data_publication_text _publ_contact_author_name 'Matthew P. Shores' _publ_contact_author_address ;Colorado State University 1872 Campus Delivery Fort Collins, CO 80523 ; _publ_contact_author_email shores@lamar.colostate.edu loop_ _publ_author_name _publ_author_address 'Shores, Matthew P. ' ;Colorado State University 1872 Campus Delivery Fort Collins, CO 80523 ; data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound 1 in text' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H86 Cr2 N2 P8' _chemical_formula_weight 1018.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3602(2) _cell_length_b 12.7197(2) _cell_length_c 34.7671(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.2980(10) _cell_angle_gamma 90.00 _cell_volume 5456.96(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8442 _exptl_absorpt_correction_T_max 0.9426 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The dmpe ligands surrounding one of the Cr atoms were disordered over two sites, and the occupancies for the ligands were allowed to refine freely to values of 90% and 10%. For the 10% occupied ligands, hydrogen atoms were not included in the refinement. Carbon and phosphorus atoms in the 90% occupied ligands were refined anisotropically. The methylcyclopentane molecule was modeled with two of the carbon atoms in the ring being disordered over two sites at 50% occupancy. Substitution of the NN moiety by (CC)2- caused R1 to increase from 4.65 % to 5.50 % for Fo > 4sigma(Fo), and the mean Ueq parameter decreased from 0.017 A2 to 0.007 A2 supporting the assignment of dinitrogen as the bridging species. The short inter-hydrogen A level alert arises from the short distance between H atoms of different disordered dmpe groups. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76045 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0538 _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 -35 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11158 _reflns_number_gt 8086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0437P)^2^+6.3466P] 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 11158 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Cr1 Cr 0.00172(4) 0.59672(3) 0.131966(13) 0.01711(11) Uani 1 1 d . . . Cr2 Cr -0.22893(3) 0.90064(3) 0.093529(13) 0.01666(11) Uani 1 1 d . A . P1 P -0.10144(7) 0.52740(7) 0.18013(2) 0.0213(3) Uani 0.910(2) 1 d P A 1 P1B P -0.0629(7) 0.5840(7) 0.1931(3) 0.019(2) Uiso 0.090(2) 1 d P A 2 P2 P -0.11242(13) 0.49041(12) 0.09288(4) 0.0223(3) Uani 0.910(2) 1 d P A 1 P2B P -0.1093(17) 0.4921(16) 0.1034(5) 0.027(3) Uiso 0.090(2) 1 d P A 2 P3 P 0.1364(3) 0.6772(3) 0.17077(9) 0.0218(4) Uani 0.910(2) 1 d P A 1 P3B P 0.140(4) 0.669(4) 0.1755(12) 0.027(3) Uiso 0.090(2) 1 d P A 2 P4 P 0.12159(9) 0.62601(10) 0.08435(3) 0.0224(2) Uani 0.910(2) 1 d P A 1 P4B P 0.0988(11) 0.5939(10) 0.0776(4) 0.027(3) Uiso 0.090(2) 1 d P A 2 P5 P -0.40125(6) 0.82792(6) 0.09893(2) 0.02093(17) Uani 1 1 d . . . P6 P -0.26800(6) 0.86319(6) 0.02763(2) 0.02377(18) Uani 1 1 d . . . P7 P -0.21049(6) 0.96910(6) 0.15567(2) 0.02262(18) Uani 1 1 d . . . P8 P -0.08388(6) 1.01099(6) 0.08360(2) 0.02351(18) Uani 1 1 d . . . N2 N -0.14219(18) 0.78298(18) 0.10777(6) 0.0165(5) Uani 1 1 d . . . N1 N -0.08471(18) 0.71395(18) 0.11857(6) 0.0159(5) Uani 1 1 d . A . C1 C 0.0878(2) 0.4625(2) 0.14397(8) 0.0224(6) Uani 1 1 d . A . C2 C 0.1337(2) 0.3786(2) 0.15001(9) 0.0238(7) Uani 1 1 d . . . C3 C -0.3126(2) 1.0359(2) 0.08185(8) 0.0212(6) Uani 1 1 d . . . C4 C -0.3569(2) 1.1199(2) 0.07496(8) 0.0218(6) Uani 1 1 d . A . C5 C 0.1826(2) 0.2759(2) 0.15391(9) 0.0220(6) Uani 1 1 d . A . C6 C -0.4036(2) 1.2217(2) 0.06683(9) 0.0223(7) Uani 1 1 d . . . C7 C 0.1750(3) 0.2155(3) 0.18725(10) 0.0333(8) Uani 1 1 d . . . H7 H 0.1390 0.2433 0.2084 0.040 Uiso 1 1 calc R A . C8 C 0.2197(3) 0.1149(3) 0.18981(10) 0.0375(9) Uani 1 1 d . A . H8 H 0.2127 0.0745 0.2125 0.045 Uiso 1 1 calc R . . C9 C 0.2739(3) 0.0735(2) 0.15972(10) 0.0314(8) Uani 1 1 d . . . H9 H 0.3050 0.0053 0.1617 0.038 Uiso 1 1 calc R A . C10 C 0.2824(2) 0.1326(2) 0.12657(9) 0.0274(7) Uani 1 1 d . A . H10 H 0.3198 0.1048 0.1057 0.033 Uiso 1 1 calc R . . C11 C 0.2370(2) 0.2315(2) 0.12357(9) 0.0248(7) Uani 1 1 d . . . H11 H 0.2427 0.2703 0.1004 0.030 Uiso 1 1 calc R A . C12 C -0.3738(3) 1.2805(3) 0.03512(9) 0.0303(7) Uani 1 1 d . A . H12 H -0.3234 1.2523 0.0183 0.036 Uiso 1 1 calc R . . C13 C -0.4172(3) 1.3796(3) 0.02812(11) 0.0402(9) Uani 1 1 d . . . H13 H -0.3963 1.4185 0.0064 0.048 Uiso 1 1 calc R A . C14 C -0.4899(3) 1.4223(3) 0.05210(13) 0.0476(11) Uani 1 1 d . A . H14 H -0.5187 1.4906 0.0473 0.057 Uiso 1 1 calc R . . C15 C -0.5206(3) 1.3647(3) 0.08321(12) 0.0423(9) Uani 1 1 d . . . H15 H -0.5713 1.3936 0.0998 0.051 Uiso 1 1 calc R A . C16 C -0.4788(2) 1.2654(3) 0.09068(10) 0.0314(8) Uani 1 1 d . A . H16 H -0.5013 1.2267 0.1122 0.038 Uiso 1 1 calc R . . C17 C 0.2333(3) 0.7132(3) 0.10283(10) 0.0312(9) Uani 0.910(2) 1 d P A 1 H17A H 0.2973 0.7043 0.0873 0.037 Uiso 0.910(2) 1 calc PR A 1 H17B H 0.2101 0.7877 0.1012 0.037 Uiso 0.910(2) 1 calc PR A 1 C17B C 0.140(3) 0.655(3) 0.2239(10) 0.018(7) Uiso 0.090(2) 1 d P A 2 H17C H 0.1716 0.5867 0.2325 0.022 Uiso 0.090(2) 1 calc PR A 2 H17D H 0.1794 0.7128 0.2374 0.022 Uiso 0.090(2) 1 calc PR A 2 C18 C 0.2621(3) 0.6834(3) 0.14468(11) 0.0320(9) Uani 0.910(2) 1 d P A 1 H18A H 0.3119 0.7364 0.1568 0.038 Uiso 0.910(2) 1 calc PR A 1 H18B H 0.2990 0.6143 0.1458 0.038 Uiso 0.910(2) 1 calc PR A 1 C18B C 0.013(2) 0.659(2) 0.2308(9) 0.014(6) Uiso 0.090(2) 1 d P A 2 H18C H -0.0120 0.7334 0.2302 0.017 Uiso 0.090(2) 1 calc PR A 2 H18D H -0.0007 0.6298 0.2564 0.017 Uiso 0.090(2) 1 calc PR A 2 C19 C -0.1732(3) 0.4080(3) 0.16148(10) 0.0311(8) Uani 0.910(2) 1 d P A 1 H19A H -0.1220 0.3483 0.1609 0.037 Uiso 0.910(2) 1 calc PR A 1 H19B H -0.2317 0.3891 0.1785 0.037 Uiso 0.910(2) 1 calc PR A 1 C20 C -0.2207(3) 0.4307(3) 0.12114(11) 0.0327(9) Uani 0.910(2) 1 d P A 1 H20A H -0.2826 0.4798 0.1222 0.039 Uiso 0.910(2) 1 calc PR A 1 H20B H -0.2471 0.3648 0.1087 0.039 Uiso 0.910(2) 1 calc PR A 1 C21 C -0.0850(3) 1.0512(3) 0.16044(10) 0.0379(8) Uani 1 1 d . . . H21A H -0.0915 1.1033 0.1813 0.046 Uiso 1 1 calc R . . H21B H -0.0216 1.0059 0.1672 0.046 Uiso 1 1 calc R . . C22 C -0.0690(3) 1.1071(3) 0.12300(10) 0.0370(8) Uani 1 1 d . . . H22A H 0.0040 1.1392 0.1236 0.044 Uiso 1 1 calc R . . H22B H -0.1235 1.1637 0.1190 0.044 Uiso 1 1 calc R . . C23 C -0.4694(3) 0.8139(3) 0.05030(10) 0.0398(9) Uani 1 1 d . . . H23A H -0.5290 0.7621 0.0512 0.048 Uiso 1 1 calc R . . H23B H -0.5012 0.8822 0.0420 0.048 Uiso 1 1 calc R . . C24 C -0.3913(3) 0.7787(3) 0.02209(10) 0.0400(9) Uani 1 1 d . . . H24A H -0.4244 0.7847 -0.0044 0.048 Uiso 1 1 calc R . . H24B H -0.3715 0.7042 0.0268 0.048 Uiso 1 1 calc R . . C25 C 0.1223(3) 0.8129(3) 0.18662(12) 0.0337(9) Uani 0.910(2) 1 d P A 1 H25A H 0.1909 0.8367 0.1993 0.051 Uiso 0.910(2) 1 calc PR A 1 H25B H 0.0648 0.8172 0.2048 0.051 Uiso 0.910(2) 1 calc PR A 1 H25C H 0.1038 0.8577 0.1643 0.051 Uiso 0.910(2) 1 calc PR A 1 C26 C 0.1909(3) 0.6173(3) 0.21632(11) 0.0378(10) Uani 0.910(2) 1 d P A 1 H26A H 0.2610 0.6491 0.2239 0.057 Uiso 0.910(2) 1 calc PR A 1 H26B H 0.2002 0.5415 0.2126 0.057 Uiso 0.910(2) 1 calc PR A 1 H26C H 0.1402 0.6294 0.2365 0.057 Uiso 0.910(2) 1 calc PR A 1 C27 C 0.2023(4) 0.5185(3) 0.06554(14) 0.0388(11) Uani 0.910(2) 1 d P A 1 H27A H 0.1539 0.4670 0.0525 0.058 Uiso 0.910(2) 1 calc PR A 1 H27B H 0.2439 0.4843 0.0869 0.058 Uiso 0.910(2) 1 calc PR A 1 H27C H 0.2521 0.5467 0.0472 0.058 Uiso 0.910(2) 1 calc PR A 1 C28 C 0.0790(4) 0.6920(4) 0.03932(12) 0.0342(10) Uani 0.910(2) 1 d P A 1 H28A H 0.1428 0.7195 0.0272 0.051 Uiso 0.910(2) 1 calc PR A 1 H28B H 0.0301 0.7502 0.0447 0.051 Uiso 0.910(2) 1 calc PR A 1 H28C H 0.0412 0.6418 0.0219 0.051 Uiso 0.910(2) 1 calc PR A 1 C29 C -0.0625(3) 0.3740(3) 0.06890(11) 0.0372(9) Uani 0.910(2) 1 d P A 1 H29A H -0.1238 0.3353 0.0566 0.056 Uiso 0.910(2) 1 calc PR A 1 H29B H -0.0238 0.3288 0.0879 0.056 Uiso 0.910(2) 1 calc PR A 1 H29C H -0.0132 0.3954 0.0493 0.056 Uiso 0.910(2) 1 calc PR A 1 C30 C -0.1922(3) 0.5522(3) 0.05329(11) 0.0326(9) Uani 0.910(2) 1 d P A 1 H30A H -0.1480 0.5587 0.0309 0.049 Uiso 0.910(2) 1 calc PR A 1 H30B H -0.2154 0.6222 0.0612 0.049 Uiso 0.910(2) 1 calc PR A 1 H30C H -0.2561 0.5090 0.0465 0.049 Uiso 0.910(2) 1 calc PR A 1 C31 C -0.2139(3) 0.6069(4) 0.19853(13) 0.0294(11) Uani 0.910(2) 1 d P A 1 H31A H -0.2697 0.5598 0.2077 0.044 Uiso 0.910(2) 1 calc PR A 1 H31B H -0.2454 0.6513 0.1778 0.044 Uiso 0.910(2) 1 calc PR A 1 H31C H -0.1857 0.6513 0.2199 0.044 Uiso 0.910(2) 1 calc PR A 1 C32 C -0.0476(4) 0.4725(6) 0.2252(2) 0.0378(15) Uani 0.910(2) 1 d P A 1 H32A H -0.0212 0.5293 0.2423 0.057 Uiso 0.910(2) 1 calc PR A 1 H32B H 0.0123 0.4247 0.2203 0.057 Uiso 0.910(2) 1 calc PR A 1 H32C H -0.1048 0.4336 0.2374 0.057 Uiso 0.910(2) 1 calc PR A 1 C33 C 0.0524(2) 0.9555(3) 0.08231(10) 0.0315(8) Uani 1 1 d . . . H33A H 0.1062 1.0111 0.0874 0.047 Uiso 1 1 calc R . . H33B H 0.0619 0.9250 0.0569 0.047 Uiso 1 1 calc R . . H33C H 0.0621 0.9007 0.1020 0.047 Uiso 1 1 calc R . . C34 C -0.0825(3) 1.0994(3) 0.04183(11) 0.0380(8) Uani 1 1 d . . . H34A H -0.1522 1.1360 0.0386 0.057 Uiso 1 1 calc R . . H34B H -0.0704 1.0583 0.0186 0.057 Uiso 1 1 calc R . . H34C H -0.0241 1.1510 0.0460 0.057 Uiso 1 1 calc R . . C35 C -0.1868(3) 0.8812(3) 0.19691(9) 0.0327(8) Uani 1 1 d . . . H35A H -0.1644 0.9226 0.2198 0.049 Uiso 1 1 calc R . . H35B H -0.1295 0.8310 0.1915 0.049 Uiso 1 1 calc R . . H35C H -0.2536 0.8430 0.2016 0.049 Uiso 1 1 calc R . . C36 C -0.3085(3) 1.0603(3) 0.17411(10) 0.0411(9) Uani 1 1 d . . . H36A H -0.3781 1.0245 0.1761 0.062 Uiso 1 1 calc R . . H36B H -0.3179 1.1202 0.1565 0.062 Uiso 1 1 calc R . . H36C H -0.2822 1.0854 0.1996 0.062 Uiso 1 1 calc R . . C37 C -0.5081(3) 0.8983(3) 0.12270(11) 0.0387(9) Uani 1 1 d . . . H37A H -0.5787 0.8675 0.1149 0.058 Uiso 1 1 calc R . . H37B H -0.5073 0.9726 0.1152 0.058 Uiso 1 1 calc R . . H37C H -0.4955 0.8924 0.1507 0.058 Uiso 1 1 calc R . . C38 C -0.4206(3) 0.6958(3) 0.11810(11) 0.0356(8) Uani 1 1 d . . . H38A H -0.4055 0.6964 0.1461 0.053 Uiso 1 1 calc R . . H38B H -0.3711 0.6469 0.1063 0.053 Uiso 1 1 calc R . . H38C H -0.4956 0.6734 0.1122 0.053 Uiso 1 1 calc R . . C39 C -0.3111(4) 0.9688(3) -0.00577(10) 0.0490(10) Uani 1 1 d . . . H39A H -0.2485 1.0126 -0.0112 0.074 Uiso 1 1 calc R . . H39B H -0.3660 1.0122 0.0059 0.074 Uiso 1 1 calc R . . H39C H -0.3417 0.9382 -0.0299 0.074 Uiso 1 1 calc R . . C40 C -0.1791(3) 0.7929(3) -0.00374(10) 0.0390(9) Uani 1 1 d . . . H40A H -0.2172 0.7810 -0.0289 0.058 Uiso 1 1 calc R . . H40B H -0.1585 0.7252 0.0080 0.058 Uiso 1 1 calc R . . H40C H -0.1138 0.8349 -0.0071 0.058 Uiso 1 1 calc R . . C94A C -0.5540(9) 1.3833(8) 0.2475(3) 0.073(3) Uiso 0.50 1 d P B 3 H94A H -0.6340 1.3880 0.2446 0.088 Uiso 0.50 1 calc PR B 3 H94B H -0.5274 1.4412 0.2646 0.088 Uiso 0.50 1 calc PR B 3 C94B C -0.4408(14) 1.3890(13) 0.2521(5) 0.136(6) Uiso 0.50 1 d P B 4 H94C H -0.4478 1.4517 0.2686 0.163 Uiso 0.50 1 calc PR B 4 H94D H -0.3638 1.3718 0.2487 0.163 Uiso 0.50 1 calc PR B 4 C95 C -0.5214(9) 1.2790(6) 0.2653(2) 0.184(5) Uani 1 1 d . . . H95A H -0.4548 1.2871 0.2823 0.221 Uiso 1 1 calc R B 3 H95B H -0.5798 1.2518 0.2809 0.221 Uiso 1 1 calc R B 3 C96 C -0.5032(6) 1.2106(6) 0.23545(19) 0.110(2) Uani 1 1 d . B . H96A H -0.5617 1.1577 0.2323 0.132 Uiso 1 1 calc R . . H96B H -0.4328 1.1741 0.2397 0.132 Uiso 1 1 calc R . . C97 C -0.5028(7) 1.2868(5) 0.19924(18) 0.116(2) Uani 1 1 d . . . H97A H -0.4344 1.2791 0.1860 0.139 Uiso 1 1 calc R B . H97B H -0.5642 1.2702 0.1807 0.139 Uiso 1 1 calc R . . C98 C -0.5129(13) 1.3922(6) 0.2138(3) 0.228(7) Uani 1 1 d . B . H98 H -0.4355 1.4023 0.2232 0.273 Uiso 1 1 calc R C 3 C99 C -0.5196(5) 1.4758(5) 0.18744(17) 0.100(2) Uani 1 1 d . . . H99A H -0.5905 1.4746 0.1733 0.150 Uiso 1 1 calc R B . H99B H -0.4624 1.4686 0.1693 0.150 Uiso 1 1 calc R . . H99C H -0.5107 1.5425 0.2013 0.150 Uiso 1 1 calc R . . C19B C -0.036(3) 0.433(3) 0.0599(12) 0.037(10) Uiso 0.090(2) 1 d P A 2 H19C H 0.0152 0.3772 0.0691 0.044 Uiso 0.090(2) 1 calc PR A 2 H19D H -0.0901 0.4005 0.0413 0.044 Uiso 0.090(2) 1 calc PR A 2 C26B C 0.289(3) 0.660(3) 0.1688(14) 0.043(10) Uiso 0.090(2) 1 d P A 2 H26D H 0.3283 0.6479 0.1939 0.064 Uiso 0.090(2) 1 calc PR A 2 H26E H 0.3145 0.7253 0.1576 0.064 Uiso 0.090(2) 1 calc PR A 2 H26F H 0.3036 0.6010 0.1516 0.064 Uiso 0.090(2) 1 calc PR A 2 C30B C -0.242(4) 0.546(4) 0.0822(14) 0.053(12) Uiso 0.090(2) 1 d P A 2 H30D H -0.2712 0.4984 0.0619 0.079 Uiso 0.090(2) 1 calc PR A 2 H30E H -0.2302 0.6156 0.0712 0.079 Uiso 0.090(2) 1 calc PR A 2 H30F H -0.2938 0.5514 0.1024 0.079 Uiso 0.090(2) 1 calc PR A 2 C20B C 0.022(4) 0.516(4) 0.0409(14) 0.059(13) Uiso 0.090(2) 1 d P A 2 H20C H -0.0295 0.5617 0.0260 0.071 Uiso 0.090(2) 1 calc PR A 2 H20D H 0.0727 0.4849 0.0229 0.071 Uiso 0.090(2) 1 calc PR A 2 C27B C 0.239(4) 0.541(4) 0.0767(15) 0.040(14) Uiso 0.090(2) 1 d P A 2 H27D H 0.2425 0.4712 0.0889 0.060 Uiso 0.090(2) 1 calc PR A 2 H27E H 0.2898 0.5883 0.0908 0.060 Uiso 0.090(2) 1 calc PR A 2 H27F H 0.2595 0.5345 0.0499 0.060 Uiso 0.090(2) 1 calc PR A 2 C29B C -0.157(3) 0.374(3) 0.1235(10) 0.024(8) Uiso 0.090(2) 1 d P A 2 H29D H -0.1540 0.3795 0.1516 0.037 Uiso 0.090(2) 1 calc PR A 2 H29E H -0.1123 0.3149 0.1158 0.037 Uiso 0.090(2) 1 calc PR A 2 H29F H -0.2326 0.3618 0.1140 0.037 Uiso 0.090(2) 1 calc PR A 2 C25B C 0.159(3) 0.835(3) 0.1752(10) 0.013(6) Uiso 0.090(2) 1 d P A 2 H25D H 0.0888 0.8681 0.1684 0.019 Uiso 0.090(2) 1 calc PR A 2 H25E H 0.2110 0.8545 0.1563 0.019 Uiso 0.090(2) 1 calc PR A 2 H25F H 0.1854 0.8587 0.2009 0.019 Uiso 0.090(2) 1 calc PR A 2 C28B C 0.122(4) 0.711(5) 0.0428(18) 0.051(18) Uiso 0.090(2) 1 d P A 2 H28D H 0.1490 0.6844 0.0187 0.077 Uiso 0.090(2) 1 calc PR A 2 H28E H 0.1760 0.7595 0.0549 0.077 Uiso 0.090(2) 1 calc PR A 2 H28F H 0.0539 0.7488 0.0374 0.077 Uiso 0.090(2) 1 calc PR A 2 C32B C -0.020(4) 0.467(5) 0.226(2) 0.013(6) Uiso 0.090(2) 1 d P A 2 H32D H -0.0850 0.4354 0.2363 0.019 Uiso 0.090(2) 1 calc PR A 2 H32E H 0.0281 0.4920 0.2474 0.019 Uiso 0.090(2) 1 calc PR A 2 H32F H 0.0172 0.4145 0.2111 0.019 Uiso 0.090(2) 1 calc PR A 2 C31B C -0.190(3) 0.582(3) 0.1954(14) 0.013(3) Uiso 0.090(2) 1 d P A 2 H31D H -0.2078 0.5856 0.2225 0.019 Uiso 0.090(2) 1 calc PR A 2 H31E H -0.2187 0.5174 0.1837 0.019 Uiso 0.090(2) 1 calc PR A 2 H31F H -0.2211 0.6431 0.1815 0.019 Uiso 0.090(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0198(2) 0.0176(2) 0.0140(2) 0.00181(18) 0.00118(18) 0.00297(18) Cr2 0.0164(2) 0.0174(2) 0.0160(3) 0.00071(18) -0.00109(18) 0.00109(18) P1 0.0246(5) 0.0223(5) 0.0171(5) 0.0023(4) 0.0025(4) -0.0003(4) P2 0.0320(6) 0.0177(5) 0.0166(8) -0.0016(6) -0.0027(6) -0.0026(4) P3 0.0230(6) 0.0263(9) 0.0154(11) 0.0036(6) -0.0041(7) 0.0019(5) P4 0.0220(5) 0.0272(6) 0.0184(5) 0.0025(4) 0.0040(4) 0.0034(4) P5 0.0171(4) 0.0235(4) 0.0221(4) 0.0004(3) 0.0001(3) 0.0011(3) P6 0.0223(4) 0.0307(4) 0.0182(4) -0.0005(3) -0.0002(3) 0.0019(3) P7 0.0265(4) 0.0241(4) 0.0168(4) -0.0011(3) -0.0022(3) -0.0004(3) P8 0.0234(4) 0.0192(4) 0.0283(5) -0.0001(3) 0.0047(3) -0.0023(3) N2 0.0165(11) 0.0201(12) 0.0127(13) -0.0003(10) 0.0003(9) -0.0026(10) N1 0.0176(12) 0.0198(12) 0.0105(12) 0.0003(10) 0.0007(9) -0.0004(10) C1 0.0244(15) 0.0253(16) 0.0177(16) 0.0018(12) 0.0033(12) 0.0031(12) C2 0.0252(15) 0.0277(17) 0.0185(17) 0.0003(13) 0.0014(13) 0.0033(13) C3 0.0192(14) 0.0257(16) 0.0184(16) -0.0003(12) 0.0000(12) -0.0002(12) C4 0.0195(14) 0.0277(17) 0.0179(16) 0.0007(12) -0.0019(12) -0.0009(12) C5 0.0211(15) 0.0217(15) 0.0229(17) 0.0020(12) -0.0011(12) 0.0036(12) C6 0.0198(15) 0.0214(15) 0.0246(17) 0.0032(13) -0.0076(13) -0.0018(12) C7 0.042(2) 0.0335(18) 0.0251(19) 0.0029(15) 0.0094(15) 0.0127(15) C8 0.050(2) 0.0339(19) 0.030(2) 0.0100(15) 0.0099(17) 0.0155(16) C9 0.0322(18) 0.0226(16) 0.040(2) 0.0018(14) 0.0033(15) 0.0082(13) C10 0.0278(16) 0.0268(16) 0.0283(19) -0.0053(14) 0.0070(14) 0.0026(13) C11 0.0289(16) 0.0248(16) 0.0208(17) 0.0030(13) 0.0027(13) 0.0002(13) C12 0.0248(16) 0.0373(19) 0.0275(19) 0.0063(15) -0.0091(14) -0.0084(14) C13 0.040(2) 0.034(2) 0.043(2) 0.0209(17) -0.0231(18) -0.0140(16) C14 0.046(2) 0.0226(18) 0.070(3) 0.0122(19) -0.030(2) 0.0016(16) C15 0.035(2) 0.0329(19) 0.058(3) 0.0009(18) -0.0039(18) 0.0154(16) C16 0.0259(17) 0.0287(17) 0.039(2) 0.0078(15) -0.0029(15) 0.0053(14) C17 0.0190(17) 0.042(2) 0.032(2) 0.0064(17) 0.0016(15) -0.0006(15) C18 0.0232(18) 0.041(2) 0.031(2) 0.0046(17) -0.0011(16) -0.0005(16) C19 0.039(2) 0.0266(19) 0.028(2) 0.0020(15) 0.0097(16) -0.0069(16) C20 0.038(2) 0.0262(19) 0.034(2) -0.0002(16) 0.0006(17) -0.0111(16) C21 0.047(2) 0.0348(19) 0.031(2) -0.0065(16) -0.0077(16) -0.0117(16) C22 0.039(2) 0.0329(19) 0.040(2) -0.0089(16) 0.0081(16) -0.0072(15) C23 0.0299(18) 0.058(2) 0.031(2) -0.0017(17) -0.0052(15) -0.0124(17) C24 0.0291(18) 0.060(2) 0.030(2) -0.0066(18) -0.0055(15) -0.0076(17) C25 0.038(2) 0.031(2) 0.031(2) -0.0072(18) -0.0084(19) -0.0059(18) C26 0.040(2) 0.047(2) 0.025(2) 0.0081(18) -0.0110(18) -0.005(2) C27 0.041(3) 0.039(3) 0.039(3) -0.001(2) 0.019(2) 0.008(2) C28 0.041(3) 0.043(3) 0.020(2) 0.0080(17) 0.0014(19) -0.002(2) C29 0.055(3) 0.026(2) 0.030(2) -0.0092(17) -0.0010(19) -0.0001(18) C30 0.037(2) 0.0280(19) 0.031(2) 0.0008(16) -0.0113(17) -0.0076(16) C31 0.025(2) 0.037(3) 0.027(2) 0.0020(19) 0.0105(17) 0.0123(16) C32 0.033(3) 0.047(3) 0.034(3) 0.0175(19) 0.009(3) 0.009(3) C33 0.0209(16) 0.0307(18) 0.042(2) -0.0018(15) -0.0026(14) -0.0035(13) C34 0.040(2) 0.0297(18) 0.045(2) 0.0077(16) 0.0095(17) -0.0019(15) C35 0.0388(19) 0.0368(19) 0.0223(18) 0.0051(14) -0.0007(15) 0.0014(15) C36 0.047(2) 0.046(2) 0.029(2) -0.0161(17) -0.0038(17) 0.0180(18) C37 0.0265(17) 0.037(2) 0.053(2) -0.0060(17) 0.0105(16) 0.0037(15) C38 0.0239(17) 0.0312(18) 0.051(2) 0.0109(16) -0.0001(16) -0.0022(14) C39 0.075(3) 0.045(2) 0.025(2) 0.0032(17) -0.0112(19) 0.012(2) C40 0.040(2) 0.047(2) 0.030(2) -0.0072(16) 0.0021(16) 0.0033(17) C95 0.305(13) 0.124(7) 0.139(7) 0.030(6) 0.143(8) 0.093(8) C96 0.118(5) 0.118(6) 0.091(5) -0.004(4) -0.026(4) 0.013(4) C97 0.173(7) 0.103(5) 0.069(4) -0.015(4) -0.030(4) 0.020(5) C98 0.51(2) 0.072(5) 0.097(7) 0.006(5) -0.033(10) -0.022(9) C99 0.128(5) 0.093(5) 0.080(4) 0.009(4) 0.017(4) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 1.877(2) . ? Cr1 C1 2.042(3) . ? Cr1 P2B 2.12(2) . ? Cr1 P4B 2.295(14) . ? Cr1 P4 2.3146(11) . ? Cr1 P1B 2.319(9) . ? Cr1 P3 2.320(4) . ? Cr1 P2 2.3334(15) . ? Cr1 P1 2.3350(9) . ? Cr1 P3B 2.40(5) . ? Cr2 N2 1.890(2) . ? Cr2 C3 2.036(3) . ? Cr2 P8 2.3184(9) . ? Cr2 P7 2.3283(9) . ? Cr2 P5 2.3395(9) . ? Cr2 P6 2.3626(9) . ? P1 C32 1.807(7) . ? P1 C19 1.856(4) . ? P1 C31 1.862(4) . ? P1B C31B 1.57(4) . ? P1B C18B 1.84(3) . ? P1B C32B 1.93(7) . ? P2 C29 1.824(4) . ? P2 C30 1.825(4) . ? P2 C20 1.866(4) . ? P2B C29B 1.78(4) . ? P2B C30B 1.89(5) . ? P2B C19B 1.96(4) . ? P3 C25 1.823(6) . ? P3 C18 1.846(5) . ? P3 C26 1.849(4) . ? P3B C17B 1.69(5) . ? P3B C26B 1.88(6) . ? P3B C25B 2.13(6) . ? P4 C28 1.827(4) . ? P4 C27 1.835(4) . ? P4 C17 1.857(4) . ? P4B C20B 1.83(5) . ? P4B C27B 1.87(5) . ? P4B C28B 1.95(6) . ? P5 C38 1.828(3) . ? P5 C37 1.831(3) . ? P5 C23 1.854(3) . ? P6 C40 1.826(3) . ? P6 C39 1.835(4) . ? P6 C24 1.866(3) . ? P7 C36 1.820(3) . ? P7 C35 1.828(3) . ? P7 C21 1.869(3) . ? P8 C33 1.829(3) . ? P8 C22 1.837(3) . ? P8 C34 1.837(3) . ? N2 N1 1.177(3) . ? C1 C2 1.222(4) . ? C2 C5 1.441(4) . ? C3 C4 1.218(4) . ? C4 C6 1.440(4) . ? C5 C7 1.399(4) . ? C5 C11 1.402(4) . ? C6 C16 1.395(4) . ? C6 C12 1.399(4) . ? C7 C8 1.393(4) . ? C8 C9 1.379(5) . ? C9 C10 1.385(5) . ? C10 C11 1.379(4) . ? C12 C13 1.386(5) . ? C13 C14 1.373(6) . ? C14 C15 1.378(5) . ? C15 C16 1.384(4) . ? C17 C18 1.526(5) . ? C17B C18B 1.60(4) . ? C19 C20 1.517(5) . ? C21 C22 1.507(5) . ? C23 C24 1.485(5) . ? C94A C98 1.309(13) . ? C94A C95 1.508(12) . ? C94B C98 1.557(18) . ? C94B C95 1.793(17) . ? C95 C96 1.383(9) . ? C96 C97 1.589(9) . ? C97 C98 1.441(9) . ? C98 C99 1.404(9) . ? C19B C20B 1.46(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 C1 175.68(11) . . ? N1 Cr1 P2B 92.2(6) . . ? C1 Cr1 P2B 83.5(6) . . ? N1 Cr1 P4B 97.2(3) . . ? C1 Cr1 P4B 82.2(3) . . ? P2B Cr1 P4B 87.7(6) . . ? N1 Cr1 P4 94.20(7) . . ? C1 Cr1 P4 86.17(9) . . ? P2B Cr1 P4 101.0(5) . . ? P4B Cr1 P4 13.5(3) . . ? N1 Cr1 P1B 93.5(2) . . ? C1 Cr1 P1B 87.6(2) . . ? P2B Cr1 P1B 97.9(6) . . ? P4B Cr1 P1B 167.7(4) . . ? P4 Cr1 P1B 159.3(2) . . ? N1 Cr1 P3 99.95(11) . . ? C1 Cr1 P3 84.37(12) . . ? P2B Cr1 P3 166.9(6) . . ? P4B Cr1 P3 95.4(3) . . ? P4 Cr1 P3 82.96(10) . . ? P1B Cr1 P3 76.8(3) . . ? N1 Cr1 P2 89.97(8) . . ? C1 Cr1 P2 85.70(9) . . ? P2B Cr1 P2 7.6(5) . . ? P4B Cr1 P2 80.7(3) . . ? P4 Cr1 P2 93.85(5) . . ? P1B Cr1 P2 105.4(2) . . ? P3 Cr1 P2 169.75(10) . . ? N1 Cr1 P1 98.71(7) . . ? C1 Cr1 P1 80.64(8) . . ? P2B Cr1 P1 74.5(5) . . ? P4B Cr1 P1 156.5(3) . . ? P4 Cr1 P1 166.43(4) . . ? P1B Cr1 P1 23.9(2) . . ? P3 Cr1 P1 98.79(9) . . ? P2 Cr1 P1 82.07(4) . . ? N1 Cr1 P3B 103.2(10) . . ? C1 Cr1 P3B 81.1(10) . . ? P2B Cr1 P3B 162.7(11) . . ? P4B Cr1 P3B 98.0(11) . . ? P4 Cr1 P3B 85.9(11) . . ? P1B Cr1 P3B 73.6(11) . . ? P3 Cr1 P3B 4.5(10) . . ? P2 Cr1 P3B 166.8(10) . . ? P1 Cr1 P3B 95.1(10) . . ? N2 Cr2 C3 174.31(11) . . ? N2 Cr2 P8 94.96(7) . . ? C3 Cr2 P8 81.20(8) . . ? N2 Cr2 P7 91.68(7) . . ? C3 Cr2 P7 83.71(9) . . ? P8 Cr2 P7 82.90(3) . . ? N2 Cr2 P5 99.86(7) . . ? C3 Cr2 P5 84.02(8) . . ? P8 Cr2 P5 165.18(3) . . ? P7 Cr2 P5 96.57(3) . . ? N2 Cr2 P6 100.11(7) . . ? C3 Cr2 P6 84.48(9) . . ? P8 Cr2 P6 95.41(3) . . ? P7 Cr2 P6 168.19(3) . . ? P5 Cr2 P6 82.06(3) . . ? C32 P1 C19 97.5(3) . . ? C32 P1 C31 99.0(2) . . ? C19 P1 C31 102.3(2) . . ? C32 P1 Cr1 125.38(18) . . ? C19 P1 Cr1 109.15(12) . . ? C31 P1 Cr1 119.38(15) . . ? C31B P1B C18B 116.0(19) . . ? C31B P1B C32B 101(2) . . ? C18B P1B C32B 83(2) . . ? C31B P1B Cr1 116.3(18) . . ? C18B P1B Cr1 115.4(10) . . ? C32B P1B Cr1 120.0(19) . . ? C29 P2 C30 100.79(19) . . ? C29 P2 C20 100.49(19) . . ? C30 P2 C20 101.52(19) . . ? C29 P2 Cr1 121.84(15) . . ? C30 P2 Cr1 118.16(13) . . ? C20 P2 Cr1 110.91(13) . . ? C29B P2B C30B 99(2) . . ? C29B P2B C19B 99.0(19) . . ? C30B P2B C19B 105(2) . . ? C29B P2B Cr1 124.9(15) . . ? C30B P2B Cr1 118.8(18) . . ? C19B P2B Cr1 106.8(16) . . ? C25 P3 C18 101.9(3) . . ? C25 P3 C26 99.7(3) . . ? C18 P3 C26 99.4(2) . . ? C25 P3 Cr1 121.1(2) . . ? C18 P3 Cr1 109.2(2) . . ? C26 P3 Cr1 122.0(2) . . ? C17B P3B C26B 100(3) . . ? C17B P3B C25B 97(3) . . ? C26B P3B C25B 87(2) . . ? C17B P3B Cr1 123(3) . . ? C26B P3B Cr1 125(3) . . ? C25B P3B Cr1 116.7(18) . . ? C28 P4 C27 100.0(2) . . ? C28 P4 C17 101.2(2) . . ? C27 P4 C17 99.2(2) . . ? C28 P4 Cr1 121.47(16) . . ? C27 P4 Cr1 121.21(15) . . ? C17 P4 Cr1 110.03(13) . . ? C20B P4B C27B 104(2) . . ? C20B P4B C28B 94(2) . . ? C27B P4B C28B 95(2) . . ? C20B P4B Cr1 108.0(17) . . ? C27B P4B Cr1 123.4(18) . . ? C28B P4B Cr1 127.0(19) . . ? C38 P5 C37 99.88(16) . . ? C38 P5 C23 100.49(17) . . ? C37 P5 C23 99.03(17) . . ? C38 P5 Cr2 122.10(11) . . ? C37 P5 Cr2 121.77(12) . . ? C23 P5 Cr2 109.45(11) . . ? C40 P6 C39 98.23(18) . . ? C40 P6 C24 99.92(17) . . ? C39 P6 C24 98.70(19) . . ? C40 P6 Cr2 125.55(12) . . ? C39 P6 Cr2 120.11(13) . . ? C24 P6 Cr2 109.66(12) . . ? C36 P7 C35 101.15(17) . . ? C36 P7 C21 100.26(17) . . ? C35 P7 C21 100.18(16) . . ? C36 P7 Cr2 122.26(12) . . ? C35 P7 Cr2 120.12(12) . . ? C21 P7 Cr2 109.13(12) . . ? C33 P8 C22 102.84(16) . . ? C33 P8 C34 99.56(16) . . ? C22 P8 C34 100.19(17) . . ? C33 P8 Cr2 119.42(11) . . ? C22 P8 Cr2 109.69(11) . . ? C34 P8 Cr2 122.05(12) . . ? N1 N2 Cr2 175.4(2) . . ? N2 N1 Cr1 174.8(2) . . ? C2 C1 Cr1 175.8(3) . . ? C1 C2 C5 174.6(3) . . ? C4 C3 Cr2 176.2(2) . . ? C3 C4 C6 177.0(3) . . ? C7 C5 C11 117.3(3) . . ? C7 C5 C2 121.9(3) . . ? C11 C5 C2 120.7(3) . . ? C16 C6 C12 118.0(3) . . ? C16 C6 C4 121.0(3) . . ? C12 C6 C4 121.0(3) . . ? C8 C7 C5 120.8(3) . . ? C9 C8 C7 120.7(3) . . ? C8 C9 C10 119.2(3) . . ? C11 C10 C9 120.5(3) . . ? C10 C11 C5 121.4(3) . . ? C13 C12 C6 120.5(3) . . ? C14 C13 C12 120.9(3) . . ? C13 C14 C15 119.1(3) . . ? C14 C15 C16 121.1(4) . . ? C15 C16 C6 120.4(3) . . ? C18 C17 P4 108.0(2) . . ? C18B C17B P3B 102(3) . . ? C17 C18 P3 108.8(2) . . ? C17B C18B P1B 110(2) . . ? C20 C19 P1 108.6(2) . . ? C19 C20 P2 108.2(2) . . ? C22 C21 P7 109.7(2) . . ? C21 C22 P8 108.5(2) . . ? C24 C23 P5 110.7(2) . . ? C23 C24 P6 108.4(2) . . ? C98 C94A C95 109.5(9) . . ? C98 C94B C95 86.6(10) . . ? C96 C95 C94A 107.3(7) . . ? C96 C95 C94B 100.4(8) . . ? C94A C95 C94B 49.3(6) . . ? C95 C96 C97 102.7(6) . . ? C98 C97 C96 106.5(6) . . ? C94A C98 C99 129.7(11) . . ? C94A C98 C97 106.3(8) . . ? C99 C98 C97 118.5(7) . . ? C94A C98 C94B 57.8(8) . . ? C99 C98 C94B 125.9(10) . . ? C97 C98 C94B 102.7(10) . . ? C20B C19B P2B 109(3) . . ? C19B C20B P4B 109(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.792 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.076 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_common 'compound 2 in text' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H104 Cr2 N2 P8 Si2' _chemical_formula_weight 1093.25 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.0902(5) _cell_length_b 19.6306(5) _cell_length_c 34.3510(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12198.