#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:39:24 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255722 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705294.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7705294 loop_ _publ_author_name 'Kar, Aranya' 'Pradeep, Chullikkattil P.' _publ_section_title ; Post-functionalization through covalent modification of organic counter ions: a stepwise and controlled approach for novel hybrid polyoxometalate materials ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT01410A _journal_year 2020 _chemical_formula_moiety 'O40 Si W12, 4(C9 H11 O S), 2(C3 H7 N O)' _chemical_formula_sum 'C42 H58 N2 O46 S4 Si W12' _chemical_formula_weight 3689.43 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_date 2019-11-06 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _audit_update_record ; 2020-01-12 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 92.730(4) _cell_angle_beta 101.278(5) _cell_angle_gamma 104.065(5) _cell_formula_units_Z 2 _cell_length_a 13.3509(8) _cell_length_b 14.4698(7) _cell_length_c 19.8148(11) _cell_measurement_reflns_used 6568 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 28.1270 _cell_measurement_theta_min 1.8790 _cell_volume 3623.2(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 15.9974 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.9840 _diffrn_measured_fraction_theta_max 0.8465 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -52.00 66.00 1.00 38.18 -- 26.84 -77.00 90.00 118 2 \w -53.00 66.00 1.00 38.18 -- 26.84 -77.00-150.00 119 3 \w -52.00 67.00 1.00 38.18 -- 26.84 -77.00 -30.00 119 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0528140000 _diffrn_orient_matrix_UB_12 -0.0243992000 _diffrn_orient_matrix_UB_13 -0.0158083000 _diffrn_orient_matrix_UB_21 -0.0176030000 _diffrn_orient_matrix_UB_22 0.0171508000 _diffrn_orient_matrix_UB_23 0.0289119000 _diffrn_orient_matrix_UB_31 -0.0060617000 _diffrn_orient_matrix_UB_32 0.0411784000 _diffrn_orient_matrix_UB_33 -0.0166279000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_unetI/netI 0.0752 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19311 _diffrn_reflns_theta_full 28.46 _diffrn_reflns_theta_max 28.46 _diffrn_reflns_theta_min 1.72 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 19.193 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_correction_T_min 0.733 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 3.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_description triclinic _exptl_crystal_F_000 2764.000 _exptl_crystal_size_max 0.237 _exptl_crystal_size_mid 0.088 _exptl_crystal_size_min 0.068 _refine_diff_density_max 4.017 _refine_diff_density_min -4.125 _refine_diff_density_rms 0.403 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 966 _refine_ls_number_reflns 14724 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0602 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+21.3553P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1408 _refine_ls_wR_factor_ref 0.1625 _reflns_number_gt 10869 _reflns_number_total 14724 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL CELL 0.71073 13.350882 14.469826 19.814782 92.7299 101.2784 104.0651 ZERR 2 0.000837 0.000705 0.001053 0.0041 0.0049 0.0048 LATT 1 SFAC C H N O S Si W UNIT 84 116 4 92 8 2 24 L.S. 30 0 0 PLAN 10 fmap 2 acta OMIT -3 16 9 OMIT -1 11 6 OMIT -5 4 21 OMIT -11 3 0 OMIT 10 -2 16 OMIT -15 5 4 OMIT -4 1 20 OMIT 1 -10 4 OMIT 11 -13 10 OMIT 1 15 6 OMIT -3 2 19 OMIT 15 -4 6 OMIT 2 -14 8 OMIT -13 9 4 OMIT -2 12 13 OMIT -7 17 5 OMIT -3 3 3 OMIT -3 1 20 OMIT -13 1 13 OMIT -3 1 18 OMIT -13 0 1 OMIT -5 12 9 OMIT -9 -1 11 OMIT -4 -15 4 OMIT 4 0 13 OMIT -5 -1 17 OMIT -6 13 9 OMIT -10 14 12 OMIT -1 12 13 OMIT 6 -1 12 OMIT -7 -7 15 OMIT -13 0 14 OMIT -4 -9 11 OMIT 8 3 13 OMIT -9 12 9 OMIT -3 15 10 OMIT 3 -7 22 OMIT -14 1 6 OMIT 9 -1 17 OMIT -4 -8 10 OMIT 2 -15 7 OMIT 1 14 7 OMIT 8 -5 15 OMIT -4 -11 10 OMIT 12 -7 13 OMIT 6 0 18 OMIT 10 -2 10 OMIT 3 -15 1 OMIT -5 -10 6 OMIT -11 14 12 OMIT -15 4 3 OMIT 13 0 1 OMIT -4 16 9 OMIT -12 4 18 OMIT 0 -10 4 OMIT -11 4 1 OMIT -14 0 14 OMIT 11 -2 6 OMIT -2 3 20 OMIT -4 -8 7 OMIT -4 2 25 OMIT -6 -3 24 OMIT -12 11 11 OMIT -7 15 4 OMIT -8 4 22 OMIT 7 -5 16 OMIT -4 2 22 OMIT -13 1 6 OMIT 9 2 8 OMIT 5 0 19 OMIT -13 9 11 OMIT -11 7 12 OMIT 9 2 12 OMIT -4 -7 9 OMIT -13 8 3 OMIT -16 5 10 OMIT -5 12 4 OMIT -12 -3 19 OMIT -3 -3 24 OMIT -3 16 2 OMIT -16 6 9 OMIT -11 3 2 OMIT -15 5 10 OMIT -3 -15 4 OMIT 11 4 12 OMIT 5 -11 8 OMIT -5 -7 17 OMIT -7 4 14 OMIT 1 -3 20 OMIT -8 17 5 OMIT -3 15 3 OMIT -10 14 6 OMIT -3 -1 18 OMIT 9 2 1 OMIT -1 11 12 OMIT -1 -13 16 OMIT 4 1 20 OMIT -6 13 16 OMIT -11 -6 11 OMIT 2 5 3 OMIT -8 1 9 OMIT -14 1 8 OMIT 8 -6 5 OMIT -14 13 0 OMIT -3 2 25 OMIT -3 2 17 OMIT 2 13 11 OMIT -11 4 8 OMIT -5 12 2 OMIT 13 1 0 OMIT 11 5 11 OMIT -1 11 14 OMIT 1 5 10 OMIT -1 12 11 OMIT -4 8 12 OMIT 15 -4 1 OMIT 1 -12 20 OMIT 12 -1 5 OMIT 3 -5 5 OMIT -5 13 9 OMIT 3 1 20 OMIT -3 15 4 OMIT -2 -3 21 OMIT -7 10 8 OMIT 5 0 13 OMIT -2 16 9 OMIT -4 -7 17 OMIT -6 14 15 OMIT 1 -13 13 OMIT -5 -12 9 OMIT -1 -9 11 OMIT 7 11 9 OMIT 4 -10 15 OMIT -7 16 0 OMIT -4 8 6 OMIT -7 -7 8 OMIT 6 -4 17 OMIT -9 1 13 OMIT -7 15 10 OMIT 15 -5 2 OMIT 5 -4 17 OMIT -15 0 11 OMIT 0 11 6 OMIT -5 -6 23 OMIT 1 5 18 OMIT -9 -2 5 OMIT 0 -14 6 OMIT -7 16 6 OMIT -10 -2 20 OMIT 8 5 8 OMIT -5 -6 20 OMIT 2 -7 5 OMIT -11 -5 17 OMIT 9 -10 11 OMIT -2 14 7 OMIT -9 5 17 OMIT 2 -6 5 OMIT -14 1 13 OMIT -7 1 21 OMIT -5 -8 18 OMIT -8 8 8 OMIT -11 4 14 OMIT -3 15 1 OMIT 0 2 23 OMIT -10 1 21 OMIT 2 4 11 OMIT -6 -10 9 OMIT -10 15 11 OMIT -3 -3 21 OMIT -4 14 14 OMIT 11 -1 2 OMIT -4 -9 20 OMIT 12 -5 7 OMIT -6 12 4 OMIT -2 2 19 OMIT -1 13 6 OMIT -1 -9 22 OMIT 4 -11 7 OMIT -5 -13 13 OMIT 1 6 17 OMIT -1 -5 14 OMIT -4 -13 7 OMIT 0 0 21 OMIT 6 -5 16 OMIT -5 -7 12 OMIT -6 3 3 OMIT -16 2 1 OMIT -1 11 4 OMIT 7 5 5 OMIT -10 13 11 OMIT -2 -3 24 OMIT 13 -2 8 OMIT -6 4 20 OMIT 2 14 7 OMIT 4 4 9 OMIT 3 -15 14 OMIT -4 -8 16 OMIT -4 -6 16 OMIT -3 -7 9 OMIT -2 11 6 OMIT 2 -3 12 OMIT -9 -10 7 OMIT -10 13 5 OMIT -9 13 5 OMIT -2 -8 18 OMIT -3 0 20 OMIT -7 -7 9 OMIT 12 -6 12 OMIT 2 -6 15 OMIT -4 0 25 OMIT -2 13 8 OMIT -4 -12 8 OMIT -4 1 22 OMIT -5 -9 19 OMIT 12 -5 8 OMIT 10 -2 6 OMIT 0 15 6 OMIT -3 -9 14 OMIT -6 15 10 OMIT 1 13 12 OMIT -2 -3 25 OMIT -6 -7 8 OMIT 9 1 0 OMIT 10 0 5 OMIT -3 14 7 OMIT 6 -15 10 OMIT -8 7 0 OMIT -5 -1 11 OMIT -15 5 2 OMIT -2 15 2 OMIT -10 0 18 OMIT -4 -11 9 OMIT -11 4 7 OMIT 7 -9 1 OMIT -10 0 10 OMIT -3 14 14 OMIT -6 -7 15 OMIT 8 2 13 OMIT 2 -3 20 OMIT -5 13 8 OMIT -8 4 21 OMIT 5 5 14 OMIT 9 -1 15 OMIT -7 4 20 OMIT 13 -9 11 OMIT -3 -9 7 OMIT -11 11 11 OMIT -10 9 0 OMIT -16 2 7 OMIT -2 -9 7 OMIT 2 -5 14 OMIT -6 10 1 OMIT 5 3 19 OMIT 7 -15 10 OMIT 1 -11 21 OMIT 0 -6 13 OMIT -16 6 1 OMIT -7 16 9 OMIT -5 -11 14 OMIT 0 11 4 OMIT -5 -12 14 OMIT 6 11 9 OMIT 5 -1 6 OMIT -4 -1 20 OMIT 6 7 11 OMIT 8 2 14 OMIT 1 15 8 OMIT -8 3 22 OMIT 11 -3 7 OMIT 3 -9 9 OMIT -7 5 22 OMIT -8 16 0 OMIT -4 2 16 OMIT -5 -4 16 OMIT -9 14 4 OMIT 4 -10 8 OMIT -9 8 8 OMIT -3 -12 9 OMIT 1 -2 11 OMIT -4 -14 12 OMIT -4 -7 12 OMIT -11 12 6 OMIT -3 18 2 OMIT -13 -8 9 OMIT -2 14 13 OMIT -13 -5 17 OMIT -9 7 18 OMIT 0 -6 18 OMIT 7 -2 1 OMIT -8 7 2 OMIT -11 3 6 OMIT 10 7 0 OMIT -7 -1 1 OMIT 