# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Paul Low' _publ_contact_author_email P.J.LOW@DURHAM.AC.UK _publ_section_title ; Some transition metal complexes derived from mono- and di-ethynyl perfluorobenzenes ; loop_ _publ_author_name 'Paul Low' 'David J Armitt' 'M Bruce' 'Mark Fox' 'Maryka Gaudio' 'J Halet' 'Boris Le Guennic' ; B.W.Skelton ; 'A H White' 'Natasha N. Zaitseva' #===END data_br1282_compound_6 _database_code_depnum_ccdc_archive 'CCDC 656421' _audit_creation_date 2006-07-14T14:55:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #--------------------------------------------------------------------------- # CHEMICAL INFORMATION # #--------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_sum 'C41 H22 Co3 F5 O7 P2' _chemical_formula_moiety 'C41 H22 Co3 F5 O7 P2' _chemical_formula_weight 960.32 #--------------------------------------------------------------------------- # UNIT CELL INFORMATION # #--------------------------------------------------------------------------- _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 11.6170(10) _cell_length_b 17.643(2) _cell_length_c 19.108(3) _cell_angle_alpha 97.855(9) _cell_angle_beta 91.445(11) _cell_angle_gamma 93.438(7) _cell_volume 3870.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 35639 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 34.1063 #--------------------------------------------------------------------------- # CRYSTAL INFORMATION # #-------------------------------------------------------------------------- _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- # ABSORPTION CORRECTION # #--------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 1.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.91814 _exptl_absorpt_correction_T_max 1 #-------------------------------------------------------------------------- # DATA COLLECTION # #--------------------------------------------------------------------------- _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0283055087 _diffrn_orient_matrix_ub_12 0.0098214312 _diffrn_orient_matrix_ub_13 0.0321844559 _diffrn_orient_matrix_ub_21 -0.0422159249 _diffrn_orient_matrix_ub_22 0.0181802051 _diffrn_orient_matrix_ub_23 -0.0181926576 _diffrn_orient_matrix_ub_31 -0.0343438482 _diffrn_orient_matrix_ub_32 -0.0351391959 _diffrn_orient_matrix_ub_33 -0.0064131153 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_unetI/netI 0.0536 _diffrn_reflns_number 76417 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 34.14 _diffrn_reflns_theta_full 34.14 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 29976 _reflns_number_gt 20530 _reflns_threshold_expression >2sigma(I) #--------------------------------------------------------------------------- # COMPUTER PROGRAMS USED # #--------------------------------------------------------------------------- _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET) (compiled Jun 12 2006,17:01:16) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #--------------------------------------------------------------------------- # REFINEMENT INFORMATION # #--------------------------------------------------------------------------- _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^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 29976 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.694 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.083 #--------------------------------------------------------------------------- # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #--------------------------------------------------------------------------- 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Co1 Co 0.370384(16) 0.598379(10) 0.278160(10) 0.01176(4) Uani 1 1 d . . . Co2 Co 0.421385(16) 0.547656(11) 0.156259(10) 0.01224(4) Uani 1 1 d . . . Co3 Co 0.555361(16) 0.642526(11) 0.230260(11) 0.01306(4) Uani 1 1 d . . . C11 C 0.27107(13) 0.66022(8) 0.24499(8) 0.0168(3) Uani 1 1 d . . . O11 O 0.20985(10) 0.69980(7) 0.22174(6) 0.0252(3) Uani 1 1 d . . . C12 C 0.39450(13) 0.64001(9) 0.36797(8) 0.0190(3) Uani 1 1 d . . . O12 O 0.40627(11) 0.66758(7) 0.42566(7) 0.0319(3) Uani 1 1 d . . . C21 C 0.35538(13) 0.60736(8) 0.09827(8) 0.0169(3) Uani 1 1 d . . . O21 O 0.31642(10) 0.64585(7) 0.06157(6) 0.0251(3) Uani 1 1 d . . . C22 C 0.52423(13) 0.50248(9) 0.09883(8) 0.0189(3) Uani 1 1 d . . . O22 O 0.59158(10) 0.47396(7) 0.06321(7) 0.0287(3) Uani 1 1 d . . . C31 C 0.49777(13) 0.72353(8) 0.19614(8) 0.0172(3) Uani 1 1 d . . . O31 O 0.45792(10) 0.77313(6) 0.17352(7) 0.0252(3) Uani 1 1 d . . . C32 C 0.68019(13) 0.62250(9) 0.17987(9) 0.0193(3) Uani 1 1 d . . . O32 O 0.75976(10) 0.60975(7) 0.14693(7) 0.0295(3) Uani 1 1 d . . . C33 C 0.62685(13) 0.68799(9) 0.31125(9) 0.0208(3) Uani 1 1 d . . . O33 O 0.67457(12) 0.71942(8) 0.36077(7) 0.0334(3) Uani 1 1 d . . . C1 C 0.49604(12) 0.54069(8) 0.24539(8) 0.0131(3) Uani 1 1 d . . . C2 C 0.55870(12) 0.48275(8) 0.26861(8) 0.0140(3) Uani 1 1 d . . . C3 C 0.61152(13) 0.43215(8) 0.28887(9) 0.0184(3) Uani 1 1 d . . . C131 C 0.67918(12) 0.37684(8) 0.31562(8) 0.0157(3) Uani 1 1 d . . . C132 C 0.71809(14) 0.38545(9) 0.38576(9) 0.0222(3) Uani 1 1 d . . . C133 C 0.78844(16) 0.33402(11) 0.41120(9) 0.0272(4) Uani 1 1 d . . . C134 C 0.82115(15) 0.27155(10) 0.36592(10) 0.0257(4) Uani 1 1 d . . . C135 C 0.78295(14) 0.26018(9) 0.29653(9) 0.0225(3) Uani 1 1 d . . . C136 C 0.71351(13) 0.31248(9) 0.27199(8) 0.0185(3) Uani 1 1 d . . . F132 F 0.68845(10) 0.44575(6) 0.43055(6) 0.0344(3) Uani 1 1 d . . . F133 F 0.82619(11) 0.34493(7) 0.47926(6) 0.0453(3) Uani 1 1 d . . . F134 F 0.88961(10) 0.22163(6) 0.39072(6) 0.0398(3) Uani 1 1 d . . . F135 F 0.81257(9) 0.19875(6) 0.25295(6) 0.0317(2) Uani 1 1 d . . . F136 F 0.68074(9) 0.30171(6) 0.20336(5) 0.0272(2) Uani 1 1 d . . . P1 P 0.25269(3) 0.50270(2) 0.30032(2) 0.01284(7) Uani 1 1 d . . . C111 C 0.27031(14) 0.46199(8) 0.38234(8) 0.0178(3) Uani 1 1 d . . . C112 C 0.38110(15) 0.45606(10) 0.41011(8) 0.0229(3) Uani 1 1 d . . . H112 H 0.4456 0.4794 0.3898 0.027 Uiso 1 1 calc R . . C113 C 0.39801(18) 0.41637(10) 0.46723(9) 0.0301(4) Uani 1 1 d . . . H113 H 0.4739 0.4119 0.4852 0.036 Uiso 1 1 calc R . . C114 C 0.3049(2) 0.38349(11) 0.49772(10) 0.0367(5) Uani 1 1 d . . . H114 H 0.3167 0.356 0.5365 0.044 Uiso 1 1 calc R . . C115 C 0.1943(2) 0.39034(12) 0.47213(10) 0.0400(5) Uani 1 1 d . . . H115 H 0.1303 0.3684 0.4939 0.048 Uiso 1 1 calc R . . C116 C 0.17625(16) 0.42933(10) 0.41439(9) 0.0292(4) Uani 1 1 d . . . H116 H 0.1 0.4337 0.3969 0.035 Uiso 1 1 calc R . . C121 C 0.09995(12) 0.52136(8) 0.29889(8) 0.0151(3) Uani 1 1 d . . . C122 C 0.01383(13) 0.46947(9) 0.26448(8) 0.0184(3) Uani 1 1 d . . . H122 H 0.0339 0.422 0.2396 0.022 Uiso 1 1 calc R . . C123 C -0.10142(13) 0.48757(9) 0.26676(9) 0.0208(3) Uani 1 1 d . . . H123 H -0.1593 0.453 0.2422 0.025 Uiso 1 1 calc R . . C124 C -0.13201(14) 0.55543(10) 0.30451(9) 0.0244(3) Uani 1 1 d . . . H124 H -0.2108 0.567 0.3064 0.029 Uiso 1 1 calc R . . C125 C -0.04722(15) 0.60701(10) 0.33976(10) 0.0273(4) Uani 1 1 d . . . H125 H -0.0682 0.6535 0.3661 0.033 Uiso 1 1 calc R . . C126 C 0.06818(14) 0.59034(9) 0.33624(9) 0.0210(3) Uani 1 1 d . . . H126 H 0.1259 0.6261 0.3594 0.025 Uiso 1 1 calc R . . C10 C 0.27365(12) 0.41824(8) 0.23559(7) 0.0140(3) Uani 1 1 d . . . H10A H 0.2048 0.382 0.2332 0.017 Uiso 1 1 calc R . . H10B H 0.3411 0.3919 0.2505 0.017 Uiso 1 1 calc R . . P2 P 0.29714(3) 0.44718(2) 0.14793(2) 0.01221(7) Uani 1 1 d . . . C211 C 0.35118(12) 0.36344(8) 0.09536(8) 0.0142(3) Uani 1 1 d . . . C212 C 0.43053(13) 0.31900(8) 0.12462(8) 0.0178(3) Uani 1 1 d . . . H212 H 0.4488 0.3279 0.1739 0.021 Uiso 1 1 calc R . . C213 C 0.48294(14) 0.26154(9) 0.08143(8) 0.0199(3) Uani 1 1 d . . . H213 H 0.5367 0.2314 0.1014 0.024 Uiso 1 1 calc R . . C214 C 0.45669(14) 0.24855(9) 0.00964(9) 0.0213(3) Uani 1 1 d . . . H214 H 0.4931 0.2098 -0.0197 0.026 Uiso 1 1 calc R . . C215 C 0.37749(14) 0.29186(9) -0.01955(8) 0.0215(3) Uani 1 1 d . . . H215 H 0.3584 0.282 -0.0687 0.026 Uiso 1 1 calc R . . C216 C 0.32591(13) 0.34952(9) 0.02272(8) 0.0188(3) Uani 1 1 d . . . H216 H 0.273 0.3798 0.0022 0.023 Uiso 1 1 calc R . . C221 C 0.14931(12) 0.44818(9) 0.11311(8) 0.0161(3) Uani 1 1 d . . . C222 C 0.08209(14) 0.37853(10) 0.09781(9) 0.0228(3) Uani 1 1 d . . . H222 H 0.1163 0.3314 0.1007 0.027 Uiso 1 1 calc R . . C223 C -0.03365(15) 0.37842(11) 0.07861(10) 0.0300(4) Uani 1 1 d . . . H223 H -0.0785 0.3312 0.0684 0.036 Uiso 1 1 calc R . . C224 C -0.08461(15) 0.44687(12) 0.07425(10) 0.0310(4) Uani 1 1 d . . . H224 H -0.1642 0.4465 0.0613 0.037 Uiso 1 1 calc R . . C225 C -0.01910(15) 0.51579(11) 0.08889(9) 0.0271(4) Uani 1 1 d . . . H225 H -0.0538 0.5627 0.0856 0.033 Uiso 1 1 calc R . . C226 C 0.09741(13) 0.51661(9) 0.10833(8) 0.0197(3) Uani 1 1 d . . . H226 H 0.1417 0.5641 0.1184 0.024 Uiso 1 1 calc R . . Co4 Co 0.122581(17) 0.056662(11) 0.271561(11) 0.01381(4) Uani 1 1 d . . . Co5 Co 0.306767(17) 0.089012(11) 0.214829(11) 0.01339(4) Uani 1 1 d . . . Co6 Co 0.234320(17) 0.179168(11) 0.313258(11) 0.01503(4) Uani 1 1 d . . . C41 C 0.01526(14) 0.07984(9) 0.20915(9) 0.0237(3) Uani 1 1 d . . . O41 O -0.05168(13) 0.09556(8) 0.16975(8) 0.0412(4) Uani 1 1 d . . . C42 C 0.04203(14) 0.05935(9) 0.35050(9) 0.0216(3) Uani 1 1 d . . . O42 O -0.00623(12) 0.06296(7) 0.40193(7) 0.0346(3) Uani 1 1 d . . . C51 C 0.24150(14) 0.13268(9) 0.14525(9) 0.0215(3) Uani 1 1 d . . . O51 O 0.19740(12) 0.16357(8) 0.10397(7) 0.0352(3) Uani 1 1 d . . . C52 C 0.45575(14) 0.12358(9) 0.21572(8) 0.0185(3) Uani 1 1 d . . . O52 O 0.55042(10) 0.14463(7) 0.21621(7) 0.0280(3) Uani 1 1 d . . . C61 C 0.12520(14) 0.23064(9) 0.27391(9) 0.0227(3) Uani 1 1 d . . . O61 O 0.05684(11) 0.26444(7) 0.25026(8) 0.0344(3) Uani 1 1 d . . . C62 C 0.35911(14) 0.24414(9) 0.31265(8) 0.0191(3) Uani 1 1 d . . . O62 O 0.43691(10) 0.28679(6) 0.31160(7) 0.0254(3) Uani 1 1 d . . . C63 C 0.20973(14) 0.19230(9) 0.40681(9) 0.0215(3) Uani 1 1 d . . . O63 O 0.19765(11) 0.19893(8) 0.46609(7) 0.0326(3) Uani 1 1 d . . . C4 C 0.27754(12) 0.07417(8) 0.30916(8) 0.0141(3) Uani 1 1 d . . . C5 C 0.32340(12) 0.03681(8) 0.36289(8) 0.0162(3) Uani 1 1 d . . . C6 C 0.35314(13) -0.00012(9) 0.40820(8) 0.0194(3) Uani 1 1 d . . . C231 C 0.37395(13) -0.04649(9) 0.46245(8) 0.0189(3) Uani 1 1 d . . . C232 C 0.31405(15) -0.03810(9) 0.52534(9) 0.0232(3) Uani 1 1 d . . . C233 C 0.33125(16) -0.08429(10) 0.57718(9) 0.0273(4) Uani 1 1 d . . . C234 C 0.41063(16) -0.13985(10) 0.56719(10) 0.0292(4) Uani 1 1 d . . . C235 C 0.47200(15) -0.14960(9) 0.50645(10) 0.0265(4) Uani 1 1 d . . . C236 C 0.45285(14) -0.10354(9) 0.45476(9) 0.0226(3) Uani 1 1 d . . . F232 F 0.23825(9) 0.01621(6) 0.53621(6) 0.0331(2) Uani 1 1 d . . . F233 F 0.27243(11) -0.07509(7) 0.63675(6) 0.0428(3) Uani 1 1 d . . . F234 F 0.42889(11) -0.18341(7) 0.61821(6) 0.0440(3) Uani 1 1 d . . . F235 F 0.55077(10) -0.20237(6) 0.49834(7) 0.0391(3) Uani 1 1 d . . . F236 F 0.51352(9) -0.11423(6) 0.39569(6) 0.0326(2) Uani 1 1 d . . . P4 P 0.12738(3) -0.06897(2) 0.24684(2) 0.01248(7) Uani 1 1 d . . . C411 C 0.08951(13) -0.12258(8) 0.31889(8) 0.0157(3) Uani 1 1 d . . . C412 C -0.02344(13) -0.12139(9) 0.34226(9) 0.0208(3) Uani 1 1 d . . . H412 H -0.0788 -0.0957 0.3185 0.025 Uiso 1 1 calc R . . C413 C -0.05587(15) -0.15725(10) 0.39962(9) 0.0251(3) Uani 1 1 d . . . H413 H -0.1333 -0.1567 0.4145 0.03 Uiso 1 1 calc R . . C414 C 0.02581(15) -0.19439(9) 0.43570(9) 0.0245(3) Uani 1 1 d . . . H414 H 0.0045 -0.2181 0.4757 0.029 Uiso 1 1 calc R . . C415 C 0.13744(15) -0.19622(9) 0.41258(9) 0.0222(3) Uani 1 1 d . . . H415 H 0.1928 -0.2218 0.4365 0.027 Uiso 1 1 calc R . . C416 C 0.16968(13) -0.16090(8) 0.35460(8) 0.0175(3) Uani 1 1 d . . . H416 H 0.2467 -0.1628 0.3391 0.021 Uiso 1 1 calc R . . C421 C 0.04288(12) -0.12018(8) 0.17085(8) 0.0139(3) Uani 1 1 d . . . C422 C 0.00402(13) -0.19750(9) 0.16820(9) 0.0187(3) Uani 1 1 d . . . H422 H 0.0173 -0.2235 0.2078 0.022 Uiso 1 1 calc R . . C423 C -0.05355(14) -0.23599(9) 0.10814(9) 0.0239(3) Uani 1 1 d . . . H423 H -0.0797 -0.2882 0.1068 0.029 Uiso 1 1 calc R . . C424 C -0.07340(14) -0.19876(9) 0.04962(9) 0.0228(3) Uani 1 1 d . . . H424 H -0.1131 -0.2253 0.0086 0.027 Uiso 1 1 calc R . . C425 C -0.03449(13) -0.12226(9) 0.05181(8) 0.0201(3) Uani 1 1 d . . . H425 H -0.0472 -0.0967 0.0119 0.024 Uiso 1 1 calc R . . C426 C 0.02239(12) -0.08343(8) 0.11150(8) 0.0161(3) Uani 1 1 d . . . H426 H 0.048 -0.0311 0.1125 0.019 Uiso 1 1 calc R . . C20 C 0.27473(12) -0.09549(8) 0.22744(8) 0.0137(3) Uani 1 1 d . . . H20A H 0.2729 -0.1488 0.203 0.016 Uiso 1 1 calc R . . H20B H 0.321 -0.0926 0.2721 0.016 Uiso 1 1 calc R . . P5 P 0.34111(3) -0.02976(2) 0.17106(2) 0.01321(7) Uani 1 1 d . . . C511 C 0.49287(12) -0.05303(8) 0.17568(8) 0.0149(3) Uani 1 1 d . . . C512 C 0.54763(13) -0.05051(9) 0.24220(9) 0.0221(3) Uani 1 1 d . . . H512 H 0.5082 -0.033 0.2837 0.026 Uiso 1 1 calc R . . C513 C 0.65922(14) -0.07349(10) 0.24756(10) 0.0275(4) Uani 1 1 d . . . H513 H 0.6955 -0.0728 0.2928 0.033 Uiso 1 1 calc R . . C514 C 0.71860(14) -0.09772(10) 0.18643(10) 0.0270(4) Uani 1 1 d . . . H514 H 0.7945 -0.1144 0.1901 0.032 Uiso 1 1 calc R . . C515 C 0.66636(14) -0.09728(9) 0.12122(10) 0.0240(3) Uani 1 1 d . . . H515 H 0.7072 -0.1127 0.0797 0.029 Uiso 1 1 calc R . . C516 C 0.55409(13) -0.07447(8) 0.11521(8) 0.0182(3) Uani 1 1 d . . . H516 H 0.5193 -0.0736 0.0698 0.022 Uiso 1 1 calc R . . C521 C 0.29588(12) -0.07307(8) 0.08117(8) 0.0151(3) Uani 1 1 d . . . C522 C 0.28264(13) -0.15261(9) 0.06377(8) 0.0185(3) Uani 1 1 d . . . H522 H 0.2944 -0.1843 0.0994 0.022 Uiso 1 1 calc R . . C523 C 0.25257(13) -0.18619(9) -0.00481(8) 0.0196(3) Uani 1 1 d . . . H523 H 0.2446 -0.2404 -0.0158 0.023 Uiso 1 1 calc R . . C524 C 0.23411(15) -0.14058(10) -0.05721(9) 0.0237(3) Uani 1 1 d . . . H524 H 0.213 -0.1634 -0.1041 0.028 Uiso 1 1 calc R . . C525 C 0.24678(16) -0.06116(10) -0.04050(9) 0.0276(4) Uani 1 1 d . . . H525 H 0.2336 -0.0297 -0.0761 0.033 