(15) C38 0.0317(18) 0.0392(19) 0.0325(18) 0.0129(15) -0.0042(15) 0.0114(15) _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 Cl1 2.4967(7) . ? Re1 Cl2 2.4747(7) . ? Re1 P1 2.4249(7) . ? Re1 P2 2.4668(8) . ? Re1 P3 2.4325(8) . ? Re1 C1 2.179(3) . ? Re1 C2 1.933(3) . ? P1 C11 1.829(3) . ? P1 C17 1.832(3) . ? P1 C18 1.835(3) . ? P2 C21 1.837(3) . ? P2 C27 1.824(3) . ? P2 C28 1.828(3) . ? P3 C31 1.827(3) . ? P3 C37 1.831(4) . ? P3 C38 1.820(4) . ? F1 C9 1.365(7) . ? F1A C9 1.299(8) . ? F1B C9 1.344(10) . ? F2 C9 1.332(6) . ? F2A C9 1.432(8) . ? F2B C9 1.286(8) . ? F3 C9 1.372(7) . ? F3A C9 1.318(9) . ? F3B C9 1.376(9) . ? C1 C2 1.400(5) . ? C2 C3 1.465(4) . ? C3 C4 1.396(5) . ? C3 C8 1.402(5) . ? C4 C5 1.386(5) . ? C5 C6 1.384(5) . ? C6 C7 1.387(5) . ? C6 C9 1.493(5) . ? C7 C8 1.384(5) . ? C11 C12 1.399(5) . ? C11 C16 1.401(4) . ? C12 C13 1.395(5) . ? C13 C14 1.374(5) . ? C14 C15 1.384(5) . ? C15 C16 1.381(5) . ? C21 C22 1.396(5) . ? C21 C26 1.395(5) . ? C22 C23 1.386(5) . ? C23 C24 1.378(6) . ? C24 C25 1.388(6) . ? C25 C26 1.388(5) . ? C31 C32 1.400(5) . ? C31 C36 1.385(5) . ? C32 C33 1.382(6) . ? C33 C34 1.381(7) . ? C34 C35 1.379(7) . ? C35 C36 1.389(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Re1 Cl1 79.08(2) . . ? P1 Re1 Cl1 156.26(2) . . ? P1 Re1 Cl2 78.40(2) . . ? P1 Re1 P2 98.10(3) . . ? P1 Re1 P3 91.88(3) . . ? P2 Re1 Cl1 87.44(3) . . ? P2 Re1 Cl2 85.31(3) . . ? P3 Re1 Cl1 81.68(3) . . ? P3 Re1 Cl2 92.51(3) . . ? P3 Re1 P2 169.12(3) . . ? C1 Re1 Cl1 127.04(9) . . ? C1 Re1 Cl2 153.38(9) . . ? C1 Re1 P1 76.22(9) . . ? C1 Re1 P2 90.41(9) . . ? C1 Re1 P3 96.20(9) . . ? C2 Re1 Cl1 87.82(10) . . ? C2 Re1 Cl2 166.09(10) . . ? C2 Re1 P1 115.16(10) . . ? C2 Re1 P2 89.48(9) . . ? C2 Re1 P3 90.19(9) . . ? C2 Re1 C1 39.23(13) . . ? C11 P1 Re1 118.82(10) . . ? C11 P1 C17 100.77(15) . . ? C11 P1 C18 99.81(15) . . ? C17 P1 Re1 120.59(11) . . ? C17 P1 C18 98.05(16) . . ? C18 P1 Re1 114.92(11) . . ? C21 P2 Re1 115.09(10) . . ? C27 P2 Re1 112.64(12) . . ? C27 P2 C21 101.50(16) . . ? C27 P2 C28 100.37(17) . . ? C28 P2 Re1 121.39(11) . . ? C28 P2 C21 103.13(16) . . ? C31 P3 Re1 115.81(11) . . ? C31 P3 C37 100.12(17) . . ? C37 P3 Re1 114.73(13) . . ? C38 P3 Re1 117.07(13) . . ? C38 P3 C31 106.02(17) . . ? C38 P3 C37 100.76(19) . . ? C2 C1 Re1 60.83(17) . . ? C1 C2 Re1 79.9(2) . . ? C1 C2 C3 129.1(3) . . ? C3 C2 Re1 150.8(3) . . ? C4 C3 C2 117.5(3) . . ? C4 C3 C8 117.9(3) . . ? C8 C3 C2 124.6(3) . . ? C5 C4 C3 121.7(3) . . ? C6 C5 C4 119.6(3) . . ? C5 C6 C7 119.7(3) . . ? C5 C6 C9 119.8(3) . . ? C7 C6 C9 