7 -6 9 OMIT -1 10 7 OMIT 3 10 9 OMIT 6 3 8 OMIT 14 -10 3 OMIT -8 6 14 OMIT 7 -2 3 OMIT -10 12 3 OMIT -9 14 10 OMIT 3 4 20 OMIT -12 6 18 OMIT -9 -2 10 OMIT 2 -17 3 OMIT -4 -10 16 OMIT -13 8 6 OMIT 0 -14 4 OMIT -7 2 5 OMIT 6 4 18 OMIT -5 7 22 OMIT 3 6 7 OMIT 12 -7 11 OMIT -12 -2 20 OMIT -3 8 6 OMIT -1 13 8 OMIT -3 5 22 OMIT -1 14 7 OMIT -13 -5 16 OMIT -7 -6 22 OMIT -6 3 2 OMIT -6 15 4 OMIT 4 -7 17 OMIT -13 -1 2 OMIT 11 -6 13 OMIT -1 -6 18 OMIT -4 -15 8 OMIT -8 8 13 OMIT -13 12 0 OMIT -11 12 12 OMIT 3 11 15 OMIT 6 3 14 OMIT 6 12 5 OMIT -5 14 4 OMIT 1 -3 15 OMIT -8 -3 5 OMIT -5 -10 7 OMIT -9 -10 14 OMIT 4 -11 9 OMIT 6 9 12 OMIT -1 -17 6 OMIT -3 -2 17 OMIT 7 -3 12 OMIT -9 14 12 OMIT -8 -3 2 OMIT 3 9 18 OMIT -13 -3 4 OMIT 3 -7 17 OMIT -12 4 7 OMIT 0 -3 5 OMIT 5 1 2 OMIT 1 2 0 OMIT 1 -4 7 OMIT 4 0 7 OMIT 12 -5 2 OMIT -7 14 2 OMIT 3 0 10 OMIT -2 -4 18 OMIT 2 12 12 OMIT 0 -7 17 OMIT -8 -3 13 OMIT -6 -7 13 OMIT -2 15 4 OMIT -7 -12 10 OMIT -7 6 3 OMIT 3 1 14 OMIT 7 6 1 OMIT -12 6 11 OMIT 2 -13 18 OMIT -5 -11 8 OMIT 8 -1 10 OMIT -7 -11 17 OMIT -5 -9 13 OMIT -4 -14 5 OMIT -1 13 16 OMIT 5 -12 7 OMIT 10 -5 3 OMIT -4 16 2 OMIT 7 -4 15 OMIT -2 -7 19 OMIT -7 9 9 OMIT -12 8 4 OMIT 6 -1 6 OMIT -14 10 14 OMIT -8 5 22 OMIT -14 0 17 OMIT -3 2 21 OMIT -9 6 1 OMIT 5 -9 18 OMIT -7 17 3 OMIT -10 16 6 OMIT 8 3 9 OMIT -12 -4 9 OMIT 2 4 17 OMIT -15 -3 6 OMIT -1 11 8 OMIT -3 -4 14 OMIT -1 1 18 OMIT -12 9 11 OMIT 0 2 17 OMIT 13 -8 1 OMIT -7 3 15 OMIT 6 4 15 OMIT -5 -9 11 OMIT -1 -9 16 OMIT 5 -17 12 OMIT -12 7 5 OMIT -8 5 21 OMIT 14 -12 1 OMIT -8 -11 8 OMIT -6 -6 14 OMIT 3 -7 16 OMIT -11 4 18 OMIT 12 -1 9 OMIT 4 -15 3 OMIT 5 4 7 OMIT -11 -6 18 OMIT -3 0 19 OMIT 4 -1 21 OMIT -1 -7 19 OMIT 2 2 22 OMIT -5 7 16 OMIT 7 0 18 OMIT -5 3 22 OMIT 9 -1 3 OMIT 3 -17 8 OMIT 1 10 0 OMIT -10 9 15 OMIT -6 -9 19 OMIT -5 13 16 OMIT -5 9 13 OMIT 3 8 11 OMIT -7 2 14 OMIT -3 -4 18 OMIT -8 11 6 OMIT 15 -4 3 OMIT 8 4 7 OMIT -3 12 6 OMIT -5 14 2 OMIT -9 7 9 OMIT -5 -4 24 OMIT 10 -2 9 OMIT 10 -1 15 OMIT -4 -8 21 OMIT 1 -12 5 OMIT -10 -7 12 OMIT -7 3 5 OMIT -9 1 8 OMIT -15 -1 12 OMIT 10 0 6 OMIT -5 6 23 OMIT -2 12 5 OMIT 2 11 3 OMIT 3 10 11 OMIT -6 13 8 OMIT 1 -2 19 OMIT -10 1 13 OMIT -14 13 2 OMIT -2 -2 12 OMIT 4 -9 15 OMIT -12 -2 18 OMIT -13 -5 4 OMIT 1 14 9 OMIT -7 -6 14 OMIT -13 -2 17 OMIT 8 -6 7 OMIT -6 16 9 OMIT -2 -4 17 OMIT -12 4 14 OMIT -3 -9 1 OMIT 1 -5 22 OMIT -8 -13 6 OMIT -4 -15 5 OMIT -1 2 17 OMIT -14 1 16 OMIT -8 16 6 OMIT -3 13 8 OMIT 10 -3 3 OMIT -1 14 13 OMIT -5 10 7 OMIT 8 0 14 OMIT 5 3 8 OMIT -4 9 18 OMIT -6 4 23 OMIT -10 -1 5 OMIT -3 -8 19 OMIT 4 15 5 OMIT -8 -7 12 OMIT -7 2 15 OMIT 10 -3 10 OMIT 3 1 3 OMIT 5 13 0 OMIT -4 0 20 OMIT -8 10 14 OMIT -12 6 15 OMIT 0 0 4 OMIT 8 6 8 OMIT -7 2 3 OMIT 2 9 7 OMIT -8 1 8 OMIT 3 -14 13 OMIT 8 2 12 OMIT -2 2 22 OMIT -3 -14 8 OMIT -8 10 8 OMIT -8 6 1 OMIT -9 9 0 OMIT -5 -1 23 OMIT 4 5 20 OMIT 7 3 15 OMIT -7 3 21 OMIT -6 14 3 OMIT 3 7 8 OMIT -10 12 9 OMIT -12 5 0 OMIT -9 -2 20 OMIT 1 1 0 OMIT 11 -5 5 OMIT -5 3 4 OMIT 8 -9 9 OMIT -3 13 6 OMIT 0 -13 15 OMIT 8 4 9 OMIT -13 9 17 OMIT -8 7 1 OMIT -8 12 9 OMIT 2 10 18 OMIT -15 9 8 OMIT -15 2 13 OMIT 0 -6 19 OMIT -10 15 2 OMIT 7 5 7 OMIT 7 5 0 OMIT -3 1 16 OMIT 1 -12 14 OMIT -14 11 2 OMIT 3 -10 8 OMIT 0 1 16 OMIT -15 4 5 OMIT -3 -11 17 OMIT 4 -17 2 OMIT -10 -7 2 OMIT -11 -5 4 OMIT 9 -2 11 OMIT -12 5 17 OMIT -8 3 16 OMIT 5 -12 16 OMIT 0 -3 14 OMIT -11 -5 2 OMIT -1 -14 4 OMIT 2 -5 22 OMIT -4 0 13 OMIT -11 -4 1 OMIT -9 0 1 OMIT 9 -1 16 OMIT 13 -1 9 OMIT -15 7 1 OMIT -8 9 9 OMIT -7 7 12 OMIT 8 -5 10 OMIT 10 -1 6 OMIT 11 -5 2 OMIT 9 -12 15 OMIT -14 1 17 OMIT -11 5 17 OMIT -4 11 6 OMIT -13 6 8 OMIT -9 -6 20 OMIT -2 13 6 OMIT -6 -6 22 OMIT -8 6 8 OMIT -14 12 1 OMIT 4 -7 16 OMIT 13 -7 11 OMIT -11 -10 13 OMIT 2 13 12 OMIT -15 -1 4 OMIT -13 1 0 OMIT 2 6 7 OMIT 9 -1 4 OMIT -9 -1 4 OMIT -1 9 4 OMIT 9 8 4 OMIT 11 -1 15 OMIT 3 -12 10 OMIT -4 12 11 OMIT -3 -1 19 OMIT -15 6 3 OMIT -12 8 13 OMIT -3 1 9 OMIT -1 14 8 OMIT 7 3 14 OMIT -13 0 3 OMIT 0 0 23 OMIT -13 4 18 OMIT 13 1 9 OMIT -3 14 15 OMIT -9 0 14 OMIT 7 3 11 OMIT -9 8 0 OMIT -1 -8 21 OMIT 0 1 25 OMIT 8 2 1 OMIT -6 -8 10 OMIT 11 -3 5 OMIT -4 -3 24 OMIT -14 0 18 OMIT -5 -3 9 OMIT 15 -7 3 OMIT 13 -2 2 OMIT 3 4 17 OMIT -6 -1 24 OMIT 7 4 14 OMIT -12 5 8 OMIT -2 -9 3 OMIT 4 1 14 OMIT 5 9 14 OMIT -2 11 12 OMIT -14 6 8 OMIT 1 10 5 OMIT -10 4 1 OMIT -10 8 0 OMIT 11 4 10 OMIT -11 3 17 OMIT -6 15 9 OMIT 14 -4 3 OMIT 10 4 8 OMIT -4 -8 9 OMIT -10 14 10 OMIT -4 -8 8 OMIT -13 14 12 OMIT -11 -5 11 OMIT 11 5 4 OMIT -5 -8 11 OMIT 12 3 11 OMIT -12 -3 8 OMIT 11 -1 6 OMIT 6 5 14 OMIT -9 -7 13 OMIT 8 2 11 OMIT 3 -15 3 OMIT -10 -5 17 OMIT -6 3 4 OMIT 11 -4 7 OMIT -5 -9 5 OMIT 3 -9 15 OMIT -10 -2 16 OMIT -13 -1 8 OMIT 6 10 8 OMIT -8 2 16 OMIT -11 3 8 OMIT 14 -8 3 OMIT 11 -2 10 OMIT 1 -10 17 OMIT -12 8 3 OMIT 13 1 3 OMIT -9 -4 3 OMIT 12 -7 8 OMIT 0 -10 15 OMIT -3 -1 20 OMIT -10 2 5 OMIT 5 -8 15 OMIT -7 17 7 OMIT -3 8 12 OMIT 3 -4 11 OMIT -8 -2 12 OMIT -4 3 22 OMIT -2 -2 6 OMIT -3 -3 7 OMIT -15 2 1 OMIT 14 0 2 OMIT -8 11 1 OMIT -16 7 2 OMIT -12 -1 2 OMIT -10 -10 9 OMIT 1 -3 17 OMIT 1 -18 2 OMIT -11 -7 12 OMIT -13 8 5 OMIT 9 -11 12 OMIT 10 -10 11 OMIT 12 -13 4 OMIT 6 -16 4 OMIT 11 1 2 OMIT -5 8 16 OMIT 15 -5 5 OMIT 5 1 12 OMIT 1 -16 6 OMIT 13 -11 4 OMIT -8 -11 14 OMIT -1 0 9 OMIT -13 2 20 OMIT -14 10 11 OMIT 8 0 4 OMIT -7 10 19 OMIT -1 -10 15 OMIT -10 11 5 OMIT 0 14 7 OMIT -13 8 2 OMIT -1 -11 3 OMIT 5 -1 8 OMIT -8 -4 12 OMIT 8 -4 1 OMIT 3 -4 12 OMIT 9 -13 7 OMIT -14 6 14 OMIT 4 5 21 OMIT 11 0 3 OMIT 3 9 12 OMIT 1 -9 20 OMIT -8 2 14 OMIT -4 10 1 OMIT 6 -7 2 OMIT -9 -10 15 OMIT -3 -11 10 OMIT 6 2 3 OMIT -12 6 12 OMIT -1 10 0 OMIT 5 4 9 OMIT 9 -9 12 OMIT -3 0 18 OMIT -5 11 1 OMIT -8 3 21 OMIT 1 -12 2 OMIT -1 -13 12 OMIT 5 2 11 OMIT -1 -12 17 OMIT -4 2 24 OMIT 7 -7 8 OMIT 7 -16 2 OMIT 10 -11 2 OMIT -9 -7 14 OMIT -6 12 10 OMIT -5 15 5 OMIT -3 6 13 OMIT 5 9 2 OMIT 8 3 0 OMIT -10 -6 11 OMIT -3 -9 13 OMIT 1 -13 8 OMIT 4 9 13 OMIT -15 12 8 OMIT -4 -14 11 OMIT -16 3 2 OMIT 0 -13 13 OMIT -3 -13 4 OMIT 1 13 8 OMIT 4 -8 21 OMIT -3 15 2 OMIT 2 -8 8 OMIT -2 -13 2 OMIT -8 -4 1 OMIT -2 1 1 OMIT 1 1 25 OMIT 10 1 15 OMIT -1 -10 14 OMIT 9 6 7 OMIT -1 4 11 OMIT -3 -2 14 OMIT -2 1 18 OMIT -11 -4 16 OMIT -12 14 4 OMIT 6 -1 13 OMIT -15 -1 2 OMIT 7 -17 1 OMIT -5 6 15 OMIT 0 -16 1 OMIT -12 14 10 OMIT 2 -8 18 OMIT 7 -1 6 OMIT -2 14 3 OMIT 8 3 11 OMIT -7 3 4 OMIT -7 0 1 OMIT 12 -12 3 OMIT 5 9 8 OMIT 6 -1 19 OMIT 2 -4 12 OMIT -12 13 8 OMIT -3 -3 13 OMIT -12 4 11 OMIT -5 11 3 OMIT -8 1 20 OMIT 11 -1 7 OMIT -1 11 5 OMIT -3 -4 17 OMIT -4 -5 20 OMIT -2 -13 9 OMIT -14 8 5 OMIT -1 -6 24 OMIT -6 -12 14 OMIT -1 2 9 OMIT 1 -6 2 OMIT -10 16 7 OMIT 4 -13 10 OMIT -12 0 14 OMIT -8 4 11 OMIT -11 11 16 OMIT 0 9 14 OMIT -4 -13 4 OMIT -16 5 4 OMIT 9 -3 2 OMIT -2 -15 9 OMIT 12 -4 7 OMIT -9 6 14 OMIT 12 7 4 OMIT -13 -4 4 OMIT -2 -4 23 OMIT -13 -4 11 OMIT 9 7 8 OMIT -13 -3 10 OMIT 3 6 0 OMIT 9 -14 13 OMIT -5 -13 11 OMIT 7 3 4 OMIT 12 -4 6 OMIT 8 6 6 OMIT 12 -4 5 OMIT -4 -4 21 OMIT -15 5 13 OMIT -1 1 9 OMIT 9 5 7 OMIT 12 -2 8 OMIT 13 -1 8 OMIT 10 0 16 OMIT 9 6 11 OMIT -3 -3 16 OMIT 10 2 8 OMIT 9 -4 1 OMIT -5 -7 4 OMIT -7 3 11 OMIT 6 3 4 OMIT 10 -1 2 OMIT -1 1 11 OMIT 0 -9 11 OMIT 1 -2 2 OMIT -3 -1 3 OMIT -8 1 14 OMIT 5 -4 5 OMIT -16 1 9 OMIT 8 -1 3 OMIT 8 3 6 OMIT -4 -10 7 