Uiso 1 1 calc R . . C526 C 0.27845(15) -0.02744(9) 0.02772(9) 0.0225(3) Uani 1 1 d . . . H526 H 0.2884 0.0268 0.0383 0.027 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 Co1 0.01101(9) 0.01053(8) 0.01381(9) 0.00139(7) 0.00067(7) 0.00181(7) Co2 0.01243(9) 0.01121(8) 0.01339(9) 0.00226(7) 0.00112(7) 0.00174(7) Co3 0.01153(9) 0.01112(8) 0.01683(10) 0.00300(7) 0.00042(7) 0.00087(7) C11 0.0143(7) 0.0157(7) 0.0199(7) 0.0004(5) 0.0035(5) -0.0001(5) O11 0.0263(6) 0.0228(6) 0.0288(7) 0.0074(5) 0.0008(5) 0.0114(5) C12 0.0192(7) 0.0174(7) 0.0198(8) 0.0005(6) -0.0012(6) -0.0002(6) O12 0.0365(7) 0.0344(7) 0.0217(6) -0.0047(5) -0.0014(5) -0.0019(6) C21 0.0178(7) 0.0155(7) 0.0164(7) 0.0000(5) 0.0006(5) -0.0010(5) O21 0.0290(6) 0.0223(6) 0.0259(6) 0.0097(5) -0.0039(5) 0.0045(5) C22 0.0192(7) 0.0177(7) 0.0190(8) 0.0015(6) -0.0004(6) -0.0008(6) O22 0.0227(6) 0.0317(7) 0.0302(7) -0.0032(5) 0.0081(5) 0.0026(5) C31 0.0155(7) 0.0141(6) 0.0216(8) 0.0017(5) 0.0012(6) 0.0000(5) O31 0.0239(6) 0.0180(5) 0.0349(7) 0.0078(5) -0.0021(5) 0.0034(5) C32 0.0182(7) 0.0170(7) 0.0236(8) 0.0064(6) 0.0007(6) 0.0005(6) O32 0.0192(6) 0.0337(7) 0.0372(7) 0.0073(6) 0.0105(5) 0.0049(5) C33 0.0173(7) 0.0216(7) 0.0245(8) 0.0070(6) 0.0022(6) 0.0008(6) O33 0.0386(8) 0.0351(7) 0.0245(7) 0.0034(5) -0.0072(6) -0.0082(6) C1 0.0114(6) 0.0118(6) 0.0160(7) 0.0015(5) 0.0009(5) 0.0009(5) C2 0.0126(6) 0.0141(6) 0.0146(7) 0.0006(5) 0.0010(5) -0.0010(5) C3 0.0152(7) 0.0149(7) 0.0260(8) 0.0052(6) 0.0034(6) 0.0025(5) C131 0.0125(6) 0.0145(6) 0.0213(7) 0.0058(5) 0.0020(5) 0.0030(5) C132 0.0244(8) 0.0206(7) 0.0220(8) 0.0015(6) 0.0001(6) 0.0085(6) C133 0.0307(9) 0.0323(9) 0.0195(8) 0.0056(7) -0.0074(7) 0.0071(7) C134 0.0224(8) 0.0229(8) 0.0341(10) 0.0094(7) -0.0032(7) 0.0096(6) C135 0.0193(8) 0.0151(7) 0.0330(9) 0.0006(6) 0.0019(6) 0.0054(6) C136 0.0154(7) 0.0178(7) 0.0226(8) 0.0039(6) -0.0015(6) 0.0020(5) F132 0.0447(7) 0.0314(6) 0.0257(6) -0.0065(4) -0.0037(5) 0.0179(5) F133 0.0585(8) 0.0555(8) 0.0236(6) 0.0060(5) -0.0124(5) 0.0227(6) F134 0.0436(7) 0.0329(6) 0.0469(7) 0.0134(5) -0.0110(6) 0.0227(5) F135 0.0288(5) 0.0225(5) 0.0425(7) -0.0048(4) -0.0014(5) 0.0127(4) F136 0.0299(5) 0.0304(5) 0.0204(5) -0.0022(4) -0.0060(4) 0.0093(4) P1 0.01327(17) 0.01231(16) 0.01311(17) 0.00201(13) 0.00107(13) 0.00130(13) C111 0.0259(8) 0.0132(6) 0.0143(7) 0.0012(5) 0.0025(6) 0.0024(6) C112 0.0292(9) 0.0259(8) 0.0143(7) 0.0022(6) 0.0012(6) 0.0091(7) C113 0.0443(11) 0.0295(9) 0.0175(8) 0.0027(7) -0.0035(7) 0.0138(8) C114 0.0673(15) 0.0249(9) 0.0188(9) 0.0084(7) -0.0056(9) 0.0010(9) C115 0.0548(13) 0.0397(11) 0.0269(10) 0.0178(8) 0.0005(9) -0.0152(10) C116 0.0309(9) 0.0334(9) 0.0243(9) 0.0115(7) 0.0024(7) -0.0078(8) C121 0.0128(6) 0.0166(7) 0.0165(7) 0.0033(5) 0.0026(5) 0.0017(5) C122 0.0153(7) 0.0196(7) 0.0204(8) 0.0031(6) 0.0040(6) 0.0010(6) C123 0.0130(7) 0.0265(8) 0.0229(8) 0.0048(6) 0.0031(6) -0.0030(6) C124 0.0168(7) 0.0272(8) 0.0307(9) 0.0077(7) 0.0043(6) 0.0047(6) C125 0.0226(8) 0.0208(8) 0.0381(10) 0.0001(7) 0.0087(7) 0.0045(6) C126 0.0176(7) 0.0178(7) 0.0267(8) -0.0008(6) 0.0049(6) 0.0011(6) C10 0.0152(7) 0.0127(6) 0.0146(7) 0.0033(5) 0.0028(5) 0.0024(5) P2 0.01244(16) 0.01108(15) 0.01308(17) 0.00108(12) 0.00063(13) 0.00177(12) C211 0.0147(6) 0.0117(6) 0.0156(7) 0.0001(5) 0.0011(5) 0.0003(5) C212 0.0199(7) 0.0175(7) 0.0162(7) 0.0012(5) 0.0001(6) 0.0053(6) C213 0.0193(7) 0.0184(7) 0.0222(8) 0.0008(6) 0.0021(6) 0.0077(6) C214 0.0222(8) 0.0178(7) 0.0228(8) -0.0035(6) 0.0026(6) 0.0052(6) C215 0.0243(8) 0.0239(8) 0.0151(7) -0.0019(6) 0.0008(6) 0.0020(6) C216 0.0204(7) 0.0185(7) 0.0176(7) 0.0012(5) 0.0032(6) 0.0045(6) C221 0.0132(6) 0.0202(7) 0.0147(7) 0.0012(5) 0.0011(5) 0.0022(5) C222 0.0180(7) 0.0227(8) 0.0256(8) -0.0034(6) 0.0001(6) 0.0008(6) C223 0.0190(8) 0.0383(10) 0.0290(9) -0.0056(7) -0.0024(7) -0.0047(7) C224 0.0145(8) 0.0533(12) 0.0249(9) 0.0030(8) -0.0010(6) 0.0056(8) C225 0.0217(8) 0.0370(10) 0.0257(9) 0.0105(7) 0.0031(7) 0.0110(7) C226 0.0168(7) 0.0254(8) 0.0177(7) 0.0041(6) 0.0018(6) 0.0049(6) Co4 0.01152(9) 0.01162(9) 0.01815(10) 0.00114(7) 0.00041(7) 0.00167(7) Co5 0.01311(9) 0.01186(9) 0.01551(10) 0.00255(7) 0.00114(7) 0.00160(7) Co6 0.01587(10) 0.01105(9) 0.01798(10) 0.00109(7) 0.00167(7) 0.00098(7) C41 0.0227(8) 0.0164(7) 0.0308(9) -0.0031(6) -0.0040(7) 0.0080(6) O41 0.0438(8) 0.0340(7) 0.0430(9) -0.0096(6) -0.0217(7) 0.0225(6) C42 0.0181(7) 0.0163(7) 0.0288(9) -0.0029(6) 0.0044(6) -0.0003(6) O42 0.0368(8) 0.0300(7) 0.0353(8) -0.0024(5) 0.0183(6) -0.0022(6) C51 0.0227(8) 0.0205(7) 0.0217(8) 0.0035(6) 0.0010(6) 0.0037(6) O51 0.0431(8) 0.0362(7) 0.0287(7) 0.0104(6) -0.0059(6) 0.0121(6) C52 0.0221(8) 0.0164(7) 0.0169(7) 0.0021(5) 0.0011(6) 0.0016(6) O52 0.0194(6) 0.0267(6) 0.0373(7) 0.0048(5) 0.0026(5) -0.0045(5) C61 0.0207(8) 0.0132(7) 0.0342(9) 0.0035(6) 0.0026(7) 0.0005(6) O61 0.0256(7) 0.0206(6) 0.0583(9) 0.0118(6) -0.0075(6) 0.0016(5) C62 0.0212(8) 0.0160(7) 0.0208(8) 0.0036(6) 0.0005(6) 0.0035(6) O62 0.0230(6) 0.0186(5) 0.0345(7) 0.0049(5) -0.0008(5) -0.0024(5) C63 0.0229(8) 0.0162(7) 0.0249(8) 0.0015(6) 0.0042(6) -0.0020(6) O63 0.0360(7) 0.0359(7) 0.0245(7) 0.0000(5) 0.0102(5) -0.0026(6) C4 0.0127(6) 0.0118(6) 0.0181(7) 0.0022(5) 0.0018(5) 0.0013(5) C5 0.0126(6) 0.0144(6) 0.0208(7) -0.0001(5) 0.0018(5) -0.0006(5) C6 0.0187(7) 0.0176(7) 0.0210(8) 0.0004(6) -0.0005(6) 0.0004(6) C231 0.0200(7) 0.0159(7) 0.0204(8) 0.0041(6) -0.0059(6) -0.0027(6) C232 0.0259(8) 0.0210(8) 0.0224(8) 0.0035(6) -0.0041(6) -0.0002(6) C233 0.0327(9) 0.0313(9) 0.0177(8) 0.0066(7) -0.0045(7) -0.0061(7) C234 0.0359(10) 0.0260(8) 0.0267(9) 0.0139(7) -0.0156(8) -0.0055(7) C235 0.0260(9) 0.0182(7) 0.0348(10) 0.0053(7) -0.0127(7) -0.0001(6) C236 0.0236(8) 0.0197(7) 0.0238(8) 0.0025(6) -0.0059(6) -0.0020(6) F232 0.0366(6) 0.0326(6) 0.0314(6) 0.0047(5) 0.0048(5) 0.0100(5) F233 0.0525(8) 0.0550(8) 0.0218(6) 0.0106(5) 0.0036(5) -0.0008(6) F234 0.0516(7) 0.0454(7) 0.0394(7) 0.0282(6) -0.0171(6) -0.0037(6) F235 0.0364(6) 0.0268(6) 0.0557(8) 0.0101(5) -0.0129(6) 0.0110(5) F236 0.0344(6) 0.0327(6) 0.0325(6) 0.0059(5) 0.0056(5) 0.0112(5) P4 0.01042(16) 0.01179(16) 0.01536(17) 0.00199(13) 0.00099(13) 0.00124(12) C411 0.0179(7) 0.0143(6) 0.0147(7) 0.0015(5) 0.0019(5) -0.0001(5) C412 0.0179(7) 0.0227(8) 0.0231(8) 0.0060(6) 0.0038(6) 0.0025(6) C413 0.0249(8) 0.0255(8) 0.0261(9) 0.0065(7) 0.0093(7) 0.0009(7) C414 0.0325(9) 0.0234(8) 0.0183(8) 0.0057(6) 0.0051(7) -0.0015(7) C415 0.0255(8) 0.0224(8) 0.0192(8) 0.0052(6) -0.0016(6) 0.0016(6) C416 0.0184(7) 0.0142(6) 0.0200(7) 0.0029(5) 0.0014(6) 0.0002(5) C421 0.0099(6) 0.0143(6) 0.0174(7) 0.0010(5) 0.0011(5) 0.0024(5) C422 0.0144(7) 0.0170(7) 0.0246(8) 0.0026(6) 0.0008(6) 0.0015(5) C423 0.0215(8) 0.0152(7) 0.0330(9) -0.0024(6) 0.0000(7) -0.0007(6) C424 0.0182(7) 0.0252(8) 0.0228(8) -0.0040(6) -0.0025(6) 0.0010(6) C425 0.0174(7) 0.0248(8) 0.0185(7) 0.0028(6) -0.0010(6) 0.0053(6) C426 0.0150(7) 0.0146(6) 0.0192(7) 0.0030(5) 0.0010(5) 0.0026(5) C20 0.0118(6) 0.0132(6) 0.0159(7) 0.0016(5) -0.0005(5) 0.0014(5) P5 0.01094(16) 0.01267(16) 0.01598(18) 0.00161(13) 0.00099(13) 0.00106(13) C511 0.0134(6) 0.0109(6) 0.0202(7) 0.0012(5) 0.0003(5) 0.0011(5) C512 0.0164(7) 0.0256(8) 0.0235(8) -0.0004(6) 0.0005(6) 0.0038(6) C513 0.0175(8) 0.0345(9) 0.0296(9) 0.0001(7) -0.0038(7) 0.0062(7) C514 0.0146(7) 0.0259(8) 0.0399(11) -0.0001(7) 0.0036(7) 0.0051(6) C515 0.0163(7) 0.0214(8) 0.0340(10) 0.0008(7) 0.0079(6) 0.0022(6) C516 0.0170(7) 0.0165(7) 0.0213(8) 0.0022(6) 0.0037(6) 0.0007(5) C521 0.0121(6) 0.0172(7) 0.0161(7) 0.0023(5) 0.0027(5) 0.0011(5) C522 0.0176(7) 0.0176(7) 0.0203(8) 0.0021(6) -0.0017(6) 0.0037(6) C523 0.0185(7) 0.0176(7) 0.0219(8) -0.0005(6) -0.0028(6) 0.0041(6) C524 0.0277(9) 0.0266(8) 0.0154(7) -0.0007(6) -0.0036(6) 0.0005(7) C525 0.0399(10) 0.0252(8) 0.0181(8) 0.0062(6) -0.0018(7) -0.0004(7) C526 0.0322(9) 0.0159(7) 0.0194(8) 0.0040(6) -0.0006(6) -0.0024(6) #--------------------------------------------------------------------------- # MOLECULAR GEOMETRY # #--------------------------------------------------------------------------- _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 Co1 C12 1.7803(16) . ? Co1 C11 1.7962(16) . ? Co1 C1 1.8998(14) . ? Co1 P1 2.2014(5) . ? Co1 Co2 2.4781(5) . ? Co1 Co3 2.4810(4) . ? Co2 C22 1.7912(16) . ? Co2 C21 1.8162(16) . ? Co2 C1 1.9140(15) . ? Co2 P2 2.2035(4) . ? Co2 Co3 2.4805(4) . ? Co3 C32 1.7871(16) . ? Co3 C33 1.8012(17) . ? Co3 C31 1.8063(15) . ? Co3 C1 1.9468(14) . ? C11 O11 1.1486(18) . ? C12 O12 1.1437(19) . ? C21 O21 1.1440(18) . ? C22 O22 1.1441(19) . ? C31 O31 1.1440(18) . ? C32 O32 1.1475(19) . ? C33 O33 1.142(2) . ? C1 C2 1.403(2) . ? C2 C3 1.213(2) . ? C3 C131 1.428(2) . ? C131 C132 1.389(2) . ? C131 C136 1.399(2) . ? C132 F132 1.3389(19) . ? C132 C133 1.385(2) . ? C133 F133 1.347(2) . ? C133 C134 1.383(3) . ? C134 F134 1.3461(18) . ? C134 C135 1.372(2) . ? C135 F135 1.3413(19) . ? C135 C136 1.382(2) . ? C136 F136 1.3413(18) . ? P1 C111 1.8229(15) . ? P1 C121 1.8242(15) . ? P1 C10 1.8343(15) . ? C111 C112 1.395(2) . ? C111 C116 1.398(2) . ? C112 C113 1.391(2) . ? C112 H112 0.95 . ? C113 C114 1.377(3) . ? C113 H113 0.95 . ? C114 C115 1.380(3) . ? C114 H114 0.95 . ? C115 C116 1.396(2) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.399(2) . ? C121 C122 1.401(2) . ? C122 C123 1.395(2) . ? C122 H122 0.95 . ? C123 C124 1.381(2) . ? C123 H123 0.95 . ? C124 C125 1.394(2) . ? C124 H124 0.95 . ? C125 C126 1.391(2) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 P2 1.8387(14) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? P2 C211 1.8230(15) . ? P2 C221 1.8279(15) . ? C211 C216 1.397(2) . ? C211 C212 1.399(2) . ? C212 C213 1.396(2) . ? C212 H212 0.95 . ? C213 C214 1.383(2) . ? C213 H213 0.95 . ? C214 C215 1.384(2) . ? C214 H214 0.95 . ? C215 C216 1.385(2) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.394(2) . ? C221 C222 1.407(2) . ? C222 C223 1.385(2) . ? C222 H222 0.95 . ? C223 C224 1.388(3) . ? C223 H223 0.95 . ? C224 C225 1.386(3) . ? C224 H224 0.95 . ? C225 C226 1.393(2) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? Co4 C42 1.7916(17) . ? Co4 C41 1.8064(17) . ? Co4 C4 1.9130(14) . ? Co4 P4 2.2067(5) . ? Co4 Co6 2.4763(4) . ? Co4 Co5 2.4938(4) . ? Co5 C51 1.7986(17) . ? Co5 C52 1.7990(16) . ? Co5 C4 1.8926(15) . ? Co5 P5 2.2108(5) . ? Co5 Co6 2.4897(4) . ? Co6 C62 1.7947(16) . ? Co6 C63 1.8031(17) . ? Co6 C61 1.8092(17) . ? Co6 C4 1.9401(14) . ? C41 O41 1.141(2) . ? C42 O42 1.140(2) . ? C51 O51 1.1456(19) . ? C52 O52 1.1389(19) . ? C61 O61 1.141(2) . ? C62 O62 1.1432(18) . ? C63 O63 1.136(2) . ? C4 C5 1.404(2) . ? C5 C6 1.208(2) . ? C6 C231 1.430(2) . ? C231 C236 1.397(2) . ? C231 C232 1.399(2) . ? C232 F232 1.339(2) . ? C232 C233 1.384(2) . ? C233 F233 1.338(2) . ? C233 C234 1.383(3) . ? C234 F234 1.3416(19) . ? C234 C235 1.374(3) . ? C235 F235 1.341(2) . ? C235 C236 1.384(2) . ? C236 F236 1.343(2) . ? P4 C411 1.8221(15) . ? P4 C421 1.8306(15) . ? P4 C20 1.8350(14) . ? C411 C412 1.397(2) . ? C411 C416 1.400(2) . ? C412 C413 1.387(2) . ? C412 H412 0.95 . ? C413 C414 1.404(2) . ? C413 H413 0.95 . ? C414 C415 1.381(2) . ? C414 H414 0.95 . ? C415 C416 1.392(2) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 C426 1.403(2) . ? C421 C422 1.405(2) . ? C422 C423 1.385(2) . ? C422 H422 0.95 . ? C423 C424 1.393(2) . ? C423 H423 0.95 . ? C424 C425 1.392(2) . ? C424 H424 0.95 . ? C425 C426 1.379(2) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? C20 P5 1.8375(14) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P5 C521 1.8324(15) . ? P5 C511 1.8366(15) . ? C511 C516 1.392(2) . ? C511 C512 1.401(2) . ? C512 C513 1.387(2) . ? C512 H512 0.95 . ? C513 C514 1.401(3) . ? C513 H513 0.95 . ? C514 C515 1.373(3) . ? C514 H514 0.95 . ? C515 C516 1.394(2) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C522 1.395(2) . ? C521 C526 1.402(2) . ? C522 C523 1.389(2) . ? C522 H522 0.95 . ? C523 C524 1.388(2) . ? C523 H523 0.95 . ? C524 C525 1.392(2) . ? C524 H524 0.95 . ? C525 C526 1.388(2) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? 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 C12 Co1 C11 102.92(7) . . ? C12 Co1 C1 111.10(7) . . ? C11 Co1 C1 138.44(7) . . ? C12 Co1 P1 95.83(5) . . ? C11 Co1 P1 101.36(5) . . ? C1 Co1 P1 98.27(4) . . ? C12 Co1 Co2 157.14(5) . . ? C11 Co1 Co2 90.94(5) . . ? C1 Co1 Co2 49.73(4) . . ? P1 Co1 Co2 99.192(16) . . ? C12 Co1 Co3 98.88(5) . . ? C11 Co1 Co3 101.97(5) . . ? C1 Co1 Co3 50.67(4) . . ? P1 Co1 Co3 148.762(14) . . ? Co2 Co1 Co3 60.026(12) . . ? C22 Co2 C21 100.68(7) . . ? C22 Co2 C1 99.14(7) . . ? C21 Co2 C1 148.02(6) . . ? C22 Co2 P2 95.77(5) . . ? C21 Co2 P2 102.46(5) . . ? C1 Co2 P2 100.22(4) . . ? C22 Co2 Co1 148.10(5) . . ? C21 Co2 Co1 106.48(5) . . ? C1 Co2 Co1 49.23(4) . . ? P2 Co2 Co1 94.426(16) . . ? C22 Co2 Co3 98.63(5) . . ? C21 Co2 Co3 101.49(5) . . ? C1 Co2 Co3 50.61(4) . . ? P2 Co2 Co3 149.131(15) . . ? Co1 Co2 Co3 60.045(12) . . ? C32 Co3 C33 98.53(7) . . ? C32 Co3 C31 104.74(7) . . ? C33 Co3 C31 101.49(7) . . ? C32 Co3 C1 102.47(6) . . ? C33 Co3 C1 107.84(7) . . ? C31 Co3 C1 136.04(6) . . ? C32 Co3 Co2 96.04(5) . . ? C33 Co3 Co2 155.51(5) . . ? C31 Co3 Co2 93.65(5) . . ? C1 Co3 Co2 49.44(4) . . ? C32 Co3 Co1 150.11(5) . . ? C33 Co3 Co1 99.29(5) . . ? C31 Co3 Co1 94.96(5) . . ? C1 Co3 Co1 49.01(4) . . ? Co2 Co3 Co1 59.929(12) . . ? O11 C11 Co1 177.61(14) . . ? O12 C12 Co1 177.68(15) . . ? O21 C21 Co2 178.31(14) . . ? O22 C22 Co2 178.62(15) . . ? O31 C31 Co3 177.51(14) . . ? O32 C32 Co3 179.34(15) . . ? O33 C33 Co3 176.65(14) . . ? C2 C1 Co1 136.34(11) . . ? C2 C1 Co2 131.39(11) . . ? Co1 C1 Co2 81.05(6) . . ? C2 C1 Co3 127.20(10) . . ? Co1 C1 Co3 80.32(5) . . ? Co2 C1 Co3 79.95(5) . . ? C3 C2 C1 179.14(16) . . ? C2 C3 C131 175.82(16) . . ? C132 C131 C136 116.31(14) . . ? C132 C131 C3 121.86(14) . . ? C136 C131 C3 121.78(14) . . ? F132 C132 C133 118.32(15) . . ? F132 C132 C131 119.53(14) . . ? C133 C132 C131 122.14(15) . . ? F133 C133 C134 119.96(15) . . ? F133 C133 C132 120.51(16) . . ? C134 C133 C132 119.53(16) . . ? F134 C134 C135 120.35(16) . . ? F134 C134 C133 119.46(16) . . ? C135 C134 C133 120.19(15) . . ? F135 C135 C134 120.26(15) . . ? F135 C135 C136 120.32(15) . . ? C134 C135 C136 119.42(15) . . ? F136 C136 C135 118.37(14) . . ? F136 C136 C131 119.22(13) . . ? C135 C136 C131 122.39(15) . . ? C111 P1 C121 102.61(7) . . ? C111 P1 C10 100.25(7) . . ? C121 P1 C10 108.42(7) . . ? C111 P1 Co1 120.11(5) . . ? C121 P1 Co1 115.02(5) . . ? C10 P1 Co1 109.03(5) . . ? C112 C111 C116 118.75(15) . . ? C112 C111 P1 119.38(12) . . ? C116 C111 P1 121.55(13) . . ? C113 C112 C111 120.63(16) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C114 C113 C112 120.09(18) . . ? C114 C113 H113 120 . . ? C112 C113 H113 120 . . ? C113 C114 C115 120.15(16) . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C114 C115 C116 120.33(18) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 120.02(18) . . ? C115 C116 H116 120 . . ? C111 C116 H116 120 . . ? C126 C121 C122 119.02(14) . . ? C126 C121 P1 117.47(11) . . ? C122 C121 P1 123.48(11) . . ? C123 C122 C121 119.98(14) . . ? C123 C122 H122 120 . . ? C121 C122 H122 120 . . ? C124 C123 C122 120.52(15) . . ? C124 C123 H123 119.7 . . ? C122 C123 H123 119.7 . . ? C123 C124 C125 119.98(15) . . ? C123 C124 H124 120 . . ? C125 C124 H124 120 . . ? C126 C125 C124 119.89(16) . . ? C126 C125 H125 120.1 . . ? C124 C125 H125 120.1 . . ? C125 C126 C121 120.59(15) . . ? C125 C126 H126 119.7 . . ? C121 C126 H126 119.7 . . ? P1 C10 P2 110.09(7) . . ? P1 C10 H10A 109.6 . . ? P2 C10 H10A 109.6 . . ? P1 C10 H10B 109.6 . . ? P2 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? C211 P2 C221 103.07(7) . . ? C211 P2 C10 105.04(7) . . ? C221 P2 C10 101.84(7) . . ? C211 P2 Co2 111.96(5) . . ? C221 P2 Co2 122.78(5) . . ? C10 P2 Co2 110.42(5) . . ? C216 C211 C212 119.02(14) . . ? C216 C211 P2 119.57(11) . . ? C212 C211 P2 120.81(11) . . ? C213 C212 C211 120.07(14) . . ? C213 C212 H212 120 . . ? C211 C212 H212 120 . . ? C214 C213 C212 120.07(15) . . ? C214 C213 H213 120 . . ? C212 C213 H213 120 . . ? C213 C214 C215 120.16(15) . . ? C213 C214 H214 119.9 . . ? C215 C214 H214 119.9 . . ? C214 C215 C216 120.21(15) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C215 C216 C211 120.46(15) . . ? C215 C216 H216 119.8 . . ? C211 C216 H216 119.8 . . ? C226 C221 C222 118.87(14) . . ? C226 C221 P2 121.67(12) . . ? C222 C221 P2 119.11(12) . . ? C223 C222 C221 120.25(16) . . ? C223 C222 H222 119.9 . . ? C221 C222 H222 119.9 . . ? C222 C223 C224 120.44(17) . . ? C222 C223 H223 119.8 . . ? C224 C223 H223 119.8 . . ? C225 C224 C223 119.80(16) . . ? C225 C224 H224 120.1 . . ? C223 C224 H224 120.1 . . ? C224 C225 C226 120.26(17) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C225 C226 C221 120.38(15) . . ? C225 C226 H226 119.8 . . ? C221 C226 H226 119.8 . . ? C42 Co4 C41 101.47(8) . . ? C42 Co4 C4 101.68(7) . . ? C41 Co4 C4 147.33(7) . . ? C42 Co4 P4 97.96(5) . . ? C41 Co4 P4 103.46(5) . . ? C4 Co4 P4 95.81(4) . . ? C42 Co4 Co6 93.54(5) . . ? C41 Co4 Co6 105.33(5) . . ? C4 Co4 Co6 50.49(4) . . ? P4 Co4 Co6 146.079(14) . . ? C42 Co4 Co5 148.32(5) . . ? C41 Co4 Co5 102.40(6) . . ? C4 Co4 Co5 48.71(4) . . ? P4 Co4 Co5 96.426(15) . . ? Co6 Co4 Co5 60.122(11) . . ? C51 Co5 C52 103.40(7) . . ? C51 Co5 C4 138.54(7) . . ? C52 Co5 C4 105.42(7) . . ? C51 Co5 P5 107.78(5) . . ? C52 Co5 P5 94.15(5) . . ? C4 Co5 P5 99.21(5) . . ? C51 Co5 Co6 95.47(5) . . ? C52 Co5 Co6 100.69(5) . . ? C4 Co5 Co6 50.33(4) . . ? P5 Co5 Co6 148.676(15) . . ? C51 Co5 Co4 95.82(5) . . ? C52 Co5 Co4 153.95(5) . . ? C4 Co5 Co4 49.41(4) . . ? P5 Co5 Co4 96.565(15) . . ? Co6 Co5 Co4 59.591(12) . . ? C62 Co6 C63 99.16(7) . . ? C62 Co6 C61 101.25(7) . . ? C63 Co6 C61 105.73(8) . . ? C62 Co6 C4 111.14(7) . . ? C63 Co6 C4 95.24(7) . . ? C61 Co6 C4 137.83(7) . . ? C62 Co6 Co4 151.97(5) . . ? C63 Co6 Co4 102.51(5) . . ? C61 Co6 Co4 89.81(5) . . ? C4 Co6 Co4 49.53(4) . . ? C62 Co6 Co5 91.79(5) . . ? C63 Co6 Co5 143.60(5) . . ? C61 Co6 Co5 105.96(6) . . ? C4 Co6 Co5 48.66(4) . . ? Co4 Co6 Co5 60.287(11) . . ? O41 C41 Co4 178.96(16) . . ? O42 C42 Co4 177.50(15) . . ? O51 C51 Co5 175.94(16) . . ? O52 C52 Co5 179.23(14) . . ? O61 C61 Co6 178.48(16) . . ? O62 C62 Co6 178.30(15) . . ? O63 C63 Co6 177.42(16) . . ? C5 C4 Co5 139.50(11) . . ? C5 C4 Co4 124.45(10) . . ? Co5 C4 Co4 81.88(6) . . ? C5 C4 Co6 129.37(11) . . ? Co5 C4 Co6 81.01(6) . . ? Co4 C4 Co6 79.98(6) . . ? C6 C5 C4 173.54(15) . . ? C5 C6 C231 173.10(16) . . ? C236 C231 C232 116.63(14) . . ? C236 C231 C6 121.88(15) . . ? C232 C231 C6 121.47(15) . . ? F232 C232 C233 118.75(16) . . ? F232 C232 C231 119.45(14) . . ? C233 C232 C231 121.80(16) . . ? F233 C233 C234 120.11(16) . . ? F233 C233 C232 120.48(17) . . ? C234 C233 C232 119.41(17) . . ? F234 C234 C235 120.07(17) . . ? F234 C234 C233 119.24(18) . . ? C235 C234 C233 120.68(15) . . ? F235 C235 C234 119.96(16) . . ? F235 C235 C236 120.82(17) . . ? C234 C235 C236 119.21(17) . . ? F236 C236 C235 118.22(16) . . ? F236 C236 C231 119.51(14) . . ? C235 C236 C231 122.26(17) . . ? C411 P4 C421 103.74(7) . . ? C411 P4 C20 103.13(7) . . ? C421 P4 C20 102.71(7) . . ? C411 P4 Co4 115.25(5) . . ? C421 P4 Co4 119.65(5) . . ? C20 P4 Co4 110.45(5) . . ? C412 C411 C416 118.55(14) . . ? C412 C411 P4 118.19(12) . . ? C416 C411 P4 123.15(11) . . ? C413 C412 C411 120.96(15) . . ? C413 C412 H412 119.5 . . ? C411 C412 H412 119.5 . . ? C412 C413 C414 119.94(16) . . ? C412 C413 H413 120 . . ? C414 C413 H413 120 . . ? C415 C414 C413 119.38(15) . . ? C415 C414 H414 120.3 . . ? C413 C414 H414 120.3 . . ? C414 C415 C416 120.66(15) . . ? C414 C415 H415 119.7 . . ? C416 C415 H415 119.7 . . ? C415 C416 C411 120.49(15) . . ? C415 C416 H416 119.8 . . ? C411 C416 H416 119.8 . . ? C426 C421 C422 118.54(13) . . ? C426 C421 P4 119.68(11) . . ? C422 C421 P4 121.65(11) . . ? C423 C422 C421 120.26(15) . . ? C423 C422 H422 119.9 . . ? C421 C422 H422 119.9 . . ? C422 C423 C424 120.59(15) . . ? C422 C423 H423 119.7 . . ? C424 C423 H423 119.7 . . ? C425 C424 C423 119.39(15) . . ? C425 C424 H424 120.3 . . ? C423 C424 H424 120.3 . . ? C426 C425 C424 120.40(15) . . ? C426 C425 H425 119.8 . . ? C424 C425 H425 119.8 . . ? C425 C426 C421 120.83(14) . . ? C425 C426 H426 119.6 . . ? C421 C426 H426 119.6 . . ? P4 C20 P5 109.46(7) . . ? P4 C20 H20A 109.8 . . ? P5 C20 H20A 109.8 . . ? P4 C20 H20B 109.8 . . ? P5 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? C521 P5 C511 102.11(7) . . ? C521 P5 C20 103.91(7) . . ? C511 P5 C20 101.22(7) . . ? C521 P5 Co5 123.02(5) . . ? C511 P5 Co5 115.31(5) . . ? C20 P5 Co5 108.68(5) . . ? C516 C511 C512 119.21(14) . . ? C516 C511 P5 121.98(12) . . ? C512 C511 P5 118.79(12) . . ? C513 C512 C511 120.14(15) . . ? C513 C512 H512 119.9 . . ? C511 C512 H512 119.9 . . ? C512 C513 C514 120.15(17) . . ? C512 C513 H513 119.9 . . ? C514 C513 H513 119.9 . . ? C515 C514 C513 119.58(16) . . ? C515 C514 H514 120.2 . . ? C513 C514 H514 120.2 . . ? C514 C515 C516 120.74(16) . . ? C514 C515 H515 119.6 . . ? C516 C515 H515 119.6 . . ? C511 C516 C515 120.06(15) . . ? C511 C516 H516 120 . . ? C515 C516 H516 120 . . ? C522 C521 C526 118.49(14) . . ? C522 C521 P5 120.50(11) . . ? C526 C521 P5 120.96(11) . . ? C523 C522 C521 121.04(14) . . ? C523 C522 H522 119.5 . . ? C521 C522 H522 119.5 . . ? C524 C523 C522 120.09(14) . . ? C524 C523 H523 120 . . ? C522 C523 H523 120 . . ? C523 C524 C525 119.43(15) . . ? C523 C524 H524 120.3 . . ? C525 C524 H524 120.3 . . ? C526 C525 C524 120.63(15) . . ? C526 C525 H525 119.7 . . ? C524 C525 H525 119.7 . . ? C525 C526 C521 120.30(15) . . ? C525 C526 H526 119.8 . . ? C521 C526 H526 119.8 . . ? # Attachment 'combinedcif.doc' ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_br1249_compound_1 _database_code_depnum_ccdc_archive 'CCDC 660619' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C52 H38 F5 P2 Ru1' _chemical_formula_moiety 'C49 H35 F5 P2 Ru, 0.5(C6 H6)' _chemical_formula_weight 920.88 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_21/n _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.1626(7) _cell_length_b 24.5128(2) _cell_length_c 17.0993(8) _cell_angle_alpha 90.00000 _cell_angle_beta 96.323(5) _cell_angle_gamma 90.00000 _cell_volume 4233.8(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 29951 _cell_measurement_theta_min 2.5854 _cell_measurement_theta_max 30.0508 _cell_measurement_temperature 100 _exptl_absorpt_coefficient_mu .504 _exptl_crystal_description plate _exptl_crystal_size_max .26 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour pale_yellow _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SCALE3 ABSPACK ; _exptl_absorpt_correction_T_min .96 _exptl_absorpt_correction_T_max 1.04 _diffrn_reflns_number 92469 _reflns_number_total 11272 _reflns_Friedel_coverage 0 _reflns_number_gt 8793 _reflns_threshold_expression 'I > 2.00 sig(I)' _diffrn_reflns_theta_max 29.13 _diffrn_reflns_theta_full 29.1 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .067 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .068 _refine_ls_wR_factor_gt .085 _refine_ls_goodness_of_fit_gt 1.106 _refine_ls_number_reflns 11272 _refine_ls_number_parameters 526 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w =1/(sig^2(F^2) + .008F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .02 _refine_diff_density_min -2.172 _refine_diff_density_max 1.79 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.5 (release 22-02-2006 CrysAlis171 .NET) ; _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 208 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 152 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 20 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .67783(4) .69878(2) .61911(3) .0188(2) Uani ? ? 1.00000 ? ? P1 .60072(14) .67215(6) .49370(9) .0196(6) Uani ? ? 1.00000 ? ? C111 .5825(5) .7326(2) .4305(3) .021(2) Uani ? ? 1.00000 ? ? C112 .6905(6) .7508(3) .3927(4) .028(3) Uani ? ? 1.00000 ? ? C113 .6877(6) .8024(3) .3570(4) .031(3) Uani ? ? 1.00000 ? ? C114 .5789(7) .8349(3) .3578(4) .031(3) Uani ? ? 1.00000 ? ? C115 .4690(6) .8169(3) .3933(4) .029(3) Uani ? ? 1.00000 ? ? C116 .4724(6) .7668(3) .4296(4) .025(3) Uani ? ? 1.00000 ? ? C121 .7164(6) .6298(2) .4430(3) .022(3) Uani ? ? 1.00000 ? ? C122 .8193(6) .6019(3) .4858(4) .025(3) Uani ? ? 1.00000 ? ? C123 .9030(6) .5686(3) .4479(4) .025(3) Uani ? ? 1.00000 ? ? C124 .8846(6) .5632(3) .3664(4) .025(3) Uani ? ? 1.00000 ? ? C125 .7807(7) .5901(3) .3238(4) .029(3) Uani ? ? 1.00000 ? ? C126 .6952(6) .6226(3) .3619(4) .027(3) Uani ? ? 1.00000 ? ? C131 .4537(5) .6295(2) .4670(4) .022(3) Uani ? ? 1.00000 ? ? C132 .4475(6) .5815(2) .5093(4) .023(3) Uani ? ? 1.00000 ? ? C133 .3485(6) .5428(3) .4885(4) .028(3) Uani ? ? 1.00000 ? ? C134 .2551(6) .5532(3) .4245(4) .029(3) Uani ? ? 1.00000 ? ? C135 .2592(6) .6015(3) .3831(4) .034(3) Uani ? ? 1.00000 ? ? C136 .3590(6) .6393(3) .4036(4) .028(3) Uani ? ? 1.00000 ? ? P2 .48254(14) .71069(6) .67122(8) .0199(6) Uani ? ? 1.00000 ? ? C211 .3791(6) .7715(3) .6471(4) .024(3) Uani ? ? 1.00000 ? ? C212 .4275(6) .8137(3) .6038(4) .027(3) Uani ? ? 1.00000 ? ? C213 .3481(7) .8604(3) .5846(4) .032(3) Uani ? ? 1.00000 ? ? C214 .2230(7) .8640(3) .6098(4) .036(3) Uani ? ? 1.00000 ? ? C215 .1768(7) .8222(3) .6540(4) .033(3) Uani ? ? 1.00000 ? ? C216 .2543(6) .7762(3) .6728(4) .028(3) Uani ? ? 1.00000 ? ? C221 .5205(5) .7195(3) .7786(3) .021(3) Uani ? ? 1.00000 ? ? C222 .5798(6) .6769(3) .8238(3) .025(3) Uani ? ? 1.00000 ? ? C223 .6145(6) .6831(3) .9047(4) .029(3) Uani ? ? 1.00000 ? ? C224 .5949(6) .7333(3) .9407(4) .028(3) Uani ? ? 1.00000 ? ? C225 .5434(6) .7760(3) .8962(4) .028(3) Uani ? ? 1.00000 ? ? C226 .5054(6) .7697(3) .8150(3) .024(3) Uani ? ? 1.00000 ? ? C231 .3517(5) .6589(2) .6598(3) .021(3) Uani ? ? 1.00000 ? ? C232 .3419(6) .6154(3) .7107(4) .026(3) Uani ? ? 1.00000 ? ? C233 .2369(7) .5781(3) .6979(4) .031(3) Uani ? ? 1.00000 ? ? C234 .1413(6) .5849(3) .6335(4) .029(3) Uani ? ? 1.00000 ? ? C235 .1525(6) .6273(3) .5813(4) .026(3) Uani ? ? 1.00000 ? ? C236 .2579(6) .6636(3) .5938(3) .023(3) Uani ? ? 1.00000 ? ? C1 .6780(6) .6225(3) .6590(3) .022(3) Uani ? ? 1.00000 ? ? C2 .6885(6) .5774(3) .6898(4) .027(3) Uani ? ? 1.00000 ? ? C21 .7141(6) .5304(2) .7377(4) .025(3) Uani ? ? 1.00000 ? ? C22 .6190(7) .4912(3) .7495(4) .032(3) Uani ? ? 1.00000 ? ? F22 .4980(4) .4960(2) .7118(4) .062(3) Uani ? ? 1.00000 ? ? C23 .6447(8) .4467(3) .7992(5) .040(4) Uani ? ? 1.00000 ? ? F23 .5504(6) .4103(2) .8087(4) .069(3) Uani ? ? 1.00000 ? ? C24 .7696(10) .4403(3) .8379(5) .047(4) Uani ? ? 1.00000 ? ? F24 .7967(7) .3980(2) .8879(3) .071(3) Uani ? ? 1.00000 ? ? C25 .8656(10) .4774(3) .8274(6) .056(5) Uani ? ? 1.00000 ? ? F25 .9906(7) .4704(3) .8639(5) .108(5) Uani ? ? 1.00000 ? ? C26 .8395(8) .5205(3) .7778(5) .042(4) Uani ? ? 1.00000 ? ? F26 .9376(5) .5557(2) .7671(4) .068(3) Uani ? ? 1.00000 ? ? C101 .8943(5) .7056(3) .6577(4) .028(3) Uani ? ? 1.00000 ? ? C102 .8696(6) .7305(3) .5828(4) .028(3) Uani ? ? 1.00000 ? ? C103 .7835(6) .7761(3) .5898(4) .028(3) Uani ? ? 1.00000 ? ? C104 .7565(6) .7782(3) .6696(4) .026(3) Uani ? ? 1.00000 ? ? C105 .8249(6) .7350(3) .7118(3) .027(3) Uani ? ? 1.00000 ? ? C01 .392(4) .5468(12) .9313(15) .126(12) Uiso ? ? .50000 ? ? C02 .529(4) .5367(15) .9439(17) .43(7) Uiso ? ? .50000 ? ? C03 .578(2) .4981(18) .9998(19) .20(2) Uiso ? ? .50000 ? ? C04 .491(4) .4695(12) 1.0431(15) .091(9) Uiso ? ? .50000 ? ? C05 .355(4) .4795(15) 1.0305(17) .32(4) Uiso ? ? .50000 ? ? C06 .306(2) .5182(18) .9745(19) .156(16) Uiso ? ? .50000 ? ? H01 .359(7) .5731(15) .8935(19) .13800 Uiso ? ? .50000 ? ? H02 .588(6) .556(2) .915(2) .45800 Uiso ? ? .50000 ? ? H03 .671(2) .491(3) 1.008(3) .27500 Uiso ? ? .50000 ? ? H04 .525(7) .4433(15) 1.0811(19) .15300 Uiso ? ? .50000 ? ? H05 .296(6) .460(2) 1.060(2) .33000 Uiso ? ? .50000 ? ? H06 .213(2) .525(3) .966(3) .21300 Uiso ? ? .50000 ? ? H112 .76627 .72741 .39260 .03200 Uiso ? ? 