# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Eugenio Coronado' 'Jose R. Galan-Mascaros' 'Carlos Gimenez-Saiz' 'Carlos J. Gomez-Garcia' 'Eugenia Martinez-Ferrero' 'Manuel Almeida' 'Elsa B. Lopes' 'Silvia C. Capelli' 'Rosa Llusar' 'Jose-Ramon Galan-Mascaros' 'Elsa B. Lopes' _publ_contact_author_name 'Prof Eugenio Coronado' _publ_contact_author_address ; Instituto de Ciencia Molecular Universidad de Valencia Dr. Moliner, 50 Burjasot 46100 SPAIN ; _publ_contact_author_email EUGENIO.CORONADO@UV.ES _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; New conducting radical salts based upon Keggin-type polyoxometalates and perylene ; #========================================================================= data_compound1 _database_code_depnum_ccdc_archive 'CCDC 232004' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C121 H74 Cl2 Mo12 O40 P' _chemical_formula_weight 3420.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.059(3) _cell_length_b 14.270(3) _cell_length_c 27.053(5) _cell_angle_alpha 88.27(3) _cell_angle_beta 86.65(3) _cell_angle_gamma 86.02(3) _cell_volume 5403.2(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5327 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 30.66 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3346 _exptl_absorpt_coefficient_mu 1.499 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7000(2) _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type 'MAR345 image plate' _diffrn_measurement_method '179 frames at 2deg rotation width' _diffrn_detector_area_resol_mean 6.6666666667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71471 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.28 _reflns_number_total 24856 _reflns_number_gt 20438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MAR345 software' _computing_cell_refinement 'CrysAlisRED 1.167 (Oxford-diffraction 2000)' _computing_data_reduction 'CrysAlisRED 1.167 (Oxford-diffraction 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+61.2681P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00142(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 24856 _refine_ls_number_parameters 1591 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2164 _refine_ls_wR_factor_gt 0.1822 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.089 _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 P1 P 0.48994(12) 0.54378(10) 0.24861(6) 0.021 Uani 1 1 d D . . Mo1 Mo 0.29655(5) 0.43713(5) 0.31297(3) 0.034 Uani 1 1 d . . . Mo2 Mo 0.48511(5) 0.49700(4) 0.37914(2) 0.032 Uani 1 1 d . . . Mo3 Mo 0.32774(5) 0.66988(4) 0.33280(3) 0.034 Uani 1 1 d . . . Mo4 Mo 0.30590(5) 0.69361(4) 0.19800(3) 0.033 Uani 1 1 d . . . Mo5 Mo 0.31332(5) 0.45587(5) 0.17647(3) 0.032 Uani 1 1 d . . . Mo6 Mo 0.48373(5) 0.29616(4) 0.24205(3) 0.030 Uani 1 1 d . . . Mo7 Mo 0.67356(5) 0.38651(4) 0.29503(3) 0.031 Uani 1 1 d . . . Mo8 Mo 0.66564(5) 0.63969(4) 0.31652(3) 0.032 Uani 1 1 d . . . Mo9 Mo 0.50771(5) 0.79017(4) 0.25492(3) 0.033 Uani 1 1 d . . . Mo10 Mo 0.68393(5) 0.65735(4) 0.18877(3) 0.032 Uani 1 1 d . . . Mo11 Mo 0.48294(6) 0.59092(5) 0.11894(3) 0.036 Uani 1 1 d . . . Mo12 Mo 0.65260(5) 0.40804(4) 0.16884(3) 0.033 Uani 1 1 d . . . O1 O 0.2108(5) 0.3722(4) 0.3373(3) 0.045 Uani 1 1 d . A . O2 O 0.5031(6) 0.4795(5) 0.4393(2) 0.051 Uani 1 1 d . A . O3 O 0.2477(5) 0.7434(5) 0.3630(3) 0.050 Uani 1 1 d . A . O4 O 0.2528(4) 0.5564(4) 0.3336(3) 0.045 Uani 1 1 d . A . O5 O 0.3796(5) 0.4315(4) 0.3720(2) 0.045 Uani 1 1 d . A . O6 O 0.3939(5) 0.6124(4) 0.3836(2) 0.045 Uani 1 1 d . A . O7 O 0.2825(5) 0.6819(4) 0.2641(2) 0.043 Uani 1 1 d . A . O8 O 0.2714(5) 0.4539(4) 0.2483(2) 0.043 Uani 1 1 d . A . O9 O 0.3956(4) 0.3395(4) 0.2897(2) 0.038 Uani 1 1 d . A . O10 O 0.5725(5) 0.4151(4) 0.3486(2) 0.043 Uani 1 1 d . A . O11 O 0.5751(5) 0.5940(4) 0.3594(2) 0.041 Uani 1 1 d . A . O12 O 0.4207(5) 0.7450(4) 0.3098(2) 0.043 Uani 1 1 d . A . O13 O 0.4137(5) 0.7673(4) 0.2140(2) 0.042 Uani 1 1 d . A . O14 O 0.2262(5) 0.7769(4) 0.1797(3) 0.050 Uani 1 1 d . A . O15 O 0.2502(5) 0.5862(4) 0.1812(2) 0.041 Uani 1 1 d . A . O16 O 0.2273(5) 0.4026(5) 0.1515(3) 0.050 Uani 1 1 d . A . O17 O 0.3977(4) 0.3596(4) 0.1938(2) 0.040 Uani 1 1 d . A . O18 O 0.4635(5) 0.1826(4) 0.2374(3) 0.050 Uani 1 1 d . A . O19 O 0.5875(5) 0.2865(4) 0.2822(2) 0.042 Uani 1 1 d . A . O20 O 0.7554(5) 0.3231(4) 0.3261(3) 0.046 Uani 1 1 d . A . O21 O 0.7038(4) 0.5064(4) 0.3018(2) 0.038 Uani 1 1 d . A . O22 O 0.7513(5) 0.6664(4) 0.3526(2) 0.044 Uani 1 1 d . A . O23 O 0.6031(5) 0.7569(4) 0.3058(2) 0.043 Uani 1 1 d . A . O24 O 0.4976(5) 0.9068(4) 0.2615(3) 0.047 Uani 1 1 d . A . O25 O 0.6078(5) 0.7763(4) 0.2081(2) 0.044 Uani 1 1 d . A . O26 O 0.3842(5) 0.6813(4) 0.1337(2) 0.045 Uani 1 1 d . A . O27 O 0.3823(5) 0.4975(4) 0.1212(2) 0.044 Uani 1 1 d . A . O28 O 0.5803(5) 0.3064(4) 0.1849(2) 0.043 Uani 1 1 d . A . O29 O 0.7223(5) 0.3730(4) 0.2307(2) 0.043 Uani 1 1 d . A . O30 O 0.7342(4) 0.6590(4) 0.2500(2) 0.041 Uani 1 1 d . A . O31 O 0.5776(5) 0.6529(4) 0.1427(2) 0.046 Uani 1 1 d . A . O32 O 0.5643(5) 0.4738(4) 0.1320(3) 0.047 Uani 1 1 d . A . O33 O 0.7030(5) 0.5315(4) 0.1805(2) 0.041 Uani 1 1 d . A . O34 O 0.7689(5) 0.7023(5) 0.1514(3) 0.052 Uani 1 1 d . A . O35 O 0.4996(5) 0.6047(5) 0.0573(2) 0.049 Uani 1 1 d . A . O36 O 0.7331(5) 0.3610(4) 0.1275(3) 0.048 Uani 1 1 d . A . O37A O 0.4275(4) 0.5390(4) 0.29690(19) 0.025 Uiso 0.85 1 d PD A 1 O38A O 0.4254(4) 0.5625(4) 0.2049(2) 0.026 Uiso 0.85 1 d PD A 1 O39A O 0.5486(4) 0.4500(3) 0.2419(2) 0.024 Uiso 0.85 1 d PD A 1 O40A O 0.5578(4) 0.6233(3) 0.2514(2) 0.021 Uiso 0.85 1 d PD A 1 O37B O 0.4234(19) 0.4643(16) 0.2420(12) 0.026 Uiso 0.15 1 d PD A 2 O38B O 0.430(3) 0.6368(16) 0.2566(15) 0.043 Uiso 0.15 1 d PD A 2 O39B O 0.560(2) 0.524(3) 0.2898(10) 0.036 Uiso 0.15 1 d PD A 2 O40B O 0.556(3) 0.551(3) 0.2016(10) 0.050 Uiso 0.15 1 d PD A 2 C1A C 0.8797(6) 0.8885(5) 0.5141(3) 0.031 Uani 1 1 d . . . C2A C 0.8654(6) 0.9102(5) 0.4644(3) 0.033 Uani 1 1 d . . . C3A C 0.8602(6) 1.0075(5) 0.4465(3) 0.034 Uani 1 1 d . . . C4A C 0.8729(5) 1.0785(5) 0.4802(3) 0.030 Uani 1 1 d . . . C5A C 0.8880(6) 1.0580(5) 0.5307(3) 0.032 Uani 1 1 d . . . C6A C 0.8908(6) 0.9603(5) 0.5489(3) 0.031 Uani 1 1 d . . . C7A C 0.9081(7) 0.9329(6) 0.5981(3) 0.043 Uani 1 1 d . . . H7A H 0.9175 0.9786 0.6208 0.052 Uiso 1 1 calc R . . C8A C 0.9113(8) 0.8402(7) 0.6134(3) 0.048 Uani 1 1 d . . . H8A H 0.9221 0.8243 0.6463 0.058 Uiso 1 1 calc R . . C9A C 0.8989(7) 0.7714(6) 0.5813(4) 0.047 Uani 1 1 d . . . H9A H 0.9013 0.7090 0.5925 0.057 Uiso 1 1 calc R . . C10A C 0.8825(7) 0.7935(5) 0.5316(3) 0.039 Uani 1 1 d . . . C11A C 0.8718(8) 0.7228(6) 0.4966(4) 0.051 Uani 1 1 d . . . H11A H 0.8753 0.6601 0.5073 0.062 Uiso 1 1 calc R . . C12A C 0.8568(8) 0.7430(7) 0.4492(4) 0.053 Uani 1 1 d . . . H12A H 0.8494 0.6950 0.4276 0.064 Uiso 1 1 calc R . . C13A C 0.8524(7) 0.8367(6) 0.4320(3) 0.045 Uani 1 1 d . . . H13A H 0.8409 0.8507 0.3990 0.054 Uiso 1 1 calc R . . C14A C 0.8414(7) 1.0328(6) 0.3974(3) 0.042 Uani 1 1 d . . . H14A H 0.8318 0.9864 0.3751 0.050 Uiso 1 1 calc R . . C15A C 0.8370(7) 1.1263(7) 0.3814(4) 0.051 Uani 1 1 d . . . H15A H 0.8238 1.1423 0.3489 0.061 Uiso 1 1 calc R . . C16A C 0.8523(8) 1.1954(6) 0.4139(4) 0.051 Uani 1 1 d . . . H16A H 0.8518 1.2576 0.4026 0.062 Uiso 1 1 calc R . . C17A C 0.8685(6) 1.1740(5) 0.4634(3) 0.037 Uani 1 1 d . . . C18A C 0.8808(7) 1.2452(6) 0.4970(4) 0.047 Uani 1 1 d . . . H18A H 0.8787 1.3076 0.4859 0.057 Uiso 1 1 calc R . . C19A C 0.8957(7) 1.2240(6) 0.5454(4) 0.044 Uani 1 1 d . . . H19A H 0.9034 1.2719 0.5671 0.053 Uiso 1 1 calc R . . C20A C 0.8997(7) 1.1302(6) 0.5628(3) 0.043 Uani 1 1 d . . . H20A H 0.9103 1.1162 0.5959 0.052 Uiso 1 1 calc R . . C1B C 0.6291(6) 0.8885(6) 0.5109(3) 0.038 Uani 1 1 d . . . C2B C 0.6129(6) 0.8975(6) 0.4599(3) 0.040 Uani 1 1 d . . . C3B C 0.6073(7) 0.9906(6) 0.4365(4) 0.045 Uani 1 1 d . . . C4B C 0.6166(7) 1.0703(6) 0.4653(4) 0.044 Uani 1 1 d . . . C5B C 0.6341(6) 1.0603(6) 0.5168(4) 0.040 Uani 1 1 d . . . C6B C 0.6409(6) 0.9676(6) 0.5395(3) 0.038 Uani 1 1 d . . . C7B C 0.6585(8) 0.9536(7) 0.5899(4) 0.051 Uani 1 1 d . . . H7B H 0.6660 1.0053 0.6091 0.061 Uiso 1 1 calc R . . C8B C 0.6648(9) 0.8646(8) 0.6116(4) 0.060 Uani 1 1 d . . . H8B H 0.6794 0.8569 0.6447 0.072 Uiso 1 1 calc R . . C9B C 0.6499(7) 0.7877(7) 0.5849(4) 0.051 Uani 1 1 d . . . H9B H 0.6491 0.7287 0.6005 0.061 Uiso 1 1 calc R . . C10B C 0.6358(7) 0.7977(6) 0.5338(4) 0.044 Uani 1 1 d . . . C11B C 0.6232(7) 0.7188(7) 0.5062(4) 0.052 Uani 1 1 d . . . H11B H 0.6249 0.6595 0.5215 0.063 Uiso 1 1 calc R . . C12B C 0.6082(8) 0.7285(7) 0.4569(5) 0.062 Uani 1 1 d . . . H12B H 0.6023 0.6752 0.4386 0.074 Uiso 1 1 calc R . . C13B C 0.6018(8) 0.8167(7) 0.4331(4) 0.054 Uani 1 1 d . . . H13B H 0.5901 0.8219 0.3996 0.064 Uiso 1 1 calc R . . C14B C 0.5902(8) 1.0051(8) 0.3866(4) 0.056 Uani 1 1 d . . . H14B H 0.5833 0.9535 0.3673 0.067 Uiso 1 1 calc R . . C15B C 0.5832(9) 1.0945(9) 0.3649(5) 0.068 Uani 1 1 d . . . H15B H 0.5729 1.1019 0.3313 0.081 Uiso 1 1 calc R . . C16B C 0.5913(9) 1.1718(8) 0.3926(5) 0.069 Uani 1 1 d . . . H16B H 0.5856 1.2313 0.3777 0.083 Uiso 1 1 calc R . . C17B C 0.6080(8) 1.1628(7) 0.4431(4) 0.055 Uani 1 1 d . . . C18B C 0.6186(9) 1.2397(7) 0.4722(6) 0.070 Uani 1 1 d . . . H18B H 0.6132 1.2996 0.4577 0.083 Uiso 1 1 calc R . . C19B C 0.6365(10) 1.2304(7) 0.5208(5) 0.069 Uani 1 1 d . . . H19B H 0.6446 1.2831 0.5391 0.083 Uiso 1 1 calc R . . C20B C 0.6425(8) 1.1414(7) 0.5429(5) 0.055 Uani 1 1 d . . . H20B H 0.6524 1.1358 0.5766 0.066 Uiso 1 1 calc R . . C1C C 0.3771(6) 0.9590(6) -0.0369(3) 0.040 Uani 1 1 d . . . C2C C 0.3697(7) 1.0595(6) -0.0414(4) 0.046 Uani 1 1 d . . . C3C C 0.3665(7) 1.1140(7) 0.0032(4) 0.049 Uani 1 1 d . . . C4C C 0.3707(7) 1.0675(7) 0.0500(4) 0.046 Uani 1 1 d . . . C5C C 0.3775(6) 0.9682(7) 0.0545(4) 0.044 Uani 1 1 d . . . C6C C 0.3818(7) 0.9132(6) 0.0099(3) 0.041 Uani 1 1 d . . . C7C C 0.3901(11) 0.8151(7) 0.0118(5) 0.069 Uani 1 1 d . . . H7C H 0.3923 0.7836 0.0424 0.083 Uiso 1 1 calc R . . C8C C 0.3950(12) 0.7645(8) -0.0304(5) 0.076 Uani 1 1 d . . . H8C H 0.4012 0.6993 -0.0281 0.091 Uiso 1 1 calc R . . C9C C 0.3909(10) 0.8079(8) -0.0758(5) 0.068 Uani 1 1 d . . . H9C H 0.3942 0.7719 -0.1040 0.081 Uiso 1 1 calc R . . C10C C 0.3819(7) 0.9050(7) -0.0805(4) 0.047 Uani 1 1 d . . . C11C C 0.3764(9) 0.9508(9) -0.1272(4) 0.066 Uani 1 1 d . . . H11C H 0.3788 0.9159 -0.1558 0.079 Uiso 1 1 calc R . . C12C C 0.3678(12) 1.0455(10) -0.1302(4) 0.082 Uani 1 1 d . . . H12C H 0.3651 1.0748 -0.1613 0.099 Uiso 1 1 calc R . . C13C C 0.3630(10) 1.0999(9) -0.0895(4) 0.067 Uani 1 1 d . . . H13C H 0.3550 1.1649 -0.0934 0.081 Uiso 1 1 calc R . . C14C C 0.3589(12) 1.2118(8) 0.0022(6) 0.086 Uani 1 1 d . . . H14C H 0.3554 1.2434 -0.0283 0.103 Uiso 1 1 calc R . . C15C C 0.3563(14) 1.2632(10) 0.0438(7) 0.103 Uani 1 1 d . . . H15C H 0.3508 1.3284 0.0414 0.124 Uiso 1 1 calc R . . C16C C 0.3616(11) 1.2190(10) 0.0891(6) 0.084 Uani 1 1 d . . . H16C H 0.3615 1.2545 0.1174 0.100 Uiso 1 1 calc R . . C17C C 0.3672(8) 1.1206(8) 0.0936(4) 0.056 Uani 1 1 d . . . C18C C 0.3702(9) 1.0721(10) 0.1405(5) 0.070 Uani 1 1 d . . . H18C H 0.3666 1.1064 0.1693 0.084 Uiso 1 1 calc R . . C19C C 0.3780(12) 0.9790(11) 0.1436(5) 0.083 Uani 1 1 d . . . H19C H 0.3801 0.9492 0.1746 0.099 Uiso 1 1 calc R . . C20C C 0.3829(11) 0.9258(9) 0.1019(4) 0.072 Uani 1 1 d . . . H20C H 0.3900 0.8607 0.1051 0.087 Uiso 1 1 calc R . . C1D C 0.1260(6) 0.9866(6) -0.0450(3) 0.039 Uani 1 1 d . . . C2D C 0.1185(6) 1.0861(6) -0.0447(3) 0.040 Uani 1 1 d . . . C3D C 0.1155(8) 1.1323(7) 0.0025(4) 0.047 Uani 1 1 d . . . C4D C 0.1193(6) 1.0780(7) 0.0473(3) 0.042 Uani 1 1 d . . . C5D C 0.1264(7) 0.9784(7) 0.0468(4) 0.047 Uani 1 1 d . . . C6D C 0.1275(7) 0.9323(7) -0.0007(4) 0.048 Uani 1 1 d . . . C7D C 0.1366(10) 0.8346(8) -0.0040(4) 0.070 Uani 1 1 d . . . H7D H 0.1403 0.7982 0.0250 0.084 Uiso 1 1 calc R . . C8D C 0.1404(11) 0.7901(8) -0.0486(5) 0.074 Uani 1 1 d . . . H8D H 0.1468 0.7249 -0.0493 0.089 Uiso 1 1 calc R . . C9D C 0.1346(9) 0.8418(8) -0.0919(5) 0.065 Uani 1 1 d . . . H9D H 0.1355 0.8114 -0.1219 0.078 Uiso 1 1 calc R . . C10D C 0.1273(7) 0.9420(7) -0.0914(4) 0.045 Uani 1 1 d . . . C11D C 0.1236(9) 0.9969(8) -0.1359(4) 0.061 Uani 1 1 d . . . H11D H 0.1249 0.9673 -0.1661 0.073 Uiso 1 1 calc R . . C12D C 0.1182(11) 1.0916(9) -0.1349(4) 0.074 Uani 1 1 d . . . H12D H 0.1163 1.1270 -0.1643 0.089 Uiso 1 1 calc R . . C13D C 0.1154(10) 1.1358(8) -0.0899(4) 0.065 Uani 1 1 d . . . H13D H 0.1113 1.2011 -0.0898 0.079 Uiso 1 1 calc R . . C14D C 0.1098(12) 1.2308(8) 0.0054(4) 0.076 Uani 1 1 d . . . H14D H 0.1062 1.2671 -0.0237 0.091 Uiso 1 1 calc R . . C15D C 0.1094(13) 1.2749(9) 0.0500(5) 0.084 Uani 1 1 d . . . H15D H 0.1070 1.3401 0.0507 0.101 Uiso 1 1 calc R . . C16D C 0.1127(10) 1.2225(9) 0.0940(5) 0.070 Uani 1 1 d . . . H16D H 0.1104 1.2526 0.1241 0.083 Uiso 1 1 calc R . . C17D C 0.1195(7) 1.1236(8) 0.0930(4) 0.049 Uani 1 1 d . . . C18D C 0.1224(10) 1.0701(9) 0.1371(4) 0.070 Uani 1 1 d . . . H18D H 0.1201 1.0999 0.1673 0.084 Uiso 1 1 calc R . . C19D C 0.1285(11) 0.9758(10) 0.1361(4) 0.077 Uani 1 1 d . . . H19D H 0.1311 0.9409 0.1656 0.093 Uiso 1 1 calc R . . C20D C 0.1310(10) 0.9299(8) 0.0916(4) 0.068 Uani 1 1 d . . . H20D H 0.1360 0.8646 0.0919 0.081 Uiso 1 1 calc R . . C1E C 1.0974(6) 1.0695(6) 0.2651(3) 0.035 Uani 1 1 d . . . C2E C 1.0849(6) 0.9731(5) 0.2759(3) 0.037 Uani 1 1 d . . . C3E C 0.9880(7) 0.9395(6) 0.2776(3) 0.041 Uani 1 1 d . . . C4E C 0.9088(6) 1.0021(6) 0.2664(3) 0.040 Uani 1 1 d . . . C5E C 0.9219(7) 1.1000(6) 0.2547(3) 0.040 Uani 1 1 d . . . C6E C 1.0164(7) 1.1333(5) 0.2561(3) 0.040 Uani 1 1 d . . . C7E C 1.0333(9) 1.2277(7) 0.2475(4) 0.058 Uani 1 1 d . . . H7E H 0.9824 1.2711 0.2418 0.069 Uiso 1 1 calc R . . C8E C 1.1242(9) 1.2574(7) 0.2472(4) 0.063 Uani 1 1 d . . . H8E H 1.1332 1.3209 0.2418 0.075 Uiso 1 1 calc R . . C9E C 1.2017(8) 1.1969(8) 0.2545(5) 0.060 Uani 1 1 d . . . H9E H 1.2625 1.2191 0.2528 0.072 Uiso 1 1 calc R . . C10E C 1.1900(7) 1.1016(6) 0.2644(4) 0.046 Uani 1 1 d . . . C11E C 1.2686(7) 1.0374(9) 0.2728(4) 0.056 Uani 1 1 d . . . H11E H 1.3301 1.0579 0.2708 0.067 Uiso 1 1 calc R . . C12E C 1.2546(8) 0.9457(8) 0.2839(5) 0.065 Uani 1 1 d . . . H12E H 1.3064 0.9045 0.2912 0.078 Uiso 1 1 calc R . . C13E C 1.1630(8) 0.9125(7) 0.2845(4) 0.052 Uani 1 1 d . . . H13E H 1.1550 0.8491 0.2908 0.063 Uiso 1 1 calc R . . C14E C 0.9727(9) 0.8461(7) 0.2893(5) 0.065 Uani 1 1 d . . . H14E H 1.0239 0.8049 0.2975 0.078 Uiso 1 1 calc R . . C15E C 0.8815(10) 0.8133(9) 0.2891(6) 0.078 Uani 1 1 d . . . H15E H 0.8723 0.7505 0.2969 0.094 Uiso 1 1 calc R . . C16E C 0.8052(9) 0.8737(9) 0.2772(5) 0.068 Uani 1 1 d . . . H16E H 0.7449 0.8507 0.2768 0.082 Uiso 1 1 calc R . . C17E C 0.8157(8) 0.9683(7) 0.2659(4) 0.051 Uani 1 1 d . . . C18E C 0.7381(8) 1.0322(9) 0.2543(5) 0.064 Uani 1 1 d . . . H18E H 0.6767 1.0116 0.2547 0.077 Uiso 1 1 calc R . . C19E C 0.7526(8) 1.1229(8) 0.2428(4) 0.059 Uani 1 1 d . . . H19E H 0.7012 1.1633 0.2338 0.071 Uiso 1 1 calc R . . C20E C 0.8426(7) 1.1574(8) 0.2439(4) 0.054 Uani 1 1 d . . . H20E H 0.8493 1.2210 0.2371 0.065 Uiso 1 1 calc R . . C1F C 1.0909(12) 0.6393(8) 0.1000(5) 0.080 Uani 1 1 d . . . H1F H 1.0918 0.6747 0.1283 0.096 Uiso 1 1 calc R . . C2F C 1.1758(13) 0.6169(10) 0.0732(6) 0.088 Uani 1 1 d . . . H2F H 1.2330 0.6380 0.0827 0.106 Uiso 1 1 calc R . . C3F C 1.1739(10) 0.5634(9) 0.0323(5) 0.071 Uani 1 1 d . . . C4F C 1.0867(8) 0.5320(7) 0.0165(4) 0.051 Uani 1 1 d . . . C5F C 0.9992(9) 0.5547(7) 0.0434(3) 0.053 Uani 1 1 d . . . C6F C 1.0021(13) 0.6098(9) 0.0856(5) 0.082 Uani 1 1 d . . . H6F H 0.9459 0.6269 0.1040 0.098 Uiso 1 1 calc R . . C7F C 1.2615(10) 0.5353(12) 0.0063(6) 0.086 Uani 1 1 d . . . H7F H 1.3193 0.5513 0.0175 0.103 Uiso 1 1 calc R . . C8F C 0.7409(11) 0.5144(14) 0.0346(7) 0.107 Uani 1 1 d . . . H8F H 0.6832 0.5307 0.0517 0.129 Uiso 1 1 calc R . . C9F C 0.8228(10) 0.5430(11) 0.0530(6) 0.082 Uani 1 1 d . . . H9F H 0.8199 0.5761 0.0823 0.098 Uiso 1 1 calc R . . C10F C 0.9114(8) 0.5216(7) 0.0271(4) 0.050 Uani 1 1 d . . . C1G C -0.0126(10) 0.5039(10) 0.3621(4) 0.069 Uani 1 1 d . . . H1G H 0.0059 0.5089 0.3286 0.083 Uiso 1 1 calc R . . C2G C -0.1034(9) 0.4860(8) 0.3759(4) 0.062 Uani 1 1 d . . . H2G H -0.1459 0.4761 0.3518 0.074 Uiso 1 1 calc R . . C3G C -0.1352(7) 0.4821(6) 0.4264(4) 0.047 Uani 1 1 d . . . C4G C -0.0677(6) 0.4909(5) 0.4631(3) 0.035 Uani 1 1 d . . . C5G C 0.0291(6) 0.5070(5) 0.4479(3) 0.037 Uani 1 1 d . . . C6G C 0.0546(9) 0.5152(8) 0.3978(4) 0.058 Uani 1 1 d . . . H6G H 0.1167 0.5283 0.3876 0.070 Uiso 1 1 calc R . . C7G C -0.2319(7) 0.4711(6) 0.4413(4) 0.052 Uani 1 1 d . . . H7G H -0.2764 0.4650 0.4176 0.063 Uiso 1 1 calc R . . C8G C 0.2596(7) 0.5303(7) 0.5100(5) 0.053 Uani 1 1 d . . . H8G H 0.3238 0.5356 0.5007 0.064 Uiso 1 1 calc R . . C9G C 0.1950(7) 0.5242(6) 0.4735(4) 0.044 Uani 1 1 d . . . H9G H 0.2166 0.5264 0.4403 0.053 Uiso 1 1 calc R . . C10G C 0.0986(6) 0.5147(5) 0.4857(3) 0.036 Uani 1 1 d . . . Cl1 Cl 0.9489(13) 0.4084(12) 0.1612(6) 0.103 Uiso 0.30 1 d PD B 3 C21 C 0.9306(11) 0.4769(9) 0.2136(5) 0.108 Uiso 0.30 1 d PD B 3 H21A H 0.8792 0.5248 0.2090 0.130 Uiso 0.30 1 calc PR B 3 H21B H 0.9136 0.4381 0.2424 0.130 Uiso 0.30 1 calc PR B 3 Cl2 Cl 1.0356(12) 0.5279(11) 0.2215(6) 0.139 Uiso 0.30 1 d PD B 3 Cl3 Cl 1.0146(13) 0.6435(10) 0.2310(7) 0.108 Uiso 0.30 1 d PD C 4 C22 C 1.0356(12) 0.5279(11) 0.2215(6) 0.139 Uiso 0.30 1 d PD C 4 H22A H 1.0664 0.4982 0.2497 0.167 Uiso 0.30 1 calc PR C 4 H22B H 1.0784 0.5186 0.1924 0.167 Uiso 0.30 1 calc PR C 4 Cl4 Cl 0.9306(11) 0.4769(9) 0.2136(5) 0.108 Uiso 0.30 1 d PD C 4 Cl5 Cl 0.9405(16) 0.4376(15) 0.1774(8) 0.124 Uiso 0.30 1 d PD D 5 C23 C 0.922(2) 0.4847(19) 0.2350(9) 0.046 Uiso 0.30 1 d PD D 5 H23A H 0.9552 0.4467 0.2597 0.055 Uiso 0.30 1 calc PR D 5 H23B H 0.8543 0.4914 0.2449 0.055 Uiso 0.30 1 calc PR D 5 Cl6 Cl 0.9690(17) 0.5924(16) 0.2257(9) 0.174 Uiso 0.30 1 d PD D 5 Cl7 Cl 1.071(2) 0.620(3) 0.2511(14) 0.083 Uiso 0.10 1 d PD E 6 C24 C 0.9690(17) 0.5924(16) 0.2257(9) 0.174 Uiso 0.10 1 d PD E 6 H24A H 0.9454 0.6432 0.2041 0.209 Uiso 0.10 1 calc PR E 6 H24B H 0.9198 0.5806 0.2514 0.209 Uiso 0.10 1 calc PR E 6 Cl8 Cl 0.999(5) 0.492(4) 0.192(3) 0.180 Uiso 0.10 1 d PD E 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 P1 0.024 0.016 0.024 0.000 -0.002 -0.001 Mo1 0.031 0.029 0.042 0.006 0.002 -0.007 Mo2 0.042 0.027 0.026 0.001 -0.002 -0.005 Mo3 0.036 0.025 0.039 -0.006 0.006 0.001 Mo4 0.035 0.025 0.039 0.002 -0.008 0.005 Mo5 0.034 0.029 0.036 -0.003 -0.009 -0.004 Mo6 0.034 0.017 0.039 -0.002 -0.003 -0.003 Mo7 0.033 0.022 0.036 0.003 -0.008 0.001 Mo8 0.034 0.026 0.037 -0.004 -0.008 -0.006 Mo9 0.040 0.017 0.041 0.000 -0.002 -0.003 Mo10 0.033 0.025 0.037 0.003 0.003 -0.006 Mo11 0.046 0.033 0.028 0.004 -0.005 0.000 Mo12 0.037 0.027 0.034 -0.006 0.001 0.004 O1 0.042 0.039 0.053 0.005 0.001 -0.016 O2 0.072 0.042 0.039 0.001 -0.002 -0.002 O3 0.050 0.046 0.050 -0.010 0.010 0.013 O4 0.036 0.033 0.067 0.002 -0.005 -0.001 O5 0.055 0.030 0.052 0.001 -0.013 -0.005 O6 0.050 0.030 0.054 -0.009 -0.003 -0.002 O7 0.048 0.045 0.037 0.003 -0.006 -0.008 O8 0.044 0.038 0.044 0.000 -0.002 0.009 O9 0.039 0.039 0.034 0.008 0.002 0.002 O10 0.053 0.026 0.049 -0.001 0.006 -0.003 O11 0.047 0.025 0.052 -0.003 0.003 -0.007 O12 0.047 0.042 0.043 0.002 -0.009 -0.010 O13 0.044 0.041 0.042 0.008 0.004 -0.012 O14 0.049 0.038 0.062 0.008 -0.016 0.002 O15 0.045 0.038 0.040 -0.002 0.003 0.002 O16 0.048 0.048 0.056 -0.016 -0.014 -0.003 O17 0.042 0.042 0.035 0.003 -0.005 0.004 O18 0.070 0.025 0.055 -0.007 -0.013 -0.008 O19 0.045 0.036 0.044 0.000 -0.002 -0.003 O20 0.051 0.032 0.054 0.004 -0.006 0.004 O21 0.039 0.024 0.048 0.000 0.010 -0.001 O22 0.042 0.046 0.048 -0.005 -0.005 -0.015 O23 0.049 0.034 0.045 -0.003 -0.004 0.006 O24 0.054 0.027 0.061 -0.003 -0.006 -0.004 O25 0.054 0.033 0.044 0.011 -0.002 0.002 O26 0.048 0.036 0.047 0.007 0.004 0.000 O27 0.050 0.035 0.047 -0.003 -0.006 -0.002 O28 0.051 0.039 0.039 -0.004 -0.008 -0.002 O29 0.043 0.041 0.046 0.004 -0.010 -0.005 O30 0.036 0.038 0.047 0.000 0.009 0.000 O31 0.053 0.030 0.055 0.003 -0.019 0.002 O32 0.056 0.030 0.056 -0.004 -0.011 -0.002 O33 0.049 0.028 0.046 0.001 -0.014 0.001 O34 0.050 0.044 0.060 0.010 0.013 -0.003 O35 0.068 0.047 0.032 0.005 -0.009 -0.001 O36 0.053 0.038 0.053 -0.011 0.005 0.003 C1A 0.034 0.022 0.037 -0.003 -0.001 0.000 C2A 0.038 0.027 0.034 -0.002 0.001 0.002 C3A 0.036 0.028 0.036 -0.003 -0.002 0.004 C4A 0.028 0.026 0.033 0.005 0.006 0.004 C5A 0.036 0.026 0.036 -0.004 -0.004 -0.001 C6A 0.037 0.029 0.025 0.001 0.001 0.003 C7A 0.051 0.042 0.034 0.001 0.009 -0.003 C8A 0.064 0.047 0.032 0.007 0.001 0.001 C9A 0.057 0.035 0.046 0.011 0.007 0.008 C10A 0.046 0.025 0.045 0.001 0.006 -0.004 C11A 0.067 0.025 0.062 0.001 -0.001 -0.002 C12A 0.064 0.038 0.060 -0.024 -0.013 -0.006 C13A 0.063 0.032 0.041 -0.004 -0.014 -0.001 C14A 0.052 0.039 0.034 0.002 -0.004 0.001 C15A 0.054 0.059 0.040 0.010 -0.019 0.011 C16A 0.055 0.035 0.061 0.015 0.005 0.009 C17A 0.039 0.024 0.048 0.005 -0.001 0.002 C18A 0.055 0.022 0.063 -0.001 0.002 0.002 C19A 0.047 0.029 0.057 -0.017 0.011 -0.006 C20A 0.055 0.033 0.042 -0.008 0.007 -0.007 C1B 0.030 0.035 0.049 0.002 0.005 -0.005 C2B 0.037 0.036 0.047 -0.003 -0.008 -0.001 C3B 0.036 0.043 0.053 0.009 0.003 0.000 C4B 0.038 0.034 0.057 0.012 0.006 0.000 C5B 0.037 0.030 0.051 -0.003 0.005 0.001 C6B 0.033 0.037 0.045 0.000 0.002 0.000 C7B 0.055 0.050 0.047 -0.005 -0.003 -0.004 C8B 0.066 0.067 0.048 0.003 -0.008 0.000 C9B 0.054 0.041 0.058 0.016 -0.011 -0.002 C10B 0.043 0.033 0.055 0.003 -0.008 0.003 C11B 0.049 0.039 0.069 -0.001 -0.001 -0.007 C12B 0.063 0.038 0.084 -0.015 -0.007 -0.003 C13B 0.053 0.047 0.061 -0.008 -0.015 -0.001 C14B 0.053 0.071 0.043 0.011 -0.006 -0.002 C15B 0.059 0.080 0.061 0.028 -0.001 0.006 C16B 0.073 0.052 0.079 0.025 0.001 0.005 C17B 0.050 0.044 0.069 0.014 0.014 -0.001 C18B 0.062 0.030 0.113 0.010 0.013 0.002 C19B 0.079 0.037 0.092 -0.010 0.002 -0.006 C20B 0.055 0.040 0.069 -0.010 0.011 -0.004 C1C 0.039 0.035 0.045 -0.004 -0.010 -0.003 C2C 0.046 0.039 0.050 0.006 -0.005 0.002 C3C 0.051 0.042 0.056 -0.004 -0.006 0.000 C4C 0.039 0.047 0.054 -0.012 -0.007 -0.002 C5C 0.035 0.049 0.047 -0.003 -0.005 0.000 C6C 0.044 0.034 0.044 0.001 -0.006 -0.002 C7C 0.112 0.037 0.060 0.000 -0.013 -0.005 C8C 0.128 0.044 0.060 -0.005 -0.008 -0.022 C9C 0.087 0.056 0.063 -0.023 -0.002 -0.010 C10C 0.046 0.055 0.041 -0.008 -0.007 -0.004 C11C 0.074 0.082 0.044 -0.003 -0.005 -0.013 C12C 0.126 0.085 0.041 0.026 -0.032 -0.030 C13C 0.093 0.058 0.049 0.021 -0.006 -0.003 C14C 0.116 0.040 0.101 -0.006 -0.011 0.014 C15C 0.141 0.045 0.125 -0.025 -0.018 0.007 C16C 0.089 0.065 0.097 -0.033 -0.009 0.012 C17C 0.045 0.059 0.065 -0.020 0.000 0.000 C18C 0.060 0.098 0.053 -0.029 0.006 -0.003 C19C 0.113 0.081 0.055 -0.016 -0.018 0.003 C20C 0.116 0.055 0.045 -0.003 0.002 -0.004 C1D 0.032 0.050 0.035 -0.003 0.000 -0.003 C2D 0.037 0.047 0.036 0.002 0.002 -0.008 C3D 0.055 0.043 0.042 -0.001 0.006 -0.007 C4D 0.031 0.055 0.037 0.000 -0.001 0.006 C5D 0.043 0.045 0.049 0.004 0.002 0.009 C6D 0.052 0.041 0.047 -0.001 0.008 0.009 C7D 0.103 0.048 0.055 0.006 0.006 0.022 C8D 0.097 0.045 0.077 -0.008 0.013 0.006 C9D 0.076 0.051 0.067 -0.021 0.003 0.004 C10D 0.043 0.049 0.044 -0.009 0.000 -0.004 C11D 0.076 0.069 0.040 -0.006 -0.003 -0.007 C12D 0.115 0.068 0.038 0.012 -0.006 -0.014 C13D 0.093 0.051 0.052 0.015 0.001 -0.008 C14D 0.131 0.053 0.045 0.004 -0.004 -0.019 C15D 0.139 0.050 0.065 -0.008 -0.005 -0.022 C16D 0.092 0.066 0.051 -0.014 0.000 -0.008 C17D 0.044 0.064 0.037 -0.003 0.010 -0.001 C18D 0.090 0.072 0.042 0.003 -0.007 0.028 C19D 0.105 0.084 0.039 0.013 -0.007 0.028 C20D 0.087 0.055 0.054 0.016 0.001 0.036 C1E 0.042 0.038 0.027 -0.007 -0.001 -0.009 C2E 0.047 0.031 0.034 -0.003 -0.004 0.004 C3E 0.046 0.037 0.041 -0.007 0.005 -0.010 C4E 0.040 0.042 0.039 -0.006 -0.003 -0.005 C5E 0.051 0.036 0.034 -0.011 -0.004 0.002 C6E 0.056 0.026 0.039 -0.002 -0.006 -0.005 C7E 0.070 0.041 0.063 0.007 -0.007 -0.009 C8E 0.083 0.040 0.066 0.004 0.005 -0.029 C9E 0.053 0.056 0.076 -0.006 0.003 -0.033 C10E 0.055 0.041 0.043 -0.002 -0.008 -0.009 C11E 0.028 0.092 0.049 -0.013 0.003 -0.010 C12E 0.045 0.061 0.086 -0.017 0.008 0.005 C13E 0.059 0.041 0.056 0.002 -0.011 0.009 C14E 0.069 0.041 0.085 0.015 -0.004 -0.012 C15E 0.074 0.051 0.112 0.016 -0.008 -0.032 C16E 0.052 0.078 0.080 -0.005 0.008 -0.042 C17E 0.049 0.059 0.045 -0.011 0.001 -0.015 C18E 0.035 0.089 0.068 -0.026 -0.003 0.004 C19E 0.048 0.065 0.064 -0.018 -0.010 0.020 C20E 0.051 0.054 0.056 -0.023 -0.013 0.017 C1F 0.131 0.050 0.065 0.002 -0.053 -0.012 C2F 0.110 0.071 0.092 0.029 -0.053 -0.036 C3F 0.081 0.067 0.066 0.037 -0.024 -0.022 C4F 0.057 0.040 0.054 0.019 -0.014 -0.006 C5F 0.081 0.042 0.035 0.007 -0.004 0.003 C6F 0.134 0.056 0.055 0.007 -0.019 0.001 C7F 0.056 0.125 0.077 0.051 -0.010 -0.036 C8F 0.058 0.160 0.095 0.076 0.012 0.009 C9F 0.064 0.092 0.083 0.020 0.015 0.012 C10F 0.053 0.051 0.041 0.008 0.009 0.010 C1G 0.082 0.085 0.040 0.002 -0.002 0.000 C2G 0.066 0.067 0.053 -0.007 -0.011 -0.007 C3G 0.053 0.029 0.058 -0.002 -0.008 0.003 C4G 0.038 0.020 0.045 0.002 0.005 -0.003 C5G 0.043 0.022 0.044 0.000 0.001 0.008 C6G 0.058 0.064 0.051 0.003 0.003 0.005 C7G 0.047 0.039 0.073 0.000 -0.022 0.002 C8G 0.040 0.039 0.082 -0.007 0.004 -0.004 C9G 0.046 0.026 0.059 0.002 0.007 -0.001 C10G 0.038 0.021 0.049 -0.003 0.010 -0.002 _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 P1 O39A 1.533(5) . ? P1 O37A 1.533(5) . ? P1 O39B 1.536(8) . ? P1 O38B 1.537(8) . ? P1 O40B 1.537(9) . ? P1 O38A 1.538(5) . ? P1 O40A 1.538(5) . ? P1 O37B 1.541(8) . ? Mo1 O1 1.664(6) . ? Mo1 O8 1.810(6) . ? Mo1 O4 1.859(6) . ? Mo1 O9 1.989(6) . ? Mo1 O5 2.028(6) . ? Mo1 O37A 2.436(5) . ? Mo2 O2 1.669(7) . ? Mo2 O10 1.816(6) . ? Mo2 O5 1.830(6) . ? Mo2 O11 1.980(6) . ? Mo2 O6 2.017(6) . ? Mo2 O37A 2.455(5) . ? Mo3 O3 1.677(6) . ? Mo3 O12 1.818(6) . ? Mo3 O6 1.844(7) . ? Mo3 O4 1.991(6) . ? Mo3 O7 1.997(6) . ? Mo3 O37A 2.446(5) . ? Mo3 O38B 2.48(4) . ? Mo4 O14 1.661(6) . ? Mo4 O7 1.805(6) . ? Mo4 O15 1.850(6) . ? Mo4 O13 1.979(6) . ? Mo4 O26 2.009(7) . ? Mo4 O38A 2.437(6) . ? Mo4 O38B 2.50(4) . ? Mo5 O16 1.659(6) . ? Mo5 O17 1.821(6) . ? Mo5 O27 1.840(7) . ? Mo5 O8 1.998(6) . ? Mo5 O15 2.009(6) . ? Mo5 O37B 2.43(3) . ? Mo5 O38A 2.435(5) . ? Mo6 O18 1.674(6) . ? Mo6 O9 1.827(6) . ? Mo6 O19 1.865(6) . ? Mo6 O17 1.986(6) . ? Mo6 O28 2.007(7) . ? Mo6 O39A 2.434(5) . ? Mo6 O37B 2.49(3) . ? Mo7 O20 1.665(6) . ? Mo7 O21 1.808(5) . ? Mo7 O29 1.843(7) . ? Mo7 O19 1.985(6) . ? Mo7 O10 2.001(7) . ? Mo7 O39A 2.444(5) . ? Mo7 O39B 2.45(3) . ? Mo8 O22 1.665(6) . ? Mo8 O11 1.814(6) . ? Mo8 O23 1.858(6) . ? Mo8 O21 1.986(5) . ? Mo8 O30 2.012(6) . ? Mo8 O40A 2.417(5) . ? Mo8 O39B 2.45(3) . ? Mo9 O24 1.674(6) . ? Mo9 O13 1.825(6) . ? Mo9 O25 1.841(7) . ? Mo9 O12 1.988(7) . ? Mo9 O23 2.002(6) . ? Mo9 O40A 2.439(5) . ? Mo9 O38B 2.51(4) . ? Mo10 O34 1.669(7) . ? Mo10 O33 1.816(6) . ? Mo10 O30 1.840(7) . ? Mo10 O31 2.006(6) . ? Mo10 O25 2.010(6) . ? Mo10 O40B 2.44(4) . ? Mo10 O40A 2.444(5) . ? Mo11 O35 1.678(6) . ? Mo11 O31 1.807(6) . ? Mo11 O26 1.862(6) . ? Mo11 O32 1.993(6) . ? Mo11 O27 2.007(6) . ? Mo11 O38A 2.449(6) . ? Mo12 O36 1.664(7) . ? Mo12 O32 1.828(7) . ? Mo12 O28 1.855(6) . ? Mo12 O33 1.984(6) . ? Mo12 O29 2.021(6) . ? Mo12 O39A 2.452(6) . ? C1A C2A 1.394(11) . ? C1A C10A 1.420(10) . ? C1A C6A 1.434(10) . ? C2A C13A 1.415(11) . ? C2A C3A 1.455(10) . ? C3A C14A 1.403(11) . ? C3A C4A 1.411(10) . ? C4A C5A 1.413(11) . ? C4A C17A 1.423(10) . ? C5A C20A 1.392(10) . ? C5A C6A 1.463(10) . ? C6A C7A 1.407(11) . ? C7A C8A 1.372(13) . ? C8A C9A 1.357(13) . ? C9A C10A 1.403(13) . ? C10A C11A 1.425(12) . ? C11A C12A 1.331(15) . ? C12A C13A 1.401(13) . ? C14A C15A 1.388(13) . ? C15A C16A 1.376(14) . ? C16A C17A 1.392(13) . ? C17A C18A 1.410(12) . ? C18A C19A 1.360(14) . ? C19A C20A 1.405(12) . ? C1B C6B 1.412(12) . ? C1B C2B 1.413(13) . ? C1B C10B 1.419(12) . ? C2B C13B 1.402(12) . ? C2B C3B 1.454(12) . ? C3B C14B 1.392(14) . ? C3B C4B 1.414(13) . ? C4B C5B 1.431(13) . ? C4B C17B 1.434(12) . ? C5B C20B 1.390(12) . ? C5B C6B 1.441(12) . ? C6B C7B 1.406(13) . ? C7B C8B 1.383(15) . ? C8B C9B 1.366(15) . ? C9B C10B 1.409(14) . ? C10B C11B 1.397(13) . ? C11B C12B 1.366(16) . ? C12B C13B 1.395(15) . ? C14B C15B 1.387(16) . ? C15B C16B 1.366(18) . ? C16B C17B 1.401(17) . ? C17B C18B 1.390(17) . ? C18B C19B 1.354(19) . ? C19B C20B 1.386(15) . ? C1C C6C 1.410(12) . ? C1C C10C 1.425(12) . ? C1C C2C 1.432(12) . ? C2C C13C 1.413(14) . ? C2C C3C 1.450(14) . ? C3C C14C 1.393(14) . ? C3C C4C 1.416(14) . ? C4C C5C 1.415(13) . ? C4C C17C 1.418(13) . ? C5C C20C 1.404(15) . ? C5C C6C 1.456(13) . ? C6C C7C 1.396(13) . ? C7C C8C 1.364(16) . ? C8C C9C 1.362(17) . ? C9C C10C 1.385(15) . ? C10C C11C 1.409(15) . ? C11C C12C 1.349(18) . ? C12C C13C 1.364(18) . ? C14C C15C 1.36(2) . ? C15C C16C 1.37(2) . ? C16C C17C 1.402(17) . ? C17C C18C 1.428(18) . ? C18C C19C 1.325(19) . ? C19C C20C 1.375(16) . ? C1D C6D 1.409(13) . ? C1D C2D 1.417(12) . ? C1D C10D 1.422(12) . ? C2D C13D 1.397(13) . ? C2D C3D 1.452(13) . ? C3D C14D 1.406(15) . ? C3D C4D 1.419(13) . ? C4D C17D 1.415(13) . ? C4D C5D 1.418(13) . ? C5D C20D 1.378(14) . ? C5D C6D 1.461(14) . ? C6D C7D 1.396(14) . ? C7D C8D 1.376(17) . ? C8D C9D 1.370(18) . ? C9D C10D 1.427(14) . ? C10D C11D 1.417(15) . ? C11D C12D 1.349(17) . ? C12D C13D 1.385(16) . ? C14D C15D 1.379(16) . ? C15D C16D 1.386(18) . ? C16D C17D 1.409(16) . ? C17D C18D 1.399(15) . ? C18D C19D 1.343(18) . ? C19D C20D 1.385(17) . ? C1E C10E 1.409(13) . ? C1E C2E 1.417(11) . ? C1E C6E 1.436(12) . ? C2E C13E 1.376(12) . ? C2E C3E 1.474(12) . ? C3E C14E 1.388(13) . ? C3E C4E 1.419(13) . ? C4E C17E 1.427(13) . ? C4E C5E 1.446(12) . ? C5E C20E 1.377(13) . ? C5E C6E 1.445(13) . ? C6E C7E 1.394(12) . ? C7E C8E 1.374(16) . ? C8E C9E 1.361(17) . ? C9E C10E 1.397(13) . ? C10E C11E 1.410(14) . ? C11E C12E 1.359(17) . ? C12E C13E 1.401(16) . ? C14E C15E 1.396(16) . ? C15E C16E 1.375(19) . ? C16E C17E 1.391(16) . ? C17E C18E 1.417(15) . ? C18E C19E 1.348(17) . ? C19E C20E 1.392(16) . ? C1F C2F 1.38(2) . ? C1F C6F 1.43(2) . ? C2F C3F 1.36(2) . ? C3F C7F 1.42(2) . ? C3F C4F 1.427(16) . ? C4F C5F 1.416(16) . ? C4F C10F 1.423(15) 2_765 ? C5F C6F 1.408(16) . ? C5F C10F 1.449(16) . ? C7F C8F 1.33(2) 2_765 ? C8F C7F 1.33(2) 2_765 ? C8F C9F 1.37(2) . ? C9F C10F 1.412(16) . ? C10F C4F 1.423(15) 2_765 ? C1G C2G 1.349(18) . ? C1G C6G 1.409(16) . ? C2G C3G 1.413(15) . ? C3G C7G 1.413(15) . ? C3G C4G 1.428(13) . ? C4G C10G 1.429(12) 2_566 ? C4G C5G 1.431(12) . ? C5G C6G 1.385(14) . ? C5G C10G 1.466(12) . ? C7G C8G 1.353(16) 2_566 ? C8G C7G 1.353(16) 2_566 ? C8G C9G 1.389(14) . ? C9G C10G 1.391(12) . ? C10G C4G 1.429(12) 2_566 ? Cl1 C21 1.743(16) . ? C21 Cl2 1.719(18) . ? Cl5 C23 1.714(19) . ? C23 Cl6 1.72(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 O39A P1 O37A 109.2(3) . . ? O39A P1 O39B 67.9(14) . . ? O37A P1 O39B 74.5(15) . . ? O39A P1 O38B 178.6(17) . . ? O37A P1 O38B 69.4(16) . . ? O39B P1 O38B 111(2) . . ? O39A P1 O40B 71.1(17) . . ? O37A P1 O40B 177.2(17) . . ? O39B P1 O40B 103(2) . . ? O38B P1 O40B 110(2) . . ? O39A P1 O38A 109.6(3) . . ? O37A P1 O38A 109.2(3) . . ? O39B P1 O38A 176.3(15) . . ? O38B P1 O38A 71.1(15) . . ? O40B P1 O38A 73.1(17) . . ? O39A P1 O40A 109.4(3) . . ? O37A P1 O40A 109.2(3) . . ? O39B P1 O40A 68.7(14) . . ? O38B P1 O40A 71.3(16) . . ? O40B P1 O40A 68.3(17) . . ? O38A P1 O40A 110.2(3) . . ? O39A P1 O37B 69.8(12) . . ? O37A P1 O37B 74.5(13) . . ? O39B P1 O37B 113.9(19) . . ? O38B P1 O37B 110(2) . . ? O40B P1 O37B 108(2) . . ? O38A P1 O37B 67.0(12) . . ? O40A P1 O37B 176.2(12) . . ? O1 Mo1 O8 105.0(3) . . ? O1 Mo1 O4 101.5(3) . . ? O8 Mo1 O4 97.5(3) . . ? O1 Mo1 O9 102.0(3) . . ? O8 Mo1 O9 85.7(3) . . ? O4 Mo1 O9 154.6(3) . . ? O1 Mo1 O5 97.9(3) . . ? O8 Mo1 O5 155.4(3) . . ? O4 Mo1 O5 86.4(3) . . ? O9 Mo1 O5 81.0(3) . . ? O1 Mo1 O37A 167.0(3) . . ? O8 Mo1 O37A 87.5(3) . . ? O4 Mo1 O37A 72.9(2) . . ? O9 Mo1 O37A 82.1(2) . . ? O5 Mo1 O37A 70.4(2) . . ? O2 Mo2 O10 103.9(3) . . ? O2 Mo2 O5 102.0(3) . . ? O10 Mo2 O5 97.6(3) . . ? O2 Mo2 O11 102.3(3) . . ? O10 Mo2 O11 85.6(3) . . ? O5 Mo2 O11 153.9(3) . . ? O2 Mo2 O6 99.1(3) . . ? O10 Mo2 O6 155.3(3) . . ? O5 Mo2 O6 86.2(3) . . ? O11 Mo2 O6 80.8(3) . . ? O2 Mo2 O37A 168.2(3) . . ? O10 Mo2 O37A 87.4(2) . . ? O5 Mo2 O37A 72.9(2) . . ? O11 Mo2 O37A 81.4(2) . . ? O6 Mo2 O37A 70.3(2) . . ? O3 Mo3 O12 103.9(3) . . ? O3 Mo3 O6 102.7(3) . . ? O12 Mo3 O6 96.7(3) . . ? O3 Mo3 O4 99.3(3) . . ? O12 Mo3 O4 155.0(3) . . ? O6 Mo3 O4 87.2(3) . . ? O3 Mo3 O7 101.1(3) . . ? O12 Mo3 O7 85.3(3) . . ? O6 Mo3 O7 154.9(3) . . ? O4 Mo3 O7 81.1(3) . . ? O3 Mo3 O37A 169.0(3) . . ? O12 Mo3 O37A 86.8(2) . . ? O6 Mo3 O37A 73.1(2) . . ? O4 Mo3 O37A 70.7(2) . . ? O7 Mo3 O37A 82.1(2) . . ? O3 Mo3 O38B 147.9(6) . . ? O12 Mo3 O38B 57.0(9) . . ? O6 Mo3 O38B 105.0(7) . . ? O4 Mo3 O38B 98.0(9) . . ? O7 Mo3 O38B 55.4(8) . . ? O37A Mo3 O38B 41.5(6) . . ? O14 Mo4 O7 104.9(3) . . ? O14 Mo4 O15 101.4(3) . . ? O7 Mo4 O15 97.1(3) . . ? O14 Mo4 O13 102.2(3) . . ? O7 Mo4 O13 85.7(3) . . ? O15 Mo4 O13 154.7(3) . . ? O14 Mo4 O26 97.8(3) . . ? O7 Mo4 O26 155.7(3) . . ? O15 Mo4 O26 86.6(3) . . ? O13 Mo4 O26 81.2(3) . . ? O14 Mo4 O38A 166.9(3) . . ? O7 Mo4 O38A 87.6(3) . . ? O15 Mo4 O38A 72.5(2) . . ? O13 Mo4 O38A 82.5(2) . . ? O26 Mo4 O38A 70.6(2) . . ? O14 Mo4 O38B 149.5(6) . . ? O7 Mo4 O38B 56.5(9) . . ? O15 Mo4 O38B 104.6(7) . . ? O13 Mo4 O38B 56.3(9) . . ? O26 Mo4 O38B 99.4(9) . . ? O38A Mo4 O38B 42.4(5) . . ? O16 Mo5 O17 103.8(3) . . ? O16 Mo5 O27 101.8(3) . . ? O17 Mo5 O27 97.2(3) . . ? O16 Mo5 O8 102.3(3) . . ? O17 Mo5 O8 84.6(3) . . ? O27 Mo5 O8 154.7(3) . . ? O16 Mo5 O15 99.5(3) . . ? O17 Mo5 O15 154.6(3) . . ? O27 Mo5 O15 87.7(3) . . ? O8 Mo5 O15 80.7(2) . . ? O16 Mo5 O37B 149.7(5) . . ? O17 Mo5 O37B 56.2(7) . . ? O27 Mo5 O37B 103.1(7) . . ? O8 Mo5 O37B 57.0(7) . . ? O15 Mo5 O37B 98.4(7) . . ? O16 Mo5 O38A 168.4(3) . . ? O17 Mo5 O38A 87.4(2) . . ? O27 Mo5 O38A 73.1(2) . . ? O8 Mo5 O38A 81.7(2) . . ? O15 Mo5 O38A 70.2(2) . . ? O37B Mo5 O38A 40.9(5) . . ? O18 Mo6 O9 104.5(3) . . ? O18 Mo6 O19 100.5(3) . . ? O9 Mo6 O19 96.3(3) . . ? O18 Mo6 O17 103.1(3) . . ? O9 Mo6 O17 85.9(3) . . ? O19 Mo6 O17 155.0(3) . . ? O18 Mo6 O28 98.4(3) . . ? O9 Mo6 O28 156.1(2) . . ? O19 Mo6 O28 86.2(3) . . ? O17 Mo6 O28 82.2(3) . . ? O18 Mo6 O39A 167.3(3) . . ? O9 Mo6 O39A 87.1(2) . . ? O19 Mo6 O39A 72.5(2) . . ? O17 Mo6 O39A 82.8(2) . . ? O28 Mo6 O39A 70.9(2) . . ? O18 Mo6 O37B 149.8(5) . . ? O9 Mo6 O37B 59.3(7) . . ? O19 Mo6 O37B 106.2(6) . . ? O17 Mo6 O37B 53.8(6) . . ? O28 Mo6 O37B 97.1(7) . . ? O39A Mo6 O37B 41.8(5) . . ? O20 Mo7 O21 103.9(3) . . ? O20 Mo7 O29 101.3(3) . . ? O21 Mo7 O29 97.1(3) . . ? O20 Mo7 O19 99.4(3) . . ? O21 Mo7 O19 155.0(3) . . ? O29 Mo7 O19 87.1(3) . . ? O20 Mo7 O10 101.5(3) . . ? O21 Mo7 O10 85.2(3) . . ? O29 Mo7 O10 155.8(3) . . ? O19 Mo7 O10 81.3(3) . . ? O20 Mo7 O39A 168.6(2) . . ? O21 Mo7 O39A 87.0(2) . . ? O29 Mo7 O39A 73.6(2) . . ? O19 Mo7 O39A 70.5(2) . . ? O10 Mo7 O39A 82.5(2) . . ? O20 Mo7 O39B 149.5(6) . . ? O21 Mo7 O39B 55.7(8) . . ? O29 Mo7 O39B 103.6(8) . . ? O19 Mo7 O39B 99.3(8) . . ? O10 Mo7 O39B 58.1(9) . . ? O39A Mo7 O39B 41.0(5) . . ? O22 Mo8 O11 104.1(3) . . ? O22 Mo8 O23 101.4(3) . . ? O11 Mo8 O23 96.6(3) . . ? O22 Mo8 O21 101.7(3) . . ? O11 Mo8 O21 86.1(2) . . ? O23 Mo8 O21 155.3(3) . . ? O22 Mo8 O30 99.0(3) . . ? O11 Mo8 O30 155.5(3) . . ? O23 Mo8 O30 86.7(3) . . ? O21 Mo8 O30 81.2(2) . . ? O22 Mo8 O40A 167.7(3) . . ? O11 Mo8 O40A 87.6(2) . . ? O23 Mo8 O40A 72.9(2) . . ? O21 Mo8 O40A 82.7(2) . . ? O30 Mo8 O40A 70.1(2) . . ? O22 Mo8 O39B 148.9(6) . . ? O11 Mo8 O39B 59.5(9) . . ? O23 Mo8 O39B 106.4(7) . . ? O21 Mo8 O39B 54.2(8) . . ? O30 Mo8 O39B 96.1(9) . . ? O40A Mo8 O39B 41.7(5) . . ? O24 Mo9 O13 104.5(3) . . ? O24 Mo9 O25 101.8(3) . . ? O13 Mo9 O25 96.5(3) . . ? O24 Mo9 O12 102.6(3) . . ? O13 Mo9 O12 86.1(3) . . ? O25 Mo9 O12 154.0(3) . . ? O24 Mo9 O23 98.7(3) . . ? O13 Mo9 O23 155.3(3) . . ? O25 Mo9 O23 86.9(3) . . ? O12 Mo9 O23 80.5(3) . . ? O24 Mo9 O40A 167.3(3) . . ? O13 Mo9 O40A 87.5(2) . . ? O25 Mo9 O40A 72.2(2) . . ? O12 Mo9 O40A 82.1(2) . . ? O23 Mo9 O40A 70.2(2) . . ? O24 Mo9 O38B 149.0(6) . . ? O13 Mo9 O38B 57.3(9) . . ? O25 Mo9 O38B 105.0(7) . . ? O12 Mo9 O38B 55.2(9) . . ? O23 Mo9 O38B 98.1(8) . . ? O40A Mo9 O38B 42.4(5) . . ? O34 Mo10 O33 103.8(3) . . ? O34 Mo10 O30 102.8(3) . . ? O33 Mo10 O30 96.6(3) . . ? O34 Mo10 O31 101.3(3) . . ? O33 Mo10 O31 86.2(3) . . ? O30 Mo10 O31 154.3(3) . . ? O34 Mo10 O25 99.8(3) . . ? O33 Mo10 O25 154.9(3) . . ? O30 Mo10 O25 86.3(3) . . ? O31 Mo10 O25 80.9(3) . . ? O34 Mo10 O40B 149.2(7) . . ? O33 Mo10 O40B 57.3(10) . . ? O30 Mo10 O40B 103.5(9) . . ? O31 Mo10 O40B 56.8(10) . . ? O25 Mo10 O40B 97.7(10) . . ? O34 Mo10 O40A 168.2(3) . . ? O33 Mo10 O40A 87.5(2) . . ? O30 Mo10 O40A 72.0(2) . . ? O31 Mo10 O40A 82.7(2) . . ? O25 Mo10 O40A 69.7(2) . . ? O40B Mo10 O40A 41.4(6) . . ? O35 Mo11 O31 103.7(3) . . ? O35 Mo11 O26 102.1(3) . . ? O31 Mo11 O26 96.8(3) . . ? O35 Mo11 O32 101.7(3) . . ? O31 Mo11 O32 86.3(3) . . ? O26 Mo11 O32 154.4(3) . . ? O35 Mo11 O27 99.0(3) . . ? O31 Mo11 O27 155.7(3) . . ? O26 Mo11 O27 86.7(3) . . ? O32 Mo11 O27 80.7(3) . . ? O35 Mo11 O38A 168.0(3) . . ? O31 Mo11 O38A 87.7(3) . . ? O26 Mo11 O38A 72.5(2) . . ? O32 Mo11 O38A 82.3(2) . . ? O27 Mo11 