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4720 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8421 _exptl_absorpt_correction_T_max 0.9392 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; dmpe positional disorder around one of the Cr atoms was modeled as in 1 with occupancies refining to 58% and 42%, respectively. Three of the carbon atoms in the ethylene moieties of dmpe ligands surrounding one of the Cr atoms were disordered over two positions and their occupancies refined to 58% and 42%. A methyl substituent on a C2SiiPr3 ligand disordered over two positions refined to a 51:49 occupancy ratio. A methyl group on one of the dmpe ligands was modeled similarly with a 71:29 occupancy ratio. Substitution of the NN moiety for CC2- caused R1 to increase from 5.17% to 5.46% (for F0 > 4sigma( F0)) and the mean Ueq parameters on the atomsto shrink from 0.0134 A2 to 0.0026 A2. Disordered carbon atoms were left as isotropic, which accounts for the A level alert in the checkcif. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62977 _diffrn_reflns_av_R_equivalents 0.1140 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 24.71 _reflns_number_total 10399 _reflns_number_gt 6929 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0850P)^2^+34.0057P] 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 10399 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1511 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.35808(4) 0.18131(4) 0.05021(2) 0.0138(2) Uani 1 1 d . B . Cr2 Cr 0.33384(4) 0.06092(4) 0.17607(2) 0.0162(2) Uani 1 1 d . . . Si1 Si 0.38293(8) 0.31196(8) -0.07728(4) 0.0225(3) Uani 1 1 d . B . Si2 Si 0.32686(7) -0.08186(7) 0.30007(4) 0.0170(3) Uani 1 1 d . B . P1 P 0.42470(7) 0.27195(7) 0.07610(4) 0.0200(3) Uani 1 1 d . . . P2 P 0.47560(7) 0.14125(7) 0.03471(4) 0.0186(3) Uani 1 1 d . . . P3 P 0.24377(7) 0.23467(7) 0.05251(4) 0.0217(3) Uani 1 1 d . . . P4 P 0.29301(7) 0.10134(7) 0.01341(4) 0.0200(3) Uani 1 1 d . . . P5 P 0.21189(7) 0.02757(8) 0.16912(4) 0.0307(4) Uani 1 1 d . B . P8 P 0.45325(10) 0.08077(10) 0.19741(5) 0.0481(5) Uani 1 1 d . B . N1 N 0.3481(2) 0.13483(19) 0.09773(11) 0.0125(8) Uani 1 1 d . . . N2 N 0.3422(2) 0.10658(19) 0.12817(12) 0.0145(9) Uani 1 1 d . B . C1 C 0.3689(3) 0.2342(2) -0.00091(15) 0.0180(11) Uani 1 1 d . . . C2 C 0.3766(3) 0.2664(3) -0.03127(15) 0.0196(11) Uani 1 1 d . B . C3 C 0.3274(3) 0.0082(2) 0.22760(14) 0.0175(11) Uani 1 1 d . B . C4 C 0.3263(3) -0.0257(3) 0.25785(14) 0.0190(11) Uani 1 1 d . . . C8 C 0.1942(3) 0.1224(4) 0.0122(2) 0.067(3) Uani 1 1 d . C . C9 C 0.4275(4) 0.2845(3) 0.12833(18) 0.0495(13) Uani 1 1 d . C . H9A H 0.4606 0.3226 0.1344 0.074 Uiso 1 1 calc R . . H9B H 0.4459 0.2430 0.1409 0.074 Uiso 1 1 calc R . . H9C H 0.3777 0.2947 0.1379 0.074 Uiso 1 1 calc R . . C10 C 0.4127(4) 0.3606(3) 0.06129(18) 0.0495(13) Uani 1 1 d . C . H10A H 0.3713 0.3807 0.0757 0.074 Uiso 1 1 calc R . . H10B H 0.4022 0.3626 0.0333 0.074 Uiso 1 1 calc R . . H10C H 0.4580 0.3862 0.0669 0.074 Uiso 1 1 calc R . . C11 C 0.5144(4) 0.0652(4) 0.0569(2) 0.0645(17) Uani 1 1 d . C . H11A H 0.5242 0.0311 0.0367 0.097 Uiso 1 1 calc R . . H11B H 0.4792 0.0466 0.0758 0.097 Uiso 1 1 calc R . . H11C H 0.5607 0.0768 0.0701 0.097 Uiso 1 1 calc R . . C12 C 0.5037(4) 0.1262(4) -0.0153(2) 0.0645(17) Uani 1 1 d . C . H12A H 0.5572 0.1186 -0.0163 0.097 Uiso 1 1 calc R . . H12B H 0.4910 0.1659 -0.0313 0.097 Uiso 1 1 calc R . . H12C H 0.4780 0.0859 -0.0254 0.097 Uiso 1 1 calc R . . C14 C 0.2275(3) 0.3207(3) 0.03441(18) 0.0348(15) Uani 1 1 d . C . H14A H 0.2480 0.3249 0.0081 0.052 Uiso 1 1 calc R . . H14B H 0.2516 0.3536 0.0517 0.052 Uiso 1 1 calc R . . H14C H 0.1743 0.3296 0.0337 0.052 Uiso 1 1 calc R . . C15 C 0.2876(5) 0.0122(3) 0.0286(2) 0.067(3) Uani 1 1 d . C . H15A H 0.2362 0.0006 0.0347 0.100 Uiso 1 1 calc R . . H15B H 0.3184 0.0053 0.0517 0.100 Uiso 1 1 calc R . . H15C H 0.3054 -0.0171 0.0075 0.100 Uiso 1 1 calc R . . C16 C 0.3106(3) 0.0885(3) -0.03825(16) 0.0345(14) Uani 1 1 d . C . H16A H 0.2749 0.0557 -0.0487 0.052 Uiso 1 1 calc R . . H16B H 0.3609 0.0709 -0.0418 0.052 Uiso 1 1 calc R . . H16C H 0.3055 0.1319 -0.0520 0.052 Uiso 1 1 calc R . . C29 C 0.4537(4) 0.2674(3) -0.1089(2) 0.0493(13) Uani 1 1 d . . . H29 H 0.4998 0.2645 -0.0929 0.059 Uiso 1 1 calc R . . C30 C 0.4330(4) 0.1944(3) -0.11895(18) 0.0438(17) Uani 1 1 d . . . H30A H 0.3791 0.1895 -0.1183 0.066 Uiso 1 1 calc R . . H30B H 0.4552 0.1634 -0.0999 0.066 Uiso 1 1 calc R . . H30C H 0.4512 0.1834 -0.1451 0.066 Uiso 1 1 calc R . . C31 C 0.4751(4) 0.3063(4) -0.1462(2) 0.0596(12) Uani 1 1 d . . . H31A H 0.5289 0.3119 -0.1471 0.089 Uiso 1 1 calc R . . H31B H 0.4514 0.3512 -0.1461 0.089 Uiso 1 1 calc R . . H31C H 0.4586 0.2805 -0.1690 0.089 Uiso 1 1 calc R . . C32 C 0.2905(4) 0.3125(4) -0.1016(2) 0.0493(13) Uani 1 1 d . . . H32 H 0.2940 0.2689 -0.1166 0.059 Uiso 1 1 calc R A 5 C34 C 0.2812(4) 0.3612(4) -0.1345(2) 0.0596(12) Uani 1 1 d . D . H34A H 0.2369 0.3492 -0.1494 0.089 Uiso 1 1 calc R . . H34B H 0.3246 0.3590 -0.1515 0.089 Uiso 1 1 calc R . . H34C H 0.2760 0.4075 -0.1242 0.089 Uiso 1 1 calc R . . C35 C 0.4152(3) 0.4020(3) -0.06884(16) 0.0287(13) Uani 1 1 d . . . H35 H 0.4158 0.4252 -0.0947 0.034 Uiso 1 1 calc R D . C36 C 0.3620(4) 0.4419(3) -0.04276(18) 0.0465(18) Uani 1 1 d . D . H36A H 0.3312 0.4100 -0.0280 0.070 Uiso 1 1 calc R . . H36B H 0.3305 0.4710 -0.0589 0.070 Uiso 1 1 calc R . . H36C H 0.3904 0.4702 -0.0246 0.070 Uiso 1 1 calc R . . C37 C 0.4942(4) 0.4050(4) -0.0527(2) 0.0596(12) Uani 1 1 d . D . H37A H 0.4950 0.4336 -0.0293 0.089 Uiso 1 1 calc R . . H37B H 0.5272 0.4246 -0.0723 0.089 Uiso 1 1 calc R . . H37C H 0.5109 0.3590 -0.0461 0.089 Uiso 1 1 calc R . . C38 C 0.2298(3) -0.0960(3) 0.31859(15) 0.0242(12) Uani 1 1 d . . . H38 H 0.2328 -0.1301 0.3401 0.029 Uiso 1 1 calc R B . C39 C 0.1960(3) -0.0311(3) 0.33561(18) 0.0348(14) Uani 1 1 d . B . H39A H 0.1505 -0.0200 0.3216 0.052 Uiso 1 1 calc R . . H39B H 0.2312 0.0065 0.3330 0.052 Uiso 1 1 calc R . . H39C H 0.1847 -0.0383 0.3632 0.052 Uiso 1 1 calc R . . C40 C 0.1786(3) -0.1257(3) 0.28719(17) 0.0345(14) Uani 1 1 d . B . H40A H 0.1300 -0.1354 0.2986 0.052 Uiso 1 1 calc R . . H40B H 0.2000 -0.1680 0.2770 0.052 Uiso 1 1 calc R . . H40C H 0.1730 -0.0928 0.2659 0.052 Uiso 1 1 calc R . . C41 C 0.3644(3) -0.1676(3) 0.28415(16) 0.0271(13) Uani 1 1 d . . . H41 H 0.3348 -0.1807 0.2607 0.033 Uiso 1 1 calc R B . C42 C 0.3528(4) -0.2256(3) 0.31378(18) 0.0406(16) Uani 1 1 d . B . H42A H 0.3832 -0.2648 0.3064 0.061 Uiso 1 1 calc R . . H42B H 0.3006 -0.2389 0.3140 0.061 Uiso 1 1 calc R . . H42C H 0.3671 -0.2098 0.3398 0.061 Uiso 1 1 calc R . . C43 C 0.4450(3) -0.1670(3) 0.27065(18) 0.0354(15) Uani 1 1 d . B . H43A H 0.4777 -0.1691 0.2934 0.053 Uiso 1 1 calc R . . H43B H 0.4548 -0.1251 0.2561 0.053 Uiso 1 1 calc R . . H43C H 0.4542 -0.2065 0.2539 0.053 Uiso 1 1 calc R . . C44 C 0.3818(3) -0.0403(3) 0.34062(14) 0.0194(11) Uani 1 1 d . . . H44 H 0.3560 0.0036 0.3463 0.023 Uiso 1 1 calc R B . C45 C 0.3806(3) -0.0807(3) 0.37896(16) 0.0320(14) Uani 1 1 d . B . H45A H 0.4312 -0.0851 0.3890 0.048 Uiso 1 1 calc R . . H45B H 0.3599 -0.1261 0.3743 0.048 Uiso 1 1 calc R . . H45C H 0.3501 -0.0566 0.3981 0.048 Uiso 1 1 calc R . . C46 C 0.4608(3) -0.0211(3) 0.32991(17) 0.0348(14) Uani 1 1 d . B . H46A H 0.4874 -0.0068 0.3534 0.052 Uiso 1 1 calc R . . H46B H 0.4601 0.0164 0.3111 0.052 Uiso 1 1 calc R . . H46C H 0.4857 -0.0605 0.3184 0.052 Uiso 1 1 calc R . . P7A P 0.38960(19) -0.03657(14) 0.15568(7) 0.0179(6) Uani 0.580(4) 1 d P B 1 C19 C 0.4885(5) -0.0337(5) 0.1684(3) 0.026(2) Uiso 0.580(4) 1 d P B 1 H19A H 0.5080 -0.0808 0.1677 0.032 Uiso 0.580(4) 1 calc PR B 1 H19B H 0.5146 -0.0074 0.1480 0.032 Uiso 0.580(4) 1 calc PR B 1 C20A C 0.5098(7) 0.0001(6) 0.2115(3) 0.0272(19) Uiso 0.580(4) 1 d P B 1 H20A H 0.5633 0.0088 0.2151 0.033 Uiso 0.580(4) 1 calc PR B 1 H20B H 0.4892 -0.0252 0.2339 0.033 Uiso 0.580(4) 1 calc PR B 1 P6A P 0.26856(15) 0.14967(12) 0.20825(7) 0.0210(8) Uani 0.580(4) 1 d P B 1 C17 C 0.1674(5) 0.1422(5) 0.1991(3) 0.034(2) Uiso 0.580(4) 1 d P B 1 H17A H 0.1398 0.1664 0.2197 0.041 Uiso 0.580(4) 1 calc PR B 1 H17B H 0.1550 0.1635 0.1738 0.041 Uiso 0.580(4) 1 calc PR B 1 C18A C 0.1458(6) 0.0697(6) 0.1986(4) 0.036(3) Uiso 0.580(4) 1 d P B 1 H18A H 0.0956 0.0643 0.1875 0.043 Uiso 0.580(4) 1 calc PR B 1 H18B H 0.1461 0.0507 0.2253 0.043 Uiso 0.580(4) 1 calc PR B 1 C25A C 0.5099(6) 0.1389(6) 0.1705(3) 0.039(3) Uiso 0.580(4) 1 d P B 1 H25A H 0.4991 0.1857 0.1787 0.058 Uiso 0.580(4) 1 calc PR B 1 H25B H 0.4995 0.1341 0.1426 0.058 Uiso 0.580(4) 1 calc PR B 1 H25C H 0.5621 0.1288 0.1753 0.058 Uiso 0.580(4) 1 calc PR B 1 C24A C 0.1673(5) 0.0311(5) 0.1186(3) 0.027(2) Uiso 0.580(4) 1 d P B 1 H24A H 0.1779 -0.0111 0.1046 0.040 Uiso 0.580(4) 1 calc PR B 1 H24B H 0.1873 0.0699 0.1041 0.040 Uiso 0.580(4) 1 calc PR B 1 H24C H 0.1136 0.0365 0.1214 0.040 Uiso 0.580(4) 1 calc PR B 1 C26A C 0.4618(7) 0.1279(6) 0.2475(4) 0.032(3) Uiso 0.580(4) 1 d P B 1 H26A H 0.5131 0.1261 0.2564 0.047 Uiso 0.580(4) 1 calc PR B 1 H26B H 0.4298 0.1056 0.2667 0.047 Uiso 0.580(4) 1 calc PR B 1 H26C H 0.4466 0.1755 0.2444 0.047 Uiso 0.580(4) 1 calc PR B 1 C23A C 0.1819(6) -0.0645(6) 0.1780(4) 0.035(3) Uiso 0.580(4) 1 d P B 1 H23A H 0.1983 -0.0930 0.1562 0.053 Uiso 0.580(4) 1 calc PR B 1 H23B H 0.1280 -0.0666 0.1800 0.053 Uiso 0.580(4) 1 calc PR B 1 H23C H 0.2042 -0.0811 0.2022 0.053 Uiso 0.580(4) 1 calc PR B 1 C27A C 0.3940(7) -0.0531(7) 0.1032(4) 0.024(4) Uiso 0.580(4) 1 d P B 1 H27A H 0.4434 -0.0697 0.0963 0.036 Uiso 0.580(4) 1 calc PR B 1 H27B H 0.3838 -0.0108 0.0889 0.036 Uiso 0.580(4) 1 calc PR B 1 H27C H 0.3571 -0.0875 0.0962 0.036 Uiso 0.580(4) 1 calc PR B 1 C28A C 0.3787(8) -0.1218(7) 0.1752(4) 0.028(4) Uiso 0.580(4) 1 d P B 1 H28A H 0.4269 -0.1447 0.1757 0.042 Uiso 0.580(4) 1 calc PR B 1 H28B H 0.3445 -0.1476 0.1587 0.042 Uiso 0.580(4) 1 calc PR B 1 H28C H 0.3589 -0.1191 0.2017 0.042 Uiso 0.580(4) 1 calc PR B 1 C21A C 0.2662(7) 0.1525(5) 0.2604(3) 0.027(3) Uiso 0.580(4) 1 d P B 1 H21A H 0.2979 0.1896 0.2696 0.041 Uiso 0.580(4) 1 calc PR B 1 H21B H 0.2841 0.1091 0.2709 0.041 Uiso 0.580(4) 1 calc PR B 1 H21C H 0.2153 0.1603 0.2691 0.041 Uiso 0.580(4) 1 calc PR B 1 C22A C 0.2852(10) 0.2392(8) 0.1989(5) 0.030(5) Uiso 0.580(4) 1 d P B 1 H22A H 0.2500 0.2667 0.2139 0.045 Uiso 0.580(4) 1 calc PR B 1 H22B H 0.2789 0.2485 0.1711 0.045 Uiso 0.580(4) 1 calc PR B 1 H22C H 0.3357 0.2509 0.2068 0.045 Uiso 0.580(4) 1 calc PR B 1 P6B P 0.3269(2) 0.15626(16) 0.21433(10) 0.0227(11) Uani 0.420(4) 1 d P B 2 P7B P 0.3493(3) -0.04777(18) 0.14775(11) 0.0194(9) Uani 0.420(4) 1 d P B 2 C18B C 0.1519(7) 0.0489(7) 0.2134(4) 0.024(3) Uiso 0.420(4) 1 d P B 2 H18C H 0.0997 0.0423 0.2068 0.036 Uiso 0.420(4) 1 calc PR B 2 H18D H 0.1601 0.0965 0.2210 0.036 Uiso 0.420(4) 1 calc PR B 2 H18E H 0.1653 0.0190 0.2351 0.036 Uiso 0.420(4) 1 calc PR B 2 C20B C 0.4987(9) 0.0119(8) 0.2043(5) 0.0272(19) Uiso 0.420(4) 1 d P B 2 H20C H 0.5461 0.0226 0.2166 0.041 Uiso 0.420(4) 1 calc PR B 2 H20D H 0.5074 -0.0105 0.1792 0.041 Uiso 0.420(4) 1 calc PR B 2 H20E H 0.4702 -0.0185 0.2212 0.041 Uiso 0.420(4) 1 calc PR B 2 C48 C 0.2550(7) -0.0792(7) 0.1339(4) 0.026(3) Uiso 0.420(4) 1 d P B 2 H48A H 0.2406 -0.0600 0.1083 0.032 Uiso 0.420(4) 1 calc PR B 2 H48B H 0.2555 -0.1294 0.1317 0.032 Uiso 0.420(4) 1 calc PR B 2 C26B C 0.4758(8) 0.1310(7) 0.2345(4) 0.020(3) Uiso 0.420(4) 1 d P B 2 H26D H 0.4671 0.1087 0.2599 0.023 Uiso 0.420(4) 1 calc PR B 2 H26E H 0.5277 0.1466 0.2329 0.023 Uiso 0.420(4) 1 calc PR B 2 C47 C 0.4187(7) 0.1914(7) 0.2267(4) 0.027(3) Uiso 0.420(4) 1 d P B 2 H47A H 0.4368 0.2201 0.2050 0.032 Uiso 0.420(4) 1 calc PR B 2 H47B H 0.4148 0.2203 0.2502 0.032 Uiso 0.420(4) 1 calc PR B 2 C23B C 0.1992(8) -0.0574(7) 0.1649(4) 0.026(3) Uiso 0.420(4) 1 d P B 2 H23D H 0.2091 -0.0807 0.1899 0.031 Uiso 0.420(4) 1 calc PR B 2 H23E H 0.1481 -0.0679 0.1565 0.031 Uiso 0.420(4) 1 calc PR B 2 C24B C 0.1578(8) 0.0717(7) 0.1326(4) 0.032(3) Uiso 0.420(4) 1 d P B 2 H24D H 0.1886 0.0803 0.1096 0.048 Uiso 0.420(4) 1 calc PR B 2 H24E H 0.1403 0.1152 0.1431 0.048 Uiso 0.420(4) 1 calc PR B 2 H24F H 0.1153 0.0436 0.1251 0.048 Uiso 0.420(4) 1 calc PR B 2 C22B C 0.2748(14) 0.2327(13) 0.1946(7) 0.039(8) Uiso 0.420(4) 1 d P B 2 H24G H 0.2445 0.2186 0.1723 0.058 Uiso 0.420(4) 1 calc PR B 2 H24H H 0.3102 0.2676 0.1862 0.058 Uiso 0.420(4) 1 calc PR B 2 H24I H 0.2428 0.2514 0.2150 0.058 Uiso 0.420(4) 1 calc PR B 2 C25B C 0.5305(6) 0.1026(7) 0.1594(3) 0.020(3) Uiso 0.420(4) 1 d P B 2 H25D H 0.5115 0.1358 0.1406 0.030 Uiso 0.420(4) 1 calc PR B 2 H25E H 0.5453 0.0610 0.1457 0.030 Uiso 0.420(4) 1 calc PR B 2 H25F H 0.5734 0.1218 0.1729 0.030 Uiso 0.420(4) 1 calc PR B 2 C27B C 0.3998(10) -0.0688(10) 0.1039(5) 0.024(5) Uiso 0.420(4) 1 d P B 2 H27D H 0.4491 -0.0481 0.1050 0.036 Uiso 0.420(4) 1 calc PR B 2 H27E H 0.3731 -0.0513 0.0812 0.036 Uiso 0.420(4) 1 calc PR B 2 H27F H 0.4047 -0.1184 0.1018 0.036 Uiso 0.420(4) 1 calc PR B 2 C28B C 0.3611(10) -0.1199(9) 0.1746(5) 0.019(5) Uiso 0.420(4) 1 d P B 2 H28D H 0.3236 -0.1216 0.1952 0.029 Uiso 0.420(4) 1 calc PR B 2 H28E H 0.4104 -0.1197 0.1864 0.029 Uiso 0.420(4) 1 calc PR B 2 H28F H 0.3559 -0.1599 0.1578 0.029 Uiso 0.420(4) 1 calc PR B 2 C21B C 0.2930(9) 0.1524(7) 0.2641(4) 0.020(3) Uiso 0.420(4) 1 d P B 2 H21D H 0.3350 0.1488 0.2821 0.030 Uiso 0.420(4) 1 calc PR B 2 H21E H 0.2609 0.1126 0.2672 0.030 Uiso 0.420(4) 1 calc PR B 2 H21F H 0.2649 0.1939 0.2700 0.030 Uiso 0.420(4) 1 calc PR B 2 C5A C 0.5247(5) 0.2538(6) 0.0739(3) 0.0248(18) Uiso 0.525(7) 1 d P C 3 H5A1 H 0.5527 0.2971 0.0728 0.030 Uiso 0.525(7) 1 calc PR C 3 H5A2 H 0.5401 0.2287 0.0975 0.030 Uiso 0.525(7) 1 calc PR C 3 C6B C 0.5411(5) 0.2129(5) 0.0392(3) 0.0218(18) Uiso 0.525(7) 1 d P C 3 H6B1 H 0.5921 0.1950 0.0410 0.026 Uiso 0.525(7) 1 calc PR C 3 H6B2 H 0.5378 0.2420 0.0157 0.026 Uiso 0.525(7) 1 calc PR C 3 C7B C 0.1832(6) 0.1926(5) 0.0128(4) 0.0277(19) Uiso 0.525(7) 1 d P C 3 H7B1 H 0.1305 0.2025 0.0180 0.033 Uiso 0.525(7) 1 calc PR C 3 H7B2 H 0.1960 0.2120 -0.0130 0.033 Uiso 0.525(7) 1 calc PR C 3 C5B C 0.5202(6) 0.2711(6) 0.0542(4) 0.0248(18) Uiso 0.475(7) 1 d P C 4 H5B1 H 0.5185 0.2855 0.0266 0.030 Uiso 0.475(7) 1 calc PR C 4 H5B2 H 0.5534 0.3022 0.0686 0.030 Uiso 0.475(7) 1 calc PR C 4 C6A C 0.5476(6) 0.1960(6) 0.0576(4) 0.0218(18) Uiso 0.475(7) 1 d P C 4 H6A1 H 0.5544 0.1834 0.0853 0.026 Uiso 0.475(7) 1 calc PR C 4 H6A2 H 0.5955 0.1904 0.0440 0.026 Uiso 0.475(7) 1 calc PR C 4 C7A C 0.1705(6) 0.1832(6) 0.0333(4) 0.0277(19) Uiso 0.475(7) 1 d P C 4 H7A1 H 0.1383 0.1689 0.0552 0.033 Uiso 0.475(7) 1 calc PR C 4 H7A2 H 0.1403 0.2116 0.0156 0.033 Uiso 0.475(7) 1 calc PR C 4 C33A C 0.2287(7) 0.3014(8) -0.0827(4) 0.050(5) Uiso 0.522(18) 1 d P D 5 H33A H 0.2055 0.3450 -0.0761 0.075 Uiso 0.522(18) 1 calc PR D 5 H33B H 0.2392 0.2760 -0.0588 0.075 Uiso 0.522(18) 1 calc PR D 5 H33C H 0.1950 0.2748 -0.0992 0.075 Uiso 0.522(18) 1 calc PR D 5 C33B C 0.2396(6) 0.2553(7) -0.0944(4) 0.028(4) Uiso 0.478(18) 1 d P D 6 H33D H 0.2468 0.2382 -0.0679 0.042 Uiso 0.478(18) 1 calc PR D 6 H33E H 0.2496 0.2187 -0.1131 0.042 Uiso 0.478(18) 1 calc PR D 6 H33F H 0.1884 0.2709 -0.0975 0.042 Uiso 0.478(18) 1 calc PR D 6 C13A C 0.1869(5) 0.2311(6) 0.0947(3) 0.0261(19) Uiso 0.643(14) 1 d P C 7 H13A H 0.1615 0.2748 0.0981 0.039 Uiso 0.643(14) 1 calc PR C 7 H13B H 0.2176 0.2218 0.1176 0.039 Uiso 0.643(14) 1 calc PR C 7 H13C H 0.1502 0.1947 0.0916 0.039 Uiso 0.643(14) 1 calc PR C 7 C13B C 0.2059(9) 0.2575(10) 0.1051(5) 0.0261(19) Uiso 0.357(14) 1 d P C 8 H13D H 0.1526 0.2658 0.1038 0.039 Uiso 0.357(14) 1 calc PR C 8 H13E H 0.2309 0.2985 0.1148 0.039 Uiso 0.357(14) 1 calc PR C 8 H13F H 0.2157 0.2194 0.1229 0.039 Uiso 0.357(14) 1 calc PR C 8 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 Cr1 0.0165(4) 0.0134(4) 0.0115(4) -0.0001(3) 0.0010(3) -0.0004(3) Cr2 0.0208(4) 0.0153(4) 0.0124(4) 0.0017(3) -0.0011(3) -0.0032(3) Si1 0.0229(8) 0.0261(8) 0.0186(8) 0.0084(6) -0.0010(6) -0.0001(6) Si2 0.0173(7) 0.0166(7) 0.0170(7) 0.0024(6) -0.0018(6) 0.0014(6) P1 0.0203(7) 0.0186(7) 0.0211(7) -0.0059(6) 0.0015(6) -0.0007(6) P2 0.0194(7) 0.0166(7) 0.0199(7) -0.0015(6) 0.0045(5) 0.0000(5) P3 0.0194(7) 0.0181(7) 0.0275(8) 0.0012(6) -0.0003(6) 0.0030(6) P4 0.0244(7) 0.0181(7) 0.0174(7) -0.0010(6) -0.0018(6) -0.0054(6) P5 0.0152(7) 0.0458(10) 0.0312(8) 0.0199(7) 0.0026(6) 0.0018(7) P8 0.0447(10) 0.0649(12) 0.0348(10) 0.0279(9) -0.0251(8) -0.0413(9) N1 0.0131(19) 0.010(2) 0.015(2) -0.0041(17) 0.0002(16) 0.0017(16) N2 0.014(2) 0.010(2) 0.019(2) -0.0023(18) 0.0005(17) -0.0005(17) C1 0.020(3) 0.016(3) 0.018(3) -0.005(2) -0.001(2) -0.002(2) C2 0.023(3) 0.019(3) 0.017(3) -0.001(2) 0.003(2) 0.001(2) C3 0.015(2) 0.016(3) 0.022(3) -0.003(2) 0.000(2) -0.004(2) C4 0.017(3) 0.020(3) 0.020(3) -0.001(2) 0.000(2) -0.001(2) C8 0.021(3) 0.092(6) 0.088(6) -0.061(5) -0.014(3) 0.010(4) C9 0.082(4) 0.034(3) 0.032(3) 0.001(2) -0.017(2) -0.024(3) C10 0.082(4) 0.034(3) 0.032(3) 0.001(2) -0.017(2) -0.024(3) C11 0.049(3) 0.097(5) 0.048(3) 0.021(3) 0.026(3) 0.038(3) C12 0.049(3) 0.097(5) 0.048(3) 0.021(3) 0.026(3) 0.038(3) C14 0.036(3) 0.031(3) 0.037(4) 0.014(3) 0.010(3) 0.016(3) C15 0.104(6) 0.042(4) 0.054(5) 0.021(4) -0.042(4) -0.050(4) C16 0.045(4) 0.035(3) 0.023(3) -0.011(3) 0.000(3) -0.016(3) C29 0.043(3) 0.052(3) 0.054(3) 0.022(3) -0.012(2) -0.008(2) C30 0.061(4) 0.036(4) 0.035(4) -0.008(3) 0.016(3) -0.001(3) C31 0.065(3) 0.057(3) 0.057(3) 0.008(2) -0.002(2) -0.011(2) C32 0.043(3) 0.052(3) 0.054(3) 0.022(3) -0.012(2) -0.008(2) C34 0.065(3) 0.057(3) 0.057(3) 0.008(2) -0.002(2) -0.011(2) C35 0.039(3) 0.019(3) 0.028(3) 0.005(2) 0.006(3) 0.001(3) C36 0.075(5) 0.031(4) 0.034(4) 0.008(3) 0.016(3) 0.015(3) C37 0.065(3) 0.057(3) 0.057(3) 0.008(2) -0.002(2) -0.011(2) C38 0.026(3) 0.025(3) 0.022(3) 0.005(2) 0.000(2) -0.003(2) C39 0.019(3) 0.042(4) 0.043(4) -0.002(3) 0.002(3) 0.005(3) C40 0.024(3) 0.046(4) 0.034(3) 0.003(3) -0.003(3) -0.010(3) C41 0.032(3) 0.023(3) 0.026(3) 0.000(2) -0.008(2) 0.006(2) C42 0.059(4) 0.018(3) 0.045(4) 0.004(3) -0.011(3) 0.008(3) C43 0.031(3) 0.036(4) 0.039(4) -0.004(3) -0.003(3) 0.013(3) C44 0.022(3) 0.019(3) 0.017(3) 0.001(2) 0.002(2) 0.003(2) C45 0.044(4) 0.028(3) 0.024(3) 0.001(3) -0.009(3) -0.002(3) C46 0.029(3) 0.046(4) 0.030(3) -0.008(3) -0.002(3) -0.007(3) P7A 0.0145(15) 0.0243(14) 0.0149(13) -0.0039(10) -0.0015(11) -0.0018(12) P6A 0.0260(18) 0.0154(12) 0.0217(13) 0.0000(10) 0.0012(10) 0.0013(10) P6B 0.026(3) 0.0165(18) 0.0254(19) 0.0003(14) 0.0051(15) 0.0002(14) P7B 0.023(2) 0.0201(19) 0.0149(18) -0.0018(14) 0.0046(17) -0.0029(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 N1 1.879(4) . ? Cr1 C1 2.050(5) . ? Cr1 P3 2.3195(15) . ? Cr1 P1 2.3258(15) . ? Cr1 P2 2.3283(15) . ? Cr1 P4 2.3342(15) . ? Cr2 N2 1.880(4) . ? Cr2 C3 2.054(5) . ? Cr2 P7A 2.274(3) . ? Cr2 P6B 2.291(3) . ? Cr2 P5 2.3135(16) . ? Cr2 P8 2.3143(17) . ? Cr2 P7B 2.362(4) . ? Cr2 P6A 2.377(2) . ? Si1 C2 1.819(5) . ? Si1 C32 1.871(6) . ? Si1 C35 1.883(6) . ? Si1 C29 1.893(7) . ? Si2 C4 1.822(5) . ? Si2 C38 1.888(5) . ? Si2 C44 1.895(5) . ? Si2 C41 1.895(5) . ? P1 C9 