#------------------------------------------------------------------------------ #$Date: 2019-06-05 03:19:39 +0300 (Wed, 05 Jun 2019) $ #$Revision: 215692 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551204.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_1551204 _journal_paper_doi 10.1039/C9SC01960J _chemical_formula_sum 'C52 H142 N7 Na O7 Si12 Th2' _chemical_formula_weight 1801.87 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-04-18 deposited with the CCDC. 2019-06-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.96(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.391(14) _cell_length_b 23.18(2) _cell_length_c 29.92(3) _cell_measurement_reflns_used 674 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 19.8 _cell_measurement_theta_min 2.74 _cell_volume 8593(15) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1747 _diffrn_reflns_av_unetI/netI 0.2616 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 31666 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 24.108 _diffrn_reflns_theta_max 24.108 _diffrn_reflns_theta_min 1.111 _exptl_absorpt_coefficient_mu 3.672 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_correction_T_min 0.5196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.393 _exptl_crystal_description block _exptl_crystal_F_000 3672 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _refine_diff_density_max 3.831 _refine_diff_density_min -2.354 _refine_diff_density_rms 0.250 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 360 _refine_ls_number_reflns 13515 _refine_ls_number_restraints 787 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.2320 _refine_ls_R_factor_gt 0.1190 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+321.6902P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1927 _refine_ls_wR_factor_ref 0.2259 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6493 _reflns_number_total 13515 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc01960j2.cif _cod_data_source_block complex_Na1 _cod_original_cell_volume 8593(16) _cod_database_code 1551204 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.527 _shelx_estimated_absorpt_t_max 0.838 _shelx_res_file ; SLS2135recry_0m_a.res created by SHELXL-2014/7 TITL twin4_a.res in P2(1)/c CELL 0.71073 12.3913 23.1761 29.9250 90.000 90.962 90.000 ZERR 4.000 0.0142 0.0247 0.0319 0.000 0.028 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C N O Na Si Th H UNIT 208 28 28 4 48 8 568 L.S. 10 SHEL 100 0.87 ACTA BOND $H FMAP 2 PLAN 20 size 0.2 0.1 0.05 eadp c49 c52 eadp c50 c51 sadi 0.01 Na1 O2 Na1 O3 Na1 O4 Na1 O5 Na1 O6 sadi 0.01 C37 C38 C39 C40 C41 C42 C43 C44 C45 C46 C47 C48 sadi 0.01 Si1 C1 Si11 C31 Si11 C32 Si11 C33 Si12 C34 Si12 C35 Si12 C36 sadi 0.01 Si1 C1 Si9 C25 Si9 C26 Si9 C27 Si10 C28 Si10 C29 Si10 C30 sadi 0.01 Si1 C1 Si7 C19 Si7 C20 Si7 C21 Si8 C22 Si8 C23 Si8 C24 sadi 0.01 Si1 C1 Si5 C13 Si5 C14 Si5 C15 Si6 C16 Si6 C17 Si6 C18 sadi 0.01 Si1 C1 Si3 C7 Si3 C8 Si3 C9 Si4 C10 Si4 C11 Si4 C12 sadi 0.01 Si1 C1 Si1 C2 Si1 C3 Si2 C4 Si2 C5 Si2 C6 eadp C37 C38 C39 C40 C41 C42 C43 C44 C45 C46 C47 C48 eadp C1 C33 C34 C35 C36 eadp C1 C19 C20 C21 C22 C23 C24 C25 C26 C27 C28 C29 C30 C31 C32 eadp C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 C17 C18 eadp Th1 N1 eadp N2 N3 N4 eadp N5 N6 N7 eadp o2 o3 o4 o5 o6 eadp Si1 Si2 Si3 Si4 Si5 Si6 Si7 Si8 Si9 Si10 Si11 Si12 sadi 0.01 O2 C37 O6 C45 O7 C46 O7 C47 O2 C48 sadi 0.01 O2 C37 O3 C38 O3 C39 O4 C40 O4 C41 O5 C42 O5 C43 O6 C44 sadi 0.01 N2 Si1 N2 Si2 N3 Si3 N3 Si4 N4 Si5 N4 Si6 sadi 0.01 N2 Si1 N5 Si7 N5 Si8 N6 Si9 N6 Si10 N7 Si11 N7 Si12 TEMP -173.020 WGHT 0.021800 321.690216 FVAR 0.09902 MOLE 1 C1 1 0.923378 0.926183 0.741283 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H1A 7 0.916244 0.910200 0.771408 11.00000 -1.50000 H1B 7 0.969713 0.960433 0.742517 11.00000 -1.50000 H1C 7 0.955622 0.897192 0.721756 11.00000 -1.50000 AFIX 0 C2 1 0.809158 0.994449 0.669940 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H2A 7 0.828470 0.971028 0.644007 11.00000 -1.50000 H2B 7 0.867830 1.021504 0.676932 11.00000 -1.50000 H2C 7 0.742907 1.016052 0.663138 11.00000 -1.50000 AFIX 0 C3 1 0.724246 0.995400 0.760546 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H3A 7 0.651503 1.006137 0.750229 11.00000 -1.50000 H3B 7 0.768378 1.030244 0.764075 11.00000 -1.50000 H3C 7 0.719928 0.975418 0.789322 11.00000 -1.50000 AFIX 0 C4 1 0.586619 0.784047 0.727569 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H4A 7 0.546585 0.789228 0.699332 11.00000 -1.50000 H4B 7 0.538413 0.768125 0.750082 11.00000 -1.50000 H4C 7 0.646902 0.757433 0.723019 11.00000 -1.50000 AFIX 0 C5 1 0.719642 0.844370 0.799813 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H5A 7 0.779319 0.817681 0.794332 11.00000 -1.50000 H5B 7 0.672969 0.828287 0.822811 11.00000 -1.50000 H5C 7 0.748621 0.881542 0.810002 11.00000 -1.50000 AFIX 0 C6 1 0.518071 0.896700 0.763886 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H6A 7 0.472255 0.904117 0.737497 11.00000 -1.50000 H6B 7 0.540655 0.933476 0.777227 11.00000 -1.50000 H6C 7 0.477422 0.874388 0.785753 11.00000 -1.50000 AFIX 0 C7 1 0.993868 0.819311 0.641851 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H7A 7 0.948976 0.828106 0.667628 11.00000 -1.50000 H7B 7 1.069490 0.816041 0.651640 11.00000 -1.50000 H7C 7 0.970253 0.782779 0.628406 11.00000 -1.50000 AFIX 0 C8 1 1.055794 0.861507 0.548071 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H8A 7 1.014814 0.833563 0.530003 11.00000 -1.50000 H8B 7 1.126422 0.845184 0.556151 11.00000 -1.50000 H8C 7 1.065820 0.896999 0.530830 11.00000 -1.50000 AFIX 0 C9 1 1.054493 0.939589 0.626412 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H9A 7 1.053508 0.972761 0.606100 11.00000 -1.50000 H9B 7 1.129353 0.928144 0.632701 11.00000 -1.50000 H9C 7 1.019583 0.950134 0.654398 11.00000 -1.50000 AFIX 0 C10 1 0.816561 0.903618 0.489757 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H10A 7 0.890685 0.892540 0.482719 11.00000 -1.50000 H10B 7 0.789315 0.930794 0.467157 11.00000 -1.50000 H10C 7 0.770687 0.869175 0.489898 11.00000 -1.50000 AFIX 0 C11 1 0.905635 1.002694 0.545424 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H11A 7 0.875261 1.032128 0.525346 11.00000 -1.50000 H11B 