Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Maravanji Balakrishna' 'Joel Mague' 'Benudhar Punji' _publ_contact_author_name 'Maravanji Balakrishna' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Powai Mumbai 400076 INDIA ; _publ_contact_author_email KRISHNA@IITB.AC.IN _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Bis(2-diphenylphosphinoxynaphthalen-1-yl)methane: Transition Metal Chemistry, Suzuki Cross-Coupling Reactions and Homogeneous Hydrogenation of Olefins ; data_msb181 _database_code_depnum_ccdc_archive 'CCDC 279236' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetracarbonyl(bis(2-diphenylphosphinoxynaphthalen-1-yl) methane)molybdenum(0) dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H36 Cl2 Mo O6 P2' _chemical_formula_sum 'C50 H36 Cl2 Mo O6 P2' _chemical_formula_weight 961.57 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7256(7) _cell_length_b 11.4602(8) _cell_length_c 17.609(1) _cell_angle_alpha 77.918(1) _cell_angle_beta 83.014(1) _cell_angle_gamma 88.284(1) _cell_volume 2100.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8313 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.26 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8182 _exptl_absorpt_correction_T_max 0.9443 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18882 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.30 _reflns_number_total 9744 _reflns_number_gt 7857 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms were placed in calculated positions (C---H = 0.95 \%A) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+1.0851P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9744 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Mo Mo 0.67261(2) 0.88016(2) 0.639063(15) 0.01156(8) Uani 1 1 d . . . P1 P 0.81048(7) 0.70968(7) 0.68655(4) 0.01116(16) Uani 1 1 d . . . P2 P 0.57726(7) 0.90188(7) 0.77345(5) 0.01180(16) Uani 1 1 d . . . O1 O 0.80075(19) 0.66448(18) 0.78182(12) 0.0127(4) Uani 1 1 d . . . O2 O 0.56418(19) 0.78321(17) 0.84487(12) 0.0129(4) Uani 1 1 d . . . O3 O 0.7883(2) 0.8573(2) 0.46943(13) 0.0257(6) Uani 1 1 d . . . O4 O 0.9006(2) 1.0526(2) 0.64063(15) 0.0267(6) Uani 1 1 d . . . O5 O 0.5389(2) 1.1015(2) 0.54437(14) 0.0256(6) Uani 1 1 d . . . O6 O 0.4612(2) 0.7104(2) 0.61193(13) 0.0201(5) Uani 1 1 d . . . C1 C 0.9737(3) 0.7549(3) 0.65819(18) 0.0145(6) Uani 1 1 d . . . C2 C 1.0292(3) 0.7750(3) 0.58036(18) 0.0162(6) Uani 1 1 d . . . H2 H 0.9858 0.7532 0.5415 0.019 Uiso 1 1 calc R . . C3 C 1.1470(3) 0.8264(3) 0.5598(2) 0.0206(7) Uani 1 1 d . . . H3 H 1.1845 0.8385 0.5070 0.025 Uiso 1 1 calc R . . C4 C 1.2103(3) 0.8602(3) 0.6153(2) 0.0217(7) Uani 1 1 d . . . H4 H 1.2908 0.8958 0.6007 0.026 Uiso 1 1 calc R . . C5 C 1.1568(3) 0.8423(3) 0.6920(2) 0.0196(7) Uani 1 1 d . . . H5 H 1.2004 0.8658 0.7302 0.023 Uiso 1 1 calc R . . C6 C 1.0387(3) 0.7899(3) 0.71373(19) 0.0176(7) Uani 1 1 d . . . H6 H 1.0022 0.7779 0.7667 0.021 Uiso 1 1 calc R . . C7 C 0.7899(3) 0.5706(3) 0.65472(17) 0.0140(6) Uani 1 1 d . . . C8 C 0.8756(3) 0.5194(3) 0.60538(19) 0.0210(7) Uani 1 1 d . . . H8 H 0.9538 0.5575 0.5854 0.025 Uiso 1 1 calc R . . C9 C 0.8486(4) 0.4137(3) 0.5850(2) 0.0272(8) Uani 1 1 d . . . H9 H 0.9078 0.3803 0.5507 0.033 Uiso 1 1 calc R . . C10 C 0.7356(3) 0.3558(3) 0.6142(2) 0.0241(8) Uani 1 1 d . . . H10 H 0.7171 0.2835 0.5997 0.029 Uiso 1 1 calc R . . C11 C 0.6505(3) 0.4043(3) 0.6644(2) 0.0224(7) Uani 1 1 d . . . H11 H 0.5735 0.3646 0.6852 0.027 Uiso 1 1 calc R . . C12 C 0.6773(3) 0.5110(3) 0.68449(18) 0.0162(6) Uani 1 1 d . . . H12 H 0.6181 0.5439 0.7190 0.019 Uiso 1 1 calc R . . C13 C 0.8586(3) 0.5658(3) 0.82470(17) 0.0125(6) Uani 1 1 d . . . C14 C 0.9661(3) 0.5117(3) 0.79302(18) 0.0151(6) Uani 1 1 d . . . H14 H 0.9972 0.5367 0.7393 0.018 Uiso 1 1 calc R . . C15 C 1.0255(3) 0.4228(3) 0.83997(18) 0.0150(6) Uani 1 1 d . . . H15 H 1.0972 0.3850 0.8183 0.018 Uiso 1 1 calc R . . C16 C 0.9820(3) 0.3859(3) 0.92048(17) 0.0126(6) Uani 1 1 d . . . C17 C 1.0490(3) 0.2993(3) 0.97037(19) 0.0155(6) Uani 1 1 d . . . H17 H 1.1236 0.2648 0.9495 0.019 Uiso 1 1 calc R . . C18 C 1.0070(3) 0.2652(3) 1.04804(19) 0.0166(7) Uani 1 1 d . . . H18 H 1.0519 0.2069 1.0810 0.020 Uiso 1 1 calc R . . C19 C 0.8972(3) 0.3165(3) 1.07885(18) 0.0166(7) Uani 1 1 d . . . H19 H 0.8683 0.2925 1.1329 0.020 Uiso 1 1 calc R . . C20 C 0.8309(3) 0.4003(3) 1.03260(18) 0.0143(6) Uani 1 1 d . . . H20 H 0.7568 0.4336 1.0551 0.017 Uiso 1 1 calc R . . C21 C 0.8707(3) 0.4386(3) 0.95152(17) 0.0125(6) Uani 1 1 d . . . C22 C 0.8053(3) 0.5281(3) 0.90082(17) 0.0115(6) Uani 1 1 d . . . C23 C 0.6845(3) 0.5855(3) 0.92947(17) 0.0115(6) Uani 1 1 d . . . H23A H 0.6999 0.6714 0.9258 0.014 Uiso 1 1 calc R . . H23B H 0.6608 0.5490 0.9853 0.014 Uiso 1 1 calc R . . C24 C 0.5746(3) 0.5735(3) 0.88434(17) 0.0117(6) Uani 1 1 d . . . C25 C 0.5229(3) 0.4585(3) 0.88636(17) 0.0126(6) Uani 1 1 d . . . C26 C 0.5655(3) 0.3516(3) 0.93366(18) 0.0150(6) Uani 1 1 d . . . H26 H 0.6301 0.3558 0.9655 0.018 Uiso 1 1 calc R . . C27 C 0.5150(3) 0.2433(3) 0.93404(19) 0.0175(7) Uani 1 1 d . . . H27 H 0.5442 0.1735 0.9665 0.021 Uiso 1 1 calc R . . C28 C 0.4207(3) 0.2341(3) 0.8871(2) 0.0187(7) Uani 1 1 d . . . H28 H 0.3872 0.1583 0.8872 0.022 Uiso 1 1 calc R . . C29 C 0.3772(3) 0.3349(3) 0.84101(19) 0.0164(6) Uani 1 1 d . . . H29 H 0.3142 0.3280 0.8087 0.020 Uiso 1 1 calc R . . C30 C 0.4242(3) 0.4488(3) 0.84073(18) 0.0135(6) Uani 1 1 d . . . C31 C 0.3749(3) 0.5538(3) 0.79656(18) 0.0140(6) Uani 1 1 d . . . H31 H 0.3097 0.5481 0.7656 0.017 Uiso 1 1 calc R . . C32 C 0.4203(3) 0.6631(3) 0.79807(17) 0.0130(6) Uani 1 1 d . . . H32 H 0.3843 0.7332 0.7699 0.016 Uiso 1 1 calc R . . C33 C 0.5204(3) 0.6721(3) 0.84122(17) 0.0110(6) Uani 1 1 d . . . C34 C 0.4205(3) 0.9688(3) 0.78675(18) 0.0144(6) Uani 1 1 d . . . C35 C 0.3834(3) 1.0649(3) 0.73112(19) 0.0174(7) Uani 1 1 d . . . H35 H 0.4401 1.0958 0.6861 0.021 Uiso 1 1 calc R . . C36 C 0.2650(3) 1.1161(3) 0.7405(2) 0.0210(7) Uani 1 1 d . . . H36 H 0.2415 1.1815 0.7020 0.025 Uiso 1 1 calc R . . C37 C 0.1810(3) 1.0722(3) 0.8059(2) 0.0212(7) Uani 1 1 d . . . H37 H 0.1000 1.1071 0.8124 0.025 Uiso 1 1 calc R . . C38 C 0.2165(3) 0.9763(3) 0.8621(2) 0.0188(7) Uani 1 1 d . . . H38 H 0.1593 0.9452 0.9068 0.023 Uiso 1 1 calc R . . C39 C 0.3356(3) 0.9261(3) 0.85263(18) 0.0153(6) Uani 1 1 d . . . H39 H 0.3596 0.8618 0.8917 0.018 Uiso 1 1 calc R . . C40 C 0.6680(3) 0.9900(3) 0.82210(18) 0.0140(6) Uani 1 1 d . . . C41 C 0.7081(3) 0.9442(3) 0.8953(2) 0.0210(7) Uani 1 1 d . . . H41 H 0.6843 0.8659 0.9223 0.025 Uiso 1 1 calc R . . C42 C 0.7822(4) 1.0119(3) 0.9286(2) 0.0274(8) Uani 1 1 d . . . H42 H 0.8096 0.9796 0.9781 0.033 Uiso 1 1 calc R . . C43 C 0.8167(3) 1.1270(3) 0.8898(2) 0.0247(8) Uani 1 1 d . . . H43 H 0.8690 1.1727 0.9122 0.030 Uiso 1 1 calc R . . C44 C 0.7746(3) 1.1744(3) 0.8188(2) 0.0242(8) Uani 1 1 d . . . H44 H 0.7961 1.2538 0.7928 0.029 Uiso 1 1 calc R . . C45 C 0.7007(3) 1.1060(3) 0.7851(2) 0.0201(7) Uani 1 1 d . . . H45 H 0.6723 1.1393 0.7361 0.024 Uiso 1 1 calc R . . C46 C 0.7482(3) 0.8645(3) 0.53158(19) 0.0156(6) Uani 1 1 d . . . C47 C 0.8189(3) 0.9907(3) 0.64313(18) 0.0171(7) Uani 1 1 d . . . C48 C 0.5832(3) 1.0215(3) 0.58246(18) 0.0168(7) Uani 1 1 d . . . C49 C 0.5353(3) 0.7708(3) 0.62523(17) 0.0137(6) Uani 1 1 d . . . C50 C 0.3427(4) 0.4795(3) 0.5839(2) 0.0304(9) Uani 1 1 d . . . H50A H 0.3354 0.5463 0.5388 0.037 Uiso 1 1 calc R . . H50B H 0.4000 0.5045 0.6175 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.19346(9) 0.44868(9) 0.63767(6) 0.0378(2) Uani 1 1 d . . . Cl2 Cl 0.40627(9) 0.35462(9) 0.55000(6) 0.0387(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.01221(14) 0.01126(13) 0.01089(13) -0.00098(9) -0.00251(9) 0.00027(9) P1 0.0106(4) 0.0127(4) 0.0098(4) -0.0011(3) -0.0018(3) 0.0001(3) P2 0.0118(4) 0.0104(4) 0.0131(4) -0.0016(3) -0.0024(3) -0.0001(3) O1 0.0120(11) 0.0139(10) 0.0100(10) 0.0020(8) -0.0007(8) 0.0020(8) O2 0.0157(11) 0.0089(10) 0.0140(11) -0.0011(8) -0.0041(8) -0.0007(8) O3 0.0315(14) 0.0295(14) 0.0147(12) -0.0028(10) -0.0004(10) -0.0012(11) O4 0.0216(13) 0.0230(13) 0.0357(15) -0.0055(11) -0.0038(11) -0.0073(11) O5 0.0328(14) 0.0214(13) 0.0207(13) -0.0005(10) -0.0049(11) 0.0106(11) O6 0.0186(12) 0.0224(12) 0.0201(12) -0.0041(10) -0.0051(10) -0.0024(10) C1 0.0122(15) 0.0128(15) 0.0171(16) -0.0002(12) -0.0013(12) 0.0016(12) C2 0.0163(16) 0.0159(16) 0.0156(16) -0.0015(12) -0.0020(12) 0.0016(12) C3 0.0175(17) 0.0225(17) 0.0172(16) 0.0032(13) 0.0026(13) 0.0020(14) C4 0.0127(16) 0.0204(17) 0.0288(19) 0.0015(14) -0.0003(14) -0.0026(13) C5 0.0154(16) 0.0202(17) 0.0239(18) -0.0032(14) -0.0081(13) 0.0005(13) C6 0.0176(16) 0.0196(17) 0.0145(16) -0.0008(13) -0.0025(12) 0.0011(13) C7 0.0156(15) 0.0168(15) 0.0098(14) -0.0013(12) -0.0059(12) 0.0041(12) C8 0.0185(17) 0.0211(17) 0.0216(17) -0.0037(14) 0.0041(13) -0.0019(13) C9 0.032(2) 0.0240(19) 0.0259(19) -0.0108(15) 0.0065(16) 0.0003(16) C10 0.037(2) 0.0151(16) 0.0215(18) -0.0081(14) -0.0017(15) -0.0030(15) C11 0.0224(18) 0.0200(17) 0.0244(18) -0.0021(14) -0.0044(14) -0.0044(14) C12 0.0163(16) 0.0169(16) 0.0154(16) -0.0028(13) -0.0036(12) 0.0037(13) C13 0.0117(15) 0.0110(14) 0.0145(15) 0.0002(12) -0.0051(12) 0.0004(11) C14 0.0134(15) 0.0179(16) 0.0142(15) -0.0050(12) 0.0003(12) 0.0005(12) C15 0.0105(15) 0.0164(15) 0.0187(16) -0.0058(13) -0.0007(12) 0.0013(12) C16 0.0116(15) 0.0113(14) 0.0150(15) -0.0010(12) -0.0040(12) -0.0019(11) C17 0.0111(15) 0.0114(15) 0.0242(17) -0.0019(13) -0.0058(12) -0.0027(12) C18 0.0178(16) 0.0119(15) 0.0194(16) 0.0034(12) -0.0109(13) -0.0003(12) C19 0.0199(16) 0.0175(16) 0.0113(15) 0.0013(12) -0.0045(12) -0.0027(13) C20 0.0126(15) 0.0143(15) 0.0158(16) -0.0026(12) -0.0023(12) -0.0015(12) C21 0.0139(15) 0.0097(14) 0.0139(15) -0.0017(12) -0.0027(12) -0.0029(11) C22 0.0091(14) 0.0121(14) 0.0143(15) -0.0042(12) -0.0026(11) -0.0010(11) C23 0.0122(15) 0.0125(14) 0.0093(14) -0.0017(11) -0.0003(11) -0.0004(11) C24 0.0109(14) 0.0129(14) 0.0106(14) -0.0023(11) 0.0014(11) -0.0001(11) C25 0.0114(15) 0.0125(14) 0.0132(15) -0.0028(12) 0.0008(11) 0.0005(12) C26 0.0105(15) 0.0164(15) 0.0165(16) -0.0013(12) 0.0008(12) -0.0012(12) C27 0.0160(16) 0.0133(15) 0.0203(17) 0.0012(13) 0.0006(13) 0.0039(12) C28 0.0159(16) 0.0108(15) 0.0292(19) -0.0053(13) 0.0002(14) -0.0026(12) C29 0.0122(15) 0.0170(16) 0.0208(17) -0.0060(13) -0.0010(12) -0.0043(12) C30 0.0097(14) 0.0153(15) 0.0150(15) -0.0038(12) 0.0023(11) -0.0006(12) C31 0.0092(14) 0.0194(16) 0.0140(15) -0.0042(12) -0.0022(11) -0.0003(12) C32 0.0129(15) 0.0144(15) 0.0101(14) 0.0005(12) -0.0005(11) 0.0017(12) C33 0.0119(14) 0.0093(14) 0.0124(15) -0.0042(11) 0.0008(11) -0.0037(11) C34 0.0125(15) 0.0125(15) 0.0201(16) -0.0054(12) -0.0052(12) -0.0004(12) C35 0.0189(17) 0.0157(16) 0.0168(16) -0.0020(13) -0.0014(13) 0.0009(13) C36 0.0211(18) 0.0159(16) 0.0260(18) -0.0034(14) -0.0057(14) 0.0047(13) C37 0.0135(16) 0.0224(17) 0.0309(19) -0.0130(15) -0.0027(14) 0.0026(13) C38 0.0154(16) 0.0190(16) 0.0233(17) -0.0084(14) 0.0012(13) -0.0046(13) C39 0.0190(16) 0.0128(15) 0.0139(15) -0.0022(12) -0.0026(12) -0.0003(12) C40 0.0113(15) 