O38A 70.3(2) . . ? O36 Mo12 O32 104.9(3) . . ? O36 Mo12 O28 101.0(3) . . ? O32 Mo12 O28 96.6(3) . . ? O36 Mo12 O33 102.6(3) . . ? O32 Mo12 O33 86.1(3) . . ? O28 Mo12 O33 154.6(3) . . ? O36 Mo12 O29 98.2(3) . . ? O32 Mo12 O29 155.6(3) . . ? O28 Mo12 O29 86.4(3) . . ? O33 Mo12 O29 81.3(2) . . ? O36 Mo12 O39A 167.4(3) . . ? O32 Mo12 O39A 86.9(3) . . ? O28 Mo12 O39A 72.8(2) . . ? O33 Mo12 O39A 82.2(2) . . ? O29 Mo12 O39A 70.7(2) . . ? Mo1 O4 Mo3 126.7(3) . . ? Mo2 O5 Mo1 126.9(3) . . ? Mo3 O6 Mo2 126.9(3) . . ? Mo4 O7 Mo3 151.0(4) . . ? Mo1 O8 Mo5 151.3(4) . . ? Mo6 O9 Mo1 149.6(3) . . ? Mo2 O10 Mo7 150.4(3) . . ? Mo8 O11 Mo2 150.5(3) . . ? Mo3 O12 Mo9 150.5(4) . . ? Mo9 O13 Mo4 150.0(3) . . ? Mo4 O15 Mo5 126.9(3) . . ? Mo5 O17 Mo6 150.8(3) . . ? Mo6 O19 Mo7 127.0(3) . . ? Mo7 O21 Mo8 150.5(3) . . ? Mo8 O23 Mo9 126.4(3) . . ? Mo9 O25 Mo10 127.8(3) . . ? Mo11 O26 Mo4 126.7(3) . . ? Mo5 O27 Mo11 126.8(3) . . ? Mo12 O28 Mo6 126.5(3) . . ? Mo7 O29 Mo12 126.2(3) . . ? Mo10 O30 Mo8 127.4(3) . . ? Mo11 O31 Mo10 149.8(3) . . ? Mo12 O32 Mo11 149.9(4) . . ? Mo10 O33 Mo12 150.4(4) . . ? P1 O37A Mo1 125.3(3) . . ? P1 O37A Mo3 125.6(3) . . ? Mo1 O37A Mo3 89.66(18) . . ? P1 O37A Mo2 125.6(3) . . ? Mo1 O37A Mo2 89.81(17) . . ? Mo3 O37A Mo2 89.62(17) . . ? P1 O38A Mo5 125.9(3) . . ? P1 O38A Mo4 125.1(3) . . ? Mo5 O38A Mo4 90.26(18) . . ? P1 O38A Mo11 124.7(3) . . ? Mo5 O38A Mo11 89.61(17) . . ? Mo4 O38A Mo11 90.22(18) . . ? P1 O39A Mo6 125.5(3) . . ? P1 O39A Mo7 125.6(3) . . ? Mo6 O39A Mo7 89.90(17) . . ? P1 O39A Mo12 125.3(3) . . ? Mo6 O39A Mo12 89.80(17) . . ? Mo7 O39A Mo12 89.49(17) . . ? P1 O40A Mo8 125.3(3) . . ? P1 O40A Mo9 124.9(3) . . ? Mo8 O40A Mo9 90.40(16) . . ? P1 O40A Mo10 124.7(3) . . ? Mo8 O40A Mo10 90.55(17) . . ? Mo9 O40A Mo10 90.21(17) . . ? P1 O37B Mo5 126.1(17) . . ? P1 O37B Mo6 121.8(16) . . ? Mo5 O37B Mo6 97.0(7) . . ? P1 O38B Mo3 123(2) . . ? P1 O38B Mo4 121(2) . . ? Mo3 O38B Mo4 95.2(9) . . ? P1 O38B Mo9 121(2) . . ? Mo3 O38B Mo9 95.0(9) . . ? Mo4 O38B Mo9 94.3(10) . . ? P1 O39B Mo7 125.4(19) . . ? P1 O39B Mo8 123.2(19) . . ? Mo7 O39B Mo8 97.0(8) . . ? P1 O40B Mo10 125(2) . . ? C2A C1A C10A 120.0(7) . . ? C2A C1A C6A 121.6(7) . . ? C10A C1A C6A 118.4(7) . . ? C1A C2A C13A 119.2(7) . . ? C1A C2A C3A 120.4(7) . . ? C13A C2A C3A 120.4(7) . . ? C14A C3A C4A 119.2(7) . . ? C14A C3A C2A 122.3(7) . . ? C4A C3A C2A 118.4(7) . . ? C3A C4A C5A 122.1(7) . . ? C3A C4A C17A 119.3(7) . . ? C5A C4A C17A 118.6(7) . . ? C20A C5A C4A 120.2(7) . . ? C20A C5A C6A 120.4(7) . . ? C4A C5A C6A 119.4(6) . . ? C7A C6A C1A 118.4(7) . . ? C7A C6A C5A 123.4(7) . . ? C1A C6A C5A 118.1(7) . . ? C8A C7A C6A 121.4(8) . . ? C9A C8A C7A 121.1(9) . . ? C8A C9A C10A 120.5(8) . . ? C9A C10A C1A 120.1(8) . . ? C9A C10A C11A 122.0(8) . . ? C1A C10A C11A 117.9(8) . . ? C12A C11A C10A 122.4(8) . . ? C11A C12A C13A 120.0(8) . . ? C12A C13A C2A 120.5(8) . . ? C15A C14A C3A 120.9(8) . . ? C16A C15A C14A 120.0(8) . . ? C15A C16A C17A 121.3(8) . . ? C16A C17A C18A 121.2(8) . . ? C16A C17A C4A 119.3(8) . . ? C18A C17A C4A 119.5(8) . . ? C19A C18A C17A 121.0(8) . . ? C18A C19A C20A 120.3(8) . . ? C5A C20A C19A 120.3(9) . . ? C6B C1B C2B 121.6(8) . . ? C6B C1B C10B 119.0(8) . . ? C2B C1B C10B 119.3(8) . . ? C13B C2B C1B 119.4(8) . . ? C13B C2B C3B 121.6(9) . . ? C1B C2B C3B 119.0(8) . . ? C14B C3B C4B 118.1(9) . . ? C14B C3B C2B 122.3(9) . . ? C4B C3B C2B 119.6(9) . . ? C3B C4B C5B 120.9(8) . . ? C3B C4B C17B 120.2(9) . . ? C5B C4B C17B 118.9(9) . . ? C20B C5B C4B 117.9(9) . . ? C20B C5B C6B 122.9(9) . . ? C4B C5B C6B 119.2(8) . . ? C7B C6B C1B 118.7(8) . . ? C7B C6B C5B 121.6(8) . . ? C1B C6B C5B 119.7(8) . . ? C8B C7B C6B 121.4(9) . . ? C9B C8B C7B 120.5(10) . . ? C8B C9B C10B 120.1(9) . . ? C11B C10B C9B 120.1(9) . . ? C11B C10B C1B 119.8(9) . . ? C9B C10B C1B 120.0(8) . . ? C12B C11B C10B 120.1(9) . . ? C11B C12B C13B 121.4(10) . . ? C12B C13B C2B 119.9(10) . . ? C15B C14B C3B 121.8(11) . . ? C16B C15B C14B 120.4(11) . . ? C15B C16B C17B 121.1(10) . . ? C18B C17B C16B 122.6(10) . . ? C18B C17B C4B 119.0(11) . . ? C16B C17B C4B 118.4(10) . . ? C19B C18B C17B 122.4(10) . . ? C18B C19B C20B 119.1(11) . . ? C19B C20B C5B 122.7(11) . . ? C6C C1C C10C 119.8(8) . . ? C6C C1C C2C 120.9(8) . . ? C10C C1C C2C 119.3(9) . . ? C13C C2C C1C 117.4(9) . . ? C13C C2C C3C 123.6(9) . . ? C1C C2C C3C 118.9(9) . . ? C14C C3C C4C 117.5(10) . . ? C14C C3C C2C 122.7(11) . . ? C4C C3C C2C 119.8(8) . . ? C5C C4C C3C 121.3(9) . . ? C5C C4C C17C 118.8(10) . . ? C3C C4C C17C 119.9(9) . . ? C20C C5C C4C 118.9(9) . . ? C20C C5C C6C 122.0(9) . . ? C4C C5C C6C 119.1(9) . . ? C7C C6C C1C 118.2(9) . . ? C7C C6C C5C 121.9(9) . . ? C1C C6C C5C 119.9(8) . . ? C8C C7C C6C 121.2(11) . . ? C9C C8C C7C 121.2(11) . . ? C8C C9C C10C 120.8(10) . . ? C9C C10C C11C 121.4(10) . . ? C9C C10C C1C 118.8(9) . . ? C11C C10C C1C 119.8(10) . . ? C12C C11C C10C 119.6(11) . . ? C11C C12C C13C 122.6(10) . . ? C12C C13C C2C 121.3(11) . . ? C15C C14C C3C 122.9(15) . . ? C14C C15C C16C 120.1(13) . . ? C15C C16C C17C 120.8(12) . . ? C16C C17C C4C 118.8(12) . . ? C16C C17C C18C 122.4(11) . . ? C4C C17C C18C 118.9(10) . . ? C19C C18C C17C 121.1(11) . . ? C18C C19C C20C 121.2(13) . . ? C19C C20C C5C 121.1(12) . . ? C6D C1D C2D 121.4(8) . . ? C6D C1D C10D 120.2(9) . . ? C2D C1D C10D 118.4(8) . . ? C13D C2D C1D 118.6(9) . . ? C13D C2D C3D 122.6(9) . . ? C1D C2D C3D 118.8(8) . . ? C14D C3D C4D 118.3(9) . . ? C14D C3D C2D 121.6(9) . . ? C4D C3D C2D 120.1(8) . . ? C17D C4D C5D 119.2(9) . . ? C17D C4D C3D 119.7(9) . . ? C5D C4D C3D 121.0(8) . . ? C20D C5D C4D 118.1(10) . . ? C20D C5D C6D 123.2(9) . . ? C4D C5D C6D 118.7(8) . . ? C7D C6D C1D 118.1(9) . . ? C7D C6D C5D 121.8(9) . . ? C1D C6D C5D 120.0(8) . . ? C8D C7D C6D 122.5(11) . . ? C9D C8D C7D 120.1(11) . . ? C8D C9D C10D 120.4(10) . . ? C11D C10D C1D 120.0(9) . . ? C11D C10D C9D 121.4(9) . . ? C1D C10D C9D 118.5(9) . . ? C12D C11D C10D 120.8(10) . . ? C11D C12D C13D 119.8(10) . . ? C12D C13D C2D 122.5(11) . . ? C15D C14D C3D 121.8(11) . . ? C14D C15D C16D 120.3(12) . . ? C15D C16D C17D 119.9(10) . . ? C18D C17D C16D 120.4(10) . . ? C18D C17D C4D 119.7(10) . . ? C16D C17D C4D 119.9(10) . . ? C19D C18D C17D 120.3(11) . . ? C18D C19D C20D 120.8(11) . . ? C5D C20D C19D 121.9(11) . . ? C10E C1E C2E 119.0(8) . . ? C10E C1E C6E 120.7(8) . . ? C2E C1E C6E 120.2(8) . . ? C13E C2E C1E 119.8(9) . . ? C13E C2E C3E 121.0(8) . . ? C1E C2E C3E 119.2(8) . . ? C14E C3E C4E 118.9(9) . . ? C14E C3E C2E 120.9(9) . . ? C4E C3E C2E 120.2(8) . . ? C3E C4E C17E 120.0(9) . . ? C3E C4E C5E 120.5(8) . . ? C17E C4E C5E 119.5(9) . . ? C20E C5E C6E 123.4(9) . . ? C20E C5E C4E 117.9(9) . . ? C6E C5E C4E 118.7(8) . . ? C7E C6E C1E 117.3(9) . . ? C7E C6E C5E 121.7(9) . . ? C1E C6E C5E 121.0(7) . . ? C8E C7E C6E 120.8(11) . . ? C9E C8E C7E 122.2(9) . . ? C8E C9E C10E 120.1(9) . . ? C9E C10E C1E 118.7(9) . . ? C9E C10E C11E 121.5(10) . . ? C1E C10E C11E 119.7(9) . . ? C12E C11E C10E 120.2(10) . . ? C11E C12E C13E 120.7(10) . . ? C2E C13E C12E 120.6(10) . . ? C3E C14E C15E 120.9(11) . . ? C16E C15E C14E 120.0(10) . . ? C15E C16E C17E 121.8(10) . . ? C16E C17E C18E 122.8(11) . . ? C16E C17E C4E 118.3(10) . . ? C18E C17E C4E 118.8(10) . . ? C19E C18E C17E 120.4(10) . . ? C18E C19E C20E 121.5(10) . . ? C5E C20E C19E 121.8(11) . . ? C2F C1F C6F 121.9(13) . . ? C3F C2F C1F 118.6(13) . . ? C2F C3F C7F 118.9(14) . . ? C2F C3F C4F 121.6(15) . . ? C7F C3F C4F 119.5(13) . . ? C5F C4F C10F 120.4(9) . 2_765 ? C5F C4F C3F 120.5(11) . . ? C10F C4F C3F 119.1(12) 2_765 . ? C6F C5F C4F 117.4(12) . . ? C6F C5F C10F 122.7(12) . . ? C4F C5F C10F 119.8(9) . . ? C5F C6F C1F 120.1(15) . . ? C8F C7F C3F 118.8(13) 2_765 . ? C7F C8F C9F 124.5(16) 2_765 . ? C8F C9F C10F 119.2(16) . . ? C9F C10F C4F 118.8(12) . 2_765 ? C9F C10F C5F 121.4(11) . . ? C4F C10F C5F 119.8(9) 2_765 . ? C2G C1G C6G 120.8(11) . . ? C1G C2G C3G 121.2(10) . . ? C7G C3G C2G 121.7(10) . . ? C7G C3G C4G 119.5(9) . . ? C2G C3G C4G 118.8(9) . . ? C3G C4G C10G 119.3(8) . 2_566 ? C3G C4G C5G 119.3(8) . . ? C10G C4G C5G 121.4(8) 2_566 . ? C6G C5G C4G 119.1(9) . . ? C6G C5G C10G 121.8(9) . . ? C4G C5G C10G 119.2(8) . . ? C5G C6G C1G 120.7(11) . . ? C8G C7G C3G 119.7(9) 2_566 . ? C7G C8G C9G 122.0(9) 2_566 . ? C8G C9G C10G 121.1(9) . . ? C9G C10G C4G 118.3(8) . 2_566 ? C9G C10G C5G 122.2(8) . . ? C4G C10G C5G 119.4(7) 2_566 . ? Cl2 C21 Cl1 107.1(11) . . ? Cl5 C23 Cl6 101.8(15) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.967 _refine_diff_density_min -2.121 _refine_diff_density_rms 0.237 #========================================================================== data_compound2 _database_code_depnum_ccdc_archive 'CCDC 232005' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H75 Mo12 N O40 P' _chemical_formula_weight 3377.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 13.9695(2) _cell_length_b 14.1207(2) _cell_length_c 27.5570(3) _cell_angle_alpha 87.3761(5) _cell_angle_beta 89.5155(5) _cell_angle_gamma 86.1853(5) _cell_volume 5418.06(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 373003 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3306 _exptl_absorpt_coefficient_mu 1.446 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 156704 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.43 _reflns_number_total 24555 _reflns_number_gt 19007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; 'HKL Denzo & Scalepack (Otwinowski & Minor 1997)' ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+7.1583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24555 _refine_ls_number_parameters 1586 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _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 P1 P 0.45037(7) 0.54479(7) 0.24341(4) 0.027 Uani 1 1 d . . . Mo1 Mo 0.26729(3) 0.40599(3) 0.295060(15) 0.036 Uani 1 1 d . . . Mo2 Mo 0.43407(3) 0.49064(3) 0.370823(14) 0.035 Uani 1 1 d . . . Mo3 Mo 0.26172(3) 0.64558(3) 0.316196(15) 0.037 Uani 1 1 d . . . Mo4 Mo 0.26197(3) 0.67862(3) 0.180925(16) 0.043 Uani 1 1 d . . . Mo5 Mo 0.29867(3) 0.43527(3) 0.162346(15) 0.036 Uani 1 1 d . . . Mo6 Mo 0.47886(3) 0.29193(3) 0.235691(16) 0.039 Uani 1 1 d . . . Mo7 Mo 0.64439(3) 0.40610(3) 0.300194(15) 0.037 Uani 1 1 d . . . Mo8 Mo 0.60075(3) 0.66190(3) 0.321420(15) 0.037 Uani 1 1 d . . . Mo9 Mo 0.43124(3) 0.79803(3) 0.253897(16) 0.038 Uani 1 1 d . . . Mo10 Mo 0.62654(3) 0.69350(3) 0.195449(17) 0.043 Uani 1 1 d . . . Mo11 Mo 0.45640(3) 0.59378(3) 0.114734(15) 0.039 Uani 1 1 d . . . Mo12 Mo 0.64002(3) 0.43195(3) 0.175241(16) 0.039 Uani 1 1 d . . . O1 O 0.1880(3) 0.3279(3) 0.31302(14) 0.052 Uani 1 1 d . . . O2 O 0.4457(3) 0.4726(3) 0.43099(12) 0.049 Uani 1 1 d . . . O3 O 0.1682(2) 0.7043(3) 0.34118(14) 0.051 Uani 1 1 d . . . O4 O 0.2048(3) 0.5194(2) 0.31193(13) 0.047 Uani 1 1 d . . . O5 O 0.3394(3) 0.4090(2) 0.35739(13) 0.047 Uani 1 1 d . . . O6 O 0.3269(3) 0.5923(2) 0.37043(13) 0.046 Uani 1 1 d . . . O7 O 0.2257(3) 0.6528(3) 0.24589(13) 0.049 Uani 1 1 d . . . O8 O 0.2476(3) 0.4237(3) 0.22955(12) 0.047 Uani 1 1 d . . . O9 O 0.3804(3) 0.3217(3) 0.27727(12) 0.048 Uani 1 1 d . . . O10 O 0.5347(2) 0.4190(2) 0.34601(13) 0.045 Uani 1 1 d . . . O11 O 0.5109(3) 0.6008(2) 0.35745(13) 0.047 Uani 1 1 d . . . O12 O 0.3441(3) 0.7367(3) 0.30043(12) 0.047 Uani 1 1 d . . . O13 O 0.3495(2) 0.7644(3) 0.20609(13) 0.048 Uani 1 1 d . . . O14 O 0.1725(3) 0.7516(3) 0.15898(15) 0.056 Uani 1 1 d . . . O15 O 0.2192(2) 0.5581(2) 0.16257(14) 0.048 Uani 1 1 d . . . O16 O 0.2236(3) 0.3713(3) 0.13289(14) 0.058 Uani 1 1 d . . . O17 O 0.3943(3) 0.3469(3) 0.18369(12) 0.048 Uani 1 1 d . . . O18 O 0.4733(3) 0.1753(2) 0.22868(14) 0.054 Uani 1 1 d . . . O19 O 0.5765(3) 0.2937(3) 0.28140(13) 0.049 Uani 1 1 d . . . O20 O 0.7293(3) 0.3500(3) 0.33538(15) 0.056 Uani 1 1 d . . . O21 O 0.6581(2) 0.5324(2) 0.30930(13) 0.046 Uani 1 1 d . . . O22 O 0.6759(3) 0.6979(3) 0.36279(14) 0.053 Uani 1 1 d . . . O23 O 0.5241(3) 0.7724(3) 0.30828(13) 0.048 Uani 1 1 d . . . O24 O 0.4037(3) 0.9133(2) 0.26031(15) 0.058 Uani 1 1 d . . . O25 O 0.5380(3) 0.7999(3) 0.21285(13) 0.048 Uani 1 1 d . . . O26 O 0.3453(3) 0.6735(2) 0.12377(13) 0.049 Uani 1 1 d . . . O27 O 0.3687(3) 0.4883(2) 0.11220(13) 0.048 Uani 1 1 d . . . O28 O 0.5807(3) 0.3185(3) 0.18625(13) 0.050 Uani 1 1 d . . . O29 O 0.7030(3) 0.4040(3) 0.23946(13) 0.047 Uani 1 1 d . . . O30 O 0.6744(2) 0.6934(3) 0.26104(13) 0.049 Uani 1 1 d . . . O31 O 0.5373(2) 0.6718(2) 0.14491(14) 0.048 Uani 1 1 d . . . O32 O 0.5517(3) 0.4887(2) 0.13347(14) 0.049 Uani 1 1 d . . . O33 O 0.6710(3) 0.5649(2) 0.19067(14) 0.049 Uani 1 1 d . . . O34 O 0.7090(3) 0.7536(3) 0.16574(15) 0.055 Uani 1 1 d . . . O35 O 0.4785(3) 0.6126(3) 0.05563(13) 0.059 Uani 1 1 d . . . O36 O 0.7320(3) 0.3977(3) 0.13968(14) 0.054 Uani 1 1 d . . . O37 O 0.3834(2) 0.5292(2) 0.28674(12) 0.039 Uani 1 1 d . . . O38 O 0.3920(2) 0.5574(2) 0.19658(12) 0.040 Uani 1 1 d . . . O39 O 0.5219(2) 0.4581(2) 0.24018(12) 0.040 Uani 1 1 d . . . O40 O 0.5043(2) 0.6344(2) 0.25029(12) 0.041 Uani 1 1 d . . . C1A C 0.8861(4) 0.9145(4) 0.5232(2) 0.044 Uani 1 1 d . . . C2A C 0.8970(4) 0.9325(4) 0.4728(2) 0.047 Uani 1 1 d . . . C3A C 0.8840(4) 1.0298(4) 0.45232(19) 0.044 Uani 1 1 d . . . C4A C 0.8596(4) 1.1046(3) 0.48367(18) 0.041 Uani 1 1 d . . . C5A C 0.8486(4) 1.0866(4) 0.53498(18) 0.043 Uani 1 1 d . . . C6A C 0.8618(4) 0.9892(4) 0.5552(2) 0.046 Uani 1 1 d . . . C7A C 0.8518(4) 0.9662(4) 0.6044(2) 0.056 Uani 1 1 d . . . H7A H 0.8372 1.0149 0.6254 0.068 Uiso 1 1 calc R . . C8A C 0.8626(5) 0.8741(5) 0.6234(2) 0.065 Uani 1 1 d . . . H8A H 0.8537 0.8613 0.6565 0.078 Uiso 1 1 calc R . . C9A C 0.8869(5) 0.8007(4) 0.5929(2) 0.067 Uani 1 1 d . . . H9A H 0.8950 0.7387 0.6058 0.080 Uiso 1 1 calc R . . C10A C 0.8994(4) 0.8192(4) 0.5431(2) 0.058 Uani 1 1 d . . . C11A C 0.9229(5) 0.7460(4) 0.5114(3) 0.072 Uani 1 1 d . . . H11A H 0.9319 0.6837 0.5239 0.086 Uiso 1 1 calc R . . C12A C 0.9326(5) 0.7642(4) 0.4633(3) 0.075 Uani 1 1 d . . . H12A H 0.9474 0.7144 0.4430 0.090 Uiso 1 1 calc R . . C13A C 0.9211(5) 0.8557(4) 0.4437(3) 0.066 Uani 1 1 d . . . H13A H 0.9295 0.8666 0.4105 0.079 Uiso 1 1 calc R . . C14A C 0.8951(4) 1.0533(4) 0.4030(2) 0.055 Uani 1 1 d . . . H14A H 0.9098 1.0048 0.3819 0.066 Uiso 1 1 calc R . . C15A C 0.8850(5) 1.1463(5) 0.3840(2) 0.063 Uani 1 1 d . . . H15A H 0.8954 1.1595 0.3511 0.075 Uiso 1 1 calc R . . C16A C 0.8593(4) 1.2188(4) 0.4144(2) 0.056 Uani 1 1 d . . . H16A H 0.8505 1.2809 0.4016 0.067 Uiso 1 1 calc R . . C17A C 0.8465(4) 1.2002(4) 0.4644(2) 0.046 Uani 1 1 d . . . C18A C 0.8226(5) 1.2733(4) 0.4955(2) 0.059 Uani 1 1 d . . . H18A H 0.8145 1.3356 0.4830 0.070 Uiso 1 1 calc R . . C19A C 0.8107(5) 1.2541(4) 0.5445(2) 0.062 Uani 1 1 d . . . H19A H 0.7940 1.3035 0.5648 0.075 Uiso 1 1 calc R . . C20A C 0.8232(4) 1.1628(4) 0.5636(2) 0.055 Uani 1 1 d . . . H20A H 0.8145 1.1515 0.5968 0.066 Uiso 1 1 calc R . . C1B C 0.6262(4) 0.9341(4) 0.5426(2) 0.045 Uani 1 1 d . . . C2B C 0.6392(3) 0.9431(4) 0.49142(19) 0.043 Uani 1 1 d . . . C3B C 0.6287(3) 1.0358(4) 0.46668(18) 0.042 Uani 1 1 d . . . C4B C 0.6053(3) 1.1170(3) 0.49449(18) 0.040 Uani 1 1 d . . . C5B C 0.5914(4) 1.1088(4) 0.54558(18) 0.043 Uani 1 1 d . . . C6B C 0.6025(4) 1.0148(4) 0.5705(2) 0.046 Uani 1 1 d . . . C7B C 0.5911(5) 1.0015(5) 0.6207(2) 0.063 Uani 1 1 d . . . H7B H 0.5766 1.0541 0.6392 0.075 Uiso 1 1 calc R . . C8B C 0.6007(5) 0.9122(5) 0.6437(2) 0.070 Uani 1 1 d . . . H8B H 0.5926 0.9054 0.6772 0.084 Uiso 1 1 calc R . . C9B C 0.6219(5) 0.8352(5) 0.6175(3) 0.073 Uani 1 1 d . . . H9B H 0.6272 0.7755 0.6333 0.088 Uiso 1 1 calc R . . C10B C 0.6361(4) 0.8428(4) 0.5669(2) 0.057 Uani 1 1 d . . . C11B C 0.6584(5) 0.7628(4) 0.5391(3) 0.070 Uani 1 1 d . . . H11B H 0.6634 0.7028 0.5546 0.084 Uiso 1 1 calc R . . C12B C 0.6727(5) 0.7710(4) 0.4906(3) 0.069 Uani 1 1 d . . . H12B H 0.6897 0.7173 0.4734 0.082 Uiso 1 1 calc R . . C13B C 0.6621(4) 0.8604(4) 0.4662(2) 0.060 Uani 1 1 d . . . H13B H 0.6704 0.8650 0.4326 0.072 Uiso 1 1 calc R . . C14B C 0.6418(4) 1.0503(4) 0.4166(2) 0.055 Uani 1 1 d . . . H14B H 0.6587 0.9983 0.3981 0.066 Uiso 1 1 calc R . . C15B C 0.6303(5) 1.1399(5) 0.3936(2) 0.062 Uani 1 1 d . . . H15B H 0.6386 1.1470 0.3601 0.074 Uiso 1 1 calc R . . C16B C 0.6071(4) 1.2170(5) 0.4201(2) 0.061 Uani 1 1 d . . . H16B H 0.6000 1.2767 0.4043 0.073 Uiso 1 1 calc R . . C17B C 0.5936(4) 1.2088(4) 0.4704(2) 0.050 Uani 1 1 d . . . C18B C 0.5691(5) 1.2880(4) 0.4976(2) 0.063 Uani 1 1 d . . . H18B H 0.5617 1.3478 0.4820 0.076 Uiso 1 1 calc R . . C19B C 0.5558(5) 1.2795(4) 0.5470(3) 0.068 Uani 1 1 d . . . H19B H 0.5394 1.3330 0.5645 0.082 Uiso 1 1 calc R . . C20B C 0.5668(5) 1.1913(4) 0.5705(2) 0.059 Uani 1 1 d . . . H20B H 0.5575 1.1863 0.6040 0.071 Uiso 1 1 calc R . . C1C C 0.3799(3) 0.9429(3) -0.04298(17) 0.037 Uani 1 1 d . . . C2C C 0.3981(3) 1.0411(3) -0.04839(18) 0.037 Uani 1 1 d . . . C3C C 0.3931(3) 1.0989(3) -0.00566(19) 0.039 Uani 1 1 d . . . C4C C 0.3714(3) 1.0551(3) 0.04020(18) 0.037 Uani 1 1 d . . . C5C C 0.3535(3) 0.9579(3) 0.04587(18) 0.039 Uani 1 1 d . . . C6C C 0.3577(3) 0.8998(3) 0.00345(18) 0.037 Uani 1 1 d . . . C7C C 0.3399(4) 0.8036(4) 0.0058(2) 0.048 Uani 1 1 d . . . H7C H 0.3237 0.7751 0.0356 0.057 Uiso 1 1 calc R . . C8C C 0.3456(4) 0.7492(4) -0.0348(2) 0.055 Uani 1 1 d . . . H8C H 0.3349 0.6848 -0.0318 0.065 Uiso 1 1 calc R . . C9C C 0.3668(4) 0.7897(4) -0.0790(2) 0.054 Uani 1 1 d . . . H9C H 0.3699 0.7526 -0.1061 0.065 Uiso 1 1 calc R . . C10C C 0.3842(4) 0.8865(4) -0.08445(19) 0.044 Uani 1 1 d . . . C11C C 0.4057(4) 0.9286(4) -0.1302(2) 0.054 Uani 1 1 d . . . H11C H 0.4076 0.8921 -0.1575 0.065 Uiso 1 1 calc R . . C12C C 0.4238(4) 1.0228(4) -0.1351(2) 0.054 Uani 1 1 d . . . H12C H 0.4387 1.0495 -0.1655 0.065 Uiso 1 1 calc R . . C13C C 0.4201(4) 1.0783(4) -0.0947(2) 0.050 Uani 1 1 d . . . H13C H 0.4325 1.1421 -0.0986 0.060 Uiso 1 1 calc R . . C14C C 0.4102(4) 1.1950(4) -0.0085(2) 0.049 Uani 1 1 d . . . H14C H 0.4238 1.2236 -0.0386 0.058 Uiso 1 1 calc R . . C15C C 0.4074(4) 1.2493(4) 0.0324(2) 0.056 Uani 1 1 d . . . H15C H 0.4200 1.3132 0.0296 0.067 Uiso 1 1 calc R . . C16C C 0.3862(4) 1.2085(4) 0.0764(2) 0.057 Uani 1 1 d . . . H16C H 0.3835 1.2454 0.1035 0.068 Uiso 1 1 calc R . . C17C C 0.3682(4) 1.1119(4) 0.0817(2) 0.046 Uani 1 1 d . . . C18C C 0.3462(4) 1.0693(5) 0.1275(2) 0.059 Uani 1 1 d . . . H18C H 0.3446 1.1057 0.1548 0.070 Uiso 1 1 calc R . . C19C C 0.3275(4) 0.9760(4) 0.1324(2) 0.054 Uani 1 1 d . . . H19C H 0.3123 0.9494 0.1627 0.064 Uiso 1 1 calc R . . C20C C 0.3310(4) 0.9201(4) 0.09174(19) 0.048 Uani 1 1 d . . . H20C H 0.3181 0.8564 0.0954 0.058 Uiso 1 1 calc R . . C1D C 0.1323(3) 0.9450(4) -0.04811(18) 0.040 Uani 1 1 d . . . C2D C 0.1489(3) 1.0440(4) -0.04982(19) 