1.812(6) . ? P1 C10 1.827(6) . ? P1 C5A 1.845(10) . ? P1 C5B 1.884(11) . ? P2 C12 1.817(7) . ? P2 C11 1.817(7) . ? P2 C6B 1.846(10) . ? P2 C6A 1.864(11) . ? P3 C13A 1.778(8) . ? P3 C7A 1.792(12) . ? P3 C14 1.822(5) . ? P3 C7B 1.935(11) . ? P3 C13B 1.984(16) . ? P4 C16 1.821(5) . ? P4 C15 1.829(6) . ? P4 C8 1.836(6) . ? P5 C23B 1.690(14) . ? P5 C18A 1.771(11) . ? P5 C24B 1.813(13) . ? P5 C23A 1.911(11) . ? P5 C24A 1.914(9) . ? P5 C18B 1.915(13) . ? P8 C20B 1.599(16) . ? P8 C26B 1.662(14) . ? P8 C25A 1.792(10) . ? P8 C20A 1.946(11) . ? P8 C26A 1.959(12) . ? P8 C25B 1.960(12) . ? N1 N2 1.188(5) . ? C1 C2 1.227(7) . ? C3 C4 1.234(7) . ? C8 C7B 1.392(13) . ? C8 C7A 1.461(14) . ? C29 C30 1.521(9) . ? C29 C31 1.540(9) . ? C32 C33A 1.311(14) . ? C32 C33B 1.474(13) . ? C32 C34 1.488(9) . ? C35 C36 1.530(8) . ? C35 C37 1.534(9) . ? C38 C39 1.528(8) . ? C38 C40 1.538(7) . ? C41 C43 1.530(8) . ? C41 C42 1.541(8) . ? C44 C46 1.523(7) . ? C44 C45 1.537(7) . ? P7A C28A 1.812(15) . ? P7A C27A 1.834(13) . ? P7A C19 1.842(10) . ? C19 C20A 1.667(15) . ? P6A C21A 1.792(11) . ? P6A C22A 1.812(16) . ? P6A C17 1.862(10) . ? C17 C18A 1.477(14) . ? P6B C21B 1.818(14) . ? P6B C47 1.848(13) . ? P6B C22B 1.90(3) . ? P7B C28B 1.704(18) . ? P7B C27B 1.809(18) . ? P7B C48 1.875(13) . ? C48 C23B 1.527(19) . ? C26B C47 1.595(18) . ? C5A C6B 1.466(15) . ? C5B C6A 1.560(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 C1 178.61(18) . . ? N1 Cr1 P3 95.97(12) . . ? C1 Cr1 P3 83.43(14) . . ? N1 Cr1 P1 95.11(12) . . ? C1 Cr1 P1 83.71(14) . . ? P3 Cr1 P1 95.93(5) . . ? N1 Cr1 P2 97.04(12) . . ? C1 Cr1 P2 83.56(14) . . ? P3 Cr1 P2 166.99(6) . . ? P1 Cr1 P2 82.69(5) . . ? N1 Cr1 P4 95.48(12) . . ? C1 Cr1 P4 85.70(14) . . ? P3 Cr1 P4 82.68(5) . . ? P1 Cr1 P4 169.41(6) . . ? P2 Cr1 P4 96.28(5) . . ? N2 Cr2 C3 177.80(19) . . ? N2 Cr2 P7A 95.51(13) . . ? C3 Cr2 P7A 82.33(15) . . ? N2 Cr2 P6B 96.72(14) . . ? C3 Cr2 P6B 85.07(16) . . ? P7A Cr2 P6B 152.71(12) . . ? N2 Cr2 P5 96.96(12) . . ? C3 Cr2 P5 83.82(14) . . ? P7A Cr2 P5 98.81(10) . . ? P6B Cr2 P5 103.78(11) . . ? N2 Cr2 P8 97.01(12) . . ? C3 Cr2 P8 82.22(14) . . ? P7A Cr2 P8 79.93(11) . . ? P6B Cr2 P8 74.43(11) . . ? P5 Cr2 P8 166.03(6) . . ? N2 Cr2 P7B 93.48(14) . . ? C3 Cr2 P7B 84.63(16) . . ? P7A Cr2 P7B 20.00(9) . . ? P6B Cr2 P7B 168.86(13) . . ? P5 Cr2 P7B 79.31(13) . . ? P8 Cr2 P7B 99.92(14) . . ? N2 Cr2 P6A 95.59(13) . . ? C3 Cr2 P6A 86.58(15) . . ? P7A Cr2 P6A 168.62(9) . . ? P6B Cr2 P6A 26.77(10) . . ? P5 Cr2 P6A 77.39(8) . . ? P8 Cr2 P6A 101.13(9) . . ? P7B Cr2 P6A 155.84(13) . . ? C2 Si1 C32 109.6(3) . . ? C2 Si1 C35 110.3(2) . . ? C32 Si1 C35 109.9(3) . . ? C2 Si1 C29 108.3(3) . . ? C32 Si1 C29 110.6(3) . . ? C35 Si1 C29 108.2(3) . . ? C4 Si2 C38 110.6(2) . . ? C4 Si2 C44 109.1(2) . . ? C38 Si2 C44 107.6(2) . . ? C4 Si2 C41 108.0(2) . . ? C38 Si2 C41 107.5(2) . . ? C44 Si2 C41 114.0(2) . . ? C9 P1 C10 98.6(3) . . ? C9 P1 C5A 92.3(4) . . ? C10 P1 C5A 106.8(4) . . ? C9 P1 C5B 111.7(5) . . ? C10 P1 C5B 90.4(5) . . ? C5A P1 C5B 23.5(4) . . ? C9 P1 Cr1 119.8(2) . . ? C10 P1 Cr1 124.1(2) . . ? C5A P1 Cr1 110.1(3) . . ? C5B P1 Cr1 108.4(4) . . ? C12 P2 C11 98.9(3) . . ? C12 P2 C6B 91.4(4) . . ? C11 P2 C6B 110.1(5) . . ? C12 P2 C6A 107.4(5) . . ? C11 P2 C6A 91.5(5) . . ? C6B P2 C6A 22.5(4) . . ? C12 P2 Cr1 121.8(2) . . ? C11 P2 Cr1 122.3(2) . . ? C6B P2 Cr1 108.0(3) . . ? C6A P2 Cr1 110.3(3) . . ? C13A P3 C7A 81.3(6) . . ? C13A P3 C14 102.8(4) . . ? C7A P3 C14 106.1(5) . . ? C13A P3 C7B 103.3(5) . . ? C7A P3 C7B 23.3(4) . . ? C14 P3 C7B 93.6(4) . . ? C13A P3 C13B 21.1(5) . . ? C7A P3 C13B 102.0(7) . . ? C14 P3 C13B 92.7(5) . . ? C7B P3 C13B 122.9(7) . . ? C13A P3 Cr1 121.7(3) . . ? C7A P3 Cr1 113.1(4) . . ? C14 P3 Cr1 123.4(2) . . ? C7B P3 Cr1 106.7(3) . . ? C13B P3 Cr1 116.1(5) . . ? C16 P4 C15 98.9(3) . . ? C16 P4 C8 100.3(3) . . ? C15 P4 C8 99.8(4) . . ? C16 P4 Cr1 122.21(19) . . ? C15 P4 Cr1 121.1(2) . . ? C8 P4 Cr1 110.6(2) . . ? C23B P5 C18A 114.7(6) . . ? C23B P5 C24B 109.8(7) . . ? C18A P5 C24B 79.0(6) . . ? C23B P5 C23A 16.6(6) . . ? C18A P5 C23A 99.2(5) . . ? C24B P5 C23A 114.2(6) . . ? C23B P5 C24A 84.3(6) . . ? C18A P5 C24A 102.5(5) . . ? C24B P5 C24A 29.2(5) . . ? C23A P5 C24A 93.4(5) . . ? C23B P5 C18B 102.0(7) . . ? C18A P5 C18B 20.2(5) . . ? C24B P5 C18B 98.1(6) . . ? C23A P5 C18B 85.4(6) . . ? C24A P5 C18B 118.2(5) . . ? C23B P5 Cr2 114.7(5) . . ? C18A P5 Cr2 116.9(4) . . ? C24B P5 Cr2 116.8(4) . . ? C23A P5 Cr2 121.4(4) . . ? C24A P5 Cr2 119.0(3) . . ? C18B P5 Cr2 113.3(4) . . ? C20B P8 C26B 105.2(8) . . ? C20B P8 C25A 108.7(7) . . ? C26B P8 C25A 83.0(6) . . ? C20B P8 C20A 6.1(9) . . ? C26B P8 C20A 99.4(6) . . ? C25A P8 C20A 110.2(5) . . ? C20B P8 C26A 103.3(7) . . ? C26B P8 C26A 13.5(6) . . ? C25A P8 C26A 96.2(5) . . ? C20A P8 C26A 97.1(5) . . ? C20B P8 C25B 85.2(7) . . ? C26B P8 C25B 101.9(6) . . ? C25A P8 C25B 27.0(4) . . ? C20A P8 C25B 88.2(5) . . ? C26A P8 C25B 115.2(5) . . ? C20B P8 Cr2 112.6(6) . . ? C26B P8 Cr2 124.9(5) . . ? C25A P8 Cr2 118.5(4) . . ? C20A P8 Cr2 115.6(4) . . ? C26A P8 Cr2 115.5(4) . . ? C25B P8 Cr2 119.4(4) . . ? N2 N1 Cr1 178.7(4) . . ? N1 N2 Cr2 179.2(4) . . ? C2 C1 Cr1 178.8(4) . . ? C1 C2 Si1 176.6(5) . . ? C4 C3 Cr2 176.7(4) . . ? C3 C4 Si2 175.2(5) . . ? C7B C8 C7A 31.0(6) . . ? C7B C8 P4 111.2(6) . . ? C7A C8 P4 117.3(6) . . ? C30 C29 C31 109.8(6) . . ? C30 C29 Si1 113.5(4) . . ? C31 C29 Si1 114.7(5) . . ? C33A C32 C33B 42.0(7) . . ? C33A C32 C34 112.7(8) . . ? C33B C32 C34 123.2(7) . . ? C33A C32 Si1 122.7(8) . . ? C33B C32 Si1 118.6(6) . . ? C34 C32 Si1 116.4(5) . . ? C36 C35 C37 110.7(5) . . ? C36 C35 Si1 112.1(4) . . ? C37 C35 Si1 112.4(4) . . ? C39 C38 C40 110.1(5) . . ? C39 C38 Si2 112.3(4) . . ? C40 C38 Si2 112.3(4) . . ? C43 C41 C42 109.6(5) . . ? C43 C41 Si2 115.0(4) . . ? C42 C41 Si2 114.6(4) . . ? C46 C44 C45 110.3(4) . . ? C46 C44 Si2 114.9(4) . . ? C45 C44 Si2 113.7(4) . . ? C28A P7A C27A 101.8(6) . . ? C28A P7A C19 92.6(6) . . ? C27A P7A C19 101.4(5) . . ? C28A P7A Cr2 127.9(5) . . ? C27A P7A Cr2 118.1(5) . . ? C19 P7A Cr2 109.4(3) . . ? C20A C19 P7A 116.6(7) . . ? C19 C20A P8 88.9(6) . . ? C21A P6A C22A 98.6(6) . . ? C21A P6A C17 98.5(5) . . ? C22A P6A C17 102.1(7) . . ? C21A P6A Cr2 120.0(4) . . ? C22A P6A Cr2 123.1(5) . . ? C17 P6A Cr2 110.6(3) . . ? C18A C17 P6A 109.7(7) . . ? C17 C18A P5 106.1(8) . . ? C21B P6B C47 95.9(6) . . ? C21B P6B C22B 101.6(9) . . ? C47 P6B C22B 103.5(9) . . ? C21B P6B Cr2 121.6(5) . . ? C47 P6B Cr2 112.8(4) . . ? C22B P6B Cr2 117.9(8) . . ? C28B P7B C27B 101.4(9) . . ? C28B P7B C48 88.8(7) . . ? C27B P7B C48 100.0(7) . . ? C28B P7B Cr2 122.8(6) . . ? C27B P7B Cr2 127.5(6) . . ? C48 P7B Cr2 107.1(4) . . ? C23B C48 P7B 109.4(9) . . ? C47 C26B P8 98.8(9) . . ? C26B C47 P6B 110.0(9) . . ? C48 C23B P5 104.3(10) . . ? C6B C5A P1 109.8(8) . . ? C5A C6B P2 110.8(7) . . ? C8 C7B P3 110.6(7) . . ? C6A C5B P1 105.7(8) . . ? C5B C6A P2 106.9(8) . . ? C8 C7A P3 115.2(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.023 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.109 #===END data_3(LT) _chemical_name_common 'compound 3(LT) in text' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H133 B Cr2 F24 N2 O1.50 P8 Si2' _chemical_formula_weight 2069.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'Cr' 'Cr' 0.3209 0.6236 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5070(4) _cell_length_b 29.6682(9) _cell_length_c 24.1919(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.531(2) _cell_angle_gamma 90.00 _cell_volume 10344.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'parallelpiped' _exptl_crystal_colour 'brown/green dichroic' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8714 _exptl_absorpt_correction_T_max 0.9407 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; Two cases of trifluoromethyl group disorder in the BArF4 anions were factored into the structure solution: fluorine atoms were allowed to refine to 89:11 and 73:27 occupancy ratios, respectively, and the fluorine atoms located on the majority-occupied sites were refined anisotropically. One of the diethyl ether solvate molecules in the structure of 3 was disordered evenly over two positions, while the other was located on an inversion center and the carbon atom adjacent to the oxygen atom was disordered equally over two positions. Hydrogen atoms for these solvent molecules were not included in the final structural refinement. ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 135312 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 24.41 _reflns_number_total 17017 _reflns_number_gt 12079 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1013P)^2^+35.1499P] 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 17017 _refine_ls_number_parameters 1140 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.005 _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 B1 B 0.6899(4) 0.83958(19) 0.4598(2) 0.0195(12) Uani 1 1 d . . . Cr1 Cr 0.30713(5) 0.71749(3) 0.65967(3) 0.01724(19) Uani 1 1 d . . . Cr2 Cr 0.16510(5) 0.85561(3) 0.72283(3) 0.0203(2) Uani 1 1 d . . . P1 P 0.42727(9) 0.71732(4) 0.73334(5) 0.0214(3) Uani 1 1 d . . . P2 P 0.42499(9) 0.74726(4) 0.61088(5) 0.0233(3) Uani 1 1 d . . . P3 P 0.19515(9) 0.70790(5) 0.58285(6) 0.0285(3) Uani 1 1 d . . . P4 P 0.21488(9) 0.66506(5) 0.70048(6) 0.0256(3) Uani 1 1 d . . . Si1 Si 0.45188(10) 0.57168(5) 0.59687(6) 0.0243(3) Uani 1 1 d . . . N1 N 0.2544(3) 0.77001(13) 0.68294(16) 0.0180(9) Uani 1 1 d . . . N2 N 0.2183(3) 0.80312(13) 0.69876(16) 0.0198(9) Uani 1 1 d . . . F1 F 0.6036(3) 0.68994(12) 0.35380(14) 0.0597(11) Uani 1 1 d . . . F2 F 0.6087(3) 0.63580(11) 0.41280(15) 0.0533(10) Uani 1 1 d . . . F3 F 0.4948(3) 0.68273(12) 0.40524(16) 0.0529(10) Uani 1 1 d . . . F4 F 0.8710(2) 0.80699(13) 0.23995(13) 0.0464(9) Uani 1 1 d . . . F5 F 0.7729(3) 0.76204(12) 0.27079(15) 0.0528(10) Uani 1 1 d . . . F6 F 0.7297(2) 0.82743(12) 0.24212(12) 0.0411(8) Uani 1 1 d . . . F8 F 1.0837(2) 0.87181(18) 0.38602(16) 0.0729(14) Uani 1 1 d . B . F10 F 0.8025(3) 1.00458(13) 0.49303(15) 0.0658(12) Uani 1 1 d . . . F11 F 0.9036(3) 0.98751(13) 0.56257(19) 0.0648(12) Uani 1 1 d . . . F12 F 0.7809(3) 1.02351(12) 0.57527(16) 0.0603(11) Uani 1 1 d . . . F16 F 0.2857(3) 0.8632(2) 0.4590(2) 0.095(2) Uani 1 1 d . . . F17 F 0.2737(2) 0.83378(13) 0.37969(13) 0.0461(9) Uani 1 1 d . . . F18 F 0.3388(2) 0.79827(18) 0.4473(2) 0.095(2) Uani 1 1 d . . . F19 F 0.5665(4) 0.98745(13) 0.35582(17) 0.0719(13) Uani 1 1 d . . . F20 F 0.4276(4) 0.97860(18) 0.3286(3) 0.118(2) Uani 1 1 d . . . F21 F 0.5323(5) 0.94755(13) 0.28733(16) 0.111(2) Uani 1 1 d . . . F22 F 0.7612(5) 0.66106(16) 0.5969(2) 0.129(3) Uani 1 1 d . . . F23 F 0.7637(2) 0.72656(16) 0.63157(15) 0.0601(11) Uani 1 1 d . . . F24 F 0.8726(2) 0.70586(15) 0.58740(15) 0.0592(11) Uani 1 1 d . . . C1 C 0.3620(3) 0.65797(16) 0.63479(19) 0.0192(10) Uani 1 1 d . . . C2 C 0.3948(3) 0.62263(17) 0.6197(2) 0.0229(11) Uani 1 1 d . . . C3 C 0.1104(3) 0.91435(17) 0.7490(2) 0.0232(11) Uani 1 1 d . . . C4 C 0.0798(4) 0.94941(19) 0.7656(2) 0.0307(13) Uani 1 1 d . . . C5 C 0.1011(4) 0.6709(2) 0.6033(3) 0.0435(16) Uani 1 1 d . . . H5A H 0.0549 0.6892 0.6204 0.052 Uiso 1 1 calc R . . H5B H 0.0692 0.6559 0.5699 0.052 Uiso 1 1 calc R . . C6 C 0.1425(4) 0.6356(2) 0.6444(2) 0.0357(14) Uani 1 1 d . . . H6A H 0.1806 0.6140 0.6257 0.043 Uiso 1 1 calc R . . H6B H 0.0925 0.6187 0.6599 0.043 Uiso 1 1 calc R . . C7 C 0.5254(3) 0.7513(2) 0.7144(2) 0.0313(13) Uani 1 1 d . . . H7A H 0.5125 0.7838 0.7188 0.038 Uiso 1 1 calc R . . H7B H 0.5827 0.7436 0.7387 0.038 Uiso 1 1 calc R . . C8 C 0.5372(4) 0.74086(19) 0.6542(2) 0.0324(13) Uani 1 1 d . . . H8A H 0.5602 0.7096 0.6512 0.039 Uiso 1 1 calc R . . H8B H 0.5833 0.7616 0.6409 0.039 Uiso 1 1 calc R . . C9 C 0.4871(4) 0.66538(18) 0.7566(2) 0.0324(13) Uani 1 1 d . . . H9A H 0.5406 0.6726 0.7836 0.049 Uiso 1 1 calc R . . H9B H 0.5082 0.6499 0.7246 0.049 Uiso 1 1 calc R . . H9C H 0.4445 0.6458 0.7742 0.049 Uiso 1 1 calc R . . C10 C 0.4051(4) 0.7412(2) 0.8001(2) 0.0371(14) Uani 1 1 d . . . H10A H 0.3674 0.7202 0.8192 0.056 Uiso 1 1 calc R . . H10B H 0.3717 0.7698 0.7938 0.056 Uiso 1 1 calc R . . H10C H 0.4642 0.7465 0.8231 0.056 Uiso 1 1 calc R . . C11 C 0.4546(4) 0.7251(2) 0.5451(2) 0.0374(14) Uani 1 1 d . . . H11A H 0.4024 0.7296 0.5163 0.056 Uiso 1 1 calc R . . H11B H 0.4682 0.6928 0.5491 0.056 Uiso 1 1 calc R . . H11C H 0.5094 0.7408 0.5346 0.056 Uiso 1 1 calc R . . C12 C 0.4211(4) 0.80732(17) 0.5951(2) 0.0314(13) Uani 1 1 d . . . H12A H 0.4790 0.8163 0.5808 0.047 Uiso 1 1 calc R . . H12B H 0.4138 0.8244 0.6290 0.047 Uiso 1 1 calc R . . H12C H 0.3686 0.8136 0.5669 0.047 Uiso 1 1 calc R . . C13 C 0.2226(5) 0.6802(2) 0.5198(2) 0.0473(17) Uani 1 1 d . . . H13A H 0.1658 0.6764 0.4942 0.071 Uiso 1 1 calc R . . H13B H 0.2501 0.6506 0.5292 0.071 Uiso 1 1 calc R . . H13C H 0.2669 0.6986 0.5020 0.071 Uiso 1 1 calc R . . C14 C 0.1308(5) 0.7563(2) 0.5532(3) 0.0443(16) Uani 1 1 d . . . H14A H 0.1670 0.7716 0.5269 0.067 Uiso 1 1 calc R . . H14B H 0.1193 0.7772 0.5830 0.067 Uiso 1 1 calc R . . H14C H 0.0715 0.7462 0.5337 0.067 Uiso 1 1 calc R . . C15 C 0.1296(4) 0.6852(2) 0.7446(3) 0.0394(14) Uani 1 1 d . . . H15A H 0.0763 0.6647 0.7415 0.059 Uiso 1 1 calc R . . H15B H 0.1089 0.7155 0.7326 0.059 Uiso 1 1 calc R . . H15C H 0.1578 0.6863 0.7834 0.059 Uiso 1 1 calc R . . C16 C 0.2640(4) 0.61807(19) 0.7430(2) 0.0367(14) Uani 1 1 d . . . H16A H 0.2907 0.6294 0.7794 0.055 Uiso 1 1 calc R . . H16B H 0.3126 0.6035 0.7243 0.055 Uiso 1 1 calc R . . H16C H 0.2151 0.5962 0.7480 0.055 Uiso 1 1 calc R . . C38 C 0.3324(5) 0.5158(2) 0.6534(4) 0.070(2) Uani 1 1 d . . . H38A H 0.2985 0.5016 0.6206 0.105 Uiso 1 1 calc R . . H38B H 0.3040 0.5450 0.6602 0.105 Uiso 1 1 calc R . . H38C H 0.3299 0.4962 0.6858 0.105 Uiso 1 1 calc R . . C39 C 0.4317(5) 0.52286(19) 0.6435(3) 0.0407(15) Uani 1 1 d . . . H39 H 0.4670 0.5295 0.6806 0.049 Uiso 1 1 calc R . . C40 C 0.4704(5) 0.4780(2) 0.6230(3) 0.0523(18) Uani 1 1 d . . . H40A H 0.4542 0.4533 0.6470 0.078 Uiso 1 1 calc R . . H40B H 0.5380 0.4801 0.6244 0.078 Uiso 1 1 calc R . . H40C H 0.4434 0.4722 0.5847 0.078 Uiso 1 1 calc R . . C41 C 0.3072(5) 0.5475(3) 0.5112(3) 0.069(2) Uani 1 1 d . . . H41A H 0.2702 0.5712 0.5263 0.103 Uiso 1 1 calc R . . H41B H 0.2963 0.5188 0.5293 0.103 Uiso 1 1 calc R . . H41C H 0.2893 0.5448 0.4711 0.103 Uiso 1 1 calc R . . C42 C 0.4095(4) 0.5596(2) 0.5220(2) 0.0373(14) Uani 1 1 d . . . H42 H 0.4451 0.5329 0.5108 0.045 Uiso 1 1 calc R . . C43 C 0.4325(6) 0.5990(2) 0.4850(2) 0.059(2) Uani 1 1 d . . . H43A H 0.4184 0.5904 0.4459 0.089 Uiso 1 1 calc R . . H43B H 0.4985 0.6064 0.4927 0.089 Uiso 1 1 calc R . . H43C H 0.3952 0.6253 0.4929 0.089 Uiso 1 1 calc R . . C44 C 0.6272(4) 0.5842(3) 0.6622(3) 0.0551(19) Uani 1 1 d . . . H44A H 0.6339 0.5529 0.6750 0.083 Uiso 1 1 calc R . . H44B H 0.5885 0.6008 0.6859 0.083 Uiso 1 1 calc R . . H44C H 0.6885 0.5984 0.6641 0.083 Uiso 1 1 calc R . . C45 C 0.5814(4) 0.5851(2) 0.6023(3) 0.0367(14) Uani 1 1 d . . . H45 H 0.5863 0.6169 0.5892 0.044 Uiso 1 1 calc R . . C46 C 0.6383(4) 0.5563(2) 0.5654(3) 0.0484(17) Uani 1 1 d . . . H46A H 0.7029 0.5666 0.5697 0.073 Uiso 1 1 calc R . . H46B H 0.6123 0.5593 0.5264 0.073 Uiso 1 1 calc R . . H46C H 0.6360 0.5246 0.5767 0.073 Uiso 1 1 calc R . . C47 C 0.7118(3) 0.87313(17) 0.5137(2) 0.0214(11) Uani 1 1 d . . . C48 C 0.6802(3) 0.86450(18) 0.5649(2) 0.0241(11) Uani 1 1 d . . . H48 H 0.6497 0.8368 0.5701 0.029 Uiso 1 1 calc R . . C49 C 0.6920(3) 0.89538(19) 0.6091(2) 0.0280(12) Uani 1 1 d . C . C50 C 0.7343(4) 0.93645(18) 0.6031(2) 0.0285(12) Uani 1 1 d . . . H50 H 0.7422 0.9574 0.6329 0.034 Uiso 1 1 calc R . . C51 C 0.7648(4) 0.94625(18) 0.5523(2) 0.0283(12) Uani 1 1 d . . . C52 C 0.7534(3) 0.91551(17) 0.5094(2) 0.0259(12) Uani 1 1 d . . . H52 H 0.7749 0.9234 0.4750 0.031 Uiso 1 1 calc R . . C53 C 0.6555(4) 0.8849(2) 0.6618(2) 0.0381(15) Uani 1 1 d . . . C54 C 0.8133(5) 0.9903(2) 0.5455(2) 0.0442(16) Uani 1 1 d . . . C55 C 0.5916(3) 0.85828(16) 0.42851(19) 0.0186(10) Uani 1 1 d . . . C56 C 0.5051(3) 0.84078(16) 0.43794(19) 0.0192(10) Uani 1 1 d . . . H56 H 0.5031 0.8147 0.4606 0.023 Uiso 1 1 calc R . . C57 C 0.4220(3) 0.86015(17) 0.41538(19) 0.0222(11) Uani 1 1 d . . . C58 C 0.4208(3) 0.89835(17) 0.3829(2) 0.0245(11) Uani 1 1 d . . . H58 H 0.3639 0.9119 0.3683 0.029 Uiso 1 1 calc R . . C59 C 0.5050(4) 0.91644(16) 0.3722(2) 0.0228(11) Uani 1 1 d . . . C60 C 0.5880(3) 0.89655(16) 0.39399(19) 0.0216(11) Uani 1 1 d . . . H60 H 0.6447 0.9093 0.3852 0.026 Uiso 1 1 calc R . . C61 C 0.3305(3) 0.8396(2) 0.4255(2) 0.0321(13) Uani 1 1 d . . . C62 C 0.5068(4) 0.95658(19) 0.3359(2) 0.0353(14) Uani 1 1 d . . . C63 C 0.7725(3) 0.84098(16) 0.4182(2) 0.0196(10) Uani 1 1 d . . . C64 C 0.7546(3) 0.82773(16) 0.3626(2) 0.0206(11) Uani 1 1 d . . . H64 H 0.6922 0.8218 0.3479 0.025 Uiso 1 1 calc R . . C65 C 0.8237(3) 0.82275(16) 0.3278(2) 0.0212(11) Uani 1 1 d . . . C66 C 0.9147(3) 0.83331(19) 0.3473(2) 0.0274(12) Uani 1 1 d . . . H66 H 0.9625 0.8308 0.3237 0.033 Uiso 1 1 calc R . . C67 C 0.9344(4) 0.8476(2) 0.4019(2) 0.0329(13) Uani 1 1 d . B . C68 C 0.8647(3) 0.85047(19) 0.4370(2) 0.0283(12) Uani 1 1 d . . . H68 H 0.8806 0.8592 0.4746 0.034 Uiso 1 1 calc R . . C69 C 0.7994(4) 0.80547(19) 0.2703(2) 0.0289(12) Uani 1 1 d . . . C70 C 1.0328(4) 0.8598(3) 0.4234(3) 0.057(2) Uani 1 1 d . . . C71 C 0.6841(3) 0.78607(17) 0.4759(2) 0.0204(11) Uani 1 1 d . . . C72 C 0.7319(3) 0.76677(17) 0.5239(2) 0.0226(11) Uani 1 1 d . . . H72 H 0.7660 0.7858 0.5504 0.027 Uiso 1 1 calc R . . C73 C 0.7309(3) 0.72084(18) 0.5337(2) 0.0267(12) Uani 1 1 d . . . C74 C 0.6838(3) 0.69146(18) 0.4963(2) 0.0259(12) Uani 1 1 d . . . H74 H 0.6832 0.6600 0.5034 0.031 Uiso 1 1 calc R . . C75 C 0.6375(3) 0.70924(17) 0.4481(2) 0.0233(11) Uani 1 1 d . . . C76 C 0.6373(3) 0.75536(17) 0.4386(2) 0.0220(11) Uani 1 1 d . . . H76 H 0.6041 0.7666 0.4053 0.026 Uiso 1 1 calc R . . C77 C 0.7818(4) 0.7030(2) 0.5873(3) 0.0435(16) Uani 1 1 d . . . C78 C 0.5879(5) 0.67933(19) 0.4056(2) 0.0389(15) Uani 1 1 d . . . O1 O 0.5000 1.0000 0.5000 0.106(3) Uani 1 2 d S . . C90 C 0.4337(8) 0.9704(4) 0.5123(5) 0.031(3) Uiso 0.50 1 d P A 9 H90A H 0.3857 0.9915 0.5227 0.038 Uiso 0.50 1 calc PR A 9 H90B H 0.4097 0.9600 0.4746 0.038 Uiso 0.50 1 calc PR A 9 C91 C 0.4160(12) 0.9339(8) 0.5429(10) 0.050(5) Uani 0.50 1 d P A 9 H91A H 0.4700 0.9138 0.5463 0.074 Uiso 0.50 1 calc PR A 9 H91B H 0.3619 0.9179 0.5246 0.074 Uiso 0.50 1 calc PR A 9 H91C H 0.4033 0.9436 0.5800 0.074 Uiso 0.50 1 calc PR A 9 C90A C 0.5025(9) 0.9593(4) 0.5286(5) 0.036(3) Uiso 0.50 1 d P A 10 H90C H 0.5460 0.9420 0.5080 0.044 Uiso 0.50 1 calc PR A 10 H90D H 0.5398 0.9679 0.5638 0.044 Uiso 0.50 1 calc PR A 10 C91A C 0.4589(11) 0.9308(7) 0.5437(10) 0.042(5) Uani 0.50 1 d P A 10 H91D H 0.4552 0.9342 0.5837 0.063 Uiso 0.50 1 calc PR A 10 H91E H 0.4879 0.9017 0.5368 0.063 Uiso 0.50 1 calc PR A 10 H91F H 0.3964 0.9318 0.5236 0.063 Uiso 0.50 1 calc PR A 10 Si2 Si 0.03561(11) 1.00119(5) 0.79641(7) 0.0336(4) Uani 1 1 d . . . C29 C 0.0202(4) 0.9878(2) 0.8722(2) 0.0383(14) Uani 1 1 d . . . H29 H -0.0088 0.9572 0.8721 0.046 Uiso 1 1 calc R . . C30 C 0.1137(4) 0.9840(2) 0.9076(3) 0.0476(16) Uani 1 1 d . . . H30A H 0.1392 1.0142 0.9155 0.071 Uiso 1 1 calc R . . H30B H 0.1565 0.9666 0.8874 0.071 Uiso 1 1 calc R . . H30C H 0.1056 0.9688 0.9426 0.071 Uiso 1 1 calc R . . C31 C -0.0448(5) 1.0198(2) 0.9001(3) 0.0503(17) Uani 1 1 d . . . H31A H -0.0495 1.0096 0.9382 0.075 Uiso 1 1 calc R . . H31B H -0.1065 1.0196 0.8789 0.075 Uiso 1 1 calc R . . H31C H -0.0196 1.0504 0.9009 0.075 Uiso 1 1 calc R . . C32 C -0.0814(4) 1.0164(2) 0.7604(3) 0.0405(15) Uani 1 1 d . . . H32 H -0.1067 1.0408 0.7828 0.049 Uiso 1 1 calc R . . C33 C -0.1482(4) 0.9776(2) 0.7588(3) 0.0532(19) Uani 1 1 d . . . H33A H -0.2110 0.9884 0.7466 0.080 Uiso 1 1 calc R . . H33B H -0.1465 0.9644 0.7961 0.080 Uiso 1 1 calc R . . H33C H -0.1307 0.9547 0.7328 0.080 Uiso 1 1 calc R . . C34 C -0.0812(5) 1.0344(3) 0.7011(3) 0.061(2) Uani 1 1 d . . . H34A H -0.0497 1.0128 0.6790 0.092 Uiso 1 1 calc R . . H34B H -0.0484 1.0633 0.7022 0.092 Uiso 1 1 calc R . . H34C H -0.1452 1.0386 0.6842 0.092 Uiso 1 1 calc R . . C35 C 0.0982(5) 1.0915(2) 0.8177(3) 0.0500(17) Uani 1 1 d . . . H35A H 0.1502 1.1126 0.8183 0.075 Uiso 1 1 calc R . . H35B H 0.0823 1.0872 0.8557 0.075 Uiso 1 1 calc R . . H35C H 0.0444 1.1037 0.7943 0.075 Uiso 1 1 calc R . . C36 C 0.1258(4) 1.0462(2) 0.7941(3) 0.0397(14) Uani 1 1 d . . . H36 H 0.1819 1.0356 0.8185 0.048 Uiso 1 1 calc R . . C37 C 0.1572(5) 1.0540(2) 0.7349(3) 0.0470(16) Uani 1 1 d . . . H37A H 0.1077 1.0694 0.7112 0.070 Uiso 1 1 calc R . . H37B H 0.1703 1.0249 0.7183 0.070 Uiso 1 1 calc R . . H37C H 0.2134 1.0727 0.7383 0.070 Uiso 1 1 calc R . . P5 P 0.17102(10) 0.83533(5) 0.81796(6) 0.0300(3) Uani 1 1 d . . . P7 P 0.14109(12) 0.89070(5) 0.63540(6) 0.0383(4) Uani 1 1 d . . . P6 P 0.30437(9) 0.89226(4) 0.75423(6) 0.0241(3) Uani 1 1 d . . . P8 P 0.00750(9) 0.83695(5) 0.70128(6) 0.0303(3) Uani 1 1 d . . . C17 C 0.2855(4) 0.8527(2) 0.8553(2) 0.0404(15) Uani 1 1 d . . . H17A H 0.2800 0.8564 0.8955 0.049 Uiso 1 1 calc R . . H17B H 0.3324 0.8291 0.8511 0.049 Uiso 1 1 calc R . . C18 C 0.3155(4) 0.8970(2) 0.8310(2) 0.0405(15) Uani 1 1 d . . . H18A H 0.3806 0.9037 0.8454 0.049 Uiso 1 1 calc R . . H18B H 0.2759 0.9219 0.8420 0.049 Uiso 1 1 calc R . . C19 C 0.0215(4) 0.8749(3) 0.6016(3) 0.0486(17) Uani 1 1 d . . . H19A H 0.0002 0.8974 0.5727 0.058 Uiso 1 1 calc R . . H19B H 0.0239 0.8451 0.5834 0.058 Uiso 1 1 calc R . . C20 C -0.0471(4) 0.8732(2) 0.6455(3) 0.0456(16) Uani 1 1 d . . . H20A H -0.1073 0.8604 0.6294 0.055 Uiso 1 1 calc R . . H20B H -0.0579 0.9038 0.6598 0.055 Uiso 1 1 calc R . . C21 C 0.2120(4) 0.8748(2) 0.5818(2) 0.0424(15) Uani 1 1 d . . . H21A H 0.1809 0.8837 0.5453 0.064 Uiso 1 1 calc R . . H21B H 0.2213 0.8421 0.5825 0.064 Uiso 1 1 calc R . . H21C H 0.2723 0.8900 0.5884 0.064 Uiso 1 1 calc R . . C22 C 0.1330(5) 0.9513(2) 0.6281(3) 0.0499(17) Uani 1 1 d . . . H22A H 0.1941 0.9647 0.6389 0.075 Uiso 1 1 calc R . . H22B H 0.0886 0.9629 0.6522 0.075 Uiso 1 1 calc R . . H22C H 0.1120 0.9589 0.5893 0.075 Uiso 1 1 calc R . . C23 C -0.0240(4) 0.7809(2) 