# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb488_0m #TrackingRef '05 msb488_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H52 Cl4 O2 P2 Ru2, C H2 Cl2' _chemical_formula_sum 'C53 H54 Cl6 O2 P2 Ru2' _chemical_formula_weight 1199.74 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.277(4) _cell_length_b 12.280(4) _cell_length_c 21.270(7) _cell_angle_alpha 95.437(4) _cell_angle_beta 91.368(4) _cell_angle_gamma 92.086(4) _cell_volume 2929.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2554 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.09 _exptl_crystal_description Slab _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6236 _exptl_absorpt_correction_T_max 0.9322 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008b)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 40 sec/frame was used. Analysis of 2750 reflections having I/\s(I) > 15 and chosen from the full data set with CELL_NOW (Sheldrick, 2008a) showed the crystal to belong to the triclinic system and to consist of one major and two minor components, the last of which was considered to be of negligible importance. The raw data were processed using the multi-component version of SAINT under control of the two-component orientation file generated by CELL_NOW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43808 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.20 _reflns_number_total 12820 _reflns_number_gt 10168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. One isopropyl group is disordered over two separate sites in a 3:2 ratio. These were refined subject to restraints that the two components of the disorder adopt approximately the same geometry. Following several attempts to model the disorder in a site partially occupied by solvent dichloromethane which proved unsuccessful, the density in this site was removed with the SQUEEZE option of PLATON (SPEK, 2010). Trial refinements with the full 2-component reflection file and with that for the major component of the crystal indicated the latter to be more satisfactory. ; _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^)+(0.0773P)^2^+7.1225P] 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 12820 _refine_ls_number_parameters 600 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _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 Ru1 Ru 0.86227(3) 0.14292(3) 0.076944(15) 0.02320(10) Uani 1 1 d . A . Ru2 Ru 0.35594(3) 0.40037(3) 0.396194(17) 0.02842(11) Uani 1 1 d . . . Cl1 Cl 0.87098(9) 0.19492(10) -0.02987(5) 0.0304(2) Uani 1 1 d . . . Cl2 Cl 0.71588(9) 0.00256(9) 0.04090(5) 0.0287(2) Uani 1 1 d . . . Cl3 Cl 0.54689(9) 0.43286(11) 0.35114(5) 0.0326(3) Uani 1 1 d . . . Cl4 Cl 0.33114(10) 0.59462(11) 0.40009(6) 0.0378(3) Uani 1 1 d . . . P1 P 0.71220(9) 0.27010(9) 0.09152(5) 0.0212(2) Uani 1 1 d . . . P2 P 0.24388(9) 0.39597(11) 0.30104(5) 0.0261(2) Uani 1 1 d . . . O1 O 0.6819(3) 0.2781(3) 0.21631(14) 0.0284(7) Uani 1 1 d . . . O2 O 0.1608(3) 0.1860(3) 0.28521(16) 0.0382(8) Uani 1 1 d . . . C1 C 1.1290(5) 0.2631(6) 0.0535(3) 0.060(2) Uani 1 1 d . . . H1A H 1.1072 0.3396 0.0614 0.090 Uiso 1 1 calc R . . H1B H 1.1174 0.2391 0.0084 0.090 Uiso 1 1 calc R . . H1C H 1.2125 0.2565 0.0659 0.090 Uiso 1 1 calc R . . C2 C 1.0530(4) 0.1935(4) 0.0909(2) 0.0332(11) Uani 1 1 d . A . C3 C 1.0451(4) 0.0777(4) 0.0754(2) 0.0282(10) Uani 1 1 d . . . H3 H 1.0893 0.0457 0.0414 0.034 Uiso 1 1 calc R . . C4 C 0.9739(4) 0.0116(4) 0.1092(2) 0.0321(10) Uani 1 1 d . A . H4 H 0.9702 -0.0652 0.0980 0.038 Uiso 1 1 calc R . . C5 C 0.9060(4) 0.0557(6) 0.1602(2) 0.0456(15) Uani 1 1 d D . . C6 C 0.9152(4) 0.1676(6) 0.1765(2) 0.0497(16) Uani 1 1 d . A . H6 H 0.8722 0.1986 0.2112 0.060 Uiso 1 1 calc R . . C7 C 0.9881(5) 0.2372(5) 0.1423(3) 0.0465(15) Uani 1 1 d . . . H7 H 0.9928 0.3138 0.1543 0.056 Uiso 1 1 calc R A . C8 C 0.8367(8) -0.0387(9) 0.1907(5) 0.042(2) Uani 0.589(6) 1 d PD A 1 H8 H 0.8114 -0.0958 0.1558 0.050 Uiso 0.589(6) 1 calc PR A 1 C9 C 0.7272(10) -0.0015(10) 0.2235(5) 0.058(2) Uani 0.589(6) 1 d PD A 1 H9A H 0.6746 0.0307 0.1935 0.087 Uiso 0.589(6) 1 calc PR A 1 H9B H 0.7494 0.0535 0.2586 0.087 Uiso 0.589(6) 1 calc PR A 1 H9C H 0.6861 -0.0642 0.2397 0.087 Uiso 0.589(6) 1 calc PR A 1 C10 C 0.9212(10) -0.0921(10) 0.2358(5) 0.057(2) Uani 0.589(6) 1 d PD A 1 H10A H 0.9912 -0.1167 0.2130 0.085 Uiso 0.589(6) 1 calc PR A 1 H10B H 0.8801 -0.1549 0.2520 0.085 Uiso 0.589(6) 1 calc PR A 1 H10C H 0.9459 -0.0384 0.2712 0.085 Uiso 0.589(6) 1 calc PR A 1 C8A C 0.8212(12) 0.0196(12) 0.2077(5) 0.042(2) Uani 0.411(6) 1 d PD A 2 H8A H 0.7450 0.0582 0.2048 0.050 Uiso 0.411(6) 1 calc PR A 2 C9A C 0.8028(16) -0.1008(13) 0.1845(8) 0.058(2) Uani 0.411(6) 1 d PD A 2 H9A1 H 0.7681 -0.1077 0.1415 0.087 Uiso 0.411(6) 1 calc PR A 2 H9A2 H 0.7490 -0.1361 0.2126 0.087 Uiso 0.411(6) 1 calc PR A 2 H9A3 H 0.8793 -0.1361 0.1844 0.087 Uiso 0.411(6) 1 calc PR A 2 C10A C 0.8731(14) 0.0361(14) 0.2748(7) 0.057(2) Uani 0.411(6) 1 d PD A 2 H10D H 0.8815 0.1147 0.2883 0.085 Uiso 0.411(6) 1 calc PR A 2 H10E H 0.9512 0.0037 0.2760 0.085 Uiso 0.411(6) 1 calc PR A 2 H10F H 0.8201 0.0007 0.3032 0.085 Uiso 0.411(6) 1 calc PR A 2 C11 C 0.5930(3) 0.2840(4) 0.0335(2) 0.0244(9) Uani 1 1 d . . . C12 C 0.5151(4) 0.3677(4) 0.0455(2) 0.0281(9) Uani 1 1 d . . . H12 H 0.5280 0.4193 0.0815 0.034 Uiso 1 1 calc R . . C13 C 0.4181(4) 0.3762(4) 0.0051(2) 0.0325(10) Uani 1 1 d . . . H13 H 0.3647 0.4336 0.0135 0.039 Uiso 1 1 calc R . . C14 C 0.3989(4) 0.3017(4) -0.0471(2) 0.0344(11) Uani 1 1 d . . . H14 H 0.3321 0.3074 -0.0745 0.041 Uiso 1 1 calc R . . C15 C 0.4769(4) 0.2187(4) -0.0596(2) 0.0338(11) Uani 1 1 d . . . H15 H 0.4637 0.1677 -0.0958 0.041 Uiso 1 1 calc R . . C16 C 0.5743(4) 0.2093(4) -0.0199(2) 0.0281(9) Uani 1 1 d . . . H16 H 0.6281 0.1525 -0.0289 0.034 Uiso 1 1 calc R . . C17 C 0.7767(3) 0.4098(3) 0.1069(2) 0.0221(8) Uani 1 1 d . . . C18 C 0.7785(5) 0.4750(5) 0.1640(2) 0.0434(13) Uani 1 1 d . . . H18 H 0.7379 0.4504 0.1990 0.052 Uiso 1 1 calc R . . C19 C 0.8395(6) 0.5764(5) 0.1703(3) 0.0516(15) Uani 1 1 d . . . H19 H 0.8394 0.6207 0.2094 0.062 Uiso 1 1 calc R . . C20 C 0.8994(4) 0.6128(4) 0.1207(3) 0.0385(12) Uani 1 1 d . . . H20 H 0.9419 0.6815 0.1254 0.046 Uiso 1 1 calc R . . C21 C 0.8976(4) 0.5490(4) 0.0637(3) 0.0377(12) Uani 1 1 d . . . H21 H 0.9384 0.5743 0.0290 0.045 Uiso 1 1 calc R . . C22 C 0.8371(4) 0.4485(4) 0.0567(2) 0.0317(10) Uani 1 1 d . . . H22 H 0.8367 0.4054 0.0171 0.038 Uiso 1 1 calc R . . C23 C 0.6299(4) 0.2527(4) 0.16662(19) 0.0231(8) Uani 1 1 d . . . C24 C 0.5053(4) 0.2072(4) 0.16497(19) 0.0227(8) Uani 1 1 d . . . C25 C 0.4625(4) 0.1220(4) 0.1213(2) 0.0263(9) Uani 1 1 d . . . H25 H 0.5110 0.0956 0.0877 0.032 Uiso 1 1 calc R . . C26 C 0.3499(4) 0.0761(4) 0.1267(2) 0.0302(10) Uani 1 1 d . . . H26 H 0.3218 0.0163 0.0979 0.036 Uiso 1 1 calc R . . C27 C 0.2782(4) 0.1180(4) 0.1746(2) 0.0278(9) Uani 1 1 d . . . H27 H 0.2017 0.0852 0.1792 0.033 Uiso 1 1 calc R . . C28 C 0.3175(4) 0.2079(4) 0.21616(19) 0.0242(9) Uani 1 1 d . . . C29 C 0.4325(4) 0.2515(4) 0.2129(2) 0.0260(9) Uani 1 1 d . . . H29 H 0.4612 0.3099 0.2424 0.031 Uiso 1 1 calc R . . C30 C 0.2341(4) 0.2497(4) 0.2654(2) 0.0282(10) Uani 1 1 d . . . C31 C 0.2795(4) 0.4764(4) 0.2348(2) 0.0282(9) Uani 1 1 d . . . C32 C 0.1920(4) 0.4868(5) 0.1890(2) 0.0345(11) Uani 1 1 d . . . H32 H 0.1147 0.4555 0.1932 0.041 Uiso 1 1 calc R . . C33 C 0.2172(4) 0.5428(5) 0.1371(2) 0.0421(13) Uani 1 1 d . . . H33 H 0.1572 0.5496 0.1057 0.051 Uiso 1 1 calc R . . C34 C 0.3295(5) 0.5890(5) 0.1308(3) 0.0415(12) Uani 1 1 d . . . H34 H 0.3471 0.6274 0.0953 0.050 Uiso 1 1 calc R . . C35 C 0.4155(4) 0.5787(5) 0.1767(3) 0.0407(12) Uani 1 1 d . . . H35 H 0.4930 0.6095 0.1721 0.049 Uiso 1 1 calc R . . C36 C 0.3919(4) 0.5247(5) 0.2291(2) 0.0354(11) Uani 1 1 d . . . H36 H 0.4515 0.5205 0.2610 0.042 Uiso 1 1 calc R . . C37 C 0.0883(4) 0.4322(5) 0.3147(2) 0.0314(10) Uani 1 1 d . . . C38 C -0.0065(4) 0.3571(5) 0.3176(2) 0.0377(12) Uani 1 1 d . . . H38 H 0.0056 0.2808 0.3115 0.045 Uiso 1 1 calc R . . C39 C -0.1203(4) 0.3955(6) 0.3296(2) 0.0441(15) Uani 1 1 d . . . H39 H -0.1853 0.3445 0.3311 0.053 Uiso 1 1 calc R . . C40 C -0.1392(4) 0.5049(6) 0.3391(2) 0.0461(14) Uani 1 1 d . . . H40 H -0.2165 0.5297 0.3475 0.055 Uiso 1 1 calc R . . C41 C -0.0449(4) 0.5792(5) 0.3365(2) 0.0424(13) Uani 1 1 d . . . H41 H -0.0577 0.6554 0.3432 0.051 Uiso 1 1 calc R . . C42 C 0.0680(4) 0.5435(5) 0.3242(2) 0.0376(12) Uani 1 1 d . . . H42 H 0.1320 0.5954 0.3222 0.045 Uiso 1 1 calc R . . C43 C 0.1184(5) 0.4394(6) 0.4845(3) 0.0511(16) Uani 1 1 d . . . H43A H 0.0601 0.4242 0.4496 0.077 Uiso 1 1 calc R . . H43B H 0.1389 0.5180 0.4901 0.077 Uiso 1 1 calc R . . H43C H 0.0847 0.4166 0.5235 0.077 Uiso 1 1 calc R . . C44 C 0.2272(4) 0.3777(5) 0.4699(2) 0.0411(13) Uani 1 1 d . . . C45 C 0.2256(4) 0.2832(5) 0.4254(2) 0.0380(12) Uani 1 1 d . . . H45 H 0.1525 0.2581 0.4050 0.046 Uiso 1 1 calc R . . C46 C 0.3298(5) 0.2254(5) 0.4106(3) 0.0411(12) Uani 1 1 d . . . H46 H 0.3256 0.1626 0.3808 0.049 Uiso 1 1 calc R . . C47 C 0.4402(5) 0.2618(5) 0.4404(3) 0.0435(13) Uani 1 1 d . . . C48 C 0.4407(5) 0.3547(5) 0.4860(3) 0.0434(13) Uani 1 1 d . . . H48 H 0.5132 0.3792 0.5073 0.052 Uiso 1 1 calc R . . C49 C 0.3398(5) 0.4098(5) 0.5001(2) 0.0394(12) Uani 1 1 d . . . H49 H 0.3445 0.4712 0.5309 0.047 Uiso 1 1 calc R . . C50 C 0.5550(6) 0.2054(6) 0.4273(4) 0.0628(18) Uani 1 1 d . . . H50 H 0.6197 0.2632 0.4272 0.075 Uiso 1 1 calc R . . C51 C 0.5799(8) 0.1377(7) 0.4837(5) 0.085(3) Uani 1 1 d . . . H51A H 0.5982 0.1874 0.5218 0.128 Uiso 1 1 calc R . . H51B H 0.6477 0.0916 0.4744 0.128 Uiso 1 1 calc R . . H51C H 0.5098 0.0914 0.4906 0.128 Uiso 1 1 calc R . . C52 C 0.5542(8) 0.1358(8) 0.3634(5) 0.094(3) Uani 1 1 d . . . H52A H 0.4953 0.0752 0.3635 0.140 Uiso 1 1 calc R . . H52B H 0.6330 0.1065 0.3564 0.140 Uiso 1 1 calc R . . H52C H 0.5339 0.1814 0.3296 0.140 Uiso 1 1 calc R . . C53 C 0.5994(7) 0.7386(7) 0.3579(4) 0.074(2) Uani 1 1 d . . . H53A H 0.5795 0.6703 0.3773 0.089 Uiso 1 1 calc R . . H53B H 0.5268 0.7812 0.3561 0.089 Uiso 1 1 calc R . . Cl5 Cl 0.6502(2) 0.7070(2) 0.28170(11) 0.0906(7) Uani 1 1 d . . . Cl6 Cl 0.7108(3) 0.8157(2) 0.40403(12) 0.1054(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01176(16) 0.0329(2) 0.02386(18) -0.00314(13) -0.00209(12) 0.00360(13) Ru2 0.01582(17) 0.0414(2) 0.02696(19) -0.00024(15) -0.00206(13) -0.00326(15) Cl1 0.0203(5) 0.0442(7) 0.0268(5) 0.0011(4) 0.0022(4) 0.0059(4) Cl2 0.0181(5) 0.0353(6) 0.0310(5) -0.0053(4) -0.0032(4) 0.0004(4) Cl3 0.0144(5) 0.0508(7) 0.0317(5) 0.0001(5) -0.0028(4) -0.0006(4) Cl4 0.0277(6) 0.0444(7) 0.0397(6) -0.0031(5) -0.0063(5) 0.0031(5) P1 0.0117(4) 0.0295(6) 0.0219(5) 0.0009(4) -0.0002(4) 0.0019(4) P2 0.0121(5) 0.0411(7) 0.0240(5) -0.0016(4) 0.0017(4) -0.0022(4) O1 0.0174(14) 0.0432(19) 0.0240(15) 0.0006(13) 0.0002(11) 0.0000(13) O2 0.0261(17) 0.049(2) 0.0372(19) -0.0041(15) 0.0096(14) -0.0153(16) C1 0.028(3) 0.069(4) 0.087(5) 0.047(4) -0.024(3) -0.019(3) C2 0.014(2) 0.039(3) 0.046(3) 0.004(2) -0.0155(18) 0.0014(18) C3 0.0118(18) 0.041(3) 0.031(2) -0.0065(18) -0.0006(15) 0.0032(17) C4 0.024(2) 0.034(3) 0.039(3) 0.006(2) -0.0123(18) 0.0038(19) C5 0.020(2) 0.091(5) 0.028(2) 0.019(3) -0.0022(18) 0.002(3) C6 0.020(2) 0.093(5) 0.032(3) -0.018(3) -0.0076(19) 0.018(3) C7 0.028(3) 0.045(3) 0.060(3) -0.026(3) -0.029(2) 0.017(2) C8 0.031(4) 0.051(7) 0.045(5) 0.014(5) -0.001(3) -0.002(5) C9 0.056(6) 0.060(6) 0.064(6) 0.032(5) 0.019(4) 0.007(5) C10 0.053(5) 0.061(6) 0.060(5) 0.028(4) -0.008(4) 0.004(4) C8A 0.031(4) 0.051(7) 0.045(5) 0.014(5) -0.001(3) -0.002(5) C9A 0.056(6) 0.060(6) 0.064(6) 0.032(5) 0.019(4) 0.007(5) C10A 0.053(5) 0.061(6) 0.060(5) 0.028(4) -0.008(4) 0.004(4) C11 0.0102(17) 0.036(2) 0.028(2) 0.0069(17) 0.0004(15) 0.0007(16) C12 0.019(2) 0.035(3) 0.030(2) 0.0054(18) -0.0021(16) 0.0008(18) C13 0.017(2) 0.037(3) 0.045(3) 0.010(2) -0.0035(18) 0.0043(18) C14 0.017(2) 0.047(3) 0.041(3) 0.016(2) -0.0114(18) -0.004(2) C15 0.024(2) 0.046(3) 0.031(2) 0.007(2) -0.0079(18) -0.006(2) C16 0.0169(19) 0.039(3) 0.028(2) 0.0067(18) 0.0003(16) -0.0039(18) C17 0.0139(18) 0.023(2) 0.030(2) 0.0066(16) -0.0035(15) 0.0019(15) C18 0.054(3) 0.048(3) 0.028(2) 0.003(2) 0.005(2) -0.013(3) C19 0.074(4) 0.046(3) 0.033(3) 0.000(2) -0.008(3) -0.016(3) C20 0.026(2) 0.031(3) 0.059(3) 0.012(2) -0.008(2) -0.005(2) C21 0.024(2) 0.034(3) 0.059(3) 0.016(2) 0.012(2) 0.010(2) C22 0.024(2) 0.036(3) 0.037(2) 0.0046(19) 0.0060(18) 0.0061(19) C23 0.0172(19) 0.028(2) 0.024(2) 0.0019(16) 0.0016(15) 0.0050(16) C24 0.0150(18) 0.028(2) 0.026(2) 0.0048(16) -0.0006(15) 0.0017(16) C25 0.019(2) 0.033(2) 0.026(2) -0.0002(17) 0.0016(16) 0.0043(18) C26 0.023(2) 0.036(3) 0.029(2) -0.0030(18) -0.0037(17) -0.0019(19) C27 0.0136(18) 0.040(3) 0.029(2) 0.0017(18) -0.0030(15) 0.0012(18) C28 0.0166(19) 0.033(2) 0.023(2) 0.0041(16) 0.0009(15) -0.0014(17) C29 0.0165(19) 0.036(3) 0.024(2) -0.0039(17) -0.0013(15) 0.0006(17) C30 0.0130(18) 0.043(3) 0.028(2) -0.0008(18) 0.0006(15) -0.0024(18) C31 0.019(2) 0.037(3) 0.027(2) -0.0030(18) 0.0030(16) 0.0000(18) C32 0.019(2) 0.054(3) 0.030(2) 0.001(2) -0.0014(17) -0.004(2) C33 0.027(2) 0.068(4) 0.032(3) 0.007(2) -0.0075(19) -0.005(2) C34 0.031(3) 0.052(3) 0.042(3) 0.011(2) 0.000(2) -0.003(2) C35 0.022(2) 0.056(3) 0.045(3) 0.015(2) 0.004(2) -0.008(2) C36 0.017(2) 0.049(3) 0.040(3) 0.009(2) -0.0022(18) -0.001(2) C37 0.0139(19) 0.056(3) 0.024(2) 0.001(2) -0.0003(15) -0.002(2) C38 0.016(2) 0.065(4) 0.030(2) -0.004(2) 0.0023(17) -0.004(2) C39 0.012(2) 0.088(5) 0.031(3) -0.002(3) 0.0027(17) -0.005(2) C40 0.019(2) 0.084(5) 0.036(3) 0.000(3) 0.0042(19) 0.010(3) C41 0.025(2) 0.068(4) 0.035(3) 0.003(2) 0.0017(19) 0.014(2) C42 0.023(2) 0.056(3) 0.033(3) -0.001(2) 0.0007(18) 0.001(2) C43 0.034(3) 0.087(5) 0.033(3) 0.006(3) 0.006(2) 0.007(3) C44 0.027(2) 0.066(4) 0.031(2) 0.005(2) 0.0023(19) -0.006(2) C45 0.026(2) 0.050(3) 0.038(3) 0.006(2) -0.0018(19) -0.012(2) C46 0.034(3) 0.040(3) 0.049(3) 0.006(2) -0.001(2) -0.008(2) C47 0.031(3) 0.043(3) 0.058(3) 0.016(3) -0.006(2) 0.000(2) C48 0.031(3) 0.058(4) 0.041(3) 0.013(2) -0.010(2) -0.007(2) C49 0.043(3) 0.045(3) 0.029(2) 0.002(2) -0.005(2) -0.003(2) C50 0.038(3) 0.060(4) 0.094(5) 0.020(4) -0.002(3) 0.013(3) C51 0.070(5) 0.070(5) 0.122(7) 0.038(5) 0.000(5) 0.023(4) C52 0.072(6) 0.082(6) 0.125(8) -0.013(5) 0.002(5) 0.040(5) C53 0.053(4) 0.094(6) 0.078(5) 0.023(4) 0.006(4) -0.001(4) Cl5 0.0921(16) 0.1003(17) 0.0783(13) 0.0213(12) 0.0018(11) -0.0422(13) Cl6 0.137(2) 0.0881(17) 0.0877(16) 0.0123(12) -0.0009(15) -0.0485(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C6 2.177(5) . ? Ru1 C7 2.183(5) . ? Ru1 C5 2.210(5) . ? Ru1 C2 2.222(4) . ? Ru1 C4 2.230(5) . ? Ru1 C3 2.239(4) . ? Ru1 P1 2.3505(13) . ? Ru1 Cl2 2.4012(12) . ? Ru1 Cl1 2.4207(14) . ? Ru2 C45 2.162(5) . ? Ru2 C44 2.192(5) . ? Ru2 C46 2.209(6) . ? Ru2 C49 2.215(5) . ? Ru2 C48 2.244(5) . ? Ru2 C47 2.250(6) . ? Ru2 P2 2.3554(13) . ? Ru2 Cl4 2.4057(16) . ? Ru2 Cl3 2.4131(13) . ? P1 C11 1.827(4) . ? P1 C17 1.836(4) . ? P1 C23 1.892(4) . ? P2 C31 1.839(5) . ? P2 C37 1.849(5) . ? P2 C30 1.881(5) . ? O1 C23 1.206(5) . ? O2 C30 1.227(6) . ? C1 C2 1.485(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.405(8) . ? C2 C3 1.427(7) . ? C3 C4 1.384(7) . ? C3 H3 0.9500 . ? C4 C5 1.420(7) . ? C4 H4 0.9500 . ? C5 C6 1.384(9) . ? C5 C8A 1.494(12) . ? C5 C8 1.573(10) . ? C6 C7 1.425(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.497(11) . ? C8 C10 1.543(11) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C8A C9A 1.518(14) . ? C8A C10A 1.522(13) . ? C8A H8A 1.0000 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11 C12 1.386(6) . ? C11 C16 1.397(6) . ? C12 C13 1.389(6) . ? C12 H12 0.9500 . ? C13 C14 1.378(7) . ? C13 H13 0.9500 . ? C14 C15 1.381(7) . ? C14 H14 0.9500 . ? C15 C16 1.385(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.389(7) . ? C17 C22 1.392(6) . ? C18 C19 1.394(8) . ? C18 H18 0.9500 . ? C19 C20 1.369(8) . ? C19 H19 0.9500 . ? C20 C21 1.378(8) . ? C20 H20 0.9500 . ? C21 C22 1.382(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.492(6) . ? C24 C25 1.395(6) . ? C24 C29 1.405(6) . ? C25 C26 1.383(6) . ? C25 H25 0.9500 . ? C26 C27 1.388(6) . ? C26 H26 0.9500 . ? C27 C28 1.400(6) . ? C27 H27 0.9500 . ? C28 C29 1.390(6) . ? C28 C30 1.492(6) . ? C29 H29 0.9500 . ? C31 C32 1.388(6) . ? C31 C36 1.393(6) . ? C32 C33 1.384(7) . ? C32 H32 0.9500 . ? C33 C34 1.384(7) . ? C33 H33 0.9500 . ? C34 C35 1.377(7) . ? C34 H34 0.9500 . ? C35 C36 1.375(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.391(8) . ? C37 C38 1.392(7) . ? C38 C39 1.404(7) . ? C38 H38 0.9500 . ? C39 C40 1.364(9) . ? C39 H39 0.9500 . ? C40 C41 1.381(8) . ? C40 H40 0.9500 . ? C41 C42 1.385(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.489(8) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.424(8) . ? C44 C49 1.435(7) . ? C45 C46 1.421(8) . ? C45 H45 0.9500 . ? C46 C47 1.421(7) . ? C46 H46 0.9500 . ? C47 C48 1.426(8) . ? C47 C50 1.509(8) . ? C48 C49 1.370(8) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C52 1.535(11) . ? C50 C51 1.549(10) . ? C50 H50 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 Cl5 1.745(8) . ? C53 Cl6 1.766(8) . ? C53 H53A 0.9900 . ? C53 H53B 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 C6 Ru1 C7 38.2(2) . . ? C6 Ru1 C5 36.8(2) . . ? C7 Ru1 C5 67.7(2) . . ? C6 Ru1 C2 67.9(2) . . ? C7 Ru1 C2 37.2(2) . . ? C5 Ru1 C2 80.30(19) . . ? C6 Ru1 C4 66.1(2) . . ? C7 Ru1 C4 78.44(19) . . ? C5 Ru1 C4 37.3(2) . . ? C2 Ru1 C4 66.58(18) . . ? C6 Ru1 C3 78.51(17) . . ? C7 Ru1 C3 66.49(17) . . ? C5 Ru1 C3 66.74(18) . . ? C2 Ru1 C3 37.31(18) . . ? C4 Ru1 C3 36.07(18) . . ? C6 Ru1 P1 91.54(15) . . ? C7 Ru1 P1 94.10(14) . . ? C5 Ru1 P1 115.23(15) . . ? C2 Ru1 P1 121.50(14) . . ? C4 Ru1 P1 152.34(13) . . ? C3 Ru1 P1 158.76(12) . . ? C6 Ru1 Cl2 120.00(19) . . ? C7 Ru1 Cl2 157.78(19) . . ? C5 Ru1 Cl2 90.75(16) . . ? C2 Ru1 Cl2 148.13(14) . . ? C4 Ru1 Cl2 87.83(13) . . ? C3 Ru1 Cl2 111.21(12) . . ? P1 Ru1 Cl2 90.03(5) . . ? C6 Ru1 Cl1 151.0(2) . . ? C7 Ru1 Cl1 113.14(19) . . ? C5 Ru1 Cl1 158.65(15) . . ? C2 Ru1 Cl1 88.80(14) . . ? C4 Ru1 Cl1 121.38(13) . . ? C3 Ru1 Cl1 93.56(12) . . ? P1 Ru1 Cl1 86.12(4) . . ? Cl2 Ru1 Cl1 88.91(4) . . ? C45 Ru2 C44 38.2(2) . . ? C45 Ru2 C46 37.9(2) . . ? C44 Ru2 C46 68.9(2) . . ? C45 Ru2 C49 67.30(19) . . ? C44 Ru2 C49 38.00(19) . . ? C46 Ru2 C49 79.0(2) . . ? C45 Ru2 C48 78.6(2) . . ? C44 Ru2 C48 67.2(2) . . ? C46 Ru2 C48 66.3(2) . . ? C49 Ru2 C48 35.8(2) . . ? C45 Ru2 C47 67.7(2) . . ? C44 Ru2 C47 81.1(2) . . ? C46 Ru2 C47 37.15(19) . . ? C49 Ru2 C47 66.4(2) . . ? C48 Ru2 C47 37.0(2) . . ? C45 Ru2 P2 86.82(14) . . ? C44 Ru2 P2 105.79(14) . . ? C46 Ru2 P2 97.14(15) . . ? C49 Ru2 P2 142.76(15) . . ? C48 Ru2 P2 163.33(15) . . ? C47 Ru2 P2 129.00(16) . . ? C45 Ru2 Cl4 124.92(16) . . ? C44 Ru2 Cl4 93.74(17) . . ? C46 Ru2 Cl4 162.32(15) . . ? C49 Ru2 Cl4 89.56(15) . . ? C48 Ru2 Cl4 111.20(16) . . ? C47 Ru2 Cl4 147.06(16) . . ? P2 Ru2 Cl4 83.79(4) . . ? C45 Ru2 Cl3 147.91(16) . . ? C44 Ru2 Cl3 157.76(14) . . ? C46 Ru2 Cl3 110.21(15) . . ? C49 Ru2 Cl3 119.87(14) . . ? C48 Ru2 Cl3 91.75(14) . . ? C47 Ru2 Cl3 86.09(15) . . ? P2 Ru2 Cl3 96.40(4) . . ? Cl4 Ru2 Cl3 87.14(5) . . ? C11 P1 C17 103.5(2) . . ? C11 P1 C23 103.24(19) . . ? C17 P1 C23 102.12(19) . . ? C11 P1 Ru1 123.72(15) . . ? C17 P1 Ru1 110.67(13) . . ? C23 P1 Ru1 111.26(14) . . ? C31 P2 C37 101.0(2) . . ? C31 P2 C30 104.8(2) . . ? C37 P2 C30 104.8(2) . . ? C31 P2 Ru2 125.17(15) . . ? C37 P2 Ru2 112.04(14) . . ? C30 P2 Ru2 107.22(15) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 117.8(5) . . ? C7 C2 C1 122.3(6) . . ? C3 C2 C1 119.9(5) . . ? C7 C2 Ru1 69.9(3) . . ? C3 C2 Ru1 72.0(2) . . ? C1 C2 Ru1 129.7(3) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 Ru1 71.6(3) . . ? C2 C3 Ru1 70.7(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? Ru1 C3 H3 130.8 . . ? C3 C4 C5 121.6(5) . . ? C3 C4 Ru1 72.3(3) . . ? C5 C4 Ru1 70.6(3) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? Ru1 C4 H4 130.6 . . ? C6 C5 C4 118.0(5) . . ? C6 C5 C8A 101.8(7) . . ? C4 C5 C8A 140.3(8) . . ? C6 C5 C8 131.7(6) . . ? C4 C5 C8 110.3(6) . . ? C6 C5 Ru1 70.3(3) . . ? C4 C5 Ru1 72.1(3) . . ? C8A C5 Ru1 126.6(6) . . ? C8 C5 Ru1 130.9(4) . . ? C5 C6 C7 121.3(5) . . ? C5 C6 Ru1 72.9(3) . . ? C7 C6 Ru1 71.1(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? Ru1 C6 H6 129.0 . . ? C2 C7 C6 120.6(5) . . ? C2 C7 Ru1 72.9(3) . . ? C6 C7 Ru1 70.7(3) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? Ru1 C7 H7 129.0 . . ? C9 C8 C10 111.2(9) . . ? C9 C8 C5 113.2(8) . . ? C10 C8 C5 109.4(7) . . ? C9 C8 H8 107.6 . . ? C10 C8 H8 107.6 . . ? C5 C8 H8 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C8A C9A 100.6(10) . . ? C5 C8A C10A 112.4(10) . . ? C9A C8A C10A 112.1(13) . . ? C5 C8A H8A 110.5 . . ? C9A C8A H8A 110.5 . . ? C10A C8A H8A 110.5 . . ? C8A C9A H9A1 109.5 . . ? C8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C8A C10A H10D 109.5 . . ? C8A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C8A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C12 C11 C16 119.7(4) . . ? C12 C11 P1 118.2(3) . . ? C16 C11 P1 122.0(3) . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 119.6(5) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? C18 C17 C22 118.3(4) . . ? C18 C17 P1 126.6(4) . . ? C22 C17 P1 114.9(3) . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.6(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.4(5) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C22 120.6(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 120.7(5) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? O1 C23 C24 120.6(4) . . ? O1 C23 P1 117.9(3) . . ? C24 C23 P1 121.5(3) . . ? C25 C24 C29 120.6(4) . . ? C25 C24 C23 123.4(4) . . ? C29 C24 C23 115.9(4) . . ? C26 C25 C24 120.3(4) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 119.4(4) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 120.2(4) . . ? C29 C28 C30 122.3(4) . . ? C27 C28 C30 117.4(4) . . ? C28 C29 C24 118.6(4) . . ? C28 C29 H29 120.7 . . ? C24 C29 H29 120.7 . . ? O2 C30 C28 119.3(4) . . ? O2 C30 P2 119.1(3) . . ? C28 C30 P2 121.6(3) . . ? C32 C31 C36 119.7(4) . . ? C32 C31 P2 118.6(3) . . ? C36 C31 P2 121.7(4) . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.1(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.3(5) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C36 C35 C34 121.5(5) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C31 119.3(4) . . ? C35 C36 H36 120.4 . . ? C31 C36 H36 120.4 . . ? C42 C37 C38 119.1(4) . . ? C42 C37 P2 115.9(4) . . ? C38 C37 P2 125.0(4) . . ? C37 C38 C39 119.3(6) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 121.2(5) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 119.5(5) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C40 C41 C42 120.5(6) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 120.4(5) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C49 116.1(5) . . ? C45 C44 C43 122.2(5) . . ? C49 C44 C43 121.8(5) . . ? C45 C44 Ru2 69.8(3) . . ? C49 C44 Ru2 71.9(3) . . ? C43 C44 Ru2 128.6(4) . . ? C46 C45 C44 122.2(5) . . ? C46 C45 Ru2 72.8(3) . . ? C44 C45 Ru2 72.1(3) . . ? C46 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? Ru2 C45 H45 128.6 . . ? C47 C46 C45 119.9(5) . . ? C47 C46 Ru2 73.0(3) . . ? C45 C46 Ru2 69.3(3) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? Ru2 C46 H46 130.2 . . ? C46 C47 C48 117.7(5) . . ? C46 C47 C50 123.3(6) . . ? C48 C47 C50 119.0(5) . . ? C46 C47 Ru2 69.9(3) . . ? C48 C47 Ru2 71.3(3) . . ? C50 C47 Ru2 131.4(4) . . ? C49 C48 C47 122.0(5) . . ? C49 C48 Ru2 71.0(3) . . ? C47 C48 Ru2 71.7(3) . . ? C49 C48 H48 119.0 . . ? C47 C48 H48 119.0 . . ? Ru2 C48 H48 131.3 . . ? C48 C49 C44 122.1(5) . . ? C48 C49 Ru2 73.2(3) . . ? C44 C49 Ru2 70.1(3) . . ? C48 C49 H49 118.9 . . ? C44 C49 H49 118.9 . . ? Ru2 C49 H49 130.5 . . ? C47 C50 C52 113.6(6) . . ? C47 C50 C51 106.8(6) . . ? C52 C50 C51 112.7(7) . . ? C47 C50 H50 107.9 . . ? C52 C50 H50 107.9 . . ? C51 C50 H50 107.9 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Cl5 C53 Cl6 109.4(4) . . ? Cl5 C53 H53A 109.8 . . ? Cl6 C53 H53A 109.8 . . ? Cl5 C53 H53B 109.8 . . ? Cl6 C53 H53B 109.8 . . ? H53A C53 H53B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.603 _refine_diff_density_min -1.605 _refine_diff_density_rms 0.123 # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 523 150 ' ' _platon_squeeze_details ; Following several attempts to model the disorder in a site partially occupied by solvent dichloromethane which proved unsuccessful, the density in this site was removed with the SQUEEZE option of PLATON (SPEK, 2010). ; _database_code_depnum_ccdc_archive 'CCDC 934905' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msbpr05 #TrackingRef '07 MSBPR05_pincer.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H23 Cl O2 P2 Pd, C H2 Cl2' _chemical_formula_sum 'C33 H25 Cl3 O2 P2 Pd' _chemical_formula_weight 728.28 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' Pd Pd -0.9988 1.0072 '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 11.789(3) _cell_length_b 12.147(2) _cell_length_c 12.8117(19) _cell_angle_alpha 62.959(14) _cell_angle_beta 68.313(17) _cell_angle_gamma 76.844(18) _cell_volume 1514.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2325 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 25.40 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.590 _exptl_crystal_size_mid 0.298 _exptl_crystal_size_min 0.279 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 7.111 _diffrn_standards_number 0 _diffrn_standards_interval_count - _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10831 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.37 _reflns_number_total 5269 _reflns_number_gt 4986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+3.2622P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5269 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1252 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Pd1 Pd 0.80331(2) 0.05755(2) 0.33049(2) 0.01207(12) Uani 1 1 d . . . Cl1 Cl 0.60587(8) 0.06741(8) 0.31900(8) 0.0195(2) Uani 1 1 d . . . P1 P 0.77763(8) 0.24936(7) 0.32759(8) 0.01267(19) Uani 1 1 d . . . P2 P 0.86145(8) -0.13902(8) 0.34319(8) 0.0141(2) Uani 1 1 d . . . O1 O 0.9597(2) 0.3675(2) 0.3113(3) 0.0231(6) Uani 1 1 d . . . O2 O 1.0946(3) -0.2454(2) 0.3299(3) 0.0292(6) Uani 1 1 d . . . C1 C 0.6709(3) 0.2745(3) 0.4595(3) 0.0142(6) Uani 1 1 d . . . C2 C 0.5776(3) 0.1950(3) 0.5364(3) 0.0159(7) Uani 1 1 d . . . H2 H 0.5708 0.1291 0.5189 0.019 Uiso 1 1 calc R . . C3 C 0.4942(3) 0.2121(3) 0.6387(3) 0.0193(7) Uani 1 1 d . . . H3 H 0.4299 0.1583 0.6910 0.023 Uiso 1 1 calc R . . C4 C 0.5050(4) 0.3075(4) 0.6645(3) 0.0236(8) Uani 1 1 d . . . H4 H 0.4481 0.3190 0.7346 0.028 Uiso 1 1 calc R . . C5 C 0.5981(4) 0.3863(4) 0.5889(4) 0.0251(8) Uani 1 1 d . . . H5 H 0.6048 0.4513 0.6076 0.030 Uiso 1 1 calc R . . C6 C 0.6820(3) 0.3711(3) 0.4856(3) 0.0198(7) Uani 1 1 d . . . H6 H 0.7459 0.4254 0.4335 0.024 Uiso 1 1 calc R . . C7 C 0.7524(3) 0.3796(3) 0.1921(3) 0.0152(7) Uani 1 1 d . . . C8 C 0.8368(4) 0.3944(4) 0.0777(3) 0.0244(8) Uani 1 1 d . . . H8 H 0.9068 0.3377 0.0724 0.029 Uiso 1 1 calc R . . C9 C 0.8196(4) 0.4909(4) -0.0283(4) 0.0298(9) Uani 1 1 d . . . H9 H 0.8785 0.5015 -0.1060 0.036 Uiso 1 1 calc R . . C10 C 0.7163(4) 0.5723(3) -0.0210(3) 0.0255(8) Uani 1 1 d . . . H10 H 0.7041 0.6385 -0.0939 0.031 Uiso 1 1 calc R . . C11 C 0.6308(4) 0.5570(3) 0.0922(3) 0.0221(8) Uani 1 1 d . . . H11 H 0.5597 0.6125 0.0969 0.027 Uiso 1 1 calc R . . C12 C 0.6488(3) 0.4608(3) 0.1990(3) 0.0173(7) Uani 1 1 d . . . H12 H 0.5902 0.4507 0.2767 0.021 Uiso 1 1 calc R . . C13 C 0.9331(3) 0.2710(3) 0.3221(3) 0.0156(7) Uani 1 1 d . . . C14 C 1.0155(3) 0.1589(3) 0.3287(3) 0.0137(6) Uani 1 1 d . . . C15 C 1.1358(3) 0.1587(3) 0.3272(3) 0.0159(7) Uani 1 1 d . . . H15 H 1.1607 0.2294 0.3244 0.019 Uiso 1 1 calc R . . C16 C 1.2180(3) 0.0566(3) 0.3298(3) 0.0190(7) Uani 1 1 d . . . H16 H 1.2985 0.0562 0.3302 0.023 Uiso 1 1 calc R . . C17 C 1.1813(3) -0.0448(3) 0.3317(3) 0.0172(7) Uani 1 1 d . . . H17 H 1.2375 -0.1145 0.3316 0.021 Uiso 1 1 calc R . . C18 C 1.0612(3) -0.0456(3) 0.3337(3) 0.0151(7) Uani 1 1 d . . . C19 C 0.9748(3) 0.0558(3) 0.3332(3) 0.0133(6) Uani 1 1 d . . . C20 C 1.0269(3) -0.1560(3) 0.3347(3) 0.0189(7) Uani 1 1 d . . . C21 C 0.8627(3) -0.1764(3) 0.2211(3) 0.0164(7) Uani 1 1 d . . . C22 C 0.8587(4) -0.0771(3) 0.1101(4) 0.0261(8) Uani 1 1 d . . . H22 H 0.8556 0.0054 0.1013 0.031 Uiso 1 1 calc R . . C23 C 0.8594(4) -0.0990(4) 0.0127(4) 0.0315(9) Uani 1 1 d . . . H23 H 0.8574 -0.0314 -0.0632 0.038 Uiso 1 1 calc R . . C24 C 0.8630(4) -0.2191(4) 0.0256(4) 0.0261(8) Uani 1 1 d . . . H24 H 0.8630 -0.2338 -0.0412 0.031 Uiso 1 1 calc R . . C25 C 0.8667(4) -0.3184(4) 0.1362(3) 0.0249(8) Uani 1 1 d . . . H25 H 0.8693 -0.4008 0.1448 0.030 Uiso 1 1 calc R . . C26 C 0.8667(4) -0.2974(3) 0.2342(3) 0.0217(7) Uani 1 1 d . . . H26 H 0.8694 -0.3652 0.3098 0.026 Uiso 1 1 calc R . . C27 C 0.7940(3) -0.2616(3) 0.4901(3) 0.0155(7) Uani 1 1 d . . . C28 C 0.8563(3) -0.3776(3) 0.5360(3) 0.0195(7) Uani 1 1 d . . . H28 H 0.9352 -0.3958 0.4877 0.023 Uiso 1 1 calc R . . C29 C 0.8030(4) -0.4655(3) 0.6518(3) 0.0222(8) Uani 1 1 d . . . H29 H 0.8450 -0.5442 0.6828 0.027 Uiso 1 1 calc R . . C30 C 0.6879(4) -0.4388(3) 0.7228(3) 0.0212(7) Uani 1 1 d . . . H30 H 0.6514 -0.4993 0.8023 0.025 Uiso 1 1 calc R . . C31 C 0.6260(3) -0.3241(3) 0.6777(3) 0.0194(7) Uani 1 1 d . . . H31 H 0.5475 -0.3061 0.7267 0.023 Uiso 1 1 calc R . . C32 C 0.6786(3) -0.2356(3) 0.5614(3) 0.0166(7) Uani 1 1 d . . . H32 H 0.6359 -0.1573 0.5305 0.020 Uiso 1 1 calc R . . C33 C 0.5821(7) 0.1040(8) 0.0411(5) 0.085(2) Uani 1 1 d . . . H33A H 0.6116 0.0167 0.0560 0.102 Uiso 1 1 calc R . . H33B H 0.5892 0.1199 0.1076 0.102 Uiso 1 1 calc R . . Cl2 Cl 0.43382(19) 0.12282(16) 0.0496(2) 0.1125(10) Uani 1 1 d . . . Cl3 Cl 0.67695(15) 0.20035(14) -0.09977(14) 0.0632(4) 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 Pd1 0.01362(17) 0.00979(17) 0.01523(17) -0.00735(12) -0.00581(11) 0.00196(10) Cl1 0.0169(4) 0.0194(4) 0.0284(5) -0.0140(4) -0.0102(3) 0.0020(3) P1 0.0149(4) 0.0099(4) 0.0155(4) -0.0073(3) -0.0057(3) 0.0015(3) P2 0.0165(4) 0.0108(4) 0.0175(4) -0.0084(3) -0.0067(3) 0.0025(3) O1 0.0220(13) 0.0162(12) 0.0358(15) -0.0135(11) -0.0109(11) -0.0001(10) O2 0.0229(14) 0.0193(13) 0.0501(18) -0.0208(13) -0.0131(13) 0.0077(11) C1 0.0180(16) 0.0131(15) 0.0124(15) -0.0058(12) -0.0079(13) 0.0039(12) C2 0.0207(17) 0.0125(15) 0.0174(16) -0.0068(13) -0.0100(13) 0.0020(13) C3 0.0220(18) 0.0192(17) 0.0163(16) -0.0070(14) -0.0053(14) -0.0023(14) C4 0.027(2) 0.0289(19) 0.0183(17) -0.0151(15) -0.0070(15) 0.0029(15) C5 0.033(2) 0.0246(19) 0.0262(19) -0.0184(16) -0.0077(16) -0.0016(16) C6 0.0249(19) 0.0171(17) 0.0209(17) -0.0105(14) -0.0072(14) -0.0016(14) C7 0.0192(17) 0.0134(15) 0.0169(16) -0.0087(13) -0.0071(13) -0.0001(13) C8 0.0255(19) 0.0260(19) 0.0184(17) -0.0106(15) -0.0051(15) 0.0044(15) C9 0.034(2) 0.034(2) 0.0175(18) -0.0105(16) -0.0042(16) -0.0012(17) C10 0.038(2) 0.0224(19) 0.0165(17) -0.0044(15) -0.0133(16) -0.0026(16) C11 0.0265(19) 0.0203(18) 0.0208(18) -0.0079(15) -0.0126(15) 0.0040(15) C12 0.0206(18) 0.0175(16) 0.0148(16) -0.0070(13) -0.0070(13) 0.0002(13) C13 0.0182(17) 0.0159(16) 0.0168(16) -0.0085(13) -0.0070(13) -0.0016(13) C14 0.0144(16) 0.0172(16) 0.0114(15) -0.0073(13) -0.0058(12) 0.0015(13) C15 0.0179(17) 0.0199(17) 0.0143(15) -0.0074(13) -0.0077(13) -0.0037(13) C16 0.0173(17) 0.0246(18) 0.0184(17) -0.0100(15) -0.0093(14) 0.0013(14) C17 0.0180(17) 0.0188(17) 0.0160(16) -0.0087(13) -0.0081(13) 0.0047(13) C18 0.0194(17) 0.0157(16) 0.0108(15) -0.0061(13) -0.0053(13) 0.0002(13) C19 0.0145(16) 0.0155(16) 0.0112(15) -0.0061(13) -0.0052(12) 0.0001(13) C20 0.0185(17) 0.0179(17) 0.0199(17) -0.0082(14) -0.0070(14) 0.0020(14) C21 0.0171(17) 0.0180(16) 0.0163(16) -0.0104(14) -0.0043(13) 0.0006(13) C22 0.039(2) 0.0172(18) 0.0225(18) -0.0092(15) -0.0115(16) 0.0031(16) C23 0.043(2) 0.029(2) 0.0203(19) -0.0108(16) -0.0122(17) 0.0063(18) C24 0.026(2) 0.038(2) 0.0237(19) -0.0211(17) -0.0080(15) 0.0006(16) C25 0.031(2) 0.0239(19) 0.0249(19) -0.0157(16) -0.0051(16) -0.0042(15) C26 0.030(2) 0.0158(17) 0.0203(17) -0.0089(14) -0.0065(15) -0.0020(14) C27 0.0225(18) 0.0127(15) 0.0158(16) -0.0065(13) -0.0095(14) -0.0015(13) C28 0.0243(18) 0.0158(16) 0.0230(18) -0.0129(14) -0.0097(14) 0.0049(14) C29 0.035(2) 0.0124(16) 0.0245(18) -0.0083(14) -0.0173(16) 0.0036(14) C30 0.031(2) 0.0188(17) 0.0178(17) -0.0063(14) -0.0106(15) -0.0054(15) C31 0.0197(17) 0.0216(18) 0.0210(17) -0.0103(14) -0.0076(14) -0.0035(14) C32 0.0217(17) 0.0149(16) 0.0190(16) -0.0084(13) -0.0121(14) 0.0016(13) C33 0.099(6) 0.089(5) 0.029(3) -0.002(3) -0.016(3) 0.009(4) Cl2 0.0778(12) 0.0460(9) 0.0986(15) 0.0040(9) 0.0371(11) 0.0209(8) Cl3 0.0574(9) 0.0569(9) 0.0583(9) -0.0153(7) -0.0169(7) 0.0069(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 Pd1 C19 2.030(3) . ? Pd1 P1 2.2651(9) . ? Pd1 P2 2.2763(9) . ? Pd1 Cl1 2.3588(10) . ? P1 C1 1.804(3) . ? P1 C7 1.810(3) . ? P1 C13 1.882(4) . ? P2 C27 1.810(3) . ? P2 C21 1.811(3) . ? P2 C20 1.881(4) . ? O1 C13 1.215(4) . ? O2 C20 1.204(4) . ? C1 C2 1.389(5) . ? C1 C6 1.402(5) . ? C2 C3 1.390(5) . ? C2 H2 0.9500 . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.380(6) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.387(5) . ? C7 C8 1.391(5) . ? C8 C9 1.381(5) . ? C8 H8 0.9500 . ? C9 C10 1.387(6) . ? C9 H9 0.9500 . ? C10 C11 1.383(5) . ? C10 H10 0.9500 . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.469(5) . ? C14 C19 1.411(5) . ? C14 C15 1.411(5) . ? C15 C16 1.385(5) . ? C15 H15 0.9500 . ? C16 C17 1.383(5) . ? C16 H16 0.9500 . ? C17 C18 1.407(5) . ? C17 H17 0.9500 . ? C18 C19 1.407(5) . ? C18 C20 1.480(5) . ? C21 C22 1.393(5) . ? C21 C26 1.393(5) . ? C22 C23 1.387(6) . ? C22 H22 0.9500 . ? C23 C24 1.384(6) . ? C23 H23 0.9500 . ? C24 C25 1.390(6) . ? C24 H24 0.9500 . ? C25 C26 1.391(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.390(5) . ? C27 C28 1.402(5) . ? C28 C29 1.383(5) . ? C28 H28 0.9500 . ? C29 C30 1.389(5) . ? C29 H29 0.9500 . ? C30 C31 1.387(5) . ? C30 H30 0.9500 . ? C31 C32 1.388(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 Cl2 1.679(9) . ? C33 Cl3 1.750(7) . ? C33 H33A 0.9900 . ? C33 H33B 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 C19 Pd1 P1 84.82(10) . . ? C19 Pd1 P2 84.63(10) . . ? P1 Pd1 P2 169.15(3) . . ? C19 Pd1 Cl1 177.46(9) . . ? P1 Pd1 Cl1 93.90(3) . . ? P2 Pd1 Cl1 96.75(4) . . ? C1 P1 C7 107.00(15) . . ? C1 P1 C13 105.76(15) . . ? C7 P1 C13 103.45(16) . . ? C1 P1 Pd1 118.56(11) . . ? C7 P1 Pd1 117.72(11) . . ? C13 P1 Pd1 102.44(11) . . ? C27 P2 C21 108.92(15) . . ? C27 P2 C20 103.35(16) . . ? C21 P2 C20 104.78(16) . . ? C27 P2 Pd1 115.80(11) . . ? C21 P2 Pd1 119.49(12) . . ? C20 P2 Pd1 102.28(12) . . ? C2 C1 C6 120.2(3) . . ? C2 C1 P1 118.7(2) . . ? C6 C1 P1 121.1(3) . . ? C1 C2 C3 119.9(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 119.0(3) . . ? C5 C6 H6 120.5 . . ? C1 C6 H6 120.5 . . ? C12 C7 C8 119.5(3) . . ? C12 C7 P1 121.8(3) . . ? C8 C7 P1 118.6(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.8(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 120.0(3) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? O1 C13 C14 126.1(3) . . ? O1 C13 P1 122.9(3) . . ? C14 C13 P1 111.0(2) . . ? C19 C14 C15 121.4(3) . . ? C19 C14 C13 120.1(3) . . ? C15 C14 C13 118.5(3) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 119.1(3) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 120.6(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 121.8(3) . . ? C19 C18 C20 119.7(3) . . ? C17 C18 C20 118.4(3) . . ? C18 C19 C14 116.4(3) . . ? C18 C19 Pd1 122.0(3) . . ? C14 C19 Pd1 121.5(2) . . ? O2 C20 C18 125.5(3) . . ? O2 C20 P2 123.5(3) . . ? C18 C20 P2 111.1(2) . . ? C22 C21 C26 120.0(3) . . ? C22 C21 P2 116.9(3) . . ? C26 C21 P2 123.1(3) . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 119.7(3) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C32 C27 C28 119.7(3) . . ? C32 C27 P2 117.7(3) . . ? C28 C27 P2 122.5(3) . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.2(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.2(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 119.9(3) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? Cl2 C33 Cl3 114.3(4) . . ? Cl2 C33 H33A 108.7 . . ? Cl3 C33 H33A 108.7 . . ? Cl2 C33 H33B 108.7 . . ? Cl3 C33 H33B 108.7 . . ? H33A C33 H33B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.742 _refine_diff_density_min -1.701 _refine_diff_density_rms 0.125 _database_code_depnum_ccdc_archive 'CCDC 934906' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb478_0m #TrackingRef '08 MSB478_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H23 Br Ni O2 P2, C H2 Cl2' _chemical_formula_sum 'C33 H25 Br Cl2 Ni O2 P2' _chemical_formula_weight 724.99 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9842(12) _cell_length_b 12.0194(12) _cell_length_c 12.7559(13) _cell_angle_alpha 63.683(1) _cell_angle_beta 67.267(1) _cell_angle_gamma 76.562(1) _cell_volume 1514.