7 0.976990 0.991164 0.534967 11.00000 -1.50000 H11C 7 0.912424 1.018486 0.575720 11.00000 -1.50000 AFIX 0 C12 1 0.677895 0.970546 0.552714 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H12A 7 0.644606 0.977187 0.523224 11.00000 -1.50000 H12B 7 0.684308 1.007301 0.568730 11.00000 -1.50000 H12C 7 0.632889 0.943983 0.569781 11.00000 -1.50000 AFIX 0 C13 1 0.373416 0.787909 0.550675 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H13A 7 0.316205 0.817105 0.550661 11.00000 -1.50000 H13B 7 0.369314 0.764601 0.577918 11.00000 -1.50000 H13C 7 0.364243 0.762931 0.524461 11.00000 -1.50000 AFIX 0 C14 1 0.613796 0.769990 0.536402 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H14A 7 0.684683 0.788750 0.537071 11.00000 -1.50000 H14B 7 0.600186 0.753379 0.506723 11.00000 -1.50000 H14C 7 0.612466 0.739303 0.558916 11.00000 -1.50000 AFIX 0 C15 1 0.503436 0.870983 0.497971 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H15A 7 0.464043 0.906584 0.504497 11.00000 -1.50000 H15B 7 0.466884 0.850416 0.473433 11.00000 -1.50000 H15C 7 0.577258 0.880503 0.489322 11.00000 -1.50000 AFIX 0 C16 1 0.504289 0.966439 0.652109 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H16A 7 0.546709 0.950306 0.677059 11.00000 -1.50000 H16B 7 0.446663 0.990850 0.663785 11.00000 -1.50000 H16C 7 0.551302 0.989629 0.633173 11.00000 -1.50000 AFIX 0 C17 1 0.349452 0.867124 0.655636 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H17A 7 0.294825 0.847061 0.637382 11.00000 -1.50000 H17B 7 0.313973 0.894668 0.675431 11.00000 -1.50000 H17C 7 0.390041 0.838942 0.673630 11.00000 -1.50000 AFIX 0 C18 1 0.357932 0.943856 0.575520 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H18A 7 0.404194 0.963071 0.553838 11.00000 -1.50000 H18B 7 0.312465 0.972600 0.590121 11.00000 -1.50000 H18C 7 0.312067 0.915489 0.560060 11.00000 -1.50000 AFIX 0 C19 1 0.991781 0.546708 0.673534 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H19A 7 0.968646 0.565324 0.701174 11.00000 -1.50000 H19B 7 1.045902 0.517125 0.680653 11.00000 -1.50000 H19C 7 0.929395 0.528716 0.658569 11.00000 -1.50000 AFIX 0 C20 1 1.137129 0.557682 0.598219 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H20A 7 1.092002 0.541136 0.574258 11.00000 -1.50000 H20B 7 1.171421 0.526516 0.615436 11.00000 -1.50000 H20C 7 1.192901 0.582169 0.585204 11.00000 -1.50000 AFIX 0 C21 1 1.148712 0.646313 0.669357 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H21A 7 1.179132 0.676480 0.650385 11.00000 -1.50000 H21B 7 1.206974 0.621635 0.680957 11.00000 -1.50000 H21C 7 1.111082 0.664183 0.694358 11.00000 -1.50000 AFIX 0 C22 1 0.994401 0.618269 0.511288 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H22A 7 1.066771 0.601217 0.511253 11.00000 -1.50000 H22B 7 0.980350 0.637677 0.482682 11.00000 -1.50000 H22C 7 0.940678 0.587818 0.515559 11.00000 -1.50000 AFIX 0 C23 1 0.878373 0.723343 0.538769 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H23A 7 0.807691 0.704537 0.540263 11.00000 -1.50000 H23B 7 0.891784 0.735187 0.507919 11.00000 -1.50000 H23C 7 0.879385 0.757368 0.558216 11.00000 -1.50000 AFIX 0 C24 1 1.117703 0.710470 0.559334 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H24A 7 1.114616 0.742083 0.581024 11.00000 -1.50000 H24B 7 1.132689 0.726132 0.529659 11.00000 -1.50000 H24C 7 1.175146 0.683532 0.568195 11.00000 -1.50000 AFIX 0 C25 1 0.971556 0.629972 0.780515 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H25A 7 0.949186 0.594030 0.794915 11.00000 -1.50000 H25B 7 1.007861 0.654827 0.802585 11.00000 -1.50000 H25C 7 1.021273 0.621146 0.756325 11.00000 -1.50000 AFIX 0 C26 1 0.769189 0.687042 0.806835 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H26A 7 0.730418 0.723210 0.801074 11.00000 -1.50000 H26B 7 0.817248 0.691802 0.832917 11.00000 -1.50000 H26C 7 0.717183 0.656195 0.812649 11.00000 -1.50000 AFIX 0 C27 1 0.905705 0.734656 0.731507 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H27A 7 0.847355 0.762672 0.726851 11.00000 -1.50000 H27B 7 0.937841 0.725172 0.702722 11.00000 -1.50000 H27C 7 0.961010 0.751249 0.751463 11.00000 -1.50000 AFIX 0 C28 1 0.570520 0.590564 0.753528 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H28A 7 0.575551 0.623876 0.773626 11.00000 -1.50000 H28B 7 0.539698 0.557725 0.769524 11.00000 -1.50000 H28C 7 0.524110 0.600223 0.727763 11.00000 -1.50000 AFIX 0 C29 1 0.772115 0.529017 0.780232 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H29A 7 0.841999 0.514132 0.770597 11.00000 -1.50000 H29B 7 0.725131 0.496698 0.788127 11.00000 -1.50000 H29C 7 0.782897 0.554018 0.806338 11.00000 -1.50000 AFIX 0 C30 1 0.691737 0.517962 0.687531 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H30A 7 0.644520 0.486526 0.697079 11.00000 -1.50000 H30B 7 0.762512 0.502278 0.679881 11.00000 -1.50000 H30C 7 0.659634 0.537077 0.661295 11.00000 -1.50000 AFIX 0 C31 1 0.497997 0.685557 0.644747 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H31A 7 0.427761 0.683473 0.659234 11.00000 -1.50000 H31B 7 0.501736 0.720896 0.626857 11.00000 -1.50000 H31C 7 0.555578 0.685927 0.667599 11.00000 -1.50000 AFIX 0 C32 1 0.444576 0.562154 0.637511 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H32A 7 0.440427 0.528045 0.618202 11.00000 -1.50000 H32B 7 0.371509 0.574631 0.645000 11.00000 -1.50000 H32C 7 0.484778 0.552585 0.665003 11.00000 -1.50000 AFIX 0 C33 1 0.433996 0.634078 0.555521 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H33A 7 0.479386 0.652547 0.533149 11.00000 -1.50000 H33B 7 0.372658 0.659204 0.562085 11.00000 -1.50000 H33C 7 0.407384 0.597093 0.543908 11.00000 -1.50000 AFIX 0 C34 1 0.808972 0.522508 0.572110 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H34A 7 0.865354 0.551807 0.576064 11.00000 -1.50000 H34B 7 0.828422 0.496432 0.547755 11.00000 -1.50000 H34C 7 0.801959 0.500396 0.599824 11.00000 -1.50000 AFIX 0 C35 1 0.584954 0.495183 0.555977 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H35A 7 0.582814 0.476921 0.585486 11.00000 -1.50000 H35B 7 0.610856 0.467274 0.534016 11.00000 -1.50000 H35C 7 0.512309 0.508128 0.547263 11.00000 -1.50000 AFIX 0 C36 1 0.678021 0.588823 0.500512 11.00000 0.01806 0.02822 = 0.05465 0.00538 -0.00069 0.00215 AFIX 137 H36A 7 0.616306 0.614868 0.496522 11.00000 -1.50000 H36B 