# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dsliu@sxu.edu.cn _publ_contact_author_name 'Liu, Diansheng' loop_ _publ_author_name 'Hongbo Tong' 'Min Li' 'Shifang Yuan' 'Shengdi Bai' 'Shuping Huang' 'Diansheng Liu' data_hs0264p _database_code_depnum_ccdc_archive 'CCDC 761269' #TrackingRef '- 2 3 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H60 Li2 N6 O2 Si2' _chemical_formula_weight 702.98 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.089(3) _cell_length_b 12.471(3) _cell_length_c 17.197(4) _cell_angle_alpha 81.586(4) _cell_angle_beta 75.624(4) _cell_angle_gamma 67.478(4) _cell_volume 2124.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 1364 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 19.91 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9647 _exptl_absorpt_correction_T_max 0.9763 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8820 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.1285 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7344 _reflns_number_gt 4162 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7344 _refine_ls_number_parameters 455 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.2789(7) 0.2648(6) 0.1675(4) 0.0328(19) Uani 1 1 d D . . Li2 Li 0.2053(7) 0.2413(6) 0.3170(5) 0.041(2) Uani 1 1 d D A . N1 N 0.1591(3) 0.3908(3) 0.2519(2) 0.0280(9) Uani 1 1 d D . . N2 N -0.0201(3) 0.2980(3) 0.3413(2) 0.0354(10) Uani 1 1 d . . . H2B H -0.0403 0.2543 0.3121 0.042 Uiso 1 1 calc R . . N3 N -0.0747(3) 0.4184(3) 0.1996(2) 0.0364(10) Uani 1 1 d . . . N4 N 0.3001(3) 0.1101(3) 0.2384(2) 0.0274(9) Uani 1 1 d . . . N5 N 0.1495(3) 0.2007(3) 0.1245(2) 0.0290(9) Uani 1 1 d . . . H5A H 0.0643 0.2416 0.1492 0.035 Uiso 1 1 calc R . . N6 N 0.0643(3) 0.0643(3) 0.2521(2) 0.0397(10) Uani 1 1 d . . . O1 O 0.4354(3) 0.2728(2) 0.08572(18) 0.0414(8) Uani 1 1 d . . . O2 O 0.2679(3) 0.2221(3) 0.41929(19) 0.0512(9) Uani 1 1 d DU . . Si1 Si -0.00646(12) 0.42081(10) 0.27968(8) 0.0311(4) Uani 1 1 d . . . Si2 Si 0.20760(12) 0.07619(10) 0.18859(8) 0.0302(3) Uani 1 1 d . . . C1 C 0.2223(4) 0.4715(3) 0.2369(3) 0.0281(11) Uani 1 1 d . . . C2 C 0.1655(4) 0.5891(4) 0.2142(3) 0.0360(12) Uani 1 1 d . . . H2A H 0.0771 0.6187 0.2087 0.043 Uiso 1 1 calc R . . C3 C 0.2357(5) 0.6629(4) 0.1997(3) 0.0482(14) Uani 1 1 d . . . H3 H 0.1930 0.7409 0.1856 0.058 Uiso 1 1 calc R . . C4 C 0.3666(5) 0.6239(4) 0.2057(3) 0.0513(15) Uani 1 1 d . . . H4 H 0.4140 0.6738 0.1948 0.062 Uiso 1 1 calc R . . C5 C 0.4261(5) 0.5080(4) 0.2283(3) 0.0574(16) Uani 1 1 d . . . H5 H 0.5146 0.4794 0.2335 0.069 Uiso 1 1 calc R . . C6 C 0.3559(4) 0.4343(4) 0.2431(3) 0.0444(14) Uani 1 1 d . . . H6 H 0.3990 0.3566 0.2578 0.053 Uiso 1 1 calc R . . C7 C -0.1097(4) 0.5556(4) 0.3347(3) 0.0476(14) Uani 1 1 d . . . H7A H -0.0599 0.5679 0.3687 0.071 Uiso 1 1 calc R . . H7B H -0.1900 0.5472 0.3671 0.071 Uiso 1 1 calc R . . H7C H -0.1322 0.6209 0.2968 0.071 Uiso 1 1 calc R . . C8 C -0.0492(4) 0.4898(4) 0.1263(3) 0.0493(14) Uani 1 1 d . . . H8A H -0.0576 0.4579 0.0813 0.074 Uiso 1 1 calc R . . H8B H 0.0395 0.4903 0.1177 0.074 Uiso 1 1 calc R . . H8C H -0.1127 0.5678 0.1320 0.074 Uiso 1 1 calc R . . C9 C -0.2136(4) 0.4246(4) 0.2169(3) 0.0572(16) Uani 1 1 d . . . H9A H -0.2727 0.5043 0.2215 0.086 Uiso 1 1 calc R . . H9B H -0.2310 0.3812 0.2666 0.086 Uiso 1 1 calc R . . H9C H -0.2279 0.3924 0.1742 0.086 Uiso 1 1 calc R . . C10 C -0.0984(4) 0.2994(4) 0.4202(3) 0.0367(12) Uani 1 1 d . . . C11 C -0.0862(4) 0.3549(4) 0.4801(3) 0.0461(14) Uani 1 1 d . . . H11 H -0.0262 0.3934 0.4684 0.055 Uiso 1 1 calc R . . C12 C -0.1614(5) 0.3542(4) 0.5570(3) 0.0531(14) Uani 1 1 d . . . H12 H -0.1514 0.3918 0.5964 0.064 Uiso 1 1 calc R . . C13 C -0.2514(5) 0.2981(5) 0.5757(3) 0.0606(16) Uani 1 1 d . . . H13 H -0.3022 0.2977 0.6276 0.073 Uiso 1 1 calc R . . C14 C -0.2650(5) 0.2431(4) 0.5173(4) 0.0575(16) Uani 