# 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 _publ_contact_author_name 'Paul Low' _publ_contact_author_email P.J.LOW@DURHAM.AC.UK _publ_section_title ; Convenient preparation of transition metal alkynyl complexes by transmetallation from alkynyl-gold(I) precursors, Au(C?CAr)(PPh3) (Ar = C6H5 or C6H4Me-4) ; loop_ _publ_author_name 'Paul Low' 'M Bruce' 'Mark A Fox' 'Maryka Gaudio' 'J Howard' 'Wan M Khairul' ; B.W.Skelton ; 'Allan H White' 'Dimitrii S Yufit' 'Natasha N Zaitseva' # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END #3. data data_4c _database_code_depnum_ccdc_archive 'CCDC 660622' _audit_creation_date 2006-07-19T12:48:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C37.50 H33.50 F5 O2 P Ru' _chemical_formula_moiety 'C36 H30 F5 O2 P Ru, 0.25(C6 H14)' _chemical_formula_weight 743.18 #----------------------------------------------------------------------------# # 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 13.027(4) _cell_length_b 16.959(5) _cell_length_c 17.133(6) _cell_angle_alpha 111.86(3) _cell_angle_beta 106.93(3) _cell_angle_gamma 93.67(2) _cell_volume 3296.7(21) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4577 _cell_measurement_theta_min 2.4792 _cell_measurement_theta_max 27.4397 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.015 _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1514 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.585 _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 0.67076 _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 0.0055224834 _diffrn_orient_matrix_ub_12 0.0002963138 _diffrn_orient_matrix_ub_13 -0.0398130749 _diffrn_orient_matrix_ub_21 -0.056260147 _diffrn_orient_matrix_ub_22 -0.0190578012 _diffrn_orient_matrix_ub_23 -0.023243604 _diffrn_orient_matrix_ub_31 -0.0132122071 _diffrn_orient_matrix_ub_32 0.0418446948 _diffrn_orient_matrix_ub_33 0.0111657421 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_unetI/netI 0.2371 _diffrn_reflns_number 27359 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.1 _diffrn_reflns_theta_full 25.1 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 11685 _reflns_number_gt 5419 _reflns_threshold_expression I>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^)+(0.0007P)^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 11685 _refine_ls_number_parameters 844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.158 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.468 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------# # 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' 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' Ru Ru -1.2594 0.8363 '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' 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 Ru1 Ru 0.78314(4) 0.35223(3) 0.85898(4) 0.02939(17) Uani 1 1 d . . . O11 O 0.9410(3) 0.3865(2) 0.8686(3) 0.0337(12) Uani 1 1 d . . . O12 O 0.9120(3) 0.2976(2) 0.8458(3) 0.0326(12) Uani 1 1 d . . . P1 P 0.72193(15) 0.26631(11) 0.70602(12) 0.0328(5) Uani 1 1 d . . . C111 C 0.6907(5) 0.1506(4) 0.6817(4) 0.0317(17) Uani 1 1 d . . . C112 C 0.7707(5) 0.1149(4) 0.7228(4) 0.0266(16) Uani 1 1 d . . . H112 H 0.8412 0.1493 0.7597 0.032 Uiso 1 1 calc R . . C113 C 0.7481(5) 0.0285(4) 0.7102(4) 0.0347(18) Uani 1 1 d . . . H113 H 0.8039 0.0039 0.737 0.042 Uiso 1 1 calc R . . C114 C 0.6460(6) -0.0206(4) 0.6592(4) 0.0425(19) Uani 1 1 d . . . H114 H 0.6304 -0.0789 0.652 0.051 Uiso 1 1 calc R . . C115 C 0.5667(6) 0.0141(4) 0.6189(4) 0.043(2) Uani 1 1 d . . . H115 H 0.4963 -0.0209 0.5829 0.052 Uiso 1 1 calc R . . C116 C 0.5868(5) 0.1007(4) 0.6294(4) 0.0365(18) Uani 1 1 d . . . H116 H 0.5307 0.1244 0.6014 0.044 Uiso 1 1 calc R . . C121 C 0.8210(5) 0.2729(4) 0.6531(4) 0.0311(17) Uani 1 1 d . . . C122 C 0.8538(5) 0.2014(4) 0.6029(4) 0.0359(18) Uani 1 1 d . . . H122 H 0.8247 0.1457 0.5965 0.043 Uiso 1 1 calc R . . C123 C 0.9291(6) 0.2092(4) 0.5612(4) 0.043(2) Uani 1 1 d . . . H123 H 0.9525 0.1595 0.528 0.051 Uiso 1 1 calc R . . C124 C 0.9686(5) 0.2899(5) 0.5690(4) 0.0432(19) Uani 1 1 d . . . H124 H 1.0183 0.2957 0.5396 0.052 Uiso 1 1 calc R . . C125 C 0.9375(6) 0.3613(5) 0.6183(5) 0.053(2) Uani 1 1 d . . . H125 H 0.9651 0.4168 0.6231 0.063 Uiso 1 1 calc R . . C126 C 0.8660(6) 0.3530(4) 0.6610(5) 0.049(2) Uani 1 1 d . . . H126 H 0.8468 0.4035 0.6971 0.059 Uiso 1 1 calc R . . C131 C 0.6001(6) 0.2839(4) 0.6345(5) 0.0321(18) Uani 1 1 d . . . C132 C 0.5264(5) 0.3266(4) 0.6702(5) 0.0356(19) Uani 1 1 d . . . H132 H 0.5407 0.3478 0.7328 0.043 Uiso 1 1 calc R . . C133 C 0.4326(6) 0.3388(4) 0.6163(5) 0.0408(19) Uani 1 1 d . . . H133 H 0.3833 0.3688 0.6418 0.049 Uiso 1 1 calc R . . C134 C 0.4108(6) 0.3073(4) 0.5249(5) 0.046(2) Uani 1 1 d . . . H134 H 0.3464 0.3154 0.4873 0.056 Uiso 1 1 calc R . . C135 C 0.4816(7) 0.2650(4) 0.4897(5) 0.050(2) Uani 1 1 d . . . H135 H 0.4662 0.2434 0.4269 0.06 Uiso 1 1 calc R . . C136 C 0.5764(6) 0.2523(4) 0.5426(5) 0.041(2) Uani 1 1 d . . . H136 H 0.6248 0.222 0.5161 0.05 Uiso 1 1 calc R . . C11 C 0.7460(5) 0.4489(4) 0.8229(4) 0.0285(17) Uani 1 1 d . . . C12 C 0.7219(5) 0.5055(4) 0.8005(4) 0.0325(18) Uani 1 1 d . . . C13 C 0.6984(6) 0.5778(4) 0.7793(4) 0.0354(18) Uani 1 1 d . . . C14 C 0.6121(6) 0.6184(4) 0.7934(5) 0.042(2) Uani 1 1 d . . . C15 C 0.5935(7) 0.6914(5) 0.7791(5) 0.049(2) Uani 1 1 d . . . C16 C 0.6599(7) 0.7257(5) 0.7454(5) 0.051(2) Uani 1 1 d . . . C17 C 0.7446(7) 0.6879(5) 0.7288(5) 0.056(2) Uani 1 1 d . . . C18 C 0.7623(6) 0.6164(5) 0.7460(5) 0.040(2) Uani 1 1 d . . . F14 F 0.5446(3) 0.5850(2) 0.8248(3) 0.0575(12) Uani 1 1 d . . . F15 F 0.5098(4) 0.7282(2) 0.7967(3) 0.0762(15) Uani 1 1 d . . . F16 F 0.6427(4) 0.7977(2) 0.7332(3) 0.0797(16) Uani 1 1 d . . . F17 F 0.8081(4) 0.7201(2) 0.6958(3) 0.0734(14) Uani 1 1 d . . . F18 F 0.8479(3) 0.5809(2) 0.7289(3) 0.0597(12) Uani 1 1 d . . . C100 C 0.7721(5) 0.5255(3) 1.0312(4) 0.0330(17) Uani 1 1 d . . . H10A H 0.8494 0.5508 1.0491 0.05 Uiso 1 1 calc R . . H10B H 0.7503 0.5409 1.0843 0.05 Uiso 1 1 calc R . . H10C H 0.7275 0.548 0.9904 0.05 Uiso 1 1 calc R . . C101 C 0.6546(5) 0.3735(4) 0.9215(4) 0.0287(17) Uani 1 1 d . . . C102 C 0.6681(5) 0.2861(4) 0.9034(4) 0.0295(17) Uani 1 1 d . . . C103 C 0.7774(5) 0.2893(4) 0.9537(4) 0.0288(17) Uani 1 1 d . . . C104 C 0.8292(5) 0.3771(4) 1.0038(4) 0.0291(18) Uani 1 1 d . . . C105 C 0.7552(5) 0.4289(4) 0.9849(4) 0.0306(17) Uani 1 1 d . . . C106 C 0.5485(5) 0.4038(4) 0.8987(4) 0.0398(19) Uani 1 1 d . . . H10D H 0.5257 0.4248 0.9515 0.06 Uiso 1 1 calc R . . H10E H 0.4923 0.3555 0.8501 0.06 Uiso 1 1 calc R . . H10F H 0.5581 0.4508 0.8798 0.06 Uiso 1 1 calc R . . C107 C 0.5810(4) 0.2064(3) 0.8477(4) 0.0317(17) Uani 1 1 d . . . H10G H 0.5474 0.1916 0.8861 0.048 Uiso 1 1 calc R . . H10H H 0.6134 0.1583 0.8184 0.048 Uiso 1 1 calc R . . H10I H 0.525 0.217 0.8023 0.048 Uiso 1 1 calc R . . C108 C 0.8257(5) 0.2112(3) 0.9534(4) 0.0334(18) Uani 1 1 d . . . H10J H 0.7708 0.1586 0.9122 0.05 Uiso 1 1 calc R . . H10K H 0.8483 0.2127 1.0138 0.05 Uiso 1 1 calc R . . H10L H 0.8893 0.2113 0.9339 0.05 Uiso 1 1 calc R . . C109 C 0.9446(5) 0.4079(4) 1.0658(4) 0.0408(19) Uani 1 1 d . . . H10M H 0.9572 0.4704 1.1017 0.061 Uiso 1 1 calc R . . H10N H 0.9941 0.3962 1.0311 0.061 Uiso 1 1 calc R . . H10O H 0.9586 0.3775 1.1054 0.061 Uiso 1 1 calc R . . Ru2 Ru 0.14738(4) 0.06375(3) 0.90734(4) 0.02756(16) Uani 1 1 d . . . O21 O -0.0167(3) 0.0196(2) 0.8671(3) 0.0369(12) Uani 1 1 d . . . O22 O 0.0044(3) 0.0964(2) 0.8567(3) 0.0346(12) Uani 1 1 d . . . P2 P 0.14954(14) 0.03625(10) 0.76511(12) 0.0284(5) Uani 1 1 d . . . C211 C 0.1767(5) 0.1346(4) 0.7499(4) 0.0267(16) Uani 1 1 d . . . C212 C 0.1142(5) 0.1986(4) 0.7738(4) 0.0280(17) Uani 1 1 d . . . H212 H 0.0576 0.1877 0.7952 0.034 Uiso 1 1 calc R . . C213 C 0.1322(5) 0.2764(4) 0.7673(4) 0.0331(18) Uani 1 1 d . . . H213 H 0.0897 0.3189 0.7848 0.04 Uiso 1 1 calc R . . C214 C 0.2142(5) 0.2914(4) 0.7346(4) 0.0331(18) Uani 1 1 d . . . H214 H 0.2272 0.3443 0.7286 0.04 Uiso 1 1 calc R . . C215 C 0.2760(5) 0.2303(4) 0.7109(4) 0.0358(18) Uani 1 1 d . . . H215 H 0.3331 0.2419 0.6903 0.043 Uiso 1 1 calc R . . C216 C 0.2564(5) 0.1513(4) 0.7166(4) 0.0346(18) Uani 1 1 d . . . H216 H 0.298 0.1086 0.6976 0.041 Uiso 1 1 calc R . . C221 C 0.0195(5) -0.0234(4) 0.6756(4) 0.0254(16) Uani 1 1 d . . . C222 C -0.0241(5) 0.0001(4) 0.6046(4) 0.0294(17) Uani 1 1 d . . . H222 H 0.0131 0.0491 0.6028 0.035 Uiso 1 1 calc R . . C223 C -0.1210(5) -0.0473(4) 0.5370(4) 0.0319(17) Uani 1 1 d . . . H223 H -0.1519 -0.0286 0.4909 0.038 Uiso 1 1 calc R . . C224 C -0.1731(5) -0.1209(4) 0.5354(4) 0.0377(18) Uani 1 1 d . . . H224 H -0.2377 -0.1547 0.487 0.045 Uiso 1 1 calc R . . C225 C -0.1308(5) -0.1455(4) 0.6048(4) 0.0399(19) Uani 1 1 d . . . H225 H -0.1677 -0.1956 0.6049 0.048 Uiso 1 1 calc R . . C226 C -0.0349(5) -0.0975(4) 0.6744(4) 0.0296(17) Uani 1 1 d . . . H226 H -0.0061 -0.1153 0.7215 0.036 Uiso 1 1 calc R . . C231 C 0.2478(5) -0.0249(4) 0.7329(4) 0.0289(17) Uani 1 1 d . . . C232 C 0.3589(6) 0.0054(4) 0.7802(4) 0.0386(19) Uani 1 1 d . . . H232 H 0.382 0.0619 0.8271 0.046 Uiso 1 1 calc R . . C233 C 0.4371(6) -0.0425(5) 0.7626(5) 0.048(2) Uani 1 1 d . . . H233 H 0.5122 -0.0181 0.7958 0.058 Uiso 1 1 calc R . . C234 C 0.4074(6) -0.1243(5) 0.6980(6) 0.057(2) Uani 1 1 d . . . H234 H 0.4612 -0.1575 0.6857 0.068 Uiso 1 1 calc R . . C235 C 0.2993(7) -0.1580(5) 0.6510(5) 0.065(2) Uani 1 1 d . . . H235 H 0.2771 -0.2159 0.6068 0.078 Uiso 1 1 calc R . . C236 C 0.2210(5) -0.1077(4) 0.6676(5) 0.044(2) Uani 1 1 d . . . H236 H 0.1462 -0.1318 0.6324 0.053 Uiso 1 1 calc R . . C21 C 0.1734(5) -0.0579(4) 0.8745(4) 0.0340(18) Uani 1 1 d . . . C22 C 0.1874(5) -0.1310(4) 0.8534(4) 0.0332(18) Uani 1 1 d . . . C23 C 0.2012(5) -0.2205(4) 0.8295(5) 0.0308(17) Uani 1 1 d . . . C24 C 0.2844(5) -0.2469(4) 0.8785(5) 0.0329(17) Uani 1 1 d . . . C25 C 0.2924(7) -0.3327(5) 0.8546(6) 0.044(2) Uani 1 1 d . . . C26 C 0.2208(7) -0.3956(5) 0.7789(6) 0.060(2) Uani 1 1 d . . . C27 C 0.1393(7) -0.3727(6) 0.7264(6) 0.063(2) Uani 1 1 d U . . C28 C 0.1303(6) -0.2861(5) 0.7524(6) 0.057(2) Uani 1 1 d . . . F24 F 0.3561(3) -0.1855(2) 0.9548(3) 0.0469(11) Uani 1 1 d . . . F25 F 0.3770(3) -0.3521(2) 0.9082(3) 0.0535(11) Uani 1 1 d . . . F26 F 0.2333(4) -0.4781(2) 0.7561(3) 0.0923(17) Uani 1 1 d . . . F27 F 0.0697(4) -0.4341(2) 0.6492(4) 0.130(2) Uani 1 1 d . . . F28 F 0.0468(4) -0.2688(2) 0.6959(3) 0.0801(15) Uani 1 1 d . . . C200 C 0.2389(4) 0.0203(3) 1.0863(4) 0.0343(17) Uani 1 1 d . . . H20A H 0.1667 0.0016 1.0873 0.051 Uiso 1 1 calc R . . H20B H 0.2915 0.0462 1.1475 0.051 Uiso 1 1 calc R . . H20C H 0.263 -0.0298 1.0501 0.051 Uiso 1 1 calc R . . C201 C 0.3111(5) 0.1058(4) 1.0109(4) 0.0259(17) Uani 1 1 d . . . C202 C 0.2881(5) 0.1791(4) 0.9934(4) 0.0305(18) Uani 1 1 d . . . C203 C 0.1929(5) 0.2022(4) 1.0155(4) 0.0252(16) Uani 1 1 d . . . C204 C 0.1610(5) 0.1423(4) 1.0499(4) 0.0263(17) Uani 1 1 d . . . C205 C 0.2323(5) 0.0851(3) 1.0471(4) 0.0267(17) Uani 1 1 d . . . C206 C 0.4109(5) 0.0680(3) 1.0110(4) 0.0335(17) Uani 1 1 d . . . H20D H 0.4622 0.0895 1.0724 0.05 Uiso 1 1 calc R . . H20E H 0.4456 0.0847 0.9743 0.05 Uiso 1 1 calc R . . H20F H 0.3908 0.0047 0.9863 0.05 Uiso 1 1 calc R . . C207 C 0.3552(5) 0.2311(3) 0.9652(4) 0.0322(18) Uani 1 1 d . . . H20G H 0.4023 0.1958 0.9377 0.048 Uiso 1 1 calc R . . H20H H 0.4006 0.2826 1.0177 0.048 Uiso 1 1 calc R . . H20I H 0.3067 0.2488 0.9218 0.048 Uiso 1 1 calc R . . C208 C 0.1404(5) 0.2749(3) 1.0061(4) 0.0352(18) Uani 1 1 d . . . H20J H 0.0719 0.2519 0.9551 0.053 Uiso 1 1 calc R . . H20K H 0.1897 0.3135 0.9963 0.053 Uiso 1 1 calc R . . H20L H 0.1249 0.3074 1.0608 0.053 Uiso 1 1 calc R . . C209 C 0.0635(5) 0.1438(4) 1.0788(4) 0.0347(18) Uani 1 1 d . . . H20M H 0.0657 0.1068 1.1115 0.052 Uiso 1 1 calc R . . H20N H -0.0032 0.1222 1.0262 0.052 Uiso 1 1 calc R . . H20O H 0.0638 0.2033 1.1179 0.052 Uiso 1 1 calc R . . C1 C 0.3040(10) 0.5806(7) 0.5755(7) 0.180(6) Uani 1 1 d . A 2 H1A H 0.3594 0.6306 0.6221 0.27 Uiso 1 1 calc R A 2 H1B H 0.2847 0.5418 0.6016 0.27 Uiso 1 1 calc R A 2 H1C H 0.2386 0.6005 0.5499 0.27 Uiso 1 1 calc R A 2 C2 C 0.3491(7) 0.5325(6) 0.5026(7) 0.119(4) Uani 1 1 d . A 2 H2A H 0.3394 0.5618 0.4613 0.142 Uiso 1 1 calc R A 2 H2B H 0.3046 0.4732 0.468 0.142 Uiso 1 1 calc R A 2 C3 C 0.4697(8) 0.5253(6) 0.5337(6) 0.117(4) Uiso 1 1 d . . 2 H3A H 0.4779 0.4987 0.5772 0.141 Uiso 1 1 calc R . 2 H3B H 0.5123 0.5853 0.5677 0.141 Uiso 1 1 calc R . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0258(4) 0.0245(3) 0.0353(4) 0.0113(3) 0.0090(3) -0.0003(3) O11 0.022(3) 0.030(3) 0.054(3) 0.022(2) 0.015(2) 0.000(2) O12 0.033(3) 0.021(2) 0.044(3) 0.012(2) 0.015(2) 0.002(2) P1 0.0367(12) 0.0266(10) 0.0319(12) 0.0111(9) 0.0097(10) -0.0011(9) C111 0.036(5) 0.027(4) 0.030(4) 0.008(4) 0.013(4) 0.000(4) C112 0.029(4) 0.018(4) 0.029(4) 0.004(3) 0.012(4) -0.001(3) C113 0.045(5) 0.029(4) 0.036(5) 0.018(4) 0.016(4) 0.010(4) C114 0.051(5) 0.033(4) 0.036(5) 0.014(4) 0.007(4) -0.004(4) C115 0.047(5) 0.030(4) 0.037(5) 0.009(4) 0.000(4) -0.009(4) C116 0.029(4) 0.035(4) 0.038(5) 0.015(4) 0.004(4) -0.003(4) C121 0.043(5) 0.025(4) 0.027(4) 0.008(4) 0.019(4) 0.007(4) C122 0.038(5) 0.048(5) 0.023(4) 0.016(4) 0.011(4) 0.006(4) C123 0.061(5) 0.042(5) 0.038(5) 0.023(4) 0.024(4) 0.026(4) C124 0.028(4) 0.065(5) 0.037(5) 0.019(5) 0.015(4) 0.001(4) C125 0.070(6) 0.037(5) 0.057(6) 0.014(4) 0.040(5) 0.001(4) C126 0.065(6) 0.028(4) 0.063(6) 0.010(4) 0.045(5) 0.012(4) C131 0.048(5) 0.017(4) 0.029(5) 0.010(4) 0.012(4) -0.007(4) C132 0.027(5) 0.036(4) 0.039(5) 0.020(4) 0.000(4) -0.008(4) C133 0.036(5) 0.046(5) 0.051(6) 0.034(5) 0.014(4) 0.004(4) C134 0.033(5) 0.046(5) 0.060(6) 0.032(5) 0.002(5) 0.001(4) C135 0.065(6) 0.037(5) 0.041(5) 0.020(4) 0.004(5) -0.002(5) C136 0.041(5) 0.032(4) 0.059(6) 0.024(5) 0.019(5) 0.011(4) C11 0.015(4) 0.027(4) 0.038(5) 0.008(4) 0.009(3) 0.001(3) C12 0.032(4) 0.025(4) 0.047(5) 0.020(4) 0.015(4) 0.008(3) C13 0.043(5) 0.031(4) 0.028(5) 0.006(4) 0.015(4) 0.002(4) C14 0.051(6) 0.022(4) 0.040(5) 0.006(4) 0.006(4) 0.007(4) C15 0.055(6) 0.036(5) 0.042(5) 0.010(4) 0.001(5) 0.032(5) C16 0.066(7) 0.035(5) 0.038(5) 0.021(4) -0.004(5) 0.001(5) C17 0.055(6) 0.050(6) 0.054(6) 0.029(5) -0.002(5) -0.007(5) C18 0.043(5) 0.039(5) 0.039(5) 0.017(4) 0.011(4) 0.020(4) F14 0.055(3) 0.050(3) 0.070(3) 0.023(2) 0.024(3) 0.019(2) F15 0.085(4) 0.060(3) 0.073(4) 0.021(3) 0.014(3) 0.040(3) F16 0.116(4) 0.035(3) 0.062(3) 0.024(2) -0.011(3) 0.012(3) F17 0.092(4) 0.059(3) 0.071(3) 0.045(3) 0.013(3) -0.013(3) F18 0.061(3) 0.055(3) 0.079(3) 0.041(3) 0.030(3) 0.008(2) C100 0.031(4) 0.026(4) 0.033(4) 0.005(4) 0.008(4) 0.001(3) C101 0.023(4) 0.031(4) 0.028(4) 0.007(4) 0.010(4) 0.006(4) C102 0.023(4) 0.022(4) 0.046(5) 0.019(4) 0.011(4) -0.007(3) C103 0.029(4) 0.037(4) 0.026(4) 0.020(4) 0.007(4) 0.007(4) C104 0.037(5) 0.013(4) 0.038(5) 0.011(4) 0.014(4) 0.001(4) C105 0.029(4) 0.021(4) 0.039(5) 0.011(4) 0.012(4) -0.003(4) C106 0.041(5) 0.037(4) 0.042(5) 0.013(4) 0.019(4) 0.013(4) C107 0.019(4) 0.032(4) 0.049(5) 0.016(4) 0.018(4) 0.003(3) C108 0.027(4) 0.035(4) 0.035(5) 0.011(4) 0.013(4) -0.006(3) C109 0.032(4) 0.044(4) 0.048(5) 0.024(4) 0.011(4) 0.006(4) Ru2 0.0232(4) 0.0251(3) 0.0333(4) 0.0119(3) 0.0092(3) 0.0001(3) O21 0.023(3) 0.033(3) 0.053(3) 0.021(3) 0.007(2) -0.009(2) O22 0.027(3) 0.027(3) 0.055(3) 0.021(2) 0.017(2) 0.005(2) P2 0.0248(11) 0.0241(10) 0.0346(12) 0.0118(9) 0.0091(10) -0.0007(9) C211 0.025(4) 0.025(4) 0.022(4) 0.004(3) 0.004(3) -0.002(3) C212 0.025(4) 0.023(4) 0.039(5) 0.014(4) 0.015(4) 0.001(3) C213 0.028(4) 0.030(4) 0.028(4) 0.001(4) 0.004(4) 0.005(4) C214 0.035(4) 0.029(4) 0.028(4) 0.011(4) 0.003(4) -0.008(4) C215 0.029(4) 0.040(5) 0.035(5) 0.010(4) 0.015(4) -0.001(4) C216 0.033(4) 0.037(4) 0.035(5) 0.019(4) 0.009(4) 0.004(4) C221 0.027(4) 0.024(4) 0.029(4) 0.012(3) 0.013(4) 0.008(3) C222 0.031(4) 0.034(4) 0.023(4) 0.010(4) 0.012(4) 0.003(4) C223 0.028(4) 0.035(4) 0.028(4) 0.010(4) 0.008(4) -0.001(4) C224 0.036(4) 0.037(4) 0.027(5) 0.006(4) 0.004(4) -0.008(4) C225 0.042(5) 0.030(4) 0.034(5) 0.006(4) 0.008(4) -0.017(4) C226 0.028(4) 0.028(4) 0.034(4) 0.016(4) 0.009(4) 0.002(3) C231 0.030(5) 0.022(4) 0.033(5) 0.008(4) 0.014(4) -0.004(4) C232 0.051(5) 0.037(4) 0.036(5) 0.007(4) 0.036(5) 0.014(4) C233 0.044(5) 0.062(6) 0.053(6) 0.028(5) 0.029(5) 0.013(5) C234 0.033(5) 0.069(6) 0.095(8) 0.045(6) 0.040(6) 0.032(5) C235 0.082(7) 0.045(5) 0.079(7) 0.014(5) 0.058(6) 0.019(5) C236 0.025(4) 0.055(5) 0.056(6) 0.016(5) 0.027(4) 0.016(4) C21 0.020(4) 0.038(4) 0.031(5) 0.004(4) 0.005(3) -0.003(4) C22 0.040(5) 0.032(4) 0.033(5) 0.012(4) 0.024(4) 0.008(4) C23 0.022(4) 0.030(4) 0.034(5) 0.008(4) 0.012(4) -0.003(4) C24 0.027(4) 0.033(5) 0.036(5) 0.009(4) 0.016(4) -0.001(4) C25 0.061(6) 0.034(5) 0.063(6) 0.033(5) 0.035(5) 0.026(5) C26 0.078(7) 0.018(5) 0.067(7) 0.009(5) 0.013(5) 0.009(5) C27 0.063(3) 0.062(3) 0.064(3) 0.0256(14) 0.0200(12) 0.0124(11) C28 0.049(6) 0.040(5) 0.072(7) 0.025(5) 0.001(5) 0.016(5) F24 0.045(3) 0.040(2) 0.047(3) 0.017(2) 0.005(2) 0.004(2) F25 0.063(3) 0.046(3) 0.075(3) 0.035(2) 0.041(3) 0.020(2) F26 0.108(4) 0.026(3) 0.127(5) 0.025(3) 0.024(3) 0.021(3) F27 0.127(5) 0.033(3) 0.135(5) 0.002(3) -0.040(4) -0.004(3) F28 0.074(3) 0.040(3) 0.084(4) 0.010(3) -0.011(3) -0.001(2) C200 0.023(4) 0.034(4) 0.048(5) 0.019(4) 0.012(4) 0.010(3) C201 0.025(4) 0.018(4) 0.039(5) 0.011(4) 0.017(4) 0.009(3) C202 0.035(5) 0.018(4) 0.029(4) 0.004(3) 0.007(4) -0.008(3) C203 0.016(4) 0.026(4) 0.027(4) 0.007(3) 0.003(3) -0.002(3) C204 0.030(4) 0.021(4) 0.021(4) 0.001(3) 0.010(3) -0.001(3) C205 0.033(4) 0.008(3) 0.039(5) 0.006(3) 0.015(4) 0.008(3) C206 0.035(4) 0.031(4) 0.029(4) 0.008(3) 0.010(4) 0.000(4) C207 0.037(4) 0.026(4) 0.037(5) 0.015(4) 0.016(4) -0.004(3) C208 0.037(4) 0.025(4) 0.036(5) 0.009(4) 0.007(4) -0.003(3) C209 0.034(4) 0.033(4) 0.043(5) 0.020(4) 0.015(4) 0.007(4) C1 0.242(16) 0.192(12) 0.130(11) 0.035(10) 0.121(12) 0.122(12) C2 0.087(8) 0.104(8) 0.135(11) 0.043(8) 0.005(8) 0.013(7) #----------------------------------------------------------------------------# # 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 Ru1 C11 1.997(6) . ? Ru1 O12 1.998(4) . ? Ru1 O11 2.042(4) . ? Ru1 C105 2.214(6) . ? Ru1 C101 2.217(6) . ? Ru1 C104 2.239(6) . ? Ru1 C103 2.266(6) . ? Ru1 C102 2.273(6) . ? Ru1 P1 2.328(2) . ? O11 O12 1.404(4) . ? P1 C121 1.800(6) . ? P1 C131 1.819(7) . ? P1 C111 1.839(6) . ? C111 C112 1.386(7) . ? C111 C116 