1.00000 ? ? H113 .76259 .81394 .33183 .03600 Uiso ? ? 1.00000 ? ? H114 .57807 .87040 .33213 .03700 Uiso ? ? 1.00000 ? ? H115 .39358 .84062 .39412 .03600 Uiso ? ? 1.00000 ? ? H116 .39697 .75444 .45523 .02900 Uiso ? ? 1.00000 ? ? H122 .83124 .60535 .54210 .02900 Uiso ? ? 1.00000 ? ? H123 .97439 .54919 .47749 .03000 Uiso ? ? 1.00000 ? ? H124 .94233 .54128 .34015 .03600 Uiso ? ? 1.00000 ? ? H125 .76513 .58626 .26727 .03900 Uiso ? ? 1.00000 ? ? H126 .62375 .64024 .33226 .03400 Uiso ? ? 1.00000 ? ? H132 .51065 .57405 .55425 .03100 Uiso ? ? 1.00000 ? ? H133 .34581 .50999 .51763 .03300 Uiso ? ? 1.00000 ? ? H134 .18789 .52738 .40961 .03800 Uiso ? ? 1.00000 ? ? H135 .19417 .60788 .33969 .04000 Uiso ? ? 1.00000 ? ? H136 .36184 .67268 .37370 .03200 Uiso ? ? 1.00000 ? ? H212 .51327 .81196 .58655 .03300 Uiso ? ? 1.00000 ? ? H213 .38040 .88945 .55503 .04100 Uiso ? ? 1.00000 ? ? H214 .16787 .89489 .59579 .04400 Uiso ? ? 1.00000 ? ? H215 .08996 .82586 .67232 .03800 Uiso ? ? 1.00000 ? ? H216 .22083 .74733 .70431 .03400 Uiso ? ? 1.00000 ? ? H222 .59732 .64302 .79924 .03500 Uiso ? ? 1.00000 ? ? H223 .64972 .65266 .93553 .03700 Uiso ? ? 1.00000 ? ? H224 .61852 .73755 .99623 .03500 Uiso ? ? 1.00000 ? ? H225 .53307 .81091 .91993 .03900 Uiso ? ? 1.00000 ? ? H226 .46833 .79994 .78411 .02700 Uiso ? ? 1.00000 ? ? H232 .40573 .61108 .75574 .03200 Uiso ? ? 1.00000 ? ? H233 .23138 .54769 .73277 .03600 Uiso ? ? 1.00000 ? ? H234 .06667 .56056 .62620 .03600 Uiso ? ? 1.00000 ? ? H235 .08885 .63118 .53573 .03300 Uiso ? ? 1.00000 ? ? H236 .26550 .69307 .55711 .03100 Uiso ? ? 1.00000 ? ? H101 .94977 .67378 .67059 .03500 Uiso ? ? 1.00000 ? ? H102 .90379 .71762 .53597 .03500 Uiso ? ? 1.00000 ? ? H103 .75234 .80087 .54833 .03200 Uiso ? ? 1.00000 ? ? H104 .70054 .80475 .69112 .03100 Uiso ? ? 1.00000 ? ? H105 .82463 .72744 .76684 .03400 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru .0164(2) .0227(2) .0177(2) -.00045(18) .00359(14) -.00016(18) P1 .0158(6) .0246(7) .0187(7) .0012(5) .0037(5) .0002(5) C111 .019(3) .028(3) .016(2) -.001(2) -.004(2) -.004(2) C112 .020(3) .033(3) .030(3) .004(2) .007(2) -.001(3) C113 .030(3) .033(3) .031(3) -.001(3) .009(3) .005(3) C114 .037(3) .032(3) .025(3) .005(3) .005(3) .008(3) C115 .029(3) .028(3) .027(3) .008(2) -.001(2) -.001(2) C116 .018(3) .032(3) .026(3) .001(2) .002(2) -.005(2) C121 .018(3) .025(3) .024(3) .000(2) .003(2) -.003(2) C122 .021(3) .029(3) .024(3) .001(2) .001(2) -.002(2) C123 .019(3) .027(3) .030(3) .002(2) -.001(2) -.000(2) C124 .018(3) .029(3) .029(3) .003(2) .006(2) -.002(2) C125 .032(3) .033(3) .022(3) .007(3) .001(2) -.005(2) C126 .018(3) .040(4) .022(3) .010(2) .001(2) .003(3) C131 .015(2) .023(3) .028(3) -.001(2) .005(2) -.004(2) C132 .018(3) .024(3) .029(3) .001(2) .004(2) -.004(2) C133 .023(3) .025(3) .037(3) -.002(2) .008(3) -.008(3) C134 .018(3) .033(3) .037(3) -.006(2) .009(2) -.012(3) C135 .024(3) .048(4) .030(3) -.001(3) -.002(3) -.011(3) C136 .027(3) .034(3) .022(3) .000(3) .006(2) -.003(2) P2 .0169(6) .0252(7) .0179(6) .0014(5) .0035(5) -.0010(5) C211 .022(3) .027(3) .023(3) .003(2) .001(2) -.004(2) C212 .025(3) .030(3) .025(3) -.003(2) .003(2) -.005(2) C213 .039(4) .035(4) .022(3) -.001(3) -.003(3) -.003(3) C214 .042(4) .030(3) .033(4) .010(3) -.006(3) -.009(3) C215 .027(3) .040(4) .030(3) .012(3) -.003(3) -.011(3) C216 .026(3) .033(3) .026(3) .005(3) .007(2) -.002(3) C221 .018(2) .031(3) .015(2) -.002(2) .005(2) .002(2) C222 .019(3) .037(3) .020(3) .007(2) .003(2) -.003(2) C223 .019(3) .046(4) .023(3) -.001(3) .003(2) .001(3) C224 .021(3) .044(4) .021(3) -.006(3) .005(2) -.002(3) C225 .024(3) .032(3) .028(3) -.009(2) .011(2) -.010(3) C226 .019(3) .030(3) .023(3) -.001(2) .001(2) -.003(2) C231 .018(2) .025(3) .020(3) -.001(2) .007(2) -.003(2) C232 .023(3) .032(3) .022(3) .002(2) .004(2) -.003(2) C233 .030(3) .030(3) .036(4) -.006(3) .012(3) .003(3) C234 .024(3) .032(3) .033(3) -.007(2) .009(2) -.003(3) C235 .019(3) .029(3) .030(3) .004(2) .005(2) -.004(2) C236 .020(3) .029(3) .022(3) .006(2) .009(2) -.003(2) C1 .018(3) .028(3) .021(3) -.003(2) .001(2) -.001(2) C2 .028(3) .031(3) .023(3) .001(2) .007(2) -.003(2) C21 .026(3) .023(3) .026(3) .002(2) .007(2) -.001(2) C22 .029(3) .032(3) .036(4) .001(3) .005(3) -.001(3) F22 .026(2) .056(3) .101(4) -.013(2) -.005(2) .012(3) C23 .047(4) .032(4) .044(4) -.010(3) .019(3) .006(3) F23 .071(4) .043(3) .099(5) -.025(3) .034(3) .012(3) C24 .070(6) .030(4) .041(4) .001(4) .002(4) .014(3) F24 .114(5) .028(2) .068(4) .003(3) -.001(3) .021(2) C25 .063(6) .035(4) .062(6) .001(4) -.023(5) .014(4) F25 .077(4) .068(4) .163(7) -.006(3) -.063(5) .051(5) C26 .036(4) .032(4) .056(5) -.006(3) -.005(3) .009(3) F26 .034(2) .046(3) .117(5) -.015(2) -.017(3) .030(3) C101 .010(2) .038(4) .035(3) -.003(2) .002(2) -.004(3) C102 .019(3) .037(4) .030(3) -.009(2) .006(2) -.002(3) C103 .029(3) .024(3) .030(3) -.007(2) .001(3) -.000(2) C104 .023(3) .026(3) .030(3) -.001(2) .007(2) -.007(2) C105 .022(3) .039(4) .020(3) -.005(3) .002(2) -.004(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Ru P1 . . 2.2954(15) ? Ru P2 . . 2.2820(16) ? Ru C1 . . 1.991(6) ? Ru C101 . . 2.232(5) ? Ru C102 . . 2.248(6) ? Ru C103 . . 2.261(6) ? Ru C104 . . 2.240(6) ? Ru C105 . . 2.239(6) ? P1 C111 . . 1.831(6) ? P1 C121 . . 1.854(6) ? P1 C131 . . 1.840(6) ? C111 C112 . . 1.407(9) ? C111 C116 . . 1.396(8) ? C112 C113 . . 1.402(10) ? C112 H112 . . .960 ? C113 C114 . . 1.364(10) ? C113 H113 . . .958 ? C114 C115 . . 1.399(10) ? C114 H114 . . .975 ? C115 C116 . . 1.375(9) ? C115 H115 . . .964 ? C116 H116 . . .972 ? C121 C122 . . 1.389(8) ? C121 C126 . . 1.391(8) ? C122 C123 . . 1.390(9) ? C122 H122 . . .960 ? C123 C124 . . 1.392(9) ? C123 H123 . . .963 ? C124 C125 . . 1.383(9) ? C124 H124 . . .945 ? C125 C126 . . 1.392(9) ? C125 H125 . . .966 ? C126 H126 . . .943 ? C131 C132 . . 1.386(9) ? C131 C136 . . 1.390(8) ? C132 C133 . . 1.401(8) ? C132 H132 . . .963 ? C133 C134 . . 1.392(9) ? C133 H133 . . .948 ? C134 C135 . . 1.382(10) ? C134 H134 . . .945 ? C135 C136 . . 1.390(10) ? C135 H135 . . .950 ? C136 H136 . . .966 ? P2 C211 . . 1.845(6) ? P2 C221 . . 1.847(6) ? P2 C231 . . 1.833(6) ? C211 C212 . . 1.392(9) ? C211 C216 . . 1.392(9) ? C212 C213 . . 1.418(9) ? C212 H212 . . .952 ? C213 C214 . . 1.390(11) ? C213 H213 . . .952 ? C214 C215 . . 1.385(10) ? C214 H214 . . .957 ? C215 C216 . . 1.392(10) ? C215 H215 . . .973 ? C216 H216 . . .974 ? C221 C222 . . 1.395(8) ? C221 C226 . . 1.393(9) ? C222 C223 . . 1.397(8) ? C222 H222 . . .957 ? C223 C224 . . 1.398(10) ? C223 H223 . . .961 ? C224 C225 . . 1.365(9) ? C224 H224 . . .959 ? C225 C226 . . 1.409(9) ? C225 H225 . . .957 ? C226 H226 . . .963 ? C231 C232 . . 1.387(9) ? C231 C236 . . 1.399(8) ? C232 C233 . . 1.403(9) ? C232 H232 . . .957 ? C233 C234 . . 1.396(9) ? C233 H233 . . .961 ? C234 C235 . . 1.383(9) ? C234 H234 . . .962 ? C235 C236 . . 1.391(8) ? C235 H235 . . .961 ? C236 H236 . . .965 ? C1 C2 . . 1.225(9) ? C2 C21 . . 1.421(9) ? C21 C22 . . 1.393(9) ? C21 C26 . . 1.400(10) ? C22 F22 . . 1.329(8) ? C22 C23 . . 1.389(10) ? C23 F23 . . 1.331(10) ? C23 C24 . . 1.375(12) ? C24 F24 . . 1.354(9) ? C24 C25 . . 1.359(13) ? C25 F25 . . 1.362(12) ? C25 C26 . . 1.364(12) ? C26 F26 . . 1.345(9) ? C101 C102 . . 1.416(9) ? C101 C105 . . 1.420(9) ? C101 H101 . . .974 ? C102 C103 . . 1.432(9) ? C102 H102 . . .961 ? C103 C104 . . 1.421(9) ? C103 H103 . . .961 ? C104 C105 . . 1.419(9) ? C104 H104 . . .965 ? C105 H105 . . .959 ? C01 C02 . . 1.40(6) ? C01 C06 . . 1.40(5) ? C01 H01 . . .95(5) ? C02 C03 . . 1.40(5) ? C02 H02 . . .95 ? C03 C04 . . 1.40(5) ? C03 H03 . . .95 ? C04 C05 . . 1.40(6) ? C04 H04 . . .95 ? C05 C06 . . 1.40(5) ? C05 H05 . . .95 ? C06 H06 . . .95 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 Ru P2 . . . 100.31(5) ? P1 Ru C1 . . . 92.29(17) ? P1 Ru C101 . . . 121.43(18) ? P1 Ru C102 . . . 93.30(17) ? P1 Ru C103 . . . 98.79(17) ? P1 Ru C104 . . . 132.64(17) ? P1 Ru C105 . . . 155.08(17) ? P2 Ru C1 . . . 87.38(17) ? P2 Ru C101 . . . 138.25(18) ? P2 Ru C102 . . . 151.80(18) ? P2 Ru C103 . . . 115.74(17) ? P2 Ru C104 . . . 91.58(17) ? P2 Ru C105 . . . 102.36(17) ? C1 Ru C101 . . . 90.3(2) ? C1 Ru C102 . . . 116.8(2) ? C1 Ru C103 . . . 151.7(2) ? C1 Ru C104 . . . 134.2(2) ? C1 Ru C105 . . . 98.9(2) ? C101 Ru C102 . . . 36.8(2) ? C101 Ru C103 . . . 61.7(2) ? C101 Ru C104 . . . 61.5(2) ? C101 Ru C105 . . . 37.0(2) ? C102 Ru C103 . . . 37.0(2) ? C102 Ru C104 . . . 61.5(2) ? C102 Ru C105 . . . 61.8(2) ? C103 Ru C104 . . . 36.8(2) ? C103 Ru C105 . . . 61.9(2) ? C104 Ru C105 . . . 36.9(2) ? Ru P1 C111 . . . 108.82(19) ? Ru P1 C121 . . . 115.31(18) ? Ru P1 C131 . . . 125.3(2) ? C111 P1 C121 . . . 101.9(3) ? C111 P1 C131 . . . 106.7(3) ? C121 P1 C131 . . . 96.0(3) ? P1 C111 C112 . . . 119.6(4) ? P1 C111 C116 . . . 121.4(5) ? C112 C111 C116 . . . 118.0(6) ? C111 C112 C113 . . . 120.4(6) ? C111 C112 H112 . . . 118.5 ? C113 C112 H112 . . . 121.0 ? C112 C113 C114 . . . 120.0(6) ? C112 C113 H113 . . . 118.9 ? C114 C113 H113 . . . 121.1 ? C113 C114 C115 . . . 120.4(6) ? C113 C114 H114 . . . 119.0 ? C115 C114 H114 . . . 120.6 ? C114 C115 C116 . . . 119.8(6) ? C114 C115 H115 . . . 119.3 ? C116 C115 H115 . . . 120.8 ? C111 C116 C115 . . . 121.4(6) ? C111 C116 H116 . . . 118.6 ? C115 C116 H116 . . . 120.0 ? P1 C121 C122 . . . 120.5(5) ? P1 C121 C126 . . . 120.0(4) ? C122 C121 C126 . . . 119.3(6) ? C121 C122 C123 . . . 120.4(6) ? C121 C122 H122 . . . 119.4 ? C123 C122 H122 . . . 120.2 ? C122 C123 C124 . . . 120.1(5) ? C122 C123 H123 . . . 120.6 ? C124 C123 H123 . . . 119.3 ? C123 C124 C125 . . . 119.5(6) ? C123 C124 H124 . . . 120.5 ? C125 C124 H124 . . . 119.9 ? C124 C125 C126 . . . 120.4(6) ? C124 C125 H125 . . . 120.8 ? C126 C125 H125 . . . 118.8 ? C121 C126 C125 . . . 120.2(5) ? C121 C126 H126 . . . 120.2 ? C125 C126 H126 . . . 119.6 ? P1 C131 C132 . . . 115.8(4) ? P1 C131 C136 . . . 124.6(5) ? C132 C131 C136 . . . 119.2(5) ? C131 C132 C133 . . . 121.0(5) ? C131 C132 H132 . . . 120.9 ? C133 C132 H132 . . . 118.1 ? C132 C133 C134 . . . 119.0(6) ? C132 C133 H133 . . . 120.2 ? C134 C133 H133 . . . 120.9 ? C133 C134 C135 . . . 120.3(6) ? C133 C134 H134 . . . 119.9 ? C135 C134 H134 . . . 119.9 ? C134 C135 C136 . . . 120.3(6) ? C134 C135 H135 . . . 118.8 ? C136 C135 H135 . . . 120.8 ? C131 C136 C135 . . . 120.3(6) ? C131 C136 H136 . . . 120.1 ? C135 C136 H136 . . . 119.6 ? Ru P2 C211 . . . 121.0(2) ? Ru P2 C221 . . . 107.93(18) ? Ru P2 C231 . . . 121.5(2) ? C211 P2 C221 . . . 100.3(3) ? C211 P2 C231 . . . 98.4(3) ? C221 P2 C231 . . . 104.9(3) ? P2 C211 C212 . . . 119.6(5) ? P2 C211 C216 . . . 120.8(5) ? C212 C211 C216 . . . 119.6(6) ? C211 C212 C213 . . . 119.9(6) ? C211 C212 H212 . . . 121.3 ? C213 C212 H212 . . . 118.8 ? C212 C213 C214 . . . 119.7(6) ? C212 C213 H213 . . . 120.4 ? C214 C213 H213 . . . 119.9 ? C213 C214 C215 . . . 120.0(6) ? C213 C214 H214 . . . 120.1 ? C215 C214 H214 . . . 119.9 ? C214 C215 C216 . . . 120.5(6) ? C214 C215 H215 . . . 118.8 ? C216 C215 H215 . . . 120.7 ? C211 C216 C215 . . . 120.4(6) ? C211 C216 H216 . . . 120.0 ? C215 C216 H216 . . . 119.5 ? P2 C221 C222 . . . 119.5(5) ? P2 C221 C226 . . . 121.7(4) ? C222 C221 C226 . . . 118.3(5) ? C221 C222 C223 . . . 120.9(6) ? C221 C222 H222 . . . 119.8 ? C223 C222 H222 . . . 119.3 ? C222 C223 C224 . . . 119.9(6) ? C222 C223 H223 . . . 119.8 ? C224 C223 H223 . . . 120.2 ? C223 C224 C225 . . . 119.6(6) ? C223 C224 H224 . . . 120.0 ? C225 C224 H224 . . . 120.4 ? C224 C225 C226 . . . 120.7(6) ? C224 C225 H225 . . . 120.2 ? C226 C225 H225 . . . 119.0 ? C221 C226 C225 . . . 120.4(6) ? C221 C226 H226 . . . 119.4 ? C225 C226 H226 . . . 120.2 ? P2 C231 C232 . . . 124.6(4) ? P2 C231 C236 . . . 116.8(4) ? C232 C231 C236 . . . 118.6(5) ? C231 C232 C233 . . . 120.6(5) ? C231 C232 H232 . . . 120.0 ? C233 C232 H232 . . . 119.3 ? C232 C233 C234 . . . 119.7(6) ? C232 C233 H233 . . . 120.3 ? C234 C233 H233 . . . 119.9 ? C233 C234 C235 . . . 119.9(6) ? C233 C234 H234 . . . 119.9 ? C235 C234 H234 . . . 120.2 ? C234 C235 C236 . . . 119.9(5) ? C234 C235 H235 . . . 120.1 ? C236 C235 H235 . . . 120.0 ? C231 C236 C235 . . . 121.1(6) ? C231 C236 H236 . . . 119.4 ? C235 C236 H236 . . . 119.6 ? Ru C1 C2 . . . 173.0(5) ? C1 C2 C21 . . . 169.2(6) ? C2 C21 C22 . . . 123.8(6) ? C2 C21 C26 . . . 121.4(6) ? C22 C21 C26 . . . 114.8(6) ? C21 C22 F22 . . . 119.2(6) ? C21 C22 C23 . . . 122.9(6) ? F22 C22 C23 . . . 117.9(6) ? C22 C23 F23 . . . 120.7(7) ? C22 C23 C24 . . . 119.0(7) ? F23 C23 C24 . . . 120.3(7) ? C23 C24 F24 . . . 120.2(8) ? C23 C24 C25 . . . 119.9(8) ? F24 C24 C25 . . . 119.8(8) ? C24 C25 F25 . . . 120.1(8) ? C24 C25 C26 . . . 120.5(8) ? F25 C25 C26 . . . 119.3(8) ? C21 C26 C25 . . . 122.8(7) ? C21 C26 F26 . . . 118.2(7) ? C25 C26 F26 . . . 119.0(7) ? Ru C101 C102 . . . 72.2(3) ? Ru C101 C105 . . . 71.7(3) ? Ru C101 H101 . . . 122.3 ? C102 C101 C105 . . . 108.6(6) ? C102 C101 H101 . . . 126.2 ? C105 C101 H101 . . . 125.2 ? Ru C102 C101 . . . 71.0(3) ? Ru C102 C103 . . . 72.0(4) ? Ru C102 H102 . . . 121.4 ? C101 C102 C103 . . . 108.0(6) ? C101 C102 H102 . . . 124.7 ? C103 C102 H102 . . . 127.3 ? Ru C103 C102 . . . 71.0(4) ? Ru C103 C104 . . . 70.8(4) ? Ru C103 H103 . . . 124.6 ? C102 C103 C104 . . . 107.0(5) ? C102 C103 H103 . . . 126.0 ? C104 C103 H103 . . . 127.0 ? Ru C104 C103 . . . 72.4(4) ? Ru C104 C105 . . . 71.5(4) ? Ru C104 H104 . . . 122.2 ? C103 C104 C105 . . . 109.0(6) ? C103 C104 H104 . . . 125.1 ? C105 C104 H104 . . . 125.8 ? Ru C105 C101 . . . 71.2(3) ? Ru C105 C104 . . . 71.6(3) ? Ru C105 H105 . . . 123.0 ? C101 C105 C104 . . . 107.3(5) ? C101 C105 H105 . . . 126.6 ? C104 C105 H105 . . . 126.2 ? C02 C01 C06 . . . 120(3) ? C02 C01 H01 . . . 120 ? C06 C01 H01 . . . 120 ? C01 C02 C03 . . . 120(3) ? C01 C02 H02 . . . 120 ? C03 C02 H02 . . . 120 ? C02 C03 C04 . . . 120(3) ? C02 C03 H03 . . . 