1 1 d . . . H14 H -0.3251 0.2046 0.5296 0.069 Uiso 1 1 calc R . . C15 C -0.1902(4) 0.2439(4) 0.4395(3) 0.0441(13) Uani 1 1 d . . . H15 H -0.2016 0.2071 0.4001 0.053 Uiso 1 1 calc R . . C16 C 0.4449(5) 0.3552(5) 0.0213(4) 0.0802(15) Uani 1 1 d . . . H16A H 0.4910 0.3145 -0.0277 0.096 Uiso 1 1 calc R . . H16B H 0.4987 0.3957 0.0308 0.096 Uiso 1 1 calc R . . C17 C 0.3203(5) 0.4384(4) 0.0095(4) 0.080(2) Uani 1 1 d . . . H17A H 0.2641 0.3992 0.0031 0.119 Uiso 1 1 calc R . . H17B H 0.3342 0.4871 -0.0379 0.119 Uiso 1 1 calc R . . H17C H 0.2782 0.4854 0.0552 0.119 Uiso 1 1 calc R . . C18 C 0.5545(4) 0.1712(4) 0.0802(3) 0.0532(15) Uani 1 1 d . . . H18A H 0.5782 0.1422 0.0270 0.064 Uiso 1 1 calc R . . H18B H 0.5367 0.1113 0.1189 0.064 Uiso 1 1 calc R . . C19 C 0.6718(5) 0.1927(5) 0.0954(4) 0.081(2) Uani 1 1 d . . . H19A H 0.7040 0.2368 0.0502 0.122 Uiso 1 1 calc R . . H19B H 0.7417 0.1196 0.1027 0.122 Uiso 1 1 calc R . . H19C H 0.6439 0.2353 0.1429 0.122 Uiso 1 1 calc R . . C20 C 0.4100(4) 0.0288(4) 0.2667(3) 0.0304(11) Uani 1 1 d . . . C21 C 0.5069(4) 0.0646(4) 0.2813(3) 0.0365(12) Uani 1 1 d . . . H21 H 0.4967 0.1426 0.2714 0.044 Uiso 1 1 calc R . . C22 C 0.6177(4) -0.0115(4) 0.3098(3) 0.0467(14) Uani 1 1 d . . . H22 H 0.6802 0.0158 0.3185 0.056 Uiso 1 1 calc R . . C23 C 0.6356(5) -0.1283(4) 0.3254(3) 0.0539(15) Uani 1 1 d . . . H23 H 0.7096 -0.1799 0.3446 0.065 Uiso 1 1 calc R . . C24 C 0.5418(5) -0.1661(4) 0.3120(3) 0.0489(14) Uani 1 1 d . . . H24 H 0.5527 -0.2442 0.3222 0.059 Uiso 1 1 calc R . . C25 C 0.4324(4) -0.0907(4) 0.2838(3) 0.0374(12) Uani 1 1 d . . . H25 H 0.3706 -0.1192 0.2757 0.045 Uiso 1 1 calc R . . C26 C 0.2967(4) -0.0497(3) 0.1240(3) 0.0426(13) Uani 1 1 d . . . H26A H 0.3839 -0.0496 0.0980 0.064 Uiso 1 1 calc R . . H26B H 0.2471 -0.0441 0.0841 0.064 Uiso 1 1 calc R . . H26C H 0.3052 -0.1206 0.1565 0.064 Uiso 1 1 calc R . . C27 C -0.0373(5) 0.0538(5) 0.2170(3) 0.0686(17) Uani 1 1 d . . . H27A H -0.0181 -0.0268 0.2109 0.103 Uiso 1 1 calc R . . H27B H -0.0371 0.0951 0.1653 0.103 Uiso 1 1 calc R . . H27C H -0.1234 0.0861 0.2516 0.103 Uiso 1 1 calc R . . C28 C 0.0771(4) -0.0053(4) 0.3276(3) 0.0547(15) Uani 1 1 d . . . H28A H -0.0066 0.0201 0.3656 0.082 Uiso 1 1 calc R . . H28B H 0.1448 0.0038 0.3488 0.082 Uiso 1 1 calc R . . H28C H 0.1015 -0.0857 0.3183 0.082 Uiso 1 1 calc R . . C29 C 0.1461(4) 0.1951(3) 0.0432(3) 0.0314(11) Uani 1 1 d . . . C30 C 0.2629(4) 0.1588(3) -0.0153(3) 0.0358(12) Uani 1 1 d . . . H30 H 0.3445 0.1401 -0.0011 0.043 Uiso 1 1 calc R . . C31 C 0.2609(5) 0.1498(4) -0.0934(3) 0.0458(13) Uani 1 1 d . . . H31 H 0.3406 0.1248 -0.1312 0.055 Uiso 1 1 calc R . . C32 C 0.1415(6) 0.1777(4) -0.1161(3) 0.0505(14) Uani 1 1 d . . . H32 H 0.1401 0.1697 -0.1687 0.061 Uiso 1 1 calc R . . C33 C 0.0242(5) 0.2174(4) -0.0600(3) 0.0545(15) Uani 1 1 d . . . H33 H -0.0572 0.2389 -0.0750 0.065 Uiso 1 1 calc R . . C34 C 0.0275(5) 0.2255(4) 0.0183(3) 0.0440(13) Uani 1 1 d . . . H34 H -0.0526 0.2522 0.0556 0.053 Uiso 1 1 calc R . . C35 C 0.2737(5) 0.3204(5) 0.4475(4) 0.081(2) Uani 1 1 d . A . H35A H 0.2171 0.3341 0.5008 0.097 Uiso 1 1 calc R . . H35B H 0.2376 0.3877 0.4125 0.097 Uiso 1 1 calc R . . C36 C 0.4114(6) 0.3099(6) 0.4514(4) 0.100(2) Uani 1 1 d . . . H36A H 0.4449 0.2482 0.4899 0.151 Uiso 1 1 calc R A . H36B H 0.4082 0.3817 0.4675 0.151 Uiso 1 1 calc R . . H36C H 0.4693 0.2931 0.3994 0.151 Uiso 1 1 calc R . . C37A C 0.3018(7) 0.1118(7) 0.4686(5) 0.0802(15) Uani 0.796(8) 1 d PDU A 1 H37A H 0.3551 0.0483 0.4337 0.096 Uiso 0.796(8) 1 calc PR A 1 H37B H 0.3554 0.1139 0.5048 0.096 Uiso 0.796(8) 1 calc PR A 1 C38A C 0.1833(7) 0.0900(7) 0.5156(5) 0.0802(15) Uani 0.796(8) 1 d PDU A 1 H38A H 0.2099 0.0149 0.5435 0.120 Uiso 0.796(8) 1 calc PR A 1 H38B H 0.1274 0.0921 0.4803 0.120 Uiso 0.796(8) 1 calc PR A 1 H38C H 0.1346 0.1486 0.5539 0.120 Uiso 0.796(8) 1 calc PR A 1 