0.041 Uani 1 1 d . . . C3D C 0.1420(3) 1.0952(4) -0.00499(19) 0.041 Uani 1 1 d . . . C4D C 0.1180(3) 1.0457(3) 0.03925(18) 0.040 Uani 1 1 d . . . C5D C 0.1010(3) 0.9472(4) 0.04079(19) 0.041 Uani 1 1 d . . . C6D C 0.1087(3) 0.8962(3) -0.00402(19) 0.040 Uani 1 1 d . . . C7D C 0.0926(4) 0.7994(4) -0.0054(2) 0.051 Uani 1 1 d . . . H7D H 0.0762 0.7663 0.0231 0.061 Uiso 1 1 calc R . . C8D C 0.1006(4) 0.7517(4) -0.0483(2) 0.060 Uani 1 1 d . . . H8D H 0.0895 0.6875 -0.0482 0.072 Uiso 1 1 calc R . . C9D C 0.1246(4) 0.7979(4) -0.0906(2) 0.060 Uani 1 1 d . . . H9D H 0.1311 0.7647 -0.1190 0.072 Uiso 1 1 calc R . . C10D C 0.1397(4) 0.8966(4) -0.0918(2) 0.049 Uani 1 1 d . . . C11D C 0.1628(4) 0.9453(5) -0.1355(2) 0.060 Uani 1 1 d . . . H11D H 0.1667 0.9128 -0.1641 0.072 Uiso 1 1 calc R . . C12D C 0.1792(4) 1.0383(5) -0.1365(2) 0.059 Uani 1 1 d . . . H12D H 0.1955 1.0689 -0.1658 0.071 Uiso 1 1 calc R . . C13D C 0.1721(4) 1.0889(4) -0.0946(2) 0.053 Uani 1 1 d . . . H13D H 0.1828 1.1533 -0.0961 0.063 Uiso 1 1 calc R . . C14D C 0.1589(4) 1.1924(4) -0.0030(2) 0.051 Uani 1 1 d . . . H14D H 0.1747 1.2256 -0.0315 0.061 Uiso 1 1 calc R . . C15D C 0.1529(4) 1.2393(4) 0.0391(2) 0.058 Uani 1 1 d . . . H15D H 0.1653 1.3033 0.0389 0.069 Uiso 1 1 calc R . . C16D C 0.1289(4) 1.1931(4) 0.0818(2) 0.056 Uani 1 1 d . . . H16D H 0.1236 1.2264 0.1101 0.067 Uiso 1 1 calc R . . C17D C 0.1122(4) 1.0959(4) 0.0831(2) 0.045 Uani 1 1 d . . . C18D C 0.0883(4) 1.0472(4) 0.1264(2) 0.054 Uani 1 1 d . . . H18D H 0.0839 1.0797 0.1550 0.065 Uiso 1 1 calc R . . C19D C 0.0711(4) 0.9522(4) 0.1277(2) 0.053 Uani 1 1 d . . . H19D H 0.0551 0.9209 0.1568 0.064 Uiso 1 1 calc R . . C20D C 0.0781(4) 0.9038(4) 0.0847(2) 0.046 Uani 1 1 d . . . H20D H 0.0668 0.8396 0.0858 0.055 Uiso 1 1 calc R . . C1E C 1.0139(4) 1.1233(4) 0.24873(19) 0.045 Uani 1 1 d . . . C2E C 1.0515(4) 1.0308(4) 0.26236(19) 0.046 Uani 1 1 d . . . C3E C 0.9849(4) 0.9581(4) 0.2781(2) 0.054 Uani 1 1 d . . . C4E C 0.8832(4) 0.9817(4) 0.2772(2) 0.051 Uani 1 1 d . . . C5E C 0.8462(4) 1.0750(4) 0.26243(19) 0.050 Uani 1 1 d . . . C6E C 0.9132(4) 1.1479(4) 0.24869(19) 0.048 Uani 1 1 d . . . C7E C 0.8818(5) 1.2386(4) 0.2345(3) 0.065 Uani 1 1 d . . . H7E H 0.8163 1.2554 0.2350 0.078 Uiso 1 1 calc R . . C8E C 0.9451(5) 1.3071(5) 0.2193(3) 0.078 Uani 1 1 d . . . H8E H 0.9211 1.3677 0.2090 0.094 Uiso 1 1 calc R . . C9E C 1.0407(5) 1.2855(5) 0.2195(3) 0.070 Uani 1 1 d . . . H9E H 1.0821 1.3320 0.2100 0.084 Uiso 1 1 calc R . . C10E C 1.0790(4) 1.1936(4) 0.2338(2) 0.053 Uani 1 1 d . . . C11E C 1.1774(4) 1.1700(4) 0.2333(2) 0.056 Uani 1 1 d . . . H11E H 1.2196 1.2160 0.2241 0.068 Uiso 1 1 calc R . . C12E C 1.2122(4) 1.0801(4) 0.2462(2) 0.057 Uani 1 1 d . . . H12E H 1.2781 1.0654 0.2456 0.068 Uiso 1 1 calc R . . C13E C 1.1506(4) 1.0094(4) 0.2604(2) 0.052 Uani 1 1 d . . . H13E H 1.1756 0.9481 0.2685 0.063 Uiso 1 1 calc R . . C14E C 1.0171(5) 0.8687(5) 0.2952(3) 0.079 Uani 1 1 d . . . H14E H 1.0828 0.8535 0.2971 0.095 Uiso 1 1 calc R . . C15E C 0.9534(6) 0.7996(6) 0.3099(4) 0.100 Uani 1 1 d . . . H15E H 0.9774 0.7395 0.3209 0.119 Uiso 1 1 calc R . . C16E C 0.8572(6) 0.8200(6) 0.3080(3) 0.092 Uani 1 1 d . . . H16E H 0.8157 0.7738 0.3176 0.111 Uiso 1 1 calc R . . C17E C 0.8195(5) 0.9115(5) 0.2916(3) 0.066 Uani 1 1 d . . . C18E C 0.7196(5) 0.9347(5) 0.2888(3) 0.074 Uani 1 1 d . . . H18E H 0.6771 0.8886 0.2972 0.089 Uiso 1 1 calc R . . C19E C 0.6853(5) 1.0229(5) 0.2743(3) 0.073 Uani 1 1 d . . . H19E H 0.6194 1.0371 0.2727 0.087 Uiso 1 1 calc R . . C20E C 0.7475(4) 1.0926(5) 0.2619(2) 0.063 Uani 1 1 d . . . H20E H 0.7221 1.1534 0.2528 0.075 Uiso 1 1 calc R . . C1F C 0.7318(5) 0.5080(6) 0.0021(4) 0.094 Uani 1 1 d . . . H1F H 0.6693 0.5005 -0.0076 0.113 Uiso 1 1 calc R . . C2F C 0.7480(5) 0.5524(6) 0.0439(3) 0.092 Uani 1 1 d . . . H2F H 0.6967 0.5731 0.0633 0.110 Uiso 1 1 calc R . . C3F C 0.8406(5) 0.5664(5) 0.0573(3) 0.075 Uani 1 1 d . . . C4F C 0.9201(4) 0.5335(4) 0.0290(2) 0.054 Uani 1 1 d . . . C5F C 0.9028(4) 0.4846(4) -0.0140(2) 0.052 Uani 1 1 d . . . C6F C 0.8079(5) 0.4744(5) -0.0257(3) 0.076 Uani 1 1 d . . . H6F H 0.7949 0.4433 -0.0537 0.091 Uiso 1 1 calc R . . C7F C 0.8580(7) 0.6171(6) 0.0988(3) 0.097 Uani 1 1 d . . . H7F H 0.8065 0.6389 0.1178 0.117 Uiso 1 1 calc R . . C8F C 1.0511(9) 0.3654(6) -0.1117(3) 0.111 Uani 1 1 d . . . H8F H 1.0414 0.3312 -0.1390 0.133 Uiso 1 1 calc R . . C9F C 0.9717(6) 0.3987(5) -0.0838(3) 0.083 Uani 1 1 d . . . H9F H 0.9102 0.3855 -0.0930 0.099 Uiso 1 1 calc R . . C10F C 0.9836(4) 0.4503(4) -0.0434(2) 0.055 Uani 1 1 d . . . C1G C 0.0176(6) 0.4962(6) 0.6353(3) 0.087 Uani 1 1 d . . . H1G H -0.0014 0.4975 0.6677 0.104 Uiso 1 1 calc R . . C2G C -0.1130(5) 0.5095(5) 0.3762(2) 0.073 Uani 1 1 d . . . H2G H -0.1584 0.5133 0.3516 0.087 Uiso 1 1 calc R . . C3G C -0.1431(4) 0.5097(4) 0.4254(2) 0.054 Uani 1 1 d . . . C4G C -0.0718(4) 0.5054(3) 0.46254(19) 0.043 Uani 1 1 d . . . C5G C -0.0284(4) 0.4994(3) 0.55030(19) 0.046 Uani 1 1 d . . . C6G C -0.0517(5) 0.5001(5) 0.5991(2) 0.068 Uani 1 1 d . . . H6G H -0.1161 0.5033 0.6081 0.082 Uiso 1 1 calc R . . C7G C -0.2403(4) 0.5158(4) 0.4381(2) 0.058 Uani 1 1 d . . . H7G H -0.2866 0.5197 0.4139 0.070 Uiso 1 1 calc R . . C8G C -0.2677(4) 0.5161(4) 0.4855(2) 0.057 Uani 1 1 d . . . H8G H -0.3326 0.5192 0.4935 0.069 Uiso 1 1 calc R . . C9G C -0.1996(4) 0.5117(4) 0.5223(2) 0.051 Uani 1 1 d . . . H9G H -0.2201 0.5135 0.5544 0.061 Uiso 1 1 calc R . . C10G C -0.1007(4) 0.5046(3) 0.51222(19) 0.044 Uani 1 1 d . . . N1 N 0.8606(6) 0.5770(9) 0.2436(4) 0.162 Uani 1 1 d . . . C21 C 0.9387(8) 0.5689(8) 0.2374(3) 0.133 Uani 1 1 d D . . C22 C 1.0380(6) 0.5536(9) 0.2277(4) 0.135 Uani 1 1 d D . . H22A H 1.0645 0.5021 0.2484 0.202 Uiso 1 1 calc R . . H22B H 1.0697 0.6102 0.2337 0.202 Uiso 1 1 calc R . . H22C H 1.0473 0.5382 0.1943 0.202 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.029 0.024 0.026 0.001 0.001 -0.001 Mo1 0.036 0.034 0.037 0.002 0.006 -0.008 Mo2 0.044 0.034 0.026 0.002 0.002 0.000 Mo3 0.035 0.039 0.037 -0.004 0.006 0.005 Mo4 0.039 0.044 0.043 0.006 -0.009 0.007 Mo5 0.040 0.038 0.033 -0.003 -0.003 -0.009 Mo6 0.051 0.026 0.039 -0.002 0.006 -0.001 Mo7 0.036 0.037 0.036 0.003 -0.003 0.007 Mo8 0.036 0.038 0.037 -0.004 -0.004 -0.006 Mo9 0.041 0.026 0.045 0.002 0.000 0.000 Mo10 0.041 0.041 0.048 0.001 0.009 -0.013 Mo11 0.041 0.046 0.029 0.008 0.001 -0.004 Mo12 0.037 0.041 0.039 -0.006 0.009 0.003 O1 0.051 0.051 0.055 0.011 0.005 -0.016 O2 0.068 0.048 0.031 0.003 0.003 0.002 O3 0.040 0.057 0.053 -0.006 0.011 0.010 O4 0.049 0.041 0.049 -0.002 -0.004 -0.001 O5 0.055 0.038 0.047 0.002 -0.007 -0.002 O6 0.053 0.038 0.047 -0.006 -0.006 0.005 O7 0.048 0.057 0.043 0.006 -0.001 -0.010 O8 0.052 0.052 0.035 0.002 0.008 0.004 O9 0.057 0.050 0.035 0.002 0.005 0.010 O10 0.050 0.036 0.049 -0.005 0.012 -0.001 O11 0.050 0.037 0.053 -0.003 0.011 -0.003 O12 0.049 0.054 0.039 0.004 -0.001 -0.010 O13 0.045 0.056 0.044 0.006 0.002 -0.013 O14 0.049 0.051 0.067 0.009 -0.011 0.009 O15 0.043 0.041 0.058 0.004 0.004 -0.004 O16 0.056 0.073 0.048 -0.014 -0.004 -0.021 O17 0.059 0.048 0.035 0.003 0.006 0.005 O18 0.073 0.031 0.057 -0.006 0.006 0.002 O19 0.058 0.045 0.043 0.002 0.000 -0.007 O20 0.046 0.052 0.066 0.014 -0.009 0.011 O21 0.044 0.041 0.054 -0.003 0.011 -0.003 O22 0.050 0.061 0.052 -0.006 -0.012 -0.011 O23 0.049 0.047 0.046 0.000 0.002 0.003 O24 0.077 0.031 0.066 0.001 0.003 0.002 O25 0.049 0.049 0.045 0.005 0.003 0.001 O26 0.049 0.044 0.052 0.009 0.008 -0.003 O27 0.049 0.046 0.049 -0.001 0.006 -0.009 O28 0.063 0.049 0.040 -0.005 0.006 -0.009 O29 0.049 0.052 0.042 0.000 0.001 -0.006 O30 0.042 0.059 0.045 0.003 0.001 0.002 O31 0.047 0.037 0.058 0.001 -0.010 0.001 O32 0.049 0.042 0.056 -0.004 -0.009 0.000 O33 0.046 0.039 0.061 -0.002 -0.006 -0.002 O34 0.050 0.053 0.064 0.005 0.012 -0.016 O35 0.073 0.066 0.036 0.010 0.002 -0.013 O36 0.049 0.060 0.051 -0.004 0.014 0.007 O37 0.042 0.038 0.038 0.000 0.001 0.000 O38 0.042 0.043 0.036 0.001 0.000 -0.001 O39 0.044 0.037 0.038 0.001 0.002 0.001 O40 0.042 0.038 0.042 0.000 0.000 -0.002 C1A 0.040 0.039 0.052 0.002 -0.003 -0.004 C2A 0.045 0.041 0.055 -0.009 -0.001 -0.006 C3A 0.042 0.047 0.043 -0.006 -0.003 -0.006 C4A 0.043 0.039 0.040 -0.003 -0.003 -0.003 C5A 0.044 0.046 0.041 -0.003 -0.002 -0.009 C6A 0.042 0.047 0.049 -0.001 -0.004 -0.011 C7A 0.064 0.060 0.046 0.006 -0.004 -0.011 C8A 0.072 0.063 0.060 0.015 -0.005 -0.014 C9A 0.075 0.051 0.074 0.021 -0.006 -0.014 C10A 0.056 0.042 0.075 0.005 -0.005 -0.008 C11A 0.080 0.040 0.095 0.000 -0.005 -0.009 C12A 0.093 0.043 0.091 -0.023 -0.003 -0.002 C13A 0.076 0.057 0.067 -0.017 0.000 -0.003 C14A 0.065 0.058 0.042 -0.010 0.001 -0.004 C15A 0.074 0.077 0.037 0.002 -0.004 -0.010 C16A 0.069 0.050 0.048 0.009 -0.009 -0.004 C17A 0.047 0.043 0.049 -0.001 -0.010 -0.001 C18A 0.076 0.041 0.059 -0.001 -0.006 -0.003 C19A 0.082 0.050 0.054 -0.013 0.000 -0.001 C20A 0.069 0.054 0.041 -0.007 -0.001 -0.001 C1B 0.039 0.046 0.050 0.003 -0.008 -0.004 C2B 0.038 0.042 0.050 -0.002 -0.007 -0.003 C3B 0.041 0.045 0.042 -0.004 -0.004 -0.005 C4B 0.041 0.039 0.040 -0.002 -0.001 -0.002 C5B 0.043 0.047 0.041 -0.004 -0.001 -0.007 C6B 0.047 0.047 0.046 0.002 -0.003 -0.006 C7B 0.071 0.073 0.046 0.002 -0.003 -0.012 C8B 0.076 0.085 0.050 0.018 -0.005 -0.019 C9B 0.070 0.064 0.082 0.036 -0.013 -0.010 C10B 0.053 0.049 0.067 0.012 -0.011 -0.005 C11B 0.069 0.040 0.100 0.013 -0.016 0.000 C12B 0.075 0.034 0.096 -0.012 -0.006 0.005 C13B 0.064 0.049 0.068 -0.012 -0.007 0.000 C14B 0.061 0.057 0.046 -0.005 0.005 0.000 C15B 0.068 0.078 0.038 0.010 0.000 -0.005 C16B 0.060 0.059 0.060 0.014 -0.003 -0.002 C17B 0.052 0.044 0.053 0.005 -0.001 -0.006 C18B 0.079 0.038 0.073 0.001 -0.005 -0.006 C19B 0.089 0.048 0.069 -0.018 0.000 -0.003 C20B 0.074 0.052 0.053 -0.013 0.003 -0.010 C1C 0.030 0.039 0.041 0.004 0.000 0.001 C2C 0.027 0.041 0.043 0.007 0.001 0.000 C3C 0.029 0.036 0.051 0.002 0.002 -0.002 C4C 0.025 0.043 0.044 -0.001 -0.002 0.002 C5C 0.032 0.044 0.040 0.005 0.000 0.006 C6C 0.028 0.039 0.043 0.005 -0.002 0.000 C7C 0.047 0.043 0.053 0.006 -0.001 -0.005 C8C 0.060 0.038 0.066 -0.004 -0.001 -0.004 C9C 0.057 0.051 0.056 -0.012 -0.003 -0.004 C10C 0.041 0.045 0.046 -0.003 0.001 0.002 C11C 0.053 0.069 0.039 -0.009 0.000 0.008 C12C 0.052 0.072 0.038 0.010 0.005 -0.002 C13C 0.042 0.050 0.056 0.012 0.004 -0.002 C14C 0.042 0.043 0.061 0.006 -0.004 -0.007 C15C 0.049 0.041 0.078 -0.007 0.002 -0.003 C16C 0.052 0.053 0.067 -0.018 -0.003 0.003 C17C 0.039 0.045 0.055 -0.008 -0.001 0.003 C18C 0.052 0.080 0.043 -0.015 0.000 0.008 C19C 0.055 0.064 0.041 0.003 0.007 0.002 C20C 0.044 0.051 0.047 0.009 0.004 -0.001 C1D 0.032 0.044 0.046 -0.001 -0.006 -0.002 C2D 0.028 0.046 0.049 0.006 -0.004 -0.004 C3D 0.027 0.046 0.049 0.003 -0.006 -0.006 C4D 0.031 0.043 0.046 0.000 -0.006 -0.003 C5D 0.030 0.044 0.047 0.003 -0.007 0.001 C6D 0.032 0.037 0.050 -0.002 -0.004 -0.001 C7D 0.053 0.039 0.061 0.004 -0.005 -0.007 C8D 0.065 0.042 0.075 -0.008 -0.008 -0.005 C9D 0.059 0.063 0.058 -0.014 -0.004 -0.004 C10D 0.038 0.059 0.049 -0.003 -0.003 -0.002 C11D 0.057 0.076 0.047 -0.008 0.000 -0.008 C12D 0.056 0.078 0.044 0.010 0.000 -0.012 C13D 0.044 0.061 0.054 0.006 -0.001 -0.010 C14D 0.049 0.042 0.062 0.010 -0.007 -0.010 C15D 0.057 0.042 0.075 -0.004 -0.015 -0.009 C16D 0.051 0.055 0.062 -0.011 -0.010 -0.004 C17D 0.036 0.048 0.050 -0.005 -0.006 -0.002 C18D 0.046 0.067 0.049 -0.005 -0.007 -0.001 C19D 0.048 0.063 0.046 0.009 -0.003 -0.001 C20D 0.043 0.044 0.051 0.005 -0.005 -0.003 C1E 0.046 0.046 0.042 -0.010 -0.002 0.003 C2E 0.046 0.049 0.042 -0.009 -0.003 0.002 C3E 0.050 0.050 0.060 -0.002 -0.005 -0.001 C4E 0.046 0.063 0.046 -0.010 0.000 -0.007 C5E 0.046 0.063 0.041 -0.013 0.001 0.003 C6E 0.049 0.056 0.039 -0.010 -0.001 0.003 C7E 0.054 0.053 0.084 -0.004 -0.011 0.012 C8E 0.079 0.051 0.105 -0.001 -0.015 0.002 C9E 0.070 0.056 0.083 -0.006 0.000 -0.007 C10E 0.060 0.055 0.046 -0.012 0.000 -0.009 C11E 0.055 0.055 0.061 -0.010 0.005 -0.010 C12E 0.045 0.069 0.056 -0.010 0.001 0.000 C13E 0.049 0.050 0.058 -0.006 -0.004 0.001 C14E 0.055 0.066 0.115 0.016 -0.009 -0.002 C15E 0.080 0.064 0.152 0.036 -0.017 -0.011 C16E 0.076 0.084 0.119 0.017 -0.005 -0.031 C17E 0.055 0.067 0.076 -0.003 -0.002 -0.012 C18E 0.059 0.080 0.086 -0.011 0.006 -0.020 C19E 0.047 0.095 0.077 -0.019 0.005 -0.008 C20E 0.051 0.076 0.061 -0.013 -0.001 0.003 C1F 0.047 0.099 0.131 0.056 -0.012 -0.004 C2F 0.059 0.104 0.104 0.052 0.025 0.014 C3F 0.078 0.075 0.066 0.023 0.018 0.016 C4F 0.058 0.050 0.051 0.015 0.002 0.002 C5F 0.049 0.052 0.052 0.016 -0.006 -0.004 C6F 0.067 0.077 0.081 0.024 -0.022 -0.013 C7F 0.119 0.100 0.066 0.008 0.029 0.033 C8F 0.184 0.089 0.056 -0.011 0.008 0.022 C9F 0.112 0.084 0.053 -0.003 -0.016 -0.013 C10F 0.066 0.057 0.043 0.008 -0.008 -0.005 C1G 0.083 0.132 0.046 0.005 0.010 -0.011 C2G 0.071 0.098 0.049 0.009 -0.004 -0.012 C3G 0.062 0.042 0.057 0.005 0.008 -0.006 C4G 0.051 0.030 0.048 0.001 0.007 -0.003 C5G 0.058 0.034 0.044 0.003 0.013 -0.003 C6G 0.062 0.095 0.046 0.005 0.012 -0.012 C7G 0.059 0.048 0.067 0.005 -0.003 -0.003 C8G 0.050 0.046 0.076 -0.004 0.005 0.001 C9G 0.054 0.041 0.057 -0.006 0.019 -0.002 C10G 0.056 0.026 0.051 -0.005 0.012 -0.004 N1 0.073 0.255 0.155 0.012 -0.008 -0.004 C21 0.228 0.120 0.055 0.026 -0.048 -0.045 C22 0.078 0.182 0.139 0.055 -0.014 -0.013 _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 P1 O37 1.528(3) . ? P1 O38 1.529(3) . ? P1 O39 1.533(3) . ? P1 O40 1.535(3) . ? Mo1 O1 1.670(3) . ? Mo1 O8 1.832(3) . ? Mo1 O4 1.849(3) . ? Mo1 O9 1.986(3) . ? Mo1 O5 2.002(3) . ? Mo1 O37 2.458(3) . ? Mo2 O2 1.674(3) . ? Mo2 O10 1.824(3) . ? Mo2 O5 1.861(4) . ? Mo2 O11 1.967(3) . ? Mo2 O6 2.003(3) . ? Mo2 O37 2.455(3) . ? Mo3 O3 1.662(3) . ? Mo3 O12 1.818(4) . ? Mo3 O6 1.860(3) . ? Mo3 O7 2.002(4) . ? Mo3 O4 2.007(3) . ? Mo3 O37 2.445(3) . ? Mo4 O14 1.666(3) . ? Mo4 O7 1.882(4) . ? Mo4 O15 1.931(4) . ? Mo4 O13 1.932(4) . ? Mo4 O26 1.951(4) . ? Mo4 O38 2.439(3) . ? Mo5 O16 1.668(4) . ? Mo5 O27 1.846(4) . ? Mo5 O17 1.848(4) . ? Mo5 O8 1.983(3) . ? Mo5 O15 1.996(3) . ? Mo5 O38 2.456(3) . ? Mo6 O18 1.674(3) . ? Mo6 O9 1.822(3) . ? Mo6 O19 1.867(4) . ? Mo6 O17 1.963(4) . ? Mo6 O28 2.003(4) . ? Mo6 O39 2.470(3) . ? Mo7 O20 1.673(3) . ? Mo7 O21 1.835(3) . ? Mo7 O29 1.857(4) . ? Mo7 O10 1.981(3) . ? Mo7 O19 1.993(4) . ? Mo7 O39 2.444(3) . ? Mo8 O22 1.675(3) . ? Mo8 O11 1.831(3) . ? Mo8 O23 1.856(3) . ? Mo8 O21 1.989(3) . ? Mo8 O30 1.998(4) . ? Mo8 O40 2.448(3) . ? Mo9 O24 1.665(4) . ? Mo9 O13 1.849(4) . ? Mo9 O25 1.865(4) . ? Mo9 O12 1.972(3) . ? Mo9 O23 1.996(4) . ? Mo9 O40 2.468(3) . ? Mo10 O34 1.664(4) . ? Mo10 O33 1.889(3) . ? Mo10 O31 1.926(3) . ? Mo10 O30 1.933(4) . ? Mo10 O25 1.956(4) . ? Mo10 O40 2.435(3) . ? Mo11 O35 1.668(4) . ? Mo11 O31 1.856(3) . ? Mo11 O26 1.878(4) . ? Mo11 O32 1.980(3) . ? Mo11 O27 1.994(3) . ? Mo11 O38 2.466(3) . ? Mo12 O36 1.668(4) . ? Mo12 O32 1.816(3) . ? Mo12 O28 1.863(4) . ? Mo12 O29 1.994(4) . ? Mo12 O33 2.020(3) . ? Mo12 O39 2.448(3) . ? C1A C2A 1.411(7) . ? C1A C6A 1.428(7) . ? C1A C10A 1.431(7) . ? C2A C13A 1.398(8) . ? C2A C3A 1.461(7) . ? C3A C14A 1.395(7) . ? C3A C4A 1.418(7) . ? C4A C17A 1.429(7) . ? C4A C5A 1.434(7) . ? C5A C20A 1.389(7) . ? C5A C6A 1.461(7) . ? C6A C7A 1.387(8) . ? C7A C8A 1.379(8) . ? C7A H7A 0.9300 . ? C8A C9A 1.386(9) . ? C8A H8A 0.9300 . ? C9A C10A 1.397(9) . ? C9A H9A 0.9300 . ? C10A C11A 1.405(9) . ? C11A C12A 1.346(10) . ? C11A H11A 0.9300 . ? C12A C13A 1.376(9) . ? C12A H12A 0.9300 . ? C13A H13A 0.9300 . ? C14A C15A 1.388(8) . ? C14A H14A 0.9300 . ? C15A C16A 1.380(9) . ? C15A H15A 0.9300 . ? C16A C17A 1.402(8) . ? C16A H16A 0.9300 . ? C17A C18A 1.392(8) . ? C18A C19A 1.376(8) . ? C18A H18A 0.9300 . ? C19A C20A 1.373(8) . ? C19A H19A 0.9300 . ? C20A H20A 0.9300 . ? C1B C6B 1.421(7) . ? C1B C2B 1.422(7) . ? C1B C10B 1.424(7) . ? C2B C13B 1.403(8) . ? C2B C3B 1.447(7) . ? C3B C14B 1.398(7) . ? C3B C4B 1.427(7) . ? C4B C5B 1.420(7) . ? C4B C17B 1.429(7) . ? C5B C20B 1.400(7) . ? C5B C6B 1.466(7) . ? C6B C7B 1.398(8) . ? C7B C8B 1.384(9) . ? C7B H7B 0.9300 . ? C8B C9B 1.349(10) . ? C8B H8B 0.9300 . ? C9B C10B 1.408(9) . ? C9B H9B 0.9300 . ? C10B C11B 1.409(9) . ? C11B C12B 1.349(10) . ? C11B H11B 0.9300 . ? C12B C13B 1.404(9) . ? C12B H12B 0.9300 . ? C13B H13B 0.9300 . ? C14B C15B 1.389(8) . ? C14B H14B 0.9300 . ? C15B C16B 1.359(9) . ? C15B H15B 0.9300 . ? C16B C17B 1.400(8) . ? C16B H16B 0.9300 . ? C17B C18B 1.397(8) . ? C18B C19B 1.372(9) . ? C18B H18B 0.9300 . ? C19B C20B 1.377(9) . ? C19B H19B 0.9300 . ? C20B H20B 0.9300 . ? C1C C10C 1.422(7) . ? C1C C2C 1.427(6) . ? C1C C6C 1.432(6) . ? C2C C13C 1.397(7) . ? C2C C3C 1.462(7) . ? C3C C14C 1.391(7) . ? C3C C4C 1.421(7) . ? C4C C5C 1.413(7) . ? C4C C17C 1.426(7) . ? C5C C20C 1.391(7) . ? C5C C6C 1.457(7) . ? C6C C7C 1.397(7) . ? C7C C8C 1.384(8) . ? C7C H7C 0.9300 . ? C8C C9C 1.361(8) . ? C8C H8C 0.9300 . ? C9C C10C 1.406(8) . ? C9C H9C 0.9300 . ? C10C C11C 1.409(8) . ? C11C C12C 1.370(8) . ? C11C H11C 0.9300 . ? C12C C13C 1.390(8) . ? C12C H12C 0.9300 . ? C13C H13C 0.9300 . ? C14C C15C 1.391(8) . ? C14C H14C 0.9300 . ? C15C C16C 1.357(8) . ? C15C H15C 0.9300 . ? C16C C17C 1.405(8) . ? C16C H16C 0.9300 . ? C17C C18C 1.412(8) . ? C18C C19C 1.361(8) . ? C18C H18C 0.9300 . ? C19C C20C 1.398(8) . ? C19C H19C 0.9300 . ? C20C H20C 0.9300 . ? C1D C10D 1.411(7) . ? C1D C6D 1.417(7) . ? C1D C2D 1.431(7) . ? C2D C13D 1.407(7) . ? C2D C3D 1.459(7) . ? C3D C14D 1.411(7) . ? C3D C4D 1.426(7) . ? C4D C5D 1.425(7) . ? C4D C17D 1.428(7) . ? C5D C20D 1.377(7) . ? C5D C6D 1.457(7) . ? C6D C7D 1.403(7) . ? C7D C8D 1.387(8) . ? C7D H7D 0.9300 . ? C8D C9D 1.359(9) . ? C8D H8D 0.9300 . ? C9D C10D 1.423(8) . ? C9D H9D 0.9300 . ? C10D C11D 1.404(8) . ? C11D C12D 1.348(9) . ? C11D H11D 0.9300 . ? C12D C13D 1.386(8) . ? C12D H12D 0.9300 . ? C13D H13D 0.9300 . ? C14D C15D 1.362(8) . ? C14D H14D 0.9300 . ? C15D C16D 1.367(8) . ? C15D H15D 0.9300 . ? C16D C17D 1.406(8) . ? C16D H16D 0.9300 . ? C17D C18D 1.400(8) . ? C18D C19D 1.376(8) . ? C18D H18D 0.9300 . ? C19D C20D 1.394(8) . ? C19D H19D 0.9300 . ? C20D H20D 0.9300 . ? C1E C2E 1.411(7) . ? C1E C6E 1.425(7) . ? C1E C10E 1.435(8) . ? C2E C13E 1.399(7) . ? C2E C3E 1.478(8) . ? C3E C14E 1.376(8) . ? C3E C4E 1.438(8) . ? C4E C17E 1.416(8) . ? C4E C5E 1.426(8) . ? C5E C20E 1.385(8) . ? C5E C6E 1.471(8) . ? C6E C7E 1.368(8) . ? C7E C8E 1.401(9) . ? C7E H7E 0.9300 . ? C8E C9E 1.351(9) . ? C8E H8E 0.9300 . ? C9E C10E 1.411(9) . ? C9E H9E 0.9300 . ? C10E C11E 1.392(8) . ? C11E C12E 1.362(8) . ? C11E H11E 0.9300 . ? C12E C13E 1.402(8) . ? C12E H12E 0.9300 . ? C13E H13E 0.9300 . ? C14E C15E 1.408(10) . ? C14E H14E 0.9300 . ? C15E C16E 1.356(11) . ? C15E H15E 0.9300 . ? C16E C17E 