#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 16 _journal_issue 1 _journal_year 2025 _journal_page_first 37 _journal_page_last 45 #============================================================================= data_PDL1611 _audit_creation_date 2024-10-29 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number '2014/7' #===END _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _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. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '4(C12 H12 O2 Si), 3(C10 H8 N4)' _chemical_formula_sum 'C78 H72 N12 O8 Si4' _chemical_formula_weight 1417.83 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2352(3) _cell_length_b 15.3274(6) _cell_length_c 20.0271(6) _cell_angle_alpha 89.879(3) _cell_angle_beta 89.988(2) _cell_angle_gamma 78.298(3) _cell_volume 3677.7(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7694 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.8250 _cell_measurement_theta_min 2.7280 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'blocky needles' _exptl_crystal_F_000 1488 _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0829 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.869 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 20569 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.869 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.104 _diffrn_reflns_theta_min 2.443 _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 16.0382 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.869 _diffrn_measurement_device_type 'Agilent Xcalibur 3 E' _diffrn_measurement_method 'omega scans' _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 12089 _reflns_number_total 20569 _reflns_special_details ; _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' _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL n/a (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _refine_diff_density_max 1.037 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.054 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 991 _refine_ls_number_reflns 20569 _refine_ls_number_restraints 649 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0470 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1013 _refine_ls_wR_factor_ref 0.1098 _refine_special_details ; Refined as a 2-component twin. ; _olex2_refinement_description ; 1. Others Fixed Sof: N40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5) H42A(0.5) C43A(0.5) C44A(0.5) H44A(0.5) C45A(0.5) H45A(0.5) N46A(0.5) N47A(0.5) C48A(0.5) C49A(0.5) H49A(0.5) C50A(0.5) H50A(0.5) N51A(0.5) C52A(0.5) H52A(0.5) C53A(0.5) H53A(0.5) Fixed Uiso: H2AA(0.062) H3AA(0.082) H4AA(0.086) H5AA(0.074) H6AA(0.051) H8AA(0.042) H9AA(0.05) H10A(0.048) H11A(0.047) H12A(0.041) H2BA(0.043) H3BA(0.053) H4BA(0.056) H5BA(0.048) H6BA(0.039) H8BA(0.038) H9BA(0.051) H10B(0.052) H11B(0.046) H12B(0.037) H2CA(0.047) H3CA(0.059) H4CA(0.064) H5CA(0.055) H6CA(0.041) H8CA(0.042) H9CA(0.054) H10C(0.055) H11C(0.051) H12C(0.042) H2DA(0.039) H3DA(0.048) H4DA(0.048) H5DA(0.047) H6DA(0.038) H8DA(0.039) H9DA(0.052) H10D(0.059) H11D(0.05) H12D(0.039) H21A(0.055) H22A(0.05) H24A(0.054) H25A(0.054) H29A(0.047) H30A(0.044) H32A(0.042) H33A(0.043) H21B(0.053) H22B(0.048) H24B(0.052) H25B(0.049) H29B(0.049) H30B(0.047) H32B(0.044) H33B(0.044) H41A(0.048) H42A(0.048) H44A(0.04) H45A(0.047) H49A(0.046) H50A(0.044) H52A(0.04) H53A(0.045) H41B(0.053) H42B(0.053) H44B(0.046) H45B(0.048) Fixed X: H2AA(0.5621) H3AA(0.4643) H4AA(0.2719) H5AA(0.177) H6AA(0.2718) H8AA(0.4037) H9AA(0.4535) H10A(0.6309) H11A(0.7572) H12A(0.7062) H2BA(1.0943) H3BA(1.0834) H4BA(0.9127) H5BA(0.7525) H6BA(0.7642) H8BA(0.8802) H9BA(0.9701) H10B(1.163) H11B(1.2668) H12B(1.1783) H2CA(0.9013) H3CA(0.7843) H4CA(0.6171) H5CA(0.5672) H6CA(0.6795) H8CA(0.7427) H9CA(0.7248) H10C(0.8588) H11C(1.0066) H12C(1.0252) H2DA(0.4261) H3DA(0.3848) H4DA(0.22) H5DA(0.1001) H6DA(0.1441) H8DA(0.2067) H9DA(0.2337) H10D(0.3976) H11D(0.5346) H12D(0.5094) H21A(0.3635) H22A(0.2511) H24A(0.3486) H25A(0.456) H29A(0.0433) H30A(-0.0644) H32A(0.017) H33A(0.1358) H21B(0.1184) H22B(0.2086) H24B(0.2449) H25B(0.1563) H29B(0.3667) H30B(0.4573) H32B(0.4931) H33B(0.3952) H41A(0.3151) H42A(0.429) H44A(0.3834) H45A(0.2695) H49A(0.5423) H50A(0.6479) H52A(0.7694) H53A(0.6639) H41B(0.8419) H42B(0.9269) H44B(0.9144) H45B(0.8319) Fixed