data_6 _manchester_internal_diff_code ostl19 _manchester_internal_STL_name 68 _manchester_internal_STL_number THEW8 _manchester_internal_coll_client EW/STL _manchester_internal_coll_user EW _manchester_internal_coll_date 8/3/16 _manchester_internal_process_date 8/3/16 _manchester_internal_process_user EW _manchester_internal_solution_date 8/3/16 _manchester_internal_solution_user EW _manchester_internal_refinement_date 8/3/16 _manchester_internal_refinement_user EW _manchester_internal_validation_date 8/3/16 _manchester_internal_validation_user EW _manchester_internal_archive_date 9/3/16 _manchester_internal_archive_user AW _refine_special_details ; The isopropyl group at C1 is disordered over two orientations. The occupanices of the orientations were allowed to freely refine, converging at final ratio of 0.33:0.67. Chemically equivalent C-Si bond distances within all isopropyl silyl groups were restrained to be approximately equal. Similarity thermal restraints were applied to all carbon atoms in the isopropyl group centred at C1. Enhanced rigid bond restraints were applied to the Na(12-crown-4-)2 cation and the isopropyl group centred at C1. ; _vrf_PLAT910_6 ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min) 48 Note RESPONSE: Missing reflections at low angle are most likely obscured by the beam stop. ; _vrf_PLAT973_6 ; PROBLEM: Check Calcd Positive Residual Density on Th1 3.75 eA-3 RESPONSE: The residual density is close to a heavy atom. It is present despite applying the correct absorption correction and is of no chemical significance. ; _audit_creation_date 2016-03-08 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5155) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C66 H150 N8 P Si6 Th2, C16 H32 Na O8, 0.5 (C4 H10 O2)' _chemical_formula_sum 'C84 H187 N8 Na O9 P Si6 Th2' _chemical_formula_weight 2139.98 _chemical_melting_point ? _chemical_oxdiff_formula 'C66 H150 Th2 P Na N8 Si6' _chemical_oxdiff_usercomment ' ' 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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' _cell_length_a 23.1479(7) _cell_length_b 17.4133(5) _cell_length_c 26.4947(9) _cell_angle_alpha 90 _cell_angle_beta 103.615(4) _cell_angle_gamma 90 _cell_volume 10379.4(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 23080 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 29.0130 _cell_measurement_theta_min 3.5850 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 3.003 _exptl_absorpt_correction_T_max 0.779 _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) 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_absorpt_special_details ? _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 4436 _exptl_crystal_size_max 0.2178 _exptl_crystal_size_mid 0.1416 _exptl_crystal_size_min 0.1077 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_unetI/netI 0.1054 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 91450 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.682 _diffrn_reflns_theta_max 25.682 _diffrn_reflns_theta_min 3.374 _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1636 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 16.00 71.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 11.3799 19.0000 -90.0000 55 #__ type_ start__ end____ width___ exp.time_ 2 omega 39.00 101.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 11.3799 178.0000 0.0000 62 #__ type_ start__ end____ width___ exp.time_ 3 omega -67.00 34.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 11.3799 -77.0000 0.0000 101 #__ type_ start__ end____ width___ exp.time_ 4 omega -12.00 84.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 11.3799 57.0000 120.0000 96 #__ type_ start__ end____ width___ exp.time_ 5 omega -79.00 -54.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -11.8486 -178.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 6 omega 36.00 68.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -11.8486 -178.0000 -30.0000 32 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0261215000 _diffrn_orient_matrix_UB_12 0.0104367000 _diffrn_orient_matrix_UB_13 0.0187129000 _diffrn_orient_matrix_UB_21 0.0044607000 _diffrn_orient_matrix_UB_22 0.0311218000 _diffrn_orient_matrix_UB_23 -0.0159166000 _diffrn_orient_matrix_UB_31 -0.0170924000 _diffrn_orient_matrix_UB_32 0.0240954000 _diffrn_orient_matrix_UB_33 0.0124714000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 13798 _reflns_number_total 19666 _reflns_odcompleteness_completeness 99.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 2.613 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.170 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1067 _refine_ls_number_reflns 19666 _refine_ls_number_restraints 963 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0557 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+34.9565P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1075 _refine_ls_wR_factor_ref 0.1271 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C3-C1 \\sim C3A-C1A \\sim C2A-C1A \\sim C2-C1 \\sim C6-C4 \\sim C5-C4 \\sim C8-C7 \\sim C9-C7 \\sim C27-C26 ~ C28-C26 \\sim C24-C23 \\sim C25-C23 \\sim C31-C29 \\sim C30-C29 \\sim C36-C34 \\sim C35-C34 \\sim C38-C37 \\sim C39-C37 \\sim C42-C40 \\sim C41-C40 \\sim C57-C56 \\sim C58-C56 \\sim C60-C59 \\sim C61-C59 \\sim C53- C51 \\sim C52-C51 \\sim C49-C48 \\sim C50-C48 \\sim C46-C45 \\sim C47-C45 \\sim C13-C12 \\sim C14-C12 ~ C20-C18 \\sim C19-C18 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C1 \\sim C2 \\sim C3 \\sim C1A \\sim C2A \\sim C3A: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 4. Rigid body (RIGU) restrains Si1, C1, C2, C3, C1A, C2A, C3A, Na1, O1, O2, O3, O4, O5, O6, O7, O8, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79, C80, C81, C82 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)= Sof(H3AB)=Sof(H3AC)=1-FVAR(1) Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)= Sof(H3C)=FVAR(1) 6.a Ternary CH refined with riding coordinates: C4(H4), C7(H7), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26), C29(H29), C34(H34), C37(H37), C40(H40), C45(H45), C48(H48), C51(H51), C56(H56), C59(H59), C62(H62), C1(H1), C1A(H1A) 6.b Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A, H32B), C33(H33A,H33B), C43(H43A,H43B), C44(H44A,H44B), C54(H54A,H54B), C55(H55A,H55B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A, H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C84(H84A,H84B) 6.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A, H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C25(H25A,H25B, H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A, H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C46(H46A,H46B, H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A, H52B,H52C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C64(H64A,H64B, H64C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB, H3AC), C83(H83A,H83B,H83C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Th1 Th 0.64611(2) 0.14002(2) 0.72411(2) 0.02065(8) Uani 1 1 d . . . . . Th2 Th 0.83565(2) 0.32849(2) 0.80067(2) 0.02098(8) Uani 1 1 d . . . . . P1 P 0.73971(8) 0.23493(12) 0.76539(8) 0.0272(5) Uani 1 1 d . . . . . Si1 Si 0.59593(10) 0.23579(14) 0.59282(9) 0.0357(6) Uani 1 1 d . U . . . Si2 Si 0.74229(8) -0.03517(12) 0.73198(8) 0.0226(5) Uani 1 1 d . . . . . Si3 Si 0.56142(9) 0.17175(12) 0.82807(8) 0.0232(5) Uani 1 1 d . . . . . Si4 Si 0.84270(9) 0.30450(13) 0.94426(8) 0.0271(5) Uani 1 1 d . . . . . Si5 Si 0.75825(9) 0.49168(12) 0.71780(9) 0.0297(5) Uani 1 1 d . . . . . Si6 Si 0.95226(8) 0.22094(12) 0.75046(8) 0.0238(5) Uani 1 1 d . . . . . N1 N 0.5838(3) 0.1840(3) 0.6451(2) 0.0268(15) Uani 1 1 d . . . . . N2 N 0.6804(2) 0.0192(3) 0.7049(2) 0.0189(13) Uani 1 1 d . . . . . N3 N 0.5841(2) 0.1168(3) 0.7816(2) 0.0231(14) Uani 1 1 d . . . . . N4 N 0.5523(2) 0.0382(3) 0.6822(2) 0.0213(13) Uani 1 1 d . . . . . N5 N 0.8507(2) 0.3556(3) 0.8903(2) 0.0266(15) Uani 1 1 d . . . . . N6 N 0.8203(2) 0.4446(3) 0.7531(2) 0.0231(14) Uani 1 1 d . . . . . N7 N 0.9302(2) 0.2797(3) 0.7945(2) 0.0239(14) Uani 1 1 d . . . . . N8 N 0.9285(2) 0.4337(3) 0.8371(2) 0.0217(14) Uani 1 1 d . . . . . C4 C 0.5716(3) 0.1891(5) 0.5257(3) 0.041(2) Uani 1 1 d D . . . . H4 H 0.5840 0.2259 0.5012 0.049 Uiso 1 1 calc R . . . . C5 C 0.6016(4) 0.1132(5) 0.5185(3) 0.049(2) Uani 1 1 d D . . . . H5A H 0.6448 0.1202 0.5269 0.074 Uiso 1 1 calc GR . . . . H5B H 0.5880 0.0962 0.4824 0.074 Uiso 1 1 calc GR . . . . H5C H 0.5912 0.0744 0.5417 0.074 Uiso 1 1 calc GR . . . . C6 C 0.5044(4) 0.1782(7) 0.5047(4) 0.070(3) Uani 1 1 d D . . . . H6A H 0.4906 0.1357 0.5231 0.105 Uiso 1 1 calc GR . . . . H6B H 0.4961 0.1664 0.4675 0.105 Uiso 1 1 calc GR . . . . H6C H 0.4836 0.2254 0.5100 0.105 Uiso 1 1 calc GR . . . . C7 C 0.6788(3) 0.2516(5) 0.6064(3) 0.037(2) Uani 1 1 d D . . . . H7 H 0.6893 0.2872 0.6368 0.044 Uiso 1 1 calc R . . . . C8 C 0.6992(4) 0.2904(6) 0.5617(3) 0.051(3) Uani 1 1 d D . . . . H8A H 0.6919 0.2560 0.5316 0.076 Uiso 1 1 calc GR . . . . H8B H 0.7418 0.3019 0.5726 0.076 Uiso 1 1 calc GR . . . . H8C H 0.6769 0.3383 0.5523 0.076 Uiso 1 1 calc GR . . . . C9 C 0.7144(3) 0.1770(5) 0.6225(3) 0.038(2) Uani 1 1 d D . . . . H9A H 0.7309 0.1773 0.6601 0.057 Uiso 1 1 calc GR . . . . H9B H 0.7468 0.1739 0.6046 0.057 Uiso 1 1 calc GR . . . . H9C H 0.6880 0.1326 0.6130 0.057 Uiso 1 1 calc GR . . . . C10 C 0.5213(3) 0.1603(5) 0.6409(3) 0.0319(19) Uani 1 1 d . . . . . H10A H 0.4953 0.1851 0.6102 0.038 Uiso 1 1 calc R . . . . H10B H 0.5084 0.1773 0.6721 0.038 Uiso 1 1 calc R . . . . C11 C 0.5155(3) 0.0737(5) 0.6357(3) 0.0300(19) Uani 1 1 d . . . . . H11A H 0.4734 0.0584 0.6316 0.036 Uiso 1 1 calc R . . . . H11B H 0.5286 0.0563 0.6046 0.036 Uiso 1 1 calc R . . . . C12 C 0.7262(3) -0.1411(4) 0.7415(3) 0.0279(18) Uani 1 1 d D . . . . H12 H 0.7660 -0.1647 0.7559 0.033 Uiso 1 1 calc R . . . . C13 C 0.6994(3) -0.1882(4) 0.6931(3) 0.034(2) Uani 1 1 d D . . . . H13A H 0.6577 -0.1737 0.6799 0.051 Uiso 1 1 calc GR . . . . H13B H 0.7018 -0.2429 0.7020 0.051 Uiso 1 1 calc GR . . . . H13C H 0.7215 -0.1783 0.6665 0.051 Uiso 1 1 calc GR . . . . C14 C 0.6908(4) -0.1558(4) 0.7830(3) 0.036(2) Uani 1 1 d D . . . . H14A H 0.7090 -0.1272 0.8146 0.053 Uiso 1 1 calc GR . . . . H14B H 0.6914 -0.2108 0.7910 0.053 Uiso 1 1 calc GR . . . . H14C H 0.6497 -0.1389 0.7700 0.053 Uiso 1 1 calc GR . . . . C15 C 0.7776(3) 0.0071(4) 0.7978(3) 0.0268(17) Uani 1 1 d . . . . . H15 H 0.7979 0.0552 0.7906 0.032 Uiso 1 1 calc R . . . . C16 C 0.8263(3) -0.0432(4) 0.8311(3) 0.038(2) Uani 1 1 d . . . . . H16A H 0.8083 -0.0893 0.8421 0.056 Uiso 1 1 calc GR . . . . H16B H 0.8470 -0.0143 0.8618 0.056 Uiso 1 1 calc GR . . . . H16C H 0.8548 -0.0582 0.8107 0.056 Uiso 1 1 calc GR . . . . C17 C 0.7338(3) 0.0322(5) 0.8303(3) 0.036(2) Uani 1 1 d . . . . . H17A H 0.7180 0.0832 0.8190 0.054 Uiso 1 1 calc GR . . . . H17B H 0.7545 0.0341 0.8671 0.054 Uiso 1 1 calc GR . . . . H17C H 0.7010 -0.0047 0.8255 0.054 Uiso 1 1 calc GR . . . . C18 C 0.7995(3) -0.0306(5) 0.6908(3) 0.0316(19) Uani 1 1 d D . . . . H18 H 0.8197 0.0200 0.6998 0.038 Uiso 1 1 calc R . . . . C19 C 0.7749(3) -0.0272(5) 0.6324(3) 0.038(2) Uani 1 1 d D . . . . H19A H 0.7575 -0.0770 0.6200 0.057 Uiso 1 1 calc GR . . . . H19B H 0.8071 -0.0151 0.6154 0.057 Uiso 1 1 calc GR . . . . H19C H 0.7443 0.0127 0.6242 0.057 Uiso 1 1 calc GR . . . . C20 C 0.8496(3) -0.0893(5) 0.7032(3) 0.039(2) Uani 1 1 d D . . . . H20A H 0.8714 -0.0836 0.7395 0.058 Uiso 1 1 calc GR . . . . H20B H 0.8768 -0.0808 0.6804 0.058 Uiso 1 1 calc GR . . . . H20C H 0.8329 -0.1411 0.6976 0.058 Uiso 1 1 calc GR . . . . C21 C 0.6397(3) -0.0133(4) 0.6582(3) 0.0262(17) Uani 1 1 d . . . . . H21A H 0.6577 -0.0600 0.6471 0.031 Uiso 1 1 calc R . . . . H21B H 0.6337 0.0246 0.6295 0.031 Uiso 1 1 calc R . . . . C22 C 0.5803(3) -0.0334(4) 0.6691(3) 0.0231(17) Uani 1 1 d . . . . . H22A H 0.5544 -0.0578 0.6382 0.028 Uiso 1 1 calc R . . . . H22B H 0.5859 -0.0700 0.6985 0.028 Uiso 1 1 calc R . . . . C23 C 0.4767(3) 0.1637(4) 0.8190(3) 0.0289(18) Uani 1 1 d D . . . . H23 H 0.4670 0.1083 0.8115 0.035 Uiso 1 1 calc R . . . . C24 C 0.4412(3) 0.2080(5) 0.7717(3) 0.042(2) Uani 1 1 d D . . . . H24A H 0.4465 0.2633 0.7780 0.064 Uiso 1 1 calc GR . . . . H24B H 0.3990 0.1951 0.7660 0.064 Uiso 1 1 calc GR . . . . H24C H 0.4555 0.1940 0.7409 0.064 Uiso 1 1 calc GR . . . . C25 C 0.4524(4) 0.1833(5) 0.8667(3) 0.043(2) Uani 1 