# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'CombinedCIF-Donahue.cif' #=================================================================== #SUBMISSION DETAILS _publ_contact_author_name 'Dr. James P. Donahue' _publ_contact_author_address ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 U.S.A. ; _publ_contact_author_email donahue@tulane.edu _publ_contact_author_fax 504-865-5596 _publ_contact_author_phone 504-862-3562 _publ_contact_letter ; # 20 August 2009 Please deposit these 12 crystal structures and provide accession numbers for them. This request is being made in anticipation of submission of a manuscript to Inorganic Chemistry. This CIF has passed the checkcif tests and generates an acceptable printcif output. Yours sincerely James P. Donahue ; #=================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; A Tungsten-Mediated Closed Cycle of Reactivity for the Reduction of CO~2~ to CO ; loop_ _publ_author_name _publ_author_footnote _publ_author_address U.Jayarathne ? ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 U.S.A. ; P.Chandrasekaran ? ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 U.S.A. ; H.Jacobsen ? ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 U.S.A. ; J.T.Mague ? ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 U.S.A. ; J.P.Donahue ? ; Department of Chemistry Tulane University 6400 Freret Street New Orleans, Louisiana 70118-5698 U.S.A. ; #=================================================================== data_jpd291_0m _database_code_depnum_ccdc_archive 'CCDC 769389' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 1, trans-[WCl2(PMePh2)4].C7H8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Dichlorotetrakis(methyldiphenylphosphine) tungsten(II) toluene solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Cl2 P4 W, C7 H8' _chemical_formula_sum 'C59 H60 Cl2 P4 W' _chemical_formula_weight 1147.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4069(8) _cell_length_b 14.3468(9) _cell_length_c 17.0921(11) _cell_angle_alpha 76.523(1) _cell_angle_beta 71.996(1) _cell_angle_gamma 84.321(1) _cell_volume 2585.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9236 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.91 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 2.499 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.5739 _exptl_absorpt_correction_T_max 0.7211 _exptl_absorpt_process_details 'APEX2 SCALE module in face-index mode (Bruker-AXS, 2009)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 30 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45623 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.25 _reflns_number_total 12641 _reflns_number_gt 12089 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.3-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+2.2213P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00050(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12641 _refine_ls_number_parameters 601 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0474 _refine_ls_wR_factor_gt 0.0466 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.755863(6) 0.760240(5) 0.746960(4) 0.00927(3) Uani 1 1 d . . . Cl1 Cl 0.58258(4) 0.65409(3) 0.80522(3) 0.01375(8) Uani 1 1 d . . . Cl2 Cl 0.92751(4) 0.86820(3) 0.69114(3) 0.01384(8) Uani 1 1 d . . . P1 P 0.84540(4) 0.63663(3) 0.65885(3) 0.01151(9) Uani 1 1 d . . . P2 P 0.68129(4) 0.86101(3) 0.62881(3) 0.01101(9) Uani 1 1 d . . . P3 P 0.62612(4) 0.85955(3) 0.84788(3) 0.01122(9) Uani 1 1 d . . . P4 P 0.86847(4) 0.68106(3) 0.85211(3) 0.01086(9) Uani 1 1 d . . . C1 C 0.97971(17) 0.66263(13) 0.56510(12) 0.0133(3) Uani 1 1 d . . . C2 C 0.98882(18) 0.63402(13) 0.49056(12) 0.0168(4) Uani 1 1 d . . . H2 H 0.9227 0.6015 0.4869 0.020 Uiso 1 1 calc R . . C3 C 1.09340(19) 0.65258(15) 0.42184(13) 0.0205(4) Uani 1 1 d . . . H3 H 1.0980 0.6332 0.3715 0.025 Uiso 1 1 calc R . . C4 C 1.1912(2) 0.69914(16) 0.42618(13) 0.0234(4) Uani 1 1 d . . . H4 H 1.2629 0.7114 0.3791 0.028 Uiso 1 1 calc R . . C5 C 1.18392(19) 0.72781(16) 0.49998(13) 0.0229(4) Uani 1 1 d . . . H5 H 1.2509 0.7594 0.5035 0.027 Uiso 1 1 calc R . . C6 C 1.07863(18) 0.71016(14) 0.56850(12) 0.0180(4) Uani 1 1 d . . . H6 H 1.0738 0.7307 0.6184 0.022 Uiso 1 1 calc R . . C7 C 0.89228(17) 0.51793(13) 0.71188(12) 0.0134(3) Uani 1 1 d . . . C8 C 1.01503(18) 0.48397(13) 0.69531(13) 0.0169(4) Uani 1 1 d . . . H8 H 1.0787 0.5233 0.6557 0.020 Uiso 1 1 calc R . . C9 C 1.04453(19) 0.39308(14) 0.73644(13) 0.0194(4) Uani 1 1 d . . . H9 H 1.1282 0.3713 0.7256 0.023 Uiso 1 1 calc R . . C10 C 0.95238(19) 0.33449(14) 0.79299(13) 0.0191(4) Uani 1 1 d . . . H10 H 0.9727 0.2722 0.8204 0.023 Uiso 1 1 calc R . . C11 C 0.83021(19) 0.36689(14) 0.80968(12) 0.0184(4) Uani 1 1 d . . . H11 H 0.7669 0.3266 0.8483 0.022 Uiso 1 1 calc R . . C12 C 0.80034(18) 0.45835(13) 0.76993(12) 0.0162(4) Uani 1 1 d . . . H12 H 0.7167 0.4805 0.7824 0.019 Uiso 1 1 calc R . . C13 C 0.73318(17) 0.59483(13) 0.61843(12) 0.0156(4) Uani 1 1 d . . . H13A H 0.7130 0.6466 0.5755 0.023 Uiso 1 1 calc R . . H13B H 0.6581 0.5760 0.6647 0.023 Uiso 1 1 calc R . . H13C H 0.7685 0.5396 0.5935 0.023 Uiso 1 1 calc R . . C14 C 0.76230(17) 0.84893(12) 0.51975(11) 0.0130(3) Uani 1 1 d . . . C15 C 0.88360(17) 0.88035(13) 0.48304(12) 0.0159(4) Uani 1 1 d . . . H15 H 0.9236 0.9037 0.5155 0.019 Uiso 1 1 calc R . . C16 C 0.94583(18) 0.87762(14) 0.39968(13) 0.0197(4) Uani 1 1 d . . . H16 H 1.0271 0.9008 0.3750 0.024 Uiso 1 1 calc R . . C17 C 0.88965(19) 0.84109(15) 0.35230(13) 0.0207(4) Uani 1 1 d . . . H17 H 0.9326 0.8388 0.2955 0.025 Uiso 1 1 calc R . . C18 C 0.77057(19) 0.80792(14) 0.38820(12) 0.0192(4) Uani 1 1 d . . . H18 H 0.7324 0.7820 0.3561 0.023 Uiso 1 1 calc R . . C19 C 0.70692(18) 0.81248(13) 0.47110(12) 0.0162(4) Uani 1 1 d . . . H19 H 0.6249 0.7906 0.4949 0.019 Uiso 1 1 calc R . . C20 C 0.52025(16) 0.85821(13) 0.63014(11) 0.0128(3) Uani 1 1 d . . . C21 C 0.46266(17) 0.77005(13) 0.65157(12) 0.0158(4) Uani 1 1 d . . . H21 H 0.5071 0.7123 0.6659 0.019 Uiso 1 1 calc R . . C22 C 0.34120(18) 0.76629(14) 0.65206(13) 0.0189(4) Uani 1 1 d . . . H22 H 0.3034 0.7061 0.6661 0.023 Uiso 1 1 calc R . . C23 C 0.27465(18) 0.85033(14) 0.63202(13) 0.0181(4) Uani 1 1 d . . . H23 H 0.1913 0.8477 0.6329 0.022 Uiso 1 1 calc R . . C24 C 0.33045(18) 0.93784(14) 0.61074(12) 0.0165(4) Uani 1 1 d . . . H24 H 0.2852 0.9954 0.5971 0.020 Uiso 1 1 calc R . . C25 C 0.45253(17) 0.94201(13) 0.60927(12) 0.0149(4) Uani 1 1 d . . . H25 H 0.4902 1.0024 0.5939 0.018 Uiso 1 1 calc R . . C26 C 0.70385(18) 0.98965(13) 0.61339(12) 0.0149(4) Uani 1 1 d . . . H26A H 0.7888 0.9998 0.6108 0.022 Uiso 1 1 calc R . . H26B H 0.6465 1.0141 0.6605 0.022 Uiso 1 1 calc R . . H26C H 0.6883 1.0237 0.5606 0.022 Uiso 1 1 calc R . . C27 C 0.48573(17) 0.92163(13) 0.82619(11) 0.0139(4) Uani 1 1 d . . . C28 C 0.39246(17) 0.86425(14) 0.82742(12) 0.0156(4) Uani 1 1 d . . . H28 H 0.4052 0.7966 0.8362 0.019 Uiso 1 1 calc R . . C29 C 0.28152(18) 0.90479(15) 0.81590(12) 0.0188(4) Uani 1 1 d . . . H29 H 0.2181 0.8649 0.8186 0.023 Uiso 1 1 calc R . . C30 C 0.26379(19) 1.00368(15) 0.80046(13) 0.0210(4) Uani 1 1 d . . . H30 H 0.1884 1.0317 0.7920 0.025 Uiso 1 1 calc R . . C31 C 0.35571(19) 1.06137(15) 0.79744(13) 0.0207(4) Uani 1 1 d . . . H31 H 0.3437 1.1291 0.7862 0.025 Uiso 1 1 calc R . . C32 C 0.46607(18) 1.02104(14) 0.81078(12) 0.0174(4) Uani 1 1 d . . . H32 H 0.5282 1.0614 0.8094 0.021 Uiso 1 1 calc R . . C33 C 0.69331(16) 0.95558(13) 0.87316(12) 0.0132(3) Uani 1 1 d . . . C34 C 0.76162(18) 1.02547(14) 0.80772(12) 0.0167(4) Uani 1 1 d . . . H34 H 0.7771 1.0201 0.7510 0.020 Uiso 1 1 calc R . . C35 C 0.80713(19) 1.10261(14) 0.82446(13) 0.0196(4) Uani 1 1 d . . . H35 H 0.8511 1.1506 0.7793 0.024 Uiso 1 1 calc R . . C36 C 0.78819(18) 1.10959(14) 0.90743(13) 0.0183(4) Uani 1 1 d . . . H36 H 0.8198 1.1620 0.9191 0.022 Uiso 1 1 calc R . . C37 C 0.72313(18) 1.03976(14) 0.97281(12) 0.0168(4) Uani 1 1 d . . . H37 H 0.7115 1.0437 1.0294 0.020 Uiso 1 1 calc R . . C38 C 0.67462(17) 0.96381(13) 0.95607(12) 0.0155(4) Uani 1 1 d . . . H38 H 0.6284 0.9171 1.0014 0.019 Uiso 1 1 calc R . . C39 C 0.54937(17) 0.78814(13) 0.95263(12) 0.0150(4) Uani 1 1 d . . . H39A H 0.6113 0.7607 0.9812 0.022 Uiso 1 1 calc R . . H39B H 0.5050 0.7363 0.9467 0.022 Uiso 1 1 calc R . . H39C H 0.4909 0.8293 0.9859 0.022 Uiso 1 1 calc R . . C40 C 0.87842(16) 0.74552(13) 0.93196(12) 0.0136(3) Uani 1 1 d . . . C41 C 0.94735(17) 0.82856(14) 0.90482(13) 0.0164(4) Uani 1 1 d . . . H41 H 0.9829 0.8531 0.8463 0.020 Uiso 1 1 calc R . . C42 C 0.96437(18) 0.87571(14) 0.96314(13) 0.0190(4) Uani 1 1 d . . . H42 H 1.0136 0.9309 0.9442 0.023 Uiso 1 1 calc R . . C43 C 0.90976(18) 0.84234(15) 1.04851(13) 0.0203(4) Uani 1 1 d . . . H43 H 0.9212 0.8748 1.0880 0.024 Uiso 1 1 calc R . . C44 C 0.83865(18) 0.76179(15) 1.07618(13) 0.0191(4) Uani 1 1 d . . . H44 H 0.7997 0.7398 1.1347 0.023 Uiso 1 1 calc R . . C45 C 0.82386(17) 0.71280(14) 1.01851(12) 0.0156(4) Uani 1 1 d . . . H45 H 0.7763 0.6567 1.0381 0.019 Uiso 1 1 calc R . . C46 C 0.82475(17) 0.56236(13) 0.91892(11) 0.0127(3) Uani 1 1 d . . . C47 C 0.69996(17) 0.54518(13) 0.96080(12) 0.0160(4) Uani 1 1 d . . . H47 H 0.6397 0.5936 0.9514 0.019 Uiso 1 1 calc R . . C48 C 0.66288(19) 0.45828(14) 1.01591(13) 0.0199(4) Uani 1 1 d . . . H48 H 0.5779 0.4481 1.0446 0.024 Uiso 1 1 calc R . . C49 C 0.7498(2) 0.38651(14) 1.02897(13) 0.0212(4) Uani 1 1 d . . . H49 H 0.7245 0.3271 1.0667 0.025 Uiso 1 1 calc R . . C50 C 0.87362(19) 0.40159(14) 0.98678(13) 0.0193(4) Uani 1 1 d . . . H50 H 0.9331 0.3520 0.9948 0.023 Uiso 1 1 calc R . . C51 C 0.91118(17) 0.48922(13) 0.93266(12) 0.0151(4) Uani 1 1 d . . . H51 H 0.9964 0.4994 0.9048 0.018 Uiso 1 1 calc R . . C52 C 1.03495(16) 0.66572(13) 0.80317(12) 0.0140(3) Uani 1 1 d . . . H52A H 1.0760 0.6447 0.8472 0.021 Uiso 1 1 calc R . . H52B H 1.0683 0.7269 0.7674 0.021 Uiso 1 1 calc R . . H52C H 1.0493 0.6174 0.7688 0.021 Uiso 1 1 calc R . . C53 C 0.6018(3) 0.5832(2) 0.3570(2) 0.0538(8) Uani 1 1 d U . . C54 C 0.5402(3) 0.6612(3) 0.3239(2) 0.0537(8) Uani 1 1 d U . . H54 H 0.5127 0.7114 0.3537 0.064 Uiso 1 1 calc R . . C55 C 0.5168(3) 0.6688(3) 0.2469(3) 0.0736(11) Uani 1 1 d U . . H55 H 0.4757 0.7244 0.2240 0.088 Uiso 1 1 calc R . . C56 C 0.5528(4) 0.5967(4) 0.2055(3) 0.0827(14) Uani 1 1 d U . . H56 H 0.5350 0.6008 0.1540 0.099 Uiso 1 1 calc R . . C57 C 0.6129(4) 0.5203(4) 0.2361(3) 0.0941(17) Uani 1 1 d U . . H57 H 0.6397 0.4707 0.2056 0.113 Uiso 1 1 calc R . . C58 C 0.6383(4) 0.5112(3) 0.3148(3) 0.0801(13) Uani 1 1 d U . . H58 H 0.6800 0.4556 0.3369 0.096 Uiso 1 1 calc R . . C59 C 0.6336(4) 0.5694(4) 0.4382(3) 0.0873(14) Uani 1 1 d U . . H59A H 0.6440 0.5008 0.4607 0.131 Uiso 1 1 calc R . . H59B H 0.5670 0.5968 0.4790 0.131 Uiso 1 1 calc R . . H59C H 0.7105 0.6017 0.4277 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.00908(4) 0.00973(4) 0.00882(4) -0.00120(2) -0.00267(3) -0.00130(2) Cl1 0.01213(19) 0.01332(19) 0.0147(2) -0.00128(15) -0.00265(16) -0.00345(15) Cl2 0.01217(19) 0.01455(19) 0.0143(2) -0.00097(15) -0.00370(16) -0.00403(15) P1 0.0132(2) 0.0106(2) 0.0113(2) -0.00237(16) -0.00430(18) -0.00077(16) P2 0.0114(2) 0.0112(2) 0.0102(2) -0.00096(16) -0.00362(17) -0.00136(16) P3 0.0105(2) 0.0119(2) 0.0108(2) -0.00196(16) -0.00257(17) -0.00091(16) P4 0.0103(2) 0.0123(2) 0.0099(2) -0.00168(16) -0.00313(17) -0.00146(16) C1 0.0160(9) 0.0110(8) 0.0120(9) -0.0017(6) -0.0038(7) 0.0006(6) C2 0.0204(10) 0.0163(9) 0.0165(10) -0.0055(7) -0.0080(8) -0.0003(7) C3 0.0246(10) 0.0241(10) 0.0142(10) -0.0084(8) -0.0048(8) 0.0007(8) C4 0.0208(10) 0.0302(11) 0.0160(10) -0.0073(8) 0.0014(8) -0.0023(8) C5 0.0196(10) 0.0314(11) 0.0187(11) -0.0084(8) -0.0029(8) -0.0073(8) C6 0.0197(10) 0.0222(10) 0.0132(9) -0.0060(7) -0.0040(8) -0.0031(7) C7 0.0190(9) 0.0108(8) 0.0129(9) -0.0039(6) -0.0072(7) -0.0003(7) C8 0.0202(9) 0.0141(9) 0.0179(10) -0.0041(7) -0.0068(8) -0.0013(7) C9 0.0207(10) 0.0175(9) 0.0231(11) -0.0061(8) -0.0106(8) 0.0028(7) C10 0.0281(11) 0.0133(9) 0.0193(10) -0.0025(7) -0.0131(8) 0.0009(7) C11 0.0266(10) 0.0142(9) 0.0144(9) -0.0020(7) -0.0063(8) -0.0031(7) C12 0.0201(9) 0.0147(9) 0.0148(9) -0.0038(7) -0.0062(8) -0.0005(7) C13 0.0174(9) 0.0150(9) 0.0167(9) -0.0036(7) -0.0075(7) -0.0023(7) C14 0.0144(8) 0.0107(8) 0.0119(9) 0.0001(6) -0.0032(7) 0.0008(6) C15 0.0148(9) 0.0162(9) 0.0159(9) -0.0022(7) -0.0045(7) -0.0001(7) C16 0.0164(9) 0.0208(10) 0.0170(10) -0.0015(7) -0.0002(8) 0.0005(7) C17 0.0238(10) 0.0225(10) 0.0122(9) -0.0031(7) -0.0023(8) 0.0044(8) C18 0.0256(10) 0.0197(9) 0.0144(10) -0.0040(7) -0.0096(8) 0.0019(8) C19 0.0178(9) 0.0147(9) 0.0160(9) -0.0016(7) -0.0060(7) -0.0013(7) C20 0.0125(8) 0.0168(9) 0.0094(8) -0.0025(6) -0.0040(7) -0.0004(6) C21 0.0164(9) 0.0157(9) 0.0160(9) -0.0032(7) -0.0059(7) 0.0002(7) C22 0.0172(9) 0.0182(9) 0.0222(10) -0.0039(8) -0.0060(8) -0.0050(7) C23 0.0137(9) 0.0233(10) 0.0193(10) -0.0056(8) -0.0068(8) -0.0003(7) C24 0.0166(9) 0.0191(9) 0.0140(9) -0.0020(7) -0.0070(7) 0.0035(7) C25 0.0171(9) 0.0151(9) 0.0118(9) -0.0012(7) -0.0043(7) -0.0007(7) C26 0.0178(9) 0.0126(8) 0.0149(9) -0.0016(7) -0.0058(7) -0.0021(7) C27 0.0134(8) 0.0172(9) 0.0093(9) -0.0022(7) -0.0020(7) 0.0016(7) C28 0.0148(9) 0.0188(9) 0.0125(9) -0.0042(7) -0.0025(7) 0.0006(7) C29 0.0136(9) 0.0291(11) 0.0140(10) -0.0058(8) -0.0037(7) 0.0005(7) C30 0.0168(9) 0.0308(11) 0.0147(10) -0.0058(8) -0.0055(8) 0.0079(8) C31 0.0234(10) 0.0204(10) 0.0156(10) -0.0025(7) -0.0050(8) 0.0074(8) C32 0.0170(9) 0.0175(9) 0.0154(10) -0.0025(7) -0.0029(8) 0.0003(7) C33 0.0107(8) 0.0134(8) 0.0157(9) -0.0040(7) -0.0039(7) 0.0004(6) C34 0.0173(9) 0.0193(9) 0.0133(9) -0.0044(7) -0.0026(7) -0.0027(7) C35 0.0212(10) 0.0185(9) 0.0176(10) -0.0030(7) -0.0022(8) -0.0063(7) C36 0.0184(9) 0.0165(9) 0.0222(10) -0.0081(8) -0.0060(8) -0.0013(7) C37 0.0185(9) 0.0203(9) 0.0134(9) -0.0067(7) -0.0056(7) 0.0014(7) C38 0.0161(9) 0.0156(9) 0.0140(9) -0.0024(7) -0.0039(7) 0.0003(7) C39 0.0154(9) 0.0153(9) 0.0125(9) -0.0005(7) -0.0033(7) -0.0007(7) C40 0.0114(8) 0.0160(9) 0.0151(9) -0.0043(7) -0.0063(7) 0.0014(6) C41 0.0148(9) 0.0173(9) 0.0168(10) -0.0039(7) -0.0040(7) -0.0009(7) C42 0.0173(9) 0.0181(9) 0.0253(11) -0.0090(8) -0.0086(8) -0.0001(7) C43 0.0196(10) 0.0253(10) 0.0223(11) -0.0137(8) -0.0105(8) 0.0049(8) C44 0.0195(10) 0.0250(10) 0.0132(9) -0.0057(7) -0.0057(8) 0.0036(8) C45 0.0141(9) 0.0176(9) 0.0151(9) -0.0039(7) -0.0047(7) 0.0012(7) C46 0.0147(9) 0.0132(8) 0.0107(9) -0.0008(6) -0.0049(7) -0.0019(6) C47 0.0151(9) 0.0167(9) 0.0155(9) -0.0008(7) -0.0051(7) -0.0008(7) C48 0.0175(9) 0.0210(10) 0.0181(10) 0.0027(8) -0.0041(8) -0.0059(7) C49 0.0270(11) 0.0168(9) 0.0181(10) 0.0042(7) -0.0087(8) -0.0055(8) C50 0.0231(10) 0.0166(9) 0.0194(10) -0.0006(7) -0.0109(8) 0.0014(7) C51 0.0144(9) 0.0175(9) 0.0147(9) -0.0034(7) -0.0061(7) -0.0004(7) C52 0.0117(8) 0.0171(9) 0.0129(9) -0.0037(7) -0.0024(7) -0.0014(6) C53 0.0459(17) 0.0540(19) 0.060(2) -0.0112(15) -0.0076(15) -0.0224(14) C54 0.0371(16) 0.067(2) 0.059(2) -0.0254(17) -0.0058(14) -0.0079(14) C55 0.049(2) 0.091(3) 0.076(3) -0.004(2) -0.0154(19) -0.0237(19) C56 0.054(2) 0.129(4) 0.068(3) -0.050(3) 0.0143(19) -0.051(2) C57 0.076(3) 0.118(4) 0.106(4) -0.077(3) -0.002(3) -0.037(3) C58 0.069(2) 0.046(2) 0.133(4) -0.029(2) -0.029(3) -0.0131(17) C59 0.101(3) 0.102(3) 0.064(3) -0.012(2) -0.023(2) -0.046(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl1 2.4270(4) . ? W1 Cl2 2.4289(4) . ? W1 P3 2.5191(5) . ? W1 P2 2.5199(5) . ? W1 P4 2.5214(5) . ? W1 P1 2.5282(5) . ? P1 C13 1.8351(19) . ? P1 C1 1.8361(19) . ? P1 C7 1.8459(18) . ? P2 C20 1.8344(19) . ? P2 C26 1.8350(18) . ? P2 C14 1.8473(19) . ? P3 C33 1.8339(19) . ? P3 C39 1.8372(19) . ? P3 C27 1.8509(19) . ? P4 C46 1.8337(19) . ? P4 C52 1.8373(18) . ? P4 C40 1.8534(19) . ? C1 C6 1.398(3) . ? C1 C2 1.399(3) . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.392(3) . ? C4 H4 0.9500 . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.398(3) . ? C7 C8 1.401(3) . ? C8 C9 1.393(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 C12 1.392(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.399(3) . ? C14 C15 1.402(3) . ? C15 C16 1.389(3) . ? C15 H15 0.9500 . ? C16 C17 1.388(3) . ? C16 H16 0.9500 . ? C17 C18 1.387(3) . ? C17 H17 0.9500 . ? C18 C19 1.392(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.399(2) . ? C20 C21 1.402(3) . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 C23 1.391(3) . ? C22 H22 0.9500 . ? C23 C24 1.384(3) . ? C23 H23 0.9500 . ? C24 C25 1.392(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.397(3) . ? C27 C28 1.401(3) . ? C28 C29 1.390(3) . ? C28 H28 0.9500 . ? C29 C30 1.387(3) . ? C29 H29 0.9500 . ? C30 C31 1.380(3) . ? C30 H30 0.9500 . ? C31 C32 1.394(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.398(3) . ? C33 C34 1.399(3) . ? C34 C35 1.389(3) . ? C34 H34 0.9500 . ? C35 C36 1.393(3) . ? C35 H35 0.9500 . ? C36 C37 1.384(3) . ? C36 H36 0.9500 . ? C37 C38 1.392(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.398(3) . ? C40 C45 1.400(3) . ? C41 C42 1.396(3) . ? C41 H41 0.9500 . ? C42 C43 1.385(3) . ? C42 H42 0.9500 . ? C43 C44 1.382(3) . ? C43 H43 0.9500 . ? C44 C45 1.394(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.397(2) . ? C46 C47 1.399(3) . ? C47 C48 1.390(3) . ? C47 H47 0.9500 . ? C48 C49 1.386(3) . ? C48 H48 0.9500 . ? C49 C50 1.386(3) . ? C49 H49 0.9500 . ? C50 C51 1.393(3) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C58 1.356(5) . ? C53 C54 1.364(5) . ? C53 C59 1.505(5) . ? C54 C55 1.400(5) . ? C54 H54 0.9500 . ? C55 C56 1.348(6) . ? C55 H55 0.9500 . ? C56 C57 1.323(7) . ? C56 H56 0.9500 . ? C57 C58 1.436(7) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 W1 Cl2 178.778(15) . . ? Cl1 W1 P3 84.118(15) . . ? Cl2 W1 P3 94.699(15) . . ? Cl1 W1 P2 96.210(16) . . ? Cl2 W1 P2 84.107(15) . . ? P3 W1 P2 91.041(15) . . ? Cl1 W1 P4 95.580(16) . . ? Cl2 W1 P4 84.115(16) . . ? P3 W1 P4 90.625(15) . . ? P2 W1 P4 168.201(15) . . ? Cl1 W1 P1 83.139(15) . . ? Cl2 W1 P1 98.045(15) . . ? P3 W1 P1 167.255(15) . . ? P2 W1 P1 90.094(16) . . ? P4 W1 P1 90.854(15) . . ? C13 P1 C1 102.78(9) . . ? C13 P1 C7 97.31(8) . . ? C1 P1 C7 100.67(8) . . ? C13 P1 W1 113.29(6) . . ? C1 P1 W1 121.10(6) . . ? C7 P1 W1 118.07(6) . . ? C20 P2 C26 102.45(9) . . ? C20 P2 C14 100.61(8) . . ? C26 P2 C14 97.48(8) . . ? C20 P2 W1 120.79(6) . . ? C26 P2 W1 113.10(6) . . ? C14 P2 W1 118.78(6) . . ? C33 P3 C39 102.46(9) . . ? C33 P3 C27 100.91(8) . . ? C39 P3 C27 97.01(8) . . ? C33 P3 W1 121.13(6) . . ? C39 P3 W1 113.53(6) . . ? C27 P3 W1 118.07(6) . . ? C46 P4 C52 103.11(8) . . ? C46 P4 C40 100.24(8) . . ? C52 P4 C40 97.38(8) . . ? C46 P4 W1 120.50(6) . . ? C52 P4 W1 112.82(6) . . ? C40 P4 W1 119.25(6) . . ? C6 C1 C2 118.29(17) . . ? C6 C1 P1 119.26(14) . . ? C2 C1 P1 122.43(15) . . ? C3 C2 C1 120.72(18) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.46(19) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.58(19) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 119.97(19) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.98(18) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C12 C7 C8 118.56(17) . . ? C12 C7 P1 118.25(14) . . ? C8 C7 P1 123.17(15) . . ? C9 C8 C7 120.54(18) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 120.24(19) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.89(18) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 120.14(19) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.62(18) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 118.36(17) . . ? C19 C14 P2 122.99(14) . . ? C15 C14 P2 118.62(14) . . ? C16 C15 C14 120.67(19) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 120.23(19) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 119.80(18) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 120.14(19) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 120.76(18) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C25 C20 C21 118.40(17) . . ? C25 C20 P2 121.85(14) . . ? C21 C20 P2 119.74(14) . . ? C22 C21 C20 120.65(17) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.27(18) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.65(18) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.35(17) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C20 120.68(18) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 118.38(17) . . ? C32 C27 P3 124.36(15) . . ? C28 C27 P3 117.24(14) . . ? C29 C28 C27 120.98(18) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C30 C29 C28 119.78(19) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 119.95(18) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.52(19) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C27 120.35(19) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C38 C33 C34 118.38(17) . . ? C38 C33 P3 122.19(14) . . ? C34 C33 P3 119.38(14) . . ? C35 C34 C33 120.93(18) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.98(19) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 119.66(18) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.40(18) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C33 120.61(18) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 118.50(17) . . ? C41 C40 P4 118.53(14) . . ? C45 C40 P4 122.93(14) . . ? C42 C41 C40 120.47(18) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 120.22(19) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 119.95(18) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.19(19) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 120.62(18) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? C51 C46 C47 118.30(17) . . ? C51 C46 P4 122.82(14) . . ? C47 C46 P4 118.83(14) . . ? C48 C47 C46 120.94(18) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C49 C48 C47 120.04(19) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C48 119.81(18) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C49 C50 C51 120.24(18) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C46 120.65(18) . . ? C50 C51 H51 119.7 . . ? C46 C51 H51 119.7 . . ? P4 C52 H52A 109.5 . . ? P4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? P4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C58 C53 C54 118.8(4) . . ? C58 C53 C59 116.0(4) . . ? C54 C53 C59 125.2(4) . . ? C53 C54 C55 121.2(4) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? C56 C55 C54 119.6(5) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C57 C56 C55 120.4(5) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C56 C57 C58 120.9(4) . . ? C56 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? C53 C58 C57 119.0(4) . . ? C53 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C53 C59 H59A 109.5 . . ? C53 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C53 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.238 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.077 #===END data_jpd196_0m _database_code_depnum_ccdc_archive 'CCDC 769390' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 2, [W(O)(CO)Cl2(PMePh2)2].0.5(C6H6) _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis,cis,trans-Dichloro(oxo)carbonylbis(methyldiphenyl phosphine)tungsten(IV) Hemibenzene solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H26 Cl2 O2 P2 W, 0.5(C6 H6)' _chemical_formula_sum 'C30 H29 Cl2 O2 P2 W' _chemical_formula_weight 738.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5417(6) _cell_length_b 14.6428(9) _cell_length_c 20.463(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.775(1) _cell_angle_gamma 90.00 _cell_volume 2858.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9848 _cell_measurement_theta_min 2.343 _cell_measurement_theta_max 28.268 _exptl_crystal_description column _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 4.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6224 _exptl_absorpt_correction_T_max 0.7984 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 20 sec/frame. From 1476 reflections chosen from the full data set and having I/\s(I) > 20 it was determined that the crystal was twinned by a 177\% rotation about b (CELL_NOW (Sheldrick, 2005)). Integration of the raw intensity data was accomplished using the multi-component version of SAINT+ as directed by the 2-component control file generated by CELL_NOW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99848 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7090 _reflns_number_gt 6335 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2007)' _publ_section_references ; Bruker-AXS (2007). APEX2, Version 2.2.0, Madison, WI. Bruker-AXS (2006). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2005). CELL_NOW. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). TWINABS, Version 2007/5. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+4.0822P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7090 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0478 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.394498(11) 0.160784(7) 0.108071(5) 0.01081(3) Uani 1 1 d . . . Cl1 Cl 0.26646(7) 0.29731(5) 0.13927(3) 0.01667(13) Uani 1 1 d . . . Cl2 Cl 0.59803(7) 0.19910(5) 0.18095(3) 0.01560(13) Uani 1 1 d . . . P1 P 0.31344(7) 0.08961(5) 0.21360(3) 0.01199(13) Uani 1 1 d . . . P2 P 0.52720(7) 0.26533(5) 0.03133(3) 0.01221(13) Uani 1 1 d . . . O1 O 0.27636(19) 0.11075(14) 0.05544(9) 0.0165(4) Uani 1 1 d . . . O2 O 0.6013(2) -0.00400(15) 0.07898(11) 0.0236(5) Uani 1 1 d . . . C1 C 0.4230(3) -0.00333(19) 0.24288(13) 0.0149(5) Uani 1 1 d . . . C2 C 0.5086(3) 0.0049(2) 0.29812(15) 0.0195(6) Uani 1 1 d . . . H2 H 0.5102 0.0604 0.3222 0.023 Uiso 1 1 calc R . . C3 C 0.5920(3) -0.0682(2) 0.31814(16) 0.0262(7) Uani 1 1 d . . . H3 H 0.6502 -0.0622 0.3559 0.031 Uiso 1 1 calc R . . C4 C 0.5911(3) -0.1486(2) 0.28388(17) 0.0255(7) Uani 1 1 d . . . H4 H 0.6479 -0.1982 0.2981 0.031 Uiso 1 1 calc R . . C5 C 0.5067(3) -0.1574(2) 0.22797(16) 0.0223(6) Uani 1 1 d . . . H5 H 0.5062 -0.2130 0.2040 0.027 Uiso 1 1 calc R . . C6 C 0.4239(3) -0.0851(2) 0.20771(14) 0.0177(6) Uani 1 1 d . . . H6 H 0.3670 -0.0911 0.1695 0.021 Uiso 1 1 calc R . . C7 C 0.1379(3) 0.04134(19) 0.20696(13) 0.0138(5) Uani 1 1 d . . . C8 C 0.1004(3) -0.0401(2) 0.23730(14) 0.0168(6) Uani 1 1 d . . . H8 H 0.1676 -0.0727 0.2628 0.020 Uiso 1 1 calc R . . C9 C -0.0358(3) -0.0740(2) 0.23018(15) 0.0203(6) Uani 1 1 d . . . H9 H -0.0609 -0.1298 0.2507 0.024 Uiso 1 1 calc R . . C10 C -0.1342(3) -0.0265(2) 0.19335(15) 0.0224(6) Uani 1 1 d . . . H10 H -0.2268 -0.0495 0.1886 0.027 Uiso 1 1 calc R . . C11 C -0.0974(3) 0.0552(2) 0.16333(16) 0.0234(7) Uani 1 1 d . . . H11 H -0.1650 0.0878 0.1381 0.028 Uiso 1 1 calc R . . C12 C 0.0378(3) 0.0890(2) 0.17016(15) 0.0200(6) Uani 1 1 d . . . H12 H 0.0624 0.1448 0.1497 0.024 Uiso 1 1 calc R . . C13 C 0.3026(3) 0.1700(2) 0.28111(14) 0.0192(6) Uani 1 1 d . . . H13A H 0.2350 0.2181 0.2700 0.029 Uiso 1 1 calc R . . H13B H 0.3950 0.1973 0.2893 0.029 Uiso 1 1 calc R . . H13C H 0.2721 0.1378 0.3204 0.029 Uiso 1 1 calc R . . C14 C 0.6978(3) 0.2206(2) 0.00854(13) 0.0145(5) Uani 1 1 d . . . C15 C 0.8217(3) 0.2497(2) 0.03857(14) 0.0188(6) Uani 1 1 d . . . H15 H 0.8198 0.2983 0.0693 0.023 Uiso 1 1 calc R . . C16 C 0.9485(3) 0.2079(2) 0.02372(15) 0.0212(6) Uani 1 1 d . . . H16 H 1.0327 0.2285 0.0441 0.025 Uiso 1 1 calc R . . C17 C 0.9527(3) 0.1369(2) -0.02027(15) 0.0222(6) Uani 1 1 d . . . H17 H 1.0393 0.1082 -0.0299 0.027 Uiso 1 1 calc R . . C18 C 0.8295(3) 0.1074(2) -0.05061(16) 0.0256(7) Uani 1 1 d . . . H18 H 0.8319 0.0589 -0.0814 0.031 Uiso 1 1 calc R . . C19 C 0.7033(3) 0.1489(2) -0.03587(15) 0.0230(7) Uani 1 1 d . . . H19 H 0.6193 0.1280 -0.0564 0.028 Uiso 1 1 calc R . . C20 C 0.4376(3) 0.29180(19) -0.04595(13) 0.0142(5) Uani 1 1 d . . . C21 C 0.3184(3) 0.2441(2) -0.06636(14) 0.0164(6) Uani 1 1 d . . . H21 H 0.2844 0.1948 -0.0409 0.020 Uiso 1 1 calc R . . C22 C 0.2488(3) 0.2689(2) -0.12428(15) 0.0215(6) Uani 1 1 d . . . H22 H 0.1675 0.2364 -0.1381 0.026 Uiso 1 1 calc R . . C23 C 0.2979(3) 0.3405(2) -0.16154(14) 0.0211(6) Uani 1 1 d . . . H23 H 0.2497 0.3574 -0.2007 0.025 Uiso 1 1 calc R . . C24 C 0.4176(4) 0.3880(2) -0.14189(15) 0.0248(7) Uani 1 1 d . . . H24 H 0.4514 0.4371 -0.1675 0.030 Uiso 1 1 calc R . . C25 C 0.4875(3) 0.3631(2) -0.08461(15) 0.0222(6) Uani 1 1 d . . . H25 H 0.5701 0.3949 -0.0716 0.027 Uiso 1 1 calc R . . C26 C 0.5629(3) 0.3768(2) 0.06712(14) 0.0181(6) Uani 1 1 d . . . H26A H 0.6077 0.3689 0.1101 0.027 Uiso 1 1 calc R . . H26B H 0.4747 0.4103 0.0719 0.027 Uiso 1 1 calc R . . H26C H 0.6255 0.4112 0.0386 0.027 Uiso 1 1 calc R . . C27 C 0.5282(3) 0.0550(2) 0.09013(13) 0.0148(5) Uani 1 1 d . . . C28 C 0.4830(4) 0.0756(3) 0.46054(17) 0.0345(8) Uani 1 1 d . . . H28 H 0.4710 0.1278 0.4335 0.041 Uiso 1 1 calc R . . C29 C 0.3862(4) 0.0056(3) 0.45797(17) 0.0340(8) Uani 1 1 d . . . H29 H 0.3081 0.0094 0.4288 0.041 Uiso 1 1 calc R . . C30 C 0.4026(4) -0.0697(3) 0.49740(17) 0.0353(9) Uani 1 1 d . . . H30 H 0.3354 -0.1175 0.4958 0.042 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01074(5) 0.01059(5) 0.01107(5) -0.00027(4) -0.00060(3) -0.00016(4) Cl1 0.0163(3) 0.0146(3) 0.0191(3) -0.0002(3) 0.0001(2) 0.0032(2) Cl2 0.0127(3) 0.0175(3) 0.0164(3) -0.0004(3) -0.0038(2) -0.0013(2) P1 0.0117(3) 0.0118(3) 0.0124(3) 0.0005(3) 0.0002(2) 0.0020(3) P2 0.0129(3) 0.0113(3) 0.0124(3) 0.0003(3) -0.0008(3) -0.0014(3) O1 0.0132(9) 0.0193(11) 0.0168(10) 0.0010(8) -0.0026(8) -0.0014(8) O2 0.0248(11) 0.0193(11) 0.0267(11) -0.0029(9) 0.0035(9) 0.0045(9) C1 0.0132(12) 0.0156(14) 0.0160(13) 0.0043(11) 0.0029(10) 0.0000(10) C2 0.0170(13) 0.0194(15) 0.0219(15) 0.0024(12) -0.0012(11) 0.0008(11) C3 0.0188(15) 0.0313(18) 0.0281(17) 0.0105(14) -0.0056(13) 0.0032(13) C4 0.0166(14) 0.0216(16) 0.0384(18) 0.0145(14) 0.0045(13) 0.0055(12) C5 0.0176(13) 0.0176(14) 0.0320(16) 0.0052(13) 0.0083(12) 0.0038(12) C6 0.0170(13) 0.0184(14) 0.0178(14) 0.0002(12) 0.0019(11) 0.0025(11) C7 0.0123(12) 0.0134(13) 0.0159(13) -0.0002(11) 0.0022(10) 0.0023(10) C8 0.0173(13) 0.0180(14) 0.0151(13) 0.0030(11) 0.0017(11) 0.0011(11) C9 0.0226(15) 0.0131(14) 0.0253(15) 0.0027(12) 0.0052(12) -0.0027(11) C10 0.0144(13) 0.0250(16) 0.0276(16) 0.0039(13) 0.0015(12) -0.0039(12) C11 0.0136(13) 0.0250(16) 0.0315(17) 0.0066(14) -0.0021(12) 0.0025(12) C12 0.0162(13) 0.0146(14) 0.0292(16) 0.0058(12) 0.0017(12) 0.0010(11) C13 0.0237(14) 0.0192(15) 0.0148(13) -0.0020(12) 0.0013(11) 0.0051(12) C14 0.0137(12) 0.0167(14) 0.0132(12) 0.0018(11) -0.0010(10) -0.0006(10) C15 0.0175(14) 0.0215(15) 0.0173(14) -0.0029(12) -0.0030(11) -0.0009(11) C16 0.0143(13) 0.0255(17) 0.0236(15) 0.0042(13) -0.0042(11) -0.0014(12) C17 0.0172(14) 0.0221(16) 0.0275(16) 0.0036(13) 0.0039(12) 0.0027(12) C18 0.0221(15) 0.0240(17) 0.0307(17) -0.0123(14) 0.0032(13) -0.0008(13) C19 0.0162(14) 0.0262(17) 0.0266(16) -0.0076(13) -0.0007(12) -0.0030(12) C20 0.0165(13) 0.0144(13) 0.0117(12) 0.0005(11) 0.0003(10) 0.0033(10) C21 0.0176(13) 0.0170(14) 0.0145(13) 0.0008(11) -0.0014(11) -0.0006(11) C22 0.0171(14) 0.0279(17) 0.0194(14) -0.0036(13) -0.0021(11) 0.0017(12) C23 0.0249(15) 0.0235(15) 0.0149(13) -0.0013(13) -0.0021(11) 0.0115(13) C24 0.0362(18) 0.0180(15) 0.0201(15) 0.0063(13) 0.0009(13) 0.0021(13) C25 0.0239(15) 0.0210(16) 0.0218(15) 0.0032(12) -0.0029(12) -0.0037(12) C26 0.0215(14) 0.0127(13) 0.0201(14) -0.0023(12) 0.0000(11) -0.0009(11) C27 0.0147(12) 0.0164(14) 0.0132(13) 0.0012(11) -0.0011(10) -0.0050(11) C28 0.056(2) 0.0261(18) 0.0213(16) -0.0005(14) 0.0002(16) -0.0044(17) C29 0.0341(19) 0.040(2) 0.0277(18) -0.0079(16) -0.0015(15) -0.0038(16) C30 0.046(2) 0.0309(19) 0.0296(18) -0.0044(16) 0.0071(16) -0.0204(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.7130(19) . ? W1 C27 2.043(3) . ? W1 Cl1 2.4326(7) . ? W1 Cl2 2.4964(7) . ? W1 P1 2.5284(7) . ? W1 P2 2.5429(7) . ? P1 C1 1.813(3) . ? P1 C13 1.819(3) . ? P1 C7 1.822(3) . ? P2 C26 1.819(3) . ? P2 C14 1.822(3) . ? P2 C20 1.829(3) . ? O2 C27 1.135(3) . ? C1 C2 1.391(4) . ? C1 C6 1.397(4) . ? C2 C3 1.392(4) . ? C2 H2 0.9500 . ? C3 C4 1.370(5) . ? C3 H3 0.9500 . ? C4 C5 1.396(5) . ? C4 H4 0.9500 . ? C5 C6 1.381(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.394(4) . ? C7 C12 1.395(4) . ? C8 C9 1.397(4) . ? C8 H8 0.9500 . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 C11 1.391(4) . ? C10 H10 0.9500 . ? C11 C12 1.387(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.390(4) . ? C14 C15 1.392(4) . ? C15 C16 1.393(4) . ? C15 H15 0.9500 . ? C16 C17 1.376(4) . ? C16 H16 0.9500 . ? C17 C18 1.391(4) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.393(4) . ? C20 C25 1.398(4) . ? C21 C22 1.399(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 C24 1.392(5) . ? C23 H23 0.9500 . ? C24 C25 1.389(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C28 C29 1.380(5) . ? C28 C30 1.384(5) 3_656 ? C28 H28 0.9500 . ? C29 C30 1.373(5) . ? C29 H29 0.9500 . ? C30 C28 1.384(5) 3_656 ? C30 H30 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 C27 88.28(10) . . ? O1 W1 Cl1 100.83(7) . . ? C27 W1 Cl1 170.83(8) . . ? O1 W1 Cl2 166.33(7) . . ? C27 W1 Cl2 78.18(8) . . ? Cl1 W1 Cl2 92.75(2) . . ? O1 W1 P1 98.88(7) . . ? C27 W1 P1 92.28(8) . . ? Cl1 W1 P1 87.37(2) . . ? Cl2 W1 P1 80.04(2) . . ? O1 W1 P2 101.43(7) . . ? C27 W1 P2 91.62(8) . . ? Cl1 W1 P2 85.61(2) . . ? Cl2 W1 P2 81.01(2) . . ? P1 W1 P2 159.42(2) . . ? C1 P1 C13 105.84(13) . . ? C1 P1 C7 105.01(13) . . ? C13 P1 C7 104.25(13) . . ? C1 P1 W1 114.21(9) . . ? C13 P1 W1 113.78(10) . . ? C7 P1 W1 112.83(9) . . ? C26 P2 C14 105.24(13) . . ? C26 P2 C20 103.94(13) . . ? C14 P2 C20 105.30(12) . . ? C26 P2 W1 112.55(10) . . ? C14 P2 W1 113.30(9) . . ? C20 P2 W1 115.51(9) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 P1 122.2(2) . . ? C6 C1 P1 118.7(2) . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.7(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.7(3) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 119.4(3) . . ? C8 C7 P1 122.7(2) . . ? C12 C7 P1 117.9(2) . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.9(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 120.3(3) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 118.8(3) . . ? C19 C14 P2 118.8(2) . . ? C15 C14 P2 122.2(2) . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C14 120.9(3) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? C21 C20 C25 119.2(3) . . ? C21 C20 P2 121.5(2) . . ? C25 C20 P2 119.2(2) . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C20 120.6(3) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C27 W1 178.6(3) . . ? C29 C28 C30 119.9(3) . 3_656 ? C29 C28 H28 120.1 . . ? C30 C28 H28 120.1 3_656 . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C28 119.9(3) . 