Y: H2AA(0.1609) H3AA(0.1264) H4AA(0.1774) H5AA(0.2635) H6AA(0.2972) H8AA(0.175) H9AA(0.0496) H10A(-0.042) H11A(-0.0058) H12A(0.1187) H2BA(0.1355) H3BA(0.0789) H4BA(0.1009) H5BA(0.1792) H6BA(0.2419) H8BA(0.1408) H9BA(0.0388) H10B(-0.0078) H11B(0.0498) H12B(0.1562) H2CA(0.8344) H3CA(0.8758) H4CA(0.8271) H5CA(0.7364) H6CA(0.6977) H8CA(0.8089) H9CA(0.9292) H10C(1.0182) H11C(0.9887) H12C(0.8702) H2DA(0.8711) H3DA(0.9386) H4DA(0.9265) H5DA(0.8448) H6DA(0.7736) H8DA(0.8563) H9DA(0.9657) H10D(1.0202) H11D(0.9656) H12D(0.8555) H21A(0.5095) H22A(0.561) H24A(0.3175) H25A(0.2748) H29A(0.6854) H30A(0.7248) H32A(0.483) H33A(0.438) H21B(0.5114) H22B(0.5633) H24B(0.319) H25B(0.2747) H29B(0.685) H30B(0.7267) H32B(0.4885) H33B(0.4412) H41A(0.5001) H42A(0.4199) H44A(0.6408) H45A(0.7209) H49A(0.5646) H50A(0.5064) H52A(0.2798) H53A(0.338) H41B(0.2704) H42B(0.3185) H44B(0.5527) H45B(0.4959) Fixed Z: H2AA(0.4107) H3AA(0.506) H4AA(0.5115) H5AA(0.4282) H6AA(0.3346) H8AA(0.1793) H9AA(0.1128) H10A(0.1232) H11A(0.1998) H12A(0.2675) H2BA(0.3957) H3BA(0.5025) H4BA(0.5574) H5BA(0.5051) H6BA(0.3997) H8BA(0.1933) H9BA(0.1161) H10B(0.1185) H11B(0.1989) H12B(0.2737) H2CA(0.0831) H3CA(-0.008) H4CA(-0.0161) H5CA(0.0658) H6CA(0.1586) H8CA(0.3111) H9CA(0.3839) H10C(0.3835) H11C(0.3093) H12C(0.2364) H2DA(0.1049) H3DA(0.002) H4DA(-0.0532) H5DA(-0.0045) H6DA(0.0973) H8DA(0.3072) H9DA(0.3821) H10D(0.3786) H11D(0.2996) H12D(0.2261) H21A(0.7389) H22A(0.6484) H24A(0.5648) H25A(0.6581) H29A(0.5031) H30A(0.4092) H32A(0.3376) H33A(0.4274) H21B(0.2353) H22B(0.1459) H24B(0.0637) H25B(0.1554) H29B(0.0075) H30B(-0.0851) H32B(-0.1625) H33B(-0.0736) H41A(0.2795) H42A(0.3619) H44A(0.4778) H45A(0.3954) H49A(0.624) H50A(0.7172) H52A(0.6147) H53A(0.5215) H41B(0.1093) H42B(0.017) H44B(0.1111) H45B(0.2019) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 Si1A Si 0.50409(5) 0.25916(5) 0.28707(4) 0.03016(18) Uani 1 1 d . . . . . O1A O 0.41799(13) 0.33584(11) 0.24739(8) 0.0412(5) Uani 1 1 d D . . . . H1A H 0.4435(7) 0.3539(6) 0.2086(2) 0.086(12) Uiso 1 1 d D . . . . O2A O 0.61032(13) 0.29281(13) 0.31752(9) 0.0456(5) Uani 1 1 d D . . . . H2A H 0.6761(3) 0.2880(15) 0.2963(3) 0.074(10) Uiso 1 1 d D . . . . C1A C 0.4273(2) 0.23173(18) 0.36199(13) 0.0343(7) Uani 1 1 d . . . . . C2A C 0.4836(3) 0.1816(2) 0.41362(15) 0.0517(9) Uani 1 1 d . . . . . H2AA H 0.5621 0.1609 0.4107 0.062 Uiso 1 1 calc R U . . . C3A C 0.4257(4) 0.1609(2) 0.47060(16) 0.0684(10) Uani 1 1 d . . . . . H3AA H 0.4643 0.1264 0.5060 0.082 Uiso 1 1 calc R U . . . C4A C 0.3117(4) 0.1919(3) 0.47367(19) 0.0720(12) Uani 1 1 d . . . . . H4AA H 0.2719 0.1774 0.5115 0.086 Uiso 1 1 calc R U . . . C5A C 0.2552(3) 0.2420(2) 0.42453(18) 0.0618(10) Uani 1 1 d . . . . . H5AA H 0.1770 0.2635 0.4282 0.074 Uiso 1 1 calc R U . . . C6A C 0.3120(2) 0.26191(18) 0.36907(14) 0.0425(7) Uani 1 1 d . . . . . H6AA H 0.2718 0.2972 0.3346 0.051 Uiso 1 1 calc R U . . . C7A C 0.5493(2) 0.16120(17) 0.23126(12) 0.0282(6) Uani 1 1 d . . . . . C8A C 0.4758(2) 0.13833(19) 0.18410(13) 0.0348(7) Uani 1 1 d . . . . . H8AA H 0.4037 0.1750 0.1793 0.042 Uiso 1 1 calc R U . . . C9A C 0.5052(3) 0.0638(2) 0.14432(14) 0.0415(7) Uani 1 1 d . . . . . H9AA H 0.4535 0.0496 0.1128 0.050 Uiso 1 1 calc R U . . . C10A C 0.6105(2) 0.00948(19) 0.15039(14) 0.0403(7) Uani 1 1 d . . . . . H10A H 0.6309 -0.0420 0.1232 0.048 Uiso 1 1 calc R U . . . C11A C 0.6847(2) 0.03063(18) 0.19579(14) 0.0392(7) Uani 1 1 d . . . . . H11A H 0.7572 -0.0058 0.1998 0.047 Uiso 1 1 calc R U . . . C12A C 0.6541(2) 0.10527(18) 0.23591(13) 0.0338(7) Uani 1 1 d . . . . . H12A H 0.7062 0.1187 0.2675 0.041 Uiso 1 1 calc R U . . . Si1B Si 0.94738(5) 0.24648(5) 0.30256(3) 0.02553(17) Uani 1 1 d . . . . . O1B O 0.82101(13) 0.28756(11) 0.27661(8) 0.0315(4) Uani 1 1 d D . . . . H1B H 0.814(2) 0.3184(4) 0.23800(18) 0.062(10) Uiso 1 1 d D . . . . O2B O 1.02276(13) 0.32118(11) 0.31247(8) 0.0349(4) Uani 1 1 d D . . . . H2B H 1.0513(6) 0.3421(5) 0.2757(2) 0.074(10) Uiso 1 1 d D . . . . C1B C 0.9313(2) 0.19707(16) 0.38623(12) 0.0263(6) Uani 1 1 d . . . . . C2B C 1.0245(2) 0.14639(17) 0.41813(13) 0.0356(7) Uani 1 1 d . . . . . H2BA H 1.0943 0.1355 0.3957 0.043 Uiso 1 1 calc R