120 ? C04 C03 H03 . . . 120 ? C03 C04 C05 . . . 120(3) ? C03 C04 H04 . . . 120 ? C05 C04 H04 . . . 120 ? C04 C05 C06 . . . 120(3) ? C04 C05 H05 . . . 120 ? C06 C05 H05 . . . 120 ? C01 C06 C05 . . . 120(3) ? C01 C06 H06 . . . 120 ? C05 C06 H06 . . . 120 ? _exptl_crystal_F_000 1876 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 33 _reflns_limit_l_min -23 _reflns_limit_l_max 23 _reflns_number_observed ? _reflns_d_resolution_high .73 _reflns_d_resolution_low 7.842 _diffrn_reflns_av_sigmaI/netI .083 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 100 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .096 _refine_ls_wR_factor_ref .135 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_shift/su_mean .0003 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_br1176_compound_2 _database_code_depnum_ccdc_archive 'CCDC 660620' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C39 H29 F5 P2 Ru1' _chemical_formula_moiety 'C39 H29 F5 P2 Ru1' _chemical_formula_weight 755.67 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 _symmetry_space_group_name_Hall p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 8.9880(10) _cell_length_b 15.065(2) _cell_length_c 23.420(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3171.2(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4117 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.24 _cell_measurement_temperature 170 _exptl_absorpt_coefficient_mu .654 _exptl_crystal_description rod _exptl_crystal_size_max .23 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .09 _exptl_crystal_size_rad ? _exptl_crystal_colour very_pale_yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .91 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 30061 _reflns_number_total 4570 _reflns_Friedel_coverage .97 _reflns_number_gt 4127 _reflns_threshold_expression 'I > 2.00 sig(I )' _diffrn_reflns_theta_max 29. _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .048 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .048 _refine_ls_wR_factor_gt .067 _refine_ls_goodness_of_fit_gt 1.195 _refine_ls_number_reflns 4127 _refine_ls_number_parameters 408 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w =1/(sig^2(F) + .002F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .045 _refine_diff_density_min -.725 _refine_diff_density_max .905 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack xabs refined' _refine_ls_abs_structure_Flack -.07(5) # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 156 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 116 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 20 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .44912(5) .52178(3) .62545(2) .0188(2) Uani ? ? 1.00000 ? ? P1 .59583(18) .50785(11) .54875(7) .0195(7) Uani ? ? 1.00000 ? ? C111 .5794(7) .3978(4) .5165(3) .023(3) Uani ? ? 1.00000 ? ? C112 .5021(8) .3841(5) .4663(3) .026(3) Uani ? ? 1.00000 ? ? C113 .4765(9) .2994(5) .4460(3) .034(4) Uani ? ? 1.00000 ? ? C114 .5309(9) .2261(5) .4755(4) .037(4) Uani ? ? 1.00000 ? ? C115 .6097(11) .2392(5) .5253(4) .044(5) Uani ? ? 1.00000 ? ? C116 .6318(11) .3244(5) .5451(4) .038(4) Uani ? ? 1.00000 ? ? C121 .5696(9) .5821(4) .4883(3) .028(3) Uani ? ? 1.00000 ? ? C122 .4618(9) .6477(5) .4890(3) .030(4) Uani ? ? 1.00000 ? ? C123 .4403(12) .7032(5) .4434(4) .045(5) Uani ? ? 1.00000 ? ? C124 .5299(13) .6943(6) .3958(4) .051(5) Uani ? ? 1.00000 ? ? C125 .6352(10) .6277(7) .3931(4) .045(5) Uani ? ? 1.00000 ? ? C126 .6553(10) .5731(6) .4396(3) .037(4) Uani ? ? 1.00000 ? ? C10 .7966(7) .5188(5) .5675(3) .023(3) Uani ? ? 1.00000 ? ? C20 .8111(7) .5562(4) .6282(3) .021(3) Uani ? ? 1.00000 ? ? P2 .66555(17) .50812(11) .67379(7) .0182(7) Uani ? ? 1.00000 ? ? C211 .7412(8) .4006(4) .6948(3) .023(3) Uani ? ? 1.00000 ? ? C212 .8837(8) .3723(5) .6793(3) .024(3) Uani ? ? 1.00000 ? ? C213 .9431(9) .2938(5) .7006(3) .029(3) Uani ? ? 1.00000 ? ? C214 .8611(9) .2434(5) .7390(3) .032(4) Uani ? ? 1.00000 ? ? C215 .7190(10) .2709(5) .7551(3) .036(4) Uani ? ? 1.00000 ? ? C216 .6601(9) .3480(5) .7328(3) .032(4) Uani ? ? 1.00000 ? ? C221 .6872(7) .5651(4) .7424(3) .020(3) Uani ? ? 1.00000 ? ? C222 .5679(9) .6074(5) .7672(3) .032(4) Uani ? ? 1.00000 ? ? C223 .5828(9) .6460(6) .8205(3) .036(4) Uani ? ? 1.00000 ? ? C224 .7152(10) .6419(5) .8496(3) .035(4) Uani ? ? 1.00000 ? ? C225 .8351(9) .5996(5) .8243(3) .034(4) Uani ? ? 1.00000 ? ? C226 .8222(8) .5609(5) .7714(3) .030(4) Uani ? ? 1.00000 ? ? C1 .5065(7) .6488(4) .6270(3) .023(3) Uani ? ? 1.00000 ? ? C2 .5442(8) .7255(4) .6278(3) .025(3) Uani ? ? 1.00000 ? ? C21 .5961(7) .8154(4) .6278(3) .022(3) Uani ? ? 1.00000 ? ? C22 .6966(9) .8457(5) .6676(3) .031(4) Uani ? ? 1.00000 ? ? F22 .7494(7) .7893(4) .7075(2) .050(3) Uani ? ? 1.00000 ? ? C23 .7517(10) .9307(6) .6668(4) .041(5) Uani ? ? 1.00000 ? ? F23 .8557(7) .9562(4) .7052(2) .059(3) Uani ? ? 1.00000 ? ? C24 .7024(9) .9899(5) .6272(4) .036(4) Uani ? ? 1.00000 ? ? F24 .7524(6) 1.0734(3) .6281(2) .053(3) Uani ? ? 1.00000 ? ? C25 .6010(9) .9627(5) .5867(3) .034(4) Uani ? ? 1.00000 ? ? F25 .5552(7) 1.0200(3) .5468(2) .056(3) Uani ? ? 1.00000 ? ? C26 .5527(8) .8769(5) .5870(3) .028(3) Uani ? ? 1.00000 ? ? F26 .4620(6) .8515(3) .5453(2) .043(3) Uani ? ? 1.00000 ? ? C104 .2901(8) .4324(6) .6718(4) .037(2) Uani ? ? 1.00000 ? ? C101 .2074(8) .5470(6) .6166(4) .043(2) Uani ? ? 1.00000 ? ? C102 .2435(9) .4772(7) .5809(4) .048(3) Uani ? ? 1.00000 ? ? C103 .2945(8) .4068(7) .6148(4) .046(3) Uani ? ? 1.00000 ? ? C105 .2338(8) .5211(6) .6745(4) .039(4) Uani ? ? 1.00000 ? ? H112 .46346 .43473 .44596 .03500 Uiso ? ? 1.00000 ? ? H113 .41929 .29012 .41154 .04100 Uiso ? ? 1.00000 ? ? H114 .51727 .16827 .45960 .04600 Uiso ? ? 1.00000 ? ? H115 .64462 .18899 .54678 .05500 Uiso ? ? 1.00000 ? ? H116 .68776 .33436 .58035 .04500 Uiso ? ? 1.00000 ? ? H122 .40133 .65388 .52308 .04200 Uiso ? ? 1.00000 ? ? H123 .36599 .74887 .44456 .05500 Uiso ? ? 1.00000 ? ? H124 .51158 .73290 .36368 .06200 Uiso ? ? 1.00000 ? ? H125 .70014 .62277 .35961 .05800 Uiso ? ? 1.00000 ? ? H126 .73050 .52598 .43791 .04900 Uiso ? ? 1.00000 ? ? H10a .84462 .46258 .56529 .03000 Uiso ? ? 1.00000 ? ? H10b .84445 .55841 .54104 .03000 Uiso ? ? 1.00000 ? ? H20a .80156 .61918 .62739 .02500 Uiso ? ? 1.00000 ? ? H20b .90683 .54150 .64347 .02500 Uiso ? ? 1.00000 ? ? H212 .94242 .40811 .65292 .03400 Uiso ? ? 1.00000 ? ? H213 1.03943 .27366 .68939 .03800 Uiso ? ? 1.00000 ? ? H214 .90342 .19084 .75561 .04400 Uiso ? ? 1.00000 ? ? H215 .66137 .23583 .78093 .04600 Uiso ? ? 1.00000 ? ? H216 .56403 .36781 .74490 .03700 Uiso ? ? 1.00000 ? ? H222 .47547 .61142 .74632 .03900 Uiso ? ? 1.00000 ? ? H223 .49958 .67520 .83812 .04500 Uiso ? ? 1.00000 ? ? H224 .72697 .66870 .88619 .04600 Uiso ? ? 1.00000 ? ? H225 .92827 .59657 .84436 .04300 Uiso ? ? 1.00000 ? ? H226 .90451 .53200 .75381 .03700 Uiso ? ? 1.00000 ? ? H101 .16994 .60525 .60616 .06700 Uiso ? ? 1.00000 ? ? H102 .23226 .47615 .54078 .06500 Uiso ? ? 1.00000 ? ? H103 .32562 .35065 .60171 .05900 Uiso ? ? 1.00000 ? ? H104 .32065 .39581 .70404 .04400 Uiso ? ? 1.00000 ? ? H105 .22013 .55550 .70871 .05400 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru .0129(2) .0203(2) .0232(2) -.0013(2) -.0000(2) .0012(2) P1 .0173(7) .0189(7) .0222(8) .0013(6) -.0005(6) .0008(6) C111 .021(3) .022(3) .026(3) .001(2) .000(3) -.003(2) C112 .031(4) .027(3) .020(3) -.008(3) -.000(3) .003(3) C113 .031(4) .033(4) .037(4) -.010(3) -.000(3) -.013(3) C114 .027(4) .031(4) .053(5) -.005(3) .002(4) -.008(3) C115 .044(5) .024(4) .063(6) .003(3) -.010(4) -.003(4) C116 .047(5) .028(4) .040(4) .000(3) -.013(4) -.000(3) C121 .041(4) .019(3) .023(3) -.012(3) -.008(3) .006(2) C122 .038(4) .029(3) .023(3) .001(3) -.005(3) .000(3) C123 .064(6) .031(4) .039(4) .000(4) -.020(5) -.001(3) C124 .080(7) .047(5) .027(4) -.019(5) -.014(5) .013(4) C125 .043(5) .055(5) .036(4) -.025(5) -.006(4) .009(4) C126 .041(4) .040(4) .029(4) -.008(4) .003(3) .004(3) C10 .021(3) .029(3) .017(3) .007(3) -.001(2) .003(3) C20 .020(3) .022(3) .022(3) -.004(2) -.007(3) -.007(3) P2 .0132(7) .0193(7) .0221(8) -.0007(6) .0000(6) .0004(6) C211 .025(3) .024(3) .021(3) .002(3) -.004(3) .006(2) C212 .020(3) .032(3) .021(3) .009(3) .001(3) .002(3) C213 .024(3) .028(3) .035(4) .007(3) -.001(3) -.001(3) C214 .035(4) .025(3) .036(4) .006(3) -.003(3) .003(3) C215 .044(5) .027(4) .038(4) -.012(3) -.000(4) .018(3) C216 .029(4) .032(4) .036(4) -.003(3) -.005(3) -.001(3) C221 .017(3) .024(3) .020(3) -.003(2) -.001(2) -.004(2) C222 .025(4) .041(4) .029(3) .000(3) .001(3) -.004(3) C223 .028(4) .047(4) .033(4) .004(3) .004(3) -.008(3) C224 .048(5) .032(4) .026(4) -.001(4) -.004(4) -.004(3) C225 .036(4) .039(4) .028(4) -.004(3) -.011(3) -.003(3) C226 .028(4) .034(4) .029(4) .007(3) -.002(3) -.008(3) C1 .021(3) .031(3) .017(3) .007(2) -.001(3) -.004(3) C2 .026(3) .023(3) .025(3) .003(3) .007(3) .001(3) C21 .023(3) .022(3) .022(3) -.000(2) .003(3) -.003(3) C22 .028(4) .036(4) .028(4) -.002(3) .005(3) .003(3) F22 .063(4) .054(3) .034(3) -.014(3) -.019(3) .006(2) C23 .050(5) .039(4) .034(4) -.018(4) .006(4) -.013(3) F23 .070(4) .069(4) .039(3) -.038(3) -.004(3) -.016(3) C24 .040(4) .025(3) .041(4) -.011(3) .015(4) -.011(3) F24 .060(4) .031(2) .066(3) -.019(3) .024(3) -.008(3) C25 .037(4) .023(3) .042(4) .005(3) .011(3) .003(3) F25 .076(4) .029(2) .063(3) -.000(3) -.001(3) .014(2) C26 .023(3) .029(3) .033(3) -.003(3) .005(3) -.008(3) F26 .049(3) .036(2) .045(3) .000(2) -.018(2) .002(2) C104 .0088(14) .050(2) .053(3) -.0053(18) -.0010(17) .007(2) C101 .0106(17) .055(3) .064(3) -.0053(18) -.0010(17) .009(2) C102 .021(3) .055(3) .069(3) .0080(12) -.0010(17) .008(2) C103 .0106(17) .061(3) .067(3) -.0046(15) -.0010(17) .008(2) C105 .016(3) .048(4) .051(5) -.005(4) .010(3) -.009(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru P1 . . 2.2383(17) ? Ru P2 . . 2.2601(16) ? Ru C1 . . 1.982(7) ? Ru C104 . . 2.244(8) ? Ru C101 . . 2.215(7) ? Ru C102 . . 2.226(9) ? Ru C103 . . 2.234(9) ? Ru C105 . . 2.250(8) ? P1 C111 . . 1.828(7) ? P1 C121 . . 1.820(7) ? P1 C10 . . 1.865(6) ? C111 C112 . . 1.381(10) ? C111 C116 . . 1.375(10) ? C112 C113 . . 1.382(10) ? C112 H112 . . .964 ? C113 C114 . . 1.391(11) ? C113 H113 . . .966 ? C114 C115 . . 1.378(13) ? C114 H114 . . .956 ? C115 C116 . . 1.378(11) ? C115 H115 . . .962 ? C116 H116 . . .980 ? C121 C122 . . 1.385(11) ? C121 C126 . . 1.382(11) ? C122 C123 . . 1.371(11) ? C122 H122 . . .970 ? C123 C124 . . 1.381(14) ? C123 H123 . . .959 ? C124 C125 . . 1.381(15) ? C124 H124 . . .965 ? C125 C126 . . 1.376(12) ? C125 H125 . . .981 ? C126 H126 . . .981 ? C10 C20 . . 1.534(9) ? C10 H10a . . .953 ? C10 H10b . . .962 ? C20 P2 . . 1.837(7) ? C20 H20a . . .953 ? C20 H20b . . .957 ? P2 C211 . . 1.824(7) ? P2 C221 . . 1.833(6) ? C211 C212 . . 1.397(10) ? C211 C216 . . 1.397(10) ? C212 C213 . . 1.391(10) ? C212 H212 . . .975 ? C213 C214 . . 1.389(11) ? C213 H213 . . .954 ? C214 C215 . . 1.394(12) ? C214 H214 . . .961 ? C215 C216 . . 1.379(11) ? C215 H215 . . .956 ? C216 H216 . . .956 ? C221 C222 . . 1.376(10) ? C221 C226 . . 1.392(10) ? C222 C223 . . 1.385(11) ? C222 H222 . . .966 ? C223 C224 . . 1.372(12) ? C223 H223 . . .960 ? C224 C225 . . 1.385(12) ? C224 H224 . . .954 ? C225 C226 . . 1.374(11) ? C225 H225 . . .961 ? C226 H226 . . .952 ? C1 C2 . . 1.205(9) ? C2 C21 . . 1.432(9) ? C21 C22 . . 1.378(10) ? C21 C26 . . 1.386(10) ? C22 F22 . . 1.349(9) ? C22 C23 . . 1.372(11) ? C23 F23 . . 1.353(10) ? C23 C24 . . 1.360(11) ? C24 F24 . . 1.336(8) ? C24 C25 . . 1.379(11) ? C25 F25 . . 1.335(9) ? C25 C26 . . 1.364(10) ? C26 F26 . . 1.329(9) ? C104 C103 . . 1.389(13) ? C104 C105 . . 1.430(13) ? C104 H104 . . .975 ? C101 C102 . . 1.383(14) ? C101 C105 . . 1.430(13) ? C101 H101 . . .971 ? C102 C103 . . 1.402(14) ? C102 H102 . . .946 ? C103 H103 . . .943 ? C105 H105 . . .963 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 Ru P2 . . . 83.48(6) ? P1 Ru C1 . . . 87.2(2) ? P1 Ru C104 . . . 135.0(2) ? P1 Ru C101 . . . 121.3(2) ? P1 Ru C102 . . . 94.9(3) ? P1 Ru C103 . . . 101.8(2) ? P1 Ru C105 . . . 156.3(2) ? P2 Ru C1 . . . 81.6(2) ? P2 Ru C104 . . . 104.6(2) ? P2 Ru C101 . . . 155.0(2) ? P2 Ru C102 . . . 157.2(3) ? P2 Ru C103 . . . 121.4(2) ? P2 Ru C105 . . . 119.0(2) ? C1 Ru C104 . . . 137.4(3) ? C1 Ru C101 . . . 95.2(3) ? C1 Ru C102 . . . 121.1(3) ? C1 Ru C103 . . . 155.8(3) ? C1 Ru C105 . . . 102.6(3) ? C104 Ru C101 . . . 61.5(3) ? C104 Ru C102 . . . 61.1(3) ? C104 Ru C103 . . . 36.1(3) ? C104 Ru C105 . . . 37.1(3) ? C101 Ru C102 . . . 36.3(4) ? C101 Ru C103 . . . 60.8(3) ? C101 Ru C105 . . . 37.3(3) ? C102 Ru C103 . . . 36.6(4) ? C102 Ru C105 . . . 61.5(3) ? C103 Ru C105 . . . 61.2(3) ? Ru P1 C111 . . . 111.6(2) ? Ru P1 C121 . . . 119.4(2) ? Ru P1 C10 . . . 111.9(2) ? C111 P1 C121 . . . 103.0(3) ? C111 P1 C10 . . . 104.9(3) ? C121 P1 C10 . . . 104.7(3) ? P1 C111 C112 . . . 121.8(5) ? P1 C111 C116 . . . 120.1(5) ? C112 C111 C116 . . . 117.8(6) ? C111 C112 C113 . . . 121.0(7) ? C111 C112 H112 . . . 119.0 ? C113 C112 H112 . . . 120.0 ? C112 C113 C114 . . . 120.2(7) ? C112 C113 H113 . . . 120.6 ? C114 C113 H113 . . . 119.2 ? C113 C114 C115 . . . 119.2(7) ? C113 C114 H114 . . . 119.0 ? C115 C114 H114 . . . 121.7 ? C114 C115 C116 . . . 119.5(8) ? C114 C115 H115 . . . 119.8 ? C116 C115 H115 . . . 120.6 ? C111 C116 C115 . . . 122.4(8) ? C111 C116 H116 . . . 117.5 ? C115 C116 H116 . . . 120.1 ? P1 C121 C122 . . . 121.3(5) ? P1 C121 C126 . . . 120.6(6) ? C122 C121 C126 . . . 118.1(6) ? C121 C122 C123 . . . 121.6(7) ? C121 C122 H122 . . . 118.1 ? C123 C122 H122 . . . 120.3 ? C122 C123 C124 . . . 119.2(9) ? C122 C123 H123 . . . 120.8 ? C124 C123 H123 . . . 120.0 ? C123 C124 C125 . . . 120.5(8) ? C123 C124 H124 . . . 118.1 ? C125 C124 H124 . . . 121.3 ? C124 C125 C126 . . . 119.2(8) ? C124 C125 H125 . . . 120.0 ? C126 C125 H125 . . . 120.6 ? C121 C126 C125 . . . 121.4(8) ? C121 C126 H126 . . . 119.2 ? C125 C126 H126 . . . 