# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _audit_creation_date 2004-02-26 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; _publ_contact_author_name 'Prof Maria Parr' _publ_contact_author_address ; Department of Chemistry Trinity College Hartford Connecticut 06106 UNITED STATES OF AMERICA ; _publ_contact_author_email MARIA.PARR@TRINCOLL.EDU _publ_section_title ; Synthesis, Characterization and Structural Investigation of New Rhenium-Oxo Complexes Containing Bidentate Phosphine Ligands: An Exploration of Chirality and Conformation in Chelate Rings of Small and Large Bite Angle Ligands ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; loop_ _publ_author_name 'Maria Parr' 'J. W. Faller' 'Carmen Perez-Acosta' #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_2307ReOCl3(diphos-F20) _database_code_depnum_ccdc_archive 'CCDC 247679' _audit_creation_date 2004-02-24 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 26.7896(5) _cell_length_b 26.7896(5) _cell_length_c 22.2608(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 15976.2(4) _cell_formula_units_Z 16 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 31556 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_Int_Tables_number 88 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2-y, +z' 3/4-y,1/4+x,1/4+z 1/4+y,1/4-x,1/4+z ' -x, -y, -z' ' +x,1/2+y, -z' 3/4+y,1/4-x,1/4-z 1/4-y,1/4+x,1/4-z 1/2+x,1/2+y,1/2+z '1/2-x, -y,1/2+z' 1/4-y,3/4+x,3/4+z 3/4+y,3/4-x,3/4+z 1/2-x,1/2-y,1/2-z '1/2+x, +y,1/2-z' 1/4+y,3/4-x,3/4-z 3/4-y,3/4+x,3/4-z #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1109.89 _chemical_formula_analytical ? _chemical_formula_sum 'C29 H11 Cl3 F20 O P2 Re ' _chemical_formula_moiety 'C26 H4 Cl3 F20 O P2 Re, C3 H7 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 8464.00 _exptl_absorpt_coefficient_mu 3.442 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 30476 _reflns_number_total 9125 _reflns_number_gt 5432 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04545 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 464 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 176 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 48 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 320 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 32 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Re 0 16 -1.598 7.232 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.156692(8) 0.011588(8) 0.739762(9) 0.03227(7) 1.000 . Uani d ? Cl(1) 0.07772(5) 0.04555(6) 0.70393(6) 0.0424(4) 1.000 . Uani d ? Cl(2) 0.18391(6) 0.00913(5) 0.63966(6) 0.0428(4) 1.000 . Uani d ? Cl(3) 0.12676(6) -0.06996(6) 0.72427(6) 0.0496(5) 1.000 . Uani d ? P(1) 0.17048(5) 0.10223(5) 0.75148(6) 0.0309(4) 1.000 . Uani d ? P(2) 0.10559(6) 0.02109(6) 0.83210(6) 0.0360(4) 1.000 . Uani d ? F(1) 0.27226(11) 0.05844(12) 0.7099(2) 0.0510(11) 1.000 . Uani d ? F(2) 0.3634(1) 0.0973(2) 0.7233(2) 0.086(2) 1.000 . Uani d ? F(3) 0.3760(1) 0.1862(2) 0.7775(2) 0.091(2) 1.000 . Uani d ? F(4) 0.2948(2) 0.23899(13) 0.8159(2) 0.0698(13) 1.000 . Uani d ? F(5) 0.20314(13) 0.20212(12) 0.8012(2) 0.0534(11) 1.000 . Uani d ? F(6) 0.21302(12) 0.12274(12) 0.63070(13) 0.0463(10) 1.000 . Uani d ? F(7) 0.1862(1) 0.18971(13) 0.5481(2) 0.0622(12) 1.000 . Uani d ? F(8) 0.1048(1) 0.24819(13) 0.5661(2) 0.0609(12) 1.000 . Uani d ? F(9) 0.05374(12) 0.24189(12) 0.6708(2) 0.0536(11) 1.000 . Uani d ? F(10) 0.07911(11) 0.17563(12) 0.7538(1) 0.0466(10) 1.000 . Uani d ? F(11) 0.0604(1) 0.0455(2) 0.9518(1) 0.0681(13) 1.000 . Uani d ? F(12) 0.0887(2) 0.0196(2) 1.0611(2) 0.096(2) 1.000 . Uani d ? F(13) 0.1680(2) -0.0413(1) 1.0788(2) 0.075(1) 1.000 . Uani d ? F(14) 0.21972(13) -0.07507(13) 0.9835(2) 0.0591(12) 1.000 . Uani d ? F(15) 0.19296(13) -0.04986(12) 0.8722(1) 0.0535(11) 1.000 . Uani d ? F(16) -0.00533(12) 0.0602(1) 0.8145(2) 0.0562(12) 1.000 . Uani d ? F(17) -0.08758(13) 0.0061(2) 0.8105(2) 0.075(1) 1.000 . Uani d ? F(18) -0.0845(2) -0.0944(2) 0.8259(2) 0.090(2) 1.000 . Uani d ? F(19) 0.0041(2) -0.1399(2) 0.8472(2) 0.089(2) 1.000 . Uani d ? F(20) 0.08803(13) -0.08679(12) 0.8527(2) 0.0543(11) 1.000 . Uani d ? O(1) 0.20903(13) 0.00389(13) 0.7790(2) 0.0366(11) 1.000 . Uani d ? C(1) 0.1433(2) 0.1167(2) 0.8257(2) 0.037(2) 1.000 . Uani d ? C(2) 0.0951(2) 0.0885(2) 0.8392(2) 0.039(2) 1.000 . Uani d ? C(3) 0.2341(2) 0.1268(2) 0.7586(2) 0.033(2) 1.000 . Uani d ? C(4) 0.2766(2) 0.1028(2) 0.7382(3) 0.042(2) 1.000 . Uani d ? C(5) 0.3239(2) 0.1217(2) 0.7438(3) 0.054(2) 1.000 . Uani d ? C(6) 0.3299(2) 0.1667(3) 0.7711(3) 0.058(2) 1.000 . Uani d ? C(7) 0.2893(3) 0.1933(2) 0.7907(3) 0.049(2) 1.000 . Uani d ? C(8) 0.2421(2) 0.1736(2) 0.7833(3) 0.042(2) 1.000 . Uani d ? C(9) 0.1465(2) 0.1452(2) 0.6953(2) 0.034(2) 1.000 . Uani d ? C(10) 0.1723(2) 0.1506(2) 0.6413(2) 0.037(2) 1.000 . Uani d ? C(11) 0.1589(2) 0.1850(2) 0.5982(3) 0.041(2) 1.000 . Uani d ? C(12) 0.1181(2) 0.2148(2) 0.6079(3) 0.044(2) 1.000 . Uani d ? C(13) 0.0923(2) 0.2114(2) 0.6598(3) 0.038(2) 1.000 . Uani d ? C(14) 0.1060(2) 0.1767(2) 0.7028(2) 0.037(2) 1.000 . Uani d ? C(15) 0.1279(2) 0.0027(2) 0.9069(2) 0.036(2) 1.000 . Uani d ? C(16) 0.1017(2) 0.0178(2) 0.9576(2) 0.048(2) 1.000 . Uani d ? C(17) 0.1159(3) 0.0044(3) 1.0145(3) 0.057(2) 1.000 . Uani d ? C(18) 0.1555(3) -0.0270(3) 1.0240(3) 0.055(2) 1.000 . Uani d ? C(19) 0.1812(2) -0.0440(2) 0.9754(3) 0.044(2) 1.000 . Uani d ? C(20) 0.1675(2) -0.0298(2) 0.9176(2) 0.037(2) 1.000 . Uani d ? C(21) 0.0461(2) -0.0116(2) 0.8313(2) 0.040(2) 1.000 . Uani d ? C(22) -0.0007(2) 0.0105(3) 0.8213(2) 0.047(2) 1.000 . Uani d ? C(23) -0.0447(3) -0.0175(3) 0.8189(3) 0.056(2) 1.000 . Uani d ? C(24) -0.0421(3) -0.0683(3) 0.8270(3) 0.063(3) 1.000 . Uani d ? C(25) 0.0024(3) -0.0913(3) 0.8380(3) 0.059(2) 1.000 . Uani d ? C(26) 0.0453(2) -0.0632(3) 0.8400(3) 0.048(2) 1.000 . Uani d ? H(1) 0.1672 0.1084 0.8556 0.044 1.000 . Uiso c ? H(2) 0.1365 0.1514 0.8272 0.044 1.000 . Uiso c ? H(3) 0.0700 0.0985 0.8116 0.047 1.000 . Uiso c ? H(4) 0.0846 0.0959 0.8790 0.047 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.0391(2) 0.0339(1) 0.02377(11) -0.00194(10) 0.00111(10) -0.00453(9) Cl(1) 0.0398(8) 0.0521(9) 0.0352(8) -0.0050(7) -0.0051(6) 0.0005(7) Cl(2) 0.0558(9) 0.0466(9) 0.0261(7) -0.0110(7) 0.0071(6) -0.0080(6) Cl(3) 0.0690(11) 0.0401(9) 0.0396(8) -0.0150(8) 0.0115(8) -0.0100(7) P(1) 0.0347(8) 0.0321(8) 0.0260(7) 0.0015(6) -0.0044(6) -0.0028(6) P(2) 0.0405(9) 0.0410(9) 0.0266(7) 0.0015(7) 0.0015(7) -0.0022(7) F(1) 0.040(2) 0.042(2) 0.071(2) 0.005(2) 0.004(2) -0.010(2) F(2) 0.037(2) 0.071(3) 0.148(4) 0.009(2) 0.001(3) -0.002(3) F(3) 0.045(2) 0.079(3) 0.151(4) -0.024(2) -0.033(3) 0.015(3) F(4) 0.085(3) 0.052(2) 0.072(3) -0.026(2) -0.018(2) -0.010(2) F(5) 0.060(2) 0.038(2) 0.063(2) -0.005(2) -0.002(2) -0.013(2) F(6) 0.059(2) 0.043(2) 0.037(2) 0.009(2) -0.000(2) -0.001(2) F(7) 0.090(3) 0.056(2) 0.041(2) 0.001(2) 0.010(2) 0.013(2) F(8) 0.072(3) 0.051(2) 0.060(2) 0.004(2) -0.012(2) 0.023(2) F(9) 0.043(2) 0.045(2) 0.073(2) 0.002(2) -0.015(2) 0.009(2) F(10) 0.037(2) 0.056(2) 0.046(2) 0.007(2) -0.000(2) 0.005(2) F(11) 0.074(3) 0.091(3) 0.039(2) 0.039(2) 0.022(2) 0.012(2) F(12) 0.141(4) 0.116(4) 0.030(2) 0.050(3) 0.019(2) 0.002(2) F(13) 0.116(4) 0.075(3) 0.033(2) 0.017(3) -0.017(2) 0.007(2) F(14) 0.058(2) 0.053(2) 0.067(3) 0.006(2) -0.006(2) 0.014(2) F(15) 0.066(2) 0.050(2) 0.044(2) 0.018(2) 0.015(2) 0.005(2) F(16) 0.042(2) 0.065(3) 0.062(2) 0.003(2) -0.001(2) 0.009(2) F(17) 0.038(2) 0.118(4) 0.069(3) -0.013(2) -0.005(2) 0.019(2) F(18) 0.061(3) 0.100(3) 0.108(4) -0.041(3) -0.001(3) 0.011(3) F(19) 0.093(3) 0.059(3) 0.116(4) -0.027(3) 0.012(3) 0.009(3) F(20) 0.059(2) 0.044(2) 0.060(2) -0.003(2) 0.007(2) 0.002(2) O(1) 0.039(2) 0.040(2) 0.031(2) 0.005(2) -0.000(2) 0.000(2) C(1) 0.042(3) 0.040(3) 0.029(3) 0.002(3) -0.009(3) -0.007(3) C(2) 0.040(4) 0.048(4) 0.029(3) 0.010(3) 0.002(3) -0.004(3) C(3) 0.037(3) 0.033(3) 0.029(3) 0.000(3) -0.008(2) -0.002(2) C(4) 0.043(4) 0.035(3) 0.046(3) -0.004(3) -0.009(3) 0.002(3) C(5) 0.036(4) 0.049(4) 0.076(5) 0.003(3) -0.010(3) 0.002(4) C(6) 0.039(4) 0.054(4) 0.083(5) -0.015(3) -0.026(4) 0.009(4) C(7) 0.060(5) 0.042(4) 0.046(4) -0.017(4) -0.016(3) 0.004(3) C(8) 0.046(4) 0.040(4) 0.040(3) -0.004(3) -0.011(3) 0.005(3) C(9) 0.039(3) 0.035(3) 0.027(3) -0.004(3) -0.009(3) -0.001(2) C(10) 0.040(4) 0.037(3) 0.033(3) 0.004(3) -0.007(3) -0.009(3) C(11) 0.052(4) 0.035(3) 0.035(3) -0.005(3) -0.004(3) 0.003(3) C(12) 0.055(4) 0.031(3) 0.046(4) -0.005(3) -0.020(3) 0.010(3) C(13) 0.033(3) 0.030(3) 0.049(4) 0.002(3) -0.014(3) -0.001(3) C(14) 0.034(3) 0.041(4) 0.036(3) -0.006(3) -0.007(3) -0.003(3) C(15) 0.043(4) 0.039(3) 0.027(3) 0.001(3) 0.000(3) -0.001(2) C(16) 0.060(4) 0.055(4) 0.029(3) 0.016(4) 0.004(3) 0.003(3) C(17) 0.081(5) 0.064(5) 0.026(3) 0.014(4) 0.012(3) -0.007(3) C(18) 0.081(5) 0.051(4) 0.032(4) 0.002(4) -0.009(3) 0.001(3) C(19) 0.045(4) 0.034(4) 0.054(4) 0.002(3) -0.010(3) 0.003(3) C(20) 0.042(4) 0.036(3) 0.032(3) -0.002(3) 0.002(3) -0.001(3) C(21) 0.043(4) 0.056(4) 0.022(3) 0.000(3) 0.005(3) 0.005(3) C(22) 0.051(4) 0.064(5) 0.025(3) -0.006(4) 0.004(3) 0.003(3) C(23) 0.042(4) 0.089(6) 0.038(4) -0.011(4) 0.006(3) 0.009(4) C(24) 0.055(5) 0.081(6) 0.054(4) -0.027(5) 0.004(4) 0.002(4) C(25) 0.065(5) 0.053(5) 0.058(4) -0.019(4) 0.009(4) 0.002(4) C(26) 0.050(4) 0.056(4) 0.038(4) -0.002(4) 0.005(3) -0.000(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; disordered hexane removed and scattering compensated with SQUEEZE Spek, A. L. "Single-crystal structure validation with the program PLATON", J. Appl. Crystallogr. 2003, 36, 7. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5432 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_all 0.0420 _refine_ls_wR_factor_ref 0.0380 _refine_ls_goodness_of_fit_all 0.866 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -0.94 _refine_diff_density_max 0.52 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re(1) Cl(1) 2.437(2) . . ? Re(1) Cl(2) 2.3454(13) . . ? Re(1) Cl(3) 2.353(1) . . ? Re(1) P(1) 2.470(1) . . ? Re(1) P(2) 2.483(1) . . ? Re(1) O(1) 1.665(4) . . ? P(1) C(1) 1.846(5) . . ? P(1) C(3) 1.832(6) . . ? P(1) C(9) 1.818(5) . . ? P(2) C(2) 1.834(6) . . ? P(2) C(15) 1.836(5) . . ? P(2) C(21) 1.819(6) . . ? F(1) C(4) 1.349(6) . . ? F(2) C(5) 1.325(7) . . ? F(3) C(6) 1.347(7) . . ? F(4) C(7) 1.354(7) . . ? F(5) C(8) 1.355(7) . . ? F(6) C(10) 1.342(6) . . ? F(7) C(11) 1.340(6) . . ? F(8) C(12) 1.339(6) . . ? F(9) C(13) 1.339(6) . . ? F(10) C(14) 1.343(6) . . ? F(11) C(16) 1.339(7) . . ? F(12) C(17) 1.331(7) . . ? F(13) C(18) 1.323(7) . . ? F(14) C(19) 1.337(6) . . ? F(15) C(20) 1.334(6) . . ? F(16) C(22) 1.348(7) . . ? F(17) C(23) 1.325(8) . . ? F(18) C(24) 1.335(7) . . ? F(19) C(25) 1.319(8) . . ? F(20) C(26) 1.337(7) . . ? C(1) C(2) 1.525(8) . . ? C(1) H(1) 0.95 . . no C(1) H(2) 0.95 . . no C(2) H(3) 0.95 . . no C(2) H(4) 0.95 . . no C(3) C(4) 1.386(8) . . ? C(3) C(8) 1.387(8) . . ? C(4) C(5) 1.370(8) . . ? C(5) C(6) 1.362(9) . . ? C(6) C(7) 1.372(9) . . ? C(7) C(8) 1.379(8) . . ? C(9) C(10) 1.395(7) . . ? C(9) C(14) 1.385(7) . . ? C(10) C(11) 1.377(7) . . ? C(11) C(12) 1.369(8) . . ? C(12) C(13) 1.350(8) . . ? C(13) C(14) 1.383(8) . . ? C(15) C(16) 1.390(7) . . ? C(15) C(20) 1.393(8) . . ? C(16) C(17) 1.370(8) . . ? C(17) C(18) 1.370(9) . . ? C(18) C(19) 1.362(8) . . ? C(19) C(20) 1.392(8) . . ? C(21) C(22) 1.404(8) . . ? C(21) C(26) 1.395(8) . . ? C(22) C(23) 1.397(9) . . ? C(23) C(24) 1.375(10) . . ? C(24) C(25) 1.364(10) . . ? C(25) C(26) 1.375(9) . . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Re(1) Cl(2) 88.25(5) . . . ? Cl(1) Re(1) Cl(3) 90.16(5) . . . ? Cl(1) Re(1) P(1) 78.31(5) . . . ? Cl(1) Re(1) P(2) 75.76(5) . . . ? Cl(1) Re(1) O(1) 161.63(13) . . . ? Cl(2) Re(1) Cl(3) 86.59(5) . . . ? Cl(2) Re(1) P(1) 94.67(5) . . . ? Cl(2) Re(1) P(2) 163.91(5) . . . ? Cl(2) Re(1) O(1) 103.49(12) . . . ? Cl(3) Re(1) P(1) 168.35(5) . . . ? Cl(3) Re(1) P(2) 91.64(5) . . . ? Cl(3) Re(1) O(1) 104.41(13) . . . ? P(1) Re(1) P(2) 83.93(5) . . . ? P(1) Re(1) O(1) 86.59(13) . . . ? P(2) Re(1) O(1) 92.44(12) . . . ? Re(1) P(1) C(1) 104.0(2) . . . ? Re(1) P(1) C(3) 120.0(2) . . . ? Re(1) P(1) C(9) 119.8(2) . . . ? C(1) P(1) C(3) 102.4(2) . . . ? C(1) P(1) C(9) 110.1(3) . . . ? C(3) P(1) C(9) 99.3(2) . . . ? Re(1) P(2) C(2) 104.9(2) . . . ? Re(1) P(2) C(15) 122.9(2) . . . ? Re(1) P(2) C(21) 115.2(2) . . . ? C(2) P(2) C(15) 103.6(3) . . . ? C(2) P(2) C(21) 110.0(3) . . . ? C(15) P(2) C(21) 99.5(3) . . . ? P(1) C(1) C(2) 114.0(4) . . . ? P(1) C(1) H(1) 108.3 . . . no P(1) C(1) H(2) 108.3 . . . no C(2) C(1) H(1) 108.3 . . . no C(2) C(1) H(2) 108.3 . . . no H(1) C(1) H(2) 109.5 . . . no P(2) C(2) C(1) 109.9(4) . . . ? P(2) C(2) H(3) 109.4 . . . no P(2) C(2) H(4) 109.4 . . . no C(1) C(2) H(3) 109.4 . . . no C(1) C(2) H(4) 109.4 . . . no H(3) C(2) H(4) 109.5 . . . no P(1) C(3) C(4) 124.8(4) . . . ? P(1) C(3) C(8) 120.2(4) . . . ? C(4) C(3) C(8) 114.9(5) . . . ? F(1) C(4) C(3) 119.3(5) . . . ? F(1) C(4) C(5) 116.6(6) . . . ? C(3) C(4) C(5) 124.0(6) . . . ? F(2) C(5) C(4) 121.7(6) . . . ? F(2) C(5) C(6) 119.8(6) . . . ? C(4) C(5) C(6) 118.6(6) . . . ? F(3) C(6) C(5) 119.9(7) . . . ? F(3) C(6) C(7) 119.5(6) . . . ? C(5) C(6) C(7) 120.5(6) . . . ? F(4) C(7) C(6) 121.0(6) . . . ? F(4) C(7) C(8) 119.6(6) . . . ? C(6) C(7) C(8) 119.4(6) . . . ? F(5) C(8) C(3) 120.5(5) . . . ? F(5) C(8) C(7) 117.1(6) . . . ? C(3) C(8) C(7) 122.5(6) . . . ? P(1) C(9) C(10) 118.9(4) . . . ? P(1) C(9) C(14) 125.4(4) . . . ? C(10) C(9) C(14) 115.5(5) . . . ? F(6) C(10) C(9) 119.8(5) . . . ? F(6) C(10) C(11) 117.6(5) . . . ? C(9) C(10) C(11) 122.6(5) . . . ? F(7) C(11) C(10) 119.9(5) . . . ? F(7) C(11) C(12) 120.8(5) . . . ? C(10) C(11) C(12) 119.3(6) . . . ? F(8) C(12) C(11) 119.4(6) . . . ? F(8) C(12) C(13) 120.3(6) . . . ? C(11) C(12) C(13) 120.3(5) . . . ? F(9) C(13) C(12) 120.7(5) . . . ? F(9) C(13) C(14) 119.1(5) . . . ? C(12) C(13) C(14) 120.1(6) . . . ? F(10) C(14) C(9) 120.6(5) . . . ? F(10) C(14) C(13) 117.2(5) . . . ? C(9) C(14) C(13) 122.2(5) . . . ? P(2) C(15) C(16) 119.6(4) . . . ? P(2) C(15) C(20) 124.8(4) . . . ? C(16) C(15) C(20) 115.2(5) . . . ? F(11) C(16) C(15) 120.0(5) . . . ? F(11) C(16) C(17) 117.6(5) . . . ? C(15) C(16) C(17) 122.4(6) . . . ? F(12) C(17) C(16) 119.3(6) . . . ? F(12) C(17) C(18) 119.5(6) . . . ? C(16) C(17) C(18) 121.1(6) . . . ? F(13) C(18) C(17) 121.1(6) . . . ? F(13) C(18) C(19) 120.5(6) . . . ? C(17) C(18) C(19) 118.4(6) . . . ? F(14) C(19) C(18) 119.5(6) . . . ? F(14) C(19) C(20) 120.0(6) . . . ? C(18) C(19) C(20) 120.5(6) . . . ? F(15) C(20) C(15) 120.7(5) . . . ? F(15) C(20) C(19) 117.1(5) . . . ? C(15) C(20) C(19) 122.1(5) . . . ? P(2) C(21) C(22) 125.5(5) . . . ? P(2) C(21) C(26) 119.3(5) . . . ? C(22) C(21) C(26) 115.2(6) . . . ? F(16) C(22) C(21) 121.2(6) . . . ? F(16) C(22) C(23) 116.6(6) . . . ? C(21) C(22) C(23) 122.2(7) . . . ? F(17) C(23) C(22) 118.8(7) . . . ? F(17) C(23) C(24) 122.3(7) . . . ? C(22) C(23) C(24) 118.9(7) . . . ? F(18) C(24) C(23) 118.3(7) . . . ? F(18) C(24) C(25) 120.7(7) . . . ? C(23) C(24) C(25) 121.0(7) . . . ? F(19) C(25) C(24) 120.2(7) . . . ? F(19) C(25) C(26) 120.5(7) . . . ? C(24) C(25) C(26) 119.3(7) . . . ? F(20) C(26) C(21) 119.0(6) . . . ? F(20) C(26) C(25) 117.6(6) . . . ? C(21) C(26) C(25) 123.4(7) . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) F(8) 3.444(4) . 7_456 no Cl(1) F(4) 3.555(4) . 11_544 no Cl(2) O(1) 3.263(4) . 11_544 no Cl(2) C(3) 3.407(5) . 11_544 no Cl(2) C(4) 3.544(6) . 11_544 no Cl(2) F(15) 3.598(4) . 11_544 no Cl(3) C(1) 3.455(5) . 11_544 no Cl(3) C(16) 3.539(7) . 11_544 no F(1) F(14) 2.816(5) . 11_544 no F(1) F(13) 3.359(5) . 10_554 no F(1) C(19) 3.474(7) . 11_544 no F(2) F(7) 2.784(6) . 4 no F(2) F(17) 2.873(6) . 14_556 no F(2) C(11) 3.382(7) . 4 no F(2) F(14) 3.576(6) . 11_544 no F(3) F(9) 2.929(5) . 13_556 no F(3) C(13) 3.191(7) . 13_556 no F(3) C(12) 3.314(7) . 4 no F(3) C(11) 3.387(7) . 4 no F(3) F(8) 3.559(5) . 4 no F(4) F(5) 3.048(5) . 13_556 no F(4) C(11) 3.056(7) . 13_556 no F(4) C(12) 3.140(7) . 13_556 no F(4) C(10) 3.229(7) . 13_556 no F(4) C(13) 3.347(7) . 13_556 no F(4) C(8) 3.367(7) . 13_556 no F(4) C(9) 3.488(6) . 13_556 no F(4) C(14) 3.513(7) . 13_556 no F(5) C(7) 3.475(7) . 13_556 no F(7) F(16) 2.909(5) . 8_556 no F(7) F(17) 2.962(5) . 8_556 no F(7) C(22) 3.415(7) . 8_556 no F(7) C(23) 3.422(8) . 8_556 no F(8) F(10) 2.790(5) . 8_556 no F(8) F(9) 3.002(5) . 8_556 no F(8) C(14) 3.038(6) . 8_556 no F(8) C(13) 3.130(7) . 8_556 no F(8) F(9) 3.343(5) . 7_456 no F(9) F(9) 2.899(6) . 7_456 no F(9) F(9) 2.899(6) . 8_556 no F(9) F(9) 2.912(7) . 2 no F(9) C(13) 3.260(6) . 8_556 no F(9) C(12) 3.477(7) . 8_556 no F(12) C(23) 2.919(7) . 5_557 no F(12) F(17) 2.940(5) . 5_557 no F(12) C(24) 3.077(8) . 5_557 no F(12) F(18) 3.217(6) . 5_557 no F(12) F(15) 3.430(6) . 4 no F(13) F(15) 2.933(5) . 4 no F(13) O(1) 3.372(6) . 4 no F(13) F(17) 3.406(6) . 5_557 no F(14) F(17) 2.717(5) . 15_546 no F(14) F(18) 3.251(6) . 15_546 no F(14) O(1) 3.395(5) . 4 no F(15) C(18) 3.358(7) . 11_544 no F(15) F(18) 3.454(6) . 15_546 no F(15) C(17) 3.581(8) . 11_544 no F(18) F(20) 3.200(5) . 16_446 no F(18) C(19) 3.516(7) . 16_446 no O(1) C(18) 3.205(8) . 11_544 no O(1) C(19) 3.224(7) . 11_544 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Re(1) P(1) C(1) C(2) . . . . -38.9(4) no Re(1) P(1) C(3) C(4) . . . . 23.3(6) no Re(1) P(1) C(3) C(8) . . . . -159.9(4) no Re(1) P(1) C(9) C(10) . . . . -78.3(5) no Re(1) P(1) C(9) C(14) . . . . 107.0(5) no Re(1) P(2) C(2) C(1) . . . . -42.8(4) no Re(1) P(2) C(15) C(16) . . . . 167.6(4) no Re(1) P(2) C(15) C(20) . . . . -18.8(6) no Re(1) P(2) C(21) C(22) . . . . -102.3(5) no Re(1) P(2) C(21) C(26) . . . . 76.4(5) no Cl(1) Re(1) P(1) C(1) . . . . 85.3(2) no Cl(1) Re(1) P(1) C(3) . . . . -161.2(2) no Cl(1) Re(1) P(1) C(9) . . . . -38.2(2) no Cl(1) Re(1) P(2) C(2) . . . . -64.1(2) no Cl(1) Re(1) P(2) C(15) . . . . 178.4(2) no Cl(1) Re(1) P(2) C(21) . . . . 56.9(2) no Cl(2) Re(1) P(1) C(1) . . . . 172.5(2) no Cl(2) Re(1) P(1) C(3) . . . . -74.0(2) no Cl(2) Re(1) P(1) C(9) . . . . 49.1(2) no Cl(2) Re(1) P(2) C(2) . . . . -70.5(3) no Cl(2) Re(1) P(2) C(15) . . . . 172.0(3) no Cl(2) Re(1) P(2) C(21) . . . . 50.5(3) no Cl(3) Re(1) P(1) C(1) . . . . 76.7(3) no Cl(3) Re(1) P(1) C(3) . . . . -169.8(3) no Cl(3) Re(1) P(1) C(9) . . . . -46.7(3) no Cl(3) Re(1) P(2) C(2) . . . . -153.9(2) no Cl(3) Re(1) P(2) C(15) . . . . 88.6(2) no Cl(3) Re(1) P(2) C(21) . . . . -32.9(2) no P(1) Re(1) P(2) C(2) . . . . 15.3(2) no P(1) Re(1) P(2) C(15) . . . . -102.2(2) no P(1) Re(1) P(2) C(21) . . . . 136.3(2) no P(1) C(1) C(2) P(2) . . . . 55.8(5) no P(1) C(3) C(4) F(1) . . . . 1.2(8) no P(1) C(3) C(4) C(5) . . . . 179.9(5) no P(1) C(3) C(8) F(5) . . . . -1.4(7) no P(1) C(3) C(8) C(7) . . . . 178.6(5) no P(1) C(9) C(10) F(6) . . . . 2.8(7) no P(1) C(9) C(10) C(11) . . . . -175.0(4) no P(1) C(9) C(14) F(10) . . . . -3.4(8) no P(1) C(9) C(14) C(13) . . . . 174.5(4) no P(2) Re(1) P(1) C(1) . . . . 8.6(2) no P(2) Re(1) P(1) C(3) . . . . 122.1(2) no P(2) Re(1) P(1) C(9) . . . . -114.8(2) no P(2) C(15) C(16) F(11) . . . . -0.1(9) no P(2) C(15) C(16) C(17) . . . . 178.6(6) no P(2) C(15) C(20) F(15) . . . . 0.9(8) no P(2) C(15) C(20) C(19) . . . . -177.0(5) no P(2) C(21) C(22) F(16) . . . . -3.8(8) no P(2) C(21) C(22) C(23) . . . . 177.3(4) no P(2) C(21) C(26) F(20) . . . . 4.3(7) no P(2) C(21) C(26) C(25) . . . . -177.5(5) no F(1) C(4) C(3) C(8) . . . . -175.7(5) no F(1) C(4) C(5) F(2) . . . . -1.0(9) no F(1) C(4) C(5) C(6) . . . . 178.9(6) no F(2) C(5) C(4) C(3) . . . . -179.8(6) no F(2) C(5) C(6) F(3) . . . . -0.2(10) no F(2) C(5) C(6) C(7) . . . . 177.7(6) no F(3) C(6) C(5) C(4) . . . . 179.8(6) no F(3) C(6) C(7) F(4) . . . . 0.5(10) no F(3) C(6) C(7) C(8) . . . . 178.9(6) no F(4) C(7) C(6) C(5) . . . . -177.5(6) no F(4) C(7) C(8) F(5) . . . . 1.0(8) no F(4) C(7) C(8) C(3) . . . . -179.1(5) no F(5) C(8) C(3) C(4) . . . . 175.7(5) no F(5) C(8) C(7) C(6) . . . . -177.5(5) no F(6) C(10) C(9) C(14) . . . . 178.0(5) no F(6) C(10) C(11) F(7) . . . . -0.2(8) no F(6) C(10) C(11) C(12) . . . . -178.8(5) no F(7) C(11) C(10) C(9) . . . . 177.7(5) no F(7) C(11) C(12) F(8) . . . . 1.5(8) no F(7) C(11) C(12) C(13) . . . . -176.7(5) no F(8) C(12) C(11) C(10) . . . . -179.9(5) no F(8) C(12) C(13) F(9) . . . . -1.1(9) no F(8) C(12) C(13) C(14) . . . . 179.7(5) no F(9) C(13) C(12) C(11) . . . . 177.0(5) no F(9) C(13) C(14) F(10) . . . . 0.2(8) no F(9) C(13) C(14) C(9) . . . . -177.8(5) no F(10) C(14) C(9) C(10) . . . . -178.3(5) no F(10) C(14) C(13) C(12) . . . . 179.3(5) no F(11) C(16) C(15) C(20) . . . . -174.2(6) no F(11) C(16) C(17) F(12) . . . . -0.5(10) no F(11) C(16) C(17) C(18) . . . . 175.1(6) no F(12) C(17) C(16) C(15) . . . . -179.2(6) no F(12) C(17) C(18) F(13) . . . . -2.0(10) no F(12) C(17) C(18) C(19) . . . . 176.8(6) no F(13) C(18) C(17) C(16) . . . . -177.5(7) no F(13) C(18) C(19) F(14) . . . . -0.6(9) no F(13) C(18) C(19) C(20) . . . . 178.8(6) no F(14) C(19) C(18) C(17) . . . . -179.4(6) no F(14) C(19) C(20) F(15) . . . . 2.5(8) no F(14) C(19) C(20) C(15) . . . . -179.5(5) no F(15) C(20) C(15) C(16) . . . . 174.7(5) no F(15) C(20) C(19) C(18) . . . . -176.9(6) no F(16) C(22) C(21) C(26) . . . . 177.4(5) no F(16) C(22) C(23) F(17) . . . . -0.2(8) no F(16) C(22) C(23) C(24) . . . . -178.6(6) no F(17) C(23) C(22) C(21) . . . . 178.7(5) no F(17) C(23) C(24) F(18) . . . . 0.2(10) no F(17) C(23) C(24) C(25) . . . . -177.3(6) no F(18) C(24) C(23) C(22) . . . . 178.5(5) no F(18) C(24) C(25) F(19) . . . . 0.6(10) no F(18) C(24) C(25) C(26) . . . . -178.5(6) no F(19) C(25) C(24) C(23) . . . . 178.1(6) no F(19) C(25) C(26) F(20) . . . . -1.0(9) no F(19) C(25) C(26) C(21) . . . . -179.3(6) no F(20) C(26) C(21) C(22) . . . . -176.9(5) no F(20) C(26) C(25) C(24) . . . . 178.1(6) no O(1) Re(1) P(1) C(1) . . . . -84.2(2) no O(1) Re(1) P(1) C(3) . . . . 29.3(2) no O(1) Re(1) P(1) C(9) . . . . 152.4(3) no O(1) Re(1) P(2) C(2) . . . . 101.6(2) no O(1) Re(1) P(2) C(15) . . . . -15.9(3) no O(1) Re(1) P(2) C(21) . . . . -137.4(3) no C(1) P(1) C(3) C(4) . . . . 137.6(5) no C(1) P(1) C(3) C(8) . . . . -45.6(5) no C(1) P(1) C(9) C(10) . . . . 161.3(4) no C(1) P(1) C(9) C(14) . . . . -13.4(6) no C(1) C(2) P(2) C(15) . . . . 87.2(4) no C(1) C(2) P(2) C(21) . . . . -167.2(3) no C(2) P(2) C(15) C(16) . . . . 49.5(6) no C(2) P(2) C(15) C(20) . . . . -136.9(5) no C(2) P(2) C(21) C(22) . . . . 15.9(6) no C(2) P(2) C(21) C(26) . . . . -165.4(4) no C(2) C(1) P(1) C(3) . . . . -164.5(4) no C(2) C(1) P(1) C(9) . . . . 90.7(4) no C(3) P(1) C(9) C(10) . . . . 54.4(5) no C(3) P(1) C(9) C(14) . . . . -120.3(5) no C(3) C(4) C(5) C(6) . . . . 0.1(10) no C(3) C(8) C(7) C(6) . . . . 2.4(9) no C(4) C(3) P(1) C(9) . . . . -109.3(5) no C(4) C(3) C(8) C(7) . . . . -4.3(8) no C(4) C(5) C(6) C(7) . . . . -2.2(10) no C(5) C(4) C(3) C(8) . . . . 3.0(9) no C(5) C(6) C(7) C(8) . . . . 1.0(10) no C(8) C(3) P(1) C(9) . . . . 67.5(5) no C(9) C(10) C(11) C(12) . . . . -1.0(9) no C(9) C(14) C(13) C(12) . . . . 1.3(9) no C(10) C(9) C(14) C(13) . . . . -0.4(8) no C(10) C(11) C(12) C(13) . . . . 1.9(9) no C(11) C(10) C(9) C(14) . . . . 0.2(8) no C(11) C(12) C(13) C(14) . . . . -2.1(9) no C(15) P(2) C(21) C(22) . . . . 124.2(5) no C(15) P(2) C(21) C(26) . . . . -57.1(5) no C(15) C(16) C(17) C(18) . . . . -3.7(11) no C(15) C(20) C(19) C(18) . . . . 1.1(9) no C(16) C(15) P(2) C(21) . . . . -63.9(5) no C(16) C(15) C(20) C(19) . . . . -3.2(8) no C(16) C(17) C(18) C(19) . . . . 1.3(11) no C(17) C(16) C(15) C(20) . . . . 4.5(9) no C(17) C(18) C(19) C(20) . . . . -0.0(10) no C(20) C(15) P(2) C(21) . . . . 109.7(5) no C(21) C(22) C(23) C(24) . . . . 0.3(9) no C(21) C(26) C(25) C(24) . . . . -0.2(10) no C(22) C(21) C(26) C(25) . . . . 1.4(9) no C(22) C(23) C(24) C(25) . . . . 1.0(10) no C(23) C(22) C(21) C(26) . . . . -1.5(8) no C(23) C(24) C(25) C(26) . . . . -1.0(11) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_2325ReXant _database_code_depnum_ccdc_archive 'CCDC 247680' _audit_creation_date 2004-03-27 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 17.2122(2) _cell_length_b 14.1969(2) _cell_length_c 28.0146(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6845.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 31883 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 887.19 _chemical_formula_analytical ? _chemical_formula_sum 'C39 H32 Cl3 O2 P2 Re ' _chemical_formula_moiety 'C39 H32 Cl3 O2 P2 Re ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3504.00 _exptl_absorpt_coefficient_mu 3.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.529 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 36833 _reflns_number_total 8543 _reflns_number_gt 4279 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.11280 _diffrn_reflns_av_sigmaI/netI 0.167 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.43 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 312 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 256 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 24 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 16 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Re 0 8 -1.598 7.232 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.55724(2) 0.57115(2) 0.885758(12) 0.02648(9) 1.000 . Uani d ? Cl(1) 0.56217(13) 0.6255(2) 0.80466(7) 0.0303(6) 1.000 . Uani d ? Cl(2) 0.68153(13) 0.6344(2) 0.90380(9) 0.0394(7) 1.000 . Uani d ? Cl(3) 0.63049(13) 0.4402(2) 0.86197(9) 0.0373(7) 1.000 . Uani d ? P(1) 0.49306(13) 0.7333(2) 0.89732(8) 0.0232(6) 1.000 . Uani d ? P(2) 0.4362(1) 0.4763(2) 0.86190(8) 0.0247(6) 1.000 . Uani d ? O(1) 0.5344(4) 0.5427(4) 0.9437(2) 0.039(2) 1.000 . Uani d ? O(2) 0.3761(3) 0.6493(4) 0.8339(2) 0.021(2) 1.000 . Uani d ? C(1) 0.4435(5) 0.7907(6) 0.8467(3) 0.022(2) 1.000 . Uani d ? C(2) 0.3892(5) 0.7428(6) 0.8199(3) 0.019(2) 1.000 . Uani d ? C(3) 0.3492(5) 0.7793(6) 0.7810(3) 0.021(2) 1.000 . Uani d ? C(4) 0.3658(5) 0.8722(6) 0.7687(3) 0.028(3) 1.000 . Uani d ? C(5) 0.4195(5) 0.9221(6) 0.7942(3) 0.035(3) 1.000 . Uani d ? C(6) 0.4586(5) 0.8827(6) 0.8329(3) 0.027(3) 1.000 . Uani d ? C(7) 0.2919(5) 0.7144(6) 0.7562(3) 0.028(3) 1.000 . Uani d ? C(8) 0.2709(5) 0.7488(7) 0.7056(3) 0.041(3) 1.000 . Uani d ? C(9) 0.2169(5) 0.7091(7) 0.7868(3) 0.042(3) 1.000 . Uani d ? C(10) 0.3673(5) 0.5877(6) 0.7956(3) 0.022(2) 1.000 . Uani d ? C(11) 0.3290(5) 0.6157(6) 0.7549(3) 0.024(2) 1.000 . Uani d ? C(12) 0.3242(5) 0.5520(6) 0.7179(3) 0.031(3) 1.000 . Uani d ? C(13) 0.3566(6) 0.4638(7) 0.7235(3) 0.036(3) 1.000 . Uani d ? C(14) 0.3918(5) 0.4351(6) 0.7651(3) 0.029(3) 1.000 . Uani d ? C(15) 0.3983(5) 0.4985(6) 0.8023(3) 0.024(2) 1.000 . Uani d ? C(16) 0.5546(5) 0.8317(6) 0.9150(3) 0.025(2) 1.000 . Uani d ? C(17) 0.6274(5) 0.8480(6) 0.8941(3) 0.030(3) 1.000 . Uani d ? C(18) 0.6658(5) 0.9303(7) 0.9017(3) 0.036(3) 1.000 . Uani d ? C(19) 0.6346(6) 1.0007(7) 0.9281(3) 0.038(3) 1.000 . Uani d ? C(20) 0.5624(6) 0.9885(7) 0.9492(3) 0.045(3) 1.000 . Uani d ? C(21) 0.5231(6) 0.9032(7) 0.9431(3) 0.041(3) 1.000 . Uani d ? C(22) 0.4225(5) 0.7296(6) 0.9457(3) 0.025(3) 1.000 . Uani d ? C(23) 0.3442(5) 0.7487(6) 0.9388(3) 0.032(3) 1.000 . Uani d ? C(24) 0.2950(5) 0.7490(7) 0.9787(4) 0.040(3) 1.000 . Uani d ? C(25) 0.3233(6) 0.7300(7) 1.0239(4) 0.045(3) 1.000 . Uani d ? C(26) 0.4005(6) 0.7092(7) 1.0296(3) 0.039(3) 1.000 . Uani d ? C(27) 0.4496(5) 0.7101(6) 0.9912(3) 0.028(3) 1.000 . Uani d ? C(28) 0.3506(5) 0.4912(6) 0.8997(3) 0.025(3) 1.000 . Uani d ? C(29) 0.3566(5) 0.5015(6) 0.9483(3) 0.031(3) 1.000 . Uani d ? C(30) 0.2918(6) 0.5054(7) 0.9765(3) 0.041(3) 1.000 . Uani d ? C(31) 0.2174(6) 0.4987(7) 0.9565(4) 0.046(3) 1.000 . Uani d ? C(32) 0.2107(5) 0.4871(7) 0.9083(4) 0.039(3) 1.000 . Uani d ? C(33) 0.2761(5) 0.4807(6) 0.8795(3) 0.031(3) 1.000 . Uani d ? C(34) 0.4504(5) 0.3478(6) 0.8633(3) 0.030(3) 1.000 . Uani d ? C(35) 0.4138(5) 0.2939(7) 0.8989(3) 0.037(3) 1.000 . Uani d ? C(36) 0.4239(6) 0.1970(7) 0.8996(4) 0.048(3) 1.000 . Uani d ? C(37) 0.4699(7) 0.1548(7) 0.8653(4) 0.057(4) 1.000 . Uani d ? C(38) 0.5064(6) 0.2063(7) 0.8306(4) 0.042(3) 1.000 . Uani d ? C(39) 0.4984(5) 0.3034(6) 0.8300(4) 0.036(3) 1.000 . Uani d ? H(1) 0.3398 0.9009 0.7425 0.033 1.000 . Uiso c ? H(2) 0.4306 0.9852 0.7853 0.042 1.000 . Uiso c ? H(3) 0.4958 0.9191 0.8500 0.032 1.000 . Uiso c ? H(4) 0.2395 0.8037 0.7078 0.049 1.000 . Uiso c ? H(5) 0.3171 0.7631 0.6886 0.049 1.000 . Uiso c ? H(6) 0.2430 0.7008 0.6893 0.049 1.000 . Uiso c ? H(7) 0.1889 0.7664 0.7839 0.050 1.000 . Uiso c ? H(8) 0.1855 0.6584 0.7759 0.050 1.000 . Uiso c ? H(9) 0.2304 0.6991 0.8193 0.050 1.000 . Uiso c ? H(10) 0.2988 0.5686 0.6890 0.037 1.000 . Uiso c ? H(11) 0.3547 0.4210 0.6974 0.044 1.000 . Uiso c ? H(12) 0.4113 0.3728 0.7683 0.035 1.000 . Uiso c ? H(13) 0.6501 0.8010 0.8744 0.036 1.000 . Uiso c ? H(14) 0.7159 0.9387 0.8881 0.043 1.000 . Uiso c ? H(15) 0.6620 1.0582 0.9321 0.045 1.000 . Uiso c ? H(16) 0.5400 1.0377 0.9676 0.054 1.000 . Uiso c ? H(17) 0.4743 0.8938 0.9583 0.049 1.000 . Uiso c ? H(18) 0.3244 0.7614 0.9078 0.039 1.000 . Uiso c ? H(19) 0.2414 0.7624 0.9746 0.048 1.000 . Uiso c ? H(20) 0.2895 0.7314 1.0507 0.054 1.000 . Uiso c ? H(21) 0.4200 0.6941 1.0604 0.047 1.000 . Uiso c ? H(22) 0.5033 0.6971 0.9959 0.034 1.000 . Uiso c ? H(23) 0.4065 0.5060 0.9625 0.037 1.000 . Uiso c ? H(24) 0.2973 0.5127 1.0100 0.049 1.000 . Uiso c ? H(25) 0.1725 0.5022 0.9761 0.055 1.000 . Uiso c ? H(26) 0.1606 0.4834 0.8942 0.047 1.000 . Uiso c ? H(27) 0.2707 0.4692 0.8463 0.037 1.000 . Uiso c ? H(28) 0.3825 0.3237 0.9224 0.044 1.000 . Uiso c ? H(29) 0.3993 0.1599 0.9234 0.057 1.000 . Uiso c ? H(30) 0.4764 0.0884 0.8658 0.068 1.000 . Uiso c ? H(31) 0.5370 0.1756 0.8070 0.051 1.000 . Uiso c ? H(32) 0.5257 0.3397 0.8070 0.043 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.0255(2) 0.0282(2) 0.0257(2) 0.0021(2) -0.0047(2) 0.0020(2) Cl(1) 0.0334(13) 0.0322(12) 0.0254(12) -0.0029(11) 0.0007(11) 0.0007(10) Cl(2) 0.0282(13) 0.0339(13) 0.056(2) -0.0017(10) -0.0138(12) 0.0030(12) Cl(3) 0.0288(12) 0.034(1) 0.049(2) 0.0072(11) -0.0001(11) -0.0070(12) P(1) 0.0228(12) 0.0290(13) 0.0178(12) -0.0020(10) 0.0001(10) -0.0013(10) P(2) 0.0277(13) 0.0233(12) 0.0230(12) 0.0009(11) 0.0016(12) 0.0012(10) O(1) 0.053(4) 0.033(4) 0.030(4) -0.000(3) 0.006(3) -0.008(3) O(2) 0.024(3) 0.022(3) 0.019(3) -0.001(3) -0.001(3) 0.002(3) C(1) 0.025(5) 0.025(5) 0.017(4) -0.004(4) -0.002(4) 0.004(4) C(2) 0.021(5) 0.022(5) 0.015(4) 0.001(4) 0.007(4) 0.001(4) C(3) 0.024(5) 0.024(5) 0.016(4) 0.002(4) 0.003(4) -0.000(4) C(4) 0.031(5) 0.030(5) 0.022(5) 0.003(4) -0.008(4) -0.004(4) C(5) 0.046(6) 0.022(5) 0.039(6) 0.003(4) 0.004(5) 0.009(5) C(6) 0.037(6) 0.021(5) 0.022(5) -0.001(4) -0.004(4) -0.006(4) C(7) 0.029(5) 0.033(5) 0.023(5) -0.004(4) -0.004(4) 0.006(5) C(8) 0.049(7) 0.037(6) 0.036(6) -0.003(5) -0.018(5) 0.004(5) C(9) 0.035(6) 0.054(7) 0.036(6) 0.005(5) -0.003(5) 0.001(5) C(10) 0.024(5) 0.022(5) 0.019(5) -0.006(4) 0.001(4) -0.002(4) C(11) 0.024(5) 0.028(5) 0.022(5) -0.003(4) -0.006(4) 0.001(4) C(12) 0.043(6) 0.027(5) 0.022(5) -0.014(4) -0.009(4) 0.007(4) C(13) 0.048(6) 0.039(6) 0.022(5) -0.015(5) 0.002(5) -0.007(5) C(14) 0.033(5) 0.025(5) 0.029(5) -0.008(4) -0.004(4) -0.001(5) C(15) 0.023(5) 0.030(5) 0.019(5) -0.007(4) 0.003(4) 0.004(4) C(16) 0.026(5) 0.026(5) 0.023(5) 0.002(4) 0.004(4) -0.005(4) C(17) 0.028(5) 0.038(6) 0.024(5) 0.002(4) -0.002(4) 0.015(4) C(18) 0.022(5) 0.047(6) 0.039(6) -0.011(5) -0.002(4) 0.022(6) C(19) 0.049(7) 0.038(6) 0.026(6) -0.020(5) -0.008(5) 0.001(5) C(20) 0.053(7) 0.049(7) 0.034(6) -0.016(6) 0.002(6) -0.022(5) C(21) 0.037(6) 0.055(7) 0.031(6) -0.018(5) 0.005(5) -0.010(5) C(22) 0.018(5) 0.025(5) 0.031(5) -0.002(4) 0.004(4) -0.002(4) C(23) 0.037(6) 0.031(5) 0.029(5) -0.000(4) 0.007(5) 0.008(5) C(24) 0.028(6) 0.041(6) 0.052(7) 0.000(5) 0.004(5) 0.005(6) C(25) 0.057(7) 0.034(6) 0.042(7) -0.006(6) 0.032(6) -0.010(5) C(26) 0.049(7) 0.040(6) 0.028(6) -0.005(5) 0.004(5) -0.001(5) C(27) 0.029(5) 0.036(5) 0.018(5) -0.008(5) 0.001(4) -0.000(4) C(28) 0.027(5) 0.017(5) 0.029(5) 0.004(4) 0.006(4) 0.005(4) C(29) 0.040(6) 0.026(5) 0.026(5) -0.004(4) 0.007(5) -0.004(5) C(30) 0.050(7) 0.037(6) 0.035(6) -0.007(5) 0.008(6) -0.004(5) C(31) 0.053(7) 0.042(7) 0.043(7) 0.002(5) 0.020(6) 0.004(6) C(32) 0.029(6) 0.038(6) 0.050(7) -0.000(5) 0.006(5) 0.011(5) C(33) 0.042(6) 0.030(5) 0.020(5) 0.003(4) 0.002(5) -0.000(4) C(34) 0.032(6) 0.024(5) 0.036(5) -0.002(4) -0.012(5) 0.000(4) C(35) 0.034(5) 0.035(6) 0.042(6) 0.002(4) -0.001(5) 0.002(5) C(36) 0.051(7) 0.027(6) 0.065(8) -0.008(5) -0.010(6) 0.013(6) C(37) 0.073(9) 0.025(6) 0.073(9) 0.004(6) -0.007(7) 0.003(6) C(38) 0.037(6) 0.036(6) 0.053(7) 0.010(5) -0.000(6) -0.016(6) C(39) 0.030(6) 0.032(6) 0.045(6) 0.002(5) 0.003(5) 0.001(5) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4279 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_all 0.0630 _refine_ls_wR_factor_ref 0.0510 _refine_ls_goodness_of_fit_all 0.960 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.77 _refine_diff_density_max 3.65 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re(1) Cl(1) 2.401(2) . . ? Re(1) Cl(2) 2.375(2) . . ? Re(1) Cl(3) 2.343(2) . . ? Re(1) P(1) 2.574(2) . . ? Re(1) P(2) 2.570(2) . . ? Re(1) O(1) 1.718(6) . . ? P(1) C(1) 1.844(8) . . ? P(1) C(16) 1.821(9) . . ? P(1) C(22) 1.821(9) . . ? P(2) C(15) 1.820(9) . . ? P(2) C(28) 1.827(9) . . ? P(2) C(34) 1.841(9) . . ? O(2) C(2) 1.402(9) . . ? O(2) C(10) 1.392(9) . . ? C(1) C(2) 1.379(11) . . ? C(1) C(6) 1.387(11) . . ? C(2) C(3) 1.388(11) . . ? C(3) C(4) 1.393(11) . . ? C(3) C(7) 1.518(11) . . ? C(4) C(5) 1.367(12) . . ? C(4) H(1) 0.95 . . no C(5) C(6) 1.394(12) . . ? C(5) H(2) 0.95 . . no C(6) H(3) 0.95 . . no C(7) C(8) 1.542(12) . . ? C(7) C(9) 1.551(12) . . ? C(7) C(11) 1.541(12) . . ? C(8) H(4) 0.95 . . no C(8) H(5) 0.95 . . no C(8) H(6) 0.95 . . no C(9) H(7) 0.95 . . no C(9) H(8) 0.95 . . no C(9) H(9) 0.95 . . no C(10) C(11) 1.376(11) . . ? C(10) C(15) 1.387(11) . . ? C(11) C(12) 1.378(12) . . ? C(12) C(13) 1.380(13) . . ? C(12) H(10) 0.95 . . no C(13) C(14) 1.377(12) . . ? C(13) H(11) 0.95 . . no C(14) C(15) 1.380(12) . . ? C(14) H(12) 0.95 . . no C(16) C(17) 1.402(11) . . ? C(16) C(21) 1.395(12) . . ? C(17) C(18) 1.359(12) . . ? C(17) H(13) 0.95 . . no C(18) C(19) 1.354(13) . . ? C(18) H(14) 0.95 . . no C(19) C(20) 1.386(13) . . ? C(19) H(15) 0.95 . . no C(20) C(21) 1.399(13) . . ? C(20) H(16) 0.95 . . no C(21) H(17) 0.95 . . no C(22) C(23) 1.390(11) . . ? C(22) C(27) 1.386(12) . . ? C(23) C(24) 1.402(12) . . ? C(23) H(18) 0.95 . . no C(24) C(25) 1.38(1) . . ? C(24) H(19) 0.95 . . no C(25) C(26) 1.371(13) . . ? C(25) H(20) 0.95 . . no C(26) C(27) 1.367(12) . . ? C(26) H(21) 0.95 . . no C(27) H(22) 0.95 . . no C(28) C(29) 1.372(12) . . ? C(28) C(33) 1.409(12) . . ? C(29) C(30) 1.368(12) . . ? C(29) H(23) 0.95 . . no C(30) C(31) 1.40(1) . . ? C(30) H(24) 0.95 . . no C(31) C(32) 1.37(1) . . ? C(31) H(25) 0.95 . . no C(32) C(33) 1.387(12) . . ? C(32) H(26) 0.95 . . no C(33) H(27) 0.95 . . no C(34) C(35) 1.407(13) . . ? C(34) C(39) 1.395(12) . . ? C(35) C(36) 1.387(13) . . ? C(35) H(28) 0.95 . . no C(36) C(37) 1.38(2) . . ? C(36) H(29) 0.95 . . no C(37) C(38) 1.37(1) . . ? C(37) H(30) 0.95 . . no C(38) C(39) 1.385(13) . . ? C(38) H(31) 0.95 . . no C(39) H(32) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Re(1) Cl(2) 92.75(8) . . . ? Cl(1) Re(1) Cl(3) 88.10(8) . . . ? Cl(1) Re(1) P(1) 81.18(7) . . . ? Cl(1) Re(1) P(2) 87.19(8) . . . ? Cl(1) Re(1) O(1) 167.8(2) . . . ? Cl(2) Re(1) Cl(3) 82.86(8) . . . ? Cl(2) Re(1) P(1) 91.24(8) . . . ? Cl(2) Re(1) P(2) 169.79(8) . . . ? Cl(2) Re(1) O(1) 95.4(2) . . . ? Cl(3) Re(1) P(1) 167.52(8) . . . ? Cl(3) Re(1) P(2) 86.94(8) . . . ? Cl(3) Re(1) O(1) 101.8(2) . . . ? P(1) Re(1) P(2) 98.83(7) . . . ? P(1) Re(1) O(1) 89.6(2) . . . ? P(2) Re(1) O(1) 86.3(2) . . . ? Re(1) P(1) C(1) 119.8(3) . . . ? Re(1) P(1) C(16) 118.1(3) . . . ? Re(1) P(1) C(22) 110.7(3) . . . ? C(1) P(1) C(16) 98.0(4) . . . ? C(1) P(1) C(22) 106.1(4) . . . ? C(16) P(1) C(22) 102.0(4) . . . ? Re(1) P(2) C(15) 116.0(3) . . . ? Re(1) P(2) C(28) 116.3(3) . . . ? Re(1) P(2) C(34) 113.9(3) . . . ? C(15) P(2) C(28) 102.9(4) . . . ? C(15) P(2) C(34) 103.8(4) . . . ? C(28) P(2) C(34) 102.1(4) . . . ? C(2) O(2) C(10) 113.3(6) . . . ? P(1) C(1) C(2) 121.0(6) . . . ? P(1) C(1) C(6) 122.9(7) . . . ? C(2) C(1) C(6) 116.1(8) . . . ? O(2) C(2) C(1) 115.0(7) . . . ? O(2) C(2) C(3) 119.6(8) . . . ? C(1) C(2) C(3) 125.4(8) . . . ? C(2) C(3) C(4) 116.6(8) . . . ? C(2) C(3) C(7) 117.0(8) . . . ? C(4) C(3) C(7) 126.4(8) . . . ? C(3) C(4) C(5) 119.9(8) . . . ? C(3) C(4) H(1) 120.0 . . . no C(5) C(4) H(1) 120.0 . . . no C(4) C(5) C(6) 121.8(9) . . . ? C(4) C(5) H(2) 119.1 . . . no C(6) C(5) H(2) 119.1 . . . no C(1) C(6) C(5) 120.2(8) . . . ? C(1) C(6) H(3) 119.9 . . . no C(5) C(6) H(3) 119.9 . . . no C(3) C(7) C(8) 112.4(7) . . . ? C(3) C(7) C(9) 108.5(7) . . . ? C(3) C(7) C(11) 107.1(7) . . . ? C(8) C(7) C(9) 109.1(7) . . . ? C(8) C(7) C(11) 111.3(7) . . . ? C(9) C(7) C(11) 108.3(7) . . . ? C(7) C(8) H(4) 109.5 . . . no C(7) C(8) H(5) 109.5 . . . no C(7) C(8) H(6) 109.5 . . . no H(4) C(8) H(5) 109.5 . . . no H(4) C(8) H(6) 109.5 . . . no H(5) C(8) H(6) 109.5 . . . no C(7) C(9) H(7) 109.5 . . . no C(7) C(9) H(8) 109.5 . . . no C(7) C(9) H(9) 109.5 . . . no H(7) C(9) H(8) 109.5 . . . no H(7) C(9) H(9) 109.5 . . . no H(8) C(9) H(9) 109.5 . . . no O(2) C(10) C(11) 120.6(7) . . . ? O(2) C(10) C(15) 115.3(7) . . . ? C(11) C(10) C(15) 124.1(8) . . . ? C(7) C(11) C(10) 116.2(8) . . . ? C(7) C(11) C(12) 126.2(8) . . . ? C(10) C(11) C(12) 117.5(8) . . . ? C(11) C(12) C(13) 119.1(8) . . . ? C(11) C(12) H(10) 120.4 . . . no C(13) C(12) H(10) 120.4 . . . no C(12) C(13) C(14) 122.8(9) . . . ? C(12) C(13) H(11) 118.6 . . . no C(14) C(13) H(11) 118.6 . . . no C(13) C(14) C(15) 118.9(9) . . . ? C(13) C(14) H(12) 120.6 . . . no C(15) C(14) H(12) 120.6 . . . no P(2) C(15) C(10) 114.8(7) . . . ? P(2) C(15) C(14) 127.5(7) . . . ? C(10) C(15) C(14) 117.5(8) . . . ? P(1) C(16) C(17) 122.2(7) . . . ? P(1) C(16) C(21) 119.0(7) . . . ? C(17) C(16) C(21) 117.6(8) . . . ? C(16) C(17) C(18) 120.8(9) . . . ? C(16) C(17) H(13) 119.6 . . . no C(18) C(17) H(13) 119.6 . . . no C(17) C(18) C(19) 121.8(9) . . . ? C(17) C(18) H(14) 119.1 . . . no C(19) C(18) H(14) 119.1 . . . no C(18) C(19) C(20) 119.8(9) . . . ? C(18) C(19) H(15) 120.1 . . . no C(20) C(19) H(15) 120.1 . . . no C(19) C(20) C(21) 119.4(9) . . . ? C(19) C(20) H(16) 120.3 . . . no C(21) C(20) H(16) 120.3 . . . no C(16) C(21) C(20) 120.7(9) . . . ? C(16) C(21) H(17) 119.7 . . . no C(20) C(21) H(17) 119.7 . . . no P(1) C(22) C(23) 122.5(7) . . . ? P(1) C(22) C(27) 117.8(6) . . . ? C(23) C(22) C(27) 119.6(8) . . . ? C(22) C(23) C(24) 118.3(9) . . . ? C(22) C(23) H(18) 120.8 . . . no C(24) C(23) H(18) 120.8 . . . no C(23) C(24) C(25) 121.2(9) . . . ? C(23) C(24) H(19) 119.4 . . . no C(25) C(24) H(19) 119.4 . . . no C(24) C(25) C(26) 119.3(9) . . . ? C(24) C(25) H(20) 120.3 . . . no C(26) C(25) H(20) 120.3 . . . no C(25) C(26) C(27) 120.4(9) . . . ? C(25) C(26) H(21) 119.8 . . . no C(27) C(26) H(21) 119.8 . . . no C(22) C(27) C(26) 121.1(9) . . . ? C(22) C(27) H(22) 119.5 . . . no C(26) C(27) H(22) 119.5 . . . no P(2) C(28) C(29) 121.8(7) . . . ? P(2) C(28) C(33) 119.2(7) . . . ? C(29) C(28) C(33) 118.5(8) . . . ? C(28) C(29) C(30) 121.1(9) . . . ? C(28) C(29) H(23) 119.5 . . . no C(30) C(29) H(23) 119.5 . . . no C(29) C(30) C(31) 120.7(9) . . . ? C(29) C(30) H(24) 119.6 . . . no C(31) C(30) H(24) 119.6 . . . no C(30) C(31) C(32) 118.8(10) . . . ? C(30) C(31) H(25) 120.6 . . . no C(32) C(31) H(25) 120.6 . . . no C(31) C(32) C(33) 120.9(10) . . . ? C(31) C(32) H(26) 119.6 . . . no C(33) C(32) H(26) 119.6 . . . no C(28) C(33) C(32) 119.9(8) . . . ? C(28) C(33) H(27) 120.1 . . . no C(32) C(33) H(27) 120.1 . . . no P(2) C(34) C(35) 119.6(8) . . . ? P(2) C(34) C(39) 120.9(7) . . . ? C(35) C(34) C(39) 119.5(9) . . . ? C(34) C(35) C(36) 119.6(10) . . . ? C(34) C(35) H(28) 120.2 . . . no C(36) C(35) H(28) 120.2 . . . no C(35) C(36) C(37) 119.4(10) . . . ? C(35) C(36) H(29) 120.3 . . . no C(37) C(36) H(29) 120.3 . . . no C(36) C(37) C(38) 121.7(10) . . . ? C(36) C(37) H(30) 119.1 . . . no C(38) C(37) H(30) 119.1 . . . no C(37) C(38) C(39) 119.5(10) . . . ? C(37) C(38) H(31) 120.2 . . . no C(39) C(38) H(31) 120.2 . . . no C(34) C(39) C(38) 120.1(10) . . . ? C(34) C(39) H(32) 119.9 . . . no C(38) C(39) H(32) 119.9 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(1) 3.581(13) . 5_667 no C(13) C(18) 3.559(13) . 3_646 no C(19) C(31) 3.53(1) . 2_567 no C(20) C(20) 3.58(2) . 5_677 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Re(1) P(1) C(1) C(2) . . . . 50.3(8) no Re(1) P(1) C(1) C(6) . . . . -128.8(7) no Re(1) P(1) C(16) C(17) . . . . 43.8(8) no Re(1) P(1) C(16) C(21) . . . . -148.9(7) no Re(1) P(1) C(22) C(23) . . . . -119.1(7) no Re(1) P(1) C(22) C(27) . . . . 63.3(7) no Re(1) P(2) C(15) C(10) . . . . -67.2(7) no Re(1) P(2) C(15) C(14) . . . . 118.1(8) no Re(1) P(2) C(28) C(29) . . . . -37.1(9) no Re(1) P(2) C(28) C(33) . . . . 150.6(6) no Re(1) P(2) C(34) C(35) . . . . 109.3(7) no Re(1) P(2) C(34) C(39) . . . . -69.2(8) no Cl(1) Re(1) P(1) C(1) . . . . 25.1(3) no Cl(1) Re(1) P(1) C(16) . . . . -94.1(3) no Cl(1) Re(1) P(1) C(22) . . . . 148.9(3) no Cl(1) Re(1) P(2) C(15) . . . . -7.7(3) no Cl(1) Re(1) P(2) C(28) . . . . -128.9(3) no Cl(1) Re(1) P(2) C(34) . . . . 112.8(4) no Cl(2) Re(1) P(1) C(1) . . . . 117.7(3) no Cl(2) Re(1) P(1) C(16) . . . . -1.5(3) no Cl(2) Re(1) P(1) C(22) . . . . -118.5(3) no Cl(2) Re(1) P(2) C(15) . . . . -97.6(6) no Cl(2) Re(1) P(2) C(28) . . . . 141.2(5) no Cl(2) Re(1) P(2) C(34) . . . . 22.8(6) no Cl(3) Re(1) P(1) C(1) . . . . 56.2(5) no Cl(3) Re(1) P(1) C(16) . . . . -62.9(5) no Cl(3) Re(1) P(1) C(22) . . . . -179.9(4) no Cl(3) Re(1) P(2) C(15) . . . . -95.9(3) no Cl(3) Re(1) P(2) C(28) . . . . 142.9(3) no Cl(3) Re(1) P(2) C(34) . . . . 24.5(4) no P(1) Re(1) P(2) C(15) . . . . 72.9(3) no P(1) Re(1) P(2) C(28) . . . . -48.2(3) no P(1) Re(1) P(2) C(34) . . . . -166.6(4) no P(1) C(1) C(2) O(2) . . . . -0.5(10) no P(1) C(1) C(2) C(3) . . . . -179.6(7) no P(1) C(1) C(6) C(5) . . . . 179.6(7) no P(1) C(16) C(17) C(18) . . . . 168.3(7) no P(1) C(16) C(21) C(20) . . . . -166.6(8) no P(1) C(22) C(23) C(24) . . . . -176.6(7) no P(1) C(22) C(27) C(26) . . . . 177.8(7) no P(2) Re(1) P(1) C(1) . . . . -60.7(3) no P(2) Re(1) P(1) C(16) . . . . -179.8(3) no P(2) Re(1) P(1) C(22) . . . . 63.2(3) no P(2) C(15) C(10) O(2) . . . . 5.5(10) no P(2) C(15) C(10) C(11) . . . . -173.4(7) no P(2) C(15) C(14) C(13) . . . . 175.7(7) no P(2) C(28) C(29) C(30) . . . . -175.0(7) no P(2) C(28) C(33) C(32) . . . . 176.8(7) no P(2) C(34) C(35) C(36) . . . . 179.2(8) no P(2) C(34) C(39) C(38) . . . . -177.8(8) no O(1) Re(1) P(1) C(1) . . . . -146.9(4) no O(1) Re(1) P(1) C(16) . . . . 93.9(4) no O(1) Re(1) P(1) C(22) . . . . -23.1(4) no O(1) Re(1) P(2) C(15) . . . . 162.0(4) no O(1) Re(1) P(2) C(28) . . . . 