0.0127(15) 0.0194(16) -0.0071(12) -0.0008(12) 0.0004(12) C41 0.0248(18) 0.0159(16) 0.0232(18) -0.0030(13) -0.0084(14) 0.0002(14) C42 0.034(2) 0.0233(18) 0.030(2) -0.0103(15) -0.0167(16) 0.0041(16) C43 0.0170(17) 0.0250(18) 0.038(2) -0.0166(16) -0.0069(15) -0.0001(14) C44 0.0225(18) 0.0171(17) 0.033(2) -0.0089(15) 0.0035(15) -0.0082(14) C45 0.0222(17) 0.0178(16) 0.0200(17) -0.0042(13) -0.0005(13) -0.0026(13) C46 0.0140(15) 0.0151(15) 0.0174(16) -0.0002(13) -0.0062(12) -0.0012(12) C47 0.0192(17) 0.0152(16) 0.0157(16) -0.0017(13) -0.0010(13) 0.0018(13) C48 0.0181(16) 0.0193(16) 0.0136(16) -0.0059(13) -0.0002(12) 0.0007(13) C49 0.0160(16) 0.0154(15) 0.0086(14) -0.0007(12) -0.0010(12) 0.0037(12) C50 0.029(2) 0.0256(19) 0.037(2) -0.0095(17) 0.0007(17) 0.0010(16) Cl1 0.0285(5) 0.0445(6) 0.0365(6) -0.0059(5) 0.0055(4) 0.0085(4) Cl2 0.0288(5) 0.0433(6) 0.0503(6) -0.0299(5) 0.0065(4) -0.0054(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 Mo C48 2.000(3) . ? Mo C46 2.008(3) . ? Mo C49 2.031(3) . ? Mo C47 2.063(3) . ? Mo P1 2.4793(8) . ? Mo P2 2.5199(8) . ? P1 O1 1.640(2) . ? P1 C1 1.821(3) . ? P1 C7 1.825(3) . ? P2 O2 1.644(2) . ? P2 C40 1.824(3) . ? P2 C34 1.837(3) . ? O1 C13 1.395(3) . ? O2 C33 1.386(3) . ? O3 C46 1.145(4) . ? O4 C47 1.135(4) . ? O5 C48 1.145(4) . ? O6 C49 1.145(4) . ? C1 C6 1.396(4) . ? C1 C2 1.401(4) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.379(5) . ? C3 H3 0.9500 . ? C4 C5 1.378(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.390(4) . ? C7 C12 1.394(4) . ? C8 C9 1.382(5) . ? C8 H8 0.9500 . ? C9 C10 1.387(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C22 1.377(4) . ? C13 C14 1.404(4) . ? C14 C15 1.365(4) . ? C14 H14 0.9500 . ? C15 C16 1.416(4) . ? C15 H15 0.9500 . ? C16 C17 1.420(4) . ? C16 C21 1.423(4) . ? C17 C18 1.365(4) . ? C17 H17 0.9500 . ? C18 C19 1.401(5) . ? C18 H18 0.9500 . ? C19 C20 1.365(4) . ? C19 H19 0.9500 . ? C20 C21 1.419(4) . ? C20 H20 0.9500 . ? C21 C22 1.437(4) . ? C22 C23 1.516(4) . ? C23 C24 1.524(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C33 1.378(4) . ? C24 C25 1.437(4) . ? C25 C30 1.425(4) . ? C25 C26 1.426(4) . ? C26 C27 1.368(4) . ? C26 H26 0.9500 . ? C27 C28 1.401(5) . ? C27 H27 0.9500 . ? C28 C29 1.371(4) . ? C28 H28 0.9500 . ? C29 C30 1.412(4) . ? C29 H29 0.9500 . ? C30 C31 1.416(4) . ? C31 C32 1.364(4) . ? C31 H31 0.9500 . ? C32 C33 1.407(4) . ? C32 H32 0.9500 . ? C34 C39 1.395(4) . ? C34 C35 1.395(4) . ? C35 C36 1.389(4) . ? C35 H35 0.9500 . ? C36 C37 1.387(5) . ? C36 H36 0.9500 . ? C37 C38 1.394(5) . ? C37 H37 0.9500 . ? C38 C39 1.391(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.387(4) . ? C40 C41 1.400(4) . ? C41 C42 1.386(5) . ? C41 H41 0.9500 . ? C42 C43 1.390(5) . ? C42 H42 0.9500 . ? C43 C44 1.380(5) . ? C43 H43 0.9500 . ? C44 C45 1.392(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C50 Cl2 1.753(4) . ? C50 Cl1 1.762(4) . ? C50 H50A 0.9900 . ? C50 H50B 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 C48 Mo C46 84.56(12) . . ? C48 Mo C49 90.35(12) . . ? C46 Mo C49 85.93(12) . . ? C48 Mo C47 88.93(13) . . ? C46 Mo C47 88.98(12) . . ? C49 Mo C47 174.91(12) . . ? C48 Mo P1 169.39(9) . . ? C46 Mo P1 85.43(9) . . ? C49 Mo P1 92.45(9) . . ? C47 Mo P1 87.37(9) . . ? C48 Mo P2 94.93(9) . . ? C46 Mo P2 179.45(9) . . ? C49 Mo P2 94.28(8) . . ? C47 Mo P2 90.81(9) . . ? P1 Mo P2 95.07(3) . . ? O1 P1 C1 103.91(13) . . ? O1 P1 C7 101.96(12) . . ? C1 P1 C7 107.88(14) . . ? O1 P1 Mo 115.61(8) . . ? C1 P1 Mo 108.90(10) . . ? C7 P1 Mo 117.50(10) . . ? O2 P2 C40 96.14(13) . . ? O2 P2 C34 100.94(13) . . ? C40 P2 C34 101.20(14) . . ? O2 P2 Mo 119.13(8) . . ? C40 P2 Mo 115.50(10) . . ? C34 P2 Mo 119.91(10) . . ? C13 O1 P1 128.33(19) . . ? C33 O2 P2 126.41(19) . . ? C6 C1 C2 118.5(3) . . ? C6 C1 P1 118.2(2) . . ? C2 C1 P1 122.4(2) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 118.3(3) . . ? C8 C7 P1 126.2(3) . . ? C12 C7 P1 115.5(2) . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 120.5(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 119.4(3) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.9(3) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C22 C13 O1 115.3(3) . . ? C22 C13 C14 122.5(3) . . ? O1 C13 C14 122.2(3) . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 121.1(3) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C17 121.0(3) . . ? C15 C16 C21 119.0(3) . . ? C17 C16 C21 120.0(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.7(3) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 121.2(3) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 121.2(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 117.3(3) . . ? C20 C21 C22 123.2(3) . . ? C16 C21 C22 119.5(3) . . ? C13 C22 C21 118.1(3) . . ? C13 C22 C23 119.6(3) . . ? C21 C22 C23 122.3(3) . . ? C22 C23 C24 114.2(2) . . ? C22 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C22 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C33 C24 C25 117.8(3) . . ? C33 C24 C23 121.4(3) . . ? C25 C24 C23 120.8(3) . . ? C30 C25 C26 117.6(3) . . ? C30 C25 C24 119.9(3) . . ? C26 C25 C24 122.5(3) . . ? C27 C26 C25 121.2(3) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 120.8(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 119.7(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 121.2(3) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C29 C30 C31 121.5(3) . . ? C29 C30 C25 119.4(3) . . ? C31 C30 C25 119.1(3) . . ? C32 C31 C30 120.6(3) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C24 C33 O2 117.3(3) . . ? C24 C33 C32 122.4(3) . . ? O2 C33 C32 120.3(3) . . ? C39 C34 C35 118.1(3) . . ? C39 C34 P2 121.3(2) . . ? C35 C34 P2 120.6(2) . . ? C36 C35 C34 121.1(3) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C37 C36 C35 120.2(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 119.4(3) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 120.1(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 121.1(3) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? C45 C40 C41 118.4(3) . . ? C45 C40 P2 119.3(2) . . ? C41 C40 P2 122.3(2) . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 120.1(3) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.7(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.0(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C40 C45 C44 121.0(3) . . ? C40 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? O3 C46 Mo 178.0(3) . . ? O4 C47 Mo 175.9(3) . . ? O5 C48 Mo 174.0(3) . . ? O6 C49 Mo 175.1(3) . . ? Cl2 C50 Cl1 111.5(2) . . ? Cl2 C50 H50A 109.3 . . ? Cl1 C50 H50A 109.3 . . ? Cl2 C50 H50B 109.3 . . ? Cl1 C50 H50B 109.3 . . ? H50A C50 H50B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.913 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.106 data_msb167b _database_code_depnum_ccdc_archive 'CCDC 279237' _audit_creation_method SHELXL-97 _chemical_name_systematic ; \h^3^-allyl(bis(2-diphenylphosphinoxynaphthalen-1-yl) methane)palladium(II) tetrafluoroborate bis(dichloro methane) solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H43 B Cl4 F4 O2 P2 Pd' _chemical_formula_sum 'C50 H43 B Cl4 F4 O2 P2 Pd' _chemical_formula_weight 1072.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 19.924(2) _cell_length_b 10.741(1) _cell_length_c 22.488(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.071(1) _cell_angle_gamma 90.00 _cell_volume 4574.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7483 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.24 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7016 _exptl_absorpt_correction_T_max 0.9433 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39221 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.31 _reflns_number_total 10938 _reflns_number_gt 9427 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two alternate locations of the allyl group were found which are related by a 180\% rotation about a line from the metal atom to the centroid of the allyl group. These are present in a 57/43 ratio and were refined with restraints making corresponding distances in the two orientations equal. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+16.8239P] 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 10938 _refine_ls_number_parameters 581 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1436 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Pd Pd 0.250608(13) 0.05823(2) 0.093291(12) 0.01457(9) Uani 1 1 d . . . P1 P 0.31983(5) 0.23042(8) 0.12698(4) 0.01386(17) Uani 1 1 d . A . P2 P 0.25398(5) 0.05091(8) -0.00744(4) 0.01522(18) Uani 1 1 d . A . O1 O 0.36471(13) 0.2580(2) 0.07925(11) 0.0155(5) Uani 1 1 d . . . O2 O 0.33362(13) 0.0267(2) -0.01017(11) 0.0174(5) Uani 1 1 d . . . C1 C 0.26445(18) 0.3658(3) 0.12296(16) 0.0160(7) Uani 1 1 d . . . C2 C 0.22090(19) 0.3705(4) 0.16130(17) 0.0204(7) Uani 1 1 d . A . H2 H 0.2233 0.3064 0.1910 0.025 Uiso 1 1 calc R . . C3 C 0.1743(2) 0.4689(4) 0.15584(19) 0.0246(8) Uani 1 1 d . . . H3 H 0.1450 0.4722 0.1821 0.029 Uiso 1 1 calc R A . C4 C 0.1701(2) 0.5629(4) 0.1121(2) 0.0286(9) Uani 1 1 d . A . H4 H 0.1386 0.6308 0.1088 0.034 Uiso 1 1 calc R . . C5 C 0.2124(2) 0.5564(4) 0.0732(2) 0.0276(9) Uani 1 1 d . . . H5 H 0.2093 0.6197 0.0429 0.033 Uiso 1 1 calc R A . C6 C 0.2590(2) 0.4586(3) 0.07827(19) 0.0211(7) Uani 1 1 d . A . H6 H 0.2873 0.4545 0.0513 0.025 Uiso 1 1 calc R . . C7 C 0.38126(18) 0.2273(3) 0.20541(16) 0.0154(6) Uani 1 1 d . . . C8 C 0.3925(2) 0.3298(4) 0.24589(17) 0.0205(7) Uani 1 1 d . A . H8 H 0.3674 0.4052 0.2325 0.025 Uiso 1 1 calc R . . C9 C 0.4404(2) 0.3207(4) 0.30553(19) 0.0257(8) Uani 1 1 d . . . H9 H 0.4482 0.3902 0.3330 0.031 Uiso 1 1 calc R A . C10 C 0.4769(2) 0.2107(4) 0.32531(18) 0.0253(8) Uani 1 1 d . A . H10 H 0.5091 0.2046 0.3664 0.030 Uiso 1 1 calc R . . C11 C 0.4664(2) 0.1095(4) 0.28521(19) 0.0237(8) Uani 1 1 d . . . H11 H 0.4922 0.0348 0.2985 0.028 Uiso 1 1 calc R A . C12 C 0.41834(19) 0.1172(3) 0.22579(18) 0.0201(7) Uani 1 1 d . A . H12 H 0.4106 0.0471 0.1987 0.024 Uiso 1 1 calc R . . C13 C 0.42593(17) 0.3298(3) 0.08817(16) 0.0146(6) Uani 1 1 d . A . C14 C 0.43616(19) 0.4407(3) 0.12308(17) 0.0178(7) Uani 1 1 d . . . H14 H 0.4043 0.4641 0.1450 0.021 Uiso 1 1 calc R A . C15 C 0.49290(19) 0.5143(3) 0.12485(18) 0.0193(7) Uani 1 1 d . A . H15 H 0.5009 0.5886 0.1489 0.023 Uiso 1 1 calc R . . C16 C 0.53969(19) 0.4813(3) 0.09143(17) 0.0178(7) Uani 1 1 d . . . C17 C 0.5966(2) 0.5616(3) 0.09069(19) 0.0221(7) Uani 1 1 d . A . H17 H 0.6037 0.6371 0.1138 0.026 Uiso 1 1 calc R . . C18 C 0.6412(2) 0.5311(4) 0.05708(19) 0.0227(8) Uani 1 1 d . . . H18 H 0.6785 0.5855 0.0563 0.027 Uiso 1 1 calc R A . C19 C 0.63106(19) 0.4188(3) 0.02398(18) 0.0207(7) Uani 1 1 d . A . H19 H 0.6625 0.3967 0.0014 0.025 Uiso 1 1 calc R . . C20 C 0.57689(19) 0.3401(3) 0.02341(17) 0.0184(7) Uani 1 1 d . . . H20 H 0.5709 0.2651 -0.0001 0.022 Uiso 1 1 calc R A . C21 C 0.52945(18) 0.3687(3) 0.05735(16) 0.0149(6) Uani 1 1 d . A . C22 C 0.47114(18) 0.2896(3) 0.05671(16) 0.0146(6) Uani 1 1 d . . . C23 C 0.45612(18) 0.1700(3) 0.01891(16) 0.0158(6) Uani 1 1 d . A . H23A H 0.4113 0.1800 -0.0155 0.019 Uiso 1 1 calc R . . H23B H 0.4942 0.1568 -0.0002 0.019 Uiso 1 1 calc R . . C24 C 0.45067(18) 0.0555(3) 0.05604(16) 0.0149(6) Uani 1 1 d . . . C25 C 0.50936(18) 0.0081(3) 0.10580(17) 0.0175(7) Uani 1 1 d . A . C26 C 0.57771(19) 0.0628(4) 0.12117(18) 0.0211(7) Uani 1 1 d . . . H26 H 0.5849 0.1332 0.0983 0.025 Uiso 1 1 calc R A . C27 C 0.6334(2) 0.0156(4) 0.16833(19) 0.0242(8) Uani 1 1 d . A . H27 H 0.6787 0.0531 0.1775 0.029 Uiso 1 1 calc R . . C28 C 0.6239(2) -0.0882(4) 0.20325(19) 0.0253(8) Uani 1 1 d . . . H28 H 0.6627 -0.1200 0.2359 0.030 Uiso 1 1 calc R A . C29 C 0.5588(2) -0.1436(4) 0.19034(18) 0.0238(8) Uani 1 1 d . A . H29 H 0.5525 -0.2131 0.2143 0.029 Uiso 1 1 calc R . . C30 C 0.50083(19) -0.0967(3) 0.14103(17) 0.0189(7) Uani 1 1 d . . . C31 C 0.4336(2) -0.1570(3) 0.12563(17) 0.0195(7) Uani 1 1 d . A . H31 H 0.4270 -0.2257 0.1498 0.023 Uiso 1 1 calc R . . C32 C 0.3790(2) -0.1161(3) 0.07623(17) 0.0187(7) Uani 1 1 d . . . H32 H 0.3348 -0.1580 0.0649 0.022 Uiso 1 1 calc R A . C33 C 0.38860(18) -0.0106(3) 0.04199(16) 0.0163(7) Uani 1 1 d . A . C34 C 0.20572(19) -0.0724(3) -0.05791(17) 0.0176(7) Uani 1 1 d . . . C35 C 0.2396(2) -0.1724(4) -0.07494(18) 0.0225(7) Uani 1 1 d . A . H35 H 0.2896 -0.1773 -0.0602 0.027 Uiso 1 1 calc R . . C36 C 0.2008(2) -0.2660(4) -0.1135(2) 0.0291(9) Uani 1 1 d . . . H36 H 0.2242 -0.3351 -0.1246 0.035 Uiso 1 1 calc R A . C37 C 0.1279(2) -0.2574(4) -0.1355(2) 0.0305(9) Uani 1 1 d . A . H37 H 0.1013 -0.3202 -0.1624 0.037 Uiso 1 1 calc R . . C38 C 0.0936(2) -0.1586(4) -0.1186(2) 0.0286(9) Uani 1 1 d . . . H38 H 0.0435 -0.1539 -0.1337 0.034 Uiso 1 1 calc R A . C39 C 0.1320(2) -0.0658(4) -0.07968(19) 0.0237(8) Uani 1 1 d . A . H39 H 0.1082 0.0020 -0.0679 0.028 Uiso 1 1 calc R . . C40 C 0.22764(19) 0.1851(3) -0.05769(16) 0.0173(7) Uani 1 1 d . . . C41 C 0.2478(2) 0.1936(4) -0.11198(19) 0.0242(8) Uani 1 1 d . A . H41 H 0.2779 0.1324 -0.1205 0.029 Uiso 1 1 calc R . . C42 C 0.2236(2) 0.2912(4) -0.15297(19) 0.0285(9) Uani 1 1 d . . . H42 H 0.2377 0.2978 -0.1895 0.034 Uiso 1 1 calc R A . C43 C 0.1785(2) 0.3804(4) -0.1407(2) 0.0303(9) Uani 1 1 d . A . H43 H 0.1602 0.4454 -0.1700 0.036 Uiso 1 1 calc R . . C44 C 0.1604(2) 0.3746(4) -0.0867(2) 0.0276(8) Uani 1 1 d . . . H44 H 0.1315 0.4375 -0.0777 0.033 Uiso 1 1 calc R A . C45 C 0.18464(19) 0.2759(4) -0.04482(18) 0.0214(7) Uani 1 1 d . A . H45 H 0.1716 0.2712 -0.0077 0.026 Uiso 1 1 calc R . . C46 C 0.1823(3) -0.1034(5) 0.0878(2) 0.0414(12) Uani 0.570(8) 1 d PD A 1 H46A H 0.2264 -0.1270 0.0833 0.050 Uiso 0.570(8) 1 calc PR A 1 H46B H 0.1395 -0.1296 0.0579 0.050 Uiso 0.570(8) 1 calc PR A 1 C47 C 0.1804(4) -0.0347(6) 0.1355(3) 0.0237(11) Uani 0.570(8) 1 d PD A 1 H47A H 0.1347 -0.0142 0.1373 0.028 Uiso 0.570(8) 1 calc PR A 1 C48 C 0.2365(2) 0.0118(4) 0.18328(19) 0.0268(8) Uani 0.570(8) 1 d PD A 1 H48A H 0.2836 -0.0053 0.1841 0.032 Uiso 0.570(8) 1 calc PR A 1 H48B H 0.2281 0.0609 0.2154 0.032 Uiso 0.570(8) 1 calc PR A 1 C46A C 0.1823(3) -0.1034(5) 0.0878(2) 0.0414(12) Uani 0.430(8) 1 d PD A 2 H46C H 0.1595 -0.0326 0.0650 0.050 Uiso 0.430(8) 1 calc PR A 2 H46D H 0.1767 -0.1827 0.0683 0.050 Uiso 0.430(8) 1 calc PR A 2 C47A C 0.2217(5) -0.0914(8) 0.1467(4) 0.0237(11) Uani 0.430(8) 1 d PD A 2 H47B H 0.2427 -0.1662 0.1665 0.028 Uiso 0.430(8) 1 calc PR A 2 C48A C 0.2365(2) 0.0118(4) 0.18328(19) 0.0268(8) Uani 0.430(8) 1 d PD A 2 H48C H 0.2173 0.0901 0.1667 0.032 Uiso 0.430(8) 1 calc PR A 2 H48D H 0.2662 0.0059 0.2254 0.032 Uiso 0.430(8) 1 calc PR A 2 B B 0.0897(3) 0.2037(5) 0.2325(2) 0.0270(9) Uani 1 1 d . . . F1 F 0.05173(17) 0.1292(3) 0.26119(13) 0.0420(7) Uani 1 1 d . . . F2 F 0.0543(2) 0.3158(3) 0.21793(17) 0.0581(9) Uani 1 1 d . . . F3 F 0.15656(18) 0.2207(5) 0.26898(17) 0.0770(13) Uani 1 1 d . . . F4 F 0.08861(15) 0.1475(3) 0.17602(12) 0.0381(6) Uani 1 1 d . . . C49 C 0.5964(2) 0.4235(4) 0.2685(2) 0.0311(9) Uani 1 1 d . . . H49A H 0.6084 0.3990 0.3131 0.037 Uiso 1 1 calc R . . H49B H 0.5511 0.4694 0.2571 0.037 Uiso 1 1 calc R . . Cl1 Cl 0.58665(6) 0.28845(10) 0.22169(5) 0.0331(2) Uani 1 1 d . . . Cl2 Cl 0.66328(6) 0.52216(12) 0.25876(6) 0.0403(3) Uani 1 1 d . . . C50 C 0.0386(3) 0.3036(4) 0.0495(2) 0.0356(10) Uani 1 1 d . . . H50A H 0.0564 0.2836 0.0947 0.043 Uiso 1 1 calc R . . H50B H 0.0746 0.3554 0.0391 0.043 Uiso 1 1 calc R . . Cl3 Cl 0.02574(9) 0.16495(16) 0.00568(8) 0.0605(4) Uani 1 1 d . . . Cl4 Cl -0.04055(9) 0.38719(17) 0.03347(11) 0.0825(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01578(14) 0.01183(13) 0.01827(14) -0.00081(9) 0.00847(10) -0.00204(9) P1 0.0153(4) 0.0117(4) 0.0169(4) -0.0016(3) 0.0083(3) -0.0008(3) P2 0.0166(4) 0.0114(4) 0.0188(4) -0.0015(3) 0.0071(3) -0.0026(3) O1 0.0152(11) 0.0142(11) 0.0206(12) -0.0039(9) 0.0109(10) -0.0038(9) O2 0.0168(12) 0.0192(12) 0.0174(12) -0.0024(10) 0.0069(10) -0.0012(10) C1 0.0146(15) 0.0133(15) 0.0203(17) -0.0034(13) 0.0060(13) 0.0000(12) C2 0.0200(17) 0.0220(18) 0.0219(18) -0.0001(14) 0.0103(14) 0.0018(14) C3 0.0228(18) 0.0247(19) 0.031(2) -0.0047(16) 0.0149(16) 0.0032(15) C4 0.026(2) 0.0203(19) 0.043(2) -0.0020(17) 0.0162(18) 0.0053(16) C5 0.032(2) 0.0152(18) 0.038(2) 0.0057(16) 0.0152(18) 0.0032(16) C6 0.0221(17) 0.0150(17) 0.032(2) 0.0017(14) 0.0165(15) 0.0020(14) C7 0.0149(15) 0.0148(16) 0.0181(16) -0.0007(13) 0.0075(13) -0.0007(12) C8 0.0235(18) 0.0184(17) 0.0218(18) -0.0027(14) 0.0102(14) 0.0028(14) C9 0.028(2) 0.026(2) 0.0236(19) -0.0073(15) 0.0081(16) -0.0012(16) C10 0.0230(18) 0.030(2) 0.0212(18) 0.0014(15) 0.0041(15) -0.0003(16) C11 0.0209(18) 0.0175(18) 0.031(2) 0.0033(15) 0.0059(15) 0.0031(14) C12 0.0209(17) 0.0140(16) 0.0275(19) -0.0020(14) 0.0104(15) -0.0018(14) C13 0.0142(15) 0.0126(15) 0.0182(16) -0.0005(12) 0.0067(13) -0.0012(12) C14 0.0188(16) 0.0144(16) 0.0227(17) -0.0015(13) 0.0103(14) 0.0013(13) C15 0.0209(17) 0.0132(16) 0.0243(18) -0.0037(13) 0.0074(14) 0.0008(13) C16 0.0187(16) 0.0129(16) 0.0219(17) 0.0004(13) 0.0064(14) 0.0009(13) C17 0.0220(18) 0.0157(17) 0.0281(19) -0.0013(14) 0.0073(15) -0.0009(14) C18 0.0170(17) 0.0198(18) 0.032(2) 0.0033(15) 0.0091(15) -0.0047(14) C19 0.0196(17) 0.0169(17) 0.0298(19) 0.0050(14) 0.0136(15) 0.0023(13) C20 0.0206(17) 0.0145(16) 0.0233(17) 0.0012(13) 0.0116(14) -0.0005(13) C21 0.0156(15) 0.0108(15) 0.0198(16) 0.0012(12) 0.0074(13) 0.0006(12) C22 0.0163(15) 0.0109(15) 0.0185(16) 0.0005(12) 0.0081(13) 0.0006(12) C23 0.0188(16) 0.0131(15) 0.0182(16) -0.0026(13) 0.0096(13) -0.0011(13) C24 0.0191(16) 0.0103(15) 0.0176(16) -0.0034(12) 0.0089(13) 0.0023(12) C25 0.0183(16) 0.0145(16) 0.0222(17) -0.0046(13) 0.0100(14) 0.0014(13) C26 0.0191(17) 0.0183(17) 0.0274(19) -0.0052(14) 0.0097(15) -0.0003(14) C27 0.0203(18) 0.0216(18) 0.030(2) -0.0070(16) 0.0070(15) 0.0012(15) C28 0.0239(18) 0.0228(19) 0.0249(19) -0.0044(15) 0.0014(15) 0.0099(15) C29 0.030(2) 0.0174(18) 0.0241(19) -0.0020(14) 0.0092(16) 0.0053(15) C30 0.0222(17) 0.0126(16) 0.0231(18) -0.0044(13) 0.0089(14) 0.0042(13) C31 0.0265(18) 0.0108(15) 0.0240(18) -0.0024(13) 0.0119(15) 0.0013(13) C32 0.0221(17) 0.0134(16) 0.0236(18) -0.0057(13) 0.0113(14) -0.0030(13) C33 0.0187(16) 0.0141(16) 0.0172(16) -0.0025(13) 0.0074(13) 0.0027(13) C34 0.0220(17) 0.0122(16) 0.0194(17) -0.0016(13) 0.0077(14) -0.0056(13) C35 0.0267(19) 0.0156(17) 0.0242(18) -0.0025(14) 0.0067(15) -0.0020(14) C36 0.040(2) 0.0174(19) 0.029(2) -0.0035(15) 0.0085(18) -0.0029(17) C37 0.040(2) 0.022(2) 0.028(2) -0.0043(16) 0.0072(18) -0.0136(17) C38 0.0248(19) 0.030(2) 0.029(2) -0.0023(17) 0.0047(16) -0.0121(17) C39 0.0230(18) 0.0219(19) 0.0270(19) -0.0024(15) 0.0089(15) -0.0048(15) C40 0.0208(17) 0.0125(16) 0.0192(16) -0.0019(13) 0.0068(13) -0.0032(13) C41 0.034(2) 0.0145(17) 0.0263(19) -0.0011(14) 0.0117(16) -0.0011(15) C42 0.039(2) 0.022(2) 0.0240(19) 0.0006(15) 0.0100(17) -0.0061(17) C43 0.036(2) 0.0158(18) 0.031(2) 0.0032(16) -0.0021(18) -0.0043(16) C44 0.0216(18) 0.0177(18) 0.041(2) 0.0000(16) 0.0053(17) 0.0026(15) C45 0.0168(16) 0.0215(18) 0.0268(19) 0.0001(15) 0.0082(14) -0.0012(14) C46 0.052(3) 0.036(3) 0.039(3) 0.000(2) 0.018(2) -0.032(2) C47 0.029(3) 0.016(3) 0.034(3) 0.005(2) 0.020(2) -0.0029(18) C48 0.031(2) 0.028(2) 0.025(2) 0.0035(16) 0.0141(16) -0.0040(17) C46A 0.052(3) 0.036(3) 0.039(3) 0.000(2) 0.018(2) -0.032(2) C47A 0.029(3) 0.016(3) 0.034(3) 0.005(2) 0.020(2) -0.0029(18) C48A 0.031(2) 0.028(2) 0.025(2) 0.0035(16) 0.0141(16) -0.0040(17) B 0.031(2) 0.025(2) 0.030(2) 0.0024(18) 0.0160(19) 0.0024(18) F1 0.069(2) 0.0265(14) 0.0424(15) -0.0008(11) 0.0341(15) -0.0127(13) F2 0.092(3) 0.0229(14) 0.076(2) 0.0125(14) 0.051(2) 0.0135(16) F3 0.0372(18) 0.144(4) 0.048(2) -0.012(2) 0.0102(15) -0.010(2) F4 0.0425(15) 0.0454(16) 0.0329(14) 0.0011(12) 0.0211(12) 0.0117(13) C49 0.032(2) 0.032(2) 0.027(2) -0.0055(17) 0.0061(17) 0.0059(18) Cl1 0.0401(6) 0.0268(5) 0.0278(5) -0.0024(4) 0.0039(4) 0.0025(4) Cl2 0.0401(6) 0.0381(6) 0.0386(6) -0.0032(5) 0.0064(5) -0.0072(5) C50 0.035(2) 0.033(2) 0.037(2) 0.0043(19) 0.0094(19) 0.0055(19) Cl3 0.0669(9) 0.0600(9) 0.0678(9) -0.0248(7) 0.0402(8) -0.0252(7) Cl4 0.0665(10) 0.0646(10) 0.1431(17) 0.0643(12) 0.0714(12) 0.0363(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 Pd C47 2.162(6) . ? Pd C48 2.185(4) . ? Pd C46 2.186(4) . ? Pd C47A 2.189(8) . ? Pd P2 2.2884(9) . ? Pd P1 2.2908(9) . ? P1 O1 1.623(2) . ? P1 C7 1.809(4) . ? P1 C1 1.811(4) . ? P2 O2 1.628(3) . ? P2 C40 1.806(4) . ? P2 C34 1.814(4) . ? O1 C13 1.404(4) . ? O2 C33 1.393(4) . ? C1 C6 1.395(5) . ? C1 C2 1.401(5) . ? C2 C3 1.387(5) . ? C2 H2 0.9500 . ? C3 C4 1.394(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 H4 0.9500 . ? C5 C6 1.383(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.394(5) . ? C7 C8 1.402(5) . ? C8 C9 1.388(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 C11 1.386(6) . ? C10 H10 0.9500 . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C22 1.376(5) . ? C13 C14 1.406(5) . ? C14 C15 1.370(5) . ? C14 H14 0.9500 . ? C15 C16 1.412(5) . ? C15 H15 0.9500 . ? C16 C21 1.413(5) . ? C16 C17 1.428(5) . ? C17 C18 1.374(5) . ? C17 H17 0.9500 . ? C18 C19 1.398(5) . ? C18 H18 0.9500 . ? C19 C20 1.368(5) . ? C19 H19 0.9500 . ? C20 C21 1.421(5) . ? C20 H20 0.9500 . ? C21 C22 1.436(5) . ? C22 C23 1.518(5) . ? C23 C24 1.509(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C33 1.375(5) . ? C24 C25 1.437(5) . ? C25 C30 1.417(5) . ? C25 C26 1.424(5) . ? C26 C27 1.373(6) . ? C26 H26 0.9500 . ? C27 C28 1.410(6) . ? C27 H27 0.9500 . ? C28 C29 1.374(6) . ? C28 H28 0.9500 . ? C29 C30 1.422(5) . ? C29 H29 0.9500 . ? C30 C31 1.430(5) . ? C31 C32 1.364(5) . ? C31 H31 0.9500 . ? C32 C33 1.416(5) . ? C32 H32 0.9500 . ? C34 C35 1.384(5) . ? C34 C39 1.399(5) . ? C35 C36 1.394(5) . ? C35 H35 0.9500 . ? C36 C37 1.384(6) . ? C36 H36 0.9500 . ? C37 C38 1.378(6) . ? C37 H37 0.9500 . ? C38 C39 1.389(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.387(5) . ? C40 C41 1.401(5) . ? C41 C42 1.380(6) . ? C41 H41 0.9500 . ? C42 C43 1.399(6) . ? C42 H42 0.9500 . ? C43 C44 1.372(6) . ? C43 H43 0.9500 . ? C44 C45 1.400(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.310(8) . ? C46 H46A 0.9500 . ? C46 H46B 0.9500 . ? C47 C48 1.382(8) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C48 H48B 0.9500 . ? C47A H47B 0.9500 . ? B F3 1.343(6) . ? B F2 1.383(6) . ? B F1 1.389(5) . ? B F4 1.401(5) . ? C49 Cl1 1.768(4) . ? C49 Cl2 1.768(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 Cl4 1.753(5) . ? C50 Cl3 1.760(5) . ? C50 H50A 0.9900 . ? C50 H50B 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 C47 Pd C48 37.1(2) . . ? C47 Pd C46 35.1(2) . . ? C48 Pd C46 67.31(17) . . ? C47 Pd C47A 26.3(3) . . ? C48 Pd C47A 36.2(2) . . ? C46 Pd C47A 35.1(3) . . ? C47 Pd P2 129.79(18) . . ? C48 Pd P2 163.86(12) . . ? C46 Pd P2 97.25(13) . . ? C47A Pd P2 127.7(2) . . ? C47 Pd P1 129.24(18) . . ? C48 Pd P1 96.60(11) . . ? C46 Pd P1 163.78(13) . . ? C47A Pd P1 130.2(2) . . ? P2 Pd P1 98.95(3) . . ? O1 P1 C7 107.65(14) . . ? O1 P1 C1 105.82(15) . . ? C7 P1 C1 106.34(16) . . ? O1 P1 Pd 109.11(9) . . ? C7 P1 Pd 117.59(12) . . ? C1 P1 Pd 109.68(11) . . ? O2 P2 C40 101.61(15) . . ? O2 P2 C34 101.16(15) . . ? C40 P2 C34 101.35(16) . . ? O2 P2 Pd 111.79(10) . . ? C40 P2 Pd 119.99(12) . . ? C34 P2 Pd 118.15(12) . . ? C13 O1 P1 129.7(2) . . ? C33 O2 P2 122.4(2) . . ? C6 C1 C2 119.5(3) . . ? C6 C1 P1 121.3(3) . . ? C2 C1 P1 118.8(3) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 120.5(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 119.4(3) . . ? C12 C7 P1 117.8(3) . . ? C8 C7 P1 122.8(3) . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.3(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.4(3) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C22 C13 O1 115.6(3) . . ? C22 C13 C14 123.3(3) . . ? O1 C13 C14 120.9(3) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 121.0(3) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C21 119.7(3) . . ? C15 C16 C17 120.8(3) . . ? C21 C16 C17 119.5(3) . . ? C18 C17 C16 120.9(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.1(3) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 121.4(3) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 121.0(3) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C16 C21 C20 117.9(3) . . ? C16 C21 C22 119.5(3) . . ? C20 C21 C22 122.5(3) . . ? C13 C22 C21 117.7(3) . . ? C13 C22 C23 120.5(3) . . ? C21 C22 C23 121.7(3) . . ? C24 C23 C22 114.5(3) . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? C22 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? C33 C24 C25 116.9(3) . . ? C33 C24 C23 120.5(3) . . ? C25 C24 C23 122.6(3) . . ? C30 C25 C26 117.6(3) . . ? C30 C25 C24 120.4(3) . . ? C26 C25 C24 121.9(3) . . ? C27 C26 C25 121.3(4) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 120.4(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 119.7(4) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C25 C30 C29 120.6(3) . . ? C25 C30 C31 119.4(3) . . ? C29 C30 C31 120.1(3) . . ? C32 C31 C30 120.1(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 119.5(3) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C24 C33 O2 117.5(3) . . ? C24 C33 C32 123.5(3) . . ? O2 C33 C32 119.0(3) . . ? C35 C34 C39 119.5(3) . . ? C35 C34 P2 122.0(3) . . ? C39 C34 P2 118.5(3) . . ? C34 C35 C36 120.5(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C37 C36 C35 119.5(4) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C38 C37 C36 120.5(4) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 120.2(4) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C34 119.8(4) . . ? C38 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? C45 C40 C41 119.9(3) . . ? C45 C40 P2 120.6(3) . . ? C41 C40 P2 119.4(3) . . ? C42 C41 C40 119.8(4) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 120.1(4) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.3(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.0(4) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C40 C45 C44 119.9(4) . . ? C40 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C47 C46 Pd 71.5(3) . . ? C47 C46 H46A 120.0 . . ? Pd C46 H46A 68.7 . . ? C47 C46 H46B 120.0 . . ? Pd C46 H46B 132.9 . . ? H46A C46 H46B 120.0 . . ? C46 C47 C48 128.2(6) . . ? C46 C47 Pd 73.5(3) . . ? C48 C47 Pd 72.4(3) . . ? C46 C47 H47A 115.9 . . ? C48 C47 H47A 115.9 . . ? Pd C47 H47A 132.2 . . ? C47 C48 Pd 70.6(3) . . ? C47 C48 H48A 120.0 . . ? Pd C48 H48A 69.6 . . ? C47 C48 H48B 120.0 . . ? Pd C48 H48B 132.9 . . ? H48A C48 H48B 120.0 . . ? Pd C47A H47B 136.4 . . ? F3 B F2 111.3(4) . . ? F3 B F1 112.0(4) . . ? F2 B F1 107.5(4) . . ? F3 B F4 110.2(4) . . ? F2 B F4 107.2(4) . . ? F1 B F4 108.4(4) . . ? Cl1 C49 Cl2 111.4(2) . . ? Cl1 C49 H49A 109.3 . . ? Cl2 C49 H49A 109.3 . . ? Cl1 C49 H49B 109.3 . . ? Cl2 C49 H49B 109.3 . . ? H49A C49 H49B 108.0 . . ? Cl4 C50 Cl3 110.6(3) . . ? Cl4 C50 H50A 109.5 . . ? Cl3 C50 H50A 109.5 . . ? Cl4 C50 H50B 109.5 . . ? Cl3 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 4.200 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.134 data_msb175 _database_code_depnum_ccdc_archive 'CCDC 279238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichloro(bis(2-diphenylphosphinoxynaphthalen-1-yl) methane)nickel(II) dichloromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H36 Cl4 Ni O2 P2' _chemical_formula_weight 883.20 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' 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 P2(1)/c 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 15.008(1) _cell_length_b 10.9488(9) _cell_length_c 26.287(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.429(1) _cell_angle_gamma 90.00 _cell_volume 4163.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8007 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.17 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7675 _exptl_absorpt_correction_T_max 0.9414 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart-APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36216 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.30 _reflns_number_total 9967 _reflns_number_gt 7845 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal contains two voids occupied by solvent dichloromethane. In one of these, the solvent molecule is only slightly disordered and coud be modeled adequately with two alternate locations of equal occupancy for one of the chlorine atoms (Cl4, Cl4a). In the other region, located about the center at 1,0,1/2, the solvent molecule was severely disordered and no satisfactory model could be devised. Consequently, the electron density in this region was removed with the SQUEEZE option of PLATON (Spek, 2005) before the final refinement. H atoms were placed in calculated positions (C---H = 0.95 \%A) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.4329P] 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 9967 _refine_ls_number_parameters 499 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.053 _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 Ni Ni 0.240544(17) 0.08391(2) 0.273510(10) 0.01786(8) Uani 1 1 d . . . Cl1 Cl 0.26722(4) 0.13995(5) 0.19888(2) 0.02657(12) Uani 1 1 d . . . Cl2 Cl 0.17971(4) -0.08747(5) 0.23888(2) 0.02703(12) Uani 1 1 d . . . P1 P 0.32114(3) 0.24651(4) 0.30104(2) 0.01739(11) Uani 1 1 d . . . P2 P 0.20382(4) 0.04809(5) 0.34652(2) 0.01853(11) Uani 1 1 d . . . O1 O 0.34744(9) 0.26001(12) 0.36532(5) 0.0195(3) Uani 1 1 d . . . O2 O 0.29178(9) 0.02297(12) 0.39659(5) 0.0197(3) Uani 1 1 d . . . C1 C 0.26052(13) 0.38732(18) 0.27694(8) 0.0202(4) Uani 1 1 d . . . C2 C 0.21804(14) 0.4511(2) 0.30987(9) 0.0261(5) Uani 1 1 d . . . H2 H 0.2240 0.4230 0.3448 0.031 Uiso 1 1 calc R . . C3 C 0.16716(16) 0.5554(2) 0.29192(11) 0.0335(5) Uani 1 1 d . . . H3 H 0.1386 0.5988 0.3146 0.040 Uiso 1 1 calc R . . C4 C 0.15781(15) 0.59670(19) 0.24101(11) 0.0337(6) Uani 1 1 d . . . H4 H 0.1227 0.6681 0.2288 0.040 Uiso 1 1 calc R . . C5 C 0.19959(16) 0.5340(2) 0.20804(10) 0.0313(5) Uani 1 1 d . . . H5 H 0.1933 0.5628 0.1732 0.038 Uiso 1 1 calc R . . C6 C 0.25053(14) 0.42965(19) 0.22539(9) 0.0239(4) Uani 1 1 d . . . H6 H 0.2787 0.3867 0.2024 0.029 Uiso 1 1 calc R . . C7 C 0.43419(14) 0.24884(17) 0.28872(8) 0.0189(4) Uani 1 1 d . . . C8 C 0.48714(14) 0.14330(18) 0.30198(8) 0.0202(4) Uani 1 1 d . . . H8 H 0.4596 0.0709 0.3107 0.024 Uiso 1 1 calc R . . C9 C 0.57931(15) 0.14321(19) 0.30256(8) 0.0230(4) Uani 1 1 d . . . H9 H 0.6152 0.0713 0.3123 0.028 Uiso 1 1 calc R . . C10 C 0.61985(15) 0.24799(19) 0.28890(8) 0.0236(4) Uani 1 1 d . . . H10 H 0.6833 0.2478 0.2891 0.028 Uiso 1 1 calc R . . C11 C 0.56719(15) 0.35281(19) 0.27491(8) 0.0242(4) Uani 1 1 d . . . H11 H 0.5948 0.4244 0.2655 0.029 Uiso 1 1 calc R . . C12 C 0.47462(14) 0.35403(18) 0.27460(8) 0.0211(4) Uani 1 1 d . . . H12 H 0.4389 0.4261 0.2648 0.025 Uiso 1 1 calc R . . C13 C 0.42493(13) 0.32390(18) 0.39556(8) 0.0187(4) Uani 1 1 d . . . C14 C 0.44335(14) 0.44268(18) 0.38046(8) 0.0219(4) Uani 1 1 d . . . H14 H 0.4049 0.4786 0.3494 0.026 Uiso 1 1 calc R . . C15 C 0.51694(14) 0.50574(19) 0.41074(8) 0.0225(4) Uani 1 1 d . . . H15 H 0.5313 0.5843 0.3997 0.027 Uiso 1 1 calc R . . C16 C 0.57189(14) 0.45581(19) 0.45814(8) 0.0205(4) Uani 1 1 d . . . C17 C 0.64643(15) 0.5234(2) 0.49047(8) 0.0243(4) Uani 1 1 d . . . H17 H 0.6617 0.6009 0.4789 0.029 Uiso 1 1 calc R . . C18 C 0.69648(16) 0.4786(2) 0.53786(9) 0.0282(5) Uani 1 1 d . . . H18 H 0.7469 0.5239 0.5590 0.034 Uiso 1 1 calc R . . C19 C 0.67277(15) 0.3650(2) 0.55503(8) 0.0261(5) Uani 1 1 d . . . H19 H 0.7060 0.3354 0.5887 0.031 Uiso 1 1 calc R . . C20 C 0.60314(15) 0.2961(2) 0.52463(8) 0.0237(4) Uani 1 1 d . . . H20 H 0.5895 0.2189 0.5373 0.028 Uiso 1 1 calc R . . C21 C 0.55027(13) 0.33749(18) 0.47420(8) 0.0188(4) Uani 1 1 d . . . C22 C 0.47622(13) 0.26897(17) 0.44082(8) 0.0173(4) Uani 1 1 d . . . C23 C 0.44916(14) 0.14304(17) 0.45652(8) 0.0189(4) Uani 1 1 d . . . H23A H 0.4890 0.1239 0.4921 0.023 Uiso 1 1 calc R . . H23B H 0.3848 0.1476 0.4593 0.023 Uiso 1 1 calc R . . C24 C 0.45541(14) 0.03704(18) 0.42021(8) 0.0186(4) Uani 1 1 d . . . C25 C 0.54212(14) -0.01351(17) 0.41776(7) 0.0185(4) Uani 1 1 d . . . C26 C 0.62843(14) 0.03534(19) 0.44679(8) 0.0231(4) Uani 1 1 d . . . H26 H 0.6296 0.1055 0.4682 0.028 Uiso 1 1 calc R . . C27 C 0.70988(15) -0.0172(2) 0.44434(9) 0.0272(5) Uani 1 1 d . . . H27 H 0.7667 0.0168 0.4643 0.033 Uiso 1 1 calc R . . C28 C 0.71086(16) -0.1207(2) 0.41271(9) 0.0301(5) Uani 1 1 d . . . H28 H 0.7680 -0.1564 0.4116 0.036 Uiso 1 1 calc R . . C29 C 0.62965(15) -0.1696(2) 0.38377(9) 0.0267(5) Uani 1 1 d . . . H29 H 0.6307 -0.2389 0.3622 0.032 Uiso 1 1 calc R . . C30 C 0.54361(15) -0.11837(18) 0.38537(8) 0.0214(4) Uani 1 1 d . . . C31 C 0.45915(15) -0.16885(18) 0.35558(8) 0.0220(4) Uani 1 1 d . . . H31 H 0.4599 -0.2372 0.3335 0.026 Uiso 1 1 calc R . . C32 C 0.37668(15) -0.12093(18) 0.35810(8) 0.0213(4) Uani 1 1 d . . . H32 H 0.3202 -0.1553 0.3379 0.026 Uiso 1 1 calc R . . C33 C 0.37648(14) -0.01953(17) 0.39108(8) 0.0182(4) Uani 1 1 d . . . C34 C 0.12753(14) -0.07905(18) 0.35105(8) 0.0218(4) Uani 1 1 d . . . C35 C 0.04274(15) -0.0927(2) 0.31356(9) 0.0261(5) Uani 1 1 d . . . H35 H 0.0260 -0.0388 0.2842 0.031 Uiso 1 1 calc R . . C36 C -0.01712(15) -0.1853(2) 0.31924(10) 