7 0.672621 0.557327 0.478738 11.00000 -1.50000 H36C 7 0.745135 0.610240 0.495953 11.00000 -1.50000 AFIX 0 C37 1 0.934574 0.162015 0.585896 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H37A 7 0.950765 0.132071 0.563387 11.00000 -1.20000 H37B 7 0.924410 0.142972 0.615138 11.00000 -1.20000 AFIX 0 C38 1 1.022347 0.203922 0.588864 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H38A 7 1.090411 0.184535 0.597993 11.00000 -1.20000 H38B 7 1.032971 0.222493 0.559472 11.00000 -1.20000 AFIX 0 C39 1 1.049637 0.299588 0.615987 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H39A 7 1.037795 0.314730 0.585361 11.00000 -1.20000 H39B 7 1.128084 0.293886 0.621013 11.00000 -1.20000 AFIX 0 C40 1 1.007306 0.339887 0.648783 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H40A 7 1.013638 0.323629 0.679307 11.00000 -1.20000 H40B 7 1.047021 0.376925 0.647927 11.00000 -1.20000 AFIX 0 C41 1 0.837577 0.386370 0.664249 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H41A 7 0.764830 0.392372 0.650869 11.00000 -1.20000 H41B 7 0.874611 0.424216 0.664995 11.00000 -1.20000 AFIX 0 C42 1 0.825920 0.365797 0.709991 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H42A 7 0.897754 0.359011 0.723994 11.00000 -1.20000 H42B 7 0.787158 0.394728 0.728021 11.00000 -1.20000 AFIX 0 C43 1 0.763251 0.283665 0.749699 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H43A 7 0.725026 0.307154 0.772084 11.00000 -1.20000 H43B 7 0.837439 0.276027 0.760987 11.00000 -1.20000 AFIX 0 C44 1 0.705945 0.229461 0.741534 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H44A 7 0.702803 0.206933 0.769590 11.00000 -1.20000 H44B 7 0.631079 0.237624 0.731331 11.00000 -1.20000 AFIX 0 C45 1 0.715077 0.140338 0.703095 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H45A 7 0.684833 0.127248 0.731780 11.00000 -1.20000 H45B 7 0.771916 0.112753 0.694310 11.00000 -1.20000 AFIX 0 C46 1 0.630228 0.142128 0.668832 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H46A 7 0.604961 0.102400 0.662464 11.00000 -1.20000 H46B 7 0.568279 0.164541 0.680035 11.00000 -1.20000 AFIX 0 C47 1 0.704698 0.125767 0.597277 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H47A 7 0.643667 0.101589 0.586588 11.00000 -1.20000 H47B 7 0.759271 0.100377 0.611703 11.00000 -1.20000 AFIX 0 C48 1 0.752041 0.156624 0.559940 11.00000 0.02744 0.03480 = 0.05790 -0.00834 -0.00179 0.00497 AFIX 23 H48A 7 0.778056 0.128208 0.537891 11.00000 -1.20000 H48B 7 0.695376 0.180241 0.545071 11.00000 -1.20000 AFIX 0 C49 1 0.460651 0.258186 0.606827 11.00000 0.01560 0.06688 = 0.04525 -0.00131 0.00713 0.00404 AFIX 137 H49A 7 0.423564 0.277469 0.581797 11.00000 -1.50000 H49B 7 0.407582 0.246106 0.628868 11.00000 -1.50000 H49C 7 0.499155 0.224250 0.595800 11.00000 -1.50000 AFIX 0 C50 1 0.541905 0.300239 0.628877 11.00000 0.01494 0.04513 = 0.05469 0.00737 0.00244 0.02060 AFIX 23 H50A 7 0.510482 0.339510 0.629121 11.00000 -1.20000 H50B 7 0.555471 0.288411 0.660260 11.00000 -1.20000 AFIX 0 C51 1 0.633174 0.326057 0.563265 11.00000 0.01494 0.04513 = 0.05469 0.00737 0.00244 0.02060 AFIX 23 H51A 7 0.589303 0.361608 0.565503 11.00000 -1.20000 H51B 7 0.594363 0.298918 0.543134 11.00000 -1.20000 AFIX 0 C52 1 0.739486 0.340487 0.543903 11.00000 0.01560 0.06688 = 0.04525 -0.00131 0.00713 0.00404 AFIX 137 H52A 7 0.781846 0.305115 0.540400 11.00000 -1.50000 H52B 7 0.778340 0.367106 0.563888 11.00000 -1.50000 H52C 7 0.728377 0.358755 0.514651 11.00000 -1.50000 AFIX 0 N1 2 0.748269 0.752480 0.636786 11.00000 0.01363 0.01254 = 0.03159 0.00170 -0.00265 -0.00133 N2 2 0.714420 0.885569 0.705400 11.00000 0.01019 0.02829 = 0.04029 -0.00438 -0.00531 -0.00226 N3 2 0.846243 0.890258 0.587770 11.00000 0.01019 0.02829 = 0.04029 -0.00438 -0.00531 -0.00226 N4 2 0.538094 0.859730 0.597644 11.00000 0.01019 0.02829 = 0.04029 -0.00438 -0.00531 -0.00226 N5 2 0.955759 0.643848 0.609100 11.00000 0.01459 0.02482 = 0.04398 0.00213 -0.00874 0.00126 N6 2 0.778442 0.631023 0.716704 11.00000 0.01459 0.02482 = 0.04398 0.00213 -0.00874 0.00126 N7 2 0.649358 0.609875 0.597630 11.00000 0.01459 0.02482 = 0.04398 0.00213 -0.00874 0.00126 NA1 4 0.796525 0.254606 0.639062 11.00000 0.00446 0.02916 = 0.04969 -0.01094 -0.00268 -0.00249 O1 3 0.644576 0.301441 0.605100 11.00000 0.02662 0.03732 = 0.04572 -0.01143 -0.00860 0.01555 O2 3 0.839788 0.193365 0.573044 11.00000 0.01298 0.03236 = 0.05971 0.00322 -0.00229 -0.00423 O3 3 0.993379 0.246216 0.621403 11.00000 0.01298 0.03236 = 0.05971 0.00322 -0.00229 -0.00423 O4 3 0.896572 0.348104 0.636277 11.00000 0.01298 0.03236 = 0.05971 0.00322 -0.00229 -0.00423 O5 3 0.766019 0.313186 0.707811 11.00000 0.01298 0.03236 = 0.05971 0.00322 -0.00229 -0.00423 O6 3 0.760397 0.196832 0.708277 11.00000 0.01298 0.03236 = 0.05971 0.00322 -0.00229 -0.00423 O7 3 0.667659 0.167872 0.628468 11.00000 0.04250 0.02316 = 0.05081 0.00392 0.00809 0.00225 SI1 5 0.786938 0.946663 0.718687 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI2 5 0.639740 0.855027 0.747086 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI3 5 0.980357 0.878192 0.599844 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI4 5 0.814653 0.938519 0.545878 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI5 5 0.507481 0.824220 0.548745 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI6 5 0.443748 0.906549 0.618438 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI7 5 1.051605 0.601882 0.635823 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI8 5 0.985654 0.671740 0.557668 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI9 5 0.850400 0.667873 0.757146 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI10 5 0.708005 0.571272 0.733857 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI11 5 0.514982 0.621500 0.607699 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 SI12 5 0.678026 0.558448 0.558197 11.00000 0.01379 0.01866 = 0.04646 0.00148 -0.00203 -0.00004 TH1 6 0.712649 0.842701 0.632071 11.00000 0.01363 0.01254 = 0.03159 0.00170 -0.00265 -0.00133 TH2 6 0.781124 0.663405 0.640199 11.00000 0.01248 0.01289 = 0.03700 0.00226 -0.00325 -0.00217 HKLF 4 REM twin4_a.res in P2(1)/c REM R1 = 0.1190 for 6493 Fo > 4sig(Fo) and 0.2320 for all 13515 data REM 360 parameters refined using 787 restraints END WGHT 0.0246 311.7520 REM Highest