C37B C 0.241(3) 0.165(2) 0.5090(11) 0.0802(15) Uani 0.204(8) 1 d PDU A 2 H37C H 0.1544 0.2067 0.5416 0.096 Uiso 0.204(8) 1 calc PR A 2 H37D H 0.3120 0.1502 0.5374 0.096 Uiso 0.204(8) 1 calc PR A 2 C38B C 0.248(3) 0.0518(16) 0.4688(17) 0.0802(15) Uani 0.204(8) 1 d PDU A 2 H38D H 0.2566 -0.0119 0.5086 0.120 Uiso 0.204(8) 1 calc PR A 2 H38E H 0.3242 0.0306 0.4249 0.120 Uiso 0.204(8) 1 calc PR A 2 H38F H 0.1682 0.0698 0.4495 0.120 Uiso 0.204(8) 1 calc PR A 2 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 Li1 0.032(4) 0.027(4) 0.035(5) 0.000(4) -0.005(4) -0.008(3) Li2 0.032(4) 0.040(5) 0.053(6) -0.004(4) -0.013(4) -0.011(4) N1 0.0208(19) 0.025(2) 0.036(2) -0.0026(17) -0.0035(17) -0.0065(16) N2 0.033(2) 0.038(2) 0.035(3) -0.0078(19) 0.0043(19) -0.0179(18) N3 0.024(2) 0.040(2) 0.042(3) 0.001(2) -0.0068(19) -0.0102(18) N4 0.025(2) 0.026(2) 0.029(2) 0.0006(17) -0.0054(17) -0.0075(16) N5 0.0221(19) 0.037(2) 0.026(2) -0.0033(18) -0.0025(17) -0.0095(17) N6 0.041(2) 0.046(3) 0.036(3) 0.005(2) -0.004(2) -0.024(2) O1 0.0370(19) 0.041(2) 0.042(2) 0.0069(17) -0.0036(16) -0.0158(16) O2 0.056(2) 0.058(2) 0.036(2) 0.0005(18) -0.0123(18) -0.0171(18) Si1 0.0252(7) 0.0278(7) 0.0366(9) -0.0041(6) -0.0023(6) -0.0072(6) Si2 0.0328(7) 0.0272(7) 0.0308(8) -0.0003(6) -0.0041(6) -0.0131(6) C1 0.027(3) 0.026(3) 0.029(3) -0.001(2) -0.008(2) -0.006(2) C2 0.037(3) 0.029(3) 0.044(3) 0.005(2) -0.012(2) -0.015(2) C3 0.059(4) 0.033(3) 0.057(4) 0.006(3) -0.018(3) -0.022(3) C4 0.055(4) 0.048(4) 0.060(4) -0.002(3) -0.003(3) -0.034(3) C5 0.033(3) 0.049(4) 0.092(5) -0.011(3) -0.007(3) -0.019(3) C6 0.030(3) 0.029(3) 0.074(4) -0.005(3) -0.013(3) -0.007(2) C7 0.035(3) 0.041(3) 0.055(4) -0.012(3) 0.004(3) -0.006(2) C8 0.050(3) 0.042(3) 0.059(4) -0.001(3) -0.022(3) -0.014(3) C9 0.034(3) 0.064(4) 0.073(4) -0.002(3) -0.009(3) -0.019(3) C10 0.030(3) 0.031(3) 0.042(3) -0.005(2) -0.001(2) -0.007(2) C11 0.040(3) 0.045(3) 0.051(4) -0.007(3) -0.004(3) -0.015(3) C12 0.061(4) 0.051(4) 0.042(4) -0.009(3) -0.007(3) -0.014(3) C13 0.062(4) 0.057(4) 0.037(4) 0.000(3) 0.015(3) -0.009(3) C14 0.048(3) 0.060(4) 0.056(4) 0.009(3) 0.005(3) -0.024(3) C15 0.040(3) 0.049(3) 0.042(4) -0.001(3) 0.002(3) -0.022(3) C16 0.069(3) 0.086(3) 0.078(4) 0.034(3) -0.023(3) -0.028(3) C17 0.074(4) 0.060(4) 0.100(6) 0.034(4) -0.032(4) -0.024(3) C18 0.038(3) 0.064(4) 0.050(4) -0.021(3) 0.007(3) -0.014(3) C19 0.041(3) 0.083(4) 0.117(6) 0.009(4) -0.020(4) -0.024(3) C20 0.034(3) 0.028(3) 0.026(3) -0.002(2) 0.000(2) -0.011(2) C21 0.035(3) 0.030(3) 0.039(3) 0.002(2) -0.010(2) -0.005(2) C22 0.038(3) 0.055(4) 0.045(4) 0.002(3) -0.015(3) -0.013(3) C23 0.050(3) 0.047(4) 0.043(4) 0.000(3) -0.016(3) 0.010(3) C24 0.056(4) 0.031(3) 0.042(4) -0.003(3) -0.007(3) 0.002(3) C25 0.039(3) 0.033(3) 0.033(3) -0.002(2) -0.004(2) -0.007(2) C26 0.050(3) 0.033(3) 0.048(4) -0.004(2) -0.013(3) -0.015(2) C27 0.069(4) 0.094(5) 0.063(4) 0.008(3) -0.008(3) -0.059(4) C28 0.047(3) 0.047(3) 0.060(4) 0.000(3) 0.005(3) -0.016(3) C29 0.039(3) 0.021(3) 0.034(3) -0.002(2) -0.009(2) -0.009(2) C30 0.036(3) 0.031(3) 0.034(3) -0.004(2) -0.006(2) -0.005(2) C31 0.062(4) 0.038(3) 0.030(3) -0.004(3) -0.001(3) -0.014(3) C32 0.077(4) 0.047(3) 0.038(4) -0.001(3) -0.024(3) -0.026(3) C33 0.056(4) 0.065(4) 0.047(4) 0.005(3) -0.026(3) -0.020(3) C34 0.036(3) 0.053(3) 0.042(4) 0.001(3) -0.012(3) -0.014(2) C35 0.064(4) 0.109(5) 0.074(5) -0.050(4) -0.017(4) -0.018(4) C36 0.091(5) 0.135(6) 0.108(6) -0.012(5) -0.044(5) -0.059(5) C37A 0.069(3) 0.086(3) 0.078(4) 0.034(3) -0.023(3) -0.028(3) C38A 0.069(3) 0.086(3) 0.078(4) 0.034(3) -0.023(3) -0.028(3) C37B 0.069(3) 0.086(3) 0.078(4) 0.034(3) -0.023(3) -0.028(3) C38B 0.069(3) 0.086(3) 0.078(4) 0.034(3) -0.023(3) -0.028(3) _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 Li1 O1 1.969(7) . ? Li1 N1 2.110(7) . ? Li1 N4 2.091(8) . ? Li1 N5 2.197(8) . ? Li2 O2 