1.390(7) . ? C112 C113 1.397(7) . ? C112 H112 0.95 . ? C113 C114 1.365(8) . ? C113 H113 0.95 . ? C114 C115 1.362(8) . ? C114 H114 0.95 . ? C115 C116 1.409(7) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.376(7) . ? C121 C126 1.386(7) . ? C122 C123 1.397(8) . ? C122 H122 0.95 . ? C123 C124 1.374(8) . ? C123 H123 0.95 . ? C124 C125 1.359(8) . ? C124 H124 0.95 . ? C125 C126 1.371(8) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.385(8) . ? C131 C136 1.389(8) . ? C132 C133 1.381(8) . ? C132 H132 0.95 . ? C133 C134 1.385(9) . ? C133 H133 0.95 . ? C134 C135 1.348(9) . ? C134 H134 0.95 . ? C135 C136 1.386(8) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C11 C12 1.187(7) . ? C12 C13 1.429(8) . ? C13 C14 1.390(9) . ? C13 C18 1.390(9) . ? C14 F14 1.348(7) . ? C14 C15 1.372(8) . ? C15 F15 1.344(8) . ? C15 C16 1.378(10) . ? C16 F16 1.334(7) . ? C16 C17 1.360(10) . ? C17 F17 1.321(8) . ? C17 C18 1.369(9) . ? C18 F18 1.355(7) . ? C100 C105 1.499(7) . ? C100 H10A 0.98 . ? C100 H10B 0.98 . ? C100 H10C 0.98 . ? C101 C105 1.426(8) . ? C101 C102 1.431(7) . ? C101 C106 1.501(7) . ? C102 C103 1.420(7) . ? C102 C107 1.497(7) . ? C103 C104 1.412(7) . ? C103 C108 1.500(7) . ? C104 C105 1.394(7) . ? C104 C109 1.490(8) . ? C106 H10D 0.98 . ? C106 H10E 0.98 . ? C106 H10F 0.98 . ? C107 H10G 0.98 . ? C107 H10H 0.98 . ? C107 H10I 0.98 . ? C108 H10J 0.98 . ? C108 H10K 0.98 . ? C108 H10L 0.98 . ? C109 H10M 0.98 . ? C109 H10N 0.98 . ? C109 H10O 0.98 . ? Ru2 C21 2.006(7) . ? Ru2 O22 2.019(4) . ? Ru2 O21 2.039(4) . ? Ru2 C205 2.202(6) . ? Ru2 C201 2.205(6) . ? Ru2 C204 2.251(6) . ? Ru2 C202 2.276(6) . ? Ru2 C203 2.289(6) . ? Ru2 P2 2.313(2) . ? O21 O22 1.400(5) . ? P2 C231 1.781(6) . ? P2 C211 1.810(6) . ? P2 C221 1.832(6) . ? C211 C216 1.382(7) . ? C211 C212 1.409(7) . ? C212 C213 1.376(7) . ? C212 H212 0.95 . ? C213 C214 1.393(8) . ? C213 H213 0.95 . ? C214 C215 1.367(8) . ? C214 H214 0.95 . ? C215 C216 1.392(7) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.393(7) . ? C221 C222 1.395(7) . ? C222 C223 1.381(7) . ? C222 H222 0.95 . ? C223 C224 1.369(7) . ? C223 H223 0.95 . ? C224 C225 1.382(7) . ? C224 H224 0.95 . ? C225 C226 1.387(7) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 C236 1.373(8) . ? C231 C232 1.388(8) . ? C232 C233 1.375(8) . ? C232 H232 0.95 . ? C233 C234 1.356(9) . ? C233 H233 0.95 . ? C234 C235 1.361(9) . ? C234 H234 0.95 . ? C235 C236 1.396(8) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C21 C22 1.198(7) . ? C22 C23 1.455(8) . ? C23 C24 1.375(8) . ? C23 C28 1.379(9) . ? C24 F24 1.347(7) . ? C24 C25 1.377(8) . ? C25 C26 1.352(9) . ? C25 F25 1.360(7) . ? C26 F26 1.341(7) . ? C26 C27 1.358(9) . ? C27 F27 1.345(8) . ? C27 C28 1.390(9) . ? C28 F28 1.359(7) . ? C200 C205 1.481(7) . ? C200 H20A 0.98 . ? C200 H20B 0.98 . ? C200 H20C 0.98 . ? C201 C202 1.414(7) . ? C201 C205 1.432(8) . ? C201 C206 1.487(7) . ? C202 C203 1.436(8) . ? C202 C207 1.495(7) . ? C203 C204 1.444(7) . ? C203 C208 1.486(7) . ? C204 C205 1.382(7) . ? C204 C209 1.491(8) . ? C206 H20D 0.98 . ? C206 H20E 0.98 . ? C206 H20F 0.98 . ? C207 H20G 0.98 . ? C207 H20H 0.98 . ? C207 H20I 0.98 . ? C208 H20J 0.98 . ? C208 H20K 0.98 . ? C208 H20L 0.98 . ? C209 H20M 0.98 . ? C209 H20N 0.98 . ? C209 H20O 0.98 . ? C1 C2 1.517(11) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.533(11) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C3 1.603(16) 2_666 ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? 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 C11 Ru1 O12 123.5(2) . . ? C11 Ru1 O11 88.8(2) . . ? O12 Ru1 O11 40.66(13) . . ? C11 Ru1 C105 86.4(2) . . ? O12 Ru1 C105 127.4(2) . . ? O11 Ru1 C105 110.9(2) . . ? C11 Ru1 C101 87.3(2) . . ? O12 Ru1 C101 148.1(2) . . ? O11 Ru1 C101 148.4(2) . . ? C105 Ru1 C101 37.5(2) . . ? C11 Ru1 C104 118.6(2) . . ? O12 Ru1 C104 93.0(2) . . ? O11 Ru1 C104 93.4(2) . . ? C105 Ru1 C104 36.48(19) . . ? C101 Ru1 C104 61.7(2) . . ? C11 Ru1 C103 146.3(2) . . ? O12 Ru1 C103 86.45(19) . . ? O11 Ru1 C103 110.46(19) . . ? C105 Ru1 C103 61.3(2) . . ? C101 Ru1 C103 61.6(2) . . ? C104 Ru1 C103 36.52(19) . . ? C11 Ru1 C102 121.1(2) . . ? O12 Ru1 C102 115.00(19) . . ? O11 Ru1 C102 146.79(19) . . ? C105 Ru1 C102 61.7(2) . . ? C101 Ru1 C102 37.13(19) . . ? C104 Ru1 C102 61.0(2) . . ? C103 Ru1 C102 36.45(19) . . ? C11 Ru1 P1 84.98(18) . . ? O12 Ru1 P1 78.65(13) . . ? O11 Ru1 P1 95.22(13) . . ? C105 Ru1 P1 152.26(18) . . ? C101 Ru1 P1 115.61(17) . . ? C104 Ru1 P1 155.05(16) . . ? C103 Ru1 P1 118.81(17) . . ? C102 Ru1 P1 101.03(17) . . ? O12 O11 Ru1 68.0(2) . . ? O11 O12 Ru1 71.4(2) . . ? C121 P1 C131 102.8(3) . . ? C121 P1 C111 103.9(3) . . ? C131 P1 C111 104.0(3) . . ? C121 P1 Ru1 114.0(2) . . ? C131 P1 Ru1 118.8(2) . . ? C111 P1 Ru1 111.8(2) . . ? C112 C111 C116 119.8(5) . . ? C112 C111 P1 118.5(5) . . ? C116 C111 P1 121.5(5) . . ? C111 C112 C113 120.2(6) . . ? C111 C112 H112 119.9 . . ? C113 C112 H112 119.9 . . ? C114 C113 C112 120.2(6) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C115 C114 C113 120.0(6) . . ? C115 C114 H114 120 . . ? C113 C114 H114 120 . . ? C114 C115 C116 121.5(6) . . ? C114 C115 H115 119.3 . . ? C116 C115 H115 119.3 . . ? C111 C116 C115 118.4(6) . . ? C111 C116 H116 120.8 . . ? C115 C116 H116 120.8 . . ? C122 C121 C126 117.4(6) . . ? C122 C121 P1 123.2(5) . . ? C126 C121 P1 119.4(5) . . ? C121 C122 C123 121.4(6) . . ? C121 C122 H122 119.3 . . ? C123 C122 H122 119.3 . . ? C124 C123 C122 118.8(6) . . ? C124 C123 H123 120.6 . . ? C122 C123 H123 120.6 . . ? C125 C124 C123 120.9(6) . . ? C125 C124 H124 119.6 . . ? C123 C124 H124 119.6 . . ? C124 C125 C126 119.6(7) . . ? C124 C125 H125 120.2 . . ? C126 C125 H125 120.2 . . ? C125 C126 C121 121.9(6) . . ? C125 C126 H126 119.1 . . ? C121 C126 H126 119.1 . . ? C132 C131 C136 118.2(7) . . ? C132 C131 P1 120.7(5) . . ? C136 C131 P1 121.0(6) . . ? C133 C132 C131 121.2(7) . . ? C133 C132 H132 119.4 . . ? C131 C132 H132 119.4 . . ? C132 C133 C134 119.8(7) . . ? C132 C133 H133 120.1 . . ? C134 C133 H133 120.1 . . ? C135 C134 C133 119.4(7) . . ? C135 C134 H134 120.3 . . ? C133 C134 H134 120.3 . . ? C134 C135 C136 121.8(7) . . ? C134 C135 H135 119.1 . . ? C136 C135 H135 119.1 . . ? C135 C136 C131 119.7(7) . . ? C135 C136 H136 120.2 . . ? C131 C136 H136 120.2 . . ? C12 C11 Ru1 178.7(6) . . ? C11 C12 C13 176.0(7) . . ? C14 C13 C18 113.6(7) . . ? C14 C13 C12 123.2(6) . . ? C18 C13 C12 123.2(7) . . ? F14 C14 C15 118.5(8) . . ? F14 C14 C13 118.0(6) . . ? C15 C14 C13 123.5(8) . . ? F15 C15 C14 119.9(8) . . ? F15 C15 C16 120.5(7) . . ? C14 C15 C16 119.6(8) . . ? F16 C16 C17 121.2(8) . . ? F16 C16 C15 119.3(8) . . ? C17 C16 C15 119.4(7) . . ? F17 C17 C16 119.7(8) . . ? F17 C17 C18 120.9(9) . . ? C16 C17 C18 119.3(8) . . ? F18 C18 C17 117.4(8) . . ? F18 C18 C13 118.1(7) . . ? C17 C18 C13 124.5(8) . . ? C105 C100 H10A 109.5 . . ? C105 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C105 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C105 C101 C102 107.5(5) . . ? C105 C101 C106 124.1(6) . . ? C102 C101 C106 126.6(6) . . ? C105 C101 Ru1 71.1(4) . . ? C102 C101 Ru1 73.6(3) . . ? C106 C101 Ru1 132.8(4) . . ? C103 C102 C101 107.4(5) . . ? C103 C102 C107 126.0(5) . . ? C101 C102 C107 126.4(6) . . ? C103 C102 Ru1 71.5(3) . . ? C101 C102 Ru1 69.3(3) . . ? C107 C102 Ru1 128.1(4) . . ? C104 C103 C102 108.0(5) . . ? C104 C103 C108 127.4(6) . . ? C102 C103 C108 124.6(6) . . ? C104 C103 Ru1 70.7(3) . . ? C102 C103 Ru1 72.1(3) . . ? C108 C103 Ru1 123.9(4) . . ? C105 C104 C103 108.9(6) . . ? C105 C104 C109 126.4(6) . . ? C103 C104 C109 124.7(6) . . ? C105 C104 Ru1 70.8(4) . . ? C103 C104 Ru1 72.8(4) . . ? C109 C104 Ru1 122.2(4) . . ? C104 C105 C101 108.2(5) . . ? C104 C105 C100 126.4(6) . . ? C101 C105 C100 125.0(6) . . ? C104 C105 Ru1 72.7(4) . . ? C101 C105 Ru1 71.3(4) . . ? C100 C105 Ru1 127.7(4) . . ? C101 C106 H10D 109.5 . . ? C101 C106 H10E 109.5 . . ? H10D C106 H10E 109.5 . . ? C101 C106 H10F 109.5 . . ? H10D C106 H10F 109.5 . . ? H10E C106 H10F 109.5 . . ? C102 C107 H10G 109.5 . . ? C102 C107 H10H 109.5 . . ? H10G C107 H10H 109.5 . . ? C102 C107 H10I 109.5 . . ? H10G C107 H10I 109.5 . . ? H10H C107 H10I 109.5 . . ? C103 C108 H10J 109.5 . . ? C103 C108 H10K 109.5 . . ? H10J C108 H10K 109.5 . . ? C103 C108 H10L 109.5 . . ? H10J C108 H10L 109.5 . . ? H10K C108 H10L 109.5 . . ? C104 C109 H10M 109.5 . . ? C104 C109 H10N 109.5 . . ? H10M C109 H10N 109.5 . . ? C104 C109 H10O 109.5 . . ? H10M C109 H10O 109.5 . . ? H10N C109 H10O 109.5 . . ? C21 Ru2 O22 124.8(2) . . ? C21 Ru2 O21 90.4(2) . . ? O22 Ru2 O21 40.36(13) . . ? C21 Ru2 C205 86.4(2) . . ? O22 Ru2 C205 127.9(2) . . ? O21 Ru2 C205 112.4(2) . . ? C21 Ru2 C201 87.3(2) . . ? O22 Ru2 C201 147.13(19) . . ? O21 Ru2 C201 150.3(2) . . ? C205 Ru2 C201 37.9(2) . . ? C21 Ru2 C204 118.0(2) . . ? O22 Ru2 C204 93.3(2) . . ? O21 Ru2 C204 93.7(2) . . ? C205 Ru2 C204 36.15(19) . . ? C201 Ru2 C204 61.9(2) . . ? C21 Ru2 C202 121.0(2) . . ? O22 Ru2 C202 113.7(2) . . ? O21 Ru2 C202 146.0(2) . . ? C205 Ru2 C202 61.6(2) . . ? C201 Ru2 C202 36.74(19) . . ? C204 Ru2 C202 61.3(2) . . ? C21 Ru2 C203 146.5(2) . . ? O22 Ru2 C203 85.29(19) . . ? O21 Ru2 C203 109.54(19) . . ? C205 Ru2 C203 61.4(2) . . ? C201 Ru2 C203 61.9(2) . . ? C204 Ru2 C203 37.07(19) . . ? C202 Ru2 C203 36.66(19) . . ? C21 Ru2 P2 82.19(19) . . ? O22 Ru2 P2 80.35(13) . . ? O21 Ru2 P2 94.90(13) . . ? C205 Ru2 P2 150.45(18) . . ? C201 Ru2 P2 114.05(17) . . ? C204 Ru2 P2 157.96(16) . . ? C202 Ru2 P2 101.85(17) . . ? C203 Ru2 P2 120.96(16) . . ? O22 O21 Ru2 69.0(2) . . ? O21 O22 Ru2 70.6(2) . . ? C231 P2 C211 105.3(3) . . ? C231 P2 C221 104.2(3) . . ? C211 P2 C221 103.9(3) . . ? C231 P2 Ru2 115.6(2) . . ? C211 P2 Ru2 112.4(2) . . ? C221 P2 Ru2 114.2(2) . . ? C216 C211 C212 117.5(6) . . ? C216 C211 P2 123.8(5) . . ? C212 C211 P2 118.8(5) . . ? C213 C212 C211 122.5(6) . . ? C213 C212 H212 118.8 . . ? C211 C212 H212 118.8 . . ? C212 C213 C214 118.4(6) . . ? C212 C213 H213 120.8 . . ? C214 C213 H213 120.8 . . ? C215 C214 C213 120.3(6) . . ? C215 C214 H214 119.8 . . ? C213 C214 H214 119.8 . . ? C214 C215 C216 120.8(6) . . ? C214 C215 H215 119.6 . . ? C216 C215 H215 119.6 . . ? C211 C216 C215 120.4(6) . . ? C211 C216 H216 119.8 . . ? C215 C216 H216 119.8 . . ? C226 C221 C222 118.3(6) . . ? C226 C221 P2 119.8(5) . . ? C222 C221 P2 121.8(5) . . ? C223 C222 C221 120.6(6) . . ? C223 C222 H222 119.7 . . ? C221 C222 H222 119.7 . . ? C224 C223 C222 120.8(6) . . ? C224 C223 H223 119.6 . . ? C222 C223 H223 119.6 . . ? C223 C224 C225 119.4(6) . . ? C223 C224 H224 120.3 . . ? C225 C224 H224 120.3 . . ? C224 C225 C226 120.5(6) . . ? C224 C225 H225 119.8 . . ? C226 C225 H225 119.8 . . ? C225 C226 C221 120.4(6) . . ? C225 C226 H226 119.8 . . ? C221 C226 H226 119.8 . . ? C236 C231 C232 114.8(6) . . ? C236 C231 P2 123.8(5) . . ? C232 C231 P2 121.0(5) . . ? C233 C232 C231 123.1(6) . . ? C233 C232 H232 118.4 . . ? C231 C232 H232 118.4 . . ? C234 C233 C232 120.3(7) . . ? C234 C233 H233 119.9 . . ? C232 C233 H233 119.9 . . ? C233 C234 C235 119.0(7) . . ? C233 C234 H234 120.5 . . ? C235 C234 H234 120.5 . . ? C234 C235 C236 120.1(7) . . ? C234 C235 H235 120 . . ? C236 C235 H235 120 . . ? C231 C236 C235 122.6(7) . . ? C231 C236 H236 118.7 . . ? C235 C236 H236 118.7 . . ? C22 C21 Ru2 178.8(6) . . ? C21 C22 C23 177.6(7) . . ? C24 C23 C28 114.6(6) . . ? C24 C23 C22 124.5(6) . . ? C28 C23 C22 120.9(6) . . ? F24 C24 C23 117.3(6) . . ? F24 C24 C25 120.2(7) . . ? C23 C24 C25 122.4(7) . . ? C26 C25 F25 120.7(6) . . ? C26 C25 C24 121.4(7) . . ? F25 C25 C24 117.8(7) . . ? F26 C26 C25 119.8(7) . . ? F26 C26 C27 121.6(8) . . ? C25 C26 C27 118.6(7) . . ? F27 C27 C26 119.4(8) . . ? F27 C27 C28 121.1(8) . . ? C26 C27 C28 119.5(8) . . ? F28 C28 C23 120.9(6) . . ? F28 C28 C27 115.7(7) . . ? C23 C28 C27 123.4(7) . . ? C205 C200 H20A 109.5 . . ? C205 C200 H20B 109.5 . . ? H20A C200 H20B 109.5 . . ? C205 C200 H20C 109.5 . . ? H20A C200 H20C 109.5 . . ? H20B C200 H20C 109.5 . . ? C202 C201 C205 107.3(6) . . ? C202 C201 C206 126.9(6) . . ? C205 C201 C206 124.5(6) . . ? C202 C201 Ru2 74.4(4) . . ? C205 C201 Ru2 70.9(4) . . ? C206 C201 Ru2 129.8(4) . . ? C201 C202 C203 108.4(5) . . ? C201 C202 C207 127.3(6) . . ? C203 C202 C207 124.0(5) . . ? C201 C202 Ru2 68.9(3) . . ? C203 C202 Ru2 72.2(3) . . ? C207 C202 Ru2 129.2(4) . . ? C202 C203 C204 106.5(5) . . ? C202 C203 C208 125.9(5) . . ? C204 C203 C208 127.6(6) . . ? C202 C203 Ru2 71.2(3) . . ? C204 C203 Ru2 70.0(3) . . ? C208 C203 Ru2 124.7(4) . . ? C205 C204 C203 108.6(6) . . ? C205 C204 C209 128.4(6) . . ? C203 C204 C209 123.0(6) . . ? C205 C204 Ru2 70.0(4) . . ? C203 C204 Ru2 72.9(3) . . ? C209 C204 Ru2 121.1(4) . . ? C204 C205 C201 109.1(6) . . ? C204 C205 C200 126.9(6) . . ? C201 C205 C200 123.5(6) . . ? C204 C205 Ru2 73.8(4) . . ? C201 C205 Ru2 71.1(4) . . ? C200 C205 Ru2 127.7(4) . . ? C201 C206 H20D 109.5 . . ? C201 C206 H20E 109.5 . . ? H20D C206 H20E 109.5 . . ? C201 C206 H20F 109.5 . . ? H20D C206 H20F 109.5 . . ? H20E C206 H20F 109.5 . . ? C202 C207 H20G 109.5 . . ? C202 C207 H20H 109.5 . . ? H20G C207 H20H 109.5 . . ? C202 C207 H20I 109.5 . . ? H20G C207 H20I 109.5 . . ? H20H C207 H20I 109.5 . . ? C203 C208 H20J 109.5 . . ? C203 C208 H20K 109.5 . . ? H20J C208 H20K 109.5 . . ? C203 C208 H20L 109.5 . . ? H20J C208 H20L 109.5 . . ? H20K C208 H20L 109.5 . . ? C204 C209 H20M 109.5 . . ? C204 C209 H20N 109.5 . . ? H20M C209 H20N 109.5 . . ? C204 C209 H20O 109.5 . . ? H20M C209 H20O 109.5 . . ? H20N C209 H20O 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 116.3(9) . . ? C1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? C1 C2 H2B 108.2 . . ? C3 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? C2 C3 C3 123.2(11) . 2_666 ? C2 C3 H3A 106.5 . . ? C3 C3 H3A 106.5 2_666 . ? C2 C3 H3B 106.5 . . ? C3 C3 H3B 106.5 2_666 . ? H3A C3 H3B 106.5 . . ? # Attachment 'Dalton.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 691297' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H36 Fe P2, 0.5 CH2Cl2' _chemical_formula_sum 'C40.50 H37 Cl Fe P2' _chemical_formula_weight 676.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5283(2) _cell_length_b 18.2097(4) _cell_length_c 19.3123(4) _cell_angle_alpha 93.20(2) _cell_angle_beta 93.13(2) _cell_angle_gamma 97.83(2) _cell_volume 3307.85(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 23275 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 31.50 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; NUMABS (Rigaku Inc., 2007) ; _exptl_absorpt_correction_T_min 0.8630 _exptl_absorpt_correction_T_max 0.9420 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'R-AXIS SPIDER' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71399 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 29.50 _reflns_number_total 18098 _reflns_number_gt 16479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0300P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18098 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.16282(2) 0.721164(12) 0.441947(11) 0.01436(5) Uani 1 1 d . . . Fe2 Fe 0.74323(2) 0.302500(12) 0.186286(11) 0.01466(5) Uani 1 1 d . . . P1 P 0.04685(4) 0.79362(2) 0.38260(2) 0.01549(8) Uani 1 1 d . . . P2 P 0.04583(4) 0.63083(2) 0.37524(2) 0.01509(8) Uani 1 1 d . . . P11 P 0.63333(5) 0.29815(2) 0.08564(2) 0.01684(8) Uani 1 1 d . . . P12 P 0.61630(4) 0.19723(2) 0.19955(2) 0.01634(8) Uani 1 1 d . . . Cl1 Cl 0.10870(8) 0.83165(4) 0.12765(4) 0.05966(19) Uani 1 1 d . . . Cl2 Cl 0.40732(7) 0.89496(3) 0.13172(3) 0.04803(14) Uani 1 1 d . . . C1 C 0.29912(18) 0.72235(9) 0.37316(8) 0.0174(3) Uani 1 1 d . . . C2 C 0.39015(18) 0.71850(9) 0.33159(8) 0.0196(3) Uani 1 1 d . . . C3 C 0.49076(17) 0.70753(9) 0.28035(8) 0.0182(3) Uani 1 1 d . . . C4 C 0.54881(19) 0.76550(10) 0.24167(9) 0.0232(3) Uani 1 1 d . . . H4A H 0.5275 0.8143 0.2517 0.028 Uiso 1 1 calc R . . C5 C 0.6375(2) 0.75274(12) 0.18858(10) 0.0296(4) Uani 1 1 d . . . H5A H 0.6748 0.7931 0.1629 0.035 Uiso 1 1 calc R . . C6 C 0.6731(2) 0.68225(13) 0.17212(10) 0.0300(4) Uani 1 1 d . . . C7 C 0.6210(2) 0.62542(11) 0.21210(10) 0.0288(4) Uani 1 1 d . . . H7A H 0.6464 0.5773 0.2032 0.035 Uiso 1 1 calc R . . C8 C 0.53182(19) 0.63723(10) 0.26535(9) 0.0226(3) Uani 1 1 d . . . H8A H 0.4981 0.5970 0.2921 0.027 Uiso 1 1 calc R . . C9 C 0.7660(3) 0.66819(17) 0.11292(12) 0.0481(6) Uani 1 1 d . . . H9A H 0.7791 0.6157 0.1097 0.072 Uiso 1 1 calc R . . H9B H 0.8586 0.6991 0.1215 0.072 Uiso 1 1 calc R . . H9C H 0.7204 0.6807 0.0693 0.072 Uiso 1 1 calc R . . C10 C 0.3323(2) 0.74512(10) 0.51726(9) 0.0241(3) Uani 1 1 d . . . H10A H 0.4331 0.7629 0.5079 0.029 Uiso 1 1 calc R . . C11 C 0.2703(2) 0.66946(10) 0.51772(9) 0.0238(3) Uani 1 1 d . . . H11A H 0.3197 0.6249 0.5103 0.029 Uiso 1 1 calc R . . C12 C 0.1257(2) 0.66948(10) 0.53333(8) 0.0241(3) Uani 1 1 d . . . H12A H 0.0553 0.6244 0.5383 0.029 Uiso 1 1 calc R . . C13 C 0.0993(2) 0.74410(10) 0.54204(9) 0.0245(4) Uani 1 1 d . . . H13A H 0.0072 0.7607 0.5538 0.029 Uiso 1 1 calc R . . C14 C 0.2280(2) 0.79119(10) 0.53222(9) 0.0241(3) Uani 1 1 d . . . H14A H 0.2420 0.8467 0.5352 0.029 Uiso 1 1 calc R . . C15 C -0.04509(19) 0.74115(9) 0.30295(9) 0.0203(3) Uani 1 1 d . . . H15A H -0.1484 0.7317 0.3088 0.024 Uiso 1 1 calc R . . H15B H -0.0297 0.7714 0.2623 0.024 Uiso 1 1 calc R . . C16 C 0.01162(18) 0.66675(9) 0.28987(8) 0.0179(3) Uani 1 1 d . . . H16A H 0.1002 0.6743 0.2651 0.022 Uiso 1 1 calc R . . H16B H -0.0593 0.6313 0.2612 0.022 Uiso 1 1 calc R . . C21 C -0.09423(18) 0.83855(9) 0.42319(8) 0.0183(3) Uani 1 1 d . . . C22 C -0.23837(19) 0.82270(10) 0.40224(10) 0.0234(3) Uani 1 1 d . . . H22A H -0.2683 0.7875 0.3644 0.028 Uiso 1 1 calc R . . C23 C -0.3396(2) 0.85798(11) 0.43630(11) 0.0285(4) Uani 1 1 d . . . H23A H -0.4370 0.8466 0.4212 0.034 Uiso 1 1 calc R . . C24 C -0.2985(2) 0.90947(11) 0.49203(11) 0.0290(4) Uani 1 1 d . . . H24A H -0.3676 0.9331 0.5150 0.035 Uiso 1 1 calc R . . C25 C -0.1558(2) 0.92621(10) 0.51401(10) 0.0268(4) Uani 1 1 d . . . H25A H -0.1270 0.9612 0.5522 0.032 Uiso 1 1 calc R . . C26 C -0.05459(19) 0.89141(9) 0.47970(9) 0.0229(3) Uani 1 1 d . . . H26A H 0.0428 0.9036 0.4947 0.028 Uiso 1 1 calc R . . C31 C 0.14519(18) 0.87727(9) 0.35072(9) 0.0192(3) Uani 1 1 d . . . C32 C 0.0800(2) 0.91947(10) 0.30390(10) 0.0247(4) Uani 1 1 d . . . H32A H -0.0146 0.9033 0.2859 0.030 Uiso 1 1 calc R . . C33 C 0.1531(2) 0.98516(10) 0.28359(11) 0.0304(4) Uani 1 1 d . . . H33A H 0.1084 1.0137 0.2515 0.037 Uiso 