difference peak 3.831, deepest hole -2.354, 1-sigma level 0.250 Q1 1 0.7068 0.8457 0.6691 11.00000 0.05 3.83 Q2 1 0.7118 0.8451 0.5955 11.00000 0.05 3.60 Q3 1 0.7800 0.6653 0.6047 11.00000 0.05 3.44 Q4 1 0.7784 0.6672 0.6796 11.00000 0.05 3.42 Q5 1 0.7136 0.8087 0.6307 11.00000 0.05 1.56 Q6 1 0.7819 0.6290 0.6406 11.00000 0.05 1.54 Q7 1 0.6762 0.1590 0.8074 11.00000 0.05 1.51 Q8 1 0.7213 0.8453 0.5580 11.00000 0.05 1.28 Q9 1 0.8545 0.4712 0.6503 11.00000 0.05 1.25 Q10 1 0.2666 0.8290 0.6817 11.00000 0.05 1.16 Q11 1 0.6498 1.0212 0.6326 11.00000 0.05 1.11 Q12 1 0.6189 0.8558 0.7065 11.00000 0.05 1.09 Q13 1 0.7078 0.8766 0.6323 11.00000 0.05 1.08 Q14 1 0.7269 1.0385 0.5789 11.00000 0.05 1.01 Q15 1 0.7978 0.6728 0.5660 11.00000 0.05 1.01 Q16 1 0.7496 0.6989 0.5375 11.00000 0.05 1.00 Q17 1 0.7741 0.7012 0.6412 11.00000 0.05 0.99 Q18 1 0.4567 0.9086 0.6492 11.00000 0.05 0.97 Q19 1 0.7086 0.5069 0.5994 11.00000 0.05 0.95 Q20 1 1.0479 0.6558 0.6788 11.00000 0.05 0.93 ; _shelx_res_checksum 90116 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp C1 C 0.9234(11) 0.9262(10) 0.7413(9) 0.0337(12) Uani 1 1 d D . H1A H 0.9162 0.9102 0.7714 0.050 Uiso 1 1 calc R U H1B H 0.9697 0.9604 0.7425 0.050 Uiso 1 1 calc R U H1C H 0.9556 0.8972 0.7218 0.050 Uiso 1 1 calc R U C2 C 0.8092(19) 0.9944(9) 0.6699(6) 0.0337(12) Uani 1 1 d D . H2A H 0.8285 0.9710 0.6440 0.050 Uiso 1 1 calc R U H2B H 0.8678 1.0215 0.6769 0.050 Uiso 1 1 calc R U H2C H 0.7429 1.0161 0.6631 0.050 Uiso 1 1 calc R U C3 C 0.7242(18) 0.9954(9) 0.7605(7) 0.0337(12) Uani 1 1 d D . H3A H 0.6515 1.0061 0.7502 0.050 Uiso 1 1 calc R U H3B H 0.7684 1.0302 0.7641 0.050 Uiso 1 1 calc R U H3C H 0.7199 0.9754 0.7893 0.050 Uiso 1 1 calc R U C4 C 0.5866(18) 0.7840(6) 0.7276(9) 0.0337(12) Uani 1 1 d D . H4A H 0.5466 0.7892 0.6993 0.050 Uiso 1 1 calc R U H4B H 0.5384 0.7681 0.7501 0.050 Uiso 1 1 calc R U H4C H 0.6469 0.7574 0.7230 0.050 Uiso 1 1 calc R U C5 C 0.7196(16) 0.8444(11) 0.7998(5) 0.0337(12) Uani 1 1 d D . H5A H 0.7793 0.8177 0.7943 0.050 Uiso 1 1 calc R U H5B H 0.6730 0.8283 0.8228 0.050 Uiso 1 1 calc R U H5C H 0.7486 0.8815 0.8100 0.050 Uiso 1 1 calc R U C6 C 0.5181(14) 0.8967(9) 0.7639(9) 0.0337(12) Uani 1 1 d D . H6A H 0.4723 0.9041 0.7375 0.050 Uiso 1 1 calc R U H6B H 0.5407 0.9335 0.7772 0.050 Uiso 1 1 calc R U H6C H 0.4774 0.8744 0.7858 0.050 Uiso 1 1 calc R U C7 C 0.994(2) 0.8193(8) 0.6419(7) 0.0337(12) Uani 1 1 d D . H7A H 0.9490 0.8281 0.6676 0.050 Uiso 1 1 calc R U H7B H 1.0695 0.8160 0.6516 0.050 Uiso 1 1 calc R U H7C H 0.9703 0.7828 0.6284 0.050 Uiso 1 1 calc R U C8 C 1.0558(18) 0.8615(10) 0.5481(6) 0.0337(12) Uani 1 1 d D . H8A H 1.0148 0.8336 0.5300 0.050 Uiso 1 1 calc R U H8B H 1.1264 0.8452 0.5562 0.050 Uiso 1 1 calc R U H8C H 1.0658 0.8970 0.5308 0.050 Uiso 1 1 calc R U C9 C 1.0545(18) 0.9396(8) 0.6264(8) 0.0337(12) Uani 1 1 d D . H9A H 1.0535 0.9728 0.6061 0.050 Uiso 1 1 calc R U H9B H 1.1294 0.9281 0.6327 0.050 Uiso 1 1 calc R U H9C H 1.0196 0.9501 0.6544 0.050 Uiso 1 1 calc R U C10 C 0.817(2) 0.9036(10) 0.4898(5) 0.0337(12) Uani 1 1 d D . H10A H 0.8907 0.8925 0.4827 0.050 Uiso 1 1 calc R U H10B H 0.7893 0.9308 0.4672 0.050 Uiso 1 1 calc R U H10C H 0.7707 0.8692 0.4899 0.050 Uiso 1 1 calc R U C11 C 0.9056(16) 1.0027(7) 0.5454(9) 0.0337(12) Uani 1 1 d D . H11A H 0.8753 1.0321 0.5253 0.050 Uiso 1 1 calc R U H11B H 0.9770 0.9912 0.5350 0.050 Uiso 1 1 calc R U H11C H 0.9124 1.0185 0.5757 0.050 Uiso 1 1 calc R U C12 C 0.6779(11) 0.9705(10) 0.5527(9) 0.0337(12) Uani 1 1 d D . H12A H 0.6446 0.9772 0.5232 0.050 Uiso 1 1 calc R U H12B H 0.6843 1.0073 0.5687 0.050 Uiso 1 1 calc R U H12C H 0.6329 0.9440 0.5698 0.050 Uiso 1 1 calc R U C13 C 0.3734(11) 0.7879(9) 0.5507(9) 0.0337(12) Uani 1 1 d D . H13A H 0.3162 0.8171 0.5507 0.050 Uiso 1 1 calc R U H13B H 0.3693 0.7646 0.5779 0.050 Uiso 1 1 calc R U H13C H 0.3642 0.7629 0.5245 0.050 Uiso 1 1 calc R U C14 C 0.6138(15) 0.7700(8) 0.5364(9) 0.0337(12) Uani 1 1 d D . H14A H 0.6847 0.7887 0.5371 0.050 Uiso 1 1 calc R U H14B H 0.6002 0.7534 0.5067 0.050 Uiso 1 1 calc R U H14C H 0.6125 0.7393 0.5589 0.050 Uiso 1 1 calc R U C15 C 0.503(2) 0.8710(9) 0.4980(6) 0.0337(12) Uani 1 1 d D . H15A H 0.4640 0.9066 0.5045 0.050 Uiso 1 1 calc R U H15B H 0.4669 0.8504 0.4734 0.050 Uiso 1 1 calc R U H15C H 0.5773 0.8805 0.4893 0.050 Uiso 1 1 calc R U C16 C 0.5043(18) 0.9664(8) 0.6521(8) 0.0337(12) Uani 1 1 d D . H16A H 0.5467 0.9503 0.6771 0.050 Uiso 1 1 calc R U H16B H 0.4467 0.9908 0.6638 0.050 Uiso 1 1 calc R U H16C H 0.5513 0.9896 0.6332 0.050 Uiso 1 1 calc R U C17 C 0.3495(16) 0.8671(9) 0.6556(8) 0.0337(12) Uani 1 1 d D . H17A H 0.2948 0.8471 0.6374 0.050 Uiso 1 1 calc R U H17B H 0.3140 0.8947 0.6754 0.050 Uiso 1 1 calc R U H17C H 0.3900 0.8389 0.6736 0.050 Uiso 1 1 calc R U C18 C 0.3579(17) 0.9439(10) 0.5755(7) 0.0337(12) Uani 1 1 d D . H18A H 0.4042 0.9631 0.5538 0.050 Uiso 1 1 calc R U H18B H 0.3125 0.9726 0.5901 0.050 Uiso 1 1 calc R U H18C H 0.3121 0.9155 0.5601 0.050 Uiso 1 1 calc R U C19 C 0.9918(18) 0.5467(8) 0.6735(8) 0.0337(12) Uani 1 1 d D . H19A H 0.9686 0.5653 0.7012 0.050 Uiso 1 1 calc R U H19B H 1.0459 0.5171 0.6807 0.050 Uiso 1 1 calc R U H19C H 0.9294 0.5287 0.6586 0.050 Uiso 1 1 calc R U C20 C 1.1371(17) 0.5577(9) 0.5982(7) 0.0337(12) Uani 1 1 d D . H20A H 1.0920 0.5411 0.5743 0.050 Uiso 1 1 calc R U H20B H 1.1714 0.5265 0.6154 0.050 Uiso 1 1 calc R U H20C H 1.1929 0.5822 0.5852 0.050 Uiso 1 1 calc R U C21 C 1.1487(16) 0.6463(9) 0.6694(8) 0.0337(12) Uani 1 1 d D . H21A H 1.1791 0.6765 0.6504 0.050 Uiso 1 1 calc R U H21B H 1.2070 0.6216 0.6810 0.050 Uiso 1 1 calc R U H21C H 1.1111 0.6642 0.6944 0.050 Uiso 1 1 calc R U C22 C 0.994(2) 0.6183(9) 0.5113(6) 0.0337(12) Uani 1 1 d D . H22A H 1.0668 0.6012 0.5113 0.050 Uiso 1 1 calc R U H22B H 0.9803 0.6377 0.4827 0.050 Uiso 1 1 calc R U H22C H 0.9407 0.5878 0.5156 0.050 Uiso 1 1 calc R U C23 C 0.8784(15) 0.7233(9) 0.5388(9) 0.0337(12) Uani 1 1 d D . H23A H 0.8077 0.7045 0.5403 0.050 Uiso 1 1 calc R U H23B H 0.8918 0.7352 0.5079 0.050 Uiso 1 1 calc R U H23C H 0.8794 0.7574 0.5582 0.050 Uiso 1 1 calc R U C24 C 1.1177(12) 0.7105(9) 0.5593(9) 0.0337(12) Uani 1 1 d D . H24A H 1.1146 0.7421 0.5810 0.050 Uiso 1 1 calc R U H24B H 1.1327 0.7261 0.5297 0.050 Uiso 1 1 calc R U H24C H 1.1751 