1.999(9) . ? Li2 N4 2.057(9) . ? Li2 N1 1.983(8) . ? Li2 N2 2.266(8) . ? N1 C1 1.395(5) . ? N1 Si1 1.682(3) . ? N2 C10 1.417(5) . ? N2 Si1 1.764(4) . ? N2 H2B 0.9100 . ? N3 C8 1.465(5) . ? N3 C9 1.468(5) . ? N3 Si1 1.737(4) . ? N4 C20 1.398(5) . ? N4 Si2 1.685(3) . ? N5 C29 1.419(5) . ? N5 Si2 1.769(3) . ? N5 H5A 0.9100 . ? N6 C27 1.458(5) . ? N6 C28 1.458(6) . ? N6 Si2 1.736(4) . ? O1 C16 1.410(5) . ? O1 C18 1.432(5) . ? O2 C37B 1.607(17) . ? O2 C35 1.411(6) . ? O2 C37A 1.474(7) . ? Si1 C7 1.867(4) . ? Si2 C26 1.858(4) . ? C1 C2 1.395(5) . ? C1 C6 1.399(5) . ? C2 C3 1.378(5) . ? C2 H2A 0.9300 . ? C3 C4 1.369(6) . ? C3 H3 0.9300 . ? C4 C5 1.381(6) . ? C4 H4 0.9300 . ? C5 C6 1.377(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.381(6) . ? C10 C15 1.389(6) . ? C11 C12 1.377(6) . ? C11 H11 0.9300 . ? C12 C13 1.378(7) . ? C12 H12 0.9300 . ? C13 C14 1.363(7) . ? C13 H13 0.9300 . ? C14 C15 1.388(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.417(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.512(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.397(5) . ? C20 C25 1.412(5) . ? C21 C22 1.386(6) . ? C21 H21 0.9300 . ? C22 C23 1.387(6) . ? C22 H22 0.9300 . ? C23 C24 1.372(6) . ? C23 H23 0.9300 . ? C24 C25 1.369(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.382(6) . ? C29 C30 1.390(5) . ? C30 C31 1.370(6) . ? C30 H30 0.9300 . ? C31 C32 1.375(6) . ? C31 H31 0.9300 . ? C32 C33 1.374(6) . ? C32 H32 0.9300 . ? C33 C34 1.375(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.500(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37A C38A 1.462(8) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C38A H38A 0.9600 . ? C38A H38B 0.9600 . ? C38A H38C 0.9600 . ? C37B C38B 1.633(18) . ? C37B H37C 0.9700 . ? C37B H37D 0.9700 . ? C38B H38D 0.9600 . ? C38B H38E 0.9600 . ? C38B H38F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 N1 125.5(4) . . ? O1 Li1 N4 117.7(3) . . ? N1 Li1 N4 101.7(3) . . ? O1 Li1 N5 114.3(4) . . ? N1 Li1 N5 108.8(3) . . ? N4 Li1 N5 78.9(3) . . ? O2 Li2 N4 118.1(4) . . ? O2 Li2 N1 122.4(4) . . ? N4 Li2 N1 107.5(4) . . ? O2 Li2 N2 110.8(4) . . ? N4 Li2 N2 112.6(4) . . ? N1 Li2 N2 79.1(3) . . ? C1 N1 Si1 126.1(3) . . ? C1 N1 Li2 128.3(3) . . ? Si1 N1 Li2 94.1(3) . . ? C1 N1 Li1 103.3(3) . . ? Si1 N1 Li1 120.4(3) . . ? Li2 N1 Li1 75.4(3) . . ? C10 N2 Si1 126.0(3) . . ? C10 N2 Li2 122.1(4) . . ? Si1 N2 Li2 82.7(2) . . ? C10 N2 H2B 107.7 . . ? Si1 N2 H2B 107.7 . . ? Li2 N2 H2B 107.7 . . ? C8 N3 C9 109.9(4) . . ? C8 N3 Si1 118.1(3) . . ? C9 N3 Si1 118.1(3) . . ? C20 N4 Si2 124.2(3) . . ? C20 N4 Li2 108.5(3) . . ? Si2 N4 Li2 118.5(3) . . ? C20 N4 Li1 131.2(3) . . ? Si2 N4 Li1 90.9(3) . . ? Li2 N4 Li1 74.3(3) . . ? C29 N5 Si2 123.3(3) . . ? C29 N5 Li1 126.8(3) . . ? Si2 N5 Li1 85.4(2) . . ? C29 N5 H5A 106.2 . . ? Si2 N5 H5A 106.2 . . ? Li1 N5 H5A 106.2 . . ? C27 N6 C28 112.0(4) . . ? C27 N6 Si2 118.8(3) . . ? C28 N6 Si2 118.3(3) . . ? C16 O1 C18 112.3(4) . . ? C16 O1 Li1 130.1(4) . . ? C18 O1 Li1 116.7(3) . . ? C37B O2 C35 92.0(7) . . ? C37B O2 C37A 36.4(8) . . ? C35 O2 C37A 118.6(6) . . ? C37B O2 Li2 138.8(9) . . ? C35 O2 Li2 118.3(4) . . ? C37A O2 Li2 123.1(5) . . ? N1 Si1 N3 111.98(18) . . ? N1 Si1 N2 103.96(16) . . ? N3 Si1 N2 103.13(18) . . ? N1 Si1 C7 117.27(19) . . ? N3 Si1 C7 109.67(19) . . ? N2 Si1 C7 109.7(2) . . ? N4 Si2 N6 111.75(19) . . ? N4 Si2 N5 104.27(16) . . ? N6 Si2 N5 104.86(17) . . ? N4 Si2 C26 116.50(18) . . ? N6 Si2 C26 111.30(19) . . ? N5 Si2 C26 107.11(19) . . ? C2 C1 N1 126.1(4) . . ? C2 C1 C6 114.9(4) . . ? N1 C1 C6 119.0(4) . . ? C3 C2 C1 122.4(4) . . ? C3 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C4 C3 C2 121.5(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 117.7(4) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 122.7(4) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 118.0(5) . . ? C11 