1 1 calc R . . C34 C 0.2911(2) 1.00942(10) 0.30987(11) 0.0319(4) Uani 1 1 d . . . H34A H 0.3405 1.0546 0.2960 0.038 Uiso 1 1 calc R . . C35 C 0.3566(2) 0.96793(10) 0.35610(11) 0.0287(4) Uani 1 1 d . . . H35A H 0.4512 0.9844 0.3739 0.034 Uiso 1 1 calc R . . C36 C 0.28395(19) 0.90197(9) 0.37669(9) 0.0225(3) Uani 1 1 d . . . H36A H 0.3293 0.8736 0.4087 0.027 Uiso 1 1 calc R . . C41 C -0.13388(17) 0.59420(9) 0.39811(8) 0.0171(3) Uani 1 1 d . . . C42 C -0.21032(18) 0.64279(9) 0.43507(9) 0.0204(3) Uani 1 1 d . . . H42A H -0.1640 0.6905 0.4518 0.024 Uiso 1 1 calc R . . C43 C -0.3519(2) 0.62226(10) 0.44743(10) 0.0246(3) Uani 1 1 d . . . H43A H -0.4029 0.6566 0.4706 0.030 Uiso 1 1 calc R . . C44 C -0.41926(19) 0.55121(10) 0.42578(9) 0.0238(3) Uani 1 1 d . . . H44A H -0.5157 0.5366 0.4348 0.029 Uiso 1 1 calc R . . C45 C -0.34369(19) 0.50175(10) 0.39072(9) 0.0237(3) Uani 1 1 d . . . H45A H -0.3888 0.4530 0.3768 0.028 Uiso 1 1 calc R . . C46 C -0.20297(19) 0.52290(9) 0.37585(9) 0.0210(3) Uani 1 1 d . . . H46A H -0.1538 0.4892 0.3507 0.025 Uiso 1 1 calc R . . C51 C 0.12892(17) 0.54763(8) 0.35577(8) 0.0171(3) Uani 1 1 d . . . C52 C 0.1370(2) 0.49605(10) 0.40579(9) 0.0233(3) Uani 1 1 d . . . H52A H 0.0969 0.5034 0.4492 0.028 Uiso 1 1 calc R . . C53 C 0.2038(2) 0.43360(10) 0.39267(11) 0.0286(4) Uani 1 1 d . . . H53A H 0.2068 0.3984 0.4270 0.034 Uiso 1 1 calc R . . C54 C 0.2658(2) 0.42197(10) 0.33047(11) 0.0267(4) Uani 1 1 d . . . H54A H 0.3106 0.3791 0.3221 0.032 Uiso 1 1 calc R . . C55 C 0.2615(2) 0.47329(10) 0.28101(10) 0.0260(4) Uani 1 1 d . . . H55A H 0.3053 0.4666 0.2385 0.031 Uiso 1 1 calc R . . C56 C 0.19265(19) 0.53545(9) 0.29342(9) 0.0217(3) Uani 1 1 d . . . H56A H 0.1891 0.5702 0.2587 0.026 Uiso 1 1 calc R . . C101 C 0.86495(17) 0.24226(9) 0.14225(8) 0.0173(3) Uani 1 1 d . . . C102 C 0.93698(18) 0.20075(9) 0.11207(9) 0.0207(3) Uani 1 1 d . . . C103 C 1.02496(18) 0.15303(9) 0.07807(9) 0.0196(3) Uani 1 1 d . . . C104 C 1.0956(2) 0.17355(10) 0.01941(9) 0.0259(4) Uani 1 1 d . . . H10B H 1.0854 0.2200 0.0010 0.031 Uiso 1 1 calc R . . C105 C 1.1814(2) 0.12713(12) -0.01307(10) 0.0308(4) Uani 1 1 d . . . H10C H 1.2281 0.1427 -0.0530 0.037 Uiso 1 1 calc R . . C106 C 1.1994(2) 0.05934(11) 0.01173(11) 0.0296(4) Uani 1 1 d . . . C107 C 1.1294(2) 0.03831(11) 0.06989(11) 0.0327(4) Uani 1 1 d . . . H10D H 1.1402 -0.0082 0.0879 0.039 Uiso 1 1 calc R . . C108 C 1.0432(2) 0.08404(10) 0.10268(10) 0.0274(4) Uani 1 1 d . . . H10E H 0.9962 0.0679 0.1424 0.033 Uiso 1 1 calc R . . C109 C 1.2922(3) 0.00909(14) -0.02426(14) 0.0438(6) Uani 1 1 d . . . H10F H 1.2928 -0.0363 0.0007 0.066 Uiso 1 1 calc R . . H10G H 1.3892 0.0351 -0.0244 0.066 Uiso 1 1 calc R . . H10H H 1.2542 -0.0039 -0.0722 0.066 Uiso 1 1 calc R . . C110 C 0.8996(2) 0.39447(10) 0.21502(10) 0.0283(4) Uani 1 1 d . . . H11B H 0.9897 0.4079 0.1916 0.034 Uiso 1 1 calc R . . C111 C 0.8824(2) 0.34924(10) 0.27144(10) 0.0274(4) Uani 1 1 d . . . H11C H 0.9578 0.3249 0.2954 0.033 Uiso 1 1 calc R . . C112 C 0.7402(2) 0.34554(10) 0.28878(9) 0.0311(4) Uani 1 1 d . . . H11D H 0.6974 0.3181 0.3277 0.037 Uiso 1 1 calc R . . C113 C 0.6687(2) 0.38828(11) 0.24337(11) 0.0341(5) Uani 1 1 d . . . H11E H 0.5679 0.3977 0.2448 0.041 Uiso 1 1 calc R . . C114 C 0.7697(3) 0.41839(10) 0.19816(10) 0.0326(5) Uani 1 1 d . . . H11F H 0.7515 0.4523 0.1607 0.039 Uiso 1 1 calc R . . C115 C 0.5613(2) 0.20103(9) 0.05485(9) 0.0247(4) Uani 1 1 d . . . H11G H 0.4644 0.2000 0.0332 0.030 Uiso 1 1 calc R . . H11H H 0.6214 0.1835 0.0189 0.030 Uiso 1 1 calc R . . C116 C 0.5558(2) 0.14860(9) 0.11343(9) 0.0236(3) Uani 1 1 d . . . H11I H 0.6165 0.1098 0.1033 0.028 Uiso 1 1 calc R . . H11J H 0.4572 0.1237 0.1155 0.028 Uiso 1 1 calc R . . C121 C 0.48153(18) 0.35043(9) 0.08057(8) 0.0194(3) Uani 1 1 d . . . C122 C 0.3458(2) 0.31742(11) 0.09224(12) 0.0319(4) Uani 1 1 d . . . H12B H 0.3290 0.2655 0.0976 0.038 Uiso 1 1 calc R . . C123 C 0.2332(2) 0.35866(12) 0.09623(12) 0.0353(5) Uani 1 1 d . . . H12C H 0.1412 0.3349 0.1046 0.042 Uiso 1 1 calc R . . C124 C 0.2553(2) 0.43389(11) 0.08805(10) 0.0289(4) Uani 1 1 d . . . H12D H 0.1790 0.4622 0.0908 0.035 Uiso 1 1 calc R . . C125 C 0.3899(2) 0.46790(10) 0.07575(10) 0.0289(4) Uani 1 1 d . . . H12E H 0.4058 0.5198 0.0701 0.035 Uiso 1 1 calc R . . C126 C 0.5021(2) 0.42649(10) 0.07155(10) 0.0243(3) Uani 1 1 d . . . H12F H 0.5936 0.4503 0.0625 0.029 Uiso 1 1 calc R . . C131 C 0.72808(19) 0.33197(9) 0.01147(8) 0.0202(3) Uani 1 1 d . . . C132 C 0.6600(2) 0.32501(10) -0.05521(9) 0.0246(3) Uani 1 1 d . . . H13B H 0.5646 0.3014 -0.0620 0.029 Uiso 1 1 calc R . . C133 C 0.7306(2) 0.35220(11) -0.11119(9) 0.0280(4) Uani 1 1 d . . . H13C H 0.6836 0.3475 -0.1562 0.034 Uiso 1 1 calc R . . C134 C 0.8700(2) 0.38639(11) -0.10147(9) 0.0270(4) Uani 1 1 d . . . H13D H 0.9188 0.4046 -0.1400 0.032 Uiso 1 1 calc R . . C135 C 0.9386(2) 0.39406(11) -0.03558(10) 0.0278(4) Uani 1 1 d . . . H13E H 1.0338 0.4180 -0.0290 0.033 Uiso 1 1 calc R . . C136 C 0.86791(19) 0.36668(10) 0.02053(9) 0.0232(3) Uani 1 1 d . . . H13F H 0.9153 0.3717 0.0655 0.028 Uiso 1 1 calc R . . C141 C 0.45478(17) 0.19811(9) 0.24831(8) 0.0176(3) Uani 1 1 d . . . C142 C 0.46977(19) 0.21030(9) 0.32084(9) 0.0208(3) Uani 1 1 d . . . H14B H 0.5612 0.2137 0.3440 0.025 Uiso 1 1 calc R . . C143 C 0.3527(2) 0.21746(10) 0.35938(9) 0.0247(4) Uani 1 1 d . . . H14C H 0.3646 0.2258 0.4085 0.030 Uiso 1 1 calc R . . C144 C 0.2184(2) 0.21248(10) 0.32615(10) 0.0260(4) Uani 1 1 d . . . H14D H 0.1387 0.2189 0.3522 0.031 Uiso 1 1 calc R . . C145 C 0.2011(2) 0.19809(12) 0.25465(10) 0.0302(4) Uani 1 1 d . . . H14E H 0.1091 0.1935 0.2319 0.036 Uiso 1 1 calc R . . C146 C 0.3184(2) 0.19031(11) 0.21612(9) 0.0266(4) Uani 1 1 d . . . H14F H 0.3053 0.1796 0.1673 0.032 Uiso 1 1 calc R . . C151 C 0.69498(18) 0.12558(9) 0.24472(9) 0.0200(3) Uani 1 1 d . . . C152 C 0.8171(2) 0.14451(9) 0.28850(9) 0.0232(3) Uani 1 1 d . . . H15C H 0.8651 0.1940 0.2914 0.028 Uiso 1 1 calc R . . C153 C 0.8693(2) 0.09167(10) 0.32792(10) 0.0283(4) Uani 1 1 d . . . H15D H 0.9524 0.1050 0.3579 0.034 Uiso 1 1 calc R . . C154 C 0.8001(2) 0.01924(10) 0.32354(11) 0.0298(4) Uani 1 1 d . . . H15E H 0.8342 -0.0167 0.3515 0.036 Uiso 1 1 calc R . . C155 C 0.6810(2) -0.00066(10) 0.27837(12) 0.0340(4) Uani 1 1 d . . . H15F H 0.6357 -0.0507 0.2742 0.041 Uiso 1 1 calc R . . C156 C 0.6279(2) 0.05210(10) 0.23931(11) 0.0284(4) Uani 1 1 d . . . H15G H 0.5458 0.0383 0.2088 0.034 Uiso 1 1 calc R . . C1S C 0.2745(2) 0.84005(12) 0.17345(12) 0.0367(5) Uani 1 1 d . . . H1SA H 0.3020 0.7900 0.1782 0.044 Uiso 1 1 calc R . . H1SB H 0.2672 0.8626 0.2207 0.044 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 Fe1 0.01473(11) 0.01626(10) 0.01184(10) 0.00037(7) 0.00062(8) 0.00159(8) Fe2 0.01430(11) 0.01513(10) 0.01415(10) -0.00125(8) -0.00005(8) 0.00194(8) P1 0.01531(19) 0.01543(17) 0.01560(18) 0.00041(13) 0.00037(15) 0.00217(14) P2 0.01627(19) 0.01522(17) 0.01340(17) 0.00044(13) 0.00140(15) 0.00081(14) P11 0.01621(19) 0.01794(18) 0.01641(18) -0.00103(14) -0.00197(15) 0.00461(14) P12 0.01571(19) 0.01610(17) 0.01669(18) -0.00171(14) 0.00200(15) 0.00112(14) Cl1 0.0487(4) 0.0519(4) 0.0739(5) 0.0023(3) -0.0271(3) 0.0042(3) Cl2 0.0540(4) 0.0468(3) 0.0418(3) 0.0073(2) -0.0002(3) 0.0008(3) C1 0.0174(8) 0.0172(7) 0.0171(7) 0.0004(5) -0.0015(6) 0.0019(6) C2 0.0192(8) 0.0209(7) 0.0180(7) 0.0001(6) 0.0007(6) 0.0012(6) C3 0.0153(7) 0.0244(8) 0.0143(7) 0.0000(6) -0.0010(6) 0.0015(6) C4 0.0218(8) 0.0259(8) 0.0214(8) 0.0029(6) 0.0015(7) 0.0011(6) C5 0.0226(9) 0.0440(11) 0.0214(8) 0.0098(7) 0.0035(7) -0.0017(8) C6 0.0168(8) 0.0544(12) 0.0187(8) -0.0028(8) 0.0027(7) 0.0061(8) C7 0.0238(9) 0.0372(10) 0.0262(9) -0.0062(7) -0.0001(7) 0.0108(8) C8 0.0203(8) 0.0262(8) 0.0216(8) 0.0011(6) 0.0013(7) 0.0044(6) C9 0.0343(12) 0.0848(19) 0.0275(11) -0.0019(11) 0.0125(9) 0.0150(12) C10 0.0222(9) 0.0328(9) 0.0159(7) 0.0002(6) -0.0042(6) 0.0017(7) C11 0.0278(9) 0.0280(8) 0.0163(7) 0.0041(6) -0.0031(7) 0.0071(7) C12 0.0280(9) 0.0303(9) 0.0128(7) 0.0044(6) 0.0008(6) -0.0017(7) C13 0.0238(9) 0.0360(9) 0.0140(7) -0.0020(6) 0.0027(6) 0.0060(7) C14 0.0309(10) 0.0242(8) 0.0154(7) -0.0048(6) -0.0032(7) 0.0015(7) C15 0.0215(8) 0.0205(7) 0.0184(7) -0.0011(6) -0.0044(6) 0.0043(6) C16 0.0205(8) 0.0187(7) 0.0141(7) 0.0008(5) -0.0001(6) 0.0016(6) C21 0.0185(8) 0.0166(7) 0.0200(7) 0.0014(6) 0.0017(6) 0.0030(6) C22 0.0187(8) 0.0239(8) 0.0270(8) -0.0011(6) -0.0003(7) 0.0027(6) C23 0.0170(8) 0.0324(9) 0.0369(10) 0.0022(8) 0.0033(8) 0.0055(7) C24 0.0263(10) 0.0302(9) 0.0334(10) 0.0029(7) 0.0099(8) 0.0107(7) C25 0.0276(9) 0.0256(8) 0.0280(9) -0.0037(7) 0.0050(8) 0.0074(7) C26 0.0194(8) 0.0230(8) 0.0259(8) -0.0028(6) 0.0005(7) 0.0034(6) C31 0.0210(8) 0.0166(7) 0.0209(7) 0.0018(6) 0.0052(6) 0.0038(6) C32 0.0264(9) 0.0227(8) 0.0268(9) 0.0056(6) 0.0048(7) 0.0067(7) C33 0.0389(11) 0.0226(8) 0.0335(10) 0.0101(7) 0.0104(9) 0.0109(8) C34 0.0373(11) 0.0189(8) 0.0407(11) 0.0060(7) 0.0164(9) 0.0014(7) C35 0.0246(9) 0.0237(8) 0.0371(10) 0.0000(7) 0.0083(8) -0.0014(7) C36 0.0219(8) 0.0205(7) 0.0255(8) 0.0006(6) 0.0054(7) 0.0030(6) C41 0.0174(8) 0.0187(7) 0.0147(7) 0.0011(5) 0.0007(6) 0.0004(6) C42 0.0208(8) 0.0179(7) 0.0217(8) -0.0009(6) 0.0041(6) -0.0001(6) C43 0.0220(9) 0.0257(8) 0.0263(9) -0.0013(7) 0.0075(7) 0.0027(7) C44 0.0185(8) 0.0289(8) 0.0232(8) 0.0019(7) 0.0041(7) -0.0011(7) C45 0.0224(9) 0.0221(8) 0.0243(8) -0.0015(6) 0.0008(7) -0.0033(6) C46 0.0214(8) 0.0199(7) 0.0208(8) -0.0020(6) 0.0014(6) 0.0007(6) C51 0.0176(8) 0.0156(6) 0.0173(7) 0.0003(5) -0.0006(6) 0.0006(5) C52 0.0235(9) 0.0250(8) 0.0223(8) 0.0068(6) 0.0043(7) 0.0037(7) C53 0.0242(9) 0.0253(8) 0.0381(10) 0.0125(7) 0.0024(8) 0.0048(7) C54 0.0212(9) 0.0184(7) 0.0406(10) 0.0008(7) -0.0005(8) 0.0044(6) C55 0.0263(9) 0.0253(8) 0.0263(9) -0.0034(7) 0.0025(7) 0.0054(7) C56 0.0260(9) 0.0209(7) 0.0192(7) 0.0017(6) 0.0028(7) 0.0060(6) C101 0.0150(7) 0.0205(7) 0.0156(7) 0.0023(5) -0.0011(6) 0.0003(6) C102 0.0179(8) 0.0233(8) 0.0205(8) 0.0015(6) -0.0008(6) 0.0026(6) C103 0.0150(7) 0.0231(7) 0.0204(7) -0.0032(6) -0.0016(6) 0.0041(6) C104 0.0268(9) 0.0280(8) 0.0241(8) 0.0013(7) 0.0043(7) 0.0075(7) C105 0.0263(10) 0.0391(10) 0.0274(9) -0.0042(8) 0.0067(8) 0.0066(8) C106 0.0191(9) 0.0338(9) 0.0352(10) -0.0126(8) -0.0015(8) 0.0079(7) C107 0.0325(11) 0.0252(9) 0.0420(11) -0.0013(8) -0.0003(9) 0.0124(8) C108 0.0276(10) 0.0262(8) 0.0296(9) 0.0025(7) 0.0034(8) 0.0077(7) C109 0.0328(12) 0.0463(12) 0.0531(14) -0.0177(11) 0.0025(10) 0.0172(10) C110 0.0290(10) 0.0257(8) 0.0258(9) -0.0058(7) 0.0038(8) -0.0093(7) C111 0.0308(10) 0.0220(8) 0.0268(9) -0.0057(7) -0.0126(8) 0.0028(7) C112 0.0425(12) 0.0275(9) 0.0181(8) -0.0075(7) 0.0063(8) -0.0114(8) C113 0.0233(9) 0.0348(10) 0.0418(11) -0.0231(9) -0.0032(8) 0.0078(8) C114 0.0530(13) 0.0165(7) 0.0263(9) -0.0035(6) -0.0122(9) 0.0054(8) C115 0.0305(10) 0.0199(7) 0.0225(8) -0.0037(6) -0.0093(7) 0.0058(7) C116 0.0285(9) 0.0198(7) 0.0200(8) -0.0054(6) 0.0035(7) -0.0033(6) C121 0.0179(8) 0.0222(7) 0.0187(7) 0.0016(6) -0.0020(6) 0.0059(6) C122 0.0195(9) 0.0278(9) 0.0501(12) 0.0138(8) 0.0011(8) 0.0051(7) C123 0.0183(9) 0.0419(11) 0.0487(12) 0.0149(9) 0.0051(9) 0.0091(8) C124 0.0271(10) 0.0370(10) 0.0263(9) 0.0036(7) 0.0016(7) 0.0177(8) C125 0.0333(10) 0.0245(8) 0.0311(9) 0.0040(7) 0.0012(8) 0.0119(7) C126 0.0222(9) 0.0232(8) 0.0281(9) 0.0039(6) 0.0025(7) 0.0046(6) C131 0.0222(8) 0.0238(8) 0.0159(7) -0.0003(6) 0.0001(6) 0.0093(6) C132 0.0252(9) 0.0297(9) 0.0190(8) -0.0016(6) -0.0026(7) 0.0076(7) C133 0.0361(11) 0.0333(9) 0.0165(8) 0.0002(7) -0.0028(7) 0.0137(8) C134 0.0334(10) 0.0321(9) 0.0184(8) 0.0029(7) 0.0051(7) 0.0129(8) C135 0.0245(9) 0.0372(10) 0.0227(8) 0.0026(7) 0.0043(7) 0.0061(7) C136 0.0221(9) 0.0316(9) 0.0166(7) 0.0005(6) 0.0007(6) 0.0070(7) C141 0.0156(7) 0.0180(7) 0.0190(7) 0.0017(5) 0.0019(6) 0.0011(6) C142 0.0180(8) 0.0243(8) 0.0193(7) 0.0006(6) -0.0001(6) 0.0012(6) C143 0.0253(9) 0.0293(9) 0.0188(8) -0.0013(6) 0.0045(7) 0.0009(7) C144 0.0188(8) 0.0310(9) 0.0296(9) 0.0033(7) 0.0094(7) 0.0045(7) C145 0.0170(8) 0.0461(11) 0.0286(9) 0.0101(8) -0.0003(7) 0.0059(8) C146 0.0195(9) 0.0412(10) 0.0186(8) 0.0062(7) -0.0006(7) 0.0018(7) C151 0.0193(8) 0.0177(7) 0.0240(8) 0.0006(6) 0.0063(6) 0.0041(6) C152 0.0232(9) 0.0201(7) 0.0266(8) 0.0021(6) 0.0021(7) 0.0040(6) C153 0.0277(10) 0.0282(9) 0.0305(9) 0.0049(7) 0.0009(8) 0.0089(7) C154 0.0313(10) 0.0242(8) 0.0378(10) 0.0103(7) 0.0100(8) 0.0117(7) C155 0.0336(11) 0.0186(8) 0.0506(12) 0.0066(8) 0.0096(9) 0.0022(7) C156 0.0229(9) 0.0204(8) 0.0412(11) 0.0023(7) 0.0023(8) 0.0001(7) C1S 0.0360(12) 0.0379(11) 0.0368(11) 0.0009(9) -0.0043(9) 0.0102(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.9068(17) . yes Fe1 C12 2.0708(17) . yes Fe1 C11 2.0809(17) . yes Fe1 C13 2.0938(17) . yes Fe1 C10 2.0962(18) . yes Fe1 C14 2.1138(17) . yes Fe1 P1 2.1687(6) . yes Fe1 P2 2.1714(7) . yes Fe2 C101 1.9031(17) . yes Fe2 C113 2.0868(18) . yes Fe2 C114 2.0891(18) . yes Fe2 C112 2.0910(18) . yes Fe2 C110 2.1115(18) . yes Fe2 C111 2.1177(18) . yes Fe2 P11 2.1492(6) . yes Fe2 P12 2.1586(6) . yes P1 C31 1.8320(17) . yes P1 C21 1.8531(17) . yes P1 C15 1.8727(17) . yes P2 C51 1.8328(16) . yes P2 C16 1.8365(16) . yes P2 C41 1.8375(17) . yes P11 C131 1.8259(18) . yes P11 C121 1.8380(17) . yes P11 C115 1.8601(17) . yes P12 C151 1.8297(17) . yes P12 C141 1.8490(17) . yes P12 C116 1.8641(17) . yes Cl1 C1S 1.752(2) . yes Cl2 C1S 1.763(2) . yes C1 C2 1.220(2) . yes C2 C3 1.439(2) . yes C3 C4 1.397(2) . yes C3 C8 1.408(2) . yes C4 C5 1.393(3) . yes C4 H4A 0.9500 . ? C5 C6 1.396(3) . yes C5 H5A 0.9500 . ? C6 C7 1.380(3) . yes C6 C9 1.515(3) . yes C7 C8 1.395(3) . yes C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C14 1.417(3) . yes C10 C11 1.424(3) . yes C10 H10A 1.0000 . ? C11 C12 1.426(3) . yes C11 H11A 1.0000 . ? C12 C13 1.418(3) . yes C12 H12A 1.0000 . ? C13 C14 1.425(3) . yes C13 H13A 1.0000 . ? C14 H14A 1.0000 . ? C15 C16 1.539(2) . yes C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C22 1.397(2) . yes C21 C26 1.414(2) . yes C22 C23 1.402(3) . yes C22 H22A 0.9500 . ? C23 C24 1.390(3) . yes C23 H23A 0.9500 . ? C24 C25 1.390(3) . yes C24 H24A 0.9500 . ? C25 C26 1.400(2) . yes C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C32 1.393(2) . yes C31 C36 1.394(2) . yes C32 C33 1.387(3) . yes C32 H32A 0.9500 . ? C33 C34 1.388(3) . yes C33 H33A 0.9500 . ? C34 C35 1.378(3) . yes C34 H34A 0.9500 . ? C35 C36 1.392(2) . yes C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.406(2) . yes C41 C42 1.409(2) . yes C42 C43 1.387(2) . yes C42 H42A 0.9500 . ? C43 C44 1.395(2) . yes C43 H43A 0.9500 . ? C44 C45 1.396(3) . yes C44 H44A 0.9500 . ? C45 C46 1.394(2) . yes C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C52 1.391(2) . yes C51 C56 1.398(2) . yes C52 C53 1.394(3) . yes C52 H52A 0.9500 . ? C53 C54 1.386(3) . yes C53 H53A 0.9500 . ? C54 C55 1.376(3) . yes C54 H54A 0.9500 . ? C55 C56 1.399(2) . yes C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C101 C102 1.232(2) . yes C102 C103 1.444(2) . yes C103 C104 1.392(3) . yes C103 C108 1.397(2) . yes C104 C105 1.400(3) . yes C104 H10B 0.9500 . ? C105 C106 1.377(3) . yes C105 H10C 0.9500 . ? C106 C107 1.383(3) . yes C106 C109 1.523(3) . yes C107 C108 1.398(3) . yes C107 H10D 0.9500 . ? C108 H10E 0.9500 . ? C109 H10F 0.9800 . ? C109 H10G 0.9800 . ? C109 H10H 0.9800 . ? C110 C114 1.395(3) . yes C110 C111 1.405(3) . yes C110 H11B 1.0000 . ? C111 C112 1.407(3) . yes C111 H11C 1.0000 . ? C112 C113 1.412(3) . yes C112 H11D 1.0000 . ? C113 C114 1.410(3) . yes C113 H11E 1.0000 . ? C114 H11F 1.0000 . ? C115 C116 1.519(2) . yes C115 H11G 0.9900 . ? C115 H11H 0.9900 . ? C116 H11I 0.9900 . ? C116 H11J 0.9900 . ? C121 C122 1.386(3) . yes C121 C126 1.394(2) . yes C122 C123 1.394(3) . yes C122 H12B 0.9500 . ? C123 C124 1.377(3) . yes C123 H12C 0.9500 . ? C124 C125 1.384(3) . yes C124 H12D 0.9500 . ? C125 C126 1.393(3) . yes C125 H12E 0.9500 . ? C126 H12F 0.9500 . ? C131 C136 1.392(3) . yes C131 C132 1.401(2) . yes C132 C133 1.384(3) . yes C132 H13B 0.9500 . ? C133 C134 1.387(3) . yes C133 H13C 0.9500 . ? C134 C135 1.389(3) . yes C134 H13D 0.9500 . ? C135 C136 1.388(3) . yes C135 H13E 0.9500 . ? C136 H13F 0.9500 . ? C141 C146 1.395(2) . yes C141 C142 1.402(2) . yes C142 C143 1.391(2) . yes C142 H14B 0.9500 . ? C143 C144 1.390(3) . yes C143 H14C 0.9500 . ? C144 C145 1.388(3) . yes C144 H14D 0.9500 . ? C145 C146 1.395(3) . yes C145 H14E 0.9500 . ? C146 H14F 0.9500 . ? C151 C152 1.393(3) . yes C151 C156 1.398(2) . yes C152 C153 1.387(2) . yes C152 H15C 0.9500 . ? C153 C154 1.388(3) . yes C153 H15D 0.9500 . ? C154 C155 1.387(3) . yes C154 H15E 0.9500 . ? C155 C156 1.386(3) . yes C155 H15F 0.9500 . ? C156 H15G 0.9500 . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C12 136.81(7) . . yes C1 Fe1 C11 98.28(7) . . yes C12 Fe1 C11 40.19(7) . . yes C1 Fe1 C13 153.39(7) . . yes C12 Fe1 C13 39.80(7) . . yes C11 Fe1 C13 67.21(7) . . yes C1 Fe1 C10 88.04(7) . . yes C12 Fe1 C10 66.66(7) . . yes C11 Fe1 C10 39.85(7) . . yes C13 Fe1 C10 66.40(7) . . yes C1 Fe1 C14 114.88(7) . . yes C12 Fe1 C14 66.61(7) . . yes C11 Fe1 C14 66.86(7) . . yes C13 Fe1 C14 39.59(7) . . yes C10 Fe1 C14 39.32(7) . . yes C1 Fe1 P1 90.19(5) . . yes C12 Fe1 P1 132.91(6) . . yes C11 Fe1 P1 166.76(5) . . yes C13 Fe1 P1 100.93(5) . . yes C10 Fe1 P1 131.14(5) . . yes C14 Fe1 P1 100.35(5) . . yes C1 Fe1 P2 84.28(5) . . yes C12 Fe1 P2 94.80(5) . . yes C11 Fe1 P2 104.93(5) . . yes C13 Fe1 P2 120.27(6) . . yes C10 Fe1 P2 142.19(5) . . yes C14 Fe1 P2 159.55(6) . . yes P1 Fe1 P2 85.95(2) . . yes C101 Fe2 C113 162.54(7) . . yes C101 Fe2 C114 127.18(8) . . yes C113 Fe2 C114 39.48(9) . . yes C101 Fe2 C112 132.20(8) . . yes C113 Fe2 C112 39.52(9) . . yes C114 Fe2 C112 65.49(8) . . yes C101 Fe2 C110 96.80(7) . . yes C113 Fe2 C110 65.95(8) . . yes C114 Fe2 C110 38.80(8) . . yes C112 Fe2 C110 65.28(8) . . yes C101 Fe2 C111 99.03(7) . . yes C113 Fe2 C111 66.11(8) . . yes C114 Fe2 C111 65.24(7) . . yes C112 Fe2 C111 39.04(8) . . yes C110 Fe2 C111 38.82(8) . . yes C101 Fe2 P11 85.32(5) . . yes C113 Fe2 P11 104.80(6) . . yes C114 Fe2 P11 93.87(6) . . yes C112 Fe2 P11 142.48(7) . . yes C110 Fe2 P11 118.17(6) . . yes C111 Fe2 P11 156.76(6) . . yes C101 Fe2 P12 83.62(5) . . yes C113 Fe2 P12 110.84(7) . . yes C114 Fe2 P12 149.15(7) . . yes C112 Fe2 P12 96.45(6) . . yes C110 Fe2 P12 155.69(6) . . yes C111 Fe2 P12 116.98(6) . . yes P11 Fe2 P12 86.13(3) . . yes C31 P1 C21 97.54(7) . . yes C31 P1 C15 104.83(8) . . yes C21 P1 C15 104.19(8) . . yes C31 P1 Fe1 118.66(6) . . yes C21 P1 Fe1 119.66(6) . . yes C15 P1 Fe1 109.99(5) . . yes C51 P2 C16 104.24(7) . . yes C51 P2 C41 104.16(7) . . yes C16 P2 C41 102.09(8) . . yes C51 P2 Fe1 119.02(6) . . yes C16 P2 Fe1 107.66(5) . . yes C41 P2 Fe1 117.64(5) . . yes C131 P11 C121 100.37(8) . . yes C131 P11 C115 102.38(8) . . yes C121 P11 C115 105.62(8) . . yes C131 P11 Fe2 120.00(6) . . yes C121 P11 Fe2 115.39(6) . . yes C115 P11 Fe2 111.32(6) . . yes C151 P12 C141 98.94(8) . . yes C151 P12 C116 102.22(8) . . yes C141 P12 C116 105.82(8) . . yes C151 P12 Fe2 119.71(6) . . yes C141 P12 Fe2 117.73(5) . . yes C116 P12 Fe2 110.44(6) . . yes C2 C1 Fe1 174.93(15) . . yes C1 C2 C3 174.84(17) . . yes C4 C3 C8 116.89(16) . . yes C4 C3 C2 121.63(15) . . yes C8 C3 C2 121.45(15) . . yes C5 C4 C3 120.92(17) . . yes C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 121.83(18) . . yes C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C7 C6 C5 117.48(17) . . yes C7 C6 C9 120.9(2) . . yes C5 C6 C9 121.6(2) . . yes C6 C7 C8 121.37(18) . . yes C6 C7 H7A 119.3 . . ? C8 C7 H7A 119.3 . . ? C7 C8 C3 121.40(17) . . yes C7 C8 H8A 119.3 . . ? C3 C8 H8A 119.3 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C11 108.92(17) . . yes C14 C10 Fe1 71.01(10) . . yes C11 C10 Fe1 69.50(10) . . yes C14 C10 H10A 125.5 . . ? C11 C10 H10A 125.5 . . ? Fe1 C10 H10A 125.5 . . ? C10 C11 C12 106.91(16) . . yes C10 C11 Fe1 70.65(10) . . yes C12 C11 Fe1 69.52(10) . . yes C10 C11 H11A 126.5 . . ? C12 C11 H11A 126.5 . . ? Fe1 C11 H11A 126.5 . . ? C13 C12 C11 108.66(16) . . yes C13 C12 Fe1 70.97(10) . . yes C11 C12 Fe1 70.29(10) . . yes C13 C12 H12A 125.7 . . ? C11 C12 H12A 125.7 . . ? Fe1 C12 H12A 125.7 . . ? C12 C13 C14 107.85(16) . . yes C12 C13 Fe1 69.22(10) . . yes C14 C13 Fe1 70.96(10) . . yes C12 C13 H13A 126.1 . . ? C14 C13 H13A 126.1 . . ? Fe1 C13 H13A 126.1 . . ? C10 C14 C13 107.66(16) . . yes C10 C14 Fe1 69.67(10) . . yes C13 C14 Fe1 69.45(10) . . yes C10 C14 H14A 126.2 . . ? C13 C14 H14A 126.2 . . ? Fe1 C14 H14A 126.2 . . ? C16 C15 P1 110.78(11) . . yes C16 C15 H15A 109.5 . . ? P1 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C15 C16 P2 106.98(11) . . yes C15 C16 H16A 110.3 . . ? P2 C16 H16A 110.3 . . ? C15 C16 H16B 110.3 . . ? P2 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C22 C21 C26 117.55(16) . . yes C22 C21 P1 124.16(13) . . yes C26 C21 P1 118.29(13) . . yes C21 C22 C23 120.98(17) . . yes C21 C22 H22A 119.5 . . ? C23 C22 H22A 119.5 . . ? C24 C23 C22 120.59(18) . . yes C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 119.63(17) . . yes C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C26 119.80(17) . . yes C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C21 121.45(17) . . yes C25 C26 H26A 119.3 . . ? C21 C26 H26A 119.3 . . ? C32 C31 C36 119.16(16) . . yes C32 C31 P1 120.76(14) . . yes C36 C31 P1 119.95(13) . . yes C33 C32 C31 120.07(18) . . yes C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 120.36(18) . . yes C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C35 C34 C33 119.97(17) . . yes C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 119.99(19) . . yes C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.45(17) . . yes C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? C46 C41 C42 118.46(15) . . yes C46 C41 P2 123.66(13) . . yes C42 C41 P2 117.66(12) . . yes C43 C42 C41 121.22(15) . . yes C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 119.93(16) . . yes C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C43 C44 C45 119.45(17) . . yes C43 C44 H44A 120.3 . . ? C45 C44 H44A 120.3 . . ? C46 C45 C44 120.94(16) . . yes C46 C45 H45A 119.5 . . ? C44 C45 H45A 119.5 . . ? C45 C46 C41 119.94(16) . . yes C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? C52 C51 C56 117.77(15) . . yes C52 C51 P2 119.62(13) . . yes C56 C51 P2 122.51(12) . . yes C51 C52 C53 120.40(17) . . yes C51 C52 H52A 119.8 . . ? C53 C52 H52A 119.8 . . ? C54 C53 C52 121.22(17) . . yes C54 C53 H53A 119.4 . . ? C52 C53 H53A 119.4 . . ? C55 C54 C53 119.15(16) . . yes C55 C54 H54A 120.4 . . ? C53 C54 H54A 120.4 . . ? C54 C55 C56 119.88(17) . . yes C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C51 C56 C55 121.55(16) . . yes C51 C56 H56A 119.2 . . ? C55 C56 H56A 119.2 . . ? C102 C101 Fe2 176.37(15) . . yes C101 C102 C103 178.30(18) . . yes C104 C103 C108 116.91(16) . . yes C104 C103 C102 121.67(16) . . yes C108 C103 C102 121.42(16) . . yes C103 C104 C105 121.34(18) . . yes C103 C104 H10B 119.3 . . ? C105 C104 H10B 119.3 . . ? C106 C105 C104 121.39(19) . . yes C106 C105 H10C 119.3 . . ? C104 C105 H10C 119.3 . . ? C105 C106 C107 117.76(17) . . yes C105 C106 C109 121.0(2) . . yes C107 C106 C109 121.3(2) . . yes C106 C107 C108 121.41(18) . . yes C106 C107 H10D 119.3 . . ? C108 C107 H10D 119.3 . . ? C103 C108 C107 121.18(18) . . yes C103 C108 H10E 119.4 . . ? C107 C108 H10E 119.4 . . ? C106 C109 H10F 109.5 . . ? C106 C109 H10G 109.5 . . ? H10F C109 H10G 109.5 . . ? C106 C109 H10H 109.5 . . ? H10F C109 H10H 109.5 . . ? H10G C109 H10H 109.5 . . ? C114 C110 C111 108.13(18) . . yes C114 C110 Fe2 69.73(11) . . yes C111 C110 Fe2 70.83(10) . . yes C114 C110 H11B 125.9 . . ? C111 C110 H11B 125.9 . . ? Fe2 C110 H11B 125.9 . . ? C110 C111 C112 107.43(17) . . yes C110 C111 Fe2 70.35(10) . . yes C112 C111 Fe2 69.45(10) . . yes C110 C111 H11C 126.3 . . ? C112 C111 H11C 126.3 . . ? Fe2 C111 H11C 126.3 . . ? C111 C112 C113 108.90(17) . . yes C111 C112 Fe2 71.50(11) . . yes C113 C112 Fe2 70.08(10) . . yes C111 C112 H11D 125.5 . . ? C113 C112 H11D 125.5 . . ? Fe2 C112 H11D 125.5 . . ? C114 C113 C112 106.46(18) . . yes C114 C113 Fe2 70.35(11) . . yes C112 C113 Fe2 70.40(11) . . yes C114 C113 H11E 126.7 . . ? C112 C113 H11E 126.7 . . ? Fe2 C113 H11E 126.7 . . ? C110 C114 C113 109.08(17) . . yes C110 C114 Fe2 71.47(10) . . yes C113 C114 Fe2 70.18(11) . . yes C110 C114 H11F 125.5 . . ? C113 C114 H11F 125.5 . . ? Fe2 C114 H11F 125.5 . . ? C116 C115 P11 112.27(11) . . yes C116 C115 H11G 109.2 . . ? P11 C115 H11G 109.2 . . ? C116 C115 H11H 109.2 . . ? P11 C115 H11H 109.2 . . ? H11G C115 H11H 107.9 . . ? C115 C116 P12 112.62(11) . . yes C115 C116 H11I 109.1 . . ? P12 C116 H11I 109.1 . . ? C115 C116 H11J 109.1 . . ? P12 C116 H11J 109.1 . . ? H11I C116 H11J 107.8 . . ? C122 C121 C126 117.85(16) . . yes C122 C121 P11 121.26(13) . . yes C126 C121 P11 120.60(14) . . yes C121 C122 C123 121.51(18) . . yes C121 C122 H12B 119.2 . . ? C123 C122 H12B 119.2 . . ? C124 C123 C122 120.01(19) . . yes C124 C123 H12C 120.0 . . ? C122 C123 H12C 120.0 . . ? C123 C124 C125 119.45(17) . . yes C123 C124 H12D 120.3 . . ? C125 C124 H12D 120.3 . . ? C124 C125 C126 120.42(17) . . yes C124 C125 H12E 119.8 . . ? C126 C125 H12E 119.8 . . ? C125 C126 C121 120.74(18) . . yes C125 C126 H12F 119.6 . . ? C121 C126 H12F 119.6 . . ? C136 C131 C132 118.96(16) . . yes C136 C131 P11 120.55(13) . . yes C132 C131 P11 120.47(14) . . yes C133 C132 C131 120.54(18) . . yes C133 C132 H13B 119.7 . . ? C131 C132 H13B 119.7 . . ? C132 C133 C134 119.89(17) . . yes C132 C133 H13C 120.1 . . ? C134 C133 H13C 120.1 . . ? C133 C134 C135 120.19(18) . . yes C133 C134 H13D 119.9 . . ? C135 C134 H13D 119.9 . . ? C136 C135 C134 119.91(18) . . yes C136 C135 H13E 120.0 . . ? C134 C135 H13E 120.0 . . ? C135 C136 C131 120.50(16) . . yes C135 C136 H13F 119.7 . . ? C131 C136 H13F 119.7 . . ? C146 C141 C142 118.14(16) . . yes C146 C141 P12 123.07(13) . . yes C142 C141 P12 118.73(13) . . yes C143 C142 C141 120.96(16) . . yes C143 C142 H14B 119.5 . . ? C141 C142 H14B 119.5 . . ? C144 C143 C142 120.07(16) . . yes C144 C143 H14C 120.0 . . ? C142 C143 H14C 120.0 . . ? C145 C144 C143 119.68(17) . . yes C145 C144 H14D 120.2 . . ? C143 C144 H14D 120.2 . . ? C144 C145 C146 120.18(18) . . yes C144 C145 H14E 119.9 . . ? C146 C145 H14E 119.9 . . ? C145 C146 C141 120.88(17) . . yes C145 C146 H14F 119.6 . . ? C141 C146 H14F 119.6 . . ? C152 C151 C156 119.20(16) . . yes C152 C151 P12 120.33(13) . . yes C156 C151 P12 120.33(14) . . yes C153 C152 C151 120.48(17) . . yes C153 C152 H15C 119.8 . . ? C151 C152 H15C 119.8 . . ? C152 C153 C154 119.93(19) . . yes C152 C153 H15D 120.0 . . ? C154 C153 H15D 120.0 . . ? C155 C154 C153 119.96(18) . . yes C155 C154 H15E 120.0 . . ? C153 C154 H15E 120.0 . . ? C156 C155 C154 120.24(18) . . yes C156 C155 H15F 119.9 . . ? C154 C155 H15F 119.9 . . ? C155 C156 C151 120.14(19) . . yes C155 C156 H15G 119.9 . . ? C151 C156 H15G 119.9 . . ? Cl1 C1S Cl2 112.13(13) . . yes Cl1 C1S H1SA 109.2 . . ? Cl2 C1S H1SA 109.2 . . ? Cl1 C1S H1SB 109.2 . . ? Cl2 C1S H1SB 109.2 . . ? H1SA C1S H1SB 107.9 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.613 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.068 # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END #3. data data_4b _database_code_depnum_ccdc_archive 'CCDC 691298' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H46 P2 Ru' _chemical_formula_sum 'C45 H46 P2 Ru' _chemical_formula_weight 749.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4106(3) _cell_length_b 11.2059(2) _cell_length_c 22.1850(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.33(1) _cell_angle_gamma 90.00 _cell_volume 3636.75(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7464 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 31.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 6000' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48050 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10598 _reflns_number_gt 7954 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.630 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.45 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.45' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0500P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10598 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.280058(9) 0.251876(12) 0.319842(7) 0.01581(5) Uani 1 1 d . . . P1 P 0.12811(3) 0.22034(4) 0.29685(2) 0.01838(10) Uani 1 1 d . . . P2 P 0.27657(3) 0.07020(4) 0.27468(2) 0.01811(10) Uani 1 1 d . . . C1 C 0.27704(12) 0.16014(17) 0.39757(9) 0.0212(4) Uani 1 1 d . . . C2 C 0.27189(13) 0.09915(19) 0.44139(9) 0.0246(4) Uani 1 1 d . . . C3 C 0.26351(13) 0.01283(17) 0.48716(9) 0.0227(4) Uani 1 1 d . . . C4 C 0.30423(14) -0.10018(19) 0.49098(10) 0.0268(4) Uani 1 1 d . . . H4A H 0.3393 -0.1188 0.4638 0.032 Uiso 1 1 calc R . . C5 C 0.29406(14) -0.18508(19) 0.53377(10) 0.0273(4) Uani 1 1 d . . . H5A H 0.3225 -0.2608 0.5353 0.033 Uiso 1 1 calc R . . C6 C 0.24346(14) -0.16228(18) 0.57433(9) 0.0254(4) Uani 1 1 d . . . C7 C 0.20098(14) -0.05098(18) 0.56955(9) 0.0264(4) Uani 1 1 d . . . H7A H 0.1642 -0.0340 0.5957 0.032 Uiso 1 1 calc R . . C8 C 0.21124(14) 0.03530(18) 0.52742(9) 0.0256(4) Uani 1 1 d . . . H8A H 0.1824 0.1107 0.5259 0.031 Uiso 1 1 calc R . . C9 C 0.23627(17) -0.25283(19) 0.62247(12) 0.0340(5) Uani 1 1 d . . . H9A H 0.2702 -0.3249 0.6186 0.051 Uiso 1 1 calc R . . H9B H 0.1719 -0.2731 0.6150 0.051 Uiso 1 1 calc R . . H9C H 0.2620 -0.2195 0.6652 0.051 Uiso 1 1 calc R . . C10 C 0.32423(13) 0.43251(16) 0.36064(9) 0.0212(4) Uani 1 1 d . . . C11 C 0.29260(13) 0.44332(16) 0.29185(9) 0.0195(4) Uani 1 1 d . . . C12 C 0.35006(13) 0.37339(16) 0.26735(9) 0.0198(4) Uani 1 1 d . . . C13 C 0.41877(12) 0.31721(17) 0.32027(9) 0.0206(4) Uani 1 1 d . . . C14 C 0.40233(13) 0.35575(17) 0.37707(9) 0.0213(4) Uani 1 1 d . . . C15 C 0.29012(15) 0.50132(19) 0.40659(10) 0.0296(4) Uani 1 1 d . . . H15A H 0.3223 0.5779 0.4160 0.044 Uiso 1 1 calc R . . H15B H 0.3014 0.4554 0.4459 0.044 Uiso 1 1 calc R . . H15C H 0.2244 0.5157 0.3879 0.044 Uiso 1 1 calc R . . C16 C 0.22090(14) 0.53001(17) 0.25578(10) 0.0259(4) Uani 1 1 d . . . H16A H 0.2498 0.6063 0.2518 0.039 Uiso 1 1 calc R . . H16B H 0.1765 0.5424 0.2785 0.039 Uiso 1 1 calc R . . H16C H 0.1896 0.4981 0.2134 0.039 Uiso 1 1 calc R . . C17 C 0.35131(14) 0.37112(19) 0.19982(9) 0.0257(4) Uani 1 1 d . . . H17A H 0.3886 0.4375 0.1930 0.039 Uiso 1 1 calc R . . H17B H 0.2888 0.3790 0.1709 0.039 Uiso 1 1 calc R . . H17C H 0.3774 0.2954 0.1917 0.039 Uiso 1 1 calc R . . C18 C 0.49890(13) 0.24714(17) 0.31470(10) 0.0250(4) Uani 1 1 d . . . H18A H 0.5493 0.3017 0.3164 0.038 Uiso 1 1 calc R . . H18B H 0.4811 0.2040 0.2742 0.038 Uiso 1 1 calc R . . H18C H 0.5186 0.1900 0.3498 0.038 Uiso 1 1 calc R . . C19 C 0.45980(14) 0.3266(2) 0.44398(9) 0.0275(4) Uani 1 1 d . . . H19A H 0.5092 0.3853 0.4585 0.041 Uiso 1 1 calc R . . H19B H 0.4860 0.2467 0.4451 0.041 Uiso 1 1 calc R . . H19C H 0.4216 0.3290 0.4719 0.041 Uiso 1 1 calc R . . C20 C 0.10800(13) 0.05782(16) 0.29534(9) 0.0213(4) Uani 1 1 d . . . H20A H 0.1288 0.0253 0.3390 0.026 Uiso 1 1 calc R . . H20B H 0.0420 0.0405 0.2764 0.026 Uiso 1 1 calc R . . C21 C 0.16166(13) 0.00101(17) 0.25559(10) 0.0235(4) Uani 1 1 d . . . H21A H 0.1281 0.0120 0.2099 0.028 Uiso 1 1 calc R . . H21B H 0.1681 -0.0857 0.2643 0.028 Uiso 1 1 calc R . . C31 C 0.04799(13) 0.26381(16) 0.21929(9) 0.0190(4) Uani 1 1 d . . . C32 C 0.08156(13) 0.30701(18) 0.17235(9) 0.0232(4) Uani 1 1 d . . . H32A H 0.1454 0.3195 0.1816 0.028 Uiso 1 1 calc R . . C33 C 0.02256(14) 0.33237(19) 0.11169(9) 0.0282(4) Uani 1 1 d . . . H33A H 0.0464 0.3621 0.0800 0.034 Uiso 1 1 calc R . . C34 C -0.07046(14) 0.31444(18) 0.09752(10) 0.0274(4) Uani 1 1 d . . . H34A H -0.1105 0.3312 0.0561 0.033 Uiso 1 1 calc R . . C35 C -0.10489(14) 0.27176(17) 0.14409(10) 0.0259(4) Uani 1 1 d . . . H35A H -0.1688 0.2593 0.1345 0.031 Uiso 1 1 calc R . . C36 C -0.04640(13) 0.24713(16) 0.20474(10) 0.0213(4) Uani 1 1 d . . . H36A H -0.0707 0.2188 0.2365 0.026 Uiso 1 1 calc R . . C41 C 0.07042(13) 0.27733(18) 0.35166(9) 0.0226(4) Uani 1 1 d . . . C42 C 0.05958(14) 0.40052(19) 0.35545(10) 0.0281(4) Uani 1 1 d . . . H42A H 0.0785 0.4516 0.3277 0.034 Uiso 1 1 calc R . . C43 C 0.02173(15) 0.4501(2) 0.39889(11) 0.0339(5) Uani 1 1 d . . . H43A H 0.0150 0.5341 0.4009 0.041 Uiso 1 1 calc R . . C44 C -0.00609(15) 0.3759(2) 0.43936(11) 0.0381(6) Uani 1 1 d . . . H44A H -0.0324 0.4089 0.4690 0.046 Uiso 1 1 calc R . . C45 C 0.00451(17) 0.2538(2) 0.43644(11) 0.0366(5) Uani 1 1 d . . . H45A H -0.0145 0.2032 0.4643 0.044 Uiso 1 1 calc R . . C46 C 0.04289(15) 0.2042(2) 0.39305(10) 0.0305(5) Uani 1 1 d . . . H46A H 0.0503 0.1202 0.3917 0.037 Uiso 1 1 calc R . . C51 C 0.29912(13) 0.06070(17) 0.19825(9) 0.0211(4) Uani 1 1 d . . . C52 C 0.23240(14) 0.09636(18) 0.14211(9) 0.0259(4) Uani 1 1 d . . . H52A H 0.1738 0.1200 0.1433 0.031 Uiso 1 1 calc R . . C53 C 0.25100(16) 0.0975(2) 0.08474(10) 0.0309(5) Uani 1 1 d . . . H53A H 0.2051 0.1212 0.0469 0.037 Uiso 1 1 calc R . . C54 C 0.33675(16) 0.06408(19) 0.08283(10) 0.0307(5) Uani 1 1 d . . . H54A H 0.3497 0.0649 0.0437 0.037 Uiso 1 1 calc R . . C55 C 0.40315(15) 0.02966(18) 0.13776(10) 0.0276(4) Uani 1 1 d . . . H55A H 0.4620 0.0073 0.1364 0.033 Uiso 1 1 calc R . . C56 C 0.38473(13) 0.02744(17) 0.19512(9) 0.0226(4) Uani 1 1 d . . . H56A H 0.4310 0.0030 0.2326 0.027 Uiso 1 1 calc R . . C61 C 0.35477(13) -0.04444(17) 0.32087(9) 0.0206(4) Uani 1 1 d . . . C62 C 0.42570(13) -0.01221(18) 0.37480(9) 0.0233(4) Uani 1 1 d . . . H62A H 0.4319 0.0686 0.3884 0.028 Uiso 1 1 calc R . . C63 C 0.48752(14) -0.09703(19) 0.40891(10) 0.0275(4) Uani 1 1 d . . . H63A H 0.5363 -0.0739 0.4453 0.033 Uiso 1 1 calc R . . C64 C 0.47808(15) -0.2150(2) 0.38984(10) 0.0302(5) Uani 1 1 d . . . H64A H 0.5199 -0.2731 0.4136 0.036 Uiso 1 1 calc R . . C65 C 0.40797(16) -0.24877(18) 0.33629(11) 0.0301(5) Uani 1 1 d . . . H65A H 0.4019 -0.3299 0.3231 0.036 Uiso 1 1 calc R . . C66 C 0.34650(14) -0.16390(18) 0.30178(9) 0.0258(4) Uani 1 1 d . . . H66A H 0.2985 -0.1872 0.2650 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01568(7) 0.01673(8) 0.01468(7) 0.00160(5) 0.00428(5) 0.00023(5) P1 0.0161(2) 0.0209(2) 0.0178(2) 0.00245(17) 0.00493(18) 0.00094(18) P2 0.0184(2) 0.0178(2) 0.0177(2) 0.00046(17) 0.00496(18) 0.00012(18) C1 0.0170(8) 0.0205(9) 0.0247(10) 0.0033(7) 0.0044(7) 0.0008(7) C2 0.0207(9) 0.0305(10) 0.0210(9) 0.0001(8) 0.0043(7) -0.0016(8) C3 0.0215(9) 0.0256(10) 0.0173(9) 0.0021(7) 0.0008(7) -0.0038(8) C4 0.0223(9) 0.0330(11) 0.0249(10) 0.0032(8) 0.0073(8) 0.0025(8) C5 0.0216(9) 0.0267(11) 0.0315(11) 0.0067(8) 0.0053(8) 0.0051(8) C6 0.0247(10) 0.0271(10) 0.0210(10) 0.0044(8) 0.0024(8) -0.0016(8) C7 0.0323(11) 0.0291(10) 0.0180(9) -0.0010(8) 0.0084(8) -0.0024(9) C8 0.0321(11) 0.0229(10) 0.0206(9) 0.0003(7) 0.0066(8) 0.0007(8) C9 0.0347(12) 0.0354(12) 0.0326(12) 0.0133(9) 0.0118(10) 0.0025(10) C10 0.0257(9) 0.0171(9) 0.0199(9) -0.0014(7) 0.0062(7) -0.0033(7) C11 0.0223(9) 0.0148(8) 0.0227(9) 0.0032(7) 0.0087(7) -0.0019(7) C12 0.0215(9) 0.0179(9) 0.0198(9) 0.0018(7) 0.0063(7) -0.0039(7) C13 0.0165(8) 0.0219(9) 0.0232(9) -0.0007(7) 0.0058(7) -0.0044(7) C14 0.0188(9) 0.0237(9) 0.0191(9) -0.0004(7) 0.0027(7) -0.0048(7) C15 0.0343(11) 0.0314(11) 0.0224(10) -0.0046(8) 0.0081(9) 0.0016(9) C16 0.0313(11) 0.0198(9) 0.0250(10) 0.0026(8) 0.0068(8) 0.0023(8) C17 0.0299(10) 0.0277(10) 0.0211(10) 0.0011(8) 0.0102(8) -0.0028(8) C18 0.0180(8) 0.0279(10) 0.0296(10) -0.0008(8) 0.0081(8) -0.0009(8) C19 0.0247(10) 0.0327(11) 0.0203(10) 0.0000(8) 0.0003(8) -0.0016(8) C20 0.0200(9) 0.0197(9) 0.0239(9) 0.0023(7) 0.0065(7) -0.0012(7) C21 0.0207(9) 0.0207(9) 0.0280(10) -0.0021(8) 0.0061(8) -0.0041(7) C31 0.0181(8) 0.0189(9) 0.0181(9) -0.0007(7) 0.0028(7) 0.0014(7) C32 0.0212(9) 0.0253(10) 0.0219(10) 0.0003(7) 0.0052(7) 0.0001(8) C33 0.0311(11) 0.0313(11) 0.0208(10) 0.0030(8) 0.0062(8) -0.0001(9) C34 0.0288(10) 0.0260(10) 0.0213(10) -0.0007(8) -0.0010(8) 0.0017(8) C35 0.0199(9) 0.0256(10) 0.0280(11) -0.0029(8) 0.0015(8) 0.0006(8) C36 0.0184(8) 0.0206(9) 0.0247(9) 0.0002(7) 0.0066(7) 0.0007(7) C41 0.0159(8) 0.0304(10) 0.0204(9) 0.0003(7) 0.0042(7) 0.0010(7) C42 0.0268(10) 0.0315(11) 0.0255(10) -0.0011(8) 0.0076(8) 0.0038(9) C43 0.0290(11) 0.0380(12) 0.0330(12) -0.0092(9) 0.0075(9) 0.0051(9) C44 0.0285(11) 0.0581(16) 0.0294(12) -0.0123(11) 0.0114(9) 0.0012(11) C45 0.0361(12) 0.0508(15) 0.0282(12) 0.0012(10) 0.0176(10) -0.0010(11) C46 0.0310(11) 0.0350(11) 0.0280(11) 0.0020(9) 0.0130(9) 0.0012(9) C51 0.0240(9) 0.0190(9) 0.0192(9) -0.0013(7) 0.0053(7) -0.0006(7) C52 0.0265(10) 0.0252(10) 0.0232(10) 0.0004(8) 0.0040(8) 0.0012(8) C53 0.0376(12) 0.0328(11) 0.0188(10) 0.0008(8) 0.0039(9) -0.0013(9) C54 0.0402(12) 0.0331(11) 0.0221(10) -0.0023(8) 