1 d D . . . . H25A H 0.4725 0.1516 0.8962 0.064 Uiso 1 1 calc GR . . . . H25B H 0.4096 0.1731 0.8588 0.064 Uiso 1 1 calc GR . . . . H25C H 0.4596 0.2377 0.8754 0.064 Uiso 1 1 calc GR . . . . C26 C 0.5862(3) 0.2732(4) 0.8213(3) 0.0320(19) Uani 1 1 d D . . . . H26 H 0.6306 0.2717 0.8311 0.038 Uiso 1 1 calc R . . . . C27 C 0.5695(3) 0.3074(5) 0.7665(3) 0.040(2) Uani 1 1 d D . . . . H27A H 0.5783 0.2701 0.7416 0.061 Uiso 1 1 calc GR . . . . H27B H 0.5924 0.3544 0.7654 0.061 Uiso 1 1 calc GR . . . . H27C H 0.5269 0.3195 0.7573 0.061 Uiso 1 1 calc GR . . . . C28 C 0.5683(4) 0.3287(4) 0.8597(3) 0.038(2) Uani 1 1 d D . . . . H28A H 0.5249 0.3340 0.8514 0.058 Uiso 1 1 calc GR . . . . H28B H 0.5864 0.3791 0.8572 0.058 Uiso 1 1 calc GR . . . . H28C H 0.5820 0.3088 0.8951 0.058 Uiso 1 1 calc GR . . . . C29 C 0.5947(3) 0.1406(4) 0.8973(3) 0.0322(19) Uani 1 1 d D . . . . H29 H 0.5748 0.1717 0.9200 0.039 Uiso 1 1 calc R . . . . C30 C 0.5839(4) 0.0565(5) 0.9081(4) 0.052(3) Uani 1 1 d D . . . . H30A H 0.5413 0.0453 0.8969 0.078 Uiso 1 1 calc GR . . . . H30B H 0.5976 0.0464 0.9454 0.078 Uiso 1 1 calc GR . . . . H30C H 0.6057 0.0237 0.8890 0.078 Uiso 1 1 calc GR . . . . C31 C 0.6616(3) 0.1578(6) 0.9149(3) 0.047(2) Uani 1 1 d D . . . . H31A H 0.6826 0.1327 0.8913 0.071 Uiso 1 1 calc GR . . . . H31B H 0.6769 0.1383 0.9502 0.071 Uiso 1 1 calc GR . . . . H31C H 0.6680 0.2134 0.9144 0.071 Uiso 1 1 calc GR . . . . C32 C 0.5604(3) 0.0374(4) 0.7756(3) 0.0267(18) Uani 1 1 d . . . . . H32A H 0.5387 0.0270 0.8030 0.032 Uiso 1 1 calc R . . . . H32B H 0.5938 0.0006 0.7801 0.032 Uiso 1 1 calc R . . . . C33 C 0.5194(3) 0.0257(4) 0.7234(3) 0.0238(17) Uani 1 1 d . . . . . H33A H 0.5031 -0.0271 0.7208 0.029 Uiso 1 1 calc R . . . . H33B H 0.4857 0.0622 0.7187 0.029 Uiso 1 1 calc R . . . . C34 C 0.9109(3) 0.3028(5) 1.0018(3) 0.039(2) Uani 1 1 d D . . . . H34 H 0.8967 0.2782 1.0307 0.046 Uiso 1 1 calc R . . . . C35 C 0.9612(3) 0.2505(5) 0.9931(4) 0.049(2) Uani 1 1 d D . . . . H35A H 0.9462 0.1980 0.9863 0.074 Uiso 1 1 calc GR . . . . H35B H 0.9940 0.2510 1.0242 0.074 Uiso 1 1 calc GR . . . . H35C H 0.9754 0.2692 0.9633 0.074 Uiso 1 1 calc GR . . . . C36 C 0.9385(4) 0.3796(5) 1.0242(3) 0.048(2) Uani 1 1 d D . . . . H36A H 0.9575 0.4045 0.9992 0.072 Uiso 1 1 calc GR . . . . H36B H 0.9682 0.3701 1.0567 0.072 Uiso 1 1 calc GR . . . . H36C H 0.9073 0.4132 1.0312 0.072 Uiso 1 1 calc GR . . . . C37 C 0.7770(3) 0.3400(5) 0.9697(3) 0.034(2) Uani 1 1 d D . . . . H37 H 0.7606 0.2935 0.9836 0.041 Uiso 1 1 calc R . . . . C38 C 0.7882(4) 0.3984(5) 1.0136(4) 0.050(3) Uani 1 1 d D . . . . H38A H 0.8061 0.4446 1.0027 0.075 Uiso 1 1 calc GR . . . . H38B H 0.8152 0.3764 1.0443 0.075 Uiso 1 1 calc GR . . . . H38C H 0.7504 0.4118 1.0220 0.075 Uiso 1 1 calc GR . . . . C39 C 0.7273(3) 0.3695(6) 0.9253(3) 0.051(3) Uani 1 1 d D . . . . H39A H 0.7405 0.4162 0.9108 0.076 Uiso 1 1 calc GR . . . . H39B H 0.6920 0.3809 0.9384 0.076 Uiso 1 1 calc GR . . . . H39C H 0.7175 0.3301 0.8981 0.076 Uiso 1 1 calc GR . . . . C40 C 0.8236(3) 0.2020(4) 0.9227(3) 0.0307(19) Uani 1 1 d D . . . . H40 H 0.7823 0.2039 0.9004 0.037 Uiso 1 1 calc R . . . . C41 C 0.8620(4) 0.1673(5) 0.8888(3) 0.039(2) Uani 1 1 d D . . . . H41A H 0.8437 0.1778 0.8522 0.058 Uiso 1 1 calc GR . . . . H41B H 0.8651 0.1117 0.8944 0.058 Uiso 1 1 calc GR . . . . H41C H 0.9018 0.1902 0.8981 0.058 Uiso 1 1 calc GR . . . . C42 C 0.8208(4) 0.1480(5) 0.9683(3) 0.045(2) Uani 1 1 d D . . . . H42A H 0.8609 0.1399 0.9898 0.067 Uiso 1 1 calc GR . . . . H42B H 0.8037 0.0986 0.9546 0.067 Uiso 1 1 calc GR . . . . H42C H 0.7959 0.1713 0.9894 0.067 Uiso 1 1 calc GR . . . . C43 C 0.8675(3) 0.4372(4) 0.9004(3) 0.0283(18) Uani 1 1 d . . . . . H43A H 0.8672 0.4507 0.9367 0.034 Uiso 1 1 calc R . . . . H43B H 0.8387 0.4707 0.8769 0.034 Uiso 1 1 calc R . . . . C44 C 0.9300(3) 0.4493(5) 0.8914(3) 0.033(2) Uani 1 1 d . . . . . H44A H 0.9430 0.5029 0.9001 0.039 Uiso 1 1 calc R . . . . H44B H 0.9586 0.4144 0.9140 0.039 Uiso 1 1 calc R . . . . C45 C 1.0175(3) 0.2668(4) 0.7279(3) 0.0306(19) Uani 1 1 d D . . . . H45 H 1.0451 0.2867 0.7601 0.037 Uiso 1 1 calc R . . . . C46 C 1.0012(3) 0.3360(5) 0.6922(3) 0.040(2) Uani 1 1 d D . . . . H46A H 0.9782 0.3189 0.6581 0.059 Uiso 1 1 calc GR . . . . H46B H 1.0376 0.3615 0.6882 0.059 Uiso 1 1 calc GR . . . . H46C H 0.9774 0.3720 0.7073 0.059 Uiso 1 1 calc GR . . . . C47 C 1.0548(4) 0.2112(5) 0.7033(4) 0.047(2) Uani 1 1 d D . . . . H47A H 1.0691 0.1690 0.7275 0.070 Uiso 1 1 calc GR . . . . H47B H 1.0888 0.2388 0.6959 0.070 Uiso 1 1 calc GR . . . . H47C H 1.0302 0.1905 0.6709 0.070 Uiso 1 1 calc GR . . . . C48 C 0.9815(3) 0.1249(4) 0.7781(3) 0.0291(19) Uani 1 1 d D . . . . H48 H 0.9960 0.0979 0.7501 0.035 Uiso 1 1 calc R . . . . C49 C 1.0346(3) 0.1283(5) 0.8255(3) 0.040(2) Uani 1 1 d D . . . . H49A H 1.0650 0.1629 0.8182 0.060 Uiso 1 1 calc GR . . . . H49B H 1.0515 0.0767 0.8329 0.060 Uiso 1 1 calc GR . . . . H49C H 1.0212 0.1472 0.8557 0.060 Uiso 1 1 calc GR . . . . C50 C 0.9334(3) 0.0734(5) 0.7914(4) 0.043(2) Uani 1 1 d D . . . . H50A H 0.9198 0.0957 0.8204 0.064 Uiso 1 1 calc GR . . . . H50B H 0.9499 0.0222 0.8011 0.064 Uiso 1 1 calc GR . . . . H50C H 0.8999 0.0692 0.7610 0.064 Uiso 1 1 calc GR . . . . C51 C 0.8854(3) 0.2025(4) 0.6955(3) 0.0318(19) Uani 1 1 d D . . . . H51 H 0.8551 0.1779 0.7116 0.038 Uiso 1 1 calc R . . . . C52 C 0.8973(4) 0.1453(6) 0.6556(3) 0.054(3) Uani 1 1 d D . . . . H52A H 0.9195 0.1707 0.6331 0.081 Uiso 1 1 calc GR . . . . H52B H 0.8595 0.1261 0.6346 0.081 Uiso 1 1 calc GR . . . . H52C H 0.9207 0.1022 0.6736 0.081 Uiso 1 1 calc GR . . . . C53 C 0.8562(3) 0.2762(5) 0.6690(3) 0.042(2) Uani 1 1 d D . . . . H53A H 0.8558 0.3155 0.6954 0.063 Uiso 1 1 calc GR . . . . H53B H 0.8154 0.2649 0.6501 0.063 Uiso 1 1 calc GR . . . . H53C H 0.8789 0.2951 0.6447 0.063 Uiso 1 1 calc GR . . . . C54 C 0.9783(3) 0.3098(4) 0.8364(3) 0.0279(18) Uani 1 1 d . . . . . H54A H 1.0162 0.2848 0.8348 0.034 Uiso 1 1 calc R . . . . H54B H 0.9699 0.2975 0.8705 0.034 Uiso 1 1 calc R . . . . C55 C 0.9842(3) 0.3972(4) 0.8314(3) 0.0274(18) Uani 1 1 d . . . . . H55A H 1.0180 0.4164 0.8586 0.033 Uiso 1 1 calc R . . . . H55B H 0.9916 0.4101 0.7970 0.033 Uiso 1 1 calc R . . . . C56 C 0.7615(3) 0.6016(4) 0.7227(3) 0.033(2) Uani 1 1 d D . . . . H56 H 0.7199 0.6187 0.7073 0.040 Uiso 1 1 calc R . . . . C57 C 0.7749(4) 0.6310(5) 0.7785(3) 0.046(2) Uani 1 1 d D . . . . H57A H 0.7466 0.6084 0.7966 0.069 Uiso 1 1 calc GR . . . . H57B H 0.7712 0.6870 0.7783 0.069 Uiso 1 1 calc GR . . . . H57C H 0.8154 0.6163 0.7963 0.069 Uiso 1 1 calc GR . . . . C58 C 0.7996(4) 0.6454(5) 0.6917(4) 0.047(2) Uani 1 1 d D . . . . H58A H 0.8416 0.6328 0.7055 0.070 Uiso 1 1 calc GR . . . . H58B H 0.7937 0.7007 0.6948 0.070 Uiso 1 1 calc GR . . . . H58C H 0.7877 0.6304 0.6551 0.070 Uiso 1 1 calc GR . . . . C59 C 0.7431(3) 0.4658(5) 0.6463(3) 0.041(2) Uani 1 1 d D . . . . H59 H 0.7282 0.4117 0.6440 0.049 Uiso 1 1 calc R . . . . C60 C 0.7985(4) 0.4643(5) 0.6239(3) 0.045(2) Uani 1 1 d D . . . . H60A H 0.8131 0.5168 0.6220 0.067 Uiso 1 1 calc GR . . . . H60B H 0.7883 0.4417 0.5891 0.067 Uiso 1 1 calc GR . . . . H60C H 0.8295 0.4333 0.6464 0.067 Uiso 1 1 calc GR . . . . C61 C 0.6943(4) 0.5123(6) 0.6096(4) 0.055(3) Uani 1 1 d D . . . . H61A H 0.6574 0.5091 0.6214 0.083 Uiso 1 1 calc GR . . . . H61B H 0.6878 0.4914 0.5743 0.083 Uiso 1 1 calc GR . . . . H61C H 0.7067 0.5661 0.6095 0.083 Uiso 1 1 calc GR . . . . C62 C 0.6923(3) 0.4585(5) 0.7429(3) 0.0321(19) Uani 1 1 d . . . . . H62 H 0.6794 0.4079 0.7261 0.039 Uiso 1 1 calc R . . . . C63 C 0.7055(3) 0.4461(5) 0.8016(3) 0.037(2) Uani 1 1 d . . . . . H63A H 0.7322 0.4021 0.8111 0.055 Uiso 1 1 calc GR . . . . H63B H 0.6683 0.4363 0.8121 0.055 Uiso 1 1 calc GR . . . . H63C H 0.7245 0.4922 0.8194 0.055 Uiso 1 1 calc GR . . . . C64 C 0.6393(3) 0.5138(4) 0.7271(3) 0.0267(18) Uani 1 1 d . . . . . H64A H 0.6500 0.5638 0.7437 0.040 Uiso 1 1 calc GR . . . . H64B H 0.6051 0.4927 0.7382 0.040 Uiso 1 1 calc GR . . . . H64C H 0.6291 0.5201 0.6893 0.040 Uiso 1 1 calc GR . . . . C65 C 0.8790(3) 0.4800(5) 0.7505(4) 0.041(2) Uani 1 1 d . . . . . H65A H 0.8718 0.5260 0.7280 0.049 Uiso 1 1 calc R . . . . H65B H 0.9021 0.4428 0.7350 0.049 Uiso 1 1 calc R . . . . C66 C 0.9141(3) 0.5023(4) 0.8042(3) 0.033(2) Uani 1 1 d . . . . . H66A H 0.9513 0.5284 0.8015 0.040 Uiso 1 1 calc R . . . . H66B H 0.8907 0.5386 0.8201 0.040 Uiso 1 1 calc R . . . . C1 C 0.5460(9) 0.3251(8) 0.5825(5) 0.055(3) Uani 0.674(18) 1 d D U P A 1 H1 H 0.5034 0.3091 0.5751 0.065 Uiso 0.674(18) 1 calc R . P A 1 C2 C 0.5561(10) 0.3793(14) 0.5380(8) 0.061(4) Uani 0.674(18) 1 d D U P A 1 H2A H 0.5967 0.3995 0.5472 0.091 Uiso 0.674(18) 1 calc GR . P A 1 H2B H 0.5278 0.4220 0.5335 0.091 Uiso 0.674(18) 1 calc GR . P A 1 H2C H 0.5501 0.3502 0.5056 0.091 Uiso 0.674(18) 1 calc GR . P A 1 C3 C 0.5605(8) 0.3741(8) 0.6315(5) 0.057(4) Uani 0.674(18) 1 d D U P A 1 H3A H 0.5537 0.3440 0.6609 0.085 Uiso 0.674(18) 1 calc GR . P A 1 H3B H 0.5349 0.4196 0.6266 0.085 Uiso 0.674(18) 1 calc GR . P A 1 H3C H 0.6022 0.3901 0.6387 0.085 Uiso 0.674(18) 1 calc GR . P A 1 C1A C 0.5716(13) 0.346(2) 0.5941(13) 0.056(4) Uani 0.326(18) 1 d D U P A 2 H1A H 0.6065 0.3793 0.6090 0.067 Uiso 0.326(18) 1 calc R . P A 2 C2A C 0.5392(17) 0.373(3) 0.5388(15) 0.059(4) Uani 0.326(18) 1 d D U P A 2 H2AA H 0.5669 0.4020 0.5233 0.088 Uiso 0.326(18) 1 calc GR . P A 2 H2AB H 0.5054 0.4055 0.5410 0.088 Uiso 0.326(18) 1 calc GR . P A 2 H2AC H 0.5248 0.3280 0.5171 0.088 Uiso 0.326(18) 1 calc GR . P A 2 C3A C 0.5224(16) 0.3558(19) 0.6234(13) 0.055(4) Uani 0.326(18) 1 d D U P A 2 H3AA H 0.4852 0.3340 0.6027 0.082 Uiso 0.326(18) 1 calc GR . P A 2 H3AB H 0.5168 0.4105 0.6293 0.082 Uiso 0.326(18) 1 calc GR . P A 2 H3AC H 0.5336 0.3291 0.6568 0.082 Uiso 0.326(18) 1 calc GR . P A 2 Na1 Na 0.75551(12) 0.73498(17) 0.97798(12) 0.0307(7) Uani 1 1 d . U . . . O1 O 0.6978(3) 0.6955(4) 1.0405(2) 0.0538(16) Uani 1 1 d . U . . . O2 O 0.7029(3) 0.6121(4) 0.9527(3) 0.0541(16) Uani 1 1 d . U . . . O3 O 0.6842(3) 0.7463(5) 0.8959(3) 0.0652(18) Uani 1 1 d . U . . . O4 O 0.6800(3) 0.8318(4) 0.9833(3) 0.0664(18) Uani 1 1 d . U . . . O5 O 0.8158(2) 0.7916(3) 1.0583(2) 0.0415(14) Uani 1 1 d . U . . . O6 O 0.8306(2) 0.6445(3) 1.0222(2) 0.0437(14) Uani 1 1 d . U . . . O7 O 0.8238(3) 0.6965(4) 0.9226(2) 0.0488(15) Uani 1 1 d . U . . . O8 O 0.8114(2) 0.8471(3) 0.9582(2) 0.0446(14) Uani 1 1 d . U . . . C67 C 0.6393(5) 0.8147(7) 1.0100(5) 0.077(3) Uani 1 1 d . U . . . H67A H 0.6065 0.7844 0.9882 0.092 Uiso 1 1 calc R . . . . H67B H 0.6224 0.8622 1.0212 0.092 Uiso 1 1 calc R . . . . C68 C 0.6694(4) 0.7701(6) 1.0549(4) 0.060(3) Uani 1 1 d . U . . . H68A H 0.6405 0.7568 1.0757 0.072 Uiso 1 1 calc R . . . . H68B H 0.7008 0.8022 1.0768 0.072 Uiso 1 1 calc R . . . . C69 C 0.6583(5) 0.6389(7) 1.0266(4) 0.068(3) Uani 1 1 d . U . . . H69A H 0.6221 0.6582 1.0022 0.081 Uiso 1 1 calc R . . . . H69B H 0.6470 0.6174 1.0575 0.081 Uiso 1 1 calc R . . . . C70 C 0.6875(4) 0.5807(6) 1.0017(4) 0.058(2) Uani 1 1 d . U . . . H70A H 0.6608 0.5358 0.9926 0.069 Uiso 1 1 calc R . . . . H70B H 0.7242 0.5633 1.0263 0.069 Uiso 1 1 calc R . . . . C71 C 0.6571(5) 0.6124(7) 0.9112(5) 0.072(3) Uani 1 1 d . U . . . H71A H 0.6205 0.6294 0.9212 0.087 Uiso 1 1 calc R . . . . H71B H 0.6503 0.5602 0.8962 0.087 Uiso 1 1 calc R . . . . C72 C 0.6720(5) 0.6652(7) 0.8739(4) 0.067(3) Uani 1 1 d . U . . . H72A H 0.6388 0.6670 0.8426 0.081 Uiso 1 1 calc R . . . . H72B H 0.7076 0.6461 0.8632 0.081 Uiso 1 1 calc R . . . . C73 C 0.6342(5) 0.7856(7) 0.8919(5) 0.079(3) Uani 1 1 d . U . . . H73A H 0.6044 0.7549 0.9045 0.094 Uiso 1 1 calc R . . . . H73B H 0.6171 0.8010 0.8555 0.094 Uiso 1 1 calc R . . . . C74 C 0.6530(4) 0.8549(6) 0.9258(5) 0.069(3) Uani 1 1 d . U . . . H74A H 0.6181 0.8885 0.9242 0.083 Uiso 1 1 calc R . . . . H74B H 0.6828 0.8843 0.9124 0.083 Uiso 1 1 calc R . . . . C75 C 0.8422(4) 0.7314(5) 1.0921(4) 0.045(2) Uani 1 1 d . U . . . H75A H 0.8112 0.7046 1.1055 0.054 Uiso 1 1 calc R . . . . H75B H 0.8713 0.7534 1.1221 0.054 Uiso 1 1 calc R . . . . C76 C 0.8735(4) 0.6739(5) 1.0642(4) 0.045(2) Uani 1 1 d . U . . . H76A H 0.9057 0.6996 1.0517 0.054 Uiso 1 1 calc R . . . . H76B H 0.8911 0.6320 1.0881 0.054 Uiso 1 1 calc R . . . . C77 C 0.8533(4) 0.6016(6) 0.9855(4) 0.054(2) Uani 1 1 d . U . . . H77A H 0.8220 0.5665 0.9665 0.065 Uiso 1 1 calc R . . . . H77B H 0.8872 0.5700 1.0041 0.065 Uiso 1 1 calc R . . . . C78 C 0.8727(4) 0.6504(6) 0.9487(4) 0.056(2) Uani 1 1 d . U . . . H78A H 0.9057 0.6837 0.9670 0.068 Uiso 1 1 calc R . . . . H78B H 0.8872 0.6187 0.9232 0.068 Uiso 1 1 calc R . . . . C79 C 0.8412(4) 0.7651(6) 0.8988(4) 0.048(2) Uani 1 1 d . U . . . H79A H 0.8072 0.7837 0.8714 0.058 Uiso 1 1 calc R . . . . H79B H 0.8742 0.7526 0.8823 0.058 Uiso 1 1 calc R . . . . C80 C 0.8606(4) 0.8270(5) 0.9384(4) 0.046(2) Uani 1 1 d . U . . . H80A H 0.8934 0.8083 0.9668 0.055 Uiso 1 1 calc R . . . . H80B H 0.8748 0.8723 0.9223 0.055 Uiso 1 1 calc R . . . . C81 C 0.8252(4) 0.8955(5) 1.0030(4) 0.048(2) Uani 1 1 d . U . . . H81A H 0.7882 0.9190 1.0084 0.058 Uiso 1 1 calc R . . . . H81B H 0.8518 0.9374 0.9971 0.058 Uiso 1 1 calc R . . . . C82 C 0.8556(4) 0.8506(5) 1.0518(4) 0.046(2) Uani 1 1 d . U . . . H82A H 0.8935 0.8283 1.0475 0.055 Uiso 1 1 calc R . . . . H82B H 0.8642 0.8850 1.0824 0.055 Uiso 1 1 calc R . . . . O9 O 1.0532(3) -0.0133(5) 0.9615(3) 0.086(3) Uani 1 1 d . . . . . C83 C 1.0583(6) -0.0574(7) 0.9193(5) 0.091(4) Uani 1 1 d . . . . . H83A H 1.0291 -0.0401 0.8883 0.137 Uiso 1 1 calc GR . . . . H83B H 1.0509 -0.1115 0.9260 0.137 Uiso 1 1 calc GR . . . . H83C H 1.0984 -0.0520 0.9136 0.137 Uiso 1 1 calc GR . . . . C84 C 0.9983(5) -0.0186(7) 0.9742(5) 0.081(4) Uani 1 1 d . . . . . H84A H 0.9870 -0.0732 0.9757 0.098 Uiso 1 1 calc R . . . . H84B H 0.9675 0.0072 0.9472 0.098 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Th1 0.01633(14) 0.02007(16) 0.02681(16) 0.00044(11) 0.00761(12) 0.00097(10) Th2 0.01669(14) 0.01857(16) 0.02980(17) 0.00098(12) 0.00971(12) 0.00068(10) P1 0.0220(10) 0.0233(11) 0.0367(12) -0.0010(9) 0.0080(9) -0.0036(8) Si1 0.0336(12) 0.0422(15) 0.0360(14) 0.0141(11) 0.0178(11) 0.0176(11) Si2 0.0190(10) 0.0202(12) 0.0301(12) 0.0007(9) 0.0089(9) 0.0003(8) Si3 0.0199(10) 0.0257(12) 0.0257(12) -0.0013(9) 0.0085(9) -0.0003(9) Si4 0.0237(11) 0.0295(13) 0.0297(12) -0.0038(10) 0.0098(10) -0.0039(9) Si5 0.0239(11) 0.0218(12) 0.0469(15) 0.0087(10) 0.0156(11) 0.0051(9) Si6 0.0164(10) 0.0260(12) 0.0302(12) -0.0027(9) 0.0078(9) 0.0018(8) N1 0.024(3) 0.021(4) 0.037(4) 0.001(3) 0.011(3) 0.005(3) N2 0.020(3) 0.025(4) 0.008(3) -0.002(2) -0.005(3) 0.001(3) N3 0.020(3) 0.020(3) 0.032(4) -0.006(3) 0.010(3) -0.007(3) N4 0.018(3) 0.020(3) 0.026(3) -0.002(3) 0.005(3) 0.005(2) N5 0.020(3) 0.022(4) 0.043(4) -0.005(3) 0.018(3) -0.005(3) N6 0.011(3) 0.028(4) 0.031(4) 0.008(3) 0.006(3) -0.002(2) N7 0.019(3) 0.025(4) 0.028(4) -0.001(3) 0.005(3) 0.000(3) N8 0.021(3) 0.015(3) 0.032(4) 0.003(3) 0.011(3) -0.004(2) C4 0.027(4) 0.066(7) 0.030(5) 0.014(4) 0.007(4) 0.007(4) C5 0.041(5) 0.073(7) 0.037(5) -0.005(5) 0.014(5) 0.002(5) C6 0.037(5) 0.122(11) 0.047(7) 0.009(7) 0.001(5) 0.020(6) C7 0.041(5) 0.043(6) 0.029(5) 0.001(4) 0.015(4) -0.003(4) C8 0.047(5) 0.060(7) 0.052(6) 0.020(5) 0.023(5) 0.006(5) C9 0.022(4) 0.051(6) 0.044(5) -0.005(4) 0.013(4) -0.005(4) C10 0.029(4) 0.040(5) 0.030(5) 0.002(4) 0.012(4) 0.006(4) C11 0.019(4) 0.040(5) 0.031(5) 0.001(4) 0.006(4) 0.003(3) C12 0.027(4) 0.025(4) 0.030(5) 0.002(4) 0.003(4) 0.004(3) C13 0.035(5) 0.024(5) 0.042(5) -0.003(4) 0.007(4) -0.001(4) C14 0.042(5) 0.025(5) 0.045(5) 0.002(4) 0.022(4) -0.004(4) C15 0.027(4) 0.025(4) 0.026(4) 0.002(3) 0.001(4) -0.003(3) C16 0.026(4) 0.024(5) 0.050(6) 0.002(4) -0.016(4) -0.004(3) C17 0.036(5) 0.036(5) 0.033(5) -0.011(4) 0.002(4) 0.005(4) C18 0.018(4) 0.041(5) 0.037(5) -0.009(4) 0.008(4) 0.004(3) C19 0.027(4) 0.047(6) 0.041(5) 0.004(4) 0.011(4) 0.005(4) C20 0.024(4) 0.048(6) 0.043(5) -0.008(4) 0.006(4) 0.006(4) C21 0.021(4) 0.029(5) 0.028(4) 0.007(3) 0.006(4) 0.004(3) C22 0.016(4) 0.025(4) 0.025(4) -0.001(3) -0.002(3) -0.003(3) C23 0.025(4) 0.029(5) 0.036(5) 0.003(4) 0.015(4) -0.001(3) C24 0.027(4) 0.052(6) 0.049(6) 0.004(5) 0.010(4) 0.007(4) C25 0.030(5) 0.056(6) 0.045(6) -0.015(5) 0.014(4) -0.006(4) C26 0.028(4) 0.026(5) 0.044(5) -0.002(4) 0.014(4) -0.007(3) C27 0.031(4) 0.030(5) 0.061(6) 0.004(4) 0.011(4) -0.004(4) C28 0.042(5) 0.025(5) 0.052(6) -0.008(4) 0.019(5) 0.001(4) C29 0.035(5) 0.035(5) 0.029(5) 0.000(4) 0.014(4) 0.007(4) C30 0.073(7) 0.044(6) 0.040(6) 0.005(5) 0.015(5) 0.003(5) C31 0.043(5) 0.060(7) 0.036(5) -0.001(5) 0.005(5) 0.009(5) C32 0.027(4) 0.033(5) 0.024(4) -0.003(3) 0.013(4) -0.002(3) C33 0.023(4) 0.026(4) 0.027(4) -0.003(3) 0.014(4) -0.004(3) C34 0.033(5) 0.048(6) 0.035(5) -0.005(4) 0.007(4) -0.002(4) C35 0.032(5) 0.063(7) 0.048(6) 0.002(5) -0.002(4) 0.008(4) C36 0.036(5) 0.068(7) 0.040(6) -0.008(5) 0.006(4) -0.019(5) C37 0.036(5) 0.040(5) 0.030(5) 0.001(4) 0.016(4) -0.005(4) C38 0.042(5) 0.061(7) 0.055(6) -0.013(5) 0.026(5) -0.013(5) C39 0.032(5) 0.070(7) 0.058(7) -0.008(5) 0.024(5) -0.003(5) C40 0.023(4) 0.039(5) 0.031(5) 0.003(4) 0.008(4) -0.003(4) C41 0.045(5) 0.035(5) 0.037(5) -0.005(4) 0.011(4) -0.002(4) C42 0.047(5) 0.036(6) 0.054(6) 0.005(5) 0.020(5) -0.004(4) C43 0.023(4) 0.029(5) 0.038(5) -0.009(4) 0.017(4) 0.000(3) C44 0.025(4) 0.028(5) 0.048(5) -0.011(4) 0.015(4) -0.009(3) C45 0.024(4) 0.032(5) 0.039(5) -0.002(4) 0.013(4) 0.007(3) C46 0.029(4) 0.040(5) 0.054(6) 0.011(4) 0.017(4) 0.008(4) C47 0.035(5) 0.056(6) 0.057(6) -0.001(5) 0.026(5) 0.012(4) C48 0.019(4) 0.035(5) 0.035(5) -0.008(4) 0.010(4) 0.005(3) C49 0.044(5) 0.027(5) 0.047(6) 0.001(4) 0.008(5) 0.007(4) C50 0.036(5) 0.036(5) 0.056(6) -0.001(4) 0.010(5) -0.006(4) C51 0.028(4) 0.041(5) 0.027(5) 0.011(4) 0.008(4) 0.001(4) C52 0.059(6) 0.064(7) 0.036(6) -0.021(5) 0.002(5) 0.000(5) C53 0.030(5) 0.050(6) 0.038(5) 0.004(4) -0.008(4) 0.000(4) C54 0.023(4) 0.026(5) 0.037(5) 0.003(4) 0.013(4) 0.011(3) C55 0.015(4) 0.030(5) 0.041(5) -0.002(4) 0.015(4) -0.002(3) C56 0.029(4) 0.020(4) 0.057(6) 0.007(4) 0.022(4) 0.001(3) C57 0.062(6) 0.027(5) 0.058(6) 0.001(4) 0.030(5) 0.009(4) C58 0.046(5) 0.028(5) 0.072(7) 0.008(5) 0.026(5) -0.006(4) C59 0.046(5) 0.022(5) 0.053(6) 0.013(4) 0.008(5) 0.000(4) C60 0.053(6) 0.040(6) 0.045(6) 0.011(4) 0.020(5) 0.009(4) C61 0.047(6) 0.071(8) 0.041(6) 0.009(5) -0.001(5) 0.004(5) C62 0.033(4) 0.025(5) 0.044(5) 0.008(4) 0.020(4) 0.006(4) C63 0.025(4) 0.042(5) 0.048(6) 0.007(4) 0.016(4) 0.001(4) C64 0.019(4) 0.014(4) 0.046(5) 0.007(4) 0.006(4) 0.010(3) C65 0.025(4) 0.044(6) 0.061(6) 0.019(5) 0.026(5) 0.013(4) C66 0.017(4) 0.029(5) 0.058(6) 0.006(4) 0.018(4) 0.001(3) C1 0.068(8) 0.047(5) 0.059(5) 0.026(4) 0.037(5) 0.031(5) C2 0.077(9) 0.053(6) 0.063(6) 0.034(5) 0.039(6) 0.037(6) C3 0.072(9) 0.044(6) 0.062(6) 0.024(5) 0.031(6) 0.036(6) C1A 0.070(8) 0.048(5) 0.060(6) 0.027(4) 0.038(6) 0.034(6) C2A 0.073(10) 0.052(7) 0.062(6) 0.030(5) 0.038(7) 0.034(7) C3A 0.068(9) 0.047(7) 0.061(7) 0.024(6) 0.037(7) 0.035(7) Na1 0.0233(14) 0.0337(18) 0.0357(17) 0.0008(14) 0.0085(13) -0.0018(12) O1 0.032(3) 0.078(4) 0.052(4) 0.010(3) 0.010(3) -0.005(3) O2 0.033(3) 0.051(4) 0.076(4) -0.015(3) 0.009(3) -0.006(3) O3 0.042(3) 0.098(5) 0.055(4) 0.024(3) 0.012(3) -0.004(3) O4 0.042(3) 0.057(4) 0.102(5) -0.005(3) 0.020(3) -0.001(3) O5 0.033(3) 0.042(3) 0.049(3) -0.009(2) 0.010(3) -0.003(2) O6 0.034(3) 0.044(3) 0.049(3) -0.004(3) 0.002(2) 0.000(2) O7 0.045(3) 0.054(4) 0.052(4) -0.005(3) 0.020(3) -0.001(3) O8 0.035(3) 0.043(3) 0.052(3) 0.005(3) 0.002(3) -0.006(2) C67 0.061(6) 0.069(7) 0.105(7) -0.005(5) 0.030(5) 0.010(5) C68 0.029(5) 0.092(6) 0.065(6) -0.006(4) 0.025(4) 0.009(4) C69 0.054(5) 0.087(6) 0.062(6) 0.011(5) 0.014(5) -0.014(4) C70 0.036(5) 0.054(5) 0.083(6) 0.009(4) 0.016(4) -0.011(4) C71 0.056(5) 0.079(7) 0.077(6) -0.010(5) 0.006(4) -0.003(5) C72 0.046(6) 0.093(6) 0.058(6) -0.004(4) 0.002(5) -0.008(5) C73 0.054(5) 0.102(7) 0.081(7) 0.019(5) 0.019(5) 0.002(5) C74 0.040(5) 0.064(6) 0.100(6) 0.018(5) 0.009(5) 0.007(4) C75 0.035(4) 0.051(5) 0.043(5) -0.005(3) -0.001(4) -0.005(3) C76 0.040(4) 0.045(5) 0.047(5) 0.002(4) 0.002(4) 0.000(4) C77 0.053(5) 0.047(5) 0.063(5) -0.005(4) 0.014(4) 0.007(4) C78 0.053(5) 0.050(5) 0.071(6) -0.006(4) 0.025(4) 0.008(4) C79 0.041(5) 0.064(5) 0.039(5) 0.009(4) 0.007(4) -0.007(4) C80 0.038(4) 0.051(5) 0.048(5) 0.015(4) 0.010(4) -0.005(4) C81 0.042(5) 0.038(5) 0.063(5) -0.001(4) 0.010(4) -0.008(4) C82 0.041(5) 0.048(5) 0.049(5) -0.013(4) 0.007(4) -0.010(4) O9 0.061(5) 0.098(7) 0.104(7) -0.027(5) 0.030(5) -0.007(4) C83 0.123(11) 0.086(10) 0.072(9) -0.012(8) 0.039(9) 0.000(9) C84 0.059(7) 0.074(9) 0.118(12) -0.017(8) 0.035(8) 0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Th1 P1 2.740(2) . ? Th1 N1 2.371(6) . ? Th1 N2 2.347(6) . ? Th1 N3 2.360(5) . ? Th1 N4 2.821(6) . ? Th2 P1 2.735(2) . ? Th2 N5 2.366(6) . ? Th2 N6 2.365(6) . ? Th2 N7 2.388(5) . ? Th2 N8 2.815(6) . ? Si1 N1 1.731(6) . ? Si1 C4 1.915(9) . ? Si1 C7 1.887(8) . ? Si1 C1 1.919(15) . ? Si1 C1A 2.00(4) . ? Si2 N2 1.727(6) . ? Si2 C12 1.910(8) . ? Si2 C15 1.891(8) . ? Si2 C18 1.906(7) . ? Si3 N3 1.737(6) . ? Si3 C23 1.923(7) . ? Si3 C26 1.879(8) . ? Si3 C29 1.894(8) . ? Si4 N5 1.729(6) . ? Si4 C34 1.920(8) . ? Si4 C37 1.906(7) . ? Si4 C40 1.893(8) . ? Si5 N6 1.725(6) . ? Si5 C56 1.918(8) . ? Si5 C59 1.897(9) . ? Si5 C62 1.893(7) . ? Si6 N7 1.718(6) . ? Si6 C45 1.922(7) . ? Si6 C48 1.886(8) . ? Si6 C51 1.885(8) . ? N1 C10 1.483(9) . ? N2 C21 1.479(9) . ? N3 C32 1.481(9) . ? N4 C11 1.461(9) . ? N4 C22 1.484(8) . ? N4 C33 1.485(8) . ? N5 C43 1.482(9) . ? N6 C65 1.507(9) . ? N7 C54 1.471(10) . ? N8 C44 1.457(9) . ? N8 C55 1.477(8) . ? N8 C66 1.471(9) . ? C4 H4 1.0000 . ? C4 C5 1.527(9) . ? C4 C6 1.536(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7 1.0000 . ? C7 C8 1.532(8) . ? C7 C9 1.542(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.517(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12 1.0000 . ? C12 C13 1.524(9) . ? C12 C14 1.540(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 1.0000 . ? C15 C16 1.534(10) . ? C15 C17 1.540(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18 1.0000 . ? C18 C19 1.518(9) . ? C18 C20 1.522(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.511(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23 1.0000 . ? C23 C24 1.536(9) . ? C23 C25 1.537(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26 1.0000 . ? C26 C27 1.533(9) . ? C26 C28 1.529(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29 1.0000 . ? C29 C30 1.524(9) . ? C29 C31 1.538(9) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.496(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34 1.0000 . ? C34 C35 1.536(9) . ? C34 C36 1.540(9) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37 1.0000 . ? C37 C38 1.520(9) . ? C37 C39 1.529(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40 1.0000 . ? C40 C41 1.529(8) . ? C40 C42 1.544(9) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.535(9) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45 1.0000 . ? C45 C46 1.524(9) . ? C45 C47 1.540(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48 1.0000 . ? C48 C49 1.539(9) . ? C48 C50 1.534(8) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51 1.0000 . ? C51 C52 1.525(9) . ? C51 C53 1.540(9) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C54 C55 1.537(10) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56 1.0000 . ? C56 C57 1.525(9) . ? C56 C58 1.540(8) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59 1.0000 . ? C59 C60 1.535(9) . ? C59 C61 1.536(9) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62 1.0000 . ? C62 C63 1.529(11) . ? C62 C64 1.538(9) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C65 C66 1.512(12) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C1 H1 1.0000 . ? C1 C2 1.568(12) . ? C1 C3 1.523(13) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C1A H1A 1.0000 . ? C1A C2A 1.555(14) . ? C1A C3A 1.531(14) . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C3A H3AA 0.9800 . ? C3A H3AB 0.9800 . ? C3A H3AC 0.9800 . ? Na1 O1 2.458(6) . ? Na1 O2 2.476(7) . ? Na1 O3 2.409(7) . ? Na1 O4 2.456(7) . ? Na1 O5 2.460(6) . ? Na1 O6 2.433(6) . ? Na1 O7 2.489(6) . ? Na1 O8 2.465(6) . ? O1 C68 1.544(11) . ? O1 C69 1.335(12) . ? O2 C70 1.527(11) . ? O2 C71 1.335(12) . ? O3 C72 1.527(13) . ? O3 C73 1.329(12) . ? O4 C67 1.338(12) . ? O4 C74 1.559(13) . ? O5 C75 1.420(10) . ? O5 C82 1.419(10) . ? O6 C76 1.403(10) . ? O6 C77 1.421(10) . ? O7 C78 1.426(11) . ? O7 C79 1.451(10) . ? O8 C80 1.404(10) . ? O8 C81 1.430(11) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C67 C68 1.453(15) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C69 C70 1.460(14) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C71 C72 1.452(14) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C73 C74 1.505(16) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C75 C76 1.523(12) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C77 C78 1.442(13) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C79 C80 1.499(12) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C81 C82 1.531(13) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? O9 C83 1.386(12) . ? O9 C84 1.393(11) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C84 1.50(2) 3_757 ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Th1 N4 178.16(12) . . ? N1 Th1 P1 114.65(15) . . ? N1 Th1 N4 66.64(19) . . ? N2 Th1 P1 110.59(14) . . ? N2 Th1 N1 105.31(19) . . ? N2 Th1 N3 105.92(19) . . ? N2 Th1 N4 67.64(17) . . ? N3 Th1 P1 112.97(15) . . ? N3 Th1 N1 106.8(2) . . ? N3 Th1 N4 67.45(18) . . ? P1 Th2 N8 175.78(12) . . ? N5 Th2 P1 112.18(14) . . ? N5 Th2 N7 102.6(2) . . ? N5 Th2 N8 66.81(17) . . ? N6 Th2 P1 108.62(14) . . ? N6 Th2 N5 109.4(2) . . ? N6 Th2 N7 107.07(19) . . ? N6 Th2 N8 68.46(18) . . ? N7 Th2 P1 116.60(15) . . ? N7 Th2 N8 67.51(18) . . ? Th2 P1 Th1 176.21(8) . . ? N1 Si1 C4 117.0(4) . . ? N1 Si1 C7 105.8(3) . . ? N1 Si1 C1 109.3(4) . . ? N1 Si1 C1A 112.7(8) . . ? C4 Si1 C1 100.1(5) . . ? C4 Si1 C1A 113.6(11) . . ? C7 Si1 C4 107.6(3) . . ? C7 Si1 C1 117.4(6) . . ? C7 Si1 C1A 97.8(10) . . ? N2 Si2 C12 114.5(3) . . ? N2 Si2 C15 107.8(3) . . ? N2 Si2 C18 111.1(3) . . ? C15 Si2 C12 108.1(3) . . ? C15 Si2 C18 107.7(3) . . ? C18 Si2 C12 107.4(3) . . ? N3 Si3 C23 109.9(3) . . ? N3 Si3 C26 107.5(3) . . ? N3 Si3 C29 114.0(3) . . ? C26 Si3 C23 112.5(3) . . ? C26 Si3 C29 107.3(3) . . ? C29 Si3 C23 105.7(3) . . ? N5 Si4 C34 115.8(3) . . ? N5 Si4 C37 112.0(3) . . ? N5 Si4 C40 107.4(3) . . ? C37 Si4 C34 107.4(3) . . ? C40 Si4 C34 108.3(4) . . ? C40 Si4 C37 105.3(3) . . ? N6 Si5 C56 115.0(3) . . ? N6 Si5 C59 111.3(3) . . ? N6 Si5 C62 107.5(3) . . ? C59 Si5 C56 107.4(3) . . ? C62 Si5 C56 107.6(3) . . ? C62 Si5 C59 107.6(4) . . ? N7 Si6 C45 110.2(3) . . ? N7 Si6 C48 113.6(3) . . ? N7 Si6 C51 107.7(3) . . ? C48 Si6 C45 104.6(3) . . ? C51 Si6 C45 113.1(3) . . ? C51 Si6 C48 107.7(3) . . ? Si1 N1 Th1 134.0(3) . . ? C10 N1 Th1 110.9(4) . . ? C10 N1 Si1 115.0(5) . . ? Si2 N2 Th1 133.7(3) . . ? C21 N2 Th1 110.0(4) . . ? C21 N2 Si2 116.2(5) . . ? Si3 N3 Th1 134.0(3) . . ? C32 N3 Th1 111.0(4) . . ? C32 N3 Si3 115.1(4) . . ? C11 N4 Th1 108.0(4) . . ? C11 N4 C22 111.0(6) . . ? C11 N4 C33 112.6(5) . . ? C22 N4 Th1 106.3(4) . . ? C22 N4 C33 112.1(5) . . ? C33 N4 Th1 106.5(4) . . ? Si4 N5 Th2 135.1(3) . . ? C43 N5 Th2 110.1(4) . . ? C43 N5 Si4 114.8(5) . . ? Si5 N6 Th2 134.2(3) . . ? C65 N6 Th2 110.4(4) . . ? C65 N6 Si5 115.2(5) . . ? Si6 N7 Th2 133.0(3) . . ? C54 N7 Th2 111.4(4) . . ? C54 N7 Si6 115.5(4) . . ? C44 N8 Th2 107.4(4) . . ? C44 N8 C55 111.3(6) . . ? C44 N8 C66 112.5(6) . . ? C55 N8 Th2 107.4(4) . . ? C66 N8 Th2 106.2(4) . . ? C66 N8 C55 111.6(5) . . ? Si1 C4 H4 105.4 . . ? C5 C4 Si1 116.1(6) . . ? C5 C4 H4 105.4 . . ? C5 C4 C6 107.4(8) . . ? C6 C4 Si1 116.2(6) . . ? C6 C4 H4 105.4 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7 106.7 . . ? C8 C7 Si1 113.6(6) . . ? C8 C7 H7 106.7 . . ? C8 C7 C9 110.1(6) . . ? C9 C7 Si1 112.5(5) . . ? C9 C7 H7 106.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? N1 C10 C11 110.3(6) . . ? H10A C10 H10B 108.1 . . ? C11 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? N4 C11 C10 108.8(6) . . ? N4 C11 H11A 109.9 . . ? N4 C11 H11B 109.9 . . ? C10 C11 H11A 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? Si2 C12 H12 104.8 . . ? C13 C12 Si2 117.6(5) . . ? C13 C12 H12 104.8 . . ? C13 C12 C14 109.4(6) . . ? C14 C12 Si2 114.1(5) . . ? C14 C12 H12 104.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15 105.7 . . ? C16 C15 Si2 114.1(5) . . ? C16 C15 H15 105.7 . . ? C16 C15 C17 109.3(7) . . ? C17 C15 Si2 115.4(5) . . ? C17 C15 H15 105.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18 104.5 . . ? C19 C18 Si2 116.1(5) . . ? C19 C18 H18 104.5 . . ? C19 C18 C20 109.2(6) . . ? C20 C18 Si2 116.4(5) . . ? C20 C18 H18 104.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 H21A 109.4 . . ? N2 C21 H21B 109.4 . . ? N2 C21 C22 111.0(6) . . ? H21A C21 H21B 108.0 . . ? C22 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? N4 C22 C21 108.5(6) . . ? N4 C22 H22A 110.0 . . ? N4 C22 H22B 110.0 . . ? C21 C22 H22A 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? Si3 C23 H23 105.7 . . ? C24 C23 Si3 113.5(5) . . ? C24 C23 H23 105.7 . . ? C24 C23 C25 109.2(6) . . ? C25 C23 Si3 116.2(5) . . ? C25 C23 H23 105.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26 105.6 . . ? C27 C26 Si3 116.1(5) . . ? C27 C26 H26 105.6 . . ? C28 C26 Si3 113.2(5) . . ? C28 C26 H26 105.6 . . ? C28 C26 C27 109.7(7) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si3 C29 H29 106.7 . . ? C30 C29 Si3 114.2(6) . . ? C30 C29 H29 106.7 . . ? C30 C29 C31 109.2(7) . . ? C31 C29 Si3 112.9(5) . . ? C31 C29 H29 106.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.4 . . ? N3 C32 H32B 109.4 . . ? N3 C32 C33 111.3(6) . . ? H32A C32 H32B 108.0 . . ? C33 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? N4 C33 C32 109.6(5) . . ? N4 C33 H33A 109.8 . . ? N4 C33 H33B 109.8 . . ? C32 C33 H33A 109.8 . . ? C32 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? Si4 C34 H34 104.9 . . ? C35 C34 Si4 113.6(6) . . ? C35 C34 H34 104.9 . . ? C35 C34 C36 108.2(7) . . ? C36 C34 Si4 118.8(6) . . ? C36 C34 H34 104.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si4 C37 H37 105.8 . . ? C38 C37 Si4 118.8(5) . . ? C38 C37 H37 105.8 . . ? C38 C37 C39 109.0(7) . . ? C39 C37 Si4 110.7(5) . . ? C39 C37 H37 105.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si4 C40 H40 105.7 . . ? C41 C40 Si4 115.1(5) . . ? C41 C40 H40 105.7 . . ? C41 C40 C42 110.9(7) . . ? C42 C40 Si4 112.8(5) . . ? C42 C40 H40 105.7 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C43 H43A 109.9 . . ? N5 C43 H43B 109.9 . . ? N5 C43 C44 108.7(6) . . ? H43A C43 H43B 108.3 . . ? C44 C43 H43A 109.9 . . ? C44 C43 H43B 109.9 . . ? N8 C44 C43 108.9(6) . . ? N8 C44 H44A 109.9 . . ? N8 C44 H44B 109.9 . . ? C43 C44 H44A 109.9 . . ? C43 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? Si6 C45 H45 105.6 . . ? C46 C45 Si6 115.1(5) . . ? C46 C45 H45 105.6 . . ? C46 C45 C47 108.4(6) . . ? C47 C45 Si6 115.5(5) . . ? C47 C45 H45 105.6 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si6 C48 H48 106.4 . . ? C49 C48 Si6 115.4(5) . . ? C49 C48 H48 106.4 . . ? C50 C48 Si6 113.2(5) . . ? C50 C48 H48 106.4 . . ? C50 C48 C49 108.5(6) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si6 C51 H51 106.0 . . ? C52 C51 Si6 113.4(6) . . ? C52 C51 H51 106.0 . . ? C52 C51 C53 111.1(7) . . ? C53 C51 Si6 113.7(6) . . ? C53 C51 H51 106.0 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N7 C54 H54A 109.5 . . ? N7 C54 H54B 109.5 . . ? N7 C54 C55 110.8(6) . . ? H54A C54 H54B 108.1 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? N8 C55 C54 108.6(5) . . ? N8 C55 H55A 110.0 . . ? N8 C55 H55B 110.0 . . ? C54 C55 H55A 110.0 . . ? C54 C55 H55B 110.0 . . ? H55A C55 H55B 108.3 . . ? Si5 C56 H56 104.6 . . ? C57 C56 Si5 113.3(5) . . ? C57 C56 H56 104.6 . . ? C57 C56 C58 109.8(7) . . ? C58 C56 Si5 118.4(5) . . ? C58 C56 H56 104.6 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? Si5 C59 H59 105.4 . . ? C60 C59 Si5 114.5(6) . . ? C60 C59 H59 105.4 . . ? C60 C59 C61 108.7(7) . . ? C61 C59 Si5 116.3(6) . . ? C61 C59 H59 105.4 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61B 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si5 C62 H62 107.2 . . ? C63 C62 Si5 114.6(6) . . ? C63 C62 H62 107.2 . . ? C63 C62 C64 108.7(6) . . ? C64 C62 Si5 111.8(5) . . ? C64 C62 H62 107.2 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63B 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N6 C65 H65A 109.5 . . ? N6 C65 H65B 109.5 . . ? N6 C65 C66 110.7(6) . . ? H65A C65 H65B 108.1 . . ? C66 C65 H65A 109.5 . . ? C66 C65 H65B 109.5 . . ? N8 C66 C65 110.1(7) . . ? N8 C66 H66A 109.6 . . ? N8 C66 H66B 109.6 . . ? C65 C66 H66A 109.6 . . ? C65 C66 H66B 109.6 . . ? H66A C66 H66B 108.2 . . ? Si1 C1 H1 109.5 . . ? C2 C1 Si1 113.8(13) . . ? C2 C1 H1 109.5 . . ? C3 C1 Si1 109.1(11) . . ? C3 C1 H1 109.5 . . ? C3 C1 C2 105.2(16) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C1A H1A 111.2 . . ? C2A C1A Si1 110(3) . . ? C2A C1A H1A 111.2 . . ? C3A C1A Si1 111(2) . . ? C3A C1A H1A 111.2 . . ? C3A C1A C2A 101(3) . . ? C1A C2A H2AA 109.5 . . ? C1A C2A H2AB 109.5 . . ? C1A C2A H2AC 109.5 . . ? H2AA C2A H2AB 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? C1A C3A H3AA 109.5 . . ? C1A C3A H3AB 109.5 . . ? C1A C3A H3AC 109.5 . . ? H3AA C3A H3AB 109.5 . . ? H3AA C3A H3AC 109.5 . . ? H3AB C3A H3AC 109.5 . . ? O1 Na1 O2 68.3(2) . . ? O1 Na1 O5 79.4(2) . . ? O1 Na1 O7 147.5(3) . . ? O1 Na1 O8 139.5(3) . . ? O2 Na1 O7 87.0(2) . . ? O3 Na1 O1 105.4(2) . . ? O3 Na1 O2 68.7(3) . . ? O3 Na1 O4 69.6(3) . . ? O3 Na1 O5 151.3(3) . . ? O3 Na1 O6 138.4(3) . . ? O3 Na1 O7 83.4(2) . . ? O3 Na1 O8 91.4(2) . . ? O4 Na1 O1 69.2(2) . . ? O4 Na1 O2 107.3(2) . . ? O4 Na1 O5 86.6(2) . . ? O4 Na1 O7 141.1(3) . . ? O4 Na1 O8 83.4(2) . . ? O5 Na1 O2 136.3(3) . . ? O5 Na1 O7 108.0(2) . . ? O5 Na1 O8 69.4(2) . . ? O6 Na1 O1 86.3(2) . . ? O6 Na1 O2 79.7(2) . . ? O6 Na1 O4 148.7(3) . . ? O6 Na1 O5 69.4(2) . . ? O6 Na1 O7 68.2(2) . . ? O6 Na1 O8 105.3(2) . . ? O8 Na1 O2 151.2(2) . . ? O8 Na1 O7 69.5(2) . . ? C68 O1 Na1 105.2(5) . . ? C69 O1 Na1 117.8(6) . . ? C69 O1 C68 112.7(7) . . ? C70 O2 Na1 106.1(5) . . ? C71 O2 Na1 117.6(7) . . ? C71 O2 C70 113.6(7) . . ? C72 O3 Na1 107.2(6) . . ? C73 O3 Na1 120.8(7) . . ? C73 O3 C72 111.5(8) . . ? C67 O4 Na1 118.5(7) . . ? C67 O4 C74 113.8(8) . . ? C74 O4 Na1 104.4(5) . . ? C75 O5 Na1 108.8(5) . . ? C82 O5 Na1 115.9(5) . . ? C82 O5 C75 114.5(6) . . ? C76 O6 Na1 115.9(5) . . ? C76 O6 C77 115.4(7) . . ? C77 O6 Na1 110.4(5) . . ? C78 O7 Na1 114.0(5) . . ? C78 O7 C79 113.8(7) . . ? C79 O7 Na1 108.3(5) . . ? C80 O8 Na1 113.2(5) . . ? C80 O8 C81 114.3(7) . . ? C81 O8 Na1 108.4(5) . . ? O4 C67 H67A 110.4 . . ? O4 C67 H67B 110.4 . . ? O4 C67 C68 106.8(9) . . ? H67A C67 H67B 108.6 . . ? C68 C67 H67A 110.4 . . ? C68 C67 H67B 110.4 . . ? O1 C68 H68A 108.9 . . ? O1 C68 H68B 108.9 . . ? C67 C68 O1 113.4(8) . . ? C67 C68 H68A 108.9 . . ? C67 C68 H68B 108.9 . . ? H68A C68 H68B 107.7 . . ? O1 C69 H69A 110.5 . . ? O1 C69 H69B 110.5 . . ? O1 C69 C70 106.2(8) . . ? H69A C69 H69B 108.7 . . ? C70 C69 H69A 110.5 . . ? C70 C69 H69B 110.5 . . ? O2 C70 H70A 109.4 . . ? O2 C70 H70B 109.4 . . ? C69 C70 O2 111.2(8) . . ? C69 C70 H70A 109.4 . . ? C69 C70 H70B 109.4 . . ? H70A C70 H70B 108.0 . . ? O2 C71 H71A 110.3 . . ? O2 C71 H71B 110.3 . . ? O2 C71 C72 107.0(9) . . ? H71A C71 H71B 108.6 . . ? C72 C71 H71A 110.3 . . ? C72 C71 H71B 110.3 . . ? O3 C72 H72A 109.2 . . ? O3 C72 H72B 109.2 . . ? C71 C72 O3 112.2(9) . . ? C71 C72 H72A 109.2 . . ? C71 C72 H72B 109.2 . . ? H72A C72 H72B 107.9 . . ? O3 C73 H73A 111.0 . . ? O3 C73 H73B 111.0 . . ? O3 C73 C74 104.0(10) . . ? H73A C73 H73B 109.0 . . ? C74 C73 H73A 111.0 . . ? C74 C73 H73B 111.0 . . ? O4 C74 H74A 109.3 . . ? O4 C74 H74B 109.3 . . ? C73 C74 O4 111.7(9) . . ? C73 C74 H74A 109.3 . . ? C73 C74 H74B 109.3 . . ? H74A C74 H74B 107.9 . . ? O5 C75 H75A 109.4 . . ? O5 C75 H75B 109.4 . . ? O5 C75 C76 111.3(7) . . ? H75A C75 H75B 108.0 . . ? C76 C75 H75A 109.4 . . ? C76 C75 H75B 109.4 . . ? O6 C76 C75 107.3(7) . . ? O6 C76 H76A 110.3 . . ? O6 C76 H76B 110.3 . . ? C75 C76 H76A 110.3 . . ? C75 C76 H76B 110.3 . . ? H76A C76 H76B 108.5 . . ? O6 C77 H77A 109.2 . . ? O6 C77 H77B 109.2 . . ? O6 C77 C78 112.1(8) . . ? H77A C77 H77B 107.9 . . ? C78 C77 H77A 109.2 . . ? C78 C77 H77B 109.2 . . ? O7 C78 C77 108.8(8) . . ? O7 C78 H78A 109.9 . . ? O7 C78 H78B 109.9 . . ? C77 C78 H78A 109.9 . . ? C77 C78 H78B 109.9 . . ? H78A C78 H78B 108.3 . . ? O7 C79 H79A 109.5 . . ? O7 C79 H79B 109.5 . . ? O7 C79 C80 110.9(7) . . ? H79A C79 H79B 108.1 . . ? C80 C79 H79A 109.5 . . ? C80 C79 H79B 109.5 . . ? O8 C80 C79 107.7(7) . . ? O8 C80 H80A 110.2 . . ? O8 C80 H80B 110.2 . . ? C79 C80 H80A 110.2 . . ? C79 C80 H80B 110.2 . . ? H80A C80 H80B 108.5 . . ? O8 C81 H81A 109.3 . . ? O8 C81 H81B 109.3 . . ? O8 C81 C82 111.7(7) . . ? H81A C81 H81B 107.9 . . ? C82 C81 H81A 109.3 . . ? C82 C81 H81B 109.3 . . ? O5 C82 C81 106.9(7) . . ? O5 C82 H82A 110.3 . . ? O5 C82 H82B 110.3 . . ? C81 C82 H82A 110.3 . . ? C81 C82 H82B 110.3 . . ? H82A C82 H82B 108.6 . . ? C83 O9 C84 114.5(9) . . ? O9 C83 H83A 109.5 . . ? O9 C83 H83B 109.5 . . ? O9 C83 H83C 109.5 . . ? H83A C83 H83B 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? O9 C84 C84 109.7(12) . 