U . . . C3B C 1.0181(3) 0.11164(18) 0.48145(14) 0.0446(7) Uani 1 1 d . . . . . H3BA H 1.0834 0.0789 0.5025 0.053 Uiso 1 1 calc R U . . . C4B C 0.9173(3) 0.12450(19) 0.51387(14) 0.0465(8) Uani 1 1 d . . . . . H4BA H 0.9127 0.1009 0.5574 0.056 Uiso 1 1 calc R U . . . C5B C 0.8226(2) 0.17173(19) 0.48314(13) 0.0400(7) Uani 1 1 d . . . . . H5BA H 0.7525 0.1792 0.5051 0.048 Uiso 1 1 calc R U . . . C6B C 0.8297(2) 0.20852(17) 0.42002(12) 0.0326(6) Uani 1 1 d . . . . . H6BA H 0.7642 0.2419 0.3997 0.039 Uiso 1 1 calc R U . . . C7B C 1.01893(19) 0.16234(16) 0.24177(12) 0.0249(6) Uani 1 1 d . . . . . C8B C 0.9593(2) 0.12398(17) 0.19419(13) 0.0320(7) Uani 1 1 d . . . . . H8BA H 0.8802 0.1408 0.1933 0.038 Uiso 1 1 calc R U . . . C9B C 1.0126(3) 0.06232(19) 0.14863(14) 0.0428(8) Uani 1 1 d . . . . . H9BA H 0.9701 0.0388 0.1161 0.051 Uiso 1 1 calc R U . . . C10B C 1.1267(3) 0.03472(19) 0.14987(14) 0.0432(8) Uani 1 1 d . . . . . H10B H 1.1630 -0.0078 0.1185 0.052 Uiso 1 1 calc R U . . . C11B C 1.1881(2) 0.06932(18) 0.19711(14) 0.0386(7) Uani 1 1 d . . . . . H11B H 1.2668 0.0498 0.1989 0.046 Uiso 1 1 calc R U . . . C12B C 1.1348(2) 0.13241(17) 0.24190(13) 0.0311(6) Uani 1 1 d . . . . . H12B H 1.1783 0.1562 0.2737 0.037 Uiso 1 1 calc R U . . . Si1C Si 0.89657(6) 0.73167(5) 0.20516(4) 0.02828(18) Uani 1 1 d . . . . . O1C O 0.85653(14) 0.64938(11) 0.24190(8) 0.0390(5) Uani 1 1 d D . . . . H1C H 0.8866(8) 0.6343(11) 0.2824(2) 0.083(11) Uiso 1 1 d D . . . . O2C O 1.02036(13) 0.70659(12) 0.17327(9) 0.0429(5) Uani 1 1 d D . . . . H2C H 1.0793(4) 0.7176(6) 0.1963(3) 0.080(11) Uiso 1 1 d D . . . . C1C C 0.80365(19) 0.76149(16) 0.13151(12) 0.0282(6) Uani 1 1 d . . . . . C2C C 0.8327(2) 0.81465(18) 0.08043(13) 0.0392(7) Uani 1 1 d . . . . . H2CA H 0.9013 0.8344 0.0831 0.047 Uiso 1 1 calc R U . . . C3C C 0.7635(3) 0.83908(19) 0.02599(14) 0.0491(8) Uani 1 1 d . . . . . H3CA H 0.7843 0.8758 -0.0080 0.059 Uiso 1 1 calc R U . . . C4C C 0.6647(3) 0.8102(2) 0.02115(16) 0.0536(9) Uani 1 1 d . . . . . H4CA H 0.6171 0.8271 -0.0161 0.064 Uiso 1 1 calc R U . . . C5C C 0.6349(2) 0.75718(19) 0.06981(15) 0.0462(8) Uani 1 1 d . . . . . H5CA H 0.5672 0.7364 0.0658 0.055 Uiso 1 1 calc R U . . . C6C C 0.70236(19) 0.73363(17) 0.12472(13) 0.0344(6) Uani 1 1 d . . . . . H6CA H 0.6795 0.6977 0.1586 0.041 Uiso 1 1 calc R U . . . C7C C 0.8857(2) 0.82583(16) 0.26471(12) 0.0264(6) Uani 1 1 d . . . . . C8C C 0.7968(2) 0.84538(18) 0.31022(13) 0.0353(7) Uani 1 1 d . . . . . H8CA H 0.7427 0.8089 0.3111 0.042 Uiso 1 1 calc R U . . . C9C C 0.7861(3) 0.9167(2) 0.35387(14) 0.0453(8) Uani 1 1 d . . . . . H9CA H 0.7248 0.9292 0.3839 0.054 Uiso 1 1 calc R U . . . C10C C 0.8653(3) 0.9696(2) 0.35337(15) 0.0457(8) Uani 1 1 d . . . . . H10C H 0.8588 1.0182 0.3835 0.055 Uiso 1 1 calc R U . . . C11C C 0.9528(2) 0.95194(19) 0.30965(15) 0.0425(8) Uani 1 1 d . . . . . H11C H 1.0066 0.9887 0.3093 0.051 Uiso 1 1 calc R U . . . C12C C 0.9636(2) 0.88149(18) 0.26617(14) 0.0353(7) Uani 1 1 d . . . . . H12C H 1.0252 0.8702 0.2364 0.042 Uiso 1 1 calc R U . . . Si1D Si 0.33088(5) 0.75940(5) 0.19499(3) 0.02441(17) Uani 1 1 d . . . . . O1D O 0.22617(12) 0.71595(11) 0.21894(7) 0.0294(4) Uani 1 1 d D . . . . H1D H 0.2416(17) 0.6837(4) 0.2566(2) 0.051(9) Uiso 1 1 d D . . . . O2D O 0.44540(13) 0.68601(11) 0.18368(8) 0.0320(4) Uani 1 1 d D . . . . H2D H 0.4836(6) 0.6693(10) 0.2216(2) 0.056(9) Uiso 1 1 d D . . . . C1D C 0.29069(19) 0.81359(16) 0.11255(11) 0.0251(6) Uani 1 1 d . . . . . C2D C 0.3599(2) 0.86450(17) 0.08252(12) 0.0323(6) Uani 1 1 d . . . . . H2DA H 0.4261 0.8711 0.1049 0.039 Uiso 1 1 calc R U . . . C3D C 0.3352(2) 0.90546(18) 0.02153(13) 0.0397(7) Uani 1 1 d . . . . . H3DA H 0.3848 0.9386 0.0020 0.048 Uiso 1 1 calc R U . . . C4D C 0.2379(2) 0.89820(18) -0.01122(13) 0.0400(7) Uani 1 1 d . . . . . H4DA H 0.2200 0.9265 -0.0532 0.048 Uiso 1 1 calc R U . . . C5D C 0.1674(2) 0.84954(19) 0.01754(13) 0.0391(7) Uani 1 1 d . . . . . H5DA H 0.1001 0.8448 -0.0045 0.047 Uiso 1 1 calc R U . . . C6D C 0.1935(2) 0.80737(17) 0.07846(12) 0.0314(6) Uani 1 1 d . . . . . H6DA H 0.1441 0.7736 0.0973 0.038 Uiso 1 1 calc R U . . . C7D C 0.35497(19) 0.84284(16) 0.25765(12) 0.0244(6) Uani 1 1 d . . . . . C8D C 0.2741(2) 0.87791(17) 0.30543(13) 0.0321(7) Uani 1 1 d . . . . . H8DA H 0.2067 0.8563 0.3072 0.039 Uiso 1 1 calc R U . . . C9D C 0.2897(3) 0.94329(19) 0.35017(14) 0.0437(8) Uani 1 1 d . . . . . H9DA H 0.2337 0.9657 0.3821 0.052 Uiso 1 1 calc R U . . . C10D C 0.3865(3) 0.9755(2) 0.34802(15) 0.0489(8) Uani 1 1 d . . . . . H10D H 0.3976 1.0202 0.3786 0.059 Uiso 1 1 calc R U . . . C11D C 0.4679(2) 0.94285(19) 0.30134(14) 0.0413(8) Uani 1 1 d . . . . . H11D H 0.5346 0.9656 0.2996 0.050 Uiso 1 1 calc R U . . . C12D C 0.4524(2) 0.87765(18) 0.25747(13) 0.0329(7) Uani 1 1 d . . . . . H12D H 0.5094 0.8555 0.2261 0.039 Uiso 1 1 calc R U . . . N20A N 0.41955(16) 0.38673(17) 0.70748(11) 0.0392(6) Uani 1 1 d . . . . . C21A C 0.3596(2) 0.4699(2) 0.70298(14) 0.0459(7) Uani 1 1 d . . . . . H21A H 0.3635 0.5095 0.7389 0.055 Uiso 1 1 calc R U . . . C22A C 0.2924(2) 0.50142(19) 0.64942(13) 0.0415(7) Uani 1 1 d . . . . . H22A H 0.2511 0.5610 0.6484 0.050 Uiso 1 1 calc R U . . . C23A C 0.28715(19) 0.44364(19) 0.59731(12) 0.0318(6) Uani 1 1 d . . . . . C24A C 0.3496(2) 0.3583(2) 0.60038(14) 0.0450(7) Uani 1 1 d . . . . . H24A H 0.3486 0.3175 0.5648 0.054 Uiso 1 1 calc R U . . . C25A C 0.4133(2) 0.33386(19) 0.65614(16) 0.0450(7) Uani 1 1 d . . . . . H25A H 0.4560 0.2748 0.6581 0.054 Uiso 1 1 calc R U . . . N26A N 0.22144(19) 0.46326(16) 0.53675(11) 0.0448(6) Uani 1 1 d . . . . . N27A N 0.16940(18) 0.53895(16) 0.53504(11) 0.0403(6) Uani 1 1 d . . . . . C28A C 0.1017(2) 0.55793(19) 0.47439(13) 0.0326(6) Uani 1 1 d . . . . . C29A C 0.0408(2) 0.64284(19) 0.46903(13) 0.0390(7) Uani 1 1 d . . . . . H29A H 0.0433 0.6854 0.5031 0.047 Uiso 1 1 calc R U . . . C30A C -0.0242(2) 0.66511(18) 0.41320(13) 0.0370(7) Uani 1 1 d . . . . . H30A H -0.0644 0.7248 0.4092 0.044 Uiso 1 1 calc R U . . . N31A N -0.03441(16) 0.60859(15) 0.36446(10) 0.0327(5) Uani 1 1 d . . . . . C32A C 0.0240(2) 0.52519(18) 0.37122(13) 0.0350(7) Uani 1 1 d . . . . . H32A H 0.0170 0.4830 0.3376 0.042 Uiso 1 1 calc R U . . . C33A C 0.0941(2) 0.49739(18) 0.42489(13) 0.0358(7) Uani 1 1 d . . . . . H33A H 0.1358 0.4380 0.4274 0.043 Uiso 1 1 calc R U . . . N20B N 0.12974(16) 0.38758(16) 0.20413(11) 0.0361(6) Uani 1 1 d . . . . . C21B C 0.1454(2) 0.4716(2) 0.19993(13) 0.0440(7) Uani 1 1 d . . . . . H21B H 0.1184 0.5114 0.2353 0.053 Uiso 1 1 calc R U . . . C22B C 0.1989(2) 0.50339(19) 0.14692(13) 0.0399(7) Uani 1 1 d . . . . . H22B H 0.2086 0.5633 0.1459 0.048 Uiso 1 1 calc R U . . . C23B C 0.23735(19) 0.44588(18) 0.09617(12) 0.0310(6) Uani 1 1 d . . . . . C24B C 0.2203(2) 0.35976(19) 0.09889(14) 0.0435(7) Uani 1 1 d . . . . . H24B H 0.2449 0.3190 0.0637 0.052 Uiso 1 1 calc R U . . . C25B C 0.1671(2) 0.33434(19) 0.15362(14) 0.0408(7) Uani 1 1 d . . . . . H25B H 0.1563 0.2747 0.1554 0.049 Uiso 1 1 calc R U . . . N26B N 0.29587(18) 0.46525(16) 0.03560(12) 0.0449(6) Uani 1 1 d . . . . . N27B N 0.31049(17) 0.54039(17) 0.03669(11) 0.0432(6) Uani 1 1 d . . . . . C28B C 0.3708(2) 0.5595(2) -0.02442(13) 0.0355(7) Uani 1 1 d . . . . . C29B C 0.3905(2) 0.64363(19) -0.02737(13) 0.0405(7) Uani 1 1 d . . . . . H29B H 0.3667 0.6850 0.0075 0.049 Uiso 1 1 calc R U . . . C30B C 0.4460(2) 0.66725(19) -0.08252(13) 0.0391(7) Uani 1 1 d . . . . . H30B H 0.4573 0.7267 -0.0851 0.047 Uiso 1 1 calc R U . . . N31B N 0.48442(16) 0.61214(15) -0.13212(10) 0.0347(5) Uani 1 1 d . . . . . C32B C 0.4658(2) 0.52944(19) -0.12783(13) 0.0368(7) Uani 1 1 d . . . . . H32B H 0.4931 0.4885 -0.1625 0.044 Uiso 1 1 calc R U . . . C33B C 0.4082(2) 0.50024(18) -0.07481(14) 0.0370(7) Uani 1 1 d . . . . . H33B H 0.3952 0.4412 -0.0736 0.044 Uiso 1 1 calc R U . . . N40A N 0.2816(5) 0.6180(4) 0.3297(2) 0.0340(13) Uani 0.5 1 d G U P A -1 C41A C 0.3289(5) 0.5286(4) 0.3197(2) 0.0398(14) Uani 0.5 1 d G U P A -1 H41A H 0.3151 0.5001 0.2795 0.048 Uiso 0.5 1 calc R U P A -1 C42A C 0.3966(4) 0.4810(3) 0.3687(2) 0.0402(13) Uani 0.5 1 d DG U P A -1 H42A H 0.4290 0.4199 0.3619 0.048 Uiso 0.5 1 calc R U P A -1 C43A C 0.4169(4) 0.5228(3) 0.4276(2) 0.0297(12) Uani 0.5 1 d DG U P A -1 C44A C 0.3695(4) 0.6122(3) 0.4376(2) 0.0337(12) Uani 0.5 1 d DG U P A -1 H44A H 0.3834 0.6408 0.4778 0.040 Uiso 0.5 1 calc R U P A -1 C45A C 0.3018(4) 0.6598(3) 0.3886(3) 0.0395(13) Uani 0.5 1 d G U P A -1 H45A H 0.2695 0.7209 0.3954 0.047 Uiso 0.5 1 calc R U P A -1 N46A N 0.4989(5) 