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9841 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 29.10 _exptl_crystal_description Plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 2.272 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5940 _exptl_absorpt_correction_T_max 0.8269 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26273 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7237 _reflns_number_gt 6304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+1.6232P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7237 _refine_ls_number_parameters 380 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.68600(2) 0.94369(3) 0.66874(3) 0.01418(8) Uani 1 1 d . . . Br1 Br 0.87430(2) 0.93030(2) 0.68922(2) 0.02009(7) Uani 1 1 d . . . P1 P 0.71735(5) 0.75949(5) 0.66810(5) 0.01453(12) Uani 1 1 d . . . P2 P 0.63757(5) 1.13300(5) 0.65839(6) 0.01633(12) Uani 1 1 d . . . O1 O 0.54277(16) 0.63371(16) 0.68331(18) 0.0264(4) Uani 1 1 d . . . O2 O 0.40601(18) 1.24469(18) 0.6847(2) 0.0373(5) Uani 1 1 d . . . C1 C 0.7410(2) 0.6312(2) 0.8045(2) 0.0172(4) Uani 1 1 d . . . C2 C 0.8478(2) 0.5549(2) 0.7983(2) 0.0201(5) Uani 1 1 d . . . H2 H 0.9097 0.5676 0.7208 0.024 Uiso 1 1 calc R . . C3 C 0.8640(2) 0.4595(2) 0.9058(2) 0.0258(5) Uani 1 1 d . . . H3 H 0.9373 0.4077 0.9017 0.031 Uiso 1 1 calc R . . C4 C 0.7735(3) 0.4403(3) 1.0186(2) 0.0285(6) Uani 1 1 d . . . H4 H 0.7842 0.3745 1.0916 0.034 Uiso 1 1 calc R . . C5 C 0.6669(3) 0.5171(3) 1.0252(2) 0.0313(6) Uani 1 1 d . . . H5 H 0.6050 0.5042 1.1027 0.038 Uiso 1 1 calc R . . C6 C 0.6509(2) 0.6123(2) 0.9187(2) 0.0262(5) Uani 1 1 d . . . H6 H 0.5782 0.6652 0.9234 0.031 Uiso 1 1 calc R . . C7 C 0.8273(2) 0.7306(2) 0.5361(2) 0.0156(4) Uani 1 1 d . . . C8 C 0.9214(2) 0.8088(2) 0.4566(2) 0.0179(4) Uani 1 1 d . . . H8 H 0.9282 0.8771 0.4718 0.022 Uiso 1 1 calc R . . C9 C 1.0055(2) 0.7864(2) 0.3549(2) 0.0232(5) Uani 1 1 d . . . H9 H 1.0698 0.8394 0.3009 0.028 Uiso 1 1 calc R . . C10 C 0.9955(2) 0.6872(3) 0.3326(3) 0.0278(6) Uani 1 1 d . . . H10 H 1.0528 0.6724 0.2631 0.033 Uiso 1 1 calc R . . C11 C 0.9020(3) 0.6090(3) 0.4114(3) 0.0294(6) Uani 1 1 d . . . H11 H 0.8955 0.5409 0.3956 0.035 Uiso 1 1 calc R . . C12 C 0.8182(2) 0.6302(2) 0.5128(2) 0.0236(5) Uani 1 1 d . . . H12 H 0.7544 0.5765 0.5668 0.028 Uiso 1 1 calc R . . C13 C 0.5668(2) 0.7311(2) 0.6737(2) 0.0175(4) Uani 1 1 d . . . C14 C 0.52588(19) 0.9460(2) 0.6667(2) 0.0147(4) Uani 1 1 d . . . C15 C 0.4834(2) 0.8431(2) 0.6704(2) 0.0155(4) Uani 1 1 d . . . C16 C 0.3658(2) 0.8426(2) 0.6738(2) 0.0183(4) Uani 1 1 d . . . H16 H 0.3416 0.7713 0.6763 0.022 Uiso 1 1 calc R . . C17 C 0.2837(2) 0.9456(2) 0.6734(2) 0.0203(5) Uani 1 1 d . . . H17 H 0.2041 0.9462 0.6738 0.024 Uiso 1 1 calc R . . C18 C 0.3202(2) 1.0475(2) 0.6725(2) 0.0196(5) Uani 1 1 d . . . H18 H 0.2646 1.1179 0.6740 0.023 Uiso 1 1 calc R . . C19 C 0.4380(2) 1.0477(2) 0.6694(2) 0.0164(4) Uani 1 1 d . . . C20 C 0.4730(2) 1.1556(2) 0.6722(2) 0.0215(5) Uani 1 1 d . . . C21 C 0.6418(2) 1.1707(2) 0.7797(2) 0.0180(4) Uani 1 1 d . . . C22 C 0.6397(2) 1.0729(2) 0.8921(2) 0.0250(5) Uani 1 1 d . . . H22 H 0.6370 0.9901 0.9028 0.030 Uiso 1 1 calc R . . C23 C 0.6417(3) 1.0959(3) 0.9889(2) 0.0304(6) Uani 1 1 d . . . H23 H 0.6395 1.0289 1.0659 0.037 Uiso 1 1 calc R . . C24 C 0.6471(2) 1.2167(3) 0.9731(2) 0.0281(6) Uani 1 1 d . . . H24 H 0.6501 1.2321 1.0388 0.034 Uiso 1 1 calc R . . C25 C 0.6479(2) 1.3145(3) 0.8621(3) 0.0279(6) Uani 1 1 d . . . H25 H 0.6502 1.3973 0.8519 0.033 Uiso 1 1 calc R . . C26 C 0.6454(2) 1.2919(2) 0.7649(2) 0.0228(5) Uani 1 1 d . . . H26 H 0.6462 1.3593 0.6884 0.027 Uiso 1 1 calc R . . C27 C 0.7057(2) 1.2555(2) 0.5107(2) 0.0178(4) Uani 1 1 d . . . C28 C 0.8213(2) 1.2303(2) 0.4366(2) 0.0192(5) Uani 1 1 d . . . H28 H 0.8644 1.1521 0.4661 0.023 Uiso 1 1 calc R . . C29 C 0.8732(2) 1.3192(2) 0.3201(2) 0.0226(5) Uani 1 1 d . . . H29 H 0.9513 1.3015 0.2693 0.027 Uiso 1 1 calc R . . C30 C 0.8109(3) 1.4342(2) 0.2776(2) 0.0262(5) Uani 1 1 d . . . H30 H 0.8469 1.4951 0.1980 0.031 Uiso 1 1 calc R . . C31 C 0.6967(3) 1.4604(2) 0.3506(2) 0.0268(5) Uani 1 1 d . . . H31 H 0.6547 1.5393 0.3212 0.032 Uiso 1 1 calc R . . C32 C 0.6434(2) 1.3715(2) 0.4669(2) 0.0241(5) Uani 1 1 d . . . H32 H 0.5646 1.3893 0.5166 0.029 Uiso 1 1 calc R . . C33 C 0.8788(8) 0.8648(9) 0.9957(10) 0.0551(15) Uani 0.4674(14) 1 d PD A 1 H33A H 0.8500 0.8798 1.0726 0.066 Uiso 0.4674(14) 1 calc PR A 1 H33B H 0.8494 0.9377 0.9333 0.066 Uiso 0.4674(14) 1 calc PR A 1 Cl1 Cl 1.0381(2) 0.8534(2) 0.9422(2) 0.0551(4) Uani 0.4674(14) 1 d PD A 1 Cl2 Cl 0.8166(2) 0.7356(2) 1.0246(2) 0.0624(4) Uani 0.4674(14) 1 d PD A 1 C33A C 0.9271(6) 0.9022(8) 0.9711(8) 0.0551(15) Uani 0.5326(14) 1 d PD A 2 H33C H 0.9279 0.9022 0.8932 0.066 Uiso 0.5326(14) 1 calc PR A 2 H33D H 0.8955 0.9860 0.9710 0.066 Uiso 0.5326(14) 1 calc PR A 2 Cl1A Cl 1.07484(18) 0.87415(19) 0.9742(2) 0.0551(4) Uani 0.5326(14) 1 d PD A 2 Cl2A Cl 0.82927(18) 0.79387(17) 1.09489(19) 0.0624(4) Uani 0.5326(14) 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 Ni1 0.01300(14) 0.01143(14) 0.01979(15) -0.00765(12) -0.00572(11) -0.00006(10) Br1 0.01613(12) 0.02001(12) 0.02869(14) -0.01220(10) -0.00934(9) -0.00044(8) P1 0.0136(3) 0.0118(3) 0.0190(3) -0.0069(2) -0.0054(2) -0.0007(2) P2 0.0162(3) 0.0127(3) 0.0222(3) -0.0089(2) -0.0069(2) 0.0006(2) O1 0.0231(9) 0.0187(8) 0.0424(11) -0.0149(8) -0.0114(8) -0.0030(7) O2 0.0246(10) 0.0262(10) 0.0720(16) -0.0304(11) -0.0195(10) 0.0088(8) C1 0.0207(11) 0.0143(10) 0.0183(11) -0.0065(9) -0.0065(9) -0.0037(8) C2 0.0198(11) 0.0198(11) 0.0212(12) -0.0081(10) -0.0074(9) -0.0012(9) C3 0.0291(13) 0.0230(12) 0.0273(13) -0.0073(11) -0.0156(11) 0.0004(10) C4 0.0427(16) 0.0235(13) 0.0209(13) -0.0034(11) -0.0156(12) -0.0074(11) C5 0.0371(15) 0.0332(15) 0.0184(12) -0.0086(11) -0.0018(11) -0.0090(12) C6 0.0266(13) 0.0246(13) 0.0238(13) -0.0112(11) -0.0032(11) -0.0005(10) C7 0.0157(10) 0.0135(10) 0.0171(11) -0.0057(9) -0.0067(9) 0.0016(8) C8 0.0184(11) 0.0154(10) 0.0208(11) -0.0068(9) -0.0079(9) -0.0009(8) C9 0.0216(12) 0.0237(12) 0.0220(12) -0.0088(10) -0.0036(10) -0.0042(9) C10 0.0274(13) 0.0321(14) 0.0270(13) -0.0189(12) -0.0040(11) -0.0011(11) C11 0.0326(14) 0.0300(14) 0.0340(15) -0.0231(12) -0.0054(12) -0.0049(11) C12 0.0250(12) 0.0197(12) 0.0273(13) -0.0118(10) -0.0048(10) -0.0053(9) C13 0.0171(11) 0.0170(11) 0.0182(11) -0.0065(9) -0.0049(9) -0.0032(8) C14 0.0134(10) 0.0159(10) 0.0138(10) -0.0053(9) -0.0040(8) -0.0012(8) C15 0.0158(10) 0.0158(10) 0.0137(10) -0.0047(9) -0.0052(8) -0.0009(8) C16 0.0186(11) 0.0205(11) 0.0168(11) -0.0064(9) -0.0064(9) -0.0041(9) C17 0.0162(11) 0.0255(12) 0.0209(12) -0.0092(10) -0.0074(9) -0.0020(9) C18 0.0161(11) 0.0212(11) 0.0199(11) -0.0080(10) -0.0070(9) 0.0031(9) C19 0.0156(10) 0.0157(10) 0.0166(11) -0.0054(9) -0.0062(9) 0.0010(8) C20 0.0181(11) 0.0187(11) 0.0289(13) -0.0113(10) -0.0088(10) 0.0022(9) C21 0.0146(10) 0.0199(11) 0.0207(11) -0.0119(10) -0.0025(9) -0.0014(8) C22 0.0296(13) 0.0199(12) 0.0231(13) -0.0090(10) -0.0053(10) -0.0021(10) C23 0.0365(15) 0.0306(14) 0.0198(13) -0.0095(11) -0.0072(11) 0.0010(12) C24 0.0249(13) 0.0396(15) 0.0255(13) -0.0217(12) -0.0042(11) -0.0008(11) C25 0.0307(14) 0.0262(13) 0.0319(14) -0.0184(12) -0.0047(11) -0.0065(11) C26 0.0265(12) 0.0190(12) 0.0224(12) -0.0086(10) -0.0052(10) -0.0046(9) C27 0.0229(11) 0.0145(10) 0.0206(11) -0.0082(9) -0.0103(9) -0.0015(9) C28 0.0199(11) 0.0180(11) 0.0235(12) -0.0084(10) -0.0111(10) -0.0005(9) C29 0.0224(12) 0.0242(12) 0.0237(12) -0.0090(10) -0.0095(10) -0.0036(10) C30 0.0363(14) 0.0205(12) 0.0243(13) -0.0048(10) -0.0141(11) -0.0079(10) C31 0.0396(15) 0.0148(11) 0.0291(14) -0.0079(10) -0.0181(12) 0.0029(10) C32 0.0291(13) 0.0180(11) 0.0282(13) -0.0121(10) -0.0122(11) 0.0039(10) C33 0.053(5) 0.059(5) 0.050(4) -0.007(4) -0.026(4) -0.011(3) Cl1 0.0440(9) 0.0432(7) 0.0596(10) -0.0165(6) -0.0077(6) 0.0057(6) Cl2 0.0603(8) 0.0440(7) 0.0597(9) 0.0015(6) -0.0194(7) -0.0081(6) C33A 0.053(5) 0.059(5) 0.050(4) -0.007(4) -0.026(4) -0.011(3) Cl1A 0.0440(9) 0.0432(7) 0.0596(10) -0.0165(6) -0.0077(6) 0.0057(6) Cl2A 0.0603(8) 0.0440(7) 0.0597(9) 0.0015(6) -0.0194(7) -0.0081(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C14 1.923(2) . ? Ni1 P1 2.1611(6) . ? Ni1 P2 2.1704(6) . ? Ni1 Br1 2.3315(4) . ? P1 C7 1.812(2) . ? P1 C1 1.812(2) . ? P1 C13 1.882(2) . ? P2 C27 1.815(2) . ? P2 C21 1.815(2) . ? P2 C20 1.876(2) . ? O1 C13 1.212(3) . ? O2 C20 1.212(3) . ? C1 C2 1.387(3) . ? C1 C6 1.394(3) . ? C2 C3 1.394(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.396(3) . ? C7 C12 1.399(3) . ? C8 C9 1.394(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(4) . ? C9 H9 0.9500 . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.473(3) . ? C14 C15 1.419(3) . ? C14 C19 1.420(3) . ? C15 C16 1.394(3) . ? C16 C17 1.390(3) . ? C16 H16 0.9500 . ? C17 C18 1.388(3) . ? C17 H17 0.9500 . ? C18 C19 1.397(3) . ? C18 H18 0.9500 . ? C19 C20 1.471(3) . ? C21 C22 1.389(4) . ? C21 C26 1.392(3) . ? C22 C23 1.389(4) . ? C22 H22 0.9500 . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C25 C26 1.394(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.397(3) . ? C27 C32 1.400(3) . ? C28 C29 1.388(4) . ? C28 H28 0.9500 . ? C29 C30 1.389(4) . ? C29 H29 0.9500 . ? C30 C31 1.384(4) . ? C30 H30 0.9500 . ? C31 C32 1.389(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 Cl2 1.709(8) . ? C33 Cl1 1.757(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33A Cl1A 1.737(7) . ? C33A Cl2A 1.737(7) . ? C33A H33C 0.9900 . ? C33A H33D 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 C14 Ni1 P1 86.74(7) . . ? C14 Ni1 P2 86.74(7) . . ? P1 Ni1 P2 172.80(3) . . ? C14 Ni1 Br1 175.11(7) . . ? P1 Ni1 Br1 92.255(19) . . ? P2 Ni1 Br1 94.494(19) . . ? C7 P1 C1 106.47(10) . . ? C7 P1 C13 105.00(10) . . ? C1 P1 C13 102.77(10) . . ? C7 P1 Ni1 120.30(8) . . ? C1 P1 Ni1 116.96(7) . . ? C13 P1 Ni1 103.11(8) . . ? C27 P2 C21 108.03(10) . . ? C27 P2 C20 103.35(11) . . ? C21 P2 C20 104.66(11) . . ? C27 P2 Ni1 116.44(8) . . ? C21 P2 Ni1 119.63(8) . . ? C20 P2 Ni1 102.52(8) . . ? C2 C1 C6 119.7(2) . . ? C2 C1 P1 121.62(18) . . ? C6 C1 P1 118.68(19) . . ? C1 C2 C3 119.9(2) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.1(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.1(2) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 119.6(2) . . ? C8 C7 P1 120.03(17) . . ? C12 C7 P1 120.34(18) . . ? C9 C8 C7 119.8(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.0(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.1(2) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? O1 C13 C15 126.4(2) . . ? O1 C13 P1 124.49(18) . . ? C15 C13 P1 109.10(15) . . ? C15 C14 C19 114.49(19) . . ? C15 C14 Ni1 122.75(16) . . ? C19 C14 Ni1 122.64(16) . . ? C16 C15 C14 122.9(2) . . ? C16 C15 C13 118.8(2) . . ? C14 C15 C13 118.20(19) . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 118.7(2) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 120.6(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 122.7(2) . . ? C18 C19 C20 119.4(2) . . ? C14 C19 C20 117.9(2) . . ? O2 C20 C19 125.8(2) . . ? O2 C20 P2 124.47(19) . . ? C19 C20 P2 109.66(16) . . ? C22 C21 C26 119.6(2) . . ? C22 C21 P2 117.45(18) . . ? C26 C21 P2 122.93(19) . . ? C21 C22 C23 120.2(2) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 120.0(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.0(2) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C32 119.5(2) . . ? C28 C27 P2 118.51(18) . . ? C32 C27 P2 121.92(19) . . ? C29 C28 C27 120.1(2) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0(2) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.4(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.1(2) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 120.0(2) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? Cl2 C33 Cl1 113.8(6) . . ? Cl2 C33 H33A 108.8 . . ? Cl1 C33 H33A 108.8 . . ? Cl2 C33 H33B 108.8 . . ? Cl1 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? Cl1A C33A Cl2A 113.8(5) . . ? Cl1A C33A H33C 108.8 . . ? Cl2A C33A H33C 108.8 . . ? Cl1A C33A H33D 108.8 . . ? Cl2A C33A H33D 108.8 . . ? H33C C33A H33D 107.7 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.063 _refine_diff_density_min -1.032 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 934907' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb509_0m #TrackingRef '09 MSB509_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H23 Br O2 P2 Pd' _chemical_formula_sum 'C32 H23 Br O2 P2 Pd' _chemical_formula_weight 687.75 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' Br Br -0.2901 2.4595 '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 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.112(4) _cell_length_b 24.206(11) _cell_length_c 12.977(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.137(6) _cell_angle_gamma 90.00 _cell_volume 2798(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9047 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.64 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 2.234 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5969 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 20 sec/frame. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48179 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.71 _reflns_number_total 7136 _reflns_number_gt 6140 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)' _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^)+(0.0305P)^2^+2.5903P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7136 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.608873(18) 0.110681(6) 0.155707(12) 0.01424(5) Uani 1 1 d . . . Br1 Br 0.51619(3) 0.204533(9) 0.185728(17) 0.02145(6) Uani 1 1 d . . . P1 P 0.68077(6) 0.13013(2) 0.00144(4) 0.01678(11) Uani 1 1 d . . . P2 P 0.57115(6) 0.07740(2) 0.31198(4) 0.01625(11) Uani 1 1 d . . . O1 O 0.8042(2) 0.05427(7) -0.11264(13) 0.0279(4) Uani 1 1 d . . . O2 O 0.5919(2) -0.03244(7) 0.36437(15) 0.0332(4) Uani 1 1 d . . . C1 C 0.8514(2) 0.17063(9) 0.01844(17) 0.0192(4) Uani 1 1 d . . . C2 C 0.9659(3) 0.15735(11) 0.1054(2) 0.0280(5) Uani 1 1 d . . . H2 H 0.9491 0.1299 0.1540 0.034 Uiso 1 1 calc R . . C3 C 1.1032(3) 0.18390(11) 0.1207(2) 0.0320(6) Uani 1 1 d . . . H3 H 1.1810 0.1744 0.1791 0.038 Uiso 1 1 calc R . . C4 C 1.1268(3) 0.22450(11) 0.0506(2) 0.0293(5) Uani 1 1 d . . . H4 H 1.2211 0.2427 0.0608 0.035 Uiso 1 1 calc R . . C5 C 1.0132(3) 0.23868(11) -0.0345(2) 0.0282(5) Uani 1 1 d . . . H5 H 1.0297 0.2670 -0.0815 0.034 Uiso 1 1 calc R . . C6 C 0.8759(3) 0.21181(10) -0.05131(19) 0.0245(5) Uani 1 1 d . . . H6 H 0.7988 0.2214 -0.1100 0.029 Uiso 1 1 calc R . . C7 C 0.5543(3) 0.15563(9) -0.11572(17) 0.0203(4) Uani 1 1 d . . . C8 C 0.4234(3) 0.18255(10) -0.10394(18) 0.0231(5) Uani 1 1 d . . . H8 H 0.3997 0.1855 -0.0363 0.028 Uiso 1 1 calc R . . C9 C 0.3276(3) 0.20515(10) -0.1918(2) 0.0274(5) Uani 1 1 d . . . H9 H 0.2388 0.2237 -0.1839 0.033 Uiso 1 1 calc R . . C10 C 0.3619(3) 0.20053(10) -0.2911(2) 0.0310(6) Uani 1 1 d . . . H10 H 0.2970 0.2164 -0.3507 0.037 Uiso 1 1 calc R . . C11 C 0.4901(3) 0.17295(11) -0.30324(19) 0.0314(6) Uani 1 1 d . . . H11 H 0.5120 0.1693 -0.3713 0.038 Uiso 1 1 calc R . . C12 C 0.5871(3) 0.15043(11) -0.21600(18) 0.0269(5) Uani 1 1 d . . . H12 H 0.6752 0.1316 -0.2245 0.032 Uiso 1 1 calc R . . C13 C 0.7560(3) 0.06149(10) -0.03349(18) 0.0204(4) Uani 1 1 d . . . C14 C 0.7555(2) 0.02024(9) 0.05071(17) 0.0190(4) Uani 1 1 d . . . C15 C 0.8202(3) -0.03165(10) 0.04191(19) 0.0238(5) Uani 1 1 d . . . H15 H 0.8638 -0.0394 -0.0169 0.029 Uiso 1 1 calc R . . C16 C 0.8211(3) -0.07170(10) 0.1181(2) 0.0271(5) Uani 1 1 d . . . H16 H 0.8663 -0.1066 0.1125 0.033 Uiso 1 1 calc R . . C17 C 0.7549(3) -0.06014(10) 0.2029(2) 0.0253(5) Uani 1 1 d . . . H17 H 0.7527 -0.0878 0.2546 0.030 Uiso 1 1 calc R . . C18 C 0.6917(3) -0.00839(9) 0.21299(17) 0.0194(4) Uani 1 1 d . . . C19 C 0.6920(2) 0.03385(9) 0.13798(17) 0.0173(4) Uani 1 1 d . . . C20 C 0.6204(3) 0.00200(9) 0.30375(18) 0.0210(4) Uani 1 1 d . . . C21 C 0.6995(2) 0.10175(9) 0.43000(17) 0.0181(4) Uani 1 1 d . . . C22 C 0.7851(3) 0.14896(9) 0.42342(18) 0.0203(4) Uani 1 1 d . . . H22 H 0.7747 0.1680 0.3583 0.024 Uiso 1 1 calc R . . C23 C 0.8861(3) 0.16819(10) 0.51240(19) 0.0249(5) Uani 1 1 d . . . H23 H 0.9436 0.2005 0.5080 0.030 Uiso 1 1 calc R . . C24 C 0.9023(3) 0.13993(10) 0.60754(19) 0.0260(5) Uani 1 1 d . . . H24 H 0.9703 0.1532 0.6682 0.031 Uiso 1 1 calc R . . C25 C 0.8195(3) 0.09250(11) 0.61403(19) 0.0267(5) Uani 1 1 d . . . H25 H 0.8324 0.0731 0.6789 0.032 Uiso 1 1 calc R . . C26 C 0.7174(3) 0.07307(10) 0.52599(18) 0.0229(5) Uani 1 1 d . . . H26 H 0.6604 0.0407 0.5309 0.028 Uiso 1 1 calc R . . C27 C 0.3846(2) 0.07637(9) 0.33889(17) 0.0189(4) Uani 1 1 d . . . C28 C 0.2745(3) 0.04718(10) 0.2692(2) 0.0260(5) Uani 1 1 d . . . H28 H 0.2993 0.0289 0.2104 0.031 Uiso 1 1 calc R . . C29 C 0.1293(3) 0.04469(11) 0.2852(2) 0.0305(6) Uani 1 1 d . . . H29 H 0.0548 0.0245 0.2378 0.037 Uiso 1 1 calc R . . C30 C 0.0932(3) 0.07145(13) 0.3698(2) 0.0374(6) Uani 1 1 d . . . H30 H -0.0065 0.0696 0.3809 0.045 Uiso 1 1 calc R . . C31 C 0.2003(3) 0.10101(17) 0.4386(3) 0.0528(9) Uani 1 1 d . . . H31 H 0.1741 0.1197 0.4965 0.063 Uiso 1 1 calc R . . C32 C 0.3470(3) 0.10350(14) 0.4234(2) 0.0385(7) Uani 1 1 d . . . H32 H 0.4209 0.1238 0.4710 0.046 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 Pd1 0.01743(9) 0.01234(8) 0.01347(8) -0.00042(6) 0.00446(6) -0.00069(6) Br1 0.02514(12) 0.01680(11) 0.02071(11) -0.00211(8) 0.00096(9) 0.00332(8) P1 0.0189(3) 0.0168(3) 0.0151(2) 0.0002(2) 0.0046(2) -0.0006(2) P2 0.0203(3) 0.0137(3) 0.0155(2) 0.00017(19) 0.0056(2) -0.0008(2) O1 0.0370(10) 0.0272(9) 0.0233(8) -0.0016(7) 0.0151(8) 0.0021(8) O2 0.0534(12) 0.0176(9) 0.0349(10) 0.0055(7) 0.0235(9) 0.0019(8) C1 0.0208(11) 0.0187(11) 0.0198(10) -0.0006(8) 0.0079(9) -0.0006(8) C2 0.0271(13) 0.0263(13) 0.0298(12) 0.0078(10) 0.0037(10) -0.0028(10) C3 0.0216(12) 0.0327(14) 0.0385(14) 0.0069(12) -0.0008(11) -0.0020(11) C4 0.0235(12) 0.0270(13) 0.0390(14) 0.0008(11) 0.0102(11) -0.0046(10) C5 0.0329(13) 0.0236(12) 0.0309(12) 0.0039(10) 0.0133(11) -0.0041(10) C6 0.0286(13) 0.0235(12) 0.0222(11) 0.0015(9) 0.0070(10) -0.0009(10) C7 0.0232(11) 0.0198(11) 0.0165(10) 0.0006(8) 0.0013(9) -0.0040(9) C8 0.0290(12) 0.0191(11) 0.0200(11) -0.0008(9) 0.0022(9) -0.0014(9) C9 0.0324(14) 0.0195(12) 0.0268(12) 0.0002(9) -0.0019(10) 0.0031(10) C10 0.0430(16) 0.0226(12) 0.0222(12) 0.0050(9) -0.0048(11) -0.0026(11) C11 0.0451(16) 0.0310(14) 0.0169(11) 0.0009(10) 0.0035(11) -0.0033(12) C12 0.0322(13) 0.0296(13) 0.0202(11) -0.0007(9) 0.0082(10) 0.0001(11) C13 0.0196(11) 0.0203(11) 0.0215(11) -0.0044(8) 0.0046(9) -0.0010(9) C14 0.0205(11) 0.0152(10) 0.0213(10) -0.0023(8) 0.0048(9) -0.0020(8) C15 0.0259(12) 0.0208(12) 0.0276(12) -0.0035(9) 0.0121(10) 0.0004(9) C16 0.0325(13) 0.0149(11) 0.0369(13) -0.0015(10) 0.0140(11) 0.0033(10) C17 0.0308(13) 0.0157(11) 0.0313(12) 0.0020(9) 0.0109(10) 0.0005(9) C18 0.0224(11) 0.0145(10) 0.0219(10) -0.0006(8) 0.0063(9) -0.0013(8) C19 0.0175(10) 0.0141(10) 0.0204(10) -0.0026(8) 0.0044(8) -0.0018(8) C20 0.0258(12) 0.0155(10) 0.0225(11) 0.0000(8) 0.0070(9) -0.0006(9) C21 0.0182(10) 0.0175(10) 0.0187(10) -0.0021(8) 0.0045(8) 0.0015(8) C22 0.0212(11) 0.0178(11) 0.0219(11) 0.0000(8) 0.0044(9) 0.0024(9) C23 0.0238(12) 0.0203(11) 0.0293(12) -0.0032(9) 0.0024(10) 0.0018(9) C24 0.0255(12) 0.0271(13) 0.0224(11) -0.0053(9) -0.0018(9) 0.0060(10) C25 0.0312(13) 0.0299(13) 0.0187(11) 0.0033(9) 0.0045(10) 0.0064(11) C26 0.0249(12) 0.0229(11) 0.0218(11) 0.0027(9) 0.0067(9) -0.0001(9) C27 0.0217(11) 0.0179(10) 0.0172(10) 0.0029(8) 0.0045(8) -0.0012(9) C28 0.0242(12) 0.0237(12) 0.0288(12) -0.0050(10) 0.0029(10) -0.0009(10) C29 0.0219(12) 0.0236(13) 0.0425(15) 0.0022(11) -0.0014(11) -0.0015(10) C30 0.0212(13) 0.0472(17) 0.0451(16) 0.0075(13) 0.0097(12) 0.0037(12) C31 0.0280(15) 0.088(3) 0.0453(18) -0.0244(18) 0.0148(14) 0.0021(16) C32 0.0221(13) 0.060(2) 0.0341(14) -0.0224(13) 0.0061(11) -0.0024(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C19 2.039(2) . ? Pd1 P2 2.2744(10) . ? Pd1 P1 2.2826(10) . ? Pd1 Br1 2.4828(10) . ? P1 C1 1.812(2) . ? P1 C7 1.812(2) . ? P1 C13 1.889(2) . ? P2 C27 1.806(2) . ? P2 C21 1.819(2) . ? P2 C20 1.888(2) . ? O1 C13 1.212(3) . ? O2 C20 1.211(3) . ? C1 C6 1.395(3) . ? C1 C2 1.403(3) . ? C2 C3 1.383(4) . ? C2 H2 0.9500 . ? C3 C4 1.387(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.395(3) . ? C7 C12 1.401(3) . ? C8 C9 1.394(3) . ? C8 H8 0.9500 . ? C9 C10 1.393(4) . ? C9 H9 0.9500 . ? C10 C11 1.383(4) . ? C10 H10 0.9500 . ? C11 C12 1.393(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.481(3) . ? C14 C15 1.402(3) . ? C14 C19 1.415(3) . ? C15 C16 1.383(3) . ? C15 H15 0.9500 . ? C16 C17 1.390(3) . ? C16 H16 0.9500 . ? C17 C18 1.397(3) . ? C17 H17 0.9500 . ? C18 C19 1.412(3) . ? C18 C20 1.481(3) . ? C21 C22 1.397(3) . ? C21 C26 1.405(3) . ? C22 C23 1.396(3) . ? C22 H22 0.9500 . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 C26 1.395(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.382(3) . ? C27 C28 1.394(3) . ? C28 C29 1.384(4) . ? C28 H28 0.9500 . ? C29 C30 1.373(4) . ? C29 H29 0.9500 . ? C30 C31 1.377(4) . ? C30 H30 0.9500 . ? C31 C32 1.393(4) . ? C31 H31 0.9500 . ? C32 H32 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 C19 Pd1 P2 84.66(7) . . ? C19 Pd1 P1 84.68(6) . . ? P2 Pd1 P1 168.56(2) . . ? C19 Pd1 Br1 177.22(6) . . ? P2 Pd1 Br1 93.67(2) . . ? P1 Pd1 Br1 96.82(2) . . ? C1 P1 C7 107.22(11) . . ? C1 P1 C13 99.19(11) . . ? C7 P1 C13 107.29(11) . . ? C1 P1 Pd1 113.70(7) . . ? C7 P1 Pd1 123.84(8) . . ? C13 P1 Pd1 102.39(8) . . ? C27 P2 C21 107.84(10) . . ? C27 P2 C20 104.03(10) . . ? C21 P2 C20 104.03(10) . . ? C27 P2 Pd1 120.14(7) . . ? C21 P2 Pd1 116.43(8) . . ? C20 P2 Pd1 102.10(7) . . ? C6 C1 C2 119.4(2) . . ? C6 C1 P1 123.88(18) . . ? C2 C1 P1 116.62(17) . . ? C3 C2 C1 120.5(2) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.6(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 120.3(2) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 119.7(2) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C8 C7 C12 119.9(2) . . ? C8 C7 P1 118.33(17) . . ? C12 C7 P1 121.77(19) . . ? C9 C8 C7 119.8(2) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.2(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 119.8(2) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? O1 C13 C14 125.9(2) . . ? O1 C13 P1 123.02(18) . . ? C14 C13 P1 111.01(16) . . ? C15 C14 C19 121.6(2) . . ? C15 C14 C13 118.5(2) . . ? C19 C14 C13 119.9(2) . . ? C16 C15 C14 120.6(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.1(2) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 120.7(2) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 121.6(2) . . ? C17 C18 C20 119.0(2) . . ? C19 C18 C20 119.3(2) . . ? C18 C19 C14 116.3(2) . . ? C18 C19 Pd1 121.88(16) . . ? C14 C19 Pd1 121.79(16) . . ? O2 C20 C18 126.1(2) . . ? O2 C20 P2 122.85(18) . . ? C18 C20 P2 111.00(15) . . ? C22 C21 C26 119.7(2) . . ? C22 C21 P2 118.84(17) . . ? C26 C21 P2 121.39(18) . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.9(2) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C25 C24 C23 120.2(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.5(2) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.5(2) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C32 C27 C28 119.4(2) . . ? C32 C27 P2 123.22(19) . . ? C28 C27 P2 117.37(18) . . ? C29 C28 C27 120.3(2) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 119.8(2) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.5(3) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 119.9(3) . . ? C27 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.987 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 934908' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb413_0m #TrackingRef '10 msb413_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Di-\m-chlorobis(\m-(3-diphenylphosphanecarbonylphenyl) diphenylphosphanylmethanone)dicopper(I) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H48 Cl2 Cu2 O4 P4, 4(C2 H3 N)' _chemical_formula_sum 'C72 H60 Cl2 Cu2 N4 O4 P4' _chemical_formula_weight 1367.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1567(18) _cell_length_b 14.4395(18) _cell_length_c 17.487(2) _cell_angle_alpha 91.137(2) _cell_angle_beta 91.028(2) _cell_angle_gamma 112.604(2) _cell_volume 3298.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4943 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.14 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7612 _exptl_absorpt_correction_T_max 0.8918 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008b)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. The scan time was 15 sec/frame. Inspection of 1758 reflections harvested form the full data set and having I/\s(I) > 15 with CELL_NOW (Sheldrick, 2008a) showed the crystal to have a triclinic cell and to be twinned by a 180 deg. rotation about c*. The raw data were integrated using the 2-component version of SAINT as directed by the 2-component control file produced by CELL_NOW. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29488 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.00 _reflns_number_total 16027 _reflns_number_gt 12638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The final refinement was performed with the full 2-component reflection file. ; _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^)+(0.0494P)^2^+2.4716P] 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 16007 _refine_ls_number_parameters 796 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Cu1 Cu 0.81549(3) 0.68479(3) 0.75343(3) 0.01681(10) Uani 1 1 d . . . Cu2 Cu 0.70251(3) 0.83636(3) 0.75337(3) 0.01702(11) Uani 1 1 d . . . Cl1 Cl 0.75532(9) 0.75660(8) 0.65086(3) 0.02056(13) Uani 1 1 d . . . Cl2 Cl 0.76349(9) 0.76476(8) 0.85310(3) 0.01953(13) Uani 1 1 d . . . P1 P 0.73458(8) 0.51621(7) 0.74350(6) 0.0175(2) Uani 1 1 d . . . P2 P 0.53056(7) 0.78952(7) 0.75181(6) 0.0169(2) Uani 1 1 d . . . P3 P 0.78318(8) 1.00402(7) 0.74294(6) 0.0176(2) Uani 1 1 d . . . P4 P 0.98711(7) 0.73135(7) 0.75123(6) 0.0167(2) Uani 1 1 d . . . O1 O 0.5860(2) 0.3972(2) 0.64250(19) 0.0358(8) Uani 1 1 d . . . O2 O 0.4181(3) 0.7031(2) 0.87418(18) 0.0396(8) Uani 1 1 d . . . O3 O 0.9266(2) 1.1194(2) 0.64540(18) 0.0339(7) Uani 1 1 d . . . O4 O 1.1131(3) 0.8276(2) 0.87155(18) 0.0412(8) Uani 1 1 d . . . C1 C 0.8051(3) 0.4662(3) 0.6801(2) 0.0230(9) Uani 1 1 d . . . C2 C 0.8283(3) 0.5114(3) 0.6100(2) 0.0271(9) Uani 1 1 d . . . H2 H 0.8066 0.5640 0.5977 0.033 Uiso 1 1 calc R . . C3 C 0.8832(3) 0.4802(3) 0.5576(3) 0.0345(11) Uani 1 1 d . . . H3 H 0.8994 0.5117 0.5097 0.041 Uiso 1 1 calc R . . C4 C 0.9141(4) 0.4037(3) 0.5751(3) 0.0479(15) Uani 1 1 d . . . H4 H 0.9508 0.3816 0.5390 0.057 Uiso 1 1 calc R . . C5 C 0.8920(4) 0.3592(3) 0.6448(4) 0.0496(14) Uani 1 1 d . . . H5 H 0.9135 0.3063 0.6567 0.060 Uiso 1 1 calc R . . C6 C 0.8383(4) 0.3909(3) 0.6980(3) 0.0371(11) Uani 1 1 d . . . H6 H 0.8245 0.3609 0.7466 0.045 Uiso 1 1 calc R . . C7 C 0.7119(3) 0.4457(3) 0.8302(2) 0.0201(8) Uani 1 1 d . . . C8 C 0.7471(3) 0.4967(3) 0.9001(2) 0.0267(8) Uani 1 1 d . . . H8 H 0.7815 0.5677 0.9018 0.032 Uiso 1 1 calc R . . C9 C 0.7318(4) 0.4440(4) 0.9674(3) 0.0380(10) Uani 1 1 d . . . H9 H 0.7555 0.4789 1.0149 0.046 Uiso 1 1 calc R . . C10 C 0.6820(4) 0.3407(4) 0.9651(3) 0.0397(12) Uani 1 1 d . . . H10 H 0.6729 0.3046 1.0111 0.048 Uiso 1 1 calc R . . C11 C 0.6454(4) 0.2898(3) 0.8961(3) 0.0352(10) Uani 1 1 d . . . H11 H 0.6106 0.2189 0.8949 0.042 Uiso 1 1 calc R . . C12 C 0.6593(3) 0.3417(3) 0.8292(3) 0.0283(10) Uani 1 1 d . . . H12 H 0.6328 0.3065 0.7821 0.034 Uiso 1 1 calc R . . C13 C 0.6022(3) 0.4530(3) 0.6983(2) 0.0211(8) Uani 1 1 d . . . C14 C 0.5186(3) 0.4720(3) 0.7372(2) 0.0198(9) Uani 1 1 d . . . C15 C 0.4269(3) 0.3908(3) 0.7497(4) 0.0317(10) Uani 1 1 d . . . H15 H 0.4175 0.3251 0.7320 0.038 Uiso 1 1 calc R . . C16 C 0.3497(4) 0.4075(3) 0.7883(3) 0.0406(12) Uani 1 1 d . . . H16 H 0.2877 0.3527 0.7981 0.049 Uiso 1 1 calc R . . C17 C 0.3627(3) 0.5038(3) 0.8126(3) 0.0308(11) Uani 1 1 d . . . H17 H 0.3103 0.5144 0.8402 0.037 Uiso 1 1 calc R . . C18 C 0.4515(3) 0.5843(3) 0.7969(2) 0.0220(8) Uani 1 1 d . . . C19 C 0.5306(3) 0.5679(3) 0.7599(2) 0.0194(8) Uani 1 1 d . . . H19 H 0.5925 0.6229 0.7503 0.023 Uiso 1 1 calc R . . C20 C 0.4582(3) 0.6868(3) 0.8181(2) 0.0230(8) Uani 1 1 d . . . C21 C 0.4591(3) 0.7367(3) 0.6633(2) 0.0193(8) Uani 1 1 d . . . C22 C 0.3525(3) 0.6932(3) 0.6612(2) 0.0234(9) Uani 1 1 d . . . H22 H 0.3158 0.6885 0.7068 0.028 Uiso 1 1 calc R . . C23 C 0.3001(3) 0.6570(3) 0.5923(3) 0.0306(10) Uani 1 1 d . . . H23 H 0.2275 0.6266 0.5911 0.037 Uiso 1 1 calc R . . C24 C 0.3527(3) 0.6646(3) 0.5254(2) 0.0272(9) Uani 1 1 d . . . H24 H 0.3159 0.6411 0.4783 0.033 Uiso 1 1 calc R . . C25 C 0.4583(3) 0.7062(3) 0.5266(2) 0.0238(9) Uani 1 1 d . . . H25 H 0.4943 0.7103 0.4807 0.029 Uiso 1 1 calc R . . C26 C 0.5116(3) 0.7419(3) 0.5957(2) 0.0205(8) Uani 1 1 d . . . H26 H 0.5843 0.7702 0.5968 0.025 Uiso 1 1 calc R . . C27 C 0.4862(3) 0.8879(3) 0.7799(2) 0.0234(9) Uani 1 1 d . . . C28 C 0.4449(3) 0.9320(3) 0.7258(3) 0.0295(10) Uani 1 1 d . . . H28 H 0.4356 0.9078 0.6741 0.035 Uiso 1 1 calc R . . C29 C 0.4172(3) 1.0112(3) 0.7467(4) 0.0388(11) Uani 1 1 d . . . H29 H 0.3891 1.0410 0.7094 0.047 Uiso 1 1 calc R . . C30 C 0.4306(3) 1.0468(3) 0.8217(3) 0.0414(12) Uani 1 1 d . . . H30 H 0.4114 1.1008 0.8361 0.050 Uiso 1 1 calc R . . C31 C 0.4719(3) 1.0035(3) 0.8758(3) 0.0397(11) Uani 1 1 d . . . H31 H 0.4802 1.0276 0.9275 0.048 Uiso 1 1 calc R . . C32 C 0.5016(3) 0.9246(3) 0.8554(3) 0.0311(10) Uani 1 1 d . . . H32 H 0.5320 0.8965 0.8924 0.037 Uiso 1 1 calc R . . C33 C 0.7094(3) 1.0481(3) 0.6782(2) 0.0238(9) Uani 1 1 d . . . C34 C 0.6805(3) 0.9953(3) 0.6083(2) 0.0252(9) Uani 1 1 d . . . H34 H 0.6996 0.9401 0.5980 0.030 Uiso 1 1 calc R . . C35 C 0.6244(3) 1.0222(3) 0.5538(3) 0.0337(11) Uani 1 1 d . . . H35 H 0.6047 0.9856 0.5065 0.040 Uiso 1 1 calc R . . C36 C 0.5972(3) 1.1026(3) 0.5690(3) 0.0371(11) Uani 1 1 d . . . H36 H 0.5591 1.1217 0.5316 0.044 Uiso 1 1 calc R . . C37 C 0.6244(4) 1.1550(3) 0.6370(3) 0.0418(12) Uani 1 1 d . . . H37 H 0.6055 1.2106 0.6463 0.050 Uiso 1 1 calc R . . C38 C 0.6796(3) 1.1280(3) 0.6931(3) 0.0327(10) Uani 1 1 d . . . H38 H 0.6968 1.1637 0.7409 0.039 Uiso 1 1 calc R . . C39 C 0.8065(3) 1.0808(3) 0.8304(2) 0.0216(9) Uani 1 1 d . . . C40 C 0.7682(3) 1.0352(3) 0.8976(2) 0.0255(8) Uani 1 1 d . . . H40 H 0.7329 0.9644 0.8981 0.031 Uiso 1 1 calc R . . C41 C 0.7807(4) 1.0917(3) 0.9648(3) 0.0324(10) Uani 1 1 d . . . H41 H 0.7534 1.0600 1.0111 0.039 Uiso 1 1 calc R . . C42 C 0.8333(4) 1.1948(3) 0.9641(2) 0.0337(10) Uani 1 1 d . . . H42 H 0.8413 1.2338 1.0100 0.040 Uiso 1 1 calc R . . C43 C 0.8738(3) 1.2412(3) 0.8979(3) 0.0326(10) Uani 1 1 d . . . H43 H 0.9099 1.3119 0.8982 0.039 Uiso 1 1 calc R . . C44 C 0.8620(3) 1.1848(3) 0.8303(2) 0.0256(9) Uani 1 1 d . . . H44 H 0.8913 1.2166 0.7846 0.031 Uiso 1 1 calc R . . C45 C 0.9130(3) 1.0661(3) 0.6994(2) 0.0223(8) Uani 1 1 d . . . C46 C 0.9999(3) 1.0501(3) 0.7386(3) 0.0231(10) Uani 1 1 d . . . C47 C 1.0931(3) 1.1308(3) 0.7511(3) 0.0312(10) Uani 1 1 d . . . H47 H 1.1014 1.1954 0.7340 0.037 Uiso 1 1 calc R . . C48 C 1.1731(3) 1.1172(3) 0.7880(3) 0.0378(12) Uani 1 1 d . . . H48 H 1.2359 1.1728 0.7975 0.045 Uiso 1 1 calc R . . C49 C 1.1628(3) 1.0229(3) 0.8115(3) 0.0286(10) Uani 1 1 d . . . H49 H 1.2176 1.0140 0.8380 0.034 Uiso 1 1 calc R . . C50 C 1.0712(3) 0.9410(3) 0.7959(2) 0.0192(9) Uani 1 1 d . . . C51 C 0.9888(3) 0.9541(3) 0.7610(2) 0.0183(8) Uani 1 1 d . . . H51 H 0.9257 0.8987 0.7524 0.022 Uiso 1 1 calc R . . C52 C 1.0662(3) 0.8393(3) 0.8167(2) 0.0232(8) Uani 1 1 d . . . C53 C 1.0320(3) 0.6355(3) 0.7815(2) 0.0212(8) Uani 1 1 d . . . C54 C 1.0758(3) 0.5890(3) 0.7302(3) 0.0308(10) Uani 1 1 d . . . H54 H 1.0860 0.6098 0.6787 0.037 Uiso 1 1 calc R . . C55 C 1.1046(3) 0.5119(3) 0.7547(4) 0.0419(12) Uani 1 1 d . . . H55 H 1.1339 0.4800 0.7198 0.050 Uiso 1 1 calc R . . C56 C 1.0908(3) 0.4822(3) 0.8288(3) 0.0428(13) Uani 1 1 d . . . H56 H 1.1113 0.4303 0.8455 0.051 Uiso 1 1 calc R . . C57 C 1.0472(3) 0.5272(3) 0.8792(3) 0.0371(11) Uani 1 1 d . . . H57 H 1.0379 0.5063 0.9306 0.044 Uiso 1 1 calc R . . C58 C 1.0168(3) 0.6027(3) 0.8558(3) 0.0285(9) Uani 1 1 d . . . H58 H 0.9853 0.6322 0.8909 0.034 Uiso 1 1 calc R . . C59 C 1.0519(3) 0.7757(3) 0.6621(2) 0.0184(8) Uani 1 1 d . . . C60 C 1.1589(3) 0.8193(3) 0.6599(2) 0.0244(9) Uani 1 1 d . . . H60 H 1.1990 0.8287 0.7056 0.029 Uiso 1 1 calc R . . C61 C 1.2059(3) 0.8484(3) 0.5910(2) 0.0266(9) Uani 1 1 d . . . H61 H 1.2784 0.8780 0.5894 0.032 Uiso 1 1 calc R . . C62 C 1.1469(3) 0.8345(3) 0.5235(2) 0.0249(9) Uani 1 1 d . . . H62 H 1.1793 0.8540 0.4761 0.030 Uiso 1 1 calc R . . C63 C 1.0420(3) 0.7928(3) 0.5260(2) 0.0242(9) Uani 1 1 d . . . H63 H 1.0021 0.7836 0.4801 0.029 Uiso 1 1 calc R . . C64 C 0.9945(3) 0.7642(3) 0.5943(2) 0.0216(9) Uani 1 1 d . . . H64 H 0.9219 0.7364 0.5954 0.026 Uiso 1 1 calc R . . N1 N 0.8201(4) 0.6450(4) 0.3981(4) 0.0677(16) Uani 1 1 d . . . C65 C 0.7461(5) 0.6222(4) 0.4266(4) 0.0554(16) Uani 1 1 d . . . C66 C 0.6457(4) 0.5912(4) 0.4638(4) 0.0664(19) Uani 1 1 d . . . H66A H 0.6561 0.6159 0.5172 0.100 Uiso 1 1 calc R . . H66B H 0.6124 0.5178 0.4623 0.100 Uiso 1 1 calc R . . H66C H 0.6022 0.6194 0.4367 0.100 Uiso 1 1 calc R . . N2 N 0.6718(4) 0.8419(4) 0.3995(4) 0.0643(15) Uani 1 1 d . . . C67 C 0.7494(5) 0.8694(4) 0.4258(4) 0.0537(16) Uani 1 1 d . . . C68 C 0.8538(4) 0.9077(4) 0.4607(5) 0.070(2) Uani 1 1 d . . . H68A H 0.8947 0.8753 0.4353 0.106 Uiso 1 1 calc R . . H68B H 0.8499 0.8927 0.5153 0.106 Uiso 1 1 calc R . . H68C H 0.8861 0.9805 0.4548 0.106 Uiso 1 1 calc R . . N3 N 0.6483(4) 0.8345(3) 0.0354(3) 0.0655(13) Uani 1 1 d . . . C69 C 0.6182(4) 0.7518(4) 0.0222(3) 0.0410(10) Uani 1 1 d . . . C70 C 0.5798(4) 0.6449(3) 0.0042(3) 0.0445(11) Uani 1 1 d . . . H70A H 0.5942 0.6099 0.0475 0.067 Uiso 1 1 calc R . . H70B H 0.6136 0.6329 -0.0412 0.067 Uiso 1 1 calc R . . H70C H 0.5058 0.6197 -0.0060 0.067 Uiso 1 1 calc R . . N4 N 0.1644(3) 0.3163(3) 0.9381(3) 0.0512(11) Uani 1 1 d . . . C71 C 0.1232(3) 0.2368(3) 0.9562(3) 0.0391(10) Uani 1 1 d . . . C72 C 0.0685(4) 0.1335(3) 0.9791(3) 0.0454(11) Uani 1 1 d . . . H72A H 0.0163 0.0973 0.9399 0.068 Uiso 1 1 calc R . . H72B H 0.0355 0.1334 1.0279 0.068 Uiso 1 1 calc R . . H72C H 0.1169 0.1003 0.9849 0.068 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 Cu1 0.0155(2) 0.0144(2) 0.0227(2) 0.00058(18) 0.0010(2) 0.0081(2) Cu2 0.0160(2) 0.0149(2) 0.0222(2) 0.00079(19) -0.0002(2) 0.0082(2) Cl1 0.0210(3) 0.0263(3) 0.0204(3) 0.0000(5) -0.0008(5) 0.0158(2) Cl2 0.0247(3) 0.0202(3) 0.0181(3) 0.0005(4) -0.0002(5) 0.0135(2) P1 0.0186(5) 0.0133(5) 0.0221(5) -0.0005(4) 0.0022(4) 0.0077(4) P2 0.0145(5) 0.0185(5) 0.0198(5) -0.0017(4) -0.0006(4) 0.0088(4) P3 0.0176(5) 0.0148(5) 0.0219(5) 0.0016(4) -0.0022(4) 0.0081(5) P4 0.0156(5) 0.0171(5) 0.0198(5) 0.0028(4) -0.0001(4) 0.0089(4) O1 0.0307(17) 0.0396(18) 0.0382(19) -0.0166(14) -0.0074(15) 0.0161(15) O2 0.053(2) 0.0394(18) 0.0319(18) 0.0029(14) 0.0206(16) 0.0234(16) O3 0.0326(17) 0.0380(17) 0.0335(18) 0.0201(14) 0.0060(14) 0.0151(15) O4 0.056(2) 0.0319(16) 0.0363(18) -0.0037(13) -0.0261(17) 0.0190(16) C1 0.020(2) 0.0178(19) 0.030(2) -0.0030(16) 0.0088(18) 0.0058(17) C2 0.022(2) 0.022(2) 0.034(3) -0.0030(17) 0.0047(19) 0.0046(19) C3 0.032(3) 0.030(2) 0.031(3) -0.0055(18) 0.015(2) 0.000(2) C4 0.041(3) 0.027(2) 0.073(4) -0.009(2) 0.033(3) 0.010(2) C5 0.051(3) 0.026(2) 0.081(4) 0.010(2) 0.033(3) 0.023(2) C6 0.039(3) 0.023(2) 0.056(3) 0.006(2) 0.016(2) 0.018(2) C7 0.020(2) 0.0166(18) 0.026(2) 0.0004(15) 0.0009(16) 0.0089(16) C8 0.029(2) 0.025(2) 0.029(2) -0.0004(15) -0.0001(16) 0.0144(18) C9 0.049(3) 0.047(3) 0.027(2) 0.0051(18) 0.0056(19) 0.027(2) C10 0.052(3) 0.048(3) 0.030(3) 0.018(2) 0.020(2) 0.030(3) C11 0.039(3) 0.028(2) 0.040(3) 0.0112(19) 0.011(2) 0.013(2) C12 0.030(2) 0.022(2) 0.031(2) 0.0013(17) 0.0064(19) 0.007(2) C13 0.024(2) 0.0158(18) 0.025(2) -0.0020(16) 0.0035(17) 0.0093(17) C14 0.012(2) 0.022(2) 0.025(2) -0.0005(16) -0.0005(16) 0.0065(18) C15 0.021(2) 0.022(2) 0.048(3) -0.004(2) 0.005(2) 0.006(2) C16 0.021(2) 0.031(2) 0.064(3) 0.006(2) 0.008(2) 0.003(2) C17 0.022(2) 0.035(3) 0.039(3) 0.005(2) 0.008(2) 0.014(2) C18 0.021(2) 0.025(2) 0.022(2) 0.0012(16) 0.0001(17) 0.0120(18) C19 0.0150(19) 0.021(2) 0.020(2) -0.0005(15) 0.0010(16) 0.0052(17) C20 0.021(2) 0.025(2) 0.025(2) 0.0016(16) 0.0022(17) 0.0102(17) C21 0.016(2) 0.0169(19) 0.027(2) 0.0025(15) 0.0002(17) 0.0090(17) C22 0.020(2) 0.030(2) 0.021(2) -0.0049(16) 0.0000(17) 0.012(2) C23 0.018(2) 0.038(3) 0.036(3) -0.004(2) -0.002(2) 0.011(2) C24 0.025(2) 0.034(2) 0.025(2) -0.0038(17) -0.0076(19) 0.014(2) C25 0.027(2) 0.028(2) 0.020(2) 0.0008(16) 0.0018(17) 0.015(2) C26 0.019(2) 0.021(2) 0.025(2) 0.0022(16) -0.0005(17) 0.0125(18) C27 0.017(2) 0.022(2) 0.034(2) -0.0066(16) -0.0002(17) 0.0112(17) C28 0.023(2) 0.026(2) 0.043(3) -0.0051(18) -0.0053(19) 0.0142(19) C29 0.027(2) 0.030(2) 0.064(3) -0.011(2) -0.012(2) 0.017(2) C30 0.023(2) 0.029(2) 0.073(4) -0.014(2) 0.001(2) 0.012(2) C31 0.037(3) 0.033(2) 0.047(3) -0.019(2) 0.002(2) 0.013(2) C32 0.029(2) 0.032(2) 0.033(2) -0.0079(18) 0.0012(19) 0.013(2) C33 0.022(2) 0.018(2) 0.032(2) 0.0032(16) -0.0010(18) 0.0073(18) C34 0.025(2) 0.023(2) 0.025(2) 0.0046(16) -0.0033(18) 0.0070(19) C35 0.030(3) 0.030(2) 0.036(3) 0.0091(19) -0.007(2) 0.006(2) C36 0.029(2) 0.034(3) 0.047(3) 0.012(2) -0.013(2) 0.011(2) C37 0.044(3) 0.029(2) 0.059(3) 0.002(2) -0.017(3) 0.022(2) C38 0.033(2) 0.024(2) 0.045(3) -0.0067(19) -0.015(2) 0.017(2) C39 0.022(2) 0.021(2) 0.022(2) -0.0016(15) -0.0063(17) 0.0093(18) C40 0.027(2) 0.024(2) 0.026(2) -0.0007(15) -0.0014(16) 0.0094(17) C41 0.040(2) 0.034(2) 0.022(2) 0.0017(16) 0.0008(18) 0.014(2) C42 0.048(3) 0.027(2) 0.030(2) -0.0065(16) -0.0092(19) 0.019(2) C43 0.039(2) 0.021(2) 0.037(2) -0.0056(17) -0.011(2) 0.0118(19) C44 0.030(2) 0.017(2) 0.030(2) 0.0005(16) -0.0024(18) 0.0099(18) C45 0.023(2) 0.0189(19) 0.026(2) 0.0034(16) 0.0067(18) 0.0088(17) C46 0.029(3) 0.018(2) 0.025(2) -0.0005(16) 0.0015(19) 0.011(2) C47 0.027(3) 0.015(2) 0.050(3) 0.005(2) 0.006(2) 0.006(2) C48 0.021(2) 0.019(2) 0.068(3) -0.001(2) -0.007(2) 0.0022(18) C49 0.016(2) 0.026(2) 0.043(3) -0.0038(18) -0.0046(19) 0.0064(17) C50 0.019(2) 0.017(2) 0.022(2) -0.0033(15) -0.0017(17) 0.0085(17) C51 0.019(2) 0.0174(19) 0.019(2) 0.0010(14) 0.0022(16) 0.0080(17) C52 0.023(2) 0.025(2) 0.024(2) 0.0021(16) -0.0020(17) 0.0122(18) C53 0.0138(18) 0.0190(19) 0.032(2) 0.0079(15) 0.0017(16) 0.0075(16) C54 0.027(2) 0.025(2) 0.046(3) 0.0134(18) 0.012(2) 0.015(2) C55 0.032(3) 0.032(2) 0.073(3) 0.015(2) 0.015(3) 0.024(2) C56 0.029(2) 0.032(2) 0.077(4) 0.028(2) 0.006(2) 0.021(2) C57 0.031(2) 0.035(2) 0.046(3) 0.020(2) -0.001(2) 0.012(2) C58 0.025(2) 0.025(2) 0.037(2) 0.0100(17) 0.0020(18) 0.0111(18) C59 0.019(2) 0.0187(19) 0.020(2) 0.0039(15) 0.0034(16) 0.0104(17) C60 0.018(2) 0.026(2) 0.030(2) 0.0034(17) -0.0034(18) 0.0095(19) C61 0.019(2) 0.033(2) 0.029(2) 0.0065(18) 0.0053(18) 0.011(2) C62 0.026(2) 0.028(2) 0.023(2) 0.0081(16) 0.0063(18) 0.013(2) C63 0.025(2) 0.026(2) 0.025(2) 0.0010(16) -0.0017(18) 0.014(2) C64 0.019(2) 0.020(2) 0.026(2) 0.0021(16) 0.0005(18) 0.0081(18) N1 0.049(3) 0.057(3) 0.101(5) -0.004(3) 0.016(3) 0.025(3) C65 0.060(4) 0.040(3) 0.069(4) -0.015(3) -0.015(4) 0.024(3) C66 0.049(3) 0.040(3) 0.125(6) 0.015(3) 0.006(4) 0.032(3) N2 0.039(3) 0.053(3) 0.102(5) 0.010(3) -0.004(3) 0.018(3) C67 0.066(4) 0.044(3) 0.066(4) 0.016(3) 0.030(4) 0.035(3) C68 0.043(3) 0.052(4) 0.126(6) 0.001(4) 0.006(4) 0.029(3) N3 0.071(3) 0.051(3) 0.071(3) -0.018(2) 0.021(3) 0.020(2) C69 0.037(3) 0.045(3) 0.041(3) -0.004(2) 0.014(2) 0.016(2) C70 0.043(3) 0.038(2) 0.053(3) 0.002(2) -0.002(2) 0.015(2) N4 0.053(3) 0.042(2) 0.059(3) 0.011(2) -0.016(2) 0.019(2) C71 0.036(2) 0.035(2) 0.045(3) 0.003(2) -0.0069(19) 0.013(2) C72 0.045(3) 0.034(2) 0.050(3) -0.001(2) -0.001(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P1 2.2584(10) . ? Cu1 P4 2.2595(11) . ? Cu1 Cl2 2.3523(9) . ? Cu1 Cl1 2.3908(10) . ? Cu2 P3 2.2579(10) . ? Cu2 P2 2.2617(11) . ? Cu2 Cl2 2.3579(9) . ? Cu2 Cl1 2.3930(10) . ? P1 C7 1.807(4) . ? P1 C1 1.819(4) . ? P1 C13 1.890(4) . ? P2 C21 1.818(4) . ? P2 C27 1.822(4) . ? P2 C20 1.880(4) . ? P3 C33 1.809(4) . ? P3 C39 1.820(4) . ? P3 C45 1.890(4) . ? P4 C53 1.815(3) . ? P4 C59 1.821(4) . ? P4 C52 1.881(4) . ? O1 C13 1.214(5) . ? O2 C20 1.206(5) . ? O3 C45 1.201(5) . ? O4 C52 1.208(4) . ? C1 C6 1.378(5) . ? C1 C2 1.386(6) . ? C2 C3 1.386(6) . ? C2 H2 0.9500 . ? C3 C4 1.372(7) . ? C3 H3 0.9500 . ? C4 C5 1.374(8) . ? C4 H4 0.9500 . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.396(5) . ? C7 C8 1.396(5) . ? C8 C9 1.388(6) . ? C8 H8 0.9500 . ? C9 C10 1.383(6) . ? C9 H9 0.9500 . ? C10 C11 1.384(7) . ? C10 H10 0.9500 . ? C11 C12 1.379(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.487(5) . ? C14 C19 1.379(5) . ? C14 C15 1.399(5) . ? C15 C16 1.389(6) . ? C15 H15 0.9500 . ? C16 C17 1.387(6) . ? C16 H16 0.9500 . ? C17 C18 1.381(6) . ? C17 H17 0.9500 . ? C18 C19 1.397(5) . ? C18 C20 1.485(5) . ? C19 H19 0.9500 . ? C21 C22 1.393(5) . ? C21 C26 1.396(5) . ? C22 C23 1.385(6) . ? C22 H22 0.9500 . ? C23 C24 1.381(6) . ? C23 H23 0.9500 . ? C24 C25 1.380(5) . ? C24 H24 0.9500 . ? C25 C26 1.393(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.390(5) . ? C27 C32 1.395(6) . ? C28 C29 1.389(5) . ? C28 H28 0.9500 . ? C29 C30 1.382(8) . ? C29 H29 0.9500 . ? C30 C31 1.383(7) . ? C30 H30 0.9500 . ? C31 C32 1.401(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.394(5) . ? C33 C34 1.396(6) . ? C34 C35 1.384(5) . ? C34 H34 0.9500 . ? C35 C36 1.379(6) . ? C35 H35 0.9500 . ? C36 C37 1.363(7) . ? C36 H36 0.9500 . ? C37 C38 1.397(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.375(6) . ? C39 C44 1.402(5) . ? C40 C41 1.386(6) . ? C40 H40 0.9500 . ? C41 C42 1.386(6) . ? C41 H41 0.9500 . ? C42 C43 1.369(6) . ? C42 H42 0.9500 . ? C43 C44 1.392(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.493(6) . ? C46 C47 1.394(5) . ? C46 C51 1.399(5) . ? C47 C48 1.374(6) . ? C47 H47 0.9500 . ? C48 C49 1.383(6) . ? C48 H48 0.9500 . ? C49 C50 1.396(5) . ? C49 H49 0.9500 . ? C50 C51 1.384(5) . ? C50 C52 1.495(5) . ? C51 H51 0.9500 . ? C53 C58 1.382(5) . ? C53 C54 1.400(6) . ? C54 C55 1.396(5) . ? C54 H54 0.9500 . ? C55 C56 1.367(8) . ? C55 H55 0.9500 . ? C56 C57 1.372(7) . ? C56 H56 0.9500 . ? C57 C58 1.385(5) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C64 1.396(5) . ? C59 C60 1.401(5) . ? C60 C61 1.380(6) . ? C60 H60 0.9500 . ? C61 C62 1.399(6) . ? C61 H61 0.9500 . ? C62 C63 1.373(5) . ? C62 H62 0.9500 . ? C63 C64 1.372(6) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? N1 C65 1.102(8) . ? C65 C66 1.483(9) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? N2 C67 1.103(7) . ? C67 C68 1.480(9) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? N3 C69 1.120(6) . ? C69 C70 1.452(6) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? N4 C71 1.124(6) . ? C71 C72 1.461(6) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu1 P4 111.09(4) . . ? P1 Cu1 Cl2 116.00(4) . . ? P4 Cu1 Cl2 112.88(4) . . ? P1 Cu1 Cl1 108.35(4) . . ? P4 Cu1 Cl1 111.15(4) . . ? Cl2 Cu1 Cl1 96.35(3) . . ? P3 Cu2 P2 111.35(4) . . ? P3 Cu2 Cl2 115.65(4) . . ? P2 Cu2 Cl2 113.11(4) . . ? P3 Cu2 Cl1 108.08(4) . . ? P2 Cu2 Cl1 111.44(4) . . ? Cl2 Cu2 Cl1 96.14(3) . . ? Cu1 Cl1 Cu2 82.96(2) . . ? Cu1 Cl2 Cu2 84.55(2) . . ? C7 P1 C1 107.64(18) . . ? C7 P1 C13 97.65(18) . . ? C1 P1 C13 99.38(18) . . ? C7 P1 Cu1 118.31(13) . . ? C1 P1 Cu1 109.15(13) . . ? C13 P1 Cu1 122.40(11) . . ? C21 P2 C27 103.92(17) . . ? C21 P2 C20 99.06(17) . . ? C27 P2 C20 101.60(18) . . ? C21 P2 Cu2 118.40(13) . . ? C27 P2 Cu2 115.12(13) . . ? C20 P2 Cu2 116.16(13) . . ? C33 P3 C39 107.04(18) . . ? C33 P3 C45 98.82(19) . . ? C39 P3 C45 98.67(19) . . ? C33 P3 Cu2 108.89(13) . . ? C39 P3 Cu2 117.38(14) . . ? C45 P3 Cu2 123.64(12) . . ? C53 P4 C59 104.69(17) . . ? C53 P4 C52 100.72(17) . . ? C59 P4 C52 99.05(18) . . ? C53 P4 Cu1 114.33(13) . . ? C59 P4 Cu1 118.66(13) . . ? C52 P4 Cu1 116.78(13) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 P1 125.0(3) . . ? C2 C1 P1 115.4(3) . . ? C1 C2 C3 120.3(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.1(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 119.8(5) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C12 C7 C8 119.1(4) . . ? C12 C7 P1 121.8(3) . . ? C8 C7 P1 119.1(3) . . ? C9 C8 C7 120.1(4) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 120.2(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 120.4(4) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? O1 C13 C14 122.0(4) . . ? O1 C13 P1 121.8(3) . . ? C14 C13 P1 116.1(3) . . ? C19 C14 C15 120.4(4) . . ? C19 C14 C13 120.7(3) . . ? C15 C14 C13 118.8(3) . . ? C16 C15 C14 119.1(4) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 119.8(3) . . ? C17 C18 C20 118.3(3) . . ? C19 C18 C20 121.9(4) . . ? C14 C19 C18 119.9(4) . . ? C14 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? O2 C20 C18 121.8(4) . . ? O2 C20 P2 121.7(3) . . ? C18 C20 P2 116.5(3) . . ? C22 C21 C26 119.2(4) . . ? C22 C21 P2 121.3(3) . . ? C26 C21 P2 119.5(3) . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.4(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.5(4) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C21 120.5(4) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 119.8(4) . . ? C28 C27 P2 120.7(3) . . ? C32 C27 P2 119.3(3) . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 120.1(5) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 119.8(4) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C32 120.8(4) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C27 C32 C31 119.1(4) . . ? C27 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C38 C33 C34 119.0(4) . . ? C38 C33 P3 125.5(3) . . ? C34 C33 P3 115.5(3) . . ? C35 C34 C33 120.9(4) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C34 119.3(4) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C37 C36 C35 120.8(4) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 120.7(4) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C33 C38 C37 119.3(4) . . ? C33 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C40 C39 C44 119.8(4) . . ? C40 C39 P3 118.8(3) . . ? C44 C39 P3 121.4(3) . . ? C39 C40 C41 120.5(4) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C40 C41 C42 119.5(4) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 120.7(4) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 119.4(4) . . ? C43 C44 H44 120.3 . . ? C39 C44 H44 120.3 . . ? O3 C45 C46 121.3(4) . . ? O3 C45 P3 122.3(3) . . ? C46 C45 P3 116.3(3) . . ? C47 C46 C51 119.9(4) . . ? C47 C46 C45 119.8(3) . . ? C51 C46 C45 120.2(4) . . ? C48 C47 C46 120.3(4) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C49 120.3(4) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C48 C49 C50 119.6(4) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C51 C50 C49 120.7(3) . . ? C51 C50 C52 121.5(4) . . ? C49 C50 C52 117.8(3) . . ? C50 C51 C46 119.0(4) . . ? C50 C51 H51 120.5 . . ? C46 C51 H51 120.5 . . ? O4 C52 C50 121.6(4) . . ? O4 C52 P4 121.7(3) . . ? C50 C52 P4 116.7(3) . . ? C58 C53 C54 118.9(3) . . ? C58 C53 P4 119.5(3) . . ? C54 C53 P4 121.5(3) . . ? C55 C54 C53 119.8(4) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C56 C55 C54 120.3(5) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C57 120.0(4) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C56 C57 C58 120.7(4) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C53 C58 C57 120.3(4) . . ? C53 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C64 C59 C60 119.0(4) . . ? C64 C59 P4 119.8(3) . . ? C60 C59 P4 121.2(3) . . ? C61 C60 C59 119.9(4) . . ? C61 C60 H60 120.1 . . ? C59 C60 H60 120.1 . . ? C60 C61 C62 120.1(4) . . ? C60 C61 H61 119.9 . . ? C62 C61 H61 119.9 . . ? C63 C62 C61 119.9(4) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C64 C63 C62 120.4(4) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C59 120.6(4) . . ? C63 C64 H64 119.7 . . ? C59 C64 H64 119.7 . . ? N1 C65 C66 179.2(8) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N2 C67 C68 179.2(7) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N3 C69 C70 179.3(6) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N4 C71 C72 179.3(5) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.762 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 934909' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb408_0m #TrackingRef '12 MSB408_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m-Diiodobis(\m-(3-diphenylphosphanecarbonylphenyl)- diphenylphosphanylmethanone)dicopper(I) tetrahydrofuran solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H48 Cu2 I2 O4 P4, C4 H8 0' _chemical_formula_sum 'C68 H56 Cu2 I2 O5 P4' _chemical_formula_weight 1457.89 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0999(19) _cell_length_b 29.083(4) _cell_length_c 18.143(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.317(2) _cell_angle_gamma 90.00 _cell_volume 6482.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9996 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.94 _exptl_crystal_description Column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 1.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7712 _exptl_absorpt_correction_T_max 0.9112 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; The diffraction data were collected in three sets of 363 frames (0.5 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 50 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54692 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.10 _reflns_number_total 14289 _reflns_number_gt 10308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.99 \%A) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. The phenyl group consisting of C7 - C12 is disordered over two approximately equal sites. The disorder was modeled by refining the two sites as rigid groups of isealized geometry. In addition to the ordered molecule of solvent THF there appeared another one in difference maps near the end of the refinement which appeared to be disordered over two sites. Various attempts to refine a 2-site model using various restraints and constraints proved unsatisfactory so the residual density at this site was removed with the SQUEEZE option of PLATON (Spek, 2009). ; _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^)+(0.0356P)^2^+10.1897P] 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 14289 _refine_ls_number_parameters 718 _refine_ls_number_restraints 187 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.093 _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 I1 I 0.67207(3) 0.128804(10) 0.137251(16) 0.03057(8) Uani 1 1 d . . . I2 I 0.81519(2) 0.129199(9) 0.385683(16) 0.02614(8) Uani 1 1 d . . . Cu1 Cu 0.80089(4) 0.178040(17) 0.25843(3) 0.02407(12) Uani 1 1 d . A . Cu2 Cu 0.68685(4) 0.080390(18) 0.26658(3) 0.02599(13) Uani 1 1 d . . . P1 P 0.97719(9) 0.18545(4) 0.26371(7) 0.0255(2) Uani 1 1 d D . . P2 P 0.75377(10) 0.01018(4) 0.25074(7) 0.0282(3) Uani 1 1 d . . . P3 P 0.72107(10) 0.24877(4) 0.24914(7) 0.0273(3) Uani 1 1 d . . . P4 P 0.52390(10) 0.07506(5) 0.28632(8) 0.0349(3) Uani 1 1 d . . . O1 O 1.1667(3) 0.15803(11) 0.3720(2) 0.0372(8) Uani 1 1 d . . . O2 O 0.8491(3) -0.02078(13) 0.1469(2) 0.0551(11) Uani 1 1 d . . . O3 O 0.5225(3) 0.28088(14) 0.1542(2) 0.0586(11) Uani 1 1 d . . . O4 O 0.4709(4) 0.10647(15) 0.4092(2) 0.0612(12) Uani 1 1 d . . . C1 C 1.0068(4) 0.18815(16) 0.1731(3) 0.0362(12) Uani 1 1 d . A . C2 C 1.1120(5) 0.18396(19) 0.1718(3) 0.0459(14) Uani 1 1 d U . . H2 H 1.1701 0.1764 0.2187 0.055 Uiso 1 1 calc R A . C3 C 1.1330(6) 0.1908(2) 0.1028(4) 0.0661(19) Uani 1 1 d U A . H3 H 1.2049 0.1875 0.1024 0.079 Uiso 1 1 calc R . . C4 C 1.0501(6) 0.2021(3) 0.0353(4) 0.076(2) Uani 1 1 d U . . H4 H 1.0647 0.2070 -0.0118 0.091 Uiso 1 1 calc R A . C5 C 0.9452(6) 0.2066(3) 0.0352(4) 0.079(2) Uani 1 1 d U A . H5 H 0.8878 0.2148 -0.0117 0.095 Uiso 1 1 calc R . . C6 C 0.9235(5) 0.1989(2) 0.1050(3) 0.0529(15) Uani 1 1 d U . . H6 H 0.8511 0.2011 0.1048 0.063 Uiso 1 1 calc R A . C7 C 1.0383(3) 0.23859(9) 0.3212(2) 0.0352(12) Uani 0.50 1 d PGD A 1 C8 C 1.1076(3) 0.26899(12) 0.3027(2) 0.0469(16) Uani 0.50 1 d PGU A 1 H8 H 1.1242 0.2646 0.2561 0.056 Uiso 0.50 1 calc PR A 1 C9 C 1.1527(3) 0.30578(11) 0.3522(3) 0.052(2) Uani 0.50 1 d PGU A 1 H9 H 1.2001 0.3266 0.3395 0.062 Uiso 0.50 1 calc PR A 1 C10 C 1.1286(3) 0.31216(12) 0.4202(3) 0.063(2) Uani 0.50 1 d PGU A 1 H10 H 1.1594 0.3373 0.4541 0.076 Uiso 0.50 1 calc PR A 1 C11 C 1.0593(4) 0.28176(15) 0.43881(19) 0.062(2) Uani 0.50 1 d PGU A 1 H11 H 1.0427 0.2861 0.4853 0.075 Uiso 0.50 1 calc PR A 1 C12 C 1.0142(3) 0.24497(12) 0.3893(2) 0.0472(15) Uani 0.50 1 d PGU A 1 H12 H 0.9668 0.2242 0.4020 0.057 Uiso 0.50 1 calc PR A 1 C7A C 1.0364(3) 0.23721(10) 0.3127(2) 0.0352(12) Uani 0.50 1 d PGD A 2 C8A C 1.0942(3) 0.26714(13) 0.2821(2) 0.0469(16) Uani 0.50 1 d PGU A 2 H8A H 1.1023 0.2605 0.2331 0.056 Uiso 0.50 1 calc PR A 2 C9A C 1.1401(3) 0.30675(12) 0.3231(3) 0.052(2) Uani 0.50 1 d PGU A 2 H9A H 1.1797 0.3272 0.3022 0.062 Uiso 0.50 1 calc PR A 2 C10A C 1.1283(3) 0.31643(10) 0.3947(3) 0.063(2) Uani 0.50 1 d PGU A 2 H10A H 1.1597 0.3435 0.4227 0.076 Uiso 0.50 1 calc PR A 2 C11A C 1.0704(3) 0.28650(13) 0.42530(19) 0.062(2) Uani 0.50 1 d PGU A 2 H11A H 1.0623 0.2931 0.4742 0.075 Uiso 0.50 1 calc PR A 2 C12A C 1.0245(3) 0.24689(11) 0.3843(2) 0.0472(15) Uani 0.50 1 d PGU A 2 H12A H 0.9849 0.2264 0.4052 0.057 Uiso 0.50 1 calc PR A 2 C13 C 1.0855(4) 0.14325(15) 0.3221(3) 0.0285(10) Uani 1 1 d . A . C14 C 1.0731(4) 0.09298(15) 0.3068(3) 0.0276(10) Uani 1 1 d . . . C15 C 1.1645(4) 0.06531(16) 0.3381(3) 0.0391(12) Uani 1 1 d . A . H15 H 1.2317 0.0786 0.3697 0.047 Uiso 1 1 calc R . . C16 C 1.1579(5) 0.01830(18) 0.3236(4) 0.0507(15) Uani 1 1 d . . . H16 H 1.2201 -0.0007 0.3455 0.061 Uiso 1 1 calc R A . C17 C 1.0584(5) -0.00089(17) 0.2762(4) 0.0490(15) Uani 1 1 d . A . H17 H 1.0543 -0.0327 0.2639 0.059 Uiso 1 1 calc R . . C18 C 0.9668(4) 0.02602(15) 0.2475(3) 0.0344(11) Uani 1 1 d . . . C19 C 0.9736(4) 0.07368(14) 0.2622(3) 0.0288(10) Uani 1 1 d . A . H19 H 0.9108 0.0925 0.2418 0.035 Uiso 1 1 calc R . . C20 C 0.8615(4) 0.00305(15) 0.2035(3) 0.0353(11) Uani 1 1 d . A . C21 C 0.8210(4) -0.02609(15) 0.3359(3) 0.0293(10) Uani 1 1 d . . . C22 C 0.8468(5) -0.00859(18) 0.4103(3) 0.0454(14) Uani 1 1 d . . . H22 H 0.8346 0.0230 0.4180 0.054 Uiso 1 1 calc R . . C23 C 0.8913(6) -0.0378(2) 0.4749(3) 0.0617(18) Uani 1 1 d . . . H23 H 0.9074 -0.0260 0.5265 0.074 Uiso 1 1 calc R . . C24 C 0.9118(4) -0.08258(19) 0.4647(3) 0.0480(14) Uani 1 1 d . . . H24 H 0.9414 -0.1020 0.5091 0.058 Uiso 1 1 calc R . . C25 C 0.8902(5) -0.09973(18) 0.3911(3) 0.0499(15) Uani 1 1 d . . . H25 H 0.9051 -0.1310 0.3838 0.060 Uiso 1 1 calc R . . C26 C 0.8470(5) -0.07170(17) 0.3279(3) 0.0520(16) Uani 1 1 d . . . H26 H 0.8342 -0.0837 0.2768 0.062 Uiso 1 1 calc R . . C27 C 0.6464(4) -0.02652(16) 0.1882(3) 0.0390(12) Uani 1 1 d . . . C28 C 0.6105(5) -0.02193(17) 0.1078(3) 0.0452(14) Uani 1 1 d U . . H28 H 0.6452 -0.0003 0.0851 0.054 Uiso 1 1 calc R . . C29 C 0.5260(6) -0.04782(19) 0.0593(3) 0.0627(18) Uani 1 1 d U . . H29 H 0.5034 -0.0443 0.0039 0.075 Uiso 1 1 calc R . . C30 C 0.4757(6) -0.0781(2) 0.0909(4) 0.076(2) Uani 1 1 d U . . H30 H 0.4177 -0.0963 0.0576 0.091 Uiso 1 1 calc R . . C31 C 0.5075(6) -0.0830(2) 0.1705(4) 0.080(2) Uani 1 1 d U . . H31 H 0.4706 -0.1043 0.1921 0.096 Uiso 1 1 calc R . . C32 C 0.5931(5) -0.05719(19) 0.2206(3) 0.0581(17) Uani 1 1 d U . . H32 H 0.6146 -0.0606 0.2760 0.070 Uiso 1 1 calc R . . C33 C 0.7448(4) 0.28351(15) 0.3377(3) 0.0317(11) Uani 1 1 d . A . C34 C 0.7828(5) 0.26285(18) 0.4110(3) 0.0475(14) Uani 1 1 d U . . H34 H 0.7932 0.2305 0.4149 0.057 Uiso 1 1 calc R A . C35 C 0.8058(6) 0.2889(2) 0.4786(3) 0.0618(18) Uani 1 1 d U A . H35 H 0.8316 0.2743 0.5286 0.074 Uiso 1 1 calc R . . C36 C 0.7913(5) 0.33607(19) 0.4739(3) 0.0529(15) Uani 1 1 d U . . H36 H 0.8102 0.3539 0.5206 0.063 Uiso 1 1 calc R A . C37 C 0.7495(5) 0.35716(18) 0.4017(3) 0.0450(13) Uani 1 1 d U A . H37 H 0.7371 0.3894 0.3982 0.054 Uiso 1 1 calc R . . C38 C 0.7256(4) 0.33080(16) 0.3337(3) 0.0395(12) Uani 1 1 d U . . H38 H 0.6957 0.3452 0.2838 0.047 Uiso 1 1 calc R A . C39 C 0.7622(4) 0.28459(15) 0.1820(3) 0.0303(10) Uani 1 1 d . A . C40 C 0.8482(4) 0.31579(16) 0.2079(3) 0.0316(10) Uani 1 1 d . . . H40 H 0.8836 0.3210 0.2625 0.038 Uiso 1 1 calc R A . C41 C 0.8821(4) 0.33905(17) 0.1541(3) 0.0373(12) Uani 1 1 d . A . H41 H 0.9405 0.3604 0.1720 0.045 Uiso 1 1 calc R . . C42 C 0.8312(4) 0.33153(17) 0.0737(3) 0.0408(12) Uani 1 1 d . . . H42 H 0.8540 0.3480 0.0369 0.049 Uiso 1 1 calc R A . C43 C 0.7482(5) 0.30015(17) 0.0481(3) 0.0434(13) Uani 1 1 d . A . H43 H 0.7144 0.2944 -0.0065 0.052 Uiso 1 1 calc R . . C44 C 0.7134(4) 0.27691(17) 0.1014(3) 0.0391(12) Uani 1 1 d . . . H44 H 0.6555 0.2554 0.0830 0.047 Uiso 1 1 calc R A . C45 C 0.5681(4) 0.25641(17) 0.2096(3) 0.0391(12) Uani 1 1 d . A . C46 C 0.5083(4) 0.23351(18) 0.2563(3) 0.0382(12) Uani 1 1 d . . . C47 C 0.4349(4) 0.2592(2) 0.2788(3) 0.0520(15) Uani 1 1 d . A . H47 H 0.4201 0.2901 0.2615 0.062 Uiso 1 1 calc R . . C48 C 0.3828(5) 0.2400(2) 0.3265(4) 0.0599(18) Uani 1 1 d . . . H48 H 0.3347 0.2582 0.3434 0.072 Uiso 1 1 calc R A . C49 C 0.4013(4) 0.1950(2) 0.3490(3) 0.0519(15) Uani 1 1 d . A . H49 H 0.3656 0.1819 0.3815 0.062 Uiso 1 1 calc R . . C50 C 0.4714(4) 0.16815(18) 0.3249(3) 0.0371(12) Uani 1 1 d . . . C51 C 0.5257(4) 0.18758(17) 0.2783(3) 0.0338(11) Uani 1 1 d . A . H51 H 0.5742 0.1695 0.2619 0.041 Uiso 1 1 calc R . . C52 C 0.4857(4) 0.11908(19) 0.3501(3) 0.0420(13) Uani 1 1 d . A . C53 C 0.3998(4) 0.07396(16) 0.2002(3) 0.0366(12) Uani 1 1 d . . . C54 C 0.2972(5) 0.0830(2) 0.2050(4) 0.0561(16) Uani 1 1 d . . . H54 H 0.2922 0.0935 0.2533 0.067 Uiso 1 1 calc R . . C55 C 0.2035(5) 0.0771(2) 0.1411(4) 0.0623(18) Uani 1 1 d . . . H55 H 0.1346 0.0841 0.1447 0.075 Uiso 1 1 calc R . . C56 C 0.2107(5) 0.06085(19) 0.0721(4) 0.0582(18) Uani 1 1 d . . . H56 H 0.1461 0.0556 0.0283 0.070 Uiso 1 1 calc R . . C57 C 0.3099(5) 0.05208(18) 0.0655(4) 0.0514(15) Uani 1 1 d . . . H57 H 0.3142 0.0416 0.0171 0.062 Uiso 1 1 calc R . . C58 C 0.4050(4) 0.05877(17) 0.1307(3) 0.0417(13) Uani 1 1 d . . . H58 H 0.4739 0.0526 0.1263 0.050 Uiso 1 1 calc R . . C59 C 0.5137(4) 0.02301(18) 0.3395(3) 0.0416(13) Uani 1 1 d . . . C60 C 0.5926(5) 0.0151(2) 0.4119(3) 0.0521(15) Uani 1 1 d U . . H60 H 0.6501 0.0365 0.4335 0.062 Uiso 1 1 calc R . . C61 C 0.5863(6) -0.0255(2) 0.4534(4) 0.0662(19) Uani 1 1 d U . . H61 H 0.6388 -0.0306 0.5042 0.079 Uiso 1 1 calc R . . C62 C 0.5080(6) -0.0569(2) 0.4227(4) 0.0620(18) Uani 1 1 d U . . H62 H 0.5054 -0.0836 0.4522 0.074 Uiso 1 1 calc R . . C63 C 0.4303(6) -0.0508(2) 0.3478(5) 0.077(2) Uani 1 1 d U . . H63 H 0.3767 -0.0736 0.3250 0.093 Uiso 1 1 calc R . . C64 C 0.4336(5) -0.0103(2) 0.3073(4) 0.070(2) Uani 1 1 d U . . H64 H 0.3802 -0.0053 0.2569 0.085 Uiso 1 1 calc R . . O5 O 0.2520(6) 0.3470(2) 0.1961(4) 0.116(2) Uani 1 1 d . . . C65 C 0.3111(8) 0.3793(2) 0.1737(4) 0.081(2) Uani 1 1 d . . . H65A H 0.3898 0.3735 0.2006 0.097 Uiso 1 1 calc R . . H65B H 0.2942 0.4103 0.1890 0.097 Uiso 