40.8(4) no O(1) Re(1) P(2) C(34) . . . . -77.6(4) no O(2) C(2) C(1) C(6) . . . . 178.7(7) no O(2) C(2) C(3) C(4) . . . . -179.1(7) no O(2) C(2) C(3) C(7) . . . . 0.8(11) no O(2) C(10) C(11) C(7) . . . . -4.7(12) no O(2) C(10) C(11) C(12) . . . . 178.4(7) no O(2) C(10) C(15) C(14) . . . . -179.3(7) no C(1) P(1) C(16) C(17) . . . . -86.3(8) no C(1) P(1) C(16) C(21) . . . . 81.1(8) no C(1) P(1) C(22) C(23) . . . . 12.3(9) no C(1) P(1) C(22) C(27) . . . . -165.3(7) no C(1) C(2) O(2) C(10) . . . . -139.9(7) no C(1) C(2) C(3) C(4) . . . . -0.1(13) no C(1) C(2) C(3) C(7) . . . . 179.9(8) no C(1) C(6) C(5) C(4) . . . . -0.1(14) no C(2) O(2) C(10) C(11) . . . . -37.0(10) no C(2) O(2) C(10) C(15) . . . . 144.0(7) no C(2) C(1) P(1) C(16) . . . . 179.2(7) no C(2) C(1) P(1) C(22) . . . . -75.8(8) no C(2) C(1) C(6) C(5) . . . . 0.5(13) no C(2) C(3) C(4) C(5) . . . . 0.5(13) no C(2) C(3) C(7) C(8) . . . . -161.7(8) no C(2) C(3) C(7) C(9) . . . . 77.5(10) no C(2) C(3) C(7) C(11) . . . . -39.2(10) no C(3) C(2) O(2) C(10) . . . . 39.2(10) no C(3) C(2) C(1) C(6) . . . . -0.4(13) no C(3) C(4) C(5) C(6) . . . . -0.4(14) no C(3) C(7) C(11) C(10) . . . . 41.3(10) no C(3) C(7) C(11) C(12) . . . . -142.1(9) no C(4) C(3) C(7) C(8) . . . . 18.2(12) no C(4) C(3) C(7) C(9) . . . . -102.5(10) no C(4) C(3) C(7) C(11) . . . . 140.7(9) no C(5) C(4) C(3) C(7) . . . . -179.5(8) no C(6) C(1) P(1) C(16) . . . . 0.1(8) no C(6) C(1) P(1) C(22) . . . . 105.1(8) no C(7) C(11) C(10) C(15) . . . . 174.2(8) no C(7) C(11) C(12) C(13) . . . . -175.9(9) no C(8) C(7) C(11) C(10) . . . . 164.5(8) no C(8) C(7) C(11) C(12) . . . . -18.9(12) no C(9) C(7) C(11) C(10) . . . . -75.6(10) no C(9) C(7) C(11) C(12) . . . . 101.1(10) no C(10) C(11) C(12) C(13) . . . . 0.7(13) no C(10) C(15) P(2) C(28) . . . . 60.9(7) no C(10) C(15) P(2) C(34) . . . . 167.0(7) no C(10) C(15) C(14) C(13) . . . . 1.1(13) no C(11) C(10) C(15) C(14) . . . . 1.8(13) no C(11) C(12) C(13) C(14) . . . . 2.2(15) no C(12) C(11) C(10) C(15) . . . . -2.7(13) no C(12) C(13) C(14) C(15) . . . . -3.1(15) no C(14) C(15) P(2) C(28) . . . . -113.8(8) no C(14) C(15) P(2) C(34) . . . . -7.6(9) no C(15) P(2) C(28) C(29) . . . . -165.0(8) no C(15) P(2) C(28) C(33) . . . . 22.6(8) no C(15) P(2) C(34) C(35) . . . . -123.6(8) no C(15) P(2) C(34) C(39) . . . . 57.8(9) no C(16) P(1) C(22) C(23) . . . . 114.4(8) no C(16) P(1) C(22) C(27) . . . . -63.2(8) no C(16) C(17) C(18) C(19) . . . . -2.3(14) no C(16) C(21) C(20) C(19) . . . . -1.9(16) no C(17) C(16) P(1) C(22) . . . . 165.3(7) no C(17) C(16) C(21) C(20) . . . . 1.3(14) no C(17) C(18) C(19) C(20) . . . . 1.7(15) no C(18) C(17) C(16) C(21) . . . . 0.8(13) no C(18) C(19) C(20) C(21) . . . . 0.4(16) no C(21) C(16) P(1) C(22) . . . . -27.3(8) no C(22) C(23) C(24) C(25) . . . . -0.4(15) no C(22) C(27) C(26) C(25) . . . . -1.6(15) no C(23) C(22) C(27) C(26) . . . . 0.1(14) no C(23) C(24) C(25) C(26) . . . . -1.0(16) no C(24) C(23) C(22) C(27) . . . . 0.9(14) no C(24) C(25) C(26) C(27) . . . . 2.1(16) no C(28) P(2) C(34) C(35) . . . . -16.9(9) no C(28) P(2) C(34) C(39) . . . . 164.6(8) no C(28) C(29) C(30) C(31) . . . . 0.2(16) no C(28) C(33) C(32) C(31) . . . . -3.4(15) no C(29) C(28) P(2) C(34) . . . . 87.5(8) no C(29) C(28) C(33) C(32) . . . . 4.2(14) no C(29) C(30) C(31) C(32) . . . . 0.7(16) no C(30) C(29) C(28) C(33) . . . . -2.6(14) no C(30) C(31) C(32) C(33) . . . . 0.9(16) no C(33) C(28) P(2) C(34) . . . . -84.8(8) no C(34) C(35) C(36) C(37) . . . . 0.2(16) no C(34) C(39) C(38) C(37) . . . . -3.2(16) no C(35) C(34) C(39) C(38) . . . . 3.6(15) no C(35) C(36) C(37) C(38) . . . . 0.3(18) no C(36) C(35) C(34) C(39) . . . . -2.2(15) no C(36) C(37) C(38) C(39) . . . . 1.2(18) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_2334ReCl3(O)(binap) _database_code_depnum_ccdc_archive 'CCDC 247681' _audit_creation_date 2003-07-22 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 11.4133(2) _cell_length_b 12.1448(2) _cell_length_c 17.4349(3) _cell_angle_alpha 84.6835(7) _cell_angle_beta 72.1592(7) _cell_angle_gamma 75.5004(7) _cell_volume 2226.87(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 7970 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1094.30 _chemical_formula_analytical ? _chemical_formula_sum 'C51 H40 Cl5 O P2 Re ' _chemical_formula_moiety 'C44 H32 Cl3 O P2 Re,C6 H6, C H2 Cl2' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1088.00 _exptl_absorpt_coefficient_mu 3.140 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 17475 _reflns_number_total 10111 _reflns_number_gt 7785 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.03330 _diffrn_reflns_av_sigmaI/netI 0.085 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 102 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 80 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 10 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 2 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Re 0 2 -1.598 7.232 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.464131(13) 0.459602(11) 0.761555(9) 0.02228(4) 1.000 . Uani d ? Cl(1) 0.55355(8) 0.51125(7) 0.85532(5) 0.0263(3) 1.000 . Uani d ? Cl(2) 0.51892(9) 0.61973(7) 0.68297(5) 0.0290(3) 1.000 . Uani d ? Cl(3) 0.26702(9) 0.58549(8) 0.82491(6) 0.0333(3) 1.000 . Uani d ? Cl(4) 0.4059(2) 0.1899(2) 0.53449(13) 0.1130(8) 1.000 . Uani d ? Cl(5) 0.18261(13) 0.2739(1) 0.48199(10) 0.0869(6) 1.000 . Uani d ? P(1) 0.67814(9) 0.34424(7) 0.69242(5) 0.0202(2) 1.000 . Uani d ? P(2) 0.42438(8) 0.31083(7) 0.86734(5) 0.0189(2) 1.000 . Uani d ? O(1) 0.4070(2) 0.3953(2) 0.69961(13) 0.0249(7) 1.000 . Uani d ? C(1) 0.6783(3) 0.1346(3) 0.7800(2) 0.0204(9) 1.000 . Uani d ? C(2) 0.6822(3) 0.1917(3) 0.7071(2) 0.0202(9) 1.000 . Uani d ? C(3) 0.6767(3) 0.1336(3) 0.6416(2) 0.0251(10) 1.000 . Uani d ? C(4) 0.6662(4) 0.0236(3) 0.6492(2) 0.0298(11) 1.000 . Uani d ? C(5) 0.6671(3) -0.0388(3) 0.7216(2) 0.0261(10) 1.000 . Uani d ? C(6) 0.6762(3) 0.0159(3) 0.7873(2) 0.0219(10) 1.000 . Uani d ? C(7) 0.6590(4) -0.1540(3) 0.7295(2) 0.0335(12) 1.000 . Uani d ? C(8) 0.6641(4) -0.2138(3) 0.7988(3) 0.0370(12) 1.000 . Uani d ? C(9) 0.6777(4) -0.1626(3) 0.8629(2) 0.0314(11) 1.000 . Uani d ? C(10) 0.6816(3) -0.0503(3) 0.8586(2) 0.0259(10) 1.000 . Uani d ? C(11) 0.6738(3) 0.1894(3) 0.8559(2) 0.0189(9) 1.000 . Uani d ? C(12) 0.5646(3) 0.2581(3) 0.9029(2) 0.0191(9) 1.000 . Uani d ? C(13) 0.5619(3) 0.2948(3) 0.9789(2) 0.0224(10) 1.000 . Uani d ? C(14) 0.6665(3) 0.2691(3) 1.0042(2) 0.0231(10) 1.000 . Uani d ? C(15) 0.7819(3) 0.2033(3) 0.9569(2) 0.0244(10) 1.000 . Uani d ? C(16) 0.7846(3) 0.1597(3) 0.8833(2) 0.0227(10) 1.000 . Uani d ? C(17) 0.8917(4) 0.1761(3) 0.9821(2) 0.0325(12) 1.000 . Uani d ? C(18) 1.0012(4) 0.1075(3) 0.9377(3) 0.0372(13) 1.000 . Uani d ? C(19) 1.0035(4) 0.0600(3) 0.8668(3) 0.0350(12) 1.000 . Uani d ? C(20) 0.8990(4) 0.0847(3) 0.8405(2) 0.0285(11) 1.000 . Uani d ? C(21) 0.8168(3) 0.3678(3) 0.7125(2) 0.0230(10) 1.000 . Uani d ? C(22) 0.9210(4) 0.2790(3) 0.7096(2) 0.0299(11) 1.000 . Uani d ? C(23) 1.0310(4) 0.2985(4) 0.7173(3) 0.0380(13) 1.000 . Uani d ? C(24) 1.0385(4) 0.4087(4) 0.7260(2) 0.0384(13) 1.000 . Uani d ? C(25) 0.9360(4) 0.4980(3) 0.7264(2) 0.0346(12) 1.000 . Uani d ? C(26) 0.8251(3) 0.4793(3) 0.7198(2) 0.0273(11) 1.000 . Uani d ? C(27) 0.7165(3) 0.3692(3) 0.5829(2) 0.0237(10) 1.000 . Uani d ? C(28) 0.8380(4) 0.3750(4) 0.5383(2) 0.0441(13) 1.000 . Uani d ? C(29) 0.8681(4) 0.3908(4) 0.4551(3) 0.055(2) 1.000 . Uani d ? C(30) 0.7781(4) 0.4019(3) 0.4160(2) 0.0410(13) 1.000 . Uani d ? C(31) 0.6580(4) 0.3971(4) 0.4603(2) 0.0393(13) 1.000 . Uani d ? C(32) 0.6268(4) 0.3823(3) 0.5431(2) 0.0352(12) 1.000 . Uani d ? C(33) 0.2874(3) 0.3638(3) 0.9536(2) 0.0211(10) 1.000 . Uani d ? C(34) 0.2824(3) 0.4549(3) 0.9992(2) 0.0244(10) 1.000 . Uani d ? C(35) 0.1771(4) 0.4956(3) 1.0626(2) 0.0268(10) 1.000 . Uani d ? C(36) 0.0739(3) 0.4476(3) 1.0810(2) 0.0327(11) 1.000 . Uani d ? C(37) 0.0752(3) 0.3609(3) 1.0348(3) 0.0354(12) 1.000 . Uani d ? C(38) 0.1814(3) 0.3188(3) 0.9714(2) 0.0270(11) 1.000 . Uani d ? C(39) 0.3911(3) 0.1805(3) 0.8433(2) 0.0211(10) 1.000 . Uani d ? C(40) 0.3620(3) 0.1656(3) 0.7739(2) 0.0280(11) 1.000 . Uani d ? C(41) 0.3373(4) 0.0626(3) 0.7617(3) 0.0369(13) 1.000 . Uani d ? C(42) 0.3404(4) -0.0230(3) 0.8180(3) 0.0377(13) 1.000 . Uani d ? C(43) 0.3666(4) -0.0085(3) 0.8881(3) 0.0341(12) 1.000 . Uani d ? C(44) 0.3914(3) 0.0932(3) 0.9010(2) 0.0275(10) 1.000 . Uani d ? C(45) 0.0135(6) -0.0584(6) 0.6250(4) 0.077(2) 1.000 . Uani d ? C(46) 0.0138(6) -0.1352(5) 0.6884(4) 0.083(2) 1.000 . Uani d ? C(47) 0.1207(11) -0.1737(5) 0.7073(4) 0.101(3) 1.000 . Uani d ? C(48) 0.2317(9) -0.1441(8) 0.6641(7) 0.115(4) 1.000 . Uani d ? C(49) 0.2259(7) -0.0673(8) 0.6017(6) 0.103(3) 1.000 . Uani d ? C(50) 0.1199(8) -0.0246(6) 0.5819(4) 0.089(2) 1.000 . Uani d ? C(51) 0.2985(5) 0.3087(4) 0.5163(3) 0.071(2) 1.000 . Uani d ? H(1) 0.6803 0.1724 0.5914 0.030 1.000 . Uiso c ? H(2) 0.6582 -0.0116 0.6052 0.036 1.000 . Uiso c ? H(3) 0.6500 -0.1898 0.6861 0.040 1.000 . Uiso c ? H(4) 0.6582 -0.2910 0.8036 0.045 1.000 . Uiso c ? H(5) 0.6845 -0.2061 0.9101 0.038 1.000 . Uiso c ? H(6) 0.6879 -0.0162 0.9036 0.031 1.000 . Uiso c ? H(7) 0.4850 0.3383 1.0125 0.027 1.000 . Uiso c ? H(8) 0.6620 0.2959 1.0547 0.028 1.000 . Uiso c ? H(9) 0.8896 0.2061 1.0310 0.039 1.000 . Uiso c ? H(10) 1.0754 0.0920 0.9546 0.045 1.000 . Uiso c ? H(11) 1.0788 0.0102 0.8368 0.042 1.000 . Uiso c ? H(12) 0.9026 0.0510 0.7925 0.034 1.000 . Uiso c ? H(13) 0.9170 0.2037 0.7021 0.036 1.000 . Uiso c ? H(14) 1.1013 0.2366 0.7167 0.045 1.000 . Uiso c ? H(15) 1.1137 0.4226 0.7317 0.046 1.000 . Uiso c ? H(16) 0.9419 0.5736 0.7313 0.041 1.000 . Uiso c ? H(17) 0.7551 0.5415 0.7202 0.033 1.000 . Uiso c ? H(18) 0.9013 0.3681 0.5645 0.053 1.000 . Uiso c ? H(19) 0.9520 0.3941 0.4250 0.066 1.000 . Uiso c ? H(20) 0.7990 0.4127 0.3592 0.049 1.000 . Uiso c ? H(21) 0.5949 0.4040 0.4339 0.047 1.000 . Uiso c ? H(22) 0.5421 0.3812 0.5729 0.042 1.000 . Uiso c ? H(23) 0.3525 0.4890 0.9862 0.029 1.000 . Uiso c ? H(24) 0.1755 0.5566 1.0935 0.032 1.000 . Uiso c ? H(25) 0.0020 0.4744 1.1254 0.039 1.000 . Uiso c ? H(26) 0.0030 0.3298 1.0465 0.042 1.000 . Uiso c ? H(27) 0.1815 0.2589 0.9399 0.032 1.000 . Uiso c ? H(28) 0.3588 0.2253 0.7348 0.034 1.000 . Uiso c ? H(29) 0.3183 0.0521 0.7138 0.044 1.000 . Uiso c ? H(30) 0.3244 -0.0931 0.8089 0.045 1.000 . Uiso c ? H(31) 0.3676 -0.0681 0.9275 0.041 1.000 . Uiso c ? H(32) 0.4087 0.1034 0.9494 0.033 1.000 . Uiso c ? H(33) -0.0626 -0.0281 0.6112 0.093 1.000 . Uiso c ? H(34) -0.0608 -0.1597 0.7174 0.099 1.000 . Uiso c ? H(35) 0.1211 -0.2237 0.7526 0.120 1.000 . Uiso c ? H(36) 0.3091 -0.1751 0.6765 0.138 1.000 . Uiso c ? H(37) 0.3005 -0.0434 0.5714 0.124 1.000 . Uiso c ? H(38) 0.1187 0.0283 0.5383 0.107 1.000 . Uiso c ? H(39) 0.2579 0.3498 0.5649 0.085 1.000 . Uiso c ? H(40) 0.3425 0.3549 0.4766 0.085 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.02419(9) 0.02017(8) 0.02094(9) -0.00547(6) -0.00517(6) 0.00299(5) Cl(1) 0.0314(5) 0.0261(5) 0.0235(5) -0.0113(4) -0.0077(4) 0.0003(4) Cl(2) 0.0408(6) 0.0240(5) 0.0246(5) -0.0122(4) -0.0112(4) 0.0065(4) Cl(3) 0.0291(5) 0.0308(5) 0.0312(5) 0.0027(4) -0.0048(4) 0.0017(4) Cl(4) 0.104(1) 0.106(1) 0.152(2) -0.0392(11) -0.0671(13) 0.0211(12) Cl(5) 0.0614(10) 0.1104(13) 0.0793(11) -0.0130(9) -0.0088(8) -0.0148(9) P(1) 0.0251(5) 0.0199(5) 0.0160(5) -0.0078(4) -0.0048(4) 0.0008(4) P(2) 0.0216(5) 0.0185(5) 0.0177(5) -0.0068(4) -0.0054(4) -0.0015(4) O(1) 0.037(2) 0.0226(13) 0.0183(13) -0.0149(11) -0.0048(11) -0.0033(10) C(1) 0.018(2) 0.020(2) 0.023(2) -0.005(1) -0.003(2) -0.003(1) C(2) 0.021(2) 0.019(2) 0.022(2) -0.008(1) -0.003(2) -0.004(1) C(3) 0.031(2) 0.025(2) 0.019(2) -0.007(2) -0.007(2) 0.000(2) C(4) 0.040(2) 0.027(2) 0.024(2) -0.013(2) -0.005(2) -0.008(2) C(5) 0.029(2) 0.021(2) 0.026(2) -0.007(2) -0.003(2) -0.003(2) C(6) 0.019(2) 0.018(2) 0.026(2) -0.003(1) -0.003(2) -0.002(1) C(7) 0.044(3) 0.023(2) 0.033(2) -0.012(2) -0.004(2) -0.008(2) C(8) 0.045(3) 0.019(2) 0.045(3) -0.014(2) -0.005(2) -0.003(2) C(9) 0.035(2) 0.023(2) 0.032(2) -0.007(2) -0.006(2) 0.005(2) C(10) 0.025(2) 0.024(2) 0.026(2) -0.006(2) -0.003(2) -0.001(2) C(11) 0.023(2) 0.016(2) 0.020(2) -0.012(1) -0.004(2) 0.0030(13) C(12) 0.020(2) 0.016(2) 0.022(2) -0.010(1) -0.006(2) 0.006(1) C(13) 0.028(2) 0.021(2) 0.021(2) -0.009(2) -0.008(2) -0.002(1) C(14) 0.035(2) 0.018(2) 0.022(2) -0.011(2) -0.014(2) 0.002(1) C(15) 0.031(2) 0.020(2) 0.029(2) -0.014(2) -0.013(2) 0.007(2) C(16) 0.024(2) 0.021(2) 0.024(2) -0.010(2) -0.007(2) 0.006(2) C(17) 0.035(2) 0.032(2) 0.040(3) -0.014(2) -0.023(2) 0.007(2) C(18) 0.032(2) 0.034(2) 0.056(3) -0.014(2) -0.028(2) 0.014(2) C(19) 0.023(2) 0.034(2) 0.047(3) -0.008(2) -0.011(2) 0.008(2) C(20) 0.028(2) 0.025(2) 0.032(2) -0.008(2) -0.009(2) 0.004(2) C(21) 0.025(2) 0.029(2) 0.015(2) -0.012(2) -0.004(2) 0.003(2) C(22) 0.028(2) 0.034(2) 0.028(2) -0.013(2) -0.005(2) 0.008(2) C(23) 0.026(2) 0.046(3) 0.040(3) -0.010(2) -0.010(2) 0.009(2) C(24) 0.031(2) 0.060(3) 0.030(2) -0.025(2) -0.007(2) 0.003(2) C(25) 0.041(3) 0.042(3) 0.024(2) -0.025(2) -0.001(2) -0.004(2) C(26) 0.026(2) 0.031(2) 0.026(2) -0.012(2) -0.003(2) -0.002(2) C(27) 0.032(2) 0.019(2) 0.018(2) -0.006(2) -0.004(2) 0.001(1) C(28) 0.036(3) 0.068(3) 0.024(2) -0.011(2) -0.007(2) 0.009(2) C(29) 0.041(3) 0.090(4) 0.027(3) -0.017(3) -0.001(2) 0.010(2) C(30) 0.062(3) 0.043(3) 0.014(2) -0.014(2) -0.007(2) 0.004(2) C(31) 0.053(3) 0.049(3) 0.023(2) -0.017(2) -0.016(2) 0.002(2) C(32) 0.037(3) 0.047(3) 0.021(2) -0.015(2) -0.005(2) -0.000(2) C(33) 0.021(2) 0.021(2) 0.021(2) -0.004(2) -0.006(2) 0.002(1) C(34) 0.028(2) 0.021(2) 0.023(2) -0.007(2) -0.005(2) 0.002(2) C(35) 0.031(2) 0.025(2) 0.025(2) -0.006(2) -0.008(2) -0.003(2) C(36) 0.026(2) 0.042(2) 0.028(2) -0.009(2) -0.002(2) -0.007(2) C(37) 0.019(2) 0.046(3) 0.041(3) -0.014(2) -0.002(2) -0.007(2) C(38) 0.028(2) 0.032(2) 0.025(2) -0.012(2) -0.007(2) -0.006(2) C(39) 0.016(2) 0.020(2) 0.027(2) -0.007(1) -0.005(2) -0.002(2) C(40) 0.027(2) 0.028(2) 0.032(2) -0.007(2) -0.009(2) -0.007(2) C(41) 0.034(2) 0.039(3) 0.043(3) -0.011(2) -0.013(2) -0.013(2) C(42) 0.028(2) 0.025(2) 0.061(3) -0.011(2) -0.006(2) -0.012(2) C(43) 0.025(2) 0.022(2) 0.049(3) -0.009(2) 0.000(2) -0.000(2) C(44) 0.026(2) 0.025(2) 0.028(2) -0.009(2) -0.002(2) -0.000(2) C(45) 0.057(4) 0.093(5) 0.067(4) 0.016(3) -0.021(3) -0.014(4) C(46) 0.083(5) 0.060(4) 0.078(5) -0.000(3) 