1.418(10) . ? C16E H16E 0.9300 . ? C17E C18E 1.414(9) . ? C18E C19E 1.349(10) . ? C18E H18E 0.9300 . ? C19E C20E 1.386(9) . ? C19E H19E 0.9300 . ? C20E H20E 0.9300 . ? C1F C2F 1.364(12) . ? C1F C6F 1.377(11) . ? C1F H1F 0.9300 . ? C2F C3F 1.378(11) . ? C2F H2F 0.9300 . ? C3F C7F 1.407(11) . ? C3F C4F 1.418(9) . ? C4F C5F 1.429(8) . ? C4F C10F 1.442(8) 2_765 ? C5F C6F 1.386(8) . ? C5F C10F 1.452(8) . ? C6F H6F 0.9300 . ? C7F C8F 1.362(13) 2_765 ? C7F H7F 0.9300 . ? C8F C7F 1.362(13) 2_765 ? C8F C9F 1.411(12) . ? C8F H8F 0.9300 . ? C9F C10F 1.376(9) . ? C9F H9F 0.9300 . ? C10F C4F 1.442(8) 2_765 ? C1G C2G 1.366(10) 2_566 ? C1G C6G 1.392(10) . ? C1G H1G 0.9300 . ? C2G C1G 1.366(10) 2_566 ? C2G C3G 1.416(9) . ? C2G H2G 0.9300 . ? C3G C7G 1.397(8) . ? C3G C4G 1.431(8) . ? C4G C10G 1.424(7) . ? C4G C5G 1.439(7) 2_566 ? C5G C6G 1.381(8) . ? C5G C4G 1.439(7) 2_566 ? C5G C10G 1.459(8) . ? C6G H6G 0.9300 . ? C7G C8G 1.359(9) . ? C7G H7G 0.9300 . ? C8G C9G 1.392(8) . ? C8G H8G 0.9300 . ? C9G C10G 1.404(7) . ? C9G H9G 0.9300 . ? N1 C21 1.101(13) . ? C21 C22 1.416(9) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 O37 P1 O38 109.82(18) . . ? O37 P1 O39 109.05(18) . . ? O38 P1 O39 109.36(19) . . ? O37 P1 O40 109.26(19) . . ? O38 P1 O40 109.30(18) . . ? O39 P1 O40 110.04(19) . . ? O1 Mo1 O8 104.20(18) . . ? O1 Mo1 O4 101.53(18) . . ? O8 Mo1 O4 96.04(16) . . ? O1 Mo1 O9 102.21(18) . . ? O8 Mo1 O9 85.75(15) . . ? O4 Mo1 O9 154.96(16) . . ? O1 Mo1 O5 98.39(17) . . ? O8 Mo1 O5 156.15(16) . . ? O4 Mo1 O5 86.75(15) . . ? O9 Mo1 O5 82.06(15) . . ? O1 Mo1 O37 167.91(16) . . ? O8 Mo1 O37 87.10(14) . . ? O4 Mo1 O37 72.54(13) . . ? O9 Mo1 O37 82.64(14) . . ? O5 Mo1 O37 71.10(13) . . ? O2 Mo2 O10 103.87(17) . . ? O2 Mo2 O5 101.61(17) . . ? O10 Mo2 O5 96.78(16) . . ? O2 Mo2 O11 102.24(17) . . ? O10 Mo2 O11 86.53(15) . . ? O5 Mo2 O11 154.36(15) . . ? O2 Mo2 O6 98.56(16) . . ? O10 Mo2 O6 156.48(15) . . ? O5 Mo2 O6 85.44(15) . . ? O11 Mo2 O6 81.85(15) . . ? O2 Mo2 O37 168.25(15) . . ? O10 Mo2 O37 87.38(14) . . ? O5 Mo2 O37 73.28(13) . . ? O11 Mo2 O37 81.51(13) . . ? O6 Mo2 O37 70.76(13) . . ? O3 Mo3 O12 104.34(18) . . ? O3 Mo3 O6 102.10(17) . . ? O12 Mo3 O6 97.38(16) . . ? O3 Mo3 O7 101.80(17) . . ? O12 Mo3 O7 86.44(15) . . ? O6 Mo3 O7 154.01(15) . . ? O3 Mo3 O4 98.13(17) . . ? O12 Mo3 O4 155.87(16) . . ? O6 Mo3 O4 86.27(15) . . ? O7 Mo3 O4 80.39(15) . . ? O3 Mo3 O37 167.71(16) . . ? O12 Mo3 O37 87.64(14) . . ? O6 Mo3 O37 73.14(13) . . ? O7 Mo3 O37 81.38(13) . . ? O4 Mo3 O37 70.52(13) . . ? O14 Mo4 O7 103.85(19) . . ? O14 Mo4 O15 100.20(17) . . ? O7 Mo4 O15 90.77(16) . . ? O14 Mo4 O13 103.12(18) . . ? O7 Mo4 O13 86.64(15) . . ? O15 Mo4 O13 156.48(15) . . ? O14 Mo4 O26 99.78(18) . . ? O7 Mo4 O26 156.31(16) . . ? O15 Mo4 O26 86.61(15) . . ? O13 Mo4 O26 86.47(15) . . ? O14 Mo4 O38 168.08(17) . . ? O7 Mo4 O38 85.41(14) . . ? O15 Mo4 O38 71.83(13) . . ? O13 Mo4 O38 84.66(14) . . ? O26 Mo4 O38 71.40(13) . . ? O16 Mo5 O27 102.33(18) . . ? O16 Mo5 O17 103.85(19) . . ? O27 Mo5 O17 96.17(16) . . ? O16 Mo5 O8 101.07(18) . . ? O27 Mo5 O8 155.41(16) . . ? O17 Mo5 O8 85.45(15) . . ? O16 Mo5 O15 98.95(18) . . ? O27 Mo5 O15 87.43(15) . . ? O17 Mo5 O15 155.54(16) . . ? O8 Mo5 O15 81.57(15) . . ? O16 Mo5 O38 168.17(17) . . ? O27 Mo5 O38 72.58(13) . . ? O17 Mo5 O38 87.47(14) . . ? O8 Mo5 O38 83.00(13) . . ? O15 Mo5 O38 70.48(13) . . ? O18 Mo6 O9 104.18(18) . . ? O18 Mo6 O19 101.79(18) . . ? O9 Mo6 O19 96.12(16) . . ? O18 Mo6 O17 101.92(18) . . ? O9 Mo6 O17 86.44(15) . . ? O19 Mo6 O17 154.73(15) . . ? O18 Mo6 O28 99.03(17) . . ? O9 Mo6 O28 155.82(16) . . ? O19 Mo6 O28 85.55(16) . . ? O17 Mo6 O28 82.23(15) . . ? O18 Mo6 O39 168.07(16) . . ? O9 Mo6 O39 87.00(14) . . ? O19 Mo6 O39 72.44(13) . . ? O17 Mo6 O39 82.63(13) . . ? O28 Mo6 O39 70.45(13) . . ? O20 Mo7 O21 103.91(18) . . ? O20 Mo7 O29 101.62(18) . . ? O21 Mo7 O29 96.02(16) . . ? O20 Mo7 O10 101.82(18) . . ? O21 Mo7 O10 85.70(15) . . ? O29 Mo7 O10 155.34(15) . . ? O20 Mo7 O19 98.78(18) . . ? O21 Mo7 O19 155.92(16) . . ? O29 Mo7 O19 87.13(15) . . ? O10 Mo7 O19 81.83(15) . . ? O20 Mo7 O39 168.42(16) . . ? O21 Mo7 O39 86.91(14) . . ? O29 Mo7 O39 72.73(13) . . ? O10 Mo7 O39 82.83(13) . . ? O19 Mo7 O39 71.19(13) . . ? O22 Mo8 O11 104.22(18) . . ? O22 Mo8 O23 101.31(18) . . ? O11 Mo8 O23 95.95(16) . . ? O22 Mo8 O21 101.60(17) . . ? O11 Mo8 O21 85.44(15) . . ? O23 Mo8 O21 155.94(16) . . ? O22 Mo8 O30 99.36(18) . . ? O11 Mo8 O30 154.93(16) . . ? O23 Mo8 O30 87.58(15) . . ? O21 Mo8 O30 81.57(15) . . ? O22 Mo8 O40 168.37(16) . . ? O11 Mo8 O40 86.67(14) . . ? O23 Mo8 O40 73.08(14) . . ? O21 Mo8 O40 83.05(13) . . ? O30 Mo8 O40 70.58(13) . . ? O24 Mo9 O13 104.61(19) . . ? O24 Mo9 O25 102.06(18) . . ? O13 Mo9 O25 94.26(16) . . ? O24 Mo9 O12 103.04(18) . . ? O13 Mo9 O12 86.21(15) . . ? O25 Mo9 O12 153.91(15) . . ? O24 Mo9 O23 99.84(18) . . ? O13 Mo9 O23 154.77(15) . . ? O25 Mo9 O23 86.55(15) . . ? O12 Mo9 O23 82.31(14) . . ? O24 Mo9 O40 168.43(17) . . ? O13 Mo9 O40 85.77(14) . . ? O25 Mo9 O40 71.59(13) . . ? O12 Mo9 O40 82.45(13) . . ? O23 Mo9 O40 70.54(13) . . ? O34 Mo10 O33 104.09(18) . . ? O34 Mo10 O31 102.59(18) . . ? O33 Mo10 O31 86.60(15) . . ? O34 Mo10 O30 100.55(18) . . ? O33 Mo10 O30 90.67(16) . . ? O31 Mo10 O30 156.67(16) . . ? O34 Mo10 O25 99.21(17) . . ? O33 Mo10 O25 156.63(16) . . ? O31 Mo10 O25 86.62(15) . . ? O30 Mo10 O25 86.79(15) . . ? O34 Mo10 O40 167.62(16) . . ? O33 Mo10 O40 86.06(14) . . ? O31 Mo10 O40 84.84(14) . . ? O30 Mo10 O40 71.85(13) . . ? O25 Mo10 O40 71.06(13) . . ? O35 Mo11 O31 104.16(18) . . ? O35 Mo11 O26 101.95(18) . . ? O31 Mo11 O26 94.75(16) . . ? O35 Mo11 O32 102.81(19) . . ? O31 Mo11 O32 85.81(15) . . ? O26 Mo11 O32 154.30(16) . . ? O35 Mo11 O27 100.12(18) . . ? O31 Mo11 O27 154.93(16) . . ? O26 Mo11 O27 86.21(15) . . ? O32 Mo11 O27 82.78(15) . . ? O35 Mo11 O38 168.48(16) . . ? O31 Mo11 O38 86.26(14) . . ? O26 Mo11 O38 71.84(13) . . ? O32 Mo11 O38 82.58(14) . . ? O27 Mo11 O38 70.20(13) . . ? O36 Mo12 O32 104.32(18) . . ? O36 Mo12 O28 101.54(18) . . ? O32 Mo12 O28 97.16(16) . . ? O36 Mo12 O29 98.39(17) . . ? O32 Mo12 O29 155.68(16) . . ? O28 Mo12 O29 86.57(16) . . ? O36 Mo12 O33 102.27(18) . . ? O32 Mo12 O33 85.96(15) . . ? O28 Mo12 O33 154.40(16) . . ? O29 Mo12 O33 80.78(15) . . ? O36 Mo12 O39 167.72(16) . . ? O32 Mo12 O39 87.44(15) . . ? O28 Mo12 O39 73.02(13) . . ? O29 Mo12 O39 70.61(13) . . ? O33 Mo12 O39 81.78(13) . . ? Mo1 O4 Mo3 127.20(19) . . ? Mo2 O5 Mo1 126.41(19) . . ? Mo3 O6 Mo2 126.54(19) . . ? Mo4 O7 Mo3 148.1(2) . . ? Mo1 O8 Mo5 150.3(2) . . ? Mo6 O9 Mo1 150.0(2) . . ? Mo2 O10 Mo7 149.7(2) . . ? Mo8 O11 Mo2 151.0(2) . . ? Mo3 O12 Mo9 150.9(2) . . ? Mo9 O13 Mo4 151.0(2) . . ? Mo4 O15 Mo5 126.11(18) . . ? Mo5 O17 Mo6 150.0(2) . . ? Mo6 O19 Mo7 127.00(19) . . ? Mo7 O21 Mo8 150.3(2) . . ? Mo8 O23 Mo9 127.20(19) . . ? Mo9 O25 Mo10 128.28(19) . . ? Mo11 O26 Mo4 127.76(19) . . ? Mo5 O27 Mo11 128.1(2) . . ? Mo12 O28 Mo6 127.04(19) . . ? Mo7 O29 Mo12 126.94(19) . . ? Mo10 O30 Mo8 125.76(18) . . ? Mo11 O31 Mo10 150.9(2) . . ? Mo12 O32 Mo11 151.3(2) . . ? Mo10 O33 Mo12 147.45(19) . . ? P1 O37 Mo3 125.65(18) . . ? P1 O37 Mo2 125.61(18) . . ? Mo3 O37 Mo2 89.54(11) . . ? P1 O37 Mo1 125.71(18) . . ? Mo3 O37 Mo1 89.60(11) . . ? Mo2 O37 Mo1 89.19(11) . . ? P1 O38 Mo4 125.11(18) . . ? P1 O38 Mo5 125.24(18) . . ? Mo4 O38 Mo5 91.30(11) . . ? P1 O38 Mo11 125.86(18) . . ? Mo4 O38 Mo11 89.00(11) . . ? Mo5 O38 Mo11 89.11(11) . . ? P1 O39 Mo7 125.90(18) . . ? P1 O39 Mo12 125.64(18) . . ? Mo7 O39 Mo12 89.58(11) . . ? P1 O39 Mo6 125.38(18) . . ? Mo7 O39 Mo6 89.34(10) . . ? Mo12 O39 Mo6 89.47(11) . . ? P1 O40 Mo10 125.18(18) . . ? P1 O40 Mo8 124.75(18) . . ? Mo10 O40 Mo8 91.52(11) . . ? P1 O40 Mo9 126.05(18) . . ? Mo10 O40 Mo9 89.06(11) . . ? Mo8 O40 Mo9 89.15(11) . . ? C2A C1A C6A 121.7(5) . . ? C2A C1A C10A 119.5(5) . . ? C6A C1A C10A 118.8(5) . . ? C13A C2A C1A 118.4(5) . . ? C13A C2A C3A 121.9(5) . . ? C1A C2A C3A 119.7(5) . . ? C14A C3A C4A 117.7(5) . . ? C14A C3A C2A 123.1(5) . . ? C4A C3A C2A 119.2(5) . . ? C3A C4A C17A 120.1(5) . . ? C3A C4A C5A 121.2(5) . . ? C17A C4A C5A 118.7(5) . . ? C20A C5A C4A 118.4(5) . . ? C20A C5A C6A 122.2(5) . . ? C4A C5A C6A 119.4(5) . . ? C7A C6A C1A 118.5(5) . . ? C7A C6A C5A 122.7(5) . . ? C1A C6A C5A 118.8(5) . . ? C8A C7A C6A 122.7(6) . . ? C8A C7A H7A 118.7 . . ? C6A C7A H7A 118.7 . . ? C7A C8A C9A 119.6(6) . . ? C7A C8A H8A 120.2 . . ? C9A C8A H8A 120.2 . . ? C8A C9A C10A 120.6(6) . . ? C8A C9A H9A 119.7 . . ? C10A C9A H9A 119.7 . . ? C9A C10A C11A 121.6(6) . . ? C9A C10A C1A 119.8(6) . . ? C11A C10A C1A 118.5(6) . . ? C12A C11A C10A 121.2(6) . . ? C12A C11A H11A 119.4 . . ? C10A C11A H11A 119.4 . . ? C11A C12A C13A 120.9(6) . . ? C11A C12A H12A 119.6 . . ? C13A C12A H12A 119.6 . . ? C12A C13A C2A 121.5(7) . . ? C12A C13A H13A 119.3 . . ? C2A C13A H13A 119.3 . . ? C15A C14A C3A 122.7(5) . . ? C15A C14A H14A 118.7 . . ? C3A C14A H14A 118.7 . . ? C16A C15A C14A 119.5(5) . . ? C16A C15A H15A 120.2 . . ? C14A C15A H15A 120.2 . . ? C15A C16A C17A 120.8(5) . . ? C15A C16A H16A 119.6 . . ? C17A C16A H16A 119.6 . . ? C18A C17A C16A 121.2(5) . . ? C18A C17A C4A 119.7(5) . . ? C16A C17A C4A 119.2(5) . . ? C19A C18A C17A 120.6(5) . . ? C19A C18A H18A 119.7 . . ? C17A C18A H18A 119.7 . . ? C20A C19A C18A 120.5(6) . . ? C20A C19A H19A 119.7 . . ? C18A C19A H19A 119.7 . . ? C19A C20A C5A 122.0(5) . . ? C19A C20A H20A 119.0 . . ? C5A C20A H20A 119.0 . . ? C6B C1B C2B 121.3(5) . . ? C6B C1B C10B 118.8(5) . . ? C2B C1B C10B 119.8(5) . . ? C13B C2B C1B 118.4(5) . . ? C13B C2B C3B 121.7(5) . . ? C1B C2B C3B 120.0(5) . . ? C14B C3B C4B 117.8(5) . . ? C14B C3B C2B 123.2(5) . . ? C4B C3B C2B 118.9(5) . . ? C5B C4B C3B 121.6(5) . . ? C5B C4B C17B 118.9(5) . . ? C3B C4B C17B 119.5(5) . . ? C20B C5B C4B 118.6(5) . . ? C20B C5B C6B 122.2(5) . . ? C4B C5B C6B 119.2(5) . . ? C7B C6B C1B 118.7(5) . . ? C7B C6B C5B 122.4(5) . . ? C1B C6B C5B 119.0(5) . . ? C8B C7B C6B 121.8(6) . . ? C8B C7B H7B 119.1 . . ? C6B C7B H7B 119.1 . . ? C9B C8B C7B 119.8(6) . . ? C9B C8B H8B 120.1 . . ? C7B C8B H8B 120.1 . . ? C8B C9B C10B 121.8(6) . . ? C8B C9B H9B 119.1 . . ? C10B C9B H9B 119.1 . . ? C9B C10B C11B 122.3(6) . . ? C9B C10B C1B 119.0(6) . . ? C11B C10B C1B 118.7(6) . . ? C12B C11B C10B 121.8(6) . . ? C12B C11B H11B 119.1 . . ? C10B C11B H11B 119.1 . . ? C11B C12B C13B 120.2(6) . . ? C11B C12B H12B 119.9 . . ? C13B C12B H12B 119.9 . . ? C2B C13B C12B 121.1(6) . . ? C2B C13B H13B 119.4 . . ? C12B C13B H13B 119.4 . . ? C15B C14B C3B 122.2(5) . . ? C15B C14B H14B 118.9 . . ? C3B C14B H14B 118.9 . . ? C16B C15B C14B 119.8(6) . . ? C16B C15B H15B 120.1 . . ? C14B C15B H15B 120.1 . . ? C15B C16B C17B 121.6(6) . . ? C15B C16B H16B 119.2 . . ? C17B C16B H16B 119.2 . . ? C18B C17B C16B 121.6(5) . . ? C18B C17B C4B 119.4(5) . . ? C16B C17B C4B 119.0(5) . . ? C19B C18B C17B 121.3(6) . . ? C19B C18B H18B 119.3 . . ? C17B C18B H18B 119.3 . . ? C18B C19B C20B 119.8(6) . . ? C18B C19B H19B 120.1 . . ? C20B C19B H19B 120.1 . . ? C19B C20B C5B 122.0(6) . . ? C19B C20B H20B 119.0 . . ? C5B C20B H20B 119.0 . . ? C10C C1C C2C 119.4(4) . . ? C10C C1C C6C 119.2(4) . . ? C2C C1C C6C 121.4(4) . . ? C13C C2C C1C 118.4(5) . . ? C13C C2C C3C 122.4(5) . . ? C1C C2C C3C 119.2(4) . . ? C14C C3C C4C 119.2(5) . . ? C14C C3C C2C 122.0(5) . . ? C4C C3C C2C 118.8(4) . . ? C5C C4C C3C 122.3(5) . . ? C5C C4C C17C 119.4(5) . . ? C3C C4C C17C 118.3(5) . . ? C20C C5C C4C 119.3(5) . . ? C20C C5C C6C 121.5(5) . . ? C4C C5C C6C 119.3(4) . . ? C7C C6C C1C 118.1(5) . . ? C7C C6C C5C 122.9(5) . . ? C1C C6C C5C 119.0(4) . . ? C8C C7C C6C 122.1(5) . . ? C8C C7C H7C 119.0 . . ? C6C C7C H7C 119.0 . . ? C9C C8C C7C 120.1(5) . . ? C9C C8C H8C 120.0 . . ? C7C C8C H8C 120.0 . . ? C8C C9C C10C 121.2(5) . . ? C8C C9C H9C 119.4 . . ? C10C C9C H9C 119.4 . . ? C9C C10C C11C 121.3(5) . . ? C9C C10C C1C 119.3(5) . . ? C11C C10C C1C 119.4(5) . . ? C12C C11C C10C 120.8(5) . . ? C12C C11C H11C 119.6 . . ? C10C C11C H11C 119.6 . . ? C11C C12C C13C 120.1(5) . . ? C11C C12C H12C 119.9 . . ? C13C C12C H12C 119.9 . . ? C12C C13C C2C 121.9(5) . . ? C12C C13C H13C 119.1 . . ? C2C C13C H13C 119.1 . . ? C3C C14C C15C 121.8(5) . . ? C3C C14C H14C 119.1 . . ? C15C C14C H14C 119.1 . . ? C16C C15C C14C 119.6(5) . . ? C16C C15C H15C 120.2 . . ? C14C C15C H15C 120.2 . . ? C15C C16C C17C 121.4(5) . . ? C15C C16C H16C 119.3 . . ? C17C C16C H16C 119.3 . . ? C16C C17C C18C 121.5(5) . . ? C16C C17C C4C 119.7(5) . . ? C18C C17C C4C 118.9(5) . . ? C19C C18C C17C 121.2(5) . . ? C19C C18C H18C 119.4 . . ? C17C C18C H18C 119.4 . . ? C18C C19C C20C 120.0(5) . . ? C18C C19C H19C 120.0 . . ? C20C C19C H19C 120.0 . . ? C5C C20C C19C 121.2(5) . . ? C5C C20C H20C 119.4 . . ? C19C C20C H20C 119.4 . . ? C10D C1D C6D 120.4(5) . . ? C10D C1D C2D 118.2(5) . . ? C6D C1D C2D 121.4(5) . . ? C13D C2D C1D 119.0(5) . . ? C13D C2D C3D 121.9(5) . . ? C1D C2D C3D 119.0(4) . . ? C14D C3D C4D 117.7(5) . . ? C14D C3D C2D 123.0(5) . . ? C4D C3D C2D 119.3(4) . . ? C5D C4D C3D 121.6(5) . . ? C5D C4D C17D 119.4(5) . . ? C3D C4D C17D 119.1(5) . . ? C20D C5D C4D 118.5(5) . . ? C20D C5D C6D 122.5(5) . . ? C4D C5D C6D 119.0(4) . . ? C7D C6D C1D 118.0(5) . . ? C7D C6D C5D 122.2(5) . . ? C1D C6D C5D 119.8(4) . . ? C8D C7D C6D 121.5(5) . . ? C8D C7D H7D 119.2 . . ? C6D C7D H7D 119.2 . . ? C9D C8D C7D 120.7(6) . . ? C9D C8D H8D 119.6 . . ? C7D C8D H8D 119.6 . . ? C8D C9D C10D 120.4(6) . . ? C8D C9D H9D 119.8 . . ? C10D C9D H9D 119.8 . . ? C11D C10D C1D 120.3(5) . . ? C11D C10D C9D 120.9(5) . . ? C1D C10D C9D 118.9(5) . . ? C12D C11D C10D 121.0(6) . . ? C12D C11D H11D 119.5 . . ? C10D C11D H11D 119.5 . . ? C11D C12D C13D 120.7(6) . . ? C11D C12D H12D 119.6 . . ? C13D C12D H12D 119.6 . . ? C12D C13D C2D 120.7(6) . . ? C12D C13D H13D 119.6 . . ? C2D C13D H13D 119.6 . . ? C15D C14D C3D 122.5(5) . . ? C15D C14D H14D 118.7 . . ? C3D C14D H14D 118.7 . . ? C14D C15D C16D 120.5(5) . . ? C14D C15D H15D 119.8 . . ? C16D C15D H15D 119.8 . . ? C15D C16D C17D 120.7(6) . . ? C15D C16D H16D 119.7 . . ? C17D C16D H16D 119.7 . . ? C18D C17D C16D 121.6(5) . . ? C18D C17D C4D 118.9(5) . . ? C16D C17D C4D 119.5(5) . . ? C19D C18D C17D 121.6(5) . . ? C19D C18D H18D 119.2 . . ? C17D C18D H18D 119.2 . . ? C18D C19D C20D 118.8(5) . . ? C18D C19D H19D 120.6 . . ? C20D C19D H19D 120.6 . . ? C5D C20D C19D 122.7(5) . . ? C5D C20D H20D 118.6 . . ? C19D C20D H20D 118.6 . . ? C2E C1E C6E 121.7(5) . . ? C2E C1E C10E 118.8(5) . . ? C6E C1E C10E 119.5(5) . . ? C13E C2E C1E 119.5(5) . . ? C13E C2E C3E 121.3(5) . . ? C1E C2E C3E 119.1(5) . . ? C14E C3E C4E 118.3(6) . . ? C14E C3E C2E 122.1(5) . . ? C4E C3E C2E 119.6(5) . . ? C17E C4E C5E 119.9(5) . . ? C17E C4E C3E 119.5(6) . . ? C5E C4E C3E 120.6(5) . . ? C20E C5E C4E 117.6(6) . . ? C20E C5E C6E 123.0(6) . . ? C4E C5E C6E 119.4(5) . . ? C7E C6E C1E 118.5(6) . . ? C7E C6E C5E 121.9(5) . . ? C1E C6E C5E 119.6(5) . . ? C6E C7E C8E 122.2(6) . . ? C6E C7E H7E 118.9 . . ? C8E C7E H7E 118.9 . . ? C9E C8E C7E 120.2(6) . . ? C9E C8E H8E 119.9 . . ? C7E C8E H8E 119.9 . . ? C8E C9E C10E 121.1(6) . . ? C8E C9E H9E 119.4 . . ? C10E C9E H9E 119.4 . . ? C11E C10E C9E 121.6(6) . . ? C11E C10E C1E 119.9(5) . . ? C9E C10E C1E 118.4(5) . . ? C12E C11E C10E 120.4(6) . . ? C12E C11E H11E 119.8 . . ? C10E C11E H11E 119.8 . . ? C11E C12E C13E 121.2(5) . . ? C11E C12E H12E 119.4 . . ? C13E C12E H12E 119.4 . . ? C2E C13E C12E 120.1(5) . . ? C2E C13E H13E 119.9 . . ? C12E C13E H13E 119.9 . . ? C3E C14E C15E 121.8(6) . . ? C3E C14E H14E 119.1 . . ? C15E C14E H14E 119.1 . . ? C16E C15E C14E 120.4(7) . . ? C16E C15E H15E 119.8 . . ? C14E C15E H15E 119.8 . . ? C15E C16E C17E 120.5(7) . . ? C15E C16E H16E 119.8 . . ? C17E C16E H16E 119.8 . . ? C18E C17E C4E 118.8(6) . . ? C18E C17E C16E 121.8(6) . . ? C4E C17E C16E 119.4(6) . . ? C19E C18E C17E 120.8(6) . . ? C19E C18E H18E 119.6 . . ? C17E C18E H18E 119.6 . . ? C18E C19E C20E 120.4(6) . . ? C18E C19E H19E 119.8 . . ? C20E C19E H19E 119.8 . . ? C5E C20E C19E 122.3(6) . . ? C5E C20E H20E 118.8 . . ? C19E C20E H20E 118.8 . . ? C2F C1F C6F 120.1(7) . . ? C2F C1F H1F 120.0 . . ? C6F C1F H1F 120.0 . . ? C1F C2F C3F 119.8(7) . . ? C1F C2F H2F 120.1 . . ? C3F C2F H2F 120.1 . . ? C2F C3F C7F 120.3(8) . . ? C2F C3F C4F 121.1(8) . . ? C7F C3F C4F 118.5(7) . . ? C3F C4F C5F 118.8(6) . . ? C3F C4F C10F 120.2(6) . 2_765 ? C5F C4F C10F 120.9(5) . 2_765 ? C6F C5F C4F 116.9(6) . . ? C6F C5F C10F 123.7(6) . . ? C4F C5F C10F 119.5(5) . . ? C1F C6F C5F 123.2(8) . . ? C1F C6F H6F 118.4 . . ? C5F C6F H6F 118.4 . . ? C8F C7F C3F 121.1(8) 2_765 . ? C8F C7F H7F 119.4 2_765 . ? C3F C7F H7F 119.4 . . ? C7F C8F C9F 120.6(8) 2_765 . ? C7F C8F H8F 119.7 2_765 . ? C9F C8F H8F 119.7 . . ? C10F C9F C8F 121.1(8) . . ? C10F C9F H9F 119.4 . . ? C8F C9F H9F 119.4 . . ? C9F C10F C4F 118.3(6) . 2_765 ? C9F C10F C5F 122.0(6) . . ? C4F C10F C5F 119.6(5) 2_765 . ? C2G C1G C6G 120.8(6) 2_566 . ? C2G C1G H1G 119.6 2_566 . ? C6G C1G H1G 119.6 . . ? C1G C2G C3G 120.3(6) 2_566 . ? C1G C2G H2G 119.8 2_566 . ? C3G C2G H2G 119.8 . . ? C7G C3G C2G 121.4(6) . . ? C7G C3G C4G 119.9(5) . . ? C2G C3G C4G 118.7(5) . . ? C10G C4G C3G 119.5(5) . . ? C10G C4G C5G 120.4(5) . 2_566 ? C3G C4G C5G 120.2(5) . 2_566 ? C6G C5G C4G 117.5(5) . 2_566 ? C6G C5G C10G 122.7(5) . . ? C4G C5G C10G 119.8(5) 2_566 . ? C5G C6G C1G 122.5(6) . . ? C5G C6G H6G 118.7 . . ? C1G C6G H6G 118.7 . . ? C8G C7G C3G 120.5(6) . . ? C8G C7G H7G 119.8 . . ? C3G C7G H7G 119.8 . . ? C7G C8G C9G 120.7(6) . . ? C7G C8G H8G 119.7 . . ? C9G C8G H8G 119.7 . . ? C8G C9G C10G 121.9(5) . . ? C8G C9G H9G 119.0 . . ? C10G C9G H9G 119.0 . . ? C9G C10G C4G 117.5(5) . . ? C9G C10G C5G 122.6(5) . . ? C4G C10G C5G 119.8(5) . . ? N1 C21 C22 176.4(14) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.628 _refine_diff_density_min -2.286 _refine_diff_density_rms 0.392 #========================================================================== data_compound3 _database_code_depnum_ccdc_archive 'CCDC 232006' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H126 N2 O40 Si W12' _chemical_formula_weight 4494.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 18.366(4) _cell_length_b 18.547(5) _cell_length_c 19.172(5) _cell_angle_alpha 83.033(7) _cell_angle_beta 84.736(7) _cell_angle_gamma 67.564(7) _cell_volume 5984(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4188 _exptl_absorpt_coefficient_mu 11.