119.4 ? P1 C10 C20 . . . 109.5(4) ? P1 C10 H10a . . . 110.2 ? P1 C10 H10b . . . 109.6 ? C20 C10 H10a . . . 109.8 ? C20 C10 H10b . . . 109.4 ? H10a C10 H10b . . . 108.3 ? C10 C20 P2 . . . 109.5(4) ? C10 C20 H20a . . . 109.8 ? C10 C20 H20b . . . 109.7 ? P2 C20 H20a . . . 109.9 ? P2 C20 H20b . . . 109.4 ? H20a C20 H20b . . . 108.6 ? Ru P2 C20 . . . 106.6(2) ? Ru P2 C211 . . . 122.5(2) ? Ru P2 C221 . . . 119.2(2) ? C20 P2 C211 . . . 104.0(3) ? C20 P2 C221 . . . 104.4(3) ? C211 P2 C221 . . . 98.0(3) ? P2 C211 C212 . . . 122.8(5) ? P2 C211 C216 . . . 118.7(5) ? C212 C211 C216 . . . 118.1(6) ? C211 C212 C213 . . . 121.2(6) ? C211 C212 H212 . . . 119.5 ? C213 C212 H212 . . . 119.3 ? C212 C213 C214 . . . 119.6(7) ? C212 C213 H213 . . . 121.4 ? C214 C213 H213 . . . 119.1 ? C213 C214 C215 . . . 119.9(7) ? C213 C214 H214 . . . 120.2 ? C215 C214 H214 . . . 119.9 ? C214 C215 C216 . . . 120.0(7) ? C214 C215 H215 . . . 120.2 ? C216 C215 H215 . . . 119.8 ? C211 C216 C215 . . . 121.2(7) ? C211 C216 H216 . . . 118.9 ? C215 C216 H216 . . . 119.8 ? P2 C221 C222 . . . 120.3(5) ? P2 C221 C226 . . . 119.9(5) ? C222 C221 C226 . . . 119.7(6) ? C221 C222 C223 . . . 120.0(7) ? C221 C222 H222 . . . 119.1 ? C223 C222 H222 . . . 120.9 ? C222 C223 C224 . . . 120.8(7) ? C222 C223 H223 . . . 120.3 ? C224 C223 H223 . . . 118.9 ? C223 C224 C225 . . . 119.0(7) ? C223 C224 H224 . . . 121.5 ? C225 C224 H224 . . . 119.5 ? C224 C225 C226 . . . 121.0(8) ? C224 C225 H225 . . . 119.4 ? C226 C225 H225 . . . 119.6 ? C221 C226 C225 . . . 119.6(7) ? C221 C226 H226 . . . 119.2 ? C225 C226 H226 . . . 121.2 ? Ru C1 C2 . . . 178.7(6) ? C1 C2 C21 . . . 177.2(7) ? C2 C21 C22 . . . 121.8(6) ? C2 C21 C26 . . . 122.7(6) ? C22 C21 C26 . . . 115.4(6) ? C21 C22 F22 . . . 119.4(7) ? C21 C22 C23 . . . 122.5(7) ? F22 C22 C23 . . . 118.1(7) ? C22 C23 F23 . . . 120.4(7) ? C22 C23 C24 . . . 120.3(8) ? F23 C23 C24 . . . 119.4(7) ? C23 C24 F24 . . . 119.8(7) ? C23 C24 C25 . . . 119.3(7) ? F24 C24 C25 . . . 120.8(7) ? C24 C25 F25 . . . 119.6(6) ? C24 C25 C26 . . . 119.1(7) ? F25 C25 C26 . . . 121.3(7) ? C21 C26 C25 . . . 123.3(7) ? C21 C26 F26 . . . 119.1(6) ? C25 C26 F26 . . . 117.6(6) ? Ru C104 C103 . . . 71.6(5) ? Ru C104 C105 . . . 71.7(5) ? Ru C104 H104 . . . 122.3 ? C103 C104 C105 . . . 108.1(8) ? C103 C104 H104 . . . 125.3 ? C105 C104 H104 . . . 126.5 ? Ru C101 C102 . . . 72.3(5) ? Ru C101 C105 . . . 72.7(4) ? Ru C101 H101 . . . 121.2 ? C102 C101 C105 . . . 109.0(8) ? C102 C101 H101 . . . 128.0 ? C105 C101 H101 . . . 122.9 ? Ru C102 C101 . . . 71.4(5) ? Ru C102 C103 . . . 72.0(5) ? Ru C102 H102 . . . 124.0 ? C101 C102 C103 . . . 108.0(9) ? C101 C102 H102 . . . 126.1 ? C103 C102 H102 . . . 125.9 ? Ru C103 C104 . . . 72.3(5) ? Ru C103 C102 . . . 71.4(5) ? Ru C103 H103 . . . 123.2 ? C104 C103 C102 . . . 109.0(9) ? C104 C103 H103 . . . 124.8 ? C102 C103 H103 . . . 126.2 ? Ru C105 C104 . . . 71.2(4) ? Ru C105 C101 . . . 70.0(4) ? Ru C105 H105 . . . 122.2 ? C104 C105 C101 . . . 105.8(8) ? C104 C105 H105 . . . 125.8 ? C101 C105 H105 . . . 128.4 ? _exptl_crystal_F_000 1528 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .723 _reflns_d_resolution_low 12.638 _diffrn_reflns_av_sigmaI/netI .051 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 170 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .056 _refine_ls_wR_factor_ref .071 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_shift/su_mean .008 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_br1177_compound_3 _database_code_depnum_ccdc_archive 'CCDC 660621' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C44 H39 F5 P2 Ru1' _chemical_formula_moiety 'C44 H39 F5 P2 Ru1' _chemical_formula_weight 825.8 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 8.6050(10) _cell_length_b 25.438(3) _cell_length_c 17.212(2) _cell_angle_alpha 90.00000 _cell_angle_beta 100.864(2) _cell_angle_gamma 90.00000 _cell_volume 3700.1(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4606 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.41 _cell_measurement_temperature 170 _exptl_absorpt_coefficient_mu .567 _exptl_crystal_description rod _exptl_crystal_size_max .36 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour very_pale_yellow _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .91 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 33123 _reflns_number_total 9336 _reflns_Friedel_coverage 0 _reflns_number_gt 7506 _reflns_threshold_expression 'I > 2.00 sig(I)' _diffrn_reflns_theta_max 28.8 _diffrn_reflns_theta_full 28.8 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .043 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .044 _refine_ls_wR_factor_gt .080 _refine_ls_goodness_of_fit_gt .962 _refine_ls_number_reflns 9336 _refine_ls_number_parameters 469 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w =1/(sig^2(F^2) + 22F^2) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -.915 _refine_diff_density_max 1.021 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 176 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 156 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 20 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .33353(3) .618800(9) .232617(14) .01468(11) Uani ? ? 1.00000 ? ? P1 .46139(9) .54481(3) .28322(5) .0172(3) Uani ? ? 1.00000 ? ? C111 .3456(4) .49131(13) .3177(2) .0223(14) Uani ? ? 1.00000 ? ? C112 .2832(4) .45189(14) .2642(2) .0268(15) Uani ? ? 1.00000 ? ? C113 .1881(4) .41289(14) .2864(3) .0346(18) Uani ? ? 1.00000 ? ? C114 .1539(5) .41223(17) .3619(3) .042(2) Uani ? ? 1.00000 ? ? C115 .2134(5) .4514(2) .4146(3) .043(2) Uani ? ? 1.00000 ? ? C116 .3080(5) .49123(16) .3933(2) .0313(17) Uani ? ? 1.00000 ? ? C121 .5743(4) .50523(12) .2236(2) .0196(13) Uani ? ? 1.00000 ? ? C122 .5622(4) .51351(14) .1431(2) .0254(15) Uani ? ? 1.00000 ? ? C123 .6510(4) .48365(14) .0997(2) .0273(16) Uani ? ? 1.00000 ? ? C124 .7530(4) .44550(15) .1370(2) .0299(17) Uani ? ? 1.00000 ? ? C125 .7643(4) .43619(14) .2169(2) .0307(17) Uani ? ? 1.00000 ? ? C126 .6745(4) .46511(13) .2598(2) .0238(15) Uani ? ? 1.00000 ? ? C10 .6154(4) .56117(13) .37170(19) .0216(14) Uani ? ? 1.00000 ? ? C20 .6505(4) .62032(13) .3749(2) .0200(13) Uani ? ? 1.00000 ? ? P2 .45857(9) .65340(3) .34854(5) .0170(3) Uani ? ? 1.00000 ? ? C211 .3795(4) .64427(13) .43936(19) .0214(14) Uani ? ? 1.00000 ? ? C212 .2363(4) .61958(15) .4372(2) .0289(16) Uani ? ? 1.00000 ? ? C213 .1739(5) .6128(2) .5053(3) .042(2) Uani ? ? 1.00000 ? ? C214 .2587(5) .62999(17) .5772(2) .036(2) Uani ? ? 1.00000 ? ? C215 .4045(5) .65390(17) .5812(2) .036(2) Uani ? ? 1.00000 ? ? C216 .4642(5) .66113(15) .5126(2) .0298(17) Uani ? ? 1.00000 ? ? C221 .4974(4) .72456(12) .3496(2) .0205(13) Uani ? ? 1.00000 ? ? C222 .6048(4) .74387(14) .3059(2) .0265(15) Uani ? ? 1.00000 ? ? C223 .6211(5) .79735(15) .2961(2) .0315(17) Uani ? ? 1.00000 ? ? C224 .5298(5) .83228(14) .3296(2) .0341(18) Uani ? ? 1.00000 ? ? C225 .4235(5) .81324(15) .3738(3) .0362(19) Uani ? ? 1.00000 ? ? C226 .4067(5) .75957(15) .3839(2) .0296(17) Uani ? ? 1.00000 ? ? C1 .5232(4) .63848(12) .18738(19) .0196(13) Uani ? ? 1.00000 ? ? C2 .6199(4) .65352(14) .1490(2) .0250(15) Uani ? ? 1.00000 ? ? C21 .7120(4) .67140(14) .09236(19) .0220(14) Uani ? ? 1.00000 ? ? C22 .7567(4) .72392(14) .0872(2) .0245(15) Uani ? ? 1.00000 ? ? F22 .7200(3) .75927(9) .13844(14) .0391(12) Uani ? ? 1.00000 ? ? C23 .8388(4) .74191(16) .0306(2) .0307(17) Uani ? ? 1.00000 ? ? F23 .8785(3) .79268(10) .02845(16) .0453(13) Uani ? ? 1.00000 ? ? C24 .8812(4) .70733(17) -.0230(2) .0329(18) Uani ? ? 1.00000 ? ? F24 .9630(3) .72377(12) -.07783(15) .0471(14) Uani ? ? 1.00000 ? ? C25 .8377(4) .65540(17) -.0207(2) .0318(18) Uani ? ? 1.00000 ? ? F25 .8775(3) .62105(11) -.07370(15) .0458(14) Uani ? ? 1.00000 ? ? C26 .7560(4) .63834(15) .0356(2) .0284(16) Uani ? ? 1.00000 ? ? F26 .7135(3) .58748(10) .03435(15) .0428(13) Uani ? ? 1.00000 ? ? C101 .1935(4) .63626(14) .1118(2) .0239(15) Uani ? ? 1.00000 ? ? C1011 .2593(5) .64114(17) .0377(2) .0323(18) Uani ? ? 1.00000 ? ? C102 .1289(4) .59015(14) .1395(2) .0220(14) Uani ? ? 1.00000 ? ? C1021 .1048(5) .53774(16) .0969(2) .0354(18) Uani ? ? 1.00000 ? ? C103 .0690(4) .60358(13) .2091(2) .0214(14) Uani ? ? 1.00000 ? ? C1031 -.0309(4) .56762(15) .2494(2) .0289(16) Uani ? ? 1.00000 ? ? C104 .0948(3) .65835(13) .2235(2) .0210(14) Uani ? ? 1.00000 ? ? C1041 .0303(4) .69173(16) .2818(2) .0307(17) Uani ? ? 1.00000 ? ? C105 .1760(4) .67878(14) .1643(2) .0230(14) Uani ? ? 1.00000 ? ? C1051 .2217(5) .73473(15) .1545(3) .0342(18) Uani ? ? 1.00000 ? ? H112 .30793 .45148 .21279 .03400 Uiso ? ? 1.00000 ? ? H113 .14322 .38677 .24914 .04200 Uiso ? ? 1.00000 ? ? H114 .09269 .38412 .37770 .04900 Uiso ? ? 1.00000 ? ? H115 .18339 .45239 .46530 .04900 Uiso ? ? 1.00000 ? ? H116 .35025 .51744 .42982 .03800 Uiso ? ? 1.00000 ? ? H122 .49117 .53947 .11733 .03100 Uiso ? ? 1.00000 ? ? H123 .64421 .49011 .04436 .03500 Uiso ? ? 1.00000 ? ? H124 .81650 .42574 .10722 .03500 Uiso ? ? 1.00000 ? ? H125 .83411 .40944 .24276 .03500 Uiso ? ? 1.00000 ? ? H126 .67794 .45789 .31454 .02900 Uiso ? ? 1.00000 ? ? H10a .57970 .55065 .41827 .02500 Uiso ? ? 1.00000 ? ? H10b .71060 .54224 .36865 .02500 Uiso ? ? 1.00000 ? ? H20a .71800 .62920 .33927 .02400 Uiso ? ? 1.00000 ? ? H20b .70202 .62993 .42755 .02400 Uiso ? ? 1.00000 ? ? H212 .17645 .60649 .38777 .03600 Uiso ? ? 1.00000 ? ? H213 .07474 .59573 .50317 .04900 Uiso ? ? 1.00000 ? ? H214 .21297 .62509 .62328 .04200 Uiso ? ? 1.00000 ? ? H215 .46187 .66525 .63097 .04300 Uiso ? ? 1.00000 ? ? H216 .56503 .67803 .51543 .03500 Uiso ? ? 1.00000 ? ? H222 .66905 .71983 .28276 .03000 Uiso ? ? 1.00000 ? ? H223 .69599 .81036 .26669 .03600 Uiso ? ? 1.00000 ? ? H224 .54228 .86890 .32294 .04000 Uiso ? ? 1.00000 ? ? H225 .35792 .83803 .39627 .04100 Uiso ? ? 1.00000 ? ? H226 .33443 .74648 .41564 .03200 Uiso ? ? 1.00000 ? ? H1011a .31927 .61016 .03107 .04700 Uiso ? ? 1.00000 ? ? H1011b .32831 .67070 .04176 .04700 Uiso ? ? 1.00000 ? ? H1011c .17659 .64543 -.00718 .04700 Uiso ? ? 1.00000 ? ? H1021a .19540 .53004 .07502 .05200 Uiso ? ? 1.00000 ? ? H1021b .01474 .54069 .05518 .05200 Uiso ? ? 1.00000 ? ? H1021c .08906 .51097 .13305 .05200 Uiso ? ? 1.00000 ? ? H1031a -.13674 .56625 .22057 .04400 Uiso ? ? 1.00000 ? ? H1031b .01231 .53303 .25321 .04400 Uiso ? ? 1.00000 ? ? H1031c -.03280 .57970 .30195 .04400 Uiso ? ? 1.00000 ? ? H1041a -.04205 .71647 .25422 .04500 Uiso ? ? 1.00000 ? ? H1041b .11553 .71011 .31435 .04500 Uiso ? ? 1.00000 ? ? H1041c -.02075 .67016 .31495 .04500 Uiso ? ? 1.00000 ? ? H1051a .18773 .75443 .19525 .04900 Uiso ? ? 1.00000 ? ? H1051b .16583 .74621 .10453 .04900 Uiso ? ? 1.00000 ? ? H1051c .33317 .73751 .15939 .04900 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru .01381(11) .01511(12) .01549(12) .00001(8) .00373(8) -.00017(8) P1 .0178(4) .0153(3) .0185(4) .0000(3) .0037(3) .0000(3) C111 .0179(14) .0213(15) .0287(17) .0015(12) .0067(12) .0055(13) C112 .0210(15) .0240(16) .038(2) .0000(13) .0105(14) -.0055(14) C113 .0264(18) .0198(16) .059(3) -.0012(14) .0124(17) -.0040(16) C114 .0251(18) .037(2) .062(3) -.0057(16) .0049(18) .022(2) C115 .032(2) .059(3) .037(2) -.010(2) .0073(17) .018(2) C116 .036(2) .033(2) .0250(17) -.0055(16) .0056(15) .0053(14) C121 .0149(13) .0164(14) .0285(16) .0013(11) .0069(12) -.0007(12) C122 .0251(16) .0239(16) .0265(17) .0020(13) .0029(13) -.0030(13) C123 .0355(19) .0298(18) .0197(15) .0039(14) .0131(14) -.0024(13) C124 .0262(17) .0293(18) .036(2) -.0045(14) .0115(15) -.0093(15) C125 .0239(17) .0228(17) .045(2) .0057(13) .0057(15) -.0019(15) C126 .0251(16) .0212(16) .0257(16) .0030(12) .0060(13) .0003(12) C10 .0217(15) .0204(15) .0200(15) .0032(12) -.0028(12) -.0001(12) C20 .0138(13) .0230(15) .0231(15) -.0010(11) .0029(11) -.0009(12) P2 .0165(3) .0166(4) .0182(4) -.0008(3) .0044(3) -.0012(3) C211 .0264(16) .0206(15) .0177(14) .0055(12) .0055(12) .0031(11) C212 .0267(17) .034(2) .0276(18) -.0017(14) .0092(14) .0033(14) C213 .039(2) .051(3) .042(2) -.004(2) .0192(18) .006(2) C214 .045(2) .040(2) .0281(19) .0119(18) .0201(17) .0108(16) C215 .050(2) .037(2) .0191(16) .0013(18) .0027(16) .0004(15) C216 .0333(19) .034(2) .0234(17) .0018(15) .0077(14) -.0043(14) C221 .0210(14) .0182(14) .0216(15) -.0017(11) .0025(12) -.0038(11) C222 .0263(16) .0268(17) .0288(17) -.0034(13) .0114(14) -.0066(14) C223 .035(2) .0289(18) .0329(19) -.0077(15) .0116(15) .0015(15) C224 .049(2) .0181(16) .036(2) -.0047(15) .0107(17) -.0009(14) C225 .049(2) .0203(17) .042(2) .0051(16) .0171(18) -.0028(16) C226 .036(2) .0260(18) .0293(18) .0009(15) .0131(15) -.0019(14) C1 .0214(14) .0182(14) .0192(14) .0013(11) .0037(11) -.0010(11) C2 .0208(15) .0288(17) .0246(16) -.0017(13) .0022(12) .0015(13) C21 .0171(14) .0300(17) .0187(14) .0012(12) .0028(11) .0073(12) C22 .0195(15) .0309(18) .0226(16) .0028(13) .0031(12) .0057(13) F22 .0515(15) .0302(12) .0395(13) .0013(10) .0186(11) .0016(10) C23 .0242(17) .033(2) .035(2) .0000(14) .0077(14) .0129(15) F23 .0485(15) .0355(13) .0554(16) -.0035(11) .0186(12) .0188(12) C24 .0234(16) .047(2) .0309(18) .0003(15) .0106(14) .0153(16) F24 .0407(13) .0661(18) .0409(14) .0039(12) .0242(11) .0225(13) C25 .0274(17) .043(2) .0282(18) .0039(16) .0126(14) .0008(16) F25 .0491(15) .0573(17) .0359(13) .0071(13) .0208(11) -.0059(12) C26 .0248(16) .034(2) .0272(17) -.0004(14) .0068(14) .0037(14) F26 .0557(16) .0330(13) .0457(14) -.0099(11) .0249(12) -.0058(11) C101 .0204(15) .0325(18) .0174(15) .0036(13) -.0004(12) -.0010(13) C1011 .0315(18) .049(2) .0164(16) -.0001(17) .0030(13) .0025(15) C102 .0150(14) .0282(17) .0211(15) -.0032(12) -.0007(11) -.0030(12) C1021 .0302(19) .033(2) .040(2) -.0013(15) -.0034(16) -.0150(16) C103 .0137(13) .0231(16) .0273(16) -.0004(12) .0035(12) .0021(13) C1031 .0215(16) .0329(19) .0333(18) -.0084(14) .0075(14) .0037(15) C104 .0114(13) .0267(16) .0243(15) .0040(11) .0019(11) -.0011(12) C1041 .0239(16) .036(2) .0337(19) .0079(14) .0088(14) -.0073(15) C105 .0195(14) .0255(16) .0226(15) .0037(12) .0004(12) .0025(13) C1051 .0312(19) .0247(18) .044(2) -.0032(14) -.0001(16) .0099(16) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru P1 . . 