120.5(3) . . ? C8 C7 C6 120.7(4) . . ? C7 C8 C3 120.4(3) . . ? F1 C9 F2A 87.0(6) . . ? F1 C9 F3 106.9(6) . . ? F1 C9 F3B 90.7(7) . . ? F1 C9 C6 112.6(4) . . ? F1A C9 F1 20.2(5) . . ? F1A C9 F1B 36.3(7) . . ? F1A C9 F2 118.7(6) . . ? F1A C9 F2A 103.5(6) . . ? F1A C9 F3 87.4(6) . . ? F1A C9 F3A 106.7(7) . . ? F1A C9 F3B 70.6(7) . . ? F1A C9 C6 116.5(5) . . ? F1B C9 F1 16.5(6) . . ? F1B C9 F2A 71.2(7) . . ? F1B C9 F3 120.2(7) . . ? F1B C9 F3B 105.6(8) . . ? F1B C9 C6 112.5(6) . . ? F2 C9 F1 106.0(6) . . ? F2 C9 F1B 91.6(7) . . ? F2 C9 F2A 23.1(4) . . ? F2 C9 F3 108.4(6) . . ? F2 C9 F3B 123.1(6) . . ? F2 C9 C6 112.0(4) . . ? F2A C9 C6 109.2(4) . . ? F2B C9 F1 121.8(6) . . ? F2B C9 F1A 127.1(6) . . ? F2B C9 F1B 110.4(8) . . ? F2B C9 F2 24.0(4) . . ? F2B C9 F2A 46.9(6) . . ? F2B C9 F3 85.7(7) . . ? F2B C9 F3A 58.3(7) . . ? F2B C9 F3B 102.3(7) . . ? F2B C9 C6 114.9(5) . . ? F3 C9 F2A 127.8(6) . . ? F3 C9 F3B 18.6(5) . . ? F3 C9 C6 110.7(4) . . ? F3A C9 F1 122.7(6) . . ? F3A C9 F1B 129.6(7) . . ? F3A C9 F2 81.6(6) . . ? F3A C9 F2A 102.9(7) . . ? F3A C9 F3 27.7(4) . . ? F3A C9 F3B 45.6(6) . . ? F3A C9 C6 116.3(5) . . ? F3B C9 F2A 138.0(6) . . ? F3B C9 C6 110.2(5) . . ? C12 C11 P1 121.3(2) . . ? C12 C11 C16 118.1(3) . . ? C16 C11 P1 120.6(2) . . ? C13 C12 C11 120.6(3) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 120.1(3) . . ? C16 C15 C14 120.3(3) . . ? C15 C16 C11 120.8(3) . . ? C22 C21 P2 119.1(3) . . ? C26 C21 P2 122.4(3) . . ? C26 C21 C22 118.5(3) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 120.8(3) . . ? C23 C24 C25 119.5(3) . . ? C24 C25 C26 120.0(4) . . ? C25 C26 C21 120.8(3) . . ? C32 C31 P3 117.6(3) . . ? C36 C31 P3 123.4(3) . . ? C36 C31 C32 118.9(3) . . ? C33 C32 C31 120.3(4) . . ? C34 C33 C32 120.2(4) . . ? C35 C34 C33 120.0(4) . . ? C34 C35 C36 120.1(4) . . ? C31 C36 C35 120.4(4) . . ? data_chen134cult_cpd10 _database_code_depnum_ccdc_archive 'CCDC 919239' #TrackingRef 'chen132_134_135.cif' _audit_creation_date 2012-05-29 _audit_creation_method ; Olex2 1.2-beta (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H39 Cl2 F3 P3 Re, 0.25(C H3 O H)' _chemical_formula_sum 'C33.25 H40 Cl2 F3 O0.25 P3 Re' _chemical_formula_weight 850.66 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 '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 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.7952(3) _cell_length_b 12.6871(4) _cell_length_c 13.8264(4) _cell_angle_alpha 90.643(3) _cell_angle_beta 98.261(2) _cell_angle_gamma 108.650(3) _cell_volume 1772.30(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9626 _cell_measurement_temperature 173.00(14) _cell_measurement_theta_max 71.4416 _cell_measurement_theta_min 4.7141 _exptl_absorpt_coefficient_mu 9.694 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 845 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_unetI/netI 0.0280 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10283 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 66.98 _diffrn_reflns_theta_min 5.46 _diffrn_ambient_temperature 173.00(14) _diffrn_detector_area_resol_mean 15.9578 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 38.00 65.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -120.0000 27 #__ type_ start__ end____ width___ exp.time_ 2 omega -24.00 40.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 0.0000 64 #__ type_ start__ end____ width___ exp.time_ 3 omega -75.00 14.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 57.0000 -30.0000 89 #__ type_ start__ end____ width___ exp.time_ 4 omega 46.00 120.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 57.0000 60.0000 74 #__ type_ start__ end____ width___ exp.time_ 5 omega 4.00 71.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -38.0000 60.0000 67 #__ type_ start__ end____ width___ exp.time_ 6 omega -141.00 -65.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 178.0000 -60.0000 76 #__ type_ start__ end____ width___ exp.time_ 7 omega -131.00 -34.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -77.0000 -150.0000 97 #__ type_ start__ end____ width___ exp.time_ 8 omega 40.00 65.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 9 omega 123.00 149.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 26.0000 26 #__ type_ start__ end____ width___ exp.time_ 10 omega 41.00 68.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 11 omega 40.00 66.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 12 omega 40.00 67.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 13 omega 38.00 71.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 60.0000 33 #__ type_ start__ end____ width___ exp.time_ 14 omega 38.00 69.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 -180.0000 31 #__ type_ start__ end____ width___ exp.time_ 15 omega 37.00 63.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 16 omega 44.00 69.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 17 omega 45.00 82.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -90.0000 37 #__ type_ start__ end____ width___ exp.time_ 18 omega 42.00 71.