0.6758(3) 0.0514(18) Uani 1 1 d . . . H23A H -0.0911 0.7795 0.6650 0.077 Uiso 1 1 calc R . . H23B H -0.0064 0.7588 0.7052 0.077 Uiso 1 1 calc R . . H23C H 0.0087 0.7742 0.6435 0.077 Uiso 1 1 calc R . . C24 C -0.0775(5) 0.8435(3) 0.7522(3) 0.0572(19) Uani 1 1 d . . . H24A H -0.1405 0.8406 0.7331 0.086 Uiso 1 1 calc R . . H24B H -0.0701 0.8732 0.7697 0.086 Uiso 1 1 calc R . . H24C H -0.0669 0.8201 0.7808 0.086 Uiso 1 1 calc R . . C25 C 0.1667(5) 0.7770(2) 0.8398(3) 0.0475(16) Uani 1 1 d . . . H25A H 0.1806 0.7752 0.8804 0.071 Uiso 1 1 calc R . . H25B H 0.2125 0.7594 0.8222 0.071 Uiso 1 1 calc R . . H25C H 0.1045 0.7648 0.8287 0.071 Uiso 1 1 calc R . . C26 C 0.0952(5) 0.8612(2) 0.8631(2) 0.0409(15) Uani 1 1 d . . . H26A H 0.0308 0.8525 0.8511 0.061 Uiso 1 1 calc R . . H26B H 0.1010 0.8941 0.8612 0.061 Uiso 1 1 calc R . . H26C H 0.1125 0.8511 0.9015 0.061 Uiso 1 1 calc R . . C27 C 0.4129(4) 0.8645(2) 0.7448(3) 0.0480(17) Uani 1 1 d . . . H27A H 0.4273 0.8694 0.7067 0.072 Uiso 1 1 calc R . . H27B H 0.4072 0.8322 0.7516 0.072 Uiso 1 1 calc R . . H27C H 0.4627 0.8771 0.7710 0.072 Uiso 1 1 calc R . . C28 C 0.3291(4) 0.9500(2) 0.7365(3) 0.0490(17) Uani 1 1 d . . . H28A H 0.3806 0.9615 0.7625 0.073 Uiso 1 1 calc R . . H28B H 0.2739 0.9687 0.7390 0.073 Uiso 1 1 calc R . . H28C H 0.3463 0.9512 0.6985 0.073 Uiso 1 1 calc R . . F7A F 1.0861(11) 0.8108(5) 0.4162(7) 0.052(2) Uiso 0.256(9) 1 d P B 3 F9A F 1.0548(14) 0.8569(8) 0.4713(9) 0.060(6) Uiso 0.256(9) 1 d P B 3 F7 F 1.0700(4) 0.8312(3) 0.4589(3) 0.080(3) Uani 0.744(9) 1 d P B 4 F9 F 1.0364(4) 0.8995(3) 0.4551(3) 0.082(3) Uani 0.744(9) 1 d P B 4 F14A F 0.5671(8) 0.9051(4) 0.6616(4) 0.052(2) Uiso 0.386(13) 1 d P C 5 F15A F 0.7089(10) 0.8939(5) 0.7049(7) 0.052(2) Uiso 0.386(13) 1 d P C 5 F13A F 0.6366(9) 0.8439(4) 0.6714(4) 0.052(2) Uiso 0.386(13) 1 d P C 5 F14 F 0.5707(5) 0.8748(4) 0.6603(3) 0.076(3) Uani 0.614(13) 1 d P C 6 F15 F 0.6869(7) 0.8392(3) 0.6796(3) 0.076(3) Uani 0.614(13) 1 d P C 6 F13 F 0.6868(7) 0.9114(3) 0.7045(3) 0.059(3) Uani 0.614(13) 1 d P C 6 C87 C -0.0643(14) 0.5987(7) 0.4726(9) 0.089(6) Uiso 0.50 1 d PD D 7 H87A H -0.0122 0.5862 0.4543 0.107 Uiso 0.50 1 calc PR D 7 H87B H -0.0474 0.6019 0.5132 0.107 Uiso 0.50 1 calc PR D 7 C88 C -0.1618(14) 0.5739(8) 0.4556(11) 0.110(7) Uiso 0.50 1 d PD D 7 H88A H -0.2121 0.5926 0.4668 0.164 Uiso 0.50 1 calc PR D 7 H88B H -0.1618 0.5447 0.4745 0.164 Uiso 0.50 1 calc PR D 7 H88C H -0.1709 0.5694 0.4153 0.164 Uiso 0.50 1 calc PR D 7 O2 O -0.1202(7) 0.6512(3) 0.4371(4) 0.054(2) Uiso 0.50 1 d P D 7 C85 C -0.0981(13) 0.7232(6) 0.4144(8) 0.065(5) Uiso 0.50 1 d P D 7 H85A H -0.1214 0.7114 0.3776 0.098 Uiso 0.50 1 calc PR D 7 H85B H -0.0424 0.7413 0.4115 0.098 Uiso 0.50 1 calc PR D 7 H85C H -0.1459 0.7421 0.4284 0.098 Uiso 0.50 1 calc PR D 7 C86 C -0.0756(12) 0.6863(6) 0.4523(7) 0.068(4) Uiso 0.50 1 d P D 7 H86A H -0.0083 0.6799 0.4545 0.082 Uiso 0.50 1 calc PR D 7 H86B H -0.0899 0.6950 0.4899 0.082 Uiso 0.50 1 calc PR D 7 O2A O -0.0495(10) 0.6536(5) 0.4670(6) 0.092(4) Uiso 0.50 1 d P E 8 C86A C -0.1200(16) 0.6809(7) 0.4153(10) 0.101(7) Uiso 0.50 1 d PD E 8 H86C H -0.1121 0.6699 0.3775 0.121 Uiso 0.50 1 calc PR E 8 H86D H -0.1864 0.6806 0.4214 0.121 Uiso 0.50 1 calc PR E 8 C88A C -0.1290(13) 0.5876(6) 0.4955(8) 0.073(4) Uiso 0.50 1 d P E 8 H88D H -0.0943 0.5600 0.4898 0.109 Uiso 0.50 1 calc PR E 8 H88E H -0.1956 0.5808 0.4919 0.109 Uiso 0.50 1 calc PR E 8 H88F H -0.1095 0.5996 0.5327 0.109 Uiso 0.50 1 calc PR E 8 C87A C -0.1159(18) 0.6116(8) 0.4655(10) 0.098(7) Uiso 0.50 1 d P E 8 H87C H -0.1780 0.6241 0.4526 0.117 Uiso 0.50 1 calc PR E 8 H87D H -0.0985 0.5933 0.4341 0.117 Uiso 0.50 1 calc PR E 8 C85A C -0.0729(16) 0.7260(6) 0.4291(9) 0.073(4) Uiso 0.50 1 d PD E 8 H85D H -0.1081 0.7429 0.4545 0.109 Uiso 0.50 1 calc PR E 8 H85E H -0.0708 0.7433 0.3948 0.109 Uiso 0.50 1 calc PR E 8 H85F H -0.0097 0.7209 0.4468 0.109 Uiso 0.50 1 calc PR E 8 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 B1 0.015(3) 0.025(3) 0.019(3) 0.006(2) 0.004(2) -0.002(2) Cr1 0.0161(4) 0.0199(4) 0.0155(4) -0.0002(3) 0.0012(3) 0.0002(3) Cr2 0.0195(4) 0.0199(4) 0.0203(4) 0.0005(3) -0.0022(3) 0.0005(3) P1 0.0208(7) 0.0243(7) 0.0182(7) 0.0014(5) -0.0010(5) 0.0006(5) P2 0.0227(7) 0.0250(7) 0.0235(7) 0.0046(5) 0.0082(5) 0.0032(5) P3 0.0253(7) 0.0344(8) 0.0234(7) -0.0050(6) -0.0070(6) 0.0070(6) P4 0.0246(7) 0.0275(7) 0.0255(7) -0.0061(6) 0.0067(6) -0.0076(6) Si1 0.0280(8) 0.0242(7) 0.0205(7) -0.0044(6) 0.0014(6) 0.0042(6) N1 0.015(2) 0.022(2) 0.015(2) -0.0008(17) -0.0028(16) -0.0018(17) N2 0.022(2) 0.020(2) 0.016(2) 0.0037(17) -0.0034(17) -0.0020(18) F1 0.111(3) 0.044(2) 0.0228(19) -0.0080(16) 0.002(2) -0.007(2) F2 0.077(3) 0.0263(19) 0.052(2) -0.0046(16) -0.0122(19) -0.0006(17) F3 0.049(2) 0.045(2) 0.057(2) 0.0029(18) -0.0247(18) -0.0128(17) F4 0.0311(18) 0.080(3) 0.0312(18) -0.0184(18) 0.0161(15) -0.0054(17) F5 0.070(3) 0.037(2) 0.051(2) -0.0119(17) 0.0050(19) -0.0126(18) F6 0.0373(19) 0.064(2) 0.0206(16) -0.0060(15) -0.0029(14) 0.0111(17) F8 0.029(2) 0.139(4) 0.050(2) 0.020(3) 0.0014(18) -0.022(2) F10 0.121(4) 0.043(2) 0.033(2) 0.0074(17) 0.009(2) -0.027(2) F11 0.052(2) 0.046(2) 0.095(3) 0.002(2) 0.004(2) -0.0216(19) F12 0.100(3) 0.033(2) 0.047(2) -0.0066(17) 0.004(2) -0.002(2) F16 0.042(2) 0.162(5) 0.091(3) -0.088(4) 0.046(2) -0.042(3) F17 0.0280(17) 0.082(3) 0.0274(18) -0.0072(17) 0.0010(14) -0.0193(17) F18 0.0218(19) 0.125(4) 0.134(4) 0.092(4) -0.008(2) -0.017(2) F19 0.122(4) 0.042(2) 0.049(2) 0.0119(19) -0.003(2) -0.029(2) F20 0.070(3) 0.088(4) 0.196(6) 0.097(4) 0.018(4) 0.031(3) F21 0.277(8) 0.034(2) 0.027(2) 0.0126(18) 0.039(3) 0.007(3) F22 0.173(6) 0.061(3) 0.122(4) 0.062(3) -0.116(4) -0.052(3) F23 0.042(2) 0.109(3) 0.028(2) 0.026(2) -0.0003(16) 0.014(2) F24 0.033(2) 0.094(3) 0.047(2) -0.009(2) -0.0113(17) 0.028(2) C1 0.019(2) 0.024(3) 0.015(2) -0.001(2) 0.0011(19) 0.000(2) C2 0.024(3) 0.029(3) 0.016(3) 0.001(2) 0.001(2) -0.004(2) C3 0.026(3) 0.020(3) 0.022(3) 0.001(2) 0.001(2) 0.004(2) C4 0.025(3) 0.037(3) 0.028(3) 0.004(2) -0.008(2) -0.002(2) C5 0.029(3) 0.045(4) 0.052(4) -0.013(3) -0.013(3) -0.002(3) C6 0.027(3) 0.040(3) 0.040(3) -0.009(3) 0.001(3) -0.005(2) C7 0.018(3) 0.039(3) 0.034(3) 0.001(3) -0.005(2) -0.001(2) C8 0.020(3) 0.036(3) 0.042(3) 0.011(3) 0.010(2) 0.005(2) C9 0.034(3) 0.031(3) 0.030(3) 0.005(2) -0.007(2) 0.003(2) C10 0.040(3) 0.045(4) 0.025(3) -0.009(3) -0.001(3) -0.004(3) C11 0.049(4) 0.038(3) 0.028(3) 0.006(3) 0.017(3) 0.004(3) C12 0.035(3) 0.027(3) 0.034(3) 0.008(2) 0.013(3) 0.001(2) C13 0.047(4) 0.065(4) 0.028(3) -0.017(3) -0.006(3) 0.016(3) C14 0.049(4) 0.044(4) 0.036(3) -0.002(3) -0.011(3) 0.015(3) C15 0.028(3) 0.051(4) 0.041(4) -0.009(3) 0.014(3) -0.007(3) C16 0.043(3) 0.032(3) 0.037(3) 0.001(3) 0.009(3) -0.007(3) C38 0.074(5) 0.035(4) 0.110(7) -0.010(4) 0.052(5) -0.005(4) C39 0.057(4) 0.031(3) 0.036(3) -0.002(3) 0.015(3) -0.002(3) C40 0.062(4) 0.031(3) 0.066(5) 0.009(3) 0.020(4) 0.013(3) C41 0.050(4) 0.073(5) 0.075(5) -0.044(4) -0.024(4) 0.017(4) C42 0.045(3) 0.038(3) 0.026(3) -0.012(3) -0.008(3) 0.018(3) C43 0.092(6) 0.066(5) 0.019(3) -0.002(3) 0.002(3) 0.034(4) C44 0.032(3) 0.072(5) 0.059(5) -0.029(4) -0.006(3) 0.009(3) C45 0.030(3) 0.036(3) 0.045(4) -0.008(3) 0.011(3) 0.004(3) C46 0.033(3) 0.057(4) 0.058(4) -0.019(3) 0.014(3) 0.004(3) C47 0.011(2) 0.033(3) 0.019(3) 0.004(2) -0.0039(19) 0.000(2) C48 0.016(2) 0.035(3) 0.022(3) -0.001(2) 0.001(2) -0.005(2) C49 0.019(3) 0.043(3) 0.021(3) -0.002(2) 0.000(2) -0.001(2) C50 0.030(3) 0.031(3) 0.023(3) -0.005(2) -0.004(2) 0.000(2) C51 0.032(3) 0.028(3) 0.023(3) 0.003(2) -0.003(2) -0.002(2) C52 0.024(3) 0.032(3) 0.022(3) 0.005(2) 0.002(2) -0.005(2) C53 0.031(3) 0.055(4) 0.028(3) -0.008(3) 0.003(3) -0.019(3) C54 0.062(4) 0.038(4) 0.030(3) -0.001(3) -0.003(3) -0.014(3) C55 0.018(2) 0.025(3) 0.013(2) -0.004(2) 0.0033(19) -0.002(2) C56 0.021(3) 0.026(3) 0.011(2) 0.002(2) 0.0026(19) 0.000(2) C57 0.019(3) 0.036(3) 0.013(2) -0.001(2) 0.005(2) -0.001(2) C58 0.026(3) 0.032(3) 0.015(2) -0.005(2) -0.002(2) 0.012(2) C59 0.030(3) 0.023(3) 0.014(2) -0.002(2) 0.000(2) 0.003(2) C60 0.026(3) 0.023(3) 0.016(2) -0.004(2) 0.005(2) -0.005(2) C61 0.016(3) 0.060(4) 0.019(3) 0.005(3) 0.000(2) 0.003(3) C62 0.050(4) 0.025(3) 0.030(3) 0.003(2) -0.002(3) 0.002(3) C63 0.016(2) 0.024(3) 0.019(3) 0.005(2) 0.004(2) 0.001(2) C64 0.016(2) 0.024(3) 0.022(3) 0.002(2) 0.002(2) -0.002(2) C65 0.019(3) 0.025(3) 0.019(3) 0.007(2) 0.004(2) 0.001(2) C66 0.019(3) 0.045(3) 0.020(3) 0.006(2) 0.010(2) 0.007(2) C67 0.019(3) 0.058(4) 0.021(3) 0.007(3) 0.003(2) -0.001(3) C68 0.022(3) 0.048(3) 0.014(3) 0.005(2) 0.000(2) -0.002(2) C69 0.023(3) 0.038(3) 0.027(3) -0.006(2) 0.009(2) -0.002(2) C70 0.026(3) 0.126(7) 0.019(3) 0.011(4) 0.005(3) -0.007(4) C71 0.011(2) 0.031(3) 0.021(3) 0.002(2) 0.0057(19) 0.002(2) C72 0.015(2) 0.027(3) 0.025(3) 0.004(2) -0.001(2) -0.004(2) C73 0.015(2) 0.036(3) 0.029(3) 0.010(2) -0.001(2) 0.002(2) C74 0.019(3) 0.027(3) 0.032(3) 0.005(2) 0.004(2) 0.001(2) C75 0.024(3) 0.030(3) 0.017(3) -0.001(2) 0.005(2) 0.001(2) C76 0.021(3) 0.030(3) 0.015(2) 0.004(2) 0.001(2) 0.005(2) C77 0.038(4) 0.035(3) 0.052(4) 0.012(3) -0.020(3) -0.005(3) C78 0.055(4) 0.028(3) 0.031(3) 0.000(3) -0.007(3) 0.000(3) O1 0.191(11) 0.068(6) 0.059(5) -0.011(4) 0.020(6) -0.030(6) C91 0.035(11) 0.061(12) 0.052(10) -0.008(8) 0.002(11) -0.011(11) C91A 0.035(10) 0.041(8) 0.048(9) -0.009(6) -0.008(10) 0.003(10) Si2 0.0282(8) 0.0320(9) 0.0393(9) -0.0015(7) -0.0022(7) 0.0058(7) C29 0.036(3) 0.041(3) 0.038(3) 0.000(3) 0.007(3) 0.004(3) C30 0.044(4) 0.053(4) 0.045(4) -0.005(3) -0.002(3) 0.012(3) C31 0.051(4) 0.058(4) 0.044(4) 0.008(3) 0.012(3) 0.014(3) C32 0.037(3) 0.040(3) 0.044(4) -0.009(3) 0.002(3) 0.011(3) C33 0.025(3) 0.060(4) 0.071(5) -0.020(4) -0.009(3) 0.009(3) C34 0.057(5) 0.087(6) 0.037(4) -0.001(4) -0.008(3) 0.025(4) C35 0.044(4) 0.044(4) 0.064(5) -0.014(3) 0.013(3) -0.003(3) C36 0.033(3) 0.037(3) 0.048(4) 0.000(3) 0.003(3) 0.003(3) C37 0.053(4) 0.036(4) 0.054(4) 0.000(3) 0.014(3) 0.001(3) P5 0.0324(8) 0.0317(8) 0.0271(8) 0.0049(6) 0.0078(6) 0.0036(6) P7 0.0526(10) 0.0386(9) 0.0228(8) 0.0035(6) 0.0011(7) 0.0134(7) P6 0.0237(7) 0.0205(7) 0.0270(7) 0.0014(5) -0.0017(6) -0.0033(5) P8 0.0216(7) 0.0291(8) 0.0382(8) -0.0010(6) -0.0051(6) -0.0007(6) C17 0.045(4) 0.048(4) 0.027(3) 0.003(3) -0.004(3) -0.003(3) C18 0.032(3) 0.052(4) 0.036(3) -0.006(3) -0.004(3) -0.010(3) C19 0.044(4) 0.070(5) 0.029(3) 0.003(3) -0.006(3) 0.020(3) C20 0.040(4) 0.051(4) 0.044(4) 0.004(3) -0.007(3) 0.003(3) C21 0.042(4) 0.059(4) 0.028(3) 0.002(3) 0.010(3) 0.002(3) C22 0.067(5) 0.045(4) 0.039(4) 0.011(3) 0.011(3) 0.008(3) C23 0.034(3) 0.041(4) 0.077(5) -0.013(3) -0.005(3) -0.007(3) C24 0.038(4) 0.085(6) 0.049(4) 0.001(4) 0.006(3) -0.005(4) C25 0.067(5) 0.038(4) 0.037(4) 0.005(3) 0.003(3) 0.001(3) C26 0.055(4) 0.042(4) 0.026(3) 0.002(3) 0.005(3) 0.001(3) C27 0.028(3) 0.046(4) 0.073(5) -0.017(3) 0.015(3) -0.005(3) C28 0.042(4) 0.037(4) 0.066(5) 0.012(3) -0.001(3) -0.010(3) F7 0.041(3) 0.080(5) 0.106(7) 0.055(5) -0.047(4) -0.016(4) F9 0.031(3) 0.116(6) 0.099(5) -0.053(5) 0.007(3) -0.034(3) F14 0.055(4) 0.138(7) 0.040(3) 0.004(3) 0.023(2) -0.034(4) F15 0.055(4) 0.138(7) 0.040(3) 0.004(3) 0.023(2) -0.034(4) F13 0.103(7) 0.053(5) 0.026(3) -0.029(4) 0.031(4) -0.041(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 B1 C55 1.634(7) . ? B1 C71 1.639(7) . ? B1 C47 1.642(7) . ? B1 C63 1.651(7) . ? Cr1 N1 1.852(4) . ? Cr1 C1 2.055(5) . ? Cr1 P4 2.3422(15) . ? Cr1 P3 2.3424(15) . ? Cr1 P1 2.3466(14) . ? Cr1 P2 2.3572(15) . ? Cr2 N2 1.861(4) . ? Cr2 C3 2.045(5) . ? Cr2 P6 2.3435(15) . ? Cr2 P7 2.3477(17) . ? Cr2 P8 2.3526(16) . ? Cr2 P5 2.3708(16) . ? P1 C9 1.825(5) . ? P1 C10 1.825(6) . ? P1 C7 1.845(5) . ? P2 C11 1.817(6) . ? P2 C12 1.822(5) . ? P2 C8 1.842(5) . ? P3 C14 1.815(6) . ? P3 C13 1.816(6) . ? P3 C5 1.861(7) . ? P4 C15 1.824(6) . ? P4 C16 1.828(6) . ? P4 C6 1.838(6) . ? Si1 C2 1.838(5) . ? Si1 C42 1.879(5) . ? Si1 C39 1.880(6) . ? Si1 C45 1.911(6) . ? N1 N2 1.196(5) . ? F1 C78 1.336(7) . ? F2 C78 1.333(7) . ? F3 C78 1.354(7) . ? F4 C69 1.340(6) . ? F5 C69 1.345(6) . ? F6 C69 1.324(6) . ? F8 C70 1.281(7) . ? F10 C54 1.331(7) . ? F11 C54 1.330(8) . ? F12 C54 1.337(7) . ? F16 C61 1.298(7) . ? F17 C61 1.315(6) . ? F18 C61 1.336(7) . ? F19 C62 1.314(7) . ? F20 C62 1.316(7) . ? F21 C62 1.298(7) . ? F22 C77 1.307(7) . ? F23 C77 1.330(8) . ? F24 C77 1.320(7) . ? C1 C2 1.224(7) . ? C3 C4 1.217(7) . ? C4 Si2 1.853(6) . ? C5 C6 1.520(9) . ? C7 C8 1.517(8) . ? C38 C39 1.501(9) . ? C39 C40 1.548(8) . ? C41 C42 1.520(9) . ? C42 C43 1.530(9) . ? C44 C45 1.524(9) . ? C45 C46 1.541(8) . ? C47 C48 1.392(7) . ? C47 C52 1.404(7) . ? C48 C49 1.404(7) . ? C49 C50 1.379(8) . ? C49 C53 1.469(8) . ? C50 C51 1.384(8) . ? C51 C52 1.378(7) . ? C51 C54 1.502(8) . ? C53 F15A 1.254(17) . ? C53 F14 1.262(9) . ? C53 F13A 1.274(14) . ? C53 F13 1.336(9) . ? C53 F14A 1.415(12) . ? C53 F15 1.478(12) . ? C55 C56 1.401(7) . ? C55 C60 1.407(7) . ? C56 C57 1.389(7) . ? C57 C58 1.378(7) . ? C57 C61 1.506(7) . ? C58 C59 1.386(7) . ? C59 C60 1.390(7) . ? C59 C62 1.482(7) . ? C63 C68 1.392(7) . ? C63 C64 1.395(7) . ? C64 C65 1.388(7) . ? C65 C66 1.386(7) . ? C65 C69 1.487(7) . ? C66 C67 1.385(8) . ? C67 C68 1.394(7) . ? C67 C70 1.508(8) . ? C70 F9A 1.17(2) . ? C70 F7 1.281(9) . ? C70 F9 1.403(10) . ? C70 F7A 1.667(18) . ? C71 C76 1.403(7) . ? C71 C72 1.404(7) . ? C72 C73 1.384(7) . ? C73 C74 1.381(7) . ? C73 C77 1.512(8) . ? C74 C75 1.381(7) . ? C75 C76 1.387(7) . ? C75 C78 1.483(8) . ? O1 C90 1.359(11) . ? O1 C90 1.359(11) 3_676 ? O1 C90A 1.390(13) . ? O1 C90A 1.390(13) 3_676 ? C90 C91 1.35(3) . ? C90A C91A 1.14(2) . ? Si2 C32 1.872(6) . ? Si2 C36 1.874(6) . ? Si2 C29 1.914(6) . ? C29 C30 1.524(8) . ? C29 C31 1.546(8) . ? C32 C33 1.501(9) . ? C32 C34 1.531(9) . ? C35 C36 1.533(8) . ? C36 C37 1.567(9) . ? P5 C26 1.808(6) . ? P5 C25 1.814(6) . ? P5 C17 1.870(6) . ? P7 C22 1.807(6) . ? P7 C21 1.808(6) . ? P7 C19 1.891(7) . ? P6 C28 1.813(6) . ? P6 C27 1.813(6) . ? P6 C18 1.851(6) . ? P8 C23 1.813(6) . ? P8 C20 1.834(6) . ? P8 C24 1.850(7) . ? C17 C18 1.525(9) . ? C19 C20 1.537(9) . ? C87 C88 1.605(17) . ? C87 O2 1.91(2) . ? O2 C86 1.258(19) . ? C85 C86 1.44(2) . ? O2A C87A 1.57(3) . ? O2A C86A 1.72(3) . ? C86A C85A 1.523(17) . ? C88A C87A 1.05(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C55 B1 C71 111.9(4) . . ? C55 B1 C47 104.0(4) . . ? C71 B1 C47 114.1(4) . . ? C55 B1 C63 111.4(4) . . ? C71 B1 C63 103.3(4) . . ? C47 B1 C63 112.4(4) . . ? N1 Cr1 C1 178.03(18) . . ? N1 Cr1 P4 98.91(13) . . ? C1 Cr1 P4 79.15(14) . . ? N1 Cr1 P3 94.02(12) . . ? C1 Cr1 P3 85.41(13) . . ? P4 Cr1 P3 82.86(6) . . ? N1 Cr1 P1 93.90(12) . . ? C1 Cr1 P1 86.65(13) . . ? P4 Cr1 P1 95.11(5) . . ? P3 Cr1 P1 172.04(6) . . ? N1 Cr1 P2 100.69(13) . . ? C1 Cr1 P2 81.26(14) . . ? P4 Cr1 P2 160.34(6) . . ? P3 Cr1 P2 97.20(6) . . ? P1 Cr1 P2 82.11(5) . . ? N2 Cr2 C3 178.2(2) . . ? N2 Cr2 P6 96.71(13) . . ? C3 Cr2 P6 81.67(15) . . ? N2 Cr2 P7 96.53(13) . . ? C3 Cr2 P7 82.97(14) . . ? P6 Cr2 P7 96.91(6) . . ? N2 Cr2 P8 99.26(13) . . ? C3 Cr2 P8 82.37(15) . . ? P6 Cr2 P8 164.00(6) . . ? P7 Cr2 P8 82.18(6) . . ? N2 Cr2 P5 96.94(12) . . ? C3 Cr2 P5 83.60(14) . . ? P6 Cr2 P5 82.44(5) . . ? P7 Cr2 P5 166.50(6) . . ? P8 Cr2 P5 94.72(6) . . ? C9 P1 C10 100.4(3) . . ? C9 P1 C7 100.7(3) . . ? C10 P1 C7 103.1(3) . . ? C9 P1 Cr1 121.45(19) . . ? C10 P1 Cr1 118.7(2) . . ? C7 P1 Cr1 109.72(18) . . ? C11 P2 C12 100.1(3) . . ? C11 P2 C8 100.3(3) . . ? C12 P2 C8 103.0(3) . . ? C11 P2 Cr1 124.0(2) . . ? C12 P2 Cr1 117.70(18) . . ? C8 P2 Cr1 108.69(18) . . ? C14 P3 C13 100.3(3) . . ? C14 P3 C5 102.3(3) . . ? C13 P3 C5 101.1(3) . . ? C14 P3 Cr1 119.7(2) . . ? C13 P3 Cr1 121.5(2) . . ? C5 P3 Cr1 108.9(2) . . ? C15 P4 C16 99.7(3) . . ? C15 P4 C6 102.7(3) . . ? C16 P4 C6 101.9(3) . . ? C15 P4 Cr1 119.1(2) . . ? C16 P4 Cr1 122.6(2) . . ? C6 P4 Cr1 108.1(2) . . ? C2 Si1 C42 109.7(2) . . ? C2 Si1 C39 110.3(2) . . ? C42 Si1 C39 112.1(3) . . ? C2 Si1 C45 106.3(2) . . ? C42 Si1 C45 108.5(3) . . ? C39 Si1 C45 109.8(3) . . ? N2 N1 Cr1 177.9(4) . . ? N1 N2 Cr2 178.3(4) . . ? C2 C1 Cr1 179.6(5) . . ? C1 C2 Si1 176.0(4) . . ? C4 C3 Cr2 178.3(5) . . ? C3 C4 Si2 175.6(5) . . ? C6 C5 P3 109.4(4) . . ? C5 C6 P4 107.8(4) . . ? C8 C7 P1 107.5(4) . . ? C7 C8 P2 109.7(3) . . ? C38 C39 C40 108.7(5) . . ? C38 C39 Si1 114.9(5) . . ? C40 C39 Si1 112.5(4) . . ? C41 C42 C43 110.6(6) . . ? C41 C42 Si1 114.6(5) . . ? C43 C42 Si1 110.4(4) . . ? C44 C45 C46 109.7(5) . . ? C44 C45 Si1 112.3(4) . . ? C46 C45 Si1 115.6(4) . . ? C48 C47 C52 114.7(5) . . ? C48 C47 B1 122.8(4) . . ? C52 C47 B1 122.0(4) . . ? C47 C48 C49 122.3(5) . . ? C50 C49 C48 120.9(5) . . ? C50 C49 C53 119.1(5) . . ? C48 C49 C53 119.9(5) . . ? C49 C50 C51 118.1(5) . . ? C52 C51 C50 120.4(5) . . ? C52 C51 C54 120.8(5) . . ? C50 C51 C54 118.8(5) . . ? C51 C52 C47 123.6(5) . . ? F15A C53 F14 125.6(9) . . ? F15A C53 F13A 100.3(10) . . ? F14 C53 F13A 63.2(7) . . ? F15A C53 F13 26.9(6) . . ? F14 C53 F13 114.0(7) . . ? F13A C53 F13 118.8(8) . . ? F15A C53 F14A 112.8(9) . . ? F14 C53 F14A 38.8(5) . . ? F13A C53 F14A 100.9(8) . . ? F13 C53 F14A 89.0(7) . . ? F15A C53 C49 115.2(9) . . ? F14 C53 C49 118.1(6) . . ? F13A C53 C49 117.8(7) . . ? F13 C53 C49 115.0(5) . . ? F14A C53 C49 108.9(6) . . ? F15A C53 F15 79.2(8) . . ? F14 C53 F15 93.3(6) . . ? F13A C53 F15 30.4(5) . . ? F13 C53 F15 104.3(7) . . ? F14A C53 F15 129.6(7) . . ? C49 C53 F15 108.5(5) . . ? F11 C54 F10 108.8(6) . . ? F11 C54 F12 105.8(5) . . ? F10 C54 F12 105.5(5) . . ? F11 C54 C51 111.7(5) . . ? F10 C54 C51 112.0(5) . . ? F12 C54 C51 112.6(5) . . ? C56 C55 C60 115.0(4) . . ? C56 C55 B1 123.4(4) . . ? C60 C55 B1 121.4(4) . . ? C57 C56 C55 122.4(5) . . ? C58 C57 C56 121.2(5) . . ? C58 C57 C61 118.1(5) . . ? C56 C57 C61 120.7(5) . . ? C57 C58 C59 118.1(5) . . ? C58 C59 C60 120.6(5) . . ? C58 C59 C62 119.8(5) . . ? C60 C59 C62 119.6(5) . . ? C59 C60 C55 122.7(5) . . ? F16 C61 F17 106.6(5) . . ? F16 C61 F18 106.1(5) . . ? F17 C61 F18 103.4(5) . . ? F16 C61 C57 113.4(5) . . ? F17 C61 C57 113.3(4) . . ? F18 C61 C57 113.2(4) . . ? F21 C62 F19 103.4(5) . . ? F21 C62 F20 108.5(6) . . ? F19 C62 F20 103.4(5) . . ? F21 C62 C59 113.3(5) . . ? F19 C62 C59 113.4(5) . . ? F20 C62 C59 113.9(5) . . ? C68 C63 C64 116.0(4) . . ? C68 C63 B1 122.9(4) . . ? C64 C63 B1 120.8(4) . . ? C65 C64 C63 123.1(4) . . ? C66 C65 C64 119.7(5) . . ? C66 C65 C69 120.7(4) . . ? C64 C65 C69 119.5(4) . . ? C67 C66 C65 118.5(5) . . ? C66 C67 C68 121.0(5) . . ? C66 C67 C70 119.1(5) . . ? C68 C67 C70 119.9(5) . . ? C63 C68 C67 121.7(5) . . ? F6 C69 F4 107.1(4) . . ? F6 C69 F5 105.9(4) . . ? F4 C69 F5 106.0(4) . . ? F6 C69 C65 113.5(4) . . ? F4 C69 C65 112.7(4) . . ? F5 C69 C65 111.1(4) . . ? F9A C70 F7 40.6(10) . . ? F9A C70 F8 127.3(11) . . ? F7 C70 F8 115.1(7) . . ? F9A C70 F9 62.0(12) . . ? F7 C70 F9 101.7(7) . . ? F8 C70 F9 99.5(7) . . ? F9A C70 C67 117.7(11) . . ? F7 C70 C67 112.4(6) . . ? F8 C70 C67 115.0(5) . . ? F9 C70 C67 111.5(6) . . ? F9A C70 F7A 87.8(13) . . ? F7 C70 F7A 47.7(7) . . ? F8 C70 F7A 81.8(7) . . ? F9 C70 F7A 143.2(8) . . ? C67 C70 F7A 100.7(8) . . ? C76 C71 C72 115.1(4) . . ? C76 C71 B1 120.6(4) . . ? C72 C71 B1 123.9(4) . . ? C73 C72 C71 122.0(5) . . ? C74 C73 C72 121.5(5) . . ? C74 C73 C77 119.9(5) . . ? C72 C73 C77 118.6(5) . . ? C75 C74 C73 118.0(5) . . ? C74 C75 C76 120.6(5) . . ? C74 C75 C78 120.5(5) . . ? C76 C75 C78 118.9(5) . . ? C75 C76 C71 122.8(4) . . ? F22 C77 F24 108.0(6) . . ? F22 C77 F23 106.7(6) . . ? F24 C77 F23 104.7(5) . . ? F22 C77 C73 112.7(5) . . ? F24 C77 C73 111.7(5) . . ? F23 C77 C73 112.6(5) . . ? F2 C78 F1 106.9(5) . . ? F2 C78 F3 106.5(5) . . ? F1 C78 F3 104.7(5) . . ? F2 C78 C75 113.8(5) . . ? F1 C78 C75 112.9(5) . . ? F3 C78 C75 111.4(5) . . ? C90 O1 C90 179.997(4) . 3_676 ? C90 O1 C90A 46.3(6) . . ? C90 O1 C90A 133.7(6) 3_676 . ? C90 O1 C90A 133.7(6) . 3_676 ? C90 O1 C90A 46.3(6) 3_676 3_676 ? C90A O1 C90A 180.0(10) . 3_676 ? C91 C90 O1 145.1(12) . . ? C91A C90A O1 145.1(14) . . ? C4 Si2 C32 110.4(3) . . ? C4 Si2 C36 107.7(3) . . ? C32 Si2 C36 114.4(3) . . ? C4 Si2 C29 107.3(3) . . ? C32 Si2 C29 107.3(3) . . ? C36 Si2 C29 109.6(3) . . ? C30 C29 C31 110.4(5) . . ? C30 C29 Si2 111.1(4) . . ? C31 C29 Si2 115.8(4) . . ? C33 C32 C34 108.3(6) . . ? C33 C32 Si2 112.1(4) . . ? C34 C32 Si2 114.9(5) . . ? C35 C36 C37 109.0(5) . . ? C35 C36 Si2 113.6(4) . . ? C37 C36 Si2 114.2(4) . . ? C26 P5 C25 100.7(3) . . ? C26 P5 C17 99.1(3) . . ? C25 P5 C17 100.4(3) . . ? C26 P5 Cr2 121.4(2) . . ? C25 P5 Cr2 121.8(2) . . ? C17 P5 Cr2 109.4(2) . . ? C22 P7 C21 103.0(3) . . ? C22 P7 C19 99.1(3) . . ? C21 P7 C19 101.2(3) . . ? C22 P7 Cr2 122.0(2) . . ? C21 P7 Cr2 119.5(2) . . ? C19 P7 Cr2 108.4(2) . . ? C28 P6 C27 101.6(3) . . ? C28 P6 C18 99.7(3) . . ? C27 P6 C18 100.5(3) . . ? C28 P6 Cr2 123.3(2) . . ? C27 P6 Cr2 118.5(2) . . ? C18 P6 Cr2 109.50(19) . . ? C23 P8 C20 102.5(3) . . ? C23 P8 C24 99.3(3) . . ? C20 P8 C24 99.4(3) . . ? C23 P8 Cr2 119.5(2) . . ? C20 P8 Cr2 110.7(2) . . ? C24 P8 Cr2 122.2(2) . . ? C18 C17 P5 109.1(4) . . ? C17 C18 P6 109.0(4) . . ? C20 C19 P7 110.1(4) . . ? C19 C20 P8 105.6(4) . . ? C88 C87 O2 86.6(14) . . ? C86 O2 C87 111.4(12) . . ? O2 C86 C85 111.9(16) . . ? C87A O2A C86A 92.5(13) . . ? C85A C86A O2A 92.2(15) . . ? C88A C87A O2A 133(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.667 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.133 #===END data_3(RT) _chemical_name_common 'compound 3(RT) in text ' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H118 B Cr2 F24 N2 P8 Si2' _chemical_formula_weight 1958.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.6116(6) _cell_length_b 30.4203(13) _cell_length_c 24.9312(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.848(2) _cell_angle_gamma 90.00 _cell_volume 11002.