0.0144(9) -0.0059(10) C55 0.0309(11) 0.0261(10) 0.0298(11) -0.0033(8) 0.0152(9) -0.0031(8) C56 0.0247(9) 0.0201(9) 0.0228(9) -0.0003(7) 0.0073(8) -0.0005(7) C61 0.0233(9) 0.0204(9) 0.0194(9) 0.0027(7) 0.0084(7) 0.0022(7) C62 0.0239(9) 0.0229(10) 0.0239(10) 0.0007(7) 0.0087(8) 0.0025(8) C63 0.0232(10) 0.0357(11) 0.0224(10) 0.0019(8) 0.0054(8) 0.0058(9) C64 0.0341(11) 0.0311(11) 0.0253(11) 0.0065(8) 0.0090(9) 0.0137(9) C65 0.0389(12) 0.0209(10) 0.0292(11) 0.0005(8) 0.0091(9) 0.0047(9) C66 0.0308(10) 0.0218(10) 0.0225(10) 0.0004(8) 0.0053(8) 0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 2.0205(19) . yes Ru1 C10 2.2344(18) . yes Ru1 C14 2.2389(18) . yes Ru1 C13 2.2567(18) . yes Ru1 C11 2.2585(18) . yes Ru1 P2 2.2622(5) . yes Ru1 P1 2.2621(5) . yes Ru1 C12 2.2726(18) . yes P1 C41 1.832(2) . yes P1 C31 1.8402(19) . yes P1 C20 1.8459(19) . yes P2 C61 1.8374(19) . yes P2 C51 1.8379(19) . yes P2 C21 1.8560(19) . yes C1 C2 1.211(3) . yes C2 C3 1.437(3) . yes C3 C8 1.401(3) . yes C3 C4 1.404(3) . yes C4 C5 1.387(3) . yes C4 H4A 0.9500 . ? C5 C6 1.387(3) . yes C5 H5A 0.9500 . ? C6 C7 1.397(3) . yes C6 C9 1.502(3) . yes C7 C8 1.388(3) . yes C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C14 1.430(3) . yes C10 C11 1.454(3) . yes C10 C15 1.499(3) . yes C11 C12 1.413(3) . yes C11 C16 1.500(3) . yes C12 C13 1.454(3) . yes C12 C17 1.504(3) . yes C13 C14 1.428(3) . yes C13 C18 1.501(3) . yes C14 C19 1.506(3) . yes C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.525(3) . yes C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C31 C32 1.388(3) . yes C31 C36 1.400(3) . yes C32 C33 1.396(3) . yes C32 H32A 0.9500 . ? C33 C34 1.382(3) . yes C33 H33A 0.9500 . ? C34 C35 1.387(3) . yes C34 H34A 0.9500 . ? C35 C36 1.391(3) . yes C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.393(3) . yes C41 C42 1.396(3) . yes C42 C43 1.390(3) . yes C42 H42A 0.9500 . ? C43 C44 1.387(3) . yes C43 H43A 0.9500 . ? C44 C45 1.382(3) . yes C44 H44A 0.9500 . ? C45 C46 1.394(3) . yes C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C51 C56 1.394(3) . yes C51 C52 1.401(3) . yes C52 C53 1.390(3) . yes C52 H52A 0.9500 . ? C53 C54 1.387(3) . yes C53 H53A 0.9500 . ? C54 C55 1.377(3) . yes C54 H54A 0.9500 . ? C55 C56 1.388(3) . yes C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.391(3) . yes C61 C66 1.398(3) . yes C62 C63 1.389(3) . yes C62 H62A 0.9500 . ? C63 C64 1.382(3) . yes C63 H63A 0.9500 . ? C64 C65 1.384(3) . yes C64 H64A 0.9500 . ? C65 C66 1.390(3) . yes C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C10 101.60(7) . . yes C1 Ru1 C14 91.24(7) . . yes C10 Ru1 C14 37.29(7) . . yes C1 Ru1 C13 115.94(7) . . yes C10 Ru1 C13 62.41(7) . . yes C14 Ru1 C13 37.04(7) . . yes C1 Ru1 C11 138.14(7) . . yes C10 Ru1 C11 37.75(7) . . yes C14 Ru1 C11 62.13(7) . . yes C13 Ru1 C11 61.98(7) . . yes C1 Ru1 P2 85.20(6) . . yes C10 Ru1 P2 163.03(5) . . yes C14 Ru1 P2 128.14(5) . . yes C13 Ru1 P2 100.63(5) . . yes C11 Ru1 P2 136.49(5) . . yes C1 Ru1 P1 79.22(5) . . yes C10 Ru1 P1 113.25(5) . . yes C14 Ru1 P1 146.72(5) . . yes C13 Ru1 P1 164.50(5) . . yes C11 Ru1 P1 104.98(5) . . yes P2 Ru1 P1 83.154(18) . . yes C1 Ru1 C12 152.15(7) . . yes C10 Ru1 C12 62.06(7) . . yes C14 Ru1 C12 61.87(7) . . yes C13 Ru1 C12 37.45(7) . . yes C11 Ru1 C12 36.34(7) . . yes P2 Ru1 C12 105.15(5) . . yes P1 Ru1 C12 127.06(5) . . yes C41 P1 C31 101.86(9) . . yes C41 P1 C20 104.02(9) . . yes C31 P1 C20 100.65(8) . . yes C41 P1 Ru1 118.68(6) . . yes C31 P1 Ru1 120.80(6) . . yes C20 P1 Ru1 108.31(6) . . yes C61 P2 C51 101.12(8) . . yes C61 P2 C21 104.28(9) . . yes C51 P2 C21 102.06(9) . . yes C61 P2 Ru1 117.52(6) . . yes C51 P2 Ru1 118.40(6) . . yes C21 P2 Ru1 111.42(7) . . yes C2 C1 Ru1 175.52(18) . . yes C1 C2 C3 171.9(2) . . yes C8 C3 C4 117.35(18) . . yes C8 C3 C2 121.80(19) . . yes C4 C3 C2 120.78(18) . . yes C5 C4 C3 121.02(19) . . yes C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 121.68(19) . . yes C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C7 117.43(18) . . yes C5 C6 C9 121.27(19) . . yes C7 C6 C9 121.30(19) . . yes C8 C7 C6 121.55(19) . . yes C8 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? C7 C8 C3 120.94(19) . . yes C7 C8 H8A 119.5 . . ? C3 C8 H8A 119.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C11 107.17(16) . . yes C14 C10 C15 125.67(17) . . yes C11 C10 C15 126.69(17) . . yes C14 C10 Ru1 71.52(10) . . yes C11 C10 Ru1 72.02(10) . . yes C15 C10 Ru1 127.89(14) . . yes C12 C11 C10 108.29(16) . . yes C12 C11 C16 126.85(17) . . yes C10 C11 C16 124.17(17) . . yes C12 C11 Ru1 72.37(10) . . yes C10 C11 Ru1 70.22(10) . . yes C16 C11 Ru1 130.51(13) . . yes C11 C12 C13 108.35(16) . . yes C11 C12 C17 126.75(17) . . yes C13 C12 C17 124.24(17) . . yes C11 C12 Ru1 71.29(10) . . yes C13 C12 Ru1 70.69(10) . . yes C17 C12 Ru1 131.07(13) . . yes C14 C13 C12 107.18(16) . . yes C14 C13 C18 127.57(17) . . yes C12 C13 C18 124.69(17) . . yes C14 C13 Ru1 70.80(10) . . yes C12 C13 Ru1 71.87(10) . . yes C18 C13 Ru1 129.24(13) . . yes C13 C14 C10 109.01(16) . . yes C13 C14 C19 126.28(18) . . yes C10 C14 C19 124.65(17) . . yes C13 C14 Ru1 72.16(10) . . yes C10 C14 Ru1 71.19(10) . . yes C19 C14 Ru1 125.14(13) . . yes C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 P1 107.69(13) . . yes C21 C20 H20A 110.2 . . ? P1 C20 H20A 110.2 . . ? C21 C20 H20B 110.2 . . ? P1 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C20 C21 P2 110.21(13) . . yes C20 C21 H21A 109.6 . . ? P2 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? P2 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C32 C31 C36 118.63(17) . . yes C32 C31 P1 119.69(14) . . yes C36 C31 P1 121.55(15) . . yes C31 C32 C33 120.73(18) . . yes C31 C32 H32A 119.6 . . ? C33 C32 H32A 119.6 . . ? C34 C33 C32 120.28(19) . . yes C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C35 119.54(19) . . yes C33 C34 H34A 120.2 . . ? C35 C34 H34A 120.2 . . ? C34 C35 C36 120.38(19) . . yes C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 C31 120.43(19) . . yes C35 C36 H36A 119.8 . . ? C31 C36 H36A 119.8 . . ? C46 C41 C42 118.4(2) . . yes C46 C41 P1 123.00(16) . . yes C42 C41 P1 118.48(16) . . yes C43 C42 C41 121.4(2) . . yes C43 C42 H42A 119.3 . . ? C41 C42 H42A 119.3 . . ? C44 C43 C42 119.5(2) . . yes C44 C43 H43A 120.3 . . ? C42 C43 H43A 120.3 . . ? C45 C44 C43 119.9(2) . . yes C45 C44 H44A 120.1 . . ? C43 C44 H44A 120.1 . . ? C44 C45 C46 120.6(2) . . yes C44 C45 H45A 119.7 . . ? C46 C45 H45A 119.7 . . ? C41 C46 C45 120.3(2) . . yes C41 C46 H46A 119.9 . . ? C45 C46 H46A 119.9 . . ? C56 C51 C52 118.27(18) . . yes C56 C51 P2 121.21(14) . . yes C52 C51 P2 120.31(15) . . yes C53 C52 C51 120.8(2) . . yes C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C54 C53 C52 119.89(19) . . yes C54 C53 H53A 120.1 . . ? C52 C53 H53A 120.1 . . ? C55 C54 C53 119.90(19) . . yes C55 C54 H54A 120.1 . . ? C53 C54 H54A 120.1 . . ? C54 C55 C56 120.5(2) . . yes C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C55 C56 C51 120.70(19) . . yes C55 C56 H56A 119.7 . . ? C51 C56 H56A 119.7 . . ? C62 C61 C66 118.78(17) . . yes C62 C61 P2 119.90(14) . . yes C66 C61 P2 121.29(15) . . yes C63 C62 C61 120.65(19) . . yes C63 C62 H62A 119.7 . . ? C61 C62 H62A 119.7 . . ? C64 C63 C62 119.97(19) . . yes C64 C63 H63A 120.0 . . ? C62 C63 H63A 120.0 . . ? C63 C64 C65 120.21(19) . . yes C63 C64 H64A 119.9 . . ? C65 C64 H64A 119.9 . . ? C64 C65 C66 119.91(19) . . yes C64 C65 H65A 120.0 . . ? C66 C65 H65A 120.0 . . ? C65 C66 C61 120.47(19) . . yes C65 C66 H66A 119.8 . . ? C61 C66 H66A 119.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.856 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.097 #===END #3. data data_5b _database_code_depnum_ccdc_archive 'CCDC 691299' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H37 Ir O3 P2, C H Cl3' _chemical_formula_sum 'C47 H38 Cl3 Ir O3 P2' _chemical_formula_weight 1011.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7735(3) _cell_length_b 19.5550(4) _cell_length_c 22.3273(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.18(2) _cell_angle_gamma 90.00 _cell_volume 4212.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10809 _cell_measurement_theta_min 1.3920 _cell_measurement_theta_max 30.5069 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 3.477 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; NUMABS (Rigaku Inc., 2007) ; _exptl_absorpt_correction_T_min 0.7126 _exptl_absorpt_correction_T_max 0.9069 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'R-AXIS SPIDER' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 10.0000 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37675 _diffrn_reflns_av_R_equivalents 0.1162 _diffrn_reflns_av_sigmaI/netI 0.1106 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9167 _reflns_number_gt 5583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0100P)^2^+15.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9167 _refine_ls_number_parameters 392 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.76450(3) 0.74950(2) 0.242558(15) 0.02958(11) Uani 1 1 d . . . P1 P 0.6797(2) 0.64967(11) 0.28240(11) 0.0286(5) Uani 1 1 d . . . P2 P 0.8355(2) 0.85393(11) 0.20550(11) 0.0319(5) Uani 1 1 d . . . O1 O 0.9746(8) 0.6692(4) 0.1890(4) 0.067(2) Uani 1 1 d . . . C1 C 0.8951(10) 0.6998(4) 0.2099(5) 0.042(3) Uani 1 1 d . . . O2 O 0.5829(7) 0.7985(3) 0.2464(3) 0.0462(17) Uani 1 1 d . . . O3 O 0.5744(7) 0.7564(3) 0.1901(3) 0.0494(17) Uani 1 1 d . . . C4 C 0.8913(9) 0.7702(4) 0.3205(5) 0.029(2) Uani 1 1 d . A . C5 C 0.9644(10) 0.7850(4) 0.3663(5) 0.037(2) Uani 1 1 d . . . C6A C 1.0692(16) 0.7985(8) 0.4197(6) 0.018(7) Uiso 0.50 1 d PG A 1 C7A C 1.1191(19) 0.8646(7) 0.4306(8) 0.039(8) Uiso 0.50 1 d PG A 1 H7AA H 1.0887 0.9001 0.4025 0.046 Uiso 0.50 1 calc PR A 1 C8A C 1.213(2) 0.8789(6) 0.4826(9) 0.056(9) Uiso 0.50 1 d PG A 1 H8AA H 1.2474 0.9241 0.4900 0.068 Uiso 0.50 1 calc PR A 1 C9A C 1.2577(18) 0.8270(8) 0.5236(7) 0.051(11) Uiso 0.50 1 d PG A 1 C10A C 1.2078(15) 0.7608(7) 0.5127(6) 0.029(4) Uiso 0.50 1 d PG A 1 H10A H 1.2382 0.7253 0.5408 0.035 Uiso 0.50 1 calc PR A 1 C11A C 1.1136(13) 0.7466(6) 0.4607(6) 0.029(4) Uiso 0.50 1 d PG A 1 H11A H 1.0795 0.7014 0.4533 0.035 Uiso 0.50 1 calc PR A 1 C12A C 1.373(2) 0.8388(10) 0.5742(10) 0.047(6) Uiso 0.50 1 d P A 1 H12A H 1.3866 0.7977 0.5997 0.071 Uiso 0.50 1 calc PR A 1 H12B H 1.3502 0.8776 0.5986 0.071 Uiso 0.50 1 calc PR A 1 H12C H 1.4579 0.8488 0.5579 0.071 Uiso 0.50 1 calc PR A 1 C6B C 1.058(2) 0.8016(11) 0.4234(8) 0.058(14) Uiso 0.50 1 d PG A 2 C7B C 1.143(2) 0.8591(9) 0.4295(9) 0.057(10) Uiso 0.50 1 d PG A 2 H7BA H 1.1365 0.8917 0.3976 0.068 Uiso 0.50 1 calc PR A 2 C8B C 1.238(2) 0.8688(8) 0.4821(10) 0.039(6) Uiso 0.50 1 d PG A 2 H8BA H 1.2963 0.9080 0.4863 0.046 Uiso 0.50 1 calc PR A 2 C9B C 1.248(2) 0.8211(10) 0.5288(8) 0.067(14) Uiso 0.50 1 d PG A 2 C10B C 1.163(2) 0.7637(9) 0.5228(7) 0.081(9) Uiso 0.50 1 d PG A 2 H10B H 1.1703 0.7311 0.5546 0.097 Uiso 0.50 1 calc PR A 2 C11B C 1.0685(17) 0.7539(8) 0.4701(9) 0.054(6) Uiso 0.50 1 d PG A 2 H11B H 1.0105 0.7147 0.4660 0.064 Uiso 0.50 1 calc PR A 2 C12B C 1.328(3) 0.8331(12) 0.5935(11) 0.061(7) Uiso 0.50 1 d P A 2 H12D H 1.3817 0.8756 0.5942 0.091 Uiso 0.50 1 calc PR A 2 H12E H 1.3913 0.7947 0.6051 0.091 Uiso 0.50 1 calc PR A 2 H12F H 1.2622 0.8367 0.6221 0.091 Uiso 0.50 1 calc PR A 2 C21 C 0.7925(5) 0.6152(3) 0.3487(2) 0.030(2) Uani 1 1 d G . . C22 C 0.7529(5) 0.6115(3) 0.4057(3) 0.041(2) Uani 1 1 d G . . H22A H 0.6624 0.6254 0.4110 0.049 Uiso 1 1 calc R . . C23 C 0.8457(7) 0.5877(3) 0.4550(2) 0.042(2) Uani 1 1 d G . . H23A H 0.8187 0.5852 0.4939 0.051 Uiso 1 1 calc R . . C24 C 0.9781(6) 0.5675(3) 0.4472(2) 0.043(3) Uani 1 1 d G . . H24A H 1.0416 0.5512 0.4809 0.052 Uiso 1 1 calc R . . C25 C 1.0177(5) 0.5711(3) 0.3902(3) 0.045(3) Uani 1 1 d G . . H25A H 1.1082 0.5573 0.3849 0.054 Uiso 1 1 calc R . . C26 C 0.9249(6) 0.5949(3) 0.3409(2) 0.033(2) Uani 1 1 d G . . H26A H 0.9519 0.5974 0.3020 0.040 Uiso 1 1 calc R . . C41 C 0.6573(6) 0.5771(2) 0.2307(3) 0.034(2) Uani 1 1 d G . . C42 C 0.6531(6) 0.5107(3) 0.2526(2) 0.041(2) Uani 1 1 d G . . H42A H 0.6617 0.5029 0.2951 0.049 Uiso 1 1 calc R . . C43 C 0.6364(7) 0.4559(2) 0.2125(3) 0.051(3) Uani 1 1 d G . . H43A H 0.6335 0.4106 0.2275 0.061 Uiso 1 1 calc R . . C44 C 0.6239(7) 0.4674(3) 0.1504(3) 0.054(3) Uani 1 1 d G . . H44A H 0.6124 0.4300 0.1230 0.065 Uiso 1 1 calc R . . C45 C 0.6281(7) 0.5338(3) 0.1285(2) 0.054(3) Uani 1 1 d G . . H45A H 0.6195 0.5417 0.0861 0.065 Uiso 1 1 calc R . . C46 C 0.6448(6) 0.5886(2) 0.1686(3) 0.042(3) Uani 1 1 d G . . H46A H 0.6477 0.6340 0.1536 0.051 Uiso 1 1 calc R . . C31 C 0.5112(4) 0.6630(3) 0.3043(3) 0.028(2) Uani 1 1 d G . . C32 C 0.3970(5) 0.6247(2) 0.2785(2) 0.032(2) Uani 1 1 d G . . H32A H 0.4073 0.5899 0.2498 0.038 Uiso 1 1 calc R . . C33 C 0.2678(4) 0.6373(3) 0.2946(3) 0.038(2) Uani 1 1 d G . . H33A H 0.1897 0.6112 0.2770 0.045 Uiso 1 1 calc R . . C34 C 0.2527(5) 0.6882(3) 0.3366(3) 0.042(2) Uani 1 1 d G . . H34A H 0.1644 0.6969 0.3476 0.050 Uiso 1 1 calc R . . C35 C 0.3669(6) 0.7265(3) 0.3623(3) 0.047(3) Uani 1 1 d G . . H35A H 0.3566 0.7613 0.3910 0.056 Uiso 1 1 calc R . . C36 C 0.4962(5) 0.7139(3) 0.3462(3) 0.037(2) Uani 1 1 d G . . H36A H 0.5742 0.7400 0.3638 0.045 Uiso 1 1 calc R . . C51 C 0.8502(6) 0.9222(3) 0.2616(2) 0.032(2) Uani 1 1 d G . . C52 C 0.7401(5) 0.9352(3) 0.2924(3) 0.044(3) Uani 1 1 d G . . H52A H 0.6574 0.9091 0.2836 0.053 Uiso 1 1 calc R . . C53 C 0.7510(6) 0.9865(3) 0.3360(3) 0.044(3) Uani 1 1 d G . . H53A H 0.6757 0.9954 0.3570 0.053 Uiso 1 1 calc R . . C54 C 0.8720(7) 1.0247(3) 0.3489(3) 0.053(3) Uani 1 1 d G . . H54A H 0.8795 1.0597 0.3787 0.064 Uiso 1 1 calc R . . C55 C 0.9822(5) 1.0117(3) 0.3181(3) 0.054(3) Uani 1 1 d G . . H55A H 1.0649 1.0378 0.3269 0.065 Uiso 1 1 calc R . . C56 C 0.9713(5) 0.9604(3) 0.2744(3) 0.038(2) Uani 1 1 d G . . H56A H 1.0466 0.9515 0.2534 0.046 Uiso 1 1 calc R . . C61 C 1.0060(5) 0.8513(3) 0.1817(3) 0.034(2) Uani 1 1 d G . . C62 C 1.1102(6) 0.8125(3) 0.2153(2) 0.041(2) Uani 1 1 d G . . H62A H 1.0908 0.7859 0.2486 0.049 Uiso 1 1 calc R . . C63 C 1.2428(5) 0.8125(3) 0.2002(3) 0.039(2) Uani 1 1 d G . . H63A H 1.3139 0.7859 0.2231 0.046 Uiso 1 1 calc R . . C64 C 1.2712(5) 0.8513(3) 0.1515(3) 0.043(2) Uani 1 1 d G . . H64A H 1.3618 0.8513 0.1412 0.052 Uiso 1 1 calc R . . C65 C 1.1670(6) 0.8902(3) 0.1179(2) 0.045(3) Uani 1 1 d G . . H65A H 1.1865 0.9167 0.0846 0.055 Uiso 1 1 calc R . . C66 C 1.0345(5) 0.8902(3) 0.1330(3) 0.038(2) Uani 1 1 d G . . H66A H 0.9633 0.9167 0.1101 0.046 Uiso 1 1 calc R . . C71 C 0.7115(5) 0.8844(3) 0.1409(3) 0.036(2) Uani 1 1 d G . . C72 C 0.6532(7) 0.9493(3) 0.1398(3) 0.046(3) Uani 1 1 d G . . H72A H 0.6830 0.9806 0.1717 0.055 Uiso 1 1 calc R . . C73 C 0.5512(7) 0.9683(3) 0.0919(3) 0.056(3) Uani 1 1 d G . . H73A H 0.5114 1.0127 0.0912 0.067 Uiso 1 1 calc R . . C74 C 0.5076(6) 0.9224(4) 0.0452(3) 0.060(3) Uani 1 1 d G . . H74A H 0.4379 0.9354 0.0126 0.072 Uiso 1 1 calc R . . C75 C 0.5659(7) 0.8575(4) 0.0464(3) 0.054(3) Uani 1 1 d G . . H75A H 0.5361 0.8261 0.0145 0.065 Uiso 1 1 calc R . . C76 C 0.6678(6) 0.8385(2) 0.0942(3) 0.048(3) Uani 1 1 d G . . H76A H 0.7077 0.7941 0.0950 0.058 Uiso 1 1 calc R . . C1S C 0.2183(12) 0.3638(4) 0.0206(4) 0.081(4) Uiso 1 1 d D . . H1SA H 0.1837 0.3481 0.0551 0.097 Uiso 1 1 d . . . Cl1A Cl 0.1702(7) 0.4499(3) 0.0049(3) 0.096(2) Uiso 0.60 1 d PD B 1 Cl2A Cl 0.3918(7) 0.3474(4) 0.0284(3) 0.102(2) Uiso 0.60 1 d P B 1 Cl3A Cl 0.1401(7) 0.3234(3) -0.0490(3) 0.104(2) Uiso 0.60 1 d PD B 1 Cl1B Cl 0.1126(13) 0.4229(6) -0.0203(6) 0.132(3) Uiso 0.40 1 d PD B 2 Cl2B Cl 0.3903(14) 0.3932(7) 0.0467(6) 0.132(3) Uiso 0.40 1 d P B 2 Cl3B Cl 0.2366(13) 0.2818(5) -0.0076(6) 0.132(3) Uiso 0.40 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02459(18) 0.02877(18) 0.03493(19) 0.00425(18) 0.00340(13) -0.00057(17) P1 0.0254(12) 0.0278(11) 0.0329(13) 0.0042(10) 0.0051(10) -0.0004(10) P2 0.0267(12) 0.0314(12) 0.0371(14) 0.0070(11) 0.0041(11) -0.0013(10) O1 0.063(6) 0.057(5) 0.083(6) -0.009(4) 0.017(5) -0.009(4) C1 0.043(6) 0.021(4) 0.066(8) -0.003(5) 0.023(6) -0.009(4) O2 0.051(4) 0.040(4) 0.048(4) -0.002(3) 0.007(4) -0.008(3) O3 0.046(4) 0.050(4) 0.053(4) 0.005(4) 0.008(3) 0.011(4) C4 0.020(4) 0.015(4) 0.051(6) 0.003(4) 0.002(4) 0.000(3) C5 0.034(6) 0.031(5) 0.046(6) 0.010(4) 0.010(5) 0.008(4) C21 0.034(5) 0.020(4) 0.035(5) 0.006(4) 0.005(4) -0.002(4) C22 0.039(6) 0.043(5) 0.040(6) 0.006(5) 0.005(5) -0.006(5) C23 0.050(7) 0.039(5) 0.035(6) -0.005(4) -0.002(5) 0.002(5) C24 0.061(7) 0.018(4) 0.043(6) 0.007(4) -0.016(5) -0.007(4) C25 0.039(6) 0.031(5) 0.063(8) 0.012(5) 0.002(6) -0.003(4) C26 0.035(5) 0.029(5) 0.035(5) 0.013(4) 0.005(4) 0.000(4) C41 0.022(5) 0.034(5) 0.047(6) -0.007(4) 0.011(4) 0.000(4) C42 0.032(5) 0.040(5) 0.048(6) -0.006(5) -0.001(5) 0.005(4) C43 0.041(6) 0.033(5) 0.078(9) -0.014(5) 0.008(6) 0.011(5) C44 0.049(7) 0.056(7) 0.056(8) -0.025(6) 0.009(6) 0.007(5) C45 0.042(7) 0.070(8) 0.051(7) -0.008(6) 0.011(6) -0.007(6) C46 0.042(6) 0.034(5) 0.053(7) -0.017(5) 0.017(5) -0.012(4) C31 0.032(5) 0.024(4) 0.031(5) 0.002(4) 0.010(4) 0.001(4) C32 0.025(5) 0.032(5) 0.039(6) 0.001(4) 0.008(4) -0.005(4) C33 0.021(5) 0.041(5) 0.052(6) 0.001(5) 0.006(4) -0.002(4) C34 0.028(5) 0.044(6) 0.056(7) 0.005(5) 0.015(5) 0.005(4) C35 0.048(7) 0.035(5) 0.059(7) -0.005(5) 0.014(6) 0.002(5) C36 0.019(5) 0.039(5) 0.054(7) 0.003(5) 0.009(4) -0.004(4) C51 0.029(5) 0.033(5) 0.034(5) 0.005(4) 0.005(4) -0.006(4) C52 0.034(6) 0.045(6) 0.055(7) -0.006(5) 0.010(5) -0.011(5) C53 0.037(6) 0.040(5) 0.056(7) -0.005(5) 0.008(5) 0.000(5) C54 0.057(7) 0.049(6) 0.051(7) -0.009(5) -0.001(6) -0.003(5) C55 0.042(7) 0.048(6) 0.070(8) -0.005(6) 0.003(6) -0.013(5) C56 0.031(5) 0.041(5) 0.045(6) -0.005(5) 0.015(5) 0.001(4) C61 0.033(5) 0.028(5) 0.043(6) -0.004(4) 0.007(5) -0.004(4) C62 0.038(6) 0.036(5) 0.050(6) 0.013(5) 0.013(5) 0.001(4) C63 0.034(5) 0.049(6) 0.031(5) -0.001(5) 0.001(4) -0.003(5) C64 0.034(6) 0.044(5) 0.056(7) -0.002(5) 0.022(5) 0.003(5) C65 0.051(7) 0.048(6) 0.043(6) 0.005(5) 0.025(5) 0.002(5) C66 0.038(6) 0.038(5) 0.038(6) 0.012(4) 0.004(5) -0.004(4) C71 0.021(5) 0.043(5) 0.043(6) 0.021(5) 0.002(4) 0.000(4) C72 0.045(6) 0.037(5) 0.052(7) 0.014(5) -0.001(5) 0.010(5) C73 0.048(7) 0.052(7) 0.068(8) 0.037(6) 0.011(6) 0.021(6) C74 0.028(6) 0.091(9) 0.060(8) 0.045(7) 0.003(6) 0.003(6) C75 0.035(6) 0.080(8) 0.047(7) 0.018(6) 0.004(5) -0.008(6) C76 0.046(6) 0.049(6) 0.048(7) 0.007(5) 0.005(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.844(10) . yes Ir1 C4 2.011(10) . yes Ir1 O2 2.030(7) . yes Ir1 O3 2.036(7) . yes Ir1 P2 2.350(2) . yes Ir1 P1 2.351(2) . yes P1 C31 1.809(4) . yes P1 C41 1.820(5) . yes P1 C21 1.828(5) . yes P2 C51 1.821(5) . yes P2 C71 1.829(5) . yes P2 C61 1.829(5) . yes O1 C1 1.139(10) . yes O2 O3 1.492(9) . yes C4 C5 1.186(12) . yes C5 C6A 1.466(16) . yes C5 C6B 1.484(18) . yes C6A C7A 1.3900 . yes C6A C11A 1.3900 . yes C7A C8A 1.3900 . yes C7A H7AA 0.9500 . ? C8A C9A 1.3900 . yes C8A H8AA 0.9500 . ? C9A C10A 1.3900 . yes C9A C12A 1.48(2) . yes C10A C11A 1.3900 . yes C10A H10A 0.9500 . ? C11A H11A 0.9500 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C6B C7B 1.3900 . yes C6B C11B 1.3900 . yes C7B C8B 1.3900 . yes C7B H7BA 0.9500 . ? C8B C9B 1.3900 . yes C8B H8BA 0.9500 . ? C9B C10B 1.3900 . yes C9B C12B 1.55(3) . yes C10B C11B 1.3900 . yes C10B H10B 0.9500 . ? C11B H11B 0.9500 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C21 C22 1.3900 . yes C21 C26 1.3900 . yes C22 C23 1.3900 . yes C22 H22A 0.9500 . ? C23 C24 1.3900 . yes C23 H23A 0.9500 . ? C24 C25 1.3900 . yes C24 H24A 0.9500 . ? C25 C26 1.3900 . yes C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C41 C42 1.3900 . yes C41 C46 1.3900 . yes C42 C43 1.3900 . yes C42 H42A 0.9500 . ? C43 C44 1.3900 . yes C43 H43A 0.9500 . ? C44 C45 1.3900 . yes C44 H44A 0.9500 . ? C45 C46 1.3900 . yes C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C31 C32 1.3900 . yes C31 C36 1.3900 . yes C32 C33 1.3900 . yes C32 H32A 0.9500 . ? C33 C34 1.3900 . yes C33 H33A 0.9500 . ? C34 C35 1.3900 . yes C34 H34A 0.9500 . ? C35 C36 1.3900 . yes C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C51 C52 1.3900 . yes C51 C56 1.3900 . yes C52 C53 1.3900 . yes C52 H52A 0.9500 . ? C53 C54 1.3900 . yes C53 H53A 0.9500 . ? C54 C55 1.3900 . yes C54 H54A 0.9500 . ? C55 C56 1.3900 . yes C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C61 C62 1.3900 . yes C61 C66 1.3900 . yes C62 C63 1.3900 . yes C62 H62A 0.9500 . ? C63 C64 1.3900 . yes C63 H63A 0.9500 . ? C64 C65 1.3900 . yes C64 H64A 0.9500 . ? C65 C66 1.3900 . yes C65 H65A 0.9500 . ? C66 H66A 0.9500 . ? C71 C72 1.3900 . yes C71 C76 1.3900 . yes C72 C73 1.3900 . yes C72 H72A 0.9500 . ? C73 C74 1.3900 . yes C73 H73A 0.9500 . ? C74 C75 1.3900 . yes C74 H74A 0.9500 . ? C75 C76 1.3900 . yes C75 H75A 0.9500 . ? C76 H76A 0.9500 . ? C1S Cl1B 1.715(9) . yes C1S Cl2A 1.707(13) . yes C1S Cl3B 1.742(6) . yes C1S Cl1A 1.768(8) . yes C1S Cl2B 1.784(17) . yes C1S Cl3A 1.802(6) . yes C1S H1SA 0.9411 . ? 