0.007(4) -0.021(3) C(47) 0.170(8) 0.042(4) 0.084(5) 0.042(5) -0.073(6) -0.028(3) C(48) 0.095(6) 0.100(7) 0.164(10) 0.058(5) -0.096(7) -0.096(7) C(49) 0.059(5) 0.122(7) 0.126(7) -0.019(5) -0.007(5) -0.073(6) C(50) 0.094(5) 0.097(5) 0.057(4) -0.015(4) -0.003(4) 0.004(3) C(51) 0.087(4) 0.068(4) 0.051(3) -0.038(3) 0.009(3) -0.013(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7785 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_all 0.0370 _refine_ls_wR_factor_ref 0.0330 _refine_ls_goodness_of_fit_all 1.011 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -1.43 _refine_diff_density_max 1.91 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RE1 CL1 2.3749(9) . . ? RE1 CL2 2.3749(9) . . ? RE1 CL3 2.3847(9) . . ? RE1 P1 2.4854(9) . . ? RE1 P2 2.4803(9) . . ? RE1 O1 1.744(2) . . ? CL4 C51 1.718(6) . . ? CL5 C51 1.761(6) . . ? P1 C2 1.838(3) . . ? P1 C21 1.815(4) . . ? P1 C27 1.837(4) . . ? P2 C12 1.838(4) . . ? P2 C33 1.832(3) . . ? P2 C39 1.829(3) . . ? C1 C2 1.384(5) . . ? C1 C6 1.442(5) . . ? C1 C11 1.517(5) . . ? C2 C3 1.421(5) . . ? C3 C4 1.361(5) . . ? C3 H1 0.95 . . no C4 C5 1.412(5) . . ? C4 H2 0.95 . . no C5 C6 1.418(5) . . ? C5 C7 1.417(5) . . ? C6 C10 1.426(5) . . ? C7 C8 1.360(6) . . ? C7 H3 0.95 . . no C8 C9 1.394(5) . . ? C8 H4 0.95 . . no C9 C10 1.369(5) . . ? C9 H5 0.95 . . no C10 H6 0.95 . . no C11 C12 1.379(4) . . ? C11 C16 1.437(5) . . ? C12 C13 1.426(5) . . ? C13 C14 1.351(5) . . ? C13 H7 0.95 . . no C14 C15 1.408(5) . . ? C14 H8 0.95 . . no C15 C16 1.422(5) . . ? C15 C17 1.405(5) . . ? C16 C20 1.424(5) . . ? C17 C18 1.365(5) . . ? C17 H9 0.95 . . no C18 C19 1.401(6) . . ? C18 H10 0.95 . . no C19 C20 1.361(5) . . ? C19 H11 0.95 . . no C20 H12 0.95 . . no C21 C22 1.382(5) . . ? C21 C26 1.401(5) . . ? C22 C23 1.382(5) . . ? C22 H13 0.95 . . no C23 C24 1.388(6) . . ? C23 H14 0.95 . . no C24 C25 1.380(6) . . ? C24 H15 0.95 . . no C25 C26 1.380(5) . . ? C25 H16 0.95 . . no C26 H17 0.95 . . no C27 C28 1.383(5) . . ? C27 C32 1.374(5) . . ? C28 C29 1.390(6) . . ? C28 H18 0.95 . . no C29 C30 1.371(6) . . ? C29 H19 0.95 . . no C30 C31 1.365(6) . . ? C30 H20 0.95 . . no C31 C32 1.382(5) . . ? C31 H21 0.95 . . no C32 H22 0.95 . . no C33 C34 1.401(5) . . ? C33 C38 1.388(5) . . ? C34 C35 1.378(5) . . ? C34 H23 0.95 . . no C35 C36 1.382(5) . . ? C35 H24 0.95 . . no C36 C37 1.377(5) . . ? C36 H25 0.95 . . no C37 C38 1.388(5) . . ? C37 H26 0.95 . . no C38 H27 0.95 . . no C39 C40 1.387(5) . . ? C39 C44 1.392(5) . . ? C40 C41 1.398(5) . . ? C40 H28 0.95 . . no C41 C42 1.364(6) . . ? C41 H29 0.95 . . no C42 C43 1.380(6) . . ? C42 H30 0.95 . . no C43 C44 1.386(5) . . ? C43 H31 0.95 . . no C44 H32 0.95 . . no C45 C46 1.378(9) . . ? C45 C50 1.357(9) . . ? C45 H33 0.95 . . no C46 C47 1.322(10) . . ? C46 H34 0.95 . . no C47 C48 1.376(11) . . ? C47 H35 0.95 . . no C48 C49 1.372(12) . . ? C48 H36 0.95 . . no C49 C50 1.327(10) . . ? C49 H37 0.95 . . no C50 H38 0.95 . . no C51 H39 0.95 . . no C51 H40 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 RE1 CL2 86.82(3) . . . ? CL1 RE1 CL3 89.80(3) . . . ? CL1 RE1 P1 87.73(3) . . . ? CL1 RE1 P2 79.55(3) . . . ? CL1 RE1 O1 169.05(8) . . . ? CL2 RE1 CL3 86.38(3) . . . ? CL2 RE1 P1 88.75(3) . . . ? CL2 RE1 P2 166.28(3) . . . ? CL2 RE1 O1 102.74(8) . . . ? CL3 RE1 P1 174.65(3) . . . ? CL3 RE1 P2 92.02(3) . . . ? CL3 RE1 O1 96.06(8) . . . ? P1 RE1 P2 92.19(3) . . . ? P1 RE1 O1 87.16(8) . . . ? P2 RE1 O1 90.97(8) . . . ? RE1 P1 C2 110.49(11) . . . ? RE1 P1 C21 120.08(11) . . . ? RE1 P1 C27 110.54(12) . . . ? C2 P1 C21 107.9(2) . . . ? C2 P1 C27 105.2(2) . . . ? C21 P1 C27 101.4(2) . . . ? RE1 P2 C12 109.59(11) . . . ? RE1 P2 C33 112.25(11) . . . ? RE1 P2 C39 119.79(12) . . . ? C12 P2 C33 108.8(2) . . . ? C12 P2 C39 103.3(2) . . . ? C33 P2 C39 102.3(2) . . . ? C2 C1 C6 119.8(3) . . . ? C2 C1 C11 124.2(3) . . . ? C6 C1 C11 116.0(3) . . . ? P1 C2 C1 123.4(3) . . . ? P1 C2 C3 117.1(3) . . . ? C1 C2 C3 119.2(3) . . . ? C2 C3 C4 121.6(3) . . . ? C2 C3 H1 119.2 . . . no C4 C3 H1 119.2 . . . no C3 C4 C5 120.9(3) . . . ? C3 C4 H2 119.6 . . . no C5 C4 H2 119.5 . . . no C4 C5 C6 118.8(3) . . . ? C4 C5 C7 121.3(3) . . . ? C6 C5 C7 119.9(4) . . . ? C1 C6 C5 119.5(3) . . . ? C1 C6 C10 122.9(3) . . . ? C5 C6 C10 117.6(3) . . . ? C5 C7 C8 120.5(4) . . . ? C5 C7 H3 119.7 . . . no C8 C7 H3 119.8 . . . no C7 C8 C9 120.4(3) . . . ? C7 C8 H4 119.8 . . . no C9 C8 H4 119.8 . . . no C8 C9 C10 120.9(4) . . . ? C8 C9 H5 119.6 . . . no C10 C9 H5 119.5 . . . no C6 C10 C9 120.7(3) . . . ? C6 C10 H6 119.7 . . . no C9 C10 H6 119.7 . . . no C1 C11 C12 122.4(3) . . . ? C1 C11 C16 118.3(3) . . . ? C12 C11 C16 119.1(3) . . . ? P2 C12 C11 121.4(3) . . . ? P2 C12 C13 118.8(3) . . . ? C11 C12 C13 119.7(3) . . . ? C12 C13 C14 121.4(3) . . . ? C12 C13 H7 119.3 . . . no C14 C13 H7 119.3 . . . no C13 C14 C15 121.2(3) . . . ? C13 C14 H8 119.4 . . . no C15 C14 H8 119.4 . . . no C14 C15 C16 118.3(3) . . . ? C14 C15 C17 121.9(3) . . . ? C16 C15 C17 119.7(3) . . . ? C11 C16 C15 120.2(3) . . . ? C11 C16 C20 122.7(3) . . . ? C15 C16 C20 117.2(3) . . . ? C15 C17 C18 121.4(4) . . . ? C15 C17 H9 119.3 . . . no C18 C17 H9 119.3 . . . no C17 C18 C19 119.5(4) . . . ? C17 C18 H10 120.3 . . . no C19 C18 H10 120.2 . . . no C18 C19 C20 120.7(4) . . . ? C18 C19 H11 119.6 . . . no C20 C19 H11 119.6 . . . no C16 C20 C19 121.5(4) . . . ? C16 C20 H12 119.3 . . . no C19 C20 H12 119.3 . . . no P1 C21 C22 120.7(3) . . . ? P1 C21 C26 119.3(3) . . . ? C22 C21 C26 119.4(3) . . . ? C21 C22 C23 120.8(4) . . . ? C21 C22 H13 119.6 . . . no C23 C22 H13 119.6 . . . no C22 C23 C24 119.8(4) . . . ? C22 C23 H14 120.1 . . . no C24 C23 H14 120.1 . . . no C23 C24 C25 119.6(4) . . . ? C23 C24 H15 120.2 . . . no C25 C24 H15 120.3 . . . no C24 C25 C26 121.1(4) . . . ? C24 C25 H16 119.4 . . . no C26 C25 H16 119.5 . . . no C21 C26 C25 119.3(3) . . . ? C21 C26 H17 120.3 . . . no C25 C26 H17 120.4 . . . no P1 C27 C28 120.2(3) . . . ? P1 C27 C32 121.6(3) . . . ? C28 C27 C32 118.2(3) . . . ? C27 C28 C29 120.2(4) . . . ? C27 C28 H18 119.9 . . . no C29 C28 H18 119.9 . . . no C28 C29 C30 120.9(4) . . . ? C28 C29 H19 119.6 . . . no C30 C29 H19 119.5 . . . no C29 C30 C31 118.7(4) . . . ? C29 C30 H20 120.7 . . . no C31 C30 H20 120.7 . . . no C30 C31 C32 120.9(4) . . . ? C30 C31 H21 119.5 . . . no C32 C31 H21 119.6 . . . no C27 C32 C31 121.0(4) . . . ? C27 C32 H22 119.5 . . . no C31 C32 H22 119.5 . . . no P2 C33 C34 121.7(3) . . . ? P2 C33 C38 119.8(3) . . . ? C34 C33 C38 118.4(3) . . . ? C33 C34 C35 120.9(3) . . . ? C33 C34 H23 119.5 . . . no C35 C34 H23 119.5 . . . no C34 C35 C36 119.9(3) . . . ? C34 C35 H24 120.1 . . . no C36 C35 H24 120.1 . . . no C35 C36 C37 120.0(3) . . . ? C35 C36 H25 120.0 . . . no C37 C36 H25 120.0 . . . no C36 C37 C38 120.4(3) . . . ? C36 C37 H26 119.8 . . . no C38 C37 H26 119.8 . . . no C33 C38 C37 120.4(3) . . . ? C33 C38 H27 119.8 . . . no C37 C38 H27 119.8 . . . no P2 C39 C40 124.5(3) . . . ? P2 C39 C44 116.4(3) . . . ? C40 C39 C44 119.1(3) . . . ? C39 C40 C41 119.9(4) . . . ? C39 C40 H28 120.1 . . . no C41 C40 H28 120.1 . . . no C40 C41 C42 120.3(4) . . . ? C40 C41 H29 119.8 . . . no C42 C41 H29 119.9 . . . no C41 C42 C43 120.4(3) . . . ? C41 C42 H30 119.8 . . . no C43 C42 H30 119.8 . . . no C42 C43 C44 119.8(4) . . . ? C42 C43 H31 120.1 . . . no C44 C43 H31 120.1 . . . no C39 C44 C43 120.5(4) . . . ? C39 C44 H32 119.8 . . . no C43 C44 H32 119.8 . . . no C46 C45 C50 121.5(6) . . . ? C46 C45 H33 119.5 . . . no C50 C45 H33 119.0 . . . no C45 C46 C47 118.0(7) . . . ? C45 C46 H34 120.7 . . . no C47 C46 H34 121.3 . . . no C46 C47 C48 122.6(8) . . . ? C46 C47 H35 118.8 . . . no C48 C47 H35 118.6 . . . no C47 C48 C49 116.8(7) . . . ? C47 C48 H36 122.1 . . . no C49 C48 H36 121.1 . . . no C48 C49 C50 122.5(8) . . . ? C48 C49 H37 119.1 . . . no C50 C49 H37 118.4 . . . no C45 C50 C49 118.6(7) . . . ? C45 C50 H38 120.8 . . . no C49 C50 H38 120.6 . . . no CL4 C51 CL5 112.1(3) . . . ? CL4 C51 H39 108.7 . . . no CL4 C51 H40 108.7 . . . no CL5 C51 H39 108.9 . . . no CL5 C51 H40 108.9 . . . no H39 C51 H40 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C14 C34 3.536(5) . 2_667 no C14 C43 3.570(5) . 2_657 no C18 C18 3.239(8) . 2_757 no C19 C42 3.569(6) . 1_655 no C25 C36 3.445(6) . 2_667 no C25 C35 3.507(5) . 2_667 no C30 C47 3.408(7) . 2_656 no C30 C48 3.584(8) . 2_656 no C36 C37 3.411(6) . 2_567 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag RE1 P1 C2 C1 . . . . -71.4(3) no RE1 P1 C2 C3 . . . . 102.4(3) no RE1 P1 C21 C22 . . . . 148.2(3) no RE1 P1 C21 C26 . . . . -40.9(3) no RE1 P1 C27 C28 . . . . 141.4(3) no RE1 P1 C27 C32 . . . . -38.6(3) no RE1 P2 C12 C11 . . . . -72.5(3) no RE1 P2 C12 C13 . . . . 103.8(3) no RE1 P2 C33 C34 . . . . -59.6(3) no RE1 P2 C33 C38 . . . . 115.7(3) no RE1 P2 C39 C40 . . . . -13.0(4) no RE1 P2 C39 C44 . . . . 169.3(2) no CL1 RE1 P1 C2 . . . . 109.84(12) no CL1 RE1 P1 C21 . . . . -16.7(1) no CL1 RE1 P1 C27 . . . . -134.10(13) no CL1 RE1 P2 C12 . . . . -42.05(11) no CL1 RE1 P2 C33 . . . . 78.98(13) no CL1 RE1 P2 C39 . . . . -161.02(13) no CL2 RE1 P1 C2 . . . . -163.30(12) no CL2 RE1 P1 C21 . . . . 70.2(1) no CL2 RE1 P1 C27 . . . . -47.23(13) no CL2 RE1 P2 C12 . . . . -48.5(2) no CL2 RE1 P2 C33 . . . . 72.6(2) no CL2 RE1 P2 C39 . . . . -167.4(2) no CL3 RE1 P1 C2 . . . . 172.4(4) no CL3 RE1 P1 C21 . . . . 45.9(4) no CL3 RE1 P1 C27 . . . . -71.6(4) no CL3 RE1 P2 C12 . . . . -131.47(11) no CL3 RE1 P2 C33 . . . . -10.44(13) no CL3 RE1 P2 C39 . . . . 109.57(13) no P1 RE1 P2 C12 . . . . 45.24(11) no P1 RE1 P2 C33 . . . . 166.27(13) no P1 RE1 P2 C39 . . . . -73.73(13) no P1 C2 C1 C6 . . . . 177.2(2) no P1 C2 C1 C11 . . . . -1.7(5) no P1 C2 C3 C4 . . . . -173.3(3) no P1 C21 C22 C23 . . . . 173.8(3) no P1 C21 C26 C25 . . . . -173.1(3) no P1 C27 C28 C29 . . . . 178.3(4) no P1 C27 C32 C31 . . . . -177.8(3) no P2 RE1 P1 C2 . . . . 30.39(12) no P2 RE1 P1 C21 . . . . -96.1(1) no P2 RE1 P1 C27 . . . . 146.46(13) no P2 C12 C11 C1 . . . . -12.0(4) no P2 C12 C11 C16 . . . . 174.0(2) no P2 C12 C13 C14 . . . . -172.6(3) no P2 C33 C34 C35 . . . . 178.2(3) no P2 C33 C38 C37 . . . . -177.7(3) no P2 C39 C40 C41 . . . . -179.6(3) no P2 C39 C44 C43 . . . . 179.7(3) no O1 RE1 P1 C2 . . . . -60.5(2) no O1 RE1 P1 C21 . . . . 173.0(2) no O1 RE1 P1 C27 . . . . 55.6(2) no O1 RE1 P2 C12 . . . . 132.4(1) no O1 RE1 P2 C33 . . . . -106.5(2) no O1 RE1 P2 C39 . . . . 13.5(2) no C1 C2 P1 C21 . . . . 61.7(3) no C1 C2 P1 C27 . . . . 169.3(3) no C1 C2 C3 C4 . . . . 0.8(5) no C1 C6 C5 C4 . . . . 2.8(5) no C1 C6 C5 C7 . . . . -177.1(3) no C1 C6 C10 C9 . . . . 179.2(3) no C1 C11 C12 C13 . . . . 171.7(3) no C1 C11 C16 C15 . . . . -175.9(3) no C1 C11 C16 C20 . . . . 2.4(5) no C2 P1 C21 C22 . . . . 20.5(3) no C2 P1 C21 C26 . . . . -168.6(3) no C2 P1 C27 C28 . . . . -99.2(3) no C2 P1 C27 C32 . . . . 80.7(3) no C2 C1 C6 C5 . . . . -5.4(5) no C2 C1 C6 C10 . . . . 175.3(3) no C2 C1 C11 C12 . . . . 77.1(5) no C2 C1 C11 C16 . . . . -108.9(4) no C2 C3 C4 C5 . . . . -3.3(6) no C3 C2 P1 C21 . . . . -124.5(3) no C3 C2 P1 C27 . . . . -16.9(3) no C3 C2 C1 C6 . . . . 3.6(5) no C3 C2 C1 C11 . . . . -175.3(3) no C3 C4 C5 C6 . . . . 1.4(6) no C3 C4 C5 C7 . . . . -178.7(4) no C4 C5 C6 C10 . . . . -177.7(3) no C4 C5 C7 C8 . . . . 177.9(4) no C5 C6 C1 C11 . . . . 173.6(3) no C5 C6 C10 C9 . . . . -0.2(5) no C5 C7 C8 C9 . . . . -0.2(6) no C6 C1 C11 C12 . . . . -101.9(4) no C6 C1 C11 C16 . . . . 72.1(4) no C6 C5 C7 C8 . . . . -2.2(6) no C6 C10 C9 C8 . . . . -2.2(6) no C7 C5 C6 C10 . . . . 2.4(5) no C7 C8 C9 C10 . . . . 2.5(6) no C10 C6 C1 C11 . . . . -5.8(5) no C11 C12 P2 C33 . . . . 164.4(3) no C11 C12 P2 C39 . . . . 56.2(3) no C11 C12 C13 C14 . . . . 3.8(5) no C11 C16 C15 C14 . . . . 4.3(5) no C11 C16 C15 C17 . . . . -178.4(3) no C11 C16 C20 C19 . . . . 178.4(3) no C12 P2 C33 C34 . . . . 61.9(3) no C12 P2 C33 C38 . . . . -122.9(3) no C12 P2 C39 C40 . . . . -135.1(3) no C12 P2 C39 C44 . . . . 47.2(3) no C12 C11 C16 C15 . . . . -1.7(5) no C12 C11 C16 C20 . . . . 176.7(3) no C12 C13 C14 C15 . . . . -1.0(5) no C13 C12 P2 C33 . . . . -19.3(3) no C13 C12 P2 C39 . . . . -127.5(3) no C13 C12 C11 C16 . . . . -2.3(5) no C13 C14 C15 C16 . . . . -2.9(5) no C13 C14 C15 C17 . . . . 179.8(3) no C14 C15 C16 C20 . . . . -174.2(3) no C14 C15 C17 C18 . . . . 176.6(4) no C15 C16 C20 C19 . . . . -3.2(5) no C15 C17 C18 C19 . . . . -2.1(6) no C16 C15 C17 C18 . . . . -0.7(6) no C16 C20 C19 C18 . . . . 0.5(6) no C17 C15 C16 C20 . . . . 3.2(5) no C17 C18 C19 C20 . . . . 2.2(6) no C21 P1 C27 C28 . . . . 13.0(3) no C21 P1 C27 C32 . . . . -167.0(3) no C21 C22 C23 C24 . . . . -1.8(6) no C21 C26 C25 C24 . . . . -0.0(6) no C22 C21 P1 C27 . . . . -89.8(3) no C22 C21 C26 C25 . . . . -2.0(5) no C22 C23 C24 C25 . . . . -0.3(6) no C23 C22 C21 C26 . . . . 2.9(6) no C23 C24 C25 C26 . . . . 1.2(6) no C26 C21 P1 C27 . . . . 81.1(3) no C27 C28 C29 C30 . . . . 0.6(7) no C27 C32 C31 C30 . . . . -1.7(7) no C28 C27 C32 C31 . . . . 2.2(6) no C28 C29 C30 C31 . . . . 0.0(7) no C29 C28 C27 C32 . . . . -1.6(6) no C29 C30 C31 C32 . . . . 0.5(7) no C33 P2 C39 C40 . . . . 111.9(3) no C33 P2 C39 C44 . . . . -65.8(3) no C33 C34 C35 C36 . . . . -1.0(6) no C33 C38 C37 C36 . . . . -0.2(6) no C34 C33 P2 C39 . . . . 170.7(3) no C34 C33 C38 C37 . . . . -2.3(6) no C34 C35 C36 C37 . . . . -1.5(6) no C35 C34 C33 C38 . . . . 2.9(6) no C35 C36 C37 C38 . . . . 2.1(7) no C38 C33 P2 C39 . . . . -14.1(3) no C39 C40 C41 C42 . . . . 0.7(6) no C39 C44 C43 C42 . . . . -0.6(6) no C40 C39 C44 C43 . . . . 1.9(5) no C40 C41 C42 C43 . . . . 0.7(6) no C41 C40 C39 C44 . . . . -2.0(5) no C41 C42 C43 C44 . . . . -0.8(6) no C45 C46 C47 C48 . . . . -3.1(9) no C45 C50 C49 C48 . . . . 0.0(11) no C46 C45 C50 C49 . . . . 0.1(10) no C46 C47 C48 C49 . . . . 3.1(10) no C47 C46 C45 C50 . . . . 