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7358 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 21.67 _exptl_crystal_description parallelepiped _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4068 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8762 _exptl_absorpt_correction_T_max 0.9600 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; The room temperature structure of 3 (RT) is isostructural with 3-2Et2O(LT) except that all ether solvate molecules are missing, creating a void space of 1237 A3 per unit cell (determined by SQUEEZE).This accounts for the A-level alert. Trifluoromethyl rotational disorder in the BArF4 anions was modeled as a combination of two sets of equally occupied fluorine positions.Significant improvements in the refinement residuals were noted when the fluorine thermal parameters were refined anisotropically. The large Ueqs and highly variable Ueqs are probably a result of the data collection temperatureas well. Two of the isopropyl groups connected to Si1 were disordered and were refined at 50% occupancy. The disordered carbon atoms were refined isotropically. The simplistic model used for CF3 rotational disorder does not account for slight differences in occupancy between CF3 groups, which leads to variable F Ueqs. A more complex model using a free variable did not cause any improvement in R1, so a reasonalbe fix for that A-level alert does not appear to be feasable. The high and low Ueqs for a variety of C and F atoms (see checkcif) are a result of disorder. An attempt was made to constrain the Ueq parameters to neighboring atoms with the EADP command, but inclusion of this parameter caused R1 to increase to 7.81% from 7.62%. ; _diffrn_ambient_temperature 296(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 197210 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 28.35 _reflns_number_total 27459 _reflns_number_gt 11736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27459 _refine_ls_number_parameters 1237 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1610 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2197 _refine_ls_wR_factor_gt 0.1959 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.005 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 B1 B 0.6950(3) 0.83358(15) 0.45533(16) 0.0578(11) Uani 1 1 d . . . Cr1 Cr 0.29606(4) 0.713446(17) 0.65654(2) 0.04879(16) Uani 1 1 d . I . Cr2 Cr 0.18036(4) 0.854144(17) 0.72052(2) 0.04896(16) Uani 1 1 d . . . P1 P 0.42199(8) 0.71005(4) 0.72470(4) 0.0736(3) Uani 1 1 d . . . P2 P 0.40972(8) 0.74026(4) 0.60468(5) 0.0752(3) Uani 1 1 d . . . P3 P 0.17841(8) 0.70338(4) 0.58446(5) 0.0778(3) Uani 1 1 d . . . P4 P 0.19896(8) 0.66979(4) 0.70285(5) 0.0780(3) Uani 1 1 d . . . P5 P 0.19147(8) 0.83889(4) 0.81568(4) 0.0748(3) Uani 1 1 d . . . P6 P 0.32746(7) 0.88690(3) 0.74358(5) 0.0707(3) Uani 1 1 d . . . P7 P 0.15378(10) 0.88381(4) 0.63177(4) 0.0890(4) Uani 1 1 d . . . P8 P 0.02016(7) 0.83678(4) 0.70602(5) 0.0760(3) Uani 1 1 d . . . Si1 Si 0.40607(13) 0.56549(5) 0.59419(6) 0.1070(5) Uani 1 1 d . . . Si2 Si 0.06524(10) 1.00553(4) 0.76770(7) 0.1018(5) Uani 1 1 d . . . N1 N 0.25250(17) 0.76764(9) 0.68062(10) 0.0431(6) Uani 1 1 d . . . N2 N 0.22505(17) 0.80027(9) 0.69713(10) 0.0430(6) Uani 1 1 d . . . C1 C 0.3398(2) 0.65385(12) 0.63126(14) 0.0567(9) Uani 1 1 d . . . C2 C 0.3659(3) 0.61796(14) 0.61668(15) 0.0709(11) Uani 1 1 d . I . C3 C 0.1339(3) 0.91416(13) 0.74139(14) 0.0588(9) Uani 1 1 d . . . C4 C 0.1066(3) 0.95045(14) 0.75264(16) 0.0708(11) Uani 1 1 d . . . C5 C 0.0982(4) 0.6604(2) 0.6032(3) 0.149(3) Uani 1 1 d . . . H5A H 0.0346 0.6698 0.5902 0.179 Uiso 1 1 calc R . . H5B H 0.1103 0.6331 0.5835 0.179 Uiso 1 1 calc R . . C6 C 0.1015(7) 0.6502(4) 0.6566(3) 0.257(6) Uani 1 1 d . . . H6A H 0.0995 0.6178 0.6597 0.309 Uiso 1 1 calc R . . H6B H 0.0446 0.6617 0.6695 0.309 Uiso 1 1 calc R . . C7 C 0.5221(4) 0.7380(2) 0.7007(3) 0.136(2) Uani 1 1 d . . . H7A H 0.5180 0.7700 0.7070 0.163 Uiso 1 1 calc R . . H7B H 0.5798 0.7271 0.7211 0.163 Uiso 1 1 calc R . . C8 C 0.5236(3) 0.7298(2) 0.6438(3) 0.135(2) Uani 1 1 d . . . H8A H 0.5416 0.6989 0.6386 0.162 Uiso 1 1 calc R . . H8B H 0.5704 0.7490 0.6301 0.162 Uiso 1 1 calc R . . C9 C 0.4739(4) 0.65693(16) 0.7469(2) 0.1185(19) Uani 1 1 d . . . H9A H 0.5220 0.6617 0.7773 0.178 Uiso 1 1 calc R . . H9B H 0.5011 0.6432 0.7170 0.178 Uiso 1 1 calc R . . H9C H 0.4263 0.6376 0.7584 0.178 Uiso 1 1 calc R . . C10 C 0.4142(4) 0.73607(18) 0.7895(2) 0.124(2) Uani 1 1 d . . . H10A H 0.3629 0.7232 0.8061 0.186 Uiso 1 1 calc R . . H10B H 0.4037 0.7677 0.7842 0.186 Uiso 1 1 calc R . . H10C H 0.4718 0.7314 0.8132 0.186 Uiso 1 1 calc R . . C11 C 0.4306(5) 0.71747(19) 0.5406(2) 0.129(2) Uani 1 1 d . . . H11A H 0.3797 0.7254 0.5130 0.194 Uiso 1 1 calc R . . H11B H 0.4349 0.6854 0.5435 0.194 Uiso 1 1 calc R . . H11C H 0.4884 0.7293 0.5303 0.194 Uiso 1 1 calc R . . C12 C 0.4168(4) 0.79850(15) 0.5891(2) 0.1141(18) Uani 1 1 d . . . H12A H 0.4648 0.8032 0.5653 0.171 Uiso 1 1 calc R . . H12B H 0.4321 0.8151 0.6226 0.171 Uiso 1 1 calc R . . H12C H 0.3574 0.8086 0.5708 0.171 Uiso 1 1 calc R . . C13 C 0.1978(4) 0.6829(2) 0.5184(2) 0.145(3) Uani 1 1 d . . . H13A H 0.1435 0.6891 0.4924 0.218 Uiso 1 1 calc R . . H13B H 0.2084 0.6511 0.5204 0.218 Uiso 1 1 calc R . . H13C H 0.2518 0.6975 0.5067 0.218 Uiso 1 1 calc R . . C14 C 0.1001(4) 0.74781(19) 0.5645(2) 0.134(2) Uani 1 1 d . . . H14A H 0.1350 0.7733 0.5541 0.202 Uiso 1 1 calc R . . H14B H 0.0663 0.7558 0.5948 0.202 Uiso 1 1 calc R . . H14C H 0.0563 0.7385 0.5337 0.202 Uiso 1 1 calc R . . C15 C 0.1433(4) 0.69333(19) 0.7581(2) 0.126(2) Uani 1 1 d . . . H15A H 0.0859 0.6775 0.7614 0.189 Uiso 1 1 calc R . . H15B H 0.1295 0.7244 0.7505 0.189 Uiso 1 1 calc R . . H15C H 0.1846 0.6908 0.7919 0.189 Uiso 1 1 calc R . . C16 C 0.2372(5) 0.61796(17) 0.7340(3) 0.149(3) Uani 1 1 d . . . H16A H 0.2836 0.6236 0.7650 0.223 Uiso 1 1 calc R . . H16B H 0.2641 0.5997 0.7076 0.223 Uiso 1 1 calc R . . H16C H 0.1845 0.6026 0.7463 0.223 Uiso 1 1 calc R . . C17 C 0.3064(5) 0.8570(3) 0.8450(2) 0.172(3) Uani 1 1 d . . . H17A H 0.3027 0.8664 0.8827 0.207 Uiso 1 1 calc R . . H17B H 0.3485 0.8314 0.8463 0.207 Uiso 1 1 calc R . . C18 C 0.3477(5) 0.8931(3) 0.8165(2) 0.154(3) Uani 1 1 d . . . H18A H 0.4149 0.8938 0.8280 0.184 Uiso 1 1 calc R . . H18B H 0.3214 0.9214 0.8269 0.184 Uiso 1 1 calc R . . C19 C 0.0293(4) 0.8707(3) 0.6054(2) 0.179(4) Uani 1 1 d . . . H19A H 0.0057 0.8941 0.5798 0.215 Uiso 1 1 calc R . . H19B H 0.0279 0.8428 0.5850 0.215 Uiso 1 1 calc R . . C20 C -0.0333(4) 0.8668(3) 0.6472(3) 0.149(3) Uani 1 1 d . . . H20A H -0.0902 0.8514 0.6319 0.179 Uiso 1 1 calc R . . H20B H -0.0508 0.8966 0.6585 0.179 Uiso 1 1 calc R . . C21 C 0.2081(4) 0.85999(18) 0.57820(18) 0.1049(16) Uani 1 1 d . . . H21A H 0.1796 0.8716 0.5435 0.157 Uiso 1 1 calc R . . H21B H 0.2007 0.8280 0.5787 0.157 Uiso 1 1 calc R . . H21C H 0.2739 0.8673 0.5830 0.157 Uiso 1 1 calc R . . C22 C 0.1540(6) 0.94025(18) 0.6174(2) 0.163(3) Uani 1 1 d . . . H22A H 0.2177 0.9509 0.6200 0.244 Uiso 1 1 calc R . . H22B H 0.1209 0.9561 0.6434 0.244 Uiso 1 1 calc R . . H22C H 0.1234 0.9454 0.5808 0.244 Uiso 1 1 calc R . . C23 C -0.0190(4) 0.78228(17) 0.6920(3) 0.143(3) Uani 1 1 d . . . H23A H -0.0850 0.7828 0.6789 0.214 Uiso 1 1 calc R . . H23B H -0.0089 0.7646 0.7251 0.214 Uiso 1 1 calc R . . H23C H 0.0151 0.7694 0.6644 0.214 Uiso 1 1 calc R . . C24 C -0.0588(4) 0.8531(2) 0.7539(3) 0.154(3) Uani 1 1 d . . . H24A H -0.1156 0.8648 0.7341 0.231 Uiso 1 1 calc R . . H24B H -0.0297 0.8757 0.7782 0.231 Uiso 1 1 calc R . . H24C H -0.0735 0.8274 0.7751 0.231 Uiso 1 1 calc R . . C25 C 0.1960(6) 0.78479(17) 0.8437(2) 0.179(4) Uani 1 1 d . . . H25A H 0.2036 0.7867 0.8832 0.268 Uiso 1 1 calc R . . H25B H 0.2483 0.7688 0.8318 0.268 Uiso 1 1 calc R . . H25C H 0.1387 0.7692 0.8313 0.268 Uiso 1 1 calc R . . C26 C 0.1264(4) 0.8688(2) 0.85982(19) 0.128(2) Uani 1 1 d . . . H26A H 0.0608 0.8621 0.8509 0.192 Uiso 1 1 calc R . . H26B H 0.1364 0.9004 0.8554 0.192 Uiso 1 1 calc R . . H26C H 0.1464 0.8603 0.8973 0.192 Uiso 1 1 calc R . . C27 C 0.4307(3) 0.8586(2) 0.7332(3) 0.144(3) Uani 1 1 d . . . H27A H 0.4306 0.8524 0.6946 0.215 Uiso 1 1 calc R . . H27B H 0.4342 0.8309 0.7534 0.215 Uiso 1 1 calc R . . H27C H 0.4841 0.8770 0.7458 0.215 Uiso 1 1 calc R . . C28 C 0.3514(4) 0.94136(19) 0.7228(4) 0.198(4) Uani 1 1 d . . . H28A H 0.3978 0.9548 0.7495 0.296 Uiso 1 1 calc R . . H28B H 0.2948 0.9589 0.7199 0.296 Uiso 1 1 calc R . . H28C H 0.3749 0.9404 0.6876 0.296 Uiso 1 1 calc R . . C29 C -0.0621(4) 1.0030(2) 0.7774(3) 0.148(3) Uani 1 1 d . . . H29 H -0.0815 1.0340 0.7834 0.178 Uiso 1 1 calc R . . C30 C 0.0692(7) 1.0408(2) 0.7055(4) 0.189(4) Uani 1 1 d . . . H30 H 0.0464 1.0204 0.6753 0.227 Uiso 1 1 calc R . . C31 C 0.1430(6) 1.0300(2) 0.8232(4) 0.190(4) Uani 1 1 d . . . H31 H 0.2012 1.0369 0.8074 0.228 Uiso 1 1 calc R . . C32 C 0.3478(8) 0.5502(3) 0.5266(3) 0.176(4) Uani 1 1 d . I . H32 H 0.3713 0.5208 0.5166 0.211 Uiso 1 1 calc R . . C35 C -0.1215(5) 0.9873(3) 0.7311(4) 0.182(3) Uani 1 1 d . . . H35A H -0.1125 0.9556 0.7270 0.273 Uiso 1 1 calc R . . H35B H -0.1064 1.0025 0.6986 0.273 Uiso 1 1 calc R . . H35C H -0.1859 0.9931 0.7361 0.273 Uiso 1 1 calc R . . C36 C -0.0715(7) 0.9775(4) 0.8318(4) 0.261(6) Uani 1 1 d . . . H36A H -0.1345 0.9807 0.8411 0.391 Uiso 1 1 calc R . . H36B H -0.0280 0.9898 0.8609 0.391 Uiso 1 1 calc R . . H36C H -0.0579 0.9463 0.8271 0.391 Uiso 1 1 calc R . . C37 C -0.0001(8) 1.0768(3) 0.6999(5) 0.281(6) Uani 1 1 d . . . H37A H 0.0180 1.0996 0.7268 0.421 Uiso 1 1 calc R . . H37B H -0.0606 1.0650 0.7056 0.421 Uiso 1 1 calc R . . H37C H -0.0033 1.0894 0.6636 0.421 Uiso 1 1 calc R . . C38 C 0.1705(7) 1.0505(3) 0.6946(5) 0.260(6) Uani 1 1 d . . . H38A H 0.1739 1.0801 0.6795 0.391 Uiso 1 1 calc R . . H38B H 0.1894 1.0289 0.6689 0.391 Uiso 1 1 calc R . . H38C H 0.2115 1.0485 0.7286 0.391 Uiso 1 1 calc R . . C39 C 0.1105(7) 1.0742(3) 0.8445(4) 0.257(6) Uani 1 1 d . . . H39A H 0.0689 1.0687 0.8718 0.386 Uiso 1 1 calc R . . H39B H 0.0778 1.0909 0.8145 0.386 Uiso 1 1 calc R . . H39C H 0.1640 1.0910 0.8606 0.386 Uiso 1 1 calc R . . C40 C 0.1721(7) 1.0016(3) 0.8721(4) 0.239(6) Uani 1 1 d . . . H40A H 0.2211 1.0165 0.8956 0.359 Uiso 1 1 calc R . . H40B H 0.1950 0.9734 0.8603 0.359 Uiso 1 1 calc R . . H40C H 0.1191 0.9966 0.8919 0.359 Uiso 1 1 calc R . . C45 C 0.3706(8) 0.5838(3) 0.4845(3) 0.217(5) Uani 1 1 d . . . H45A H 0.3576 0.5710 0.4483 0.325 Uiso 1 1 calc R I . H45B H 0.4360 0.5917 0.4912 0.325 Uiso 1 1 calc R . . H45C H 0.3329 0.6102 0.4869 0.325 Uiso 1 1 calc R . . C46 C 0.2385(9) 0.5464(4) 0.5287(5) 0.262(6) Uani 1 1 d . . . H46A H 0.2112 0.5759 0.5273 0.393 Uiso 1 1 calc R I . H46B H 0.2270 0.5318 0.5623 0.393 Uiso 1 1 calc R . . H46C H 0.2107 0.5292 0.4978 0.393 Uiso 1 1 calc R . . C47 C 0.7229(2) 0.86787(13) 0.50592(14) 0.0608(10) Uani 1 1 d . . . C48 C 0.6875(2) 0.86341(13) 0.55482(15) 0.0657(10) Uani 1 1 d . . . H48 H 0.6499 0.8386 0.5598 0.079 Uiso 1 1 calc R . . C49 C 0.7041(3) 0.89355(15) 0.59710(17) 0.0751(11) Uani 1 1 d . G . C50 C 0.7550(3) 0.93039(15) 0.5912(2) 0.0848(13) Uani 1 1 d . . . H50 H 0.7655 0.9514 0.6194 0.102 Uiso 1 1 calc R . . C51 C 0.7909(3) 0.93617(15) 0.5427(2) 0.0844(13) Uani 1 1 d . H . C52 C 0.7743(3) 0.90572(14) 0.50155(16) 0.0723(11) Uani 1 1 d . . . H52 H 0.7992 0.9110 0.4687 0.087 Uiso 1 1 calc R . . C53 C 0.6664(5) 0.8855(3) 0.6486(3) 0.1102(19) Uani 1 1 d . . . C54 C 0.8507(8) 0.9761(3) 0.5351(3) 0.123(2) Uani 1 1 d . . . C55 C 0.5984(2) 0.85505(12) 0.42481(13) 0.0558(9) Uani 1 1 d . . . C56 C 0.5109(2) 0.84094(13) 0.43317(13) 0.0596(9) Uani 1 1 d . . . H56 H 0.5052 0.8159 0.4552 0.072 Uiso 1 1 calc R . . C57 C 0.4321(3) 0.86184(15) 0.41079(15) 0.0680(11) Uani 1 1 d . E . C58 C 0.4370(3) 0.89861(15) 0.37918(16) 0.0756(12) Uani 1 1 d . . . H58 H 0.3825 0.9131 0.3639 0.091 Uiso 1 1 calc R . . C59 C 0.5229(3) 0.91402(14) 0.37018(15) 0.0708(11) Uani 1 1 d . F . C60 C 0.6011(3) 0.89185(13) 0.39302(15) 0.0640(10) Uani 1 1 d . . . H60 H 0.6597 0.9027 0.3863 0.077 Uiso 1 1 calc R . . C61 C 0.3385(3) 0.8446(3) 0.4200(2) 0.0930(15) Uani 1 1 d . . . C62 C 0.5319(6) 0.9556(2) 0.3373(2) 0.1062(18) Uani 1 1 d . . . C63 C 0.7750(2) 0.83142(13) 0.41414(13) 0.0578(9) Uani 1 1 d . . . C64 C 0.7561(2) 0.82342(13) 0.35995(15) 0.0646(10) Uani 1 1 d . . . H64 H 0.6934 0.8228 0.3446 0.078 Uiso 1 1 calc R . . C65 C 0.8233(3) 0.81620(14) 0.32609(15) 0.0695(11) Uani 1 1 d . A . C66 C 0.9141(3) 0.81712(15) 0.34593(16) 0.0800(13) Uani 1 1 d . . . H66 H 0.9605 0.8126 0.3229 0.096 Uiso 1 1 calc R . . C67 C 0.9369(3) 0.82470(18) 0.39977(17) 0.0889(15) Uani 1 1 d . B . C68 C 0.8677(3) 0.83152(15) 0.43361(16) 0.0797(12) Uani 1 1 d . . . H68 H 0.8852 0.8364 0.4711 0.096 Uiso 1 1 calc R . . C69 C 0.7963(4) 0.8062(3) 0.2678(2) 0.0994(17) Uani 1 1 d . . . C71 C 0.6828(2) 0.78310(12) 0.47367(13) 0.0563(9) Uani 1 1 d . . . C72 C 0.7317(2) 0.76470(14) 0.52087(14) 0.0614(10) Uani 1 1 d . . . H72 H 0.7685 0.7836 0.5449 0.074 Uiso 1 1 calc R . . C73 C 0.7283(3) 0.72094(14) 0.53348(16) 0.0670(10) Uani 1 1 d . C . C74 C 0.6771(3) 0.69250(14) 0.49964(16) 0.0698(10) Uani 1 1 d . . . H74 H 0.6743 0.6621 0.5082 0.084 Uiso 1 1 calc R . . C75 C 0.6297(3) 0.70890(14) 0.45299(16) 0.0679(10) Uani 1 1 d . D . C76 C 0.6323(2) 0.75292(14) 0.44046(14) 0.0617(10) Uani 1 1 d . . . H76 H 0.5984 0.7630 0.4079 0.074 Uiso 1 1 calc R . . C77 C 0.7814(4) 0.7045(2) 0.5842(2) 0.0910(14) Uani 1 1 d . . . C78 C 0.5713(6) 0.6789(2) 0.4149(3) 0.1080(18) Uani 1 1 d . . . C79 C 1.0373(4) 0.8266(5) 0.4236(3) 0.146(4) Uani 1 1 d . . . F1 F 0.7287(3) 0.83071(16) 0.24521(11) 0.1506(15) Uani 1 1 d . A 1 F2 F 0.8637(2) 0.81202(16) 0.23801(11) 0.1543(16) Uani 1 1 d . A 1 F3 F 0.7548(8) 0.7720(5) 0.2538(5) 0.133(5) Uani 0.50 1 d P A 1 F3A F 0.7842(15) 0.7615(5) 0.2663(6) 0.227(10) Uani 0.50 1 d P A 2 F4 F 1.0664(14) 0.8704(7) 0.4280(18) 0.304(17) Uani 0.50 1 d P B 1 F5 F 1.0878(11) 0.8072(9) 0.3964(12) 0.206(12) Uani 0.50 1 d P B 1 F6 F 1.0558(11) 0.8141(13) 0.4679(7) 0.211(14) Uani 0.50 1 d P B 1 F4A F 1.0878(8) 0.8389(13) 0.3882(5) 0.209(13) Uani 0.50 1 d P B 2 F5A F 1.0621(12) 0.7767(7) 0.4317(10) 0.233(8) Uani 0.50 1 d P B 2 F6A F 1.0521(8) 0.8411(12) 0.4686(8) 0.192(13) Uani 0.50 1 d P B 2 F7 F 0.7571(13) 0.6679(5) 0.6006(8) 0.161(8) Uani 0.50 1 d P C 1 F8 F 0.7704(9) 0.7320(3) 0.6261(4) 0.100(3) Uani 0.50 1 d P C 1 F9 F 0.8657(8) 0.7050(9) 0.5843(7) 0.158(9) Uani 0.50 1 d P C 1 F7A F 0.813(2) 0.6623(8) 0.5770(7) 0.224(12) Uani 0.50 1 d P C 2 F8A F 0.7348(11) 0.6965(13) 0.6204(6) 0.230(13) Uani 0.50 1 d P C 2 F9A F 0.8583(16) 0.7230(7) 0.5952(10) 0.208(14) Uani 0.50 1 d P C 2 F10 F 0.6174(17) 0.6410(8) 0.4109(15) 0.289(16) Uani 0.50 1 d P D 1 F11 F 0.4911(18) 0.6696(11) 0.4299(10) 0.235(15) Uani 0.50 1 d P D 1 F12 F 0.5563(18) 0.6902(8) 0.3642(9) 0.162(11) Uani 0.50 1 d P D 1 F10A F 0.5988(15) 0.6825(8) 0.3685(7) 0.144(6) Uani 0.50 1 d P D 2 F11A F 0.5776(15) 0.6378(4) 0.4259(6) 0.148(7) Uani 0.50 1 d P D 2 F12A F 0.4855(10) 0.6926(6) 0.4088(8) 0.143(6) Uani 0.50 1 d P D 2 F13 F 0.3352(13) 0.8394(12) 0.4706(7) 0.190(11) Uani 0.50 1 d P E 1 F14 F 0.3207(11) 0.8090(8) 0.3980(11) 0.184(8) Uani 0.50 1 d P E 1 F15 F 0.2720(5) 0.8739(6) 0.4032(12) 0.189(6) Uani 0.50 1 d P E 1 F13A F 0.3429(7) 0.8025(7) 0.4373(10) 0.180(9) Uani 0.50 1 d P E 2 F14A F 0.2826(6) 0.8398(7) 0.3777(3) 0.116(4) Uani 0.50 1 d P E 2 F15A F 0.3021(12) 0.8608(8) 0.4560(8) 0.172(11) Uani 0.50 1 d P E 2 F16 F 0.5603(4) 0.94467(12) 0.29076(16) 0.1685(17) Uani 1 1 d . F 1 F17 F 0.6085(9) 0.9775(4) 0.3562(7) 0.122(5) Uani 0.50 1 d P F 1 F18 F 0.4684(9) 0.9814(4) 0.3371(5) 0.131(4) Uani 0.50 1 d P F 1 F17A F 0.5719(18) 0.9866(6) 0.3606(8) 0.226(13) Uani 0.50 1 d P F 2 F18A F 0.4459(11) 0.9683(6) 0.3113(8) 0.236(10) Uani 0.50 1 d P F 2 F19 F 0.632(3) 0.9256(6) 0.6665(11) 0.210(9) Uani 0.50 1 d P G 1 F20 F 0.6026(19) 0.8558(10) 0.6495(7) 0.154(7) Uani 0.50 1 d P G 1 F21 F 0.7263(10) 0.8770(18) 0.6865(7) 0.214(14) Uani 0.50 1 d P G 1 F19A F 0.697(2) 0.9078(8) 0.6889(7) 0.155(8) Uani 0.50 1 d P G 2 F20A F 0.5790(10) 0.8896(12) 0.6420(6) 0.171(8) Uani 0.50 1 d P G 2 F21A F 0.682(3) 0.8461(5) 0.6668(7) 0.153(5) Uani 0.50 1 d P G 2 F22 F 0.899(2) 0.9904(8) 0.5743(6) 0.169(11) Uani 0.50 1 d P H 1 F23 F 0.8111(17) 1.0049(8) 0.5089(17) 0.198(13) Uani 0.50 1 d P H 1 F24 F 0.916(2) 0.9654(8) 0.5021(13) 0.204(10) Uani 0.50 1 d P H 1 F22A F 0.9303(14) 0.9711(8) 0.552(2) 0.229(16) Uani 0.50 1 d P H 2 F23A F 0.8133(18) 1.0117(4) 0.5635(13) 0.175(4) Uani 0.50 1 d P H 2 F24A F 0.831(3) 0.9911(10) 0.4855(10) 0.214(15) Uani 0.50 1 d P H 2 C33 C 0.4212(8) 0.5259(3) 0.6454(4) 0.102(3) Uiso 0.50 1 d P I 5 H33 H 0.4670 0.5392 0.6739 0.122 Uiso 0.50 1 calc PR I 5 C34 C 0.5477(8) 0.5886(4) 0.5766(4) 0.098(3) Uiso 0.50 1 d PD I 5 H34 H 0.5465 0.6193 0.5622 0.118 Uiso 0.50 1 calc PR I 5 C41 C 0.5929(11) 0.5858(6) 0.6438(6) 0.160(6) Uiso 0.50 1 d PD I 5 H41A H 0.5742 0.5581 0.6593 0.239 Uiso 0.50 1 calc PR I 5 H41B H 0.5699 0.6105 0.6635 0.239 Uiso 0.50 1 calc PR I 5 H41C H 0.6604 0.5871 0.6467 0.239 Uiso 0.50 1 calc PR I 5 C42 C 0.5891(12) 0.5584(6) 0.5428(7) 0.204(7) Uiso 0.50 1 d PD I 5 H42A H 0.6358 0.5737 0.5246 0.306 Uiso 0.50 1 calc PR I 5 H42B H 0.5417 0.5463 0.5157 0.306 Uiso 0.50 1 calc PR I 5 H42C H 0.6183 0.5344 0.5649 0.306 Uiso 0.50 1 calc PR I 5 C43 C 0.4642(12) 0.4822(5) 0.6314(6) 0.172(6) Uiso 0.50 1 d P I 5 H43A H 0.5190 0.4764 0.6571 0.257 Uiso 0.50 1 calc PR I 5 H43B H 0.4818 0.4837 0.5947 0.257 Uiso 0.50 1 calc PR I 5 H43C H 0.4193 0.4585 0.6334 0.257 Uiso 0.50 1 calc PR I 5 C44 C 0.3351(12) 0.5186(6) 0.6733(8) 0.163(6) Uiso 0.50 1 d P I 5 H44A H 0.3271 0.4871 0.6792 0.244 Uiso 0.50 1 calc PR I 5 H44B H 0.2812 0.5300 0.6504 0.244 Uiso 0.50 1 calc PR I 5 H44C H 0.3418 0.5339 0.7081 0.244 Uiso 0.50 1 calc PR I 5 C33A C 0.3441(10) 0.5194(4) 0.6369(5) 0.113(4) Uiso 0.50 1 d P I 6 H33A H 0.2772 0.5268 0.6361 0.136 Uiso 0.50 1 calc PR I 6 C34A C 0.5242(9) 0.5616(5) 0.5994(6) 0.128(4) Uiso 0.50 1 d P I 6 H34A H 0.5278 0.5563 0.6392 0.154 Uiso 0.50 1 calc PR I 6 C41A C 0.5893(13) 0.5981(6) 0.6080(9) 0.182(7) Uiso 0.50 1 d P I 6 H41D H 0.6409 0.5896 0.6348 0.273 Uiso 0.50 1 calc PR I 6 H41E H 0.5580 0.6237 0.6213 0.273 Uiso 0.50 1 calc PR I 6 H41F H 0.6125 0.6055 0.5739 0.273 Uiso 0.50 1 calc PR I 6 C42A C 0.571(2) 0.5238(11) 0.5925(14) 0.387(19) Uiso 0.50 1 d P I 6 H42D H 0.6293 0.5306 0.5790 0.580 Uiso 0.50 1 calc PR I 6 H42E H 0.5336 0.5050 0.5664 0.580 Uiso 0.50 1 calc PR I 6 H42F H 0.5827 0.5084 0.6271 0.580 Uiso 0.50 1 calc PR I 6 C43A C 0.3538(12) 0.4726(5) 0.6163(7) 0.181(6) Uiso 0.50 1 d P I 6 H43D H 0.3801 0.4538 0.6461 0.271 Uiso 0.50 1 calc PR I 6 H43E H 0.3945 0.4726 0.5877 0.271 Uiso 0.50 1 calc PR I 6 H43F H 0.2930 0.4614 0.6017 0.271 Uiso 0.50 1 calc PR I 6 C44A C 0.3899(11) 0.5218(5) 0.6946(6) 0.137(5) Uiso 0.50 1 d P I 6 H44D H 0.3824 0.4936 0.7126 0.205 Uiso 0.50 1 calc PR I 6 H44E H 0.3612 0.5452 0.7139 0.205 Uiso 0.50 1 calc PR I 6 H44F H 0.4556 0.5281 0.6947 0.205 Uiso 0.50 1 calc PR I 6 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 B1 0.039(2) 0.077(3) 0.058(2) -0.003(2) 0.0101(18) -0.005(2) Cr1 0.0470(3) 0.0499(3) 0.0500(3) -0.0023(2) 0.0078(2) 0.0022(3) Cr2 0.0479(3) 0.0472(3) 0.0513(3) 0.0010(2) 0.0042(2) 0.0034(3) P1 0.0704(7) 0.0698(7) 0.0760(7) 0.0017(5) -0.0106(5) 0.0072(6) P2 0.0723(7) 0.0727(7) 0.0867(7) 0.0096(6) 0.0344(6) 0.0074(6) P3 0.0759(8) 0.0798(8) 0.0725(7) -0.0179(6) -0.0131(5) 0.0145(6) P4 0.0790(8) 0.0770(8) 0.0829(7) -0.0071(6) 0.0289(6) -0.0212(6) P5 0.0872(8) 0.0787(8) 0.0603(6) 0.0114(5) 0.0168(5) 0.0161(6) P6 0.0598(7) 0.0588(7) 0.0925(8) 0.0005(5) 0.0046(5) -0.0060(5) P7 0.1168(10) 0.0908(9) 0.0591(6) 0.0137(6) 0.0096(6) 0.0321(8) P8 0.0524(6) 0.0783(8) 0.0959(8) -0.0073(6) 0.0033(5) -0.0004(6) Si1 0.1518(14) 0.0807(10) 0.0901(9) -0.0145(7) 0.0212(9) 0.0466(9) Si2 0.0918(10) 0.0639(8) 0.1472(13) -0.0211(8) 0.0036(9) 0.0259(7) N1 0.0359(15) 0.0479(17) 0.0459(14) 0.0002(12) 0.0068(11) -0.0001(13) N2 0.0353(15) 0.0503(17) 0.0430(14) 0.0050(12) 0.0026(11) -0.0011(13) C1 0.057(2) 0.057(2) 0.058(2) -0.0025(17) 0.0120(17) 0.0031(18) C2 0.083(3) 0.068(3) 0.063(2) -0.001(2) 0.013(2) 0.007(2) C3 0.060(2) 0.058(2) 0.058(2) 0.0057(18) 0.0040(17) 0.0074(19) C4 0.068(3) 0.060(3) 0.083(3) -0.007(2) 0.009(2) 0.005(2) C5 0.110(5) 0.139(5) 0.181(7) 0.012(5) -0.052(5) -0.055(4) C6 0.237(10) 0.391(15) 0.138(6) -0.004(8) -0.003(7) -0.248(11) C7 0.059(3) 0.173(6) 0.165(6) 0.039(5) -0.024(4) -0.019(3) C8 0.056(3) 0.153(6) 0.202(7) 0.046(5) 0.039(4) 0.013(3) C9 0.116(4) 0.098(4) 0.128(4) 0.024(3) -0.040(3) 0.019(3) C10 0.155(5) 0.123(5) 0.086(3) -0.020(3) -0.025(3) -0.012(4) C11 0.159(5) 0.124(5) 0.122(4) -0.012(4) 0.085(4) -0.010(4) C12 0.123(4) 0.076(3) 0.156(5) 0.019(3) 0.069(4) -0.006(3) C13 0.150(5) 0.200(7) 0.076(3) -0.053(4) -0.025(3) 0.030(5) C14 0.128(5) 0.128(5) 0.133(5) -0.015(4) -0.043(4) 0.048(4) C15 0.132(5) 0.132(5) 0.130(4) 0.004(4) 0.085(4) 0.003(4) C16 0.190(7) 0.078(4) 0.199(7) 0.048(4) 0.106(6) 0.012(4) C17 0.118(5) 0.307(11) 0.083(4) 0.010(5) -0.022(4) -0.027(6) C18 0.133(5) 0.217(8) 0.101(4) 0.000(5) -0.026(4) -0.042(5) C19 0.092(4) 0.354(12) 0.085(4) 0.047(6) -0.013(3) 0.055(6) C20 0.092(4) 0.205(7) 0.139(5) 0.057(5) -0.036(4) -0.007(4) C21 0.112(4) 0.128(4) 0.076(3) -0.007(3) 0.017(3) 0.011(3) C22 0.296(10) 0.101(4) 0.096(4) 0.044(3) 0.042(5) 0.059(5) C23 0.093(4) 0.088(4) 0.243(8) -0.034(4) 0.005(4) -0.028(3) C24 0.098(4) 0.184(7) 0.189(7) -0.040(5) 0.056(4) -0.018(4) C25 0.364(12) 0.073(4) 0.099(4) 0.029(3) 0.030(6) 0.034(5) C26 0.171(6) 0.146(5) 0.076(3) 0.010(3) 0.048(3) 0.040(4) C27 0.067(3) 0.126(5) 0.244(8) -0.044(5) 0.044(4) 0.002(3) C28 0.103(5) 0.093(5) 0.386(13) 0.084(6) -0.011(6) -0.029(4) C29 0.107(5) 0.143(6) 0.196(7) -0.044(5) 0.027(5) 0.032(4) C30 0.218(9) 0.099(5) 0.266(10) 0.048(6) 0.091(8) 0.077(6) C31 0.178(7) 0.108(5) 0.265(10) -0.083(6) -0.051(7) 0.042(5) C32 0.308(12) 0.109(5) 0.108(5) -0.035(4) 0.010(6) 0.052(7) C35 0.112(5) 0.186(8) 0.235(9) -0.068(7) -0.030(6) 0.026(5) C36 0.219(10) 0.338(15) 0.248(11) 0.116(11) 0.120(9) 0.064(9) C37 0.309(15) 0.203(10) 0.332(16) 0.082(10) 0.043(12) 0.098(10) C38 0.263(12) 0.111(6) 0.440(19) 0.073(8) 0.180(13) 0.023(7) C39 0.324(13) 0.151(7) 0.272(11) -0.129(7) -0.069(9) 0.089(8) C40 0.303(13) 0.120(6) 0.261(11) -0.037(7) -0.101(10) 0.063(7) C45 0.395(15) 0.167(7) 0.088(5) -0.008(5) 0.025(6) 0.041(8) C46 0.283(14) 0.256(13) 0.230(12) -0.090(9) -0.040(11) -0.039(11) C47 0.043(2) 0.075(3) 0.063(2) 0.0050(19) 0.0006(17) -0.0064(19) C48 