0.4665(4) 0.4750(3) 0.0411(13) Uani 0.5 1 d D U P A -1 N47A N 0.5245(5) 0.5085(5) 0.5150(3) 0.0524(14) Uani 0.5 1 d D U P A -1 C48A C 0.5932(4) 0.4568(3) 0.5640(2) 0.0358(13) Uani 0.5 1 d DG U P A -1 C49A C 0.5884(4) 0.5068(3) 0.6221(2) 0.0381(13) Uani 0.5 1 d DG U P A -1 H49A H 0.5423 0.5646 0.6240 0.046 Uiso 0.5 1 calc R U P A -1 C50A C 0.6511(5) 0.4722(4) 0.6775(2) 0.0368(13) Uani 0.5 1 d G U P A -1 H50A H 0.6479 0.5064 0.7172 0.044 Uiso 0.5 1 calc R U P A -1 N51A N 0.7186(5) 0.3876(4) 0.6747(2) 0.0344(13) Uani 0.5 1 d G U P A -1 C52A C 0.7233(4) 0.3376(3) 0.6166(3) 0.0336(12) Uani 0.5 1 d G U P A -1 H52A H 0.7694 0.2798 0.6147 0.040 Uiso 0.5 1 calc R U P A -1 C53A C 0.6606(4) 0.3722(3) 0.5612(2) 0.0376(13) Uani 0.5 1 d DG U P A -1 H53A H 0.6639 0.3380 0.5215 0.045 Uiso 0.5 1 calc R U P A -1 N40B N 0.83124(17) 0.37762(16) 0.16386(11) 0.0378(6) Uani 1 1 d . . . . . C41B C 0.8583(2) 0.3284(2) 0.10986(14) 0.0438(7) Uani 1 1 d . . . . . H41B H 0.8419 0.2704 0.1093 0.053 Uiso 1 1 calc R U . . . C42B C 0.9085(2) 0.35608(19) 0.05466(14) 0.0441(7) Uani 1 1 d . . . . . H42B H 0.9269 0.3185 0.0170 0.053 Uiso 1 1 calc R U . . . C43B C 0.9312(2) 0.43980(19) 0.05600(13) 0.0339(7) Uani 1 1 d . . . . . C44B C 0.9015(2) 0.49369(18) 0.11022(14) 0.0387(7) Uani 1 1 d . . . . . H44B H 0.9144 0.5527 0.1111 0.046 Uiso 1 1 calc R U . . . C45B C 0.8519(2) 0.4594(2) 0.16377(13) 0.0400(7) Uani 1 1 d . . . . . H45B H 0.8319 0.4959 0.2019 0.048 Uiso 1 1 calc R U . . . N46B N 0.98592(19) 0.46435(14) -0.00343(11) 0.0427(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1A 0.0259(4) 0.0310(5) 0.0331(4) 0.0018(4) 0.0053(3) -0.0047(3) O1A 0.0408(10) 0.0377(12) 0.0387(11) 0.0065(10) 0.0120(9) 0.0071(9) O2A 0.0316(11) 0.0530(13) 0.0558(13) -0.0172(10) 0.0127(9) -0.0167(10) C1A 0.0401(16) 0.0345(17) 0.0316(16) -0.0035(14) 0.0011(13) -0.0151(13) C2A 0.068(2) 0.052(2) 0.0410(19) 0.0078(17) -0.0048(17) -0.0249(18) C3A 0.118(3) 0.060(3) 0.0363(19) 0.0085(18) -0.009(2) -0.039(2) C4A 0.111(3) 0.067(3) 0.052(2) -0.018(2) 0.033(2) -0.050(3) C5A 0.069(2) 0.052(2) 0.073(2) -0.022(2) 0.035(2) -0.0298(19) C6A 0.0440(17) 0.0395(18) 0.0493(18) -0.0108(15) 0.0161(14) -0.0207(14) C7A 0.0274(14) 0.0289(16) 0.0280(14) 0.0075(12) 0.0049(12) -0.0056(12) C8A 0.0326(15) 0.0352(18) 0.0351(16) 0.0097(14) -0.0019(13) -0.0036(13) C9A 0.0532(19) 0.044(2) 0.0304(16) 0.0005(15) 0.0002(14) -0.0176(16) C10A 0.058(2) 0.0281(17) 0.0344(17) -0.0008(14) 0.0155(15) -0.0084(15) C11A 0.0373(16) 0.0297(17) 0.0468(18) 0.0047(15) 0.0106(14) 0.0018(13) C12A 0.0326(15) 0.0313(17) 0.0366(16) 0.0046(14) 0.0003(13) -0.0045(13) Si1B 0.0287(4) 0.0240(4) 0.0241(4) 0.0011(3) 0.0038(3) -0.0061(3) O1B 0.0269(9) 0.0353(11) 0.0303(10) 0.0056(9) 0.0070(8) -0.0019(8) O2B 0.0428(10) 0.0311(11) 0.0340(11) -0.0025(9) 0.0087(9) -0.0148(9) C1B 0.0371(15) 0.0192(15) 0.0237(14) -0.0032(12) 0.0010(12) -0.0083(12) C2B 0.0434(16) 0.0309(17) 0.0333(16) 0.0012(14) 0.0023(13) -0.0095(13) C3B 0.064(2) 0.0313(18) 0.0385(17) 0.0083(14) -0.0091(16) -0.0105(15) C4B 0.076(2) 0.0400(19) 0.0279(15) 0.0037(14) 0.0055(16) -0.0238(17) C5B 0.0531(19) 0.0420(19) 0.0293(16) -0.0038(15) 0.0088(14) -0.0197(15) C6B 0.0417(16) 0.0310(16) 0.0278(15) -0.0030(13) 0.0032(12) -0.0137(13) C7B 0.0289(14) 0.0214(15) 0.0252(14) 0.0023(12) 0.0040(11) -0.0068(11) C8B 0.0314(14) 0.0297(17) 0.0326(16) 0.0035(14) -0.0020(12) -0.0008(12) C9B 0.058(2) 0.0355(19) 0.0313(17) -0.0073(15) -0.0057(15) -0.0014(15) C10B 0.058(2) 0.0290(18) 0.0366(17) -0.0030(15) 0.0108(15) 0.0064(15) C11B 0.0347(15) 0.0278(17) 0.0491(19) 0.0023(15) 0.0098(14) 0.0037(13) C12B 0.0314(15) 0.0260(16) 0.0364(16) 0.0007(13) 0.0000(12) -0.0065(12) Si1C 0.0269(4) 0.0283(5) 0.0305(4) 0.0020(3) -0.0062(3) -0.0075(3) O1C 0.0529(11) 0.0310(11) 0.0369(11) 0.0062(9) -0.0150(9) -0.0174(9) O2C 0.0259(10) 0.0528(13) 0.0489(12) -0.0105(10) -0.0064(9) -0.0055(9) C1C 0.0296(14) 0.0240(15) 0.0296(15) -0.0031(12) -0.0010(11) -0.0021(12) C2C 0.0418(16) 0.0400(19) 0.0346(16) 0.0018(15) 0.0021(13) -0.0059(14) C3C 0.068(2) 0.040(2) 0.0301(17) 0.0061(15) 0.0030(16) 0.0087(17) C4C 0.064(2) 0.048(2) 0.0383(19) -0.0136(17) -0.0223(16) 0.0149(17) C5C 0.0377(16) 0.042(2) 0.054(2) -0.0139(17) -0.0198(15) 0.0032(14) C6C 0.0304(14) 0.0320(17) 