2.2694(8) ? Ru P2 . . 2.2592(8) ? Ru C1 . . 2.000(3) ? Ru C101 . . 2.242(3) ? Ru C102 . . 2.267(3) ? Ru C103 . . 2.269(3) ? Ru C104 . . 2.266(3) ? Ru C105 . . 2.224(3) ? P1 C111 . . 1.849(4) ? P1 C121 . . 1.840(4) ? P1 C10 . . 1.868(3) ? C111 C112 . . 1.398(5) ? C111 C116 . . 1.399(5) ? C112 C113 . . 1.385(5) ? C112 H112 . . .949 ? C113 C114 . . 1.386(7) ? C113 H113 . . .954 ? C114 C115 . . 1.380(6) ? C114 H114 . . .957 ? C115 C116 . . 1.391(6) ? C115 H115 . . .955 ? C116 H116 . . .941 ? C121 C122 . . 1.386(5) ? C121 C126 . . 1.404(4) ? C122 C123 . . 1.391(5) ? C122 H122 . . .951 ? C123 C124 . . 1.383(5) ? C123 H123 . . .957 ? C124 C125 . . 1.381(6) ? C124 H124 . . .959 ? C125 C126 . . 1.378(6) ? C125 H125 . . .960 ? C126 H126 . . .955 ? C10 C20 . . 1.534(5) ? C10 H10a . . .949 ? C10 H10b . . .960 ? C20 P2 . . 1.833(3) ? C20 H20a . . .948 ? C20 H20b . . .962 ? P2 C211 . . 1.834(4) ? P2 C221 . . 1.840(3) ? C211 C212 . . 1.377(5) ? C211 C216 . . 1.399(5) ? C212 C213 . . 1.390(6) ? C212 H212 . . .967 ? C213 C214 . . 1.383(6) ? C213 H213 . . .952 ? C214 C215 . . 1.384(6) ? C214 H214 . . .958 ? C215 C216 . . 1.386(6) ? C215 H215 . . .949 ? C216 H216 . . .962 ? C221 C222 . . 1.387(5) ? C221 C226 . . 1.387(5) ? C222 C223 . . 1.381(5) ? C222 H222 . . .960 ? C223 C224 . . 1.383(6) ? C223 H223 . . .950 ? C224 C225 . . 1.383(7) ? C224 H224 . . .947 ? C225 C226 . . 1.387(5) ? C225 H225 . . .974 ? C226 H226 . . .961 ? C1 C2 . . 1.217(5) ? C2 C21 . . 1.442(5) ? C21 C22 . . 1.398(5) ? C21 C26 . . 1.394(5) ? C22 F22 . . 1.338(4) ? C22 C23 . . 1.384(6) ? C23 F23 . . 1.338(5) ? C23 C24 . . 1.373(6) ? C24 F24 . . 1.346(5) ? C24 C25 . . 1.375(6) ? C25 F25 . . 1.352(5) ? C25 C26 . . 1.371(6) ? C26 F26 . . 1.344(5) ? C101 C1011 . . 1.495(5) ? C101 C102 . . 1.418(5) ? C101 C105 . . 1.435(5) ? C1011 H1011a . . .960 ? C1011 H1011b . . .953 ? C1011 H1011c . . .953 ? C102 C1021 . . 1.516(5) ? C102 C103 . . 1.432(5) ? C1021 H1021a . . .948 ? C1021 H1021b . . .956 ? C1021 H1021c . . .949 ? C103 C1031 . . 1.510(5) ? C103 C104 . . 1.425(5) ? C1031 H1031a . . .952 ? C1031 H1031b . . .953 ? C1031 H1031c . . .958 ? C104 C1041 . . 1.499(5) ? C104 C105 . . 1.437(5) ? C1041 H1041a . . .947 ? C1041 H1041b . . .957 ? C1041 H1041c . . .956 ? C105 C1051 . . 1.494(5) ? C1051 H1051a . . .952 ? C1051 H1051b . . .949 ? C1051 H1051c . . .949 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 Ru P2 . . . 82.44(3) ? P1 Ru C1 . . . 89.12(9) ? P1 Ru C101 . . . 131.08(10) ? P1 Ru C102 . . . 105.11(9) ? P1 Ru C103 . . . 108.93(9) ? P1 Ru C104 . . . 139.68(9) ? P1 Ru C105 . . . 167.12(9) ? P2 Ru C1 . . . 87.62(9) ? P2 Ru C101 . . . 145.59(10) ? P2 Ru C102 . . . 157.98(9) ? P2 Ru C103 . . . 121.26(9) ? P2 Ru C104 . . . 99.37(8) ? P2 Ru C105 . . . 109.95(9) ? C1 Ru C101 . . . 85.69(12) ? C1 Ru C102 . . . 112.80(12) ? C1 Ru C103 . . . 146.95(12) ? C1 Ru C104 . . . 131.12(12) ? C1 Ru C105 . . . 94.77(13) ? C101 Ru C102 . . . 36.66(13) ? C101 Ru C103 . . . 61.49(13) ? C101 Ru C104 . . . 61.71(12) ? C101 Ru C105 . . . 37.47(13) ? C102 Ru C103 . . . 36.81(12) ? C102 Ru C104 . . . 61.34(12) ? C102 Ru C105 . . . 62.08(12) ? C103 Ru C104 . . . 36.63(12) ? C103 Ru C105 . . . 62.09(12) ? C104 Ru C105 . . . 37.33(13) ? Ru P1 C111 . . . 118.82(11) ? Ru P1 C121 . . . 120.57(11) ? Ru P1 C10 . . . 110.26(11) ? C111 P1 C121 . . . 98.59(15) ? C111 P1 C10 . . . 104.16(15) ? C121 P1 C10 . . . 102.03(14) ? P1 C111 C112 . . . 118.7(3) ? P1 C111 C116 . . . 122.2(3) ? C112 C111 C116 . . . 118.9(3) ? C111 C112 C113 . . . 120.4(4) ? C111 C112 H112 . . . 119.8 ? C113 C112 H112 . . . 119.8 ? C112 C113 C114 . . . 120.6(4) ? C112 C113 H113 . . . 119.9 ? C114 C113 H113 . . . 119.5 ? C113 C114 C115 . . . 119.3(4) ? C113 C114 H114 . . . 120.0 ? C115 C114 H114 . . . 120.6 ? C114 C115 C116 . . . 121.0(4) ? C114 C115 H115 . . . 119.2 ? C116 C115 H115 . . . 119.6 ? C111 C116 C115 . . . 119.7(4) ? C111 C116 H116 . . . 119.5 ? C115 C116 H116 . . . 120.8 ? P1 C121 C122 . . . 121.7(2) ? P1 C121 C126 . . . 119.7(3) ? C122 C121 C126 . . . 118.6(3) ? C121 C122 C123 . . . 120.6(3) ? C121 C122 H122 . . . 119.5 ? C123 C122 H122 . . . 119.9 ? C122 C123 C124 . . . 119.9(3) ? C122 C123 H123 . . . 120.3 ? C124 C123 H123 . . . 119.8 ? C123 C124 C125 . . . 120.2(4) ? C123 C124 H124 . . . 119.7 ? C125 C124 H124 . . . 120.2 ? C124 C125 C126 . . . 120.0(3) ? C124 C125 H125 . . . 120.3 ? C126 C125 H125 . . . 119.7 ? C121 C126 C125 . . . 120.7(3) ? C121 C126 H126 . . . 118.6 ? C125 C126 H126 . . . 120.6 ? P1 C10 C20 . . . 110.6(2) ? P1 C10 H10a . . . 109.5 ? P1 C10 H10b . . . 109.0 ? C20 C10 H10a . . . 109.8 ? C20 C10 H10b . . . 109.2 ? H10a C10 H10b . . . 108.7 ? C10 C20 P2 . . . 106.2(2) ? C10 C20 H20a . . . 110.6 ? C10 C20 H20b . . . 109.6 ? P2 C20 H20a . . . 111.3 ? P2 C20 H20b . . . 110.5 ? H20a C20 H20b . . . 108.6 ? Ru P2 C20 . . . 107.26(11) ? Ru P2 C211 . . . 120.80(11) ? Ru P2 C221 . . . 116.57(10) ? C20 P2 C211 . . . 101.12(15) ? C20 P2 C221 . . . 107.20(15) ? C211 P2 C221 . . . 102.23(16) ? P2 C211 C212 . . . 120.6(2) ? P2 C211 C216 . . . 121.0(3) ? C212 C211 C216 . . . 118.4(3) ? C211 C212 C213 . . . 121.3(3) ? C211 C212 H212 . . . 120.4 ? C213 C212 H212 . . . 118.2 ? C212 C213 C214 . . . 119.5(4) ? C212 C213 H213 . . . 120.7 ? C214 C213 H213 . . . 119.8 ? C213 C214 C215 . . . 120.3(4) ? C213 C214 H214 . . . 118.0 ? C215 C214 H214 . . . 121.7 ? C214 C215 C216 . . . 119.6(3) ? C214 C215 H215 . . . 119.4 ? C216 C215 H215 . . . 121.0 ? C211 C216 C215 . . . 120.9(4) ? C211 C216 H216 . . . 119.6 ? C215 C216 H216 . . . 119.5 ? P2 C221 C222 . . . 118.8(3) ? P2 C221 C226 . . . 121.3(3) ? C222 C221 C226 . . . 119.3(3) ? C221 C222 C223 . . . 120.6(4) ? C221 C222 H222 . . . 119.6 ? C223 C222 H222 . . . 119.8 ? C222 C223 C224 . . . 120.2(4) ? C222 C223 H223 . . . 120.2 ? C224 C223 H223 . . . 119.6 ? C223 C224 C225 . . . 119.4(4) ? C223 C224 H224 . . . 119.7 ? C225 C224 H224 . . . 120.9 ? C224 C225 C226 . . . 120.6(4) ? C224 C225 H225 . . . 119.0 ? C226 C225 H225 . . . 120.4 ? C221 C226 C225 . . . 119.9(4) ? C221 C226 H226 . . . 119.7 ? C225 C226 H226 . . . 120.4 ? Ru C1 C2 . . . 168.9(3) ? C1 C2 C21 . . . 170.2(3) ? C2 C21 C22 . . . 122.5(3) ? C2 C21 C26 . . . 122.7(3) ? C22 C21 C26 . . . 114.7(3) ? C21 C22 F22 . . . 119.9(3) ? C21 C22 C23 . . . 122.9(3) ? F22 C22 C23 . . . 117.2(3) ? C22 C23 F23 . . . 120.4(4) ? C22 C23 C24 . . . 119.8(4) ? F23 C23 C24 . . . 119.9(4) ? C23 C24 F24 . . . 120.8(4) ? C23 C24 C25 . . . 119.2(4) ? F24 C24 C25 . . . 119.9(4) ? C24 C25 F25 . . . 119.8(4) ? C24 C25 C26 . . . 120.1(4) ? F25 C25 C26 . . . 120.1(4) ? C21 C26 C25 . . . 123.2(4) ? C21 C26 F26 . . . 118.8(3) ? C25 C26 F26 . . . 117.9(4) ? Ru C101 C1011 . . . 125.7(2) ? Ru C101 C102 . . . 72.61(18) ? Ru C101 C105 . . . 70.60(18) ? C1011 C101 C102 . . . 126.2(3) ? C1011 C101 C105 . . . 125.1(3) ? C102 C101 C105 . . . 108.5(3) ? C101 C1011 H1011a . . . 109.4 ? C101 C1011 H1011b . . . 109.5 ? C101 C1011 H1011c . . . 110.9 ? H1011a C1011 H1011b . . . 108.3 ? H1011a C1011 H1011c . . . 109.5 ? H1011b C1011 H1011c . . . 109.2 ? Ru C102 C101 . . . 70.72(17) ? Ru C102 C1021 . . . 129.9(2) ? Ru C102 C103 . . . 71.69(17) ? C101 C102 C1021 . . . 126.3(3) ? C101 C102 C103 . . . 108.0(3) ? C1021 C102 C103 . . . 125.2(3) ? C102 C1021 H1021a . . . 109.0 ? C102 C1021 H1021b . . . 108.2 ? C102 C1021 H1021c . . . 109.7 ? H1021a C1021 H1021b . . . 109.2 ? H1021a C1021 H1021c . . . 110.0 ? H1021b C1021 H1021c . . . 110.7 ? Ru C103 C102 . . . 71.51(18) ? Ru C103 C1031 . . . 131.3(2) ? Ru C103 C104 . . . 71.56(17) ? C102 C103 C1031 . . . 124.4(3) ? C102 C103 C104 . . . 108.0(3) ? C1031 C103 C104 . . . 126.6(3) ? C103 C1031 H1031a . . . 110.7 ? C103 C1031 H1031b . . . 110.0 ? C103 C1031 H1031c . . . 110.6 ? H1031a C1031 H1031b . . . 108.9 ? H1031a C1031 H1031c . . . 108.6 ? H1031b C1031 H1031c . . . 107.9 ? Ru C104 C103 . . . 71.81(18) ? Ru C104 C1041 . . . 130.6(2) ? Ru C104 C105 . . . 69.77(18) ? C103 C104 C1041 . . . 127.2(3) ? C103 C104 C105 . . . 108.1(3) ? C1041 C104 C105 . . . 124.1(3) ? C104 C1041 H1041a . . . 109.4 ? C104 C1041 H1041b . . . 109.2 ? C104 C1041 H1041c . . . 110.1 ? H1041a C1041 H1041b . . . 109.1 ? H1041a C1041 H1041c . . . 110.4 ? H1041b C1041 H1041c . . . 108.6 ? Ru C105 C101 . . . 71.93(19) ? Ru C105 C104 . . . 72.90(18) ? Ru C105 C1051 . . . 124.5(2) ? C101 C105 C104 . . . 107.2(3) ? C101 C105 C1051 . . . 125.9(3) ? C104 C105 C1051 . . . 126.7(3) ? C105 C1051 H1051a . . . 107.1 ? C105 C1051 H1051b . . . 107.2 ? C105 C1051 H1051c . . . 110.1 ? H1051a C1051 H1051b . . . 109.4 ? H1051a C1051 H1051c . . . 109.9 ? H1051b C1051 H1051c . . . 112.9 ? _exptl_crystal_F_000 1688 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 34 _reflns_limit_l_min -23 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .731 _reflns_d_resolution_low 14.039 _diffrn_reflns_av_sigmaI/netI .057 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 170 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .058 _refine_ls_wR_factor_ref .111 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_shift/su_mean .0002 #===END ######################################## # # # CIF generated by the Xtal System # # # ######################################## data_br1210_compound_10 _database_code_depnum_ccdc_archive 'CCDC 660624' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C82 H78 F4 P4 Ru2' _chemical_formula_moiety 'C82 H78 F4 P4 Ru2' _chemical_formula_weight 1465.55 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.9820(10) _cell_length_b 18.486(2) _cell_length_c 17.193(2) _cell_angle_alpha 90.00000 _cell_angle_beta 93.839(2) _cell_angle_gamma 90.00000 _cell_volume 3482.6(6) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6482 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 32.5 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .581 _exptl_crystal_description bar _exptl_crystal_size_max .48 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .92 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 38966 _reflns_number_total 11272 _reflns_Friedel_coverage 0 _reflns_number_gt 8907 _reflns_threshold_expression 'I > 2.00 sig(I)' _diffrn_reflns_theta_max 31.25 _diffrn_reflns_theta_full 31.25 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .036 _refine_ls_wR_factor_gt .077 _refine_ls_goodness_of_fit_gt .96 _refine_ls_number_reflns 11272 _refine_ls_number_parameters 415 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w = 1/(\s^2^(F^2^) + 12F^2^) ; _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -.93 _refine_diff_density_max .931 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 164 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 156 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 8 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .333224(16) .596470(9) .673997(10) .01805(8) Uani ? ? 1.00000 ? ? P1 .15450(6) .64268(3) .70815(4) .0227(3) Uani ? ? 1.00000 ? ? C111 .0602(2) .69821(14) .63842(17) .0302(12) Uani ? ? 1.00000 ? ? C112 -.0456(3) .73201(18) .6607(2) .0427(16) Uani ? ? 1.00000 ? ? C113 -.1115(3) .7775(2) .6085(3) .052(2) Uani ? ? 1.00000 ? ? C114 -.0747(3) .7876(2) .5338(2) .0515(19) Uani ? ? 1.00000 ? ? C115 .0296(3) .75311(19) .5108(2) .0438(16) Uani ? ? 1.00000 ? ? C116 .0965(3) .70920(15) .56408(17) .0320(12) Uani ? ? 1.00000 ? ? C121 .0447(2) .57890(14) .74393(15) .0273(11) Uani ? ? 1.00000 ? ? C122 -.0560(3) .55514(15) .69653(18) .0340(13) Uani ? ? 1.00000 ? ? C123 -.1299(3) .50039(17) .7221(2) .0407(15) Uani ? ? 1.00000 ? ? C124 -.1089(3) .47022(16) .7946(2) .0428(16) Uani ? ? 1.00000 ? ? C125 -.0097(3) .49304(17) .8420(2) .0412(15) Uani ? ? 1.00000 ? ? C126 .0673(3) .54644(16) .81663(17) .0346(13) Uani ? ? 1.00000 ? ? C10 .1883(2) .70669(15) .78913(15) .0299(12) Uani ? ? 1.00000 ? ? C20 .2940(3) .75496(16) .7684(2) .0385(14) Uani ? ? 1.00000 ? ? P2 .40201(6) .70853(3) .70611(4) .0223(3) Uani ? ? 1.00000 ? ? C211 .4226(3) .77336(13) .62692(16) .0320(12) Uani ? ? 1.00000 ? ? C212 .3287(3) .81529(17) .5933(2) .0451(16) Uani ? ? 1.00000 ? ? C213 .3464(4) .8587(2) .5276(2) .059(2) Uani ? ? 1.00000 ? ? C214 .4583(4) .8590(2) .4949(2) .059(2) Uani ? ? 1.00000 ? ? C215 .5520(4) .81798(18) .52746(19) .0478(17) Uani ? ? 1.00000 ? ? C216 .5350(3) .77561(16) .59221(17) .0387(14) Uani ? ? 1.00000 ? ? C221 .5494(2) .71962(13) .76114(14) .0252(10) Uani ? ? 1.00000 ? ? C222 .6227(2) .66038(14) .78220(14) .0271(11) Uani ? ? 1.00000 ? ? C223 .7359(3) .66974(16) .82191(16) .0323(12) Uani ? ? 1.00000 ? ? C224 .7776(3) .73865(18) .84032(17) .0373(14) Uani ? ? 1.00000 ? ? C225 .7059(3) .79812(16) .82003(18) .0393(14) Uani ? ? 1.00000 ? ? C226 .5922(3) .78912(15) .78113(17) .0349(13) Uani ? ? 1.00000 ? ? C1 .3671(2) .57342(12) .78680(13) .0225(10) Uani ? ? 1.00000 ? ? C2 .3974(2) .55365(14) .85308(14) .0259(11) Uani ? ? 1.00000 ? ? C3 .4479(2) .52756(13) .92640(13) .0237(10) Uani ? ? 1.00000 ? ? C4 .3827(2) .52439(14) .99313(14) .0250(10) Uani ? ? 1.00000 ? ? F4 .26598(14) .54871(10) .98911(10) .0354(8) Uani ? ? 1.00000 ? ? C5 .4318(2) .49861(15) 1.06354(13) .0260(11) Uani ? ? 1.00000 ? ? F5 .36121(16) .49821(11) 1.12428(9) .0400(9) Uani ? ? 1.00000 ? ? C101 .3028(3) .48572(14) .62624(16) .0333(13) Uani ? ? 1.00000 ? ? C1011 .2204(5) .4294(2) .6559(3) .068(2) Uani ? ? 1.00000 ? ? C102 .2713(2) .53603(14) .56479(15) .0278(11) Uani ? ? 1.00000 ? ? C1021 .1511(3) .5364(2) .5172(2) .0519(19) Uani ? ? 1.00000 ? ? C103 .3774(2) .57618(12) .54928(12) .0215(9) Uani ? ? 1.00000 ? ? C1031 .3906(3) .62823(15) .48363(15) .0326(12) Uani ? ? 1.00000 ? ? C104 .4769(2) .54942(14) .60016(14) .0255(10) Uani ? ? 1.00000 ? ? C1041 .6076(3) .5716(2) .59485(18) .0393(15) Uani ? ? 