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1348 _exptl_absorpt_correction_T_max 0.3924 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69750 _diffrn_reflns_av_R_equivalents 0.3147 _diffrn_reflns_av_sigmaI/netI 0.7176 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 30.89 _reflns_number_total 34799 _reflns_number_gt 7455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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. This compound crystallises as very fine needles which invariably grow as bunches of crystals. In fact, most of the crystals that were exposed to X-rays showed diffraction patterns indicating the presence of twins, making them unsuitable to allow a useful data collection. Finally, from a multiple twin a fragment was mechanically separated whose diffraction pattern initially indicated the absence of twins, although its subsequent analysis suggested a high mosaicity, indicating that the crystal was formed by highly disoriented microcrystalline blocks. In spite of this, and taking into account that this was the only crystal which gave reasonable cell parameters, a full data collection was performed. An initial solution was obtained by direct methods using SIR97 which only showed clearly the position of the two polyoxometalate units contained in the unit cell (lying on inversion centers) and one molecule of perylene very distorted. After several Fourier differences (using SHELX-97) most of the oxygen atoms of the polyoxoanions, one complete perylene molecule and several distorted fragments of the remaining perylene molecules were located. Moreover, the refinements were unstable and the carbon atoms assigned to perylene molecules deviated from their initial positions at the same time that their thermal isotropic parameters reached very high values. The approximate position of the perylene molecules could only be determined by the use of restraints about their geometry (using DFIX instructions in SHELX-97) and stablishing constant values for the thermal isotropic parameters of some carbon atoms. As these molecules were still very distorted, they were fitted to a well behaved perylene molecule (using the FRAG instruction in SHELX-97) whose coordinates were taken from the structure of compound 2. Using these restrictions it was possible to locate two additional fragments corresponding to two tetrabutylmmonium cations. Restrictions on the bonding distances were also applied to these cations and to some of the oxygen atoms of the polyoxoanions, allowing the stablishment of a complete structural model. In this model there is full confidence in the spatial distribution of the polyoxometalates, perylene molecules and tetrabutylammonium cations. This structure is reported with the aim of investigating the different types of packings that perylene molecules can afford when they are combined with bulky polyoxoanions. However, angle and bond distances are not taken into account in the discussion of the structure of 3 as they are clearly far from reality. Only W and Si atoms were refined anisotropically. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1480P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 34799 _refine_ls_number_parameters 539 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.4312 _refine_ls_R_factor_gt 0.1451 _refine_ls_wR_factor_ref 0.4150 _refine_ls_wR_factor_gt 0.3111 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.007 _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 Si1A Si 0.5000 0.5000 0.0000 0.018 Uani 1 2 d S . . W1A W 0.70312(10) 0.38853(11) -0.00869(11) 0.042 Uani 1 1 d . . . W2A W 0.57566(12) 0.32194(11) 0.10514(12) 0.053 Uani 1 1 d D . . W3A W 0.57315(11) 0.32291(11) -0.07888(12) 0.046 Uani 1 1 d D . . W4A W 0.62863(11) 0.56972(11) -0.10906(12) 0.047 Uani 1 1 d D . . W5A W 0.37064(11) 0.43722(11) -0.07545(11) 0.043 Uani 1 1 d D . . W6A W 0.50400(12) 0.50201(12) -0.18454(11) 0.049 Uani 1 1 d . . . O1A O 0.806(2) 0.331(2) -0.0148(19) 0.080 Uiso 1 1 d . . . O2A O 0.615(2) 0.237(2) 0.1581(18) 0.072 Uiso 1 1 d . . . O3A O 0.602(2) 0.244(2) -0.1163(19) 0.077 Uiso 1 1 d . . . O4A O 0.675(2) 0.330(2) 0.0733(18) 0.069 Uiso 1 1 d . . . O5A O 0.5682(17) 0.2941(15) 0.0193(7) 0.047 Uiso 1 1 d D . . O6A O 0.669(3) 0.350(3) -0.068(3) 0.138 Uiso 1 1 d . . . O7A O 0.698(2) 0.470(2) -0.0838(17) 0.064 Uiso 1 1 d . . . O8A O 0.6951(19) 0.4571(19) 0.0563(17) 0.059 Uiso 1 1 d . . . O9A O 0.442(3) 0.600(3) -0.165(2) 0.109 Uiso 1 1 d . . . O10A O 0.466(3) 0.334(3) 0.123(2) 0.117 Uiso 1 1 d . . . O11A O 0.4669(19) 0.3424(19) -0.0761(16) 0.056 Uiso 1 1 d . . . O12A O 0.566(2) 0.398(2) -0.1643(18) 0.076 Uiso 1 1 d D . . O13A O 0.693(2) 0.600(2) -0.1604(19) 0.080 Uiso 1 1 d . . . O14A O 0.6435(19) 0.5894(18) -0.0215(7) 0.065 Uiso 1 1 d D . . O15A O 0.305(2) 0.411(2) -0.113(2) 0.086 Uiso 1 1 d . . . O16A O 0.408(2) 0.484(2) -0.1575(17) 0.062 Uiso 1 1 d . . . O17A O 0.5029(16) 0.5069(16) -0.2593(14) 0.040 Uiso 1 1 d . . . O18A O 0.603(3) 0.529(3) -0.179(2) 0.111 Uiso 1 1 d . . . O19A O 0.557(2) 0.410(2) 0.009(2) 0.008 Uiso 0.50 1 d P . . O20A O 0.515(3) 0.542(3) -0.077(3) 0.040 Uiso 0.50 1 d P . . O21A O 0.583(3) 0.506(3) -0.009(3) 0.030 Uiso 0.50 1 d P . . O22A O 0.523(3) 0.553(3) 0.055(2) 0.023 Uiso 0.50 1 d P . . Si1B Si 1.0000 0.0000 -0.5000 0.005 Uani 1 2 d SDU . . W1B W 1.05993(11) 0.12661(11) -0.41592(11) 0.043 Uani 1 1 d . . . W2B W 1.00788(12) 0.00865(11) -0.68407(11) 0.045 Uani 1 1 d D . . W3B W 0.82552(11) 0.07496(12) -0.58994(12) 0.047 Uani 1 1 d . . . W4B W 0.92948(11) -0.13345(10) -0.40013(11) 0.040 Uani 1 1 d D . . W5B W 0.88610(11) 0.20149(10) -0.50755(11) 0.040 Uani 1 1 d . . . W6B W 0.81664(10) 0.06852(11) -0.40664(11) 0.043 Uani 1 1 d . . . O1B O 1.084(2) 0.183(2) -0.3729(19) 0.076 Uiso 1 1 d . . . O2B O 0.996(2) 0.004(2) -0.7555(18) 0.068 Uiso 1 1 d . . . O3B O 0.7480(18) 0.1108(18) -0.6370(15) 0.051 Uiso 1 1 d . . . O4B O 0.990(3) -0.087(3) -0.652(2) 0.103 Uiso 1 1 d . . . O5B O 0.901(2) 0.074(2) -0.661(2) 0.090 Uiso 1 1 d . . . O6B O 1.153(2) 0.027(2) -0.4054(18) 0.074 Uiso 1 1 d . . . O7B O 0.907(2) -0.130(2) -0.495(2) 0.098 Uiso 1 1 d . . . O8B O 0.945(2) 0.198(2) -0.4385(17) 0.065 Uiso 1 1 d . . . O9B O 1.1142(12) -0.054(2) -0.6640(14) 0.088 Uiso 1 1 d D . . O10B O 0.9679(17) -0.0984(14) -0.3289(12) 0.054 Uiso 1 1 d D . . O11B O 0.838(2) 0.174(2) -0.576(2) 0.083 Uiso 1 1 d . . . O12B O 0.789(2) 0.079(2) -0.499(2) 0.094 Uiso 1 1 d . . . O13B O 0.8944(18) -0.1953(17) -0.3500(15) 0.049 Uiso 1 1 d . . . O14B O 1.0343(19) -0.1976(19) -0.4207(17) 0.060 Uiso 1 1 d . . . O15B O 0.834(2) 0.299(2) -0.5082(18) 0.069 Uiso 1 1 d . . . O16B O 0.832(2) 0.166(2) -0.439(2) 0.093 Uiso 1 1 d . . . O17B O 0.726(3) 0.101(3) -0.363(2) 0.112 Uiso 1 1 d . . . O18B O 0.840(2) -0.041(2) -0.396(2) 0.088 Uiso 1 1 d . . . O19B O 0.958(2) -0.005(3) -0.5629(17) 0.041 Uiso 0.50 1 d PD . . O20B O 1.001(3) 0.0817(17) -0.512(3) 0.047 Uiso 0.50 1 d PD . . O21B O 1.0849(15) -0.057(3) -0.503(2) 0.050 Uiso 0.50 1 d PD . . O22B O 1.043(2) 0.012(3) -0.5699(14) 0.049 Uiso 0.50 1 d PD . . C1A C 0.4556(9) 0.0857(9) 0.3513(7) 0.051 Uiso 1 1 d G . . C2A C 0.5305(10) 0.0759(9) 0.3726(8) 0.048 Uiso 1 1 d G . . C3A C 0.5757(9) 0.0049(9) 0.4157(7) 0.141 Uiso 1 1 d G . . C4A C 0.5430(9) -0.0529(9) 0.4360(7) 0.061 Uiso 1 1 d G . . C5A C 0.4668(9) -0.0432(9) 0.4143(7) 0.049 Uiso 1 1 d G . . C6A C 0.4219(9) 0.0279(10) 0.3711(8) 0.068 Uiso 1 1 d G . . C7A C 0.3478(9) 0.0416(13) 0.3485(11) 0.090 Uiso 1 1 d G . . H7A H 0.3262 0.0036 0.3606 0.109 Uiso 1 1 d G . . C8A C 0.3048(10) 0.1093(14) 0.3088(12) 0.093 Uiso 1 1 d G . . H8A H 0.2547 0.1170 0.2956 0.112 Uiso 1 1 d G . . C9A C 0.3368(12) 0.1658(12) 0.2885(11) 0.091 Uiso 1 1 d G . . H9A H 0.3081 0.2112 0.2613 0.109 Uiso 1 1 d G . . C10A C 0.4117(12) 0.1551(10) 0.3088(9) 0.083 Uiso 1 1 d G . . C11A C 0.4449(15) 0.2119(10) 0.2896(11) 0.088 Uiso 1 1 d G . . H11A H 0.4171 0.2573 0.2619 0.105 Uiso 1 1 d G . . C12A C 0.5163(15) 0.2019(11) 0.3107(12) 0.120 Uiso 1 1 d G . . H12A H 0.5368 0.2407 0.2978 0.144 Uiso 1 1 d G . . C13A C 0.5596(12) 0.1350(11) 0.3509(11) 0.099 Uiso 1 1 d G . . H13A H 0.6093 0.1290 0.3640 0.119 Uiso 1 1 d G . . C14A C 0.6507(9) -0.0095(12) 0.4379(10) 0.046 Uiso 1 1 d G . . H14A H 0.6725 0.0283 0.4258 0.056 Uiso 1 1 d G . . C15A C 0.6941(10) -0.0781(13) 0.4774(11) 0.115 Uiso 1 1 d G . . H15A H 0.7447 -0.0866 0.4897 0.138 Uiso 1 1 d G . . C16A C 0.6615(11) -0.1336(12) 0.4983(10) 0.061 Uiso 1 1 d G . . H16A H 0.6898 -0.1788 0.5260 0.073 Uiso 1 1 d G . . C17A C 0.5862(11) -0.1227(9) 0.4782(8) 0.069 Uiso 1 1 d G . . C18A C 0.5535(14) -0.1791(10) 0.4979(10) 0.082 Uiso 1 1 d G . . H18A H 0.5818 -0.2248 0.5250 0.099 Uiso 1 1 d G . . C19A C 0.4798(14) -0.1680(11) 0.4775(11) 0.072 Uiso 1 1 d G . . H19A H 0.4585 -0.2059 0.4914 0.087 Uiso 1 1 d G . . C20A C 0.4375(12) -0.1014(11) 0.4368(10) 0.081 Uiso 1 1 d G . . H20A H 0.3877 -0.0950 0.4239 0.097 Uiso 1 1 d G . . C1B C 0.4543(10) 1.0385(11) 0.1713(8) 0.049 Uiso 1 1 d G . . C2B C 0.4639(10) 0.9639(11) 0.2057(9) 0.105 Uiso 1 1 d G . . C3B C 0.5361(11) 0.9179(10) 0.2421(9) 0.042 Uiso 1 1 d G . . C4B C 0.5959(10) 0.9489(11) 0.2416(8) 0.103 Uiso 1 1 d G . . C5B C 0.5862(10) 1.0247(11) 0.2067(9) 0.061 Uiso 1 1 d G . . C6B C 0.5138(11) 1.0705(10) 0.1706(8) 0.087 Uiso 1 1 d G . . C7B C 0.5004(15) 1.1439(11) 0.1354(11) 0.096 Uiso 1 1 d G . . H7B H 0.5387 1.1653 0.1356 0.116 Uiso 1 1 d G . . C8B C 0.4327(17) 1.1866(12) 0.1002(12) 0.098 Uiso 1 1 d G . . H8B H 0.4264 1.2351 0.0762 0.118 Uiso 1 1 d G . . C9B C 0.3740(14) 1.1567(13) 0.1009(12) 0.145 Uiso 1 1 d G . . H9B H 0.3280 1.1857 0.0776 0.174 Uiso 1 1 d G . . C10B C 0.3833(11) 1.0835(13) 0.1362(10) 0.097 Uiso 1 1 d G . . C11B C 0.3250(11) 1.0515(17) 0.1368(13) 0.101 Uiso 1 1 d G . . H11B H 0.2786 1.0802 0.1143 0.121 Uiso 1 1 d G . . C12B C 0.3353(12) 0.9802(17) 0.1696(14) 0.125 Uiso 1 1 d G . . H12B H 0.2962 0.9601 0.1688 0.150 Uiso 1 1 d G . . C13B C 0.4029(12) 0.9366(14) 0.2043(12) 0.108 Uiso 1 1 d G . . H13B H 0.4081 0.8879 0.2274 0.129 Uiso 1 1 d G . . C14B C 0.5495(15) 0.8444(11) 0.2781(11) 0.100 Uiso 1 1 d G . . H14B H 0.5113 0.8229 0.2781 0.120 Uiso 1 1 d G . . C15B C 0.6175(17) 0.8020(12) 0.3140(13) 0.157 Uiso 1 1 d G . . H15B H 0.6233 0.7540 0.3391 0.188 Uiso 1 1 d G . . C16B C 0.6762(14) 0.8315(14) 0.3123(12) 0.112 Uiso 1 1 d G . . H16B H 0.7225 0.8023 0.3351 0.134 Uiso 1 1 d G . . C17B C 0.6670(11) 0.9048(14) 0.2767(10) 0.098 Uiso 1 1 d G . . C18B C 0.7253(11) 0.9357(17) 0.2759(13) 0.136 Uiso 1 1 d G . . H18B H 0.7714 0.9072 0.2991 0.163 Uiso 1 1 d G . . C19B C 0.7153(12) 1.0080(18) 0.2412(14) 0.107 Uiso 1 1 d G . . H19B H 0.7550 1.0277 0.2406 0.129 Uiso 1 1 d G . . C20B C 0.6473(12) 1.0512(15) 0.2072(13) 0.155 Uiso 1 1 d G . . H20B H 0.6421 1.0998 0.1839 0.187 Uiso 1 1 d G . . C1C C 0.6855(14) 1.0174(18) 0.0410(17) 0.106 Uiso 1 1 d G . . H1C H 0.7244 1.0378 0.0418 0.127 Uiso 1 1 d G . . C2C C 0.6956(13) 0.9452(17) 0.0743(14) 0.078 Uiso 1 1 d G . . H2C H 0.7406 0.9171 0.0993 0.093 Uiso 1 1 d G . . C3C C 0.6390(15) 0.9140(13) 0.0709(12) 0.049 Uiso 1 1 d G . . C4C C 0.5692(14) 0.9565(13) 0.0346(13) 0.058 Uiso 1 1 d G . . C5C C 0.5578(11) 1.0330(12) 0.0016(9) 0.060 Uiso 1 1 d G . . C6C C 0.6177(13) 1.0602(14) 0.0062(13) 0.069 Uiso 1 1 d G . . H6C H 0.6117 1.1097 -0.0153 0.083 Uiso 1 1 d G . . C7C C 0.651(2) 0.8377(15) 0.1015(18) 0.127 Uiso 1 1 d G . . H7C H 0.6965 0.8092 0.1256 0.153 Uiso 1 1 d G . . C8C C 0.4005(18) 1.1949(18) -0.1010(16) 0.098 Uiso 1 1 d G . . H8C H 0.3911 1.2456 -0.1212 0.118 Uiso 1 1 d G . . C9C C 0.4704(15) 1.1527(14) -0.0655(13) 0.056 Uiso 1 1 d G . . H9C H 0.5063 1.1763 -0.0622 0.067 Uiso 1 1 d G . . C10C C 0.4864(12) 1.0773(14) -0.0356(12) 0.067 Uiso 1 1 d G . . C1D C 0.7333(13) 0.6326(11) 0.5419(12) 0.100 Uiso 1 1 d GD . . C2D C 0.7677(13) 0.6426(12) 0.4744(13) 0.081 Uiso 1 1 d GD . . C3D C 0.7406(14) 0.6216(12) 0.4134(12) 0.108 Uiso 1 1 d GD . . C4D C 0.6804(14) 0.5905(12) 0.4234(14) 0.161 Uiso 1 1 d GD . . C5D C 0.6452(14) 0.5804(13) 0.4919(15) 0.146 Uiso 1 1 d GD . . C6D C 0.6725(14) 0.6017(13) 0.5527(13) 0.124 Uiso 1 1 d GD . . C7D C 0.6417(19) 0.5931(19) 0.6206(14) 0.113 Uiso 1 1 d G . . H7D H 0.6014 0.5739 0.6276 0.136 Uiso 1 1 d G . . C8D C 0.668(2) 0.612(2) 0.6781(13) 0.169 Uiso 1 1 d G . . H8D H 0.6472 0.6040 0.7230 0.203 Uiso 1 1 d G . . C9D C 0.727(2) 0.6426(19) 0.6686(13) 0.213 Uiso 1 1 d G . . H9D H 0.7447 0.6559 0.7073 0.255 Uiso 1 1 d G . . C10D C 0.7598(17) 0.6537(15) 0.6014(14) 0.228 Uiso 1 1 d G . . C11D C 0.8199(19) 0.6838(18) 0.5905(18) 0.155 Uiso 1 1 d G . . H11D H 0.8376 0.6979 0.6287 0.186 Uiso 1 1 d G . . C12D C 0.8524(18) 0.6927(19) 0.526(2) 0.136 Uiso 1 1 d G . . H12D H 0.8926 0.7121 0.5201 0.163 Uiso 1 1 d G . . C13D C 0.8269(15) 0.6734(17) 0.4680(17) 0.148 Uiso 1 1 d G . . H13D H 0.8495 0.6811 0.4237 0.177 Uiso 1 1 d G . . C14D C 0.7708(19) 0.6309(17) 0.3449(13) 0.114 Uiso 1 1 d G . . H14D H 0.8111 0.6502 0.3377 0.136 Uiso 1 1 d G . . C15D C 0.743(2) 0.613(2) 0.2871(12) 0.190 Uiso 1 1 d G . . H15D H 0.7634 0.6215 0.2420 0.228 Uiso 1 1 d G . . C16D C 0.686(2) 0.5809(19) 0.2970(15) 0.260 Uiso 1 1 d G . . H16D H 0.6685 0.5670 0.2584 0.312 Uiso 1 1 d G . . C17D C 0.6530(19) 0.5695(16) 0.3644(16) 0.191 Uiso 1 1 d G . . C18D C 0.594(2) 0.5391(19) 0.375(2) 0.199 Uiso 1 1 d GD . . H18D H 0.5758 0.5257 0.3363 0.239 Uiso 1 1 d G . . C19D C 0.562(2) 0.529(2) 0.441(2) 0.191 Uiso 1 1 d GD . . H19D H 0.5228 0.5077 0.4473 0.229 Uiso 1 1 d G . . C20D C 0.5873(17) 0.5486(18) 0.498(2) 0.466 Uiso 1 1 d G . . H20D H 0.5651 0.5407 0.5427 0.560 Uiso 1 1 d G . . C1E C 0.1335(10) 0.2320(12) 0.0473(11) 0.063 Uiso 1 1 d G . . C2E C 0.1499(11) 0.2670(12) -0.0186(12) 0.122 Uiso 1 1 d G . . C3E C 0.1326(12) 0.2431(13) -0.0831(11) 0.185 Uiso 1 1 d G . . C4E C 0.1001(12) 0.1844(13) -0.0781(12) 0.151 Uiso 1 1 d G . . C5E C 0.0833(13) 0.1489(13) -0.0112(14) 0.120 Uiso 1 1 d G . . C6E C 0.1005(13) 0.1730(13) 0.0531(12) 0.117 Uiso 1 1 d G . . C7E C 0.0863(18) 0.1410(17) 0.1196(13) 0.195 Uiso 1 1 d G . . H7E H 0.0639 0.1033 0.1235 0.234 Uiso 1 1 d G . . C8E C 0.104(2) 0.163(2) 0.1802(12) 0.119 Uiso 1 1 d G . . H8E H 0.0947 0.1391 0.2239 0.143 Uiso 1 1 d G . . C9E C 0.1353(17) 0.2205(19) 0.1757(11) 0.190 Uiso 1 1 d G . . H9E H 0.1466 0.2357 0.2165 0.228 Uiso 1 1 d G . . C11E C 0.1501(13) 0.2559(15) 0.1103(12) 0.094 Uiso 1 1 d G . . C10E C 0.1828(16) 0.3138(17) 0.1042(15) 0.119 Uiso 1 1 d G . . H10E H 0.1938 0.3299 0.1448 0.143 Uiso 1 1 d G . . C12E C 0.1985(18) 0.3463(16) 0.0409(17) 0.120 Uiso 1 1 d G . . H12E H 0.2208 0.3840 0.0384 0.144 Uiso 1 1 d G . . C13E C 0.1820(15) 0.3245(14) -0.0200(15) 0.096 Uiso 1 1 d G . . H13E H 0.1924 0.3486 -0.0631 0.116 Uiso 1 1 d G . . C14E C 0.1461(16) 0.2758(17) -0.1501(11) 0.110 Uiso 1 1 d G . . H14E H 0.1684 0.3136 -0.1542 0.132 Uiso 1 1 d G . . C15E C 0.1276(19) 0.254(2) -0.2109(11) 0.119 Uiso 1 1 d G . . H15E H 0.1355 0.2787 -0.2546 0.143 Uiso 1 1 d G . . C16E C 0.0975(18) 0.196(2) -0.2062(13) 0.193 Uiso 1 1 d G . . H16E H 0.0867 0.1802 -0.2470 0.232 Uiso 1 1 d G . . C17E C 0.0829(15) 0.1602(17) -0.1405(14) 0.118 Uiso 1 1 d G . . C18E C 0.0510(19) 0.103(2) -0.1352(19) 0.329 Uiso 1 1 d G . . H18E H 0.0394 0.0870 -0.1757 0.394 Uiso 1 1 d G . . C19E C 0.037(2) 0.0682(19) -0.070(2) 0.231 Uiso 1 1 d G . . H19E H 0.0157 0.0294 -0.0676 0.277 Uiso 1 1 d G . . C20E C 0.0526(19) 0.0909(17) -0.0099(18) 0.310 Uiso 1 1 d G . . H20E H 0.0426 0.0667 0.0332 0.371 Uiso 1 1 d G . . N1 N 0.837(2) 0.320(2) 0.2300(17) 0.086 Uiso 1 1 d D . . C101 C 0.865(3) 0.236(3) 0.213(3) 0.124 Uiso 1 1 d D . . H10F H 0.8582 0.2046 0.2557 0.149 Uiso 1 1 calc R . . H10G H 0.9205 0.2183 0.2003 0.149 Uiso 1 1 calc R . . C102 C 0.825(4) 0.218(3) 0.155(3) 0.131 Uiso 1 1 d D . . H10H H 0.8435 0.2345 0.1096 0.158 Uiso 1 1 calc R . . H10I H 0.7683 0.2448 0.1603 0.158 Uiso 1 1 calc R . . C103 C 0.847(6) 0.130(4) 0.163(4) 0.226 Uiso 1 1 d D . . H10J H 0.9035 0.1021 0.1622 0.271 Uiso 1 1 calc R . . H10K H 0.8235 0.1131 0.2065 0.271 Uiso 1 1 calc R . . C104 C 0.811(6) 0.119(4) 0.099(4) 0.187 Uiso 1 1 d D . . H10L H 0.8317 0.0643 0.0920 0.281 Uiso 1 1 calc R . . H10M H 0.8248 0.1481 0.0589 0.281 Uiso 1 1 calc R . . H10N H 0.7550 0.1372 0.1067 0.281 Uiso 1 1 calc R . . C201 C 0.886(2) 0.326(2) 0.2872(19) 0.030 Uiso 1 1 d D . . H20F H 0.8830 0.2886 0.3266 0.035 Uiso 1 1 calc R . . H20G H 0.9401 0.3091 0.2696 0.035 Uiso 1 1 calc R . . C202 C 0.864(3) 0.404(3) 0.315(4) 0.123 Uiso 1 1 d D . . H20H H 0.8542 0.4443 0.2756 0.148 Uiso 1 1 calc R . . H20I H 0.8152 0.4155 0.3437 0.148 Uiso 1 1 calc R . . C203 C 0.926(4) 0.409(5) 0.358(3) 0.136 Uiso 1 1 d D . . H20J H 0.9391 0.3661 0.3951 0.163 Uiso 1 1 calc R . . H20K H 0.9050 0.4575 0.3802 0.163 Uiso 1 1 calc R . . C204 C 1.000(4) 0.405(5) 0.315(4) 0.174 Uiso 1 1 d D . . H20L H 1.0397 0.4028 0.3458 0.261 Uiso 1 1 calc R . . H20M H 0.9891 0.4504 0.2820 0.261 Uiso 1 1 calc R . . H20N H 1.0195 0.3587 0.2903 0.261 Uiso 1 1 calc R . . C301 C 0.750(2) 0.353(2) 0.251(2) 0.069 Uiso 1 1 d D . . H30F H 0.7336 0.4090 0.2533 0.083 Uiso 1 1 calc R . . H30G H 0.7209 0.3453 0.2145 0.083 Uiso 1 1 calc R . . C302 C 0.730(3) 0.316(4) 0.321(3) 0.110 Uiso 1 1 d D . . H30H H 0.7534 0.2591 0.3209 0.132 Uiso 1 1 calc R . . H30I H 0.7517 0.3307 0.3582 0.132 Uiso 1 1 calc R . . C303 C 0.642(3) 0.342(2) 0.332(4) 0.228 Uiso 1 1 d D . . H30J H 0.6162 0.3987 0.3267 0.274 Uiso 1 1 calc R . . H30K H 0.6196 0.3198 0.3004 0.274 Uiso 1 1 calc R . . C304 C 0.634(4) 0.310(4) 0.407(3) 0.119 Uiso 1 1 d D . . H30L H 0.5798 0.3283 0.4234 0.179 Uiso 1 1 calc R . . H30M H 0.6635 0.3264 0.4365 0.179 Uiso 1 1 calc R . . H30N H 0.6550 0.2534 0.4102 0.179 Uiso 1 1 calc R . . C401 C 0.842(3) 0.371(3) 0.164(2) 0.083 Uiso 1 1 d D . . H40F H 0.8306 0.4233 0.1760 0.100 Uiso 1 1 calc R . . H40G H 0.8014 0.3736 0.1333 0.100 Uiso 1 1 calc R . . C402 C 0.921(4) 0.342(4) 0.124(4) 0.148 Uiso 1 1 d D . . H40H H 0.9305 0.2904 0.1104 0.178 Uiso 1 1 calc R . . H40I H 0.9612 0.3365 0.1559 0.178 Uiso 1 1 calc R . . C403 C 0.929(6) 0.394(4) 0.059(4) 0.162 Uiso 1 1 d D . . H40J H 0.9811 0.3718 0.0363 0.195 Uiso 1 1 calc R . . H40K H 0.8900 0.4000 0.0258 0.195 Uiso 1 1 calc R . . C404 C 0.917(6) 0.472(5) 0.084(5) 0.182 Uiso 1 1 d D . . H40L H 0.9179 0.5083 0.0439 0.274 Uiso 1 1 calc R . . H40M H 0.9577 0.4658 0.1143 0.274 Uiso 1 1 calc R . . H40N H 0.8664 0.4916 0.1090 0.274 Uiso 1 1 calc R . . N2 N 0.812(3) 0.328(3) -0.2736(18) 0.103 Uiso 1 1 d D . . C501 C 0.726(2) 0.350(3) -0.290(3) 0.082 Uiso 1 1 d D . . H50F H 0.6968 0.3475 -0.2452 0.099 Uiso 1 1 calc R . . H50G H 0.7063 0.4041 -0.3091 0.099 Uiso 1 1 calc R . . C502 C 0.702(3) 0.305(4) -0.338(4) 0.139 Uiso 1 1 d D . . H50H H 0.7307 0.3061 -0.3833 0.167 Uiso 1 1 calc R . . H50I H 0.7194 0.2504 -0.3190 0.167 Uiso 1 1 calc R . . C503 C 0.616(3) 0.333(4) -0.352(3) 0.088 Uiso 1 1 d D . . H50J H 0.6079 0.3131 -0.3941 0.106 Uiso 1 1 calc R . . H50K H 0.5919 0.3893 -0.3566 0.106 Uiso 1 1 calc R . . C504 C 