3_757 ? O9 C84 H84A 109.7 . . ? O9 C84 H84B 109.7 . . ? C84 C84 H84A 109.7 3_757 . ? C84 C84 H84B 109.7 3_757 . ? H84A C84 H84B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Th1 N1 C10 C11 -67.0(6) . . . . ? Th1 N2 C21 C22 -68.2(6) . . . . ? Th1 N3 C32 C33 -66.1(6) . . . . ? Th1 N4 C11 C10 -26.9(6) . . . . ? Th1 N4 C22 C21 -27.0(6) . . . . ? Th1 N4 C33 C32 -26.8(6) . . . . ? Th2 N5 C43 C44 -69.0(7) . . . . ? Th2 N6 C65 C66 -64.0(7) . . . . ? Th2 N7 C54 C55 -64.5(6) . . . . ? Th2 N8 C44 C43 -27.1(7) . . . . ? Th2 N8 C55 C54 -29.5(7) . . . . ? Th2 N8 C66 C65 -29.7(6) . . . . ? Si1 N1 C10 C11 112.6(6) . . . . ? Si2 N2 C21 C22 113.9(6) . . . . ? Si3 N3 C32 C33 114.2(5) . . . . ? Si4 N5 C43 C44 114.2(6) . . . . ? Si5 N6 C65 C66 120.7(6) . . . . ? Si6 N7 C54 C55 113.1(5) . . . . ? N1 Si1 C7 C8 174.6(6) . . . . ? N1 Si1 C7 C9 48.6(6) . . . . ? N1 C10 C11 N4 61.5(7) . . . . ? N2 Si2 C15 C16 169.3(5) . . . . ? N2 Si2 C15 C17 41.5(6) . . . . ? N2 C21 C22 N4 62.9(7) . . . . ? N3 Si3 C26 C27 50.9(6) . . . . ? N3 Si3 C26 C28 179.1(6) . . . . ? N3 Si3 C29 C30 -55.5(6) . . . . ? N3 Si3 C29 C31 70.1(6) . . . . ? N3 C32 C33 N4 61.3(7) . . . . ? N5 Si4 C40 C41 46.2(7) . . . . ? N5 Si4 C40 C42 174.8(5) . . . . ? N5 C43 C44 N8 63.0(8) . . . . ? N6 Si5 C59 C60 -43.6(7) . . . . ? N6 Si5 C59 C61 -171.8(6) . . . . ? N6 Si5 C62 C63 37.7(7) . . . . ? N6 Si5 C62 C64 161.9(5) . . . . ? N6 C65 C66 N8 62.8(7) . . . . ? N7 Si6 C48 C49 -57.8(6) . . . . ? N7 Si6 C48 C50 68.1(6) . . . . ? N7 Si6 C51 C52 -174.9(6) . . . . ? N7 Si6 C51 C53 56.8(6) . . . . ? N7 C54 C55 N8 62.6(7) . . . . ? C4 Si1 N1 Th1 123.3(4) . . . . ? C4 Si1 N1 C10 -56.2(6) . . . . ? C4 Si1 C7 C8 48.8(7) . . . . ? C4 Si1 C7 C9 -77.2(6) . . . . ? C7 Si1 N1 Th1 3.5(5) . . . . ? C7 Si1 N1 C10 -176.0(5) . . . . ? C11 N4 C22 C21 90.2(7) . . . . ? C11 N4 C33 C32 -144.9(6) . . . . ? C12 Si2 N2 Th1 134.9(4) . . . . ? C12 Si2 N2 C21 -47.8(5) . . . . ? C12 Si2 C15 C16 45.0(6) . . . . ? C12 Si2 C15 C17 -82.8(6) . . . . ? C15 Si2 N2 Th1 14.5(5) . . . . ? C15 Si2 N2 C21 -168.1(5) . . . . ? C18 Si2 N2 Th1 -103.2(4) . . . . ? C18 Si2 N2 C21 74.1(5) . . . . ? C18 Si2 C15 C16 -70.8(6) . . . . ? C18 Si2 C15 C17 161.4(6) . . . . ? C22 N4 C11 C10 -143.0(5) . . . . ? C22 N4 C33 C32 89.2(7) . . . . ? C23 Si3 N3 Th1 132.0(4) . . . . ? C23 Si3 N3 C32 -48.3(6) . . . . ? C23 Si3 C26 C27 -70.3(6) . . . . ? C23 Si3 C26 C28 58.0(7) . . . . ? C23 Si3 C29 C30 65.4(6) . . . . ? C23 Si3 C29 C31 -169.1(6) . . . . ? C26 Si3 N3 Th1 9.3(6) . . . . ? C26 Si3 N3 C32 -171.0(5) . . . . ? C26 Si3 C29 C30 -174.4(6) . . . . ? C26 Si3 C29 C31 -48.9(6) . . . . ? C29 Si3 N3 Th1 -109.6(5) . . . . ? C29 Si3 N3 C32 70.2(6) . . . . ? C29 Si3 C26 C27 173.9(5) . . . . ? C29 Si3 C26 C28 -57.8(6) . . . . ? C33 N4 C11 C10 90.4(7) . . . . ? C33 N4 C22 C21 -143.0(6) . . . . ? C34 Si4 N5 Th2 127.2(4) . . . . ? C34 Si4 N5 C43 -57.1(6) . . . . ? C34 Si4 C40 C41 -79.6(6) . . . . ? C34 Si4 C40 C42 49.0(6) . . . . ? C37 Si4 N5 Th2 -109.0(4) . . . . ? C37 Si4 N5 C43 66.6(6) . . . . ? C37 Si4 C40 C41 165.8(6) . . . . ? C37 Si4 C40 C42 -65.6(6) . . . . ? C40 Si4 N5 Th2 6.1(5) . . . . ? C40 Si4 N5 C43 -178.3(5) . . . . ? C44 N8 C55 C54 87.8(7) . . . . ? C44 N8 C66 C65 -146.9(6) . . . . ? C45 Si6 N7 Th2 129.5(4) . . . . ? C45 Si6 N7 C54 -47.4(6) . . . . ? C45 Si6 C48 C49 62.5(6) . . . . ? C45 Si6 C48 C50 -171.6(6) . . . . ? C45 Si6 C51 C52 63.0(7) . . . . ? C45 Si6 C51 C53 -65.2(6) . . . . ? C48 Si6 N7 Th2 -113.5(4) . . . . ? C48 Si6 N7 C54 69.6(6) . . . . ? C48 Si6 C51 C52 -52.0(7) . . . . ? C48 Si6 C51 C53 179.7(5) . . . . ? C51 Si6 N7 Th2 5.7(5) . . . . ? C51 Si6 N7 C54 -171.2(5) . . . . ? C51 Si6 C48 C49 -177.0(5) . . . . ? C51 Si6 C48 C50 -51.1(6) . . . . ? C55 N8 C44 C43 -144.4(6) . . . . ? C55 N8 C66 C65 87.1(7) . . . . ? C56 Si5 N6 Th2 143.7(4) . . . . ? C56 Si5 N6 C65 -42.4(6) . . . . ? C56 Si5 C59 C60 83.1(6) . . . . ? C56 Si5 C59 C61 -45.1(7) . . . . ? C56 Si5 C62 C63 -86.7(6) . . . . ? C56 Si5 C62 C64 37.5(7) . . . . ? C59 Si5 N6 Th2 -93.8(5) . . . . ? C59 Si5 N6 C65 80.0(6) . . . . ? C59 Si5 C62 C63 157.8(6) . . . . ? C59 Si5 C62 C64 -78.0(6) . . . . ? C62 Si5 N6 Th2 23.9(6) . . . . ? C62 Si5 N6 C65 -162.3(5) . . . . ? C62 Si5 C59 C60 -161.2(6) . . . . ? C62 Si5 C59 C61 70.6(7) . . . . ? C66 N8 C44 C43 89.4(7) . . . . ? C66 N8 C55 C54 -145.6(7) . . . . ? C1 Si1 N1 Th1 -123.8(7) . . . . ? C1 Si1 N1 C10 56.7(8) . . . . ? C1 Si1 C7 C8 -63.1(8) . . . . ? C1 Si1 C7 C9 170.9(6) . . . . ? C1A Si1 N1 Th1 -102.3(12) . . . . ? C1A Si1 N1 C10 78.3(13) . . . . ? C1A Si1 C7 C8 -69.0(11) . . . . ? C1A Si1 C7 C9 164.9(10) . . . . ? Na1 O1 C68 C67 49.8(9) . . . . ? Na1 O1 C69 C70 42.9(10) . . . . ? Na1 O2 C70 C69 50.1(9) . . . . ? Na1 O2 C71 C72 36.6(11) . . . . ? Na1 O3 C72 C71 51.0(9) . . . . ? Na1 O3 C73 C74 40.1(11) . . . . ? Na1 O4 C67 C68 37.5(12) . . . . ? Na1 O4 C74 C73 51.0(8) . . . . ? Na1 O5 C75 C76 50.4(7) . . . . ? Na1 O5 C82 C81 34.9(8) . . . . ? Na1 O6 C76 C75 36.6(8) . . . . ? Na1 O6 C77 C78 51.8(9) . . . . ? Na1 O7 C78 C77 34.5(10) . . . . ? Na1 O7 C79 C80 48.1(8) . . . . ? Na1 O8 C80 C79 44.3(8) . . . . ? Na1 O8 C81 C82 52.2(7) . . . . ? O1 C69 C70 O2 -62.5(11) . . . . ? O2 C71 C72 O3 -58.7(11) . . . . ? O3 C73 C74 O4 -60.7(10) . . . . ? O4 C67 C68 O1 -59.1(12) . . . . ? O5 C75 C76 O6 -59.0(9) . . . . ? O6 C77 C78 O7 -58.1(11) . . . . ? O7 C79 C80 O8 -63.5(9) . . . . ? O8 C81 C82 O5 -59.1(9) . . . . ? C67 O4 C74 C73 -79.6(11) . . . . ? C68 O1 C69 C70 165.7(8) . . . . ? C69 O1 C68 C67 -79.8(11) . . . . ? C70 O2 C71 C72 161.4(8) . . . . ? C71 O2 C70 C69 -80.7(11) . . . . ? C72 O3 C73 C74 167.2(8) . . . . ? C73 O3 C72 C71 -83.3(11) . . . . ? C74 O4 C67 C68 160.7(9) . . . . ? C75 O5 C82 C81 162.8(7) . . . . ? C76 O6 C77 C78 -82.1(10) . . . . ? C77 O6 C76 C75 167.9(7) . . . . ? C78 O7 C79 C80 -79.8(9) . . . . ? C79 O7 C78 C77 159.4(8) . . . . ? C80 O8 C81 C82 -75.2(9) . . . . ? C81 O8 C80 C79 169.2(7) . . . . ? C82 O5 C75 C76 -81.1(9) . . . . ? C83 O9 C84 C84 169.1(13) . . . 3_757 ? _shelx_res_file ; thew8.res created by SHELXL-2014/7 TITL thew8_a.res in P2(1)/c REM Old TITL THEW8 in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.138, Rweak 0.006, Alpha 0.055, Orientation as input REM Formula found by SHELXT: C94 N52 Na7 Si3 P7 Th2 REM EXTI 0.00000(6) CELL 0.71073 23.147859 17.413321 26.494652 90 103.6146 90 ZERR 4 0.00067 0.000502 0.000928 0 0.0035 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N Na O P Si Th UNIT 336 748 32 4 36 4 24 8 SADI C3 C1 C3A C1A C2A C1A C2 C1 C6 C4 C5 C4 C8 C7 C9 C7 C27 C26 C28 C26 C24 = C23 C25 C23 C31 C29 C30 C29 C36 C34 C35 C34 C38 C37 C39 C37 C42 C40 C41 C40 = C57 C56 C58 C56 C60 C59 C61 C59 C53 C51 C52 C51 C49 C48 C50 C48 C46 C45 C47 = C45 C13 C12 C14 C12 C20 C18 C19 C18 SIMU 0.005 0.01 2 C1 > C3A RIGU Na1 O1 O2 O3 O4 O5 O6 O7 O8 C67 C68 C69 C70 C71 C72 C73 C74 C75 C76 C77 = C78 C79 C80 C81 C82 C1A C1 C2A C2 C3 C3A SI1 L.S. 16 PLAN 80 TEMP -123(2) BOND $H fmap 2 MORE -1 ACTA 52 CONF SHEL 100 0.82 OMIT 0 2 3 OMIT -3 1 3 REM REM REM WGHT 0.032500 34.956501 FVAR 0.12503 0.67422 TH1 8 0.646112 0.140020 0.724113 11.00000 0.01633 0.02007 = 0.02681 0.00044 0.00761 0.00097 TH2 8 0.835649 0.328487 0.800670 11.00000 0.01669 0.01857 = 0.02980 0.00098 0.00971 0.00068 P1 6 0.739713 0.234927 0.765388 11.00000 0.02202 0.02331 = 0.03674 -0.00103 0.00798 -0.00364 SI1 7 0.595932 0.235792 0.592823 11.00000 0.03362 0.04217 = 0.03598 0.01410 0.01779 0.01756 SI2 7 0.742293 -0.035171 0.731980 11.00000 0.01896 0.02018 = 0.03007 0.00070 0.00887 0.00029 SI3 7 0.561417 0.171746 0.828070 11.00000 0.01993 0.02569 = 0.02568 -0.00132 0.00847 -0.00026 SI4 7 0.842697 0.304498 0.944257 11.00000 0.02374 0.02954 = 0.02970 -0.00385 0.00981 -0.00393 SI5 7 0.758254 0.491678 0.717798 11.00000 0.02395 0.02180 = 0.04691 0.00865 0.01563 0.00515 SI6 7 0.952262 0.220942 0.750458 11.00000 0.01638 0.02604 = 0.03025 -0.00271 0.00776 0.00184 N1 3 0.583814 0.183954 0.645126 11.00000 0.02441 0.02142 = 0.03651 0.00107 0.01122 0.00467 N2 3 0.680376 0.019193 0.704871 11.00000 0.02049 0.02452 = 0.00757 -0.00208 -0.00507 0.00056 N3 3 0.584074 0.116751 0.781551 11.00000 0.01957 0.01960 = 0.03232 -0.00603 0.01044 -0.00737 N4 3 0.552262 0.038240 0.682240 11.00000 0.01828 0.02014 = 0.02553 -0.00246 0.00496 0.00512 N5 3 0.850680 0.355574 0.890329 11.00000 0.02033 0.02195 = 0.04277 -0.00466 0.01782 -0.00548 N6 3 0.820299 0.444634 0.753136 11.00000 0.01117 0.02817 = 0.03078 0.00777 0.00644 -0.00152 N7 3 0.930174 0.279651 0.794542 11.00000 0.01911 0.02474 = 0.02780 -0.00117 0.00514 0.00047 N8 3 0.928469 0.433684 0.837079 11.00000 0.02081 0.01513 = 0.03172 0.00313 0.01108 -0.00423 C4 1 0.571592 0.189138 0.525708 11.00000 0.02718 0.06596 = 0.03030 0.01435 0.00721 0.00691 AFIX 13 H4 2 0.583980 0.225859 0.501210 11.00000 -1.20000 AFIX 0 C5 1 0.601580 0.113162 0.518511 11.00000 0.04062 0.07317 = 0.03672 -0.00467 0.01411 0.00219 AFIX 137 H5A 2 0.644794 0.120201 0.526866 11.00000 -1.50000 H5B 2 0.588033 0.096162 0.482393 11.00000 -1.50000 H5C 2 0.591162 0.074354 0.541654 11.00000 -1.50000 AFIX 0 C6 1 0.504398 0.178176 0.504684 11.00000 0.03656 0.12205 = 0.04736 0.00914 0.00092 0.02039 AFIX 137 H6A 2 0.490640 0.135685 0.523109 11.00000 -1.50000 H6B 2 0.496072 0.166439 0.467494 11.00000 -1.50000 H6C 2 0.483601 0.225408 0.510031 11.00000 -1.50000 AFIX 0 C7 1 0.678804 0.251568 0.606406 11.00000 0.04054 0.04344 = 0.02896 0.00069 0.01451 -0.00299 AFIX 13 H7 2 0.689290 0.287237 0.636771 11.00000 -1.20000 AFIX 0 C8 1 0.699177 0.290432 0.561684 11.00000 0.04653 0.05955 = 0.05195 0.01995 0.02340 0.00623 AFIX 137 H8A 2 0.691864 0.256000 0.531589 11.00000 -1.50000 H8B 2 0.741751 0.301888 0.572581 11.00000 -1.50000 H8C 2 0.676946 0.338269 0.552278 11.00000 -1.50000 AFIX 0 C9 1 0.714388 0.177049 0.622518 11.00000 0.02235 0.05072 = 0.04395 -0.00514 0.01320 -0.00490 AFIX 137 H9A 2 0.730887 0.177254 0.660143 11.00000 -1.50000 H9B 2 0.746836 0.173895 0.604600 11.00000 -1.50000 H9C 2 0.688049 0.132650 0.613047 11.00000 -1.50000 AFIX 0 C10 1 0.521297 0.160290 0.640879 11.00000 0.02858 0.04026 = 0.02959 0.00193 0.01204 0.00601 AFIX 23 H10A 2 0.495272 0.185108 0.610193 11.00000 -1.20000 H10B 2 0.508361 0.177299 0.672139 11.00000 -1.20000 AFIX 0 C11 1 0.515452 0.073704 0.635678 11.00000 0.01878 0.03994 = 0.03148 0.00060 0.00607 0.00349 AFIX 23 H11A 2 0.473410 0.058442 0.631634 11.00000 -1.20000 H11B 2 0.528586 0.056329 0.604594 11.00000 -1.20000 AFIX 0 C12 1 0.726154 -0.141066 0.741451 11.00000 0.02655 0.02526 = 0.03023 0.00240 0.00332 0.00364 AFIX 13 H12 2 0.766010 -0.164665 0.755864 11.00000 -1.20000 AFIX 0 C13 1 0.699389 -0.188197 0.693135 11.00000 0.03535 0.02410 = 0.04163 -0.00285 0.00678 -0.00106 AFIX 137 H13A 2 0.657664 -0.173674 0.679890 11.00000 -1.50000 H13B 2 0.701839 -0.242929 0.701995 11.00000 -1.50000 H13C 2 0.721453 -0.178294 0.666451 11.00000 -1.50000 AFIX 0 C14 1 0.690836 -0.155819 0.783045 11.00000 0.04181 0.02525 = 0.04544 0.00213 0.02154 -0.00364 AFIX 137 H14A 2 0.708965 -0.127152 0.814633 11.00000 -1.50000 H14B 2 0.691425 -0.210826 0.790970 11.00000 -1.50000 H14C 2 0.649651 -0.138866 0.769992 11.00000 -1.50000 AFIX 0 C15 1 0.777552 0.007148 0.797756 11.00000 0.02651 0.02504 = 0.02650 0.00206 0.00141 -0.00337 AFIX 13 H15 2 0.797931 0.055167 0.790585 11.00000 -1.20000 AFIX 0 C16 1 0.826307 -0.043195 0.831115 11.00000 0.02646 0.02373 = 0.05008 0.00167 -0.01593 -0.00368 AFIX 137 H16A 2 0.808327 -0.089321 0.842115 11.00000 -1.50000 H16B 2 0.846976 -0.014260 0.861794 11.00000 -1.50000 H16C 2 0.854762 -0.058164 0.810745 11.00000 -1.50000 AFIX 0 C17 1 0.733801 0.032206 0.830299 11.00000 0.03583 0.03577 = 0.03285 -0.01116 0.00236 0.00533 AFIX 137 H17A 2 0.717989 0.083197 0.819001 11.00000 -1.50000 H17B 2 0.754542 0.034110 0.867067 11.00000 -1.50000 H17C 2 0.701024 -0.004739 0.825542 11.00000 -1.50000 AFIX 0 C18 1 0.799522 -0.030579 0.690802 11.00000 0.01791 0.04082 = 0.03669 -0.00864 0.00762 0.00397 AFIX 13 H18 2 0.819733 0.020042 0.699770 11.00000 -1.20000 AFIX 0 C19 1 0.774934 -0.027218 0.632436 11.00000 0.02718 0.04693 = 0.04102 0.00431 0.01112 0.00545 AFIX 137 H19A 2 0.757524 -0.077032 