C10 N2 121.7(4) . . ? C15 C10 N2 120.3(4) . . ? C12 C11 C10 121.2(5) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.5(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.2(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.8(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 120.4(5) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? O1 C16 C17 114.3(5) . . ? O1 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? O1 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C18 C19 113.4(4) . . ? O1 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? O1 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 N4 119.8(4) . . ? C21 C20 C25 115.1(4) . . ? N4 C20 C25 125.1(4) . . ? C22 C21 C20 122.6(4) . . ? C22 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C23 C22 C21 120.1(5) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 118.6(5) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 121.1(5) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C20 122.4(5) . . ? C24 C25 H25 118.8 . . ? C20 C25 H25 118.8 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 H27A 109.5 . . ? N6 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N6 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 H28A 109.5 . . ? N6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 116.8(4) . . ? C34 C29 N5 122.0(4) . . ? C30 C29 N5 121.2(4) . . ? C31 C30 C29 121.7(4) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C32 120.3(5) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 119.2(5) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 120.0(5) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C29 122.0(5) . . ? C33 C34 H34 119.0 . . ? C29 C34 H34 119.0 . . ? O2 C35 C36 114.3(5) . . ? O2 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? O2 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38A C37A O2 112.4(6) . . ? C38A C37A H37A 109.1 . . ? O2 C37A H37A 109.1 . . ? C38A C37A H37B 109.1 . . ? O2 C37A H37B 109.1 . . ? H37A C37A H37B 107.9 . . ? C37A C38A H38A 109.5 . . ? C37A C38A H38B 109.5 . . ? H38A C38A H38B 109.5 . . ? C37A C38A H38C 109.5 . . ? H38A C38A H38C 109.5 . . ? H38B C38A H38C 109.5 . . ? O2 C37B C38B 87.5(12) . . ? O2 C37B H37C 114.1 . . ? C38B C37B H37C 114.1 . . ? O2 C37B H37D 114.1 . . ? C38B C37B H37D 114.1 . . ? H37C C37B H37D 111.3 . . ? C37B C38B H38D 109.5 . . ? C37B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? 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 O2 Li2 N1 C1 38.3(7) . . . . ? N4 Li2 N1 C1 -103.4(5) . . . . ? N2 Li2 N1 C1 146.1(4) . . . . ? O2 Li2 N1 Si1 -105.8(4) . . . . ? N4 Li2 N1 Si1 112.5(3) . . . . ? N2 Li2 N1 Si1 2.0(2) . . . . ? O2 Li2 N1 Li1 133.9(5) . . . . ? N4 Li2 N1 Li1 -7.8(3) . . . . ? N2 Li2 N1 Li1 -118.3(3) . . . . ? O1 Li1 N1 C1 -2.8(5) . . . . ? N4 Li1 N1 C1 134.1(3) . . . . ? N5 Li1 N1 C1 -143.8(3) . . . . ? O1 Li1 N1 Si1 144.4(4) . . . . ? N4 Li1 N1 Si1 -78.7(4) . . . . ? N5 Li1 N1 Si1 3.5(4) . . . . ? O1 Li1 N1 Li2 -129.4(5) . . . . ? N4 Li1 N1 Li2 7.5(3) . . . . ? N5 Li1 N1 Li2 89.7(4) . . . . ? O2 Li2 N2 C10 -9.6(5) . . . . ? N4 Li2 N2 C10 125.2(4) . . . . ? N1 Li2 N2 C10 -130.3(4) . . . . ? O2 Li2 N2 Si1 118.8(3) . . . . ? N4 Li2 N2 Si1 -106.5(4) . . . . ? N1 Li2 N2 Si1 -1.9(2) . . . . ? O2 Li2 N4 C20 -6.8(5) . . . . ? N1 Li2 N4 C20 136.8(3) . . . . ? N2 Li2 N4 C20 -138.0(4) . . . . ? O2 Li2 N4 Si2 142.0(3) . . . . ? N1 Li2 N4 Si2 -74.4(4) . . . . ? N2 Li2 N4 Si2 10.8(5) . . . . ? O2 Li2 N4 Li1 -135.7(5) . . . . ? N1 Li2 N4 Li1 8.0(3) . . . . ? N2 Li2 N4 Li1 93.2(4) . . . . ? O1 Li1 N4 C20 32.7(7) . . . . ? N1 Li1 N4 C20 -108.3(4) . . . . ? N5 Li1 N4 C20 144.5(4) . . . . ? O1 Li1 N4 Si2 -106.8(4) . . . . ? N1 Li1 N4 Si2 112.1(3) . . . . ? N5 Li1 N4 Si2 4.95(19) . . . . ? O1 Li1 N4 Li2 133.8(5) . . . . ? N1 Li1 N4 Li2 -7.3(3) . . . . ? N5 Li1 N4 Li2 -114.4(3) . . . . ? O1 Li1 