0.0301(5) Uani 1 1 d . . . H36 H -0.0748 -0.1948 0.2937 0.036 Uiso 1 1 calc R . . C37 C 0.00689(17) -0.2639(2) 0.36200(11) 0.0361(6) Uani 1 1 d . . . H37 H -0.0342 -0.3272 0.3657 0.043 Uiso 1 1 calc R . . C38 C 0.09098(17) -0.2502(2) 0.39944(11) 0.0357(6) Uani 1 1 d . . . H38 H 0.1075 -0.3041 0.4288 0.043 Uiso 1 1 calc R . . C39 C 0.15134(16) -0.1571(2) 0.39405(9) 0.0278(5) Uani 1 1 d . . . H39 H 0.2087 -0.1473 0.4198 0.033 Uiso 1 1 calc R . . C40 C 0.14893(14) 0.17202(19) 0.37192(9) 0.0233(4) Uani 1 1 d . . . C41 C 0.07981(16) 0.2390(2) 0.33739(10) 0.0320(5) Uani 1 1 d . . . H41 H 0.0639 0.2221 0.3006 0.038 Uiso 1 1 calc R . . C42 C 0.03406(17) 0.3311(2) 0.35704(13) 0.0440(7) Uani 1 1 d . . . H42 H -0.0132 0.3771 0.3336 0.053 Uiso 1 1 calc R . . C43 C 0.05716(18) 0.3556(2) 0.41030(13) 0.0478(7) Uani 1 1 d . . . H43 H 0.0258 0.4185 0.4235 0.057 Uiso 1 1 calc R . . C44 C 0.12568(19) 0.2891(3) 0.44461(12) 0.0468(7) Uani 1 1 d . . . H44 H 0.1415 0.3068 0.4813 0.056 Uiso 1 1 calc R . . C45 C 0.17152(16) 0.1965(2) 0.42566(10) 0.0325(5) Uani 1 1 d . . . H45 H 0.2181 0.1502 0.4494 0.039 Uiso 1 1 calc R . . Cl3 Cl 0.14434(5) 1.02668(7) 0.06289(3) 0.05081(19) Uani 1 1 d . . . C46 C 0.22117(19) 0.9221(2) 0.10295(10) 0.0378(6) Uani 0.50 1 d PD A 1 H46A H 0.2839 0.9581 0.1122 0.045 Uiso 0.50 1 calc PR A 1 H46B H 0.2030 0.9111 0.1362 0.045 Uiso 0.50 1 calc PR A 1 Cl4 Cl 0.2261(2) 0.7809(4) 0.0753(2) 0.0642(7) Uani 0.50 1 d PD A 1 C46A C 0.22117(19) 0.9221(2) 0.10295(10) 0.0378(6) Uani 0.50 1 d PD A 2 H46C H 0.2179 0.9291 0.1400 0.045 Uiso 0.50 1 calc PR A 2 H46D H 0.2853 0.9400 0.1019 0.045 Uiso 0.50 1 calc PR A 2 Cl4A Cl 0.1894(2) 0.7710(4) 0.0788(2) 0.0642(7) Uani 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.02171(14) 0.01409(13) 0.01792(13) 0.00038(9) 0.00551(10) -0.00126(9) Cl1 0.0383(3) 0.0225(3) 0.0197(2) 0.00026(19) 0.0092(2) -0.0074(2) Cl2 0.0362(3) 0.0200(3) 0.0270(3) -0.0049(2) 0.0120(2) -0.0090(2) P1 0.0199(3) 0.0141(2) 0.0180(2) 0.00159(18) 0.0048(2) 0.00047(19) P2 0.0200(3) 0.0161(2) 0.0200(3) 0.00122(19) 0.0063(2) 0.00046(19) O1 0.0212(7) 0.0192(7) 0.0177(7) 0.0016(5) 0.0045(6) -0.0006(5) O2 0.0189(7) 0.0212(7) 0.0202(7) 0.0022(6) 0.0069(6) 0.0011(5) C1 0.0177(9) 0.0134(9) 0.0265(11) 0.0015(8) 0.0006(8) -0.0012(7) C2 0.0241(11) 0.0208(10) 0.0305(12) -0.0026(9) 0.0020(9) 0.0003(8) C3 0.0256(12) 0.0212(11) 0.0513(15) -0.0067(10) 0.0063(11) 0.0011(9) C4 0.0222(11) 0.0143(10) 0.0576(16) 0.0057(10) -0.0019(11) -0.0014(8) C5 0.0262(11) 0.0221(11) 0.0385(13) 0.0119(10) -0.0038(10) -0.0060(9) C6 0.0231(11) 0.0196(10) 0.0274(11) 0.0044(8) 0.0037(9) -0.0035(8) C7 0.0216(10) 0.0168(10) 0.0176(9) 0.0002(7) 0.0040(8) -0.0007(8) C8 0.0260(10) 0.0165(10) 0.0201(10) 0.0001(8) 0.0093(8) 0.0000(8) C9 0.0275(11) 0.0217(10) 0.0200(10) 0.0005(8) 0.0068(8) 0.0048(8) C10 0.0213(10) 0.0275(11) 0.0231(10) -0.0013(8) 0.0074(8) -0.0003(8) C11 0.0272(11) 0.0211(10) 0.0250(11) 0.0035(8) 0.0086(9) -0.0041(8) C12 0.0235(10) 0.0177(10) 0.0213(10) 0.0029(8) 0.0045(8) -0.0001(8) C13 0.0195(10) 0.0166(9) 0.0201(10) -0.0033(7) 0.0053(8) 0.0002(7) C14 0.0260(11) 0.0187(10) 0.0202(10) 0.0030(8) 0.0049(8) 0.0032(8) C15 0.0268(11) 0.0172(10) 0.0234(10) 0.0007(8) 0.0062(9) -0.0007(8) C16 0.0214(10) 0.0199(10) 0.0209(10) -0.0027(8) 0.0070(8) 0.0018(8) C17 0.0270(11) 0.0228(11) 0.0242(11) -0.0029(8) 0.0086(9) -0.0022(8) C18 0.0281(11) 0.0308(12) 0.0254(11) -0.0069(9) 0.0063(9) -0.0058(9) C19 0.0296(11) 0.0285(11) 0.0179(10) -0.0004(8) 0.0025(9) 0.0039(9) C20 0.0295(11) 0.0222(10) 0.0199(10) -0.0006(8) 0.0072(9) 0.0021(9) C21 0.0225(10) 0.0189(10) 0.0167(9) -0.0014(7) 0.0082(8) 0.0034(8) C22 0.0201(10) 0.0151(9) 0.0177(9) 0.0001(7) 0.0067(8) 0.0026(7) C23 0.0213(10) 0.0181(10) 0.0180(9) 0.0015(8) 0.0064(8) 0.0012(8) C24 0.0243(10) 0.0162(9) 0.0164(9) 0.0050(7) 0.0071(8) 0.0027(8) C25 0.0239(10) 0.0164(9) 0.0161(9) 0.0050(7) 0.0070(8) 0.0019(8) C26 0.0264(11) 0.0200(10) 0.0240(10) 0.0039(8) 0.0086(9) 0.0010(8) C27 0.0233(11) 0.0264(11) 0.0328(12) 0.0066(9) 0.0091(9) 0.0020(9) C28 0.0288(12) 0.0283(11) 0.0371(13) 0.0079(10) 0.0155(10) 0.0095(9) C29 0.0337(12) 0.0201(10) 0.0298(12) 0.0047(9) 0.0145(10) 0.0064(9) C30 0.0295(11) 0.0170(9) 0.0203(10) 0.0061(8) 0.0110(8) 0.0030(8) C31 0.0328(12) 0.0136(9) 0.0207(10) 0.0038(8) 0.0091(9) 0.0037(8) C32 0.0270(11) 0.0169(9) 0.0198(10) 0.0037(8) 0.0060(8) -0.0005(8) C33 0.0210(10) 0.0162(9) 0.0186(9) 0.0052(7) 0.0075(8) 0.0032(7) C34 0.0218(10) 0.0181(10) 0.0285(11) 0.0007(8) 0.0118(9) 0.0000(8) C35 0.0227(11) 0.0241(11) 0.0317(12) -0.0012(9) 0.0079(9) 0.0010(8) C36 0.0208(11) 0.0302(12) 0.0401(13) -0.0048(10) 0.0096(10) -0.0022(9) C37 0.0298(13) 0.0282(12) 0.0558(17) -0.0001(11) 0.0208(12) -0.0061(10) C38 0.0358(13) 0.0299(13) 0.0436(14) 0.0128(11) 0.0144(11) -0.0030(10) C39 0.0277(11) 0.0254(11) 0.0312(12) 0.0045(9) 0.0094(9) -0.0016(9) C40 0.0206(10) 0.0193(10) 0.0318(11) -0.0011(8) 0.0100(9) -0.0025(8) C41 0.0258(12) 0.0281(12) 0.0404(14) -0.0006(10) 0.0057(10) 0.0030(9) C42 0.0263(13) 0.0306(13) 0.073(2) -0.0020(13) 0.0093(13) 0.0074(10) C43 0.0331(14) 0.0320(14) 0.082(2) -0.0247(14) 0.0211(14) 0.0005(11) C44 0.0404(15) 0.0481(16) 0.0542(17) -0.0262(14) 0.0166(13) 0.0002(13) C45 0.0294(12) 0.0330(13) 0.0348(13) -0.0090(10) 0.0079(10) 0.0015(10) Cl3 0.0514(4) 0.0570(4) 0.0497(4) 0.0238(3) 0.0232(3) 0.0089(3) C46 0.0492(16) 0.0311(13) 0.0350(14) -0.0012(10) 0.0145(12) 0.0026(11) Cl4 0.095(3) 0.0383(7) 0.0577(8) -0.0180(6) 0.0176(17) 0.0023(15) C46A 0.0492(16) 0.0311(13) 0.0350(14) -0.0012(10) 0.0145(12) 0.0026(11) Cl4A 0.095(3) 0.0383(7) 0.0577(8) -0.0180(6) 0.0176(17) 0.0023(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni P1 2.1657(6) . ? Ni P2 2.1688(6) . ? Ni Cl2 2.1773(6) . ? Ni Cl1 2.1916(6) . ? P1 O1 1.6365(14) . ? P1 C7 1.810(2) . ? P1 C1 1.816(2) . ? P2 O2 1.6205(15) . ? P2 C40 1.805(2) . ? P2 C34 1.826(2) . ? O1 C13 1.408(2) . ? O2 C33 1.397(2) . ? C1 C2 1.392(3) . ? C1 C6 1.402(3) . ? C2 C3 1.385(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.393(3) . ? C7 C12 1.397(3) . ? C8 C9 1.379(3) . ? C8 H8 0.9500 . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C22 1.372(3) . ? C13 C14 1.408(3) . ? C14 C15 1.365(3) . ? C14 H14 0.9500 . ? C15 C16 1.409(3) . ? C15 H15 0.9500 . ? C16 C17 1.419(3) . ? C16 C21 1.426(3) . ? C17 C18 1.363(3) . ? C17 H17 0.9500 . ? C18 C19 1.401(3) . ? C18 H18 0.9500 . ? C19 C20 1.362(3) . ? C19 H19 0.9500 . ? C20 C21 1.426(3) . ? C20 H20 0.9500 . ? C21 C22 1.431(3) . ? C22 C23 1.525(3) . ? C23 C24 1.521(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C33 1.375(3) . ? C24 C25 1.431(3) . ? C25 C26 1.421(3) . ? C25 C30 1.433(3) . ? C26 C27 1.368(3) . ? C26 H26 0.9500 . ? C27 C28 1.408(3) . ? C27 H27 0.9500 . ? C28 C29 1.363(3) . ? C28 H28 0.9500 . ? C29 C30 1.419(3) . ? C29 H29 0.9500 . ? C30 C31 1.413(3) . ? C31 C32 1.362(3) . ? C31 H31 0.9500 . ? C32 C33 1.409(3) . ? C32 H32 0.9500 . ? C34 C39 1.386(3) . ? C34 C35 1.395(3) . ? C35 C36 1.389(3) . ? C35 H35 0.9500 . ? C36 C37 1.385(4) . ? C36 H36 0.9500 . ? C37 C38 1.387(4) . ? C37 H37 0.9500 . ? C38 C39 1.395(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.388(3) . ? C40 C41 1.392(3) . ? C41 C42 1.394(3) . ? C41 H41 0.9500 . ? C42 C43 1.376(4) . ? C42 H42 0.9500 . ? C43 C44 1.381(4) . ? C43 H43 0.9500 . ? C44 C45 1.390(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? Cl3 C46 1.761(3) . ? C46 Cl4 1.719(5) . ? C46 H46A 0.9900 . ? C46 H46B 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 P1 Ni P2 95.96(2) . . ? P1 Ni Cl2 169.38(2) . . ? P2 Ni Cl2 92.13(2) . . ? P1 Ni Cl1 81.38(2) . . ? P2 Ni Cl1 173.06(2) . . ? Cl2 Ni Cl1 91.33(2) . . ? O1 P1 C7 101.74(8) . . ? O1 P1 C1 104.13(9) . . ? C7 P1 C1 109.39(9) . . ? O1 P1 Ni 112.28(5) . . ? C7 P1 Ni 114.75(7) . . ? C1 P1 Ni 113.44(7) . . ? O2 P2 C40 100.39(9) . . ? O2 P2 C34 101.95(9) . . ? C40 P2 C34 101.14(9) . . ? O2 P2 Ni 113.93(5) . . ? C40 P2 Ni 116.09(7) . . ? C34 P2 Ni 120.45(7) . . ? C13 O1 P1 124.34(12) . . ? C33 O2 P2 122.64(12) . . ? C2 C1 C6 119.11(19) . . ? C2 C1 P1 118.61(16) . . ? C6 C1 P1 122.17(16) . . ? C3 C2 C1 120.3(2) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 119.41(19) . . ? C8 C7 P1 116.30(15) . . ? C12 C7 P1 123.58(15) . . ? C9 C8 C7 120.46(19) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.21(19) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.61(19) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.59(19) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 119.71(19) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C22 C13 O1 117.42(17) . . ? C22 C13 C14 122.83(18) . . ? O1 C13 C14 119.62(17) . . ? C15 C14 C13 119.47(19) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.79(19) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 120.66(19) . . ? C15 C16 C21 119.25(18) . . ? C17 C16 C21 120.07(19) . . ? C18 C17 C16 121.0(2) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.2(2) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C20 C19 C18 121.6(2) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 121.3(2) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 116.73(18) . . ? C20 C21 C22 123.56(18) . . ? C16 C21 C22 119.67(18) . . ? C13 C22 C21 117.83(17) . . ? C13 C22 C23 120.18(17) . . ? C21 C22 C23 121.81(17) . . ? C24 C23 C22 117.03(16) . . ? C24 C23 H23A 108.0 . . ? C22 C23 H23A 108.0 . . ? C24 C23 H23B 108.0 . . ? C22 C23 H23B 108.0 . . ? H23A C23 H23B 107.3 . . ? C33 C24 C25 117.37(18) . . ? C33 C24 C23 120.35(18) . . ? C25 C24 C23 122.12(18) . . ? C26 C25 C24 122.69(18) . . ? C26 C25 C30 117.67(18) . . ? C24 C25 C30 119.64(18) . . ? C27 C26 C25 121.0(2) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 121.1(2) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 119.8(2) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.9(2) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 121.21(19) . . ? C31 C30 C25 119.28(18) . . ? C29 C30 C25 119.5(2) . . ? C32 C31 C30 120.99(19) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 118.96(19) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C24 C33 O2 117.72(17) . . ? C24 C33 C32 123.71(18) . . ? O2 C33 C32 118.50(17) . . ? C39 C34 C35 119.93(19) . . ? C39 C34 P2 119.55(17) . . ? C35 C34 P2 120.36(16) . . ? C36 C35 C34 119.8(2) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 120.3(2) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 120.0(2) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C39 120.0(2) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C34 C39 C38 120.0(2) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C45 C40 C41 120.0(2) . . ? C45 C40 P2 120.66(17) . . ? C41 C40 P2 119.29(17) . . ? C40 C41 C42 119.6(2) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 120.2(2) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.3(2) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C45 120.2(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C40 C45 C44 119.7(2) . . ? C40 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? Cl4 C46 Cl3 115.3(2) . . ? Cl4 C46 H46A 108.5 . . ? Cl3 C46 H46A 108.5 . . ? Cl4 C46 H46B 108.5 . . ? Cl3 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.139 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.075 data_msb174 _database_code_depnum_ccdc_archive 'CCDC 279239' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Chloro(bis(2-diphenylphosphinoxynaphthalen-1-yl) methane)gold(I) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H34 Au Cl3 O2 P2' _chemical_formula_sum 'C46 H34 Au Cl3 O2 P2' _chemical_formula_weight 983.99 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.337(1) _cell_length_b 12.453(1) _cell_length_c 12.806(1) _cell_angle_alpha 84.941(1) _cell_angle_beta 88.464(1) _cell_angle_gamma 78.992(1) _cell_volume 1923.