OMIT -5 -15 6 OMIT -2 -1 9 OMIT 7 6 5 OMIT -3 2 22 OMIT 8 4 5 OMIT -6 -12 16 REM REM REM WGHT 0.073500 21.355297 FVAR 0.78388 W1 7 0.052379 0.163868 0.900725 11.00000 0.02225 0.02252 = 0.01851 0.00270 0.00134 0.00571 W2 7 0.241946 0.350259 0.738479 11.00000 0.01770 0.02075 = 0.02873 0.00471 0.00609 0.00454 W3 7 -0.214747 0.378325 0.711666 11.00000 0.01990 0.02202 = 0.02380 0.00095 0.00086 0.00773 W4 7 -0.106701 -0.004940 0.755073 11.00000 0.02637 0.01506 = 0.02898 0.00221 0.00998 0.00395 W5 7 0.119020 0.402499 0.879019 11.00000 0.02342 0.02191 = 0.02527 -0.00503 -0.00289 0.00783 W6 7 0.095913 0.195028 0.599503 11.00000 0.02192 0.02555 = 0.02209 0.00193 0.00554 0.00631 W7 7 -0.292700 0.122218 0.727942 11.00000 0.01642 0.03080 = 0.02423 0.00303 0.00278 0.00402 W8 7 0.041485 0.485393 0.710406 11.00000 0.04121 0.01620 = 0.03083 0.00354 0.00851 0.00493 W9 7 -0.136844 0.287314 0.877599 11.00000 0.02073 0.02358 = 0.02804 -0.00458 0.00797 0.00173 W10 7 0.167987 0.111375 0.755545 11.00000 0.02053 0.02193 = 0.03512 -0.00588 0.00029 0.00825 W11 7 -0.177290 0.070397 0.596120 11.00000 0.02641 0.02282 = 0.02091 -0.00309 -0.00244 0.00574 W12 7 -0.108958 0.325821 0.576214 11.00000 0.03237 0.03143 = 0.02362 0.00942 -0.00227 -0.00026 SI13 6 -0.026536 0.240710 0.736051 11.00000 0.00329 0.00591 = 0.00730 -0.00094 0.00098 0.00114 O18 4 0.089927 0.110128 0.971226 11.00000 0.03544 0.04226 = 0.03105 0.01668 -0.00164 0.00112 O21 4 -0.125499 -0.122789 0.771791 11.00000 0.04747 0.02095 = 0.03366 0.00691 0.01760 -0.00006 O22 4 0.093090 0.605343 0.708788 11.00000 0.03283 0.01992 = 0.05979 0.00705 0.00425 0.01044 O23 4 -0.421548 0.080344 0.732007 11.00000 0.02003 0.04702 = 0.03675 0.00639 0.00314 0.01063 O25 4 -0.144461 0.350469 0.493545 11.00000 0.03324 0.04482 = 0.03718 0.01626 0.00715 0.01837 O26 4 -0.240945 0.002479 0.519742 11.00000 0.01859 0.04144 = 0.03144 -0.00787 -0.00318 0.00248 O27 4 0.367698 0.418736 0.746359 11.00000 0.01765 0.04693 = 0.03212 -0.00743 -0.00915 -0.00222 O41 4 0.133373 0.170693 0.525480 11.00000 0.06444 0.03622 = 0.04285 -0.00651 0.02515 0.00635 O57 4 0.249416 0.039079 0.773052 11.00000 0.02800 0.02584 = 0.02879 -0.00649 0.00852 0.00254 O70 4 0.196171 0.491713 0.939283 11.00000 0.02242 0.03465 = 0.05838 -0.00769 -0.00538 -0.00314 O5 4 -0.099057 0.490481 0.720696 11.00000 0.03989 0.03080 = 0.02392 0.00099 0.01508 -0.00150 O7 4 -0.209969 0.308958 0.934587 11.00000 0.03503 0.03148 = 0.03806 0.01090 0.00862 0.00865 O8 4 -0.244594 0.009111 0.758163 11.00000 0.03786 0.04586 = 0.01687 0.01873 0.01439 0.01414 O9 4 -0.036398 0.101240 0.589759 11.00000 0.01774 0.03356 = 0.03370 0.01058 -0.00072 0.00148 O10 4 -0.155222 -0.026375 0.653628 11.00000 0.04426 0.06122 = 0.02347 0.00459 0.00882 0.03012 O11 4 -0.230040 0.181986 0.819302 11.00000 0.04521 0.02355 = 0.03170 0.00819 0.01203 -0.00686 O12 4 -0.300398 0.073872 0.635191 11.00000 0.03231 0.03835 = 0.04528 0.00005 0.00087 0.01995 O13 4 -0.064539 0.201811 0.925785 11.00000 0.02542 0.04125 = 0.04706 0.00988 0.00824 0.00877 O14 4 0.030354 0.025206 0.737730 11.00000 0.02958 0.04842 = 0.02914 -0.01972 0.00611 0.00035 O15 4 0.211832 0.373387 0.826057 11.00000 0.04113 0.04928 = 0.02998 0.01711 0.01614 0.02576 O16 4 -0.179312 0.197188 0.573911 11.00000 0.03528 0.02581 = 0.06053 0.00607 -0.00390 0.00254 O17 4 0.273135 0.234639 0.764857 11.00000 0.03489 0.02807 = 0.03546 -0.00633 -0.01535 -0.00362 O1 4 0.144517 0.146898 0.844157 11.00000 0.03590 O19 4 -0.050646 0.061630 0.841967 11.00000 0.02903 0.02862 = 0.03452 -0.00123 0.01127 0.00701 O20 4 0.079626 0.229971 0.713481 11.00000 0.04035 0.04401 = 0.03399 0.01224 0.01629 0.02297 O2 4 -0.217981 0.363397 0.613771 11.00000 0.03471 0.05217 = 0.04124 -0.00035 0.01883 -0.00637 O3 4 -0.011320 0.389898 0.908584 11.00000 0.02405 0.02109 = 0.08511 -0.00234 0.00374 0.00306 O4 4 0.214163 0.297647 0.643842 11.00000 0.05218 0.02248 = 0.03837 0.00468 -0.00945 0.00798 O24 4 0.158973 0.112750 0.657889 11.00000 0.04725 0.02361 = 0.03310 0.00364 -0.00390 -0.00780 O6 4 0.015744 0.285665 0.572915 11.00000 0.03939 0.02968 = 0.05721 0.00719 0.00357 0.00215 O1A 4 0.133209 0.290885 0.928593 11.00000 0.02953 0.02956 = 0.08782 0.00814 -0.00151 0.01247 O1B 4 -0.007272 0.264053 0.818942 11.00000 0.01600 0.02432 = 0.03608 -0.00178 -0.00283 0.00029 O28 4 -0.175056 0.363035 0.806581 11.00000 0.05294 0.02432 = 0.02816 -0.01263 -0.00374 -0.01601 O29 4 -0.064226 0.325793 0.697920 11.00000 0.02947 0.03791 = 0.02056 0.00290 0.00121 0.01012 O30 4 -0.016657 0.449159 0.614850 11.00000 0.04249 0.04263 = 0.03946 -0.00118 0.01880 -0.00298 O31 4 -0.314916 0.429766 0.709259 11.00000 0.05428 0.05538 = 0.05353 -0.03056 -0.02856 0.03552 O32 4 0.157199 0.434307 0.705351 11.00000 0.06387 0.07191 = 0.03399 0.01792 0.01329 0.04285 O33 4 0.065747 0.467958 0.807734 11.00000 0.05483 0.05137 = 0.02688 0.00818 0.01491 0.03357 O34 4 -0.288786 0.245054 0.700761 11.00000 0.06802 0.03171 = 0.01605 0.00192 0.00971 0.00210 O35 4 -0.119539 0.140322 0.711720 11.00000 0.02189 0.04040 = 0.02307 -0.00101 -0.00737 0.00915 C13 1 0.462143 0.400696 1.051552 11.00000 0.02471 0.01697 = 0.03097 0.01225 0.00978 0.01319 C14 1 -0.071505 0.629902 0.561871 11.00000 0.01329 0.02993 = 0.03930 0.00666 -0.01253 0.01132 AFIX 43 H14 2 -0.018916 0.613645 0.542889 11.00000 -1.20000 AFIX 0 C15 1 -0.050494 0.712865 0.609842 11.00000 0.02372 0.02464 = 0.02839 0.00376 0.00981 0.01141 C17 1 0.379355 0.294166 0.948034 11.00000 0.02921 AFIX 43 H17 2 0.318180 0.260418 0.916992 11.00000 -1.20000 AFIX 0 C18 1 -0.252446 0.593459 0.572776 11.00000 0.04397 0.04098 = 0.01941 0.01225 0.00531 0.01487 C25 1 0.477209 0.283989 0.940973 11.00000 0.03515 0.02953 = 0.01876 -0.00469 0.01225 -0.00091 C28 1 -0.176101 0.575022 0.545463 11.00000 0.04638 0.04263 = 0.02132 -0.00972 0.00066 0.01524 AFIX 43 H28 2 -0.193106 0.521896 0.513104 11.00000 -1.20000 AFIX 0 C29 1 0.374411 0.354180 1.000988 11.00000 0.03923 0.03766 = 0.03922 0.00158 -0.00122 0.00575 AFIX 43 H29 2 0.309233 0.364739 1.003619 11.00000 -1.20000 AFIX 0 S1 5 0.080401 0.782864 0.629262 11.00000 0.04596 0.02796 = 0.03438 -0.00379 0.00815 0.00735 S2 5 0.474207 0.202821 0.870335 11.00000 0.04361 0.03952 = 0.04581 -0.00118 0.00888 0.01265 C16 1 0.571191 0.331153 0.988272 11.00000 0.01200 0.04752 = 0.05048 0.00042 0.01639 0.00931 AFIX 43 H16 2 0.636592 0.323379 0.983320 11.00000 -1.20000 AFIX 0 C1 1 0.105966 0.818536 0.720060 11.00000 0.07122 0.02912 = 0.02939 -0.00251 -0.00547 0.02235 AFIX 137 H1A 2 0.055850 0.852513 0.729252 11.00000 -1.50000 H1B 2 0.176227 0.859431 0.734683 11.00000 -1.50000 H1C 2 0.099528 0.762790 0.744929 11.00000 -1.50000 AFIX 0 C20 1 0.561168 0.389926 1.042744 11.00000 0.03803 0.04101 = 0.03678 0.00145 -0.01002 -0.01026 AFIX 43 H20 2 0.621766 0.423283 1.074461 11.00000 -1.20000 AFIX 0 C23 1 0.544223 0.280812 0.817897 11.00000 0.03258 0.05618 = 0.05585 0.02205 0.01371 0.01902 AFIX 137 H23A 2 0.504671 0.325517 0.801519 11.00000 -1.50000 H23B 2 0.553339 0.243667 0.779170 11.00000 -1.50000 H23C 2 0.612199 0.315067 0.844888 11.00000 -1.50000 AFIX 0 C26 1 -0.391659 -0.169525 0.571829 11.00000 0.03205 0.03775 = 0.07037 0.00446 0.00571 0.00236 AFIX 43 H26 2 -0.320782 -0.170054 0.581110 11.00000 -1.20000 AFIX 0 C27 1 -0.447463 -0.189101 0.506578 