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 C1 Ir1 C4 94.5(4) . . yes C1 Ir1 O2 158.4(4) . . yes C4 Ir1 O2 106.9(3) . . yes C1 Ir1 O3 115.7(4) . . yes C4 Ir1 O3 149.8(3) . . yes O2 Ir1 O3 43.1(2) . . yes C1 Ir1 P2 93.3(3) . . yes C4 Ir1 P2 87.4(2) . . yes O2 Ir1 P2 85.08(18) . . yes O3 Ir1 P2 91.95(19) . . yes C1 Ir1 P1 91.1(3) . . yes C4 Ir1 P1 92.6(2) . . yes O2 Ir1 P1 90.71(18) . . yes O3 Ir1 P1 85.85(19) . . yes P2 Ir1 P1 175.58(8) . . yes C31 P1 C41 105.1(3) . . yes C31 P1 C21 107.0(3) . . yes C41 P1 C21 102.8(3) . . yes C31 P1 Ir1 111.9(2) . . yes C41 P1 Ir1 114.9(2) . . yes C21 P1 Ir1 114.2(2) . . yes C51 P2 C71 105.9(3) . . yes C51 P2 C61 104.1(3) . . yes C71 P2 C61 107.5(3) . . yes C51 P2 Ir1 113.0(2) . . yes C71 P2 Ir1 111.4(2) . . yes C61 P2 Ir1 114.3(2) . . yes O1 C1 Ir1 179.1(11) . . yes O3 O2 Ir1 68.7(4) . . yes O2 O3 Ir1 68.3(4) . . yes C5 C4 Ir1 177.4(7) . . yes C4 C5 C6A 172.5(12) . . yes C4 C5 C6B 178.3(12) . . yes C6A C5 C6B 6.1(14) . . yes C7A C6A C11A 120.0 . . yes C7A C6A C5 119.3(10) . . yes C11A C6A C5 120.6(10) . . yes C6A C7A C8A 120.0 . . yes C6A C7A H7AA 120.0 . . ? C8A C7A H7AA 120.0 . . ? C9A C8A C7A 120.0 . . yes C9A C8A H8AA 120.0 . . ? C7A C8A H8AA 120.0 . . ? C10A C9A C8A 120.0 . . yes C10A C9A C12A 118.8(13) . . yes C8A C9A C12A 120.6(13) . . yes C11A C10A C9A 120.0 . . yes C11A C10A H10A 120.0 . . ? C9A C10A H10A 120.0 . . ? C10A C11A C6A 120.0 . . yes C10A C11A H11A 120.0 . . ? C6A C11A H11A 120.0 . . ? C9A C12A H12A 109.5 . . ? C9A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C9A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C7B C6B C11B 120.0 . . yes C7B C6B C5 122.6(14) . . yes C11B C6B C5 117.2(14) . . yes C6B C7B C8B 120.0 . . yes C6B C7B H7BA 120.0 . . ? C8B C7B H7BA 120.0 . . ? C9B C8B C7B 120.0 . . yes C9B C8B H8BA 120.0 . . ? C7B C8B H8BA 120.0 . . ? C8B C9B C10B 120.0 . . yes C8B C9B C12B 124.2(16) . . yes C10B C9B C12B 114.7(16) . . yes C9B C10B C11B 120.0 . . yes C9B C10B H10B 120.0 . . ? C11B C10B H10B 120.0 . . ? C10B C11B C6B 120.0 . . yes C10B C11B H11B 120.0 . . ? C6B C11B H11B 120.0 . . ? C9B C12B H12D 109.5 . . ? C9B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C9B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C22 C21 C26 120.0 . . yes C22 C21 P1 122.7(3) . . yes C26 C21 P1 117.2(3) . . yes C23 C22 C21 120.0 . . yes C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.0 . . yes C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.0 . . yes C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C26 C25 C24 120.0 . . yes C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C21 120.0 . . yes C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? C42 C41 C46 120.0 . . yes C42 C41 P1 120.8(4) . . yes C46 C41 P1 119.2(4) . . yes C43 C42 C41 120.0 . . yes C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.0 . . yes C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C43 120.0 . . yes C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C44 120.0 . . yes C46 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C45 C46 C41 120.0 . . yes C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? C32 C31 C36 120.0 . . yes C32 C31 P1 121.1(3) . . yes C36 C31 P1 118.9(3) . . yes C33 C32 C31 120.0 . . yes C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 120.0 . . yes C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C35 C34 C33 120.0 . . yes C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . yes C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.0 . . yes C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? C52 C51 C56 120.0 . . yes C52 C51 P2 119.5(3) . . yes C56 C51 P2 120.5(3) . . yes C53 C52 C51 120.0 . . yes C53 C52 H52A 120.0 . . ? C51 C52 H52A 120.0 . . ? C52 C53 C54 120.0 . . yes C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C53 C54 C55 120.0 . . yes C53 C54 H54A 120.0 . . ? C55 C54 H54A 120.0 . . ? C56 C55 C54 120.0 . . yes C56 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? C55 C56 C51 120.0 . . yes C55 C56 H56A 120.0 . . ? C51 C56 H56A 120.0 . . ? C62 C61 C66 120.0 . . yes C62 C61 P2 118.8(3) . . yes C66 C61 P2 121.1(3) . . yes C61 C62 C63 120.0 . . yes C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C62 C63 C64 120.0 . . yes C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C65 C64 C63 120.0 . . yes C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C66 C65 C64 120.0 . . yes C66 C65 H65A 120.0 . . ? C64 C65 H65A 120.0 . . ? C65 C66 C61 120.0 . . yes C65 C66 H66A 120.0 . . ? C61 C66 H66A 120.0 . . ? C72 C71 C76 120.0 . . yes C72 C71 P2 122.0(4) . . yes C76 C71 P2 117.8(4) . . yes C73 C72 C71 120.0 . . yes C73 C72 H72A 120.0 . . ? C71 C72 H72A 120.0 . . ? C72 C73 C74 120.0 . . yes C72 C73 H73A 120.0 . . ? C74 C73 H73A 120.0 . . ? C73 C74 C75 120.0 . . yes C73 C74 H74A 120.0 . . ? C75 C74 H74A 120.0 . . ? C76 C75 C74 120.0 . . yes C76 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? C75 C76 C71 120.0 . . yes C75 C76 H76A 120.0 . . ? C71 C76 H76A 120.0 . . ? Cl1B C1S Cl2A 133.2(9) . . yes Cl1B C1S Cl3B 121.1(8) . . yes Cl2A C1S Cl3B 73.0(6) . . yes Cl1B C1S Cl1A 29.9(5) . . yes Cl2A C1S Cl1A 115.3(7) . . yes Cl3B C1S Cl1A 147.6(7) . . yes Cl1B C1S Cl2B 114.4(8) . . yes Cl2A C1S Cl2B 32.7(5) . . yes Cl3B C1S Cl2B 105.6(8) . . yes Cl1A C1S Cl2B 88.0(6) . . yes Cl1B C1S Cl3A 72.5(6) . . yes Cl2A C1S Cl3A 106.5(6) . . yes Cl3B C1S Cl3A 48.6(5) . . yes Cl1A C1S Cl3A 100.6(5) . . yes Cl2B C1S Cl3A 132.1(9) . . yes Cl1B C1S H1SA 113.0 . . ? Cl2A C1S H1SA 109.7 . . ? Cl3B C1S H1SA 93.8 . . ? Cl1A C1S H1SA 110.7 . . ? Cl2B C1S H1SA 106.3 . . ? Cl3A C1S H1SA 113.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.617 _refine_diff_density_min -1.250 _refine_diff_density_rms 0.157 # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END data_6b _database_code_depnum_ccdc_archive 'CCDC 691300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H27 Ni P' _chemical_formula_sum 'C32 H27 Ni P' _chemical_formula_weight 501.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1937(4) _cell_length_b 12.6191(4) _cell_length_c 14.9549(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.05(1) _cell_angle_gamma 90.00 _cell_volume 2516.19(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6797 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 30.22 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.7266 _exptl_absorpt_correction_T_max 0.8215 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34844 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 29.99 _reflns_number_total 7062 _reflns_number_gt 6004 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.630 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.45 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.45' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0400P)^2^+1.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7062 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.422176(12) 0.411712(13) 0.232773(11) 0.01696(5) Uani 1 1 d . . . P1 P 0.31476(2) 0.41398(2) 0.09100(2) 0.01497(7) Uani 1 1 d . . . C1 C 0.32151(10) 0.45192(11) 0.27848(9) 0.0201(2) Uani 1 1 d . . . C2 C 0.25049(10) 0.47731(11) 0.30156(9) 0.0213(3) Uani 1 1 d . . . C3 C 0.15787(10) 0.50190(10) 0.31659(10) 0.0203(2) Uani 1 1 d . . . C4 C 0.06630(11) 0.47993(12) 0.24387(10) 0.0249(3) Uani 1 1 d . . . H4A H 0.0666 0.4492 0.1860 0.030 Uiso 1 1 calc R . . C5 C -0.02458(11) 0.50258(12) 0.25554(11) 0.0269(3) Uani 1 1 d . . . H5A H -0.0854 0.4867 0.2055 0.032 Uiso 1 1 calc R . . C6 C -0.02821(11) 0.54807(11) 0.33921(11) 0.0250(3) Uani 1 1 d . . . C7 C 0.06241(12) 0.57020(12) 0.41140(11) 0.0280(3) Uani 1 1 d . . . H7A H 0.0616 0.6013 0.4690 0.034 Uiso 1 1 calc R . . C8 C 0.15408(11) 0.54771(12) 0.40082(10) 0.0258(3) Uani 1 1 d . . . H8A H 0.2147 0.5635 0.4511 0.031 Uiso 1 1 calc R . . C9 C -0.12754(12) 0.57275(13) 0.35115(14) 0.0352(4) Uani 1 1 d . . . H9A H -0.1155 0.6042 0.4140 0.053 Uiso 1 1 calc R . . H9B H -0.1662 0.5072 0.3455 0.053 Uiso 1 1 calc R . . H9C H -0.1652 0.6228 0.3017 0.053 Uiso 1 1 calc R . . C10 C 0.53635(11) 0.38923(14) 0.36353(10) 0.0314(3) Uani 1 1 d . . . H10A H 0.5277 0.3905 0.4271 0.038 Uiso 1 1 calc R . . C11 C 0.56493(10) 0.47836(13) 0.31829(11) 0.0293(3) Uani 1 1 d . . . H11A H 0.5770 0.5524 0.3435 0.035 Uiso 1 1 calc R . . C12 C 0.57043(10) 0.44311(12) 0.23161(11) 0.0250(3) Uani 1 1 d . . . H12A H 0.5877 0.4873 0.1839 0.030 Uiso 1 1 calc R . . C13 C 0.54742(10) 0.33109(12) 0.22362(10) 0.0253(3) Uani 1 1 d . . . H13A H 0.5479 0.2842 0.1699 0.030 Uiso 1 1 calc R . . C14 C 0.53191(11) 0.29712(13) 0.30740(11) 0.0297(3) Uani 1 1 d . . . H14A H 0.5188 0.2229 0.3235 0.036 Uiso 1 1 calc R . . C21 C 0.34794(9) 0.34581(10) -0.00254(9) 0.0169(2) Uani 1 1 d . . . C22 C 0.44189(10) 0.36363(11) -0.01114(9) 0.0204(2) Uani 1 1 d . . . H22A H 0.4879 0.4106 0.0319 0.024 Uiso 1 1 calc R . . C23 C 0.46882(10) 0.31354(11) -0.08179(10) 0.0231(3) Uani 1 1 d . . . H23A H 0.5328 0.3263 -0.0867 0.028 Uiso 1 1 calc R . . C24 C 0.40186(11) 0.24469(11) -0.14535(10) 0.0240(3) Uani 1 1 d . . . H24A H 0.4200 0.2105 -0.1937 0.029 Uiso 1 1 calc R . . C25 C 0.30857(10) 0.22631(11) -0.13757(10) 0.0239(3) Uani 1 1 d . . . H25A H 0.2629 0.1793 -0.1808 0.029 Uiso 1 1 calc R . . C26 C 0.28131(9) 0.27635(11) -0.06676(9) 0.0206(2) Uani 1 1 d . . . H26A H 0.2172 0.2632 -0.0621 0.025 Uiso 1 1 calc R . . C31 C 0.28694(9) 0.54942(10) 0.04470(9) 0.0170(2) Uani 1 1 d . . . C32 C 0.27682(10) 0.62923(11) 0.10610(10) 0.0201(2) Uani 1 1 d . . . H32A H 0.2817 0.6118 0.1693 0.024 Uiso 1 1 calc R . . C33 C 0.25968(10) 0.73420(11) 0.07500(10) 0.0234(3) Uani 1 1 d . . . H33A H 0.2523 0.7878 0.1168 0.028 Uiso 1 1 calc R . . C34 C 0.25346(10) 0.76003(11) -0.01730(11) 0.0243(3) Uani 1 1 d . . . H34A H 0.2434 0.8316 -0.0381 0.029 Uiso 1 1 calc R . . C35 C 0.26191(10) 0.68166(11) -0.07911(10) 0.0242(3) Uani 1 1 d . . . H35A H 0.2564 0.6996 -0.1424 0.029 Uiso 1 1 calc R . . C36 C 0.27854(10) 0.57629(11) -0.04876(9) 0.0204(2) Uani 1 1 d . . . H36A H 0.2841 0.5229 -0.0914 0.025 Uiso 1 1 calc R . . C41 C 0.19335(9) 0.35627(10) 0.07931(9) 0.0166(2) Uani 1 1 d . . . C42 C 0.19105(10) 0.26735(10) 0.13461(10) 0.0205(2) Uani 1 1 d . . . H42A H 0.2516 0.2406 0.1791 0.025 Uiso 1 1 calc R . . C43 C 0.10024(10) 0.21813(11) 0.12451(11) 0.0250(3) Uani 1 1 d . . . H43A H 0.0988 0.1577 0.1619 0.030 Uiso 1 1 calc R . . C44 C 0.01133(10) 0.25757(11) 0.05955(11) 0.0249(3) Uani 1 1 d . . . H44A H -0.0506 0.2240 0.0530 0.030 Uiso 1 1 calc R . . C45 C 0.01285(10) 0.34571(11) 0.00434(10) 0.0221(3) Uani 1 1 d . . . H45A H -0.0479 0.3724 -0.0398 0.027 Uiso 1 1 calc R . . C46 C 0.10387(10) 0.39504(10) 0.01379(9) 0.0189(2) Uani 1 1 d . . . H46A H 0.1050 0.4550 -0.0243 0.023 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 Ni1 0.01384(8) 0.01980(9) 0.01644(8) 0.00045(6) 0.00417(6) 0.00146(6) P1 0.01298(14) 0.01574(15) 0.01623(15) -0.00033(11) 0.00504(11) 0.00025(11) C1 0.0217(6) 0.0194(6) 0.0182(6) 0.0004(5) 0.0056(5) -0.0013(5) C2 0.0256(6) 0.0184(6) 0.0213(6) 0.0002(5) 0.0098(5) -0.0009(5) C3 0.0235(6) 0.0172(6) 0.0232(6) 0.0007(5) 0.0118(5) 0.0008(5) C4 0.0263(7) 0.0277(7) 0.0222(6) -0.0023(5) 0.0101(5) 0.0002(5) C5 0.0233(7) 0.0292(7) 0.0284(7) 0.0010(6) 0.0090(6) 0.0014(5) C6 0.0274(7) 0.0190(6) 0.0342(7) 0.0035(5) 0.0178(6) 0.0032(5) C7 0.0345(8) 0.0263(7) 0.0293(7) -0.0049(6) 0.0187(6) -0.0005(6) C8 0.0269(7) 0.0269(7) 0.0254(7) -0.0049(6) 0.0113(5) -0.0016(6) C9 0.0316(8) 0.0304(8) 0.0522(10) 0.0036(7) 0.0254(8) 0.0054(6) C10 0.0192(7) 0.0508(10) 0.0198(6) 0.0044(6) 0.0009(5) 0.0045(6) C11 0.0172(6) 0.0361(8) 0.0294(7) -0.0066(6) 0.0014(5) -0.0018(6) C12 0.0143(6) 0.0304(7) 0.0286(7) 0.0017(6) 0.0052(5) 0.0001(5) C13 0.0173(6) 0.0282(7) 0.0282(7) 0.0007(6) 0.0050(5) 0.0071(5) C14 0.0221(7) 0.0318(8) 0.0314(7) 0.0106(6) 0.0044(6) 0.0084(6) C21 0.0165(6) 0.0172(6) 0.0169(5) 0.0003(4) 0.0056(4) 0.0012(4) C22 0.0174(6) 0.0211(6) 0.0225(6) -0.0033(5) 0.0066(5) -0.0023(5) C23 0.0186(6) 0.0264(7) 0.0267(7) -0.0007(5) 0.0111(5) 0.0008(5) C24 0.0249(7) 0.0269(7) 0.0218(6) -0.0038(5) 0.0101(5) 0.0028(5) C25 0.0219(6) 0.0253(7) 0.0223(6) -0.0062(5) 0.0048(5) -0.0013(5) C26 0.0159(6) 0.0233(6) 0.0217(6) -0.0018(5) 0.0055(5) -0.0002(5) C31 0.0129(5) 0.0177(6) 0.0197(6) 0.0009(5) 0.0048(4) -0.0006(4) C32 0.0201(6) 0.0195(6) 0.0219(6) -0.0003(5) 0.0087(5) 0.0000(5) C33 0.0224(6) 0.0181(6) 0.0317(7) -0.0008(5) 0.0118(5) 0.0015(5) C34 0.0195(6) 0.0189(6) 0.0352(7) 0.0070(5) 0.0101(5) 0.0019(5) C35 0.0220(6) 0.0265(7) 0.0237(6) 0.0074(5) 0.0074(5) 0.0007(5) C36 0.0180(6) 0.0226(6) 0.0204(6) 0.0006(5) 0.0063(5) -0.0001(5) C41 0.0145(5) 0.0170(6) 0.0187(6) -0.0021(4) 0.0064(4) -0.0001(4) C42 0.0176(6) 0.0196(6) 0.0236(6) 0.0016(5) 0.0060(5) 0.0012(5) C43 0.0227(6) 0.0219(6) 0.0314(7) 0.0038(5) 0.0103(6) -0.0022(5) C44 0.0169(6) 0.0248(7) 0.0339(7) -0.0025(6) 0.0099(5) -0.0039(5) C45 0.0151(6) 0.0241(6) 0.0259(6) -0.0030(5) 0.0055(5) 0.0019(5) C46 0.0174(6) 0.0196(6) 0.0198(6) -0.0002(5) 0.0064(5) 0.0019(4) _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 Ni1 C1 1.8537(14) . yes Ni1 C10 2.0874(14) . yes Ni1 C13 2.0930(14) . yes Ni1 C14 2.1378(14) . yes Ni1 P1 2.1456(3) . yes Ni1 C12 2.1471(13) . yes Ni1 C11 2.1613(14) . yes P1 C41 1.8231(12) . yes P1 C31 1.8354(13) . yes P1 C21 1.8360(13) . yes C1 C2 1.2150(19) . yes C2 C3 1.4416(18) . yes C3 C8 1.4036(19) . yes C3 C4 1.4069(19) . yes C4 C5 1.389(2) . yes C4 H4A 0.9500 . ? C5 C6 1.394(2) . yes C5 H5A 0.9500 . ? C6 C7 1.395(2) . yes C6 C9 1.513(2) . yes C7 C8 1.393(2) . yes C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C14 1.422(2) . yes C10 C11 1.441(2) . yes C10 H10A 1.0000 . ? C11 C12 1.398(2) . yes C11 H11A 1.0000 . ? C12 C13 1.447(2) . yes C12 H12A 1.0000 . ? C13 C14 1.411(2) . yes C13 H13A 1.0000 . ? C14 H14A 1.0000 . ? C21 C22 1.4009(17) . yes C21 C26 1.4008(18) . yes C22 C23 1.3925(18) . yes C22 H22A 0.9500 . ? C23 C24 1.394(2) . yes C23 H23A 0.9500 . ? C24 C25 1.388(2) . yes C24 H24A 0.9500 . ? C25 C26 1.3967(18) . yes C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C31 C32 1.4031(18) . yes C31 C36 1.4030(18) . yes C32 C33 1.3973(19) . yes C32 H32A 0.9500 . ? C33 C34 1.391(2) . yes C33 H33A 0.9500 . ? C34 C35 1.387(2) . yes C34 H34A 0.9500 . ? C35 C36 1.3987(19) . yes C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C41 C46 1.3997(17) . yes C41 C42 1.4009(18) . yes C42 C43 1.3916(18) . yes C42 H42A 0.9500 . ? C43 C44 1.394(2) . yes C43 H43A 0.9500 . ? C44 C45 1.390(2) . yes C44 H44A 0.9500 . ? C45 C46 1.3969(18) . yes C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 C10 98.09(6) . . yes C1 Ni1 C13 159.47(6) . . yes C10 Ni1 C13 65.87(6) . . yes C1 Ni1 C14 120.55(6) . . yes C10 Ni1 C14 39.32(6) . . yes C13 Ni1 C14 38.95(6) . . yes C1 Ni1 P1 89.10(4) . . yes C10 Ni1 P1 171.06(5) . . yes C13 Ni1 P1 105.88(4) . . yes C14 Ni1 P1 131.95(5) . . yes C1 Ni1 C12 146.51(6) . . yes C10 Ni1 C12 65.45(6) . . yes C13 Ni1 C12 39.87(6) . . yes C14 Ni1 C12 65.70(6) . . yes P1 Ni1 C12 110.84(4) . . yes C1 Ni1 C11 111.10(6) . . yes C10 Ni1 C11 39.59(6) . . yes C13 Ni1 C11 65.35(6) . . yes C14 Ni1 C11 65.60(6) . . yes P1 Ni1 C11 141.61(5) . . yes C12 Ni1 C11 37.86(6) . . yes C41 P1 C31 105.18(6) . . yes C41 P1 C21 102.75(6) . . yes C31 P1 C21 103.12(6) . . yes C41 P1 Ni1 114.67(4) . . yes C31 P1 Ni1 111.92(4) . . yes C21 P1 Ni1 117.75(4) . . yes C2 C1 Ni1 175.09(12) . . yes C1 C2 C3 172.24(14) . . yes C8 C3 C4 117.73(12) . . yes C8 C3 C2 123.11(13) . . yes C4 C3 C2 119.15(12) . . yes C5 C4 C3 120.91(13) . . yes C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C6 C5 C4 121.29(14) . . yes C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 117.99(13) . . yes C5 C6 C9 120.90(14) . . yes C7 C6 C9 121.11(14) . . yes C6 C7 C8 121.38(13) . . yes