0.0387(16) -0.0025(13) -0.0047(12) -0.0017(12) C7C 0.0293(14) 0.0232(15) 0.0264(14) 0.0077(12) -0.0095(12) -0.0046(12) C8C 0.0427(17) 0.0312(17) 0.0323(16) 0.0041(14) -0.0032(13) -0.0078(13) C9C 0.0558(19) 0.045(2) 0.0288(16) 0.0052(15) 0.0026(14) 0.0049(16) C10C 0.071(2) 0.0276(18) 0.0355(18) -0.0035(14) -0.0175(17) -0.0016(16) C11C 0.0533(19) 0.0309(18) 0.0453(19) 0.0021(16) -0.0154(16) -0.0130(15) C12C 0.0372(16) 0.0304(17) 0.0390(17) 0.0037(14) -0.0085(13) -0.0086(13) Si1D 0.0243(4) 0.0237(4) 0.0245(4) 0.0029(3) -0.0019(3) -0.0032(3) O1D 0.0286(9) 0.0333(11) 0.0275(10) 0.0093(9) -0.0081(8) -0.0094(8) O2D 0.0303(9) 0.0306(11) 0.0311(10) 0.0016(9) -0.0039(8) 0.0029(8) C1D 0.0298(14) 0.0203(14) 0.0227(13) -0.0028(11) 0.0029(11) 0.0006(11) C2D 0.0296(14) 0.0343(17) 0.0316(15) 0.0027(13) 0.0013(12) -0.0032(12) C3D 0.0425(16) 0.0414(18) 0.0349(16) 0.0097(14) 0.0060(13) -0.0080(14) C4D 0.0557(18) 0.0382(18) 0.0227(14) 0.0082(13) -0.0027(13) -0.0015(14) C5D 0.0435(16) 0.0428(19) 0.0299(16) 0.0003(14) -0.0110(13) -0.0063(14) C6D 0.0342(14) 0.0331(17) 0.0274(15) 0.0024(13) -0.0023(12) -0.0081(12) C7D 0.0274(14) 0.0206(14) 0.0236(13) 0.0080(11) -0.0034(11) -0.0012(11) C8D 0.0368(15) 0.0291(17) 0.0310(15) 0.0032(13) 0.0021(12) -0.0078(13) C9D 0.0580(19) 0.041(2) 0.0342(17) -0.0072(15) 0.0098(15) -0.0154(16) C10D 0.077(2) 0.040(2) 0.0346(18) -0.0091(15) -0.0043(17) -0.0231(17) C11D 0.0508(18) 0.0403(19) 0.0392(18) -0.0006(15) -0.0049(15) -0.0246(15) C12D 0.0326(15) 0.0346(17) 0.0316(15) 0.0043(14) -0.0005(12) -0.0073(13) N20A 0.0273(12) 0.0493(17) 0.0385(14) 0.0146(13) -0.0043(10) -0.0018(11) C21A 0.0407(16) 0.056(2) 0.0361(17) -0.0065(16) -0.0086(14) 0.0021(15) C22A 0.0382(16) 0.0404(19) 0.0393(17) 0.0019(15) -0.0049(13) 0.0074(13) C23A 0.0262(14) 0.0435(19) 0.0260(15) 0.0108(14) -0.0060(12) -0.0083(13) C24A 0.0517(18) 0.038(2) 0.0451(18) 0.0036(15) -0.0102(15) -0.0088(15) C25A 0.0431(17) 0.0303(18) 0.058(2) 0.0090(17) -0.0062(16) 0.0000(14) N26A 0.0448(14) 0.0375(16) 0.0499(16) 0.0068(13) 0.0052(12) -0.0028(12) N27A 0.0444(14) 0.0326(15) 0.0431(15) 0.0017(12) 0.0018(11) -0.0058(12) C28A 0.0323(14) 0.0399(19) 0.0262(15) 0.0086(14) -0.0044(12) -0.0090(13) C29A 0.0466(16) 0.0367(19) 0.0350(16) -0.0005(14) -0.0081(13) -0.0116(14) C30A 0.0436(16) 0.0276(17) 0.0382(17) 0.0043(14) -0.0106(13) -0.0037(13) N31A 0.0395(12) 0.0331(15) 0.0268(12) 0.0034(11) -0.0048(10) -0.0107(11) C32A 0.0443(16) 0.0317(18) 0.0304(15) -0.0044(14) 0.0077(13) -0.0115(14) C33A 0.0353(15) 0.0274(17) 0.0415(17) 0.0154(14) 0.0068(13) 0.0013(12) N20B 0.0314(12) 0.0420(16) 0.0372(14) 0.0085(12) -0.0010(10) -0.0132(11) C21B 0.0491(17) 0.047(2) 0.0386(17) -0.0101(15) 0.0129(14) -0.0167(15) C22B 0.0471(17) 0.0331(17) 0.0441(17) 0.0007(15) 0.0063(14) -0.0191(14) C23B 0.0252(14) 0.0416(18) 0.0254(14) 0.0075(14) 0.0012(11) -0.0051(12) C24B 0.0482(17) 0.0382(19) 0.0426(17) -0.0043(15) 0.0089(14) -0.0050(14) C25B 0.0433(17) 0.0304(17) 0.0495(19) 0.0057(15) 0.0025(14) -0.0094(13) N26B 0.0472(14) 0.0330(16) 0.0537(16) 0.0052(13) -0.0112(12) -0.0065(12) N27B 0.0388(13) 0.0425(17) 0.0459(15) -0.0003(13) -0.0070(11) -0.0025(12) C28B 0.0270(14) 0.050(2) 0.0297(15) 0.0122(15) -0.0026(12) -0.0080(13) C29B 0.0402(16) 0.045(2) 0.0356(16) -0.0007(15) 0.0070(13) -0.0068(14) C30B 0.0421(16) 0.0337(18) 0.0416(17) 0.0030(15) 0.0039(14) -0.0081(13) N31B 0.0370(12) 0.0370(15) 0.0302(13) 0.0066(12) 0.0001(10) -0.0080(11) C32B 0.0404(16) 0.0385(19) 0.0288(15) -0.0032(14) -0.0078(12) -0.0016(14) C33B 0.0384(15) 0.0289(17) 0.0457(18) 0.0159(15) -0.0159(14) -0.0116(13) N40A 0.0335(16) 0.0353(16) 0.0336(16) 0.0040(10) 0.0007(10) -0.0080(10) C41A 0.0375(16) 0.0412(16) 0.0401(16) 0.0014(10) -0.0010(10) -0.0064(10) C42A 0.0399(16) 0.0402(16) 0.0405(16) 0.0010(10) -0.0028(10) -0.0080(10) C43A 0.0298(14) 0.0295(15) 0.0295(15) 0.0024(10) 0.0008(10) -0.0051(10) C44A 0.0327(15) 0.0359(15) 0.0311(15) -0.0004(10) -0.0005(10) -0.0037(10) C45A 0.0384(16) 0.0399(16) 0.0389(16) 0.0015(10) -0.0004(11) -0.0049(10) N46A 0.0449(15) 0.0381(15) 0.0393(15) -0.0037(10) 0.0073(10) -0.0060(10) N47A 0.0517(17) 0.0551(17) 0.0508(17) 0.0033(11) -0.0007(11) -0.0123(11) C48A 0.0360(15) 0.0353(16) 0.0364(15) 0.0049(10) -0.0006(10) -0.0083(10) C49A 0.0376(15) 0.0378(15) 