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6985 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.30 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 4.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5350 _exptl_absorpt_correction_T_max 0.7322 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16809 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8606 _reflns_number_gt 8125 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The molecule of solvent dichloromethane was disordered over two approximately eqally populated sites having one chlorine atom (Cl2) in common. Although the location of the carbon atom is likely different for each component of the disorder, two resolved sites for this atom could not be discerned. Because of the disorder, H atoms were not included for the solvent molecule. All other H atoms were placed in calculated positions (C---H = 0.95 \%A) and were included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. The largest features of the final difference map are within 1 \%A of thge gold atom and likely are the result of an inadequacy of the absorption correction due to the plate-like habit of the crystal. ; _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^)+(0.0524P)^2^+5.2498P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8606 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Au1 Au 0.695015(12) 0.804110(12) 0.697179(11) 0.01957(6) Uani 1 1 d . . . Cl1 Cl 0.50660(9) 0.81703(9) 0.77897(10) 0.0315(2) Uani 1 1 d . . . P1 P 0.72218(8) 0.69640(8) 0.55903(8) 0.01799(19) Uani 1 1 d . . . P2 P 0.79826(8) 0.91715(9) 0.76283(8) 0.0188(2) Uani 1 1 d . . . O1 O 0.8512(2) 0.6715(2) 0.5192(2) 0.0204(6) Uani 1 1 d . . . O2 O 0.8605(2) 0.9791(3) 0.6677(2) 0.0242(6) Uani 1 1 d . . . C1 C 0.6763(3) 0.5654(3) 0.5718(3) 0.0194(8) Uani 1 1 d . . . C2 C 0.5846(4) 0.5584(4) 0.6359(4) 0.0258(9) Uani 1 1 d . . . H2 H 0.5514 0.6193 0.6731 0.031 Uiso 1 1 calc R . . C3 C 0.5414(4) 0.4627(4) 0.6458(4) 0.0287(9) Uani 1 1 d . . . H3 H 0.4780 0.4587 0.6886 0.034 Uiso 1 1 calc R . . C4 C 0.5906(4) 0.3732(4) 0.5931(4) 0.0277(9) Uani 1 1 d . . . H4 H 0.5621 0.3072 0.6013 0.033 Uiso 1 1 calc R . . C5 C 0.6816(4) 0.3798(4) 0.5283(4) 0.0263(9) Uani 1 1 d . . . H5 H 0.7148 0.3185 0.4918 0.032 Uiso 1 1 calc R . . C6 C 0.7245(4) 0.4761(3) 0.5164(3) 0.0229(8) Uani 1 1 d . . . H6 H 0.7859 0.4810 0.4711 0.028 Uiso 1 1 calc R . . C7 C 0.6562(3) 0.7625(3) 0.4397(3) 0.0196(8) Uani 1 1 d . . . C8 C 0.6841(4) 0.7194(4) 0.3437(3) 0.0246(8) Uani 1 1 d . . . H8 H 0.7410 0.6566 0.3399 0.030 Uiso 1 1 calc R . . C9 C 0.6289(4) 0.7684(4) 0.2535(4) 0.0277(9) Uani 1 1 d . . . H9 H 0.6471 0.7384 0.1882 0.033 Uiso 1 1 calc R . . C10 C 0.5470(4) 0.8613(4) 0.2591(3) 0.0254(9) Uani 1 1 d . . . H10 H 0.5099 0.8955 0.1974 0.030 Uiso 1 1 calc R . . C11 C 0.5194(3) 0.9042(3) 0.3543(4) 0.0246(8) Uani 1 1 d . . . H11 H 0.4632 0.9678 0.3575 0.030 Uiso 1 1 calc R . . C12 C 0.5732(3) 0.8549(3) 0.4454(3) 0.0213(8) Uani 1 1 d . . . H12 H 0.5535 0.8841 0.5108 0.026 Uiso 1 1 calc R . . C13 C 0.9368(3) 0.6380(3) 0.5920(3) 0.0213(8) Uani 1 1 d . . . C14 C 0.9478(4) 0.5297(4) 0.6393(4) 0.0276(9) Uani 1 1 d . . . H14 H 0.8965 0.4856 0.6235 0.033 Uiso 1 1 calc R . . C15 C 1.0312(4) 0.4877(4) 0.7075(4) 0.0302(10) Uani 1 1 d . . . H15 H 1.0378 0.4148 0.7391 0.036 Uiso 1 1 calc R . . C16 C 1.1078(3) 0.5526(4) 0.7313(3) 0.0247(9) Uani 1 1 d . . . C17 C 1.1973(4) 0.5091(4) 0.8011(4) 0.0303(10) Uani 1 1 d . . . H17 H 1.2030 0.4372 0.8347 0.036 Uiso 1 1 calc R . . C18 C 1.2747(4) 0.5705(4) 0.8198(4) 0.0330(10) Uani 1 1 d . . . H18 H 1.3344 0.5404 0.8654 0.040 Uiso 1 1 calc R . . C19 C 1.2664(4) 0.6768(4) 0.7723(4) 0.0314(10) Uani 1 1 d . . . H19 H 1.3206 0.7187 0.7855 0.038 Uiso 1 1 calc R . . C20 C 1.1801(3) 0.7214(4) 0.7064(3) 0.0250(9) Uani 1 1 d . . . H20 H 1.1747 0.7947 0.6761 0.030 Uiso 1 1 calc R . . C21 C 1.0986(3) 0.6604(3) 0.6826(3) 0.0208(8) Uani 1 1 d . . . C22 C 1.0093(3) 0.7056(3) 0.6111(3) 0.0195(8) Uani 1 1 d . . . C23 C 1.0084(3) 0.8226(3) 0.5626(3) 0.0226(8) Uani 1 1 d . . . H23A H 1.0275 0.8648 0.6192 0.027 Uiso 1 1 calc R . . H23B H 1.0699 0.8181 0.5109 0.027 Uiso 1 1 calc R . . C24 C 0.9081(3) 0.8914(3) 0.5088(3) 0.0194(8) Uani 1 1 d . . . C25 C 0.8898(3) 0.8913(3) 0.3989(3) 0.0211(8) Uani 1 1 d . . . C26 C 0.9582(4) 0.8177(4) 0.3359(4) 0.0266(9) Uani 1 1 d . . . H26 H 1.0172 0.7654 0.3672 0.032 Uiso 1 1 calc R . . C27 C 0.9406(4) 0.8206(4) 0.2297(4) 0.0321(10) Uani 1 1 d . . . H27 H 0.9877 0.7708 0.1887 0.039 Uiso 1 1 calc R . . C28 C 0.8536(4) 0.8968(4) 0.1818(4) 0.0337(11) Uani 1 1 d . . . H28 H 0.8422 0.8983 0.1086 0.040 Uiso 1 1 calc R . . C29 C 0.7851(4) 0.9689(4) 0.2403(4) 0.0303(10) Uani 1 1 d . . . H29 H 0.7262 1.0199 0.2073 0.036 Uiso 1 1 calc R . . C30 C 0.8012(4) 0.9684(4) 0.3497(3) 0.0241(8) Uani 1 1 d . . . C31 C 0.7313(3) 1.0427(4) 0.4107(4) 0.0254(9) Uani 1 1 d . . . H31 H 0.6708 1.0924 0.3787 0.030 Uiso 1 1 calc R . . C32 C 0.7500(3) 1.0436(4) 0.5153(4) 0.0242(8) Uani 1 1 d . . . H32 H 0.7033 1.0942 0.5559 0.029 Uiso 1 1 calc R . . C33 C 0.8395(3) 0.9688(3) 0.5625(3) 0.0207(8) Uani 1 1 d . . . C34 C 0.7328(3) 1.0309(3) 0.8352(3) 0.0204(8) Uani 1 1 d . . . C35 C 0.6743(3) 1.0055(4) 0.9261(3) 0.0242(8) Uani 1 1 d . . . H35 H 0.6693 0.9314 0.9465 0.029 Uiso 1 1 calc R . . C36 C 0.6234(4) 1.0888(4) 0.9865(4) 0.0295(10) Uani 1 1 d . . . H36 H 0.5849 1.0713 1.0491 0.035 Uiso 1 1 calc R . . C37 C 0.6286(4) 1.1967(4) 0.9557(4) 0.0312(10) Uani 1 1 d . . . H37 H 0.5942 1.2532 0.9975 0.037 Uiso 1 1 calc R . . C38 C 0.6839(4) 1.2233(4) 0.8641(4) 0.0308(10) Uani 1 1 d . . . H38 H 0.6852 1.2979 0.8420 0.037 Uiso 1 1 calc R . . C39 C 0.7378(3) 1.1396(4) 0.8041(4) 0.0259(9) Uani 1 1 d . . . H39 H 0.7776 1.1572 0.7425 0.031 Uiso 1 1 calc R . . C40 C 0.9090(3) 0.8495(3) 0.8478(3) 0.0209(8) Uani 1 1 d . . . C41 C 0.9859(4) 0.9073(4) 0.8826(4) 0.0287(9) Uani 1 1 d . . . H41 H 0.9804 0.9832 0.8614 0.034 Uiso 1 1 calc R . . C42 C 1.0706(4) 0.8528(4) 0.9485(4) 0.0311(10) Uani 1 1 d . . . H42 H 1.1242 0.8911 0.9710 0.037 Uiso 1 1 calc R . . C43 C 1.0770(4) 0.7432(4) 0.9812(4) 0.0303(10) Uani 1 1 d . . . H43 H 1.1345 0.7069 1.0269 0.036 Uiso 1 1 calc R . . C44 C 1.0014(4) 0.6862(4) 0.9487(4) 0.0332(10) Uani 1 1 d . . . H44 H 1.0060 0.6109 0.9722 0.040 Uiso 1 1 calc R . . C45 C 0.9170(4) 0.7393(4) 0.8804(4) 0.0296(9) Uani 1 1 d . . . H45 H 0.8653 0.6996 0.8565 0.036 Uiso 1 1 calc R . . Cl2 Cl 0.77869(13) 0.51020(13) 0.85243(15) 0.0549(4) Uani 1 1 d . . . Cl3 Cl 0.6602(3) 0.6584(3) 0.9909(2) 0.0492(5) Uani 0.474(3) 1 d P . . Cl3A Cl 0.5559(2) 0.5049(3) 0.9370(2) 0.0492(5) Uani 0.526(3) 1 d P . . C46 C 0.6563(7) 0.5756(7) 0.9094(7) 0.072(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01710(9) 0.01992(9) 0.02229(9) -0.00664(6) -0.00369(5) -0.00235(6) Cl1 0.0209(5) 0.0317(5) 0.0417(6) -0.0093(5) 0.0067(4) -0.0025(4) P1 0.0145(4) 0.0182(5) 0.0218(5) -0.0059(4) -0.0031(4) -0.0021(4) P2 0.0151(5) 0.0214(5) 0.0206(5) -0.0073(4) -0.0019(4) -0.0024(4) O1 0.0147(13) 0.0209(14) 0.0254(14) -0.0048(11) -0.0037(11) -0.0010(10) O2 0.0236(15) 0.0287(15) 0.0231(15) -0.0080(12) 0.0000(11) -0.0099(12) C1 0.0189(18) 0.0181(18) 0.0221(19) -0.0039(15) -0.0061(15) -0.0037(15) C2 0.023(2) 0.026(2) 0.028(2) -0.0081(17) 0.0022(17) -0.0015(16) C3 0.023(2) 0.031(2) 0.034(2) -0.0057(19) 0.0029(18) -0.0097(18) C4 0.031(2) 0.025(2) 0.030(2) -0.0020(17) -0.0068(18) -0.0116(18) C5 0.029(2) 0.021(2) 0.030(2) -0.0082(17) -0.0016(17) -0.0040(17) C6 0.022(2) 0.024(2) 0.024(2) -0.0062(16) 0.0001(15) -0.0059(16) C7 0.0162(18) 0.0228(19) 0.0209(19) -0.0033(15) -0.0024(14) -0.0058(15) C8 0.022(2) 0.023(2) 0.028(2) -0.0066(17) -0.0009(16) -0.0003(16) C9 0.029(2) 0.029(2) 0.025(2) -0.0059(17) -0.0030(17) -0.0046(18) C10 0.020(2) 0.029(2) 0.027(2) -0.0001(17) -0.0080(16) -0.0059(17) C11 0.0180(19) 0.0206(19) 0.035(2) -0.0052(17) -0.0046(16) -0.0023(15) C12 0.0176(18) 0.0211(19) 0.027(2) -0.0076(16) -0.0023(15) -0.0047(15) C13 0.0141(18) 0.023(2) 0.025(2) -0.0045(16) -0.0041(15) 0.0013(15) C14 0.023(2) 0.022(2) 0.039(2) -0.0036(18) -0.0085(18) -0.0035(16) C15 0.028(2) 0.022(2) 0.040(3) 0.0015(18) -0.0099(19) -0.0026(17) C16 0.0188(19) 0.028(2) 0.026(2) -0.0062(17) -0.0020(16) 0.0025(16) C17 0.024(2) 0.030(2) 0.033(2) -0.0036(19) -0.0082(18) 0.0058(18) C18 0.021(2) 0.043(3) 0.032(2) -0.007(2) -0.0087(18) 0.0023(19) C19 0.019(2) 0.043(3) 0.033(2) -0.008(2) -0.0053(17) -0.0046(19) C20 0.0174(19) 0.031(2) 0.027(2) -0.0050(17) -0.0019(16) -0.0040(16) C21 0.0134(17) 0.025(2) 0.0229(19) -0.0080(16) 0.0007(14) 0.0020(15) C22 0.0145(18) 0.0218(19) 0.0216(19) -0.0042(15) 0.0006(14) -0.0008(14) C23 0.0160(18) 0.025(2) 0.027(2) -0.0035(16) -0.0018(15) -0.0037(15) C24 0.0149(18) 0.0203(18) 0.0234(19) -0.0031(15) -0.0006(14) -0.0039(14) C25 0.0209(19) 0.0228(19) 0.0210(19) -0.0028(15) -0.0003(15) -0.0071(15) C26 0.026(2) 0.026(2) 0.028(2) -0.0048(17) 0.0055(17) -0.0056(17) C27 0.041(3) 0.032(2) 0.026(2) -0.0067(18) 0.0094(19) -0.013(2) C28 0.042(3) 0.044(3) 0.020(2) -0.0006(19) -0.0007(19) -0.022(2) C29 0.031(2) 0.036(2) 0.026(2) 0.0037(18) -0.0050(18) -0.0136(19) C30 0.022(2) 0.026(2) 0.026(2) 0.0003(17) -0.0034(16) -0.0097(17) C31 0.0177(19) 0.022(2) 0.036(2) 0.0005(17) -0.0056(17) -0.0036(15) C32 0.0146(18) 0.024(2) 0.034(2) -0.0058(17) 0.0020(16) -0.0022(15) C33 0.0179(19) 0.024(2) 0.0219(19) -0.0044(15) -0.0003(15) -0.0068(15) C34 0.0125(17) 0.025(2) 0.0239(19) -0.0097(16) -0.0050(14) 0.0006(15) C35 0.0180(19) 0.027(2) 0.026(2) -0.0047(17) -0.0049(15) 0.0023(16) C36 0.022(2) 0.041(3) 0.025(2) -0.0117(19) -0.0037(16) 0.0035(18) C37 0.024(2) 0.035(2) 0.035(2) -0.020(2) -0.0081(18) 0.0047(18) C38 0.028(2) 0.022(2) 0.044(3) -0.0103(19) -0.0111(19) -0.0024(17) C39 0.020(2) 0.027(2) 0.033(2) -0.0080(17) -0.0052(16) -0.0047(16) C40 0.0170(18) 0.024(2) 0.0219(19) -0.0080(15) -0.0007(14) -0.0016(15) C41 0.021(2) 0.032(2) 0.034(2) -0.0040(19) -0.0061(17) -0.0049(17) C42 0.022(2) 0.040(3) 0.033(2) -0.006(2) -0.0070(18) -0.0074(19) C43 0.022(2) 0.041(3) 0.025(2) -0.0087(19) -0.0056(16) 0.0054(18) C44 0.036(3) 0.023(2) 0.038(3) -0.0051(19) -0.006(2) 0.0014(19) C45 0.030(2) 0.024(2) 0.036(2) -0.0096(18) -0.0090(19) -0.0039(18) Cl2 0.0475(8) 0.0406(7) 0.0777(11) -0.0044(7) -0.0009(7) -0.0109(6) Cl3 0.0473(11) 0.0554(12) 0.0433(10) -0.0048(9) -0.0084(8) -0.0041(9) Cl3A 0.0473(11) 0.0554(12) 0.0433(10) -0.0048(9) -0.0084(8) -0.0041(9) C46 