1.00000 ? ? C105 .4309(3) .49351(14) .64678(15) .0326(12) Uani ? ? 1.00000 ? ? C1051 .5041(4) .4476(2) .70536(18) .061(2) Uani ? ? 1.00000 ? ? H112 -.07331 .72475 .71196 .05000 Uiso ? ? 1.00000 ? ? H113 -.18350 .80174 .62440 .06000 Uiso ? ? 1.00000 ? ? H114 -.12238 .81691 .49727 .06000 Uiso ? ? 1.00000 ? ? H115 .05642 .76084 .45901 .05200 Uiso ? ? 1.00000 ? ? H116 .16833 .68546 .54839 .04000 Uiso ? ? 1.00000 ? ? H122 -.07356 .57649 .64603 .04200 Uiso ? ? 1.00000 ? ? H123 -.19638 .48248 .68834 .04900 Uiso ? ? 1.00000 ? ? H124 -.16389 .43423 .81111 .05200 Uiso ? ? 1.00000 ? ? H125 .00462 .47204 .89329 .04900 Uiso ? ? 1.00000 ? ? H126 .13755 .56051 .84946 .04100 Uiso ? ? 1.00000 ? ? H10a .11832 .73497 .79775 .03600 Uiso ? ? 1.00000 ? ? H10b .21158 .68045 .83598 .03600 Uiso ? ? 1.00000 ? ? H20a .33747 .77148 .81484 .04700 Uiso ? ? 1.00000 ? ? H20b .26097 .79663 .74062 .04700 Uiso ? ? 1.00000 ? ? H212 .25051 .81632 .61722 .05500 Uiso ? ? 1.00000 ? ? H213 .28083 .88708 .50584 .07000 Uiso ? ? 1.00000 ? ? H214 .46915 .88815 .44945 .06700 Uiso ? ? 1.00000 ? ? H215 .62996 .81855 .50507 .06000 Uiso ? ? 1.00000 ? ? H216 .60100 .74779 .61573 .04500 Uiso ? ? 1.00000 ? ? H222 .59451 .61259 .76859 .03100 Uiso ? ? 1.00000 ? ? H223 .78568 .62923 .83618 .03800 Uiso ? ? 1.00000 ? ? H224 .85605 .74453 .86740 .04400 Uiso ? ? 1.00000 ? ? H225 .73518 .84598 .83261 .04700 Uiso ? ? 1.00000 ? ? H226 .54180 .83008 .76738 .04000 Uiso ? ? 1.00000 ? ? H1011a .21614 .38919 .62248 .10300 Uiso ? ? 1.00000 ? ? H1011b .13921 .44977 .65786 .10300 Uiso ? ? 1.00000 ? ? H1011c .24741 .41549 .70768 .10300 Uiso ? ? 1.00000 ? ? H1021a .14809 .57706 .48186 .07400 Uiso ? ? 1.00000 ? ? H1021b .08493 .54036 .54962 .07400 Uiso ? ? 1.00000 ? ? H1021c .14188 .49346 .48665 .07400 Uiso ? ? 1.00000 ? ? H1031a .31127 .64298 .46316 .04800 Uiso ? ? 1.00000 ? ? H1031b .43153 .60528 .44332 .04800 Uiso ? ? 1.00000 ? ? H1031c .43488 .66974 .50194 .04800 Uiso ? ? 1.00000 ? ? H1041a .65292 .56347 .64295 .06100 Uiso ? ? 1.00000 ? ? H1041b .61162 .62213 .58227 .06100 Uiso ? ? 1.00000 ? ? H1041c .64323 .54508 .55476 .06100 Uiso ? ? 1.00000 ? ? H1051a .57343 .47468 .72554 .08800 Uiso ? ? 1.00000 ? ? H1051b .53107 .40524 .68085 .08800 Uiso ? ? 1.00000 ? ? H1051c .45542 .43448 .74722 .08800 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru .02009(8) .01722(8) .01669(8) .00044(6) .00008(6) .00017(5) P1 .0217(3) .0229(3) .0234(3) .0017(2) .0020(2) -.0005(2) C111 .0249(12) .0276(11) .0376(13) .0031(9) -.0011(10) .0044(10) C112 .0330(15) .0391(15) .057(2) .0105(12) .0086(13) .0064(14) C113 .0322(16) .0485(19) .074(3) .0146(14) .0033(16) .0112(18) C114 .0415(18) .0438(17) .067(2) .0080(14) -.0129(16) .0200(17) C115 .0438(17) .0437(16) .0429(17) .0027(13) -.0053(13) .0139(14) C116 .0288(12) .0319(12) .0349(13) .0035(10) -.0016(10) .0058(10) C121 .0232(11) .0281(11) .0312(12) .0024(9) .0063(9) .0002(9) C122 .0278(13) .0317(13) .0423(15) -.0019(10) .0008(11) -.0034(11) C123 .0276(14) .0334(14) .061(2) -.0005(11) .0039(13) -.0040(13) C124 .0302(14) .0300(13) .071(2) -.0006(11) .0211(14) .0015(14) C125 .0433(17) .0354(14) .0469(17) .0053(12) .0178(13) .0114(13) C126 .0328(14) .0389(14) .0325(13) -.0009(11) .0058(11) .0043(11) C10 .0307(13) .0314(12) .0284(12) .0008(10) .0080(10) -.0036(10) C20 .0392(15) .0283(12) .0484(17) -.0042(11) .0061(12) -.0171(12) P2 .0250(3) .0190(2) .0224(3) -.0020(2) -.0011(2) -.0011(2) C211 .0429(15) .0206(10) .0308(12) -.0090(10) -.0089(11) .0018(9) C212 .0462(18) .0304(14) .056(2) -.0062(12) -.0162(15) .0103(13) C213 .074(3) .0446(18) .053(2) -.0077(18) -.033(2) .0144(16) C214 .086(3) .0457(19) .0420(18) -.026(2) -.0179(19) .0143(15) C215 .071(2) .0401(16) .0320(14) -.0225(16) .0001(14) .0019(12) C216 .0546(19) .0303(13) .0310(13) -.0121(12) .0002(12) .0003(11) C221 .0271(11) .0243(10) .0234(10) -.0054(8) -.0032(8) .0001(8) C222 .0293(12) .0288(11) .0228(11) -.0030(9) -.0001(9) -.0021(9) C223 .0284(12) .0365(13) .0311(12) -.0007(10) -.0046(10) -.0022(10) C224 .0363(15) .0461(16) .0284(12) -.0087(12) -.0064(11) -.0042(12) C225 .0482(17) .0332(14) .0344(14) -.0138(12) -.0111(12) -.0039(11) C226 .0446(16) .0266(12) .0319(13) -.0069(11) -.0098(11) -.0020(10) C1 .0241(10) .0222(10) .0213(10) .0012(8) .0027(8) -.0010(8) C2 .0230(11) .0289(11) .0256(11) .0014(9) .0001(8) .0017(9) C3 .0247(11) .0274(11) .0193(9) .0015(8) .0024(8) .0020(8) C4 .0210(11) .0296(11) .0243(10) .0035(8) .0020(8) .0015(9) F4 .0246(8) .0509(10) .0308(8) .0103(7) .0032(6) .0055(7) C5 .0260(11) .0348(12) .0178(10) .0013(9) .0056(8) .0038(9) F5 .0326(9) .0649(12) .0237(7) .0121(8) .0103(6) .0106(8) C101 .0507(16) .0204(10) .0306(12) -.0074(10) .0164(11) -.0053(9) C1011 .110(4) .0310(16) .069(3) -.032(2) .045(3) -.0107(16) C102 .0243(11) .0304(12) .0283(11) -.0027(9) -.0005(9) -.0116(9) C1021 .0261(14) .075(2) .054(2) -.0035(14) -.0057(13) -.0395(19) C103 .0270(11) .0216(9) .0159(9) .0013(8) .0002(8) -.0017(7) C1031 .0466(16) .0307(12) .0208(11) .0032(11) .0044(10) .0037(9) C104 .0253(11) .0292(11) .0218(10) .0064(9) -.0000(8) -.0041(9) C1041 .0225(12) .0575(19) .0381(15) .0027(12) .0033(11) -.0162(14) C105 .0487(16) .0243(11) .0250(11) .0132(11) .0040(11) .0009(9) C1051 .107(3) .051(2) .0264(14) .051(2) .0112(17) .0089(13) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru P1 . . 2.2542(7) ? Ru P2 . . 2.2607(7) ? Ru C1 . . 1.996(2) ? Ru C101 . . 2.223(3) ? Ru C102 . . 2.251(3) ? Ru C103 . . 2.261(2) ? Ru C104 . . 2.264(3) ? Ru C105 . . 2.249(3) ? P1 C111 . . 1.843(3) ? P1 C121 . . 1.823(3) ? P1 C10 . . 1.846(3) ? C111 C112 . . 1.395(4) ? C111 C116 . . 1.379(4) ? C112 C113 . . 1.396(5) ? C112 H112 . . .962 ? C113 C114 . . 1.385(6) ? C113 H113 . . .964 ? C114 C115 . . 1.391(5) ? C114 H114 . . .958 ? C115 C116 . . 1.395(4) ? C115 H115 . . .967 ? C116 H116 . . .957 ? C121 C122 . . 1.400(4) ? C121 C126 . . 1.394(4) ? C122 C123 . . 1.387(4) ? C122 H122 . . .961 ? C123 C124 . . 1.371(5) ? C123 H123 . . .960 ? C124 C125 . . 1.382(5) ? C124 H124 . . .955 ? C125 C126 . . 1.389(4) ? C125 H125 . . .967 ? C126 H126 . . .961 ? C10 C20 . . 1.525(4) ? C10 H10a . . .949 ? C10 H10b . . .960 ? C20 P2 . . 1.861(3) ? C20 H20a . . .953 ? C20 H20b . . .964 ? P2 C211 . . 1.839(3) ? P2 C221 . . 1.830(2) ? C211 C212 . . 1.386(4) ? C211 C216 . . 1.407(5) ? C212 C213 . . 1.409(5) ? C212 H212 . . .977 ? C213 C214 . . 1.386(7) ? C213 H213 . . .948 ? C214 C215 . . 1.367(6) ? C214 H214 . . .963 ? C215 C216 . . 1.384(4) ? C215 H215 . . .962 ? C216 H216 . . .956 ? C221 C222 . . 1.393(4) ? C221 C226 . . 1.403(4) ? C222 C223 . . 1.389(4) ? C222 H222 . . .960 ? C223 C224 . . 1.383(4) ? C223 H223 . . .949 ? C224 C225 . . 1.384(4) ? C224 H224 . . .957 ? C225 C226 . . 1.386(4) ? C225 H225 . . .961 ? C226 H226 . . .958 ? C1 C2 . . 1.221(3) ? C2 C3 . . 1.427(3) ? C3 C4 . . 1.394(3) ? C3 C5 . '3 667' 1.406(3) ? C4 F4 . . 1.356(3) ? C4 C5 . . 1.377(3) ? C5 F5 . . 1.342(3) ? C101 C1011 . . 1.491(5) ? C101 C102 . . 1.433(4) ? C101 C105 . . 1.434(4) ? C1011 H1011a . . .939 ? C1011 H1011b . . .971 ? C1011 H1011c . . .955 ? C102 C1021 . . 1.505(4) ? C102 C103 . . 1.422(4) ? C1021 H1021a . . .966 ? C1021 H1021b . . .948 ? C1021 H1021c . . .954 ? C103 C1031 . . 1.498(3) ? C103 C104 . . 1.441(3) ? C1031 H1031a . . .957 ? C1031 H1031b . . .951 ? C1031 H1031c . . .951 ? C104 C1041 . . 1.501(4) ? C104 C105 . . 1.421(4) ? C1041 H1041a . . .948 ? C1041 H1041b . . .961 ? C1041 H1041c . . .951 ? C105 C1051 . . 1.508(5) ? C1051 H1051a . . .957 ? C1051 H1051b . . .946 ? C1051 H1051c . . .956 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P1 Ru P2 . . . 82.62(2) ? P1 Ru C1 . . . 86.38(7) ? P1 Ru C101 . . . 109.48(8) ? P1 Ru C102 . . . 100.69(7) ? P1 Ru C103 . . . 123.76(6) ? P1 Ru C104 . . . 160.62(6) ? P1 Ru C105 . . . 144.15(8) ? P2 Ru C1 . . . 85.45(7) ? P2 Ru C101 . . . 166.83(8) ? P2 Ru C102 . . . 137.39(7) ? P2 Ru C103 . . . 107.11(6) ? P2 Ru C104 . . . 104.77(7) ? P2 Ru C105 . . . 132.07(8) ? C1 Ru C101 . . . 100.13(10) ? C1 Ru C102 . . . 136.96(10) ? C1 Ru C103 . . . 147.99(9) ? C1 Ru C104 . . . 111.78(9) ? C1 Ru C105 . . . 87.76(10) ? C101 Ru C102 . . . 37.35(10) ? C101 Ru C103 . . . 62.19(9) ? C101 Ru C104 . . . 62.11(10) ? C101 Ru C105 . . . 37.41(11) ? C102 Ru C103 . . . 36.75(9) ? C102 Ru C104 . . . 61.62(9) ? C102 Ru C105 . . . 61.85(10) ? C103 Ru C104 . . . 37.13(8) ? C103 Ru C105 . . . 61.76(9) ? C104 Ru C105 . . . 36.71(10) ? Ru P1 C111 . . . 120.17(9) ? Ru P1 C121 . . . 116.74(9) ? Ru P1 C10 . . . 107.75(9) ? C111 P1 C121 . . . 102.97(12) ? C111 P1 C10 . . . 102.09(12) ? C121 P1 C10 . . . 105.32(12) ? P1 C111 C112 . . . 120.9(2) ? P1 C111 C116 . . . 120.0(2) ? C112 C111 C116 . . . 119.0(3) ? C111 C112 C113 . . . 120.0(3) ? C111 C112 H112 . . . 120.6 ? C113 C112 H112 . . . 119.4 ? C112 C113 C114 . . . 120.4(3) ? C112 C113 H113 . . . 119.9 ? C114 C113 H113 . . . 119.8 ? C113 C114 C115 . . . 119.9(3) ? C113 C114 H114 . . . 120.2 ? C115 C114 H114 . . . 119.9 ? C114 C115 C116 . . . 119.2(3) ? C114 C115 H115 . . . 120.0 ? C116 C115 H115 . . . 120.7 ? C111 C116 C115 . . . 121.5(3) ? C111 C116 H116 . . . 119.2 ? C115 C116 H116 . . . 119.3 ? P1 C121 C122 . . . 121.4(2) ? P1 C121 C126 . . . 119.9(2) ? C122 C121 C126 . . . 118.2(3) ? C121 C122 C123 . . . 120.1(3) ? C121 C122 H122 . . . 120.0 ? C123 C122 H122 . . . 120.0 ? C122 C123 C124 . . . 121.2(3) ? C122 C123 H123 . . . 119.8 ? C124 C123 H123 . . . 118.9 ? C123 C124 C125 . . . 119.4(3) ? C123 C124 H124 . . . 118.8 ? C125 C124 H124 . . . 121.8 ? C124 C125 C126 . . . 120.3(3) ? C124 C125 H125 . . . 119.3 ? C126 C125 H125 . . . 120.5 ? C121 C126 C125 . . . 120.8(3) ? C121 C126 H126 . . . 119.9 ? C125 C126 H126 . . . 119.3 ? P1 C10 C20 . . . 108.5(2) ? P1 C10 H10a . . . 110.3 ? P1 C10 H10b . . . 109.7 ? C20 C10 H10a . . . 110.5 ? C20 C10 H10b . . . 109.1 ? H10a C10 H10b . . . 108.7 ? C10 C20 P2 . . . 112.9(2) ? C10 C20 H20a . . . 109.8 ? C10 C20 H20b . . . 108.5 ? P2 C20 H20a . . . 109.1 ? P2 C20 H20b . . . 108.4 ? H20a C20 H20b . . . 108.1 ? Ru P2 C20 . . . 110.35(10) ? Ru P2 C211 . . . 118.17(9) ? Ru P2 C221 . . . 119.89(8) ? C20 P2 C211 . . . 103.92(13) ? C20 P2 C221 . . . 103.09(13) ? C211 P2 C221 . . . 99.27(12) ? P2 C211 C212 . . . 123.2(2) ? P2 C211 C216 . . . 119.2(2) ? C212 C211 C216 . . . 117.1(3) ? C211 C212 C213 . . . 120.9(3) ? C211 C212 H212 . . . 119.1 ? C213 C212 H212 . . . 119.9 ? C212 C213 C214 . . . 120.1(4) ? C212 C213 H213 . . . 119.3 ? C214 C213 H213 . . . 120.6 ? C213 C214 C215 . . . 119.7(4) ? C213 C214 H214 . . . 119.5 ? C215 C214 H214 . . . 120.8 ? C214 C215 C216 . . . 120.3(4) ? C214 C215 H215 . . . 119.7 ? C216 C215 H215 . . . 120.0 ? C211 C216 C215 . . . 121.8(3) ? C211 C216 H216 . . . 117.8 ? C215 C216 H216 . . . 120.4 ? P2 C221 C222 . . . 121.46(19) ? P2 C221 C226 . . . 120.0(2) ? C222 C221 C226 . . . 118.5(2) ? C221 C222 C223 . . . 120.9(2) ? C221 C222 H222 . . . 119.3 ? C223 C222 H222 . . . 119.9 ? C222 C223 C224 . . . 119.9(3) ? C222 C223 H223 . . . 120.6 ? C224 C223 H223 . . . 119.4 ? C223 C224 C225 . . . 120.0(3) ? C223 C224 H224 . . . 119.3 ? C225 C224 H224 . . . 120.7 ? C224 C225 C226 . . . 120.4(3) ? C224 C225 H225 . . . 119.9 ? C226 C225 H225 . . . 119.8 ? C221 C226 C225 . . . 120.3(3) ? C221 C226 H226 . . . 119.0 ? C225 C226 H226 . . . 120.7 ? Ru C1 C2 . . . 172.6(2) ? C1 C2 C3 . . . 172.2(3) ? C2 C3 C4 . . . 123.4(2) ? C2 C3 C5 . . '3 667' 122.1(2) ? C4 C3 C5 . . '3 667' 114.5(2) ? C3 C4 F4 . . . 118.7(2) ? C3 C4 C5 . . . 123.1(2) ? F4 C4 C5 . . . 118.2(2) ? C4 C5 F5 . . . 118.3(2) ? C4 C5 C3 . . '3 667' 122.4(2) ? F5 C5 C3 . . '3 667' 119.3(2) ? Ru C101 C1011 . . . 126.6(2) ? Ru C101 C102 . . . 72.39(15) ? Ru C101 C105 . . . 72.30(15) ? C1011 C101 C102 . . . 125.7(3) ? C1011 C101 C105 . . . 126.4(3) ? C102 C101 C105 . . . 107.5(2) ? C101 C1011 H1011a . . . 110.5 ? C101 C1011 H1011b . . . 108.7 ? C101 C1011 H1011c . . . 110.5 ? H1011a C1011 H1011b . . . 108.6 ? H1011a C1011 H1011c . . . 110.9 ? H1011b C1011 H1011c . . . 107.5 ? Ru C102 C101 . . . 70.26(15) ? Ru C102 C1021 . . . 131.0(2) ? Ru C102 C103 . . . 72.03(13) ? C101 C102 C1021 . . . 124.3(3) ? C101 C102 C103 . . . 108.4(2) ? C1021 C102 C103 . . . 126.6(2) ? C102 C1021 H1021a . . . 109.7 ? C102 C1021 H1021b . . . 111.1 ? C102 C1021 H1021c . . . 110.7 ? H1021a C1021 H1021b . . . 108.3 ? H1021a C1021 H1021c . . . 107.6 ? H1021b C1021 H1021c . . . 109.3 ? Ru C103 C102 . . . 71.22(14) ? Ru C103 C1031 . . . 130.22(17) ? Ru C103 C104 . . . 71.55(13) ? C102 C103 C1031 . . . 126.7(2) ? C102 C103 C104 . . . 107.8(2) ? C1031 C103 C104 . . . 124.8(2) ? C103 C1031 H1031a . . . 109.2 ? C103 C1031 H1031b . . . 109.7 ? C103 C1031 H1031c . . . 110.0 ? H1031a C1031 H1031b . . . 108.8 ? H1031a C1031 H1031c . . . 109.0 ? H1031b C1031 H1031c . . . 110.2 ? Ru C104 C103 . . . 71.33(14) ? Ru C104 C1041 . . . 129.4(2) ? Ru C104 C105 . . . 71.07(15) ? C103 C104 C1041 . . . 124.0(2) ? C103 C104 C105 . . . 107.9(2) ? C1041 C104 C105 . . . 127.6(2) ? C104 C1041 H1041a . . . 110.6 ? C104 C1041 H1041b . . . 109.7 ? C104 C1041 H1041c . . . 110.2 ? H1041a C1041 H1041b . . . 108.7 ? H1041a C1041 H1041c . . . 109.5 ? H1041b C1041 H1041c . . . 108.1 ? Ru C105 C101 . . . 70.29(15) ? Ru C105 C104 . . . 72.22(15) ? Ru C105 C1051 . . . 125.3(2) ? C101 C105 C104 . . . 108.3(2) ? C101 C105 C1051 . . . 125.3(3) ? C104 C105 C1051 . . . 126.3(3) ? C105 C1051 H1051a . . . 108.8 ? C105 C1051 H1051b . . . 109.7 ? C105 C1051 H1051c . . . 110.2 ? H1051a C1051 H1051b . . . 109.2 ? H1051a C1051 H1051c . . . 109.3 ? H1051b C1051 H1051c . . . 109.5 ? _exptl_crystal_F_000 1508 _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min -25 _reflns_limit_l_max 25 _reflns_number_observed ? _reflns_d_resolution_high .685 _reflns_d_resolution_low 12.543 _diffrn_reflns_av_sigmaI/netI .05 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .051 _refine_ls_wR_factor_ref .101 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_shift/su_mean .0001 #===END