0.0389(15) 0.0021(10) -0.0031(10) -0.0073(10) C50A 0.0360(16) 0.0377(16) 0.0373(16) 0.0005(10) -0.0033(10) -0.0090(10) N51A 0.0342(16) 0.0357(16) 0.0339(16) 0.0032(10) 0.0011(10) -0.0082(10) C52A 0.0329(15) 0.0354(15) 0.0334(15) 0.0005(10) -0.0036(10) -0.0088(10) C53A 0.0370(15) 0.0394(15) 0.0354(15) 0.0016(10) -0.0001(10) -0.0051(10) N40B 0.0368(13) 0.0433(16) 0.0347(14) 0.0112(12) -0.0092(11) -0.0111(11) C41B 0.0527(18) 0.0395(19) 0.0421(18) 0.0108(16) -0.0081(15) -0.0163(15) C42B 0.0594(18) 0.0380(19) 0.0376(17) 0.0042(15) -0.0033(14) -0.0162(15) C43B 0.0337(15) 0.0416(19) 0.0260(15) 0.0094(14) -0.0045(12) -0.0070(13) C44B 0.0399(16) 0.0329(17) 0.0463(18) 0.0122(15) -0.0080(14) -0.0146(13) C45B 0.0389(16) 0.045(2) 0.0361(16) -0.0014(15) -0.0029(13) -0.0099(14) N46B 0.0570(15) 0.0350(16) 0.0373(13) 0.0036(13) -0.0059(11) -0.0126(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1A O1A 1.6176(18) . ? Si1A O2A 1.6126(18) . ? Si1A C1A 1.862(3) . ? Si1A C7A 1.865(3) . ? C1A C2A 1.384(4) . ? C1A C6A 1.400(4) . ? C2A C3A 1.412(4) . ? C3A C4A 1.381(5) . ? C4A C5A 1.349(5) . ? C5A C6A 1.376(4) . ? C7A C8A 1.397(3) . ? C7A C12A 1.394(3) . ? C8A C9A 1.381(4) . ? C9A C10A 1.390(4) . ? C10A C11A 1.370(4) . ? C11A C12A 1.387(4) . ? Si1B O1B 1.6314(17) . ? Si1B O2B 1.6218(17) . ? Si1B C1B 1.864(2) . ? Si1B C7B 1.860(3) . ? C1B C2B 1.397(3) . ? C1B C6B 1.395(3) . ? C2B C3B 1.383(3) . ? C3B C4B 1.372(4) . ? C4B C5B 1.379(4) . ? C5B C6B 1.393(3) . ? C7B C8B 1.401(3) . ? C7B C12B 1.399(3) . ? C8B C9B 1.380(4) . ? C9B C10B 1.374(4) . ? C10B C11B 1.380(4) . ? C11B C12B 1.383(4) . ? Si1C O1C 1.6183(17) . ? Si1C O2C 1.6169(18) . ? Si1C C1C 1.861(2) . ? Si1C C7C 1.858(3) . ? C1C C2C 1.397(3) . ? C1C C6C 1.397(3) . ? C2C C3C 1.384(4) . ? C3C C4C 1.372(4) . ? C4C C5C 1.364(4) . ? C5C C6C 1.378(4) . ? C7C C8C 1.404(3) . ? C7C C12C 1.402(3) . ? C8C C9C 1.387(4) . ? C9C C10C 1.383(4) . ? C10C C11C 1.368(4) . ? C11C C12C 1.374(4) . ? Si1D O1D 1.6308(16) . ? Si1D O2D 1.6253(17) . ? Si1D C1D 1.867(2) . ? Si1D C7D 1.859(3) . ? C1D C2D 1.397(3) . ? C1D C6D 1.391(3) . ? C2D C3D 1.377(3) . ? C3D C4D 1.383(3) . ? C4D C5D 1.376(4) . ? C5D C6D 1.386(3) . ? C7D C8D 1.403(3) . ? C7D C12D 1.401(3) . ? C8D C9D 1.387(4) . ? C9D C10D 1.373(4) . ? C10D C11D 1.385(4) . ? C11D C12D 1.374(4) . ? N20A C21A 1.339(3) . ? N20A C25A 1.322(3) . ? C21A C22A 1.377(4) . ? C22A C23A 1.380(4) . ? C23A C24A 1.376(4) . ? C23A N26A 1.452(3) . ? C24A C25A 1.369(4) . ? N26A N27A 1.205(3) . ? N27A C28A 1.465(3) . ? C28A C29A 1.366(4) . ? C28A C33A 1.375(4) . ? C29A C30A 1.374(3) . ? C30A N31A 1.329(3) . ? N31A C32A 1.338(3) . ? C32A C33A 1.387(3) . ? N20B C21B 1.342(3) . ? N20B C25B 1.323(3) . ? C21B C22B 1.386(3) . ? C22B C23B 1.366(3) . ? C23B C24B 1.379(4) . ? C23B N26B 1.469(3) . ? C24B C25B 1.370(4) . ? N26B N27B 1.201(3) . ? N27B C28B 1.488(3) . ? C28B C29B 1.360(4) . ? C28B C33B 1.374(4) . ? C29B C30B 1.382(3) . ? C30B N31B 1.328(3) . ? N31B C32B 1.335(3) . ? C32B C33B 1.397(3) . ? N40A C41A 1.3900 . ? N40A C45A 1.3900 . ? C41A C42A 1.3900 . ? C42A C43A 1.3900 . ? C43A C44A 1.3900 . ? C43A N46A 1.515(5) . ? C44A C45A 1.3900 . ? N46A N47A 1.113(5) . ? N47A C48A 1.423(5) . ? C48A C49A 1.3900 . ? C48A C53A 1.3900 . ? C49A C50A 1.3900 . ? C50A N51A 1.3900 . ? N51A C52A 1.3900 . ? C52A C53A 1.3900 . ? N40B C41B 1.323(3) . ? N40B C45B 1.328(3) . ? C41B C42B 1.372(3) . ? C42B C43B 1.367(3) . ? C43B C44B 1.369(4) . ? C43B N46B 1.451(3) . ? C44B C45B 1.386(3) . ? N46B N46B 1.219(4) 2_765 ? 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 O1A Si1A C1A 105.92(11) . . ? O1A Si1A C7A 109.47(11) . . ? O2A Si1A O1A 113.68(10) . . ? O2A Si1A C1A 104.10(10) . . ? O2A Si1A C7A 111.02(10) . . ? C1A Si1A C7A 112.50(11) . . ? C2A C1A Si1A 120.6(2) . . ? C2A C1A C6A 117.5(3) . . ? C6A C1A Si1A 121.9(2) . . ? C1A C2A C3A 120.7(3) . . ? C4A C3A C2A 118.5(3) . . ? C5A C4A C3A 121.9(3) . . ? C4A C5A C6A 119.4(3) . . ? C5A C6A C1A 121.9(3) . . ? C8A C7A Si1A 120.5(2) . . ? C12A C7A Si1A 122.7(2) . . ? C12A C7A C8A 116.7(2) . . ? C9A C8A C7A 121.7(3) . . ? C8A C9A C10A 120.0(3) . . ? C11A C10A C9A 119.6(3) . . ? C10A C11A C12A 120.0(3) . . ? C11A C12A C7A 122.0(3) . . ? O1B Si1B C1B 105.81(10) . . ? O1B Si1B C7B 109.57(10) . . ? O2B Si1B O1B 