3_656 ? C29 C30 H30 120.1 . . ? C28 C30 H30 120.1 3_656 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.963 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.112 #===END data_jpd196a_0m _database_code_depnum_ccdc_archive 'CCDC 769391' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 3c, [W(O)Cl2(PMePh2)3] _audit_creation_method SHELXL-97 _chemical_name_systematic ; mer-Oxodichlorotris(methyldiphenylphosphine)tungsten(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H39 Cl2 O P3 W' _chemical_formula_sum 'C39 H39 Cl2 O P3 W' _chemical_formula_weight 871.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8636(8) _cell_length_b 10.3088(9) _cell_length_c 18.7068(15) _cell_angle_alpha 78.530(1) _cell_angle_beta 83.485(1) _cell_angle_gamma 73.102(1) _cell_volume 1780.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2223 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.13 _exptl_crystal_description column _exptl_crystal_colour purple _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 3.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4462 _exptl_absorpt_correction_T_max 0.7470 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 10 sec/frame. From 1400 reflections chosen from the final data set and having I/\s(I) > 20 it was determined that the crystal consisted of two components with one of them being relatively minor (CELL_NOW (Sheldrick, 2007)). The data were integrated with the multi-component version of SAINT+ as directed by the 2-component control file generated by CELL_NOW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX I CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15955 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.00 _reflns_number_total 8508 _reflns_number_gt 7879 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2007)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2007)' _publ_section_references ; Bruker-AXS (2007). APEX2, Version 2.2.0, Madison, WI. Bruker-AXS (2006). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2005). CELL_NOW. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). TWINABS, Version 2007/5. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The final model was refined with the reflection file containing only contributions from the major component of the crystal as extracted by TWINABS. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.9568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8508 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.145175(9) 0.185418(9) 0.253662(5) 0.01267(3) Uani 1 1 d . . . Cl1 Cl 0.35370(6) -0.01499(6) 0.27901(3) 0.01867(12) Uani 1 1 d . . . Cl2 Cl 0.29273(6) 0.29952(6) 0.15924(3) 0.01859(12) Uani 1 1 d . . . P1 P 0.26200(6) 0.27034(6) 0.34334(3) 0.01477(12) Uani 1 1 d . . . P2 P -0.04809(6) 0.40556(6) 0.22242(3) 0.01401(12) Uani 1 1 d . . . P3 P 0.10943(6) 0.08016(6) 0.14750(3) 0.01447(12) Uani 1 1 d . . . O1 O 0.02393(17) 0.12274(17) 0.31308(9) 0.0178(3) Uani 1 1 d . . . C1 C 0.1938(3) 0.4458(2) 0.36283(13) 0.0167(5) Uani 1 1 d . . . C2 C 0.2640(3) 0.5466(3) 0.33703(15) 0.0250(6) Uani 1 1 d . . . H2 H 0.3528 0.5241 0.3102 0.030 Uiso 1 1 calc R . . C3 C 0.2046(3) 0.6807(3) 0.35045(17) 0.0323(7) Uani 1 1 d . . . H3 H 0.2542 0.7484 0.3336 0.039 Uiso 1 1 calc R . . C4 C 0.0743(3) 0.7151(3) 0.38802(16) 0.0326(7) Uani 1 1 d . . . H4 H 0.0330 0.8070 0.3960 0.039 Uiso 1 1 calc R . . C5 C 0.0039(3) 0.6157(3) 0.41398(16) 0.0318(7) Uani 1 1 d . . . H5 H -0.0858 0.6389 0.4401 0.038 Uiso 1 1 calc R . . C6 C 0.0640(3) 0.4820(3) 0.40200(14) 0.0243(6) Uani 1 1 d . . . H6 H 0.0157 0.4139 0.4209 0.029 Uiso 1 1 calc R . . C7 C 0.2671(3) 0.1656(2) 0.43496(13) 0.0178(5) Uani 1 1 d . . . C8 C 0.3468(3) 0.1849(3) 0.48734(14) 0.0250(6) Uani 1 1 d . . . H8 H 0.3968 0.2532 0.4753 0.030 Uiso 1 1 calc R . . C9 C 0.3535(3) 0.1053(3) 0.55681(15) 0.0300(6) Uani 1 1 d . . . H9 H 0.4098 0.1174 0.5916 0.036 Uiso 1 1 calc R . . C10 C 0.2775(3) 0.0081(3) 0.57520(15) 0.0287(6) Uani 1 1 d . . . H10 H 0.2804 -0.0453 0.6229 0.034 Uiso 1 1 calc R . . C11 C 0.1978(3) -0.0111(3) 0.52426(15) 0.0287(6) Uani 1 1 d . . . H11 H 0.1454 -0.0772 0.5372 0.034 Uiso 1 1 calc R . . C12 C 0.1938(3) 0.0660(3) 0.45400(14) 0.0244(6) Uani 1 1 d . . . H12 H 0.1406 0.0505 0.4189 0.029 Uiso 1 1 calc R . . C13 C 0.4479(3) 0.2569(3) 0.31527(14) 0.0216(5) Uani 1 1 d . . . H13A H 0.4920 0.2836 0.3524 0.032 Uiso 1 1 calc R . . H13B H 0.4543 0.3182 0.2685 0.032 Uiso 1 1 calc R . . H13C H 0.4973 0.1617 0.3099 0.032 Uiso 1 1 calc R . . C14 C -0.1887(3) 0.4524(2) 0.29379(13) 0.0174(5) Uani 1 1 d . . . C15 C -0.1966(3) 0.3699(3) 0.36193(14) 0.0239(5) Uani 1 1 d . . . H15 H -0.1293 0.2825 0.3725 0.029 Uiso 1 1 calc R . . C16 C -0.3022(3) 0.4145(3) 0.41476(15) 0.0286(6) Uani 1 1 d . . . H16 H -0.3058 0.3580 0.4613 0.034 Uiso 1 1 calc R . . C17 C -0.4019(3) 0.5407(3) 0.39973(16) 0.0275(6) Uani 1 1 d . . . H17 H -0.4729 0.5714 0.4361 0.033 Uiso 1 1 calc R . . C18 C -0.3979(3) 0.6225(3) 0.33125(16) 0.0255(6) Uani 1 1 d . . . H18 H -0.4673 0.7084 0.3204 0.031 Uiso 1 1 calc R . . C19 C -0.2930(3) 0.5787(3) 0.27898(14) 0.0221(5) Uani 1 1 d . . . H19 H -0.2913 0.6349 0.2322 0.027 Uiso 1 1 calc R . . C20 C -0.1591(2) 0.4181(2) 0.14774(13) 0.0165(5) Uani 1 1 d . . . C21 C -0.1421(3) 0.4937(3) 0.07816(14) 0.0212(5) Uani 1 1 d . . . H21 H -0.0776 0.5487 0.0695 0.025 Uiso 1 1 calc R . . C22 C -0.2194(3) 0.4886(3) 0.02156(15) 0.0274(6) Uani 1 1 d . . . H22 H -0.2059 0.5387 -0.0259 0.033 Uiso 1 1 calc R . . C23 C -0.3156(3) 0.4113(3) 0.03383(16) 0.0303(7) Uani 1 1 d . . . H23 H -0.3669 0.4070 -0.0052 0.036 Uiso 1 1 calc R . . C24 C -0.3372(3) 0.3398(3) 0.10355(17) 0.0285(6) Uani 1 1 d . . . H24 H -0.4061 0.2896 0.1125 0.034 Uiso 1 1 calc R . . C25 C -0.2585(3) 0.3416(3) 0.15976(15) 0.0211(5) Uani 1 1 d . . . H25 H -0.2720 0.2906 0.2069 0.025 Uiso 1 1 calc R . . C26 C 0.0116(3) 0.5607(2) 0.19665(15) 0.0208(5) Uani 1 1 d . . . H26A H 0.0859 0.5486 0.1571 0.031 Uiso 1 1 calc R . . H26B H 0.0497 0.5779 0.2390 0.031 Uiso 1 1 calc R . . H26C H -0.0685 0.6392 0.1801 0.031 Uiso 1 1 calc R . . C27 C -0.0501(2) 0.0214(2) 0.15837(14) 0.0172(5) Uani 1 1 d . . . C28 C -0.0947(3) -0.0376(3) 0.22743(14) 0.0226(5) Uani 1 1 d . . . H28 H -0.0406 -0.0486 0.2682 0.027 Uiso 1 1 calc R . . C29 C -0.2179(3) -0.0804(3) 0.23685(15) 0.0265(6) Uani 1 1 d . . . H29 H -0.2467 -0.1220 0.2839 0.032 Uiso 1 1 calc R . . C30 C -0.2989(3) -0.0627(3) 0.17806(16) 0.0281(6) Uani 1 1 d . . . H30 H -0.3848 -0.0890 0.1850 0.034 Uiso 1 1 calc R . . C31 C -0.2542(3) -0.0067(3) 0.10932(16) 0.0266(6) Uani 1 1 d . . . H31 H -0.3088 0.0040 0.0688 0.032 Uiso 1 1 calc R . . C32 C -0.1299(3) 0.0340(3) 0.09909(14) 0.0224(5) Uani 1 1 d . . . H32 H -0.0990 0.0706 0.0514 0.027 Uiso 1 1 calc R . . C33 C 0.2509(2) -0.0738(2) 0.13146(13) 0.0166(5) Uani 1 1 d . . . C34 C 0.2370(3) -0.2055(3) 0.15824(15) 0.0240(6) Uani 1 1 d . . . H34 H 0.1505 -0.2168 0.1831 0.029 Uiso 1 1 calc R . . C35 C 0.3490(3) -0.3212(3) 0.14890(16) 0.0277(6) Uani 1 1 d . . . H35 H 0.3392 -0.4109 0.1677 0.033 Uiso 1 1 calc R . . C36 C 0.4739(3) -0.3048(3) 0.11227(15) 0.0246(6) Uani 1 1 d . . . H36 H 0.5507 -0.3835 0.1064 0.029 Uiso 1 1 calc R . . C37 C 0.4878(3) -0.1751(3) 0.08418(16) 0.0256(6) Uani 1 1 d . . . H37 H 0.5732 -0.1647 0.0577 0.031 Uiso 1 1 calc R . . C38 C 0.3776(3) -0.0592(3) 0.09432(15) 0.0229(5) Uani 1 1 d . . . H38 H 0.3887 0.0301 0.0759 0.027 Uiso 1 1 calc R . . C39 C 0.1034(3) 0.1854(3) 0.05660(13) 0.0212(5) Uani 1 1 d . . . H39A H 0.1071 0.1283 0.0199 0.032 Uiso 1 1 calc R . . H39B H 0.1848 0.2241 0.0475 0.032 Uiso 1 1 calc R . . H39C H 0.0152 0.2604 0.0535 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01327(5) 0.01182(5) 0.01238(5) -0.00186(3) -0.00161(3) -0.00246(3) Cl1 0.0171(3) 0.0148(3) 0.0217(3) -0.0033(2) -0.0039(2) 0.0005(2) Cl2 0.0187(3) 0.0214(3) 0.0161(3) -0.0007(2) 0.0006(2) -0.0086(2) P1 0.0146(3) 0.0161(3) 0.0137(3) -0.0025(2) -0.0020(2) -0.0042(2) P2 0.0139(3) 0.0139(3) 0.0134(3) -0.0012(2) -0.0006(2) -0.0035(2) P3 0.0149(3) 0.0142(3) 0.0146(3) -0.0037(2) -0.0005(2) -0.0037(2) O1 0.0186(9) 0.0170(9) 0.0176(9) -0.0024(7) -0.0003(7) -0.0056(7) C1 0.0192(12) 0.0160(11) 0.0159(11) -0.0028(9) -0.0038(9) -0.0052(9) C2 0.0255(14) 0.0223(13) 0.0290(15) -0.0028(11) -0.0038(11) -0.0095(11) C3 0.0418(17) 0.0204(14) 0.0371(17) -0.0023(12) -0.0092(14) -0.0116(12) C4 0.0466(18) 0.0191(14) 0.0286(15) -0.0073(12) -0.0095(13) 0.0011(12) C5 0.0337(16) 0.0296(16) 0.0251(15) -0.0071(12) 0.0014(12) 0.0028(12) C6 0.0270(14) 0.0231(14) 0.0214(13) -0.0016(11) 0.0008(11) -0.0070(11) C7 0.0199(12) 0.0154(12) 0.0149(12) -0.0016(9) -0.0022(9) 0.0000(9) C8 0.0259(14) 0.0291(14) 0.0203(13) -0.0058(11) -0.0041(11) -0.0058(11) C9 0.0329(15) 0.0377(17) 0.0171(13) -0.0088(12) -0.0070(11) -0.0015(12) C10 0.0326(15) 0.0288(15) 0.0164(13) -0.0010(11) -0.0033(11) 0.0030(12) C11 0.0377(16) 0.0258(14) 0.0202(14) 0.0049(11) -0.0043(12) -0.0101(12) C12 0.0297(14) 0.0259(14) 0.0176(13) -0.0001(11) -0.0067(11) -0.0081(11) C13 0.0146(12) 0.0274(14) 0.0242(13) -0.0072(11) -0.0027(10) -0.0055(10) C14 0.0167(11) 0.0189(12) 0.0166(12) -0.0040(9) 0.0008(9) -0.0049(9) C15 0.0237(13) 0.0244(14) 0.0201(13) -0.0018(11) 0.0014(10) -0.0034(10) C16 0.0289(15) 0.0305(15) 0.0210(14) -0.0006(11) 0.0053(11) -0.0048(12) C17 0.0231(14) 0.0304(15) 0.0268(15) -0.0113(12) 0.0079(11) -0.0031(11) C18 0.0187(13) 0.0234(14) 0.0316(15) -0.0071(11) 0.0020(11) -0.0014(10) C19 0.0226(13) 0.0212(13) 0.0203(13) -0.0030(10) -0.0014(10) -0.0029(10) C20 0.0152(11) 0.0153(11) 0.0163(12) -0.0041(9) -0.0019(9) 0.0013(9) C21 0.0195(12) 0.0210(13) 0.0188(13) -0.0025(10) -0.0010(10) 0.0004(10) C22 0.0268(14) 0.0302(15) 0.0170(13) -0.0051(11) -0.0041(11) 0.0067(11) C23 0.0272(14) 0.0321(15) 0.0287(15) -0.0154(12) -0.0134(12) 0.0074(12) C24 0.0219(13) 0.0236(14) 0.0434(17) -0.0133(12) -0.0098(12) -0.0038(11) C25 0.0191(12) 0.0193(13) 0.0239(13) -0.0053(10) -0.0011(10) -0.0029(10) C26 0.0198(12) 0.0165(12) 0.0255(13) 0.0006(10) -0.0034(10) -0.0062(9) C27 0.0147(11) 0.0167(12) 0.0206(12) -0.0068(10) -0.0008(9) -0.0027(9) C28 0.0254(13) 0.0246(14) 0.0218(13) -0.0083(11) -0.0003(10) -0.0105(11) C29 0.0314(15) 0.0314(15) 0.0229(14) -0.0118(12) 0.0072(11) -0.0170(12) C30 0.0185(13) 0.0346(16) 0.0368(16) -0.0165(13) 0.0038(11) -0.0111(11) C31 0.0221(13) 0.0314(15) 0.0293(15) -0.0101(12) -0.0060(11) -0.0071(11) C32 0.0225(13) 0.0265(14) 0.0194(13) -0.0063(11) -0.0013(10) -0.0069(10) C33 0.0166(11) 0.0173(12) 0.0169(12) -0.0077(9) -0.0018(9) -0.0026(9) C34 0.0204(13) 0.0207(13) 0.0297(15) -0.0058(11) 0.0060(10) -0.0055(10) C35 0.0311(15) 0.0148(13) 0.0353(16) -0.0055(11) 0.0017(12) -0.0037(11) C36 0.0229(13) 0.0231(13) 0.0266(14) -0.0106(11) -0.0026(11) 0.0001(10) C37 0.0171(12) 0.0308(15) 0.0306(15) -0.0108(12) 0.0026(11) -0.0072(11) C38 0.0211(13) 0.0209(13) 0.0280(14) -0.0067(11) 0.0023(10) -0.0078(10) C39 0.0257(13) 0.0199(13) 0.0171(12) -0.0041(10) -0.0021(10) -0.0041(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.7161(17) . ? W1 Cl1 2.4668(6) . ? W1 Cl2 2.4915(6) . ? W1 P2 2.5172(6) . ? W1 P3 2.5463(6) . ? W1 P1 2.5530(6) . ? P1 C13 1.822(3) . ? P1 C1 1.832(2) . ? P1 C7 1.832(2) . ? P2 C26 1.821(2) . ? P2 C20 1.834(2) . ? P2 C14 1.840(2) . ? P3 C27 1.822(2) . ? P3 C39 1.823(3) . ? P3 C33 1.834(2) . ? C1 C6 1.390(4) . ? C1 C2 1.391(3) . ? C2 C3 1.397(4) . ? C2 H2 0.9500 . ? C3 C4 1.379(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.390(4) . ? C7 C8 1.400(3) . ? C8 C9 1.390(4) . ? C8 H8 0.9500 . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 C11 1.378(4) . ? C10 H10 0.9500 . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.392(3) . ? C14 C19 1.404(3) . ? C15 C16 1.394(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(4) . ? C16 H16 0.9500 . ? C17 C18 1.390(4) . ? C17 H17 0.9500 . ? C18 C19 1.381(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.398(3) . ? C20 C25 1.400(3) . ? C21 C22 1.390(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.392(4) . ? C23 H23 0.9500 . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.395(4) . ? C27 C32 1.395(3) . ? C28 C29 1.392(4) . ? C28 H28 0.9500 . ? C29 C30 1.384(4) . ? C29 H29 0.9500 . ? C30 C31 1.380(4) . ? C30 H30 0.9500 . ? C31 C32 1.390(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.391(4) . ? C33 C38 1.392(3) . ? C34 C35 1.395(4) . ? C34 H34 0.9500 . ? C35 C36 1.378(4) . ? C35 H35 0.9500 . ? C36 C37 1.376(4) . ? C36 H36 0.9500 . ? C37 C38 1.391(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 Cl1 97.99(6) . . ? O1 W1 Cl2 172.19(6) . . ? Cl1 W1 Cl2 89.46(2) . . ? O1 W1 P2 88.03(6) . . ? Cl1 W1 P2 173.54(2) . . ? Cl2 W1 P2 84.63(2) . . ? O1 W1 P3 95.26(6) . . ? Cl1 W1 P3 86.63(2) . . ? Cl2 W1 P3 82.77(2) . . ? P2 W1 P3 95.18(2) . . ? O1 W1 P1 99.25(6) . . ? Cl1 W1 P1 80.54(2) . . ? Cl2 W1 P1 84.24(2) . . ? P2 W1 P1 96.24(2) . . ? P3 W1 P1 161.80(2) . . ? C13 P1 C1 103.29(12) . . ? C13 P1 C7 104.15(12) . . ? C1 P1 C7 102.28(11) . . ? C13 P1 W1 111.09(9) . . ? C1 P1 W1 121.46(8) . . ? C7 P1 W1 112.79(8) . . ? C26 P2 C20 102.87(12) . . ? C26 P2 C14 102.16(12) . . ? C20 P2 C14 99.14(11) . . ? C26 P2 W1 115.22(8) . . ? C20 P2 W1 117.51(8) . . ? C14 P2 W1 117.34(8) . . ? C27 P3 C39 104.74(12) . . ? C27 P3 C33 103.10(11) . . ? C39 P3 C33 100.72(11) . . ? C27 P3 W1 114.30(8) . . ? C39 P3 W1 117.56(9) . . ? C33 P3 W1 114.52(8) . . ? C6 C1 C2 118.4(2) . . ? C6 C1 P1 119.12(19) . . ? C2 C1 P1 122.4(2) . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.2(3) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C12 C7 C8 118.7(2) . . ? C12 C7 P1 121.45(19) . . ? C8 C7 P1 119.9(2) . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 120.4(2) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 118.2(2) . . ? C15 C14 P2 123.52(19) . . ? C19 C14 P2 118.25(19) . . ? C14 C15 C16 120.6(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.8(2) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 119.9(2) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 121.1(2) . . ? C18 C19 H19 119.4 . . ? C14 C19 H19 119.4 . . ? C21 C20 C25 118.8(2) . . ? C21 C20 P2 122.54(19) . . ? C25 C20 P2 118.49(19) . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.9(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C20 120.5(3) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.8(2) . . ? C28 C27 P3 119.64(19) . . ? C32 C27 P3 121.6(2) . . ? C29 C28 C27 120.3(2) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 119.7(3) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.4(3) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C27 120.4(3) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C34 C33 C38 119.0(2) . . ? C34 C33 P3 121.49(19) . . ? C38 C33 P3 119.48(19) . . ? C33 C34 C35 120.5(2) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 120.3(2) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C33 120.1(2) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.770 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.094 #===END data_jpd203a_0m _database_code_depnum_ccdc_archive 'CCDC 769392' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 3e, [W(O)Cl2(dppe)(PMePh2)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; mer-Oxodichloro(1,2-bis(diphenylphosphino)ethane) (methyldiphenylphosphine)tungsten(IV) Dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 O P3 W, C H2 Cl2' _chemical_formula_sum 'C40 H39 Cl4 O P3 W' _chemical_formula_weight 954.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.532(2) _cell_length_b 14.265(1) _cell_length_c 25.620(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.896(1) _cell_angle_gamma 90.00 _cell_volume 8271.3(11) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9797 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.12 _exptl_crystal_description Plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 3.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6585 _exptl_absorpt_correction_T_max 0.7931 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 71260 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10263 _reflns_number_gt 8625 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2008)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2008.2-0, Madison, WI. Bruker-AXS (2006a. SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008). SADABS, Version 2008/2. University of G\"ottingen, Germany. Spek, A. L. (2007). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. In the final stages of refinement two isolated peaks of height 2-3 e/\%A^3^ were seen on the two-fold axes. As no reasonable model involving additional solvent of crystallization could be devised, ther were removed with the SQUEEZE option of the PLATON package (Spek, 2007). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+13.3580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10263 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.295359(5) 0.629367(7) 0.839638(4) 0.03129(4) Uani 1 1 d . . . Cl1 Cl 0.32694(4) 0.74240(5) 0.78136(3) 0.04220(16) Uani 1 1 d . . . Cl2 Cl 0.34995(3) 0.51051(5) 0.80095(3) 0.04035(16) Uani 1 1 d . . . P1 P 0.26906(3) 0.48095(5) 0.87715(3) 0.03421(15) Uani 1 1 d . . . P2 P 0.21090(3) 0.57717(5) 0.76167(3) 0.03459(15) Uani 1 1 d . . . P3 P 0.39116(3) 0.65549(5) 0.91164(3) 0.03481(16) Uani 1 1 d . . . O1 O 0.25527(9) 0.70061(14) 0.86968(8) 0.0395(5) Uani 1 1 d . . . C1 C 0.32630(13) 0.4046(2) 0.91809(11) 0.0382(6) Uani 1 1 d . . . C2 C 0.35507(14) 0.3377(2) 0.89485(13) 0.0447(7) Uani 1 1 d . . . H2 H 0.3438 0.3296 0.8566 0.054 Uiso 1 1 calc R . . C3 C 0.39946(16) 0.2832(2) 0.92659(15) 0.0547(9) Uani 1 1 d . . . H3 H 0.4184 0.2376 0.9101 0.066 Uiso 1 1 calc R . . C4 C 0.41674(15) 0.2943(3) 0.98207(15) 0.0560(9) Uani 1 1 d . . . H4 H 0.4472 0.2561 1.0039 0.067 Uiso 1 1 calc R . . C5 C 0.38951(16) 0.3612(3) 1.00586(14) 0.0573(10) Uani 1 1 d . . . H5 H 0.4017 0.3695 1.0441 0.069 Uiso 1 1 calc R . . C6 C 0.34447(14) 0.4164(2) 0.97428(12) 0.0459(7) Uani 1 1 d . . . H6 H 0.3260 0.4622 0.9910 0.055 Uiso 1 1 calc R . . C7 C 0.21407(13) 0.4844(2) 0.91614(11) 0.0406(7) Uani 1 1 d . . . C8 C 0.20035(16) 0.4011(3) 0.93821(13) 0.0524(8) Uani 1 1 d . . . H8 H 0.2216 0.3455 0.9354 0.063 Uiso 1 1 calc R . . C9 C 0.15567(18) 0.3985(3) 0.96437(15) 0.0627(10) Uani 1 1 d . . . H9 H 0.1465 0.3415 0.9794 0.075 Uiso 1 1 calc R . . C10 C 0.12491(18) 0.4788(3) 0.96823(16) 0.0691(12) Uani 1 1 d . . . H10 H 0.0944 0.4772 0.9860 0.083 Uiso 1 1 calc R . . C11 C 0.13800(18) 0.5616(3) 0.94658(17) 0.0688(11) Uani 1 1 d . . . H11 H 0.1166 0.6170 0.9494 0.083 Uiso 1 1 calc R . . C12 C 0.18260(15) 0.5642(3) 0.92054(14) 0.0533(8) Uani 1 1 d . . . H12 H 0.1915 0.6216 0.9056 0.064 Uiso 1 1 calc R . . C13 C 0.22940(13) 0.4079(2) 0.81915(11) 0.0376(6) Uani 1 1 d . . . H13A H 0.2573 0.3846 0.7994 0.045 Uiso 1 1 calc R . . H13B H 0.2115 0.3531 0.8323 0.045 Uiso 1 1 calc R . . C14 C 0.18141(13) 0.4668(2) 0.78134(11) 0.0386(6) Uani 1 1 d . . . H14A H 0.1505 0.4814 0.7996 0.046 Uiso 1 1 calc R . . H14B H 0.1628 0.4300 0.7483 0.046 Uiso 1 1 calc R . . C15 C 0.14713(14) 0.6557(2) 0.74357(12) 0.0402(7) Uani 1 1 d . . . C16 C 0.15172(15) 0.7475(2) 0.76124(13) 0.0457(7) Uani 1 1 d . . . H16 H 0.1882 0.7704 0.7837 0.055 Uiso 1 1 calc R . . C17 C 0.10275(16) 0.8067(2) 0.74610(14) 0.0526(8) Uani 1 1 d . . . H17 H 0.1059 0.8698 0.7584 0.063 Uiso 1 1 calc R . . C18 C 0.05053(17) 0.7746(3) 0.71386(15) 0.0600(10) Uani 1 1 d . . . H18 H 0.0174 0.8154 0.7036 0.072 Uiso 1 1 calc R . . C19 C 0.04550(18) 0.6839(3) 0.69624(17) 0.0734(12) Uani 1 1 d . . . H19 H 0.0088 0.6618 0.6739 0.088 Uiso 1 1 calc R . . C20 C 0.09342(17) 0.6241(3) 0.71064(16) 0.0644(10) Uani 1 1 d . . . H20 H 0.0896 0.5612 0.6980 0.077 Uiso 1 1 calc R . . C21 C 0.22510(13) 0.5533(2) 0.69635(10) 0.0359(6) Uani 1 1 d . . . C22 C 0.22662(18) 0.6278(2) 0.66170(13) 0.0521(8) Uani 1 1 d . . . H22 H 0.2203 0.6900 0.6721 0.062 Uiso 1 1 calc R . . C23 C 0.23743(19) 0.6109(3) 0.61198(14) 0.0594(10) Uani 1 1 d . . . H23 H 0.2378 0.6616 0.5881 0.071 Uiso 1 1 calc R . . C24 C 0.24757(17) 0.5211(3) 0.59696(13) 0.0540(9) Uani 1 1 d . . . H24 H 0.2548 0.5100 0.5628 0.065 Uiso 1 1 calc R . . C25 C 0.24721(15) 0.4475(2) 0.63161(12) 0.0492(8) Uani 1 1 d . . . H25 H 0.2551 0.3858 0.6215 0.059 Uiso 1 1 calc R . . C26 C 0.23549(14) 0.4627(2) 0.68106(12) 0.0419(7) Uani 1 1 d . . . H26 H 0.2346 0.4114 0.7045 0.050 Uiso 1 1 calc R . . C27 C 0.38554(14) 0.6585(2) 0.98147(11) 0.0398(6) Uani 1 1 d . . . C28 C 0.43476(17) 0.6429(3) 1.02479(14) 0.0671(12) Uani 1 1 d . . . H28 H 0.4719 0.6298 1.0184 0.081 Uiso 1 1 calc R . . C29 C 0.4299(2) 0.6466(4) 1.07785(15) 0.0891(16) Uani 1 1 d . . . H29 H 0.4638 0.6357 1.1074 0.107 Uiso 1 1 calc R . . C30 C 0.3770(2) 0.6657(3) 1.08761(14) 0.0731(12) Uani 1 1 d . . . H30 H 0.3742 0.6681 1.1239 0.088 Uiso 1 1 calc R . . C31 C 0.32795(17) 0.6815(3) 1.04539(13) 0.0557(9) Uani 1 1 d . . . H31 H 0.2912 0.6954 1.0523 0.067 Uiso 1 1 calc R . . C32 C 0.33206(15) 0.6772(2) 0.99222(12) 0.0465(7) Uani 1 1 d . . . H32 H 0.2978 0.6873 0.9630 0.056 Uiso 1 1 calc R . . C33 C 0.42610(13) 0.7677(2) 0.90605(11) 0.0385(6) Uani 1 1 d . . . C34 C 0.47506(16) 0.7760(3) 0.88684(16) 0.0585(9) Uani 1 1 d . . . H34 H 0.4936 0.7214 0.8779 0.070 Uiso 1 1 calc R . . C35 C 0.49759(19) 0.8643(3) 0.8804(2) 0.0741(13) Uani 1 1 d . . . H35 H 0.5315 0.8693 0.8672 0.089 Uiso 1 1 calc R . . C36 C 0.47174(18) 0.9432(3) 0.89269(16) 0.0647(11) Uani 1 1 d . . . H36 H 0.4882 1.0029 0.8893 0.078 Uiso 1 1 calc R . . C37 C 0.4218(2) 0.9364(3) 0.91005(16) 0.0689(11) Uani 1 1 d . . . H37 H 0.4025 0.9915 0.9172 0.083 Uiso 1 1 calc R . . C38 C 0.39951(19) 0.8484(2) 0.91721(16) 0.0599(10) Uani 1 1 d . . . H38 H 0.3653 0.8439 0.9300 0.072 Uiso 1 1 calc R . . C39 C 0.44841(14) 0.5686(2) 0.91304(14) 0.0485(8) Uani 1 1 d . . . H39A H 0.4548 0.5637 0.8769 0.073 Uiso 1 1 calc R . . H39B H 0.4360 0.5076 0.9237 0.073 Uiso 1 1 calc R . . H39C H 0.4853 0.5879 0.9393 0.073 Uiso 1 1 calc R . . C40 C 0.6077(3) 0.6206(3) 0.8055(2) 0.0931(17) Uani 1 1 d . . . H40A H 0.5911 0.6421 0.7677 0.112 Uiso 1 1 calc R . . H40B H 0.6464 0.5909 0.8082 0.112 Uiso 1 1 calc R . . Cl3 Cl 0.61779(7) 0.71781(11) 0.84971(7) 0.1176(6) Uani 1 1 d . . . Cl4 Cl 0.56205(10) 0.54156(11) 0.82092(10) 0.1609(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.04189(7) 0.02851(6) 0.02527(6) -0.00116(4) 0.01222(4) -0.00089(5) Cl1 0.0602(4) 0.0340(4) 0.0357(3) 0.0057(3) 0.0188(3) -0.0008(3) Cl2 0.0571(4) 0.0345(3) 0.0350(3) -0.0004(3) 0.0220(3) 0.0046(3) P1 0.0465(4) 0.0328(4) 0.0252(3) -0.0007(3) 0.0130(3) -0.0045(3) P2 0.0447(4) 0.0335(4) 0.0264(3) -0.0022(3) 0.0112(3) 0.0014(3) P3 0.0395(4) 0.0369(4) 0.0298(3) 0.0005(3) 0.0123(3) -0.0021(3) O1 0.0471(11) 0.0387(11) 0.0339(10) -0.0049(8) 0.0134(9) -0.0012(9) C1 0.0468(16) 0.0348(15) 0.0337(14) 0.0051(12) 0.0121(12) -0.0072(13) C2 0.0550(19) 0.0377(16) 0.0417(16) 0.0037(13) 0.0138(14) -0.0030(14) C3 0.060(2) 0.0456(19) 0.059(2) 0.0098(16) 0.0168(17) -0.0012(16) C4 0.0487(19) 0.056(2) 0.060(2) 0.0206(18) 0.0081(16) -0.0054(16) C5 0.056(2) 0.069(2) 0.0409(18) 0.0167(17) 0.0045(15) -0.0188(18) C6 0.0534(18) 0.0482(18) 0.0357(15) 0.0035(13) 0.0114(14) -0.0095(15) C7 0.0482(17) 0.0479(18) 0.0283(14) -0.0058(12) 0.0149(12) -0.0133(14) C8 0.064(2) 0.055(2) 0.0415(17) 0.0006(15) 0.0205(16) -0.0167(17) C9 0.071(2) 0.076(3) 0.048(2) -0.0019(19) 0.0271(18) -0.030(2) C10 0.064(2) 0.094(3) 0.060(2) -0.016(2) 0.0353(19) -0.031(2) C11 0.062(2) 0.081(3) 0.075(3) -0.019(2) 0.038(2) -0.011(2) C12 0.060(2) 0.057(2) 0.0513(19) -0.0095(16) 0.0299(17) -0.0097(17) C13 0.0532(17) 0.0329(14) 0.0288(13) -0.0028(11) 0.0147(12) -0.0071(13) C14 0.0481(16) 0.0394(16) 0.0291(13) -0.0055(12) 0.0118(12) -0.0056(13) C15 0.0476(16) 0.0427(16) 0.0329(14) -0.0009(12) 0.0153(12) 0.0062(13) C16 0.0567(19) 0.0415(17) 0.0424(17) 0.0035(13) 0.0195(14) 0.0030(15) C17 0.071(2) 0.0433(18) 0.054(2) 0.0122(15) 0.0344(18) 0.0142(17) C18 0.057(2) 0.075(3) 0.053(2) 0.0141(19) 0.0241(17) 0.0252(19) C19 0.055(2) 0.085(3) 0.071(3) -0.011(2) 0.0014(19) 0.015(2) C20 0.060(2) 0.063(2) 0.062(2) -0.0193(19) 0.0039(18) 0.0084(19) C21 0.0435(15) 0.0402(16) 0.0244(12) -0.0037(11) 0.0101(11) 0.0002(12) C22 0.085(2) 0.0357(17) 0.0390(17) 0.0015(13) 0.0224(17) 0.0028(16) C23 0.097(3) 0.048(2) 0.0410(18) 0.0111(15) 0.0321(19) 0.0050(19) C24 0.076(2) 0.056(2) 0.0371(17) -0.0005(15) 0.0276(16) 0.0029(18) C25 0.070(2) 0.0440(18) 0.0384(16) -0.0034(14) 0.0224(16) 0.0077(16) C26 0.0574(18) 0.0376(16) 0.0336(15) 0.0008(12) 0.0175(13) 0.0031(14) C27 0.0469(16) 0.0427(16) 0.0305(14) -0.0005(12) 0.0120(12) -0.0107(13) C28 0.051(2) 0.113(4) 0.0361(17) 0.0102(19) 0.0089(15) -0.010(2) C29 0.074(3) 0.158(5) 0.0292(18) 0.016(2) 0.0029(18) -0.017(3) C30 0.094(3) 0.100(3) 0.0285(17) 0.0041(19) 0.0220(19) -0.020(3) C31 0.071(2) 0.064(2) 0.0400(18) 0.0008(16) 0.0297(17) -0.0007(19) C32 0.0582(19) 0.0489(19) 0.0343(15) -0.0001(14) 0.0161(14) 0.0008(15) C33 0.0434(16) 0.0431(16) 0.0292(13) 0.0020(12) 0.0104(12) -0.0083(13) C34 0.056(2) 0.055(2) 0.071(2) 0.0146(18) 0.0293(18) 0.0001(17) C35 0.058(2) 0.072(3) 0.099(3) 0.031(2) 0.034(2) -0.009(2) C36 0.072(3) 0.053(2) 0.061(2) 0.0116(18) 0.005(2) -0.022(2) C37 0.102(3) 0.045(2) 0.066(2) -0.0019(18) 0.033(2) -0.009(2) C38 0.080(3) 0.044(2) 0.067(2) -0.0038(17) 0.039(2) -0.0078(18) C39 0.0443(17) 0.0450(18) 0.0561(19) 0.0000(15) 0.0135(15) 0.0030(14) C40 0.112(4) 0.094(4) 0.096(4) -0.038(3) 0.067(3) -0.031(3) Cl3 0.1349(12) 0.1138(11) 0.1362(13) -0.0554(10) 0.0916(11) -0.0292(9) Cl4 0.224(2) 0.0839(10) 0.244(2) -0.0253(12) 0.182(2) -0.0402(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.707(2) . ? W1 Cl1 2.4474(7) . ? W1 P1 2.4729(7) . ? W1 Cl2 2.4910(7) . ? W1 P2 2.5140(7) . ? W1 P3 2.5191(8) . ? P1 C1 1.824(3) . ? P1 C7 1.839(3) . ? P1 C13 1.845(3) . ? P2 C21 1.826(3) . ? P2 C15 1.828(3) . ? P2 C14 1.846(3) . ? P3 C33 1.822(3) . ? P3 C39 1.824(3) . ? P3 C27 1.830(3) . ? C1 C6 1.395(4) . ? C1 C2 1.395(4) . ? C2 C3 1.375(5) . ? C2 H2 0.9500 . ? C3 C4 1.376(5) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.389(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.379(5) . ? C7 C8 1.392(4) . ? C8 C9 1.393(5) . ? C8 H8 0.9500 . ? C9 C10 1.373(6) . ? C9 H9 0.9500 . ? C10 C11 1.375(6) . ? C10 H10 0.9500 . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.523(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.380(4) . ? C15 C20 1.388(5) . ? C16 C17 1.395(4) . ? C16 H16 0.9500 . ? C17 C18 1.359(5) . ? C17 H17 0.9500 . ? C18 C19 1.365(6) . ? C18 H18 0.9500 . ? C19 C20 1.381(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.391(4) . ? C21 C26 1.392(4) . ? C22 C23 1.387(5) . ? C22 H22 0.9500 . ? C23 C24 1.376(5) . ? C23 H23 0.9500 . ? C24 C25 1.377(5) . ? C24 H24 0.9500 . ? C25 C26 1.385(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.385(5) . ? C27 C32 1.386(4) . ? C28 C29 1.396(5) . ? C28 H28 0.9500 . ? C29 C30 1.363(6) . ? C29 H29 0.9500 . ? C30 C31 1.367(5) . ? C30 H30 0.9500 . ? C31 C32 1.393(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.376(4) . ? C33 C38 1.378(5) . ? C34 C35 1.394(5) . ? C34 H34 0.9500 . ? C35 C36 1.357(6) . ? C35 H35 0.9500 . ? C36 C37 1.369(6) . ? C36 H36 0.9500 . ? C37 C38 1.392(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 Cl4 1.677(5) . ? C40 Cl3 1.764(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 Cl1 100.40(7) . . ? O1 W1 P1 96.11(7) . . ? Cl1 W1 P1 162.05(2) . . ? O1 W1 Cl2 173.59(7) . . ? Cl1 W1 Cl2 85.97(3) . . ? P1 W1 Cl2 77.48(2) . . ? O1 W1 P2 96.91(7) . . ? Cl1 W1 P2 90.94(3) . . ? P1 W1 P2 80.08(2) . . ? Cl2 W1 P2 82.17(3) . . ? O1 W1 P3 94.36(7) . . ? Cl1 W1 P3 89.37(3) . . ? P1 W1 P3 96.38(2) . . ? Cl2 W1 P3 86.36(3) . . ? P2 W1 P3 168.47(2) . . ? C1 P1 C7 102.86(14) . . ? C1 P1 C13 104.90(14) . . ? C7 P1 C13 100.19(13) . . ? C1 P1 W1 120.69(10) . . ? C7 P1 W1 118.43(11) . . ? C13 P1 W1 107.20(9) . . ? C21 P2 C15 103.02(13) . . ? C21 P2 C14 105.55(13) . . ? C15 P2 C14 104.37(14) . . ? C21 P2 W1 118.70(10) . . ? C15 P2 W1 115.82(10) . . ? C14 P2 W1 108.07(9) . . ? C33 P3 C39 104.55(15) . . ? C33 P3 C27 102.20(13) . . ? C39 P3 C27 104.32(16) . . ? C33 P3 W1 113.88(10) . . ? C39 P3 W1 114.97(11) . . ? C27 P3 W1 115.44(10) . . ? C6 C1 C2 118.4(3) . . ? C6 C1 P1 119.4(2) . . ? C2 C1 P1 122.1(2) . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 118.8(3) . . ? C12 C7 P1 122.7(2) . . ? C8 C7 P1 118.2(3) . . ? C7 C8 C9 120.5(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 120.7(4) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 P1 108.9(2) . . ? C14 C13 H13A 109.9 . . ? P1 C13 H13A 109.9 . . ? C14 C13 H13B 109.9 . . ? P1 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C13 C14 P2 112.0(2) . . ? C13 C14 H14A 109.2 . . ? P2 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? P2 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C20 118.9(3) . . ? C16 C15 P2 120.9(3) . . ? C20 C15 P2 120.2(3) . . ? C15 C16 C17 119.9(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.2(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 120.2(4) . . ? C19 C20 H20 119.9 . . ? C15 C20 H20 119.9 . . ? C22 C21 C26 119.5(3) . . ? C22 C21 P2 119.1(2) . . ? C26 C21 P2 121.4(2) . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 119.8(3) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C28 C27 C32 118.5(3) . . ? C28 C27 P3 120.7(3) . . ? C32 C27 P3 120.7(2) . . ? C27 C28 C29 120.1(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.6(4) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.2(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C27 C32 C31 120.8(3) . . ? C27 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C38 118.3(3) . . ? C34 C33 P3 122.9(3) . . ? C38 C33 P3 118.5(2) . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.9(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 119.7(4) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 119.6(4) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C33 C38 C37 121.2(4) . . ? C33 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Cl4 C40 Cl3 111.1(3) . . ? Cl4 C40 H40A 109.4 . . ? Cl3 C40 H40A 109.4 . . ? Cl4 C40 H40B 109.4 . . ? Cl3 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.863 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.075 #===END data_jpd289_0m _database_code_depnum_ccdc_archive 'CCDC 769393' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 4a, trans-[WCl4(PMe3)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Tetrachlprobis(trimethylphosphine)tungsten(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Cl4 P2 W' _chemical_formula_sum 'C6 H18 Cl4 P2 W' _chemical_formula_weight 477.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.5351(6) _cell_length_b 8.4615(8) _cell_length_c 13.3258(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.7170(10) _cell_angle_gamma 90.00 _cell_volume 726.30(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8602 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 28.71 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 8.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2564 _exptl_absorpt_correction_T_max 0.3189 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 10 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12445 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 28.71 _reflns_number_total 1869 _reflns_number_gt 1720 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.3-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.7309P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0085(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1869 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.0000 0.0000 0.0000 0.01776(10) Uani 1 2 d S . . Cl1 Cl 0.25088(14) -0.00120(6) -0.10352(7) 0.02407(18) Uani 1 1 d . . . Cl2 Cl -0.18072(10) 0.19969(8) -0.10217(5) 0.01853(14) Uani 1 1 d . . . P1 P 0.18730(10) 0.21874(8) 0.10991(5) 0.01394(14) Uani 1 1 d . . . C1 C 0.3717(4) 0.3285(3) 0.04911(19) 0.0222(5) Uani 1 1 d . . . H1A H 0.4308 0.4149 0.0938 0.033 Uiso 1 1 calc R . . H1B H 0.3007 0.3721 -0.0156 0.033 Uiso 1 1 calc R . . H1C H 0.4832 0.2577 0.0363 0.033 Uiso 1 1 calc R . . C2 C 0.3316(4) 0.1562(3) 0.23148(18) 0.0215(5) Uani 1 1 d . . . H2A H 0.4404 0.0817 0.2203 0.032 Uiso 1 1 calc R . . H2B H 0.2374 0.1044 0.2712 0.032 Uiso 1 1 calc R . . H2C H 0.3952 0.2485 0.2688 0.032 Uiso 1 1 calc R . . C3 C 0.0088(4) 0.3675(3) 0.14187(19) 0.0214(5) Uani 1 1 d . . . H3A H -0.0818 0.3205 0.1853 0.032 Uiso 1 1 calc R . . H3B H -0.0758 0.4077 0.0793 0.032 Uiso 1 1 calc R . . H3C H 0.0876 0.4548 0.1782 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02070(13) 0.01214(12) 0.01700(13) 0.00059(4) -0.00674(7) 0.00168(4) Cl1 0.0223(4) 0.0258(4) 0.0246(4) 0.00190(18) 0.0055(3) 0.00221(18) Cl2 0.0194(3) 0.0169(3) 0.0178(3) 0.0039(2) -0.0014(2) 0.0044(2) P1 0.0137(3) 0.0136(3) 0.0139(3) 0.0007(2) 0.0008(2) -0.0005(2) C1 0.0226(12) 0.0208(11) 0.0247(13) 0.0019(9) 0.0081(10) -0.0018(9) C2 0.0224(12) 0.0222(11) 0.0177(11) 0.0022(8) -0.0028(9) -0.0021(9) C3 0.0227(12) 0.0183(10) 0.0232(12) -0.0031(9) 0.0042(9) 0.0023(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl1 2.3140(8) . ? W1 Cl1 2.3141(8) 3 ? W1 Cl2 2.3581(6) 3 ? W1 Cl2 2.3581(6) . ? W1 P1 2.5424(7) 3 ? W1 P1 2.5424(7) . ? P1 C2 1.811(2) . ? P1 C3 1.815(2) . ? P1 C1 1.817(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 W1 Cl1 180.0 . 3 ? Cl1 W1 Cl2 90.28(2) . 3 ? Cl1 W1 Cl2 89.72(2) 3 3 ? Cl1 W1 Cl2 89.72(2) . . ? Cl1 W1 Cl2 90.28(2) 3 . ? Cl2 W1 Cl2 180.0 3 . ? Cl1 W1 P1 88.51(2) . 3 ? Cl1 W1 P1 91.49(2) 3 3 ? Cl2 W1 P1 87.51(3) 3 3 ? Cl2 W1 P1 92.49(3) . 3 ? Cl1 W1 P1 91.49(2) . . ? Cl1 W1 P1 88.51(2) 3 . ? Cl2 W1 P1 92.49(3) 3 . ? Cl2 W1 P1 87.51(3) . . ? P1 W1 P1 180.0 3 . ? C2 P1 C3 104.56(12) . . ? C2 P1 C1 105.30(12) . . ? C3 P1 C1 104.54(12) . . ? C2 P1 W1 115.46(8) . . ? C3 P1 W1 111.97(8) . . ? C1 P1 W1 113.97(8) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.71 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.942 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.143 #===END data_jpd251 _database_code_depnum_ccdc_archive 'CCDC 769394' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 4b, trans-[WCl4(PMe2Ph)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Tetrachlorobis(dimethylphenylphosphine) tungsten(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H22 Cl4 P2 W' _chemical_formula_sum 'C16 H22 Cl4 P2 W' _chemical_formula_weight 601.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.644(1) _cell_length_b 13.781(2) _cell_length_c 8.203(1) _cell_angle_alpha 90.00 _cell_angle_beta 106.744(2) _cell_angle_gamma 90.00 _cell_volume 1044.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9911 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 29.16 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 6.