C6 C7 H7A 119.3 . . ? C8 C7 H7A 119.3 . . ? C7 C8 C3 120.71(14) . . yes C7 C8 H8A 119.6 . . ? C3 C8 H8A 119.6 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C11 108.87(14) . . yes C14 C10 Ni1 72.25(8) . . yes C11 C10 Ni1 72.97(8) . . yes C14 C10 H10A 125.4 . . ? C11 C10 H10A 125.4 . . ? Ni1 C10 H10A 125.4 . . ? C12 C11 C10 107.54(14) . . yes C12 C11 Ni1 70.52(8) . . yes C10 C11 Ni1 67.44(8) . . yes C12 C11 H11A 126.2 . . ? C10 C11 H11A 126.2 . . ? Ni1 C11 H11A 126.2 . . ? C11 C12 C13 107.74(13) . . yes C11 C12 Ni1 71.62(8) . . yes C13 C12 Ni1 68.05(7) . . yes C11 C12 H12A 126.1 . . ? C13 C12 H12A 126.1 . . ? Ni1 C12 H12A 126.1 . . ? C14 C13 C12 108.85(13) . . yes C14 C13 Ni1 72.24(8) . . yes C12 C13 Ni1 72.08(8) . . yes C14 C13 H13A 125.5 . . ? C12 C13 H13A 125.5 . . ? Ni1 C13 H13A 125.5 . . ? C13 C14 C10 106.68(14) . . yes C13 C14 Ni1 68.81(8) . . yes C10 C14 Ni1 68.43(8) . . yes C13 C14 H14A 126.7 . . ? C10 C14 H14A 126.7 . . ? Ni1 C14 H14A 126.7 . . ? C22 C21 C26 118.53(11) . . yes C22 C21 P1 119.71(10) . . yes C26 C21 P1 121.76(9) . . yes C23 C22 C21 120.95(12) . . yes C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 120.00(12) . . yes C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 119.62(12) . . yes C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 120.55(12) . . yes C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C21 120.35(12) . . yes C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? C32 C31 C36 119.06(12) . . yes C32 C31 P1 118.59(10) . . yes C36 C31 P1 122.32(10) . . yes C33 C32 C31 120.52(12) . . yes C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C34 C33 C32 119.79(13) . . yes C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C35 C34 C33 120.24(13) . . yes C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 120.35(13) . . yes C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C35 C36 C31 120.02(12) . . yes C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? C46 C41 C42 119.60(11) . . yes C46 C41 P1 121.90(10) . . yes C42 C41 P1 118.42(9) . . yes C43 C42 C41 120.11(12) . . yes C43 C42 H42A 119.9 . . ? C41 C42 H42A 119.9 . . ? C42 C43 C44 119.99(13) . . yes C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C43 120.33(12) . . yes C45 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C44 C45 C46 119.92(12) . . yes C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C45 C46 C41 120.05(12) . . yes C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.344 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.053 # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END data_7a _database_code_depnum_ccdc_archive 'CCDC 691301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 P2 Pt' _chemical_formula_sum 'C52 H40 P2 Pt' _chemical_formula_weight 921.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' _symmetry_int_tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.9771(3) _cell_length_b 9.5527(1) _cell_length_c 22.9326(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3938.2(1) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 3.681 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; XPREP (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.3872 _exptl_absorpt_correction_T_max 0.7485 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 6000' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51715 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5741 _reflns_number_gt 4178 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.630 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.45 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.45' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5741 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0508 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.5000 0.0000 0.01360(3) Uani 1 2 d S . . P1 P 0.05969(2) 0.36329(4) 0.068789(17) 0.01427(8) Uani 1 1 d . . . C1 C -0.07571(9) 0.54072(17) 0.06172(7) 0.0175(3) Uani 1 1 d . . . C2 C -0.11532(9) 0.56171(18) 0.10333(7) 0.0200(4) Uani 1 1 d . . . C3 C -0.15490(9) 0.58467(18) 0.15714(7) 0.0195(3) Uani 1 1 d . . . C4 C -0.13007(12) 0.5205(2) 0.20839(9) 0.0259(4) Uani 1 1 d . . . C5 C -0.16690(12) 0.5438(2) 0.26090(9) 0.0327(5) Uani 1 1 d . . . C6 C -0.22762(12) 0.6300(2) 0.26332(9) 0.0366(5) Uani 1 1 d . . . C7 C -0.25210(12) 0.6959(3) 0.21320(10) 0.0385(5) Uani 1 1 d . . . C8 C -0.21632(10) 0.6736(2) 0.16049(9) 0.0285(4) Uani 1 1 d . . . C11 C 0.06047(9) 0.43652(17) 0.14220(7) 0.0156(3) Uani 1 1 d . . . C12 C 0.06626(10) 0.35042(19) 0.19106(7) 0.0206(3) Uani 1 1 d . . . C13 C 0.07174(10) 0.4094(2) 0.24622(8) 0.0244(4) Uani 1 1 d . . . C14 C 0.07044(11) 0.5531(2) 0.25306(8) 0.0256(4) Uani 1 1 d . . . C15 C 0.06473(10) 0.6387(2) 0.20471(7) 0.0238(4) Uani 1 1 d . . . C16 C 0.05990(9) 0.58099(17) 0.14950(7) 0.0190(3) Uani 1 1 d . . . C21 C 0.15726(9) 0.31782(16) 0.05753(7) 0.0165(3) Uani 1 1 d . . . C22 C 0.21293(9) 0.3593(2) 0.09572(8) 0.0219(4) Uani 1 1 d . . . C23 C 0.28598(10) 0.3162(2) 0.08677(8) 0.0273(4) Uani 1 1 d . . . C24 C 0.30393(10) 0.2316(2) 0.04050(8) 0.0270(4) Uani 1 1 d . . . C25 C 0.24949(12) 0.1894(3) 0.00192(8) 0.0294(4) Uani 1 1 d . . . C26 C 0.17647(11) 0.2337(2) 0.00995(8) 0.0257(4) Uani 1 1 d . . . C31 C 0.01311(9) 0.19442(18) 0.07722(7) 0.0173(3) Uani 1 1 d . . . C32 C 0.05255(11) 0.0712(2) 0.08512(10) 0.0336(5) Uani 1 1 d . . . C33 C 0.01460(13) -0.0549(2) 0.09351(11) 0.0371(5) Uani 1 1 d . . . C34 C -0.06100(12) -0.0587(2) 0.09554(8) 0.0263(4) Uani 1 1 d . . . C35 C -0.10073(11) 0.0637(2) 0.08743(9) 0.0279(4) Uani 1 1 d . . . C36 C -0.06400(10) 0.18944(19) 0.07825(8) 0.0230(4) Uani 1 1 d . . . H4 H -0.0876(11) 0.467(2) 0.2033(8) 0.023(5) Uiso 1 1 d . . . H5 H -0.1502(12) 0.4996(18) 0.2928(9) 0.028(6) Uiso 1 1 d . . . H6 H -0.2502(12) 0.646(2) 0.2985(9) 0.050(7) Uiso 1 1 d . . . H7 H -0.2919(12) 0.763(2) 0.2128(10) 0.050(7) Uiso 1 1 d . . . H8 H -0.2330(10) 0.721(2) 0.1286(9) 0.025(5) Uiso 1 1 d . . . H12 H 0.0670(9) 0.249(2) 0.1864(7) 0.018(4) Uiso 1 1 d . . . H13 H 0.0766(11) 0.350(2) 0.2765(9) 0.038(6) Uiso 1 1 d . . . H14 H 0.0742(10) 0.590(2) 0.2901(8) 0.025(5) Uiso 1 1 d . . . H15 H 0.0640(10) 0.739(2) 0.2085(8) 0.031(5) Uiso 1 1 d . . . H16 H 0.0565(9) 0.6409(18) 0.1155(8) 0.020(4) Uiso 1 1 d . . . H22 H 0.2023(10) 0.416(2) 0.1267(8) 0.023(5) Uiso 1 1 d . . . H23 H 0.3237(10) 0.344(2) 0.1128(8) 0.033(5) Uiso 1 1 d . . . H24 H 0.3515(11) 0.198(2) 0.0340(9) 0.032(5) Uiso 1 1 d . . . H25 H 0.2597(10) 0.137(2) -0.0299(9) 0.028(5) Uiso 1 1 d . . . H26 H 0.1393(11) 0.205(2) -0.0143(8) 0.022(5) Uiso 1 1 d . . . H32 H 0.1082(11) 0.071(2) 0.0836(8) 0.029(5) Uiso 1 1 d . . . H33 H 0.0400(13) -0.132(2) 0.1024(9) 0.046(7) Uiso 1 1 d . . . H34 H -0.0857(11) -0.144(2) 0.1035(9) 0.040(6) Uiso 1 1 d . . . H35 H -0.1552(11) 0.064(2) 0.0903(7) 0.021(5) Uiso 1 1 d . . . H36 H -0.0894(9) 0.2737(19) 0.0767(8) 0.019(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01530(5) 0.01335(5) 0.01217(5) 0.00135(3) -0.00060(3) 0.00217(3) P1 0.01621(18) 0.01311(18) 0.01350(17) 0.00127(16) -0.00169(17) 0.00184(17) C1 0.0175(8) 0.0165(8) 0.0185(8) 0.0023(7) -0.0028(7) 0.0033(6) C2 0.0199(8) 0.0170(9) 0.0232(9) 0.0011(7) -0.0013(7) 0.0001(7) C3 0.0168(8) 0.0202(8) 0.0215(9) -0.0028(7) 0.0031(7) -0.0030(7) C4 0.0264(10) 0.0267(10) 0.0246(10) 0.0014(8) 0.0039(8) -0.0013(8) C5 0.0382(12) 0.0381(12) 0.0218(10) -0.0001(9) 0.0029(9) -0.0107(10) C6 0.0354(11) 0.0427(13) 0.0318(11) -0.0157(10) 0.0175(9) -0.0108(10) C7 0.0280(11) 0.0406(12) 0.0469(14) -0.0107(11) 0.0132(10) 0.0053(10) C8 0.0229(9) 0.0314(11) 0.0311(11) -0.0015(9) 0.0037(8) 0.0035(8) C11 0.0150(7) 0.0177(8) 0.0140(7) 0.0012(6) -0.0008(6) 0.0018(7) C12 0.0230(8) 0.0180(9) 0.0209(8) 0.0030(7) -0.0020(7) 0.0027(7) C13 0.0272(10) 0.0289(10) 0.0170(8) 0.0048(7) -0.0022(7) 0.0015(8) C14 0.0281(10) 0.0330(11) 0.0156(8) -0.0069(8) -0.0012(7) -0.0036(9) C15 0.0286(9) 0.0195(9) 0.0234(9) -0.0046(8) -0.0007(8) -0.0023(8) C16 0.0215(8) 0.0179(8) 0.0175(8) 0.0022(7) -0.0003(7) -0.0010(7) C21 0.0194(8) 0.0140(8) 0.0160(8) 0.0041(6) -0.0003(6) 0.0032(6) C22 0.0208(8) 0.0236(9) 0.0214(8) -0.0033(8) -0.0003(7) -0.0015(8) C23 0.0173(9) 0.0378(11) 0.0269(10) 0.0009(8) -0.0033(8) -0.0004(8) C24 0.0185(9) 0.0345(11) 0.0279(10) 0.0064(8) 0.0025(8) 0.0080(8) C25 0.0307(11) 0.0351(12) 0.0225(10) -0.0041(8) 0.0006(8) 0.0141(9) C26 0.0246(10) 0.0315(11) 0.0212(10) -0.0063(8) -0.0060(8) 0.0089(8) C31 0.0231(9) 0.0153(8) 0.0133(8) 0.0004(6) -0.0037(6) -0.0008(6) C32 0.0250(10) 0.0203(10) 0.0555(14) 0.0075(9) -0.0051(10) 0.0017(8) C33 0.0401(13) 0.0127(10) 0.0584(15) 0.0072(11) -0.0075(11) 0.0023(9) C34 0.0407(12) 0.0180(9) 0.0201(8) 0.0008(7) -0.0065(8) -0.0119(9) C35 0.0281(11) 0.0262(11) 0.0295(10) 0.0002(8) -0.0013(8) -0.0066(9) C36 0.0227(9) 0.0186(8) 0.0276(10) 0.0018(7) -0.0012(8) 0.0010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.0017(17) . yes Pt1 C1 2.0018(17) 5_565 yes Pt1 P1 2.3120(4) 5_565 yes Pt1 P1 2.3121(4) . yes P1 C11 1.8232(16) . yes P1 C21 1.8254(16) . yes P1 C31 1.8279(17) . yes C1 C2 1.207(2) . yes C2 C3 1.441(2) . yes C3 C8 1.395(2) . yes C3 C4 1.399(3) . yes C4 C5 1.392(3) . yes C4 H4 0.927(19) . ? C5 C6 1.369(3) . yes C5 H5 0.90(2) . ? C6 C7 1.382(3) . yes C6 H6 0.92(2) . ? C7 C8 1.386(3) . yes C7 H7 0.96(2) . ? C8 H8 0.91(2) . ? C11 C16 1.390(2) . yes C11 C12 1.394(2) . yes C12 C13 1.388(2) . yes C12 H12 0.971(18) . ? C13 C14 1.382(3) . yes C13 H13 0.90(2) . ? C14 C15 1.381(3) . yes C14 H14 0.922(18) . ? C15 C16 1.384(2) . yes C15 H15 0.96(2) . ? C16 H16 0.970(17) . ? C21 C22 1.388(2) . yes C21 C26 1.398(2) . yes C22 C23 1.391(2) . yes C22 H22 0.912(18) . ? C23 C24 1.373(3) . yes C23 H23 0.943(19) . ? C24 C25 1.379(3) . yes C24 H24 0.924(19) . ? C25 C26 1.391(3) . yes C25 H25 0.90(2) . ? C26 H26 0.913(18) . ? C31 C32 1.386(2) . yes C31 C36 1.387(2) . yes C32 C33 1.397(3) . yes C32 H32 1.001(19) . ? C33 C34 1.360(3) . yes C33 H33 0.89(2) . ? C34 C35 1.383(3) . yes C34 H34 0.95(2) . ? C35 C36 1.387(3) . yes C35 H35 0.982(19) . ? C36 H36 0.926(18) . ? 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 C1 Pt1 C1 180.0 . 5_565 yes C1 Pt1 P1 93.27(5) . 5_565 yes C1 Pt1 P1 86.73(5) 5_565 5_565 yes C1 Pt1 P1 86.73(5) . . yes C1 Pt1 P1 93.27(5) 5_565 . yes P1 Pt1 P1 180.0 5_565 . yes C11 P1 C21 102.39(7) . . yes C11 P1 C31 104.15(8) . . yes C21 P1 C31 104.20(7) . . yes C11 P1 Pt1 114.64(5) . . yes C21 P1 Pt1 118.94(5) . . yes C31 P1 Pt1 110.98(5) . . yes C2 C1 Pt1 172.78(15) . . yes C1 C2 C3 173.27(18) . . yes C8 C3 C4 118.25(17) . . yes C8 C3 C2 122.03(16) . . yes C4 C3 C2 119.68(16) . . yes C5 C4 C3 120.33(19) . . yes C5 C4 H4 126.0(12) . . ? C3 C4 H4 113.6(12) . . ? C6 C5 C4 120.7(2) . . yes C6 C5 H5 121.2(14) . . ? C4 C5 H5 118.1(14) . . ? C5 C6 C7 119.63(19) . . yes C5 C6 H6 119.4(14) . . ? C7 C6 H6 120.9(14) . . ? C6 C7 C8 120.5(2) . . yes C6 C7 H7 123.3(14) . . ? C8 C7 H7 116.1(14) . . ? C7 C8 C3 120.6(2) . . yes C7 C8 H8 118.2(12) . . ? C3 C8 H8 121.2(12) . . ? C16 C11 C12 119.32(15) . . yes C16 C11 P1 119.47(11) . . yes C12 C11 P1 121.09(13) . . yes C13 C12 C11 119.87(16) . . yes C13 C12 H12 120.2(10) . . ? C11 C12 H12 119.9(10) . . ? C14 C13 C12 120.37(16) . . yes C14 C13 H13 122.5(13) . . ? C12 C13 H13 117.2(13) . . ? C15 C14 C13 119.86(16) . . yes C15 C14 H14 121.2(12) . . ? C13 C14 H14 118.9(12) . . ? C14 C15 C16 120.25(17) . . yes C14 C15 H15 121.2(12) . . ? C16 C15 H15 118.6(12) . . ? C15 C16 C11 120.33(16) . . yes C15 C16 H16 120.4(10) . . ? C11 C16 H16 119.3(10) . . ? C22 C21 C26 118.59(16) . . yes C22 C21 P1 122.40(13) . . yes C26 C21 P1 118.97(13) . . yes C21 C22 C23 120.21(17) . . yes C21 C22 H22 120.6(11) . . ? C23 C22 H22 119.2(11) . . ? C24 C23 C22 120.67(18) . . yes C24 C23 H23 119.1(11) . . ? C22 C23 H23 120.2(12) . . ? C23 C24 C25 120.06(18) . . yes C23 C24 H24 122.9(13) . . ? C25 C24 H24 117.0(13) . . ? C24 C25 C26 119.73(19) . . yes C24 C25 H25 122.4(12) . . ? C26 C25 H25 117.8(12) . . ? C25 C26 C21 120.72(18) . . yes C25 C26 H26 121.2(12) . . ? C21 C26 H26 118.0(12) . . ? C32 C31 C36 118.67(16) . . yes C32 C31 P1 121.93(14) . . yes C36 C31 P1 119.33(13) . . yes C31 C32 C33 120.0(2) . . yes C31 C32 H32 120.3(12) . . ? C33 C32 H32 119.7(12) . . ? C34 C33 C32 121.0(2) . . yes C34 C33 H33 118.8(15) . . ? C32 C33 H33 119.6(15) . . ? C33 C34 C35 119.27(19) . . yes C33 C34 H34 119.9(13) . . ? C35 C34 H34 120.8(13) . . ? C34 C35 C36 120.45(19) . . yes C34 C35 H35 120.7(11) . . ? C36 C35 H35 118.7(11) . . ? C35 C36 C31 120.53(18) . . yes C35 C36 H36 121.7(11) . . ? C31 C36 H36 117.5(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.401 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.068 # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END data_7b _database_code_depnum_ccdc_archive 'CCDC 691302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H44 P2 Pt' _chemical_formula_sum 'C54 H44 P2 Pt' _chemical_formula_weight 949.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.5550(2) _cell_length_b 8.5121(1) _cell_length_c 18.0271(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.30(1) _cell_angle_gamma 90.00 _cell_volume 2079.97(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8948 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 33.12 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 3.487 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; XPREP (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.45314 _exptl_absorpt_correction_T_max 0.82820 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 6000' _diffrn_measurement_method '0.20\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25528 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 29.00 _reflns_number_total 5541 _reflns_number_gt 4659 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.630 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.45 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.45' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0200P)^2^+0.1000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5541 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0411 _refine_ls_wR_factor_gt 0.0398 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.0000 0.0000 0.01262(3) Uani 1 2 d S . . P1 P 0.51446(3) 0.13351(5) 0.10972(2) 0.01377(8) Uani 1 1 d . . . C1 C 0.64443(12) -0.0541(2) 0.01379(9) 0.0154(3) Uani 1 1 d . . . C2 C 0.72856(12) -0.08348(19) 0.02645(9) 0.0187(3) Uani 1 1 d . . . C3 C 0.83049(12) -0.11504(19) 0.04504(9) 0.0180(3) Uani 1 1 d . . . C4 C 0.89241(13) -0.1996(2) -0.00263(10) 0.0225(4) Uani 1 1 d . . . C5 C 0.99057(13) -0.2276(2) 0.01634(10) 0.0234(4) Uani 1 1 d . . . C6 C 1.03022(12) -0.1732(2) 0.08265(10) 0.0215(3) Uani 1 1 d . . . C7 C 0.96836(13) -0.0923(2) 0.13065(10) 0.0222(4) Uani 1 1 d . . . C8 C 0.87050(13) -0.0633(2) 0.11231(10) 0.0209(3) Uani 1 1 d . . . C9 C 1.13799(14) -0.1981(3) 0.10130(13) 0.0300(4) Uani 1 1 d . . . C11 C 0.52600(12) 0.00203(17) 0.18917(9) 0.0139(3) Uani 1 1 d . . . C12 C 0.50519(12) 0.0567(2) 0.26073(9) 0.0167(3) Uani 1 1 d . . . C13 C 0.50928(13) -0.0451(2) 0.32099(10) 0.0191(3) Uani 1 1 d . . . C14 C 0.53424(13) -0.2017(2) 0.31037(10) 0.0206(3) Uani 1 1 d . . . C15 C 0.55594(13) -0.2557(2) 0.23969(10) 0.0208(3) Uani 1 1 d . . . C16 C 0.55233(12) -0.1552(2) 0.17941(9) 0.0187(3) Uani 1 1 d . . . C21 C 0.61699(11) 0.27115(19) 0.11238(9) 0.0165(3) Uani 1 1 d . . . C22 C 0.66671(12) 0.3085(2) 0.17786(10) 0.0187(3) Uani 1 1 d . . . C23 C 0.73473(13) 0.4306(2) 0.17880(11) 0.0229(4) Uani 1 1 d . . . C24 C 0.75271(15) 0.5160(2) 0.11506(12) 0.0264(4) Uani 1 1 d . . . C25 C 0.70415(16) 0.4791(2) 0.04942(12) 0.0289(4) Uani 1 1 d . . . C26 C 0.63730(13) 0.3549(2) 0.04799(10) 0.0240(4) Uani 1 1 d . . . C31 C 0.41134(12) 0.25782(19) 0.13716(9) 0.0162(3) Uani 1 1 d . . . C32 C 0.41877(14) 0.4213(2) 0.14116(10) 0.0210(3) Uani 1 1 d . . . C33 C 0.33901(15) 0.5104(2) 0.16451(12) 0.0267(4) Uani 1 1 d . . . C34 C 0.25171(14) 0.4380(3) 0.18479(11) 0.0265(4) Uani 1 1 d . . . C35 C 0.24342(13) 0.2763(2) 0.18015(10) 0.0239(4) Uani 1 1 d . . . C36 C 0.32208(13) 0.1864(2) 0.15597(9) 0.0202(3) Uani 1 1 d . . . H4 H 0.8686(16) -0.234(3) -0.0498(13) 0.035(6) Uiso 1 1 d . . . H5 H 1.0306(17) -0.283(3) -0.0137(12) 0.034(6) Uiso 1 1 d . . . H7 H 0.9934(16) -0.056(3) 0.1807(13) 0.032(6) Uiso 1 1 d . . . H8 H 0.832(2) -0.010(2) 0.1447(16) 0.028(7) Uiso 1 1 d . . . H91 H 1.1547(13) -0.167(2) 0.1479(11) 0.013(4) Uiso 1 1 d . . . H92 H 1.1826(19) -0.133(3) 0.0716(14) 0.054(7) Uiso 1 1 d . . . H93 H 1.1590(19) -0.296(3) 0.0914(15) 0.056(8) Uiso 1 1 d . . . H12 H 0.4864(13) 0.159(2) 0.2671(10) 0.012(4) Uiso 1 1 d . . . H13 H 0.4967(17) -0.0084(19) 0.3658(14) 0.020(6) Uiso 1 1 d . . . H14 H 0.5353(13) -0.271(2) 0.3509(11) 0.018(5) Uiso 1 1 d . . . H15 H 0.5723(13) -0.364(2) 0.2307(10) 0.019(5) Uiso 1 1 d . . . H16 H 0.5632(15) -0.184(2) 0.1350(12) 0.024(5) Uiso 1 1 d . . . H22 H 0.6563(13) 0.254(2) 0.2209(10) 0.016(5) Uiso 1 1 d . . . H23 H 0.7700(17) 0.461(3) 0.2221(13) 0.026(6) Uiso 1 1 d . . . H24 H 0.7991(15) 0.603(3) 0.1158(11) 0.030(6) Uiso 1 1 d . . . H25 H 0.7150(17) 0.536(3) 0.0091(14) 0.029(6) Uiso 1 1 d . . . H26 H 0.6039(13) 0.326(2) 0.0033(11) 0.019(5) Uiso 1 1 d . . . H32 H 0.4764(18) 0.467(2) 0.1262(13) 0.027(6) Uiso 1 1 d . . . H33 H 0.3447(14) 0.627(2) 0.1687(10) 0.023(5) Uiso 1 1 d . . . H34 H 0.200(2) 0.503(2) 0.2014(16) 0.032(7) Uiso 1 1 d . . . H35 H 0.1906(16) 0.228(3) 0.1931(11) 0.029(6) Uiso 1 1 d . . . H36 H 0.3149(14) 0.078(3) 0.1522(11) 0.019(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01195(4) 0.01419(4) 0.01172(4) -0.00064(3) 0.00017(3) 0.00057(3) P1 0.01380(18) 0.01450(18) 0.01303(18) -0.00059(15) 0.00002(14) 0.00018(15) C1 0.0200(8) 0.0135(7) 0.0126(7) -0.0008(6) 0.0016(6) -0.0001(6) C2 0.0210(8) 0.0176(8) 0.0174(8) 0.0008(6) 0.0017(6) -0.0007(6) C3 0.0177(8) 0.0176(8) 0.0186(8) 0.0044(6) 0.0000(6) -0.0006(6) C4 0.0214(8) 0.0298(9) 0.0164(8) 0.0010(7) -0.0006(7) 0.0038(7) C5 0.0207(9) 0.0307(10) 0.0188(8) 0.0030(7) 0.0032(7) 0.0054(7) C6 0.0178(8) 0.0213(8) 0.0254(9) 0.0090(7) -0.0009(7) 0.0000(7) C7 0.0250(9) 0.0182(8) 0.0233(9) 0.0008(7) -0.0060(7) 0.0000(7) C8 0.0216(8) 0.0189(8) 0.0222(9) -0.0014(7) 0.0006(7) 0.0014(7) C9 0.0181(9) 0.0353(11) 0.0365(12) 0.0119(9) -0.0032(8) 0.0012(8) C11 0.0128(7) 0.0152(7) 0.0137(7) 0.0008(6) -0.0005(5) -0.0018(6) C12 0.0157(8) 0.0169(7) 0.0175(8) -0.0011(7) -0.0004(6) 0.0017(6) C13 0.0192(8) 0.0250(8) 0.0131(8) -0.0006(7) 0.0013(6) 0.0015(7) C14 0.0224(8) 0.0218(8) 0.0177(8) 0.0043(7) 0.0003(6) 0.0007(7) C15 0.0248(9) 0.0161(8) 0.0214(9) 0.0008(7) 0.0007(7) 0.0021(7) C16 0.0216(8) 0.0181(8) 0.0165(8) -0.0029(7) 0.0013(6) 0.0003(7) C21 0.0143(7) 0.0146(7) 0.0205(8) -0.0004(6) 0.0004(6) 0.0001(6) C22 0.0172(8) 0.0194(8) 0.0196(8) 0.0011(7) 0.0008(6) 0.0002(6) C23 0.0196(8) 0.0225(9) 0.0264(10) -0.0027(8) -0.0049(7) -0.0014(7) C24 0.0236(9) 0.0225(9) 0.0330(11) 0.0021(8) -0.0023(8) -0.0079(7) C25 0.0325(10) 0.0289(10) 0.0253(10) 0.0081(8) -0.0004(8) -0.0100(8) C26 0.0273(9) 0.0256(9) 0.0189(8) 0.0021(7) -0.0021(7) -0.0052(8) C31 0.0168(7) 0.0199(8) 0.0119(7) -0.0016(6) -0.0010(6) 0.0039(6) C32 0.0202(8) 0.0218(9) 0.0210(9) -0.0015(7) -0.0010(7) 0.0018(7) C33 0.0268(10) 0.0241(9) 0.0293(10) -0.0056(8) -0.0031(8) 0.0083(8) C34 0.0221(9) 0.0344(10) 0.0229(9) -0.0048(8) -0.0005(7) 0.0126(8) C35 0.0171(8) 0.0369(10) 0.0179(8) 0.0006(8) 0.0017(6) 0.0031(8) C36 0.0196(8) 0.0227(9) 0.0184(8) 0.0001(7) -0.0003(6) 0.0007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.0252(17) 3_655 yes Pt1 C1 2.0252(17) . yes Pt1 P1 2.2887(4) . yes Pt1 P1 2.2887(4) 3_655 yes P1 C21 1.8181(16) . yes P1 C31 1.8236(16) . yes P1 C11 1.8239(16) . yes C1 C2 1.188(2) . yes C2 C3 1.445(2) . yes C3 C8 1.397(2) . yes C3 C4 1.403(2) . yes C4 C5 1.393(2) . yes C4 H4 0.95(2) . ? C5 C6 1.388(3) . yes C5 H5 0.90(2) . ? C6 C7 1.391(2) . yes C6 C9 1.512(2) . yes C7 C8 1.387(2) . yes C7 H7 1.01(2) . ? C8 H8 0.91(3) . ? C9 H91 0.907(19) . ? C9 H92 0.98(3) . ? C9 H93 0.90(3) . ? C11 C16 1.397(2) . yes C11 C12 1.401(2) . yes C12 C13 1.390(3) . yes C12 H12 0.913(18) . ? C13 C14 1.389(3) . yes C13 H13 0.88(2) . ? C14 C15 1.388(2) . yes C14 H14 0.937(19) . ? C15 C16 1.384(2) . yes C15 H15 0.963(19) . ? C16 H16 0.85(2) . ? C21 C26 1.391(2) . yes C21 C22 1.393(2) . yes C22 C23 1.389(2) . yes C22 H22 0.915(18) . ? C23 C24 1.383(3) . yes C23 H23 0.95(2) . ? C24 C25 1.387(3) . yes C24 H24 0.97(2) . ? C25 C26 1.392(3) . yes C25 H25 0.89(2) . ? C26 H26 0.953(19) . ? C31 C32 1.397(2) . yes C31 C36 1.398(2) . yes C32 C33 1.388(3) . yes C32 H32 0.91(2) . ? C33 C34 1.385(3) . yes C33 H33 1.00(2) . ? C34 C35 1.383(3) . yes C34 H34 0.94(3) . ? C35 C36 1.385(2) . yes C35 H35 0.86(2) . ? C36 H36 0.93(2) . ? 