11.00000 0.05386 0.02718 = 0.06731 0.02951 0.03078 0.01057 O1C 4 0.372629 0.478410 1.116999 11.00000 0.08926 0.08942 = 0.05824 -0.00555 0.02377 0.05842 C2 1 0.449969 0.461667 1.108679 11.00000 0.06245 0.06283 = 0.01621 0.00471 -0.01023 0.02266 AFIX 43 H2 2 0.510866 0.490021 1.141871 11.00000 -1.20000 AFIX 0 C30 1 -0.539021 -0.145599 0.611504 11.00000 0.04730 0.03397 = 0.05450 0.00632 0.01260 0.01706 C31 1 0.073998 0.896845 0.597473 11.00000 0.05323 0.04400 = 0.04732 0.01876 0.02320 0.01180 AFIX 137 H31A 2 0.063002 0.890607 0.547944 11.00000 -1.50000 H31B 2 0.139101 0.943878 0.616638 11.00000 -1.50000 H31C 2 0.016494 0.916554 0.610961 11.00000 -1.50000 AFIX 0 C32 1 -0.130940 0.734278 0.638900 11.00000 0.08071 0.04372 = 0.03759 -0.01462 0.00631 0.03723 AFIX 43 H32 2 -0.115951 0.788514 0.669994 11.00000 -1.20000 AFIX 0 C36 1 -0.236073 0.673020 0.620919 11.00000 0.03882 0.07321 = 0.03577 0.00017 0.01083 0.02509 AFIX 43 H36 2 -0.290436 0.685224 0.640036 11.00000 -1.20000 AFIX 0 C37 1 -0.434337 -0.149800 0.622483 11.00000 0.05273 0.03076 = 0.06457 0.00255 -0.02712 0.00004 AFIX 43 H37 2 -0.393651 -0.138182 0.667309 11.00000 -1.20000 AFIX 0 C39 1 -0.362454 0.516962 0.549665 11.00000 0.04055 0.11452 = 0.10671 0.07233 0.02811 0.03943 AFIX 43 H39 2 -0.373655 0.457173 0.525802 11.00000 -1.20000 AFIX 0 C40 1 0.564346 0.134045 0.902645 11.00000 0.05214 0.05054 = 0.07931 0.03240 0.02941 0.02950 AFIX 137 H40A 2 0.635215 0.174309 0.912744 11.00000 -1.50000 H40B 2 0.558450 0.082581 0.868483 11.00000 -1.50000 H40C 2 0.547825 0.108278 0.944075 11.00000 -1.50000 AFIX 0 S3 5 -0.381023 -0.212569 0.442730 11.00000 0.05099 0.06779 = 0.06314 -0.00077 0.01026 0.00678 O1D 4 -0.674960 -0.115056 0.663290 11.00000 0.06340 0.05388 = 0.05449 -0.00337 0.00283 0.00073 C3 1 -0.600998 -0.164197 0.546932 11.00000 0.02928 0.06968 = 0.05825 0.00026 0.00226 0.00104 AFIX 43 H3 2 -0.671605 -0.162933 0.539432 11.00000 -1.20000 AFIX 0 C4 1 -0.391100 -0.125179 0.385617 11.00000 0.04962 0.06797 = 0.03377 0.00312 0.01314 -0.00968 AFIX 137 H4A 2 -0.463584 -0.123133 0.372362 11.00000 -1.50000 H4B 2 -0.366333 -0.140546 0.345226 11.00000 -1.50000 H4C 2 -0.348916 -0.063878 0.407904 11.00000 -1.50000 AFIX 0 C5 1 0.140134 0.886360 0.897390 11.00000 0.08692 0.03165 = 0.02666 -0.01058 -0.02314 0.02542 AFIX 43 H5 2 0.157302 0.952917 0.902973 11.00000 -1.20000 AFIX 0 C22 1 0.090009 0.689341 0.887733 11.00000 0.09333 0.04618 = 0.06521 -0.01269 0.00806 0.05213 AFIX 43 H22 2 0.074529 0.622959 0.886363 11.00000 -1.20000 AFIX 0 C6 1 -0.554679 -0.185971 0.490223 11.00000 0.08211 0.06620 = 0.03806 0.00668 0.00938 0.03592 AFIX 43 H6 2 -0.593464 -0.197463 0.444882 11.00000 -1.20000 AFIX 0 C24 1 0.218362 0.842911 0.885571 11.00000 0.02652 0.05542 = 0.03844 -0.00750 -0.01178 0.02166 O1E 4 -0.432097 0.549640 0.568582 11.00000 0.08648 0.13578 = 0.14749 -0.04587 0.01393 -0.01839 C7 1 0.189559 0.740355 0.882769 11.00000 0.07826 0.05594 = 0.06279 -0.01805 -0.02722 0.04341 AFIX 43 H7 2 0.239588 0.707258 0.877440 11.00000 -1.20000 AFIX 0 C8 1 -0.585292 -0.122363 0.670951 11.00000 0.03553 0.02989 = 0.04581 0.01421 0.00512 -0.01138 AFIX 43 H8 2 -0.543621 -0.113196 0.715424 11.00000 -1.20000 AFIX 0 S4 5 -0.116897 0.678788 0.897996 11.00000 0.08049 0.03094 = 0.03745 0.00219 0.01233 0.02541 C9 1 0.009858 0.737668 0.895004 11.00000 0.08839 0.03172 = 0.02811 -0.00565 0.00639 0.02906 C10 1 -0.111601 0.562944 0.922493 11.00000 0.07361 0.03270 = 0.04400 0.00901 0.01813 0.02769 AFIX 137 H10A 2 -0.080993 0.532326 0.890724 11.00000 -1.50000 H10B 2 -0.181814 0.525151 0.921613 11.00000 -1.50000 H10C 2 -0.069143 0.568913 0.968348 11.00000 -1.50000 AFIX 0 C11 1 0.038904 0.837931 0.901437 11.00000 0.06260 0.02441 = 0.05052 0.00410 -0.01345 0.01913 AFIX 43 H11 2 -0.009740 0.871829 0.908409 11.00000 -1.20000 AFIX 0 O1F 4 0.388429 0.859594 0.864498 11.00000 0.09472 0.10408 = 0.17148 -0.05441 -0.00115 0.03267 C12 1 0.321817 0.898240 0.878017 11.00000 0.06423 0.05724 = 0.05664 -0.00325 -0.01059 0.03208 AFIX 43 H12 2 0.337590 0.964745 0.883633 11.00000 -1.20000 AFIX 0 C19 1 -0.473259 -0.309020 0.391893 11.00000 0.03643 0.21416 = 0.04849 -0.01985 0.02527 -0.02812 AFIX 137 H19A 2 -0.474431 -0.366043 0.414919 11.00000 -1.50000 H19B 2 -0.454276 -0.317300 0.348124 11.00000 -1.50000 H19C 2 -0.541986 -0.296960 0.384573 11.00000 -1.50000 AFIX 0 C1A 1 -0.182241 0.650283 0.807157 11.00000 0.06093 0.02282 = 0.05130 -0.00304 -0.00260 0.01322 AFIX 137 H1AA 2 -0.173138 0.707836 0.784305 11.00000 -1.50000 H1AB 2 -0.256263 0.621955 0.803392 11.00000 -1.50000 H1AC 2 -0.151796 0.606019 0.785850 11.00000 -1.50000 AFIX 0 N16 3 0.400057 0.639206 0.700777 11.00000 0.04725 0.04129 = 0.07470 0.02079 -0.00226 -0.00434 C1B 1 0.361131 0.663807 0.758178 11.00000 0.04167 0.04323 = 0.07431 -0.01511 -0.00672 -0.00292 AFIX 137 H1BA 2 0.329313 0.715929 0.748870 11.00000 -1.50000 H1BB 2 0.418253 0.682742 0.797994 11.00000 -1.50000 H1BC 2 0.309223 0.609563 0.766901 11.00000 -1.50000 AFIX 0 C1C 1 0.333245 0.610348 0.634216 11.00000 0.12143 0.06476 = 0.07477 0.02356 -0.03409 -0.04159 AFIX 137 H1CA 2 0.264910 0.574042 0.638885 11.00000 -1.50000 H1CB 2 0.363517 0.571519 0.607646 11.00000 -1.50000 H1CC 2 0.326135 0.665970 0.611111 11.00000 -1.50000 AFIX 0 O1G 4 0.565436 0.664818 0.766262 11.00000 0.11614 0.08115 = 0.31957 -0.06749 -0.07081 0.02286 C1D 1 0.503057 0.637300 0.709190 11.00000 0.09676 0.07992 = 0.17668 -0.04296 0.00947 -0.00756 AFIX 43 H1D 2 0.527231 0.615319 0.672131 11.00000 -1.20000 AFIX 0 N1E 3 0.674436 0.911392 0.916866 11.00000 0.04903 0.04219 = 0.03795 0.01321 0.01465 0.01111 C1F 1 0.753349 1.002260 0.931145 11.00000 0.03034 0.05113 = 0.05795 0.01099 0.01257 0.00460 AFIX 137 H1FA 2 0.730554 1.046008 0.958893 11.00000 -1.50000 H1FB 2 0.762709 1.028062 0.888389 11.00000 -1.50000 H1FC 2 0.819143 0.992999 0.955626 11.00000 -1.50000 AFIX 0 C1G 1 0.608106 0.889763 0.959243 11.00000 0.10472 0.07363 = 0.05930 0.00734 0.04733 -0.00468 AFIX 43 H1G 2 0.553843 0.834009 0.946335 11.00000 -1.20000 AFIX 0 O1H 4 0.610978 0.935205 1.013044 11.00000 0.16015 0.12868 = 0.08271 -0.03968 0.08073 -0.06473 C1E 1 0.666978 0.844021 0.860749 11.00000 0.27057 0.09002 = 0.07422 0.01169 0.07002 0.01140 AFIX 137 H1EA 2 0.655650 0.872880 0.818225 11.00000 -1.50000 H1EB 2 0.608860 0.789428 0.859830 11.00000 -1.50000 H1EC 2 0.731366 0.824056 0.866128 11.00000 -1.50000 HKLF 4 REM REM R1 = 0.0602 for 10869 Fo > 4sig(Fo) and 0.0846 for all 14724 data REM 966 parameters refined using 0 restraints END WGHT 0.0735 21.3283 REM Highest difference peak 4.017, deepest hole -4.125, 1-sigma level 0.403 Q1 1 -0.0799 0.2881 0.5653 11.00000 0.05 4.02 Q2 1 0.1034 0.4915 0.7025 11.00000 0.05 3.90 Q3 1 -0.1601 0.3113 0.8436 11.00000 0.05 3.61 Q4 1 0.1677 0.0864 0.7917 11.00000 0.05 3.47 Q5 1 0.1668 0.4250 0.8586 11.00000 0.05 3.39 Q6 1 -0.1201 0.0835 0.5796 11.00000 0.05 3.10 Q7 1 0.1192 0.0874 0.7801 11.00000 0.05 2.94 Q8 1 0.5689 0.2403 0.8913 11.00000 0.05 2.87 Q9 1 -0.2977 0.1767 0.7400 11.00000 0.05 2.84 Q10 1 -0.3559 0.1085 0.7450 11.00000 0.05 2.73 REM The information below was added by Olex2. REM REM R1 = 0.0602 for 10869 Fo > 4sig(Fo) and 0.0846 for all 20346 data REM n/a parameters refined using n/a restraints REM Highest difference peak 