0.049(2) 0.079(3) 0.070(2) -0.006(2) 0.0106(18) -0.0162(19) C49 0.059(3) 0.090(3) 0.077(3) -0.016(2) 0.007(2) -0.005(2) C50 0.079(3) 0.076(3) 0.093(3) -0.015(3) -0.016(3) -0.006(3) C51 0.082(3) 0.070(3) 0.094(3) 0.012(3) -0.019(3) -0.016(2) C52 0.063(3) 0.081(3) 0.071(3) 0.009(2) -0.0012(19) -0.017(2) C53 0.092(5) 0.151(7) 0.091(4) -0.042(5) 0.023(4) -0.019(5) C54 0.153(8) 0.092(5) 0.117(6) 0.018(5) -0.022(6) -0.024(5) C55 0.050(2) 0.066(2) 0.0522(19) -0.0002(18) 0.0113(16) -0.0054(18) C56 0.043(2) 0.084(3) 0.0526(19) 0.0011(18) 0.0091(16) -0.0026(19) C57 0.046(2) 0.101(3) 0.058(2) -0.013(2) 0.0081(17) -0.004(2) C58 0.065(3) 0.094(3) 0.066(2) -0.010(2) 0.000(2) 0.013(2) C59 0.074(3) 0.075(3) 0.063(2) 0.000(2) 0.006(2) 0.004(2) C60 0.052(2) 0.071(3) 0.069(2) -0.002(2) 0.0075(18) -0.005(2) C61 0.053(3) 0.148(6) 0.079(3) -0.006(4) 0.010(3) -0.002(3) C62 0.147(6) 0.087(4) 0.083(4) 0.009(3) 0.009(4) 0.012(5) C63 0.041(2) 0.079(3) 0.054(2) 0.0088(18) 0.0069(16) -0.0046(18) C64 0.043(2) 0.088(3) 0.064(2) -0.004(2) 0.0086(17) -0.0064(19) C65 0.053(2) 0.092(3) 0.064(2) -0.003(2) 0.0120(19) 0.002(2) C66 0.050(2) 0.130(4) 0.062(2) 0.004(2) 0.0138(19) 0.001(2) C67 0.041(2) 0.158(5) 0.068(3) 0.014(3) 0.0069(19) -0.001(3) C68 0.056(3) 0.128(4) 0.057(2) 0.015(2) 0.0119(19) -0.002(2) C69 0.060(3) 0.165(6) 0.074(3) -0.020(4) 0.014(3) 0.011(4) C71 0.044(2) 0.078(3) 0.0497(19) 0.0029(18) 0.0161(16) -0.0052(18) C72 0.038(2) 0.084(3) 0.062(2) -0.006(2) 0.0059(16) -0.0066(19) C73 0.055(2) 0.076(3) 0.070(2) 0.013(2) 0.0066(19) -0.005(2) C74 0.065(3) 0.069(3) 0.076(3) 0.001(2) 0.010(2) -0.006(2) C75 0.060(2) 0.076(3) 0.067(2) -0.009(2) 0.0029(19) -0.007(2) C76 0.056(2) 0.077(3) 0.051(2) -0.0021(19) 0.0010(17) -0.003(2) C77 0.077(4) 0.095(4) 0.093(4) 0.014(3) -0.017(3) -0.003(3) C78 0.135(7) 0.090(5) 0.094(5) -0.020(3) -0.006(4) -0.014(4) C79 0.058(4) 0.302(13) 0.078(4) 0.010(7) 0.013(3) 0.017(6) F1 0.124(3) 0.257(5) 0.0668(17) -0.019(2) -0.0054(17) 0.040(3) F2 0.099(2) 0.291(5) 0.0754(17) -0.044(2) 0.0242(17) -0.022(3) F3 0.141(7) 0.152(11) 0.094(5) -0.012(5) -0.040(5) -0.072(8) F3A 0.40(2) 0.118(8) 0.136(11) -0.063(8) -0.068(10) 0.051(11) F4 0.133(12) 0.275(18) 0.46(4) 0.15(2) -0.145(18) -0.130(13) F5 0.063(8) 0.31(3) 0.24(2) -0.062(18) 0.002(10) 0.051(12) F6 0.114(9) 0.40(4) 0.101(11) 0.059(16) -0.050(8) 0.045(13) F4A 0.040(6) 0.50(4) 0.085(5) 0.015(11) 0.010(4) -0.076(13) F5A 0.171(13) 0.33(2) 0.180(15) -0.028(15) -0.054(10) 0.131(15) F6A 0.040(5) 0.38(3) 0.153(16) -0.118(18) -0.011(6) -0.007(9) F7 0.191(19) 0.087(8) 0.179(16) 0.070(8) -0.086(12) -0.039(10) F8 0.092(7) 0.143(7) 0.062(4) 0.029(4) -0.012(4) 0.000(4) F9 0.055(7) 0.28(2) 0.136(7) 0.009(11) -0.008(6) 0.064(10) F7A 0.30(2) 0.212(17) 0.142(10) 0.002(9) -0.064(12) 0.151(17) F8A 0.121(10) 0.47(4) 0.105(9) 0.161(18) 0.049(9) 0.085(19) F9A 0.18(2) 0.180(12) 0.23(2) 0.108(12) -0.140(17) -0.083(12) F10 0.228(19) 0.178(18) 0.43(3) -0.20(2) -0.085(17) 0.028(13) F11 0.21(2) 0.31(3) 0.205(17) -0.141(17) 0.086(14) -0.19(2) F12 0.21(2) 0.133(9) 0.111(10) -0.002(6) -0.103(14) -0.024(11) F10A 0.189(16) 0.152(13) 0.082(10) -0.054(9) -0.020(8) -0.006(11) F11A 0.217(16) 0.054(6) 0.148(8) 0.015(6) -0.085(10) -0.041(7) F12A 0.079(7) 0.167(11) 0.171(14) -0.043(8) -0.038(9) -0.035(7) F13 0.126(13) 0.36(3) 0.091(7) 0.015(11) 0.045(8) -0.104(16) F14 0.071(9) 0.211(18) 0.28(2) -0.144(16) 0.053(10) -0.064(9) F15 0.043(4) 0.207(11) 0.327(19) 0.122(12) 0.065(8) 0.044(6) F13A 0.060(5) 0.219(15) 0.250(19) 0.105(16) -0.034(9) -0.066(7) F14A 0.035(4) 0.225(13) 0.083(4) -0.018(6) -0.006(3) 0.001(5) F15A 0.109(11) 0.28(2) 0.138(15) -0.100(16) 0.076(11) -0.043(11) F16 0.271(6) 0.122(3) 0.120(3) 0.043(2) 0.056(3) -0.002(3) F17 0.119(5) 0.057(6) 0.186(12) 0.045(7) 0.002(6) -0.029(5) F18 0.121(9) 0.099(6) 0.167(9) 0.029(6) -0.009(7) 0.063(7) F17A 0.43(4) 0.091(9) 0.151(11) -0.021(8) 0.009(19) -0.016(15) F18A 0.133(9) 0.248(17) 0.31(2) 0.203(16) -0.052(11) -0.009(10) F19 0.27(2) 0.188(14) 0.184(14) -0.053(11) 0.097(13) 0.071(16) F20 0.153(14) 0.222(17) 0.095(7) -0.051(9) 0.050(8) -0.098(13) F21 0.105(7) 0.46(4) 0.076(10) 0.053(17) 0.001(6) 0.00(2) F19A 0.20(2) 0.181(15) 0.095(8) -0.058(10) 0.044(11) -0.060(13) F20A 0.109(8) 0.28(2) 0.137(9) 0.016(13) 0.070(6) -0.007(12) F21A 0.23(2) 0.167(10) 0.075(7) 0.006(6) 0.053(9) -0.039(11) F22 0.21(3) 0.130(15) 0.148(8) -0.004(8) -0.057(10) -0.092(16) F23 0.205(14) 0.119(14) 0.25(3) 0.058(18) -0.066(18) -0.044(9) F24 0.203(17) 0.211(19) 0.207(14) -0.027(16) 0.063(15) -0.146(16) F22A 0.092(8) 0.124(15) 0.44(5) 0.081(19) -0.085(18) -0.054(10) F23A 0.202(14) 0.075(6) 0.244(16) -0.038(8) 0.009(11) -0.023(6) F24A 0.37(4) 0.130(15) 0.131(10) 0.054(11) -0.022(13) -0.135(19) _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 B1 C71 1.618(6) . ? B1 C63 1.646(5) . ? B1 C47 1.650(6) . ? B1 C55 1.656(5) . ? Cr1 N1 1.891(3) . ? Cr1 C1 2.047(4) . ? Cr1 P4 2.3453(12) . ? Cr1 P1 2.3534(11) . ? Cr1 P3 2.3541(11) . ? Cr1 P2 2.3679(12) . ? Cr2 N2 1.882(3) . ? Cr2 C3 2.037(4) . ? Cr2 P6 2.3766(12) . ? Cr2 P7 2.3782(12) . ? Cr2 P8 2.3848(12) . ? Cr2 P5 2.4040(11) . ? P1 C10 1.815(5) . ? P1 C9 1.842(5) . ? P1 C7 1.852(6) . ? P2 C11 1.800(5) . ? P2 C12 1.820(5) . ? P2 C8 1.853(6) . ? P3 C14 1.803(5) . ? P3 C13 1.815(5) . ? P3 C5 1.853(6) . ? P4 C16 1.816(5) . ? P4 C6 1.822(7) . ? P4 C15 1.827(5) . ? P5 C25 1.786(5) . ? P5 C26 1.786(5) . ? P5 C17 1.834(7) . ? P6 C28 1.783(5) . ? P6 C27 1.782(5) . ? P6 C18 1.817(6) . ? P7 C22 1.754(5) . ? P7 C21 1.787(5) . ? P7 C19 1.901(7) . ? P8 C23 1.775(5) . ? P8 C20 1.823(6) . ? P8 C24 1.824(6) . ? Si1 C34A 1.720(13) . ? Si1 C33 1.750(11) . ? Si1 C2 1.813(4) . ? Si1 C32 1.854(8) . ? Si1 C33A 2.037(13) . ? Si1 C34 2.277(12) . ? Si2 C4 1.835(4) . ? Si2 C31 1.841(7) . ? Si2 C30 1.892(8) . ? Si2 C29 1.907(7) . ? N1 N2 1.164(3) . ? C1 C2 1.226(5) . ? C3 C4 1.218(5) . ? C5 C6 1.363(9) . ? C7 C8 1.442(9) . ? C17 C18 1.475(9) . ? C19 C20 1.471(8) . ? C29 C35 1.441(9) . ? C29 C36 1.581(11) . ? C30 C37 1.486(10) . ? C30 C38 1.565(11) . ? C31 C40 1.512(11) . ? C31 C39 1.539(8) . ? C32 C45 1.530(10) . ? C32 C46 1.608(13) . ? C47 C48 1.387(5) . ? C47 C52 1.386(5) . ? C48 C49 1.396(5) . ? C49 C50 1.362(6) . ? C49 C53 1.478(7) . ? C50 C51 1.387(6) . ? C51 C52 1.381(6) . ? C51 C54 1.520(8) . ? C53 F21 1.235(15) . ? C53 F19A 1.249(13) . ? C53 F20A 1.274(15) . ? C53 F21A 1.291(15) . ? C53 F20 1.301(16) . ? C53 F19 1.412(15) . ? C54 F23 1.20(2) . ? C54 F22A 1.201(17) . ? C54 F22 1.216(15) . ? C54 F24A 1.32(2) . ? C54 F24 1.37(2) . ? C54 F23A 1.437(15) . ? C55 C60 1.375(5) . ? C55 C56 1.388(5) . ? C56 C57 1.374(5) . ? C57 C58 1.375(6) . ? C57 C61 1.507(6) . ? C58 C59 1.383(6) . ? C59 C60 1.389(5) . ? C59 C62 1.522(7) . ? C61 F15A 1.202(14) . ? C61 F14 1.227(12) . ? C61 F14A 1.264(9) . ? C61 F13 1.277(18) . ? C61 F15 1.348(10) . ? C61 F13A 1.350(16) . ? C62 F17A 1.22(2) . ? C62 F18 1.214(11) . ? C62 F16 1.322(7) . ? C62 F17 1.338(16) . ? C62 F18A 1.397(15) . ? C63 C64 1.368(5) . ? C63 C68 1.383(5) . ? C64 C65 1.387(5) . ? C65 C66 1.359(5) . ? C65 C69 1.491(6) . ? C66 C67 1.363(6) . ? C67 C68 1.407(5) . ? C67 C79 1.517(7) . ? C69 F3 1.235(12) . ? C69 F1 1.310(6) . ? C69 F2 1.314(5) . ? C69 F3A 1.371(18) . ? C71 C76 1.388(5) . ? C71 C72 1.417(5) . ? C72 C73 1.370(5) . ? C73 C74 1.368(5) . ? C73 C77 1.489(6) . ? C74 C75 1.374(5) . ? C75 C76 1.377(5) . ? C75 C78 1.507(6) . ? C77 F8A 1.220(12) . ? C77 F9 1.231(13) . ? C77 F7 1.252(11) . ? C77 F9A 1.258(17) . ? C77 F8 1.364(11) . ? C77 F7A 1.385(17) . ? C78 F11A 1.281(13) . ? C78 F10A 1.27(2) . ? C78 F12 1.30(2) . ? C78 F11 1.302(19) . ? C78 F12A 1.314(17) . ? C78 F10 1.34(2) . ? C79 F6 1.170(15) . ? C79 F6A 1.201(17) . ? C79 F5 1.22(2) . ? C79 F4A 1.273(17) . ? C79 F4 1.40(2) . ? C79 F5A 1.57(2) . ? C33 C44 1.524(19) . ? C33 C43 1.529(16) . ? C34 C42 1.430(14) . ? C34 C41 1.730(14) . ? C33A C44A 1.513(18) . ? C33A C43A 1.527(17) . ? C34A C42A 1.36(3) . ? C34A C41A 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C71 B1 C63 104.4(3) . . ? C71 B1 C47 114.2(3) . . ? C63 B1 C47 111.9(3) . . ? C71 B1 C55 112.8(3) . . ? C63 B1 C55 111.0(3) . . ? C47 B1 C55 102.8(3) . . ? N1 Cr1 C1 178.25(13) . . ? N1 Cr1 P4 95.23(8) . . ? C1 Cr1 P4 83.08(10) . . ? N1 Cr1 P1 94.18(8) . . ? C1 Cr1 P1 86.42(10) . . ? P4 Cr1 P1 94.96(5) . . ? N1 Cr1 P3 96.49(8) . . ? C1 Cr1 P3 82.88(10) . . ? P4 Cr1 P3 82.68(5) . . ? P1 Cr1 P3 169.24(5) . . ? N1 Cr1 P2 99.07(8) . . ? C1 Cr1 P2 82.64(10) . . ? P4 Cr1 P2 165.63(5) . . ? P1 Cr1 P2 82.56(5) . . ? P3 Cr1 P2 97.12(5) . . ? N2 Cr2 C3 176.38(13) . . ? N2 Cr2 P6 95.90(8) . . ? C3 Cr2 P6 83.19(11) . . ? N2 Cr2 P7 93.81(8) . . ? C3 Cr2 P7 82.83(10) . . ? P6 Cr2 P7 96.24(5) . . ? N2 Cr2 P8 97.51(8) . . ? C3 Cr2 P8 83.49(11) . . ? P6 Cr2 P8 166.55(5) . . ? P7 Cr2 P8 83.95(5) . . ? N2 Cr2 P5 98.78(8) . . ? C3 Cr2 P5 84.62(10) . . ? P6 Cr2 P5 83.65(4) . . ? P7 Cr2 P5 167.36(5) . . ? P8 Cr2 P5 93.23(5) . . ? C10 P1 C9 100.5(3) . . ? C10 P1 C7 102.9(3) . . ? C9 P1 C7 100.8(3) . . ? C10 P1 Cr1 119.8(2) . . ? C9 P1 Cr1 120.95(17) . . ? C7 P1 Cr1 109.0(2) . . ? C11 P2 C12 99.5(3) . . ? C11 P2 C8 99.5(3) . . ? C12 P2 C8 102.1(3) . . ? C11 P2 Cr1 123.76(19) . . ? C12 P2 Cr1 120.92(17) . . ? C8 P2 Cr1 107.3(2) . . ? C14 P3 C13 99.7(3) . . ? C14 P3 C5 101.5(3) . . ? C13 P3 C5 99.1(4) . . ? C14 P3 Cr1 119.68(19) . . ? C13 P3 Cr1 124.0(2) . . ? C5 P3 Cr1 109.0(2) . . ? C16 P4 C6 99.5(5) . . ? C16 P4 C15 99.2(3) . . ? C6 P4 C15 102.7(4) . . ? C16 P4 Cr1 121.9(2) . . ? C6 P4 Cr1 110.3(3) . . ? C15 P4 Cr1 119.93(19) . . ? C25 P5 C26 103.1(3) . . ? C25 P5 C17 97.5(4) . . ? C26 P5 C17 97.5(3) . . ? C25 P5 Cr2 124.0(2) . . ? C26 P5 Cr2 122.10(18) . . ? C17 P5 Cr2 106.6(2) . . ? C28 P6 C27 101.9(3) . . ? C28 P6 C18 100.4(4) . . ? C27 P6 C18 99.0(4) . . ? C28 P6 Cr2 121.5(2) . . ? C27 P6 Cr2 121.3(2) . . ? C18 P6 Cr2 108.7(2) . . ? C22 P7 C21 103.5(3) . . ? C22 P7 C19 99.2(4) . . ? C21 P7 C19 98.6(3) . . ? C22 P7 Cr2 123.9(2) . . ? C21 P7 Cr2 120.24(17) . . ? C19 P7 Cr2 106.6(2) . . ? C23 P8 C20 102.3(3) . . ? C23 P8 C24 99.6(3) . . ? C20 P8 C24 98.4(4) . . ? C23 P8 Cr2 121.6(2) . . ? C20 P8 Cr2 109.2(2) . . ? C24 P8 Cr2 121.8(2) . . ? C34A Si1 C33 81.9(6) . . ? C34A Si1 C2 113.4(5) . . ? C33 Si1 C2 113.4(4) . . ? C34A Si1 C32 113.5(6) . . ? C33 Si1 C32 119.7(5) . . ? C2 Si1 C32 111.8(3) . . ? C34A Si1 C33A 114.7(6) . . ? C33 Si1 C33A 34.0(4) . . ? C2 Si1 C33A 105.2(4) . . ? C32 Si1 C33A 96.8(5) . . ? C34A Si1 C34 27.0(5) . . ? C33 Si1 C34 108.3(5) . . ? C2 Si1 C34 97.1(3) . . ? C32 Si1 C34 103.4(5) . . ? C33A Si1 C34 141.7(5) . . ? C4 Si2 C31 109.6(3) . . ? C4 Si2 C30 107.9(3) . . ? C31 Si2 C30 108.1(5) . . ? C4 Si2 C29 109.8(3) . . ? C31 Si2 C29 116.4(4) . . ? C30 Si2 C29 104.6(4) . . ? N2 N1 Cr1 177.6(2) . . ? N1 N2 Cr2 177.3(2) . . ? C2 C1 Cr1 179.3(3) . . ? C1 C2 Si1 178.7(4) . . ? C4 C3 Cr2 178.4(3) . . ? C3 C4 Si2 178.5(4) . . ? C6 C5 P3 117.1(5) . . ? C5 C6 P4 118.6(5) . . ? C8 C7 P1 110.1(4) . . ? C7 C8 P2 111.7(4) . . ? C18 C17 P5 116.1(5) . . ? C17 C18 P6 112.2(5) . . ? C20 C19 P7 115.0(4) . . ? C19 C20 P8 111.6(5) . . ? C35 C29 C36 114.8(8) . . ? C35 C29 Si2 114.5(6) . . ? C36 C29 Si2 108.3(6) . . ? C37 C30 C38 119.5(8) . . ? C37 C30 Si2 114.0(7) . . ? C38 C30 Si2 111.8(7) . . ? C40 C31 C39 106.9(8) . . ? C40 C31 Si2 117.6(6) . . ? C39 C31 Si2 115.0(6) . . ? C45 C32 C46 111.7(8) . . ? C45 C32 Si1 110.0(7) . . ? C46 C32 Si1 109.8(6) . . ? C48 C47 C52 114.4(4) . . ? C48 C47 B1 121.8(3) . . ? C52 C47 B1 123.5(3) . . ? C47 C48 C49 123.3(4) . . ? C50 C49 C48 120.5(4) . . ? C50 C49 C53 119.7(5) . . ? C48 C49 C53 119.9(5) . . ? C49 C50 C51 117.8(4) . . ? C52 C51 C50 120.7(4) . . ? C52 C51 C54 119.8(6) . . ? C50 C51 C54 119.5(5) . . ? C51 C52 C47 123.2(4) . . ? F21 C53 F19A 49.3(13) . . ? F21 C53 F20A 136.6(11) . . ? F19A C53 F20A 108.0(13) . . ? F21 C53 F21A 57.2(15) . . ? F19A C53 F21A 101.1(13) . . ? F20A C53 F21A 105.6(13) . . ? F21 C53 F20 106.6(17) . . ? F19A C53 F20 123.6(10) . . ? F20A C53 F20 50.3(9) . . ? F21A C53 F20 56.4(11) . . ? F21 C53 F19 100.8(15) . . ? F19A C53 F19 52.0(9) . . ? F20A C53 F19 64.3(11) . . ? F21A C53 F19 138.3(10) . . ? F20 C53 F19 108.2(13) . . ? F21 C53 C49 113.3(9) . . ? F19A C53 C49 118.2(9) . . ? F20A C53 C49 110.1(8) . . ? F21A C53 C49 112.9(8) . . ? F20 C53 C49 118.2(7) . . ? F19 C53 C49 108.3(10) . . ? F23 C54 F22A 132.1(15) . . ? F23 C54 F22 111.7(16) . . ? F22A C54 F22 46.8(17) . . ? F23 C54 F24A 37(2) . . ? F22A C54 F24A 118(2) . . ? F22 C54 F24A 132.1(13) . . ? F23 C54 F24 99.9(18) . . ? F22A C54 F24 58.1(17) . . ? F22 C54 F24 101.1(16) . . ? F24A C54 F24 67.0(16) . . ? F23 C54 F23A 62.0(16) . . ? F22A C54 F23A 109.1(17) . . ? F22 C54 F23A 63.2(10) . . ? F24A C54 F23A 98.5(18) . . ? F24 C54 F23A 143.8(10) . . ? F23 C54 C51 113.9(12) . . ? F22A C54 C51 113.6(10) . . ? F22 C54 C51 118.1(10) . . ? F24A C54 C51 109.3(12) . . ? F24 C54 C51 109.6(10) . . ? F23A C54 C51 106.4(9) . . ? C60 C55 C56 115.4(3) . . ? C60 C55 B1 120.2(3) . . ? C56 C55 B1 124.0(3) . . ? C57 C56 C55 122.6(4) . . ? C56 C57 C58 120.7(4) . . ? C56 C57 C61 120.6(4) . . ? C58 C57 C61 118.7(4) . . ? C57 C58 C59 118.6(4) . . ? C58 C59 C60 119.2(4) . . ? C58 C59 C62 120.5(5) . . ? C60 C59 C62 120.3(5) . . ? C55 C60 C59 123.5(4) . . ? F15A C61 F14 127.3(13) . . ? F15A C61 F14A 111.8(10) . . ? F14 C61 F14A 56.2(11) . . ? F15A C61 F13 40.6(15) . . ? F14 C61 F13 107.5(17) . . ? F14A C61 F13 135.5(10) . . ? F15A C61 F15 66.1(11) . . ? F14 C61 F15 109.7(11) . . ? F14A C61 F15 56.3(9) . . ? F13 C61 F15 106.1(13) . . ? F15A C61 F13A 99.0(15) . . ? F14 C61 F13A 46.0(11) . . ? F14A C61 F13A 99.1(10) . . ? F13 C61 F13A 64.7(12) . . ? F15 C61 F13A 136.9(7) . . ? F15A C61 C57 117.5(10) . . ? F14 C61 C57 112.8(6) . . ? F14A C61 C57 114.9(6) . . ? F13 C61 C57 109.6(10) . . ? F15 C61 C57 110.9(6) . . ? F13A C61 C57 111.7(7) . . ? F17A C62 F18 80.0(13) . . ? F17A C62 F16 115.4(14) . . ? F18 C62 F16 118.6(9) . . ? F17A C62 F17 27.8(16) . . ? F18 C62 F17 106.7(11) . . ? F16 C62 F17 95.5(10) . . ? F17A C62 F18A 111.2(14) . . ? F18 C62 F18A 34.5(10) . . ? F16 C62 F18A 91.2(10) . . ? F17 C62 F18A 134.0(10) . . ? F17A C62 C59 117.1(10) . . ? F18 C62 C59 115.1(9) . . ? F16 C62 C59 108.6(5) . . ? F17 C62 C59 110.2(8) . . ? F18A C62 C59 110.4(9) . . ? C64 C63 C68 114.9(3) . . ? C64 C63 B1 123.3(3) . . ? C68 C63 B1 121.3(3) . . ? C63 C64 C65 123.7(3) . . ? C66 C65 C64 120.4(4) . . ? C66 C65 C69 119.5(4) . . ? C64 C65 C69 120.1(4) . . ? C65 C66 C67 118.4(4) . . ? C66 C67 C68 120.4(4) . . ? C66 C67 C79 120.2(5) . . ? C68 C67 C79 119.3(5) . . ? C63 C68 C67 122.2(4) . . ? F3 C69 F1 92.2(8) . . ? F3 C69 F2 109.3(9) . . ? F1 C69 F2 105.0(5) . . ? F3 C69 F3A 25.6(10) . . ? F1 C69 F3A 117.6(9) . . ? F2 C69 F3A 102.8(10) . . ? F3 C69 C65 120.7(7) . . ? F1 C69 C65 113.7(5) . . ? F2 C69 C65 113.2(4) . . ? F3A C69 C65 104.3(8) . . ? C76 C71 C72 114.4(3) . . ? C76 C71 B1 121.8(3) . . ? C72 C71 B1 123.2(3) . . ? C73 C72 C71 123.1(3) . . ? C74 C73 C72 120.3(4) . . ? C74 C73 C77 120.1(4) . . ? C72 C73 C77 119.5(4) . . ? C73 C74 C75 118.4(4) . . ? C74 C75 C76 121.3(4) . . ? C74 C75 C78 120.2(5) . . ? C76 C75 C78 118.4(4) . . ? C75 C76 C71 122.4(3) . . ? F8A C77 F9 130.3(11) . . ? F8A C77 F7 51.4(12) . . ? F9 C77 F7 109.4(13) . . ? F8A C77 F9A 119.3(14) . . ? F9 C77 F9A 29.2(14) . . ? F7 C77 F9A 127.5(10) . . ? F8A C77 F8 55.0(15) . . ? F9 C77 F8 101.5(11) . . ? F7 C77 F8 103.4(11) . . ? F9A C77 F8 75.0(13) . . ? F8A C77 F7A 98.0(14) . . ? F9 C77 F7A 70.0(11) . . ? F7 C77 F7A 48.1(10) . . ? F9A C77 F7A 97.9(14) . . ? F8 C77 F7A 137.8(8) . . ? F8A C77 C73 114.6(7) . . ? F9 C77 C73 114.7(9) . . ? F7 C77 C73 115.9(7) . . ? F9A C77 C73 113.3(9) . . ? F8 C77 C73 110.2(6) . . ? F7A C77 C73 110.7(9) . . ? F11A C78 F10A 105.0(14) . . ? F11A C78 F12 117.8(13) . . ? F10A C78 F12 29.7(14) . . ? F11A C78 F11 76.8(14) . . ? F10A C78 F11 132.2(14) . . ? F12 C78 F11 106.4(16) . . ? F11A C78 F12A 112.3(13) . . ? F10A C78 F12A 105.5(12) . . ? F12 C78 F12A 75.8(13) . . ? F11 C78 F12A 39.0(15) . . ? F11A C78 F10 32.4(17) . . ? F10A C78 F10 78.1(18) . . ? F12 C78 F10 100.6(17) . . ? F11 C78 F10 108.2(17) . . ? F12A C78 F10 138.1(12) . . ? F11A C78 C75 115.8(7) . . ? F10A C78 C75 107.6(11) . . ? F12 C78 C75 117.9(12) . . ? F11 C78 C75 114.3(10) . . ? F12A C78 C75 109.9(9) . . ? F10 C78 C75 108.4(10) . . ? F6 C79 F6A 40.7(18) . . ? F6 C79 F5 106.4(18) . . ? F6A C79 F5 130.3(12) . . ? F6 C79 F4A 131.5(11) . . ? F6A C79 F4A 119.0(16) . . ? F5 C79 F4A 46.7(14) . . ? F6 C79 F4 101.8(19) . . ? F6A C79 F4 63.8(17) . . ? F5 C79 F4 107.9(17) . . ? F4A C79 F4 65.0(14) . . ? F6 C79 C67 117.5(10) . . ? F6A C79 C67 116.0(9) . . ? F5 C79 C67 112.7(12) . . ? F4A C79 C67 110.7(8) . . ? F4 C79 C67 109.8(10) . . ? F6 C79 F5A 62.5(17) . . ? F6A C79 F5A 102.9(16) . . ? F5 C79 F5A 56.8(14) . . ? F4A C79 F5A 103.2(18) . . ? F4 C79 F5A 148.0(10) . . ? C67 C79 F5A 102.2(10) . . ? C44 C33 C43 111.1(11) . . ? C44 C33 Si1 113.2(10) . . ? C43 C33 Si1 116.8(9) . . ? C42 C34 C41 113.5(11) . . ? C42 C34 Si1 111.9(10) . . ? C41 C34 Si1 92.8(7) . . ? C44A C33A C43A 108.4(11) . . ? C44A C33A Si1 106.9(9) . . ? C43A C33A Si1 113.5(10) . . ? C42A C34A C41A 109.7(19) . . ? C42A C34A Si1 124.2(19) . . ? C41A C34A Si1 126.0(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.680 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.088 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_common 'compound 4 in text' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122.50 H158 B2 Cr2 F48 N2 O3.50 P8 Si2' _chemical_formula_weight 3056.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'Cr' 'Cr' 0.3209 0.6236 '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 14.2386(5) _cell_length_b 17.1753(6) _cell_length_c 31.8445(11) _cell_angle_alpha 88.101(2) _cell_angle_beta 86.562(2) _cell_angle_gamma 69.587(2) _cell_volume 7284.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3146 _exptl_absorpt_coefficient_mu 0.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8897 _exptl_absorpt_correction_T_max 0.9716 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; One of the methyl carbon atoms on a C2SiiPr3 ligand was disordered over two sitesand modeled with a 62:38 occupancy ratio. Two of the tetrahydrofuran solvent molecules were refined anisotropically, and hydrogen atoms were added to ideal positions as described above. Three other tetrahydrofuran residues were found in the difference map; all were modeled at 50% occupancy. Two of these resided on inversion centers, and hydrogen atoms were not added to the disordered solvent molecules. Attempts to remedy A level alerts regarding unusual thermal parameters for F and C atoms were met with an increase in R1 (from 9.3 to 10.1) and were therefore abandoned. Suspect bond distances in the heavily disordered THF molecules could not be fixed and were also left alone. The SQUEEZE routine was used to try and cut out the problematic THF, but this too did not result in a structural improvement. ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94905 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 0.64 _diffrn_reflns_theta_max 24.11 _reflns_number_total 23162 _reflns_number_gt 16139 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1370P)^2^+49.0856P] 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 23162 _refine_ls_number_parameters 1705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.2768 _refine_ls_wR_factor_gt 0.2470 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.177 _refine_ls_shift/su_mean 0.002 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 Cr1 Cr -0.02394(7) 0.14669(6) 0.80357(3) 0.0098(2) Uani 1 1 d . . . Cr2 Cr 0.05321(7) 0.34005(6) 0.70090(3) 0.0112(2) Uani 1 1 d . . . Si1 Si -0.10434(14) -0.05686(11) 0.90772(5) 0.0166(4) Uani 1 1 d . . . Si2 Si 0.13557(16) 0.54102(12) 0.59563(6) 0.0268(5) Uani 1 1 d . A . P1 P -0.09175(13) 0.24309(10) 0.86098(5) 0.0182(4) Uani 1 1 d . . . P2 P -0.19633(13) 0.17844(10) 0.78897(6) 0.0191(4) Uani 1 1 d . . . P3 P 0.13991(13) 0.08695(10) 0.83285(5) 0.0167(4) Uani 1 1 d . . . P4 P 0.04404(13) 0.03312(10) 0.75526(5) 0.0204(4) Uani 1 1 d . . . P8 P 0.20939(13) 0.24245(10) 0.67040(5) 0.0198(4) Uani 1 1 d . . . P9 P -0.05641(13) 0.32722(11) 0.64756(6) 0.0216(4) Uani 1 1 d . . . P10 P -0.09039(13) 0.45964(10) 0.72146(6) 0.0204(4) Uani 1 1 d . . . P12 P 0.16867(13) 0.37494(11) 0.74405(5) 0.0190(4) Uani 1 1 d . . . N1 N 0.0048(4) 0.2216(3) 0.76564(16) 0.0110(11) Uani 1 1 d . . . N2 N 0.0234(4) 0.2671(3) 0.74034(15) 0.0123(11) Uani 1 1 d . . . F1 F -0.0950(8) 0.0924(15) 0.4185(4) 0.362(15) Uani 1 1 d . . . F2 F -0.0401(4) 0.1034(4) 0.3568(2) 0.081(2) Uani 1 1 d . . . F3 F 0.0090(9) -0.0095(7) 0.3895(3) 0.163(5) Uani 1 1 d . . . F4 F 0.0246(5) 0.2330(7) 0.5167(3) 0.151(5) Uani 1 1 d . . . F5 F 0.1707(4) 0.2328(3) 0.51235(15) 0.0587(15) Uani 1 1 d . . . F6 F 0.1446(8) 0.1280(4) 0.53711(17) 0.113(3) Uani 1 1 d . . . F7 F 0.3206(4) -0.2400(4) 0.3573(2) 0.077(2) Uani 1 1 d . . . F8 F 0.4400(4) -0.2384(3) 0.31539(15) 0.0521(13) Uani 1 1 d . . . F9 F 0.4736(6) -0.3202(3) 0.36763(19) 0.079(2) Uani 1 1 d . . . F10 F 0.5934(6) -0.2243(3) 0.4874(2) 0.101(3) Uani 1 1 d . . . F11 F 0.6109(5) -0.1085(4) 0.4811(2) 0.083(2) Uani 1 1 d . . . F12 F 0.4859(5) -0.1143(5) 0.51304(17) 0.091(2) Uani 1 1 d . . . F13 F 0.5877(3) 0.0079(3) 0.23852(14) 0.0410(12) Uani 1 1 d . . . F14 F 0.5013(3) 0.0093(3) 0.18599(13) 0.0509(14) Uani 1 1 d . . . F15 F 0.5287(4) -0.0882(3) 0.23225(16) 0.0496(13) Uani 1 1 d . . . F16 F 0.0906(3) 0.2498(3) 0.26659(14) 0.0463(13) Uani 1 1 d . . . F17 F 0.1887(4) 0.2630(3) 0.21603(17) 0.0549(14) Uani 1 1 d . . . F18 F 0.1195(3) 0.1716(3) 0.21381(15) 0.0448(12) Uani 1 1 d . . . F19 F 0.3494(6) 0.3609(3) 0.44560(18) 0.091(3) Uani 1 1 d . . . F20 F 0.4341(5) 0.3932(3) 0.3954(2) 0.0688(17) Uani 1 1 d . . . F21 F 0.2946(5) 0.3845(3) 0.3855(2) 0.087(2) Uani 1 1 d . . . F22 F 0.7308(4) 0.1569(4) 0.3733(3) 0.093(2) Uani 1 1 d . . . F23 F 0.7041(5) 0.0759(4) 0.3311(2) 0.088(2) Uani 1 1 d . . . F24 F 0.7252(4) 0.0405(4) 0.3950(2) 0.083(2) Uani 1 1 d . . . F25 F 0.7478(4) 0.6148(4) 0.92205(19) 0.0658(17) Uani 1 1 d . . . F26 F 0.7550(5) 0.5515(7) 0.8657(3) 0.131(4) Uani 1 1 d . . . F27 F 0.7297(6) 0.4987(6) 0.9210(5) 0.192(7) Uani 1 1 d . . . F28 F 0.4610(5) 0.8656(3) 0.8921(3) 0.091(2) Uani 1 1 d . . . F29 F 0.3527(4) 0.8488(3) 0.93750(15) 0.0521(14) Uani 1 1 d . . . F30 F 0.3259(5) 0.8556(3) 0.87309(18) 0.076(2) Uani 1 1 d . . . F31 F 0.1978(4) 0.6388(4) 1.01567(15) 0.0593(15) Uani 1 1 d . . . F32 F 0.0437(5) 0.7074(3) 1.00279(16) 0.0725(19) Uani 1 1 d . . . F33 F 0.0886(5) 0.5806(4) 1.02039(15) 0.0632(15) Uani 1 1 d . . . F34 F -0.0904(3) 0.6471(3) 0.87089(16) 0.0428(12) Uani 1 1 d . . . F35 F -0.0312(4) 0.5151(3) 0.8717(2) 0.0587(15) Uani 1 1 d . . . F36 F 0.0132(4) 0.5833(4) 0.82174(16) 0.0617(16) Uani 1 1 d . . . F37 F 0.2076(7) 0.7839(4) 0.7588(3) 0.137(4) Uani 1 1 d . . . F38 F 0.1324(5) 0.7101(5) 0.7433(4) 0.160(5) Uani 1 1 d . . . F39 F 0.2345(6) 0.7351(5) 0.7006(2) 0.128(4) Uani 1 1 d . . . F40 F 0.5512(4) 0.5106(3) 0.68377(14) 0.0500(13) Uani 1 1 d . . . F41 F 0.6253(3) 0.4516(3) 0.73956(14) 0.0382(11) Uani 1 1 d . . . F42 F 0.5242(4) 0.4055(3) 0.71125(16) 0.0514(13) Uani 1 1 d . . . F43 F 0.5279(6) 0.3810(3) 1.00164(16) 0.074(2) Uani 1 1 d . . . F44 F 0.6449(5) 0.2830(5) 0.9738(2) 0.089(2) Uani 1 1 d . . . F45 F 0.5160(7) 0.2610(4) 0.99774(18) 0.094(3) Uani 1 1 d . . . F46 F 0.5169(5) 0.1554(3) 0.85200(18) 0.0655(17) Uani 1 1 d . . . F47 F 0.4987(4) 0.2403(3) 0.80118(16) 0.0463(12) Uani 1 1 d . . . F48 F 0.3692(3) 0.2327(3) 0.83392(17) 0.0467(13) Uani 1 1 d . . . O1 O 0.6285(6) 0.6356(4) 0.7473(2) 0.062(2) Uani 1 1 d . . . O2 O 0.1807(5) 0.2749(4) 0.91480(19) 0.0478(15) Uani 1 1 d . . . C120 C 0.7251(11) 0.1864(9) 0.4918(5) 0.034(4) Uani 0.50 1 d P . . B1 B 0.3431(6) 0.0673(5) 0.3741(2) 0.0197(16) Uani 1 1 d . . . B2 B 0.3686(6) 0.5428(4) 0.8685(2) 0.0185(16) Uani 1 1 d . . . C1 C -0.0556(4) 0.0622(4) 0.84366(19) 0.0135(13) Uani 1 1 d . . . C2 C -0.0759(4) 0.0139(4) 0.86842(19) 0.0142(13) Uani 1 1 d . . . C3 C 0.0854(5) 0.4206(4) 0.6582(2) 0.0161(14) Uani 1 1 d . . . C4 C 0.1056(5) 0.4687(4) 0.6336(2) 0.0221(15) Uani 1 1 d . . . C5 C 0.1972(5) -0.0174(4) 0.8104(2) 0.0240(16) Uani 1 1 d . . . H5A H 0.2702 -0.0386 0.8147 0.029 Uiso 1 1 calc R . . H5B H 0.1674 -0.0558 0.8249 0.029 Uiso 1 1 calc R . . C6 C 0.1795(5) -0.0136(4) 0.7633(2) 0.0257(16) Uani 1 1 d . . . H6A H 0.2060 -0.0703 0.7516 0.031 Uiso 1 1 calc R . . H6B H 0.2154 0.0202 0.7484 0.031 Uiso 1 1 calc R . . C7 C -0.1832(6) 0.3965(5) 0.6644(2) 0.0332(18) Uani 1 1 d . . . H7A H -0.2275 0.4078 0.6404 0.040 Uiso 1 1 calc R . . H7B H -0.2114 0.3692 0.6871 0.040 Uiso 1 1 calc R . . C8 C -0.1786(6) 0.4792(5) 0.6803(2) 0.0301(17) Uani 1 1 d . . . H8A H -0.2461 0.5144 0.6913 0.036 Uiso 1 1 calc R . . H8B H -0.1578 0.5095 0.6567 0.036 Uiso 1 1 calc R . . C9 C 0.3081(5) 0.2796(5) 0.6850(2) 0.0299(17) Uani 1 1 d . . . H9A H 0.3745 0.2365 0.6789 0.036 Uiso 1 1 calc R . . H9B H 0.3048 0.3300 0.6682 0.036 Uiso 1 1 calc R . . C10 C 0.2951(5) 0.2995(5) 0.7314(2) 0.0282(17) Uani 1 1 d . . . H10A H 0.3463 0.3229 0.7389 0.034 Uiso 1 1 calc R . . H10B H 0.3051 0.2479 0.7482 0.034 Uiso 1 1 calc R . . C11 C -0.2691(5) 0.2290(4) 0.8363(2) 0.0252(16) Uani 1 1 d . . . H11A H -0.3401 0.2579 0.8297 0.030 Uiso 1 1 calc R . . H11B H -0.2667 0.1868 0.8585 0.030 Uiso 1 1 calc R . . C12 C -0.2248(5) 0.2921(4) 0.8520(3) 0.0302(17) Uani 1 1 d . . . H12A H -0.2613 0.3167 0.8785 0.036 Uiso 1 1 calc R . . H12B H -0.2342 0.3374 0.8309 0.036 Uiso 1 1 calc R . . C13 C -0.2454(5) 0.0978(4) 0.7787(2) 0.0285(17) Uani 1 1 d . . . H13A H -0.3189 0.1209 0.7799 0.034 Uiso 1 1 calc R . . H13B H -0.2232 0.0534 0.7999 0.034 Uiso 1 1 calc R . . H13C H -0.2208 0.0751 0.7507 0.034 Uiso 1 1 calc R . . C14 C -0.2503(6) 0.2522(4) 0.7476(2) 0.0312(18) Uani 1 1 d . . . H14A H -0.2183 0.2297 0.7204 0.037 Uiso 1 1 calc R . . H14B H -0.2395 0.3044 0.7524 0.037 Uiso 1 1 calc R . . H14C H -0.3225 0.2626 0.7475 0.037 Uiso 1 1 calc R . . C15 C -0.0910(6) 0.2031(5) 0.9148(2) 0.0322(18) Uani 1 1 d . . . H15A H -0.0233 0.1876 0.9251 0.039 Uiso 1 1 calc R . . H15B H -0.1114 0.1541 0.9154 0.039 Uiso 1 1 calc R . . H15C H -0.1380 0.2460 0.9329 0.039 Uiso 1 1 calc R . . C16 C -0.0479(5) 0.3294(4) 0.8670(2) 0.0247(16) Uani 1 1 d . . . H16A H -0.0436 0.3555 0.8394 0.030 Uiso 1 1 calc R . . H16B H 0.0185 0.3089 0.8787 0.030 Uiso 1 1 calc R . . H16C H -0.0951 0.3703 0.8860 0.030 Uiso 1 1 calc R . . C17 C 0.1505(6) 0.0674(5) 0.8891(2) 0.0263(16) Uani 1 1 d . . . H17A H 0.2187 0.0304 0.8946 0.032 Uiso 1 1 calc R . . H17B H 0.1023 0.0412 0.8994 0.032 Uiso 1 1 calc R . . H17C H 0.1361 0.1201 0.9035 0.032 Uiso 1 1 calc R . . C18 C 0.2334(5) 0.1357(4) 0.8218(2) 0.0262(16) Uani 1 1 d . . . H18A H 0.2184 0.1842 0.8398 0.031 Uiso 1 1 calc R . . H18B H 0.2321 0.1534 0.7922 0.031 Uiso 1 1 calc R . . H18C H 0.3000 0.0959 0.8274 0.031 Uiso 1 1 calc R . . C19 C -0.0001(6) -0.0544(4) 0.7577(2) 0.0292(17) Uani 1 1 d . . . H19A H -0.0721 -0.0346 0.7530 0.035 Uiso 1 1 calc R . . H19B H 0.0117 -0.0813 0.7855 0.035 Uiso 1 1 calc R . . H19C H 0.0363 -0.0944 0.7360 0.035 Uiso 1 1 calc R . . C20 C 0.0407(6) 0.0593(5) 0.6992(2) 0.0321(18) Uani 1 1 d . . . H20A H 0.0865 0.0120 0.6833 0.039 Uiso 1 1 calc R . . H20B H 0.0614 0.1077 0.6942 0.039 Uiso 1 1 calc R . . H20C H -0.0277 0.0723 0.6901 0.039 Uiso 1 1 calc R . . C21 C -0.0764(6) 0.2306(5) 0.6377(3) 0.0379(19) Uani 1 1 d . . . H21A H -0.1312 0.2414 0.6187 0.045 Uiso 1 1 calc R . . H21B H -0.0938 0.2075 0.6644 0.045 Uiso 1 1 calc R . . H21C H -0.0149 0.1908 0.6248 0.045 Uiso 1 1 calc R . . C22 C -0.0404(6) 0.3643(5) 0.5948(2) 0.0346(19) Uani 1 1 d . . . H22A H 0.0257 0.3309 0.5825 0.042 Uiso 1 1 calc R . . H22B H -0.0453 0.4226 0.5957 0.042 Uiso 1 1 calc R . . H22C H -0.0928 0.3596 0.5775 0.042 Uiso 1 1 calc R . . C23 C -0.1635(5) 0.4535(5) 0.7694(2) 0.0280(16) Uani 1 1 d . . . H23A H -0.2336 0.4891 0.7665 0.034 Uiso 1 1 calc R . . H23B H -0.1365 0.4720 0.7932 0.034 Uiso 1 1 calc R . . H23C H -0.1599 0.3959 0.7743 0.034 Uiso 1 1 calc R . . C24 C -0.0788(6) 0.5611(4) 0.7266(2) 0.0296(17) Uani 1 1 d . . . H24A H -0.0419 0.5730 0.7017 0.035 Uiso 1 1 calc R . . H24B H -0.0423 0.5612 0.7518 0.035 Uiso 1 1 calc R . . H24C H -0.1457 0.6038 0.7292 0.035 Uiso 1 1 calc R . . C25 C 0.1888(6) 0.4740(4) 0.7365(2) 0.0282(17) Uani 1 1 d . . . H25A H 0.1258 0.5197 0.7429 0.034 Uiso 1 1 calc R . . H25B H 0.2117 0.4792 0.7073 0.034 Uiso 1 1 calc R . . H25C H 0.2398 0.4762 0.7554 0.034 Uiso 1 1 calc R . . C26 C 0.1513(6) 0.3688(5) 0.8010(2) 0.0274(16) Uani 1 1 d . . . H26A H 0.2086 0.3751 0.8141 0.033 Uiso 1 1 calc R . . H26B H 0.1463 0.3147 0.8090 0.033 Uiso 1 1 calc R . . H26C H 0.0896 0.4132 0.8104 0.033 Uiso 1 1 calc R . . C27 C 0.2570(6) 0.1342(4) 0.6875(2) 0.0304(17) Uani 1 1 d . . . H27A H 0.2133 0.1056 0.6782 0.037 Uiso 1 1 calc R . . H27B H 0.2581 0.1313 0.7182 0.037 Uiso 1 1 calc R . . H27C H 0.3251 0.1075 0.6752 0.037 Uiso 1 1 calc R . . C28 C 0.2276(6) 0.2314(5) 0.6135(2) 0.0369(19) Uani 1 1 d . . . H28A H 0.2981 0.1993 0.6061 0.044 Uiso 1 1 calc R . . H28B H 0.2096 0.2865 0.6001 0.044 Uiso 1 1 calc R . . H28C H 0.1849 0.2024 0.6036 0.044 Uiso 1 1 calc R . . C29 C -0.2280(7) -0.1579(5) 0.9138(3) 0.051(3) Uani 1 1 d . . . H29A H -0.2563 -0.1374 0.9418 0.062 Uiso 1 1 calc R . . H29B H -0.1651 -0.2048 0.9165 0.062 Uiso 1 1 calc R . . H29C H -0.2757 -0.1761 0.8995 0.062 Uiso 1 1 calc R . . C30 C -0.3062(6) -0.0162(5) 0.8822(3) 0.038(2) Uani 1 1 d . . . H30A H -0.3511 -0.0353 0.8666 0.045 Uiso 1 1 calc R . . H30B H -0.2927 0.0292 0.8665 0.045 Uiso 1 1 calc R . . H30C H -0.3380 0.0037 0.9099 0.045 Uiso 1 1 calc R . . C31 C -0.1381(10) -0.0575(6) 0.9977(2) 0.065(3) Uani 1 1 d . . . H31A H -0.1306 -0.0308 1.0234 0.077 Uiso 1 1 calc R . . H31B H -0.0834 -0.1110 0.9945 0.077 Uiso 1 1 calc R . . H31C H -0.2025 -0.0664 0.9995 0.077 Uiso 1 1 calc R . . C32 C -0.2304(6) 0.0756(5) 0.9613(2) 0.0340(18) Uani 1 1 d . . . H32A H -0.2887 0.0590 0.9580 0.041 Uiso 1 1 calc R . . H32B H -0.2261 0.1142 0.9385 0.041 Uiso 1 1 calc R . . H32C H -0.2374 0.1029 0.9884 0.041 Uiso 1 1 calc R . . C33 C 0.0971(6) -0.1364(5) 0.9330(3) 0.047(2) Uani 1 1 d . . . H33A H 0.1546 -0.1883 0.9350 0.057 Uiso 1 1 calc R . . H33B H 0.0747 -0.1141 0.9613 0.057 Uiso 1 1 calc R . . H33C H 0.1169 -0.0959 0.9157 0.057 Uiso 1 1 calc R . . C34 C 0.0488(6) -0.1975(5) 0.8711(2) 0.0346(19) Uani 1 1 d . . . H34A H 0.0711 -0.1613 0.8516 0.042 Uiso 1 1 calc R . . H34B H -0.0058 -0.2103 0.8590 0.042 Uiso 1 1 calc R . . H34C H 0.1050 -0.2492 0.8758 0.042 Uiso 1 1 calc R . . C35 C 0.3342(7) 0.4970(6) 0.6232(3) 0.056(3) Uani 1 1 d . A . H35A H 0.3664 0.4765 0.5957 0.068 Uiso 1 1 calc R . . H35B H 0.3185 0.4525 0.6387 0.068 Uiso 1 1 calc R . . H35C H 0.3798 0.5149 0.6391 0.068 Uiso 1 1 calc R . . C36 C 0.2646(11) 0.6378(8) 0.5919(4) 0.092(4) Uani 1 1 d . A . H36A H 0.3309 0.6377 0.5985 0.110 Uiso 1 1 calc R . . H36B H 0.2136 0.6915 0.5993 0.110 Uiso 1 1 calc R . . H36C H 0.2640 0.6285 0.5617 0.110 Uiso 1 1 calc R . . C37 C 0.2541(12) 0.4087(9) 0.5426(5) 0.053(5) Uiso 0.62(2) 1 d P A 1 H37A H 0.2602 0.3819 0.5154 0.079 Uiso 0.62(2) 1 calc PR A 1 H37B H 0.2429 0.3721 0.5651 0.079 Uiso 0.62(2) 1 calc PR A 1 H37C H 0.3160 0.4195 0.5471 0.079 Uiso 0.62(2) 1 calc PR A 1 C37A C 0.1452(19) 0.4267(15) 0.5289(8) 0.049(8) Uiso 0.38(2) 1 d P A 2 H37D H 0.2063 0.3819 0.5193 0.074 Uiso 0.38(2) 1 calc PR A 2 H37E H 0.1011 0.4467 0.5055 0.074 Uiso 0.38(2) 1 calc PR A 2 H37F H 0.1104 0.4056 0.5516 0.074 Uiso 0.38(2) 1 calc PR A 2 C38 C 0.1666(10) 0.5469(8) 0.5061(3) 0.081(4) Uani 1 1 d . A . H38A H 0.2155 0.5743 0.5097 0.098 Uiso 1 1 calc R . . H38B H 0.0993 0.5889 0.5049 0.098 Uiso 1 1 calc R . . H38C H 0.1836 0.5156 0.4798 0.098 Uiso 1 1 calc R . . C39 C -0.0072(13) 0.6898(7) 0.6300(4) 0.130(8) Uani 1 1 d . A . H39A H -0.0442 0.7479 0.6227 0.156 Uiso 1 1 calc R . . H39B H 0.0535 0.6861 0.6441 0.156 Uiso 1 1 calc R . . H39C H -0.0498 0.6683 0.6489 0.156 Uiso 1 1 calc R . . C40 C -0.0665(9) 0.6183(9) 0.5743(6) 0.130(8) Uani 1 1 d . A . H40A H -0.0642 0.5637 0.5853 0.156 Uiso 1 1 calc R . . H40B H -0.0628 0.6179 0.5435 0.156 Uiso 1 1 calc R . . H40C H -0.1293 0.6608 0.5844 0.156 Uiso 1 1 calc R . . C41 C 0.0115(5) -0.1536(4) 0.9129(2) 0.0256(16) Uani 1 1 d . . . H41 H -0.0084 -0.1931 0.9321 0.031 Uiso 1 1 calc R . . C42 C -0.2074(5) -0.0882(5) 0.8880(2) 0.0268(16) Uani 1 1 d . . . H42 H -0.1835 -0.1112 0.8593 0.032 Uiso 1 1 calc R . . C43 C -0.1346(6) -0.0017(4) 0.9597(2) 0.0265(16) Uani 1 1 d . . . H43 H -0.0781 0.0187 0.9639 0.032 Uiso 1 1 calc R . . C44 C 0.1689(9) 0.4877(6) 0.5430(3) 0.062(3) Uani 1 1 d . . . H44 H 0.1104 0.4700 0.5387 0.074 Uiso 1 1 calc R A 1 C45 C 0.0222(8) 0.6380(6) 0.5897(3) 0.070(4) Uani 1 1 d . . . H45 H 0.0409 0.6731 0.5674 0.084 Uiso 1 1 calc R A . C46 C 0.2412(8) 0.5677(6) 0.6172(3) 0.052(3) Uani 1 1 d . . . H46 H 0.2166 0.5905 0.6459 0.062 Uiso 1 1 calc R A . C47 C 0.4506(5) -0.0511(4) 0.4256(2) 0.0248(16) Uani 1 1 d . . . H47 H 0.4578 -0.0078 0.4414 0.030 Uiso 1 1 calc R . . C48 C 0.4814(5) -0.1968(4) 0.4182(2) 0.0268(16) Uani 1 1 d . . . H48 H 0.5087 -0.2526 0.4281 0.032 Uiso 1 1 calc R . . C49 C 0.3906(5) -0.0966(4) 0.3670(2) 0.0238(16) Uani 1 1 d . . . H49 H 0.3566 -0.0858 0.3415 0.029 Uiso 1 1 calc R . . C50 C 0.1550(6) 0.0769(5) 0.3874(2) 0.0304(17) Uani 1 1 d . . . H50 H 0.1612 0.0515 0.3608 0.037 Uiso 1 1 calc R . . C51 C 0.2209(6) 0.1291(4) 0.4413(2) 0.0276(17) Uani 1 1 d . . . H51 H 0.2745 0.1410 0.4527 0.033 Uiso 1 1 calc R . . C52 C 0.0536(6) 0.1292(5) 0.4504(3) 0.041(2) Uani 1 1 d . . . H52 H -0.0079 0.1412 0.4666 0.050 Uiso 1 1 calc R . . C53 C 0.2523(5) 0.1341(4) 0.3033(2) 0.0181(14) Uani 1 1 d . . . H53 H 0.1960 0.1669 0.3202 0.022 Uiso 1 1 calc R . . C54 C 0.4141(5) 0.0312(4) 0.2959(2) 0.0180(14) Uani 1 1 d . . . H54 H 0.4711 -0.0087 0.3078 0.022 Uiso 1 1 calc R . . C55 C 0.3328(5) 0.0998(4) 0.2337(2) 0.0204(15) Uani 1 1 d . . . H55 H 0.3326 0.1076 0.2040 0.024 Uiso 1 1 calc R . . C56 C 0.3684(5) 0.2097(4) 0.3919(2) 0.0225(15) Uani 1 1 d . . . H56 H 0.2975 0.2346 0.3952 0.027 Uiso 1 1 calc R . . C57 C 0.5132(5) 0.0936(4) 0.3778(2) 0.0234(15) Uani 1 1 d . . . H57 H 0.5453 0.0362 0.3720 0.028 Uiso 1 1 calc R . . C58 C 0.5297(6) 0.2261(5) 0.3898(2) 0.0317(18) Uani 1 1 d . . . H58 H 0.5699 0.2596 0.3922 0.038 Uiso 1 1 calc R . . C59 C 0.1742(5) 0.5645(4) 0.8696(2) 0.0231(15) Uani 1 1 d . . . H59 H 0.1852 0.5456 0.8414 0.028 Uiso 1 1 calc R . . C60 C 0.2345(5) 0.5950(4) 0.9324(2) 0.0255(16) Uani 1 1 d . . . H60 H 0.2865 0.5998 0.9483 0.031 Uiso 1 1 calc R . . C61 C 0.0605(5) 0.6081(4) 0.9296(2) 0.0269(16) Uani 1 1 d . . . H61 H -0.0047 0.6207 0.9427 0.032 Uiso 1 1 calc R . . C62 C 0.2938(5) 0.6253(4) 0.7988(2) 0.0210(15) Uani 1 1 d . . . H62 H 0.2383 0.6590 0.8158 0.025 Uiso 1 1 calc R . . C63 C 0.4462(5) 0.5126(4) 0.7903(2) 0.0194(15) Uani 1 1 d . . . H63 H 0.4984 0.4667 0.8013 0.023 Uiso 1 1 calc R . . C64 C 0.3765(6) 0.5955(4) 0.7296(2) 0.0243(16) Uani 1 1 d . . . H64 H 0.3780 0.6067 0.7002 0.029 Uiso 1 1 calc R . . C65 C 0.4597(5) 0.4216(4) 0.9221(2) 0.0226(15) Uani 1 1 d . . . H65 H 0.4583 0.4641 0.9408 0.027 Uiso 1 1 calc R . . C66 C 0.4212(5) 0.3794(4) 0.8572(2) 0.0202(15) Uani 1 1 d . . . H66 H 0.3934 0.3920 0.8304 0.024 Uiso 1 1 calc R . . C67 C 0.5018(5) 0.2748(4) 0.9091(2) 0.0240(16) Uani 1 1 d . . . H67 H 0.5293 0.2183 0.9179 0.029 Uiso 1 1 calc R . . C68 C 0.5367(5) 0.5643(4) 0.8901(2) 0.0232(15) Uani 1 1 d . . . H68 H 0.5692 0.5059 0.8874 0.028 Uiso 1 1 calc R . . C69 C 0.3905(5) 0.6850(4) 0.8887(2) 0.0211(15) Uani 1 1 d . . . H69 H 0.3204 0.7115 0.8857 0.025 Uiso 1 1 calc R . . C70 C 0.5517(6) 0.6961(5) 0.9027(2) 0.0299(17) Uani 1 1 d . . . H70 H 0.5907 0.7289 0.9089 0.036 Uiso 1 1 calc R . . C71 C 0.3330(5) 0.0764(4) 0.3228(2) 0.0177(14) Uani 1 1 d . . . C72 C 0.2516(5) 0.1452(4) 0.2597(2) 0.0196(15) Uani 1 1 d . . . C73 C 0.4141(5) 0.0428(4) 0.2527(2) 0.0162(14) Uani 1 1 d . . . C74 C 0.4108(5) 0.1243(4) 0.38327(19) 0.0183(14) Uani 1 1 d . . . C75 C 0.5724(6) 0.1424(5) 0.3804(2) 0.0327(18) Uani 1 1 d . . . C76 C 0.4268(6) 0.2588(4) 0.3956(2) 0.0259(16) Uani 1 1 d . . . C77 C 0.3989(5) -0.0299(4) 0.3885(2) 0.0214(15) Uani 1 1 d . . . C78 C 0.4300(5) -0.1778(4) 0.3814(2) 0.0233(15) Uani 1 1 d . . . C79 C 0.4918(5) -0.1318(4) 0.4401(2) 0.0250(16) Uani 1 1 d . . . C80 C 0.2351(5) 0.0951(4) 0.4008(2) 0.0223(15) Uani 1 1 d . . . C81 C 0.1323(6) 0.1458(5) 0.4650(2) 0.0306(17) Uani 1 1 d . . . C82 C 0.0662(7) 0.0943(6) 0.4112(3) 0.046(2) Uani 1 1 d . . . C83 C 0.3679(5) 0.5587(4) 0.8179(2) 0.0169(14) Uani 1 1 d . . . C84 C 0.2987(5) 0.6433(4) 0.7566(2) 0.0232(16) Uani 1 1 d . . . C85 C 0.4516(5) 0.5305(4) 0.7478(2) 0.0204(15) Uani 1 1 d . . . C86 C 0.4205(5) 0.4443(4) 0.8822(2) 0.0183(14) Uani 1 1 d . . . C87 C 0.4614(5) 0.2967(4) 0.8701(2) 0.0218(15) Uani 1 1 d . . . C88 C 0.5000(5) 0.3399(4) 0.9350(2) 0.0223(15) Uani 1 1 d . . . C89 C 0.4336(5) 0.5979(4) 0.88455(19) 0.0165(14) Uani 1 1 d . . . C90 C 0.5942(5) 0.6118(5) 0.8993(2) 0.0292(17) Uani 1 1 d . . . C91 C 0.4481(6) 0.7327(4) 0.8968(2) 0.0233(16) Uani 1 1 d . . . C92 C 0.2556(5) 0.5707(4) 0.8905(2) 0.0191(14) Uani 1 1 d . . . C93 C 0.0785(5) 0.5850(4) 0.8885(2) 0.0224(15) Uani 1 1 d . . . C94 C 0.1380(6) 0.6127(4) 0.9516(2) 0.0274(17) Uani 1 1 d . . . C95 C 0.5449(7) -0.1482(6) 0.4801(3) 0.043(2) Uani 1 1 d . . . C96 C 0.4167(6) -0.2445(5) 0.3566(3) 0.0357(19) Uani 1 1 d . . . C97 C 0.3774(7) 0.3487(4) 0.4062(3) 0.0349(19) Uani 1 1 d . . . C98 C 0.6831(7) 0.1050(6) 0.3713(3) 0.051(2) Uani 1 1 d . . . C99 C 0.5070(5) -0.0063(4) 0.2271(2) 0.0248(16) Uani 1 1 d . . . C100 C 0.1641(6) 0.2069(4) 0.2393(2) 0.0283(17) Uani 1 1 d . . . C101 C -0.0174(11) 0.0717(9) 0.3953(4) 0.082(4) Uiso 1 1 d . . . C102 C 0.1205(7) 0.1829(7) 0.5075(3) 0.049(2) Uani 1 1 d . . . C103 C -0.0067(5) 0.5831(5) 0.8632(3) 0.0311(18) Uani 1 1 d . . . C104 C 0.1186(6) 0.6361(5) 0.9970(3) 0.038(2) Uani 1 1 d . . . C105 C 0.3972(6) 0.8255(5) 0.9005(2) 0.0344(19) Uani 1 1 d . . . C106 C 0.7053(7) 0.5691(7) 0.9044(4) 0.059(3) Uani 1 1 d . . . C107 C 0.5443(7) 0.3179(5) 0.9776(2) 0.042(2) Uani 1 1 d . . . C108 C 0.4610(6) 0.2306(4) 0.8411(3) 0.0324(19) Uani 1 1 d . . . C109 C 0.5374(6) 0.4759(5) 0.7206(2) 0.0284(17) Uani 1 1 d . . . C110 C 0.2169(6) 0.7139(5) 0.7385(3) 0.039(2) Uani 1 1 d . . . C111 C 0.5868(8) 0.6744(6) 0.7867(3) 0.055(3) Uani 1 1 d . . . H11C H 0.6373 0.6901 0.8010 0.066 Uiso 1 1 calc R . . H11D H 0.5649 0.6361 0.8054 0.066 Uiso 1 1 calc R . . C112 C 0.5010(8) 0.7485(6) 0.7770(3) 0.060(3) Uani 1 1 d . . . H11E H 0.5040 0.7973 0.7918 0.072 Uiso 1 1 calc R . . H11F H 0.4373 0.7401 0.7859 0.072 Uiso 1 1 calc R . . C113 C 0.5073(8) 0.7617(6) 0.7298(3) 0.051(2) Uani 1 1 d . . . H11G H 0.4502 0.7539 0.7165 0.061 Uiso 1 1 calc R . . H11H H 0.5077 0.8182 0.7227 0.061 Uiso 1 1 calc R . . C114 C 0.6029(8) 0.6980(6) 0.7159(3) 0.053(2) Uani 1 1 d . . . H11I H 0.5957 0.6742 0.6889 0.064 Uiso 1 1 calc R . . H11J H 0.6560 0.7228 0.7117 0.064 Uiso 1 1 calc R . . C115 C 0.1722(8) 0.3593(5) 0.9191(3) 0.052(2) Uani 1 1 d . . . H11K H 0.1019 0.3959 0.9154 0.063 Uiso 1 1 calc R . . H11L H 0.2155 0.3740 0.8971 0.063 Uiso 1 1 calc R . . C116 C 0.2025(9) 0.3717(6) 0.9607(3) 0.064(3) Uani 1 1 d . . . H11M H 0.1449 0.4094 0.9776 0.076 Uiso 1 1 calc R . . H11N H 0.2567 0.3955 0.9583 0.076 Uiso 1 1 calc R . . C117 C 0.2388(10) 0.2868(7) 0.9802(3) 0.073(3) Uani 1 1 d . . . H11O H 0.3079 0.2729 0.9895 0.088 Uiso 1 1 calc R . . H11P H 0.1944 0.2832 1.0048 0.088 Uiso 1 1 calc R . . C118 C 0.2360(18) 0.2312(8) 0.9472(5) 0.167(11) Uani 1 1 d . . . H11Q H 0.3053 0.2001 0.9365 0.201 Uiso 1 1 calc R . . H11R H 0.2061 0.1906 0.9590 0.201 Uiso 1 1 calc R . . O3 O 0.820(3) 0.191(3) 0.5384(14) 0.238(18) Uiso 0.50 1 d P . . C121 C 0.834(2) 0.1198(19) 0.5427(9) 0.088(8) Uiso 0.50 1 d P . . C122 C 0.7719(13) 0.0987(11) 0.5139(6) 0.043(4) Uiso 0.50 1 d P . . C123 C 0.530(2) -0.496(2) 0.5194(10) 0.052(9) Uiso 0.50 1 d P . . O4 O 0.4637(18) -0.3842(15) 0.4595(7) 0.129(8) Uiso 0.50 1 d P . . C131 C -0.5366(15) 0.0017(13) 0.9737(6) 0.056(5) Uiso 0.50 1 d P . . C130 C -0.4894(17) -0.0657(14) 0.9878(7) 0.063(6) Uiso 0.50 1 d P . . O5 O -0.529(2) 0.0768(18) 0.9622(9) 0.158(10) Uiso 0.50 1 d P . . C125 C 0.4174(19) -0.4319(16) 0.4551(8) 0.076(7) Uiso 0.50 1 d P . . C119 C 0.767(2) 0.2335(19) 0.5153(10) 0.097(9) Uiso 0.50 1 d P . . C126 C 0.520(3) -0.475(2) 0.5160(13) 0.083(14) Uiso 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 Cr1 0.0112(5) 0.0096(5) 0.0089(5) -0.0030(4) 0.0030(4) -0.0043(4) Cr2 0.0122(5) 0.0119(5) 0.0092(5) -0.0003(4) 0.0012(4) -0.0039(4) Si1 0.0205(10) 0.0192(9) 0.0130(9) 0.0043(7) -0.0020(7) -0.0106(8) Si2 0.0314(11) 0.0225(10) 0.0218(11) 0.0089(8) 0.0073(9) -0.0054(9) P1 0.0198(9) 0.0173(8) 0.0181(9) -0.0042(7) 0.0030(7) -0.0073(7) P2 0.0162(9) 0.0187(9) 0.0235(10) -0.0021(7) -0.0021(7) -0.0071(7) P3 0.0170(9) 0.0166(8) 0.0155(9) 0.0016(7) -0.0024(7) -0.0046(7) P4 0.0227(10) 0.0169(9) 0.0196(9) -0.0045(7) -0.0036(7) -0.0035(7) P8 0.0187(9) 0.0180(9) 0.0188(9) -0.0001(7) 0.0033(7) -0.0021(7) P9 0.0193(9) 0.0244(9) 0.0207(10) 0.0013(7) -0.0061(7) -0.0065(8) P10 0.0189(9) 0.0179(9) 0.0199(9) 0.0013(7) 0.0003(7) -0.0012(7) P12 0.0196(9) 0.0224(9) 0.0157(9) -0.0005(7) -0.0011(7) -0.0082(7) N1 0.009(3) 0.010(2) 0.013(3) -0.004(2) 0.003(2) -0.003(2) N2 0.010(3) 0.015(3) 0.011(3) -0.007(2) 0.002(2) -0.002(2) F1 0.118(8) 0.87(4) 0.196(12) -0.34(2) 0.118(9) -0.290(17) F2 0.043(3) 0.075(4) 0.127(6) -0.017(4) -0.038(4) -0.016(3) F3 0.270(13) 0.214(11) 0.116(7) 0.079(7) -0.107(8) -0.216(11) F4 0.051(4) 0.276(12) 0.103(6) -0.142(8) 0.010(4) -0.017(6) F5 0.085(4) 0.065(3) 0.037(3) -0.028(3) 0.006(3) -0.038(3) F6 0.262(11) 0.094(5) 0.021(3) 0.003(3) -0.028(4) -0.107(6) F7 0.063(4) 0.087(4) 0.107(5) -0.045(4) 0.015(3) -0.057(4) F8 0.073(4) 0.054(3) 0.041(3) -0.017(2) -0.008(3) -0.036(3) F9 0.133(6) 0.024(3) 0.074(4) 0.000(3) -0.053(4) -0.013(3) F10 0.163(7) 0.036(3) 0.088(5) 0.007(3) -0.095(5) -0.001(4) F11 0.092(5) 0.102(5) 0.075(4) 0.030(4) -0.060(4) -0.053(4) F12 0.087(5) 0.138(6) 0.026(3) -0.009(3) -0.019(3) -0.008(4) F13 0.016(2) 0.066(3) 0.039(3) -0.021(2) 0.0057(19) -0.012(2) F14 0.034(3) 0.081(4) 0.011(2) -0.003(2) 0.0019(19) 0.013(2) F15 0.045(3) 0.030(3) 0.063(3) -0.017(2) 0.024(3) -0.003(2) F16 0.032(3) 0.057(3) 0.028(3) -0.009(2) -0.006(2) 0.014(2) F17 0.039(3) 0.044(3) 0.074(4) 0.034(3) -0.014(3) -0.006(2) F18 0.039(3) 0.042(3) 0.048(3) -0.011(2) -0.027(2) -0.002(2) F19 0.169(7) 0.027(3) 0.050(4) -0.006(2) 0.034(4) -0.005(4) F20 0.084(4) 0.037(3) 0.092(4) -0.006(3) 0.015(3) -0.031(3) F21 0.079(4) 0.028(3) 0.141(6) -0.008(3) -0.047(4) 0.007(3) F22 0.032(3) 0.071(4) 0.182(8) -0.006(4) 0.021(4) -0.027(3) F23 0.052(4) 0.100(5) 0.090(5) -0.022(4) 0.032(4) -0.002(4) F24 0.020(3) 0.088(5) 0.128(6) 0.048(4) -0.011(3) -0.007(3) F25 0.030(3) 0.093(4) 0.078(4) -0.031(3) -0.010(3) -0.022(3) F26 0.039(4) 0.204(10) 0.129(7) -0.096(7) -0.003(4) -0.009(5) F27 0.060(5) 0.118(7) 0.411(19) 0.135(10) -0.126(8) -0.043(5) F28 0.085(5) 0.029(3) 0.158(7) -0.012(3) 0.039(5) -0.028(3) F29 0.069(4) 0.033(3) 0.034(3) -0.010(2) 0.000(3) 0.008(2) F30 0.131(6) 0.024(3) 0.059(4) 0.008(2) -0.052(4) -0.002(3) F31 0.064(4) 0.084(4) 0.028(3) -0.024(3) 0.003(3) -0.023(3) F32 0.085(4) 0.058(3) 0.033(3) -0.020(3) -0.006(3) 0.030(3) F33 0.080(4) 0.081(4) 0.030(3) 0.001(3) 0.011(3) -0.032(3) F34 0.029(3) 0.032(2) 0.061(3) -0.011(2) -0.010(2) 0.000(2) F35 0.043(3) 0.031(3) 0.111(5) -0.003(3) -0.017(3) -0.022(2) F36 0.036(3) 0.115(5) 0.036(3) -0.021(3) -0.003(2) -0.025(3) F37 0.159(8) 0.027(3) 0.181(9) 0.001(4) -0.080(7) 0.034(4) F38 0.033(4) 0.138(7) 0.301(13) 0.171(8) -0.071(5) -0.024(4) F39 0.086(5) 0.139(7) 0.084(5) 0.083(5) 0.003(4) 0.045(5) F40 0.052(3) 0.056(3) 0.024(3) 0.009(2) 0.010(2) 0.002(2) F41 0.027(2) 0.048(3) 0.034(3) -0.004(2) 0.003(2) -0.007(2) F42 0.058(3) 0.039(3) 0.056(3) -0.023(2) 0.012(3) -0.015(2) F43 0.142(6) 0.042(3) 0.031(3) 0.003(2) -0.033(3) -0.019(3) F44 0.065(4) 0.116(6) 0.060(4) 0.000(4) -0.037(3) 0.007(4) F45 0.186(8) 0.089(5) 0.043(3) 0.043(3) -0.045(4) -0.089(5) F46 0.092(4) 0.020(2) 0.076(4) -0.002(2) -0.051(3) -0.001(3) F47 0.047(3) 0.050(3) 0.049(3) -0.017(2) 0.002(2) -0.025(2) F48 0.028(3) 0.047(3) 0.076(4) -0.017(3) -0.008(2) -0.024(2) O1 