0.056(4) 0.073(5) 0.083(6) 0.016(4) 0.013(4) -0.013(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 Au1 P1 2.2926(10) . ? Au1 P2 2.2938(10) . ? Au1 Cl1 2.5064(11) . ? P1 O1 1.639(3) . ? P1 C7 1.807(4) . ? P1 C1 1.819(4) . ? P2 O2 1.637(3) . ? P2 C40 1.800(4) . ? P2 C34 1.809(4) . ? O1 C13 1.404(5) . ? O2 C33 1.400(5) . ? C1 C2 1.392(6) . ? C1 C6 1.398(6) . ? C2 C3 1.391(6) . ? C2 H2 0.9500 . ? C3 C4 1.385(7) . ? C3 H3 0.9500 . ? C4 C5 1.389(7) . ? C4 H4 0.9500 . ? C5 C6 1.396(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.393(6) . ? C7 C8 1.393(6) . ? C8 C9 1.389(6) . ? C8 H8 0.9500 . ? C9 C10 1.390(6) . ? C9 H9 0.9500 . ? C10 C11 1.382(6) . ? C10 H10 0.9500 . ? C11 C12 1.393(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C22 1.380(6) . ? C13 C14 1.412(6) . ? C14 C15 1.363(6) . ? C14 H14 0.9500 . ? C15 C16 1.409(6) . ? C15 H15 0.9500 . ? C16 C21 1.415(6) . ? C16 C17 1.432(6) . ? C17 C18 1.370(7) . ? C17 H17 0.9500 . ? C18 C19 1.394(7) . ? C18 H18 0.9500 . ? C19 C20 1.376(6) . ? C19 H19 0.9500 . ? C20 C21 1.425(6) . ? C20 H20 0.9500 . ? C21 C22 1.448(5) . ? C22 C23 1.531(6) . ? C23 C24 1.509(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C33 1.376(6) . ? C24 C25 1.431(6) . ? C25 C26 1.415(6) . ? C25 C30 1.430(6) . ? C26 C27 1.379(7) . ? C26 H26 0.9500 . ? C27 C28 1.404(8) . ? C27 H27 0.9500 . ? C28 C29 1.370(7) . ? C28 H28 0.9500 . ? C29 C30 1.419(6) . ? C29 H29 0.9500 . ? C30 C31 1.413(6) . ? C31 C32 1.367(6) . ? C31 H31 0.9500 . ? C32 C33 1.413(6) . ? C32 H32 0.9500 . ? C34 C39 1.389(6) . ? C34 C35 1.398(6) . ? C35 C36 1.392(6) . ? C35 H35 0.9500 . ? C36 C37 1.380(7) . ? C36 H36 0.9500 . ? C37 C38 1.388(7) . ? C37 H37 0.9500 . ? C38 C39 1.402(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.384(6) . ? C40 C41 1.399(6) . ? C41 C42 1.394(6) . ? C41 H41 0.9500 . ? C42 C43 1.380(7) . ? C42 H42 0.9500 . ? C43 C44 1.369(7) . ? C43 H43 0.9500 . ? C44 C45 1.404(7) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? Cl2 C46 1.747(8) . ? Cl3 C46 1.537(10) . ? Cl3A C46 1.665(8) . ? Cl3A Cl3A 2.105(6) 2_667 ? 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 132.56(4) . . ? P1 Au1 Cl1 113.28(4) . . ? P2 Au1 Cl1 113.73(4) . . ? O1 P1 C7 100.14(17) . . ? O1 P1 C1 106.71(17) . . ? C7 P1 C1 102.60(18) . . ? O1 P1 Au1 112.75(11) . . ? C7 P1 Au1 113.71(14) . . ? C1 P1 Au1 118.85(14) . . ? O2 P2 C40 103.92(18) . . ? O2 P2 C34 101.90(18) . . ? C40 P2 C34 102.61(18) . . ? O2 P2 Au1 110.50(11) . . ? C40 P2 Au1 115.41(14) . . ? C34 P2 Au1 120.51(13) . . ? C13 O1 P1 120.3(3) . . ? C33 O2 P2 121.3(3) . . ? C2 C1 C6 119.9(4) . . ? C2 C1 P1 116.8(3) . . ? C6 C1 P1 123.2(3) . . ? C3 C2 C1 120.2(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 119.5(4) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? C12 C7 C8 120.1(4) . . ? C12 C7 P1 119.0(3) . . ? C8 C7 P1 120.8(3) . . ? C9 C8 C7 120.0(4) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.8(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.2(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.4(4) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? C22 C13 O1 121.4(4) . . ? C22 C13 C14 122.3(4) . . ? O1 C13 C14 116.2(4) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.9(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C21 119.7(4) . . ? C15 C16 C17 120.7(4) . . ? C21 C16 C17 119.6(4) . . ? C18 C17 C16 120.5(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.4(4) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.4(4) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 121.5(4) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C16 C21 C20 117.6(4) . . ? C16 C21 C22 120.4(4) . . ? C20 C21 C22 122.0(4) . . ? C13 C22 C21 116.9(4) . . ? C13 C22 C23 127.4(4) . . ? C21 C22 C23 115.7(3) . . ? C24 C23 C22 122.1(3) . . ? C24 C23 H23A 106.8 . . ? C22 C23 H23A 106.8 . . ? C24 C23 H23B 106.8 . . ? C22 C23 H23B 106.8 . . ? H23A C23 H23B 106.6 . . ? C33 C24 C25 117.5(4) . . ? C33 C24 C23 119.4(4) . . ? C25 C24 C23 122.4(4) . . ? C26 C25 C30 118.2(4) . . ? C26 C25 C24 122.0(4) . . ? C30 C25 C24 119.9(4) . . ? C27 C26 C25 121.0(4) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 120.5(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 120.2(4) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.7(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 121.2(4) . . ? C31 C30 C25 119.5(4) . . ? C29 C30 C25 119.4(4) . . ? C32 C31 C30 120.5(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 119.5(4) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C24 C33 O2 119.7(4) . . ? C24 C33 C32 123.1(4) . . ? O2 C33 C32 117.1(4) . . ? C39 C34 C35 119.9(4) . . ? C39 C34 P2 123.3(3) . . ? C35 C34 P2 116.9(3) . . ? C36 C35 C34 119.9(4) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 120.1(4) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.5(4) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C39 119.8(4) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C34 C39 C38 119.8(4) . . ? C34 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C45 C40 C41 119.7(4) . . ? C45 C40 P2 119.5(3) . . ? C41 C40 P2 120.8(3) . . ? C42 C41 C40 119.5(4) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C43 C42 C41 120.2(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 120.8(4) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 119.7(4) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C40 C45 C44 120.1(4) . . ? C40 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C46 Cl3A Cl3A 134.4(4) . 2_667 ? Cl3 C46 Cl3A 111.3(5) . . ? Cl3 C46 Cl2 119.9(5) . . ? Cl3A C46 Cl2 118.8(5) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 4.816 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.148 data_msb173 _database_code_depnum_ccdc_archive 'CCDC 279240' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichloro(bis(2-diphenylphosphinoxynaphthalen-1-yl) methane)digold(I) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H34 Au2 Cl2 O2 P2' _chemical_formula_sum 'C45 H34 Au2 Cl2 O2 P2' _chemical_formula_weight 1133.49 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 16.935(2) _cell_length_b 12.521(2) _cell_length_c 20.620(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.936(2) _cell_angle_gamma 90.00 _cell_volume 4319.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6791 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 24.74 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 7.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4250 _exptl_absorpt_correction_T_max 0.6356 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29492 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 24.74 _reflns_number_total 7379 _reflns_number_gt 5889 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART (Bruker-AXS, 2000)' _computing_cell_refinement 'Bruker SMART (Bruker-AXS, 2000)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker-AXS, 2000a)' _computing_publication_material 'Bruker SHELXTL (Bruker-AXS, 2000a)' _publ_section_references ; Bruker-AXS (2000). SMART, Version 5.625, Madison, WI. Bruker-AXS (2000a). SHELXTL, Version 6.10, Madison, WI. Bruker-AXS (2004). SAINT+, Version 7.03, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2002). SADABS, Version 2.05. University of G\"ottingen, Germany. Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, THe Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A seriously disordered molecule of solvent dichloromethane having only partial occupancy of a void in the lattice was detected. Reasonable attempts to model this region of electron density were unsuccessful so it was removed with the SQUEEZE option of PLATON (Spek, 2005). H-atoms were placed in calculated positions (C---H = 0.95 \%A) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+42.7502P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7379 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _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 Au1 Au 0.63999(3) 0.74661(4) 0.49868(2) 0.03485(14) Uani 1 1 d . . . Au2 Au 0.91316(3) 0.36220(4) 0.57236(2) 0.03573(14) Uani 1 1 d . . . Cl1 Cl 0.60048(19) 0.6817(3) 0.39567(15) 0.0507(9) Uani 1 1 d . . . Cl2 Cl 1.01005(18) 0.2819(3) 0.64595(15) 0.0469(8) Uani 1 1 d . . . P1 P 0.67663(17) 0.8186(3) 0.59660(14) 0.0305(7) Uani 1 1 d . . . P2 P 0.81199(18) 0.4383(3) 0.50820(14) 0.0337(7) Uani 1 1 d . . . O1 O 0.7023(4) 0.7368(6) 0.6560(3) 0.0322(18) Uani 1 1 d . . . O2 O 0.7837(4) 0.5501(6) 0.5366(3) 0.0329(18) Uani 1 1 d . . . C1 C 0.7610(6) 0.9048(10) 0.6012(6) 0.034(3) Uani 1 1 d . . . C2 C 0.7846(7) 0.9426(11) 0.5451(7) 0.047(3) Uani 1 1 d . . . H2 H 0.7568 0.9209 0.5036 0.056 Uiso 1 1 calc R . . C3 C 0.8489(8) 1.0125(10) 0.5480(8) 0.052(4) Uani 1 1 d . . . H3 H 0.8645 1.0390 0.5088 0.062 Uiso 1 1 calc R . . C4 C 0.8897(8) 1.0432(13) 0.6081(9) 0.066(5) Uani 1 1 d . . . H4 H 0.9335 1.0912 0.6105 0.079 Uiso 1 1 calc R . . C5 C 0.8666(7) 1.0034(11) 0.6651(8) 0.051(4) Uani 1 1 d . . . H5 H 0.8957 1.0230 0.7065 0.062 Uiso 1 1 calc R . . C6 C 0.8025(7) 0.9365(10) 0.6624(6) 0.039(3) Uani 1 1 d . . . H6 H 0.7861 0.9116 0.7017 0.047 Uiso 1 1 calc R . . C7 C 0.5991(6) 0.8986(9) 0.6229(5) 0.031(3) Uani 1 1 d . . . C8 C 0.5713(7) 0.9884(9) 0.5855(6) 0.035(3) Uani 1 1 d . . . H8 H 0.5939 1.0061 0.5475 0.041 Uiso 1 1 calc R . . C9 C 0.5112(7) 1.0514(9) 0.6036(6) 0.036(3) Uani 1 1 d . . . H9 H 0.4907 1.1101 0.5770 0.043 Uiso 1 1 calc R . . C10 C 0.4813(7) 1.0285(12) 0.6604(6) 0.047(4) Uani 1 1 d . . . H10 H 0.4425 1.0743 0.6743 0.057 Uiso 1 1 calc R . . C11 C 0.5065(7) 0.9412(9) 0.6968(6) 0.036(3) Uani 1 1 d . . . H11 H 0.4834 0.9247 0.7348 0.043 Uiso 1 1 calc R . . C12 C 0.5662(6) 0.8755(9) 0.6788(5) 0.032(3) Uani 1 1 d . . . H12 H 0.5841 0.8150 0.7047 0.039 Uiso 1 1 calc R . . C13 C 0.6842(7) 0.6293(10) 0.6536(5) 0.033(3) Uani 1 1 d . . . C14 C 0.6031(7) 0.5971(10) 0.6422(5) 0.033(3) Uani 1 1 d . . . H14 H 0.5614 0.6485 0.6344 0.040 Uiso 1 1 calc R . . C15 C 0.5859(7) 0.4899(10) 0.6426(5) 0.036(3) Uani 1 1 d . . . H15 H 0.5317 0.4671 0.6347 0.043 Uiso 1 1 calc R . . C16 C 0.6466(7) 0.4139(9) 0.6543(5) 0.032(3) Uani 1 1 d . . . C17 C 0.6286(7) 0.3045(10) 0.6522(5) 0.038(3) Uani 1 1 d . . . H17 H 0.5744 0.2821 0.6433 0.046 Uiso 1 1 calc R . . C18 C 0.6887(8) 0.2288(10) 0.6630(5) 0.042(3) Uani 1 1 d . . . H18 H 0.6762 0.1548 0.6615 0.050 Uiso 1 1 calc R . . C19 C 0.7690(7) 0.2634(11) 0.6762(5) 0.040(3) Uani 1 1 d . . . H19 H 0.8105 0.2119 0.6842 0.049 Uiso 1 1 calc R . . C20 C 0.7878(7) 0.3675(9) 0.6778(5) 0.034(3) Uani 1 1 d . . . H20 H 0.8424 0.3880 0.6871 0.041 Uiso 1 1 calc R . . C21 C 0.7283(6) 0.4475(9) 0.6658(5) 0.030(3) Uani 1 1 d . . . C22 C 0.7458(6) 0.5594(10) 0.6641(5) 0.033(3) Uani 1 1 d . . . C23 C 0.8307(6) 0.6018(9) 0.6773(5) 0.031(3) Uani 1 1 d . . . H23A H 0.8332 0.6558 0.7127 0.037 Uiso 1 1 calc R . . H23B H 0.8660 0.5421 0.6949 0.037 Uiso 1 1 calc R . . C24 C 0.8659(6) 0.6513(9) 0.6218(5) 0.029(3) Uani 1 1 d . . . C25 C 0.9297(6) 0.7274(8) 0.6369(5) 0.029(3) Uani 1 1 d . . . C26 C 0.9642(7) 0.7495(11) 0.7020(6) 0.042(3) Uani 1 1 d . . . H26 