0.580(6) 0.299(5) -0.288(3) 0.226 Uiso 1 1 d D . . H50L H 0.5238 0.3198 -0.2895 0.340 Uiso 1 1 calc R . . H50M H 0.5946 0.3133 -0.2459 0.340 Uiso 1 1 calc R . . H50N H 0.5999 0.2431 -0.2868 0.340 Uiso 1 1 calc R . . C601 C 0.853(3) 0.342(3) -0.342(3) 0.101 Uiso 1 1 d D . . H60F H 0.9089 0.3175 -0.3342 0.122 Uiso 1 1 calc R . . H60G H 0.8423 0.3121 -0.3749 0.122 Uiso 1 1 calc R . . C602 C 0.842(5) 0.420(4) -0.382(2) 0.142 Uiso 1 1 d D . . H60H H 0.8538 0.4501 -0.3493 0.170 Uiso 1 1 calc R . . H60I H 0.7860 0.4455 -0.3888 0.170 Uiso 1 1 calc R . . C603 C 0.882(5) 0.435(6) -0.452(3) 0.199 Uiso 1 1 d D . . H60J H 0.8857 0.3980 -0.4844 0.239 Uiso 1 1 calc R . . H60K H 0.8561 0.4881 -0.4729 0.239 Uiso 1 1 calc R . . C604 C 0.962(5) 0.423(6) -0.427(5) 0.192 Uiso 1 1 d D . . H60L H 0.9960 0.4281 -0.4675 0.288 Uiso 1 1 calc R . . H60M H 0.9848 0.3713 -0.4035 0.288 Uiso 1 1 calc R . . H60N H 0.9569 0.4612 -0.3960 0.288 Uiso 1 1 calc R . . C701 C 0.819(3) 0.381(2) -0.222(2) 0.113 Uiso 1 1 d D . . H70F H 0.8060 0.4327 -0.2460 0.135 Uiso 1 1 calc R . . H70G H 0.7788 0.3842 -0.1841 0.135 Uiso 1 1 calc R . . C702 C 0.897(3) 0.356(4) -0.189(3) 0.106 Uiso 1 1 d D . . H70H H 0.9385 0.3497 -0.2266 0.127 Uiso 1 1 calc R . . H70I H 0.9088 0.3065 -0.1616 0.127 Uiso 1 1 calc R . . C703 C 0.899(5) 0.417(5) -0.143(4) 0.156 Uiso 1 1 d D . . H70J H 0.8473 0.4389 -0.1192 0.187 Uiso 1 1 calc R . . H70K H 0.9367 0.3904 -0.1073 0.187 Uiso 1 1 calc R . . C704 C 0.919(8) 0.483(6) -0.182(6) 0.295 Uiso 1 1 d D . . H70L H 0.8723 0.5287 -0.1879 0.443 Uiso 1 1 calc R . . H70M H 0.9441 0.4678 -0.2268 0.443 Uiso 1 1 calc R . . H70N H 0.9550 0.4937 -0.1549 0.443 Uiso 1 1 calc R . . C801 C 0.846(4) 0.245(2) -0.239(3) 0.121 Uiso 1 1 d D . . H80F H 0.9013 0.2314 -0.2325 0.145 Uiso 1 1 calc R . . H80G H 0.8416 0.2095 -0.2705 0.145 Uiso 1 1 calc R . . C802 C 0.805(4) 0.233(2) -0.169(3) 0.144 Uiso 1 1 d D . . H80H H 0.8140 0.2640 -0.1353 0.173 Uiso 1 1 calc R . . H80I H 0.7483 0.2521 -0.1740 0.173 Uiso 1 1 calc R . . C803 C 0.834(4) 0.148(3) -0.140(3) 0.111 Uiso 1 1 d D . . H80J H 0.8908 0.1276 -0.1353 0.133 Uiso 1 1 calc R . . H80K H 0.8092 0.1421 -0.0934 0.133 Uiso 1 1 calc R . . C804 C 0.813(4) 0.105(3) -0.190(2) 0.124 Uiso 1 1 d D . . H80L H 0.8280 0.0509 -0.1731 0.186 Uiso 1 1 calc R . . H80M H 0.8395 0.1095 -0.2352 0.186 Uiso 1 1 calc R . . H80N H 0.7567 0.1276 -0.1958 0.186 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1A 0.016 0.008 0.029 -0.007 -0.004 -0.001 W1A 0.014 0.035 0.067 0.008 0.003 -0.003 W2A 0.040 0.026 0.086 0.026 -0.008 -0.012 W3A 0.036 0.020 0.083 -0.012 0.009 -0.011 W4A 0.028 0.029 0.080 0.010 0.016 -0.015 W5A 0.025 0.030 0.073 -0.003 -0.010 -0.010 W6A 0.039 0.046 0.050 0.000 -0.004 -0.003 Si1B 0.006 0.005 0.005 0.000 0.000 -0.002 W1B 0.031 0.025 0.076 -0.008 -0.007 -0.012 W2B 0.043 0.036 0.045 0.003 0.000 -0.005 W3B 0.024 0.037 0.079 0.015 -0.018 -0.013 W4B 0.030 0.028 0.064 0.014 0.001 -0.019 W5B 0.038 0.014 0.061 0.002 -0.007 -0.003 W6B 0.022 0.042 0.063 -0.001 0.009 -0.012 _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 Si1A O21A 1.57(5) . ? Si1A O21A 1.57(5) 2_665 ? Si1A O19A 1.60(4) . ? Si1A O19A 1.60(4) 2_665 ? Si1A O20A 1.63(5) . ? Si1A O20A 1.63(5) 2_665 ? Si1A O22A 1.71(5) 2_665 ? Si1A O22A 1.71(5) . ? W1A O6A 1.70(5) . ? W1A O1A 1.78(4) . ? W1A O8A 1.84(3) . ? W1A O7A 1.94(3) . ? W1A O4A 1.94(3) . ? W1A O21A 2.44(5) . ? W2A O2A 1.71(4) . ? W2A O5A 1.816(15) . ? W2A O9A 1.86(4) 2_665 ? W2A O4A 1.93(3) . ? W2A O10A 1.95(5) . ? W2A O19A 2.26(4) . ? W2A O20A 2.46(6) 2_665 ? W3A O3A 1.60(4) . ? W3A O11A 1.84(3) . ? W3A O5A 1.896(15) . ? W3A O12A 2.00(4) . ? W3A O6A 2.03(5) . ? W3A O22A 2.37(5) 2_665 ? W3A O19A 2.40(4) . ? W4A O13A 1.69(4) . ? W4A O18A 1.80(4) . ? W4A O14A 1.827(16) . ? W4A O7A 1.84(3) . ? W4A O10A 1.97(5) 2_665 ? W4A O20A 2.34(6) . ? W4A O21A 2.39(5) . ? W5A O15A 1.71(4) . ? W5A O14A 1.884(16) 2_665 ? W5A O16A 1.90(3) . ? W5A O8A 1.93(3) 2_665 ? W5A O11A 1.96(3) . ? W5A O22A 2.10(5) 2_665 ? W5A O21A 2.40(5) 2_665 ? W6A O17A 1.43(3) . ? W6A O9A 1.81(4) . ? W6A O12A 1.84(4) . ? W6A O16A 1.93(3) . ? W6A O18A 2.08(5) . ? W6A O20A 2.34(5) . ? O8A W5A 1.93(3) 2_665 ? O9A W2A 1.86(4) 2_665 ? O10A W4A 1.97(5) 2_665 ? O14A W5A 1.884(16) 2_665 ? O19A O20A 1.81(7) 2_665 ? O20A O21A 1.78(7) . ? O20A O19A 1.81(7) 2_665 ? O20A W2A 2.46(6) 2_665 ? O21A O22A 1.66(7) . ? O21A W5A 2.40(5) 2_665 ? O22A W5A 2.10(5) 2_665 ? O22A W3A 2.37(5) 2_665 ? Si1B O20B 1.513(19) 2_754 ? Si1B O20B 1.513(19) . ? Si1B O21B 1.516(19) 2_754 ? Si1B O21B 1.516(19) . ? Si1B O19B 1.519(19) . ? Si1B O19B 1.519(19) 2_754 ? Si1B O22B 1.528(19) . ? Si1B O22B 1.528(19) 2_754 ? W1B O1B 1.61(4) . ? W1B O7B 1.76(4) 2_754 ? W1B O4B 1.77(4) 2_754 ? W1B O6B 1.98(4) . ? W1B O8B 2.06(3) . ? W1B O19B 2.48(5) 2_754 ? W2B O2B 1.42(3) . ? W2B O9B 1.902(16) . ? W2B O5B 1.91(4) . ? W2B O10B 1.928(16) 2_754 ? W2B O4B 1.95(5) . ? W2B O22B 2.35(4) . ? W2B O19B 2.44(4) . ? W3B O3B 1.63(3) . ? W3B O6B 1.79(4) 2_754 ? W3B O12B 1.81(4) . ? W3B O5B 1.86(4) . ? W3B O11B 1.99(4) . ? W3B O19B 2.39(4) . ? W3B O21B 2.45(5) 2_754 ? W4B O13B 1.68(3) . ? W4B O18B 1.87(4) . ? W4B O14B 1.87(3) . ? W4B O10B 1.879(15) . ? W4B O7B 1.89(4) . ? W4B O20B 2.35(5) 2_754 ? W4B O22B 2.49(4) 2_754 ? W5B O15B 1.69(3) . ? W5B O8B 1.77(3) . ? W5B O16B 1.78(4) . ? W5B O11B 1.87(4) . ? W5B O14B 1.90(3) 2_754 ? W5B O20B 2.42(5) . ? W5B O21B 2.51(5) 2_754 ? W6B O17B 1.71(5) . ? W6B O12B 1.85(4) . ? W6B O9B 1.868(16) 2_754 ? W6B O18B 1.90(4) . ? W6B O16B 1.96(4) . ? W6B O21B 2.35(4) 2_754 ? W6B O22B 2.47(4) 2_754 ? O4B W1B 1.77(4) 2_754 ? O6B W3B 1.79(4) 2_754 ? O7B W1B 1.76(4) 2_754 ? O9B W6B 1.868(16) 2_754 ? O10B W2B 1.928(16) 2_754 ? O14B W5B 1.90(3) 2_754 ? O19B O22B 1.695(19) . ? O19B O21B 1.75(6) 2_754 ? O19B W1B 2.48(5) 2_754 ? O20B O22B 1.71(7) . ? O20B O21B 1.79(7) 2_754 ? O20B W4B 2.35(5) 2_754 ? O21B O22B 1.699(19) . ? O21B O19B 1.75(6) 2_754 ? O21B O20B 1.79(7) 2_754 ? O21B W6B 2.35(4) 2_754 ? O21B W3B 2.45(5) 2_754 ? O21B W5B 2.51(5) 2_754 ? O22B W6B 2.47(4) 2_754 ? O22B W4B 2.49(4) 2_754 ? C1A C2A 1.4107 . ? C1A C6A 1.4278 . ? C1A C10A 1.4306 . ? C2A C13A 1.3985 . ? C2A C3A 1.4611 . ? C3A C14A 1.3952 . ? C3A C4A 1.4178 . ? C4A C17A 1.4287 . ? C4A C5A 1.4338 . ? C5A C20A 1.3887 . ? C5A C6A 1.4605 . ? C6A C7A 1.3868 . ? C7A C8A 1.3790 . ? C7A H7A 0.9300 . ? C8A C9A 1.3863 . ? C8A H8A 0.9300 . ? C9A C10A 1.3974 . ? C9A H9A 0.9300 . ? C10A C11A 1.4052 . ? C11A C12A 1.3457 . ? C11A H11A 0.9300 . ? C12A C13A 1.3762 . ? C12A H12A 0.9300 . ? C13A H13A 0.9301 . ? C14A C15A 1.3885 . ? C14A H14A 0.9300 . ? C15A C16A 1.3802 . ? C15A H15A 0.9300 . ? C16A C17A 1.4022 . ? C16A H16A 0.9300 . ? C17A C18A 1.3925 . ? C18A C19A 1.3756 . ? C18A H18A 0.9300 . ? C19A C20A 1.3727 . ? C19A H19A 0.9300 . ? C20A H20A 0.9300 . ? C1B C2B 1.4107 . ? C1B C6B 1.4278 . ? C1B C10B 1.4306 . ? C2B C13B 1.3985 . ? C2B C3B 1.4610 . ? C3B C14B 1.3952 . ? C3B C4B 1.4178 . ? C4B C17B 1.4287 . ? C4B C5B 1.4338 . ? C5B C20B 1.3887 . ? C5B C6B 1.4605 . ? C6B C7B 1.3868 . ? C7B C8B 1.3790 . ? C7B H7B 0.9300 . ? C8B C9B 1.3863 . ? C8B H8B 0.9300 . ? C9B C10B 1.3974 . ? C9B H9B 0.9300 . ? C10B C11B 1.4052 . ? C11B C12B 1.3458 . ? C11B H11B 0.9300 . ? C12B C13B 1.3761 . ? C12B H12B 0.9300 . ? C13B H13B 0.9300 . ? C14B C15B 1.3885 . ? C14B H14B 0.9300 . ? C15B C16B 1.3802 . ? C15B H15B 0.9300 . ? C16B C17B 1.4022 . ? C16B H16B 0.9300 . ? C17B C18B 1.3925 . ? C18B C19B 1.3756 . ? C18B H18B 0.9300 . ? C19B C20B 1.3726 . ? C19B H19B 0.9300 . ? C20B H20B 0.9300 . ? C1C C2C 1.3644 . ? C1C C6C 1.3770 . ? C1C H1C 0.9300 . ? C2C C3C 1.3785 . ? C2C H2C 0.9300 . ? C3C C7C 1.4072 . ? C3C C4C 1.4176 . ? C4C C10C 1.38(4) 2_675 ? C4C C5C 1.4287 . ? C5C C6C 1.3860 . ? C5C C10C 1.4523 . ? C6C H6C 0.9300 . ? C7C C8C 1.30(7) 2_675 ? C7C H7C 0.9300 . ? C8C C7C 1.30(8) 2_675 ? C8C C9C 1.4106 . ? C8C H8C 0.9300 . ? C9C C10C 1.3764 . ? C9C H9C 0.9300 . ? C10C C4C 1.38(5) 2_675 ? C1D C2D 1.4107 . ? C1D C6D 1.4278 . ? C1D C10D 1.4306 . ? C2D C13D 1.3985 . ? C2D C3D 1.4611 . ? C3D C14D 1.3952 . ? C3D C4D 1.4178 . ? C4D C17D 1.4287 . ? C4D C5D 1.4338 . ? C5D C20D 1.3887 . ? C5D C6D 1.4605 . ? C6D C7D 1.3868 . ? C7D C8D 1.3791 . ? C7D H7D 0.9300 . ? C8D C9D 1.3863 . ? C8D H8D 0.9300 . ? C9D C10D 1.3974 . ? C9D H9D 0.9300 . ? C10D C11D 1.4052 . ? C11D C12D 1.3457 . ? C11D H11D 0.9300 . ? C12D C13D 1.3762 . ? C12D H12D 0.9300 . ? C13D H13D 0.9300 . ? C14D C15D 1.3885 . ? C14D H14D 0.9300 . ? C15D C16D 1.3802 . ? C15D H15D 0.9300 . ? C16D C17D 1.4022 . ? C16D H16D 0.9300 . ? C17D C18D 1.3925 . ? C18D C19D 1.3756 . ? C18D H18D 0.9300 . ? C19D C20D 1.3727 . ? C19D H19D 0.9300 . ? C20D H20D 0.9300 . ? C1E C2E 1.4107 . ? C1E C6E 1.4278 . ? C1E C11E 1.4306 . ? C2E C13E 1.3985 . ? C2E C3E 1.4610 . ? C3E C14E 1.3952 . ? C3E C4E 1.4178 . ? C4E C17E 1.4287 . ? C4E C5E 1.4338 . ? C5E C20E 1.3887 . ? C5E C6E 1.4605 . ? C6E C7E 1.3868 . ? C7E C8E 1.3790 . ? C7E H7E 0.9300 . ? C8E C9E 1.3863 . ? C8E H8E 0.9300 . ? C9E C11E 1.3974 . ? C9E H9E 0.9300 . ? C11E C10E 1.4053 . ? C10E C12E 1.3457 . ? C10E H10E 0.9300 . ? C12E C13E 1.3762 . ? C12E H12E 0.9300 . ? C13E H13E 0.9300 . ? C14E C15E 1.3885 . ? C14E H14E 0.9300 . ? C15E C16E 1.3802 . ? C15E H15E 0.9300 . ? C16E C17E 1.4022 . ? C16E H16E 0.9300 . ? C17E C18E 1.3925 . ? C18E C19E 1.3756 . ? C18E H18E 0.9300 . ? C19E C20E 1.3726 . ? C19E H19E 0.9300 . ? C20E H20E 0.9300 . ? N1 C401 1.504(19) . ? N1 C101 1.506(19) . ? N1 C201 1.513(19) . ? N1 C301 1.514(19) . ? C101 C102 1.51(2) . ? C101 H10F 0.9700 . ? C101 H10G 0.9700 . ? C102 C103 1.51(2) . ? C102 H10H 0.9700 . ? C102 H10I 0.9700 . ? C103 C104 1.51(2) . ? C103 H10J 0.9700 . ? C103 H10K 0.9700 . ? C104 H10L 0.9600 . ? C104 H10M 0.9600 . ? C104 H10N 0.9600 . ? C201 C202 1.505(19) . ? C201 H20F 0.9700 . ? C201 H20G 0.9700 . ? C202 C203 1.50(2) . ? C202 H20H 0.9700 . ? C202 H20I 0.9700 . ? C203 C204 1.51(2) . ? C203 H20J 0.9700 . ? C203 H20K 0.9700 . ? C204 H20L 0.9600 . ? C204 H20M 0.9600 . ? C204 H20N 0.9600 . ? C301 C302 1.512(19) . ? C301 H30F 0.9700 . ? C301 H30G 0.9700 . ? C302 C303 1.51(2) . ? C302 H30H 0.9700 . ? C302 H30I 0.9700 . ? C303 C304 1.51(2) . ? C303 H30J 0.9700 . ? C303 H30K 0.9700 . ? C304 H30L 0.9600 . ? C304 H30M 0.9600 . ? C304 H30N 0.9600 . ? C401 C402 1.51(2) . ? C401 H40F 0.9700 . ? C401 H40G 0.9700 . ? C402 C403 1.52(2) . ? C402 H40H 0.9700 . ? C402 H40I 0.9700 . ? C403 C404 1.50(2) . ? C403 H40J 0.9700 . ? C403 H40K 0.9700 . ? C404 H40L 0.9600 . ? C404 H40M 0.9600 . ? C404 H40N 0.9600 . ? N2 C601 1.504(19) . ? N2 C801 1.510(19) . ? N2 C701 1.520(19) . ? N2 C501 1.525(19) . ? C501 C502 1.51(2) . ? C501 H50F 0.9700 . ? C501 H50G 0.9700 . ? C502 C503 1.51(2) . ? C502 H50H 0.9700 . ? C502 H50I 0.9700 . ? C503 C504 1.51(2) . ? C503 H50J 0.9700 . ? C503 H50K 0.9700 . ? C504 H50L 0.9600 . ? C504 H50M 0.9600 . ? C504 H50N 0.9600 . ? C601 C602 1.50(2) . ? C601 H60F 0.9700 . ? C601 H60G 0.9700 . ? C602 C603 1.52(2) . ? C602 H60H 0.9700 . ? C602 H60I 0.9700 . ? C603 C604 1.50(2) . ? C603 H60J 0.9700 . ? C603 H60K 0.9700 . ? C604 H60L 0.9600 . ? C604 H60M 0.9600 . ? C604 H60N 0.9600 . ? C701 C702 1.51(2) . ? C701 H70F 0.9700 . ? C701 H70G 0.9700 . ? C702 C703 1.52(2) . ? C702 H70H 0.9700 . ? C702 H70I 0.9700 . ? C703 C704 1.51(2) . ? C703 H70J 0.9700 . ? C703 H70K 0.9700 . ? C704 H70L 0.9600 . ? C704 H70M 0.9600 . ? C704 H70N 0.9600 . ? C801 C802 1.52(2) . ? C801 H80F 0.9700 . ? C801 H80G 0.9700 . ? C802 C803 1.515(19) . ? C802 H80H 0.9700 . ? C802 H80I 0.9700 . ? C803 C804 1.495(19) . ? C803 H80J 0.9700 . ? C803 H80K 0.9700 . ? C804 H80L 0.9600 . ? C804 H80M 0.9600 . ? C804 H80N 0.9600 . ? 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 O21A Si1A O21A 180(4) . 2_665 ? O21A Si1A O19A 78(2) . . ? O21A Si1A O19A 102(2) 2_665 . ? O21A Si1A O19A 102(2) . 2_665 ? O21A Si1A O19A 78(2) 2_665 2_665 ? O19A Si1A O19A 180(3) . 2_665 ? O21A Si1A O20A 67(3) . . ? O21A Si1A O20A 113(3) 2_665 . ? O19A Si1A O20A 112(2) . . ? O19A Si1A O20A 68(2) 2_665 . ? O21A Si1A O20A 113(3) . 2_665 ? O21A Si1A O20A 67(3) 2_665 2_665 ? O19A Si1A O20A 68(2) . 2_665 ? O19A Si1A O20A 112(2) 2_665 2_665 ? O20A Si1A O20A 180(5) . 2_665 ? O21A Si1A O22A 119(2) . 2_665 ? O21A Si1A O22A 61(2) 2_665 2_665 ? O19A Si1A O22A 69(2) . 2_665 ? O19A Si1A O22A 111(2) 2_665 2_665 ? O20A Si1A O22A 79(2) . 2_665 ? O20A Si1A O22A 101(2) 2_665 2_665 ? O21A Si1A O22A 61(2) . . ? O21A Si1A O22A 119(2) 2_665 . ? O19A Si1A O22A 111(2) . . ? O19A Si1A O22A 69(2) 2_665 . ? O20A Si1A O22A 101(2) . . ? O20A Si1A O22A 79(2) 2_665 . ? O22A Si1A O22A 180(3) 2_665 . ? O6A W1A O1A 101(2) . . ? O6A W1A O8A 155(2) . . ? O1A W1A O8A 103.4(15) . . ? O6A W1A O7A 85(2) . . ? O1A W1A O7A 99.5(16) . . ? O8A W1A O7A 89.6(14) . . ? O6A W1A O4A 96(2) . . ? O1A W1A O4A 97.9(16) . . ? O8A W1A O4A 82.5(14) . . ? O7A W1A O4A 162.1(14) . . ? O6A W1A O21A 92(2) . . ? O1A W1A O21A 158.0(17) . . ? O8A W1A O21A 63.8(15) . . ? O7A W1A O21A 64.1(15) . . ? O4A W1A O21A 98.0(16) . . ? O2A W2A O5A 106.7(14) . . ? O2A W2A O9A 103.6(18) . 2_665 ? O5A W2A O9A 149.7(16) . 2_665 ? O2A W2A O4A 95.4(16) . . ? O5A W2A O4A 89.3(13) . . ? O9A W2A O4A 89.4(17) 2_665 . ? O2A W2A O10A 96.9(18) . . ? O5A W2A O10A 86.5(16) . . ? O9A W2A O10A 88.3(19) 2_665 . ? O4A W2A O10A 167.6(18) . . ? O2A W2A O19A 159.8(15) . . ? O5A W2A O19A 59.6(12) . . ? O9A W2A O19A 91.5(17) 2_665 . ? O4A W2A O19A 71.0(14) . . ? O10A W2A O19A 96.8(17) . . ? O2A W2A O20A 155.3(17) . 2_665 ? O5A W2A O20A 92.4(15) . 2_665 ? O9A W2A O20A 58.2(19) 2_665 2_665 ? O4A W2A O20A 100.6(17) . 2_665 ? O10A W2A O20A 68.0(19) . 2_665 ? O19A W2A O20A 44.9(16) . 2_665 ? O3A W3A O11A 96.8(16) . . ? O3A W3A O5A 106.5(15) . . ? O11A W3A O5A 86.5(13) . . ? O3A W3A O12A 98.8(17) . . ? O11A W3A O12A 92.4(15) . . ? O5A W3A O12A 154.6(12) . . ? O3A W3A O6A 108(2) . . ? O11A W3A O6A 154.5(18) . . ? O5A W3A O6A 90.1(17) . . ? O12A W3A O6A 80.0(18) . . ? O3A W3A O22A 151.7(17) . 2_665 ? O11A W3A O22A 58.3(15) . 2_665 ? O5A W3A O22A 86.6(14) . 2_665 ? O12A W3A O22A 71.4(15) . 2_665 ? O6A W3A O22A 96.3(19) . 2_665 ? O3A W3A O19A 159.5(16) . . ? O11A W3A O19A 92.8(13) . . ? O5A W3A O19A 55.9(12) . . ? O12A W3A O19A 98.9(14) . . ? O6A W3A O19A 64.8(17) . . ? O22A W3A O19A 46.4(15) 2_665 . ? O13A W4A O18A 93.7(19) . . ? O13A W4A O14A 102.5(15) . . ? O18A W4A O14A 162.3(17) . . ? O13A W4A O7A 97.0(16) . . ? O18A W4A O7A 86.7(18) . . ? O14A W4A O7A 84.4(15) . . ? O13A W4A O10A 97.8(19) . 2_665 ? O18A W4A O10A 91(2) . 2_665 ? O14A W4A O10A 94.0(17) . 2_665 ? O7A W4A O10A 165.0(17) . 2_665 ? O13A W4A O20A 158.9(18) . . ? O18A W4A O20A 70(2) . . ? O14A W4A O20A 95.8(16) . . ? O7A W4A O20A 95.1(17) . . ? O10A W4A O20A 70.2(19) 2_665 . ? O13A W4A O21A 156.7(17) . . ? O18A W4A O21A 101.1(19) . . ? O14A W4A O21A 61.3(15) . . ? O7A W4A O21A 66.4(16) . . ? O10A W4A O21A 99.8(18) 2_665 . ? O20A W4A O21A 44.1(18) . . ? O15A W5A O14A 103.9(16) . 2_665 ? O15A W5A O16A 98.6(16) . . ? O14A W5A O16A 157.1(13) 2_665 . ? O15A W5A O8A 100.5(16) . 2_665 ? O14A W5A O8A 85.8(14) 2_665 2_665 ? O16A W5A O8A 86.0(14) . 2_665 ? O15A W5A O11A 102.9(16) . . ? O14A W5A O11A 88.0(14) 2_665 . ? O16A W5A O11A 91.2(14) . . ? O8A W5A O11A 156.6(13) 2_665 . ? O15A W5A O22A 160.5(18) . 2_665 ? O14A W5A O22A 88.7(16) 2_665 2_665 ? O16A W5A O22A 70.8(16) . 2_665 ? O8A W5A O22A 95.2(16) 2_665 2_665 ? O11A W5A O22A 62.2(16) . 2_665 ? O15A W5A O21A 156.9(18) . 2_665 ? O14A W5A O21A 60.4(14) 2_665 2_665 ? O16A W5A O21A 96.9(16) . 2_665 ? O8A W5A O21A 63.5(15) 2_665 2_665 ? O11A W5A O21A 93.9(15) . 2_665 ? O22A W5A O21A 42.6(17) 2_665 2_665 ? O17A W6A O9A 102.8(18) . . ? O17A W6A O12A 101.2(15) . . ? O9A W6A O12A 156.0(17) . . ? O17A W6A O16A 100.4(15) . . ? O9A W6A O16A 82.1(18) . . ? O12A W6A O16A 92.2(15) . . ? O17A W6A O18A 97.7(17) . . ? O9A W6A O18A 89.5(19) . . ? O12A W6A O18A 88.6(17) . . ? O16A W6A O18A 161.3(15) . . ? O17A W6A O20A 155.8(18) . . ? O9A W6A O20A 61(2) . . ? O12A W6A O20A 96.2(17) . . ? O16A W6A O20A 95.6(17) . . ? O18A W6A O20A 65.7(18) . . ? W2A O4A W1A 130.6(19) . . ? W2A O5A W3A 144.0(15) . . ? W1A O6A W3A 138(3) . . ? W4A O7A W1A 136.2(19) . . ? W1A O8A W5A 138.0(18) . 2_665 ? W6A O9A W2A 145(3) . 2_665 ? W2A O10A W4A 128(3) . 2_665 ? W3A O11A W5A 134.6(18) . . ? W6A O12A W3A 132.8(19) . . ? W4A O14A W5A 143.6(16) . 2_665 ? W5A O16A W6A 134.7(18) . . ? W4A O18A W6A 128(2) . . ? Si1A O19A O20A 57(2) . 2_665 ? Si1A O19A W2A 130(2) . . ? O20A O19A W2A 73(2) 2_665 . ? Si1A O19A W3A 122(2) . . ? O20A O19A W3A 139(3) 2_665 . ? W2A O19A W3A 98.6(15) . . ? Si1A O20A O21A 54(2) . . ? Si1A O20A O19A 55(2) . 2_665 ? O21A O20A O19A 86(3) . 2_665 ? Si1A O20A W6A 125(3) . . ? O21A O20A W6A 135(3) . . ? O19A O20A W6A 133(3) 2_665 . ? Si1A O20A W4A 124(3) . . ? O21A O20A W4A 69(2) . . ? O19A O20A W4A 123(3) 2_665 . ? W6A O20A W4A 96(2) . . ? Si1A O20A W2A 117(3) . 2_665 ? O21A O20A W2A 128(3) . 2_665 ? O19A O20A W2A 62(2) 2_665 2_665 ? W6A O20A W2A 93.9(19) . 2_665 ? W4A O20A W2A 94(2) . 2_665 ? Si1A O21A O22A 64(3) . . ? Si1A O21A O20A 58(2) . . ? O22A O21A O20A 97(4) . . ? Si1A O21A W4A 124(3) . . ? O22A O21A W4A 124(3) . . ? O20A O21A W4A 67(2) . . ? Si1A O21A W5A 122(3) . 2_665 ? O22A O21A W5A 59(2) . 2_665 ? O20A O21A W5A 136(3) . 2_665 ? W4A O21A W5A 94.7(18) . 2_665 ? Si1A O21A W1A 121(3) . . ? O22A O21A W1A 133(3) . . ? O20A O21A W1A 126(3) . . ? W4A O21A W1A 93.1(17) . . ? W5A O21A W1A 93.4(17) 2_665 . ? O21A O22A Si1A 55(2) . . ? O21A O22A W5A 79(3) . 2_665 ? Si1A O22A W5A 133(3) . 2_665 ? O21A O22A W3A 142(3) . 2_665 ? Si1A O22A W3A 118(2) . 2_665 ? W5A O22A W3A 103.2(19) 2_665 2_665 ? O20B Si1B O20B 180.000(7) 2_754 . ? O20B Si1B O21B 107(3) 2_754 2_754 ? O20B Si1B O21B 73(3) . 2_754 ? O20B Si1B O21B 73(3) 2_754 . ? O20B Si1B O21B 107(3) . . ? O21B Si1B O21B 180.000(5) 2_754 . ? O20B Si1B O19B 77(3) 2_754 . ? O20B Si1B O19B 103(3) . . ? O21B Si1B O19B 70(3) 2_754 . ? O21B Si1B O19B 110(3) . . ? O20B Si1B O19B 103(3) 2_754 2_754 ? O20B Si1B O19B 77(3) . 2_754 ? O21B Si1B O19B 110(3) 2_754 2_754 ? O21B Si1B O19B 70(3) . 2_754 ? O19B Si1B O19B 180.000(5) . 2_754 ? O20B Si1B O22B 112(3) 2_754 . ? O20B Si1B O22B 68(3) . . ? O21B Si1B O22B 112.2(11) 2_754 . ? O21B Si1B O22B 67.8(11) . . ? O19B Si1B O22B 67.6(11) . . ? O19B Si1B O22B 112.4(11) 2_754 . ? O20B Si1B O22B 68(3) 2_754 2_754 ? O20B Si1B O22B 112(3) . 2_754 ? O21B Si1B O22B 67.8(11) 2_754 2_754 ? O21B Si1B O22B 112.2(11) . 2_754 ? O19B Si1B O22B 112.4(11) . 2_754 ? O19B Si1B O22B 67.6(11) 2_754 2_754 ? O22B Si1B O22B 180.000(4) . 2_754 ? O1B W1B O7B 111.9(19) . 2_754 ? O1B W1B O4B 100.6(19) . 