0.084(5) 0.043(4) 0.040(4) 0.005(3) -0.007(3) 0.004(3) O2 0.058(4) 0.039(3) 0.048(4) -0.001(3) -0.018(3) -0.016(3) C120 0.026(8) 0.029(8) 0.045(10) 0.005(7) 0.003(7) -0.008(7) B1 0.022(4) 0.024(4) 0.014(4) -0.005(3) -0.004(3) -0.007(3) B2 0.015(4) 0.014(4) 0.026(4) -0.002(3) -0.003(3) -0.003(3) C1 0.011(3) 0.017(3) 0.013(3) -0.003(3) -0.001(3) -0.006(3) C2 0.010(3) 0.018(3) 0.015(3) -0.002(3) -0.002(3) -0.004(3) C3 0.015(3) 0.017(3) 0.014(3) -0.005(3) 0.000(3) -0.002(3) C4 0.026(4) 0.019(3) 0.018(4) 0.003(3) 0.002(3) -0.004(3) C5 0.020(4) 0.018(3) 0.028(4) 0.002(3) -0.007(3) 0.001(3) C6 0.024(4) 0.019(3) 0.026(4) -0.004(3) -0.001(3) 0.002(3) C7 0.030(4) 0.035(4) 0.030(4) 0.007(3) -0.011(3) -0.004(3) C8 0.026(4) 0.032(4) 0.025(4) 0.007(3) -0.005(3) 0.000(3) C9 0.024(4) 0.029(4) 0.032(4) -0.003(3) 0.009(3) -0.005(3) C10 0.015(4) 0.040(4) 0.030(4) 0.001(3) -0.003(3) -0.010(3) C11 0.016(4) 0.024(4) 0.037(4) -0.008(3) 0.009(3) -0.010(3) C12 0.027(4) 0.027(4) 0.042(5) -0.007(3) 0.002(3) -0.017(3) C13 0.023(4) 0.025(4) 0.042(5) -0.003(3) -0.010(3) -0.011(3) C14 0.028(4) 0.028(4) 0.035(4) 0.009(3) -0.013(3) -0.005(3) C15 0.048(5) 0.027(4) 0.022(4) -0.008(3) 0.004(4) -0.016(4) C16 0.021(4) 0.020(3) 0.036(4) -0.002(3) 0.000(3) -0.010(3) C17 0.030(4) 0.033(4) 0.022(4) 0.003(3) -0.007(3) -0.017(3) C18 0.024(4) 0.030(4) 0.029(4) 0.000(3) -0.001(3) -0.015(3) C19 0.039(5) 0.021(4) 0.029(4) -0.005(3) -0.003(3) -0.011(3) C20 0.040(5) 0.031(4) 0.020(4) -0.006(3) -0.003(3) -0.007(4) C21 0.036(5) 0.034(4) 0.045(5) -0.004(4) -0.015(4) -0.011(4) C22 0.037(5) 0.043(5) 0.020(4) -0.003(3) -0.011(3) -0.007(4) C23 0.023(4) 0.032(4) 0.027(4) -0.001(3) 0.002(3) -0.007(3) C24 0.032(4) 0.019(4) 0.033(4) -0.001(3) 0.002(3) -0.002(3) C25 0.032(4) 0.029(4) 0.028(4) -0.001(3) -0.002(3) -0.015(3) C26 0.033(4) 0.034(4) 0.016(4) 0.001(3) -0.002(3) -0.012(3) C27 0.030(4) 0.019(4) 0.036(5) 0.001(3) 0.000(3) -0.001(3) C28 0.041(5) 0.040(5) 0.022(4) -0.007(3) 0.004(4) -0.004(4) C29 0.038(5) 0.034(5) 0.088(8) 0.004(5) 0.008(5) -0.023(4) C30 0.028(4) 0.056(5) 0.038(5) 0.007(4) -0.010(4) -0.024(4) C31 0.132(10) 0.050(6) 0.011(4) 0.005(4) 0.011(5) -0.034(6) C32 0.036(5) 0.045(5) 0.021(4) -0.009(3) 0.009(3) -0.015(4) C33 0.036(5) 0.034(5) 0.069(6) 0.006(4) -0.029(5) -0.004(4) C34 0.034(4) 0.026(4) 0.040(5) 0.008(3) -0.004(4) -0.005(3) C35 0.047(6) 0.078(7) 0.058(6) 0.014(5) -0.010(5) -0.040(6) C36 0.120(11) 0.082(9) 0.101(10) 0.027(7) 0.003(8) -0.074(9) C38 0.118(10) 0.090(9) 0.020(5) 0.018(5) 0.005(6) -0.017(8) C39 0.176(15) 0.041(6) 0.099(10) 0.023(7) 0.094(11) 0.037(8) C40 0.033(7) 0.111(11) 0.215(19) 0.101(12) 0.009(9) 0.001(7) C41 0.031(4) 0.019(3) 0.028(4) 0.008(3) -0.008(3) -0.009(3) C42 0.028(4) 0.037(4) 0.024(4) -0.008(3) 0.009(3) -0.023(3) C43 0.038(4) 0.032(4) 0.013(4) 0.002(3) 0.001(3) -0.017(3) C44 0.096(9) 0.061(6) 0.027(5) 0.006(4) 0.000(5) -0.028(6) C45 0.071(7) 0.038(5) 0.067(7) 0.028(5) 0.044(6) 0.014(5) C46 0.079(7) 0.056(6) 0.034(5) 0.000(4) 0.008(5) -0.043(6) C47 0.030(4) 0.029(4) 0.014(4) -0.009(3) 0.001(3) -0.009(3) C48 0.022(4) 0.024(4) 0.027(4) 0.001(3) 0.000(3) 0.001(3) C49 0.017(4) 0.032(4) 0.023(4) 0.002(3) -0.005(3) -0.008(3) C50 0.035(4) 0.036(4) 0.023(4) -0.016(3) 0.008(3) -0.016(4) C51 0.028(4) 0.036(4) 0.015(4) -0.005(3) 0.004(3) -0.006(3) C52 0.033(5) 0.055(5) 0.037(5) -0.015(4) 0.014(4) -0.018(4) C53 0.021(4) 0.018(3) 0.017(4) -0.009(3) 0.000(3) -0.008(3) C54 0.013(3) 0.022(3) 0.017(4) -0.002(3) -0.003(3) -0.003(3) C55 0.028(4) 0.022(3) 0.010(3) -0.008(3) -0.004(3) -0.005(3) C56 0.021(4) 0.027(4) 0.017(4) 0.000(3) -0.001(3) -0.004(3) C57 0.018(4) 0.026(4) 0.023(4) -0.006(3) 0.003(3) -0.004(3) C58 0.035(5) 0.032(4) 0.032(4) 0.001(3) -0.003(4) -0.016(4) C59 0.025(4) 0.015(3) 0.027(4) -0.003(3) 0.004(3) -0.005(3) C60 0.027(4) 0.022(4) 0.025(4) -0.003(3) 0.001(3) -0.004(3) C61 0.020(4) 0.025(4) 0.033(4) -0.004(3) 0.007(3) -0.006(3) C62 0.020(4) 0.016(3) 0.029(4) -0.006(3) -0.002(3) -0.007(3) C63 0.017(4) 0.014(3) 0.027(4) 0.001(3) -0.005(3) -0.004(3) C64 0.042(5) 0.019(4) 0.017(4) 0.003(3) -0.006(3) -0.017(3) C65 0.028(4) 0.023(4) 0.016(4) -0.003(3) 0.005(3) -0.009(3) C66 0.016(3) 0.023(4) 0.022(4) 0.005(3) -0.003(3) -0.007(3) C67 0.017(4) 0.023(4) 0.033(4) 0.009(3) -0.003(3) -0.010(3) C68 0.020(4) 0.019(3) 0.030(4) 0.001(3) -0.001(3) -0.006(3) C69 0.022(4) 0.022(4) 0.017(4) 0.002(3) -0.004(3) -0.005(3) C70 0.040(5) 0.032(4) 0.027(4) 0.000(3) -0.008(3) -0.024(4) C71 0.022(4) 0.021(3) 0.014(3) -0.002(3) -0.002(3) -0.012(3) C72 0.019(4) 0.017(3) 0.022(4) -0.006(3) -0.006(3) -0.005(3) C73 0.014(3) 0.016(3) 0.017(4) -0.009(3) 0.001(3) -0.003(3) C74 0.024(4) 0.022(3) 0.008(3) -0.003(3) -0.002(3) -0.007(3) C75 0.027(4) 0.041(5) 0.029(4) -0.005(3) 0.003(3) -0.010(4) C76 0.041(5) 0.027(4) 0.011(4) 0.002(3) -0.004(3) -0.012(3) C77 0.020(4) 0.030(4) 0.015(4) -0.005(3) 0.006(3) -0.009(3) C78 0.014(3) 0.025(4) 0.031(4) -0.007(3) 0.001(3) -0.008(3) C79 0.025(4) 0.026(4) 0.020(4) -0.001(3) 0.001(3) -0.004(3) C80 0.024(4) 0.017(3) 0.022(4) 0.000(3) 0.000(3) -0.002(3) C81 0.029(4) 0.038(4) 0.020(4) -0.010(3) 0.002(3) -0.006(3) C82 0.043(5) 0.078(7) 0.035(5) -0.024(5) 0.011(4) -0.042(5) C83 0.019(4) 0.014(3) 0.020(4) 0.000(3) -0.004(3) -0.009(3) C84 0.028(4) 0.010(3) 0.027(4) 0.002(3) -0.007(3) -0.001(3) C85 0.026(4) 0.018(3) 0.020(4) 0.001(3) -0.004(3) -0.011(3) C86 0.009(3) 0.016(3) 0.027(4) -0.001(3) 0.004(3) -0.002(3) C87 0.015(3) 0.018(3) 0.034(4) -0.001(3) -0.007(3) -0.007(3) C88 0.024(4) 0.025(4) 0.018(4) 0.004(3) -0.002(3) -0.009(3) C89 0.022(4) 0.015(3) 0.013(3) 0.000(3) 0.003(3) -0.007(3) C90 0.024(4) 0.032(4) 0.034(4) 0.002(3) -0.006(3) -0.012(3) C91 0.041(5) 0.019(3) 0.012(3) -0.002(3) -0.001(3) -0.013(3) C92 0.020(4) 0.014(3) 0.021(4) 0.001(3) 0.002(3) -0.004(3) C93 0.018(4) 0.020(3) 0.029(4) -0.001(3) 0.000(3) -0.007(3) C94 0.037(4) 0.022(4) 0.020(4) -0.001(3) 0.000(3) -0.006(3) C95 0.048(5) 0.048(5) 0.029(5) 0.009(4) -0.008(4) -0.012(5) C96 0.039(5) 0.040(5) 0.035(5) 0.001(4) -0.010(4) -0.021(4) C97 0.052(5) 0.021(4) 0.033(5) 0.007(3) -0.008(4) -0.015(4) C98 0.035(5) 0.042(5) 0.076(7) 0.002(5) -0.001(5) -0.013(4) C99 0.020(4) 0.031(4) 0.018(4) -0.005(3) 0.002(3) -0.002(3) C100 0.029(4) 0.025(4) 0.023(4) -0.009(3) -0.004(3) 0.000(3) C102 0.039(5) 0.084(7) 0.030(5) -0.022(5) 0.018(4) -0.030(5) C103 0.022(4) 0.030(4) 0.046(5) -0.013(3) 0.005(3) -0.015(3) C104 0.031(5) 0.047(5) 0.029(5) -0.007(4) 0.003(4) -0.005(4) C105 0.051(5) 0.025(4) 0.033(5) 0.004(3) -0.005(4) -0.020(4) C106 0.033(5) 0.061(7) 0.094(9) 0.019(6) -0.021(6) -0.030(5) C107 0.070(7) 0.034(5) 0.024(4) 0.004(4) -0.007(4) -0.022(5) C108 0.034(4) 0.021(4) 0.043(5) 0.003(3) -0.024(4) -0.007(3) C109 0.031(4) 0.030(4) 0.022(4) -0.001(3) -0.001(3) -0.009(3) C110 0.039(5) 0.024(4) 0.039(5) 0.007(4) -0.001(4) 0.005(4) C111 0.078(7) 0.071(7) 0.025(5) -0.002(4) 0.000(5) -0.038(6) C112 0.071(7) 0.059(6) 0.048(6) -0.006(5) 0.001(5) -0.022(6) C113 0.064(6) 0.038(5) 0.054(6) 0.006(4) -0.011(5) -0.020(5) C114 0.065(7) 0.055(6) 0.031(5) 0.007(4) 0.006(5) -0.013(5) C115 0.065(7) 0.039(5) 0.055(6) 0.006(4) -0.021(5) -0.019(5) C116 0.094(8) 0.053(6) 0.055(6) -0.005(5) -0.017(6) -0.037(6) C117 0.107(10) 0.084(8) 0.045(6) 0.014(6) -0.027(6) -0.052(7) C118 0.34(3) 0.068(9) 0.150(15) 0.066(9) -0.179(18) -0.123(14) _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 Cr1 N1 1.867(5) . ? Cr1 C1 2.050(6) . ? Cr1 P2 2.3926(19) . ? Cr1 P4 2.4108(19) . ? Cr1 P1 2.4269(19) . ? Cr1 P3 2.4275(19) . ? Cr2 N2 1.878(5) . ? Cr2 C3 2.052(6) . ? Cr2 P10 2.4139(19) . ? Cr2 P8 2.4387(19) . ? Cr2 P9 2.440(2) . ? Cr2 P12 2.4418(19) . ? Si1 C2 1.841(6) . ? Si1 C42 1.877(7) . ? Si1 C43 1.887(7) . ? Si1 C41 1.900(7) . ? Si2 C4 1.843(7) . ? Si2 C45 1.885(9) . ? Si2 C46 1.889(10) . ? Si2 C44 1.891(10) . ? P1 C16 1.817(6) . ? P1 C12 1.822(8) . ? P1 C15 1.825(7) . ? P2 C13 1.802(7) . ? P2 C14 1.808(7) . ? P2 C11 1.836(7) . ? P3 C17 1.816(7) . ? P3 C18 1.816(7) . ? P3 C5 1.839(7) . ? P4 C19 1.818(7) . ? P4 C20 1.826(7) . ? P4 C6 1.843(7) . ? P8 C27 1.819(7) . ? P8 C9 1.822(8) . ? P8 C28 1.822(7) . ? P9 C22 1.808(8) . ? P9 C21 1.818(8) . ? P9 C7 1.841(8) . ? P10 C8 1.811(7) . ? P10 C23 1.816(7) . ? P10 C24 1.821(7) . ? P12 C26 1.819(7) . ? P12 C25 1.827(7) . ? P12 C10 1.845(7) . ? N1 N2 1.187(7) . ? F1 C101 1.240(15) . ? F2 C101 1.336(14) . ? F3 C101 1.327(16) . ? F4 C102 1.357(11) . ? F5 C102 1.310(10) . ? F6 C102 1.284(12) . ? F7 C96 1.342(10) . ? F8 C96 1.344(9) . ? F9 C96 1.318(9) . ? F10 C95 1.268(10) . ? F11 C95 1.343(11) . ? F12 C95 1.317(11) . ? F13 C99 1.328(8) . ? F14 C99 1.329(8) . ? F15 C99 1.337(8) . ? F16 C100 1.339(8) . ? F17 C100 1.326(9) . ? F18 C100 1.338(8) . ? F19 C97 1.295(10) . ? F20 C97 1.318(9) . ? F21 C97 1.327(10) . ? F22 C98 1.301(11) . ? F23 C98 1.367(12) . ? F24 C98 1.301(11) . ? F25 C106 1.302(11) . ? F26 C106 1.373(14) . ? F27 C106 1.244(12) . ? F28 C105 1.330(9) . ? F29 C105 1.309(9) . ? F30 C105 1.330(10) . ? F31 C104 1.322(10) . ? F32 C104 1.323(9) . ? F33 C104 1.358(10) . ? F34 C103 1.326(9) . ? F35 C103 1.347(8) . ? F36 C103 1.335(9) . ? F37 C110 1.347(11) . ? F38 C110 1.227(11) . ? F39 C110 1.284(10) . ? F40 C109 1.333(8) . ? F41 C109 1.348(9) . ? F42 C109 1.331(9) . ? F43 C107 1.293(9) . ? F44 C107 1.345(11) . ? F45 C107 1.317(10) . ? F46 C108 1.306(8) . ? F47 C108 1.378(9) . ? F48 C108 1.329(9) . ? O1 C114 1.409(10) . ? O1 C111 1.436(11) . ? O2 C118 1.373(13) . ? O2 C115 1.422(10) . ? C120 C119 1.42(3) . ? C120 C122 1.58(2) . ? B1 C80 1.635(10) . ? B1 C74 1.638(10) . ? B1 C77 1.643(10) . ? B1 C71 1.648(10) . ? B2 C83 1.626(10) . ? B2 C92 1.631(10) . ? B2 C89 1.647(9) . ? B2 C86 1.649(9) . ? C1 C2 1.221(9) . ? C3 C4 1.215(9) . ? C5 C6 1.533(10) . ? C7 C8 1.548(11) . ? C9 C10 1.515(10) . ? C11 C12 1.539(9) . ? C29 C42 1.532(10) . ? C30 C42 1.531(11) . ? C31 C43 1.527(10) . ? C32 C43 1.535(11) . ? C33 C41 1.530(11) . ? C34 C41 1.526(11) . ? C35 C46 1.468(14) . ? C36 C46 1.546(12) . ? C37 C44 1.471(18) . ? C37A C44 1.31(2) . ? C38 C44 1.522(13) . ? C39 C45 1.538(17) . ? C40 C45 1.53(2) . ? C47 C79 1.381(10) . ? C47 C77 1.398(10) . ? C48 C78 1.387(10) . ? C48 C79 1.391(10) . ? C49 C78 1.383(10) . ? C49 C77 1.396(10) . ? C50 C82 1.377(11) . ? C50 C80 1.377(10) . ? C51 C81 1.375(10) . ? C51 C80 1.408(10) . ? C52 C81 1.359(11) . ? C52 C82 1.378(11) . ? C53 C71 1.392(9) . ? C53 C72 1.395(9) . ? C54 C73 1.385(9) . ? C54 C71 1.403(9) . ? C55 C73 1.385(9) . ? C55 C72 1.389(9) . ? C56 C76 1.387(10) . ? C56 C74 1.408(9) . ? C57 C74 1.368(10) . ? C57 C75 1.387(10) . ? C58 C76 1.377(11) . ? C58 C75 1.387(11) . ? C59 C93 1.387(10) . ? C59 C92 1.409(10) . ? C60 C92 1.394(10) . ? C60 C94 1.405(10) . ? C61 C93 1.363(10) . ? C61 C94 1.369(11) . ? C62 C84 1.372(10) . ? C62 C83 1.407(9) . ? C63 C85 1.381(9) . ? C63 C83 1.398(9) . ? C64 C85 1.387(10) . ? C64 C84 1.392(10) . ? C65 C88 1.377(9) . ? C65 C86 1.406(10) . ? C66 C86 1.388(9) . ? C66 C87 1.392(9) . ? C67 C87 1.387(10) . ? C67 C88 1.404(10) . ? C68 C90 1.392(10) . ? C68 C89 1.397(10) . ? C69 C91 1.385(10) . ? C69 C89 1.413(9) . ? C70 C90 1.365(10) . ? C70 C91 1.409(11) . ? C72 C100 1.492(10) . ? C73 C99 1.504(9) . ? C75 C98 1.494(12) . ? C76 C97 1.496(10) . ? C78 C96 1.484(10) . ? C79 C95 1.489(11) . ? C81 C102 1.491(11) . ? C82 C101 1.495(16) . ? C84 C110 1.487(10) . ? C85 C109 1.500(10) . ? C87 C108 1.487(10) . ? C88 C107 1.510(11) . ? C90 C106 1.510(12) . ? C91 C105 1.508(10) . ? C93 C103 1.505(10) . ? C94 C104 1.497(11) . ? C111 C112 1.463(14) . ? C112 C113 1.516(14) . ? C113 C114 1.472(13) . ? C115 C116 1.464(13) . ? C116 C117 1.493(14) . ? C117 C118 1.454(17) . ? O3 C121 1.17(4) . ? O3 C119 1.13(5) . ? C121 C122 1.45(3) . ? C123 C125 1.45(4) 2_646 ? C123 C126 1.54(3) 2_646 ? C123 C123 1.57(6) 2_646 ? O4 C125 1.23(3) . ? C131 C130 1.21(3) . ? C131 O5 1.36(3) . ? C131 C130 1.81(3) 2_457 ? C131 C131 2.01(4) 2_457 ? C130 O5 1.62(3) 2_457 ? C130 C131 1.81(3) 2_457 ? O5 C130 1.62(3) 2_457 ? C125 C123 1.45(4) 2_646 ? C125 C126 1.78(5) 2_646 ? C126 C123 1.54(3) 2_646 ? C126 C126 1.60(8) 2_646 ? C126 C125 1.78(5) 2_646 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 C1 178.2(2) . . ? N1 Cr1 P2 98.23(16) . . ? C1 Cr1 P2 81.23(17) . . ? N1 Cr1 P4 92.46(15) . . ? C1 Cr1 P4 85.90(18) . . ? P2 Cr1 P4 96.66(7) . . ? N1 Cr1 P1 96.90(15) . . ? C1 Cr1 P1 84.76(17) . . ? P2 Cr1 P1 84.20(6) . . ? P4 Cr1 P1 170.38(7) . . ? N1 Cr1 P3 98.33(16) . . ? C1 Cr1 P3 82.22(17) . . ? P2 Cr1 P3 163.43(7) . . ? P4 Cr1 P3 82.91(6) . . ? P1 Cr1 P3 93.54(7) . . ? N2 Cr2 C3 179.5(2) . . ? N2 Cr2 P10 95.13(15) . . ? C3 Cr2 P10 84.45(18) . . ? N2 Cr2 P8 97.85(15) . . ? C3 Cr2 P8 82.57(18) . . ? P10 Cr2 P8 166.89(7) . . ? N2 Cr2 P9 96.18(16) . . ? C3 Cr2 P9 84.11(18) . . ? P10 Cr2 P9 83.25(7) . . ? P8 Cr2 P9 97.18(7) . . ? N2 Cr2 P12 95.92(16) . . ? C3 Cr2 P12 83.78(18) . . ? P10 Cr2 P12 94.65(7) . . ? P8 Cr2 P12 82.16(7) . . ? P9 Cr2 P12 167.86(7) . . ? C2 Si1 C42 108.0(3) . . ? C2 Si1 C43 107.5(3) . . ? C42 Si1 C43 115.1(3) . . ? C2 Si1 C41 109.0(3) . . ? C42 Si1 C41 108.6(3) . . ? C43 Si1 C41 108.6(3) . . ? C4 Si2 C45 110.1(4) . . ? C4 Si2 C46 107.0(4) . . ? C45 Si2 C46 110.2(5) . . ? C4 Si2 C44 107.6(4) . . ? C45 Si2 C44 108.2(5) . . ? C46 Si2 C44 113.7(5) . . ? C16 P1 C12 104.5(3) . . ? C16 P1 C15 101.9(3) . . ? C12 P1 C15 103.4(4) . . ? C16 P1 Cr1 120.2(2) . . ? C12 P1 Cr1 105.3(3) . . ? C15 P1 Cr1 119.5(2) . . ? C13 P2 C14 100.7(4) . . ? C13 P2 C11 104.1(3) . . ? C14 P2 C11 102.9(4) . . ? C13 P2 Cr1 121.4(2) . . ? C14 P2 Cr1 119.5(3) . . ? C11 P2 Cr1 105.8(2) . . ? C17 P3 C18 101.0(3) . . ? C17 P3 C5 103.2(3) . . ? C18 P3 C5 104.4(3) . . ? C17 P3 Cr1 120.3(3) . . ? C18 P3 Cr1 119.7(2) . . ? C5 P3 Cr1 106.2(2) . . ? C19 P4 C20 102.2(4) . . ? C19 P4 C6 104.5(3) . . ? C20 P4 C6 102.9(3) . . ? C19 P4 Cr1 121.0(3) . . ? C20 P4 Cr1 117.0(2) . . ? C6 P4 Cr1 107.2(2) . . ? C27 P8 C9 102.1(4) . . ? C27 P8 C28 100.9(4) . . ? C9 P8 C28 104.3(4) . . ? C27 P8 Cr2 121.5(3) . . ? C9 P8 Cr2 105.8(2) . . ? C28 P8 Cr2 119.8(3) . . ? C22 P9 C21 102.0(4) . . ? C22 P9 C7 102.6(4) . . ? C21 P9 C7 102.4(4) . . ? C22 P9 Cr2 118.5(3) . . ? C21 P9 Cr2 123.0(3) . . ? C7 P9 Cr2 105.5(3) . . ? C8 P10 C23 104.3(4) . . ? C8 P10 C24 101.9(3) . . ? C23 P10 C24 101.4(3) . . ? C8 P10 Cr2 107.2(3) . . ? C23 P10 Cr2 118.8(2) . . ? C24 P10 Cr2 120.9(3) . . ? C26 P12 C25 102.2(3) . . ? C26 P12 C10 105.0(3) . . ? C25 P12 C10 101.9(3) . . ? C26 P12 Cr2 118.2(3) . . ? C25 P12 Cr2 120.6(3) . . ? C10 P12 Cr2 106.9(2) . . ? N2 N1 Cr1 177.5(4) . . ? N1 N2 Cr2 179.2(5) . . ? C114 O1 C111 107.3(7) . . ? C118 O2 C115 106.9(7) . . ? C119 C120 C122 99.8(18) . . ? C80 B1 C74 113.8(5) . . ? C80 B1 C77 103.8(5) . . ? C74 B1 C77 111.5(6) . . ? C80 B1 C71 113.7(6) . . ? C74 B1 C71 103.0(5) . . ? C77 B1 C71 111.4(5) . . ? C83 B2 C92 112.3(5) . . ? C83 B2 C89 103.5(5) . . ? C92 B2 C89 112.6(5) . . ? C83 B2 C86 113.7(5) . . ? C92 B2 C86 104.2(5) . . ? C89 B2 C86 110.8(5) . . ? C2 C1 Cr1 178.0(6) . . ? C1 C2 Si1 177.3(6) . . ? C4 C3 Cr2 178.6(6) . . ? C3 C4 Si2 179.1(6) . . ? C6 C5 P3 109.7(4) . . ? C5 C6 P4 109.6(5) . . ? C8 C7 P9 109.9(5) . . ? C7 C8 P10 110.6(5) . . ? C10 C9 P8 109.7(5) . . ? C9 C10 P12 110.4(5) . . ? C12 C11 P2 109.3(5) . . ? C11 C12 P1 111.4(5) . . ? C34 C41 C33 110.1(7) . . ? C34 C41 Si1 112.5(5) . . ? C33 C41 Si1 112.9(5) . . ? C30 C42 C29 109.5(6) . . ? C30 C42 Si1 114.5(5) . . ? C29 C42 Si1 114.1(6) . . ? C31 C43 C32 108.9(7) . . ? C31 C43 Si1 114.4(5) . . ? C32 C43 Si1 114.8(5) . . ? C37A C44 C37 67.9(13) . . ? C37A C44 C38 107.1(14) . . ? C37 C44 C38 116.3(10) . . ? C37A C44 Si2 129.6(13) . . ? C37 C44 Si2 115.1(9) . . ? C38 C44 Si2 113.6(7) . . ? C40 C45 C39 111.3(11) . . ? C40 C45 Si2 111.7(8) . . ? C39 C45 Si2 112.7(9) . . ? C35 C46 C36 110.1(9) . . ? C35 C46 Si2 115.4(7) . . ? C36 C46 Si2 112.9(8) . . ? C79 C47 C77 123.1(6) . . ? C78 C48 C79 118.1(6) . . ? C78 C49 C77 122.5(7) . . ? C82 C50 C80 122.3(7) . . ? C81 C51 C80 122.4(7) . . ? C81 C52 C82 117.6(7) . . ? C71 C53 C72 122.0(6) . . ? C73 C54 C71 122.2(6) . . ? C73 C55 C72 117.5(6) . . ? C76 C56 C74 122.1(7) . . ? C74 C57 C75 123.1(7) . . ? C76 C58 C75 117.5(7) . . ? C93 C59 C92 122.5(7) . . ? C92 C60 C94 121.5(7) . . ? C93 C61 C94 118.8(7) . . ? C84 C62 C83 122.4(6) . . ? C85 C63 C83 123.4(6) . . ? C85 C64 C84 116.7(6) . . ? C88 C65 C86 122.1(6) . . ? C86 C66 C87 122.3(6) . . ? C87 C67 C88 116.9(6) . . ? C90 C68 C89 123.3(6) . . ? C91 C69 C89 121.4(6) . . ? C90 C70 C91 117.8(6) . . ? C53 C71 C54 115.8(6) . . ? C53 C71 B1 124.1(6) . . ? C54 C71 B1 119.7(6) . . ? C55 C72 C53 121.2(6) . . ? C55 C72 C100 117.5(6) . . ? C53 C72 C100 121.3(6) . . ? C55 C73 C54 121.2(6) . . ? C55 C73 C99 121.0(6) . . ? C54 C73 C99 117.7(6) . . ? C57 C74 C56 115.4(6) . . ? C57 C74 B1 121.4(6) . . ? C56 C74 B1 122.8(6) . . ? C58 C75 C57 120.8(7) . . ? C58 C75 C98 119.6(7) . . ? C57 C75 C98 119.5(7) . . ? C58 C76 C56 121.0(7) . . ? C58 C76 C97 119.4(7) . . ? C56 C76 C97 119.6(7) . . ? C49 C77 C47 115.3(6) . . ? C49 C77 B1 122.8(6) . . ? C47 C77 B1 121.7(6) . . ? C49 C78 C48 120.8(6) . . ? C49 C78 C96 118.7(7) . . ? C48 C78 C96 120.5(6) . . ? C47 C79 C48 120.2(7) . . ? C47 C79 C95 119.2(7) . . ? C48 C79 C95 120.5(7) . . ? C50 C80 C51 115.0(6) . . ? C50 C80 B1 121.7(6) . . ? C51 C80 B1 122.8(6) . . ? C52 C81 C51 121.2(7) . . ? C52 C81 C102 118.5(7) . . ? C51 C81 C102 120.3(7) . . ? C50 C82 C52 121.6(7) . . ? C50 C82 C101 119.8(8) . . ? C52 C82 C101 118.6(8) . . ? C63 C83 C62 114.4(6) . . ? C63 C83 B2 122.7(6) . . ? C62 C83 B2 122.6(6) . . ? C62 C84 C64 122.0(6) . . ? C62 C84 C110 119.5(7) . . ? C64 C84 C110 118.4(6) . . ? C63 C85 C64 121.0(6) . . ? C63 C85 C109 119.3(6) . . ? C64 C85 C109 119.6(6) . . ? C66 C86 C65 116.0(6) . . ? C66 C86 B2 122.9(6) . . ? C65 C86 B2 120.9(6) . . ? C67 C87 C66 121.4(6) . . ? C67 C87 C108 119.5(6) . . ? C66 C87 C108 119.1(6) . . ? C65 C88 C67 121.3(6) . . ? C65 C88 C107 120.6(6) . . ? C67 C88 C107 118.1(6) . . ? C68 C89 C69 115.3(6) . . ? C68 C89 B2 122.9(6) . . ? C69 C89 B2 121.4(6) . . ? C70 C90 C68 120.7(7) . . ? C70 C90 C106 120.2(7) . . ? C68 C90 C106 119.0(7) . . ? C69 C91 C70 121.4(6) . . ? C69 C91 C105 118.6(7) . . ? C70 C91 C105 120.0(6) . . ? C60 C92 C59 115.3(6) . . ? C60 C92 B2 122.6(6) . . ? C59 C92 B2 121.9(6) . . ? C61 C93 C59 120.7(7) . . ? C61 C93 C103 119.6(6) . . ? C59 C93 C103 119.7(6) . . ? C61 C94 C60 121.1(7) . . ? C61 C94 C104 118.7(7) . . ? C60 C94 C104 120.2(7) . . ? F10 C95 F12 110.4(8) . . ? F10 C95 F11 106.4(8) . . ? F12 C95 F11 99.3(8) . . ? F10 C95 C79 114.4(8) . . ? F12 C95 C79 113.1(7) . . ? F11 C95 C79 112.0(7) . . ? F9 C96 F7 109.3(7) . . ? F9 C96 F8 104.7(7) . . ? F7 C96 F8 103.2(6) . . ? F9 C96 C78 114.1(7) . . ? F7 C96 C78 112.2(7) . . ? F8 C96 C78 112.5(6) . . ? F19 C97 F20 108.5(7) . . ? F19 C97 F21 105.2(8) . . ? F20 C97 F21 104.1(6) . . ? F19 C97 C76 113.3(6) . . ? F20 C97 C76 112.9(7) . . ? F21 C97 C76 112.1(7) . . ? F24 C98 F22 109.2(8) . . ? F24 C98 F23 104.7(8) . . ? F22 C98 F23 104.3(8) . . ? F24 C98 C75 112.6(8) . . ? F22 C98 C75 114.4(8) . . ? F23 C98 C75 110.9(8) . . ? F13 C99 F14 106.5(6) . . ? F13 C99 F15 105.1(6) . . ? F14 C99 F15 106.8(6) . . ? F13 C99 C73 112.0(6) . . ? F14 C99 C73 113.9(6) . . ? F15 C99 C73 112.0(6) . . ? F17 C100 F18 106.2(6) . . ? F17 C100 F16 105.9(6) . . ? F18 C100 F16 104.6(6) . . ? F17 C100 C72 112.9(6) . . ? F18 C100 C72 112.8(6) . . ? F16 C100 C72 113.7(6) . . ? F1 C101 F3 106.6(16) . . ? F1 C101 F2 109.0(15) . . ? F3 C101 F2 103.0(11) . . ? F1 C101 C82 114.6(11) . . ? F3 C101 C82 112.0(11) . . ? F2 C101 C82 111.0(11) . . ? F6 C102 F5 106.8(8) . . ? F6 C102 F4 106.9(9) . . ? F5 C102 F4 102.1(9) . . ? F6 C102 C81 112.9(8) . . ? F5 C102 C81 115.5(7) . . ? F4 C102 C81 111.7(8) . . ? F34 C103 F36 106.4(7) . . ? F34 C103 F35 105.4(6) . . ? F36 C103 F35 105.9(6) . . ? F34 C103 C93 112.8(6) . . ? F36 C103 C93 113.5(6) . . ? F35 C103 C93 112.3(7) . . ? F31 C104 F32 109.1(7) . . ? F31 C104 F33 104.4(7) . . ? F32 C104 F33 103.9(7) . . ? F31 C104 C94 114.5(7) . . ? F32 C104 C94 112.3(7) . . ? F33 C104 C94 111.9(7) . . ? F29 C105 F28 108.1(7) . . ? F29 C105 F30 105.4(7) . . ? F28 C105 F30 105.4(7) . . ? F29 C105 C91 113.6(6) . . ? F28 C105 C91 111.8(7) . . ? F30 C105 C91 111.9(6) . . ? F27 C106 F25 111.0(10) . . ? F27 C106 F26 101.2(12) . . ? F25 C106 F26 104.0(8) . . ? F27 C106 C90 115.2(8) . . ? F25 C106 C90 114.0(9) . . ? F26 C106 C90 110.0(8) . . ? F43 C107 F45 109.7(7) . . ? F43 C107 F44 104.6(8) . . ? F45 C107 F44 103.8(8) . . ? F43 C107 C88 114.2(7) . . ? F45 C107 C88 112.5(7) . . ? F44 C107 C88 111.2(7) . . ? F46 C108 F48 110.0(6) . . ? F46 C108 F47 103.4(7) . . ? F48 C108 F47 102.1(6) . . ? F46 C108 C87 114.7(6) . . ? F48 C108 C87 113.1(6) . . ? F47 C108 C87 112.4(6) . . ? F42 C109 F40 105.8(6) . . ? F42 C109 F41 104.9(6) . . ? F40 C109 F41 107.2(6) . . ? F42 C109 C85 111.7(6) . . ? F40 C109 C85 113.8(6) . . ? F41 C109 C85 112.7(6) . . ? F38 C110 F39 111.4(9) . . ? F38 C110 F37 102.8(9) . . ? F39 C110 F37 100.3(8) . . ? F38 C110 C84 115.7(7) . . ? F39 C110 C84 115.6(7) . . ? F37 C110 C84 109.1(7) . . ? O1 C111 C112 106.7(7) . . ? C111 C112 C113 106.5(8) . . ? C114 C113 C112 104.0(8) . . ? O1 C114 C113 107.7(7) . . ? O2 C115 C116 109.8(7) . . ? C115 C116 C117 104.6(8) . . ? C118 C117 C116 105.1(9) . . ? O2 C118 C117 110.8(11) . . ? C121 O3 C119 124(5) . . ? O3 C121 C122 108(3) . . ? C121 C122 C120 98.6(17) . . ? C125 C123 C126 109(3) 2_646 2_646 ? C125 C123 C123 122(3) 2_646 2_646 ? C126 C123 C123 13.0(19) 2_646 2_646 ? C130 C131 O5 142(2) . . ? C130 C131 C130 98.8(18) . 2_457 ? O5 C131 C130 59.6(16) . 2_457 ? C130 C131 C131 62.5(16) . 2_457 ? O5 C131 C131 91.1(19) . 2_457 ? C130 C131 C131 36.3(10) 2_457 2_457 ? C131 C130 O5 120(2) . 2_457 ? C131 C130 C131 81.2(18) . 2_457 ? O5 C130 C131 46.5(13) 2_457 2_457 ? C131 O5 C130 74.0(18) . 2_457 ? O4 C125 C123 103(2) . 2_646 ? O4 C125 C126 107(2) . 2_646 ? C123 C125 C126 4(2) 2_646 2_646 ? O3 C119 C120 109(4) . . ? C123 C126 C126 13(2) 2_646 2_646 ? C123 C126 C125 105(2) 2_646 2_646 ? C126 C126 C125 92(3) 2_646 2_646 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.822 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.153 #===END