4.02, deepest hole -4.13 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0846 REM R1_gt = 0.0602 REM wR_ref = 0.1625 REM GOOF = 1.026 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 20346 REM Reflections_gt = 10869 REM Parameters = n/a REM Hole = -4.13 REM Peak = 4.02 REM Flack = n/a ; _cod_data_source_file d0dt01410a2.cif _cod_data_source_block ak_47a_lt_cu _cod_original_cell_volume 3623.2(3) _cod_database_code 7705294 _chemical_oxdiff_formula 'C84 H118 Mo24 N4 O92 S8 Si2 ' _reflns_odcompleteness_completeness 98.40 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C14(H14), C17(H17), C28(H28), C29(H29), C16(H16), C20(H20), C26(H26), C2(H2), C32(H32), C36(H36), C37(H37), C39(H39), C3(H3), C5(H5), C22(H22), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C1D(H1D), C1G(H1G) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C40(H40A,H40B, H40C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C1A(H1AA, H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1F(H1FA,H1FB,H1FC), C1E(H1EA,H1EB,H1EC) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.736 _oxdiff_exptl_absorpt_empirical_full_min 0.773 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn W1 W 0.05238(5) 0.16387(4) 0.90073(3) 0.02151(14) Uani 1 d . . . W2 W 0.24195(5) 0.35026(4) 0.73848(3) 0.02223(15) Uani 1 d . . . W3 W -0.21475(5) 0.37833(4) 0.71167(3) 0.02208(15) Uani 1 d . . . W4 W -0.10670(5) -0.00494(4) 0.75507(3) 0.02314(15) Uani 1 d . . . W5 W 0.11902(5) 0.40250(4) 0.87902(3) 0.02457(15) Uani 1 d . . . W6 W 0.09591(5) 0.19503(4) 0.59950(3) 0.02305(15) Uani 1 d . . . W7 W -0.29270(5) 0.12222(5) 0.72794(3) 0.02439(15) Uani 1 d . . . W8 W 0.04148(6) 0.48539(4) 0.71041(4) 0.02969(17) Uani 1 d . . . W9 W -0.13684(5) 0.28731(4) 0.87760(3) 0.02468(15) Uani 1 d . . . W10 W 0.16799(5) 0.11138(4) 0.75554(4) 0.02646(16) Uani 1 d . . . W11 W -0.17729(5) 0.07040(4) 0.59612(3) 0.02472(15) Uani 1 d . . . W12 W -0.10896(6) 0.32582(5) 0.57621(3) 0.03158(17) Uani 1 d . . . Si13 Si -0.0265(2) 0.2407(2) 0.73605(16) 0.0056(6) Uani 1 d . . . O18 O 0.0899(10) 0.1101(8) 0.9712(6) 0.039(3) Uani 1 d . . . O21 O -0.1255(10) -0.1228(7) 0.7718(6) 0.034(3) Uani 1 d . . . O22 O 0.0931(9) 0.6053(7) 0.7088(7) 0.038(3) Uani 1 d . . . O23 O -0.4215(9) 0.0803(8) 0.7320(6) 0.035(3) Uani 1 d . . . O25 O -0.1445(10) 0.3505(8) 0.4935(6) 0.037(3) Uani 1 d . . . O26 O -0.2409(9) 0.0025(8) 0.5197(6) 0.033(3) Uani 1 d . . . O27 O 0.3677(9) 0.4187(8) 0.7464(6) 0.037(3) Uani 1 d . . . O41 O 0.1334(12) 0.1707(9) 0.5255(7) 0.047(3) Uani 1 d . . . O57 O 0.2494(9) 0.0391(7) 0.7731(6) 0.028(2) Uani 1 d . . . O70 O 0.1962(9) 0.4917(8) 0.9393(7) 0.043(3) Uani 1 d . . . O5 O -0.0991(9) 0.4905(8) 0.7207(6) 0.032(3) Uani 1 d . . . O7 O -0.2100(9) 0.3090(8) 0.9346(6) 0.034(3) Uani 1 d . . . O8 O -0.2446(9) 0.0091(8) 0.7582(5) 0.031(3) Uani 1 d . . . O9 O -0.0364(8) 0.1012(8) 0.5898(6) 0.030(3) Uani 1 d . . . O10 O -0.1552(10) -0.0264(9) 0.6536(6) 0.040(3) Uani 1 d . . . O11 O -0.2300(10) 0.1820(8) 0.8193(6) 0.036(3) Uani 1 d . . . O12 O -0.3004(10) 0.0739(8) 0.6352(6) 0.038(3) Uani 1 d . . . O13 O -0.0645(9) 0.2018(8) 0.9258(6) 0.038(3) Uani 1 d . . . O14 O 0.0304(9) 0.0252(9) 0.7377(6) 0.038(3) Uani 1 d . . . O15 O 0.2118(10) 0.3734(9) 0.8261(6) 0.036(3) Uani 1 d . . . O16 O -0.1793(10) 0.1972(8) 0.5739(7) 0.043(3) Uani 1 d . . . O17 O 0.2731(10) 0.2346(8) 0.7649(6) 0.038(3) Uani 1 d . . . O1 O 0.1445(10) 0.1469(8) 0.8442(6) 0.036(3) Uiso 1 d . . . O19 O -0.0506(9) 0.0616(8) 0.8420(6) 0.030(3) Uani 1 d . . . O20 O 0.0796(10) 0.2300(8) 0.7135(6) 0.036(3) Uani 1 d . . . O2 O -0.2180(10) 0.3634(9) 0.6138(7) 0.044(3) Uani 1 d . . . O3 O -0.0113(9) 0.3899(8) 0.9086(8) 0.045(3) Uani 1 d . . . O4 O 0.2142(11) 0.2976(8) 0.6438(6) 0.041(3) Uani 1 d . . . O24 O 0.1590(10) 0.1127(8) 0.6579(6) 0.039(3) Uani 1 d . . . O6 O 0.0157(10) 0.2857(8) 0.5729(7) 0.044(3) Uani 1 d . . . O1A O 0.1332(10) 0.2909(8) 0.9286(8) 0.050(4) Uani 1 d . . . O1B O -0.0073(8) 0.2641(7) 0.8189(6) 0.028(2) Uani 1 d . . . O28 O -0.1751(10) 0.3630(8) 0.8066(6) 0.042(3) Uani 1 d . . . O29 O -0.0642(9) 0.3258(8) 0.6979(5) 0.030(3) Uani 1 d . . . O30 O -0.0167(10) 0.4492(9) 0.6148(6) 0.043(3) Uani 1 d . . . O31 O -0.3149(11) 0.4298(10) 0.7093(7) 0.057(4) Uani 1 d . . . O32 O 0.1572(12) 0.4343(10) 0.7054(7) 0.051(4) Uani 1 d . . . O33 O 0.0657(11) 0.4680(9) 0.8077(6) 0.040(3) Uani 1 d . . . O34 O -0.2888(11) 0.2451(8) 0.7008(6) 0.040(3) Uani 1 d . . . O35 O -0.1195(9) 0.1403(8) 0.7117(5) 0.030(3) Uani 1 d . . . C13 C 0.4621(12) 0.4007(10) 1.0516(8) 0.022(3) Uani 1 d . . . C14 C -0.0715(12) 0.6299(11) 0.5619(9) 0.029(4) Uani 1 d . . . H14 H -0.0189 0.6136 0.5429 0.035 Uiso 1 calc . . R C15 C -0.0505(12) 0.7129(11) 0.6098(8) 0.024(3) Uani 1 d . . . C17 C 0.3794(13) 0.2942(11) 0.9480(9) 0.029(4) Uiso 1 d . . . H17 H 0.3182 0.2604 0.9170 0.035 Uiso 1 calc . . R C18 C -0.2524(15) 0.5935(13) 0.5728(8) 0.034(4) Uani 1 d . . . C25 C 0.4772(14) 0.2840(11) 0.9410(8) 0.029(4) Uani 1 d . . . C28 C -0.1761(15) 0.5750(13) 0.5455(8) 0.037(4) Uani 1 d . . . H28 H -0.1931 0.5219 0.5131 0.045 Uiso 1 calc . . R C29 C 0.3744(16) 0.3542(12) 1.0010(9) 0.041(4) Uani 1 d . . . H29 H 0.3092 0.3647 1.0036 0.049 Uiso 1 calc . . R S1 S 0.0804(4) 0.7829(3) 0.6293(2) 0.0368(10) Uani 1 d . . . S2 S 0.4742(4) 0.2028(3) 0.8703(3) 0.0429(11) Uani 1 d . . . C16 C 0.5712(13) 0.3312(12) 0.9883(9) 0.035(4) Uani 1 d . . . H16 H 0.6366 0.3234 0.9833 0.042 Uiso 1 calc . . R C1 C 0.1060(17) 0.8185(12) 0.7201(9) 0.044(5) Uani 1 d . . . H1A H 0.0559 0.8525 0.7293 0.066 Uiso 1 calc . . GR H1B H 0.1762 0.8594 0.7347 0.066 Uiso 1 calc . . GR H1C H 0.0995 0.7628 0.7449 0.066 Uiso 1 calc . . GR C20 C 0.5612(15) 0.3899(13) 1.0427(10) 0.045(5) Uani 1 d . . . H20 H 0.6218 0.4233 1.0745 0.054 Uiso 1 calc . . R C23 C 0.5442(15) 0.2808(14) 0.8179(11) 0.046(5) Uani 1 d . . . H23A H 0.5047 0.3255 0.8015 0.069 Uiso 1 calc . . GR H23B H 0.5533 0.2437 0.7792 0.069 Uiso 1 calc . . GR H23C H 0.6122 0.3151 0.8449 0.069 Uiso 1 calc . . GR C26 C -0.3917(16) -0.1695(14) 0.5718(12) 0.049(5) Uani 1 d . . . H26 H -0.3208 -0.1701 0.5811 0.058 Uiso 1 calc . . R C27 C -0.4475(17) -0.1891(12) 0.5066(12) 0.046(5) Uani 1 d . . . O1C O 0.3726(15) 0.4784(12) 1.1170(8) 0.072(5) Uani 1 d . . . C2 C 0.4500(18) 0.4617(15) 1.1087(9) 0.049(5) Uani 1 d . . . H2 H 0.5109 0.4900 1.1419 0.058 Uiso 1 calc . . R C30 C -0.5390(17) -0.1456(13) 0.6115(11) 0.044(5) Uani 1 d . . . C31 C 0.0740(17) 0.8968(13) 0.5975(10) 0.046(5) Uani 1 d . . . H31A H 0.0630 0.8906 0.5479 0.069 Uiso 1 calc . . GR H31B H 0.1391 0.9439 0.6166 0.069 Uiso 1 calc . . GR H31C H 0.0165 0.9166 0.6110 0.069 Uiso 1 calc . . GR C32 C -0.1309(19) 0.7343(14) 0.6389(10) 0.052(6) Uani 1 d . . . H32 H -0.1160 0.7885 0.6700 0.062 Uiso 1 calc . . R C36 C -0.2361(16) 0.6730(15) 0.6209(10) 0.047(5) Uani 1 d . . . H36 H -0.2904 0.6852 0.6400 0.057 Uiso 1 calc . . R C37 C -0.4343(18) -0.1498(13) 0.6225(12) 0.057(6) Uani 1 d . . . H37 H -0.3937 -0.1382 0.6673 0.068 Uiso 1 calc . . R C39 C -0.3625(19) 0.517(2) 0.5497(16) 0.080(9) Uani 1 d . . . H39 H -0.3737 0.4572 0.5258 0.096 Uiso 1 calc . . R C40 C 0.5643(17) 0.1340(14) 0.9026(12) 0.055(6) Uani 1 d . . . H40A H 0.6352 0.1743 0.9127 0.082 Uiso 1 calc . . GR H40B H 0.5584 0.0826 