0.6835 0.5682 0.050 Uiso 1 1 calc R U C25 C 0.9716(13) 0.6300(10) 0.7805(9) 0.0337(12) Uani 1 1 d D . H25A H 0.9492 0.5940 0.7949 0.050 Uiso 1 1 calc R U H25B H 1.0079 0.6548 0.8026 0.050 Uiso 1 1 calc R U H25C H 1.0213 0.6211 0.7563 0.050 Uiso 1 1 calc R U C26 C 0.7692(18) 0.6870(10) 0.8068(6) 0.0337(12) Uani 1 1 d D . H26A H 0.7304 0.7232 0.8011 0.050 Uiso 1 1 calc R U H26B H 0.8172 0.6918 0.8329 0.050 Uiso 1 1 calc R U H26C H 0.7172 0.6562 0.8126 0.050 Uiso 1 1 calc R U C27 C 0.9057(18) 0.7347(7) 0.7315(8) 0.0337(12) Uani 1 1 d D . H27A H 0.8474 0.7627 0.7269 0.050 Uiso 1 1 calc R U H27B H 0.9378 0.7252 0.7027 0.050 Uiso 1 1 calc R U H27C H 0.9610 0.7512 0.7515 0.050 Uiso 1 1 calc R U C28 C 0.5705(11) 0.5906(10) 0.7535(9) 0.0337(12) Uani 1 1 d D . H28A H 0.5756 0.6239 0.7736 0.050 Uiso 1 1 calc R U H28B H 0.5397 0.5577 0.7695 0.050 Uiso 1 1 calc R U H28C H 0.5241 0.6002 0.7278 0.050 Uiso 1 1 calc R U C29 C 0.7721(18) 0.5290(9) 0.7802(7) 0.0337(12) Uani 1 1 d D . H29A H 0.8420 0.5141 0.7706 0.050 Uiso 1 1 calc R U H29B H 0.7251 0.4967 0.7881 0.050 Uiso 1 1 calc R U H29C H 0.7829 0.5540 0.8063 0.050 Uiso 1 1 calc R U C30 C 0.692(2) 0.5180(9) 0.6875(6) 0.0337(12) Uani 1 1 d D . H30A H 0.6445 0.4865 0.6971 0.050 Uiso 1 1 calc R U H30B H 0.7625 0.5023 0.6799 0.050 Uiso 1 1 calc R U H30C H 0.6596 0.5371 0.6613 0.050 Uiso 1 1 calc R U C31 C 0.498(2) 0.6856(7) 0.6447(7) 0.0337(12) Uani 1 1 d D . H31A H 0.4278 0.6835 0.6592 0.050 Uiso 1 1 calc R U H31B H 0.5017 0.7209 0.6269 0.050 Uiso 1 1 calc R U H31C H 0.5556 0.6859 0.6676 0.050 Uiso 1 1 calc R U C32 C 0.4446(18) 0.5622(8) 0.6375(8) 0.0337(12) Uani 1 1 d D . H32A H 0.4404 0.5280 0.6182 0.050 Uiso 1 1 calc R U H32B H 0.3715 0.5746 0.6450 0.050 Uiso 1 1 calc R U H32C H 0.4848 0.5526 0.6650 0.050 Uiso 1 1 calc R U C33 C 0.4340(17) 0.6341(10) 0.5555(6) 0.0337(12) Uani 1 1 d D . H33A H 0.4794 0.6525 0.5331 0.050 Uiso 1 1 calc R U H33B H 0.3727 0.6592 0.5621 0.050 Uiso 1 1 calc R U H33C H 0.4074 0.5971 0.5439 0.050 Uiso 1 1 calc R U C34 C 0.8090(12) 0.5225(10) 0.5721(9) 0.0337(12) Uani 1 1 d D . H34A H 0.8654 0.5518 0.5761 0.050 Uiso 1 1 calc R U H34B H 0.8284 0.4964 0.5478 0.050 Uiso 1 1 calc R U H34C H 0.8020 0.5004 0.5998 0.050 Uiso 1 1 calc R U C35 C 0.5850(16) 0.4952(7) 0.5560(9) 0.0337(12) Uani 1 1 d D . H35A H 0.5828 0.4769 0.5855 0.050 Uiso 1 1 calc R U H35B H 0.6109 0.4673 0.5340 0.050 Uiso 1 1 calc R U H35C H 0.5123 0.5081 0.5473 0.050 Uiso 1 1 calc R U C36 C 0.678(2) 0.5888(10) 0.5005(5) 0.0337(12) Uani 1 1 d D . H36A H 0.6163 0.6149 0.4965 0.050 Uiso 1 1 calc R U H36B H 0.6726 0.5573 0.4787 0.050 Uiso 1 1 calc R U H36C H 0.7451 0.6102 0.4960 0.050 Uiso 1 1 calc R U C37 C 0.9346(14) 0.1620(9) 0.5859(9) 0.040(2) Uani 1 1 d D . H37A H 0.9508 0.1321 0.5634 0.048 Uiso 1 1 calc R U H37B H 0.9244 0.1430 0.6151 0.048 Uiso 1 1 calc R U C38 C 1.0223(18) 0.2039(9) 0.5889(8) 0.040(2) Uani 1 1 d D . H38A H 1.0904 0.1845 0.5980 0.048 Uiso 1 1 calc R U H38B H 1.0330 0.2225 0.5595 0.048 Uiso 1 1 calc R U C39 C 1.0496(19) 0.2996(7) 0.6160(9) 0.040(2) Uani 1 1 d D . H39A H 1.0378 0.3147 0.5854 0.048 Uiso 1 1 calc R U H39B H 1.1281 0.2939 0.6210 0.048 Uiso 1 1 calc R U C40 C 1.0073(13) 0.3399(11) 0.6488(8) 0.040(2) Uani 1 1 d D . H40A H 1.0136 0.3236 0.6793 0.048 Uiso 1 1 calc R U H40B H 1.0470 0.3769 0.6479 0.048 Uiso 1 1 calc R U C41 C 0.838(2) 0.3864(10) 0.6642(7) 0.040(2) Uani 1 1 d D . H41A H 0.7648 0.3924 0.6509 0.048 Uiso 1 1 calc R U H41B H 0.8746 0.4242 0.6650 0.048 Uiso 1 1 calc R U C42 C 0.826(2) 0.3658(8) 0.7100(8) 0.040(2) Uani 1 1 d D . H42A H 0.8978 0.3590 0.7240 0.048 Uiso 1 1 calc R U H42B H 0.7872 0.3947 0.7280 0.048 Uiso 1 1 calc R U C43 C 0.763(2) 0.2837(9) 0.7497(7) 0.040(2) Uani 1 1 d D . H43A H 0.7250 0.3072 0.7721 0.048 Uiso 1 1 calc R U H43B H 0.8374 0.2760 0.7610 0.048 Uiso 1 1 calc R U C44 C 0.7059(18) 0.2295(9) 0.7415(8) 0.040(2) Uani 1 1 d D . H44A H 0.7028 0.2069 0.7696 0.048 Uiso 1 1 calc R U H44B H 0.6311 0.2376 0.7313 0.048 Uiso 1 1 calc R U C45 C 0.7151(19) 0.1403(7) 0.7031(9) 0.040(2) Uani 1 1 d D . H45A H 0.6848 0.1272 0.7318 0.048 Uiso 1 1 calc R U H45B H 0.7719 0.1128 0.6943 0.048 Uiso 1 1 calc R U C46 C 0.6302(18) 0.1421(11) 0.6688(6) 0.040(2) Uani 1 1 d D . H46A H 0.6050 0.1024 0.6625 0.048 Uiso 1 1 calc R U H46B H 0.5683 0.1645 0.6800 0.048 Uiso 1 1 calc R U C47 C 0.705(2) 0.1258(9) 0.5973(7) 0.040(2) Uani 1 1 d D . H47A H 0.6437 0.1016 0.5866 0.048 Uiso 1 1 calc R U H47B H 0.7593 0.1004 0.6117 0.048 Uiso 1 1 calc R U C48 C 0.7520(16) 0.1566(10) 0.5599(8) 0.040(2) Uani 1 1 d D . H48A H 0.7781 0.1282 0.5379 0.048 Uiso 1 1 calc R U H48B H 0.6954 0.1802 0.5451 0.048 Uiso 1 1 calc R U C49 C 0.461(2) 0.2582(13) 0.6068(9) 0.043(5) Uani 1 1 d . . H49A H 0.4236 0.2775 0.5818 0.064 Uiso 1 1 calc R U H49B H 0.4076 0.2461 0.6289 0.064 Uiso 1 1 calc R U H49C H 0.4992 0.2243 0.5958 0.064 Uiso 1 1 calc R U C50 C 0.5419(19) 0.3002(11) 0.6289(10) 0.038(5) Uani 1 1 d . . H50A H 0.5105 0.3395 0.6291 0.046 Uiso 1 1 calc R U H50B H 0.5555 0.2884 0.6603 0.046 Uiso 1 1 calc R U C51 C 0.6332(19) 0.3261(12) 0.5633(10) 0.038(5) Uani 1 1 d . . H51A H 0.5893 0.3616 0.5655 0.046 Uiso 1 1 calc R U H51B H 0.5944 0.2989 0.5431 0.046 Uiso 1 1 calc R U C52 C 0.7395(18) 0.3405(14) 0.5439(9) 0.043(5) Uani 1 1 d . . H52A H 0.7818 0.3051 0.5404 0.064 Uiso 1 1 calc R U H52B H 0.7783 0.3671 0.5639 0.064 Uiso 1 1 calc R U H52C H 0.7284 0.3588 0.5147 0.064 Uiso 1 1 calc R U N1 N 0.7483(17) 0.7525(8) 0.6368(7) 0.0193(3) Uani 1 1 d . . N2 N 0.7144(12) 0.8856(6) 0.7054(5) 0.026(3) Uani 1 1 d D . N3 N 0.8462(9) 0.8903(7) 0.5878(5) 0.026(3) Uani 1 1 d D . N4 N 0.5381(11) 0.8597(6) 0.5976(4) 0.026(3) Uani 1 1 d D . N5 N 0.9558(11) 0.6438(7) 0.6091(4) 0.028(3) Uani 1 1 d D . N6 N 0.7784(13) 0.6310(5) 0.7167(5) 0.028(3) Uani 1 1 d D . N7 N 0.6494(9) 0.6099(7) 0.5976(5) 0.028(3) Uani 1 1 d D . Na1 Na 0.7965(7) 0.2546(3) 0.6391(3) 0.028(3) Uani 1 1 d D . O1 O 0.6446(14) 0.3014(7) 0.6051(7) 0.037(5) Uani 1 1 d . . O2 O 0.8398(11) 0.1934(6) 0.5730(5) 0.035(2) Uani 1 1 d D . O3 O 0.9934(9) 0.2462(6) 0.6214(6) 0.035(2) Uani 1 1 d D . O4 O 0.8966(10) 0.3481(5) 0.6363(6) 0.035(2) Uani 1 1 d D . O5 O 0.7660(12) 0.3132(6) 0.7078(5) 0.035(2) Uani 1 1 d D . O6 O 0.7604(12) 0.1968(6) 0.7083(5) 0.035(2) Uani 1 1 