N5 C29 -18.0(5) . . . . ? N1 Li1 N5 C29 127.7(4) . . . . ? N4 Li1 N5 C29 -133.6(4) . . . . ? O1 Li1 N5 Si2 110.8(3) . . . . ? N1 Li1 N5 Si2 -103.5(3) . . . . ? N4 Li1 N5 Si2 -4.73(19) . . . . ? N1 Li1 O1 C16 -61.5(7) . . . . ? N4 Li1 O1 C16 167.6(5) . . . . ? N5 Li1 O1 C16 77.6(6) . . . . ? N1 Li1 O1 C18 130.9(4) . . . . ? N4 Li1 O1 C18 0.0(6) . . . . ? N5 Li1 O1 C18 -90.0(4) . . . . ? N4 Li2 O2 C37B -86.9(17) . . . . ? N1 Li2 O2 C37B 135.2(16) . . . . ? N2 Li2 O2 C37B 45.1(17) . . . . ? N4 Li2 O2 C35 140.7(4) . . . . ? N1 Li2 O2 C35 2.8(6) . . . . ? N2 Li2 O2 C35 -87.3(5) . . . . ? N4 Li2 O2 C37A -42.5(6) . . . . ? N1 Li2 O2 C37A 179.6(5) . . . . ? N2 Li2 O2 C37A 89.5(5) . . . . ? C1 N1 Si1 N3 101.5(4) . . . . ? Li2 N1 Si1 N3 -113.3(3) . . . . ? Li1 N1 Si1 N3 -37.8(3) . . . . ? C1 N1 Si1 N2 -147.8(3) . . . . ? Li2 N1 Si1 N2 -2.6(3) . . . . ? Li1 N1 Si1 N2 72.9(3) . . . . ? C1 N1 Si1 C7 -26.5(4) . . . . ? Li2 N1 Si1 C7 118.6(3) . . . . ? Li1 N1 Si1 C7 -165.8(3) . . . . ? C8 N3 Si1 N1 -53.2(3) . . . . ? C9 N3 Si1 N1 170.5(3) . . . . ? C8 N3 Si1 N2 -164.4(3) . . . . ? C9 N3 Si1 N2 59.3(3) . . . . ? C8 N3 Si1 C7 78.8(3) . . . . ? C9 N3 Si1 C7 -57.5(4) . . . . ? C10 N2 Si1 N1 127.0(4) . . . . ? Li2 N2 Si1 N1 2.3(3) . . . . ? C10 N2 Si1 N3 -116.0(4) . . . . ? Li2 N2 Si1 N3 119.3(3) . . . . ? C10 N2 Si1 C7 0.8(4) . . . . ? Li2 N2 Si1 C7 -123.9(3) . . . . ? C20 N4 Si2 N6 97.2(3) . . . . ? Li2 N4 Si2 N6 -46.3(3) . . . . ? Li1 N4 Si2 N6 -119.0(2) . . . . ? C20 N4 Si2 N5 -150.0(3) . . . . ? Li2 N4 Si2 N5 66.4(3) . . . . ? Li1 N4 Si2 N5 -6.2(2) . . . . ? C20 N4 Si2 C26 -32.3(4) . . . . ? Li2 N4 Si2 C26 -175.8(3) . . . . ? Li1 N4 Si2 C26 111.5(3) . . . . ? C27 N6 Si2 N4 170.3(3) . . . . ? C28 N6 Si2 N4 -48.3(4) . . . . ? C27 N6 Si2 N5 58.0(4) . . . . ? C28 N6 Si2 N5 -160.6(3) . . . . ? C27 N6 Si2 C26 -57.5(4) . . . . ? C28 N6 Si2 C26 83.9(4) . . . . ? C29 N5 Si2 N4 137.7(3) . . . . ? Li1 N5 Si2 N4 6.0(2) . . . . ? C29 N5 Si2 N6 -104.7(3) . . . . ? Li1 N5 Si2 N6 123.5(2) . . . . ? C29 N5 Si2 C26 13.7(4) . . . . ? Li1 N5 Si2 C26 -118.1(2) . . . . ? Si1 N1 C1 C2 -24.2(6) . . . . ? Li2 N1 C1 C2 -157.8(5) . . . . ? Li1 N1 C1 C2 120.4(5) . . . . ? Si1 N1 C1 C6 157.0(3) . . . . ? Li2 N1 C1 C6 23.5(6) . . . . ? Li1 N1 C1 C6 -58.3(5) . . . . ? N1 C1 C2 C3 -179.3(4) . . . . ? C6 C1 C2 C3 -0.5(7) . . . . ? C1 C2 C3 C4 1.1(8) . . . . ? C2 C3 C4 C5 -1.2(8) . . . . ? C3 C4 C5 C6 0.9(8) . . . . ? C4 C5 C6 C1 -0.5(8) . . . . ? C2 C1 C6 C5 0.3(7) . . . . ? N1 C1 C6 C5 179.1(4) . . . . ? Si1 N2 C10 C11 -53.9(6) . . . . ? Li2 N2 C10 C11 51.9(6) . . . . ? Si1 N2 C10 C15 126.3(4) . . . . ? Li2 N2 C10 C15 -127.9(4) . . . . ? C15 C10 C11 C12 0.8(7) . . . . ? N2 C10 C11 C12 -179.0(4) . . . . ? C10 C11 C12 C13 -0.3(8) . . . . ? C11 C12 C13 C14 0.1(8) . . . . ? C12 C13 C14 C15 -0.4(8) . . . . ? C13 C14 C15 C10 1.0(8) . . . . ? C11 C10 C15 C14 -1.2(7) . . . . ? N2 C10 C15 C14 178.7(4) . . . . ? C18 O1 C16 C17 161.2(5) . . . . ? Li1 O1 C16 C17 -6.8(9) . . . . ? C16 O1 C18 C19 70.3(6) . . . . ? Li1 O1 C18 C19 -120.0(5) . . . . ? Si2 N4 C20 C21 157.6(3) . . . . ? Li2 N4 C20 C21 -55.8(5) . . . . ? Li1 N4 C20 C21 29.2(6) . . . . ? Si2 N4 C20 C25 -23.4(6) . . . . ? Li2 N4 C20 C25 123.2(5) . . . . ? Li1 N4 C20 C25 -151.7(4) . . . . ? N4 C20 C21 C22 179.6(4) . . . . ? C25 C20 C21 C22 0.5(6) . . . . ? C20 C21 C22 C23 -0.3(7) . . . . ? C21 C22 C23 C24 0.0(7) . . . . ? C22 C23 C24 C25 -0.1(7) . . . . ? C23 C24 C25 C20 0.4(7) . . . . ? C21 C20 C25 C24 -0.5(6) . . . . ? N4 C20 C25 C24 -179.6(4) . . . . ? Si2 N5 C29 C34 110.0(4) . . . . ? Li1 N5 C29 C34 -138.2(4) . . . . ? Si2 N5 C29 C30 -70.2(5) . . . . ? Li1 N5 C29 C30 41.6(6) . . . . ? C34 C29 C30 C31 -2.1(6) . . . . ? N5 C29 C30 C31 178.1(4) . . . . ? C29 C30 C31 C32 0.5(7) . . . . ? C30 C31 C32 C33 1.7(7) . . . . ? C31 C32 C33 C34 -2.0(7) . . . . ? C32 C33 C34 C29 