1 1 calc R . . C66 C 0.1802(8) 0.3245(3) 0.1231(5) 0.102(3) Uani 1 1 d U . . H66A H 0.1733 0.2911 0.1315 0.122 Uiso 1 1 calc R . . H66B H 0.1068 0.3385 0.1047 0.122 Uiso 1 1 calc R . . C67 C 0.2339(7) 0.3323(3) 0.0684(5) 0.091(3) Uani 1 1 d . . . H67A H 0.1813 0.3329 0.0139 0.109 Uiso 1 1 calc R . . H67B H 0.2890 0.3082 0.0726 0.109 Uiso 1 1 calc R . . C68 C 0.2857(7) 0.3774(3) 0.0911(5) 0.091(3) Uani 1 1 d . . . H68A H 0.3524 0.3799 0.0775 0.109 Uiso 1 1 calc R . . H68B H 0.2352 0.4025 0.0647 0.109 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 I1 0.03998(18) 0.02777(16) 0.02140(15) 0.00132(12) 0.00744(13) -0.01121(13) I2 0.03392(16) 0.02085(14) 0.02230(15) -0.00013(11) 0.00804(12) 0.00223(12) Cu1 0.0268(3) 0.0202(3) 0.0261(3) -0.0008(2) 0.0102(2) -0.0005(2) Cu2 0.0285(3) 0.0243(3) 0.0253(3) 0.0018(2) 0.0095(2) -0.0037(2) P1 0.0260(6) 0.0193(5) 0.0339(6) -0.0022(5) 0.0138(5) -0.0004(5) P2 0.0381(7) 0.0182(5) 0.0255(6) -0.0006(5) 0.0074(5) -0.0060(5) P3 0.0302(7) 0.0209(6) 0.0316(6) 0.0029(5) 0.0118(5) 0.0032(5) P4 0.0282(7) 0.0447(8) 0.0321(7) 0.0127(6) 0.0109(6) -0.0056(6) O1 0.036(2) 0.0343(19) 0.0376(19) -0.0023(16) 0.0077(16) 0.0029(16) O2 0.080(3) 0.042(2) 0.050(2) -0.0220(19) 0.033(2) -0.008(2) O3 0.041(2) 0.060(3) 0.068(3) 0.035(2) 0.011(2) 0.012(2) O4 0.078(3) 0.070(3) 0.050(2) 0.020(2) 0.041(2) 0.008(2) C1 0.041(3) 0.031(3) 0.046(3) 0.008(2) 0.026(3) 0.003(2) C2 0.046(3) 0.053(3) 0.048(3) 0.018(3) 0.028(3) 0.019(3) C3 0.063(4) 0.080(4) 0.074(4) 0.025(3) 0.047(3) 0.019(3) C4 0.074(4) 0.107(5) 0.060(4) 0.033(4) 0.042(4) 0.015(4) C5 0.074(4) 0.113(5) 0.057(4) 0.037(4) 0.032(3) 0.010(4) C6 0.047(3) 0.070(4) 0.049(3) 0.020(3) 0.026(3) 0.008(3) C7 0.023(2) 0.020(2) 0.054(3) -0.007(2) 0.003(2) 0.0055(19) C8 0.033(3) 0.029(3) 0.074(4) -0.016(3) 0.013(3) -0.007(2) C9 0.028(3) 0.029(3) 0.080(5) 0.004(3) -0.004(3) 0.002(2) C10 0.056(4) 0.039(3) 0.063(5) -0.003(3) -0.019(3) 0.013(3) C11 0.076(4) 0.040(3) 0.046(3) -0.005(3) -0.010(3) 0.021(3) C12 0.053(3) 0.032(3) 0.041(3) -0.005(2) -0.004(2) 0.009(2) C7A 0.023(2) 0.020(2) 0.054(3) -0.007(2) 0.003(2) 0.0055(19) C8A 0.033(3) 0.029(3) 0.074(4) -0.016(3) 0.013(3) -0.007(2) C9A 0.028(3) 0.029(3) 0.080(5) 0.004(3) -0.004(3) 0.002(2) C10A 0.056(4) 0.039(3) 0.063(5) -0.003(3) -0.019(3) 0.013(3) C11A 0.076(4) 0.040(3) 0.046(3) -0.005(3) -0.010(3) 0.021(3) C12A 0.053(3) 0.032(3) 0.041(3) -0.005(2) -0.004(2) 0.009(2) C13 0.032(3) 0.027(2) 0.032(3) -0.002(2) 0.019(2) -0.001(2) C14 0.034(3) 0.025(2) 0.032(2) 0.0006(19) 0.022(2) 0.0036(19) C15 0.039(3) 0.027(3) 0.057(3) 0.006(2) 0.025(3) 0.004(2) C16 0.041(3) 0.030(3) 0.084(4) 0.001(3) 0.025(3) 0.012(2) C17 0.059(4) 0.022(3) 0.077(4) -0.006(3) 0.038(3) 0.008(2) C18 0.048(3) 0.022(2) 0.041(3) -0.004(2) 0.026(3) 0.000(2) C19 0.038(3) 0.018(2) 0.033(2) 0.0010(19) 0.017(2) 0.0034(19) C20 0.055(3) 0.017(2) 0.036(3) -0.001(2) 0.018(3) 0.000(2) C21 0.036(3) 0.021(2) 0.030(2) 0.0012(19) 0.010(2) -0.0040(19) C22 0.063(4) 0.033(3) 0.032(3) -0.001(2) 0.006(3) 0.007(3) C23 0.088(5) 0.048(4) 0.030(3) 0.008(3) -0.003(3) 0.011(3) C24 0.041(3) 0.040(3) 0.051(3) 0.023(3) 0.000(3) 0.002(3) C25 0.064(4) 0.023(3) 0.055(4) 0.009(2) 0.011(3) 0.003(3) C26 0.083(5) 0.025(3) 0.040(3) -0.002(2) 0.011(3) -0.001(3) C27 0.051(3) 0.025(3) 0.029(3) 0.003(2) -0.001(2) -0.007(2) C28 0.061(3) 0.029(3) 0.034(3) 0.001(2) 0.001(2) -0.003(2) C29 0.087(4) 0.035(3) 0.040(3) 0.006(2) -0.012(3) -0.008(3) C30 0.084(4) 0.050(3) 0.057(4) 0.011(3) -0.023(3) -0.027(3) C31 0.088(5) 0.062(4) 0.060(4) 0.018(3) -0.010(3) -0.044(4) C32 0.063(4) 0.047(3) 0.042(3) 0.014(3) -0.009(3) -0.030(3) C33 0.036(3) 0.024(2) 0.040(3) 0.000(2) 0.019(2) 0.005(2) C34 0.073(4) 0.030(3) 0.044(3) -0.001(2) 0.027(3) 0.016(3) C35 0.108(5) 0.044(3) 0.041(3) 0.000(3) 0.036(3) 0.016(3) C36 0.082(4) 0.042(3) 0.049(3) -0.010(3) 0.040(3) 0.003(3) C37 0.064(4) 0.025(2) 0.056(3) -0.003(2) 0.033(3) 0.000(2) C38 0.055(3) 0.023(2) 0.043(3) 0.001(2) 0.020(3) 0.004(2) C39 0.033(3) 0.020(2) 0.037(3) 0.0026(19) 0.012(2) 0.0047(19) C40 0.032(3) 0.030(2) 0.032(3) -0.003(2) 0.010(2) 0.003(2) C41 0.037(3) 0.032(3) 0.044(3) 0.000(2) 0.015(2) -0.006(2) C42 0.054(3) 0.032(3) 0.037(3) 0.006(2) 0.017(3) -0.003(2) C43 0.060(4) 0.035(3) 0.030(3) 0.000(2) 0.009(3) -0.009(3) C44 0.053(3) 0.031(3) 0.030(3) -0.004(2) 0.010(2) -0.009(2) C45 0.037(3) 0.033(3) 0.043(3) 0.005(2) 0.010(2) 0.006(2) C46 0.024(2) 0.043(3) 0.043(3) 0.005(2) 0.004(2) 0.009(2) C47 0.040(3) 0.060(4) 0.051(3) 0.007(3) 0.009(3) 0.023(3) C48 0.043(3) 0.090(5) 0.050(4) 0.005(3) 0.021(3) 0.032(3) C49 0.032(3) 0.083(5) 0.042(3) 0.013(3) 0.014(3) 0.008(3) C50 0.023(2) 0.052(3) 0.035(3) 0.004(2) 0.007(2) 0.002(2) C51 0.025(2) 0.041(3) 0.038(3) 0.006(2) 0.015(2) 0.003(2) C52 0.030(3) 0.057(4) 0.043(3) 0.011(3) 0.019(2) -0.002(2) C53 0.033(3) 0.028(3) 0.043(3) 0.011(2) 0.006(2) -0.007(2) C54 0.036(3) 0.074(4) 0.056(4) 0.010(3) 0.013(3) -0.004(3) C55 0.027(3) 0.072(5) 0.072(5) 0.004(4) -0.003(3) -0.010(3) C56 0.048(4) 0.038(3) 0.062(4) 0.012(3) -0.014(3) -0.008(3) C57 0.050(4) 0.038(3) 0.053(4) -0.002(3) 0.000(3) -0.005(3) C58 0.041(3) 0.030(3) 0.044(3) 0.005(2) 0.002(3) -0.005(2) C59 0.030(3) 0.047(3) 0.056(3) 0.026(3) 0.026(3) 0.010(2) C60 0.066(4) 0.048(3) 0.037(3) 0.005(2) 0.012(3) 0.016(3) C61 0.099(5) 0.060(4) 0.036(3) 0.013(3) 0.020(3) 0.034(4) C62 0.071(4) 0.066(4) 0.067(4) 0.033(3) 0.047(3) 0.024(3) C63 0.052(4) 0.073(4) 0.109(5) 0.050(4) 0.030(4) 0.000(3) C64 0.043(3) 0.073(4) 0.087(4) 0.052(3) 0.012(3) -0.006(3) O5 0.179(7) 0.088(4) 0.091(4) 0.003(4) 0.059(4) -0.030(4) C65 0.141(8) 0.052(4) 0.058(4) 0.003(3) 0.046(5) -0.028(4) C66 0.151(6) 0.084(5) 0.085(5) -0.014(4) 0.057(5) -0.050(5) C67 0.111(7) 0.095(6) 0.078(5) -0.008(5) 0.046(5) -0.007(5) C68 0.102(7) 0.115(7) 0.074(5) -0.017(5) 0.053(5) -0.029(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.6749(6) . ? I1 Cu2 2.6853(7) . ? I2 Cu2 2.6435(6) . ? I2 Cu1 2.6614(7) . ? Cu1 P3 2.2871(13) . ? Cu1 P1 2.2882(13) . ? Cu2 P2 2.2795(13) . ? Cu2 P4 2.2890(14) . ? P1 C7A 1.783(3) . ? P1 C1 1.817(5) . ? P1 C7 1.881(3) . ? P1 C13 1.897(5) . ? P2 C27 1.815(5) . ? P2 C21 1.824(5) . ? P2 C20 1.899(5) . ? P3 C39 1.820(5) . ? P3 C33 1.831(5) . ? P3 C45 1.892(5) . ? P4 C53 1.823(5) . ? P4 C59 1.824(5) . ? P4 C52 1.905(6) . ? O1 C13 1.211(5) . ? O2 C20 1.202(5) . ? O3 C45 1.207(6) . ? O4 C52 1.211(6) . ? C1 C6 1.372(7) . ? C1 C2 1.392(7) . ? C2 C3 1.387(7) . ? C2 H2 0.9500 . ? C3 C4 1.365(9) . ? C3 H3 0.9500 . ? C4 C5 1.379(9) . ? C4 H4 0.9500 . ? C5 C6 1.408(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C8 H8 0.9500 . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C7A C8A 1.3900 . ? C7A C12A 1.3901 . ? C8A C9A 1.3900 . ? C8A H8A 0.9500 . ? C9A C10A 1.3900 . ? C9A H9A 0.9500 . ? C10A C11A 1.3900 . ? C10A H10A 0.9500 . ? C11A C12A 1.3900 . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13 C14 1.487(6) . ? C14 C15 1.389(6) . ? C14 C19 1.391(6) . ? C15 C16 1.389(7) . ? C15 H15 0.9500 . ? C16 C17 1.404(8) . ? C16 H16 0.9500 . ? C17 C18 1.374(7) . ? C17 H17 0.9500 . ? C18 C19 1.408(6) . ? C18 C20 1.491(7) . ? C19 H19 0.9500 . ? C21 C22 1.372(7) . ? C21 C26 1.389(7) . ? C22 C23 1.399(7) . ? C22 H22 0.9500 . ? C23 C24 1.356(8) . ? C23 H23 0.9500 . ? C24 C25 1.360(8) . ? C24 H24 0.9500 . ? C25 C26 1.359(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.376(7) . ? C27 C32 1.383(7) . ? C28 C29 1.375(8) . ? C28 H28 0.9500 . ? C29 C30 1.341(9) . ? C29 H29 0.9500 . ? C30 C31 1.366(9) . ? C30 H30 0.9500 . ? C31 C32 1.392(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.385(7) . ? C33 C38 1.396(6) . ? C34 C35 1.384(7) . ? C34 H34 0.9500 . ? C35 C36 1.383(8) . ? C35 H35 0.9500 . ? C36 C37 1.377(8) . ? C36 H36 0.9500 . ? C37 C38 1.392(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.395(6) . ? C39 C44 1.396(6) . ? C40 C41 1.381(7) . ? C40 H40 0.9500 . ? C41 C42 1.394(7) . ? C41 H41 0.9500 . ? C42 C43 1.372(7) . ? C42 H42 0.9500 . ? C43 C44 1.380(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.495(7) . ? C46 C47 1.385(7) . ? C46 C51 1.391(7) . ? C47 C48 1.391(8) . ? C47 H47 0.9500 . ? C48 C49 1.370(8) . ? C48 H48 0.9500 . ? C49 C50 1.386(7) . ? C49 H49 0.9500 . ? C50 C51 1.398(7) . ? C50 C52 1.490(7) . ? C51 H51 0.9500 . ? C53 C58 1.359(7) . ? C53 C54 1.403(7) . ? C54 C55 1.376(8) . ? C54 H54 0.9500 . ? C55 C56 1.372(9) . ? C55 H55 0.9500 . ? C56 C57 1.370(9) . ? C56 H56 0.9500 . ? C57 C58 1.403(7) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.380(7) . ? C59 C64 1.399(8) . ? C60 C61 1.420(8) . ? C60 H60 0.9500 . ? C61 C62 1.342(9) . ? C61 H61 0.9500 . ? C62 C63 1.398(9) . ? C62 H62 0.9500 . ? C63 C64 1.397(8) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? O5 C65 1.365(8) . ? O5 C66 1.485(9) . ? C65 C68 1.418(9) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.421(10) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.470(10) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 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 Cu1 I1 Cu2 74.28(2) . . ? Cu2 I2 Cu1 75.18(2) . . ? P3 Cu1 P1 110.33(5) . . ? P3 Cu1 I2 115.88(4) . . ? P1 Cu1 I2 104.36(4) . . ? P3 Cu1 I1 106.21(4) . . ? P1 Cu1 I1 115.11(4) . . ? I2 Cu1 I1 105.16(2) . . ? P2 Cu2 P4 112.30(5) . . ? P2 Cu2 I2 114.89(4) . . ? P4 Cu2 I2 105.75(4) . . ? P2 Cu2 I1 105.89(4) . . ? P4 Cu2 I1 112.58(4) . . ? I2 Cu2 I1 105.38(2) . . ? C7A P1 C1 102.8(2) . . ? C1 P1 C7 106.4(2) . . ? C7A P1 C13 99.00(19) . . ? C1 P1 C13 100.4(2) . . ? C7 P1 C13 97.45(18) . . ? C7A P1 Cu1 111.00(12) . . ? C1 P1 Cu1 119.72(18) . . ? C7 P1 Cu1 109.26(11) . . ? C13 P1 Cu1 120.73(15) . . ? C27 P2 C21 103.3(2) . . ? C27 P2 C20 100.9(2) . . ? C21 P2 C20 95.9(2) . . ? C27 P2 Cu2 110.92(18) . . ? C21 P2 Cu2 120.32(15) . . ? C20 P2 Cu2 122.22(14) . . ? C39 P3 C33 105.8(2) . . ? C39 P3 C45 101.5(2) . . ? C33 P3 C45 95.9(2) . . ? C39 P3 Cu1 109.29(15) . . ? C33 P3 Cu1 119.86(16) . . ? C45 P3 Cu1 122.04(16) . . ? C53 P4 C59 103.4(2) . . ? C53 P4 C52 100.9(2) . . ? C59 P4 C52 98.9(2) . . ? C53 P4 Cu2 118.01(18) . . ? C59 P4 Cu2 112.48(16) . . ? C52 P4 Cu2 120.34(17) . . ? C6 C1 C2 119.2(5) . . ? C6 C1 P1 118.1(4) . . ? C2 C1 P1 122.4(4) . . ? C3 C2 C1 120.7(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 119.9(6) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.4(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 120.0(6) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 125.2(2) . . ? C12 C7 P1 114.7(2) . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C8A C7A C12A 120.0 . . ? C8A C7A P1 122.2(2) . . ? C12A C7A P1 117.8(2) . . ? C9A C8A C7A 120.0 . . ? C9A C8A H8A 120.0 . . ? C7A C8A H8A 120.0 . . ? C8A C9A C10A 120.0 . . ? C8A C9A H9A 120.0 . . ? C10A C9A H9A 120.0 . . ? C9A C10A C11A 120.0 . . ? C9A C10A H10A 120.0 . . ? C11A C10A H10A 120.0 . . ? C12A C11A C10A 120.0 . . ? C12A C11A H11A 120.0 . . ? C10A C11A H11A 120.0 . . ? C11A C12A C7A 120.0 . . ? C11A C12A H12A 120.0 . . ? C7A C12A H12A 120.0 . . ? O1 C13 C14 119.9(4) . . ? O1 C13 P1 118.7(3) . . ? C14 C13 P1 121.3(3) . . ? C15 C14 C19 120.3(4) . . ? C15 C14 C13 118.1(4) . . ? C19 C14 C13 121.7(4) . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.4(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 120.6(5) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.9(5) . . ? C17 C18 C20 118.1(4) . . ? C19 C18 C20 121.9(4) . . ? C14 C19 C18 119.5(4) . . ? C14 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? O2 C20 C18 122.7(5) . . ? O2 C20 P2 123.2(4) . . ? C18 C20 P2 113.9(3) . . ? C22 C21 C26 118.1(5) . . ? C22 C21 P2 120.0(4) . . ? C26 C21 P2 121.9(4) . . ? C21 C22 C23 119.2(5) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 120.9(5) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.4(5) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C21 122.1(5) . . ? C25 C26 H26 119.0 . . ? C21 C26 H26 119.0 . . ? C28 C27 C32 118.4(5) . . ? C28 C27 P2 120.7(4) . . ? C32 C27 P2 120.6(4) . . ? C29 C28 C27 121.9(5) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C30 C29 C28 119.5(6) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.3(6) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C32 121.0(6) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C27 C32 C31 118.8(5) . . ? C27 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C34 C33 C38 118.4(5) . . ? C34 C33 P3 119.9(4) . . ? C38 C33 P3 121.7(4) . . ? C35 C34 C33 120.6(5) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 120.1(5) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 119.4(5) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C37 C38 C33 121.1(5) . . ? C37 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? C40 C39 C44 118.6(4) . . ? C40 C39 P3 122.7(4) . . ? C44 C39 P3 118.4(4) . . ? C41 C40 C39 120.1(4) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.5(5) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 119.6(5) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.3(5) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 120.9(5) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? O3 C45 C46 122.0(5) . . ? O3 C45 P3 122.5(4) . . ? C46 C45 P3 115.3(3) . . ? C47 C46 C51 119.6(5) . . ? C47 C46 C45 118.8(5) . . ? C51 C46 C45 121.7(4) . . ? C46 C47 C48 120.6(6) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C47 119.6(5) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 120.9(5) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C49 C50 C51 119.6(5) . . ? C49 C50 C52 118.0(5) . . ? C51 C50 C52 122.4(5) . . ? C46 C51 C50 119.7(5) . . ? C46 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? O4 C52 C50 121.3(5) . . ? O4 C52 P4 119.4(4) . . ? C50 C52 P4 119.3(4) . . ? C58 C53 C54 118.5(5) . . ? C58 C53 P4 118.9(4) . . ? C54 C53 P4 122.1(4) . . ? C55 C54 C53 121.1(6) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C56 C55 C54 119.3(6) . . ? C56 C55 H55 120.4 . . ? C54 C55 H55 120.4 . . ? C57 C56 C55 120.8(6) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 119.4(6) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C53 C58 C57 120.8(5) . . ? C53 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C60 C59 C64 119.1(5) . . ? C60 C59 P4 118.3(4) . . ? C64 C59 P4 122.5(4) . . ? C59 C60 C61 118.8(6) . . ? C59 C60 H60 120.6 . . ? C61 C60 H60 120.6 . . ? C62 C61 C60 121.5(6) . . ? C62 C61 H61 119.2 . . ? C60 C61 H61 119.2 . . ? C61 C62 C63 120.7(6) . . ? C61 C62 H62 119.6 . . ? C63 C62 H62 119.6 . . ? C64 C63 C62 118.3(7) . . ? C64 C63 H63 120.9 . . ? C62 C63 H63 120.9 . . ? C63 C64 C59 121.4(6) . . ? C63 C64 H64 119.3 . . ? C59 C64 H64 119.3 . . ? C65 O5 C66 106.7(6) . . ? O5 C65 C68 109.8(7) . . ? O5 C65 H65A 109.7 . . ? C68 C65 H65A 109.7 . . ? O5 C65 H65B 109.7 . . ? C68 C65 H65B 109.7 . . ? H65A C65 H65B 108.2 . . ? C67 C66 O5 103.8(7) . . ? C67 C66 H66A 111.0 . . ? O5 C66 H66A 111.0 . . ? C67 C66 H66B 111.0 . . ? O5 C66 H66B 111.0 . . ? H66A C66 H66B 109.0 . . ? C66 C67 C68 103.8(7) . . ? C66 C67 H67A 111.0 . . ? C68 C67 H67A 111.0 . . ? C66 C67 H67B 111.0 . . ? C68 C67 H67B 111.0 . . ? H67A C67 H67B 109.0 . . ? C65 C68 C67 104.3(7) . . ? C65 C68 H68A 110.9 . . ? C67 C68 H68A 110.9 . . ? C65 C68 H68B 110.9 . . ? C67 C68 H68B 110.9 . . ? H68A C68 H68B 108.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.881 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.105 _database_code_depnum_ccdc_archive 'CCDC 934910' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_msb487a_0m #TrackingRef '14 MSB487a_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H48 Ag2 Cl2 O8 P4), 3(C H2 Cl2)' _chemical_formula_sum 'C131 H102 Ag4 Cl10 O16 P8' _chemical_formula_weight 2965.86 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.296(3) _cell_length_b 29.654(7) _cell_length_c 15.474(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.318(3) _cell_angle_gamma 90.00 _cell_volume 6409(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9870 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.06 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2988 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6486 _exptl_absorpt_correction_T_max 0.9175 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 60 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53590 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.14 _reflns_number_total 14041 _reflns_number_gt 10252 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)' _computing_cell_refinement 'Bruker SAINT (Bruker-AXS, 2009)' _computing_data_reduction 'Bruker SAINT (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS, 2008)' _computing_publication_material 'Bruker SHELXTL(Bruker-AXS, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.99 \%A) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. Two of the phenyl rings are disordered and were refined as rigid groups in two alternate locations each. ; _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^)+(0.0546P)^2^+22.0977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 14041 _refine_ls_number_parameters 759 _refine_ls_number_restraints 146 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.28089(3) 0.779923(12) 0.29540(2) 0.02344(10) Uani 1 1 d . A . Ag2 Ag 0.27286(3) 0.903302(12) 0.23852(3) 0.02330(10) Uani 1 1 d . A . Cl1 Cl 0.20688(10) 0.83123(4) 0.16326(8) 0.0296(3) Uani 1 1 d . . . Cl2 Cl 0.39393(9) 0.85926(4) 0.44987(8) 0.0237(2) Uani 1 1 d . A . P1 P 0.17577(10) 0.75743(4) 0.39392(8) 0.0220(3) Uani 1 1 d . . . P2 P 0.14340(9) 0.95285(4) 0.25913(8) 0.0195(3) Uani 1 1 d D . . P3 P 0.38596(9) 0.73306(4) 0.22624(8) 0.0205(3) Uani 1 1 d . . . P4 P 0.42666(10) 0.93347(4) 0.22479(9) 0.0263(3) Uani 1 1 d D . . O1 O 0.1582(3) 0.79680(12) 0.5479(2) 0.0294(8) Uani 1 1 d . . . O2 O -0.0417(3) 0.93583(13) 0.1883(2) 0.0356(9) Uani 1 1 d . . . O3 O 0.4507(3) 0.74969(13) 0.0762(2) 0.0343(9) Uani 1 1 d . . . O4 O 0.6028(3) 0.93607(13) 0.3361(3) 0.0382(10) Uani 1 1 d . . . O5 O 0.3071(3) 0.85970(17) 0.3823(3) 0.0614(15) Uani 1 1 d . . . O6 O 0.4416(4) 0.81701(16) 0.4462(4) 0.0670(16) Uani 1 1 d . . . O7 O 0.3703(4) 0.86289(17) 0.5332(3) 0.0585(14) Uani 1 1 d . . . O8 O 0.4542(3) 0.89611(14) 0.4356(3) 0.0423(10) Uani 1 1 d . . . C1 C 0.2280(4) 0.71425(16) 0.4737(3) 0.0262(11) Uani 1 1 d . . . C2 C 0.1862(4) 0.67224(18) 0.4780(4) 0.0353(13) Uani 1 1 d . . . H2 H 0.1261 0.6656 0.4403 0.042 Uiso 1 1 calc R . . C3 C 0.2317(5) 0.6403(2) 0.5367(5) 0.0496(17) Uani 1 1 d . . . H3 H 0.2027 0.6117 0.5398 0.059 Uiso 1 1 calc R . . C4 C 0.3197(5) 0.6497(2) 0.5913(4) 0.0430(16) Uani 1 1 d . . . H4 H 0.3511 0.6273 0.6311 0.052 Uiso 1 1 calc R . . C5 C 0.3619(4) 0.6915(2) 0.5883(4) 0.0375(14) Uani 1 1 d . . . H5 H 0.4218 0.6981 0.6265 0.045 Uiso 1 1 calc R . . C6 C 0.3159(4) 0.72382(18) 0.5290(4) 0.0304(12) Uani 1 1 d . . . H6 H 0.3447 0.7525 0.5262 0.036 Uiso 1 1 calc R . . C7 C 0.0639(4) 0.73487(16) 0.3299(3) 0.0255(11) Uani 1 1 d . . . C8 C -0.0168(4) 0.72912(17) 0.3640(4) 0.0305(12) Uani 1 1 d . . . H8 H -0.0152 0.7364 0.4241 0.037 Uiso 1 1 calc R . . C9 C -0.1012(5) 0.7126(2) 0.3102(4) 0.0413(15) Uani 1 1 d . . . H9 H -0.1577 0.7096 0.3328 0.050 Uiso 1 1 calc R . . C10 C -0.1015(5) 0.7005(2) 0.2230(4) 0.0473(17) Uani 1 1 d . . . H10 H -0.1582 0.6887 0.1866 0.057 Uiso 1 1 calc R . . C11 C -0.0209(5) 0.7055(2) 0.1890(4) 0.0412(15) Uani 1 1 d . . . H11 H -0.0218 0.6969 0.1297 0.049 Uiso 1 1 calc