0.8685 0.082 Uiso 1 calc . . GR H40C H 0.5478 0.1083 0.9441 0.082 Uiso 1 calc . . GR S3 S -0.3810(5) -0.2126(5) 0.4427(3) 0.0627(15) Uani 1 d . . . O1D O -0.6750(13) -0.1151(10) 0.6633(8) 0.061(4) Uani 1 d . . . C3 C -0.6010(17) -0.1642(16) 0.5469(11) 0.056(6) Uani 1 d . . . H3 H -0.6716 -0.1629 0.5394 0.067 Uiso 1 calc . . R C4 C -0.3911(17) -0.1252(15) 0.3856(10) 0.054(6) Uani 1 d . . . H4A H -0.4636 -0.1231 0.3724 0.081 Uiso 1 calc . . GR H4B H -0.3663 -0.1405 0.3452 0.081 Uiso 1 calc . . GR H4C H -0.3489 -0.0639 0.4079 0.081 Uiso 1 calc . . GR C5 C 0.1401(19) 0.8864(14) 0.8974(9) 0.052(6) Uani 1 d . . . H5 H 0.1573 0.9529 0.9030 0.062 Uiso 1 calc . . R C22 C 0.090(2) 0.6893(16) 0.8877(12) 0.064(7) Uani 1 d . . . H22 H 0.0745 0.6230 0.8864 0.077 Uiso 1 calc . . R C6 C -0.555(2) -0.1860(16) 0.4902(11) 0.060(6) Uani 1 d . . . H6 H -0.5935 -0.1975 0.4449 0.071 Uiso 1 calc . . R C24 C 0.2184(15) 0.8429(14) 0.8856(10) 0.041(5) Uani 1 d . . . O1E O -0.4321(19) 0.5496(18) 0.5686(13) 0.135(9) Uani 1 d . . . C7 C 0.190(2) 0.7404(16) 0.8828(12) 0.068(8) Uani 1 d . . . H7 H 0.2396 0.7073 0.8774 0.081 Uiso 1 calc . . R C8 C -0.5853(16) -0.1224(12) 0.6710(10) 0.041(5) Uani 1 d . . . H8 H -0.5436 -0.1132 0.7154 0.049 Uiso 1 calc . . R S4 S -0.1169(5) 0.6788(3) 0.8980(3) 0.0477(13) Uani 1 d . . . C9 C 0.0099(19) 0.7377(13) 0.8950(9) 0.048(6) Uani 1 d . . . C10 C -0.1116(18) 0.5629(12) 0.9225(10) 0.047(5) Uani 1 d . . . H10A H -0.0810 0.5323 0.8907 0.070 Uiso 1 calc . . GR H10B H -0.1818 0.5252 0.9216 0.070 Uiso 1 calc . . GR H10C H -0.0691 0.5689 0.9683 0.070 Uiso 1 calc . . GR C11 C 0.0389(18) 0.8379(13) 0.9014(10) 0.048(5) Uani 1 d . . . H11 H -0.0097 0.8718 0.9084 0.058 Uiso 1 calc . . R O1F O 0.3884(19) 0.8596(16) 0.8645(13) 0.129(9) Uani 1 d . . . C12 C 0.322(2) 0.8982(17) 0.8780(12) 0.060(6) Uani 1 d . . . H12 H 0.3376 0.9647 0.8836 0.072 Uiso 1 calc . . R C19 C -0.4733(19) -0.309(2) 0.3919(13) 0.109(13) Uani 1 d . . . H19A H -0.4744 -0.3660 0.4149 0.164 Uiso 1 calc . . GR H19B H -0.4543 -0.3173 0.3481 0.164 Uiso 1 calc . . GR H19C H -0.5420 -0.2970 0.3846 0.164 Uiso 1 calc . . GR C1A C -0.1822(17) 0.6503(12) 0.8072(10) 0.047(5) Uani 1 d . . . H1AA H -0.1731 0.7078 0.7843 0.070 Uiso 1 calc . . GR H1AB H -0.2563 0.6220 0.8034 0.070 Uiso 1 calc . . GR H1AC H -0.1518 0.6060 0.7859 0.070 Uiso 1 calc . . GR N16 N 0.4001(16) 0.6392(12) 0.7008(11) 0.059(5) Uani 1 d . . . C1B C 0.3611(17) 0.6638(15) 0.7582(12) 0.059(6) Uani 1 d . . . H1BA H 0.3293 0.7159 0.7489 0.088 Uiso 1 calc . . GR H1BB H 0.4183 0.6827 0.7980 0.088 Uiso 1 calc . . GR H1BC H 0.3092 0.6096 0.7669 0.088 Uiso 1 calc . . GR C1C C 0.333(3) 0.6103(18) 0.6342(14) 0.106(12) Uani 1 d . . . H1CA H 0.2649 0.5740 0.6389 0.159 Uiso 1 calc . . GR H1CB H 0.3635 0.5715 0.6076 0.159 Uiso 1 calc . . GR H1CC H 0.3261 0.6660 0.6111 0.159 Uiso 1 calc . . GR O1G O 0.565(2) 0.6648(17) 0.766(2) 0.192(17) Uani 1 d . . . C1D C 0.503(3) 0.637(2) 0.709(2) 0.128(15) Uani 1 d . . . H1D H 0.5272 0.6153 0.6721 0.153 Uiso 1 calc . . R N1E N 0.6744(13) 0.9114(11) 0.9169(8) 0.042(4) Uani 1 d . . . C1F C 0.7533(15) 1.0023(14) 0.9311(11) 0.047(5) Uani 1 d . . . H1FA H 0.7306 1.0460 0.9589 0.070 Uiso 1 calc . . GR H1FB H 0.7627 1.0281 0.8884 0.070 Uiso 1 calc . . GR H1FC H 0.8191 0.9930 0.9556 0.070 Uiso 1 calc . . GR C1G C 0.608(2) 0.8898(19) 0.9592(13) 0.080(8) Uani 1 d . . . H1G H 0.5538 0.8340 0.9463 0.096 Uiso 1 calc . . R O1H O 0.611(2) 0.9352(16) 1.0130(11) 0.136(11) Uani 1 d . . . C1E C 0.667(4) 0.844(2) 0.8607(16) 0.146(18) Uani 1 d . . . H1EA H 0.6557 0.8729 0.8182 0.220 Uiso 1 calc . . GR H1EB H 0.6089 0.7894 0.8598 0.220 Uiso 1 calc . . GR H1EC H 0.7314 0.8241 0.8661 0.220 Uiso 1 calc . . GR 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 W1 0.0223(3) 0.0225(3) 0.0185(3) 0.0027(2) 0.0013(3) 0.0057(2) W2 0.0177(3) 0.0208(3) 0.0287(3) 0.0047(2) 0.0061(3) 0.0045(2) W3 0.0199(3) 0.0220(3) 0.0238(3) 0.0010(2) 0.0009(3) 0.0077(2) W4 0.0264(3) 0.0151(3) 0.0290(3) 0.0022(2) 0.0100(3) 0.0040(2) W5 0.0234(3) 0.0219(3) 0.0253(3) -0.0050(2) -0.0029(3) 0.0078(2) W6 0.0219(3) 0.0256(3) 0.0221(3) 0.0019(2) 0.0055(3) 0.0063(2) W7 0.0164(3) 0.0308(3) 0.0242(3) 0.0030(3) 0.0028(3) 0.0040(2) W8 0.0412(4) 0.0162(3) 0.0308(4) 0.0035(3) 0.0085(3) 0.0049(3) W9 0.0207(3) 0.0236(3) 0.0280(4) -0.0046(3) 0.0080(3) 0.0017(2) W10 0.0205(3) 0.0219(3) 0.0351(4) -0.0059(3) 0.0003(3) 0.0082(3) W11 0.0264(4) 0.0228(3) 0.0209(3) -0.0031(2) -0.0024(3) 0.0057(3) W12 0.0324(4) 0.0314(4) 0.0236(4) 0.0094(3) -0.0023(3) -0.0003(3) Si13 0.0033(16) 0.0059(16) 0.0073(16) -0.0009(12) 0.0010(13) 0.0011(12) O18 0.035(7) 0.042(7) 0.031(7) 0.017(5) -0.002(6) 0.001(5) O21 0.047(8) 0.021(6) 0.034(7) 0.007(5) 0.018(6) 0.000(5) O22 0.033(7) 0.020(6) 0.060(8) 0.007(5) 0.004(6) 0.010(5) O23 0.020(6) 0.047(7) 0.037(7) 0.006(6) 0.003(5) 0.011(5) O25 0.033(7) 0.045(7) 0.037(7) 0.016(6) 0.007(6) 0.018(6) O26 0.019(6) 0.041(7) 0.031(6) -0.008(5) -0.003(5) 0.002(5) O27 0.018(6) 0.047(7) 0.032(7) -0.007(5) -0.009(5) -0.002(5) O41 0.064(10) 0.036(7) 0.043(8) -0.007(6) 0.025(7) 0.006(6) O57 0.028(6) 0.026(6) 0.029(6) -0.006(5) 0.009(5) 0.003(5) O70 0.022(7) 0.035(7) 0.058(9) -0.008(6) -0.005(6) -0.003(5) O5 0.040(7) 0.031(6) 0.024(6) 0.001(5) 0.015(5) -0.002(5) O7 0.035(7) 0.031(6) 0.038(7) 0.011(5) 0.009(6) 0.009(5) O8 0.038(7) 0.046(7) 0.017(6) 0.019(5) 0.014(5) 0.014(6) O9 0.018(6) 0.034(6) 0.034(6) 0.011(5) -0.001(5) 0.001(5) O10 0.044(8) 0.061(8) 0.023(6) 0.005(6) 0.009(6) 0.030(7) O11 0.045(8) 0.024(6) 0.032(7) 0.008(5) 0.012(6) -0.007(5) O12 0.032(7) 0.038(7) 0.045(8) 0.000(6) 0.001(6) 0.020(6) O13 0.025(7) 0.041(7) 0.047(8) 0.010(6) 0.008(6) 0.009(5) O14 0.030(7) 0.048(8) 0.029(6) -0.020(5) 0.006(5) 0.000(6) O15 0.041(8) 0.049(7) 0.030(7) 0.017(6) 0.016(6) 0.026(6) O16 0.035(8) 0.026(6) 0.061(9) 0.006(6) -0.004(7) 0.003(5) O17 0.035(7) 0.028(6) 0.035(7) -0.006(5) -0.015(6) -0.004(5) O19 0.029(7) 0.029(6) 0.035(7) -0.001(5) 0.011(5) 0.007(5) O20 0.040(8) 0.044(7) 0.034(7) 0.012(6) 0.016(6) 0.023(6) O2 0.035(8) 0.052(8) 0.041(8) 0.000(6) 0.019(6) -0.006(6) O3 0.024(7) 0.021(6) 0.085(10) -0.002(6) 0.004(7) 0.003(5) O4 0.052(8) 0.022(6) 0.038(7) 0.005(5) -0.009(6) 0.008(5) O24 0.047(8) 0.024(6) 0.033(7) 0.004(5) -0.004(6) -0.008(5) O6 0.039(8) 0.030(7) 0.057(9) 0.007(6) 0.004(7) 0.002(5) O1A 0.030(7) 0.030(7) 0.088(11) 0.008(7) -0.002(7) 0.012(5) O1B 0.016(6) 0.024(6) 0.036(7) -0.002(5) -0.003(5) 0.000(4) O28 0.053(9) 0.024(6) 0.028(6) -0.013(5) -0.004(6) -0.016(5) O29 0.029(7) 0.038(7) 0.021(6) 0.003(5) 0.001(5) 0.010(5) O30 0.042(8) 0.043(7) 0.039(7) -0.001(6) 0.019(6) -0.003(6) O31 0.054(9) 0.055(9) 0.054(9) -0.031(7) -0.029(7) 0.036(7) O32 0.064(10) 0.072(10) 0.034(7) 0.018(7) 0.013(7) 0.043(8) O33 0.055(9) 0.051(8) 0.027(6) 0.008(6) 0.015(6) 0.034(7) O34 0.068(10) 0.032(7) 0.016(6) 0.002(5) 0.010(6) 0.002(6) O35 0.022(6) 0.040(7) 0.023(6) -0.001(5) -0.007(5) 0.009(5) C13 0.025(8) 0.017(7) 0.031(9) 0.012(6) 0.010(7) 0.013(6) C14 0.013(8) 0.030(8) 0.039(10) 0.007(7) -0.013(7) 0.011(6) C15 0.024(8) 0.025(8) 0.028(8) 0.004(6) 0.010(7) 0.011(6) C18 0.044(11) 0.041(10) 0.019(8) 0.012(7) 0.005(8) 0.015(8) C25 0.035(10) 0.030(9) 0.019(8) -0.005(6) 0.012(7) -0.001(7) C28 0.046(12) 0.043(11) 0.021(9) -0.010(7) 