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -38.0000 120.0000 29 #__ type_ start__ end____ width___ exp.time_ 19 omega 47.00 176.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 0.0000 -60.0000 129 #__ type_ start__ end____ width___ exp.time_ 20 omega 40.00 102.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 26.0000 62 #__ type_ start__ end____ width___ exp.time_ 21 omega 95.00 177.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 64.0000 -30.0000 82 #__ type_ start__ end____ width___ exp.time_ 22 omega 50.00 148.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -92.0000 90.0000 98 #__ type_ start__ end____ width___ exp.time_ 23 omega 53.00 130.00 1.0000 17.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -93.0000 -112.0000 77 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0184868000 _diffrn_orient_matrix_UB_12 0.1133234000 _diffrn_orient_matrix_UB_13 -0.0453797000 _diffrn_orient_matrix_UB_21 -0.0403129000 _diffrn_orient_matrix_UB_22 -0.0589572000 _diffrn_orient_matrix_UB_23 -0.1031739000 _diffrn_orient_matrix_UB_31 -0.1458773000 _diffrn_orient_matrix_UB_32 -0.0129310000 _diffrn_orient_matrix_UB_33 0.0044350000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35 _diffrn_source_power 1.75 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6070 _reflns_number_total 6168 _reflns_odcompleteness_completeness 98.49 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.631 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.085 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 393 _refine_ls_number_reflns 6168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0212 _refine_ls_R_factor_gt 0.0208 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.0584 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.472119(7) 0.232703(6) 0.251153(6) 0.01772(5) Uani 1 1 d . . . Cl1 Cl 0.56851(6) 0.07199(5) 0.25926(4) 0.02981(12) Uani 1 1 d . . . Cl2 Cl 0.70472(5) 0.35605(5) 0.27845(4) 0.03035(12) Uani 1 1 d . . . P1 P 0.27555(5) 0.07541(4) 0.22703(4) 0.02034(11) Uani 1 1 d . . . P2 P 0.49680(6) 0.24877(5) 0.07884(4) 0.02142(12) Uani 1 1 d . . . P3 P 0.50351(6) 0.25064(5) 0.42987(4) 0.02443(13) Uani 1 1 d . . . F1 F 0.0726(2) 0.4715(2) 0.2667(3) 0.0873(9) Uani 1 1 d . . . F2 F 0.0792(3) 0.4766(2) 0.1154(3) 0.0986(11) Uani 1 1 d . . . F3 F 0.0695(3) 0.6191(2) 0.1946(3) 0.1079(13) Uani 1 1 d . . . C1 C 0.3772(2) 0.32240(18) 0.24227(16) 0.0210(4) Uani 1 1 d . . . C2 C 0.2838(2) 0.38583(18) 0.23403(18) 0.0250(4) Uani 1 1 d . . . H2A H 0.2331 0.3695 0.2894 0.030 Uiso 1 1 calc R . . H2B H 0.2200 0.3596 0.1728 0.030 Uiso 1 1 calc R . . C3 C 0.3486(2) 