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4969 _exptl_absorpt_correction_T_max 0.5792 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18282 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.98 _reflns_number_total 2740 _reflns_number_gt 2461 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008b)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008b)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2008.2-0, Madison, WI. Bruker-AXS (2008a). SAINT, Version 7.53A, Madison, WI Bruker-AXS (2008b). SHELXTL, Version 2008/3, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+0.7916P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2740 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0178 _refine_ls_R_factor_gt 0.0146 _refine_ls_wR_factor_ref 0.0351 _refine_ls_wR_factor_gt 0.0336 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 1.0000 0.0000 0.5000 0.01217(4) Uani 1 2 d S . . Cl1 Cl 0.87390(5) 0.06114(3) 0.68370(6) 0.01804(9) Uani 1 1 d . . . Cl2 Cl 1.14428(5) 0.13965(3) 0.54379(6) 0.01877(9) Uani 1 1 d . . . P1 P 0.82877(5) 0.07603(4) 0.23408(6) 0.01461(9) Uani 1 1 d . . . C1 C 0.66681(19) 0.13209(14) 0.2619(2) 0.0154(4) Uani 1 1 d . . . C2 C 0.5717(2) 0.07350(14) 0.3181(2) 0.0187(4) Uani 1 1 d . . . H2 H 0.5942 0.0070 0.3424 0.022 Uiso 1 1 calc R . . C3 C 0.4447(2) 0.11147(16) 0.3389(3) 0.0215(4) Uani 1 1 d . . . H3 H 0.3796 0.0707 0.3749 0.026 Uiso 1 1 calc R . . C4 C 0.4128(2) 0.20894(16) 0.3070(3) 0.0235(4) Uani 1 1 d . . . H4 H 0.3262 0.2353 0.3219 0.028 Uiso 1 1 calc R . . C5 C 0.5073(2) 0.26789(16) 0.2533(3) 0.0255(4) Uani 1 1 d . . . H5 H 0.4856 0.3348 0.2324 0.031 Uiso 1 1 calc R . . C6 C 0.6342(2) 0.22989(15) 0.2297(3) 0.0201(4) Uani 1 1 d . . . H6 H 0.6981 0.2706 0.1917 0.024 Uiso 1 1 calc R . . C8 C 0.7584(3) -0.01209(15) 0.0649(3) 0.0237(4) Uani 1 1 d . . . H8A H 0.6991 0.0213 -0.0369 0.035 Uiso 1 1 calc R . . H8B H 0.6990 -0.0600 0.1023 0.035 Uiso 1 1 calc R . . H8C H 0.8392 -0.0450 0.0381 0.035 Uiso 1 1 calc R . . C7 C 0.9160(2) 0.16715(15) 0.1379(3) 0.0228(4) Uani 1 1 d . . . H7A H 0.8479 0.1899 0.0315 0.034 Uiso 1 1 calc R . . H7B H 1.0012 0.1389 0.1138 0.034 Uiso 1 1 calc R . . H7C H 0.9459 0.2219 0.2164 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01104(5) 0.01225(6) 0.01387(6) -0.00059(4) 0.00465(4) 0.00035(3) Cl1 0.0177(2) 0.0194(2) 0.0198(2) -0.00244(17) 0.00980(17) 0.00163(17) Cl2 0.0174(2) 0.0162(2) 0.0235(2) -0.00246(17) 0.00721(18) -0.00441(16) P1 0.0137(2) 0.0164(2) 0.0144(2) 0.00090(18) 0.00521(18) 0.00076(17) C1 0.0132(8) 0.0168(9) 0.0152(9) -0.0002(7) 0.0027(7) 0.0006(7) C2 0.0191(9) 0.0169(9) 0.0205(9) 0.0010(7) 0.0062(7) -0.0006(7) C3 0.0159(9) 0.0303(11) 0.0191(9) 0.0018(8) 0.0062(8) -0.0024(8) C4 0.0167(9) 0.0330(11) 0.0219(10) 0.0060(9) 0.0074(8) 0.0080(8) C5 0.0259(11) 0.0242(10) 0.0279(11) 0.0073(9) 0.0102(9) 0.0086(9) C6 0.0198(9) 0.0198(9) 0.0213(10) 0.0047(8) 0.0072(8) 0.0028(7) C8 0.0250(10) 0.0285(11) 0.0165(9) -0.0050(8) 0.0044(8) 0.0017(8) C7 0.0205(9) 0.0252(10) 0.0256(10) 0.0086(8) 0.0113(8) 0.0017(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl2 2.3411(5) . ? W1 Cl2 2.3411(5) 3_756 ? W1 Cl1 2.3486(5) . ? W1 Cl1 2.3486(5) 3_756 ? W1 P1 2.5510(5) . ? W1 P1 2.5510(5) 3_756 ? P1 C7 1.814(2) . ? P1 C1 1.8150(19) . ? P1 C8 1.822(2) . ? C1 C6 1.392(3) . ? C1 C2 1.397(3) . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 W1 Cl2 180.0 . 3_756 ? Cl2 W1 Cl1 90.078(17) . . ? Cl2 W1 Cl1 89.924(18) 3_756 . ? Cl2 W1 Cl1 89.922(18) . 3_756 ? Cl2 W1 Cl1 90.076(17) 3_756 3_756 ? Cl1 W1 Cl1 180.00(2) . 3_756 ? Cl2 W1 P1 90.188(17) . . ? Cl2 W1 P1 89.812(17) 3_756 . ? Cl1 W1 P1 94.244(18) . . ? Cl1 W1 P1 85.757(18) 3_756 . ? Cl2 W1 P1 89.812(17) . 3_756 ? Cl2 W1 P1 90.188(17) 3_756 3_756 ? Cl1 W1 P1 85.756(18) . 3_756 ? Cl1 W1 P1 94.244(18) 3_756 3_756 ? P1 W1 P1 180.0 . 3_756 ? C7 P1 C1 106.49(9) . . ? C7 P1 C8 104.33(11) . . ? C1 P1 C8 103.56(10) . . ? C7 P1 W1 112.91(7) . . ? C1 P1 W1 115.83(6) . . ? C8 P1 W1 112.65(7) . . ? C6 C1 C2 119.25(17) . . ? C6 C1 P1 122.94(15) . . ? C2 C1 P1 117.82(14) . . ? C3 C2 C1 120.66(18) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 119.87(19) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.90(19) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 119.75(19) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? P1 C8 H8A 109.5 . . ? P1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.98 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.632 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.085 #===END data_jpd154 _database_code_depnum_ccdc_archive 'CCDC 769395' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 4c, trans-[WCl4(PMePh2)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Bis(diphenylmethylphosphine)tungsten(IV) tetrachloride ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Cl4 P2 W' _chemical_formula_weight 726.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.860(3) _cell_length_b 9.491(3) _cell_length_c 9.765(3) _cell_angle_alpha 66.983(4) _cell_angle_beta 89.510(4) _cell_angle_gamma 63.041(4) _cell_volume 659.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6029 _cell_measurement_theta_min 2.316 _cell_measurement_theta_max 28.2885 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 354 _exptl_absorpt_coefficient_mu 4.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3896 _exptl_absorpt_correction_T_max 0.4711 _exptl_absorpt_process_details 'SADABS (Sheldrick 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 606 frames, each of width 0.3 deg. in \w, collected at \f = 0.00, 120.00 and 240.00 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6008 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3047 _reflns_number_gt 3047 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008b)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008b)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2008.2-0, Madison, WI. Bruker-AXS (2008a). SAINT, Version 7.53A, Madison, WI Bruker-AXS (2008b). SHELXTL, Version 2008/3, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.2164P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3047 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0152 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0388 _refine_ls_wR_factor_gt 0.0388 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.5000 0.0000 1.0000 0.00867(4) Uani 1 2 d S . . Cl1 Cl 0.27372(5) 0.27992(6) 0.94772(5) 0.01276(9) Uani 1 1 d . . . Cl2 Cl 0.32611(6) -0.03126(6) 0.84662(5) 0.01435(9) Uani 1 1 d . . . P1 P 0.39775(6) -0.14436(6) 1.23487(5) 0.00958(9) Uani 1 1 d . . . C1 C 0.5735(3) -0.2843(3) 1.4009(2) 0.0143(4) Uani 1 1 d . . . H1A H 0.621(3) -0.219(4) 1.420(3) 0.020(7) Uiso 1 1 d . . . H1B H 0.539(4) -0.348(4) 1.489(3) 0.025(7) Uiso 1 1 d . . . H1C H 0.666(4) -0.369(4) 1.377(3) 0.031(8) Uiso 1 1 d . . . C2 C 0.3235(2) -0.2921(2) 1.2262(2) 0.0120(3) Uani 1 1 d . . . C3 C 0.4279(3) -0.4235(3) 1.1822(2) 0.0154(4) Uani 1 1 d . . . H3 H 0.532(4) -0.422(4) 1.147(3) 0.023(7) Uiso 1 1 d . . . C4 C 0.3767(3) -0.5401(3) 1.1771(2) 0.0173(4) Uani 1 1 d . . . H4 H 0.453(3) -0.629(4) 1.151(3) 0.019(6) Uiso 1 1 d . . . C5 C 0.2203(3) -0.5267(3) 1.2143(2) 0.0176(4) Uani 1 1 d . . . H5 H 0.184(4) -0.600(4) 1.205(3) 0.021(7) Uiso 1 1 d . . . C6 C 0.1169(3) -0.3981(3) 1.2592(2) 0.0173(4) Uani 1 1 d . . . H6 H 0.012(3) -0.390(3) 1.285(3) 0.014(6) Uiso 1 1 d . . . C7 C 0.1673(2) -0.2809(3) 1.2652(2) 0.0147(4) Uani 1 1 d . . . H7 H 0.091(3) -0.195(4) 1.296(3) 0.020(6) Uiso 1 1 d . . . C8 C 0.2235(2) 0.0092(2) 1.2868(2) 0.0115(3) Uani 1 1 d . . . C9 C 0.2432(3) 0.0182(3) 1.4244(2) 0.0137(4) Uani 1 1 d . . . H9 H 0.356(3) -0.060(3) 1.500(3) 0.016(6) Uiso 1 1 d . . . C10 C 0.1048(3) 0.1396(3) 1.4579(2) 0.0173(4) Uani 1 1 d . . . H10 H 0.119(3) 0.143(3) 1.555(3) 0.018(6) Uiso 1 1 d . . . C11 C -0.0532(3) 0.2502(3) 1.3558(2) 0.0174(4) Uani 1 1 d . . . H11 H -0.151(4) 0.335(4) 1.377(3) 0.026(7) Uiso 1 1 d . . . C12 C -0.0734(3) 0.2419(3) 1.2189(2) 0.0167(4) Uani 1 1 d . . . H12 H -0.186(4) 0.320(4) 1.146(4) 0.030(8) Uiso 1 1 d . . . C13 C 0.0642(3) 0.1234(3) 1.1832(2) 0.0141(4) Uani 1 1 d . . . H13 H 0.047(3) 0.119(3) 1.086(3) 0.017(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.00847(6) 0.00883(6) 0.00883(6) -0.00388(4) 0.00175(4) -0.00428(4) Cl1 0.01107(19) 0.01030(19) 0.0154(2) -0.00562(17) 0.00317(16) -0.00407(16) Cl2 0.0151(2) 0.0152(2) 0.0139(2) -0.00620(17) -0.00033(17) -0.00842(17) P1 0.0096(2) 0.0094(2) 0.0092(2) -0.00401(17) 0.00207(17) -0.00423(17) C1 0.0133(8) 0.0145(9) 0.0113(9) -0.0035(7) 0.0006(7) -0.0056(7) C2 0.0140(8) 0.0121(8) 0.0103(8) -0.0038(7) 0.0022(7) -0.0076(7) C3 0.0168(9) 0.0160(9) 0.0157(9) -0.0078(8) 0.0070(7) -0.0090(7) C4 0.0239(10) 0.0160(9) 0.0158(9) -0.0090(8) 0.0070(8) -0.0111(8) C5 0.0242(10) 0.0182(9) 0.0139(9) -0.0055(8) 0.0019(8) -0.0143(8) C6 0.0141(9) 0.0204(10) 0.0187(10) -0.0071(8) 0.0028(8) -0.0105(8) C7 0.0128(9) 0.0155(9) 0.0154(9) -0.0062(8) 0.0023(7) -0.0070(7) C8 0.0123(8) 0.0113(8) 0.0115(8) -0.0046(7) 0.0046(7) -0.0066(7) C9 0.0149(9) 0.0158(9) 0.0124(9) -0.0066(7) 0.0038(7) -0.0089(7) C10 0.0206(10) 0.0195(10) 0.0163(9) -0.0108(8) 0.0075(8) -0.0109(8) C11 0.0171(9) 0.0148(9) 0.0213(10) -0.0099(8) 0.0090(8) -0.0068(8) C12 0.0141(9) 0.0137(9) 0.0187(10) -0.0062(8) 0.0032(8) -0.0046(7) C13 0.0146(9) 0.0132(9) 0.0125(9) -0.0048(7) 0.0024(7) -0.0060(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl1 2.3378(7) 2_657 ? W1 Cl1 2.3379(7) . ? W1 Cl2 2.3466(6) 2_657 ? W1 Cl2 2.3466(6) . ? W1 P1 2.5672(7) 2_657 ? W1 P1 2.5672(7) . ? P1 C8 1.8140(19) . ? P1 C1 1.817(2) . ? P1 C2 1.827(2) . ? C2 C7 1.400(3) . ? C2 C3 1.401(3) . ? C3 C4 1.389(3) . ? C4 C5 1.392(3) . ? C5 C6 1.386(3) . ? C6 C7 1.393(3) . ? C8 C9 1.397(3) . ? C8 C13 1.403(3) . ? C9 C10 1.394(3) . ? C10 C11 1.389(3) . ? C11 C12 1.387(3) . ? C12 C13 1.389(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 W1 Cl1 180.0 2_657 . ? Cl1 W1 Cl2 89.84(3) 2_657 2_657 ? Cl1 W1 Cl2 90.16(3) . 2_657 ? Cl1 W1 Cl2 90.16(3) 2_657 . ? Cl1 W1 Cl2 89.84(3) . . ? Cl2 W1 Cl2 180.000(1) 2_657 . ? Cl1 W1 P1 92.10(2) 2_657 2_657 ? Cl1 W1 P1 87.90(2) . 2_657 ? Cl2 W1 P1 90.34(3) 2_657 2_657 ? Cl2 W1 P1 89.66(3) . 2_657 ? Cl1 W1 P1 87.90(2) 2_657 . ? Cl1 W1 P1 92.10(2) . . ? Cl2 W1 P1 89.66(3) 2_657 . ? Cl2 W1 P1 90.34(3) . . ? P1 W1 P1 180.0 2_657 . ? C8 P1 C1 106.08(9) . . ? C8 P1 C2 104.89(9) . . ? C1 P1 C2 103.03(9) . . ? C8 P1 W1 114.44(6) . . ? C1 P1 W1 110.90(7) . . ? C2 P1 W1 116.39(6) . . ? C7 C2 C3 118.81(18) . . ? C7 C2 P1 122.24(15) . . ? C3 C2 P1 118.94(15) . . ? C4 C3 C2 120.41(19) . . ? C3 C4 C5 120.42(19) . . ? C6 C5 C4 119.54(19) . . ? C5 C6 C7 120.48(19) . . ? C6 C7 C2 120.33(18) . . ? C9 C8 C13 119.50(17) . . ? C9 C8 P1 122.40(15) . . ? C13 C8 P1 118.10(14) . . ? C10 C9 C8 119.87(18) . . ? C11 C10 C9 120.29(19) . . ? C10 C11 C12 120.06(19) . . ? C13 C12 C11 120.20(19) . . ? C12 C13 C8 120.07(19) . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.400 _refine_diff_density_min -1.356 _refine_diff_density_rms 0.114 #===END data_jpd254_0m _database_code_depnum_ccdc_archive 'CCDC 769396' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 4e, [WCl4(dppe)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrachloro(1,2-bis(diphenylphosphino)ethane)tungsten(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl4 P2 W' _chemical_formula_sum 'C26 H24 Cl4 P2 W' _chemical_formula_weight 724.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.300(4) _cell_length_b 21.711(9) _cell_length_c 13.943(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.633(4) _cell_angle_gamma 90.00 _cell_volume 3222(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.27 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 4.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6720 _exptl_absorpt_correction_T_max 0.8271 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in \w) at \f = 0, 120 and 240 deg. A scan time of 70 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27568 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.31 _reflns_number_total 7232 _reflns_number_gt 5712 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2008)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008b)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008b)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2008.6-1, Madison, WI. Bruker-AXS (2008a). SAINT, Version 7.53A, Madison, WI Bruker-AXS (2008b). SHELXTL, Version 2008/3, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. Spek, A. L. (2008). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The phenyl ring built on C21 is disordered over two well-resolved sites in a 56/44 ratio. The two components of the disorder were refined as rigid groups. Some lesser disorder is evident in the other phenyl group attached to P2 from the appearance of the displacement ellipsoids but a reasonable two-site model could not be easily devised. Several scattered peaks of height equal to ca. half a carbon atom and well-separated from the main molecule were removed with the SQUEEZE option of the PLATON package (Spek, 2008) as they could not be modeled in any sensible way by solvent molecules. The largest residual peak is very close (< 1 \%A) to the tungsten atom but attempts to account for it as part of the minor component of a "whole molecule" disorder were unsuccessful. We therefore attribute it to an inadequacy of the empirical absorption correction (the irregular habit of the crystal fragment used made a face- indexed absorption correction unsatisfactory). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+20.6033P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7232 _refine_ls_number_parameters 293 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.79208(3) 0.839346(15) 0.18176(2) 0.04285(11) Uani 1 1 d . A . Cl1 Cl 0.79286(19) 0.93239(10) 0.10805(17) 0.0599(5) Uani 1 1 d . . . Cl2 Cl 0.9480(2) 0.85876(12) 0.33759(15) 0.0621(6) Uani 1 1 d . . . Cl3 Cl 0.62928(18) 0.86752(10) 0.24632(15) 0.0503(4) Uani 1 1 d . . . Cl4 Cl 0.77761(15) 0.73416(9) 0.20953(13) 0.0432(4) Uani 1 1 d . . . P1 P 0.64037(15) 0.80255(9) 0.00528(13) 0.0366(4) Uani 1 1 d . A . P2 P 0.95251(15) 0.80956(10) 0.09893(14) 0.0416(4) Uani 1 1 d D . . C1 C 0.5676(6) 0.8621(3) -0.0867(6) 0.0404(16) Uani 1 1 d . . . C2 C 0.5041(6) 0.9089(3) -0.0555(6) 0.0440(17) Uani 1 1 d . . . H2 H 0.4993 0.9084 0.0112 0.053 Uiso 1 1 calc R . . C3 C 0.4487(7) 0.9558(4) -0.1215(6) 0.0523(19) Uani 1 1 d . . . H3 H 0.4039 0.9870 -0.1004 0.063 Uiso 1 1 calc R . . C4 C 0.4567(7) 0.9584(4) -0.2190(7) 0.057(2) Uani 1 1 d . . . H4 H 0.4208 0.9917 -0.2633 0.068 Uiso 1 1 calc R . . C5 C 0.5183(8) 0.9114(5) -0.2494(7) 0.066(3) Uani 1 1 d . . . H5 H 0.5224 0.9118 -0.3163 0.080 Uiso 1 1 calc R . . C6 C 0.5738(8) 0.8638(4) -0.1847(6) 0.057(2) Uani 1 1 d . . . H6 H 0.6164 0.8321 -0.2070 0.068 Uiso 1 1 calc R . . C7 C 0.5120(6) 0.7512(3) 0.0007(5) 0.0356(14) Uani 1 1 d . . . C8 C 0.4447(7) 0.7593(4) 0.0660(7) 0.058(2) Uani 1 1 d . . . H8 H 0.4674 0.7914 0.1152 0.069 Uiso 1 1 calc R . . C9 C 0.3446(8) 0.7213(5) 0.0606(7) 0.067(3) Uani 1 1 d . . . H9 H 0.2976 0.7278 0.1048 0.080 Uiso 1 1 calc R . . C10 C 0.3132(7) 0.6740(4) -0.0088(7) 0.054(2) Uani 1 1 d . . . H10 H 0.2462 0.6470 -0.0109 0.065 Uiso 1 1 calc R . . C11 C 0.3775(7) 0.6655(4) -0.0748(7) 0.057(2) Uani 1 1 d . . . H11 H 0.3543 0.6333 -0.1237 0.069 Uiso 1 1 calc R . . C12 C 0.4770(7) 0.7041(4) -0.0701(6) 0.053(2) Uani 1 1 d . . . H12 H 0.5219 0.6981 -0.1161 0.063 Uiso 1 1 calc R . . C13 C 0.7421(6) 0.7585(3) -0.0461(5) 0.0367(15) Uani 1 1 d . . . H13A H 0.7624 0.7185 -0.0101 0.044 Uiso 1 1 calc R A . H13B H 0.6973 0.7499 -0.1191 0.044 Uiso 1 1 calc R . . C14 C 0.8633(6) 0.7930(4) -0.0348(5) 0.0449(17) Uani 1 1 d . A . H14A H 0.8430 0.8321 -0.0732 0.054 Uiso 1 1 calc R . . H14B H 0.9157 0.7679 -0.0643 0.054 Uiso 1 1 calc R . . C15 C 1.0421(6) 0.7406(4) 0.1523(6) 0.0500(19) Uani 1 1 d . A . C16 C 1.0362(8) 0.6889(5) 0.0964(8) 0.067(2) Uani 1 1 d . . . H16 H 0.9841 0.6881 0.0269 0.081 Uiso 1 1 calc R A . C17 C 1.1053(9) 0.6374(6) 0.1397(9) 0.079(3) Uani 1 1 d . A . H17 H 1.1013 0.6019 0.0990 0.095 Uiso 1 1 calc R . . C18 C 1.1779(9) 0.6366(6) 0.2380(10) 0.085(3) Uani 1 1 d . . . H18 H 1.2227 0.6005 0.2681 0.102 Uiso 1 1 calc R A . C19 C 1.1852(10) 0.6886(7) 0.2929(10) 0.101(4) Uani 1 1 d . A . H19 H 1.2387 0.6887 0.3620 0.121 Uiso 1 1 calc R . . C20 C 1.1188(9) 0.7419(5) 0.2539(8) 0.083(3) Uani 1 1 d . . . H20 H 1.1254 0.7777 0.2947 0.099 Uiso 1 1 calc R A . C21 C 1.0673(8) 0.8642(5) 0.0864(7) 0.046(2) Uani 0.558(7) 1 d PGD A 1 C22 C 1.1012(10) 0.8690(5) -0.0003(6) 0.066(4) Uani 0.558(7) 1 d PG A 1 H22 H 1.0603 0.8444 -0.0583 0.079 Uiso 0.558(7) 1 calc PR A 1 C23 C 1.1951(10) 0.9099(6) -0.0022(7) 0.081(5) Uani 0.558(7) 1 d PG A 1 H23 H 1.2182 0.9132 -0.0615 0.097 Uiso 0.558(7) 1 calc PR A 1 C24 C 1.2550(10) 0.9459(6) 0.0826(9) 0.070(3) Uani 0.558(7) 1 d PG A 1 H24 H 1.3191 0.9739 0.0813 0.084 Uiso 0.558(7) 1 calc PR A 1 C25 C 1.2211(10) 0.9411(5) 0.1693(7) 0.073(4) Uani 0.558(7) 1 d PG A 1 H25 H 1.2621 0.9657 0.2273 0.087 Uiso 0.558(7) 1 calc PR A 1 C26 C 1.1273(9) 0.9002(5) 0.1713(6) 0.057(3) Uani 0.558(7) 1 d PG A 1 H26 H 1.1041 0.8969 0.2306 0.069 Uiso 0.558(7) 1 calc PR A 1 C21A C 1.0694(10) 0.8685(6) 0.0993(10) 0.046(2) Uani 0.442(7) 1 d PGD A 2 C22A C 1.0254(8) 0.9208(7) 0.0407(10) 0.066(4) Uani 0.442(7) 1 d PG A 2 H22A H 0.9377 0.9264 0.0075 0.079 Uiso 0.442(7) 1 calc