113.39(9) . . ? O2B Si1B C1B 107.31(10) . . ? O2B Si1B C7B 108.40(10) . . ? C7B Si1B C1B 112.39(11) . . ? C2B C1B Si1B 119.63(19) . . ? C6B C1B Si1B 123.32(19) . . ? C6B C1B C2B 117.0(2) . . ? C3B C2B C1B 121.9(3) . . ? C4B C3B C2B 119.8(3) . . ? C3B C4B C5B 119.9(3) . . ? C4B C5B C6B 120.1(3) . . ? C5B C6B C1B 121.0(3) . . ? C8B C7B Si1B 121.72(18) . . ? C12B C7B Si1B 121.98(19) . . ? C12B C7B C8B 116.3(2) . . ? C9B C8B C7B 121.6(2) . . ? C10B C9B C8B 120.6(3) . . ? C9B C10B C11B 119.5(3) . . ? C10B C11B C12B 119.9(3) . . ? C11B C12B C7B 122.1(2) . . ? O1C Si1C C1C 106.48(10) . . ? O1C Si1C C7C 109.19(10) . . ? O2C Si1C O1C 114.25(10) . . ? O2C Si1C C1C 103.97(10) . . ? O2C Si1C C7C 110.80(10) . . ? C7C Si1C C1C 112.03(11) . . ? C2C C1C Si1C 120.50(18) . . ? C2C C1C C6C 116.9(2) . . ? C6C C1C Si1C 122.57(19) . . ? C3C C2C C1C 121.3(3) . . ? C4C C3C C2C 120.0(3) . . ? C5C C4C C3C 120.0(3) . . ? C4C C5C C6C 120.4(3) . . ? C5C C6C C1C 121.3(3) . . ? C8C C7C Si1C 120.93(19) . . ? C12C C7C Si1C 122.5(2) . . ? C12C C7C C8C 116.6(2) . . ? C9C C8C C7C 121.6(2) . . ? C10C C9C C8C 119.5(3) . . ? C11C C10C C9C 120.1(3) . . ? C10C C11C C12C 120.6(3) . . ? C11C C12C C7C 121.6(3) . . ? O1D Si1D C1D 106.43(9) . . ? O1D Si1D C7D 109.26(10) . . ? O2D Si1D O1D 113.39(9) . . ? O2D Si1D C1D 107.22(10) . . ? O2D Si1D C7D 109.66(10) . . ? C7D Si1D C1D 110.83(11) . . ? C2D C1D Si1D 119.53(18) . . ? C6D C1D Si1D 123.70(18) . . ? C6D C1D C2D 116.8(2) . . ? C3D C2D C1D 122.2(2) . . ? C2D C3D C4D 119.8(2) . . ? C5D C4D C3D 119.4(2) . . ? C4D C5D C6D 120.6(2) . . ? C5D C6D C1D 121.3(2) . . ? C8D C7D Si1D 121.81(18) . . ? C12D C7D Si1D 121.8(2) . . ? C12D C7D C8D 116.3(2) . . ? C9D C8D C7D 121.9(2) . . ? C10D C9D C8D 119.7(3) . . ? C9D C10D C11D 120.1(3) . . ? C12D C11D C10D 120.0(3) . . ? C11D C12D C7D 122.0(3) . . ? C25A N20A C21A 116.3(2) . . ? N20A C21A C22A 123.9(3) . . ? C21A C22A C23A 117.8(3) . . ? C22A C23A N26A 126.6(2) . . ? C24A C23A C22A 119.2(2) . . ? C24A C23A N26A 114.2(3) . . ? C25A C24A C23A 118.1(3) . . ? N20A C25A C24A 124.6(3) . . ? N27A N26A C23A 112.6(2) . . ? N26A N27A C28A 112.3(2) . . ? C29A C28A N27A 115.5(3) . . ? C29A C28A C33A 119.3(2) . . ? C33A C28A N27A 125.3(2) . . ? C28A C29A C30A 118.4(3) . . ? N31A C30A C29A 124.3(3) . . ? C30A N31A C32A 116.6(2) . . ? N31A C32A C33A 123.2(3) . . ? C28A C33A C32A 118.3(2) . . ? C25B N20B C21B 116.5(2) . . ? N20B C21B C22B 123.6(3) . . ? C23B C22B C21B 117.9(3) . . ? C22B C23B C24B 119.4(2) . . ? C22B C23B N26B 127.1(2) . . ? C24B C23B N26B 113.5(2) . . ? C25B C24B C23B 118.4(3) . . ? N20B C25B C24B 124.1(3) . . ? N27B N26B C23B 110.5(2) . . ? N26B N27B C28B 110.4(2) . . ? C29B C28B N27B 114.2(3) . . ? C29B C28B C33B 119.8(2) . . ? C33B C28B N27B 125.9(3) . . ? C28B C29B C30B 118.2(3) . . ? N31B C30B C29B 124.2(3) . . ? C30B N31B C32B 116.8(2) . . ? N31B C32B C33B 123.1(3) . . ? C28B C33B C32B 118.0(2) . . ? C41A N40A C45A 120.0 . . ? N40A C41A C42A 120.0 . . ? C43A C42A C41A 120.0 . . ? C42A C43A C44A 120.0 . . ? C42A C43A N46A 115.3(3) . . ? C44A C43A N46A 124.5(3) . . ? C45A C44A C43A 120.0 . . ? C44A C45A N40A 120.0 . . ? N47A N46A C43A 110.6(4) . . ? N46A N47A C48A 112.2(6) . . ? C49A C48A N47A 108.5(4) . . ? C49A C48A C53A 120.0 . . ? C53A C48A N47A 131.5(4) . . ? C48A C49A C50A 120.0 . . ? N51A C50A C49A 120.0 . . ? C52A N51A C50A 120.0 . . ? N51A C52A C53A 120.0 . . ? C52A C53A C48A 120.0 . . ? C41B N40B C45B 117.7(2) . . ? N40B C41B C42B 124.0(3) . . ? C43B C42B C41B 117.5(3) . . ? C42B C43B C44B 120.3(2) . . ? C42B C43B N46B 114.7(2) . . ? C44B C43B N46B 125.1(2) . . ? C43B C44B C45B 117.9(3) . . ? N40B C45B C44B 122.6(3) . . ? N46B N46B C43B 111.6(3) 2_765 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1A H1A N31B 0.9000(1) 1.892(3) 2.787(3) 172.6(8) 2_665 O2A H2A O1B 0.9000(1) 1.815(4) 2.690(2) 163.7(11) . O1B H1B N40B 0.9000(1) 1.774(6) 2.660(3) 168(3) . O2B H2B N20B 0.9000(1) 1.931(3) 2.826(3) 172.4(7) 1_655 O1C H1C N31A 0.9000(1) 1.907(3) 2.802(3) 172.8(14) 1_655 O2C H2C O1D 0.9000(1) 1.849(3) 2.710(2) 159.5(6) 1_655 O1D H1D N40A 0.9000(1) 1.785(5) 2.684(4) 176.2(19) . O2D H2D N20A 0.9000(1) 1.935(4) 2.823(3) 168.6(12) 2_666 _olex2_submission_special_instructions 'No special instructions were received'