1.4(9) no C47 C48 C49 C50 . . . . -1.5(11) no #============================================================================== data_2337Re(O)Cl3Biphep-100sqz _database_code_depnum_ccdc_archive 'CCDC 247682' #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 10.6209(3) _cell_length_b 11.6561(3) _cell_length_c 16.7301(5) _cell_angle_alpha 69.9318(13) _cell_angle_beta 85.4535(13) _cell_angle_gamma 69.6000(13) _cell_volume 1821.48(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 6174 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 905.25 _chemical_formula_analytical ? _chemical_formula_sum 'C40 H38 Cl3 O2 P2 Re ' _chemical_formula_moiety 'C36 H28 Cl3 O P2 Re, C4 H10 O' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 900.00 _exptl_absorpt_coefficient_mu 3.680 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 13931 _reflns_number_total 8302 _reflns_number_gt 5172 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04856 _diffrn_reflns_av_sigmaI/netI 0.107 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 80 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 76 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 6 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Re 0 2 -1.598 7.232 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.24059(3) 0.19756(2) 0.19142(2) 0.03341(8) 1.000 . Uani d ? Cl(1) 0.2460(2) 0.0908(1) 0.33899(9) 0.0435(5) 1.000 . Uani d ? Cl(2) 0.0069(2) 0.2982(2) 0.19821(10) 0.0462(5) 1.000 . Uani d ? Cl(3) 0.1830(2) 0.0373(2) 0.16105(10) 0.0480(5) 1.000 . Uani d ? P(1) 0.2706(2) 0.37898(13) 0.22359(8) 0.0262(4) 1.000 . Uani d ? P(2) 0.4812(2) 0.06011(13) 0.21703(9) 0.0270(4) 1.000 . Uani d ? O(1) 0.2760(3) 0.2831(3) 0.0841(2) 0.0236(10) 1.000 . Uani d ? C(1) 0.4293(6) 0.3996(5) 0.1881(3) 0.025(2) 1.000 . Uani d ? C(2) 0.5564(6) 0.3101(5) 0.2253(3) 0.024(2) 1.000 . Uani d ? C(3) 0.6736(6) 0.3361(5) 0.1933(4) 0.031(2) 1.000 . Uani d ? C(4) 0.6685(6) 0.4442(6) 0.1247(4) 0.037(2) 1.000 . Uani d ? C(5) 0.5446(7) 0.5312(6) 0.0863(4) 0.038(2) 1.000 . Uani d ? C(6) 0.4270(6) 0.5086(5) 0.1187(3) 0.031(2) 1.000 . Uani d ? C(7) 0.5583(5) 0.0743(5) 0.3060(3) 0.026(2) 1.000 . Uani d ? C(8) 0.5785(5) 0.1896(5) 0.3020(3) 0.025(2) 1.000 . Uani d ? C(9) 0.6382(6) 0.1884(5) 0.3737(4) 0.034(2) 1.000 . Uani d ? C(10) 0.6678(6) 0.0811(6) 0.4491(4) 0.038(2) 1.000 . Uani d ? C(11) 0.6449(6) -0.0286(6) 0.4526(4) 0.038(2) 1.000 . Uani d ? C(12) 0.5914(6) -0.0327(5) 0.3810(3) 0.035(2) 1.000 . Uani d ? C(13) 0.1423(6) 0.5346(5) 0.1647(4) 0.033(2) 1.000 . Uani d ? C(14) 0.0959(6) 0.6333(6) 0.1984(4) 0.042(2) 1.000 . Uani d ? C(15) -0.0012(8) 0.7541(6) 0.1504(5) 0.056(2) 1.000 . Uani d ? C(16) -0.0483(7) 0.7719(6) 0.0732(5) 0.048(2) 1.000 . Uani d ? C(17) 0.0012(8) 0.6761(7) 0.0388(4) 0.055(2) 1.000 . Uani d ? C(18) 0.0955(7) 0.5556(6) 0.0824(4) 0.046(2) 1.000 . Uani d ? C(19) 0.2531(6) 0.3790(5) 0.3335(3) 0.029(2) 1.000 . Uani d ? C(20) 0.3436(7) 0.4042(5) 0.3726(3) 0.034(2) 1.000 . Uani d ? C(21) 0.3244(7) 0.4102(6) 0.4536(4) 0.042(2) 1.000 . Uani d ? C(22) 0.2109(8) 0.3926(6) 0.4961(4) 0.050(2) 1.000 . Uani d ? C(23) 0.1174(7) 0.3699(6) 0.4550(4) 0.045(2) 1.000 . Uani d ? C(24) 0.1387(7) 0.3608(5) 0.3742(4) 0.037(2) 1.000 . Uani d ? C(25) 0.5860(6) 0.0965(5) 0.1258(3) 0.029(2) 1.000 . Uani d ? C(26) 0.7114(6) 0.0977(5) 0.1350(4) 0.033(2) 1.000 . Uani d ? C(27) 0.7933(6) 0.1170(5) 0.0655(4) 0.040(2) 1.000 . Uani d ? C(28) 0.7442(7) 0.1341(5) -0.0136(4) 0.044(2) 1.000 . Uani d ? C(29) 0.6182(7) 0.1291(6) -0.0228(4) 0.043(2) 1.000 . Uani d ? C(30) 0.5368(6) 0.1110(5) 0.0456(4) 0.035(2) 1.000 . Uani d ? C(31) 0.5213(7) -0.1142(5) 0.2436(3) 0.033(2) 1.000 . Uani d ? C(32) 0.6389(7) -0.1863(6) 0.2167(4) 0.046(2) 1.000 . Uani d ? C(33) 0.6752(8) -0.3211(6) 0.2354(5) 0.062(3) 1.000 . Uani d ? C(34) 0.5896(9) -0.3841(6) 0.2836(5) 0.060(3) 1.000 . Uani d ? C(35) 0.4707(9) -0.3112(7) 0.3091(5) 0.063(3) 1.000 . Uani d ? C(36) 0.4374(7) -0.1786(6) 0.2899(4) 0.043(2) 1.000 . Uani d ? H(1) 0.7585 0.2772 0.2199 0.037 1.000 . Uiso c ? H(2) 0.7490 0.4597 0.1039 0.044 1.000 . Uiso c ? H(3) 0.5399 0.6055 0.0378 0.046 1.000 . Uiso c ? H(4) 0.3425 0.5699 0.0927 0.037 1.000 . Uiso c ? H(5) 0.6592 0.2623 0.3713 0.040 1.000 . Uiso c ? H(6) 0.7040 0.0848 0.4980 0.045 1.000 . Uiso c ? H(7) 0.6658 -0.1016 0.5036 0.046 1.000 . Uiso c ? H(8) 0.5767 -0.1096 0.3832 0.041 1.000 . Uiso c ? H(9) 0.1279 0.6211 0.2532 0.051 1.000 . Uiso c ? H(10) -0.0330 0.8230 0.1732 0.067 1.000 . Uiso c ? H(11) -0.1163 0.8511 0.0429 0.058 1.000 . Uiso c ? H(12) -0.0298 0.6912 -0.0169 0.066 1.000 . Uiso c ? H(13) 0.1278 0.4895 0.0574 0.054 1.000 . Uiso c ? H(14) 0.4202 0.4178 0.3435 0.041 1.000 . Uiso c ? H(15) 0.3892 0.4260 0.4806 0.050 1.000 . Uiso c ? H(16) 0.1971 0.3964 0.5521 0.060 1.000 . Uiso c ? H(17) 0.0389 0.3593 0.4831 0.053 1.000 . Uiso c ? H(18) 0.0759 0.3429 0.3471 0.045 1.000 . Uiso c ? H(19) 0.7442 0.0855 0.1897 0.039 1.000 . Uiso c ? H(20) 0.8810 0.1182 0.0725 0.048 1.000 . Uiso c ? H(21) 0.7974 0.1493 -0.0619 0.053 1.000 . Uiso c ? H(22) 0.5871 0.1380 -0.0771 0.052 1.000 . Uiso c ? H(23) 0.4499 0.1085 0.0389 0.043 1.000 . Uiso c ? H(24) 0.6974 -0.1434 0.1847 0.055 1.000 . Uiso c ? H(25) 0.7564 -0.3685 0.2157 0.074 1.000 . Uiso c ? H(26) 0.6124 -0.4754 0.2984 0.072 1.000 . Uiso c ? H(27) 0.4104 -0.3531 0.3405 0.076 1.000 . Uiso c ? H(28) 0.3559 -0.1309 0.3091 0.051 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.0265(2) 0.0364(2) 0.0396(2) -0.0126(1) -0.0002(1) -0.01341(11) Cl(1) 0.0453(11) 0.0411(9) 0.0388(9) -0.0156(8) -0.0026(8) -0.0054(7) Cl(2) 0.0246(9) 0.0603(10) 0.0474(10) -0.0144(8) -0.0011(7) -0.0101(8) Cl(3) 0.0584(12) 0.0508(10) 0.0463(9) -0.0289(9) -0.0061(8) -0.0179(8) P(1) 0.0226(9) 0.0239(8) 0.0235(8) -0.0045(7) -0.0016(7) -0.0008(6) P(2) 0.0302(10) 0.0242(8) 0.0245(8) -0.0107(7) 0.0007(7) -0.0042(6) O(1) 0.018(2) 0.022(2) 0.027(2) -0.004(2) -0.001(2) -0.006(2) C(1) 0.023(3) 0.023(3) 0.025(3) -0.006(3) 0.001(3) -0.005(2) C(2) 0.026(4) 0.020(3) 0.022(3) -0.007(3) -0.005(3) -0.002(2) C(3) 0.026(4) 0.023(3) 0.042(4) -0.008(3) -0.005(3) -0.008(3) C(4) 0.033(4) 0.040(4) 0.036(3) -0.019(3) 0.008(3) -0.005(3) C(5) 0.043(4) 0.035(4) 0.032(3) -0.014(3) 0.009(3) -0.008(3) C(6) 0.026(4) 0.028(3) 0.030(3) -0.007(3) 0.002(3) -0.002(2) C(7) 0.021(3) 0.020(3) 0.029(3) -0.005(3) -0.001(3) -0.001(2) C(8) 0.017(3) 0.027(3) 0.024(3) -0.001(3) -0.003(2) -0.006(2) C(9) 0.029(4) 0.027(3) 0.041(4) -0.011(3) -0.003(3) -0.005(3) C(10) 0.039(4) 0.036(4) 0.030(3) -0.005(3) -0.014(3) -0.005(3) C(11) 0.040(4) 0.032(3) 0.029(3) -0.007(3) -0.010(3) 0.002(3) C(12) 0.043(4) 0.024(3) 0.029(3) -0.009(3) -0.008(3) 0.000(3) C(13) 0.020(4) 0.031(3) 0.038(4) -0.006(3) 0.008(3) -0.004(3) C(14) 0.034(4) 0.043(4) 0.041(4) -0.003(3) 0.010(3) -0.014(3) C(15) 0.054(5) 0.028(4) 0.062(5) 0.006(3) 0.016(4) -0.010(3) C(16) 0.031(4) 0.040(4) 0.049(5) -0.001(3) -0.005(3) 0.006(3) C(17) 0.050(5) 0.047(5) 0.048(4) -0.009(4) -0.023(4) 0.007(4) C(18) 0.042(5) 0.036(4) 0.041(4) -0.005(3) -0.017(3) 0.004(3) C(19) 0.029(4) 0.022(3) 0.024(3) -0.002(3) 0.005(3) -0.004(2) C(20) 0.045(4) 0.027(3) 0.024(3) -0.013(3) 0.005(3) -0.002(2) C(21) 0.062(5) 0.032(4) 0.033(4) -0.018(3) 0.007(4) -0.011(3) C(22) 0.081(6) 0.036(4) 0.021(3) -0.010(4) 0.013(4) -0.007(3) C(23) 0.047(5) 0.040(4) 0.045(4) -0.018(4) 0.013(4) -0.011(3) C(24) 0.043(4) 0.038(4) 0.027(3) -0.011(3) 0.006(3) -0.010(3) C(25) 0.038(4) 0.022(3) 0.025(3) -0.011(3) 0.008(3) -0.007(2) C(26) 0.027(4) 0.028(3) 0.039(4) -0.007(3) 0.007(3) -0.011(3) C(27) 0.039(4) 0.034(4) 0.049(4) -0.013(3) 0.005(3) -0.018(3) C(28) 0.058(5) 0.028(3) 0.041(4) -0.014(3) 0.016(4) -0.010(3) C(29) 0.057(5) 0.040(4) 0.029(4) -0.014(4) -0.007(3) -0.008(3) C(30) 0.035(4) 0.041(4) 0.031(3) -0.014(3) 0.011(3) -0.014(3) C(31) 0.043(4) 0.025(3) 0.030(3) -0.010(3) -0.007(3) -0.008(3) C(32) 0.043(5) 0.029(4) 0.059(4) -0.009(3) 0.005(4) -0.009(3) C(33) 0.072(6) 0.035(4) 0.078(5) -0.013(4) 0.017(4) -0.026(4) C(34) 0.076(6) 0.029(4) 0.078(5) -0.022(4) 0.016(5) -0.020(4) C(35) 0.093(7) 0.039(4) 0.060(5) -0.032(5) 0.010(5) -0.011(4) C(36) 0.060(5) 0.030(4) 0.034(3) -0.019(3) 0.016(3) -0.006(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; disordered ether removed and scattering compensated with SQUEEZE Spek, A. L. "Single-crystal structure validation with the program PLATON", J. Appl. Crystallogr. 2003, 36, 7. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5172 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_all 0.0530 _refine_ls_wR_factor_ref 0.0460 _refine_ls_goodness_of_fit_all 1.292 _refine_ls_goodness_of_fit_ref 1.450 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.52 _refine_diff_density_max 2.84 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re(1) Cl(1) 2.348(2) . . ? Re(1) Cl(2) 2.359(2) . . ? Re(1) Cl(3) 2.371(2) . . ? Re(1) P(1) 2.478(2) . . ? Re(1) P(2) 2.476(2) . . ? Re(1) O(1) 1.813(4) . . ? P(1) C(1) 1.811(7) . . ? P(1) C(13) 1.838(7) . . ? P(1) C(19) 1.833(7) . . ? P(2) C(7) 1.836(7) . . ? P(2) C(25) 1.834(7) . . ? P(2) C(31) 1.821(7) . . ? C(1) C(2) 1.416(9) . . ? C(1) C(6) 1.391(8) . . ? C(2) C(3) 1.405(9) . . ? C(2) C(8) 1.502(8) . . ? C(3) C(4) 1.371(8) . . ? C(3) H(1) 0.95 . . no C(4) C(5) 1.389(10) . . ? C(4) H(2) 0.95 . . no C(5) C(6) 1.395(10) . . ? C(5) H(3) 0.95 . . no C(6) H(4) 0.95 . . no C(7) C(8) 1.412(8) . . ? C(7) C(12) 1.395(8) . . ? C(8) C(9) 1.394(9) . . ? C(9) C(10) 1.401(9) . . ? C(9) H(5) 0.95 . . no C(10) C(11) 1.364(10) . . ? C(10) H(6) 0.95 . . no C(11) C(12) 1.387(9) . . ? C(11) H(7) 0.95 . . no C(12) H(8) 0.95 . . no C(13) C(14) 1.375(10) . . ? C(13) C(18) 1.413(10) . . ? C(14) C(15) 1.426(10) . . ? C(14) H(9) 0.95 . . no C(15) C(16) 1.345(11) . . ? C(15) H(10) 0.95 . . no C(16) C(17) 1.356(11) . . ? C(16) H(11) 0.95 . . no C(17) C(18) 1.393(10) . . ? C(17) H(12) 0.95 . . no C(18) H(13) 0.95 . . no C(19) C(20) 1.367(10) . . ? C(19) C(24) 1.391(10) . . ? C(20) C(21) 1.377(9) . . ? C(20) H(14) 0.95 . . no C(21) C(22) 1.391(11) . . ? C(21) H(15) 0.95 . . no C(22) C(23) 1.395(11) . . ? C(22) H(16) 0.95 . . no C(23) C(24) 1.386(10) . . ? C(23) H(17) 0.95 . . no C(24) H(18) 0.95 . . no C(25) C(26) 1.357(9) . . ? C(25) C(30) 1.414(10) . . ? C(26) C(27) 1.399(10) . . ? C(26) H(19) 0.95 . . no C(27) C(28) 1.385(10) . . ? C(27) H(20) 0.95 . . no C(28) C(29) 1.382(11) . . ? C(28) H(21) 0.95 . . no C(29) C(30) 1.380(10) . . ? C(29) H(22) 0.95 . . no C(30) H(23) 0.95 . . no C(31) C(32) 1.382(10) . . ? C(31) C(36) 1.384(10) . . ? C(32) C(33) 1.405(10) . . ? C(32) H(24) 0.95 . . no C(33) C(34) 1.400(12) . . ? C(33) H(25) 0.95 . . no C(34) C(35) 1.384(12) . . ? C(34) H(26) 0.95 . . no C(35) C(36) 1.383(10) . . ? C(35) H(27) 0.96 . . no C(36) H(28) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Re(1) Cl(2) 87.54(7) . . . ? Cl(1) Re(1) Cl(3) 92.32(6) . . . ? Cl(1) Re(1) P(1) 87.57(6) . . . ? Cl(1) Re(1) P(2) 79.90(6) . . . ? Cl(1) Re(1) O(1) 165.4(1) . . . ? Cl(2) Re(1) Cl(3) 85.36(7) . . . ? Cl(2) Re(1) P(1) 87.58(7) . . . ? Cl(2) Re(1) P(2) 167.11(6) . . . ? Cl(2) Re(1) O(1) 103.6(1) . . . ? Cl(3) Re(1) P(1) 172.93(7) . . . ? Cl(3) Re(1) P(2) 92.24(7) . . . ? Cl(3) Re(1) O(1) 97.88(13) . . . ? P(1) Re(1) P(2) 94.69(6) . . . ? P(1) Re(1) O(1) 83.59(13) . . . ? P(2) Re(1) O(1) 89.29(13) . . . ? Re(1) P(1) C(1) 111.8(2) . . . ? Re(1) P(1) C(13) 110.6(3) . . . ? Re(1) P(1) C(19) 118.5(2) . . . ? C(1) P(1) C(13) 104.7(3) . . . ? C(1) P(1) C(19) 107.8(3) . . . ? C(13) P(1) C(19) 102.2(3) . . . ? Re(1) P(2) C(7) 111.8(2) . . . ? Re(1) P(2) C(25) 114.7(2) . . . ? Re(1) P(2) C(31) 117.0(3) . . . ? C(7) P(2) C(25) 106.2(3) . . . ? C(7) P(2) C(31) 104.1(3) . . . ? C(25) P(2) C(31) 101.7(3) . . . ? P(1) C(1) C(2) 124.1(4) . . . ? P(1) C(1) C(6) 118.2(5) . . . ? C(2) C(1) C(6) 117.7(6) . . . ? C(1) C(2) C(3) 119.6(5) . . . ? C(1) C(2) C(8) 125.2(6) . . . ? C(3) C(2) C(8) 115.1(6) . . . ? C(2) C(3) C(4) 121.6(6) . . . ? C(2) C(3) H(1) 119.2 . . . no C(4) C(3) H(1) 119.2 . . . no C(3) C(4) C(5) 119.4(6) . . . ? C(3) C(4) H(2) 120.3 . . . no C(5) C(4) H(2) 120.4 . . . no C(4) C(5) C(6) 119.8(6) . . . ? C(4) C(5) H(3) 120.2 . . . no C(6) C(5) H(3) 120.0 . . . no C(1) C(6) C(5) 122.0(6) . . . ? C(1) C(6) H(4) 118.9 . . . no C(5) C(6) H(4) 119.1 . . . no P(2) C(7) C(8) 122.7(4) . . . ? P(2) C(7) C(12) 117.2(5) . . . ? C(8) C(7) C(12) 120.1(6) . . . ? C(2) C(8) C(7) 126.9(6) . . . ? C(2) C(8) C(9) 115.4(6) . . . ? C(7) C(8) C(9) 117.3(5) . . . ? C(8) C(9) C(10) 121.6(6) . . . ? C(8) C(9) H(5) 119.1 . . . no C(10) C(9) H(5) 119.3 . . . no C(9) C(10) C(11) 120.2(6) . . . ? C(9) C(10) H(6) 119.8 . . . no C(11) C(10) H(6) 120.0 . . . no C(10) C(11) C(12) 119.5(6) . . . ? C(10) C(11) H(7) 120.1 . . . no C(12) C(11) H(7) 120.4 . . . no C(7) C(12) C(11) 121.1(6) . . . ? C(7) C(12) H(8) 119.4 . . . no C(11) C(12) H(8) 119.5 . . . no P(1) C(13) C(14) 120.6(6) . . . ? P(1) C(13) C(18) 119.9(6) . . . ? C(14) C(13) C(18) 119.5(7) . . . ? C(13) C(14) C(15) 119.4(7) . . . ? C(13) C(14) H(9) 120.3 . . . no C(15) C(14) H(9) 120.3 . . . no C(14) C(15) C(16) 120.7(8) . . . ? C(14) C(15) H(10) 119.7 . . . no C(16) C(15) H(10) 119.6 . . . no C(15) C(16) C(17) 119.8(7) . . . ? C(15) C(16) H(11) 120.2 . . . no C(17) C(16) H(11) 120.0 . . . no C(16) C(17) C(18) 122.3(8) . . . ? C(16) C(17) H(12) 119.0 . . . no C(18) C(17) H(12) 118.6 . . . no C(13) C(18) C(17) 118.2(8) . . . ? C(13) C(18) H(13) 120.9 . . . no C(17) C(18) H(13) 120.9 . . . no P(1) C(19) C(20) 121.8(5) . . . ? P(1) C(19) C(24) 117.3(6) . . . ? C(20) C(19) C(24) 120.7(6) . . . ? C(19) C(20) C(21) 120.6(7) . . . ? C(19) C(20) H(14) 119.6 . . . no C(21) C(20) H(14) 119.8 . . . no C(20) C(21) C(22) 120.1(8) . . . ? C(20) C(21) H(15) 119.8 . . . no C(22) C(21) H(15) 120.2 . . . no C(21) C(22) C(23) 119.0(7) . . . ? C(21) C(22) H(16) 120.5 . . . no C(23) C(22) H(16) 120.5 . . . no C(22) C(23) C(24) 120.8(7) . . . ? C(22) C(23) H(17) 119.4 . . . no C(24) C(23) H(17) 119.7 . . . no C(19) C(24) C(23) 118.8(7) . . . ? C(19) C(24) H(18) 120.7 . . . no C(23) C(24) H(18) 120.5 . . . no P(2) C(25) C(26) 122.1(5) . . . ? P(2) C(25) C(30) 117.2(5) . . . ? C(26) C(25) C(30) 120.3(6) . . . ? C(25) C(26) C(27) 121.3(7) . . . ? C(25) C(26) H(19) 119.4 . . . no C(27) C(26) H(19) 119.3 . . . no C(26) C(27) C(28) 118.5(7) . . . ? C(26) C(27) H(20) 120.6 . . . no C(28) C(27) H(20) 120.9 . . . no C(27) C(28) C(29) 120.5(7) . . . ? C(27) C(28) H(21) 119.9 . . . no C(29) C(28) H(21) 119.7 . . . no C(28) C(29) C(30) 121.1(7) . . . ? C(28) C(29) H(22) 119.4 . . . no C(30) C(29) H(22) 119.4 . . . no C(25) C(30) C(29) 118.3(7) . . . ? C(25) C(30) H(23) 120.8 . . . no C(29) C(30) H(23) 120.9 . . . no P(2) C(31) C(32) 119.6(5) . . . ? P(2) C(31) C(36) 122.4(6) . . . ? C(32) C(31) C(36) 117.9(6) . . . ? C(31) C(32) C(33) 122.2(7) . . . ? C(31) C(32) H(24) 118.9 . . . no C(33) C(32) H(24) 119.0 . . . no C(32) C(33) C(34) 118.7(8) . . . ? C(32) C(33) H(25) 120.6 . . . no C(34) C(33) H(25) 120.7 . . . no C(33) C(34) C(35) 119.0(7) . . . ? C(33) C(34) H(26) 120.7 . . . no C(35) C(34) H(26) 120.3 . . . no C(34) C(35) C(36) 121.2(8) . . . ? C(34) C(35) H(27) 119.4 . . . no C(36) C(35) H(27) 119.4 . . . no C(31) C(36) C(35) 121.1(8) . . . ? C(31) C(36) H(28) 119.4 . . . no C(35) C(36) H(28) 119.