PR A 2 C23A C 1.1097(12) 0.9649(6) 0.0307(11) 0.081(5) Uani 0.442(7) 1 d PG A 2 H23A H 1.0796 1.0007 -0.0093 0.097 Uiso 0.442(7) 1 calc PR A 2 C24A C 1.2379(11) 0.9567(6) 0.0793(12) 0.070(3) Uani 0.442(7) 1 d PG A 2 H24A H 1.2955 0.9868 0.0725 0.084 Uiso 0.442(7) 1 calc PR A 2 C25A C 1.2820(8) 0.9044(7) 0.1379(11) 0.073(4) Uani 0.442(7) 1 d PG A 2 H25A H 1.3696 0.8987 0.1711 0.087 Uiso 0.442(7) 1 calc PR A 2 C26A C 1.1977(11) 0.8603(5) 0.1479(10) 0.057(3) Uani 0.442(7) 1 d PG A 2 H26A H 1.2278 0.8245 0.1879 0.069 Uiso 0.442(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.03174(15) 0.0617(2) 0.03810(16) 0.00064(14) 0.01564(11) -0.00475(13) Cl1 0.0496(11) 0.0659(13) 0.0591(12) 0.0052(10) 0.0114(9) -0.0090(9) Cl2 0.0501(11) 0.0931(16) 0.0379(10) -0.0021(10) 0.0079(8) -0.0161(11) Cl3 0.0459(10) 0.0610(11) 0.0527(11) -0.0038(9) 0.0279(8) -0.0006(8) Cl4 0.0360(8) 0.0594(11) 0.0367(8) 0.0026(7) 0.0155(7) -0.0037(7) P1 0.0246(8) 0.0539(11) 0.0356(9) -0.0058(8) 0.0159(7) -0.0032(7) P2 0.0208(7) 0.0670(12) 0.0365(9) 0.0055(9) 0.0090(7) -0.0029(8) C1 0.021(3) 0.051(4) 0.052(4) -0.002(3) 0.016(3) -0.003(3) C2 0.034(3) 0.050(4) 0.042(4) -0.013(3) 0.005(3) -0.001(3) C3 0.044(4) 0.047(4) 0.054(5) -0.014(4) 0.001(3) -0.002(3) C4 0.043(4) 0.052(5) 0.069(6) 0.015(4) 0.011(4) 0.001(4) C5 0.061(5) 0.092(7) 0.052(5) 0.024(5) 0.026(4) 0.014(5) C6 0.051(5) 0.074(6) 0.056(5) 0.013(4) 0.031(4) 0.020(4) C7 0.027(3) 0.046(4) 0.033(3) -0.001(3) 0.009(3) 0.000(3) C8 0.046(4) 0.078(6) 0.060(5) -0.024(4) 0.031(4) -0.022(4) C9 0.058(5) 0.084(7) 0.070(6) -0.010(5) 0.038(5) -0.023(5) C10 0.041(4) 0.060(5) 0.057(5) 0.000(4) 0.012(4) -0.013(4) C11 0.040(4) 0.061(5) 0.066(5) -0.019(4) 0.012(4) -0.012(4) C12 0.032(4) 0.073(6) 0.056(5) -0.018(4) 0.019(3) -0.003(3) C13 0.024(3) 0.058(4) 0.029(3) -0.010(3) 0.010(2) 0.003(3) C14 0.027(3) 0.075(5) 0.032(3) 0.001(3) 0.009(3) 0.002(3) C15 0.019(3) 0.072(5) 0.058(5) 0.009(4) 0.012(3) 0.000(3) C16 0.048(5) 0.088(7) 0.070(6) 0.000(5) 0.026(4) 0.013(5) C17 0.055(6) 0.095(8) 0.088(8) -0.001(6) 0.023(5) 0.022(5) C18 0.049(5) 0.086(8) 0.110(10) 0.009(7) 0.014(6) 0.025(5) C19 0.057(6) 0.124(10) 0.086(8) 0.038(8) -0.023(6) 0.034(7) C20 0.064(6) 0.095(8) 0.058(6) 0.005(5) -0.021(5) 0.007(5) C21 0.026(3) 0.079(6) 0.031(4) 0.008(4) 0.007(3) -0.010(3) C22 0.047(7) 0.092(10) 0.058(7) 0.016(7) 0.016(5) -0.021(6) C23 0.055(8) 0.114(13) 0.074(9) 0.025(9) 0.022(7) -0.026(8) C24 0.044(5) 0.099(9) 0.069(6) 0.007(6) 0.022(5) -0.028(6) C25 0.049(8) 0.095(12) 0.063(8) 0.005(8) 0.005(6) -0.024(7) C26 0.034(6) 0.091(9) 0.047(6) -0.003(6) 0.012(5) -0.015(5) C21A 0.026(3) 0.079(6) 0.031(4) 0.008(4) 0.007(3) -0.010(3) C22A 0.047(7) 0.092(10) 0.058(7) 0.016(7) 0.016(5) -0.021(6) C23A 0.055(8) 0.114(13) 0.074(9) 0.025(9) 0.022(7) -0.026(8) C24A 0.044(5) 0.099(9) 0.069(6) 0.007(6) 0.022(5) -0.028(6) C25A 0.049(8) 0.095(12) 0.063(8) 0.005(8) 0.005(6) -0.024(7) C26A 0.034(6) 0.091(9) 0.047(6) -0.003(6) 0.012(5) -0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl1 2.268(2) . ? W1 Cl2 2.330(2) . ? W1 Cl4 2.331(2) . ? W1 Cl3 2.3837(19) . ? W1 P2 2.5388(19) . ? W1 P1 2.6072(19) . ? P1 C1 1.813(8) . ? P1 C7 1.813(7) . ? P1 C13 1.817(6) . ? P2 C21 1.809(7) . ? P2 C15 1.820(8) . ? P2 C14 1.832(7) . ? P2 C21A 1.838(8) . ? C1 C6 1.393(11) . ? C1 C2 1.394(10) . ? C2 C3 1.374(11) . ? C2 H2 0.9500 . ? C3 C4 1.393(12) . ? C3 H3 0.9500 . ? C4 C5 1.379(12) . ? C4 H4 0.9500 . ? C5 C6 1.375(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.379(10) . ? C7 C12 1.385(10) . ? C8 C9 1.383(11) . ? C8 H8 0.9500 . ? C9 C10 1.373(12) . ? C9 H9 0.9500 . ? C10 C11 1.363(12) . ? C10 H10 0.9500 . ? C11 C12 1.386(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.522(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.355(13) . ? C15 C20 1.391(12) . ? C16 C17 1.381(14) . ? C16 H16 0.9500 . ? C17 C18 1.340(15) . ? C17 H17 0.9500 . ? C18 C19 1.352(17) . ? C18 H18 0.9500 . ? C19 C20 1.387(15) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A H22A 0.9500 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 W1 Cl2 98.31(8) . . ? Cl1 W1 Cl4 163.55(7) . . ? Cl2 W1 Cl4 95.48(8) . . ? Cl1 W1 Cl3 93.64(8) . . ? Cl2 W1 Cl3 92.25(8) . . ? Cl4 W1 Cl3 94.74(7) . . ? Cl1 W1 P2 84.76(8) . . ? Cl2 W1 P2 92.20(8) . . ? Cl4 W1 P2 85.80(6) . . ? Cl3 W1 P2 175.45(6) . . ? Cl1 W1 P1 86.95(7) . . ? Cl2 W1 P1 170.69(8) . . ? Cl4 W1 P1 78.23(6) . . ? Cl3 W1 P1 95.10(7) . . ? P2 W1 P1 80.57(6) . . ? C1 P1 C7 104.3(3) . . ? C1 P1 C13 107.1(3) . . ? C7 P1 C13 105.5(3) . . ? C1 P1 W1 116.6(2) . . ? C7 P1 W1 119.1(2) . . ? C13 P1 W1 103.3(2) . . ? C21 P2 C15 105.1(4) . . ? C21 P2 C14 101.4(4) . . ? C15 P2 C14 107.1(4) . . ? C15 P2 C21A 105.7(5) . . ? C14 P2 C21A 106.8(5) . . ? C21 P2 W1 121.5(4) . . ? C15 P2 W1 114.1(3) . . ? C14 P2 W1 106.2(2) . . ? C21A P2 W1 116.4(5) . . ? C6 C1 C2 119.2(7) . . ? C6 C1 P1 123.5(6) . . ? C2 C1 P1 117.2(6) . . ? C3 C2 C1 119.8(7) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.3(8) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 118.3(8) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C6 C5 C4 121.3(8) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C1 120.0(8) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 118.4(7) . . ? C8 C7 P1 120.7(6) . . ? C12 C7 P1 120.8(5) . . ? C7 C8 C9 120.7(8) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 119.9(8) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.4(8) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 119.6(8) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 120.9(7) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 P1 111.5(5) . . ? C14 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C13 C14 P2 111.8(5) . . ? C13 C14 H14A 109.3 . . ? P2 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? P2 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C20 119.8(9) . . ? C16 C15 P2 122.2(7) . . ? C20 C15 P2 118.0(8) . . ? C15 C16 C17 120.5(10) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 121.4(11) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 117.9(11) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C18 C19 C20 123.6(10) . . ? C18 C19 H19 118.2 . . ? C20 C19 H19 118.2 . . ? C19 C20 C15 116.9(11) . . ? C19 C20 H20 121.6 . . ? C15 C20 H20 121.6 . . ? C22 C21 C26 120.0 . . ? C22 C21 P2 123.3(6) . . ? C26 C21 P2 116.6(6) . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C22A C21A C26A 120.0 . . ? C22A C21A P2 116.9(7) . . ? C26A C21A P2 122.9(7) . . ? C21A C22A C23A 120.0 . . ? C21A C22A H22A 120.0 . . ? C23A C22A H22A 120.0 . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C25A C26A C21A 120.0 . . ? C25A C26A H26A 120.0 . . ? C21A C26A H26A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.006 _refine_diff_density_min -1.690 _refine_diff_density_rms 0.143 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.008 0.500 0.000 346 109 ' ' 2 0.061 0.000 0.500 346 109 ' ' _platon_squeeze_details ; ; #===END data_jpd272_0m _database_code_depnum_ccdc_archive 'CCDC 769397' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound [Cp*2Co][4c], [Cp*2Co][WCl4(PMePh2)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(\h^5^-pentamethylcyclopentadienyl)cobalt(III) trans- tetrachlorobis(methyldiphenylphosphine)tungstate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cl4 P2 W, C20 H30 Co' _chemical_formula_sum 'C46 H56 Cl4 Co P2 W' _chemical_formula_weight 1055.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.227(10) _cell_length_b 11.087(4) _cell_length_c 17.943(6) _cell_angle_alpha 90.00 _cell_angle_beta 125.829(4) _cell_angle_gamma 90.00 _cell_volume 4392(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 28.73 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 3.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4995 _exptl_absorpt_correction_T_max 0.6227 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36325 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.75 _reflns_number_total 5653 _reflns_number_gt 5427 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2008). APEX2, Version 2009.1-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+42.7460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00050(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5653 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.340 _refine_ls_restrained_S_all 1.340 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.7500 -0.2500 0.5000 0.01162(9) Uani 1 2 d S . . Cl1 Cl 0.66778(5) -0.10596(9) 0.42369(8) 0.0174(2) Uani 1 1 d . . . Cl2 Cl 0.74657(5) -0.24995(9) 0.63183(8) 0.0172(2) Uani 1 1 d . . . P1 P 0.82785(5) -0.07991(9) 0.58205(8) 0.0126(2) Uani 1 1 d . . . C1 C 0.8641(2) -0.0267(4) 0.5290(3) 0.0155(8) Uani 1 1 d . . . C2 C 0.9266(2) -0.0126(4) 0.5770(4) 0.0224(9) Uani 1 1 d . . . H2 H 0.9527 -0.0376 0.6393 0.027 Uiso 1 1 calc R . . C3 C 0.9511(2) 0.0375(5) 0.5347(4) 0.0270(11) Uani 1 1 d . . . H3 H 0.9937 0.0461 0.5679 0.032 Uiso 1 1 calc R . . C4 C 0.9137(3) 0.0746(4) 0.4449(4) 0.0285(11) Uani 1 1 d . . . H4 H 0.9306 0.1096 0.4163 0.034 Uiso 1 1 calc R . . C5 C 0.8515(2) 0.0614(4) 0.3956(4) 0.0244(10) Uani 1 1 d . . . H5 H 0.8259 0.0874 0.3335 0.029 Uiso 1 1 calc R . . C6 C 0.8267(2) 0.0103(4) 0.4372(3) 0.0195(9) Uani 1 1 d . . . H6 H 0.7841 0.0004 0.4031 0.023 Uiso 1 1 calc R . . C7 C 0.80747(19) 0.0617(4) 0.6098(3) 0.0140(8) Uani 1 1 d . . . C8 C 0.8226(3) 0.1741(4) 0.5947(4) 0.0262(11) Uani 1 1 d . . . H8 H 0.8397 0.1796 0.5613 0.031 Uiso 1 1 calc R . . C9 C 0.8133(3) 0.2792(5) 0.6278(4) 0.0299(12) Uani 1 1 d . . . H9 H 0.8246 0.3553 0.6180 0.036 Uiso 1 1 calc R . . C10 C 0.7876(2) 0.2720(4) 0.6746(3) 0.0223(10) Uani 1 1 d . . . H10 H 0.7811 0.3430 0.6973 0.027 Uiso 1 1 calc R . . C11 C 0.7713(3) 0.1603(5) 0.6884(4) 0.0296(12) Uani 1 1 d . . . H11 H 0.7538 0.1552 0.7211 0.036 Uiso 1 1 calc R . . C12 C 0.7801(2) 0.0565(5) 0.6552(4) 0.0256(10) Uani 1 1 d . . . H12 H 0.7674 -0.0190 0.6634 0.031 Uiso 1 1 calc R . . C13 C 0.8905(2) -0.1293(4) 0.6966(3) 0.0190(9) Uani 1 1 d . . . H13A H 0.9108 -0.1983 0.6913 0.029 Uiso 1 1 calc R . . H13B H 0.8749 -0.1531 0.7317 0.029 Uiso 1 1 calc R . . H13C H 0.9195 -0.0631 0.7283 0.029 Uiso 1 1 calc R . . Co1 Co 0.5000 1.0000 0.5000 0.01144(16) Uani 1 2 d S . . C14 C 0.5022(2) 0.8407(4) 0.5595(3) 0.0202(9) Uani 1 1 d . . . C15 C 0.5328(2) 0.8281(4) 0.5171(3) 0.0169(8) Uani 1 1 d . . . C16 C 0.49046(19) 0.8561(4) 0.4214(3) 0.0135(8) Uani 1 1 d . . . C17 C 0.43380(19) 0.8850(4) 0.4064(3) 0.0159(8) Uani 1 1 d . . . C18 C 0.4414(2) 0.8749(4) 0.4917(3) 0.0185(9) Uani 1 1 d . . . C19 C 0.5295(3) 0.8171(5) 0.6585(4) 0.0319(12) Uani 1 1 d . . . H19A H 0.5159 0.7383 0.6648 0.048 Uiso 1 1 calc R . . H19B H 0.5167 0.8801 0.6821 0.048 Uiso 1 1 calc R . . H19C H 0.5737 0.8174 0.6937 0.048 Uiso 1 1 calc R . . C20 C 0.5972(2) 0.7893(5) 0.5629(4) 0.0281(11) Uani 1 1 d . . . H20A H 0.6222 0.8187 0.6264 0.042 Uiso 1 1 calc R . . H20B H 0.6124 0.8228 0.5293 0.042 Uiso 1 1 calc R . . H20C H 0.5992 0.7011 0.5627 0.042 Uiso 1 1 calc R . . C21 C 0.5037(2) 0.8520(5) 0.3515(3) 0.0224(10) Uani 1 1 d . . . H21A H 0.5039 0.7679 0.3347 0.034 Uiso 1 1 calc R . . H21B H 0.5434 0.8883 0.3772 0.034 Uiso 1 1 calc R . . H21C H 0.4725 0.8970 0.2966 0.034 Uiso 1 1 calc R . . C22 C 0.3758(2) 0.9165(5) 0.3156(3) 0.0253(10) Uani 1 1 d . . . H22A H 0.3850 0.9469 0.2738 0.038 Uiso 1 1 calc R . . H22B H 0.3543 0.9787 0.3249 0.038 Uiso 1 1 calc R . . H22C H 0.3504 0.8444 0.2891 0.038 Uiso 1 1 calc R . . C23 C 0.3925(3) 0.8911(5) 0.5044(4) 0.0285(11) Uani 1 1 d . . . H23A H 0.3672 0.9600 0.4679 0.043 Uiso 1 1 calc R . . H23B H 0.4106 0.9059 0.5695 0.043 Uiso 1 1 calc R . . H23C H 0.3676 0.8180 0.4844 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01136(13) 0.00991(12) 0.01527(13) 0.00254(8) 0.00874(10) 0.00159(8) Cl1 0.0175(5) 0.0139(4) 0.0219(5) 0.0055(4) 0.0121(4) 0.0057(4) Cl2 0.0181(5) 0.0179(5) 0.0188(5) 0.0033(4) 0.0127(4) 0.0013(4) P1 0.0132(5) 0.0112(5) 0.0151(5) 0.0004(4) 0.0093(4) 0.0006(4) C1 0.019(2) 0.0111(18) 0.023(2) -0.0010(16) 0.0161(18) -0.0014(15) C2 0.019(2) 0.023(2) 0.026(2) -0.0053(19) 0.014(2) -0.0045(18) C3 0.026(2) 0.026(2) 0.040(3) -0.010(2) 0.026(2) -0.009(2) C4 0.041(3) 0.019(2) 0.049(3) -0.007(2) 0.039(3) -0.009(2) C5 0.036(3) 0.019(2) 0.027(3) 0.0009(19) 0.023(2) -0.001(2) C6 0.023(2) 0.0142(19) 0.026(2) 0.0021(18) 0.017(2) 0.0005(17) C7 0.0135(18) 0.0155(19) 0.0116(19) -0.0002(15) 0.0066(16) 0.0015(15) C8 0.041(3) 0.019(2) 0.029(3) 0.004(2) 0.026(3) 0.001(2) C9 0.050(3) 0.012(2) 0.036(3) 0.004(2) 0.030(3) 0.003(2) C10 0.022(2) 0.017(2) 0.022(2) -0.0060(18) 0.009(2) 0.0044(18) C11 0.037(3) 0.029(3) 0.037(3) -0.013(2) 0.030(3) -0.005(2) C12 0.038(3) 0.021(2) 0.033(3) -0.008(2) 0.029(3) -0.007(2) C13 0.016(2) 0.021(2) 0.016(2) 0.0029(17) 0.0069(18) 0.0022(17) Co1 0.0131(3) 0.0121(4) 0.0092(3) -0.0031(3) 0.0066(3) -0.0008(3) C14 0.032(2) 0.0135(19) 0.016(2) -0.0033(16) 0.014(2) -0.0037(18) C15 0.018(2) 0.0133(18) 0.016(2) -0.0029(16) 0.0078(18) 0.0021(16) C16 0.0139(18) 0.0158(18) 0.0090(18) -0.0050(15) 0.0056(16) -0.0015(15) C17 0.0124(18) 0.0153(19) 0.015(2) -0.0067(16) 0.0051(17) -0.0024(15) C18 0.026(2) 0.016(2) 0.020(2) -0.0047(17) 0.017(2) -0.0038(17) C19 0.052(3) 0.027(3) 0.019(2) 0.000(2) 0.022(3) -0.002(2) C20 0.023(2) 0.021(2) 0.026(3) -0.003(2) 0.006(2) 0.0063(19) C21 0.026(2) 0.029(2) 0.021(2) -0.0119(19) 0.018(2) -0.0076(19) C22 0.016(2) 0.031(3) 0.022(2) -0.004(2) 0.0074(19) 0.0002(19) C23 0.038(3) 0.025(2) 0.041(3) -0.010(2) 0.034(3) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl1 2.4182(12) 7_646 ? W1 Cl1 2.4182(12) . ? W1 Cl2 2.4213(13) 7_646 ? W1 Cl2 2.4214(13) . ? W1 P1 2.5619(12) 7_646 ? W1 P1 2.5619(12) . ? P1 C1 1.824(4) . ? P1 C13 1.825(5) . ? P1 C7 1.829(4) . ? C1 C2 1.396(6) . ? C1 C6 1.399(6) . ? C2 C3 1.385(7) . ? C2 H2 0.9500 . ? C3 C4 1.372(8) . ? C3 H3 0.9500 . ? C4 C5 1.385(7) . ? C4 H4 0.9500 . ? C5 C6 1.386(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.389(6) . ? C7 C12 1.389(6) . ? C8 C9 1.398(7) . ? C8 H8 0.9500 . ? C9 C10 1.372(7) . ? C9 H9 0.9500 . ? C10 C11 1.386(7) . ? C10 H10 0.9500 . ? C11 C12 1.380(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Co1 C17 2.037(4) . ? Co1 C17 2.037(4) 5_676 ? Co1 C16 2.043(4) 5_676 ? Co1 C16 2.043(4) . ? Co1 C14 2.047(5) 5_676 ? Co1 C14 2.048(5) . ? Co1 C15 2.050(4) . ? Co1 C15 2.050(4) 5_676 ? Co1 C18 2.052(5) 5_676 ? Co1 C18 2.052(5) . ? C14 C18 1.416(7) . ? C14 C15 1.427(6) . ? C14 C19 1.493(7) . ? C15 C16 1.433(6) . ? C15 C20 1.501(6) . ? C16 C17 1.438(6) . ? C16 C21 1.496(6) . ? C17 C18 1.423(6) . ? C17 C22 1.502(6) . ? C18 C23 1.488(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 W1 Cl1 180.0 7_646 . ? Cl1 W1 Cl2 90.05(4) 7_646 7_646 ? Cl1 W1 Cl2 89.96(4) . 7_646 ? Cl1 W1 Cl2 89.95(4) 7_646 . ? Cl1 W1 Cl2 90.04(4) . . ? Cl2 W1 Cl2 180.00(5) 7_646 . ? Cl1 W1 P1 91.12(4) 7_646 7_646 ? Cl1 W1 P1 88.88(4) . 7_646 ? Cl2 W1 P1 86.01(4) 7_646 7_646 ? Cl2 W1 P1 93.99(4) . 7_646 ? Cl1 W1 P1 88.88(4) 7_646 . ? Cl1 W1 P1 91.12(4) . . ? Cl2 W1 P1 93.98(4) 7_646 . ? Cl2 W1 P1 86.01(4) . . ? P1 W1 P1 180.0 7_646 . ? C1 P1 C13 104.5(2) . . ? C1 P1 C7 102.0(2) . . ? C13 P1 C7 100.6(2) . . ? C1 P1 W1 117.16(15) . . ? C13 P1 W1 109.86(16) . . ? C7 P1 W1 120.50(14) . . ? C2 C1 C6 118.5(4) . . ? C2 C1 P1 123.5(4) . . ? C6 C1 P1 117.8(3) . . ? C3 C2 C1 120.7(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 119.9(5) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 120.4(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 118.4(4) . . ? C8 C7 P1 123.0(3) . . ? C12 C7 P1 118.4(3) . . ? C7 C8 C9 121.0(5) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 119.8(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 119.5(4) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 120.9(5) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C7 120.4(5) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C17 Co1 C17 179.999(1) . 5_676 ? C17 Co1 C16 138.73(16) . 5_676 ? C17 Co1 C16 41.27(16) 5_676 5_676 ? C17 Co1 C16 41.27(16) . . ? C17 Co1 C16 138.73(16) 5_676 . ? C16 Co1 C16 179.997(1) 5_676 . ? C17 Co1 C14 111.61(19) . 5_676 ? C17 Co1 C14 68.39(19) 5_676 5_676 ? C16 Co1 C14 68.86(17) 5_676 5_676 ? C16 Co1 C14 111.14(17) . 5_676 ? C17 Co1 C14 68.39(19) . . ? C17 Co1 C14 111.61(19) 5_676 . ? C16 Co1 C14 111.14(17) 5_676 . ? C16 Co1 C14 68.86(17) . . ? C14 Co1 C14 180.0(3) 5_676 . ? C17 Co1 C15 68.84(18) . . ? C17 Co1 C15 111.16(18) 5_676 . ? C16 Co1 C15 138.99(17) 5_676 . ? C16 Co1 C15 41.01(17) . . ? C14 Co1 C15 139.24(18) 5_676 . ? C14 Co1 C15 40.76(18) . . ? C17 Co1 C15 111.16(18) . 5_676 ? C17 Co1 C15 68.84(18) 5_676 5_676 ? C16 Co1 C15 41.00(17) 5_676 5_676 ? C16 Co1 C15 138.99(17) . 5_676 ? C14 Co1 C15 40.77(18) 5_676 5_676 ? C14 Co1 C15 139.23(18) . 5_676 ? C15 Co1 C15 180.0(3) . 5_676 ? C17 Co1 C18 139.27(18) . 5_676 ? C17 Co1 C18 40.73(18) 5_676 5_676 ? C16 Co1 C18 69.03(17) 5_676 5_676 ? C16 Co1 C18 110.97(17) . 5_676 ? C14 Co1 C18 40.40(19) 5_676 5_676 ? C14 Co1 C18 139.60(19) . 5_676 ? C15 Co1 C18 111.47(18) . 