d D . O7 O 0.6677(14) 0.1679(7) 0.6285(6) 0.039(5) Uani 1 1 d D . Si1 Si 0.7869(5) 0.9467(3) 0.7187(3) 0.0263(6) Uani 1 1 d D . Si2 Si 0.6397(5) 0.8550(3) 0.7471(3) 0.0263(6) Uani 1 1 d D . Si3 Si 0.9804(5) 0.8782(3) 0.5998(3) 0.0263(6) Uani 1 1 d D . Si4 Si 0.8147(5) 0.9385(3) 0.5459(3) 0.0263(6) Uani 1 1 d D . Si5 Si 0.5075(5) 0.8242(3) 0.5487(3) 0.0263(6) Uani 1 1 d D . Si6 Si 0.4437(5) 0.9065(3) 0.6184(3) 0.0263(6) Uani 1 1 d D . Si7 Si 1.0516(5) 0.6019(3) 0.6358(3) 0.0263(6) Uani 1 1 d D . Si8 Si 0.9857(5) 0.6717(3) 0.5577(2) 0.0263(6) Uani 1 1 d D . Si9 Si 0.8504(5) 0.6679(3) 0.7571(2) 0.0263(6) Uani 1 1 d D . Si10 Si 0.7080(5) 0.5713(3) 0.7339(3) 0.0263(6) Uani 1 1 d D . Si11 Si 0.5150(5) 0.6215(3) 0.6077(3) 0.0263(6) Uani 1 1 d D . Si12 Si 0.6780(5) 0.5584(3) 0.5582(3) 0.0263(6) Uani 1 1 d D . Th1 Th 0.71265(7) 0.84270(4) 0.63207(3) 0.0193(3) Uani 1 1 d . . Th2 Th 0.78112(7) 0.66341(4) 0.64020(3) 0.0208(3) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C2 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C3 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C4 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C5 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C6 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C7 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C8 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C9 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C10 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C11 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C12 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C13 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C14 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C15 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C16 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C17 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C18 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C19 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C20 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C21 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C22 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C23 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C24 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C25 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C26 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C27 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C28 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C29 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C30 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C31 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C32 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C33 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C34 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C35 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C36 0.018(2) 0.028(2) 0.055(3) 0.005(2) -0.001(2) 0.0022(19) C37 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C38 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C39 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C40 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C41 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C42 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C43 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C44 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C45 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C46 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C47 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C48 0.027(5) 0.035(5) 0.058(6) -0.008(5) -0.002(4) 0.005(4) C49 0.016(10) 0.067(14) 0.045(14) -0.001(13) 0.007(10) 0.004(11) C50 0.015(10) 0.045(13) 0.055(16) 0.007(11) 0.002(10) 0.021(9) C51 0.015(10) 0.045(13) 0.055(16) 0.007(11) 0.002(10) 0.021(9) C52 0.016(10) 0.067(14) 0.045(14) -0.001(13) 0.007(10) 0.004(11) N1 0.0136(5) 0.0125(4) 0.0316(7) 0.0017(5) -0.0027(4) -0.0013(4) N2 0.010(6) 0.028(7) 0.040(9) -0.004(6) -0.005(6) -0.002(5) N3 0.010(6) 0.028(7) 0.040(9) -0.004(6) -0.005(6) -0.002(5) N4 0.010(6) 0.028(7) 0.040(9) -0.004(6) -0.005(6) -0.002(5) N5 0.015(7) 0.025(7) 0.044(9) 0.002(6) -0.009(6) 0.001(5) N6 0.015(7) 0.025(7) 0.044(9) 0.002(6) -0.009(6) 0.001(5) N7 0.015(7) 0.025(7) 0.044(9) 0.002(6) -0.009(6) 0.001(5) Na1 0.004(5) 0.029(5) 0.050(7) -0.011(5) -0.003(5) -0.002(4) O1 0.027(11) 0.037(11) 0.046(14) -0.011(10) -0.009(10) 0.016(9) O2 0.013(4) 0.032(4) 0.060(6) 0.003(5) -0.002(4) -0.004(3) O3 0.013(4) 0.032(4) 0.060(6) 0.003(5) -0.002(4) -0.004(3) O4 0.013(4) 0.032(4) 0.060(6) 0.003(5) -0.002(4) -0.004(3) O5 0.013(4) 0.032(4) 0.060(6) 0.003(5) -0.002(4) -0.004(3) O6 0.013(4) 0.032(4) 0.060(6) 0.003(5) -0.002(4) -0.004(3) O7 0.042(11) 0.023(10) 0.051(13) 0.004(10) 0.008(10) 0.002(9) Si1 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si2 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si3 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si4 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si5 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si6 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si7 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si8 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si9 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si10 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si11 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Si12 0.0138(10) 0.0187(10) 0.0465(16) 0.0015(10) -0.0020(10) 0.0000(8) Th1 0.0136(5) 0.0125(4) 0.0316(7) 0.0017(5) -0.0027(4) -0.0013(4) Th2 0.0125(5) 0.0129(4) 0.0370(7) 0.0023(5) -0.0033(5) -0.0022(4) 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' 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' Na Na 0.0362 0.0249 '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' Th Th -7.2400 8.8979 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Si1 C1 H1A 109.5 Si1 C1 H1B 109.5 H1A C1 H1B 109.5 Si1 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 Si1 C2 H2A 109.5 Si1 C2 H2B 109.5 H2A C2 H2B 109.5 Si1 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 Si1 C3 H3A 109.5 Si1 C3 H3B 109.5 H3A C3 H3B 109.5 Si1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 Si2 C4 