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(10) 3.432(7) . 2_656 no Cl(1) C(11) 3.514(7) . 2_656 no Cl(2) C(3) 3.415(7) . 1_455 no Cl(2) C(4) 3.511(8) . 1_455 no Cl(3) C(28) 3.560(8) . 2_655 no O(1) C(17) 3.526(9) . 2_565 no C(5) C(5) 3.48(2) . 2_665 no C(5) C(29) 3.526(10) . 2_665 no C(5) C(6) 3.591(10) . 2_665 no C(11) C(11) 3.31(2) . 2_656 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Re(1) P(1) C(1) C(2) . . . . -69.2(6) no Re(1) P(1) C(1) C(6) . . . . 109.3(5) no Re(1) P(1) C(13) C(14) . . . . 148.8(5) no Re(1) P(1) C(13) C(18) . . . . -34.3(6) no Re(1) P(1) C(19) C(20) . . . . 134.0(5) no Re(1) P(1) C(19) C(24) . . . . -50.2(6) no Re(1) P(2) C(7) C(8) . . . . -67.9(6) no Re(1) P(2) C(7) C(12) . . . . 109.1(5) no Re(1) P(2) C(25) C(26) . . . . 139.4(5) no Re(1) P(2) C(25) C(30) . . . . -46.8(6) no Re(1) P(2) C(31) C(32) . . . . 146.4(6) no Re(1) P(2) C(31) C(36) . . . . -33.2(7) no Cl(1) Re(1) P(1) C(1) . . . . 115.2(2) no Cl(1) Re(1) P(1) C(13) . . . . -128.6(2) no Cl(1) Re(1) P(1) C(19) . . . . -11.1(3) no Cl(1) Re(1) P(2) C(7) . . . . -49.6(2) no Cl(1) Re(1) P(2) C(25) . . . . -170.6(2) no Cl(1) Re(1) P(2) C(31) . . . . 70.4(3) no Cl(2) Re(1) P(1) C(1) . . . . -157.2(2) no Cl(2) Re(1) P(1) C(13) . . . . -41.0(2) no Cl(2) Re(1) P(1) C(19) . . . . 76.5(3) no Cl(2) Re(1) P(2) C(7) . . . . -62.6(4) no Cl(2) Re(1) P(2) C(25) . . . . 176.4(3) no Cl(2) Re(1) P(2) C(31) . . . . 57.3(4) no Cl(3) Re(1) P(1) C(1) . . . . -155.6(5) no Cl(3) Re(1) P(1) C(13) . . . . -39.4(6) no Cl(3) Re(1) P(1) C(19) . . . . 78.1(5) no Cl(3) Re(1) P(2) C(7) . . . . -141.5(2) no Cl(3) Re(1) P(2) C(25) . . . . 97.4(2) no Cl(3) Re(1) P(2) C(31) . . . . -21.6(3) no P(1) Re(1) P(2) C(7) . . . . 37.1(2) no P(1) Re(1) P(2) C(25) . . . . -83.9(2) no P(1) Re(1) P(2) C(31) . . . . 157.1(3) no P(1) C(1) C(2) C(3) . . . . -179.4(5) no P(1) C(1) C(2) C(8) . . . . -3.5(9) no P(1) C(1) C(6) C(5) . . . . -179.0(6) no P(1) C(13) C(14) C(15) . . . . 178.5(6) no P(1) C(13) C(18) C(17) . . . . -178.1(6) no P(1) C(19) C(20) C(21) . . . . 176.6(5) no P(1) C(19) C(24) C(23) . . . . -175.2(5) no P(2) Re(1) P(1) C(1) . . . . 35.5(2) no P(2) Re(1) P(1) C(13) . . . . 151.7(2) no P(2) Re(1) P(1) C(19) . . . . -90.7(3) no P(2) C(7) C(8) C(2) . . . . -7.1(9) no P(2) C(7) C(8) C(9) . . . . -179.9(5) no P(2) C(7) C(12) C(11) . . . . -177.4(6) no P(2) C(25) C(26) C(27) . . . . 175.6(5) no P(2) C(25) C(30) C(29) . . . . -175.4(5) no P(2) C(31) C(32) C(33) . . . . 179.9(7) no P(2) C(31) C(36) C(35) . . . . 180.0(6) no O(1) Re(1) P(1) C(1) . . . . -53.2(3) no O(1) Re(1) P(1) C(13) . . . . 63.0(3) no O(1) Re(1) P(1) C(19) . . . . -179.5(3) no O(1) Re(1) P(2) C(7) . . . . 120.6(2) no O(1) Re(1) P(2) C(25) . . . . -0.4(3) no O(1) Re(1) P(2) C(31) . . . . -119.4(3) no C(1) P(1) C(13) C(14) . . . . -90.6(6) no C(1) P(1) C(13) C(18) . . . . 86.2(6) no C(1) P(1) C(19) C(20) . . . . 5.8(6) no C(1) P(1) C(19) C(24) . . . . -178.4(5) no C(1) C(2) C(3) C(4) . . . . -2.3(10) no C(1) C(2) C(8) C(7) . . . . 71.8(9) no C(1) C(2) C(8) C(9) . . . . -115.2(7) no C(1) C(6) C(5) C(4) . . . . -1.2(11) no C(2) C(1) P(1) C(13) . . . . 171.1(6) no C(2) C(1) P(1) C(19) . . . . 62.7(6) no C(2) C(1) C(6) C(5) . . . . -0.4(10) no C(2) C(3) C(4) C(5) . . . . 0.7(11) no C(2) C(8) C(7) C(12) . . . . 176.0(7) no C(2) C(8) C(9) C(10) . . . . -178.5(6) no C(3) C(2) C(1) C(6) . . . . 2.1(9) no C(3) C(2) C(8) C(7) . . . . -112.1(7) no C(3) C(2) C(8) C(9) . . . . 60.9(8) no C(3) C(4) C(5) C(6) . . . . 1.0(11) no C(4) C(3) C(2) C(8) . . . . -178.5(6) no C(6) C(1) P(1) C(13) . . . . -10.4(6) no C(6) C(1) P(1) C(19) . . . . -118.8(6) no C(6) C(1) C(2) C(8) . . . . 178.0(6) no C(7) P(2) C(25) C(26) . . . . 15.3(6) no C(7) P(2) C(25) C(30) . . . . -170.9(5) no C(7) P(2) C(31) C(32) . . . . -89.6(6) no C(7) P(2) C(31) C(36) . . . . 90.8(7) no C(7) C(8) C(9) C(10) . . . . -4.8(10) no C(7) C(12) C(11) C(10) . . . . -1.1(12) no C(8) C(7) P(2) C(25) . . . . 57.9(6) no C(8) C(7) P(2) C(31) . . . . 164.9(6) no C(8) C(7) C(12) C(11) . . . . -0.3(11) no C(8) C(9) C(10) C(11) . . . . 3.5(11) no C(9) C(8) C(7) C(12) . . . . 3.2(10) no C(9) C(10) C(11) C(12) . . . . -0.5(11) no C(12) C(7) P(2) C(25) . . . . -125.1(6) no C(12) C(7) P(2) C(31) . . . . -18.1(6) no C(13) P(1) C(19) C(20) . . . . -104.2(6) no C(13) P(1) C(19) C(24) . . . . 71.6(6) no C(13) C(14) C(15) C(16) . . . . 0.5(12) no C(13) C(18) C(17) C(16) . . . . -1.2(13) no C(14) C(13) P(1) C(19) . . . . 21.8(7) no C(14) C(13) C(18) C(17) . . . . -1.2(11) no C(14) C(15) C(16) C(17) . . . . -2.9(13) no C(15) C(14) C(13) C(18) . . . . 1.6(11) no C(15) C(16) C(17) C(18) . . . . 3.4(14) no C(18) C(13) P(1) C(19) . . . . -161.4(6) no C(19) C(20) C(21) C(22) . . . . -1.1(11) no C(19) C(24) C(23) C(22) . . . . -2.1(11) no C(20) C(19) C(24) C(23) . . . . 0.6(10) no C(20) C(21) C(22) C(23) . . . . -0.5(11) no C(21) C(20) C(19) C(24) . . . . 1.0(10) no C(21) C(22) C(23) C(24) . . . . 2.1(11) no C(25) P(2) C(31) C(32) . . . . 20.6(7) no C(25) P(2) C(31) C(36) . . . . -159.0(6) no C(25) C(26) C(27) C(28) . . . . -0.6(10) no C(25) C(30) C(29) C(28) . . . . -0.5(11) no C(26) C(25) P(2) C(31) . . . . -93.3(6) no C(26) C(25) C(30) C(29) . . . . -1.4(10) no C(26) C(27) C(28) C(29) . . . . -1.4(11) no C(27) C(26) C(25) C(30) . . . . 2.0(10) no C(27) C(28) C(29) C(30) . . . . 2.0(11) no C(30) C(25) P(2) C(31) . . . . 80.5(6) no C(31) C(32) C(33) C(34) . . . . -0.6(14) no C(31) C(36) C(35) C(34) . . . . 0.8(14) no C(32) C(31) C(36) C(35) . . . . 0.4(12) no C(32) C(33) C(34) C(35) . . . . 1.8(15) no C(33) C(32) C(31) C(36) . . . . -0.5(12) no C(33) C(34) C(35) C(36) . . . . -1.9(15) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_2402Re(O)Cl3(DPEPHOS)-100 _database_code_depnum_ccdc_archive 'CCDC 247683' _audit_creation_date 2004-08-16 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 9.7531(2) _cell_length_b 13.2526(3) _cell_length_c 17.0097(5) _cell_angle_alpha 71.8177(10) _cell_angle_beta 74.7252(10) _cell_angle_gamma 69.7270(10) _cell_volume 1929.41(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 6708 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1017.00 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H32 Cl7 O2 P2 Re ' _chemical_formula_moiety 'C36 H28 Cl3 O2 P2 Re, 2(C H2 Cl2)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1000.00 _exptl_absorpt_coefficient_mu 3.752 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector CCD _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 14760 _reflns_number_total 8598 _reflns_number_gt 5665 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04890 _diffrn_reflns_av_sigmaI/netI 0.113 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.33 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 76 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 14 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Re 0 2 -1.598 7.232 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Re(1) 0.78182(3) 0.64649(2) 0.77486(1) 0.02126(6) 1.000 . Uani d ? Cl(1) 1.0090(1) 0.69032(10) 0.71034(9) 0.0296(4) 1.000 . Uani d ? Cl(2) 0.9018(2) 0.49060(10) 0.87165(9) 0.0305(4) 1.000 . Uani d ? Cl(3) 0.8385(2) 0.51972(10) 0.68982(9) 0.0374(4) 1.000 . Uani d ? Cl(4) 0.6281(2) 0.3521(1) 0.6493(1) 0.0730(7) 1.000 . Uani d ? Cl(5) 0.3822(2) 0.5532(1) 0.62035(12) 0.0610(6) 1.000 . Uani d ? Cl(6) 0.9516(2) 0.8065(2) 1.1774(2) 0.0769(7) 1.000 . Uani d ? Cl(7) 1.2462(2) 0.83112(12) 1.14771(11) 0.0505(5) 1.000 . Uani d ? P(1) 0.7538(2) 0.74615(10) 0.88438(9) 0.0190(4) 1.000 . Uani d ? P(2) 0.6927(2) 0.80384(10) 0.65180(9) 0.0211(4) 1.000 . Uani d ? O(1) 0.6017(4) 0.6519(3) 0.8124(2) 0.0276(11) 1.000 . Uani d ? O(2) 0.7772(4) 0.9275(3) 0.7480(2) 0.0209(10) 1.000 . Uani d ? C(1) 0.6168(6) 0.8827(4) 0.8733(3) 0.019(1) 1.000 . Uani d ? C(2) 0.6442(6) 0.9625(4) 0.7999(3) 0.021(2) 1.000 . Uani d ? C(3) 0.5465(6) 1.0690(4) 0.7841(3) 0.025(2) 1.000 . Uani d ? C(4) 0.4194(6) 1.0938(4) 0.8435(4) 0.031(2) 1.000 . Uani d ? C(5) 0.3903(6) 1.0159(4) 0.9158(4) 0.030(2) 1.000 . Uani d ? C(6) 0.4891(6) 0.9103(4) 0.9313(3) 0.027(2) 1.000 . Uani d ? C(7) 0.7622(5) 0.9252(4) 0.6105(3) 0.020(1) 1.000 . Uani d ? C(8) 0.7884(5) 0.9775(4) 0.6623(3) 0.019(1) 1.000 . Uani d ? C(9) 0.8302(6) 1.0734(4) 0.6321(4) 0.025(2) 1.000 . Uani d ? C(10) 0.8423(6) 1.1229(4) 0.5468(4) 0.028(2) 1.000 . Uani d ? C(11) 0.8157(6) 1.0758(4) 0.4930(3) 0.029(2) 1.000 . Uani d ? C(12) 0.7756(6) 0.9777(4) 0.5246(3) 0.026(2) 1.000 . Uani d ? C(13) 0.9192(6) 0.7655(4) 0.9014(3) 0.020(2) 1.000 . Uani d ? C(14) 0.9181(6) 0.8667(4) 0.9092(3) 0.024(2) 1.000 . Uani d ? C(15) 1.0412(6) 0.8775(4) 0.9275(3) 0.027(2) 1.000 . Uani d ? C(16) 1.1662(6) 0.7889(5) 0.9378(4) 0.033(2) 1.000 . Uani d ? C(17) 1.1697(6) 0.6878(4) 0.9294(3) 0.029(2) 1.000 . Uani d ? C(18) 1.0469(6) 0.6756(4) 0.9107(3) 0.025(2) 1.000 . Uani d ? C(19) 0.6814(6) 0.6696(4) 0.9879(3) 0.019(1) 1.000 . Uani d ? C(20) 0.7451(6) 0.6462(4) 1.0579(4) 0.028(2) 1.000 . Uani d ? C(21) 0.6848(7) 0.5901(5) 1.1352(4) 0.036(2) 1.000 . Uani d ? C(22) 0.5606(7) 0.5578(4) 1.1444(4) 0.034(2) 1.000 . Uani d ? C(23) 0.4964(6) 0.5801(4) 1.0755(4) 0.028(2) 1.000 . Uani d ? C(24) 0.5552(6) 0.6350(4) 0.9974(3) 0.026(2) 1.000 . Uani d ? C(25) 0.4920(6) 0.8630(4) 0.6734(3) 0.020(2) 1.000 . Uani d ? C(26) 0.4002(6) 0.7932(4) 0.7042(3) 0.031(2) 1.000 . Uani d ? C(27) 0.2476(6) 0.8370(5) 0.7233(4) 0.038(2) 1.000 . Uani d ? C(28) 0.1864(6) 0.9492(6) 0.7139(4) 0.040(2) 1.000 . Uani d ? C(29) 0.2723(7) 1.0184(5) 0.6822(4) 0.036(2) 1.000 . Uani d ? C(30) 0.4253(6) 0.9765(4) 0.6615(3) 0.026(2) 1.000 . Uani d ? C(31) 0.7266(6) 0.7546(4) 0.5571(3) 0.026(2) 1.000 . Uani d ? C(32) 0.6132(7) 0.7651(4) 0.5177(4) 0.032(2) 1.000 . Uani d ? C(33) 0.6459(8) 0.7227(5) 0.4471(4) 0.046(2) 1.000 . Uani d ? C(34) 0.7903(9) 0.6727(5) 0.4155(4) 0.049(2) 1.000 . Uani d ? C(35) 0.9034(8) 0.6631(5) 0.4535(4) 0.044(2) 1.000 . Uani d ? C(36) 0.8749(7) 0.7034(4) 0.5239(4) 0.033(2) 1.000 . Uani d ? C(37) 1.1409(7) 0.7413(4) 1.1605(4) 0.038(2) 1.000 . Uani d ? C(38) 0.5736(8) 0.4933(5) 0.5973(4) 0.052(2) 1.000 . Uani d ? H(1) 0.5661 1.1232 0.7342 0.030 1.000 . Uiso c ? H(2) 0.3513 1.1661 0.8339 0.037 1.000 . Uiso c ? H(3) 0.3023 1.0344 0.9553 0.036 1.000 . Uiso c ? H(4) 0.4691 0.8569 0.9817 0.032 1.000 . Uiso c ? H(5) 0.8505 1.1052 0.6691 0.030 1.000 . Uiso c ? H(6) 0.8693 1.1900 0.5252 0.033 1.000 . Uiso c ? H(7) 0.8245 1.1101 0.4345 0.035 1.000 . Uiso c ? H(8) 0.7570 0.9456 0.4872 0.031 1.000 . Uiso c ? H(9) 0.8325 0.9287 0.9019 0.029 1.000 . Uiso c ? H(10) 1.0396 0.9471 0.9330 0.032 1.000 . Uiso c ? H(11) 1.2501 0.7972 0.9507 0.039 1.000 . Uiso c ? H(12) 1.2561 0.6265 0.9365 0.035 1.000 . Uiso c ? H(13) 1.0498 0.6062 0.9042 0.030 1.000 . Uiso c ? H(14) 0.8301 0.6687 1.0527 0.034 1.000 . Uiso c ? H(15) 0.7299 0.5736 1.1826 0.043 1.000 . Uiso c ? H(16) 0.5194 0.5203 1.1980 0.041 1.000 . Uiso c ? H(17) 0.4110 0.5575 1.0818 0.034 1.000 . Uiso c ? H(18) 0.5107 0.6496 0.9502 0.031 1.000 . Uiso c ? H(19) 0.4427 0.7152 0.7122 0.037 1.000 . Uiso c ? H(20) 0.1856 0.7894 0.7428 0.045 1.000 . Uiso c ? H(21) 0.0823 0.9786 0.7298 0.048 1.000 . Uiso c ? H(22) 0.2280 1.0962 0.6741 0.043 1.000 . Uiso c ? H(23) 0.4848 1.0259 0.6391 0.031 1.000 . Uiso c ? H(24) 0.5134 0.8009 0.5386 0.039 1.000 . Uiso c ? H(25) 0.5678 0.7285 0.4208 0.055 1.000 . Uiso c ? H(26) 0.8118 0.6447 0.3672 0.059 1.000 . Uiso c ? H(27) 1.0029 0.6284 0.4312 0.052 1.000 . Uiso c ? H(28) 0.9541 0.6967 0.5496 0.040 1.000 . Uiso c ? H(29) 1.1643 0.6805 1.2073 0.046 1.000 . Uiso c ? H(30) 1.1660 0.7148 1.1111 0.046 1.000 . Uiso c ? H(31) 0.6227 0.5317 0.6141 0.062 1.000 . Uiso c ? H(32) 0.6018 0.5001 0.5384 0.062 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.02583(13) 0.01628(11) 0.02309(13) -0.00716(9) -0.00796(10) -0.00243(8) Cl(1) 0.0244(8) 0.0307(7) 0.0343(9) -0.0077(6) -0.0045(7) -0.0094(6) Cl(2) 0.0388(9) 0.0191(7) 0.0348(9) -0.0050(6) -0.0183(7) -0.0020(6) Cl(3) 0.0627(11) 0.0208(7) 0.0334(9) -0.0095(7) -0.0180(8) -0.0079(6) Cl(4) 0.082(2) 0.0370(10) 0.106(2) -0.0126(10) -0.0322(13) -0.0177(10) Cl(5) 0.0603(13) 0.0595(11) 0.0630(13) -0.0083(10) -0.0183(10) -0.0185(10) Cl(6) 0.0434(12) 0.0552(12) 0.115(2) -0.0071(10) 0.0100(12) -0.0248(12) Cl(7) 0.0593(11) 0.0333(8) 0.0676(12) -0.0203(8) -0.0144(10) -0.0137(8) P(1) 0.0199(8) 0.0164(7) 0.0203(8) -0.0049(6) -0.0062(6) -0.0020(6) P(2) 0.0227(8) 0.0196(7) 0.0227(8) -0.0083(6) -0.0058(7) -0.0036(6) O(1) 0.020(2) 0.035(2) 0.029(2) -0.016(2) -0.007(2) 0.002(2) O(2) 0.021(2) 0.018(2) 0.020(2) -0.002(2) -0.004(2) -0.003(2) C(1) 0.021(3) 0.014(3) 0.026(3) -0.004(2) -0.006(3) -0.009(2) C(2) 0.022(3) 0.018(3) 0.028(3) -0.003(2) -0.013(3) -0.009(2) C(3) 0.029(3) 0.016(3) 0.030(3) -0.005(3) -0.014(3) -0.003(2) C(4) 0.027(3) 0.025(3) 0.040(4) -0.001(3) -0.007(3) -0.012(3) C(5) 0.023(3) 0.031(3) 0.032(4) -0.002(3) 0.002(3) -0.013(3) C(6) 0.027(3) 0.029(3) 0.027(3) -0.010(3) -0.002(3) -0.010(3) C(7) 0.019(3) 0.013(3) 0.026(3) -0.003(2) -0.005(3) -0.002(2) C(8) 0.013(3) 0.017(3) 0.023(3) 0.000(2) -0.003(2) -0.004(2) C(9) 0.024(3) 0.020(3) 0.034(4) -0.009(3) -0.006(3) -0.006(3) C(10) 0.026(3) 0.017(3) 0.037(4) -0.008(3) -0.003(3) -0.002(3) C(11) 0.033(4) 0.029(3) 0.019(3) -0.010(3) -0.003(3) 0.004(3) C(12) 0.026(3) 0.026(3) 0.024(3) -0.006(3) -0.002(3) -0.007(3) C(13) 0.022(3) 0.024(3) 0.018(3) -0.010(2) -0.005(2) -0.004(2) C(14) 0.026(3) 0.024(3) 0.020(3) -0.005(3) -0.003(3) -0.004(2) C(15) 0.033(4) 0.025(3) 0.030(3) -0.012(3) -0.010(3) -0.010(3) C(16) 0.030(4) 0.040(4) 0.037(4) -0.019(3) -0.009(3) -0.010(3) C(17) 0.024(3) 0.031(3) 0.032(4) -0.007(3) -0.006(3) -0.007(3) C(18) 0.026(3) 0.019(3) 0.028(3) -0.004(3) -0.007(3) -0.005(2) C(19) 0.021(3) 0.013(3) 0.022(3) -0.004(2) -0.004(3) -0.004(2) C(20) 0.030(3) 0.026(3) 0.026(4) -0.009(3) -0.005(3) -0.001(3) C(21) 0.044(4) 0.034(3) 0.026(4) -0.007(3) -0.011(3) -0.003(3) C(22) 0.048(4) 0.022(3) 0.024(4) -0.007(3) 0.004(3) -0.005(3) C(23) 0.027(3) 0.020(3) 0.032(4) -0.012(3) 0.008(3) -0.004(3) C(24) 0.028(3) 