5_676 ? C15 Co1 C18 68.53(18) 5_676 5_676 ? C17 Co1 C18 40.73(18) . . ? C17 Co1 C18 139.27(18) 5_676 . ? C16 Co1 C18 110.97(17) 5_676 . ? C16 Co1 C18 69.03(17) . . ? C14 Co1 C18 139.60(19) 5_676 . ? C14 Co1 C18 40.40(19) . . ? C15 Co1 C18 68.53(18) . . ? C15 Co1 C18 111.47(18) 5_676 . ? C18 Co1 C18 179.999(1) 5_676 . ? C18 C14 C15 108.6(4) . . ? C18 C14 C19 126.0(5) . . ? C15 C14 C19 125.3(5) . . ? C18 C14 Co1 69.9(3) . . ? C15 C14 Co1 69.7(3) . . ? C19 C14 Co1 127.9(3) . . ? C14 C15 C16 107.9(4) . . ? C14 C15 C20 126.7(4) . . ? C16 C15 C20 125.4(4) . . ? C14 C15 Co1 69.5(3) . . ? C16 C15 Co1 69.2(2) . . ? C20 C15 Co1 128.0(3) . . ? C15 C16 C17 107.1(4) . . ? C15 C16 C21 125.4(4) . . ? C17 C16 C21 127.4(4) . . ? C15 C16 Co1 69.8(2) . . ? C17 C16 Co1 69.2(2) . . ? C21 C16 Co1 127.4(3) . . ? C18 C17 C16 108.4(4) . . ? C18 C17 C22 125.7(4) . . ? C16 C17 C22 125.9(4) . . ? C18 C17 Co1 70.2(2) . . ? C16 C17 Co1 69.6(2) . . ? C22 C17 Co1 127.6(3) . . ? C14 C18 C17 108.0(4) . . ? C14 C18 C23 126.8(4) . . ? C17 C18 C23 125.1(5) . . ? C14 C18 Co1 69.6(3) . . ? C17 C18 Co1 69.1(2) . . ? C23 C18 Co1 129.4(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.209 _refine_diff_density_min -2.849 _refine_diff_density_rms 0.154 #===END data_jpd341_0m _database_code_depnum_ccdc_archive 'CCDC 769398' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound [Cp*2Co][4c], [Cp*2Co][WCl4(PMePh2)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(\h^5^-pentamethylcyclopentadienyl)cobalt(III) tetrachlorobis(methydiphenylphosphine)tungstate(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cl4 P2 W, C20 H30 Co' _chemical_formula_sum 'C46 H56 Cl4 Co P2 W' _chemical_formula_weight 1055.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5995(15) _cell_length_b 11.0472(18) _cell_length_c 21.228(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.333(2) _cell_angle_gamma 90.00 _cell_volume 2247.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9819 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.71 _exptl_crystal_description Column _exptl_crystal_colour Orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1062 _exptl_absorpt_coefficient_mu 3.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6483 _exptl_absorpt_correction_T_max 0.7917 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, collected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39415 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.72 _reflns_number_total 5776 _reflns_number_gt 5022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.9-0, Madison, WI. Bruker-AXS (2009a). SAINT, Version 7.68A, Madison, WI Bruker-AXS (2008). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS and SHELXL. Acta Cryst. A64, 112-122. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+1.6725P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5776 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 1.0000 1.0000 0.0000 0.01439(4) Uani 1 2 d S . . Cl1 Cl 1.22622(5) 1.01221(4) 0.05784(2) 0.02108(9) Uani 1 1 d . . . Cl2 Cl 0.97670(5) 1.21637(4) 0.00888(2) 0.02170(10) Uani 1 1 d . . . P1 P 0.89017(5) 0.95810(4) 0.10329(2) 0.01591(9) Uani 1 1 d . . . C1 C 0.9801(2) 0.84521(18) 0.15423(9) 0.0203(4) Uani 1 1 d . . . C2 C 1.0736(2) 0.8764(2) 0.20431(10) 0.0278(5) Uani 1 1 d . . . H2 H 1.0905 0.9593 0.2139 0.033 Uiso 1 1 calc R . . C3 C 1.1422(2) 0.7872(2) 0.24031(11) 0.0361(6) Uani 1 1 d . . . H3 H 1.2048 0.8096 0.2746 0.043 Uiso 1 1 calc R . . C4 C 1.1201(3) 0.6657(2) 0.22671(12) 0.0388(6) Uani 1 1 d . . . H4 H 1.1677 0.6051 0.2514 0.047 Uiso 1 1 calc R . . C5 C 1.0286(3) 0.6334(2) 0.17715(11) 0.0356(5) Uani 1 1 d . . . H5 H 1.0129 0.5503 0.1676 0.043 Uiso 1 1 calc R . . C6 C 0.9590(2) 0.72247(19) 0.14097(10) 0.0265(4) Uani 1 1 d . . . H6 H 0.8964 0.6994 0.1068 0.032 Uiso 1 1 calc R . . C7 C 0.8717(2) 1.08861(17) 0.15479(9) 0.0179(4) Uani 1 1 d . . . C8 C 0.9855(2) 1.16736(19) 0.16407(10) 0.0243(4) Uani 1 1 d . . . H8 H 1.0705 1.1501 0.1451 0.029 Uiso 1 1 calc R . . C9 C 0.9745(2) 1.27065(19) 0.20090(10) 0.0274(4) Uani 1 1 d . . . H9 H 1.0528 1.3225 0.2080 0.033 Uiso 1 1 calc R . . C10 C 0.8497(2) 1.29815(19) 0.22721(9) 0.0261(4) Uani 1 1 d . . . H10 H 0.8420 1.3697 0.2516 0.031 Uiso 1 1 calc R . . C11 C 0.7362(2) 1.22144(18) 0.21799(9) 0.0235(4) Uani 1 1 d . . . H11 H 0.6507 1.2403 0.2362 0.028 Uiso 1 1 calc R . . C12 C 0.7471(2) 1.11653(17) 0.18207(9) 0.0196(4) Uani 1 1 d . . . H12 H 0.6692 1.0638 0.1762 0.024 Uiso 1 1 calc R . . C13 C 0.7155(2) 0.89506(18) 0.09138(10) 0.0215(4) Uani 1 1 d . . . H13A H 0.6833 0.8672 0.1319 0.032 Uiso 1 1 calc R . . H13B H 0.7172 0.8267 0.0620 0.032 Uiso 1 1 calc R . . H13C H 0.6518 0.9574 0.0738 0.032 Uiso 1 1 calc R . . Co1 Co 0.5000 0.5000 0.0000 0.01351(7) Uani 1 2 d S . . C14 C 0.48927(19) 0.65101(17) 0.05679(9) 0.0186(4) Uani 1 1 d . . . C15 C 0.5996(2) 0.57222(16) 0.07931(9) 0.0181(4) Uani 1 1 d . . . C16 C 0.6946(2) 0.55784(17) 0.03039(10) 0.0204(4) Uani 1 1 d . . . C17 C 0.6424(2) 0.62803(17) -0.02270(9) 0.0215(4) Uani 1 1 d . . . C18 C 0.5164(2) 0.68506(17) -0.00618(9) 0.0208(4) Uani 1 1 d . . . C19 C 0.3714(2) 0.6951(2) 0.09375(11) 0.0313(5) Uani 1 1 d . . . H19A H 0.3451 0.6319 0.1232 0.047 Uiso 1 1 calc R . . H19B H 0.2912 0.7146 0.0648 0.047 Uiso 1 1 calc R . . H19C H 0.4007 0.7678 0.1174 0.047 Uiso 1 1 calc R . . C20 C 0.6150(3) 0.5191(2) 0.14430(11) 0.0322(5) Uani 1 1 d . . . H20A H 0.6660 0.5759 0.1726 0.048 Uiso 1 1 calc R . . H20B H 0.6667 0.4428 0.1430 0.048 Uiso 1 1 calc R . . H20C H 0.5224 0.5040 0.1598 0.048 Uiso 1 1 calc R . . C21 C 0.8262(2) 0.4848(2) 0.03355(14) 0.0358(6) Uani 1 1 d . . . H21A H 0.8331 0.4399 -0.0060 0.054 Uiso 1 1 calc R . . H21B H 0.8250 0.4277 0.0689 0.054 Uiso 1 1 calc R . . H21C H 0.9067 0.5389 0.0398 0.054 Uiso 1 1 calc R . . C22 C 0.7109(3) 0.6430(2) -0.08352(11) 0.0386(6) Uani 1 1 d . . . H22A H 0.7713 0.7146 -0.0811 0.058 Uiso 1 1 calc R . . H22B H 0.6394 0.6532 -0.1180 0.058 Uiso 1 1 calc R . . H22C H 0.7670 0.5711 -0.0915 0.058 Uiso 1 1 calc R . . C23 C 0.4311(3) 0.77227(19) -0.04696(12) 0.0352(5) Uani 1 1 d . . . H23A H 0.4715 0.8535 -0.0426 0.053 Uiso 1 1 calc R . . H23B H 0.3351 0.7736 -0.0337 0.053 Uiso 1 1 calc R . . H23C H 0.4313 0.7465 -0.0911 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01512(5) 0.01103(5) 0.01736(5) -0.00107(4) 0.00388(4) 0.00090(4) Cl1 0.0175(2) 0.0212(2) 0.0244(2) -0.00111(18) 0.00058(18) 0.00093(17) Cl2 0.0248(2) 0.0122(2) 0.0282(2) -0.00189(17) 0.00331(19) 0.00236(17) P1 0.0165(2) 0.0139(2) 0.0177(2) -0.00124(18) 0.00341(18) -0.00108(17) C1 0.0184(9) 0.0230(10) 0.0200(9) 0.0026(7) 0.0058(8) 0.0024(7) C2 0.0211(10) 0.0360(12) 0.0264(11) 0.0011(9) 0.0031(9) -0.0016(9) C3 0.0205(10) 0.0589(17) 0.0287(12) 0.0073(11) -0.0005(9) 0.0057(10) C4 0.0339(13) 0.0479(15) 0.0354(13) 0.0155(11) 0.0082(11) 0.0203(11) C5 0.0426(14) 0.0279(12) 0.0373(13) 0.0088(10) 0.0114(11) 0.0114(10) C6 0.0331(11) 0.0225(10) 0.0244(10) 0.0024(8) 0.0053(9) 0.0045(9) C7 0.0197(9) 0.0158(9) 0.0183(9) -0.0018(7) 0.0032(7) 0.0007(7) C8 0.0212(10) 0.0248(10) 0.0273(10) -0.0053(8) 0.0047(8) -0.0016(8) C9 0.0284(11) 0.0233(10) 0.0300(11) -0.0076(9) -0.0007(9) -0.0044(8) C10 0.0375(12) 0.0217(10) 0.0189(9) -0.0047(8) 0.0002(9) 0.0069(9) C11 0.0280(10) 0.0250(10) 0.0179(9) 0.0003(8) 0.0057(8) 0.0102(8) C12 0.0205(9) 0.0213(9) 0.0171(9) 0.0032(7) 0.0024(8) 0.0027(7) C13 0.0197(9) 0.0201(10) 0.0248(10) 0.0004(8) 0.0031(8) -0.0040(7) Co1 0.01321(15) 0.01080(15) 0.01640(16) -0.00077(13) -0.00021(13) -0.00026(12) C14 0.0177(9) 0.0148(9) 0.0229(9) -0.0042(7) -0.0006(8) -0.0008(7) C15 0.0198(9) 0.0131(8) 0.0208(9) -0.0016(7) -0.0034(7) -0.0019(7) C16 0.0150(8) 0.0143(9) 0.0316(11) -0.0069(8) -0.0005(8) -0.0014(7) C17 0.0240(10) 0.0178(9) 0.0231(10) -0.0038(7) 0.0047(8) -0.0090(7) C18 0.0241(10) 0.0103(8) 0.0271(10) -0.0005(7) -0.0061(8) -0.0034(7) C19 0.0226(10) 0.0302(12) 0.0415(13) -0.0175(10) 0.0065(10) -0.0010(9) C20 0.0437(14) 0.0296(12) 0.0220(10) 0.0032(9) -0.0088(10) -0.0093(10) C21 0.0168(10) 0.0264(12) 0.0635(17) -0.0164(11) -0.0045(11) 0.0029(8) C22 0.0459(14) 0.0418(14) 0.0296(12) -0.0090(10) 0.0153(11) -0.0240(11) C23 0.0452(14) 0.0163(10) 0.0416(13) 0.0063(9) -0.0177(11) -0.0010(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl2 2.4092(6) . ? W1 Cl2 2.4092(6) 3_775 ? W1 Cl1 2.4355(6) 3_775 ? W1 Cl1 2.4355(6) . ? W1 P1 2.5303(6) . ? W1 P1 2.5304(6) 3_775 ? P1 C13 1.820(2) . ? P1 C7 1.8242(19) . ? P1 C1 1.833(2) . ? C1 C2 1.394(3) . ? C1 C6 1.397(3) . ? C2 C3 1.390(3) . ? C2 H2 0.9500 . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.378(4) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.393(3) . ? C7 C8 1.402(3) . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.395(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Co1 C16 2.0433(19) . ? Co1 C16 2.0434(19) 3_665 ? Co1 C17 2.0441(19) 3_665 ? Co1 C17 2.0441(19) . ? Co1 C15 2.0486(19) . ? Co1 C15 2.0487(19) 3_665 ? Co1 C18 2.0552(19) . ? Co1 C18 2.0552(19) 3_665 ? Co1 C14 2.0643(18) . ? Co1 C14 2.0643(18) 3_665 ? C14 C18 1.427(3) . ? C14 C15 1.431(3) . ? C14 C19 1.496(3) . ? C15 C16 1.431(3) . ? C15 C20 1.499(3) . ? C16 C17 1.434(3) . ? C16 C21 1.497(3) . ? C17 C18 1.426(3) . ? C17 C22 1.492(3) . ? C18 C23 1.505(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 W1 Cl2 180.0 . 3_775 ? Cl2 W1 Cl1 90.587(16) . 3_775 ? Cl2 W1 Cl1 89.413(16) 3_775 3_775 ? Cl2 W1 Cl1 89.413(16) . . ? Cl2 W1 Cl1 90.587(16) 3_775 . ? Cl1 W1 Cl1 180.0 3_775 . ? Cl2 W1 P1 93.925(16) . . ? Cl2 W1 P1 86.073(16) 3_775 . ? Cl1 W1 P1 91.288(19) 3_775 . ? Cl1 W1 P1 88.713(19) . . ? Cl2 W1 P1 86.074(16) . 3_775 ? Cl2 W1 P1 93.928(16) 3_775 3_775 ? Cl1 W1 P1 88.712(19) 3_775 3_775 ? Cl1 W1 P1 91.287(19) . 3_775 ? P1 W1 P1 179.999(10) . 3_775 ? C13 P1 C7 105.35(9) . . ? C13 P1 C1 102.71(9) . . ? C7 P1 C1 104.07(9) . . ? C13 P1 W1 112.12(7) . . ? C7 P1 W1 115.77(6) . . ? C1 P1 W1 115.46(6) . . ? C2 C1 C6 118.21(19) . . ? C2 C1 P1 122.80(16) . . ? C6 C1 P1 118.94(16) . . ? C3 C2 C1 120.5(2) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.7(2) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.1(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.0(2) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C12 C7 C8 119.02(18) . . ? C12 C7 P1 122.68(15) . . ? C8 C7 P1 118.20(14) . . ? C9 C8 C7 120.27(19) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.05(19) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.13(18) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.33(19) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 Co1 C16 180.0 . 3_665 ? C16 Co1 C17 138.92(8) . 3_665 ? C16 Co1 C17 41.08(8) 3_665 3_665 ? C16 Co1 C17 41.08(8) . . ? C16 Co1 C17 138.92(8) 3_665 . ? C17 Co1 C17 180.0 3_665 . ? C16 Co1 C15 40.93(8) . . ? C16 Co1 C15 139.07(8) 3_665 . ? C17 Co1 C15 111.24(8) 3_665 . ? C17 Co1 C15 68.76(8) . . ? C16 Co1 C15 139.07(8) . 3_665 ? C16 Co1 C15 40.93(8) 3_665 3_665 ? C17 Co1 C15 68.76(8) 3_665 3_665 ? C17 Co1 C15 111.24(8) . 3_665 ? C15 Co1 C15 180.00(9) . 3_665 ? C16 Co1 C18 68.71(8) . . ? C16 Co1 C18 111.29(8) 3_665 . ? C17 Co1 C18 139.30(8) 3_665 . ? C17 Co1 C18 40.70(8) . . ? C15 Co1 C18 68.36(7) . . ? C15 Co1 C18 111.64(7) 3_665 . ? C16 Co1 C18 111.29(8) . 3_665 ? C16 Co1 C18 68.71(8) 3_665 3_665 ? C17 Co1 C18 40.70(8) 3_665 3_665 ? C17 Co1 C18 139.30(8) . 3_665 ? C15 Co1 C18 111.64(7) . 3_665 ? C15 Co1 C18 68.36(7) 3_665 3_665 ? C18 Co1 C18 180.0 . 3_665 ? C16 Co1 C14 68.82(7) . . ? C16 Co1 C14 111.18(7) 3_665 . ? C17 Co1 C14 111.39(8) 3_665 . ? C17 Co1 C14 68.61(8) . . ? C15 Co1 C14 40.72(7) . . ? C15 Co1 C14 139.28(7) 3_665 . ? C18 Co1 C14 40.54(7) . . ? C18 Co1 C14 139.46(7) 3_665 . ? C16 Co1 C14 111.18(7) . 3_665 ? C16 Co1 C14 68.82(7) 3_665 3_665 ? C17 Co1 C14 68.61(8) 3_665 3_665 ? C17 Co1 C14 111.39(8) . 3_665 ? C15 Co1 C14 139.28(7) . 3_665 ? C15 Co1 C14 40.72(7) 3_665 3_665 ? C18 Co1 C14 139.46(7) . 3_665 ? C18 Co1 C14 40.54(7) 3_665 3_665 ? C14 Co1 C14 180.00(10) . 3_665 ? C18 C14 C15 107.53(17) . . ? C18 C14 C19 126.18(19) . . ? C15 C14 C19 126.20(19) . . ? C18 C14 Co1 69.39(11) . . ? C15 C14 Co1 69.05(10) . . ? C19 C14 Co1 129.40(14) . . ? C16 C15 C14 108.41(17) . . ? C16 C15 C20 126.27(19) . . ? C14 C15 C20 125.26(19) . . ? C16 C15 Co1 69.34(11) . . ? C14 C15 Co1 70.23(11) . . ? C20 C15 Co1 128.36(14) . . ? C15 C16 C17 107.56(16) . . ? C15 C16 C21 126.8(2) . . ? C17 C16 C21 125.6(2) . . ? C15 C16 Co1 69.73(10) . . ? C17 C16 Co1 69.49(11) . . ? C21 C16 Co1 126.81(14) . . ? C18 C17 C16 107.97(17) . . ? C18 C17 C22 125.9(2) . . ? C16 C17 C22 126.1(2) . . ? C18 C17 Co1 70.07(11) . . ? C16 C17 Co1 69.43(11) . . ? C22 C17 Co1 127.98(14) . . ? C17 C18 C14 108.52(17) . . ? C17 C18 C23 125.62(19) . . ? C14 C18 C23 125.77(19) . . ? C17 C18 Co1 69.23(11) . . ? C14 C18 Co1 70.07(11) . . ? C23 C18 Co1 129.22(14) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.844 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.077 #===END data_jpd270_0m _database_code_depnum_ccdc_archive 'CCDC 769399' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound [Cp*2Co][5c], [Cp*2Co][WCl5(PMePh2)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(\h^5^-pentamethylcyclopentadienyl)cobalt(II) Pentachloro(diphenylmethylphosphine)tungstate(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H13 Cl5 P W, C20 H30 Co' _chemical_formula_sum 'C33 H43 Cl5 Co P W' _chemical_formula_weight 890.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6543(11) _cell_length_b 10.1624(12) _cell_length_c 17.949(2) _cell_angle_alpha 80.677(2) _cell_angle_beta 80.642(2) _cell_angle_gamma 89.713(2) _cell_volume 1714.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9830 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 28.76 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 4.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5721 _exptl_absorpt_correction_T_max 0.8107 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in \w, collected at \f = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in \f, collected at \w = -30.00 and 210.00 deg. The scan time was 15 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30759 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.77 _reflns_number_total 8671 _reflns_number_gt 8132 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.1-0, Madison, WI. Bruker-AXS (2008). SAINT, Version 7.60A, Madison, WI Bruker-AXS (2008a). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+11.0636P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8671 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.687331(17) 0.735961(17) 0.726719(9) 0.01744(6) Uani 1 1 d . . . Cl1 Cl 0.90998(12) 0.79015(13) 0.75437(6) 0.0273(2) Uani 1 1 d . . . Cl2 Cl 0.66780(16) 0.95795(11) 0.67008(7) 0.0319(3) Uani 1 1 d . . . Cl3 Cl 0.47496(12) 0.68001(14) 0.69053(7) 0.0301(2) Uani 1 1 d . . . Cl4 Cl 0.71869(13) 0.51464(11) 0.78208(7) 0.0284(2) Uani 1 1 d . . . Cl5 Cl 0.56975(12) 0.78288(13) 0.84845(6) 0.0271(2) Uani 1 1 d . . . P1 P 0.80965(11) 0.68290(10) 0.59757(6) 0.01468(19) Uani 1 1 d . . . C1 C 0.7976(4) 0.8112(4) 0.5158(2) 0.0168(7) Uani 1 1 d . . . C2 C 0.6664(5) 0.8573(4) 0.5013(2) 0.0194(8) Uani 1 1 d . . . H2 H 0.5836 0.8195 0.5336 0.023 Uiso 1 1 calc R . . C3 C 0.6558(5) 0.9577(5) 0.4404(2) 0.0233(9) Uani 1 1 d . . . H3 H 0.5660 0.9871 0.4304 0.028 Uiso 1 1 calc R . . C4 C 0.7770(6) 1.0156(4) 0.3938(2) 0.0254(9) Uani 1 1 d . . . H4 H 0.7699 1.0855 0.3526 0.031 Uiso 1 1 calc R . . C5 C 0.9073(5) 0.9713(5) 0.4075(3) 0.0245(9) Uani 1 1 d . . . H5 H 0.9898 1.0109 0.3757 0.029 Uiso 1 1 calc R . . C6 C 0.9184(5) 0.8683(4) 0.4681(2) 0.0209(8) Uani 1 1 d . . . H6 H 1.0083 0.8373 0.4769 0.025 Uiso 1 1 calc R . . C7 C 0.7558(4) 0.5274(4) 0.5705(2) 0.0186(8) Uani 1 1 d . . . C8 C 0.7871(5) 0.4077(5) 0.6143(3) 0.0250(9) Uani 1 1 d . . . H8 H 0.8326 0.4095 0.6572 0.030 Uiso 1 1 calc R . . C9 C 0.7524(6) 0.2870(5) 0.5954(3) 0.0306(11) Uani 1 1 d . . . H9 H 0.7745 0.2062 0.6254 0.037 Uiso 1 1 calc R . . C10 C 0.6856(5) 0.2830(5) 0.5331(3) 0.0304(11) Uani 1 1 d . . . H10 H 0.6607 0.1997 0.5208 0.036 Uiso 1 1 calc R . . C11 C 0.6554(5) 0.4004(5) 0.4890(3) 0.0289(10) Uani 1 1 d . . . H11 H 0.6111 0.3978 0.4457 0.035 Uiso 1 1 calc R . . C12 C 0.6898(4) 0.5238(5) 0.5077(3) 0.0225(9) Uani 1 1 d . . . H12 H 0.6680 0.6045 0.4775 0.027 Uiso 1 1 calc R . . C13 C 0.9959(4) 0.6570(5) 0.5952(3) 0.0220(8) Uani 1 1 d . . . H13A H 1.0361 0.6282 0.5469 0.033 Uiso 1 1 calc R . . H13B H 1.0103 0.5882 0.6381 0.033 Uiso 1 1 calc R . . H13C H 1.0420 0.7405 0.5994 0.033 Uiso 1 1 calc R . . Co1 Co 0.23234(6) 0.24589(5) 0.86560(3) 0.01386(11) Uani 1 1 d . . . C14 C 0.0539(4) 0.1458(4) 0.8556(3) 0.0192(8) Uani 1 1 d . . . C15 C 0.1625(4) 0.0537(4) 0.8718(3) 0.0198(8) Uani 1 1 d . . . C16 C 0.2003(5) 0.0732(4) 0.9431(3) 0.0211(8) Uani 1 1 d . . . C17 C 0.1169(5) 0.1778(5) 0.9707(2) 0.0216(8) Uani 1 1 d . . . C18 C 0.0267(4) 0.2226(5) 0.9165(3) 0.0208(8) Uani 1 1 d . . . C19 C -0.0214(5) 0.1552(5) 0.7882(3) 0.0286(10) Uani 1 1 d . . . H19A H -0.0944 0.0850 0.7982 0.043 Uiso 1 1 calc R . . H19B H 0.0456 0.1441 0.7426 0.043 Uiso 1 1 calc R . . H19C H -0.0647 0.2427 0.7799 0.043 Uiso 1 1 calc R . . C20 C 0.2219(5) -0.0457(5) 0.8231(3) 0.0296(10) Uani 1 1 d . . . H20A H 0.3168 -0.0683 0.8329 0.044 Uiso 1 1 calc R . . H20B H 0.2258 -0.0077 0.7690 0.044 Uiso 1 1 calc R . . H20C H 0.1620 -0.1265 0.8354 0.044 Uiso 1 1 calc R . . C21 C 0.3067(5) -0.0035(5) 0.9838(3) 0.0323(11) Uani 1 1 d . . . H21A H 0.2589 -0.0731 1.0238 0.048 Uiso 1 1 calc R . . H21B H 0.3587 0.0572 1.0070 0.048 Uiso 1 1 calc R . . H21C H 0.3723 -0.0447 0.9471 0.048 Uiso 1 1 calc R . . C22 C 0.1189(6) 0.2271(7) 1.0448(3) 0.0353(12) Uani 1 1 d . . . H22A