0.620037 11.00000 -1.50000 H19B 2 0.807116 -0.015116 0.615430 11.00000 -1.50000 H19C 2 0.744286 0.012663 0.624160 11.00000 -1.50000 AFIX 0 C20 1 0.849620 -0.089250 0.703199 11.00000 0.02399 0.04807 = 0.04333 -0.00822 0.00559 0.00598 AFIX 137 H20A 2 0.871361 -0.083584 0.739505 11.00000 -1.50000 H20B 2 0.876806 -0.080797 0.680428 11.00000 -1.50000 H20C 2 0.832945 -0.141142 0.697644 11.00000 -1.50000 AFIX 0 C21 1 0.639658 -0.013263 0.658201 11.00000 0.02145 0.02920 = 0.02816 0.00731 0.00608 0.00355 AFIX 23 H21A 2 0.657670 -0.059956 0.647054 11.00000 -1.20000 H21B 2 0.633729 0.024561 0.629543 11.00000 -1.20000 AFIX 0 C22 1 0.580287 -0.033357 0.669130 11.00000 0.01613 0.02481 = 0.02497 -0.00064 -0.00225 -0.00281 AFIX 23 H22A 2 0.554394 -0.057785 0.638211 11.00000 -1.20000 H22B 2 0.585930 -0.069990 0.698461 11.00000 -1.20000 AFIX 0 C23 1 0.476746 0.163655 0.819047 11.00000 0.02505 0.02940 = 0.03591 0.00310 0.01459 -0.00136 AFIX 13 H23 2 0.467036 0.108254 0.811503 11.00000 -1.20000 AFIX 0 C24 1 0.441200 0.208030 0.771725 11.00000 0.02675 0.05201 = 0.04942 0.00367 0.01036 0.00671 AFIX 137 H24A 2 0.446516 0.263322 0.778032 11.00000 -1.50000 H24B 2 0.398957 0.195064 0.766015 11.00000 -1.50000 H24C 2 0.455454 0.194009 0.740940 11.00000 -1.50000 AFIX 0 C25 1 0.452382 0.183296 0.866687 11.00000 0.02977 0.05558 = 0.04547 -0.01482 0.01393 -0.00581 AFIX 137 H25A 2 0.472454 0.151631 0.896203 11.00000 -1.50000 H25B 2 0.409559 0.173082 0.858826 11.00000 -1.50000 H25C 2 0.459600 0.237696 0.875401 11.00000 -1.50000 AFIX 0 C26 1 0.586195 0.273234 0.821337 11.00000 0.02791 0.02619 = 0.04448 -0.00249 0.01388 -0.00684 AFIX 13 H26 2 0.630623 0.271724 0.831052 11.00000 -1.20000 AFIX 0 C27 1 0.569459 0.307380 0.766476 11.00000 0.03070 0.02978 = 0.06060 0.00373 0.01072 -0.00384 AFIX 137 H27A 2 0.578304 0.270072 0.741640 11.00000 -1.50000 H27B 2 0.592450 0.354362 0.765408 11.00000 -1.50000 H27C 2 0.526929 0.319530 0.757317 11.00000 -1.50000 AFIX 0 C28 1 0.568261 0.328744 0.859700 11.00000 0.04155 0.02520 = 0.05249 -0.00793 0.01899 0.00114 AFIX 137 H28A 2 0.524896 0.333987 0.851380 11.00000 -1.50000 H28B 2 0.586372 0.379052 0.857230 11.00000 -1.50000 H28C 2 0.582022 0.308766 0.895076 11.00000 -1.50000 AFIX 0 C29 1 0.594732 0.140584 0.897296 11.00000 0.03519 0.03499 = 0.02931 0.00036 0.01368 0.00747 AFIX 13 H29 2 0.574760 0.171687 0.920004 11.00000 -1.20000 AFIX 0 C30 1 0.583860 0.056500 0.908116 11.00000 0.07344 0.04406 = 0.04012 0.00456 0.01519 0.00318 AFIX 137 H30A 2 0.541267 0.045296 0.896944 11.00000 -1.50000 H30B 2 0.597595 0.046397 0.945408 11.00000 -1.50000 H30C 2 0.605730 0.023746 0.888952 11.00000 -1.50000 AFIX 0 C31 1 0.661629 0.157796 0.914909 11.00000 0.04279 0.06050 = 0.03588 -0.00134 0.00475 0.00854 AFIX 137 H31A 2 0.682573 0.132657 0.891308 11.00000 -1.50000 H31B 2 0.676899 0.138307 0.950236 11.00000 -1.50000 H31C 2 0.668043 0.213393 0.914407 11.00000 -1.50000 AFIX 0 C32 1 0.560394 0.037423 0.775608 11.00000 0.02680 0.03253 = 0.02443 -0.00316 0.01325 -0.00203 AFIX 23 H32A 2 0.538747 0.027005 0.802960 11.00000 -1.20000 H32B 2 0.593825 0.000630 0.780123 11.00000 -1.20000 AFIX 0 C33 1 0.519376 0.025741 0.723389 11.00000 0.02262 0.02554 = 0.02729 -0.00281 0.01379 -0.00422 AFIX 23 H33A 2 0.503124 -0.027080 0.720827 11.00000 -1.20000 H33B 2 0.485731 0.062227 0.718705 11.00000 -1.20000 AFIX 0 C34 1 0.910924 0.302831 1.001779 11.00000 0.03280 0.04791 = 0.03474 -0.00487 0.00656 -0.00239 AFIX 13 H34 2 0.896696 0.278188 1.030732 11.00000 -1.20000 AFIX 0 C35 1 0.961167 0.250537 0.993139 11.00000 0.03171 0.06275 = 0.04764 0.00220 -0.00232 0.00821 AFIX 137 H35A 2 0.946190 0.197992 0.986347 11.00000 -1.50000 H35B 2 0.993964 0.251045 1.024225 11.00000 -1.50000 H35C 2 0.975401 0.269212 0.963334 11.00000 -1.50000 AFIX 0 C36 1 0.938498 0.379645 1.024247 11.00000 0.03583 0.06770 = 0.04005 -0.00828 0.00624 -0.01943 AFIX 137 H36A 2 0.957530 0.404512 0.999180 11.00000 -1.50000 H36B 2 0.968241 0.370116 1.056652 11.00000 -1.50000 H36C 2 0.907268 0.413184 1.031204 11.00000 -1.50000 AFIX 0 C37 1 0.777000 0.339962 0.969748 11.00000 0.03606 0.04031 = 0.03049 0.00052 0.01591 -0.00538 AFIX 13 H37 2 0.760553 0.293498 0.983599 11.00000 -1.20000 AFIX 0 C38 1 0.788189 0.398395 1.013592 11.00000 0.04157 0.06132 = 0.05533 -0.01255 0.02626 -0.01258 AFIX 137 H38A 2 0.806141 0.444641 1.002726 11.00000 -1.50000 H38B 2 0.815209 0.376388 1.044300 11.00000 -1.50000 H38C 2 0.750431 0.411832 1.022021 11.00000 -1.50000 AFIX 0 C39 1 0.727304 0.369455 0.925262 11.00000 0.03183 0.06951 = 0.05788 -0.00834 0.02420 -0.00287 AFIX 137 H39A 2 0.740548 0.416227 0.910760 11.00000 -1.50000 H39B 2 0.692042 0.380917 0.938379 11.00000 -1.50000 H39C 2 0.717470 0.330126 0.898134 11.00000 -1.50000 AFIX 0 C40 1 0.823633 0.202041 0.922735 11.00000 0.02257 0.03913 = 0.03094 0.00308 0.00757 -0.00274 AFIX 13 H40 2 0.782312 0.203855 0.900379 11.00000 -1.20000 AFIX 0 C41 1 0.862000 0.167297 0.888817 11.00000 0.04481 0.03466 = 0.03727 -0.00509 0.01113 -0.00214 AFIX 137 H41A 2 0.843747 0.177801 0.852196 11.00000 -1.50000 H41B 2 0.865056 0.111669 0.894418 11.00000 -1.50000 H41C 2 0.901785 0.190152 0.898100 11.00000 -1.50000 AFIX 0 C42 1 0.820768 0.148029 0.968313 11.00000 0.04742 0.03628 = 0.05372 0.00514 0.01962 -0.00446 AFIX 137 H42A 2 0.860948 0.139881 0.989823 11.00000 -1.50000 H42B 2 0.803672 0.098629 0.954634 11.00000 -1.50000 H42C 2 0.795867 0.171300 0.989406 11.00000 -1.50000 AFIX 0 C43 1 0.867523 0.437214 0.900446 11.00000 0.02257 0.02939 = 0.03792 -0.00919 0.01711 -0.00009 AFIX 23 H43A 2 0.867211 0.450684 0.936683 11.00000 -1.20000 H43B 2 0.838657 0.470693 0.876867 11.00000 -1.20000 AFIX 0 C44 1 0.929979 0.449344 0.891397 11.00000 0.02537 0.02793 = 0.04814 -0.01108 0.01486 -0.00947 AFIX 23 H44A 2 0.943024 0.502872 0.900065 11.00000 -1.20000 H44B 2 0.958551 0.414415 0.914025 11.00000 -1.20000 AFIX 0 C45 1 1.017466 0.266754 0.727908 11.00000 0.02363 0.03169 = 0.03908 -0.00242 0.01284 0.00690 AFIX 13 H45 2 1.045068 0.286704 0.760105 11.00000 -1.20000 AFIX 0 C46 1 1.001219 0.335962 0.692190 11.00000 0.02879 0.03957 = 0.05400 0.01096 0.01696 0.00800 AFIX 137 H46A 2 0.978226 0.318891 0.658117 11.00000 -1.50000 H46B 2 1.037603 0.361546 0.688230 11.00000 -1.50000 H46C 2 0.977378 0.371960 0.707251 11.00000 -1.50000 AFIX 0 C47 1 1.054777 0.211187 0.703325 11.00000 0.03482 0.05569 = 0.05741 -0.00071 0.02569 0.01164 AFIX 137 H47A 2 1.069137 0.168952 0.727467 11.00000 -1.50000 H47B 2 1.088761 0.238759 0.695925 11.00000 -1.50000 H47C 2 1.030179 0.190487 0.670939 11.00000 -1.50000 AFIX 0 C48 1 0.981520 0.124931 0.778077 11.00000 0.01880 0.03470 = 0.03535 -0.00785 0.00970 0.00486 AFIX 13 H48 2 0.995955 0.097899 0.750083 11.00000 -1.20000 AFIX 0 C49 1 1.034622 0.128256 0.825537 11.00000 0.04442 0.02652 = 0.04693 0.00066 0.00849 0.00676 AFIX 137 H49A 2 1.064972 0.162950 0.818211 11.00000 -1.50000 H49B 2 1.051509 0.076724 0.832939 11.00000 -1.50000 H49C 2 1.021205 0.147213 0.855689 11.00000 -1.50000 AFIX 0 C50 1 0.933431 0.073363 0.791353 11.00000 0.03599 0.03587 = 0.05579 -0.00067 0.00992 -0.00637 AFIX 137 H50A 2 0.919774 0.095742 0.820440 11.00000 -1.50000 H50B 2 0.949942 0.022177 0.801061 11.00000 -1.50000 H50C 2 0.899857 0.069228 0.761038 11.00000 -1.50000 AFIX 0 C51 1 0.885415 0.202539 0.695542 11.00000 0.02799 0.04130 = 0.02691 0.01102 0.00788 0.00071 AFIX 13 H51 2 0.855083 0.177897 0.711641 11.00000 -1.20000 AFIX 0 C52 1 0.897340 0.145272 0.655648 11.00000 0.05881 0.06357 = 0.03567 -0.02146 0.00189 0.00050 AFIX 137 H52A 2 0.919493 0.170698 0.633092 11.00000 -1.50000 H52B 2 0.859472 0.126108 0.634609 11.00000 -1.50000 H52C 2 0.920719 0.102205 0.673604 11.00000 -1.50000 AFIX 0 C53 1 0.856206 0.276218 0.669043 11.00000 0.03003 0.04958 = 0.03838 0.00423 -0.00805 -0.00047 AFIX 137 H53A 2 0.855750 0.315494 0.695438 11.00000 -1.50000 H53B 2 0.815361 0.264948 0.650137 11.00000 -1.50000 H53C 2 0.878925 0.295088 0.644694 11.00000 -1.50000 AFIX 0 C54 1 0.978286 0.309798 0.836403 11.00000 0.02307 0.02639 = 0.03731 0.00290 0.01305 0.01071 AFIX 23 H54A 2 1.016248 0.284829 0.834837 11.00000 -1.20000 H54B 2 0.969879 0.297512 0.870452 11.00000 -1.20000 AFIX 0 C55 1 0.984181 0.397242 0.831370 11.00000 0.01485 0.03044 = 0.04109 -0.00221 0.01525 -0.00163 AFIX 23 H55A 2 1.018049 0.416384 0.858606 11.00000 -1.20000 H55B 2 0.991596 0.410082 0.797043 11.00000 -1.20000 AFIX 0 C56 1 0.761530 0.601560 0.722697 11.00000 0.02869 0.01966 = 0.05672 0.00656 0.02154 0.00111 AFIX 13 H56 2 0.719886 0.618721 0.707280 11.00000 -1.20000 AFIX 0 C57 1 0.774882 0.630955 0.778454 11.00000 0.06186 0.02689 = 0.05781 0.00053 0.02969 0.00880 AFIX 137 H57A 2 0.746608 0.608408 0.796559 11.00000 -1.50000 H57B 2 0.771199 0.687024 0.778320 11.00000 -1.50000 H57C 2 0.815421 0.616324 0.796318 11.00000 -1.50000 AFIX 0 C58 1 0.799582 0.645352 0.691703 11.00000 0.04646 0.02811 = 0.07150 0.00828 0.02611 -0.00562 AFIX 137 H58A 2 0.841617 0.632836 0.705493 11.00000 -1.50000 H58B 2 0.793674 0.700719 0.694829 11.00000 -1.50000 H58C 2 0.787666 0.630367 0.655065 11.00000 -1.50000 AFIX 0 C59 1 0.743098 0.465815 0.646315 11.00000 0.04642 0.02175 = 0.05296 0.01312 0.00771 -0.00002 AFIX 13 H59 2 0.728224 0.411709 0.643956 11.00000 -1.20000 AFIX 0 C60 1 0.798519 0.464272 0.623922 11.00000 0.05270 0.03995 = 0.04516 0.01063 0.01963 0.00917 AFIX 137 H60A 2 0.813090 0.516772 0.621972 11.00000 -1.50000 H60B 2 0.788312 0.441743 0.589054 11.00000 -1.50000 H60C 2 0.829534 0.433316 0.646445 11.00000 -1.50000 AFIX 0 C61 1 0.694342 0.512303 0.609558 11.00000 0.04688 0.07148 = 0.04133 0.00885 -0.00082 0.00371 AFIX 137 H61A 2 0.657381 0.509106 0.621418 11.00000 -1.50000 H61B 2 0.687800 0.491355 0.574334 11.00000 -1.50000 H61C 2 0.706742 0.566105 0.609473 11.00000 -1.50000 AFIX 0 C62 1 0.692316 0.458488 0.742876 11.00000 0.03261 0.02544 = 0.04374 0.00795 0.01977 0.00642 AFIX 13 H62 2 0.679397 0.407892 0.726133 11.00000 -1.20000 AFIX 0 C63 1 0.705525 0.446144 0.801621 11.00000 0.02475 0.04210 = 0.04761 0.00662 0.01602 0.00107 AFIX 137 H63A 2 0.732189 0.402052 0.811076 11.00000 -1.50000 H63B 2 0.668303 0.436289 0.812056 11.00000 -1.50000 H63C 2 0.724550 0.492179 0.819381 11.00000 -1.50000 AFIX 0 C64 1 0.639322 0.513795 0.727088 11.00000 0.01889 0.01418 = 0.04626 0.00719 0.00619 0.00964 AFIX 137 H64A 2 0.649986 0.563761 0.743695 11.00000 -1.50000 H64B 2 0.605081 0.492716 0.738237 11.00000 -1.50000 H64C 2 0.629133 0.520149 0.689273 11.00000 -1.50000 AFIX 0 C65 1 0.878972 0.479973 0.750549 11.00000 0.02476 0.04405 = 0.06101 0.01915 0.02594 0.01255 AFIX 23 H65A 2 0.871831 0.526041 0.728040 11.00000 -1.20000 H65B 2 0.902144 0.442768 0.735038 11.00000 -1.20000 AFIX 0 C66 1 0.914150 0.502333 0.804158 11.00000 0.01694 0.02899 = 0.05761 0.00558 0.01752 0.00067 AFIX 23 H66A 2 0.951339 0.528369 0.801500 11.00000 -1.20000 H66B 2 0.890677 0.538627 0.820066 11.00000 -1.20000 AFIX 0 PART 1 C1 1 0.546025 0.325148 0.582506 21.00000 0.06800 0.04731 = 0.05921 0.02583 0.03683 0.03144 AFIX 13 H1 2 0.503382 0.309066 0.575050 21.00000 -1.20000 AFIX 0 C2 1 0.556100 0.379267 0.538038 21.00000 0.07745 0.05251 = 0.06323 0.03397 0.03940 0.03747 AFIX 137 H2A 2 0.596736 0.399501 0.547218 21.00000 -1.50000 H2B 2 0.527761 0.421959 0.533548 21.00000 -1.50000 H2C 2 0.550097 0.350155 0.505561 21.00000 -1.50000 AFIX 0 C3 1 0.560524 0.374053 0.631513 21.00000 0.07233 0.04421 = 0.06200 0.02414 0.03134 0.03616 AFIX 137 H3A 2 0.553750 0.343987 0.660854 21.00000 -1.50000 H3B 2 0.534907 0.419569 0.626568 21.00000 -1.50000 H3C 2 0.602247 0.390077 0.638658 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C1A 1 0.571578 0.345789 0.594110 -21.00000 0.07027 0.04772 = 0.06039 0.02671 0.03813 0.03409 AFIX 13 H1A 2 0.606482 0.379336 0.609035 -21.00000 -1.20000 AFIX 0 C2A 1 0.539185 0.372816 0.538752 -21.00000 0.07313 0.05243 = 0.06222 0.02967 0.03835 0.03430 AFIX 137 H2AA 2 0.566882 0.402001 0.523303 -21.00000 -1.50000 H2AB 2 0.505421 0.405518 0.540985 -21.00000 -1.50000 H2AC 2 0.524834 0.327964 0.517073 -21.00000 -1.50000 AFIX 0 C3A 1 0.522372 0.355757 0.623380 -21.00000 0.06827 0.04663 = 0.06078 0.02377 0.03684 0.03524 AFIX 137 H3AA 2 0.485217 0.334040 0.602737 -21.00000 -1.50000 H3AB 2 0.516786 0.410524 0.629303 -21.00000 -1.50000 H3AC 2 0.533623 0.329086 0.656832 -21.00000 -1.50000 AFIX 0 PART 0 NA1 4 0.755510 0.734982 0.977981 11.00000 0.02335 0.03372 = 0.03575 0.00078 0.00853 -0.00180 O1 5 0.697771 0.695528 1.040479 11.00000 0.03193 