R . . C12 C 0.0617(4) 0.72311(18) 0.2417(3) 0.0322(12) Uani 1 1 d . . . H12 H 0.1172 0.7272 0.2179 0.039 Uiso 1 1 calc R . . C13 C 0.1315(4) 0.79937(16) 0.4679(3) 0.0238(10) Uani 1 1 d . . . C14 C 0.0612(4) 0.83460(15) 0.4252(3) 0.0220(10) Uani 1 1 d . . . C15 C -0.0215(4) 0.83977(16) 0.4576(3) 0.0259(11) Uani 1 1 d . . . H15 H -0.0307 0.8220 0.5062 0.031 Uiso 1 1 calc R . . C16 C -0.0906(4) 0.87051(17) 0.4197(3) 0.0276(11) Uani 1 1 d . . . H16 H -0.1478 0.8734 0.4411 0.033 Uiso 1 1 calc R . . C17 C -0.0758(4) 0.89726(16) 0.3500(3) 0.0248(10) Uani 1 1 d . A . H17 H -0.1237 0.9180 0.3228 0.030 Uiso 1 1 calc R . . C18 C 0.0089(4) 0.89364(16) 0.3201(3) 0.0210(10) Uani 1 1 d . . . C19 C 0.0771(4) 0.86152(15) 0.3560(3) 0.0210(10) Uani 1 1 d . A . H19 H 0.1336 0.8580 0.3336 0.025 Uiso 1 1 calc R . . C20 C 0.0231(4) 0.92614(16) 0.2498(3) 0.0225(10) Uani 1 1 d . A . C21 C 0.1654(3) 0.97877(15) 0.3676(3) 0.0200(10) Uani 1 1 d . A . C22 C 0.2607(4) 0.98016(17) 0.4158(4) 0.0277(11) Uani 1 1 d . . . H22 H 0.3102 0.9666 0.3924 0.033 Uiso 1 1 calc R A . C23 C 0.2823(4) 1.00141(19) 0.4978(4) 0.0350(13) Uani 1 1 d . A . H23 H 0.3467 1.0026 0.5300 0.042 Uiso 1 1 calc R . . C24 C 0.2105(4) 1.02081(18) 0.5326(4) 0.0321(12) Uani 1 1 d . . . H24 H 0.2259 1.0354 0.5885 0.038 Uiso 1 1 calc R A . C25 C 0.1159(4) 1.01907(18) 0.4861(4) 0.0303(12) Uani 1 1 d . A . H25 H 0.0667 1.0322 0.5104 0.036 Uiso 1 1 calc R . . C26 C 0.0938(4) 0.99809(16) 0.4043(3) 0.0241(10) Uani 1 1 d . . . H26 H 0.0291 0.9969 0.3728 0.029 Uiso 1 1 calc R A . C27 C 0.1114(7) 0.9972(3) 0.1756(5) 0.0284(13) Uani 0.544(7) 1 d PGDU A 1 C28 C 0.0908(8) 1.0411(3) 0.1970(5) 0.027(2) Uani 0.544(7) 1 d PGU A 1 H28 H 0.0953 1.0494 0.2571 0.033 Uiso 0.544(7) 1 calc PR A 1 C29 C 0.0634(7) 1.0730(2) 0.1305(6) 0.0430(17) Uani 0.544(7) 1 d PGU A 1 H29 H 0.0493 1.1030 0.1452 0.052 Uiso 0.544(7) 1 calc PR A 1 C30 C 0.0567(7) 1.0609(2) 0.0426(5) 0.054(3) Uani 0.544(7) 1 d PGU A 1 H30 H 0.0380 1.0827 -0.0029 0.065 Uiso 0.544(7) 1 calc PR A 1 C31 C 0.0773(7) 1.0171(3) 0.0212(4) 0.060(3) Uani 0.544(7) 1 d PGU A 1 H31 H 0.0727 1.0088 -0.0389 0.072 Uiso 0.544(7) 1 calc PR A 1 C32 C 0.1046(7) 0.9852(2) 0.0877(5) 0.043(2) Uani 0.544(7) 1 d PGU A 1 H32 H 0.1187 0.9552 0.0730 0.051 Uiso 0.544(7) 1 calc PR A 1 C27A C 0.1193(8) 1.0003(3) 0.1831(6) 0.0284(13) Uani 0.456(7) 1 d PGDU A 2 C28A C 0.0641(9) 1.0372(4) 0.1965(7) 0.027(2) Uani 0.456(7) 1 d PGU A 2 H28A H 0.0342 1.0378 0.2457 0.033 Uiso 0.456(7) 1 calc PR A 2 C29A C 0.0527(8) 1.0733(3) 0.1378(8) 0.0430(17) Uani 0.456(7) 1 d PGU A 2 H29A H 0.0150 1.0985 0.1469 0.052 Uiso 0.456(7) 1 calc PR A 2 C30A C 0.0964(8) 1.0724(3) 0.0657(7) 0.054(3) Uani 0.456(7) 1 d PGU A 2 H30A H 0.0886 1.0971 0.0256 0.065 Uiso 0.456(7) 1 calc PR A 2 C31A C 0.1516(8) 1.0355(4) 0.0524(6) 0.060(3) Uani 0.456(7) 1 d PGU A 2 H31A H 0.1815 1.0350 0.0031 0.072 Uiso 0.456(7) 1 calc PR A 2 C32A C 0.1630(8) 0.9995(3) 0.1110(7) 0.043(2) Uani 0.456(7) 1 d PGU A 2 H32A H 0.2007 0.9742 0.1019 0.051 Uiso 0.456(7) 1 calc PR A 2 C33 C 0.3154(4) 0.69255(17) 0.1516(3) 0.0238(10) Uani 1 1 d . . . C34 C 0.2450(4) 0.70971(18) 0.0821(3) 0.0293(12) Uani 1 1 d . . . H34 H 0.2377 0.7414 0.0740 0.035 Uiso 1 1 calc R . . C35 C 0.1856(4) 0.6803(2) 0.0248(4) 0.0352(13) Uani 1 1 d . . . H35 H 0.1386 0.6919 -0.0229 0.042 Uiso 1 1 calc R . . C36 C 0.1951(4) 0.6344(2) 0.0374(4) 0.0354(13) Uani 1 1 d . . . H36 H 0.1546 0.6144 -0.0017 0.042 Uiso 1 1 calc R . . C37 C 0.2631(4) 0.61726(18) 0.1064(4) 0.0326(12) Uani 1 1 d . . . H37 H 0.2690 0.5856 0.1150 0.039 Uiso 1 1 calc R . . C38 C 0.3236(4) 0.64644(17) 0.1638(4) 0.0296(12) Uani 1 1 d . . . H38 H 0.3703 0.6345 0.2113 0.036 Uiso 1 1 calc R . . C39 C 0.4816(4) 0.70318(16) 0.2998(3) 0.0244(10) Uani 1 1 d . . . C40 C 0.4896(4) 0.70769(19) 0.3903(4) 0.0336(13) Uani 1 1 d . . . H40 H 0.4433 0.7246 0.4121 0.040 Uiso 1 1 calc R . . C41 C 0.5649(5) 0.6876(2) 0.4491(4) 0.0416(15) Uani 1 1 d . . . H41 H 0.5696 0.6907 0.5110 0.050 Uiso 1 1 calc R . . C42 C 0.6333(5) 0.6630(2) 0.4181(4) 0.0441(16) Uani 1 1 d . . . H42 H 0.6852 0.6496 0.4586 0.053 Uiso 1 1 calc R . . C43 C 0.6259(4) 0.6582(2) 0.3280(4) 0.0391(14) Uani 1 1 d . . . H43 H 0.6727 0.6413 0.3067 0.047 Uiso 1 1 calc R . . C44 C 0.5500(4) 0.67806(18) 0.2681(4) 0.0296(12) Uani 1 1 d . . . H44 H 0.5449 0.6745 0.2062 0.035 Uiso 1 1 calc R . . C45 C 0.4601(4) 0.75976(16) 0.1528(3) 0.0251(11) Uani 1 1 d . . . C46 C 0.5339(4) 0.79273(17) 0.1975(3) 0.0246(11) Uani 1 1 d . . . C47 C 0.6304(4) 0.78338(19) 0.2045(4) 0.0321(12) Uani 1 1 d . . . H47 H 0.6495 0.7561 0.1811 0.038 Uiso 1 1 calc R . . C48 C 0.6989(4) 0.8141(2) 0.2458(4) 0.0371(13) Uani 1 1 d . . . H48 H 0.7650 0.8071 0.2541 0.045 Uiso 1 1 calc R . . C49 C 0.6702(4) 0.8553(2) 0.2751(4) 0.0320(12) Uani 1 1 d . A . H49 H 0.7170 0.8766 0.3022 0.038 Uiso 1 1 calc R . . C50 C 0.5730(4) 0.86549(18) 0.2648(3) 0.0262(11) Uani 1 1 d . . . C51 C 0.5052(4) 0.83316(16) 0.2295(3) 0.0241(10) Uani 1 1 d . A . H51 H 0.4393 0.8387 0.2272 0.029 Uiso 1 1 calc R . . C52 C 0.5469(4) 0.91237(18) 0.2865(3) 0.0295(12) Uani 1 1 d . A . C53 C 0.4428(4) 0.92675(19) 0.1120(4) 0.0332(12) Uani 1 1 d . A . C54 C 0.3892(5) 0.8945(3) 0.0582(4) 0.0548(19) Uani 1 1 d . . . H54 H 0.3407 0.8782 0.0783 0.066 Uiso 1 1 calc R A . C55 C 0.4070(7) 0.8860(3) -0.0252(5) 0.075(3) Uani 1 1 d . A . H55 H 0.3716 0.8633 -0.0615 0.090 Uiso 1 1 calc R . . C56 C 0.4752(6) 0.9100(3) -0.0554(5) 0.065(2) Uani 1 1 d . . . H56 H 0.4851 0.9049 -0.1134 0.079 Uiso 1 1 calc R A . C57 C 0.5290(5) 0.9414(2) -0.0022(5) 0.0511(18) Uani 1 1 d . A . H57 H 0.5771 0.9576 -0.0229 0.061 Uiso 1 1 calc R . . C58 C 0.5138(4) 0.9496(2) 0.0821(4) 0.0382(14) Uani 1 1 d . . . H58 H 0.5523 0.9711 0.1193 0.046 Uiso 1 1 calc R A . C59 C 0.4313(3) 0.99221(12) 0.2583(4) 0.0295(15) Uani 0.516(10) 1 d PGDU A 1 C60 C 0.3876(5) 1.02269(15) 0.1940(4) 0.045(2) Uani 0.516(10) 1 d PGU A 1 H60 H 0.3612 1.0125 0.1357 0.054 Uiso 0.516(10) 1 calc PR A 1 C61 C 0.3825(6) 1.06807(13) 0.2150(5) 0.044(2) Uani 0.516(10) 1 d PGU A 1 H61 H 0.3526 1.0889 0.1710 0.053 Uiso 0.516(10) 1 calc PR A 1 C62 C 0.4211(5) 1.08297(15) 0.3003(7) 0.046(2) Uani 0.516(10) 1 d PGU A 1 H62 H 0.4176 1.1140 0.3147 0.055 Uiso 0.516(10) 1 calc PR A 1 C63 C 0.4648(4) 1.0525(2) 0.3646(6) 0.052(3) Uani 0.516(10) 1 d PGU A 1 H63 H 0.4911 1.0627 0.4230 0.063 Uiso 0.516(10) 1 calc PR A 1 C64 C 0.4699(4) 1.0071(2) 0.3436(5) 0.050(3) Uani 0.516(10) 1 d PGU A 1 H64 H 0.4997 0.9863 0.3876 0.060 Uiso 0.516(10) 1 calc PR A 1 C59A C 0.4227(4) 0.99573(12) 0.2338(4) 0.0295(15) Uani 0.484(10) 1 d PGDU A 2 C60A C 0.3556(5) 1.01915(19) 0.1717(3) 0.045(2) Uani 0.484(10) 1 d PGU A 2 H60A H 0.3201 1.0039 0.1212 0.054 Uiso 0.484(10) 1 calc PR A 2 C61A C 0.3405(7) 1.06483(19) 0.1836(5) 0.044(2) Uani 0.484(10) 1 d PGU A 2 H61A H 0.2946 1.0808 0.1411 0.053 Uiso 0.484(10) 1 calc PR A 2 C62A C 0.3924(6) 1.08709(12) 0.2575(6) 0.046(2) Uani 0.484(10) 1 d PGU A 2 H62A H 0.3820 1.1183 0.2655 0.055 Uiso 0.484(10) 1 calc PR A 2 C63A C 0.4595(4) 1.06367(19) 0.3195(6) 0.052(3) Uani 0.484(10) 1 d PGU A 2 H63A H 0.4950 1.0789 0.3700 0.063 Uiso 0.484(10) 1 calc PR A 2 C64A C 0.4746(3) 1.01798(19) 0.3077(5) 0.050(3) Uani 0.484(10) 1 d PGU A 2 H64A H 0.5205 1.0020 0.3501 0.060 Uiso 0.484(10) 1 calc PR A 2 C65 C 0.7967(5) 0.0955(2) 0.3884(5) 0.0515(18) Uani 1 1 d . . . H65A H 0.7941 0.1283 0.3999 0.062 Uiso 1 1 calc R . . H65B H 0.7846 0.0794 0.4410 0.062 Uiso 1 1 calc R . . Cl3 Cl 0.91025(14) 0.08173(6) 0.37335(13) 0.0583(5) Uani 1 1 d . . . Cl4 Cl 0.70631(16) 0.08153(9) 0.29571(17) 0.0779(6) Uani 1 1 d . . . C66 C 0.8186(8) 0.0130(4) 0.1635(8) 0.035(3) Uani 0.50 1 d P . . H66A H 0.8447 0.0341 0.2124 0.042 Uiso 0.50 1 calc PR . . H66B H 0.8733 -0.0018 0.1452 0.042 Uiso 0.50 1 calc PR . . Cl5 Cl 0.7479(2) -0.02824(11) 0.2016(2) 0.0485(8) Uani 0.50 1 d P . . Cl6 Cl 0.7534(3) 0.04310(12) 0.0753(2) 0.0501(8) Uani 0.50 1 d P . . 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 Ag1 0.0307(2) 0.01900(18) 0.02097(19) -0.00102(14) 0.00631(15) 0.00327(15) Ag2 0.0258(2) 0.01839(18) 0.0256(2) -0.00310(14) 0.00542(15) -0.00003(14) Cl1 0.0451(8) 0.0181(6) 0.0205(6) -0.0012(5) -0.0042(5) -0.0013(5) Cl2 0.0253(6) 0.0252(6) 0.0190(6) -0.0026(5) 0.0008(5) -0.0022(5) P1 0.0297(7) 0.0167(6) 0.0185(6) 0.0005(5) 0.0028(5) 0.0004(5) P2 0.0247(6) 0.0149(6) 0.0194(6) -0.0002(5) 0.0054(5) -0.0007(5) P3 0.0253(6) 0.0173(6) 0.0178(6) -0.0019(5) 0.0020(5) 0.0021(5) P4 0.0290(7) 0.0209(6) 0.0304(7) -0.0082(5) 0.0100(6) -0.0044(5) O1 0.042(2) 0.0259(19) 0.0195(19) -0.0001(14) 0.0054(16) 0.0007(16) O2 0.036(2) 0.042(2) 0.024(2) 0.0096(17) -0.0055(17) -0.0109(18) O3 0.048(2) 0.033(2) 0.023(2) -0.0105(16) 0.0101(17) -0.0045(18) O4 0.041(2) 0.031(2) 0.039(2) -0.0116(18) 0.0012(19) -0.0145(18) O5 0.052(3) 0.064(3) 0.050(3) 0.032(2) -0.030(2) -0.031(2) O6 0.061(3) 0.033(3) 0.116(5) -0.007(3) 0.040(3) 0.009(2) O7 0.090(4) 0.063(3) 0.029(2) -0.003(2) 0.027(2) -0.007(3) O8 0.040(2) 0.037(2) 0.045(3) 0.0055(19) -0.0026(19) -0.0168(18) C1 0.038(3) 0.017(2) 0.023(3) 0.0017(19) 0.004(2) 0.006(2) C2 0.050(4) 0.020(3) 0.029(3) 0.003(2) -0.006(3) -0.003(2) C3 0.064(4) 0.026(3) 0.052(4) 0.006(3) -0.004(3) 0.001(3) C4 0.062(4) 0.029(3) 0.035(3) 0.010(3) 0.005(3) 0.021(3) C5 0.037(3) 0.048(4) 0.025(3) 0.007(3) -0.001(2) 0.012(3) C6 0.034(3) 0.027(3) 0.030(3) 0.006(2) 0.005(2) 0.001(2) C7 0.035(3) 0.014(2) 0.024(3) 0.0013(19) -0.002(2) 0.002(2) C8 0.040(3) 0.021(3) 0.028(3) 0.002(2) 0.003(2) -0.002(2) C9 0.037(3) 0.034(3) 0.049(4) 0.009(3) 0.001(3) -0.007(3) C10 0.055(4) 0.033(3) 0.041(4) 0.000(3) -0.019(3) -0.010(3) C11 0.055(4) 0.036(3) 0.026(3) -0.007(2) -0.007(3) -0.004(3) C12 0.044(3) 0.027(3) 0.021(3) -0.004(2) 0.000(2) 0.004(2) C13 0.034(3) 0.016(2) 0.023(3) 0.0005(19) 0.009(2) -0.004(2) C14 0.031(3) 0.013(2) 0.022(2) -0.0021(18) 0.006(2) -0.0041(19) C15 0.035(3) 0.020(2) 0.025(3) 0.000(2) 0.010(2) -0.003(2) C16 0.027(3) 0.029(3) 0.031(3) 0.002(2) 0.015(2) -0.002(2) C17 0.027(3) 0.022(2) 0.026(3) 0.000(2) 0.007(2) -0.003(2) C18 0.029(3) 0.018(2) 0.016(2) -0.0007(18) 0.0048(19) -0.0056(19) C19 0.026(2) 0.016(2) 0.023(2) -0.0021(18) 0.008(2) -0.0024(19) C20 0.030(3) 0.019(2) 0.016(2) -0.0011(18) -0.001(2) -0.003(2) C21 0.021(2) 0.014(2) 0.024(2) 0.0001(18) 0.0022(19) -0.0030(18) C22 0.025(3) 0.026(3) 0.030(3) -0.004(2) 0.001(2) 0.000(2) C23 0.032(3) 0.034(3) 0.035(3) -0.012(2) 0.000(2) -0.001(2) C24 0.037(3) 0.028(3) 0.029(3) -0.008(2) 0.003(2) -0.008(2) C25 0.031(3) 0.029(3) 0.034(3) -0.008(2) 0.014(2) -0.005(2) C26 0.021(2) 0.022(2) 0.031(3) -0.003(2) 0.009(2) -0.0064(19) C27 0.034(3) 0.024(2) 0.027(3) 0.005(2) 0.006(2) -0.006(2) C28 0.028(5) 0.024(3) 0.030(3) 0.002(2) 0.002(3) -0.002(3) C29 0.056(4) 0.024(3) 0.045(3) 0.004(2) 0.000(3) 0.000(3) C30 0.065(5) 0.040(4) 0.051(4) 0.012(3) -0.002(4) -0.007(4) C31 0.076(5) 0.057(4) 0.047(4) 0.008(4) 0.015(4) 0.002(4) C32 0.054(4) 0.038(4) 0.037(4) 0.007(3) 0.008(3) 0.000(3) C27A 0.034(3) 0.024(2) 0.027(3) 0.005(2) 0.006(2) -0.006(2) C28A 0.028(5) 0.024(3) 0.030(3) 0.002(2) 0.002(3) -0.002(3) C29A 0.056(4) 0.024(3) 0.045(3) 0.004(2) 0.000(3) 0.000(3) C30A 0.065(5) 0.040(4) 0.051(4) 0.012(3) -0.002(4) -0.007(4) C31A 0.076(5) 0.057(4) 0.047(4) 0.008(4) 0.015(4) 0.002(4) C32A 0.054(4) 0.038(4) 0.037(4) 0.007(3) 0.008(3) 0.000(3) C33 0.023(3) 0.027(3) 0.021(3) -0.006(2) 0.005(2) -0.001(2) C34 0.031(3) 0.028(3) 0.025(3) -0.004(2) -0.003(2) 0.004(2) C35 0.028(3) 0.045(3) 0.028(3) -0.007(2) -0.004(2) 0.000(2) C36 0.029(3) 0.044(3) 0.033(3) -0.020(3) 0.008(2) -0.011(2) C37 0.039(3) 0.020(3) 0.039(3) -0.009(2) 0.010(3) -0.008(2) C38 0.034(3) 0.023(3) 0.031(3) -0.004(2) 0.003(2) -0.002(2) C39 0.030(3) 0.020(2) 0.022(3) 0.0001(19) 0.003(2) -0.001(2) C40 0.038(3) 0.033(3) 0.024(3) -0.004(2) -0.006(2) 0.008(2) C41 0.051(4) 0.042(4) 0.026(3) -0.004(3) -0.005(3) 0.010(3) C42 0.039(3) 0.045(4) 0.039(4) -0.003(3) -0.012(3) 0.014(3) C43 0.037(3) 0.035(3) 0.042(3) -0.002(3) 0.002(3) 0.012(3) C44 0.032(3) 0.027(3) 0.028(3) -0.002(2) 0.002(2) 0.007(2) C45 0.029(3) 0.019(2) 0.027(3) -0.002(2) 0.004(2) 0.006(2) C46 0.030(3) 0.023(2) 0.020(2) -0.0017(19) 0.002(2) 0.000(2) C47 0.032(3) 0.034(3) 0.031(3) -0.001(2) 0.007(2) 0.005(2) C48 0.023(3) 0.042(3) 0.047(4) 0.000(3) 0.008(2) 0.001(2) C49 0.024(3) 0.041(3) 0.032(3) -0.001(2) 0.007(2) -0.009(2) C50 0.030(3) 0.029(3) 0.020(2) -0.003(2) 0.006(2) -0.008(2) C51 0.024(3) 0.024(2) 0.025(3) -0.005(2) 0.006(2) -0.003(2) C52 0.038(3) 0.028(3) 0.023(3) -0.006(2) 0.009(2) -0.014(2) C53 0.040(3) 0.032(3) 0.031(3) -0.001(2) 0.012(2) 0.003(2) C54 0.061(5) 0.068(5) 0.041(4) -0.015(3) 0.021(3) -0.019(4) C55 0.087(6) 0.103(7) 0.043(4) -0.034(4) 0.030(4) -0.021(5) C56 0.087(6) 0.078(6) 0.041(4) 0.001(4) 0.034(4) 0.008(5) C57 0.058(4) 0.048(4) 0.056(4) 0.018(3) 0.032(4) 0.012(3) C58 0.041(3) 0.035(3) 0.042(3) 0.010(3) 0.018(3) 0.004(3) C59 0.034(3) 0.029(3) 0.030(4) -0.009(3) 0.017(3) -0.007(2) C60 0.065(5) 0.034(3) 0.038(4) 0.001(3) 0.017(4) 0.003(3) C61 0.052(5) 0.042(4) 0.042(4) 0.007(3) 0.016(4) 0.001(3) C62 0.047(4) 0.041(4) 0.052(5) -0.006(4) 0.016(4) -0.013(3) C63 0.049(4) 0.049(4) 0.057(5) -0.019(4) 0.006(4) -0.003(3) C64 0.045(4) 0.048(4) 0.055(5) -0.013(4) 0.005(4) -0.001(3) C59A 0.034(3) 0.029(3) 0.030(4) -0.009(3) 0.017(3) -0.007(2) C60A 0.065(5) 0.034(3) 0.038(4) 0.001(3) 0.017(4) 0.003(3) C61A 0.052(5) 0.042(4) 0.042(4) 0.007(3) 0.016(4) 0.001(3) C62A 0.047(4) 0.041(4) 0.052(5) -0.006(4) 0.016(4) -0.013(3) C63A 0.049(4) 0.049(4) 0.057(5) -0.019(4) 0.006(4) -0.003(3) C64A 0.045(4) 0.048(4) 0.055(5) -0.013(4) 0.005(4) -0.001(3) C65 0.075(5) 0.033(3) 0.049(4) -0.003(3) 0.020(4) -0.002(3) Cl3 0.0622(11) 0.0485(10) 0.0618(12) 0.0035(8) 0.0076(9) 0.0022(8) Cl4 0.0603(13) 0.0881(16) 0.0840(16) -0.0153(13) 0.0127(11) -0.0053(11) C66 0.039(7) 0.030(6) 0.033(6) 0.011(5) 0.002(5) 0.016(5) Cl5 0.0392(16) 0.0377(16) 0.064(2) 0.0226(15) 0.0003(15) 0.0008(13) Cl6 0.059(2) 0.055(2) 0.0377(17) 0.0191(14) 0.0116(15) 0.0320(16) _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 Ag1 P1 2.4506(14) . ? Ag1 P3 2.4533(13) . ? Ag1 Cl1 2.5868(13) . ? Ag1 O5 2.707(5) . ? Ag2 P4 2.4246(15) . ? Ag2 P2 2.4368(13) . ? Ag2 Cl1 2.5189(13) . ? Ag2 O5 2.529(4) . ? Cl2 O7 1.405(4) . ? Cl2 O6 1.433(5) . ? Cl2 O8 1.437(4) . ? Cl2 O5 1.442(4) . ? P1 C7 1.819(5) . ? P1 C1 1.824(5) . ? P1 C13 1.889(5) . ? P2 C21 1.811(5) . ? P2 C27A 1.819(7) . ? P2 C27 1.833(6) . ? P2 C20 1.871(5) . ? P3 C39 1.813(5) . ? P3 C33 1.816(5) . ? P3 C45 1.885(6) . ? P4 C59 1.815(4) . ? P4 C53 1.820(6) . ? P4 C59A 1.854(4) . ? P4 C52 1.886(6) . ? O1 C13 1.217(6) . ? O2 C20 1.212(6) . ? O3 C45 1.202(6) . ? O4 C52 1.209(6) . ? C1 C2 1.390(7) . ? C1 C6 1.390(7) . ? C2 C3 1.376(8) . ? C2 H2 0.9500 . ? C3 C4 1.386(9) . ? C3 H3 0.9500 . ? C4 C5 1.384(9) . ? C4 H4 0.9500 . ? C5 C6 1.392(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.378(8) . ? C7 C12 1.403(7) . ? C8 C9 1.401(8) . ? C8 H8 0.9500 . ? C9 C10 1.396(9) . ? C9 H9 0.9500 . ? C10 C11 1.371(10) . ? C10 H10 0.9500 . ? C11 C12 1.386(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.501(7) . ? C14 C15 1.389(7) . ? C14 C19 1.393(7) . ? C15 C16 1.379(7) . ? C15 H15 0.9500 . ? C16 C17 1.391(7) . ? C16 H16 0.9500 . ? C17 C18 1.389(7) . ? C17 H17 0.9500 . ? C18 C19 1.391(7) . ? C18 C20 1.500(6) . ? C19 H19 0.9500 . ? C21 C26 1.394(7) . ? C21 C22 1.408(7) . ? C22 C23 1.391(7) . ? C22 H22 0.9500 . ? C23 C24 1.382(8) . ? C23 H23 0.9500 . ? C24 C25 1.390(8) . ? C24 H24 0.9500 . ? C25 C26 1.386(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9500 . ? C29 C30 1.3900 . ? C29 H29 0.9500 . ? C30 C31 1.3900 . ? C30 H30 0.9500 . ? C31 C32 1.3900 . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C27A C28A 1.3900 . ? C27A C32A 1.3900 . ? C28A C29A 1.3900 . ? C28A H28A 0.9500 . ? C29A C30A 1.3900 . ? C29A H29A 0.9500 . ? C30A C31A 1.3900 . ? C30A H30A 0.9500 . ? C31A C32A 1.3900 . ? C31A H31A 0.9500 . ? C32A H32A 0.9500 . ? C33 C38 1.382(7) . ? C33 C34 1.403(7) . ? C34 C35 1.394(7) . ? C34 H34 0.9500 . ? C35 C36 1.378(8) . ? C35 H35 0.9500 . ? C36 C37 1.379(8) . ? C36 H36 0.9500 . ? C37 C38 1.399(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.387(7) . ? C39 C44 1.399(7) . ? C40 C41 1.387(8) . ? C40 H40 0.9500 . ? C41 C42 1.385(9) . ? C41 H41 0.9500 . ? C42 C43 1.383(9) . ? C42 H42 0.9500 . ? C43 C44 1.398(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.496(7) . ? C46 C47 1.389(7) . ? C46 C51 1.392(7) . ? C47 C48 1.390(8) . ? C47 H47 0.9500 . ? C48 C49 1.394(8) . ? C48 H48 0.9500 . ? C49 C50 1.397(8) . ? C49 H49 0.9500 . ? C50 C51 1.389(7) . ? C50 C52 1.496(7) . ? C51 H51 0.9500 . ? C53 C58 1.379(8) . ? C53 C54 1.387(9) . ? C54 C55 1.391(9) . ? C54 H54 0.9500 . ? C55 C56 1.368(11) . ? C55 H55 0.9500 . ? C56 C57 1.364(11) . ? C56 H56 0.9500 . ? C57 C58 1.390(9) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C60 H60 0.9500 . ? C61 C62 1.3900 . ? C61 H61 0.9500 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C59A C60A 1.3899 . ? C59A C64A 1.3900 . ? C60A C61A 1.3901 . ? C60A H60A 0.9500 . ? C61A C62A 1.3900 . ? C61A H61A 0.9500 . ? C62A C63A 1.3900 . ? C62A H62A 0.9500 . ? C63A C64A 1.3901 . ? C63A H63A 0.9500 . ? C64A H64A 0.9500 . ? C65 Cl3 1.737(8) . ? C65 Cl4 1.764(8) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 Cl6 1.728(10) . ? C66 Cl5 1.766(12) . ? C66 H66A 0.9900 . ? C66 H66B 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 Ag1 P3 129.12(5) . . ? P1 Ag1 Cl1 116.75(5) . . ? P3 Ag1 Cl1 100.00(5) . . ? P1 Ag1 O5 88.13(11) . . ? P3 Ag1 O5 132.75(12) . . ? Cl1 Ag1 O5 82.44(9) . . ? P4 Ag2 P2 121.15(5) . . ? P4 Ag2 Cl1 121.98(5) . . ? P2 Ag2 Cl1 110.62(5) . . ? P4 Ag2 O5 104.87(11) . . ? P2 Ag2 O5 101.72(14) . . ? Cl1 Ag2 O5 87.48(12) . . ? Ag2 Cl1 Ag1 94.81(4) . . ? O7 Cl2 O6 108.2(3) . . ? O7 Cl2 O8 110.6(3) . . ? O6 Cl2 O8 110.7(3) . . ? O7 Cl2 O5 109.1(3) . . ? O6 Cl2 O5 108.8(3) . . ? O8 Cl2 O5 109.5(2) . . ? C7 P1 C1 107.2(2) . . ? C7 P1 C13 101.7(2) . . ? C1 P1 C13 101.2(2) . . ? C7 P1 Ag1 110.23(18) . . ? C1 P1 Ag1 113.28(18) . . ? C13 P1 Ag1 121.81(16) . . ? C21 P2 C27A 104.0(4) . . ? C21 P2 C27 108.4(3) . . ? C21 P2 C20 103.1(2) . . ? C27A P2 C20 103.5(4) . . ? C27 P2 C20 99.3(3) . . ? C21 P2 Ag2 112.99(16) . . ? C27A P2 Ag2 115.2(4) . . ? C27 P2 Ag2 115.0(3) . . ? C20 P2 Ag2 116.49(16) . . ? C39 P3 C33 108.5(2) . . ? C39 P3 C45 97.9(2) . . ? C33 P3 C45 101.6(2) . . ? C39 P3 Ag1 116.94(17) . . ? C33 P3 Ag1 110.11(17) . . ? C45 P3 Ag1 120.00(15) . . ? C59 P4 C53 112.0(3) . . ? C53 P4 C59A 101.2(3) . . ? C59 P4 C52 101.6(2) . . ? C53 P4 C52 99.3(3) . . ? C59A P4 C52 109.4(2) . . ? C59 P4 Ag2 107.90(17) . . ? C53 P4 Ag2 110.3(2) . . ? C59A P4 Ag2 108.55(16) . . ? C52 P4 Ag2 125.36(17) . . ? Cl2 O5 Ag2 128.2(3) . . ? Cl2 O5 Ag1 111.0(3) . . ? Ag2 O5 Ag1 91.70(16) . . ? C2 C1 C6 119.7(5) . . ? C2 C1 P1 122.9(4) . . ? C6 C1 P1 117.3(4) . . ? C3 C2 C1 120.0(6) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.3(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.4(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.4(6) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 120.2(5) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C12 119.7(5) . . ? C8 C7 P1 123.2(4) . . ? C12 C7 P1 117.1(4) . . ? C7 C8 C9 120.1(5) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 119.3(6) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 120.9(6) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.7(6) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 120.3(6) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? O1 C13 C14 121.8(4) . . ? O1 C13 P1 120.1(4) . . ? C14 C13 P1 118.1(3) . . ? C15 C14 C19 120.4(5) . . ? C15 C14 C13 117.3(4) . . ? C19 C14 C13 122.3(5) . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.6(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.1(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.5(4) . . ? C17 C18 C20 117.0(4) . . ? C19 C18 C20 122.5(4) . . ? C18 C19 C14 118.9(5) . . ? C18 C19 H19 120.6 . . ? C14 C19 H19 120.6 . . ? O2 C20 C18 121.6(5) . . ? O2 C20 P2 119.7(4) . . ? C18 C20 P2 118.7(3) . . ? C26 C21 C22 118.9(5) . . ? C26 C21 P2 123.7(4) . . ? C22 C21 P2 117.4(4) . . ? C23 C22 C21 119.9(5) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.3(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.7(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 120.9(5) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C28 C27 C32 120.0 . . ? C28 C27 P2 122.5(5) . . ? C32 C27 P2 117.4(5) . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C28A C27A C32A 120.0 . . ? C28A C27A P2 123.2(6) . . ? C32A C27A P2 116.7(6) . . ? C27A C28A C29A 120.0 . . ? C27A C28A H28A 120.0 . . ? C29A C28A H28A 120.0 . . ? C30A C29A C28A 120.0 . . ? C30A C29A H29A 120.0 . . ? C28A C29A H29A 120.0 . . ? C29A C30A C31A 120.0 . . ? C29A C30A H30A 120.0 . . ? C31A C30A H30A 120.0 . . ? C32A C31A C30A 120.0 . . ? C32A C31A H31A 120.0 . . ? C30A C31A H31A 120.0 . . ? C31A C32A C27A 120.0 . . ? C31A C32A H32A 120.0 . . ? C27A C32A H32A 120.0 . . ? C38 C33 C34 119.3(5) . . ? C38 C33 P3 123.3(4) . . ? C34 C33 P3 117.3(4) . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 120.0(5) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.4(5) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 120.1(5) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C33 C38 C37 120.2(5) . . ? C33 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C44 119.5(5) . . ? C40 C39 P3 118.4(4) . . ? C44 C39 P3 122.0(4) . . ? C39 C40 C41 120.4(5) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 120.3(6) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 119.7(5) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.5(6) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 119.6(5) . . ? C43 C44 H44 120.2 . . ? C39 C44 H44 120.2 . . ? O3 C45 C46 122.5(5) . . ? O3 C45 P3 122.1(4) . . ? C46 C45 P3 115.3(4) . . ? C47 C46 C51 120.5(5) . . ? C47 C46 C45 119.8(5) . . ? C51 C46 C45 119.7(5) . . ? C46 C47 C48 119.7(5) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C47 C48 C49 119.8(5) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? C48 C49 C50 120.4(5) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 119.3(5) . . ? C51 C50 C52 122.9(5) . . ? C49 C50 C52 117.7(5) . . ? C50 C51 C46 120.0(5) . . ? C50 C51 H51 120.0 . . ? C46 C51 H51 120.0 . . ? O4 C52 C50 121.3(5) . . ? O4 C52 P4 122.4(4) . . ? C50 C52 P4 116.0(4) . . ? C58 C53 C54 119.4(6) . . ? C58 C53 P4 121.3(5) . . ? C54 C53 P4 118.9(5) . . ? C53 C54 C55 119.6(7) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C56 C55 C54 120.5(8) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C57 C56 C55 120.0(7) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C58 120.4(7) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C53 C58 C57 120.1(6) . . ? C53 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C60 C59 C64 120.0 . . ? C60 C59 P4 115.9(3) . . ? C64 C59 P4 124.0(3) . . ? C61 C60 C59 120.0 . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C62 120.0 . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C63 C62 C61 120.0 . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 H64 120.0 . . ? C59 C64 H64 120.0 . . ? C60A C59A C64A 120.0 . . ? C60A C59A P4 118.2(3) . . ? C64A C59A P4 121.0(3) . . ? C59A C60A C61A 120.0 . . ? C59A C60A H60A 120.0 . . ? C61A C60A H60A 120.0 . . ? C62A C61A C60A 120.0 . . ? C62A C61A H61A 120.0 . . ? C60A C61A H61A 120.0 . . ? C63A C62A C61A 120.0 . . ? C63A C62A H62A 120.0 . . ? C61A C62A H62A 120.0 . . ? C62A C63A C64A 120.0 . . ? C62A C63A H63A 120.0 . . ? C64A C63A H63A 120.0 . . ? C59A C64A C63A 120.0 . . ? C59A C64A H64A 120.0 . . ? C63A C64A H64A 120.0 . . ? Cl3 C65 Cl4 112.3(4) . . ? Cl3 C65 H65A 109.2 . . ? Cl4 C65 H65A 109.2 . . ? Cl3 C65 H65B 109.2 . . ? Cl4 C65 H65B 109.2 . . ? H65A C65 H65B 107.9 . . ? Cl6 C66 Cl5 111.7(7) . . ? Cl6 C66 H66A 109.3 . . ? Cl5 C66 H66A 109.3 . . ? Cl6 C66 H66B 109.3 . . ? Cl5 C66 H66B 109.3 . . ? H66A C66 H66B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.345 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.124 _iucr_refine_instructions_details ; TITL MSB487a_0m in P2(1)/n CELL 0.71073 14.2961 29.6539 15.4740 90.000 102.318 90.000 ZERR 2.00 0.0032 0.0065 0.0034 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H O P Cl Ag UNIT 262 204 32 16 20 8 L.S. 6 ACTA BOND $H BIND Ag1 O5 FMAP 2 PLAN 5 SIZE 0.09 0.11 0.21 EADP C64 C64a EADP C63 C63a EADP C62 C62a EADP C61 C61a EADP C60 C60a EADP C59 C59a EADP C32 C32a EADP C31 C31a EADP C30 C30a EADP C29 C29a EADP C28 C28a EADP C27 C27a SADI P4 C59 P4 C59a SADI P2 C27 P2 C27a TEMP -173 ISOR 0.007 C27 > C32a C59 > C64a WGHT 0.054600 22.097700 FVAR 0.05963 0.54395 0.51617 MOLE 1 AG1 6 0.280891 0.779923 0.295397 11.00000 0.03072 0.01900 = 0.02097 -0.00102 0.00631 0.00327 AG2 6 0.272864 0.903302 0.238522 11.00000 0.02584 0.01839 = 0.02565 -0.00310 0.00542 -0.00003 CL1 5 0.206882 0.831229 0.163264 11.00000 0.04510 0.01809 = 0.02053 -0.00121 -0.00424 -0.00133 CL2 5 0.393931 0.859257 0.449870 11.00000 0.02534 0.02515 = 0.01897 -0.00265 0.00081 -0.00218 P1 4 0.175765 0.757431 0.393923 11.00000 0.02967 0.01675 = 0.01850 0.00050 0.00277 0.00036 P2 4 0.143398 0.952849 0.259126 11.00000 0.02466 0.01488 = 0.01942 -0.00021 0.00545 -0.00074 P3 4 0.385959 0.733056 0.226238 11.00000 0.02527 0.01732 = 0.01780 -0.00194 0.00197 0.00205 P4 4 0.426657 0.933466 0.224791 11.00000 0.02904 0.02092 = 0.03043 -0.00817 0.00997 -0.00438 O1 3 0.158210 0.796803 0.547865 11.00000 0.04229 0.02594 = 0.01946 -0.00012 0.00541 0.00066 O2 3 -0.041696 0.935830 0.188272 11.00000 0.03645 0.04153 = 0.02363 0.00962 -0.00550 -0.01089 O3 3 0.450661 0.749694 0.076172 11.00000 0.04754 0.03305 = 0.02342 -0.01052 0.01006 -0.00447 O4 3 0.602798 0.936065 0.336145 11.00000 0.04086 0.03142 = 0.03911 -0.01156 0.00122 -0.01449 O5 3 0.307129 0.859700 0.382270 11.00000 0.05169 0.06399 = 0.05038 0.03198 -0.02953 -0.03080 O6 3 0.441606 0.817013 0.446201 11.00000 0.06149 0.03275 = 0.11587 -0.00708 0.03962 0.00902 O7 3 0.370317 0.862888 0.533221 11.00000 0.08984 0.06288 = 0.02935 -0.00324 0.02722 -0.00742 O8 3 0.454196 0.896113 0.435649 11.00000 0.03953 0.03676 = 0.04544 0.00551 -0.00262 -0.01676 C1 1 0.227996 0.714252 0.473688 11.00000 0.03786 0.01707 = 0.02264 0.00166 0.00442 0.00611 C2 1 0.186173 0.672238 0.477957 11.00000 0.04984 0.02012 = 0.02935 0.00264 -0.00620 -0.00335 AFIX 43 H2 2 0.126107 0.665557 0.440315 11.00000 -1.20000 AFIX 0 C3 1 0.231702 0.640302 0.536674 11.00000 0.06370 0.02583 = 0.05182 0.00619 -0.00419 0.00088 AFIX 43 H3 2 0.202706 0.611688 0.539752 11.00000 -1.20000 AFIX 0 C4 1 0.319681 0.649700 0.591346 11.00000 0.06240 0.02859 = 0.03536 0.01001 0.00481 0.02133 AFIX 43 H4 2 0.351137 0.627329 0.631090 11.00000 -1.20000 AFIX 0 C5 1 0.361939 0.691491 0.588348 11.00000 0.03677 0.04778 = 0.02468 0.00651 -0.00084 0.01170 AFIX 43 H5 2 0.421786 0.698063 0.626460 11.00000 -1.20000 AFIX 0 C6 1 0.315925 0.723816 0.528951 11.00000 0.03361 0.02719 = 0.02956 0.00644 0.00483 0.00148 AFIX 43 H6 2 0.344705 0.752506 0.526171 11.00000 -1.20000 AFIX 0 C7 1 0.063923 0.734871 0.329917 11.00000 0.03508 0.01399 = 0.02372 0.00127 -0.00204 0.00160 C8 1 -0.016822 0.729124 0.363997 11.00000 0.04016 0.02123 = 0.02819 0.00174 0.00303 -0.00168 AFIX 43 H8 2 -0.015231 0.736411 0.424077 11.00000 -1.20000 AFIX 0 C9 1 -0.101216 0.712557 0.310201 11.00000 0.03661 0.03387 = 0.04947 0.00910 0.00052 -0.00724 AFIX 43 H9 2 -0.157665 0.709551 0.332838 11.00000 -1.20000 AFIX 0 C10 1 -0.101459 0.700511 0.222955 11.00000 0.05482 0.03302 = 0.04096 0.00014 -0.01907 -0.01048 AFIX 43 H10 2 -0.158181 0.688693 0.186574 11.00000 -1.20000 AFIX 0 C11 1 -0.020924 0.705506 0.189042 11.00000 0.05483 0.03602 = 0.02560 -0.00659 -0.00728 -0.00367 AFIX 43 H11 2 -0.021778 0.696936 0.129722 11.00000 -1.20000 AFIX 0 C12 1 0.061736 0.723111 0.241678 11.00000 0.04449 0.02743 = 0.02147 -0.00388 -0.00009 0.00380 AFIX 43 H12 2 0.117156 0.727232 0.217896 11.00000 -1.20000 AFIX 0 C13 1 0.131493 0.799369 0.467901 11.00000 0.03409 0.01556 = 0.02324 0.00046 0.00938 -0.00369 C14 1 0.061240 0.834602 0.425180 11.00000 0.03089 0.01346 = 0.02154 -0.00208 0.00551 -0.00413 C15 1 -0.021532 0.839767 0.457574 11.00000 0.03514 0.01982 = 0.02456 -0.00015 0.01045 -0.00305 AFIX 43 H15 2 -0.030672 0.821997 0.506184 11.00000 -1.20000 AFIX 0 C16 1 -0.090571 0.870510 0.419685 11.00000 0.02735 0.02883 = 0.03075 0.00169 0.01531 -0.00195 AFIX 43 H16 2 -0.147837 0.873396 0.441058 11.00000 -1.20000 AFIX 0 C17 1 -0.075804 0.897258 0.349980 11.00000 0.02707 0.02159 = 0.02628 -0.00019 0.00723 -0.00275 AFIX 43 H17 2 -0.123691 0.918029 0.322753 11.00000 -1.20000 AFIX 0 C18 1 0.008890 0.893636 0.320127 11.00000 0.02875 0.01785 = 0.01631 -0.00066 0.00482 -0.00557 C19 1 0.077134 0.861516 0.355956 11.00000 0.02553 0.01588 = 0.02281 -0.00205 0.00763 -0.00245 AFIX 43 H19 2 0.133632 0.858000 0.333577 11.00000 -1.20000 AFIX 0 C20 1 0.023063 0.926137 0.249764 11.00000 0.02965 0.01903 = 0.01614 -0.00110 -0.00133 -0.00289 C21 1 0.165378 0.978769 0.367573 11.00000 0.02059 0.01378 = 0.02434 0.00009 0.00222 -0.00302 C22 1 0.260692 0.980159 0.415805 11.00000 0.02494 0.02588 = 0.02984 -0.00421 0.00065 0.00010 AFIX 43 H22 2 0.310175 0.966603 0.392399 11.00000 -1.20000 AFIX 0 C23 1 0.282308 1.001410 0.497783 11.00000 0.03217 0.03427 = 0.03506 -0.01164 -0.00034 -0.00078 AFIX 43 H23 2 0.346742 1.002593 0.530016 11.00000 -1.20000 AFIX 0 C24 1 0.210548 1.020808 0.532573 11.00000 0.03701 0.02800 = 0.02919 -0.00810 0.00267 -0.00835 AFIX 43 H24 2 0.225906 1.035398 0.588470 11.00000 -1.20000 AFIX 0 C25 1 0.115946 1.019070 0.486135 11.00000 0.03148 0.02881 = 0.03366 -0.00809 0.01367 -0.00464 AFIX 43 H25 2 0.066662 1.032210 0.510423 11.00000 -1.20000 AFIX 0 C26 1 0.093850 0.998092 0.404282 11.00000 0.02065 0.02248 = 0.03083 -0.00280 0.00921 -0.00639 AFIX 43 H26 2 0.029138 0.996859 0.372770 11.00000 -1.20000 PART 1 AFIX 76 C27 1 0.111370 0.997247 0.175584 21.00000 0.03377 0.02400 = 0.02723 0.00536 0.00595 -0.00587 C28 1 0.090753 1.041131 0.197015 21.00000 0.02755 0.02361 = 0.02951 0.00201 0.00216 -0.00230 AFIX 43 H28 2 0.095346 1.049356 0.257111 21.00000 -1.20000 AFIX 75 C29 1 0.063416 1.072983 0.130516 21.00000 0.05587 0.02372 = 0.04471 0.00376 -0.00003 -0.00033 AFIX 43 H29 2 0.049326 1.102976 0.145164 21.00000 -1.20000 AFIX 75 C30 1 0.056696 1.060949 0.042587 21.00000 0.06460 0.04014 = 0.05073 0.01158 -0.00157 -0.00718 AFIX 43 H30 2 0.038013 1.082718 -0.002862 21.00000 -1.20000 AFIX 75 C31 1 0.077313 1.017065 0.021155 21.00000 0.07585 0.05738 = 0.04700 0.00779 0.01470 0.00235 AFIX 43 H31 2 0.072720 1.008840 -0.038941 21.00000 -1.20000 AFIX 75 C32 1 0.104649 0.985213 0.087652 21.00000 0.05351 0.03770 = 0.03654 0.00701 0.00768 0.00048 AFIX 43 H32 2 0.118740 0.955219 0.073004 21.00000 -1.20000 PART 2 AFIX 76 C27A 1 0.119285 1.000286 0.183101 -21.00000 0.03377 0.02400 = 0.02723 0.00536 0.00595 -0.00587 C28A 1 0.064108 1.037187 0.196471 -21.00000 0.02755 0.02361 = 0.02951 0.00201 0.00216 -0.00230 AFIX 43 H28A 2 0.034220 1.037755 0.245718 -21.00000 -1.20000 AFIX 75 C29A 1 0.052662 1.073257 0.137786 -21.00000 0.05587 0.02372 = 0.04471 0.00376 -0.00003 -0.00033 AFIX 43 H29A 2 0.014950 1.098478 0.146924 -21.00000 -1.20000 AFIX 75 C30A 1 0.096392 1.072427 0.065730 -21.00000 0.06460 0.04014 = 0.05073 0.01158 -0.00157 -0.00718 AFIX 43 H30A 2 0.088569 1.097079 0.025621 -21.00000 -1.20000 AFIX 75 C31A 1 0.151570 1.035526 0.052359 -21.00000 0.07585 0.05738 = 0.04700 0.00779 0.01470 0.00235 AFIX 43 H31A 2 0.181458 1.034958 0.003112 -21.00000 -1.20000 AFIX 75 C32A 1 0.163017 0.999455 0.111043 -21.00000 0.05351 0.03770 = 0.03654 0.00701 0.00768 0.00048 AFIX 43 H32A 2 0.200729 0.974235 0.101905 -21.00000 -1.20000 PART 0 AFIX 0 C33 1 0.315440 0.692548 0.151592 11.00000 0.02307 0.02725 = 0.02122 -0.00589 0.00528 -0.00111 C34 1 0.244952 0.709705 0.082066 11.00000 0.03083 0.02804 = 0.02494 -0.00398 -0.00303 0.00392 AFIX 43 H34 2 0.237673 0.741369 0.074006 11.00000 -1.20000 AFIX 0 C35 1 0.185591 0.680313 0.024805 11.00000 0.02830 0.04462 = 0.02812 -0.00711 -0.00414 -0.00032 AFIX 43 H35 2 0.138598 0.691935 -0.022850 11.00000 -1.20000 AFIX 0 C36 1 0.195124 0.634394 0.037374 11.00000 0.02867 0.04449 = 0.03347 -0.02024 0.00751 -0.01087 AFIX 43 H36 2 0.154599 0.614434 -0.001727 11.00000 -1.20000 AFIX 0 C37 1 0.263141 0.617262 0.106375 11.00000 0.03888 0.02031 = 0.03923 -0.00917 0.00955 -0.00837 AFIX 43 H37 2 0.268978 0.585581 0.114959 11.00000 -1.20000 AFIX 0 C38 1 0.323563 0.646442 0.163758 11.00000 0.03362 0.02324 = 0.03055 -0.00407 0.00348 -0.00226 AFIX 43 H38 2 0.370339 0.634522 0.211250 11.00000 -1.20000 AFIX 0 C39 1 0.481617 0.703176 0.299782 11.00000 0.02994 0.01987 = 0.02202 0.00005 0.00262 -0.00075 C40 1 0.489640 0.707686 0.390274 11.00000 0.03783 0.03294 = 0.02443 -0.00446 -0.00591 0.00823 AFIX 43 H40 2 0.443260 0.724648 0.412117 11.00000 -1.20000 AFIX 0 C41 1 0.564931 0.687597 0.449103 11.00000 0.05097 0.04234 = 0.02570 -0.00370 -0.00476 0.01045 AFIX 43 H41 2 0.569582 0.690709 0.510979 11.00000 -1.20000 AFIX 0 C42 1 0.633348 0.663030 0.418113 11.00000 0.03927 0.04459 = 0.03939 -0.00345 -0.01188 0.01357 AFIX 43 H42 2 0.685167 0.649550 0.458561 11.00000 -1.20000 AFIX 0 C43 1 0.625888 0.658208 0.327993 11.00000 0.03696 0.03531 = 0.04193 -0.00152 0.00178 0.01249 AFIX 43 H43 2 0.672673 0.641280 0.306662 11.00000 -1.20000 AFIX 0 C44 1 0.550017 0.678060 0.268081 11.00000 0.03179 0.02651 = 0.02840 -0.00198 0.00197 0.00737 AFIX 43 H44 2 0.544939 0.674517 0.206235 11.00000 -1.20000 AFIX 0 C45 1 0.460064 0.759761 0.152790 11.00000 0.02877 0.01905 = 0.02668 -0.00223 0.00430 0.00641 C46 1 0.533897 0.792731 0.197471 11.00000 0.02954 0.02264 = 0.02046 -0.00174 0.00246 0.00026 C47 1 0.630395 0.783376 0.204469 11.00000 0.03189 0.03364 = 0.03097 -0.00066 0.00739 0.00547 AFIX 43 H47 2 0.649533 0.756082 0.181133 11.00000 -1.20000 AFIX 0 C48 1 0.698857 0.814146 0.245788 11.00000 0.02264 0.04197 = 0.04722 0.00039 0.00831 0.00142 AFIX 43 H48 2 0.765014 0.807135 0.254051 11.00000 -1.20000 AFIX 0 C49 1 0.670181 0.855320 0.275069 11.00000 0.02366 0.04074 = 0.03214 -0.00141 0.00726 -0.00924 AFIX 43 H49 2 0.717010 0.876599 0.302182 11.00000 -1.20000 AFIX 0 C50 1 0.573005 0.865487 0.264790 11.00000 0.02998 0.02900 = 0.01986 -0.00315 0.00599 -0.00777 C51 1 0.505239 0.833163 0.229512 11.00000 0.02377 0.02376 = 0.02511 -0.00549 0.00602 -0.00280 AFIX 43 H51 2 0.439292 0.838654 0.227250 11.00000 -1.20000 AFIX 0 C52 1 0.546887 0.912365 0.286494 11.00000 0.03834 0.02842 = 0.02282 -0.00632 0.00925 -0.01385 C53 1 0.442812 0.926751 0.111973 11.00000 0.03952 0.03154 = 0.03075 -0.00050 0.01215 0.00342 C54 1 0.389235 0.894451 0.058221 11.00000 0.06078 0.06767 = 0.04051 -0.01473 0.02127 -0.01900 AFIX 43 H54 2 0.340652 0.878216 0.078280 11.00000 -1.20000 AFIX 0 C55 1 0.407021 0.885961 -0.025194 11.00000 0.08706 0.10331 = 0.04258 -0.03374 0.03014 -0.02082 AFIX 43 H55 2 0.371585 0.863288 -0.061472 11.00000 -1.20000 AFIX 0 C56 1 0.475198 0.910036 -0.055370 11.00000 0.08672 0.07798 = 0.04086 0.00071 0.03396 0.00778 AFIX 43 H56 2 0.485074 0.904937 -0.113375 11.00000 -1.20000 AFIX 0 C57 1 0.529004 0.941357 -0.002213 11.00000 0.05754 0.04833 = 0.05619 0.01834 0.03168 0.01186 AFIX 43 H57 2 0.577137 0.957596 -0.022947 11.00000 -1.20000 AFIX 0 C58 1 0.513775 0.949640 0.082138 11.00000 0.04139 0.03536 = 0.04208 0.00957 0.01839 0.00401 AFIX 43 H58 2 0.552275 0.971084 0.119269 11.00000 -1.20000 PART 1 AFIX 76 C59 1 0.431257 0.992208 0.258309 31.00000 0.03371 0.02869 = 0.03046 -0.00944 0.01682 -0.00743 C60 1 0.387564 1.022685 0.193996 31.00000 0.06456 0.03386 = 0.03828 0.00096 0.01662 0.00254 AFIX 43 H60 2 0.361184 1.012498 0.135683 31.00000 -1.20000 AFIX 75 C61 1 0.382469 1.068066 0.215005 31.00000 0.05194 0.04175 = 0.04158 0.00748 0.01596 0.00144 AFIX 43 H61 2 0.352607 1.088896 0.171050 31.00000 -1.20000 AFIX 75 C62 1 0.421067 1.082971 0.300326 31.00000 0.04706 0.04067 = 0.05211 -0.00571 0.01644 -0.01274 AFIX 43 H62 2 0.417585 1.113987 0.314684 31.00000 -1.20000 AFIX 75 C63 1 0.464760 1.052495 0.364640 31.00000 0.04897 0.04866 = 0.05722 -0.01900 0.00557 -0.00268 AFIX 43 H63 2 0.491140 1.062682 0.422953 31.00000 -1.20000 AFIX 75 C64 1 0.469856 1.007113 0.343632 31.00000 0.04536 0.04761 = 0.05490 -0.01263 0.00489 -0.00101 AFIX 43 H64 2 0.499718 0.986284 0.387587 31.00000 -1.20000 PART 2 AFIX 5 C59A 1 0.422703 0.995733 0.233825 -31.00000 0.03371 0.02869 = 0.03046 -0.00944 0.01682 -0.00743 C60A 1 0.355613 1.019153 0.171748 -31.00000 0.06456 0.03386 = 0.03828 0.00096 0.01662 0.00254 AFIX 43 H60A 2 0.320115 1.003942 0.121245 -31.00000 -1.20000 AFIX 5 C61A 1 0.340460 1.064834 0.183567 -31.00000 0.05194 0.04175 = 0.04158 0.00748 0.01596 0.00144 AFIX 43 H61A 2 0.294607 1.080844 0.141139 -31.00000 -1.20000 AFIX 5 C62A 1 0.392397 1.087090 0.257464 -31.00000 0.04706 0.04067 = 0.05211 -0.00571 0.01644 -0.01274 AFIX 43 H62A 2 0.382039 1.118309 0.265542 -31.00000 -1.20000 AFIX 5 C63A 1 0.459491 1.063665 0.319542 -31.00000 0.04897 0.04866 = 0.05722 -0.01900 0.00557 -0.00268 AFIX 43 H63A 2 0.494989 1.078875 0.370046 -31.00000 -1.20000 AFIX 5 C64A 1 0.474643 1.017984 0.307723 -31.00000 0.04536 0.04761 = 0.05490 -0.01263 0.00489 -0.00101 AFIX 43 H64A 2 0.520495 1.001973 0.350150 -31.00000 -1.20000 PART 0 AFIX 0 C65 1 0.796728 0.095541 0.388429 11.00000 0.07513 0.03329 = 0.04899 -0.00278 0.01961 -0.00246 AFIX 23 H65A 2 0.794089 0.128309 0.399929 11.00000 -1.20000 H65B 2 0.784636 0.079400 0.440975 11.00000 -1.20000 AFIX 0 CL3 5 0.910250 0.081727 0.373354 11.00000 0.06224 0.04846 = 0.06177 0.00354 0.00761 0.00220 CL4 5 0.706315 0.081525 0.295708 11.00000 0.06026 0.08812 = 0.08404 -0.01533 0.01266 -0.00529 C66 1 0.818645 0.013023 0.163490 10.50000 0.03920 0.02991 = 0.03306 0.01146 0.00220 0.01605 AFIX 23 H66A 2 0.844694 0.034058 0.212389 10.50000 -1.20000 H66B 2 0.873323 -0.001840 0.145177 10.50000 -1.20000 AFIX 0 CL5 5 0.747941 -0.028236 0.201581 10.50000 0.03925 0.03772 = 0.06385 0.02259 0.00029 0.00081 CL6 5 0.753363 0.043105 0.075288 10.50000 0.05856 0.05468 = 0.03774 0.01912 0.01160 0.03199 HKLF 4 REM MSB487a_0m in P2(1)/n REM R1 = 0.0565 for 10252 Fo > 4sig(Fo) and 0.0843 for all 14041 data REM 759 parameters refined using 146 restraints END WGHT 0.0545 22.2529 REM Highest difference peak 1.345, deepest hole -1.110, 1-sigma level 0.124 Q1 1 0.2242 0.7799 0.3149 11.00000 0.05 1.35 Q2 1 0.3358 0.7812 0.2765 11.00000 0.05 1.33 Q3 1 0.2182 0.9038 0.2598 11.00000 0.05 1.30 Q4 1 0.3272 0.9033 0.2160 11.00000 0.05 1.20 Q5 1 0.3063 0.7807 0.3545 11.00000 0.05 1.04 ; _database_code_depnum_ccdc_archive 'CCDC 934911'