H4A 109.5 Si2 C4 H4B 109.5 H4A C4 H4B 109.5 Si2 C4 H4C 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 Si2 C5 H5A 109.5 Si2 C5 H5B 109.5 H5A C5 H5B 109.5 Si2 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 Si2 C6 H6A 109.5 Si2 C6 H6B 109.5 H6A C6 H6B 109.5 Si2 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 Si3 C7 H7A 109.5 Si3 C7 H7B 109.5 H7A C7 H7B 109.5 Si3 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 Si3 C8 H8A 109.5 Si3 C8 H8B 109.5 H8A C8 H8B 109.5 Si3 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 Si3 C9 H9A 109.5 Si3 C9 H9B 109.5 H9A C9 H9B 109.5 Si3 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 Si4 C10 H10A 109.5 Si4 C10 H10B 109.5 H10A C10 H10B 109.5 Si4 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 Si4 C11 H11A 109.5 Si4 C11 H11B 109.5 H11A C11 H11B 109.5 Si4 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 Si4 C12 H12A 109.5 Si4 C12 H12B 109.5 H12A C12 H12B 109.5 Si4 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 Si5 C13 H13A 109.5 Si5 C13 H13B 109.5 H13A C13 H13B 109.5 Si5 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 Si5 C14 H14A 109.5 Si5 C14 H14B 109.5 H14A C14 H14B 109.5 Si5 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 Si5 C15 H15A 109.5 Si5 C15 H15B 109.5 H15A C15 H15B 109.5 Si5 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 Si6 C16 H16A 109.5 Si6 C16 H16B 109.5 H16A C16 H16B 109.5 Si6 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 Si6 C17 H17A 109.5 Si6 C17 H17B 109.5 H17A C17 H17B 109.5 Si6 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 Si6 C18 H18A 109.5 Si6 C18 H18B 109.5 H18A C18 H18B 109.5 Si6 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 Si7 C19 H19A 109.5 Si7 C19 H19B 109.5 H19A C19 H19B 109.5 Si7 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 Si7 C20 H20A 109.5 Si7 C20 H20B 109.5 H20A C20 H20B 109.5 Si7 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 Si7 C21 H21A 109.5 Si7 C21 H21B 109.5 H21A C21 H21B 109.5 Si7 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 Si8 C22 H22A 109.5 Si8 C22 H22B 109.5 H22A C22 H22B 109.5 Si8 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 Si8 C23 H23A 109.5 Si8 C23 H23B 109.5 H23A C23 H23B 109.5 Si8 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 Si8 C24 H24A 109.5 Si8 C24 H24B 109.5 H24A C24 H24B 109.5 Si8 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 Si9 C25 H25A 109.5 Si9 C25 H25B 109.5 H25A C25 H25B 109.5 Si9 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 Si9 C26 H26A 109.5 Si9 C26 H26B 109.5 H26A C26 H26B 109.5 Si9 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 Si9 C27 H27A 109.5 Si9 C27 H27B 109.5 H27A C27 H27B 109.5 Si9 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 Si10 C28 H28A 109.5 Si10 C28 H28B 109.5 H28A C28 H28B 109.5 Si10 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 Si10 C29 H29A 109.5 Si10 C29 H29B 109.5 H29A C29 H29B 109.5 Si10 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 Si10 C30 H30A 109.5 Si10 C30 H30B 109.5 H30A C30 H30B 109.5 Si10 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 Si11 C31 H31A 109.5 Si11 C31 H31B 109.5 H31A C31 H31B 109.5 Si11 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 Si11 C32 H32A 109.5 Si11 C32 H32B 109.5 H32A C32 H32B 109.5 Si11 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 Si11 C33 H33A 109.5 Si11 C33 H33B 109.5 H33A C33 H33B 109.5 Si11 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 Si12 C34 H34A 109.5 Si12 C34 H34B 109.5 H34A C34 H34B 109.5 Si12 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 Si12 C35 H35A 109.5 Si12 C35 H35B 109.5 H35A C35 H35B 109.5 Si12 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 Si12 C36 H36A 109.5 Si12 C36 H36B 109.5 H36A C36 H36B 109.5 Si12 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 O2 C37 C38 106.6(18) O2 C37 H37A 110.4 C38 C37 H37A 110.4 O2 C37 H37B 110.4 C38 C37 H37B 110.4 H37A C37 H37B 108.6 O3 C38 C37 107.6(18) O3 C38 H38A 110.2 C37 C38 H38A 110.2 O3 C38 H38B 110.2 C37 C38 H38B 110.2 H38A C38 H38B 108.5 O3 C39 C40 107.2(19) O3 C39 H39A 110.3 C40 C39 H39A 110.3 O3 C39 H39B 110.3 C40 C39 H39B 110.3 H39A C39 H39B 108.5 O4 C40 C39 105.3(18) O4 C40 H40A 110.7 C39 C40 H40A 110.7 O4 C40 H40B 110.7 C39 C40 H40B 110.7 H40A C40 H40B 108.8 O4 C41 C42 114(2) O4 C41 H41A 108.8 C42 C41 H41A 108.8 O4 C41 H41B 108.8 C42 C41 H41B 108.8 H41A C41 H41B 107.7 O5 C42 C41 107.2(19) O5 C42 H42A 110.3 C41 C42 H42A 110.3 O5 C42 H42B 110.3 C41 C42 H42B 110.3 H42A C42 H42B 108.5 O5 C43 C44 106.5(19) O5 C43 H43A 110.4 C44 C43 H43A 110.4 O5 C43 H43B 110.4 C44 C43 H43B 110.4 H43A C43 H43B 108.6 O6 C44 C43 109.7(19) O6 C44 H44A 109.7 C43 C44 H44A 109.7 O6 C44 H44B 109.7 C43 C44 H44B 109.7 H44A C44 H44B 108.2 O6 C45 C46 109.1(18) O6 C45 H45A 109.9 C46 C45 H45A 109.9 O6 C45 H45B 109.9 C46 C45 H45B 109.9 H45A C45 H45B 108.3 O7 C46 C45 111(2) O7 C46 H46A 109.3 C45 C46 H46A 109.3 O7 C46 H46B 109.3 C45 C46 H46B 109.3 H46A C46 H46B 108.0 O7 C47 C48 107.6(19) O7 C47 H47A 110.2 C48 C47 H47A 110.2 O7 C47 H47B 110.2 C48 C47 H47B 110.2 H47A C47 H47B 108.5 O2 C48 C47 113.3(19) O2 C48 H48A 108.9 C47 C48 H48A 108.9 O2 C48 H48B 108.9 C47 C48 H48B 108.9 H48A C48 H48B 107.7 C50 C49 H49A 109.5 C50 C49 H49B 109.5 H49A C49 H49B 109.5 C50 C49 H49C 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 O1 C50 C49 112(2) O1 C50 H50A 109.3 C49 C50 H50A 109.3 O1 C50 H50B 109.3 C49 C50 H50B 109.3 H50A C50 H50B 107.9 O1 C51 C52 112(2) O1 C51 H51A 109.3 C52 C51 H51A 109.3 O1 C51 H51B 109.3 C52 C51 H51B 109.3 H51A C51 H51B 108.0 C51 C52 H52A 109.5 C51 C52 H52B 109.5 H52A C52 H52B 109.5 C51 C52 H52C 109.5 H52A C52 H52C 109.5 H52B C52 H52C 109.5 Th2 N1 Th1 178.8(12) Si2 N2 Si1 117.2(8) Si2 N2 Th1 119.7(5) Si1 N2 Th1 123.2(6) Si3 N3 Si4 117.8(8) Si3 N3 Th1 118.8(6) Si4 N3 Th1 123.3(5) Si5 N4 Si6 118.0(8) Si5 N4 Th1 118.0(5) Si6 N4 Th1 124.0(6) Si8 N5 Si7 118.2(8) Si8 N5 Th2 118.9(5) Si7 N5 Th2 122.9(6) Si9 N6 Si10 116.7(8) Si9 N6 Th2 119.9(5) Si10 N6 Th2 123.3(6) Si12 N7 Si11 116.2(8) Si12 N7 Th2 125.2(5) Si11 N7 Th2 118.6(5) O1 Na1 O2 95.7(6) O1 Na1 O4 88.8(6) O2 Na1 O4 110.7(6) O1 Na1 O5 88.5(6) O2 Na1 O5 175.7(7) O4 Na1 O5 68.8(5) O1 Na1 O3 135.1(7) O2 Na1 O3 64.4(5) O4 Na1 O3 64.9(5) O5 Na1 O3 112.1(6) O1 Na1 O6 116.3(7) O2 