0.51199(18) 0.23367(16) 0.0235(4) Uani 1 1 d . . . C4 C 0.2725(3) 0.5842(2) 0.2191(2) 0.0349(6) Uani 1 1 d . . . C5 C 0.3345(3) 0.6985(2) 0.2219(2) 0.0423(7) Uani 1 1 d . . . H5 H 0.2825 0.7465 0.2128 0.051 Uiso 1 1 calc R . . C6 C 0.4702(3) 0.7433(2) 0.2377(2) 0.0396(7) Uani 1 1 d . . . H6 H 0.5115 0.8218 0.2394 0.048 Uiso 1 1 calc R . . C7 C 0.5465(3) 0.6739(2) 0.25108(19) 0.0349(5) Uani 1 1 d . . . H7 H 0.6404 0.7044 0.2616 0.042 Uiso 1 1 calc R . . C8 C 0.4849(2) 0.55874(19) 0.24906(17) 0.0267(5) Uani 1 1 d . . . H8 H 0.5379 0.5115 0.2585 0.032 Uiso 1 1 calc R . . C9 C 0.1248(4) 0.5384(3) 0.2000(4) 0.0631(11) Uani 1 1 d . . . C11 C 0.1233(2) 0.11006(18) 0.21360(17) 0.0235(4) Uani 1 1 d . . . C12 C 0.0668(2) 0.1339(2) 0.12247(18) 0.0287(5) Uani 1 1 d . . . H12 H 0.1016 0.1228 0.0653 0.034 Uiso 1 1 calc R . . C13 C -0.0398(3) 0.1738(2) 0.1148(2) 0.0372(6) Uani 1 1 d . . . H13 H -0.0779 0.1893 0.0526 0.045 Uiso 1 1 calc R . . C14 C -0.0908(3) 0.1911(2) 0.1983(2) 0.0405(6) Uani 1 1 d . . . H14 H -0.1625 0.2199 0.1933 0.049 Uiso 1 1 calc R . . C15 C -0.0369(3) 0.1663(2) 0.2885(2) 0.0384(6) Uani 1 1 d . . . H15 H -0.0724 0.1771 0.3453 0.046 Uiso 1 1 calc R . . C16 C 0.0686(2) 0.1256(2) 0.29648(19) 0.0312(5) Uani 1 1 d . . . H16 H 0.1043 0.1081 0.3587 0.037 Uiso 1 1 calc R . . C17 C 0.2490(2) -0.02109(19) 0.12156(17) 0.0280(5) Uani 1 1 d . . . H17A H 0.2423 0.0179 0.0612 0.042 Uiso 1 1 calc R . . H17B H 0.1669 -0.0832 0.1218 0.042 Uiso 1 1 calc R . . H17C H 0.3235 -0.0499 0.1249 0.042 Uiso 1 1 calc R . . C18 C 0.2546(3) -0.02540(19) 0.32193(18) 0.0304(5) Uani 1 1 d . . . H18A H 0.3302 -0.0532 0.3311 0.046 Uiso 1 1 calc R . . H18B H 0.1729 -0.0878 0.3020 0.046 Uiso 1 1 calc R . . H18C H 0.2496 0.0108 0.3836 0.046 Uiso 1 1 calc R . . C21 C 0.3504(2) 0.23363(19) -0.01154(17) 0.0242(4) Uani 1 1 d . . . C22 C 0.2931(2) 0.1425(2) -0.07953(17) 0.0291(5) Uani 1 1 d . . . H22 H 0.3314 0.0849 -0.0810 0.035 Uiso 1 1 calc R . . C23 C 0.1796(3) 0.1362(2) -0.14523(19) 0.0385(6) Uani 1 1 d . . . H23 H 0.1396 0.0732 -0.1901 0.046 Uiso 1 1 calc R . . C24 C 0.1249(3) 0.2209(3) -0.1455(2) 0.0436(7) Uani 1 1 d . . . H24 H 0.0485 0.2165 -0.1911 0.052 Uiso 1 1 calc R . . C25 C 0.1816(3) 0.3124(3) -0.0791(2) 0.0411(6) Uani 1 1 d . . . H25 H 0.1442 0.3708 -0.0792 0.049 Uiso 1 1 calc R . . C26 C 0.2929(3) 0.3183(2) -0.01284(19) 0.0306(5) Uani 1 1 d . . . H26 H 0.3311 0.3810 0.0327 0.037 Uiso 1 1 calc R . . C27 C 0.5740(3) 0.1573(3) 0.0288(2) 0.0373(6) Uani 1 1 d . . . H27A H 0.6645 0.1738 0.0635 0.056 Uiso 1 1 calc R . . H27B H 0.5764 