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 C1 Pt1 C1 180.0 3_655 . yes C1 Pt1 P1 94.10(5) 3_655 . yes C1 Pt1 P1 85.90(5) . . yes C1 Pt1 P1 85.90(5) 3_655 3_655 yes C1 Pt1 P1 94.10(5) . 3_655 yes P1 Pt1 P1 180.0 . 3_655 yes C21 P1 C31 101.88(7) . . yes C21 P1 C11 108.19(7) . . yes C31 P1 C11 101.88(7) . . yes C21 P1 Pt1 113.88(6) . . yes C31 P1 Pt1 117.40(5) . . yes C11 P1 Pt1 112.37(5) . . yes C2 C1 Pt1 175.88(15) . . yes C1 C2 C3 177.32(18) . . yes C8 C3 C4 117.55(15) . . yes C8 C3 C2 120.60(15) . . yes C4 C3 C2 121.85(15) . . yes C5 C4 C3 120.75(17) . . yes C5 C4 H4 119.0(13) . . ? C3 C4 H4 120.1(13) . . ? C6 C5 C4 121.30(17) . . yes C6 C5 H5 117.4(14) . . ? C4 C5 H5 121.2(14) . . ? C5 C6 C7 117.99(16) . . yes C5 C6 C9 120.93(17) . . yes C7 C6 C9 121.07(18) . . yes C8 C7 C6 121.23(17) . . yes C8 C7 H7 118.4(13) . . ? C6 C7 H7 120.3(13) . . ? C7 C8 C3 121.15(17) . . yes C7 C8 H8 118.9(17) . . ? C3 C8 H8 120.0(17) . . ? C6 C9 H91 113.7(11) . . ? C6 C9 H92 113.5(15) . . ? H91 C9 H92 101.1(18) . . ? C6 C9 H93 113.2(17) . . ? H91 C9 H93 112(2) . . ? H92 C9 H93 102(2) . . ? C16 C11 C12 119.14(15) . . yes C16 C11 P1 120.67(13) . . yes C12 C11 P1 120.16(12) . . yes C13 C12 C11 120.33(16) . . yes C13 C12 H12 120.3(11) . . ? C11 C12 H12 119.3(11) . . ? C14 C13 C12 119.94(17) . . yes C14 C13 H13 120.9(12) . . ? C12 C13 H13 119.2(12) . . ? C15 C14 C13 119.85(16) . . yes C15 C14 H14 120.3(12) . . ? C13 C14 H14 119.8(11) . . ? C16 C15 C14 120.63(16) . . yes C16 C15 H15 117.8(11) . . ? C14 C15 H15 121.5(11) . . ? C15 C16 C11 120.10(16) . . yes C15 C16 H16 123.5(14) . . ? C11 C16 H16 116.3(14) . . ? C26 C21 C22 119.55(15) . . yes C26 C21 P1 117.57(13) . . yes C22 C21 P1 122.40(13) . . yes C23 C22 C21 119.95(16) . . yes C23 C22 H22 118.2(12) . . ? C21 C22 H22 121.9(12) . . ? C24 C23 C22 120.20(18) . . yes C24 C23 H23 116.9(14) . . ? C22 C23 H23 122.9(14) . . ? C23 C24 C25 120.33(17) . . yes C23 C24 H24 120.4(12) . . ? C25 C24 H24 119.3(12) . . ? C24 C25 C26 119.59(18) . . yes C24 C25 H25 119.6(15) . . ? C26 C25 H25 120.8(15) . . ? C21 C26 C25 120.35(17) . . yes C21 C26 H26 118.7(11) . . ? C25 C26 H26 121.0(11) . . ? C32 C31 C36 118.91(16) . . yes C32 C31 P1 122.46(13) . . yes C36 C31 P1 118.62(13) . . yes C33 C32 C31 120.23(18) . . yes C33 C32 H32 121.8(13) . . ? C31 C32 H32 117.9(13) . . ? C34 C33 C32 120.37(17) . . yes C34 C33 H33 119.2(11) . . ? C32 C33 H33 120.4(11) . . ? C35 C34 C33 119.71(18) . . yes C35 C34 H34 123.1(14) . . ? C33 C34 H34 117.2(14) . . ? C34 C35 C36 120.45(18) . . yes C34 C35 H35 121.8(14) . . ? C36 C35 H35 117.8(14) . . ? C35 C36 C31 120.29(17) . . yes C35 C36 H36 119.4(12) . . ? C31 C36 H36 120.3(12) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.253 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.071 # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END data_8b _database_code_depnum_ccdc_archive 'CCDC 691303' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 P2 Pt' _chemical_formula_sum 'C24 H32 P2 Pt' _chemical_formula_weight 577.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3805(5) _cell_length_b 5.7372(2) _cell_length_c 17.1229(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.86(1) _cell_angle_gamma 90.00 _cell_volume 1169.92(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6318 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.75 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 6.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.2293 _exptl_absorpt_correction_T_max 0.7096 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'normalfocus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K' _diffrn_measurement_method '0.30\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10382 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 29.98 _reflns_number_total 3307 _reflns_number_gt 2656 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.630 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.45 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.45' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0100P)^2^+1.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3307 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0414 _refine_ls_wR_factor_gt 0.0383 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 1.0000 0.0000 0.01306(4) Uani 1 2 d S . . P1 P 0.40643(5) 0.78981(11) 0.07498(4) 0.01484(12) Uani 1 1 d . . . C1 C 0.6218(2) 1.0674(4) 0.10136(16) 0.0170(5) Uani 1 1 d . . . C2 C 0.6970(2) 1.1097(4) 0.16189(16) 0.0178(5) Uani 1 1 d . . . C3 C 0.79034(19) 1.1710(4) 0.22941(15) 0.0156(5) Uani 1 1 d . . . C4 C 0.84475(19) 1.3865(4) 0.23109(15) 0.0166(5) Uani 1 1 d . . . H4A H 0.8185 1.4934 0.1877 0.020 Uiso 1 1 calc R . . C5 C 0.9362(2) 1.4453(4) 0.29514(16) 0.0172(5) Uani 1 1 d . . . H5A H 0.9718 1.5918 0.2947 0.021 Uiso 1 1 calc R . . C6 C 0.97708(19) 1.2937(5) 0.36020(15) 0.0176(5) Uani 1 1 d . . . C7 C 0.9228(2) 1.0807(5) 0.35909(16) 0.0181(5) Uani 1 1 d . . . H7A H 0.9490 0.9746 0.4028 0.022 Uiso 1 1 calc R . . C8 C 0.8307(2) 1.0208(4) 0.29483(15) 0.0178(5) Uani 1 1 d . . . H8A H 0.7947 0.8749 0.2957 0.021 Uiso 1 1 calc R . . C9 C 1.0786(2) 1.3576(5) 0.42822(17) 0.0247(6) Uani 1 1 d . . . H9A H 1.0954 1.2311 0.4682 0.037 Uiso 1 1 calc R . . H9B H 1.0632 1.5010 0.4544 0.037 Uiso 1 1 calc R . . H9C H 1.1430 1.3822 0.4063 0.037 Uiso 1 1 calc R . . C10 C 0.3241(2) 0.9835(5) 0.11979(17) 0.0230(5) Uani 1 1 d . . . H10A H 0.2845 0.8922 0.1517 0.035 Uiso 1 1 calc R . . H10B H 0.2694 1.0669 0.0767 0.035 Uiso 1 1 calc R . . H10C H 0.3740 1.0960 0.1552 0.035 Uiso 1 1 calc R . . C11 C 0.4916(2) 0.6275(5) 0.16052(17) 0.0256(6) Uani 1 1 d . . . H11A H 0.4427 0.5451 0.1877 0.038 Uiso 1 1 calc R . . H11B H 0.5403 0.7352 0.1989 0.038 Uiso 1 1 calc R . . H11C H 0.5378 0.5144 0.1413 0.038 Uiso 1 1 calc R . . C12 C 0.3058(2) 0.5774(5) 0.02088(18) 0.0243(6) Uani 1 1 d . . . H12A H 0.2714 0.4988 0.0589 0.036 Uiso 1 1 calc R . . H12B H 0.3439 0.4623 -0.0045 0.036 Uiso 1 1 calc R . . H12C H 0.2473 0.6561 -0.0212 0.036 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 Pt1 0.01225(6) 0.01422(6) 0.01301(6) -0.00036(6) 0.00397(4) -0.00169(6) P1 0.0157(3) 0.0149(3) 0.0149(3) 0.0009(2) 0.0057(2) -0.0013(2) C1 0.0173(11) 0.0164(11) 0.0187(12) 0.0007(9) 0.0075(10) -0.0006(9) C2 0.0183(11) 0.0168(12) 0.0197(13) 0.0001(10) 0.0073(10) 0.0012(10) C3 0.0119(10) 0.0179(12) 0.0176(12) -0.0004(9) 0.0051(9) 0.0013(9) C4 0.0154(11) 0.0183(13) 0.0162(12) 0.0019(10) 0.0043(9) 0.0018(9) C5 0.0153(11) 0.0158(13) 0.0218(13) -0.0007(9) 0.0071(9) -0.0011(8) C6 0.0143(11) 0.0227(12) 0.0161(12) -0.0040(10) 0.0046(9) 0.0008(10) C7 0.0181(11) 0.0206(12) 0.0148(12) 0.0021(10) 0.0034(9) 0.0032(10) C8 0.0182(11) 0.0148(12) 0.0209(12) 0.0002(10) 0.0066(9) 0.0002(10) C9 0.0199(13) 0.0307(15) 0.0217(14) -0.0013(11) 0.0026(10) -0.0010(11) C10 0.0278(13) 0.0191(13) 0.0263(13) 0.0010(12) 0.0144(10) 0.0006(11) C11 0.0262(13) 0.0235(14) 0.0257(15) 0.0091(11) 0.0048(11) 0.0020(11) C12 0.0260(14) 0.0209(12) 0.0275(15) -0.0019(11) 0.0098(11) -0.0087(11) _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 Pt1 C1 2.001(3) 3_675 yes Pt1 C1 2.001(3) . yes Pt1 P1 2.2929(6) . yes Pt1 P1 2.2929(6) 3_675 yes P1 C12 1.807(3) . yes P1 C11 1.811(3) . yes P1 C10 1.814(3) . yes C1 C2 1.214(4) . yes C2 C3 1.437(3) . yes C3 C8 1.393(3) . yes C3 C4 1.404(3) . yes C4 C5 1.386(4) . yes C4 H4A 0.9500 . ? C5 C6 1.395(4) . yes C5 H5A 0.9500 . ? C6 C7 1.392(4) . yes C6 C9 1.506(4) . yes C7 C8 1.394(3) . yes C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 C1 180.0 3_675 . yes C1 Pt1 P1 90.45(7) 3_675 . yes C1 Pt1 P1 89.55(7) . . yes C1 Pt1 P1 89.55(7) 3_675 3_675 yes C1 Pt1 P1 90.45(7) . 3_675 yes P1 Pt1 P1 180.00(2) . 3_675 yes C12 P1 C11 103.61(14) . . yes C12 P1 C10 103.97(13) . . yes C11 P1 C10 104.06(13) . . yes C12 P1 Pt1 116.80(9) . . yes C11 P1 Pt1 116.86(9) . . yes C10 P1 Pt1 110.06(9) . . yes C2 C1 Pt1 178.7(2) . . yes C1 C2 C3 175.3(3) . . yes C8 C3 C4 117.6(2) . . yes C8 C3 C2 121.9(2) . . yes C4 C3 C2 120.5(2) . . yes C5 C4 C3 120.9(2) . . yes C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 121.3(2) . . yes C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C6 C5 117.9(2) . . yes C7 C6 C9 121.4(2) . . yes C5 C6 C9 120.6(2) . . yes C6 C7 C8 121.0(2) . . yes C6 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C3 C8 C7 121.2(2) . . yes C3 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.566 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.102 # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END data_9 _database_code_depnum_ccdc_archive 'CCDC 691304' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Au F6 P3' _chemical_formula_sum 'C6 H18 Au F6 P3' _chemical_formula_weight 494.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_space_group_name_Hall '-P 2ac 2n ' _symmetry_int_tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 11.5118(2) _cell_length_b 8.5384(2) _cell_length_c 14.3292(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1408.45(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7577 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 33.14 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 10.826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2003) ; _exptl_absorpt_correction_T_min 0.0646 _exptl_absorpt_correction_T_max 0.8126 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 6000' _diffrn_measurement_method '0.20\% \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19470 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 31.50 _reflns_number_total 2477 _reflns_number_gt 2394 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART Ver. 5.630 (Bruker-AXS, 2003)' _computing_cell_refinement 'SAINT Ver. 6.45 (Bruker-AXS, 2003)' _computing_data_reduction 'SAINT Ver. 6.45' _computing_structure_solution 'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)' _computing_structure_refinement 'SHELXTL Ver. 6.14' _computing_molecular_graphics 'SHELXTL Ver. 6.14' _computing_publication_material 'SHELXTL Ver. 6.14' _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^)+(0.0260P)^2^+2.8000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2477 _refine_ls_number_parameters 106 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 Au1 Au 0.087430(9) 0.2500 0.619164(8) 0.01576(5) Uani 1 2 d S . . P1 P 0.01909(7) 0.2500 0.77012(5) 0.01563(14) Uani 1 2 d S . . P2 P 0.15217(7) 0.2500 0.46714(5) 0.01648(14) Uani 1 2 d S . . P3 P 0.27361(9) -0.2500 0.61424(6) 0.02144(17) Uani 1 2 d S . . C1 C -0.1381(3) 0.2500 0.7775(3) 0.0247(7) Uani 1 2 d SD . . H11 H -0.168(4) 0.2500 0.8485(18) 0.030 Uiso 1 2 d SD . . H12 H -0.166(3) 0.137(3) 0.752(2) 0.030 Uiso 1 1 d D . . C2 C 0.0638(2) 0.0816(4) 0.8371(2) 0.0292(5) Uani 1 1 d . . . H21 H 0.0310 0.0883 0.9001 0.035 Uiso 1 1 calc R . . H22 H 0.1488 0.0790 0.8410 0.035 Uiso 1 1 calc R . . H23 H 0.0360 -0.0140 0.8066 0.035 Uiso 1 1 calc R . . C3 C 0.1037(2) 0.0822(3) 0.4014(2) 0.0246(5) Uani 1 1 d . . . H31 H 0.0186 0.0804 0.3999 0.045(11) Uiso 1 1 calc R . . H32 H 0.1324 -0.0137 0.4310 0.032(9) Uiso 1 1 calc R . . H33 H 0.1338 0.0888 0.3375 0.031(9) Uiso 1 1 calc R . . C4 C 0.3086(3) 0.2500 0.4549(3) 0.0241(6) Uani 1 2 d SD . . H41 H 0.341(5) 0.2500 0.3844(18) 0.029 Uiso 1 2 d SD . . H42 H 0.341(3) 0.145(3) 0.486(2) 0.029 Uiso 1 1 d D . . F1 F 0.1638(3) -0.2500 0.5470(3) 0.0621(10) Uani 1 2 d S . . F4 F 0.3817(3) -0.2500 0.6833(2) 0.0526(8) Uani 1 2 d S . . F2 F 0.1901(9) -0.1754(12) 0.6919(7) 0.071(3) Uiso 0.33 1 d P . 1 F3A F 0.3014(7) -0.0754(9) 0.5791(6) 0.0494(17) Uiso 0.33 1 d P . 1 F2B F 0.2170(5) -0.1183(8) 0.6830(5) 0.0321(11) Uiso 0.33 1 d P A 2 F3B F 0.3299(5) -0.1138(8) 0.5533(4) 0.0320(11) Uiso 0.33 1 d P . 2 F2C F 0.2423(8) -0.0819(12) 0.6498(8) 0.067(2) Uiso 0.33 1 d P . 3 F3C F 0.3563(7) -0.1733(10) 0.5373(6) 0.0575(19) Uiso 0.33 1 d P . 3 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 Au1 0.01614(7) 0.01781(7) 0.01333(7) 0.000 0.00082(3) 0.000 P1 0.0146(3) 0.0185(3) 0.0139(3) 0.000 0.0006(3) 0.000 P2 0.0209(3) 0.0147(3) 0.0139(3) 0.000 0.0011(3) 0.000 P3 0.0263(4) 0.0173(4) 0.0208(4) 0.000 -0.0001(3) 0.000 C1 0.0168(13) 0.0324(17) 0.0248(16) 0.000 0.0023(12) 0.000 C2 0.0282(11) 0.0316(13) 0.0279(12) 0.0129(11) 0.0026(10) 0.0068(10) C3 0.0335(12) 0.0196(11) 0.0206(10) -0.0042(9) -0.0008(9) -0.0036(9) C4 0.0236(15) 0.0241(15) 0.0247(16) 0.000 0.0049(12) 0.000 F1 0.0546(19) 0.056(2) 0.075(3) 0.000 -0.0361(19) 0.000 F4 0.0570(18) 0.056(2) 0.0448(18) 0.000 -0.0246(15) 0.000 _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 Au1 P1 2.3016(8) . yes Au1 P2 2.3023(8) . yes P1 C2 1.804(3) 7_565 yes P1 C2 1.804(3) . yes P1 C1 1.813(4) . yes P2 C3 1.803(3) 7_565 yes P2 C3 1.803(3) . yes P2 C4 1.810(4) . yes P3 F2C 1.565(10) 7 yes P3 F2C 1.565(10) . yes P3 F4 1.590(3) . yes P3 F1 1.590(3) . yes P3 F3B 1.592(6) . yes P3 F3B 1.592(6) 7 yes P3 F3C 1.597(8) . yes P3 F3C 1.597(8) 7 yes P3 F2 1.602(10) 7 yes P3 F2 1.602(10) . yes P3 F3A 1.605(8) . yes P3 F3A 1.605(8) 7 yes C1 H11 1.074(19) . ? C1 H12 1.077(18) . ? C2 H21 0.9800 . ? C2 H22 0.9800 . ? C2 H23 0.9800 . ? C3 H31 0.9800 . ? C3 H32 0.9800 . ? C3 H33 0.9800 . ? C4 H41 1.079(19) . ? C4 H42 1.071(18) . ? F2 F2 1.27(2) 7 yes F3C F3C 1.310(18) 7 yes 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 P1 Au1 P2 178.90(3) . . yes C2 P1 C2 105.7(2) 7_565 . yes C2 P1 C1 104.69(12) 7_565 . yes C2 P1 C1 104.69(12) . . yes C2 P1 Au1 113.74(10) 7_565 . yes C2 P1 Au1 113.74(10) . . yes C1 P1 Au1 113.35(13) . . yes C3 P2 C3 105.20(19) 7_565 . yes C3 P2 C4 104.91(12) 7_565 . yes C3 P2 C4 104.91(12) . . yes C3 P2 Au1 113.23(9) 7_565 . yes C3 P2 Au1 113.23(9) . . yes C4 P2 Au1 114.43(13) . . yes F2C P3 F2C 133.0(8) 7 . yes F2C P3 F4 88.7(4) 7 . yes F2C P3 F4 88.7(4) . . yes F2C P3 F1 90.8(4) 7 . yes F2C P3 F1 90.8(4) . . yes F4 P3 F1 178.9(2) . . yes F2C P3 F3B 160.4(5) 7 . yes F2C P3 F3B 66.6(5) . . yes F4 P3 F3B 91.3(2) . . yes F1 P3 F3B 89.5(2) . . yes F2C P3 F3B 66.6(5) 7 7 yes F2C P3 F3B 160.4(5) . 7 yes F4 P3 F3B 91.3(2) . 7 yes F1 P3 F3B 89.5(2) . 7 yes F3B P3 F3B 93.9(6) . 7 yes F2C P3 F3C 137.6(5) 7 . yes F2C P3 F3C 89.2(5) . . yes F4 P3 F3C 87.9(3) . . yes F1 P3 F3C 93.2(3) . . yes F3B P3 F3C 22.9(3) . . yes F3B P3 F3C 71.3(5) 7 . yes F2C P3 F3C 89.2(5) 7 7 yes F2C P3 F3C 137.6(5) . 7 yes F4 P3 F3C 87.9(3) . 7 yes F1 P3 F3C 93.2(3) . 7 yes F3B P3 F3C 71.3(5) . 7 yes F3B P3 F3C 22.9(3) 7 7 yes F3C P3 F3C 48.5(7) . 7 yes F2C P3 F2 43.2(5) 7 7 yes F2C P3 F2 90.0(6) . 7 yes F4 P3 F2 92.2(4) . 7 yes F1 P3 F2 86.8(4) . 7 yes F3B P3 F2 156.2(5) . 7 yes F3B P3 F2 109.5(5) 7 7 yes F3C P3 F2 179.2(5) . 7 yes F3C P3 F2 132.3(5) 7 7 yes F2C P3 F2 90.0(6) 7 . yes F2C P3 F2 43.2(5) . . yes F4 P3 F2 92.2(4) . . yes F1 P3 F2 86.8(4) . . yes F3B P3 F2 109.5(5) . . yes F3B P3 F2 156.3(5) 7 . yes F3C P3 F2 132.3(5) . . yes F3C P3 F2 179.2(5) 7 . yes F2 P3 F2 46.8(8) 7 . yes F2C P3 F3A 178.0(5) 7 . yes F2C P3 F3A 45.3(5) . . yes F4 P3 F3A 92.2(3) . . yes F1 P3 F3A 88.2(3) . . yes F3B P3 F3A 21.4(3) . . yes F3B P3 F3A 115.1(5) 7 . yes F3C P3 F3A 44.2(4) . . yes F3C P3 F3A 92.6(5) 7 . yes F2 P3 F3A 134.9(5) 7 . yes F2 P3 F3A 88.2(5) . . yes F2C P3 F3A 45.3(5) 7 7 yes F2C P3 F3A 178.0(5) . 7 yes F4 P3 F3A 92.3(3) . 7 yes F1 P3 F3A 88.2(3) . 7 yes F3B P3 F3A 115.2(5) . 7 yes F3B P3 F3A 21.4(3) 7 7 yes F3C P3 F3A 92.6(5) . 7 yes F3C P3 F3A 44.2(4) 7 7 yes F2 P3 F3A 88.2(5) 7 7 yes F2 P3 F3A 134.9(5) . 7 yes F3A P3 F3A 136.4(6) . 7 yes P1 C1 H11 112(3) . . ? P1 C1 H12 106.4(18) . . ? H11 C1 H12 103(2) . . ? P1 C2 H21 109.5 . . ? P1 C2 H22 109.5 . . ? H21 C2 H22 109.5 . . ? P1 C2 H23 109.5 . . ? H21 C2 H23 109.5 . . ? H22 C2 H23 109.5 . . ? P2 C3 H31 109.5 . . ? P2 C3 H32 109.5 . . ? H31 C3 H32 109.5 . . ? P2 C3 H33 109.5 . . ? H31 C3 H33 109.5 . . ? H32 C3 H33 109.5 . . ? P2 C4 H41 116(3) . . ? P2 C4 H42 107.7(19) . . ? H41 C4 H42 106(2) . . ? F2 F2 P3 66.6(4) 7 . yes F3C F3C P3 65.8(3) 7 . yes _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.280 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.143 # File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison. #===END