Na1 O6 113.1(6) O4 Na1 O6 125.8(6) O5 Na1 O6 65.1(5) O3 Na1 O6 108.6(6) O1 Na1 O7 79.6(6) O2 Na1 O7 66.5(5) O4 Na1 O7 167.6(7) O5 Na1 O7 115.0(6) O3 Na1 O7 121.0(6) O6 Na1 O7 64.4(5) C51 O1 C50 111.8(19) C51 O1 Na1 130.0(15) C50 O1 Na1 118.0(15) C37 O2 C48 112.9(17) C37 O2 Na1 105.2(13) C48 O2 Na1 112.5(13) C39 O3 C38 112.8(16) C39 O3 Na1 115.7(12) C38 O3 Na1 116.8(12) C41 O4 C40 115.3(17) C41 O4 Na1 105.1(13) C40 O4 Na1 110.5(13) C42 O5 C43 112.9(16) C42 O5 Na1 114.6(13) C43 O5 Na1 117.9(13) C44 O6 C45 111.7(17) C44 O6 Na1 112.6(14) C45 O6 Na1 118.2(15) C47 O7 C46 112.2(18) C47 O7 Na1 114.0(14) C46 O7 Na1 115.4(14) N2 Si1 C2 113.2(10) N2 Si1 C3 115.6(10) C2 Si1 C3 103.6(11) N2 Si1 C1 109.9(10) C2 Si1 C1 106.9(12) C3 Si1 C1 107.1(12) N2 Si2 C4 109.2(10) N2 Si2 C5 112.6(10) C4 Si2 C5 109.2(12) N2 Si2 C6 115.4(11) C4 Si2 C6 105.0(11) C5 Si2 C6 105.1(12) N3 Si3 C7 109.7(9) N3 Si3 C8 110.9(11) C7 Si3 C8 111.6(11) N3 Si3 C9 115.7(10) C7 Si3 C9 103.5(12) C8 Si3 C9 105.2(12) N3 Si4 C12 112.0(10) N3 Si4 C10 111.6(11) C12 Si4 C10 107.3(12) N3 Si4 C11 113.2(10) C12 Si4 C11 103.5(11) C10 Si4 C11 108.8(12) N4 Si5 C14 110.2(10) N4 Si5 C13 112.0(11) C14 Si5 C13 109.6(11) N4 Si5 C15 114.7(11) C14 Si5 C15 103.9(12) C13 Si5 C15 106.0(12) N4 Si6 C16 113.3(9) N4 Si6 C18 115.2(10) C16 Si6 C18 104.3(11) N4 Si6 C17 110.1(10) C16 Si6 C17 107.0(12) C18 Si6 C17 106.4(12) N5 Si7 C21 111.8(10) N5 Si7 C20 115.1(10) C21 Si7 C20 105.1(12) N5 Si7 C19 112.9(9) C21 Si7 C19 108.2(12) C20 Si7 C19 102.9(11) N5 Si8 C22 115.7(11) N5 Si8 C24 111.1(11) C22 Si8 C24 106.1(12) N5 Si8 C23 110.5(10) C22 Si8 C23 104.5(12) C24 Si8 C23 108.6(11) N6 Si9 C27 108.2(10) N6 Si9 C26 113.6(10) C27 Si9 C26 109.7(11) N6 Si9 C25 115.8(11) C27 Si9 C25 104.3(11) C26 Si9 C25 104.8(12) N6 Si10 C29 115.7(10) N6 Si10 C30 111.1(10) C29 Si10 C30 104.2(12) N6 Si10 C28 111.8(10) C29 Si10 C28 105.7(12) C30 Si10 C28 107.8(12) N7 Si11 C32 115.5(10) N7 Si11 C33 112.8(11) C32 Si11 C33 105.5(12) N7 Si11 C31 110.4(9) C32 Si11 C31 104.1(12) C33 Si11 C31 108.0(12) N7 Si12 C36 112.2(11) N7 Si12 C34 110.2(10) C36 Si12 C34 111.2(12) N7 Si12 C35 115.8(10) C36 Si12 C35 105.9(12) C34 Si12 C35 101.1(11) N1 Th1 N3 109.9(7) N1 Th1 N2 110.1(7) N3 Th1 N2 108.5(5) N1 Th1 N4 111.7(7) N3 Th1 N4 108.1(5) N2 Th1 N4 108.4(5) N1 Th2 N7 110.6(7) N1 Th2 N6 110.2(7) N7 Th2 N6 108.9(5) N1 Th2 N5 109.8(7) N7 Th2 N5 107.7(5) N6 Th2 N5 109.6(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 Si1 1.871(8) C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 Si1 1.856(8) C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 C3 Si1 1.866(8) C3 H3A 0.9800 C3 H3B 0.9800 C3 H3C 0.9800 C4 Si2 1.862(8) C4 H4A 0.9800 C4 H4B 0.9800 C4 H4C 0.9800 C5 Si2 1.865(8) C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C6 Si2 1.867(8) C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 Si3 1.861(8) C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 Si3 1.863(8) C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 Si3 1.864(8) C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 Si4 1.865(8) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 Si4 1.867(8) C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 Si4 1.864(8) C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 Si5 1.864(8) C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 Si5 1.862(8) C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 Si5 1.866(8) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 Si6 1.865(8) C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 Si6 1.866(8) C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 Si6 1.866(8) C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 Si7 1.867(8) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 Si7 1.865(8) C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 Si7 1.864(8) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 Si8 1.865(8) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 Si8 1.869(8) C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 Si8 1.866(8) C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 Si9 1.865(8) C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 Si9 1.863(8) C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 Si9 1.863(8) C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 Si10 1.866(8) C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 Si10 1.865(8) C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C30 Si10 1.865(8) C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C31 Si11 1.867(8) C31 H31A 0.9800 C31 H31B 0.9800 C31 H31C 0.9800 C32 Si11 1.864(8) C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 C33 Si11 1.865(8) C33 H33A 0.9800 C33 H33B 0.9800 C33 H33C 0.9800 C34 Si12 1.865(8) C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 Si12 1.866(8) C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 Si12 1.864(8) C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C37 O2 1.428(10) C37 C38 1.460(15) C37 H37A 0.9900 C37 H37B 0.9900 C38 O3 1.432(10) C38 H38A 0.9900 C38 H38B 0.9900 C39 O3 1.430(10) C39 C40 1.459(15) C39 H39A 0.9900 C39 H39B 0.9900 C40 O4 1.429(10) C40 H40A 0.9900 C40 H40B 0.9900 C41 O4 1.429(10) C41 C42 1.459(15) C41 H41A 0.9900 C41 H41B 0.9900 C42 O5 1.428(10) C42 H42A 0.9900 C42 H42B 0.9900 C43 O5 1.429(10) C43 C44 1.462(15) C43 H43A 0.9900 C43 H43B 0.9900 C44 O6 1.428(10) C44 H44A 0.9900 C44 H44B 0.9900 C45 O6 1.432(10) C45 C46 1.457(15) C45 H45A 0.9900 C45 H45B 0.9900 C46 O7 1.431(10) C46 H46A 0.9900 C46 H46B 0.9900 C47 O7 1.431(10) C47 C48 1.458(15) C47 H47A 0.9900 C47 H47B 0.9900 C48 O2 1.431(10) C48 H48A 0.9900 C48 H48B 0.9900 C49 C50 1.54(4) C49 H49A 0.9800 C49 H49B 0.9800 C49 H49C 0.9800 C50 O1 1.47(3) C50 H50A 0.9900 C50 H50B 0.9900 C51 O1 1.38(3) C51 C52 1.49(3) C51 H51A 0.9900 C51 H51B 0.9900 C52 H52A 0.9800 C52 H52B 0.9800 C52 H52C 0.9800 N1 Th2 2.106(19) N1 Th1 2.141(19) N2 Si2 1.718(8) N2 Si1 1.720(8) N2 Th1 2.409(13) N3 Si3 1.718(8) N3 Si4 1.720(8) N3 Th1 2.405(13) N4 Si5 1.716(8) N4 Si6 1.719(8) N4 Th1 2.413(13) N5 Si8 1.716(8) N5 Si7 1.722(8) N5 Th2 2.413(13) N6 Si9 1.718(8) N6 Si10 1.720(8) N6 Th2 2.410(14) N7 Si12 1.719(8) N7 Si11 1.718(8) N7 Th2 2.400(13) Na1 O1 2.39(2) Na1 O2 2.498(10) Na1 O4 2.499(10) Na1 O5 2.499(10) Na1 O3 2.512(11) Na1 O6 2.513(10) Na1 O7 2.583(19)