0.07762 = 0.05182 0.00975 0.00974 -0.00533 O2 5 0.702925 0.612054 0.952679 11.00000 0.03320 0.05101 = 0.07628 -0.01451 0.00947 -0.00559 O3 5 0.684229 0.746253 0.895855 11.00000 0.04198 0.09834 = 0.05521 0.02447 0.01154 -0.00439 O4 5 0.680031 0.831758 0.983346 11.00000 0.04153 0.05748 = 0.10162 -0.00519 0.01994 -0.00056 O5 5 0.815761 0.791598 1.058331 11.00000 0.03292 0.04248 = 0.04918 -0.00922 0.00999 -0.00310 O6 5 0.830630 0.644498 1.022160 11.00000 0.03403 0.04387 = 0.04937 -0.00392 0.00209 0.00023 O7 5 0.823812 0.696496 0.922568 11.00000 0.04535 0.05359 = 0.05152 -0.00453 0.01965 -0.00075 O8 5 0.811359 0.847077 0.958153 11.00000 0.03464 0.04284 = 0.05231 0.00522 0.00228 -0.00586 C67 1 0.639278 0.814660 1.009985 11.00000 0.06118 0.06915 = 0.10516 -0.00511 0.03021 0.01039 AFIX 23 H67A 2 0.606540 0.784400 0.988155 11.00000 -1.20000 H67B 2 0.622431 0.862220 1.021168 11.00000 -1.20000 AFIX 0 C68 1 0.669391 0.770137 1.054895 11.00000 0.02853 0.09245 = 0.06466 -0.00649 0.02458 0.00931 AFIX 23 H68A 2 0.640464 0.756836 1.075713 11.00000 -1.20000 H68B 2 0.700803 0.802238 1.076837 11.00000 -1.20000 AFIX 0 C69 1 0.658306 0.638950 1.026608 11.00000 0.05445 0.08660 = 0.06211 0.01150 0.01417 -0.01428 AFIX 23 H69A 2 0.622052 0.658185 1.002159 11.00000 -1.20000 H69B 2 0.646963 0.617362 1.057474 11.00000 -1.20000 AFIX 0 C70 1 0.687454 0.580654 1.001691 11.00000 0.03627 0.05407 = 0.08339 0.00876 0.01595 -0.01108 AFIX 23 H70A 2 0.660806 0.535754 0.992551 11.00000 -1.20000 H70B 2 0.724228 0.563267 1.026300 11.00000 -1.20000 AFIX 0 C71 1 0.657069 0.612388 0.911244 11.00000 0.05572 0.07932 = 0.07669 -0.01036 0.00619 -0.00334 AFIX 23 H71A 2 0.620464 0.629418 0.921175 11.00000 -1.20000 H71B 2 0.650311 0.560212 0.896167 11.00000 -1.20000 AFIX 0 C72 1 0.671997 0.665249 0.873893 11.00000 0.04575 0.09278 = 0.05832 -0.00389 0.00182 -0.00832 AFIX 23 H72A 2 0.638761 0.667029 0.842596 11.00000 -1.20000 H72B 2 0.707608 0.646068 0.863246 11.00000 -1.20000 AFIX 0 C73 1 0.634165 0.785631 0.891904 11.00000 0.05433 0.10224 = 0.08136 0.01922 0.01936 0.00207 AFIX 23 H73A 2 0.604417 0.754938 0.904527 11.00000 -1.20000 H73B 2 0.617057 0.801025 0.855480 11.00000 -1.20000 AFIX 0 C74 1 0.652991 0.854887 0.925793 11.00000 0.04015 0.06425 = 0.09963 0.01751 0.00852 0.00693 AFIX 23 H74A 2 0.618137 0.888541 0.924201 11.00000 -1.20000 H74B 2 0.682822 0.884341 0.912440 11.00000 -1.20000 AFIX 0 C75 1 0.842226 0.731402 1.092066 11.00000 0.03485 0.05137 = 0.04305 -0.00501 -0.00118 -0.00533 AFIX 23 H75A 2 0.811175 0.704607 1.105453 11.00000 -1.20000 H75B 2 0.871337 0.753372 1.122067 11.00000 -1.20000 AFIX 0 C76 1 0.873486 0.673928 1.064229 11.00000 0.04002 0.04501 = 0.04692 0.00228 0.00230 -0.00012 AFIX 23 H76A 2 0.905679 0.699563 1.051742 11.00000 -1.20000 H76B 2 0.891097 0.631953 1.088137 11.00000 -1.20000 AFIX 0 C77 1 0.853305 0.601641 0.985465 11.00000 0.05268 0.04688 = 0.06259 -0.00545 0.01404 0.00734 AFIX 23 H77A 2 0.822041 0.566460 0.966511 11.00000 -1.20000 H77B 2 0.887191 0.569996 1.004081 11.00000 -1.20000 AFIX 0 C78 1 0.872698 0.650434 0.948680 11.00000 0.05298 0.05025 = 0.07129 -0.00584 0.02519 0.00772 AFIX 23 H78A 2 0.905698 0.683716 0.966981 11.00000 -1.20000 H78B 2 0.887194 0.618685 0.923213 11.00000 -1.20000 AFIX 0 C79 1 0.841206 0.765097 0.898802 11.00000 0.04096 0.06425 = 0.03859 0.00888 0.00743 -0.00705 AFIX 23 H79A 2 0.807245 0.783671 0.871431 11.00000 -1.20000 H79B 2 0.874206 0.752625 0.882268 11.00000 -1.20000 AFIX 0 C80 1 0.860578 0.827037 0.938447 11.00000 0.03839 0.05079 = 0.04844 0.01513 0.00968 -0.00522 AFIX 23 H80A 2 0.893418 0.808314 0.966816 11.00000 -1.20000 H80B 2 0.874802 0.872308 0.922267 11.00000 -1.20000 AFIX 0 C81 1 0.825247 0.895473 1.003010 11.00000 0.04155 0.03785 = 0.06334 -0.00066 0.00989 -0.00849 AFIX 23 H81A 2 0.788215 0.918960 1.008398 11.00000 -1.20000 H81B 2 0.851778 0.937422 0.997127 11.00000 -1.20000 AFIX 0 C82 1 0.855623 0.850633 1.051756 11.00000 0.04058 0.04780 = 0.04860 -0.01327 0.00700 -0.01020 AFIX 23 H82A 2 0.893502 0.828251 1.047493 11.00000 -1.20000 H82B 2 0.864228 0.884957 1.082403 11.00000 -1.20000 AFIX 0 O9 5 1.053233 -0.013325 0.961549 11.00000 0.06147 0.09808 = 0.10396 -0.02685 0.02988 -0.00706 C83 1 1.058300 -0.057433 0.919263 11.00000 0.12350 0.08561 = 0.07200 -0.01167 0.03903 -0.00003 AFIX 137 H83A 2 1.029125 -0.040065 0.888281 11.00000 -1.50000 H83B 2 1.050915 -0.111458 0.925994 11.00000 -1.50000 H83C 2 1.098443 -0.051966 0.913615 11.00000 -1.50000 AFIX 0 C84 1 0.998286 -0.018596 0.974238 11.00000 0.05928 0.07377 = 0.11849 -0.01702 0.03516 0.00123 AFIX 23 H84A 2 0.986981 -0.073236 0.975715 11.00000 -1.20000 H84B 2 0.967537 0.007180 0.947237 11.00000 -1.20000 AFIX 0 HKLF 4 REM thew8_a.res in P2(1)/c REM R1 = 0.0557 for 13798 Fo > 4sig(Fo) and 0.0923 for all 19666 data REM 1067 parameters refined using 963 restraints END WGHT 0.0326 34.8197 REM Highest difference peak 2.613, deepest hole -1.313, 1-sigma level 0.170 Q1 1 0.4580 0.3282 0.6483 11.00000 0.05 2.61 Q2 1 1.0264 0.1411 0.8774 11.00000 0.05 2.22 Q3 1 0.8351 0.3283 0.7619 11.00000 0.05 2.03 Q4 1 0.6539 0.1396 0.6874 11.00000 0.05 1.92 Q5 1 0.6391 0.1420 0.7619 11.00000 0.05 1.90 Q6 1 0.8348 -0.0485 0.7994 11.00000 0.05 1.79 Q7 1 0.8284 0.3274 0.8405 11.00000 0.05 1.75 Q8 1 0.6205 0.1749 0.6918 11.00000 0.05 1.75 Q9 1 0.8121 0.2923 0.7706 11.00000 0.05 1.68 Q10 1 0.8099 0.3640 0.7717 11.00000 0.05 1.68 Q11 1 0.8595 0.2929 0.8324 11.00000 0.05 1.62 Q12 1 0.6471 0.7048 1.0443 11.00000 0.05 1.61 Q13 1 1.0275 0.5160 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0.05 0.64 Q57 1 0.8089 0.2086 0.8191 11.00000 0.05 0.63 Q58 1 1.0098 -0.0345 0.9318 11.00000 0.05 0.63 Q59 1 0.8582 0.2779 0.7850 11.00000 0.05 0.63 Q60 1 0.7204 0.1789 0.8188 11.00000 0.05 0.63 Q61 1 0.7638 0.1884 0.7522 11.00000 0.05 0.62 Q62 1 0.6722 0.3032 0.6505 11.00000 0.05 0.62 Q63 1 0.9701 0.2511 0.7807 11.00000 0.05 0.62 Q64 1 0.5683 0.0111 0.6786 11.00000 0.05 0.61 Q65 1 0.5774 0.1828 0.8691 11.00000 0.05 0.61 Q66 1 0.7458 0.3619 0.9023 11.00000 0.05 0.61 Q67 1 0.8099 0.8109 1.0187 11.00000 0.05 0.61 Q68 1 0.8413 0.1283 0.8692 11.00000 0.05 0.60 Q69 1 0.8392 0.2415 0.8484 11.00000 0.05 0.60 Q70 1 0.8391 0.0197 0.8039 11.00000 0.05 0.60 Q71 1 0.8411 0.2875 0.7300 11.00000 0.05 0.60 Q72 1 0.6918 0.2354 0.7010 11.00000 0.05 0.59 Q73 1 0.6237 0.2576 0.7425 11.00000 0.05 0.59 Q74 1 0.8768 0.2328 0.8775 11.00000 0.05 0.59 Q75 1 0.8261 0.7439 0.7967 11.00000 0.05 0.59 Q76 1 0.8584 0.2056 0.7382 11.00000 0.05 0.59 Q77 1 0.9596 0.0320 0.9818 11.00000 0.05 0.59 Q78 1 0.7699 0.3650 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104.06 34.45 -11 3 -7 33.49 18.19 -11 -3 -7 77.82 31.48 11 -3 8 155.30 29.85 -11 -3 -8 187.71 33.62 11 -3 8 181.27 34.03 11 3 8 230.97 48.16 -11 3 -8 180.20 43.83 -11 -3 -8 216.47 48.48 11 -3 8 240.26 51.48 -11 -3 -9 1.61 4.48 11 -3 9 -6.20 10.07 11 3 9 37.89 23.60 -11 3 -9 13.20 16.20 -11 -3 -9 21.06 21.68 11 -3 9 -6.37 7.23 11 -3 10 99.73 20.96 -11 -3 -10 121.99 25.16 11 -3 10 125.28 25.36 11 3 10 136.01 43.83 -11 3 -10 88.34 30.33 11 -3 10 153.42 47.03 -11 -3 -10 146.96 43.75 -11 -3 -11 40.55 13.12 11 -3 11 36.82 12.49 11 3 11 83.78 35.35 11 -3 11 61.23 18.25 -11 3 -11 36.53 20.86 11 -3 11 97.52 41.22 -11 -3 -11 40.76 28.32 -11 -3 -12 16.97 4.94 11 3 12 33.23 25.37 -11 -3 -13 -5.60 8.42 11 3 13 33.80 28.30 11 -3 13 37.11 31.37 -11 -3 -14 59.68 12.80 11 3 14 91.63 38.19 11 -3 14 40.49 5.15 11 3 15 144.53 20.00 11 3 15 195.97 53.81 11 -3 15 164.34 49.14 11 3 16 158.06 47.52 11 -3 16 45.09 26.11 11 3 17 328.57 76.01 11 -3 17 405.85 85.65 11 3 18 8.65 18.31 11 -3 18 -175.40 58.52 11 3 19 374.97 88.15 11 -3 19 294.67 70.58 11 3 20 -36.35 33.84 11 3 21 294.02 77.46 11 -3 21 272.48 81.14 11 3 22 -43.34 42.71 11 -3 22 149.16 58.51 11 3 23 -12.91 44.24 11 -3 23 149.71 62.58 11 3 24 -114.83 53.72 11 -3 24 170.34 68.12 11 -3 25 100.16 50.71 11 3 25 -120.42 56.42 11 3 26 -59.29 48.03 11 -3 26 72.79 46.75 -11 4 35 144.73 57.17 -11 4 34 35.65 28.84 -11 4 34 40.35 32.72 -11 -4 34 41.30 24.91 -11 4 33 136.12 47.75 -11 4 33 74.28 37.48 -11 -4 33 149.60 62.71 -11 4 32 72.22 36.69 -11 4 32 42.67 29.00 -11 -4 32 91.72 51.29 -11 4 31 60.69 32.80 -11 4 31 81.62 39.77 -11 -4 31 84.37 39.86 -11 4 30 61.40 26.69 -11 4 30 89.85 45.63 -11 -4 30 79.32 41.37 -11 -4 29 20.47 18.19 -11 4 29 12.36 20.97 -11 4 29 -0.26 4.65 -11 -4 29 25.39 26.91 -11 -4 28 60.06 24.20 -11 4 28 69.19 37.57 -11 4 28 28.18 12.34 -11 -4 28 30.33 17.62 -11 4 27 17.63 18.60 -11 4 27 27.59 19.30 -11 -4 27 15.27 8.71 11 -4 -27 66.88 33.33 -11 -4 27 14.74 17.19 -11 4 26 132.07 46.55 -11 4 26 138.98 50.03 -11 -4 26 133.77 38.39 -11 -4 26 119.74 50.41 11 -4 -26 136.50 47.08 -11 4 25 127.04 30.64 -11 4 25 100.43 39.75 -11 4 25 121.20 43.29 -11 -4 25 114.78 33.01 11 -4 -25 100.06 30.71 -11 -4 25 82.04 34.88 -11 4 24 79.07 33.59 -11 4 24 52.21 32.25 -11 4 24 77.63 23.25 -11 -4 24 84.36 30.41 11 -4 -24 82.12 32.50 11 -4 -24 44.57 25.56 -11 -4 24 77.73 37.54 11 4 -24 51.61 21.56 -11 4 23 442.04 53.27 -11 4 23 341.85 75.50 -11 4 23 502.18 85.09 11 -4 -23 381.90 74.21 -11 -4 23 486.68 63.87 11 -4 -23 434.56 74.44 -11 -4 23 365.60 80.24 11 4 -23 442.46 68.05 -11 4 22 -21.40 18.85 -11 4 22 -14.20 20.02 -11 -4 22 19.13 11.87 -11 4 22 0.36 4.34 11 4 -22 -22.37 20.11 -11 -4 22 -16.36 21.30 11 -4 -22 -16.17 15.76 -11 4 21 596.02 85.40 -11 4 21 471.75 82.73 -11 4 21 555.62 55.98 -11 -4 21 607.67 66.62 11 -4 -21 501.32 83.55 11 -4 -21 534.79 76.50 -11 -4 21 545.14 95.22 11 4 -21 588.04 72.78 -11 4 20 7.79 10.22 -11 4 20 9.52 11.47 11 -4 -20 13.29 6.26 -11 -4 20 31.68 14.59 11 -4 -20 9.94 12.52 11 4 -20 51.24 25.05 -11 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3.56 11 4 -11 0.14 5.30 11 -4 -11 5.05 1.65 11 4 -10 854.43 54.12 -11 4 10 717.13 89.00 11 -4 -10 823.44 82.75 11 4 -10 825.22 91.10 11 -4 -10 703.32 84.07 -11 -4 10 889.94 95.44 11 -4 -10 838.20 96.81 -11 -4 10 879.73 93.01 -11 -4 10 778.12 48.58 -11 -4 10 788.11 89.87 11 -4 -10 802.88 60.75 11 -4 -10 779.57 64.75 -11 4 9 18.31 10.31 11 -4 -9 17.08 11.83 11 -4 -9 27.23 12.67 11 -4 -9 13.57 2.83 -11 -4 9 53.55 27.53 11 -4 -9 32.70 20.04 11 4 -9 19.11 5.25 -11 -4 9 29.88 9.48 -11 -4 9 -0.03 9.77 11 -4 -9 32.35 13.66 -11 -4 9 18.57 7.85 -11 4 8 45.62 20.62 11 -4 -8 50.54 18.84 11 -4 -8 55.46 16.02 11 -4 -8 69.39 24.48 11 4 -8 57.89 22.60 -11 -4 8 75.99 30.98 -11 -4 8 51.86 8.56 -11 -4 8 52.40 24.34 -11 -4 8 56.53 23.41 11 -4 -8 29.43 6.37 11 -4 -8 63.14 28.64 11 -4 -7 1023.96 91.44 -11 -4 7 1044.34 105.44 -11 -4 7 1119.20 104.69 11 -4 -7 1097.40 101.35 11 -4 -7 949.33 99.18 11 4 -7 1184.68 104.99 -11 -4 7 1089.46 96.91 11 -4 -7 952.10 71.29 -11 -4 7 1198.86 59.90 11 -4 -7 1018.66 67.50 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11 -4 -1 129.75 28.91 -11 4 1 96.44 23.88 -11 -4 1 136.94 26.94 11 4 0 941.82 97.75 11 -4 0 947.26 89.68 11 -4 0 924.11 87.33 11 4 0 853.51 69.23 -11 -4 0 903.86 72.29 11 -4 0 836.98 69.49 -11 4 0 770.63 73.53 -11 -4 0 916.97 68.55 11 -4 1 162.90 36.91 11 -4 1 99.66 26.86 11 4 1 130.67 28.61 -11 -4 -1 49.90 12.97 11 -4 1 129.50 26.98 -11 4 -1 139.73 31.51 -11 -4 -1 150.76 31.02 11 4 1 135.45 37.09 11 -4 2 294.81 51.99 11 -4 2 310.24 48.75 -11 -4 -2 323.43 40.70 11 4 2 312.19 43.68 11 -4 2 310.41 45.55 11 4 2 328.30 56.20 -11 4 -2 277.34 46.01 -11 -4 -2 336.35 45.13 11 -4 3 289.73 47.32 11 4 3 285.72 42.17 11 -4 3 296.27 47.24 -11 4 -3 210.29 38.33 -11 -4 -3 304.14 45.29 11 4 3 294.02 54.10 -11 -4 -3 329.45 36.36 11 -4 3 274.65 49.20 -11 -4 -4 103.47 20.23 11 -4 4 63.69 18.94 11 4 4 96.38 27.44 11 -4 4 68.07 21.94 -11 4 -4 49.99 14.75 11 -4 4 84.03 23.98 -11 -4 -5 1136.74 58.03 11 -4 5 1118.51 88.77 11 4 5 1113.97 95.10 11 -4 5 1094.70 98.61 -11 4 -5 956.44 92.99 -11 -4 -5 1211.35 100.77 11 -4 6 420.10 53.51 11 -4 6 422.48 57.26 11 4 6 435.10 64.25 11 -4 6 409.08 62.51 -11 4 -6 369.75 60.89 -11 -4 -6 505.12 69.45 -11 -4 -6 440.21 32.48 11 -4 7 1062.19 86.20 11 -4 7 1177.60 90.77 11 4 7 1104.29 105.21 11 -4 7 1000.54 100.60 -11 4 -7 1069.50 104.44 -11 -4 -7 1185.78 108.57 11 -4 8 57.50 18.96 11 -4 8 59.55 19.65 11 -4 8 42.89 15.08 11 4 8 78.25 26.20 -11 4 -8 71.60 26.15 -11 -4 -8 80.19 29.54 11 -4 9 430.59 49.71 11 -4 9 551.81 58.36 11 4 9 462.05 70.89 11 -4 9 426.88 67.29 -11 4 -9 379.93 65.32 -11 -4 -9 523.41 78.24 11 -4 10 116.03 23.75 -11 -4 -10 164.34 32.31 11 -4 10 146.48 29.42 11 -4 10 79.78 34.10 11 4 10 106.08 33.73 -11 4 -10 