0.020(3) 0.025(3) -0.004(3) -0.006(3) -0.002(2) C(25) 0.021(3) 0.025(3) 0.017(3) -0.012(2) -0.004(2) -0.000(2) C(26) 0.033(4) 0.037(3) 0.022(3) -0.013(3) -0.010(3) 0.002(3) C(27) 0.030(4) 0.063(5) 0.027(4) -0.030(4) -0.008(3) 0.001(3) C(28) 0.021(4) 0.067(5) 0.026(4) -0.005(3) -0.005(3) -0.010(3) C(29) 0.031(4) 0.038(4) 0.034(4) 0.000(3) -0.009(3) -0.011(3) C(30) 0.022(3) 0.032(3) 0.024(3) -0.007(3) -0.004(3) -0.006(3) C(31) 0.037(4) 0.014(3) 0.027(3) -0.011(3) -0.006(3) -0.002(2) C(32) 0.044(4) 0.031(3) 0.029(4) -0.019(3) -0.011(3) -0.002(3) C(33) 0.076(5) 0.046(4) 0.031(4) -0.033(4) -0.017(4) -0.005(3) C(34) 0.085(6) 0.036(4) 0.032(4) -0.025(4) -0.004(4) -0.011(3) C(35) 0.056(5) 0.035(4) 0.034(4) -0.012(3) 0.006(4) -0.012(3) C(36) 0.041(4) 0.029(3) 0.027(4) -0.012(3) -0.002(3) -0.004(3) C(37) 0.040(4) 0.024(3) 0.046(4) -0.007(3) -0.007(3) -0.005(3) C(38) 0.066(5) 0.049(4) 0.047(5) -0.024(4) -0.017(4) -0.007(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5665 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_all 0.0700 _refine_ls_wR_factor_ref 0.0320 _refine_ls_goodness_of_fit_all 1.522 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.79 _refine_diff_density_max 1.25 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re(1) Cl(1) 2.3799(13) . . ? Re(1) Cl(2) 2.3589(12) . . ? Re(1) Cl(3) 2.3817(11) . . ? Re(1) P(1) 2.5111(12) . . ? Re(1) P(2) 2.5424(13) . . ? Re(1) O(1) 1.688(3) . . ? Cl(4) C(38) 1.758(6) . . ? Cl(5) C(38) 1.746(7) . . ? Cl(6) C(37) 1.734(6) . . ? Cl(7) C(37) 1.758(6) . . ? P(1) C(1) 1.827(4) . . ? P(1) C(13) 1.825(5) . . ? P(1) C(19) 1.831(5) . . ? P(2) C(7) 1.827(5) . . ? P(2) C(25) 1.822(5) . . ? P(2) C(31) 1.831(5) . . ? O(2) C(2) 1.383(5) . . ? O(2) C(8) 1.392(5) . . ? C(1) C(2) 1.395(6) . . ? C(1) C(6) 1.385(6) . . ? C(2) C(3) 1.392(6) . . ? C(3) C(4) 1.389(7) . . ? C(3) H(1) 0.95 . . no C(4) C(5) 1.372(7) . . ? C(4) H(2) 0.95 . . no C(5) C(6) 1.388(6) . . ? C(5) H(3) 0.95 . . no C(6) H(4) 0.95 . . no C(7) C(8) 1.395(6) . . ? C(7) C(12) 1.401(7) . . ? C(8) C(9) 1.373(6) . . ? C(9) C(10) 1.386(7) . . ? C(9) H(5) 0.95 . . no C(10) C(11) 1.374(7) . . ? C(10) H(6) 0.95 . . no C(11) C(12) 1.393(7) . . ? C(11) H(7) 0.95 . . no C(12) H(8) 0.95 . . no C(13) C(14) 1.384(6) . . ? C(13) C(18) 1.398(6) . . ? C(14) C(15) 1.380(7) . . ? C(14) H(9) 0.95 . . no C(15) C(16) 1.374(7) . . ? C(15) H(10) 0.95 . . no C(16) C(17) 1.378(7) . . ? C(16) H(11) 0.95 . . no C(17) C(18) 1.389(7) . . ? C(17) H(12) 0.95 . . no C(18) H(13) 0.95 . . no C(19) C(20) 1.388(7) . . ? C(19) C(24) 1.410(7) . . ? C(20) C(21) 1.383(7) . . ? C(20) H(14) 0.95 . . no C(21) C(22) 1.376(8) . . ? C(21) H(15) 0.95 . . no C(22) C(23) 1.376(7) . . ? C(22) H(16) 0.95 . . no C(23) C(24) 1.382(7) . . ? C(23) H(17) 0.95 . . no C(24) H(18) 0.95 . . no C(25) C(26) 1.399(7) . . ? C(25) C(30) 1.388(6) . . ? C(26) C(27) 1.386(7) . . ? C(26) H(19) 0.95 . . no C(27) C(28) 1.371(7) . . ? C(27) H(20) 0.95 . . no C(28) C(29) 1.349(8) . . ? C(28) H(21) 0.95 . . no C(29) C(30) 1.389(7) . . ? C(29) H(22) 0.95 . . no C(30) H(23) 0.95 . . no C(31) C(32) 1.385(7) . . ? C(31) C(36) 1.415(7) . . ? C(32) C(33) 1.398(7) . . ? C(32) H(24) 0.95 . . no C(33) C(34) 1.375(8) . . ? C(33) H(25) 0.95 . . no C(34) C(35) 1.370(9) . . ? C(34) H(26) 0.95 . . no C(35) C(36) 1.384(7) . . ? C(35) H(27) 0.95 . . no C(36) H(28) 0.95 . . no C(37) H(29) 0.95 . . no C(37) H(30) 0.95 . . no C(38) H(31) 0.95 . . no C(38) H(32) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Re(1) Cl(2) 91.40(5) . . . ? Cl(1) Re(1) Cl(3) 90.34(5) . . . ? Cl(1) Re(1) P(1) 88.78(4) . . . ? Cl(1) Re(1) P(2) 81.02(4) . . . ? Cl(1) Re(1) O(1) 164.86(11) . . . ? Cl(2) Re(1) Cl(3) 84.66(4) . . . ? Cl(2) Re(1) P(1) 83.38(4) . . . ? Cl(2) Re(1) P(2) 169.94(4) . . . ? Cl(2) Re(1) O(1) 101.69(11) . . . ? Cl(3) Re(1) P(1) 167.99(4) . . . ? Cl(3) Re(1) P(2) 88.75(4) . . . ? Cl(3) Re(1) O(1) 98.34(11) . . . ? P(1) Re(1) P(2) 102.93(4) . . . ? P(1) Re(1) O(1) 85.26(11) . . . ? P(2) Re(1) O(1) 86.76(11) . . . ? Re(1) P(1) C(1) 115.2(2) . . . ? Re(1) P(1) C(13) 118.5(2) . . . ? Re(1) P(1) C(19) 109.9(1) . . . ? C(1) P(1) C(13) 105.4(2) . . . ? C(1) P(1) C(19) 102.6(2) . . . ? C(13) P(1) C(19) 103.4(2) . . . ? Re(1) P(2) C(7) 122.8(2) . . . ? Re(1) P(2) C(25) 110.7(2) . . . ? Re(1) P(2) C(31) 111.7(2) . . . ? C(7) P(2) C(25) 103.7(2) . . . ? C(7) P(2) C(31) 101.7(2) . . . ? C(25) P(2) C(31) 104.3(2) . . . ? C(2) O(2) C(8) 118.1(3) . . . ? P(1) C(1) C(2) 116.3(3) . . . ? P(1) C(1) C(6) 124.7(4) . . . ? C(2) C(1) C(6) 119.0(4) . . . ? O(2) C(2) C(1) 114.2(4) . . . ? O(2) C(2) C(3) 124.4(5) . . . ? C(1) C(2) C(3) 121.3(5) . . . ? C(2) C(3) C(4) 118.1(5) . . . ? C(2) C(3) H(1) 120.9 . . . no C(4) C(3) H(1) 120.9 . . . no C(3) C(4) C(5) 121.2(4) . . . ? C(3) C(4) H(2) 119.4 . . . no C(5) C(4) H(2) 119.4 . . . no C(4) C(5) C(6) 120.3(5) . . . ? C(4) C(5) H(3) 119.9 . . . no C(6) C(5) H(3) 119.9 . . . no C(1) C(6) C(5) 120.0(5) . . . ? C(1) C(6) H(4) 120.0 . . . no C(5) C(6) H(4) 120.0 . . . no P(2) C(7) C(8) 122.7(4) . . . ? P(2) C(7) C(12) 120.5(4) . . . ? C(8) C(7) C(12) 116.5(4) . . . ? O(2) C(8) C(7) 118.2(4) . . . ? O(2) C(8) C(9) 118.8(4) . . . ? C(7) C(8) C(9) 122.9(5) . . . ? C(8) C(9) C(10) 118.9(5) . . . ? C(8) C(9) H(5) 120.5 . . . no C(10) C(9) H(5) 120.5 . . . no C(9) C(10) C(11) 120.6(5) . . . ? C(9) C(10) H(6) 119.7 . . . no C(11) C(10) H(6) 119.7 . . . no C(10) C(11) C(12) 119.7(5) . . . ? C(10) C(11) H(7) 120.2 . . . no C(12) C(11) H(7) 120.2 . . . no C(7) C(12) C(11) 121.4(4) . . . ? C(7) C(12) H(8) 119.3 . . . no C(11) C(12) H(8) 119.3 . . . no P(1) C(13) C(14) 121.0(4) . . . ? P(1) C(13) C(18) 119.7(3) . . . ? C(14) C(13) C(18) 119.3(4) . . . ? C(13) C(14) C(15) 120.1(4) . . . ? C(13) C(14) H(9) 120.0 . . . no C(15) C(14) H(9) 120.0 . . . no C(14) C(15) C(16) 120.7(4) . . . ? C(14) C(15) H(10) 119.6 . . . no C(16) C(15) H(10) 119.6 . . . no C(15) C(16) C(17) 120.0(5) . . . ? C(15) C(16) H(11) 120.0 . . . no C(17) C(16) H(11) 120.0 . . . no C(16) C(17) C(18) 120.0(5) . . . ? C(16) C(17) H(12) 120.0 . . . no C(18) C(17) H(12) 120.0 . . . no C(13) C(18) C(17) 119.9(4) . . . ? C(13) C(18) H(13) 120.0 . . . no C(17) C(18) H(13) 120.0 . . . no P(1) C(19) C(20) 122.0(4) . . . ? P(1) C(19) C(24) 119.2(4) . . . ? C(20) C(19) C(24) 118.7(5) . . . ? C(19) C(20) C(21) 120.1(5) . . . ? C(19) C(20) H(14) 120.0 . . . no C(21) C(20) H(14) 120.0 . . . no C(20) C(21) C(22) 121.0(5) . . . ? C(20) C(21) H(15) 119.5 . . . no C(22) C(21) H(15) 119.5 . . . no C(21) C(22) C(23) 119.6(5) . . . ? C(21) C(22) H(16) 120.2 . . . no C(23) C(22) H(16) 120.2 . . . no C(22) C(23) C(24) 120.6(5) . . . ? C(22) C(23) H(17) 119.7 . . . no C(24) C(23) H(17) 119.7 . . . no C(19) C(24) C(23) 120.0(5) . . . ? C(19) C(24) H(18) 120.0 . . . no C(23) C(24) H(18) 120.0 . . . no P(2) C(25) C(26) 119.8(4) . . . ? P(2) C(25) C(30) 122.2(4) . . . ? C(26) C(25) C(30) 118.0(4) . . . ? C(25) C(26) C(27) 120.4(5) . . . ? C(25) C(26) H(19) 119.8 . . . no C(27) C(26) H(19) 119.8 . . . no C(26) C(27) C(28) 119.9(5) . . . ? C(26) C(27) H(20) 120.1 . . . no C(28) C(27) H(20) 120.1 . . . no C(27) C(28) C(29) 120.8(5) . . . ? C(27) C(28) H(21) 119.6 . . . no C(29) C(28) H(21) 119.6 . . . no C(28) C(29) C(30) 120.3(5) . . . ? C(28) C(29) H(22) 119.8 . . . no C(30) C(29) H(22) 119.8 . . . no C(25) C(30) C(29) 120.6(5) . . . ? C(25) C(30) H(23) 119.7 . . . no C(29) C(30) H(23) 119.7 . . . no P(2) C(31) C(32) 122.6(4) . . . ? P(2) C(31) C(36) 118.1(4) . . . ? C(32) C(31) C(36) 119.3(5) . . . ? C(31) C(32) C(33) 119.9(5) . . . ? C(31) C(32) H(24) 120.1 . . . no C(33) C(32) H(24) 120.1 . . . no C(32) C(33) C(34) 120.3(6) . . . ? C(32) C(33) H(25) 119.8 . . . no C(34) C(33) H(25) 119.8 . . . no C(33) C(34) C(35) 120.2(5) . . . ? C(33) C(34) H(26) 119.9 . . . no C(35) C(34) H(26) 119.9 . . . no C(34) C(35) C(36) 121.0(5) . . . ? C(34) C(35) H(27) 119.5 . . . no C(36) C(35) H(27) 119.5 . . . no C(31) C(36) C(35) 119.3(5) . . . ? C(31) C(36) H(28) 120.3 . . . no C(35) C(36) H(28) 120.3 . . . no Cl(6) C(37) Cl(7) 112.2(3) . . . ? Cl(6) C(37) H(29) 108.8 . . . no Cl(6) C(37) H(30) 108.8 . . . no Cl(7) C(37) H(29) 108.8 . . . no Cl(7) C(37) H(30) 108.8 . . . no H(29) C(37) H(30) 109.5 . . . no Cl(4) C(38) Cl(5) 112.3(4) . . . ? Cl(4) C(38) H(31) 108.8 . . . no Cl(4) C(38) H(32) 108.8 . . . no Cl(5) C(38) H(31) 108.8 . . . no Cl(5) C(38) H(32) 108.8 . . . no H(31) C(38) H(32) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(27) 3.594(5) . 1_655 no Cl(2) C(37) 3.460(5) . 2_767 no Cl(2) C(17) 3.526(5) . 2_767 no Cl(3) C(38) 3.520(6) . . no Cl(3) C(37) 3.575(6) . 2_767 no Cl(4) C(9) 3.598(5) . 1_545 no Cl(6) C(4) 3.470(6) . 2_677 no Cl(7) C(3) 3.351(5) . 2_777 no O(1) C(23) 3.380(6) . 2_667 no O(1) C(22) 3.454(6) . 2_667 no C(10) C(12) 3.510(7) . 2_776 no C(10) C(11) 3.515(7) . 2_776 no C(11) C(11) 3.489(10) . 2_776 no C(15) C(28) 3.490(8) . 1_655 no C(16) C(27) 3.424(8) . 1_655 no C(16) C(37) 3.596(8) . . no C(17) C(27) 3.477(7) . 1_655 no C(23) C(37) 3.581(7) . 1_455 no C(32) C(38) 3.550(8) . . no C(33) C(38) 3.458(8) . . no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Re(1) P(1) C(1) C(2) . . . . -62.3(4) no Re(1) P(1) C(1) C(6) . . . . 116.3(4) no Re(1) P(1) C(13) C(14) . . . . 135.0(4) no Re(1) P(1) C(13) C(18) . . . . -48.0(4) no Re(1) P(1) C(19) C(20) . . . . 131.8(3) no Re(1) P(1) C(19) C(24) . . . . -49.5(4) no Re(1) P(2) C(7) C(8) . . . . -40.6(4) no Re(1) P(2) C(7) C(12) . . . . 146.7(3) no Re(1) P(2) C(25) C(26) . . . . -48.1(4) no Re(1) P(2) C(25) C(30) . . . . 130.8(4) no Re(1) P(2) C(31) C(32) . . . . 119.3(4) no Re(1) P(2) C(31) C(36) . . . . -60.3(4) no Cl(1) Re(1) P(1) C(1) . . . . 104.7(2) no Cl(1) Re(1) P(1) C(13) . . . . -21.5(2) no Cl(1) Re(1) P(1) C(19) . . . . -140.0(2) no Cl(1) Re(1) P(2) C(7) . . . . -35.8(2) no Cl(1) Re(1) P(2) C(25) . . . . -158.9(2) no Cl(1) Re(1) P(2) C(31) . . . . 85.3(2) no Cl(2) Re(1) P(1) C(1) . . . . -163.8(2) no Cl(2) Re(1) P(1) C(13) . . . . 70.1(2) no Cl(2) Re(1) P(1) C(19) . . . . -48.5(2) no Cl(2) Re(1) P(2) C(7) . . . . -77.3(3) no Cl(2) Re(1) P(2) C(25) . . . . 159.6(3) no Cl(2) Re(1) P(2) C(31) . . . . 43.8(3) no Cl(3) Re(1) P(1) C(1) . . . . -169.4(3) no Cl(3) Re(1) P(1) C(13) . . . . 64.4(3) no Cl(3) Re(1) P(1) C(19) . . . . -54.1(3) no Cl(3) Re(1) P(2) C(7) . . . . -126.4(2) no Cl(3) Re(1) P(2) C(25) . . . . 110.5(2) no Cl(3) Re(1) P(2) C(31) . . . . -5.3(2) no P(1) Re(1) P(2) C(7) . . . . 50.8(2) no P(1) Re(1) P(2) C(25) . . . . -72.3(2) no P(1) Re(1) P(2) C(31) . . . . 171.9(2) no P(1) C(1) C(2) O(2) . . . . -3.5(5) no P(1) C(1) C(2) C(3) . . . . 179.1(4) no P(1) C(1) C(6) C(5) . . . . -178.4(4) no P(1) C(13) C(14) C(15) . . . . 175.8(4) no P(1) C(13) C(18) C(17) . . . . -175.6(4) no P(1) C(19) C(20) C(21) . . . . 178.6(4) no P(1) C(19) C(24) C(23) . . . . -178.1(3) no P(2) Re(1) P(1) C(1) . . . . 24.2(2) no P(2) Re(1) P(1) C(13) . . . . -102.0(2) no P(2) Re(1) P(1) C(19) . . . . 139.5(2) no P(2) C(7) C(8) O(2) . . . . 7.5(6) no P(2) C(7) C(8) C(9) . . . . -175.1(4) no P(2) C(7) C(12) C(11) . . . . 174.2(4) no P(2) C(25) C(26) C(27) . . . . 178.1(4) no P(2) C(25) C(30) C(29) . . . . -177.1(4) no P(2) C(31) C(32) C(33) . . . . -178.0(4) no P(2) C(31) C(36) C(35) . . . . 178.5(4) no O(1) Re(1) P(1) C(1) . . . . -61.4(2) no O(1) Re(1) P(1) C(13) . . . . 172.5(2) no O(1) Re(1) P(1) C(19) . . . . 53.9(2) no O(1) Re(1) P(2) C(7) . . . . 135.2(2) no O(1) Re(1) P(2) C(25) . . . . 12.1(2) no O(1) Re(1) P(2) C(31) . . . . -103.7(2) no O(2) C(2) C(1) C(6) . . . . 177.8(4) no O(2) C(2) C(3) C(4) . . . . -177.6(4) no O(2) C(8) C(7) C(12) . . . . -179.5(4) no O(2) C(8) C(9) C(10) . . . . 179.6(4) no C(1) P(1) C(13) C(14) . . . . 4.3(5) no C(1) P(1) C(13) C(18) . . . . -178.7(4) no C(1) P(1) C(19) C(20) . . . . -105.1(4) no C(1) P(1) C(19) C(24) . . . . 73.6(4) no C(1) C(2) O(2) C(8) . . . . 153.5(4) no C(1) C(2) C(3) C(4) . . . . -0.5(7) no C(1) C(6) C(5) C(4) . . . . -0.7(8) no C(2) O(2) C(8) C(7) . . . . -95.6(5) no C(2) O(2) C(8) C(9) . . . . 86.9(5) no C(2) C(1) P(1) C(13) . . . . 70.4(4) no C(2) C(1) P(1) C(19) . . . . 178.3(4) no C(2) C(1) C(6) C(5) . . . . 0.2(7) no C(2) C(3) C(4) C(5) . . . . -0.0(8) no C(3) C(2) O(2) C(8) . . . . -29.2(6) no C(3) C(2) C(1) C(6) . . . . 0.4(7) no C(3) C(4) C(5) C(6) . . . . 0.6(8) no C(6) C(1) P(1) C(13) . . . . -111.0(4) no C(6) C(1) P(1) C(19) . . . . -3.1(5) no C(7) P(2) C(25) C(26) . . . . 178.3(4) no C(7) P(2) C(25) C(30) . . . . -2.8(5) no C(7) P(2) C(31) C(32) . . . . -108.0(4) no C(7) P(2) C(31) C(36) . . . . 72.4(4) no C(7) C(8) C(9) C(10) . . . . 2.2(7) no C(7) C(12) C(11) C(10) . . . . -0.2(8) no C(8) C(7) P(2) C(25) . . . . 85.7(4) no C(8) C(7) P(2) C(31) . . . . -166.2(4) no C(8) C(7) C(12) C(11) . . . . 1.1(7) no C(8) C(9) C(10) C(11) . . . . -1.2(8) no C(9) C(8) C(7) C(12) . . . . -2.1(7) no C(9) C(10) C(11) C(12) . . . . 0.2(8) no C(12) C(7) P(2) C(25) . . . . -87.0(4) no C(12) C(7) P(2) C(31) . . . . 21.1(4) no C(13) P(1) C(19) C(20) . . . . 4.3(4) no C(13) P(1) C(19) C(24) . . . . -177.0(3) no C(13) C(14) C(15) C(16) . . . . 0.3(8) no C(13) C(18) C(17) C(16) . . . . -0.8(8) no C(14) C(13) P(1) C(19) . . . . -103.0(4) no C(14) C(13) C(18) C(17) . . . . 1.5(7) no C(14) C(15) C(16) C(17) . . . . 0.3(8) no C(15) C(14) C(13) C(18) . . . . -1.2(7) no C(15) C(16) C(17) C(18) . . . . -0.1(8) no C(18) C(13) P(1) C(19) . . . . 73.9(4) no C(19) C(20) C(21) C(22) . . . . -0.8(8) no C(19) C(24) C(23) C(22) . . . . -0.5(7) no C(20) C(19) C(24) C(23) . . . . 0.7(7) no C(20) C(21) C(22) C(23) . . . . 0.9(8) no C(21) C(20) C(19) C(24) . . . . -0.0(7) no C(21) C(22) C(23) C(24) . . . . -0.3(7) no C(25) P(2) C(31) C(32) . . . . -0.4(5) no C(25) P(2) C(31) C(36) . . . . -179.9988 no C(25) C(26) C(27) C(28) . . . . -1.7(8) no C(25) C(30) C(29) C(28) . . . . -0.3(8) no C(26) C(25) P(2) C(31) . . . . 72.2(4) no C(26) C(25) C(30) C(29) . . . . 1.9(7) no C(26) C(27) C(28) C(29) . . . . 3.3(9) no C(27) C(26) C(25) C(30) . . . . -0.9(7) no C(27) C(28) C(29) C(30) . . . . -2.4(9) no C(30) C(25) P(2) C(31) . . . . -108.9(4) no C(31) C(32) C(33) C(34) . . . . -1.3(8) no C(31) C(36) C(35) C(34) . . . . 0.3(8) no C(32) C(31) C(36) C(35) . . . . -1.1(8) no C(32) C(33) C(34) C(35) . . . . 0.6(9) no C(33) C(32) C(31) C(36) . . . . 1.6(8) no C(33) C(34) C(35) C(36) . . . . -0.1(9) no