0.3(7) . . . . ? C30 C29 C34 C33 1.8(7) . . . . ? N5 C29 C34 C33 -178.5(4) . . . . ? C37B O2 C35 C36 92.0(13) . . . . ? C37A O2 C35 C36 65.9(7) . . . . ? Li2 O2 C35 C36 -117.1(5) . . . . ? C37B O2 C37A C38A 52.4(15) . . . . ? C35 O2 C37A C38A 100.1(9) . . . . ? Li2 O2 C37A C38A -76.7(10) . . . . ? C35 O2 C37B C38B -175.8(18) . . . . ? C37A O2 C37B C38B -36.4(12) . . . . ? Li2 O2 C37B C38B 45(3) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.418 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.051 #END data_s099b _database_code_depnum_ccdc_archive 'CCDC 761270' #TrackingRef '- 2 3 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H60 Li2 N10 Si2' _chemical_formula_weight 967.22 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' Li Li -0.0003 0.0001 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.660(4) _cell_length_b 11.667(6) _cell_length_c 12.924(7) _cell_angle_alpha 115.39(4) _cell_angle_beta 97.71(3) _cell_angle_gamma 105.45(4) _cell_volume 1341.5(11) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2434 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 26.89 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9776 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6270 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4570 _reflns_number_gt 3819 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.5324P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4618 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1697 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li Li 0.4070(5) 0.5814(5) 0.4990(4) 0.0386(11) Uani 1 1 d . . . N1 N 0.2632(2) 0.4708(2) 0.3311(2) 0.0322(5) Uani 1 1 d . . . N2 N 0.1187(2) 0.3272(2) 0.3761(2) 0.0333(5) Uani 1 1 d . . . H2A H 0.0355 0.2809 0.3642 0.040 Uiso 1 1 calc R . . N3 N 0.2959(2) 0.5102(2) 0.5985(2) 0.0342(6) Uani 1 1 d . . . N4 N 0.3820(2) 0.3170(2) 0.4567(2) 0.0316(5) Uani 1 1 d . . . N5 N 0.5305(2) 0.2113(2) 0.3987(2) 0.0348(6) Uani 1 1 d . . . Si Si 0.24012(7) 0.33931(8) 0.49135(7) 0.0310(2) Uani 1 1 d . . . C1 C 0.3049(3) 0.5091(3) 0.2476(2) 0.0316(6) Uani 1 1 d . . . C2 C 0.3755(3) 0.6466(3) 0.2876(3) 0.0378(7) Uani 1 1 d . . . H2 H 0.3897 0.7108 0.3664 0.045 Uiso 1 1 calc R . . C3 C 0.4241(3) 0.6873(3) 0.2107(3) 0.0462(8) Uani 1 1 d . . . H3 H 0.4703 0.7792 0.2379 0.055 Uiso 1 1 calc R . . C4 C 0.4052(3) 0.5942(4) 0.0946(3) 0.0500(8) Uani 1 1 d . . . H4 H 0.4381 0.6229 0.0433 0.060 Uiso 1 1 calc R . . C5 C 0.3372(3) 0.4578(4) 0.0541(3) 0.0463(8) Uani 1 1 d . . . H5 H 0.3242 0.3945 -0.0247 0.056 Uiso 1 1 calc R . . C6 C 0.2883(3) 0.4147(3) 0.1301(3) 0.0386(7) Uani 1 1 d . . . H6 H 0.2442 0.3224 0.1027 0.046 Uiso 1 1 calc R . . C7 C 0.1424(3) 0.3833(3) 0.3041(2) 0.0307(6) Uani 1 1 d . . . C8 C 0.0241(3) 0.3404(3) 0.2023(2) 0.0327(6) Uani 1 1 d . . . C9 C 0.0048(3) 0.4334(3) 0.1665(3) 0.0379(7) Uani 1 1 d . . . H9 H 0.0682 0.5216 0.2040 0.045 Uiso 1 1 calc R . . C10 C -0.1074(3) 0.3947(3) 0.0762(3) 0.0479(8) Uani 1 1 d . . . H10 H -0.1193 0.4573 0.0531 0.057 Uiso 1 1 calc R . . C11 C -0.2024(3) 0.2650(4) 0.0194(3) 0.0510(9) Uani 1 1 d . . . H11 H -0.2775 0.2393 -0.0424 0.061 Uiso 1 1 calc R . . C12 C -0.1851(3) 0.1729(3) 0.0553(3) 0.0481(8) Uani 1 1 d . . . H12 H -0.2498 0.0854 0.0184 0.058 Uiso 1 1 calc R . . C13 C -0.0729(3) 0.2099(3) 0.1452(3) 0.0380(7) Uani 1 1 d . . . H13 H -0.0618 0.1468 0.1679 0.046 Uiso 1 1 calc R . . C14 C 0.1403(3) 0.2257(3) 0.5410(3) 0.0472(8) Uani 1 1 d . . . H14A H 0.1015 0.1342 0.4757 0.071 Uiso 1 1 calc R . . H14B H 0.0690 0.2558 0.5668 0.071 Uiso 1 1 calc R . . H14C H 0.1989 0.2285 0.6060 0.071 Uiso 1 1 calc R . . C15 C 0.3924(4) 0.5527(4) 0.7119(3) 0.0531(9) Uani 1 1 d . . . H15A H 0.4396 0.6494 0.7520 0.080 Uiso 1 1 calc R . . H15B H 0.4567 0.5078 0.6964 0.080 Uiso 1 1 calc R . . H15C H 0.3442 0.5285 0.7615 0.080 Uiso 1 1 calc R . . C16 C 0.1935(3) 