150.71 41.17 -11 -4 -10 164.67 45.92 11 -4 10 212.97 57.86 11 -4 11 226.02 33.35 -11 -4 -11 276.55 39.10 -11 4 -11 199.12 47.72 11 4 11 210.05 49.01 11 -4 11 300.07 64.63 11 -4 12 33.62 11.77 -11 -4 -12 52.50 18.21 11 4 12 49.17 19.85 11 -4 12 77.98 46.93 -11 -4 -13 116.04 24.49 11 -4 13 87.30 18.38 11 4 13 72.23 32.88 11 4 14 30.21 15.10 -11 -4 -14 66.51 16.17 -11 -4 -15 450.46 41.60 11 4 15 487.77 88.82 11 -4 15 504.22 91.49 -11 -4 -16 -8.48 6.21 11 4 16 -1.75 3.83 11 -4 16 -0.56 25.75 11 4 17 307.02 72.46 11 -4 17 378.68 84.72 11 4 18 -56.45 41.14 11 -4 18 -24.84 33.87 11 4 19 359.30 83.76 11 -4 19 301.86 67.35 11 4 20 -9.50 35.39 11 -4 20 -128.77 53.15 11 4 21 -54.91 45.35 11 -4 21 -59.51 70.38 11 4 22 83.60 34.52 11 -4 22 5.23 40.62 11 4 23 -17.91 48.25 11 -4 23 -18.12 7.10 11 4 24 -15.87 39.09 11 -4 24 252.04 84.76 11 4 25 -107.41 70.13 11 -4 25 107.95 67.06 11 4 26 17.19 28.23 11 -4 26 235.79 83.79 -11 5 35 17.00 17.37 -11 5 34 11.41 20.55 -11 5 34 -33.69 27.94 -11 5 33 -10.55 24.27 -11 5 33 10.07 18.81 -11 -5 33 -23.92 25.65 -11 5 32 92.43 41.40 -11 5 32 126.08 51.65 -11 -5 32 114.75 53.94 -11 5 31 17.29 16.94 -11 5 31 -2.21 16.99 -11 -5 31 -13.89 23.20 -11 5 30 300.55 75.46 -11 5 30 302.42 79.15 -11 -5 30 349.69 92.64 -11 5 29 72.88 30.79 11 -5 -29 184.13 60.02 -11 5 29 98.36 46.40 -11 -5 29 104.47 37.17 -11 -5 29 98.12 46.86 -11 5 28 517.51 95.76 -11 5 28 546.16 100.02 -11 -5 28 582.21 81.47 11 -5 -28 467.59 90.26 -11 -5 28 541.03 113.64 -11 5 27 126.82 47.48 -11 5 27 107.61 44.22 11 -5 -27 132.87 44.00 -11 -5 27 106.19 35.09 -11 -5 27 114.23 53.92 -11 5 26 338.40 72.96 11 -5 -26 354.70 72.05 -11 5 26 329.86 74.31 -11 -5 26 360.41 63.31 -11 -5 26 375.77 92.59 -11 5 25 104.06 40.47 -11 5 25 129.17 48.04 11 -5 -25 146.10 47.08 -11 -5 25 126.73 35.37 -11 -5 25 82.49 39.49 -11 5 24 161.11 49.49 -11 5 24 197.72 56.24 11 -5 -24 166.75 51.78 -11 -5 24 236.93 48.67 -11 5 24 186.82 30.89 11 5 -24 235.97 54.12 -11 -5 24 203.54 64.28 -11 5 23 17.01 13.63 -11 5 23 4.91 11.56 11 -5 -23 32.55 16.86 -11 -5 23 58.48 23.84 11 5 -23 37.54 22.56 -11 -5 23 23.81 14.93 -11 5 23 25.42 10.52 -11 5 22 41.23 20.65 -11 5 22 71.53 31.15 -11 5 22 58.01 16.33 11 -5 -22 60.05 25.82 -11 -5 22 85.54 28.73 11 -5 -22 94.94 36.01 11 5 -22 84.64 34.19 -11 -5 22 45.15 24.09 -11 5 21 24.70 16.37 -11 5 21 20.08 12.30 11 -5 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29.83 20.10 21 -9 12 87.76 47.95 21 9 13 137.11 54.59 21 9 13 122.48 55.39 21 9 14 41.13 27.64 21 9 15 18.34 21.27 21 -10 -23 30.52 33.61 21 -10 -22 64.96 39.81 -21 -10 22 17.36 10.46 21 -10 -21 19.58 25.72 -21 -10 21 26.58 28.10 21 -10 -20 34.50 13.44 -21 -10 20 73.70 43.11 21 -10 -19 -14.46 29.90 -21 -10 19 -9.05 21.71 21 -10 -18 47.08 17.44 -21 -10 18 71.28 41.38 21 -10 -17 30.59 20.71 -21 -10 17 41.50 36.04 21 -10 -16 281.50 90.99 -21 -10 16 276.61 85.17 21 10 -15 298.59 81.60 21 -10 -15 238.51 79.53 -21 -10 15 259.45 82.16 21 10 -14 185.33 64.18 21 -10 -14 200.99 71.39 -21 -10 14 155.89 60.58 21 10 -13 309.20 80.70 21 -10 -13 310.51 88.46 -21 -10 13 398.73 97.92 21 10 -12 203.12 67.37 21 -10 -12 205.42 71.34 -21 -10 12 180.05 61.36 21 -10 -12 156.56 45.85 21 10 -11 491.18 104.25 21 -10 -11 455.67 107.93 -21 -10 11 482.91 102.62 21 -10 -11 394.62 66.81 21 -10 -10 86.96 46.40 21 10 -10 63.39 33.02 21 -10 -10 94.11 35.67 21 -10 -10 104.23 42.34 -21 -10 10 74.68 40.66 21 -10 -9 353.25 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144.45 56.31 23 -4 4 93.81 41.10 23 4 5 343.33 87.94 23 4 5 312.99 65.05 23 -4 5 309.75 75.26 23 4 6 155.20 58.52 23 4 6 169.77 50.86 23 -4 6 171.41 59.47 23 4 7 158.80 51.95 23 -4 7 178.62 60.11 23 4 7 187.08 63.77 23 4 8 354.82 91.52 23 4 8 253.20 67.09 23 -4 8 237.60 67.28 23 4 9 -21.20 20.32 23 4 9 -11.09 15.19 23 -4 9 -5.11 17.93 23 4 10 203.29 72.91 23 4 10 174.64 51.98 23 -4 10 129.49 55.97 23 4 11 -42.86 34.70 23 -4 11 1.26 16.84 23 4 12 76.55 35.45 23 -4 12 59.12 23.91 23 4 13 47.78 25.83 23 -4 13 20.05 29.93 23 4 14 -20.38 31.90 23 -4 14 -94.64 50.29 23 4 15 114.53 48.41 23 -5 -25 51.21 50.64 -23 5 24 -21.71 35.03 23 -5 -24 45.33 38.42 -23 -5 24 -4.92 21.39 -23 5 23 -12.26 21.37 23 -5 -23 65.02 50.19 -23 -5 23 31.49 29.01 -23 5 22 144.53 60.93 23 -5 -22 209.61 74.36 -23 -5 22 158.96 63.00 -23 5 21 114.53 47.04 23 -5 -21 177.01 71.24 -23 -5 21 129.27 56.13 -23 -5 20 565.15 115.94 23 -5 -20 548.65 115.31 -23 5 20 443.66 98.83 -23 5 19 151.65 56.87 23 5 -19 175.07 66.24 23 -5 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81.00 23 6 7 79.74 49.56 23 6 7 -17.65 23.54 23 -6 7 121.80 51.57 23 6 8 246.43 68.40 23 6 8 425.79 105.50 23 -6 8 304.68 79.00 23 6 9 -56.31 37.34 23 6 9 65.56 41.56 23 -6 9 80.14 53.07 23 -6 10 38.19 29.17 23 6 10 94.28 51.38 23 6 11 12.02 14.31 23 -6 11 68.19 38.06 23 6 12 -29.19 31.45 23 -6 12 6.81 17.58 23 6 13 -41.45 41.13 23 6 14 -13.66 25.08 23 6 15 14.30 14.62 23 -7 -23 20.45 27.13 -23 -7 23 -14.35 9.32 23 -7 -22 141.95 62.03 -23 -7 22 170.66 66.35 23 -7 -21 46.85 38.78 -23 -7 21 12.84 21.42 23 -7 -20 281.82 90.34 -23 -7 20 221.60 79.08 23 -7 -19 44.07 32.82 -23 -7 19 33.73 21.23 23 7 -18 212.21 63.91 23 -7 -18 163.36 62.47 -23 -7 18 153.78 60.40 23 7 -17 162.13 63.32 23 -7 -17 104.26 51.44 -23 -7 17 141.77 62.33 23 7 -16 -7.46 16.99 23 -7 -16 6.35 6.30 -23 -7 16 13.98 6.05 23 7 -15 229.53 68.31 23 -7 -15 162.24 57.40 -23 -7 15 255.40 76.13 23 -7 -14 25.89 35.62 23 7 -14 3.91 18.68 -23 -7 14 17.24 12.04 23 7 -13 434.26 100.81 23 -7 -13 378.75 93.54 -23 -7 13 421.30 95.52 23 -7 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13 46.23 33.93 -29 -7 12 8.69 12.04 -29 -7 11 21.69 15.95 -29 -7 10 45.07 32.02 -29 -7 9 -18.64 21.05 -29 -7 8 86.35 42.70 -29 -7 7 20.96 19.84 29 -7 -6 49.02 46.53 29 -7 -5 20.43 18.08 29 -7 -5 129.51 71.56 29 -7 -4 102.08 60.14 29 -7 -4 12.67 22.13 29 -7 -3 261.09 88.88 29 -7 -3 184.15 69.78 29 -7 -2 153.48 67.45 29 -7 -1 231.75 78.12 29 -7 -1 354.56 92.20 29 -7 0 228.38 75.71 -29 -8 14 185.02 71.72 -29 -8 13 235.92 78.46 -29 -8 12 279.24 86.77 -29 -8 11 149.30 61.48 -29 -8 10 86.83 46.79 -29 -8 9 123.55 53.15 -29 -8 8 24.10 21.11 29 -8 -3 81.31 58.64 29 -8 -3 2.20 11.41 29 -8 -2 69.81 41.82 29 -8 -2 104.99 58.71 29 -8 -1 65.15 53.94 29 -8 0 86.57 57.13 -29 -9 13 -2.52 21.90 -29 -9 12 53.83 35.05 -29 -9 11 140.93 59.27 -29 -9 10 51.95 34.50 -29 -10 12 77.47 46.32 -29 -10 11 18.52 24.78 30 0 -16 -2.64 15.42 30 0 -15 28.25 28.62 -30 0 14 88.93 40.93 30 0 -14 78.59 47.07 -30 0 13 13.76 7.80 30 0 -13 -13.34 19.52 30 0 -12 252.26 81.07 -30 0 12 178.21 62.38 30 0 -11 -13.85 23.65 -30 0 11 5.78 22.61 30 0 -10 413.87 103.74 30 0 -9 4.81 16.30 30 0 -8 326.58 93.35 30 0 -7 -3.68 18.02 30 0 -6 40.11 30.13 30 0 -5 -6.46 9.48 30 0 -4 6.22 7.60 30 1 -17 271.01 84.51 30 1 -16 39.39 37.19 -30 -1 15 185.45 68.28 30 1 -15 227.74 79.63 30 -1 -15 218.83 74.07 -30 -1 14 15.84 19.16 30 1 -14 28.19 30.86 30 -1 -14 4.90 23.77 -30 1 14 27.46 31.69 -30 -1 13 78.92 42.57 30 1 -13 141.51 59.34 30 -1 -13 148.65 60.59 -30 1 13 107.13 46.18 -30 -1 12 28.21 21.91 30 1 -12 100.74 54.50 30 -1 -12 61.49 39.46 -30 -1 11 23.01 27.78 30 -1 -11 42.75 38.21 30 1 -11 58.01 35.35 30 1 -10 192.34 79.95 30 -1 -10 165.89 65.43 -30 -1 10 129.99 55.41 30 1 -9 24.76 6.46 30 -1 -9 14.77 26.26 -30 -1 9 7.91 20.81 30 1 -8 172.07 68.51 30 -1 -8 196.32 73.83 30 1 -7 49.22 41.41 30 -1 -7 30.42 31.21 30 1 -6 214.08 78.73 30 -1 -6 173.70 67.66 30 1 -5 -31.67 32.58 30 -1 -5 -37.16 32.71 30 -1 -4 47.59 41.53 30 -1 -3 41.67 38.16 30 2 -18 31.39 29.12 30 2 -17 -12.25 17.72 30 2 -16 34.37 29.48 -30 -2 15 -7.44 26.17 30 2 -15 44.81 42.15 -30 -2 14 3.93 20.07 30 2 -14 19.15 26.92 -30 -2 13 129.53 56.89 30 2 -13 87.16 52.71 30 -2 -13 86.54 48.80 30 -2 -12 4.47 15.76 -30 -2 12 -7.64 13.50 30 2 -12 26.98 26.50 -30 -2 11 40.21 34.02 30 -2 -11 42.98 26.05 30 2 -11 10.20 8.83 -30 -2 10 67.63 37.49 30 2 -10 65.15 42.54 30 -2 -10 48.66 33.16 30 2 -9 -19.72 21.38 30 -2 -9 -22.01 20.79 -30 -2 9 -12.86 15.66 30 2 -8 57.97 34.58 30 -2 -8 43.25 36.77 -30 -2 8 39.40 28.87 30 2 -7 133.93 61.43 30 -2 -7 87.93 49.29 30 2 -6 -4.71 8.53 30 -2 -6 4.06 12.84 30 -2 -5 242.14 79.41 30 -2 -4 1.19 20.57 30 -2 -3 364.14 103.22 30 3 -18 2.16 13.16 30 3 -17 369.42 99.51 30 3 -16 30.80 34.28 -30 -3 15 473.80 111.86 30 3 -15 512.40 121.42 -30 -3 14 38.57 35.22 30 3 -14 41.74 36.64 -30 -3 13 188.69 67.98 30 3 -13 240.30 83.40 -30 -3 12 38.11 28.41 30 3 -12 42.88 35.70 -30 -3 11 35.75 22.22 30 -3 -11 36.99 28.58 30 3 -11 22.62 23.27 -30 -3 10 10.19 5.26 30 -3 -10 -0.42 18.83 30 3 -10 2.19 10.57 -30 -3 9 30.12 29.13 30 3 -9 5.04 19.57 30 -3 -9 -11.90 27.40 -30 -3 8 12.51 15.54 30 -3 -8 7.08 7.26 30 -3 -7 80.49 44.61 -30 -3 7 51.61 31.90 30 -3 -6 -4.39 18.53 -30 -3 6 -5.86 17.50 30 -3 -5 102.12 48.99 30 -3 -4 1.68 10.47 30 -3 -3 67.04 48.18 30 -3 -2 17.84 20.67 -30 -4 14 -10.64 26.23 -30 -4 13 57.03 36.77 -30 -4 12 55.18 32.94 -30 -4 11 85.32 46.08 -30 -4 10 102.81 46.66 30 -4 -10 87.44 50.34 -30 -4 9 39.16 18.71 30 -4 -9 41.67 28.96 -30 -4 8 292.78 79.09 30 -4 -8 284.19 84.57 30 -4 -7 15.68 32.94 -30 -4 7 25.73 29.95 30 -4 -6 86.44 50.54 30 -4 -5 159.04 64.69 30 -4 -4 40.66 26.04 30 -4 -3 199.24 76.72 30 -4 -2 37.90 31.36 -30 -5 14 5.12 4.05 -30 -5 13 -28.26 28.14 -30 -5 12 75.47 41.00 -30 -5 11 -11.94 22.50 -30 -5 10 84.19 45.57 -30 -5 9 62.17 28.90 -30 -5 8 152.95 57.50 30 -5 -8 165.42 65.18 -30 -5 7 90.92 42.07 30 -5 -7 80.64 45.53 30 -5 -6 40.34 30.15 30 -5 -5 29.85 24.97 30 -5 -4 6.41 13.08 30 -5 -3 14.84 20.39 30 -5 -2 0.27 18.72 -30 -6 14 56.94 37.56 -30 -6 13 50.75 34.01 -30 -6 12 101.38 52.21 -30 -6 11 63.24 34.65 -30 -6 10 178.60 63.31 -30 -6 9 149.83 57.48 -30 -6 8 160.14 58.30 30 -6 -6 21.16 21.94 30 -6 -5 48.90 33.47 30 -6 -4 29.84 26.31 30 -6 -3 87.82 43.86 30 -6 -2 30.14 28.67 -30 -7 13 246.61 80.14 -30 -7 12 21.18 21.45 -30 -7 11 97.44 47.87 -30 -7 10 31.33 27.26 -30 -7 9 100.42 50.57 -30 -8 12 49.73 34.53 -30 -8 11 86.44 48.29 -30 -8 10 26.63 19.63 31 0 -14 44.23 31.55 31 0 -13 22.93 27.25 31 0 -12 220.51 84.68 -31 0 12 171.44 68.47 31 0 -11 22.34 31.27 31 0 -10 173.27 72.67 31 0 -9 0.26 11.79 31 0 -8 147.10 66.29 31 1 -14 256.83 88.84 -31 -1 13 26.87 27.50 31 1 -13 -20.69 20.91 31 -1 -13 24.08 32.89 31 1 -12 279.33 89.44 31 -1 -12 289.56 92.81 -31 -1 12 279.54 84.67 31 -1 -11 16.05 24.10 -31 -1 11 5.77 19.71 31 1 -11 41.06 40.55 31 1 -10 222.80 83.94 31 -1 -10 196.40 73.58 -31 -1 10 183.81 68.56 31 -1 -9 42.77 38.29 31 -1 -8 67.21 48.79 31 -1 -7 138.37 63.57 -31 -2 13 37.56 26.97 31 -2 -12 51.17 35.95 -31 -2 12 48.51 28.35 -31 -2 11 -4.55 20.45 31 -2 -11 21.01 24.59 31 -2 -10 68.77 41.17 -31 -2 10 52.28 35.25 31 -2 -9 105.50 51.05 -31 -2 9 106.97 52.08 31 -2 -8 59.01 35.47 31 -2 -7 166.14 72.53 31 -2 -6 -17.61 25.27 -31 -3 13 -0.57 10.69 -31 -3 12 -0.50 10.36 -31 -3 11 -28.17 27.18 -31 -3 10 -7.70 21.68 31 -3 -10 -7.78 24.20 -31 -3 9 1.88 10.45 31 -3 -9 -2.82 15.66 31 -3 -8 28.85 29.78 -31 -3 8 44.26 25.65 31 -3 -7 124.91 61.54 31 -3 -6 52.71 33.12 -31 -4 13 17.14 14.25 -31 -4 12 27.76 20.96 -31 -4 11 14.58 17.52 -31 -4 10 19.55 19.49 -31 -4 9 131.27 54.66 -31 -4 8 27.67 28.00 31 -4 -7 164.31 67.00 31 -4 -6 23.65 29.88 31 -4 -5 63.74 49.50 -31 -5 12 274.50 84.17 -31 -5 11 93.42 49.28 -31 -5 10 308.11 85.01 -31 -5 9 52.76 35.54 -31 -6 12 54.34 36.40 -32 -2 10 9.64 26.79 0 0 0 0.00 0.00 TITL ostl19 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 23.147859 17.413321 26.494652 90.0000 103.6146 90.0000 ZERR 4.00 0.000670 0.000502 0.000928 0.0000 0.0035 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N Na Si P Th UNIT 264.00 600.00 32.00 4.00 24.00 4.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 64878 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _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 -23 17 0 0.0388 -22.9988 16.9986 -0.0043 -0.4234 0.4265 0.8026 0 1 -36 0.1207 0.0000 1.0004 -36.0093 -0.6634 0.6043 -0.4250 14 22 -5 0.0089 14.0051 21.9987 -5.0017 0.5018 0.8267 0.2283 -16 -21 7 0.0901 -16.0051 -20.9988 7.0018 -0.5062 -0.8364 -0.1451 -8 23 13 0.0605 -7.9964 22.9982 13.0002 0.2744 0.4732 0.8530 -2 3 37 0.0800 -1.9995 2.9993 37.0089 0.6716 -0.5046 0.5680 25 -15 1 0.0691 24.9993 -14.9987 1.0046 0.5153 -0.3713 -0.7762 11 -8 -35 0.1232 10.9993 -7.9989 -35.0069 -0.4512 0.3573 -0.8173 -22 -17 -4 0.0937 -22.0049 -16.9990 -4.0020 -0.8271 -0.5635 -0.0834 _olex2_submission_special_instructions 'No special instructions were received'