0.001(8) 0.015(9) C29 0.039(11) 0.038(10) 0.039(11) 0.002(8) -0.001(9) 0.006(8) S1 0.046(3) 0.028(2) 0.034(2) -0.0038(18) 0.008(2) 0.0073(19) S2 0.044(3) 0.040(3) 0.046(3) -0.001(2) 0.009(2) 0.013(2) C16 0.012(8) 0.048(11) 0.050(11) 0.000(9) 0.016(8) 0.009(7) C1 0.071(15) 0.029(9) 0.029(10) -0.003(7) -0.005(10) 0.022(9) C20 0.038(11) 0.041(11) 0.037(11) 0.001(8) -0.010(9) -0.010(8) C23 0.033(11) 0.056(12) 0.056(13) 0.022(10) 0.014(10) 0.019(9) C26 0.032(11) 0.038(11) 0.070(16) 0.004(10) 0.006(11) 0.002(8) C27 0.054(13) 0.027(9) 0.067(15) 0.030(9) 0.031(12) 0.011(9) O1C 0.089(14) 0.089(13) 0.058(10) -0.006(9) 0.024(10) 0.058(11) C2 0.062(15) 0.063(14) 0.016(9) 0.005(9) -0.010(9) 0.023(11) C30 0.047(12) 0.034(10) 0.055(13) 0.006(9) 0.013(10) 0.017(9) C31 0.053(13) 0.044(11) 0.047(12) 0.019(9) 0.023(10) 0.012(9) C32 0.081(17) 0.044(12) 0.038(11) -0.015(9) 0.006(11) 0.037(12) C36 0.039(12) 0.073(15) 0.036(11) 0.000(10) 0.011(9) 0.025(11) C37 0.053(14) 0.031(11) 0.065(15) 0.003(10) -0.027(12) 0.000(9) C39 0.041(14) 0.11(2) 0.11(2) 0.072(19) 0.028(15) 0.039(15) C40 0.052(14) 0.051(12) 0.079(16) 0.032(12) 0.029(12) 0.030(11) S3 0.051(4) 0.068(4) 0.063(4) -0.001(3) 0.010(3) 0.007(3) O1D 0.063(11) 0.054(9) 0.054(10) -0.003(7) 0.003(8) 0.001(8) C3 0.029(11) 0.070(15) 0.058(14) 0.000(11) 0.002(10) 0.001(10) C4 0.050(14) 0.068(14) 0.034(11) 0.003(10) 0.013(10) -0.010(10) C5 0.087(18) 0.032(10) 0.027(10) -0.011(8) -0.023(11) 0.025(11) C22 0.09(2) 0.046(13) 0.065(15) -0.013(11) 0.008(15) 0.052(14) C6 0.082(18) 0.066(15) 0.038(12) 0.007(10) 0.009(12) 0.036(14) C24 0.027(10) 0.055(12) 0.038(11) -0.007(9) -0.012(8) 0.022(9) O1E 0.086(19) 0.14(2) 0.15(2) -0.046(17) 0.014(17) -0.018(15) C7 0.078(19) 0.056(14) 0.063(15) -0.018(12) -0.027(14) 0.043(14) C8 0.036(11) 0.030(9) 0.046(12) 0.014(8) 0.005(9) -0.011(8) S4 0.080(4) 0.031(2) 0.037(3) 0.002(2) 0.012(3) 0.025(3) C9 0.088(17) 0.032(10) 0.028(10) -0.006(8) 0.006(11) 0.029(11) C10 0.074(15) 0.033(10) 0.044(11) 0.009(8) 0.018(11) 0.028(10) C11 0.063(15) 0.024(9) 0.051(12) 0.004(8) -0.013(11) 0.019(9) O1F 0.095(18) 0.104(17) 0.17(2) -0.054(16) -0.001(16) 0.033(14) C12 0.064(16) 0.057(14) 0.057(14) -0.003(11) -0.011(12) 0.032(13) C19 0.036(15) 0.21(4) 0.048(16) -0.020(19) 0.025(12) -0.028(18) C1A 0.061(14) 0.023(9) 0.051(12) -0.003(8) -0.003(11) 0.013(9) N16 0.047(12) 0.041(10) 0.075(14) 0.021(10) -0.002(11) -0.004(8) C1B 0.042(13) 0.043(12) 0.074(16) -0.015(11) -0.007(12) -0.003(9) C1C 0.12(3) 0.065(17) 0.075(19) 0.024(14) -0.034(19) -0.042(16) O1G 0.12(2) 0.081(17) 0.32(4) -0.07(2) -0.07(3) 0.023(15) C1D 0.10(3) 0.08(2) 0.18(4) -0.04(2) 0.01(3) -0.01(2) N1E 0.049(10) 0.042(9) 0.038(9) 0.013(7) 0.015(8) 0.011(8) C1F 0.030(11) 0.051(12) 0.058(13) 0.011(10) 0.013(10) 0.005(9) C1G 0.10(2) 0.074(18) 0.059(17) 0.007(14) 0.047(17) -0.005(15) O1H 0.16(2) 0.129(19) 0.083(15) -0.040(14) 0.081(16) -0.065(16) C1E 0.27(6) 0.09(3) 0.07(2) 0.012(19) 0.07(3) 0.01(3) 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' S S 0.1246 0.1234 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -16 18 0.0437 14 2 12 0.0585 3 16 -17 0.0301 18 -2 -13 0.0492 16 -10 8 0.0407 -4 16 16 0.1005 -15 16 8 0.0783 -19 8 2 0.0463 -11 9 -18 0.0406 -2 1 -26 0.0631 -4 17 -16 0.0364 -16 -6 6 0.0338 16 6 -6 0.0338 -13 15 -10 0.0405 -3 -17 14 0.0484 0 10 22 0.1099 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 O18 W1 O13 99.2(6) . . ? O18 W1 O1 103.8(6) . . ? O18 W1 O19 102.6(5) . . ? O18 W1 O1A 100.7(6) . . ? O18 W1 O1B 167.4(5) . . ? O13 W1 O1B 71.0(4) . . ? O1 W1 O13 156.9(5) . . ? O1 W1 O19 86.4(5) . . ? O1 W1 O1A 90.3(6) . . ? O1 W1 O1B 86.5(4) . . ? O19 W1 O13 86.5(5) . . ? O19 W1 O1B 85.1(4) . . ? O1A W1 O13 87.5(5) . . ? O1A W1 O19 156.6(5) . . ? O1A W1 O1B 71.5(5) . . ? O27 W2 O15 103.6(6) . . ? O27 W2 O17 98.8(5) . . ? O27 W2 O20 167.3(5) . . ? O27 W2 O4 99.7(6) . . ? O27 W2 O32 103.3(6) . . ? O15 W2 O17 89.8(5) . . ? O15 W2 O20 86.4(5) . . ? O15 W2 O4 156.7(6) . . ? O15 W2 O32 87.2(5) . . ? O17 W2 O20 73.0(4) . . ? O17 W2 O4 88.0(5) . . ? O17 W2 O32 157.8(6) . . ? O4 W2 O20 70.8(5) . . ? O32 W2 O20 84.8(5) . . ? O32 W2 O4 86.1(5) . . ? O5 W3 O2 88.9(5) . . ? O5 W3 O29 72.7(4) . . ? O2 W3 O29 72.3(5) . . ? O28 W3 O5 90.9(5) . . ? O28 W3 O2 157.8(6) . . ? O28 W3 O29 86.4(5) . . ? O28 W3 O34 86.1(5) . . ? O31 W3 O5 100.0(6) . . ? O31 W3 O2 99.1(6) . . ? O31 W3 O28 102.8(6) . . ? O31 W3 O29 168.6(6) . . ? O31 W3 O34 101.0(7) . . ? O34 W3 O5 158.9(5) . . ? O34 W3 O2 86.2(5) . . ? O34 W3 O29 86.3(5) . . ? O21 W4 O8 98.6(5) . . ? O21 W4 O10 98.1(5) . . ? O21 W4 O14 102.6(6) . . ? O21 W4 O19 103.2(5) . . ? O21 W4 O35 165.8(5) . . ? O8 W4 O10 86.9(5) . . ? O8 W4 O35 72.7(4) . . ? O10 W4 O35 70.8(4) . . ? O14 W4 O8 158.3(5) . . ? O14 W4 O10 85.5(5) . . ? O14 W4 O35 85.7(5) . . ? O19 W4 O8 91.5(5) . . ? O19 W4 O10 158.6(5) . . ? O19 W4 O14 88.3(5) . . ? O19 W4 O35 88.3(4) . . ? O70 W5 O15 104.4(6) . . ? O70 W5 O3 98.4(6) . . ? O70 W5 O1A 100.1(6) . . ? O70 W5 O1B 165.4(5) . . ? O70 W5 O33 103.3(6) . . ? O15 W5 O3 157.1(6) . . ? O15 W5 O1A 88.0(5) . . ? O15 W5 O1B 86.7(5) . . ? O3 W5 O1A 86.5(5) . . ? O3 W5 O1B 70.5(5) . . ? O1A W5 O1B 70.5(5) . . ? O33 W5 O15 89.0(5) . . ? O33 W5 O3 87.3(6) . . ? O33 W5 O1A 156.4(6) . . ? O33 W5 O1B 85.9(5) . . ? O41 W6 O9 102.4(6) . . ? O41 W6 O20 168.2(6) . . ? O41 W6 O4 100.4(6) . . ? O41 W6 O24 100.2(6) . . ? O41 W6 O6 101.6(6) . . ? O9 W6 O20 85.8(5) . . ? O9 W6 O24 87.4(5) . . ? O4 W6 O9 157.2(5) . . ? O4 W6 O20 71.4(5) . . ? O4 W6 O24 86.9(5) . . ? O4 W6 O6 89.9(5) . . ? O24 W6 O20 71.5(4) . . ? O6 W6 O9 87.2(5) . . ? O6 W6 O20 87.1(5) . . ? O6 W6 O24 158.2(6) . . ? O23 W7 O8 97.5(5) . . ? O23 W7 O11 102.3(5) . . ? O23 W7 O12 99.3(6) . . ? O23 W7 O34 102.0(6) . . ? O23 W7 O35 165.6(5) . . ? O8 W7 O35 71.4(4) . . ? O11 W7 O8 87.0(5) . . ? O11 W7 O12 158.3(5) . . ? O11 W7 O35 86.6(5) . . ? O12 W7 O8 87.5(4) . . ? O12 W7 O35 71.7(4) . . ? O34 W7 O8 160.4(6) . . ? O34 W7 O11 87.2(5) . . ? O34 W7 O12 91.0(5) . . ? O34 W7 O35 89.5(5) . . ? O22 W8 O5 97.8(5) . . ? O22 W8 O29 167.3(5) . . ? O22 W8 O30 100.0(6) . . ? O22 W8 O32 102.8(6) . . ? O22 W8 O33 103.8(6) . . ? O5 W8 O29 72.5(4) . . ? O30 W8 O5 87.6(5) . . ? O30 W8 O29 72.0(4) . . ? O30 W8 O33 155.8(6) . . ? O32 W8 O5 159.3(6) . . ? O32 W8 O29 87.5(5) . . ? O32 W8 O30 91.2(6) . . ? O32 W8 O33 87.8(5) . . ? O33 W8 O5 84.9(5) . . ? O33 W8 O29 83.7(5) . . ? O7 W9 O11 102.3(6) . . ? O7 W9 O13 100.5(5) . . ? O7 W9 O3 100.5(6) . . ? O7 W9 O1B 168.2(5) . . ? O7 W9 O28 101.6(5) . . ? O11 W9 O13 89.7(5) . . ? O11 W9 O3 157.0(6) . . ? O11 W9 O1B 86.8(5) . . ? O11 W9 O28 86.3(5) . . ? O13 W9 O1B 71.7(4) . . ? O3 W9 O13 89.0(5) . . ? O3 W9 O1B 71.0(5) . . ? O28 W9 O13 157.9(6) . . ? O28 W9 O3 86.3(5) . . ? O28 W9 O1B 86.4(5) . . ? O57 W10 O14 103.5(5) . . ? O57 W10 O17 99.5(5) . . ? O57 W10 O1 103.6(5) . . ? O57 W10 O20 166.5(5) . . ? O57 W10 O24 99.6(5) . . ? O14 W10 O17 157.0(5) . . ? O14 W10 O1 87.3(5) . . ? O14 W10 O20 85.9(5) . . ? O14 W10 O24 89.5(5) . . ? O17 W10 O20 71.4(5) . . ? O1 W10 O17 87.9(5) . . ? O1 W10 O20 86.3(4) . . ? O1 W10 O24 156.7(5) . . ? O24 W10 O17 86.1(5) . . ? O24 W10 O20 70.5(5) . . ? O26 W11 O9 103.5(5) . . ? O26 W11 O10 100.5(5) . . ? O26 W11 O12 99.0(5) . . ? O26 W11 O16 