0.1690 -0.0410 0.056 Uiso 1 1 calc R . . H27C H 0.5230 0.0796 0.0367 0.056 Uiso 1 1 calc R . . C28 C 0.6027(3) 0.3856(2) 0.0512(2) 0.0372(6) Uani 1 1 d . . . H28A H 0.5710 0.4435 0.0757 0.056 Uiso 1 1 calc R . . H28B H 0.6002 0.3889 -0.0198 0.056 Uiso 1 1 calc R . . H28C H 0.6938 0.3977 0.0828 0.056 Uiso 1 1 calc R . . C31 C 0.3613(3) 0.2155(2) 0.49423(18) 0.0327(5) Uani 1 1 d . . . C32 C 0.3278(4) 0.1204(3) 0.5477(2) 0.0517(8) Uani 1 1 d . . . H32 H 0.3825 0.0745 0.5528 0.062 Uiso 1 1 calc R . . C33 C 0.2177(5) 0.0918(4) 0.5927(3) 0.0741(14) Uani 1 1 d . . . H33 H 0.1969 0.0272 0.6294 0.089 Uiso 1 1 calc R . . C34 C 0.1381(4) 0.1571(5) 0.5846(3) 0.0826(17) Uani 1 1 d . . . H34 H 0.0593 0.1353 0.6130 0.099 Uiso 1 1 calc R . . C35 C 0.1707(4) 0.2556(4) 0.5351(3) 0.0689(12) Uani 1 1 d . . . H35 H 0.1171 0.3023 0.5326 0.083 Uiso 1 1 calc R . . C36 C 0.2833(3) 0.2841(3) 0.4893(2) 0.0445(7) Uani 1 1 d . . . H36 H 0.3064 0.3503 0.4549 0.053 Uiso 1 1 calc R . . C37 C 0.6108(4) 0.1790(3) 0.4921(2) 0.0520(8) Uani 1 1 d . . . H37A H 0.5702 0.0985 0.4777 0.078 Uiso 1 1 calc R . . H37B H 0.6234 0.1958 0.5629 0.078 Uiso 1 1 calc R . . H37C H 0.6968 0.2043 0.4693 0.078 Uiso 1 1 calc R . . C38 C 0.5881(3) 0.3941(2) 0.4781(2) 0.0380(6) Uani 1 1 d . . . H38A H 0.6775 0.4196 0.4610 0.057 Uiso 1 1 calc R . . H38B H 0.5936 0.3979 0.5495 0.057 Uiso 1 1 calc R . . H38C H 0.5386 0.4420 0.4498 0.057 Uiso 1 1 calc R . . O1S O -0.0709(10) 0.3691(8) 0.4668(7) 0.053(2) Uiso 0.25 1 d P . . C1S C -0.008(2) 0.4778(13) 0.5055(15) 0.062(4) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01884(7) 0.01466(7) 0.01998(7) 0.00197(4) 0.00278(4) 0.00597(5) Cl1 0.0332(3) 0.0249(3) 0.0367(3) 0.0045(2) 0.0058(2) 0.0166(2) Cl2 0.0211(3) 0.0319(3) 0.0338(3) -0.0005(2) 0.0020(2) 0.0037(2) P1 0.0231(3) 0.0159(2) 0.0210(2) 0.00219(19) 0.0049(2) 0.0043(2) P2 0.0216(3) 0.0206(3) 0.0215(3) 0.0024(2) 0.0046(2) 0.0054(2) P3 0.0318(3) 0.0215(3) 0.0208(3) 0.0011(2) 0.0013(2) 0.0111(2) F1 0.0443(11) 0.0721(15) 0.161(3) 0.0244(17) 0.0403(15) 0.0291(11) F2 0.0666(15) 0.0832(18) 0.130(3) -0.0202(17) -0.0516(17) 0.0321(14) F3 0.0615(14) 0.0636(15) 0.210(4) 0.0058(19) -0.0110(19) 0.0494(13) C1 0.0210(10) 0.0165(10) 0.0226(10) -0.0003(8) 0.0039(8) 0.0020(8) C2 0.0237(11) 0.0196(11) 0.0330(12) 0.0042(9) 0.0050(9) 0.0086(9) C3 0.0318(12) 0.0208(11) 0.0186(10) 0.0011(8) 0.0023(8) 0.0102(9) C4 0.0416(14) 0.0303(13) 0.0378(14) 0.0039(10) 0.0001(11) 0.0210(11) C5 0.0631(19) 0.0299(14) 0.0409(14) 0.0023(11) 0.0023(13) 0.0274(13) C6 0.065(2) 0.0170(11) 0.0346(13) 