H 0.9440 0.7148 0.7370 0.050 Uiso 1 1 calc R . . C27 C 1.0266(8) 0.8205(12) 0.7162(7) 0.052(4) Uani 1 1 d . . . H27 H 1.0471 0.8362 0.7607 0.062 Uiso 1 1 calc R . . C28 C 1.0601(8) 0.8693(12) 0.6667(7) 0.056(4) Uani 1 1 d . . . H28 H 1.1049 0.9153 0.6771 0.068 Uiso 1 1 calc R . . C29 C 1.0281(7) 0.8504(10) 0.6026(7) 0.047(3) Uani 1 1 d . . . H29 H 1.0494 0.8860 0.5684 0.056 Uiso 1 1 calc R . . C30 C 0.9630(7) 0.7778(9) 0.5865(6) 0.036(3) Uani 1 1 d . . . C31 C 0.9315(8) 0.7548(10) 0.5209(6) 0.044(3) Uani 1 1 d . . . H31 H 0.9522 0.7909 0.4866 0.052 Uiso 1 1 calc R . . C32 C 0.8722(7) 0.6822(10) 0.5055(6) 0.038(3) Uani 1 1 d . . . H32 H 0.8514 0.6676 0.4609 0.045 Uiso 1 1 calc R . . C33 C 0.8420(6) 0.6292(10) 0.5560(5) 0.035(3) Uani 1 1 d . . . C34 C 0.8258(7) 0.4617(11) 0.4249(5) 0.043(3) Uani 1 1 d . . . C35 C 0.8979(7) 0.4389(9) 0.4041(6) 0.037(3) Uani 1 1 d . . . H35 H 0.9409 0.4101 0.4340 0.044 Uiso 1 1 calc R . . C36 C 0.9073(8) 0.4581(11) 0.3399(7) 0.052(4) Uani 1 1 d . . . H36 H 0.9571 0.4436 0.3260 0.063 Uiso 1 1 calc R . . C37 C 0.8454(8) 0.4979(13) 0.2960(7) 0.058(4) Uani 1 1 d . . . H37 H 0.8513 0.5074 0.2513 0.069 Uiso 1 1 calc R . . C38 C 0.7743(8) 0.5243(17) 0.3169(7) 0.081(6) Uani 1 1 d . . . H38 H 0.7321 0.5554 0.2871 0.097 Uiso 1 1 calc R . . C39 C 0.7648(8) 0.5055(16) 0.3805(6) 0.077(6) Uani 1 1 d . . . H39 H 0.7155 0.5228 0.3945 0.093 Uiso 1 1 calc R . . C40 C 0.7190(7) 0.3637(10) 0.4992(5) 0.034(3) Uani 1 1 d . . . C41 C 0.6455(7) 0.4139(11) 0.4962(6) 0.043(3) Uani 1 1 d . . . H41 H 0.6428 0.4889 0.5024 0.051 Uiso 1 1 calc R . . C42 C 0.5760(7) 0.3538(12) 0.4841(6) 0.048(3) Uani 1 1 d . . . H42 H 0.5256 0.3866 0.4846 0.058 Uiso 1 1 calc R . . C43 C 0.5808(8) 0.2457(12) 0.4713(6) 0.047(3) Uani 1 1 d . . . H43 H 0.5332 0.2051 0.4607 0.057 Uiso 1 1 calc R . . C44 C 0.6535(8) 0.1968(12) 0.4737(7) 0.053(4) Uani 1 1 d . . . H44 H 0.6565 0.1222 0.4659 0.064 Uiso 1 1 calc R . . C45 C 0.7227(8) 0.2573(11) 0.4875(6) 0.045(3) Uani 1 1 d . . . H45 H 0.7732 0.2238 0.4889 0.054 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 Au1 0.0307(2) 0.0454(3) 0.0286(2) -0.0065(2) 0.00504(17) 0.0031(2) Au2 0.0318(2) 0.0439(3) 0.0311(2) -0.0078(2) 0.00384(18) 0.0019(2) Cl1 0.0434(18) 0.072(2) 0.0360(17) -0.0174(16) 0.0037(14) -0.0013(17) Cl2 0.0386(17) 0.055(2) 0.0438(18) -0.0053(15) -0.0048(14) 0.0031(15) P1 0.0282(15) 0.0367(18) 0.0267(15) -0.0007(13) 0.0050(12) 0.0027(13) P2 0.0317(16) 0.0420(19) 0.0280(15) -0.0059(14) 0.0064(12) 0.0034(14) O1 0.041(4) 0.023(4) 0.030(4) -0.004(3) -0.001(3) 0.008(4) O2 0.035(4) 0.039(5) 0.025(4) -0.005(3) 0.009(3) 0.005(4) C1 0.026(6) 0.039(7) 0.038(7) -0.004(6) 0.008(5) 0.004(5) C2 0.032(7) 0.059(9) 0.050(8) 0.003(7) 0.010(6) 0.012(6) C3 0.053(8) 0.027(7) 0.082(11) 0.016(7) 0.033(8) 0.005(6) C4 0.031(8) 0.065(11) 0.099(13) -0.029(10) 0.004(8) 0.016(7) C5 0.035(7) 0.050(9) 0.069(10) -0.026(8) 0.005(7) 0.013(7) C6 0.038(7) 0.038(8) 0.043(7) -0.006(6) 0.008(6) 0.006(6) C7 0.027(6) 0.034(7) 0.031(6) -0.006(5) -0.003(5) 0.000(5) C8 0.034(6) 0.032(7) 0.039(7) -0.001(5) 0.012(5) 0.003(5) C9 0.042(7) 0.021(6) 0.044(7) 0.007(5) 0.002(6) 0.005(5) C10 0.029(7) 0.074(10) 0.038(7) -0.020(7) 0.003(5) -0.005(7) C11 0.041(7) 0.032(7) 0.036(7) 0.002(6) 0.012(5) 0.006(6) C12 0.037(6) 0.033(7) 0.027(6) 0.005(5) 0.003(5) 0.006(5) C13 0.039(7) 0.039(7) 0.020(5) 0.001(5) 0.007(5) 0.007(6) C14 0.032(6) 0.041(8) 0.027(6) -0.002(5) 0.006(5) 0.012(5) C15 0.032(6) 0.042(8) 0.034(6) 0.000(6) 0.007(5) 0.010(6) C16 0.037(7) 0.027(7) 0.031(6) -0.005(5) 0.010(5) -0.004(5) C17 0.040(7) 0.050(8) 0.025(6) -0.008(6) 0.007(5) -0.002(6) C18 0.062(9) 0.039(8) 0.027(6) 0.002(5) 0.014(6) 0.000(6) C19 0.048(8) 0.050(9) 0.023(6) 0.002(6) 0.006(5) 0.019(7) C20 0.047(7) 0.030(7) 0.025(6) -0.002(5) 0.006(5) 0.015(6) C21 0.037(6) 0.038(7) 0.016(5) -0.004(5) 0.008(5) 0.009(5) C22 0.029(6) 0.044(8) 0.026(6) 0.002(5) 0.007(5) 0.006(5) C23 0.035(7) 0.028(7) 0.026(6) -0.009(5) -0.001(5) 0.000(5) C24 0.027(6) 0.031(7) 0.031(6) -0.003(5) 0.008(5) 0.011(5) C25 0.026(6) 0.024(7) 0.038(6) -0.003(5) 0.007(5) 0.009(5) C26 0.028(6) 0.059(9) 0.039(7) 0.003(7) 0.007(5) 0.005(6) C27 0.041(8) 0.060(10) 0.050(8) 0.000(7) -0.007(6) 0.000(7) C28 0.035(7) 0.060(10) 0.074(10) -0.001(8) 0.009(7) -0.011(7) C29 0.038(7) 0.042(8) 0.067(9) 0.009(7) 0.027(7) -0.003(6) C30 0.042(7) 0.029(7) 0.041(7) -0.008(5) 0.017(6) 0.003(5) C31 0.055(8) 0.034(7) 0.048(8) 0.002(6) 0.028(6) 0.007(7) C32 0.043(7) 0.042(8) 0.030(6) -0.004(6) 0.008(5) 0.002(6) C33 0.030(6) 0.047(8) 0.030(6) -0.011(6) 0.007(5) 0.004(6) C34 0.030(6) 0.073(10) 0.026(6) -0.008(6) 0.008(5) 0.006(6) C35 0.035(7) 0.035(7) 0.043(7) 0.008(6) 0.015(5) 0.000(5) C36 0.041(8) 0.061(10) 0.059(9) 0.009(7) 0.022(7) 0.019(7) C37 0.052(9) 0.084(12) 0.042(8) -0.001(8) 0.024(7) 0.002(8) C38 0.033(8) 0.169(19) 0.039(8) 0.007(10) -0.001(6) 0.015(10) C39 0.040(8) 0.165(19) 0.030(7) 0.008(9) 0.016(6) 0.026(10) C40 0.041(7) 0.037(7) 0.023(6) -0.002(5) 0.006(5) -0.002(6) C41 0.036(7) 0.061(9) 0.031(6) -0.010(6) 0.006(5) 0.004(7) C42 0.027(7) 0.077(11) 0.039(7) -0.007(7) 0.002(5) 0.004(7) C43 0.040(7) 0.070(10) 0.032(7) -0.011(7) 0.005(5) -0.009(7) C44 0.048(8) 0.053(9) 0.059(9) 0.004(7) 0.009(7) -0.014(7) C45 0.042(7) 0.055(9) 0.037(7) 0.005(7) 0.007(5) 0.003(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 Au1 P1 2.210(3) . ? Au1 Cl1 2.276(3) . ? Au2 P2 2.211(3) . ? Au2 Cl2 2.288(3) . ? P1 O1 1.603(8) . ? P1 C1 1.782(12) . ? P1 C7 1.800(11) . ? P2 O2 1.619(8) . ? P2 C34 1.793(11) . ? P2 C40 1.815(12) . ? O1 C13 1.379(14) . ? O2 C33 1.412(14) . ? C1 C2 1.366(17) . ? C1 C6 1.403(16) . ? C2 C3 1.391(18) . ? C2 H2 0.9500 . ? C3 C4 1.38(2) . ? C3 H3 0.9500 . ? C4 C5 1.39(2) . ? C4 H4 0.9500 . ? C5 C6 1.365(18) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.387(15) . ? C7 C8 1.403(16) . ? C8 C9 1.385(15) . ? C8 H8 0.9500 . ? C9 C10 1.376(17) . ? C9 H9 0.9500 . ? C10 C11 1.356(17) . ? C10 H10 0.9500 . ? C11 C12 1.399(15) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C22 1.354(15) . ? C13 C14 1.416(16) . ? C14 C15 1.374(16) . ? C14 H14 0.9500 . ? C15 C16 1.394(15) . ? C15 H15 0.9500 . ? C16 C17 1.403(16) . ? C16 C21 1.430(15) . ? C17 C18 1.384(17) . ? C17 H17 0.9500 . ? C18 C19 1.412(18) . ? C18 H18 0.9500 . ? C19 C20 1.340(17) . ? C19 H19 0.9500 . ? C20 C21 1.414(15) . ? C20 H20 0.9500 . ? C21 C22 1.433(16) . ? C22 C23 1.517(15) . ? C23 C24 1.504(15) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C33 1.383(15) . ? C24 C25 1.439(15) . ? C25 C26 1.405(16) . ? C25 C30 1.407(16) . ? C26 C27 1.378(18) . ? C26 H26 0.9500 . ? C27 C28 1.384(19) . ? C27 H27 0.9500 . ? C28 C29 1.369(19) . ? C28 H28 0.9500 . ? C29 C30 1.428(17) . ? C29 H29 0.9500 . ? C30 C31 1.404(17) . ? C31 C32 1.356(17) . ? C31 H31 0.9500 . ? C32 C33 1.397(16) . ? C32 H32 0.9500 . ? C34 C39 1.382(18) . ? C34 C35 1.386(15) . ? C35 C36 1.379(17) . ? C35 H35 0.9500 . ? C36 C37 1.368(18) . ? C36 H36 0.9500 . ? C37 C38 1.381(18) . ? C37 H37 0.9500 . ? C38 C39 1.368(18) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.357(17) . ? C40 C41 1.388(16) . ? C41 C42 1.385(17) . ? C41 H41 0.9500 . ? C42 C43 1.384(19) . ? C42 H42 0.9500 . ? C43 C44 1.368(19) . ? C43 H43 0.9500 . ? C44 C45 1.387(18) . ? C44 H44 0.9500 . ? C45 H45 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 P1 Au1 Cl1 176.84(13) . . ? P2 Au2 Cl2 174.63(12) . . ? O1 P1 C1 103.1(5) . . ? O1 P1 C7 104.4(5) . . ? C1 P1 C7 105.2(5) . . ? O1 P1 Au1 116.2(3) . . ? C1 P1 Au1 113.9(4) . . ? C7 P1 Au1 112.8(4) . . ? O2 P2 C34 107.2(5) . . ? O2 P2 C40 100.5(5) . . ? C34 P2 C40 103.0(5) . . ? O2 P2 Au2 113.7(3) . . ? C34 P2 Au2 116.1(4) . . ? C40 P2 Au2 114.8(4) . . ? C13 O1 P1 124.3(7) . . ? C33 O2 P2 118.4(7) . . ? C2 C1 C6 119.5(12) . . ? C2 C1 P1 120.2(9) . . ? C6 C1 P1 120.3(9) . . ? C1 C2 C3 120.7(13) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 119.7(14) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.6(14) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.8(13) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 119.7(12) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 118.7(10) . . ? C12 C7 P1 122.7(9) . . ? C8 C7 P1 118.6(9) . . ? C9 C8 C7 120.4(11) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.6(11) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 120.9(12) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 120.3(11) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.0(11) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C22 C13 O1 117.7(10) . . ? C22 C13 C14 123.1(11) . . ? O1 C13 C14 119.2(10) . . ? C15 C14 C13 118.6(11) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 121.0(11) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 120.6(11) . . ? C15 C16 C21 119.8(11) . . ? C17 C16 C21 119.5(11) . . ? C18 C17 C16 120.9(12) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 118.8(12) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 121.4(12) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 121.6(12) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C20 C21 C16 117.7(11) . . ? C20 C21 C22 123.5(11) . . ? C16 C21 C22 118.8(10) . . ? C13 C22 C21 118.6(11) . . ? C13 C22 C23 119.2(11) . . ? C21 C22 C23 122.1(10) . . ? C24 C23 C22 118.9(9) . . ? C24 C23 H23A 107.6 . . ? C22 C23 H23A 107.6 . . ? C24 C23 H23B 107.6 . . ? C22 C23 H23B 107.6 . . ? H23A C23 H23B 107.0 . . ? C33 C24 C25 116.1(10) . . ? C33 C24 C23 125.1(10) . . ? C25 C24 C23 118.7(9) . . ? C26 C25 C30 117.6(11) . . ? C26 C25 C24 121.6(11) . . ? C30 C25 C24 120.7(10) . . ? C27 C26 C25 121.4(12) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 121.2(13) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 119.3(13) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 120.6(12) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C25 118.9(11) . . ? C31 C30 C29 121.2(11) . . ? C25 C30 C29 119.9(11) . . ? C32 C31 C30 121.3(11) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 119.2(11) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C24 C33 C32 123.5(11) . . ? C24 C33 O2 120.2(10) . . ? C32 C33 O2 116.3(9) . . ? C39 C34 C35 118.7(11) . . ? C39 C34 P2 120.3(9) . . ? C35 C34 P2 121.0(9) . . ? C36 C35 C34 120.0(11) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 120.5(12) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.8(13) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 119.7(14) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C34 121.1(12) . . ? C38 C39 H39 119.4 . . ? C34 C39 H39 119.4 . . ? C45 C40 C41 120.1(12) . . ? C45 C40 P2 117.4(9) . . ? C41 C40 P2 122.0(10) . . ? C42 C41 C40 119.6(13) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 119.5(12) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C44 C43 C42 120.6(13) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 119.3(14) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C40 C45 C44 120.8(13) . . ? C40 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.74 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.546 _refine_diff_density_min -1.764 _refine_diff_density_rms 0.184