2_754 ? O7B W1B O4B 147(2) 2_754 2_754 ? O1B W1B O6B 101.7(17) . . ? O7B W1B O6B 84.8(17) 2_754 . ? O4B W1B O6B 88.7(18) 2_754 . ? O1B W1B O8B 101.0(16) . . ? O7B W1B O8B 92.6(17) 2_754 . ? O4B W1B O8B 80.9(17) 2_754 . ? O6B W1B O8B 156.5(15) . . ? O1B W1B O19B 156.3(15) . 2_754 ? O7B W1B O19B 85.8(17) 2_754 2_754 ? O4B W1B O19B 63.0(17) 2_754 2_754 ? O6B W1B O19B 63.1(14) . 2_754 ? O8B W1B O19B 93.4(14) . 2_754 ? O2B W2B O9B 108.7(16) . . ? O2B W2B O5B 96.2(18) . . ? O9B W2B O5B 154.9(14) . . ? O2B W2B O10B 113.2(16) . 2_754 ? O9B W2B O10B 87.4(14) . 2_754 ? O5B W2B O10B 85.3(15) . 2_754 ? O2B W2B O4B 93.0(19) . . ? O9B W2B O4B 83.2(18) . . ? O5B W2B O4B 92.9(18) . . ? O10B W2B O4B 153.7(14) 2_754 . ? O2B W2B O22B 173.1(16) . . ? O9B W2B O22B 64.9(12) . . ? O5B W2B O22B 90.4(15) . . ? O10B W2B O22B 65.3(13) 2_754 . ? O4B W2B O22B 88.6(16) . . ? O2B W2B O19B 144.5(16) . . ? O9B W2B O19B 94.0(14) . . ? O5B W2B O19B 62.7(16) . . ? O10B W2B O19B 94.2(13) 2_754 . ? O4B W2B O19B 62.2(17) . . ? O22B W2B O19B 41.4(4) . . ? O3B W3B O6B 98.4(16) . 2_754 ? O3B W3B O12B 106.1(17) . . ? O6B W3B O12B 97.1(17) 2_754 . ? O3B W3B O5B 98.5(16) . . ? O6B W3B O5B 90.6(17) 2_754 . ? O12B W3B O5B 152.8(18) . . ? O3B W3B O11B 99.1(16) . . ? O6B W3B O11B 161.5(16) 2_754 . ? O12B W3B O11B 83.7(17) . . ? O5B W3B O11B 81.0(17) . . ? O3B W3B O19B 156.5(13) . . ? O6B W3B O19B 67.5(16) 2_754 . ? O12B W3B O19B 94.6(16) . . ? O5B W3B O19B 64.4(16) . . ? O11B W3B O19B 94.0(16) . . ? O3B W3B O21B 160.9(13) . 2_754 ? O6B W3B O21B 96.4(16) 2_754 2_754 ? O12B W3B O21B 59.9(16) . 2_754 ? O5B W3B O21B 93.4(15) . 2_754 ? O11B W3B O21B 67.9(16) . 2_754 ? O19B W3B O21B 42.4(11) . 2_754 ? O13B W4B O18B 99.0(16) . . ? O13B W4B O14B 102.7(14) . . ? O18B W4B O14B 158.0(16) . . ? O13B W4B O10B 98.9(12) . . ? O18B W4B O10B 86.4(15) . . ? O14B W4B O10B 86.9(14) . . ? O13B W4B O7B 109.5(16) . . ? O18B W4B O7B 86.6(17) . . ? O14B W4B O7B 89.4(16) . . ? O10B W4B O7B 151.5(15) . . ? O13B W4B O20B 162.5(14) . 2_754 ? O18B W4B O20B 95.7(17) . 2_754 ? O14B W4B O20B 63.6(16) . 2_754 ? O10B W4B O20B 91.5(15) . 2_754 ? O7B W4B O20B 61.8(19) . 2_754 ? O13B W4B O22B 155.9(12) . 2_754 ? O18B W4B O22B 65.8(15) . 2_754 ? O14B W4B O22B 92.5(14) . 2_754 ? O10B W4B O22B 62.9(11) . 2_754 ? O7B W4B O22B 89.0(15) . 2_754 ? O20B W4B O22B 41.3(12) 2_754 2_754 ? O15B W5B O8B 94.3(16) . . ? O15B W5B O16B 100.2(18) . . ? O8B W5B O16B 83.8(17) . . ? O15B W5B O11B 102.0(17) . . ? O8B W5B O11B 163.5(16) . . ? O16B W5B O11B 90.9(18) . . ? O15B W5B O14B 101.6(15) . 2_754 ? O8B W5B O14B 94.3(15) . 2_754 ? O16B W5B O14B 158.1(16) . 2_754 ? O11B W5B O14B 84.8(15) . 2_754 ? O15B W5B O20B 157.3(15) . . ? O8B W5B O20B 73.1(17) . . ? O16B W5B O20B 97.1(17) . . ? O11B W5B O20B 92.2(17) . . ? O14B W5B O20B 61.8(15) 2_754 . ? O15B W5B O21B 159.9(14) . 2_754 ? O8B W5B O21B 95.5(15) . 2_754 ? O16B W5B O21B 63.6(16) . 2_754 ? O11B W5B O21B 68.2(16) . 2_754 ? O14B W5B O21B 95.1(13) 2_754 2_754 ? O20B W5B O21B 42.7(11) . 2_754 ? O17B W6B O12B 101(2) . . ? O17B W6B O9B 103.1(17) . 2_754 ? O12B W6B O9B 154.7(16) . 2_754 ? O17B W6B O18B 100(2) . . ? O12B W6B O18B 93.3(17) . . ? O9B W6B O18B 88.7(16) 2_754 . ? O17B W6B O16B 103(2) . . ? O12B W6B O16B 81.0(17) . . ? O9B W6B O16B 87.5(17) 2_754 . ? O18B W6B O16B 157.2(17) . . ? O17B W6B O21B 159.8(17) . 2_754 ? O12B W6B O21B 61.8(17) . 2_754 ? O9B W6B O21B 92.9(15) 2_754 2_754 ? O18B W6B O21B 92.7(17) . 2_754 ? O16B W6B O21B 65.1(17) . 2_754 ? O17B W6B O22B 158.9(17) . 2_754 ? O12B W6B O22B 95.2(15) . 2_754 ? O9B W6B O22B 62.7(12) 2_754 2_754 ? O18B W6B O22B 65.9(16) . 2_754 ? O16B W6B O22B 92.5(16) . 2_754 ? O21B W6B O22B 41.2(4) 2_754 2_754 ? W1B O4B W2B 142(2) 2_754 . ? W3B O5B W2B 137(2) . . ? W3B O6B W1B 137(2) 2_754 . ? W1B O7B W4B 148(3) 2_754 . ? W5B O8B W1B 131.9(18) . . ? W6B O9B W2B 137.8(15) 2_754 . ? W4B O10B W2B 137.3(14) . 2_754 ? W5B O11B W3B 132(2) . . ? W3B O12B W6B 145(2) . . ? W4B O14B W5B 137.7(19) . 2_754 ? W5B O16B W6B 139(2) . . ? W4B O18B W6B 138(2) . . ? Si1B O19B O22B 56.5(9) . . ? Si1B O19B O21B 54.7(15) . 2_754 ? O22B O19B O21B 94(2) . 2_754 ? Si1B O19B W3B 125(3) . . ? O22B O19B W3B 133(3) . . ? O21B O19B W3B 71(2) 2_754 . ? Si1B O19B W2B 123(2) . . ? O22B O19B W2B 67(2) . . ? O21B O19B W2B 136(3) 2_754 . ? W3B O19B W2B 93.1(12) . . ? Si1B O19B W1B 123(3) . 2_754 ? O22B O19B W1B 128(3) . 2_754 ? O21B O19B W1B 129(3) 2_754 2_754 ? W3B O19B W1B 92.4(10) . 2_754 ? W2B O19B W1B 90.9(12) . 2_754 ? Si1B O20B O22B 56.3(16) . . ? Si1B O20B O21B 53.8(16) . 2_754 ? O22B O20B O21B 92(3) . 2_754 ? Si1B O20B W4B 129(3) . 2_754 ? O22B O20B W4B 74(2) . 2_754 ? O21B O20B W4B 143(3) 2_754 2_754 ? Si1B O20B W5B 125(3) . . ? O22B O20B W5B 137(3) . . ? O21B O20B W5B 71(2) 2_754 . ? W4B O20B W5B 95.2(11) 2_754 . ? Si1B O21B O22B 56.4(9) . . ? Si1B O21B O19B 54.8(15) . 2_754 ? O22B O21B O19B 94(2) . 2_754 ? Si1B O21B O20B 53.6(17) . 2_754 ? O22B O21B O20B 92(2) . 2_754 ? O19B O21B O20B 84(2) 2_754 2_754 ? Si1B O21B W6B 129(2) . 2_754 ? O22B O21B W6B 73(2) . 2_754 ? O19B O21B W6B 136(3) 2_754 2_754 ? O20B O21B W6B 137(3) 2_754 2_754 ? Si1B O21B W3B 122(3) . 2_754 ? O22B O21B W3B 137(3) . 2_754 ? O19B O21B W3B 67(2) 2_754 2_754 ? O20B O21B W3B 122(3) 2_754 2_754 ? W6B O21B W3B 93.4(12) 2_754 2_754 ? Si1B O21B W5B 120(3) . 2_754 ? O22B O21B W5B 129(3) . 2_754 ? O19B O21B W5B 126(3) 2_754 2_754 ? O20B O21B W5B 66(2) 2_754 2_754 ? W6B O21B W5B 92.2(13) 2_754 2_754 ? W3B O21B W5B 90.8(11) 2_754 2_754 ? Si1B O22B O19B 55.9(9) . . ? Si1B O22B O21B 55.8(9) . . ? O19B O22B O21B 94(2) . . ? Si1B O22B O20B 55.4(16) . . ? O19B O22B O20B 89(3) . . ? O21B O22B O20B 92(3) . . ? Si1B O22B W2B 128(2) . . ? O19B O22B W2B 72(2) . . ? O21B O22B W2B 135(3) . . ? O20B O22B W2B 129(3) . . ? Si1B O22B W6B 121(2) . 2_754 ? O19B O22B W6B 135(3) . 2_754 ? O21B O22B W6B 66(2) . 2_754 ? O20B O22B W6B 130(3) . 2_754 ? W2B O22B W6B 93.7(12) . 2_754 ? Si1B O22B W4B 120(3) . 2_754 ? O19B O22B W4B 132(3) . 2_754 ? O21B O22B W4B 124(3) . 2_754 ? O20B O22B W4B 65(2) . 2_754 ? W2B O22B W4B 94.2(10) . 2_754 ? W6B O22B W4B 90.4(10) 2_754 2_754 ? C2A C1A C6A 121.7 . . ? C2A C1A C10A 119.5 . . ? C6A C1A C10A 118.8 . . ? C13A C2A C1A 118.4 . . ? C13A C2A C3A 121.9 . . ? C1A C2A C3A 119.7 . . ? C14A C3A C4A 117.7 . . ? C14A C3A C2A 123.1 . . ? C4A C3A C2A 119.2 . . ? C3A C4A C17A 120.0 . . ? C3A C4A C5A 121.2 . . ? C17A C4A C5A 118.7 . . ? C20A C5A C4A 118.4 . . ? C20A C5A C6A 122.2 . . ? C4A C5A C6A 119.4 . . ? C7A C6A C1A 118.5 . . ? C7A C6A C5A 122.7 . . ? C1A C6A C5A 118.8 . . ? C8A C7A C6A 122.7 . . ? C8A C7A H7A 118.7 . . ? C6A C7A H7A 118.7 . . ? C7A C8A C9A 119.6 . . ? C7A C8A H8A 120.2 . . ? C9A C8A H8A 120.2 . . ? C8A C9A C10A 120.6 . . ? C8A C9A H9A 119.7 . . ? C10A C9A H9A 119.7 . . ? C9A C10A C11A 121.6 . . ? C9A C10A C1A 119.8 . . ? C11A C10A C1A 118.5 . . ? C12A C11A C10A 121.2 . . ? C12A C11A H11A 119.4 . . ? C10A C11A H11A 119.4 . . ? C11A C12A C13A 120.9 . . ? C11A C12A H12A 119.6 . . ? C13A C12A H12A 119.6 . . ? C12A C13A C2A 121.5 . . ? C12A C13A H13A 119.3 . . ? C2A C13A H13A 119.3 . . ? C15A C14A C3A 122.7 . . ? C15A C14A H14A 118.7 . . ? C3A C14A H14A 118.7 . . ? C16A C15A C14A 119.5 . . ? C16A C15A H15A 120.2 . . ? C14A C15A H15A 120.2 . . ? C15A C16A C17A 120.8 . . ? C15A C16A H16A 119.6 . . ? C17A C16A H16A 119.6 . . ? C18A C17A C16A 121.2 . . ? C18A C17A C4A 119.7 . . ? C16A C17A C4A 119.2 . . ? C19A C18A C17A 120.6 . . ? C19A C18A H18A 119.7 . . ? C17A C18A H18A 119.7 . . ? C20A C19A C18A 120.5 . . ? C20A C19A H19A 119.7 . . ? C18A C19A H19A 119.7 . . ? C19A C20A C5A 122.0 . . ? C19A C20A H20A 119.0 . . ? C5A C20A H20A 119.0 . . ? C2B C1B C6B 121.7 . . ? C2B C1B C10B 119.5 . . ? C6B C1B C10B 118.8 . . ? C13B C2B C1B 118.4 . . ? C13B C2B C3B 121.9 . . ? C1B C2B C3B 119.7 . . ? C14B C3B C4B 117.7 . . ? C14B C3B C2B 123.1 . . ? C4B C3B C2B 119.2 . . ? C3B C4B C17B 120.1 . . ? C3B C4B C5B 121.2 . . ? C17B C4B C5B 118.7 . . ? C20B C5B C4B 118.4 . . ? C20B C5B C6B 122.2 . . ? C4B C5B C6B 119.4 . . ? C7B C6B C1B 118.5 . . ? C7B C6B C5B 122.7 . . ? C1B C6B C5B 118.8 . . ? C8B C7B C6B 122.7 . . ? C8B C7B H7B 118.6 . . ? C6B C7B H7B 118.7 . . ? C7B C8B C9B 119.6 . . ? C7B C8B H8B 120.2 . . ? C9B C8B H8B 120.2 . . ? C8B C9B C10B 120.6 . . ? C8B C9B H9B 119.7 . . ? C10B C9B H9B 119.7 . . ? C9B C10B C11B 121.6 . . ? C9B C10B C1B 119.8 . . ? C11B C10B C1B 118.5 . . ? C12B C11B C10B 121.2 . . ? C12B C11B H11B 119.4 . . ? C10B C11B H11B 119.4 . . ? C11B C12B C13B 120.9 . . ? C11B C12B H12B 119.6 . . ? C13B C12B H12B 119.6 . . ? C12B C13B C2B 121.5 . . ? C12B C13B H13B 119.3 . . ? C2B C13B H13B 119.3 . . ? C15B C14B C3B 122.7 . . ? C15B C14B H14B 118.7 . . ? C3B C14B H14B 118.7 . . ? C16B C15B C14B 119.5 . . ? C16B C15B H15B 120.2 . . ? C14B C15B H15B 120.2 . . ? C15B C16B C17B 120.8 . . ? C15B C16B H16B 119.6 . . ? C17B C16B H16B 119.6 . . ? C18B C17B C16B 121.2 . . ? C18B C17B C4B 119.7 . . ? C16B C17B C4B 119.2 . . ? C19B C18B C17B 120.6 . . ? C19B C18B H18B 119.7 . . ? C17B C18B H18B 119.7 . . ? C20B C19B C18B 120.5 . . ? C20B C19B H19B 119.7 . . ? C18B C19B H19B 119.7 . . ? C19B C20B C5B 122.0 . . ? C19B C20B H20B 119.0 . . ? C5B C20B H20B 119.0 . . ? C2C C1C C6C 120.1 . . ? C2C C1C H1C 120.0 . . ? C6C C1C H1C 120.0 . . ? C1C C2C C3C 119.8 . . ? C1C C2C H2C 120.1 . . ? C3C C2C H2C 120.1 . . ? C2C C3C C7C 120.3 . . ? C2C C3C C4C 121.1 . . ? C7C C3C C4C 118.5 . . ? C10C C4C C3C 118(2) 2_675 . ? C10C C4C C5C 123(2) 2_675 . ? C3C C4C C5C 118.8 . . ? C6C C5C C4C 116.9 . . ? C6C C5C C10C 123.7 . . ? C4C C5C C10C 119.5 . . ? C1C C6C C5C 123.2 . . ? C1C C6C H6C 118.4 . . ? C5C C6C H6C 118.4 . . ? C8C C7C C3C 123(3) 2_675 . ? C8C C7C H7C 117.0 2_675 . ? C3C C7C H7C 119.4 . . ? C7C C8C C9C 118(3) 2_675 . ? C7C C8C H8C 122.0 2_675 . ? C9C C8C H8C 119.7 . . ? C10C C9C C8C 121.1 . . ? C10C C9C H9C 119.4 . . ? C8C C9C H9C 119.4 . . ? C9C C10C C4C 120(2) . 2_675 ? C9C C10C C5C 122.0 . . ? C4C C10C C5C 117(2) 2_675 . ? C2D C1D C6D 121.7 . . ? C2D C1D C10D 119.5 . . ? C6D C1D C10D 118.8 . . ? C13D C2D C1D 118.4 . . ? C13D C2D C3D 121.9 . . ? C1D C2D C3D 119.7 . . ? C14D C3D C4D 117.7 . . ? C14D C3D C2D 123.1 . . ? C4D C3D C2D 119.2 . . ? C3D C4D C17D 120.1 . . ? C3D C4D C5D 121.2 . . ? C17D C4D C5D 118.7 . . ? C20D C5D C4D 118.4 . . ? C20D C5D C6D 122.2 . . ? C4D C5D C6D 119.4 . . ? C7D C6D C1D 118.5 . . ? C7D C6D C5D 122.7 . . ? C1D C6D C5D 118.8 . . ? C8D C7D C6D 122.7 . . ? C8D C7D H7D 118.7 . . ? C6D C7D H7D 118.7 . . ? C7D C8D C9D 119.6 . . ? C7D C8D H8D 120.2 . . ? C9D C8D H8D 120.2 . . ? C8D C9D C10D 120.6 . . ? C8D C9D H9D 119.7 . . ? C10D C9D H9D 119.7 . . ? C9D C10D C11D 121.6 . . ? C9D C10D C1D 119.8 . . ? C11D C10D C1D 118.5 . . ? C12D C11D C10D 121.2 . . ? C12D C11D H11D 119.4 . . ? C10D C11D H11D 119.4 . . ? C11D C12D C13D 120.9 . . ? C11D C12D H12D 119.6 . . ? C13D C12D H12D 119.6 . . ? C12D C13D C2D 121.5 . . ? C12D C13D H13D 119.3 . . ? C2D C13D H13D 119.3 . . ? C15D C14D C3D 122.7 . . ? C15D C14D H14D 118.7 . . ? C3D C14D H14D 118.7 . . ? C16D C15D C14D 119.5 . . ? C16D C15D H15D 120.2 . . ? C14D C15D H15D 120.2 . . ? C15D C16D C17D 120.8 . . ? C15D C16D H16D 119.6 . . ? C17D C16D H16D 119.6 . . ? C18D C17D C16D 121.2 . . ? C18D C17D C4D 119.7 . . ? C16D C17D C4D 119.2 . . ? C19D C18D C17D 120.6 . . ? C19D C18D H18D 119.7 . . ? C17D C18D H18D 119.7 . . ? C20D C19D C18D 120.5 . . ? C20D C19D H19D 119.7 . . ? C18D C19D H19D 119.7 . . ? C19D C20D C5D 122.0 . . ? C19D C20D H20D 119.0 . . ? C5D C20D H20D 119.0 . . ? C2E C1E C6E 121.7 . . ? C2E C1E C11E 119.5 . . ? C6E C1E C11E 118.8 . . ? C13E C2E C1E 118.4 . . ? C13E C2E C3E 121.9 . . ? C1E C2E C3E 119.7 . . ? C14E C3E C4E 117.7 . . ? C14E C3E C2E 123.1 . . ? C4E C3E C2E 119.2 . . ? C3E C4E C17E 120.1 . . ? C3E C4E C5E 121.2 . . ? C17E C4E C5E 118.7 . . ? C20E C5E C4E 118.4 . . ? C20E C5E C6E 122.2 . . ? C4E C5E C6E 119.4 . . ? C7E C6E C1E 118.5 . . ? C7E C6E C5E 122.7 . . ? C1E C6E C5E 118.8 . . ? C8E C7E C6E 122.7 . . ? C8E C7E H7E 118.7 . . ? C6E C7E H7E 118.7 . . ? C7E C8E C9E 119.6 . . ? C7E C8E H8E 120.2 . . ? C9E C8E H8E 120.2 . . ? C8E C9E C11E 120.6 . . ? C8E C9E H9E 119.7 . . ? C11E C9E H9E 119.7 . . ? C9E C11E C10E 121.6 . . ? C9E C11E C1E 119.8 . . ? C10E C11E C1E 118.5 . . ? C12E C10E C11E 121.2 . . ? C12E C10E H10E 119.4 . . ? C11E C10E H10E 119.4 . . ? C10E C12E C13E 120.9 . . ? C10E C12E H12E 119.6 . . ? C13E C12E H12E 119.6 . . ? C12E C13E C2E 121.5 . . ? C12E C13E H13E 119.3 . . ? C2E C13E H13E 119.3 . . ? C15E C14E C3E 122.7 . . ? C15E C14E H14E 118.7 . . ? C3E C14E H14E 118.7 . . ? C16E C15E C14E 119.5 . . ? C16E C15E H15E 120.2 . . ? C14E C15E H15E 120.2 . . ? C15E C16E C17E 120.8 . . ? C15E C16E H16E 119.6 . . ? C17E C16E H16E 119.6 . . ? C18E C17E C16E 121.2 . . ? C18E C17E C4E 119.7 . . ? C16E C17E C4E 119.2 . . ? C19E C18E C17E 120.6 . . ? C19E C18E H18E 119.7 . . ? C17E C18E H18E 119.7 . . ? C20E C19E C18E 120.5 . . ? C20E C19E H19E 119.7 . . ? C18E C19E H19E 119.7 . . ? C19E C20E C5E 122.0 . . ? C19E C20E H20E 119.0 . . ? C5E C20E H20E 119.0 . . ? C401 N1 C101 109(4) . . ? C401 N1 C201 113(4) . . ? C101 N1 C201 110(3) . . ? C401 N1 C301 102(3) . . ? C101 N1 C301 112(3) . . ? C201 N1 C301 111(3) . . ? N1 C101 C102 118(4) . . ? N1 C101 H10F 107.7 . . ? C102 C101 H10F 107.7 . . ? N1 C101 H10G 107.7 . . ? C102 C101 H10G 107.7 . . ? H10F C101 H10G 107.1 . . ? C101 C102 C103 107(5) . . ? C101 C102 H10H 110.4 . . ? C103 C102 H10H 110.4 . . ? C101 C102 H10I 110.4 . . ? C103 C102 H10I 110.4 . . ? H10H C102 H10I 108.6 . . ? C104 C103 C102 101.4(18) . . ? C104 C103 H10J 111.5 . . ? C102 C103 H10J 111.5 . . ? C104 C103 H10K 111.5 . . ? C102 C103 H10K 111.5 . . ? H10J C103 H10K 109.3 . . ? C103 C104 H10L 109.5 . . ? C103 C104 H10M 109.5 . . ? H10L C104 H10M 109.5 . . ? C103 C104 H10N 109.5 . . ? H10L C104 H10N 109.5 . . ? H10M C104 H10N 109.5 . . ? C202 C201 N1 118(4) . . ? C202 C201 H20F 107.8 . . ? N1 C201 H20F 107.8 . . ? C202 C201 H20G 107.8 . . ? N1 C201 H20G 107.8 . . ? H20F C201 H20G 107.1 . . ? C203 C202 C201 114(5) . . ? C203 C202 H20H 108.8 . . ? C201 C202 H20H 108.8 . . ? C203 C202 H20I 108.8 . . ? C201 C202 H20I 108.8 . . ? H20H C202 H20I 107.7 . . ? C202 C203 C204 113(2) . . ? C202 C203 H20J 109.0 . . ? C204 C203 H20J 109.0 . . ? C202 C203 H20K 109.0 . . ? C204 C203 H20K 109.0 . . ? H20J C203 H20K 107.8 . . ? C203 C204 H20L 109.5 . . ? C203 C204 H20M 109.5 . . ? H20L C204 H20M 109.5 . . ? C203 C204 H20N 109.5 . . ? H20L C204 H20N 109.5 . . ? H20M C204 H20N 109.5 . . ? C302 C301 N1 112.7(19) . . ? C302 C301 H30F 109.0 . . ? N1 C301 H30F 109.0 . . ? C302 C301 H30G 109.0 . . ? N1 C301 H30G 109.0 . . ? H30F C301 H30G 107.8 . . ? C303 C302 C301 110(4) . . ? C303 C302 H30H 109.7 . . ? C301 C302 H30H 109.7 . . ? C303 C302 H30I 109.7 . . ? C301 C302 H30I 109.7 . . ? H30H C302 H30I 108.2 . . ? C304 C303 C302 101(5) . . ? C304 C303 H30J 111.5 . . ? C302 C303 H30J 111.5 . . ? C304 C303 H30K 111.5 . . ? C302 C303 H30K 111.5 . . ? H30J C303 H30K 109.3 . . ? C303 C304 H30L 109.5 . . ? C303 C304 H30M 109.5 . . ? H30L C304 H30M 109.5 . . ? C303 C304 H30N 109.5 . . ? H30L C304 H30N 109.5 . . ? H30M C304 H30N 109.5 . . ? N1 C401 C402 114(4) . . ? N1 C401 H40F 108.9 . . ? C402 C401 H40F 108.9 . . ? N1 C401 H40G 108.9 . . ? C402 C401 H40G 108.9 . . ? H40F C401 H40G 107.7 . . ? C401 C402 C403 115(6) . . ? C401 C402 H40H 108.5 . . ? C403 C402 H40H 108.5 . . ? C401 C402 H40I 108.5 . . ? C403 C402 H40I 108.5 . . ? H40H C402 H40I 107.5 . . ? C404 C403 C402 106(7) . . ? C404 C403 H40J 110.5 . . ? C402 C403 H40J 110.5 . . ? C404 C403 H40K 110.5 . . ? C402 C403 H40K 110.5 . . ? H40J C403 H40K 108.7 . . ? C403 C404 H40L 109.5 . . ? C403 C404 H40M 109.5 . . ? H40L C404 H40M 109.5 . . ? C403 C404 H40N 109.5 . . ? H40L C404 H40N 109.5 . . ? H40M C404 H40N 109.5 . . ? C601 N2 C801 115(4) . . ? C601 N2 C701 108(4) . . ? C801 N2 C701 106.6(17) . . ? C601 N2 C501 105.9(17) . . ? C801 N2 C501 111(4) . . ? C701 N2 C501 111(4) . . ? C502 C501 N2 121(4) . . ? C502 C501 H50F 107.0 . . ? N2 C501 H50F 107.0 . . ? C502 C501 H50G 107.0 . . ? N2 C501 H50G 107.0 . . ? H50F C501 H50G 106.7 . . ? C503 C502 C501 117(5) . . ? C503 C502 H50H 108.1 . . ? C501 C502 H50H 108.1 . . ? C503 C502 H50I 108.1 . . ? C501 C502 H50I 108.1 . . ? H50H C502 H50I 107.3 . . ? C502 C503 C504 105(6) . . ? C502 C503 H50J 110.8 . . ? C504 C503 H50J 110.8 . . ? C502 C503 H50K 110.8 . . ? C504 C503 H50K 110.8 . . ? H50J C503 H50K 108.9 . . ? C503 C504 H50L 109.5 . . ? C503 C504 H50M 109.5 . . ? H50L C504 H50M 109.5 . . ? C503 C504 H50N 109.5 . . ? H50L C504 H50N 109.5 . . ? H50M C504 H50N 109.5 . . ? C602 C601 N2 127(5) . . ? C602 C601 H60F 105.6 . . ? N2 C601 H60F 105.6 . . ? C602 C601 H60G 105.6 . . ? N2 C601 H60G 105.6 . . ? H60F C601 H60G 106.1 . . ? C601 C602 C603 127(6) . . ? C601 C602 H60H 105.5 . . ? C603 C602 H60H 105.5 . . ? C601 C602 H60I 105.5 . . ? C603 C602 H60I 105.5 . . ? H60H C602 H60I 106.1 . . ? C604 C603 C602 100(7) . . ? C604 C603 H60J 111.8 . . ? C602 C603 H60J 111.8 . . ? C604 C603 H60K 111.8 . . ? C602 C603 H60K 111.8 . . ? H60J C603 H60K 109.5 . . ? C603 C604 H60L 109.5 . . ? C603 C604 H60M 109.5 . . ? H60L C604 H60M 109.5 . . ? C603 C604 H60N 109.5 . . ? H60L C604 H60N 109.5 . . ? H60M C604 H60N 109.5 . . ? C702 C701 N2 117(4) . . ? C702 C701 H70F 108.1 . . ? N2 C701 H70F 108.1 . . ? C702 C701 H70G 108.1 . . ? N2 C701 H70G 108.1 . . ? H70F C701 H70G 107.3 . . ? C701 C702 C703 112(6) . . ? C701 C702 H70H 109.2 . . ? C703 C702 H70H 109.2 . . ? C701 C702 H70I 109.2 . . ? C703 C702 H70I 109.2 . . ? H70H C702 H70I 107.9 . . ? C704 C703 C702 115(8) . . ? C704 C703 H70J 108.6 . . ? C702 C703 H70J 108.6 . . ? C704 C703 H70K 108.6 . . ? C702 C703 H70K 108.6 . . ? H70J C703 H70K 107.6 . . ? C703 C704 H70L 109.5 . . ? C703 C704 H70M 109.5 . . ? H70L C704 H70M 109.5 . . ? C703 C704 H70N 109.5 . . ? H70L C704 H70N 109.5 . . ? H70M C704 H70N 109.5 . . ? N2 C801 C802 113(4) . . ? N2 C801 H80F 108.9 . . ? C802 C801 H80F 108.9 . . ? N2 C801 H80G 108.9 . . ? C802 C801 H80G 108.9 . . ? H80F C801 H80G 107.7 . . ? C803 C802 C801 112(5) . . ? C803 C802 H80H 109.3 . . ? C801 C802 H80H 109.3 . . ? C803 C802 H80I 109.3 . . ? C801 C802 H80I 109.3 . . ? H80H C802 H80I 107.9 . . ? C804 C803 C802 106.4(18) . . ? C804 C803 H80J 110.4 . . ? C802 C803 H80J 110.4 . . ? C804 C803 H80K 110.4 . . ? C802 C803 H80K 110.4 . . ? H80J C803 H80K 108.6 . . ? C803 C804 H80L 109.5 . . ? C803 C804 H80M 109.5 . . ? H80L C804 H80M 109.5 . . ? C803 C804 H80N 109.5 . . ? H80L C804 H80N 109.5 . . ? H80M C804 H80N 109.5 . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 30.89 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 8.285 _refine_diff_density_min -4.388 _refine_diff_density_rms 0.527 #===END