0.0034(10) 0.0099(13) 0.0091(13) C7 0.0403(14) 0.0264(12) 0.0324(12) 0.0028(10) 0.0087(10) 0.0018(10) C8 0.0326(12) 0.0214(11) 0.0262(11) 0.0023(9) 0.0045(9) 0.0089(9) C9 0.0467(18) 0.0463(19) 0.102(3) 0.003(2) -0.0061(19) 0.0311(16) C11 0.0203(10) 0.0193(10) 0.0283(11) 0.0003(8) 0.0061(8) 0.0019(8) C12 0.0253(11) 0.0279(12) 0.0306(12) 0.0005(9) 0.0060(9) 0.0049(9) C13 0.0274(12) 0.0386(14) 0.0426(14) -0.0018(11) -0.0033(11) 0.0106(10) C14 0.0233(12) 0.0412(14) 0.0564(17) -0.0073(13) 0.0043(11) 0.0108(10) C15 0.0279(12) 0.0433(15) 0.0428(15) -0.0081(12) 0.0130(11) 0.0068(11) C16 0.0290(12) 0.0308(12) 0.0307(12) -0.0013(10) 0.0080(10) 0.0040(9) C17 0.0341(12) 0.0193(10) 0.0288(11) -0.0020(9) 0.0095(9) 0.0043(9) C18 0.0394(13) 0.0205(11) 0.0272(11) 0.0058(9) 0.0061(10) 0.0033(9) C21 0.0240(10) 0.0221(11) 0.0237(10) 0.0058(8) 0.0054(8) 0.0031(8) C22 0.0342(12) 0.0271(11) 0.0226(11) 0.0049(9) 0.0066(9) 0.0042(9) C23 0.0373(14) 0.0386(14) 0.0265(12) 0.0029(10) 0.0017(10) -0.0044(11) C24 0.0324(13) 0.0529(17) 0.0387(14) 0.0161(13) -0.0029(11) 0.0078(12) C25 0.0367(14) 0.0441(15) 0.0457(15) 0.0162(13) 0.0047(12) 0.0180(12) C26 0.0324(12) 0.0282(12) 0.0314(12) 0.0060(10) 0.0035(10) 0.0107(10) C27 0.0398(14) 0.0497(16) 0.0325(13) 0.0009(11) 0.0087(11) 0.0272(12) C28 0.0348(13) 0.0339(13) 0.0319(12) 0.0088(10) 0.0051(10) -0.0044(10) C31 0.0392(13) 0.0311(13) 0.0228(11) -0.0028(9) 0.0078(10) 0.0035(10) C32 0.079(2) 0.0356(15) 0.0289(13) -0.0016(11) 0.0180(14) -0.0016(14) C33 0.088(3) 0.061(2) 0.049(2) -0.0071(17) 0.039(2) -0.022(2) C34 0.053(2) 0.121(4) 0.0414(19) -0.023(2) 0.0231(17) -0.023(2) C35 0.0482(19) 0.113(4) 0.0453(18) -0.023(2) 0.0083(16) 0.027(2) C36 0.0412(15) 0.0585(18) 0.0332(13) -0.0074(13) 0.0063(12) 0.0157(13) C37 0.072(2) 0.065(2) 0.0325(14) 0.0020(14) -0.0051(14) 0.0472(18) C38 0.0409(14) 0.0303(13) 0.0354(13) -0.0096(10) 0.0077(11) 0.0011(10) _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 Cl1 2.5655(5) . ? Re1 Cl2 2.4694(5) . ? Re1 P1 2.3812(5) . ? Re1 P2 2.4387(6) . ? Re1 P3 2.4434(6) . ? Re1 C1 1.753(2) . ? P1 C11 1.818(2) . ? P1 C17 1.823(2) . ? P1 C18 1.829(2) . ? P2 C21 1.824(2) . ? P2 C27 1.814(3) . ? P2 C28 1.827(2) . ? P3 C31 1.819(3) . ? P3 C37 1.820(3) . ? P3 C38 1.824(3) . ? F1 C9 1.322(5) . ? F2 C9 1.339(5) . ? F3 C9 1.338(4) . ? C1 C2 1.472(3) . ? C2 C3 1.529(3) . ? C3 C4 1.411(3) . ? C3 C8 1.383(4) . ? C4 C5 1.387(4) . ? C4 C9 1.494(5) . ? C5 C6 1.375(5) . ? C6 C7 1.383(4) . ? C7 C8 1.397(3) . ? C11 C12 1.399(3) . ? C11 C16 1.402(3) . ? C12 C13 1.389(4) . ? C13 C14 1.392(4) . ? C14 