102.6(6) . . ? O26 W11 O35 166.9(5) . . ? O9 W11 O10 90.8(5) . . ? O9 W11 O12 157.3(5) . . ? O9 W11 O16 87.3(5) . . ? O9 W11 O35 87.4(5) . . ? O10 W11 O12 87.9(5) . . ? O10 W11 O16 156.7(5) . . ? O10 W11 O35 71.6(4) . . ? O12 W11 O35 70.7(4) . . ? O16 W11 O12 85.0(5) . . ? O16 W11 O35 85.0(5) . . ? O25 W12 O16 103.3(6) . . ? O25 W12 O2 99.0(6) . . ? O25 W12 O6 101.0(6) . . ? O25 W12 O29 167.2(5) . . ? O25 W12 O30 99.0(6) . . ? O16 W12 O2 90.4(6) . . ? O16 W12 O6 87.8(5) . . ? O16 W12 O29 86.6(5) . . ? O16 W12 O30 157.7(5) . . ? O2 W12 O29 72.4(5) . . ? O6 W12 O2 159.7(6) . . ? O6 W12 O29 87.3(5) . . ? O6 W12 O30 86.7(5) . . ? O30 W12 O2 87.4(5) . . ? O30 W12 O29 71.5(5) . . ? O20 Si13 O1B 111.3(6) . . ? O20 Si13 O35 109.3(6) . . ? O1B Si13 O35 109.0(6) . . ? O29 Si13 O20 108.6(6) . . ? O29 Si13 O1B 109.7(6) . . ? O29 Si13 O35 109.0(6) . . ? W3 O5 W8 123.1(6) . . ? W4 O8 W7 122.6(6) . . ? W11 O9 W6 149.6(6) . . ? W11 O10 W4 124.4(6) . . ? W9 O11 W7 148.7(6) . . ? W7 O12 W11 124.4(6) . . ? W1 O13 W9 124.8(6) . . ? W4 O14 W10 148.1(6) . . ? W5 O15 W2 149.3(7) . . ? W12 O16 W11 149.8(7) . . ? W2 O17 W10 124.5(6) . . ? W1 O1 W10 150.1(7) . . ? W4 O19 W1 149.6(7) . . ? W2 O20 W10 91.1(4) . . ? W6 O20 W2 92.2(4) . . ? W6 O20 W10 92.0(4) . . ? Si13 O20 W2 124.4(6) . . ? Si13 O20 W6 125.5(7) . . ? Si13 O20 W10 122.0(6) . . ? W3 O2 W12 123.4(7) . . ? W5 O3 W9 125.7(7) . . ? W6 O4 W2 125.4(7) . . ? W10 O24 W6 126.0(7) . . ? W12 O6 W6 146.6(7) . . ? W1 O1A W5 125.7(7) . . ? W5 O1B W1 92.2(4) . . ? W9 O1B W1 92.4(4) . . ? W9 O1B W5 92.7(4) . . ? Si13 O1B W1 124.1(5) . . ? Si13 O1B W5 121.9(6) . . ? Si13 O1B W9 124.6(6) . . ? W3 O28 W9 150.3(7) . . ? W8 O29 W3 91.7(4) . . ? W12 O29 W3 91.8(4) . . ? W12 O29 W8 91.5(4) . . ? Si13 O29 W3 124.8(6) . . ? Si13 O29 W8 123.6(6) . . ? Si13 O29 W12 123.8(6) . . ? W8 O30 W12 125.0(6) . . ? W8 O32 W2 148.9(8) . . ? W5 O33 W8 148.3(6) . . ? W7 O34 W3 147.8(7) . . ? W4 O35 W7 93.3(4) . . ? W4 O35 W11 93.2(4) . . ? W7 O35 W11 93.2(4) . . ? Si13 O35 W4 122.9(5) . . ? Si13 O35 W7 122.5(6) . . ? Si13 O35 W11 123.5(6) . . ? C29 C13 C20 117.1(16) . . ? C29 C13 C2 119.8(16) . . ? C20 C13 C2 123.0(17) . . ? C28 C14 C15 115.5(15) . . ? C14 C15 S1 115.5(11) . . ? C32 C15 C14 120.9(16) . . ? C32 C15 S1 123.6(14) . . ? C29 C17 C25 118.6(17) . . ? C28 C18 C36 122.6(19) . . ? C28 C18 C39 114.8(19) . . ? C36 C18 C39 122.6(19) . . ? C17 C25 S2 114.8(13) . . ? C17 C25 C16 122.4(15) . . ? C16 C25 S2 122.8(13) . . ? C18 C28 C14 124.3(17) . . ? C17 C29 C13 123.0(18) . . ? C15 S1 C1 104.2(9) . . ? C15 S1 C31 105.0(9) . . ? C1 S1 C31 98.7(9) . . ? C25 S2 C23 101.5(9) . . ? C25 S2 C40 105.8(10) . . ? C40 S2 C23 103.1(9) . . ? C20 C16 C25 116.5(15) . . ? C16 C20 C13 122.2(16) . . ? C37 C26 C27 121(2) . . ? C26 C27 S3 117.3(17) . . ? C26 C27 C6 121(2) . . ? C6 C27 S3 121.8(18) . . ? O1C C2 C13 127(2) . . ? C37 C30 C8 120(2) . . ? C3 C30 C37 120(2) . . ? C3 C30 C8 119.2(19) . . ? C15 C32 C36 120.3(16) . . ? C18 C36 C32 116.3(17) . . ? C26 C37 C30 122(2) . . ? O1E C39 C18 109(3) . . ? C27 S3 C4 105.6(10) . . ? C19 S3 C27 101.9(11) . . ? C19 S3 C4 98.3(13) . . ? C30 C3 C6 118(2) . . ? C11 C5 C24 124.9(19) . . ? C7 C22 C9 121(2) . . ? C27 C6 C3 117(2) . . ? C5 C24 C7 115(2) . . ? C5 C24 C12 122(2) . . ? C7 C24 C12 123.1(19) . . ? C22 C7 C24 122(2) . . ? O1D C8 C30 122.3(19) . . ? C9 S4 C10 106.1(10) . . ? C9 S4 C1A 103.2(10) . . ? C10 S4 C1A 101.0(9) . . ? C22 C9 S4 123.3(17) . . ? C11 C9 C22 118(2) . . ? C11 C9 S4 119.2(16) . . ? C5 C11 C9 120(2) . . ? O1F C12 C24 122(2) . . ? C1B N16 C1C 122(2) . . ? C1D N16 C1B 120(3) . . ? C1D N16 C1C 118(3) . . ? O1G C1D N16 121(4) . . ? C1G N1E C1F 118.4(19) . . ? C1G N1E C1E 119(2) . . ? C1E N1E C1F 123(2) . . ? O1H C1G N1E 127(3) . . ? 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 W1 O18 1.681(11) . ? W1 O13 1.918(12) . ? W1 O1 1.868(12) . ? W1 O19 1.912(11) . ? W1 O1A 1.885(13) . ? W1 O1B 2.375(10) . ? W2 O27 1.703(12) . ? W2 O15 1.889(11) . ? W2 O17 1.893(11) . ? W2 O20 2.374(13) . ? W2 O4 1.920(12) . ? W2 O32 1.909(12) . ? W3 O5 1.923(11) . ? W3 O2 1.932(12) . ? W3 O28 1.890(12) . ? W3 O29 2.372(11) . ? W3 O31 1.675(12) . ? W3 O34 1.922(12) . ? W4 O21 1.720(10) . ? W4 O8 1.913(11) . ? W4 O10 1.972(11) . ? W4 O14 1.879(12) . ? W4 O19 1.855(11) . ? W4 O35 2.340(11) . ? W5 O70 1.697(12) . ? W5 O15 1.880(11) . ? W5 O3 1.913(13) . ? W5 O1A 1.959(12) . ? W5 O1B 2.370(10) . ? W5 O33 1.860(11) . ? W6 O41 1.688(12) . ? W6 O9 1.917(11) . ? W6 O20 2.354(11) . ? W6 O4 1.914(12) . ? W6 O24 1.924(11) . ? W6 O6 1.916(12) . ? W7 O23 1.699(12) . ? W7 O8 1.976(10) . ? W7 O11 1.906(12) . ? W7 O12 1.910(12) . ? W7 O34 1.873(11) . ? W7 O35 2.350(11) . ? W8 O22 1.709(11) . ? W8 O5 1.945(12) . ? W8 O29 2.369(11) . ? W8 O30 1.896(13) . ? W8 O32 1.885(13) . ? W8 O33 1.931(11) . ? W9 O7 1.695(12) . ? W9 O11 1.885(11) . ? W9 O13 1.925(11) . ? W9 O3 1.921(12) . ? W9 O1B 2.343(11) . ? W9 O28 1.892(12) . ? W10 O57 1.684(10) . ? W10 O14 1.910(12) . ? W10 O17 1.959(11) . ? W10 O1 1.911(12) . ? W10 O20 2.401(10) . ? W10 O24 1.916(12) . ? W11 O26 1.711(11) . ? W11 O9 1.856(11) . ? W11 O10 1.889(12) . ? W11 O12 1.959(12) . ? W11 O16 1.912(11) . ? W11 O35 2.361(10) . ? W12 O25 1.694(11) . ? W12 O16 1.864(12) . ? W12 O2 1.933(13) . ? W12 O6 1.903(13) . ? W12 O29 2.368(10) . ? W12 O30 1.929(12) . ? Si13 O20 1.607(12) . ? Si13 O1B 1.618(12) . ? Si13 O29 1.606(11) . ? Si13 O35 1.645(12) . ? C13 C29 1.39(2) . ? C13 C20 1.41(2) . ? C13 C2 1.46(2) . ? C14 C15 1.43(2) . ? C14 C28 1.39(2) . ? C15 S1 1.751(16) . ? C15 C32 1.40(2) . ? C17 C25 1.38(2) . ? C17 C29 1.35(2) . ? C18 C28 1.32(2) . ? C18 C36 1.41(3) . ? C18 C39 1.58(3) . ? C25 S2 1.772(16) . ? C25 C16 1.41(2) . ? S1 C1 1.790(17) . ? S1 C31 1.808(17) . ? S2 C23 1.790(19) . ? S2 C40 1.786(18) . ? C16 C20 1.39(2) . ? C26 C27 1.34(3) . ? C26 C37 1.30(3) . ? C27 S3 1.75(2) . ? C27 C6 1.42(3) . ? O1C C2 1.16(2) . ? C30 C37 1.39(3) . ? C30 C3 1.36(3) . ? C30 C8 1.49(3) . ? C32 C36 1.43(3) . ? C39 O1E 1.25(3) . ? S3 C4 1.75(2) . ? S3 C19 1.74(3) . ? O1D C8 1.21(2) . ? C3 C6 1.44(3) . ? C5 C24 1.39(3) . ? C5 C11 1.38(3) . ? C22 C7 1.38(4) . ? C22 C9 1.44(3) . ? C24 C7 1.44(3) . ? C24 C12 1.46(3) . ? S4 C9 1.71(3) . ? S4 C10 1.781(16) . ? S4 C1A 1.820(19) . ? C9 C11 1.40(2) . ? O1F C12 1.22(3) . ? N16 C1B 1.40(3) . ? N16 C1C 1.42(3) . ? N16 C1D 1.36(4) . ? O1G C1D 1.25(4) . ? N1E C1F 1.45(2) . ? N1E C1G 1.33(3) . ? N1E C1E 1.42(3) . ? C1G O1H 1.21(3) . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.9946 -15.9995 18.0032 0.0532 0.2286 -0.9642 13.9974 1.9993 12.0030 -0.9778 0.1349 -0.2021 3.0053 15.9992 -17.0032 -0.2803 -0.2701 0.9233 18.0047 -2.0026 -13.0052 -0.6964 -0.7273 0.0246 15.9984 -10.0015 8.0001 -0.7274 -0.2219 -0.6418 -4.0046 16.0017 16.0071 -0.4320 0.8077 0.4170 -15.0029 16.0024 8.0054 0.2754 0.7700 0.6168 -19.0015 8.0023 2.0028 0.7766 0.5296 0.4114 -10.9953 9.0004 -18.0035 0.6457 -0.1726 0.7366 -1.9926 0.9988 -26.0075 0.4920 -0.6997 0.4857 -3.9953 17.0000 -16.0023 0.0492 -0.1008 0.9903 -16.0027 -5.9982 6.0020 0.8966 0.3524 -0.2498 16.0027 5.9982 -6.0020 -0.8966 -0.3524 0.2498 -12.9976 15.0012 -10.0002 0.4785 0.1970 0.8628 -3.0045 -16.9994 14.0021 0.3521 0.1662 -0.9146 -0.0062 10.0015 22.0079 -0.5916 0.8079 0.0459