H 0.0930 0.3211 1.0394 0.053 Uiso 1 1 calc R . . H22B H 0.2134 0.2181 1.0581 0.053 Uiso 1 1 calc R . . H22C H 0.0517 0.1744 1.0853 0.053 Uiso 1 1 calc R . . C23 C -0.0798(5) 0.3298(5) 0.9234(3) 0.0307(10) Uani 1 1 d . . . H23A H -0.1032 0.3641 0.8728 0.046 Uiso 1 1 calc R . . H23B H -0.0410 0.4025 0.9441 0.046 Uiso 1 1 calc R . . H23C H -0.1648 0.2928 0.9579 0.046 Uiso 1 1 calc R . . C24 C 0.2692(5) 0.4081(5) 0.7812(3) 0.0281(10) Uani 1 1 d . . . C25 C 0.3621(5) 0.3044(5) 0.7625(2) 0.0226(9) Uani 1 1 d . . . C26 C 0.4428(4) 0.2728(4) 0.8216(2) 0.0187(8) Uani 1 1 d . . . C27 C 0.4032(5) 0.3570(5) 0.8771(2) 0.0221(9) Uani 1 1 d . . . C28 C 0.2960(5) 0.4415(5) 0.8521(3) 0.0284(10) Uani 1 1 d . . . C29 C 0.1678(6) 0.4737(6) 0.7330(4) 0.0414(14) Uani 1 1 d . . . H29A H 0.0864 0.5028 0.7661 0.062 Uiso 1 1 calc R . . H29B H 0.1368 0.4101 0.7032 0.062 Uiso 1 1 calc R . . H29C H 0.2137 0.5512 0.6982 0.062 Uiso 1 1 calc R . . C30 C 0.3754(6) 0.2438(7) 0.6911(3) 0.0362(12) Uani 1 1 d . . . H30A H 0.4350 0.3018 0.6493 0.054 Uiso 1 1 calc R . . H30B H 0.2822 0.2340 0.6775 0.054 Uiso 1 1 calc R . . H30C H 0.4179 0.1560 0.6998 0.054 Uiso 1 1 calc R . . C31 C 0.5581(5) 0.1733(5) 0.8231(3) 0.0292(10) Uani 1 1 d . . . H31A H 0.6463 0.2161 0.7950 0.044 Uiso 1 1 calc R . . H31B H 0.5346 0.0983 0.7990 0.044 Uiso 1 1 calc R . . H31C H 0.5689 0.1406 0.8762 0.044 Uiso 1 1 calc R . . C32 C 0.4672(6) 0.3619(7) 0.9473(3) 0.0385(13) Uani 1 1 d . . . H32A H 0.5010 0.2734 0.9657 0.058 Uiso 1 1 calc R . . H32B H 0.3964 0.3891 0.9872 0.058 Uiso 1 1 calc R . . H32C H 0.5460 0.4263 0.9349 0.058 Uiso 1 1 calc R . . C33 C 0.2309(7) 0.5534(6) 0.8897(4) 0.0498(18) Uani 1 1 d . . . H33A H 0.2914 0.6335 0.8734 0.075 Uiso 1 1 calc R . . H33B H 0.2204 0.5281 0.9455 0.075 Uiso 1 1 calc R . . H33C H 0.1385 0.5719 0.8750 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02005(9) 0.01936(9) 0.01308(9) -0.00266(6) -0.00316(6) -0.00092(6) Cl1 0.0246(5) 0.0413(6) 0.0170(5) -0.0069(4) -0.0039(4) -0.0100(5) Cl2 0.0582(8) 0.0165(5) 0.0209(5) -0.0018(4) -0.0072(5) 0.0072(5) Cl3 0.0211(5) 0.0464(7) 0.0239(5) -0.0071(5) -0.0055(4) -0.0038(5) Cl4 0.0355(6) 0.0219(5) 0.0238(5) 0.0037(4) -0.0002(4) 0.0013(4) Cl5 0.0289(5) 0.0379(6) 0.0145(4) -0.0071(4) -0.0013(4) 0.0085(5) P1 0.0151(4) 0.0145(5) 0.0141(4) -0.0011(4) -0.0025(4) 0.0004(4) C1 0.0213(19) 0.0146(18) 0.0156(18) -0.0049(14) -0.0040(15) 0.0027(15) C2 0.023(2) 0.021(2) 0.0156(18) -0.0062(15) -0.0052(15) 0.0048(16) C3 0.034(2) 0.023(2) 0.0170(19) -0.0085(16) -0.0109(17) 0.0098(18) C4 0.048(3) 0.016(2) 0.0143(19) -0.0039(15) -0.0082(18) 0.0046(19) C5 0.035(2) 0.019(2) 0.017(2) -0.0017(16) 0.0012(17) -0.0036(18) C6 0.023(2) 0.022(2) 0.0174(19) -0.0036(16) -0.0013(16) -0.0001(16) C7 0.0177(18) 0.019(2) 0.0182(19) -0.0050(15) 0.0012(15) -0.0006(15) C8 0.031(2) 0.020(2) 0.023(2) -0.0044(17) 0.0003(18) 0.0020(18) C9 0.035(3) 0.019(2) 0.033(3) -0.0040(19) 0.010(2) -0.0012(19) C10 0.024(2) 0.025(2) 0.042(3) -0.019(2) 0.011(2) -0.0068(18) C11 0.019(2) 0.037(3) 0.034(3) -0.020(2) -0.0007(18) -0.0011(19) C12 0.0175(19) 0.025(2) 0.027(2) -0.0094(18) -0.0026(16) 0.0003(16) C13 0.0146(18) 0.025(2) 0.025(2) -0.0017(17) -0.0037(16) 0.0031(16) Co1 0.0163(2) 0.0140(2) 0.0118(2) -0.00298(19) -0.00296(19) 0.00225(19) C14 0.0182(18) 0.019(2) 0.022(2) -0.0050(16) -0.0056(15) 0.0018(15) C15 0.0186(19) 0.0138(18) 0.027(2) -0.0029(16) -0.0048(16) 0.0003(15) C16 0.0192(19) 0.022(2) 0.020(2) 0.0049(16) -0.0052(16) -0.0027(16) C17 0.0203(19) 0.028(2) 0.0158(19) -0.0015(16) -0.0009(15) -0.0061(17) C18 0.0178(18) 0.023(2) 0.022(2) -0.0072(17) -0.0018(16) -0.0007(16) C19 0.026(2) 0.036(3) 0.028(2) -0.008(2) -0.0135(19) 0.0014(19) C20 0.030(2) 0.019(2) 0.043(3) -0.015(2) -0.006(2) 0.0031(18) C21 0.030(2) 0.028(2) 0.035(3) 0.013(2) -0.012(2) -0.003(2) C22 0.033(3) 0.058(4) 0.015(2) -0.011(2) 0.0020(18) -0.009(2) C23 0.022(2) 0.031(3) 0.040(3) -0.014(2) -0.001(2) 0.0063(19) C24 0.021(2) 0.028(2) 0.029(2) 0.0130(19) -0.0028(18) 0.0004(18) C25 0.0197(19) 0.030(2) 0.0166(19) -0.0037(17) 0.0004(15) -0.0055(17) C26 0.0177(18) 0.0179(19) 0.0201(19) -0.0039(15) -0.0009(15) -0.0017(15) C27 0.023(2) 0.025(2) 0.0165(19) -0.0032(16) 0.0013(16) -0.0088(17) C28 0.026(2) 0.016(2) 0.039(3) -0.0079(19) 0.010(2) -0.0024(17) C29 0.026(2) 0.043(3) 0.047(3) 0.020(3) -0.008(2) 0.004(2) C30 0.031(3) 0.058(4) 0.021(2) -0.013(2) -0.0007(19) -0.006(2) C31 0.021(2) 0.026(2) 0.040(3) -0.003(2) -0.0038(19) 0.0026(18) C32 0.042(3) 0.054(4) 0.022(2) -0.012(2) -0.004(2) -0.021(3) C33 0.047(3) 0.020(3) 0.075(5) -0.020(3) 0.020(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 Cl2 2.3395(11) . ? W1 Cl4 2.3462(11) . ? W1 Cl3 2.3480(11) . ? W1 Cl1 2.3701(11) . ? W1 Cl5 2.4116(11) . ? W1 P1 2.5627(11) . ? P1 C13 1.810(4) . ? P1 C1 1.817(4) . ? P1 C7 1.829(4) . ? C1 C6 1.397(6) . ? C1 C2 1.397(6) . ? C2 C3 1.386(6) . ? C2 H2 0.9500 . ? C3 C4 1.395(7) . ? C3 H3 0.9500 . ? C4 C5 1.380(7) . ? C4 H4 0.9500 . ? C5 C6 1.400(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.386(6) . ? C7 C8 1.397(6) . ? C8 C9 1.380(7) . ? C8 H8 0.9500 . ? C9 C10 1.385(8) . ? C9 H9 0.9500 . ? C10 C11 1.379(8) . ? C10 H10 0.9500 . ? C11 C12 1.405(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? Co1 C24 2.040(5) . ? Co1 C18 2.043(4) . ? Co1 C17 2.044(4) . ? Co1 C16 2.045(4) . ? Co1 C28 2.049(5) . ? Co1 C15 2.050(4) . ? Co1 C14 2.052(4) . ? Co1 C26 2.060(4) . ? Co1 C27 2.060(4) . ? Co1 C25 2.061(4) . ? C14 C18 1.433(6) . ? C14 C15 1.436(6) . ? C14 C19 1.499(6) . ? C15 C16 1.430(6) . ? C15 C20 1.493(6) . ? C16 C17 1.434(7) . ? C16 C21 1.500(6) . ? C17 C18 1.428(6) . ? C17 C22 1.499(6) . ? C18 C23 1.500(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.427(7) . ? C24 C28 1.432(8) . ? C24 C29 1.493(7) . ? C25 C26 1.412(6) . ? C25 C30 1.495(7) . ? C26 C27 1.421(6) . ? C26 C31 1.500(6) . ? C27 C28 1.424(7) . ? C27 C32 1.499(7) . ? C28 C33 1.499(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 W1 Cl4 177.24(5) . . ? Cl2 W1 Cl3 90.45(5) . . ? Cl4 W1 Cl3 91.91(5) . . ? Cl2 W1 Cl1 89.21(5) . . ? Cl4 W1 Cl1 88.33(5) . . ? Cl3 W1 Cl1 175.86(4) . . ? Cl2 W1 Cl5 91.06(4) . . ? Cl4 W1 Cl5 90.27(4) . . ? Cl3 W1 Cl5 92.27(4) . . ? Cl1 W1 Cl5 91.86(4) . . ? Cl2 W1 P1 89.53(4) . . ? Cl4 W1 P1 89.17(4) . . ? Cl3 W1 P1 87.03(4) . . ? Cl1 W1 P1 88.84(4) . . ? Cl5 W1 P1 179.09(4) . . ? C13 P1 C1 105.0(2) . . ? C13 P1 C7 100.8(2) . . ? C1 P1 C7 105.38(19) . . ? C13 P1 W1 112.49(16) . . ? C1 P1 W1 115.03(13) . . ? C7 P1 W1 116.58(14) . . ? C6 C1 C2 119.0(4) . . ? C6 C1 P1 120.9(3) . . ? C2 C1 P1 120.1(3) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 120.1(4) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C12 C7 C8 119.4(4) . . ? C12 C7 P1 122.9(3) . . ? C8 C7 P1 117.7(3) . . ? C9 C8 C7 120.4(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.7(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.3(5) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 119.8(5) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C24 Co1 C18 113.36(19) . . ? C24 Co1 C17 143.4(2) . . ? C18 Co1 C17 40.89(17) . . ? C24 Co1 C16 175.0(2) . . ? C18 Co1 C16 68.82(18) . . ? C17 Co1 C16 41.04(19) . . ? C24 Co1 C28 41.0(2) . . ? C18 Co1 C28 110.41(18) . . ? C17 Co1 C28 113.42(19) . . ? C16 Co1 C28 143.2(2) . . ? C24 Co1 C15 135.0(2) . . ? C18 Co1 C15 69.11(18) . . ? C17 Co1 C15 69.18(18) . . ? C16 Co1 C15 40.88(18) . . ? C28 Co1 C15 175.7(2) . . ? C24 Co1 C14 109.80(19) . . ? C18 Co1 C14 40.95(17) . . ? C17 Co1 C14 68.88(17) . . ? C16 Co1 C14 68.67(17) . . ? C28 Co1 C14 136.03(19) . . ? C15 Co1 C14 40.97(16) . . ? C24 Co1 C26 68.16(18) . . ? C18 Co1 C26 175.88(17) . . ? C17 Co1 C26 135.72(18) . . ? C16 Co1 C26 109.99(17) . . ? C28 Co1 C26 68.01(18) . . ? C15 Co1 C26 112.77(17) . . ? C14 Co1 C26 142.76(17) . . ? C24 Co1 C27 68.57(19) . . ? C18 Co1 C27 136.04(18) . . ? C17 Co1 C27 110.20(17) . . ? C16 Co1 C27 113.25(18) . . ? C28 Co1 C27 40.6(2) . . ? C15 Co1 C27 142.57(18) . . ? C14 Co1 C27 176.19(18) . . ? C26 Co1 C27 40.37(17) . . ? C24 Co1 C25 40.7(2) . . ? C18 Co1 C25 143.43(18) . . ? C17 Co1 C25 175.19(19) . . ? C16 Co1 C25 135.00(19) . . ? C28 Co1 C25 68.32(19) . . ? C15 Co1 C25 109.38(19) . . ? C14 Co1 C25 113.27(18) . . ? C26 Co1 C25 40.09(17) . . ? C27 Co1 C25 67.95(17) . . ? C18 C14 C15 108.1(4) . . ? C18 C14 C19 126.3(4) . . ? C15 C14 C19 125.6(4) . . ? C18 C14 Co1 69.2(2) . . ? C15 C14 Co1 69.4(2) . . ? C19 C14 Co1 128.9(3) . . ? C16 C15 C14 107.5(4) . . ? C16 C15 C20 126.9(4) . . ? C14 C15 C20 125.6(4) . . ? C16 C15 Co1 69.4(2) . . ? C14 C15 Co1 69.6(2) . . ? C20 C15 Co1 127.3(3) . . ? C15 C16 C17 108.5(4) . . ? C15 C16 C21 126.4(4) . . ? C17 C16 C21 125.1(4) . . ? C15 C16 Co1 69.7(2) . . ? C17 C16 Co1 69.4(2) . . ? C21 C16 Co1 127.6(3) . . ? C18 C17 C16 107.7(4) . . ? C18 C17 C22 126.0(4) . . ? C16 C17 C22 126.2(4) . . ? C18 C17 Co1 69.5(2) . . ? C16 C17 Co1 69.5(2) . . ? C22 C17 Co1 128.5(3) . . ? C17 C18 C14 108.2(4) . . ? C17 C18 C23 125.5(4) . . ? C14 C18 C23 126.3(4) . . ? C17 C18 Co1 69.6(2) . . ? C14 C18 Co1 69.9(2) . . ? C23 C18 Co1 127.1(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C28 107.6(4) . . ? C25 C24 C29 125.6(5) . . ? C28 C24 C29 126.7(5) . . ? C25 C24 Co1 70.4(3) . . ? C28 C24 Co1 69.8(3) . . ? C29 C24 Co1 127.4(4) . . ? C26 C25 C24 108.0(4) . . ? C26 C25 C30 126.1(5) . . ? C24 C25 C30 125.9(5) . . ? C26 C25 Co1 69.9(2) . . ? C24 C25 Co1 68.9(3) . . ? C30 C25 Co1 128.7(4) . . ? C25 C26 C27 108.7(4) . . ? C25 C26 C31 125.7(4) . . ? C27 C26 C31 125.5(4) . . ? C25 C26 Co1 70.0(2) . . ? C27 C26 Co1 69.8(2) . . ? C31 C26 Co1 129.2(3) . . ? C26 C27 C28 107.7(4) . . ? C26 C27 C32 126.6(5) . . ? C28 C27 C32 125.7(5) . . ? C26 C27 Co1 69.8(2) . . ? C28 C27 Co1 69.3(3) . . ? C32 C27 Co1 128.7(3) . . ? C27 C28 C24 107.9(4) . . ? C27 C28 C33 126.1(5) . . ? C24 C28 C33 125.7(5) . . ? C27 C28 Co1 70.2(3) . . ? C24 C28 Co1 69.2(3) . . ? C33 C28 Co1 130.0(4) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.77 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 6.436 _refine_diff_density_min -2.032 _refine_diff_density_rms 0.162 #===END data_jpd349_0m _database_code_depnum_ccdc_archive 'CCDC 769400' #TrackingRef 'CombinedCIF-Donahue.cif' # Compound 6, [WCl3(NMe2)(PMePh2)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-Trichloro(dimethylamido)bis(methyldiphenylphosphine) tungsten(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H32 Cl3 N P2 W' _chemical_formula_sum 'C28 H32 Cl3 N P2 W' _chemical_formula_weight 734.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.8088(8) _cell_length_b 13.2473(8) _cell_length_c 16.0074(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.997(1) _cell_angle_gamma 90.00 _cell_volume 2921.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9845 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.68 _exptl_crystal_description Column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 4.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6553 _exptl_absorpt_correction_T_max 0.7925 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, collected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24988 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3526 _reflns_number_gt 3269 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _publ_section_references ; Bruker-AXS (2009). APEX2, Version 2009.9-0, Madison, WI. Bruker-AXS (2009a). SAINT, Version 7.68A, Madison, WI Bruker-AXS (2008). SHELXTL, Version 2008/4, Madison, WI Sheldrick, G. M. (2008). SHELXS and SHELXL. Acta Cryst. A64, 112-122. Sheldrick, G, M. (2008a). SADABS, Version 2008/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+3.1402P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3526 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0350 _refine_ls_wR_factor_gt 0.0339 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.5000 0.794647(8) 0.7500 0.01236(4) Uani 1 2 d S . . Cl1 Cl 0.34860(3) 0.78926(3) 0.66744(3) 0.01676(9) Uani 1 1 d . . . Cl2 Cl 0.5000 0.60970(5) 0.7500 0.01844(13) Uani 1 2 d S . . P1 P 0.59888(4) 0.77569(4) 0.62117(3) 0.01483(10) Uani 1 1 d . . . N1 N 0.5000 0.94020(16) 0.7500 0.0147(5) Uani 1 2 d S . . C1 C 0.53572(14) 0.72945(14) 0.52515(12) 0.0174(4) Uani 1 1 d . . . C2 C 0.45855(14) 0.78490(14) 0.48678(13) 0.0186(4) Uani 1 1 d . . . H2 H 0.4400 0.8470 0.5107 0.022 Uiso 1 1 calc R . . C3 C 0.40910(15) 0.74991(16) 0.41429(13) 0.0225(4) Uani 1 1 d . . . H3 H 0.3574 0.7885 0.3884 0.027 Uiso 1 1 calc R . . C4 C 0.43469(16) 0.65889(17) 0.37931(14) 0.0282(5) Uani 1 1 d . . . H4 H 0.4006 0.6351 0.3296 0.034 Uiso 1 1 calc R . . C5 C 0.51014(17) 0.60273(17) 0.41713(15) 0.0317(5) Uani 1 1 d . . . H5 H 0.5275 0.5401 0.3935 0.038 Uiso 1 1 calc R . . C6 C 0.56042(16) 0.63779(16) 0.48945(14) 0.0260(5) Uani 1 1 d . . . H6 H 0.6122 0.5989 0.5149 0.031 Uiso 1 1 calc R . . C7 C 0.66177(13) 0.89074(14) 0.59260(12) 0.0163(4) Uani 1 1 d . . . C8 C 0.65983(14) 0.92809(14) 0.51135(12) 0.0176(4) Uani 1 1 d . . . H8 H 0.6215 0.8954 0.4678 0.021 Uiso 1 1 calc R . . C9 C 0.71383(15) 1.01312(15) 0.49356(13) 0.0205(4) Uani 1 1 d . . . H9 H 0.7123 1.0380 0.4378 0.025 Uiso 1 1 calc R . . C10 C 0.76978(15) 1.06170(15) 0.55647(13) 0.0213(4) Uani 1 1 d . . . H10 H 0.8070 1.1194 0.5439 0.026 Uiso 1 1 calc R . . C11 C 0.77125(15) 1.02563(16) 0.63800(13) 0.0225(4) Uani 1 1 d . . . H11 H 0.8090 1.0592 0.6814 0.027 Uiso 1 1 calc R . . C12 C 0.71790(15) 0.94098(15) 0.65634(13) 0.0212(4) Uani 1 1 d . . . H12 H 0.7192 0.9167 0.7123 0.025 Uiso 1 1 calc R . . C13 C 0.69998(15) 0.68912(15) 0.64221(13) 0.0224(4) Uani 1 1 d . . . H13A H 0.7381 0.6851 0.5929 0.034 Uiso 1 1 calc R . . H13B H 0.6750 0.6220 0.6549 0.034 Uiso 1 1 calc R . . H13C H 0.7413 0.7137 0.6902 0.034 Uiso 1 1 calc R . . C14 C 0.47102(15) 1.00473(15) 0.67785(12) 0.0206(4) Uani 1 1 d . . . H14A H 0.4119 1.0419 0.6890 0.031 Uiso 1 1 calc R . . H14B H 0.4586 0.9627 0.6279 0.031 Uiso 1 1 calc R . . H14C H 0.5232 1.0527 0.6686 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01299(6) 0.01261(5) 0.01116(6) 0.000 -0.00134(4) 0.000 Cl1 0.0154(2) 0.0190(2) 0.0153(2) 0.00025(17) -0.00344(17) -0.00085(17) Cl2 0.0199(3) 0.0130(3) 0.0218(3) 0.000 -0.0033(3) 0.000 P1 0.0143(2) 0.0163(2) 0.0137(2) -0.00132(17) -0.00063(19) 0.00121(17) N1 0.0157(11) 0.0139(10) 0.0140(11) 0.000 -0.0030(9) 0.000 C1 0.0169(10) 0.0193(9) 0.0159(10) -0.0032(7) 0.0010(8) -0.0017(7) C2 0.0182(10) 0.0195(10) 0.0179(10) -0.0011(7) 0.0003(8) 0.0003(7) C3 0.0210(11) 0.0249(10) 0.0212(11) 0.0010(8) -0.0018(9) -0.0001(8) C4 0.0273(12) 0.0346(12) 0.0219(12) -0.0094(9) -0.0038(9) -0.0035(9) C5 0.0310(12) 0.0287(12) 0.0345(13) -0.0175(10) -0.0037(10) 0.0043(9) C6 0.0229(11) 0.0252(11) 0.0292(12) -0.0080(9) -0.0033(9) 0.0056(9) C7 0.0127(9) 0.0187(9) 0.0177(10) -0.0025(7) 0.0014(8) 0.0003(7) C8 0.0163(9) 0.0205(10) 0.0159(10) -0.0032(7) -0.0002(8) 0.0017(7) C9 0.0215(10) 0.0215(10) 0.0186(10) 0.0010(8) 0.0015(8) 0.0034(8) C10 0.0189(10) 0.0172(9) 0.0281(12) -0.0007(8) 0.0049(9) -0.0018(7) C11 0.0192(10) 0.0269(11) 0.0213(11) -0.0058(8) 0.0002(9) -0.0028(8) C12 0.0200(10) 0.0267(10) 0.0168(10) -0.0023(8) 0.0001(8) -0.0022(8) C13 0.0210(10) 0.0245(11) 0.0213(11) -0.0025(8) -0.0016(8) 0.0061(8) C14 0.0242(11) 0.0180(9) 0.0191(10) 0.0025(8) -0.0026(9) 0.0012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N1 1.928(2) . ? W1 Cl1 2.3953(4) . ? W1 Cl1 2.3953(4) 2_656 ? W1 Cl2 2.4500(6) . ? W1 P1 2.5638(5) . ? W1 P1 2.5638(5) 2_656 ? P1 C1 1.820(2) . ? P1 C13 1.820(2) . ? P1 C7 1.828(2) . ? N1 C14 1.470(2) 2_656 ? N1 C14 1.470(2) . ? C1 C6 1.394(3) . ? C1 C2 1.400(3) . ? C2 C3 1.385(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.390(3) . ? C7 C12 1.405(3) . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.389(3) . ? C10 H10 0.9500 . ? C11 C12 1.384(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 W1 Cl1 91.708(11) . . ? N1 W1 Cl1 91.707(11) . 2_656 ? Cl1 W1 Cl1 176.58(2) . 2_656 ? N1 W1 Cl2 180.0 . . ? Cl1 W1 Cl2 88.292(11) . . ? Cl1 W1 Cl2 88.293(11) 2_656 . ? N1 W1 P1 95.623(11) . . ? Cl1 W1 P1 92.671(16) . . ? Cl1 W1 P1 86.994(16) 2_656 . ? Cl2 W1 P1 84.377(11) . . ? N1 W1 P1 95.622(11) . 2_656 ? Cl1 W1 P1 86.993(16) . 2_656 ? Cl1 W1 P1 92.672(16) 2_656 2_656 ? Cl2 W1 P1 84.378(11) . 2_656 ? P1 W1 P1 168.76(2) . 2_656 ? C1 P1 C13 105.10(9) . . ? C1 P1 C7 106.11(9) . . ? C13 P1 C7 101.53(9) . . ? C1 P1 W1 117.49(7) . . ? C13 P1 W1 110.95(7) . . ? C7 P1 W1 114.11(6) . . ? C14 N1 C14 108.9(2) 2_656 . ? C14 N1 W1 125.57(10) 2_656 . ? C14 N1 W1 125.57(10) . . ? C6 C1 C2 118.52(18) . . ? C6 C1 P1 121.51(16) . . ? C2 C1 P1 119.94(14) . . ? C3 C2 C1 120.51(19) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.3(2) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.2(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.7(2) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C8 C7 C12 118.98(18) . . ? C8 C7 P1 123.53(15) . . ? C12 C7 P1 117.45(15) . . ? C7 C8 C9 120.27(18) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.49(19) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.64(19) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.32(19) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 120.30(19) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 H14A 109.5 . . ? N1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.837 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.080 #===END