C15 1.382(4) . ? C15 C16 1.384(4) . ? C21 C22 1.398(3) . ? C21 C26 1.402(4) . ? C22 C23 1.396(4) . ? C23 C24 1.381(5) . ? C24 C25 1.387(5) . ? C25 C26 1.383(4) . ? C31 C32 1.397(4) . ? C31 C36 1.388(4) . ? C32 C33 1.369(6) . ? C33 C34 1.366(8) . ? C34 C35 1.400(8) . ? C35 C36 1.398(5) . ? O1S C1S 1.86(2) 2_566 ? O1S C1S 1.39(2) . ? C1S O1S 1.86(2) 2_566 ? C1S C1S 0.56(3) 2_566 ? 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 Cl2 Re1 Cl1 85.56(2) . . ? P1 Re1 Cl1 78.835(19) . . ? P1 Re1 Cl2 164.39(2) . . ? P1 Re1 P2 96.283(19) . . ? P1 Re1 P3 97.91(2) . . ? P2 Re1 Cl1 90.023(19) . . ? P2 Re1 Cl2 83.536(19) . . ? P2 Re1 P3 165.55(2) . . ? P3 Re1 Cl1 90.071(19) . . ? P3 Re1 Cl2 82.06(2) . . ? C1 Re1 Cl1 169.15(7) . . ? C1 Re1 Cl2 105.30(7) . . ? C1 Re1 P1 90.31(7) . . ? C1 Re1 P2 91.26(7) . . ? C1 Re1 P3 91.36(7) . . ? C11 P1 Re1 114.34(7) . . ? C11 P1 C17 103.03(11) . . ? C11 P1 C18 103.57(11) . . ? C17 P1 Re1 117.86(8) . . ? C17 P1 C18 98.36(11) . . ? C18 P1 Re1 117.27(8) . . ? C21 P2 Re1 118.77(8) . . ? C21 P2 C28 99.90(11) . . ? C27 P2 Re1 116.33(9) . . ? C27 P2 C21 103.81(12) . . ? C27 P2 C28 101.60(15) . . ? C28 P2 Re1 113.85(9) . . ? C31 P3 Re1 120.39(8) . . ? C31 P3 C37 104.58(16) . . ? C31 P3 C38 100.08(12) . . ? C37 P3 Re1 115.24(11) . . ? C37 P3 C38 101.56(16) . . ? C38 P3 Re1 112.41(9) . . ? C2 C1 Re1 173.25(17) . . ? C1 C2 C3 114.48(19) . . ? C4 C3 C2 121.6(2) . . ? C8 C3 C2 120.3(2) . . ? C8 C3 C4 118.0(2) . . ? C3 C4 C9 120.5(2) . . ? C5 C4 C3 120.1(3) . . ? C5 C4 C9 119.4(3) . . ? C6 C5 C4 120.9(3) . . ? C5 C6 C7 119.8(2) . . ? C6 C7 C8 119.6(3) . . ? C3 C8 C7 121.4(2) . . ? F1 C9 F2 104.5(3) . . ? F1 C9 F3 107.0(4) . . ? F1 C9 C4 114.1(3) . . ? F2 C9 C4 112.3(4) . . ? F3 C9 F2 106.3(3) . . ? F3 C9 C4 112.1(3) . . ? C12 C11 P1 120.94(18) . . ? C12 C11 C16 118.5(2) . . ? C16 C11 P1 120.16(19) . . ? C13 C12 C11 120.6(2) . . ? C12 C13 C14 120.1(3) . . ? C15 C14 C13 119.8(3) . . ? C14 C15 C16 120.5(3) . . ? C15 C16 C11 120.6(2) . . ? C22 C21 P2 123.59(19) . . ? C22 C21 C26 118.4(2) . . ? C26 C21 P2 118.02(18) . . ? C23 C22 C21 120.1(3) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 120.1(2) . . ? C26 C25 C24 119.7(3) . . ? C25 C26 C21 121.3(3) . . ? C32 C31 P3 121.6(3) . . ? C36 C31 P3 119.3(2) . . ? C36 C31 C32 119.1(3) . . ? C33 C32 C31 121.5(4) . . ? C34 C33 C32 119.4(4) . . ? C33 C34 C35 121.1(3) . . ? C36 C35 C34 119.1(4) . . ? C31 C36 C35 119.8(4) . . ? C1S O1S C1S 10.7(14) . 2_566 ? O1S C1S O1S 169.3(14) . 2_566 ? C1S C1S O1S 27(4) 2_566 2_566 ? C1S C1S O1S 142(5) 2_566 . ?