0.5734(3) 0.6211(3) 0.0470(8) Uani 1 1 d . . . H16A H 0.1308 0.5293 0.6512 0.071 Uiso 1 1 calc R . . H16B H 0.1452 0.5642 0.5480 0.071 Uiso 1 1 calc R . . H16C H 0.2374 0.6682 0.6789 0.071 Uiso 1 1 calc R . . C17 C 0.4033(3) 0.2022(3) 0.3928(2) 0.0311(6) Uani 1 1 d . . . C18 C 0.2847(3) 0.0691(3) 0.3258(2) 0.0340(7) Uani 1 1 d . . . C19 C 0.1779(3) 0.0481(3) 0.2384(3) 0.0437(8) Uani 1 1 d . . . H19 H 0.1827 0.1136 0.2146 0.052 Uiso 1 1 calc R . . C20 C 0.0635(3) -0.0694(4) 0.1856(3) 0.0566(9) Uani 1 1 d . . . H20 H -0.0073 -0.0832 0.1259 0.068 Uiso 1 1 calc R . . C21 C 0.0543(4) -0.1666(4) 0.2218(4) 0.0644(11) Uani 1 1 d . . . H21 H -0.0237 -0.2442 0.1884 0.077 Uiso 1 1 calc R . . C22 C 0.1607(4) -0.1476(4) 0.3070(4) 0.0630(10) Uani 1 1 d . . . H22 H 0.1553 -0.2130 0.3309 0.076 Uiso 1 1 calc R . . C23 C 0.2772(3) -0.0308(3) 0.3583(3) 0.0479(8) Uani 1 1 d . . . H23 H 0.3502 -0.0199 0.4145 0.057 Uiso 1 1 calc R . . C24 C 0.5709(3) 0.1098(3) 0.3208(3) 0.0352(7) Uani 1 1 d . . . C25 C 0.5131(3) 0.0366(3) 0.1970(3) 0.0384(7) Uani 1 1 d . . . H25 H 0.4372 0.0474 0.1634 0.046 Uiso 1 1 calc R . . C26 C 0.5670(3) -0.0515(3) 0.1234(3) 0.0467(8) Uani 1 1 d . . . H26 H 0.5270 -0.0991 0.0412 0.056 Uiso 1 1 calc R . . C27 C 0.6786(4) -0.0694(3) 0.1706(4) 0.0537(9) Uani 1 1 d . . . H27 H 0.7140 -0.1294 0.1208 0.064 Uiso 1 1 calc R . . C28 C 0.7376(3) 0.0017(3) 0.2916(4) 0.0537(9) Uani 1 1 d . . . H28 H 0.8139 -0.0096 0.3238 0.064 Uiso 1 1 calc R . . C29 C 0.6846(3) 0.0908(3) 0.3668(3) 0.0450(8) Uani 1 1 d . . . H29 H 0.7257 0.1382 0.4488 0.054 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 Li 0.032(2) 0.038(3) 0.035(3) 0.014(2) 0.006(2) 0.006(2) N1 0.0278(12) 0.0340(12) 0.0335(12) 0.0172(11) 0.0077(10) 0.0085(10) N2 0.0248(12) 0.0363(13) 0.0399(13) 0.0215(11) 0.0100(10) 0.0073(10) N3 0.0312(12) 0.0388(13) 0.0332(13) 0.0149(11) 0.0101(10) 0.0177(10) N4 0.0265(12) 0.0331(12) 0.0339(12) 0.0149(11) 0.0086(10) 0.0115(10) N5 0.0271(12) 0.0343(12) 0.0342(13) 0.0099(11) 0.0060(10) 0.0113(10) Si 0.0271(4) 0.0353(4) 0.0328(4) 0.0179(4) 0.0104(3) 0.0114(3) C1 0.0217(13) 0.0396(16) 0.0371(15) 0.0215(13) 0.0068(12) 0.0123(12) C2 0.0341(15) 0.0364(16) 0.0426(17) 0.0196(14) 0.0090(13) 0.0124(13) C3 0.0399(17) 0.0458(18) 0.062(2) 0.0339(17) 0.0184(16) 0.0146(14) C4 0.0480(19) 0.067(2) 0.059(2) 0.044(2) 0.0289(17) 0.0271(17) C5 0.0447(18) 0.059(2) 0.0406(18) 0.0244(16) 0.0179(15) 0.0243(16) C6 0.0340(15) 0.0380(16) 0.0393(16) 0.0148(14) 0.0096(13) 0.0135(13) C7 0.0300(15) 0.0295(14) 0.0308(14) 0.0122(12) 0.0091(12) 0.0123(12) C8 0.0284(14) 0.0358(15) 0.0329(15) 0.0150(13) 0.0099(12) 0.0124(12) C9 0.0309(15) 0.0387(16) 0.0436(17) 0.0218(14) 0.0088(13) 0.0096(13) C10 0.0380(17) 0.060(2) 0.054(2) 0.0362(18) 0.0095(15) 0.0171(16) C11 0.0333(17) 0.066(2) 0.0447(19) 0.0269(18) -0.0016(14) 0.0120(16) C12 0.0343(17) 0.0458(18) 0.0466(19) 0.0189(16) 0.0014(15) 0.0000(14) C13 0.0348(16) 0.0366(16) 0.0379(16) 0.0176(14) 0.0065(13) 0.0087(13) C14 0.0450(18) 0.054(2) 0.053(2) 0.0343(17) 0.0215(16) 0.0165(15) C15 0.056(2) 0.058(2) 0.0378(17) 0.0155(16) 0.0070(15) 0.0260(17) C16 0.0445(18) 0.0441(18) 0.055(2) 0.0179(16) 0.0239(16) 0.0251(15) C17 0.0290(14) 0.0356(15) 0.0261(13) 0.0139(12) 0.0061(11) 0.0105(12) C18 0.0293(14) 0.0321(15) 0.0363(15) 0.0111(13) 0.0129(12) 0.0121(12) C19 0.0357(16) 0.0419(17) 0.0435(18) 0.0129(15) 0.0087(14) 0.0143(14) C20 0.0337(17) 0.052(2) 0.058(2) 0.0097(18) 0.0057(16) 0.0103(15) C21 0.039(2) 0.043(2) 0.081(3) 0.012(2) 0.0166(19) 0.0015(16) C22 0.056(2) 0.043(2) 0.085(3) 0.030(2) 0.026(2) 0.0112(17) C23 0.0406(18) 0.0428(18) 0.060(2) 0.0249(17) 0.0147(16) 0.0140(14) C24 0.0304(15) 0.0315(15) 0.0409(16) 0.0165(13) 0.0106(13) 0.0089(12) C25 0.0312(15) 0.0379(16) 0.0392(16) 0.0159(14) 0.0097(13) 0.0075(13) C26 0.0458(19) 0.0370(17) 0.0458(18) 0.0131(15) 0.0220(15) 0.0060(14) C27 0.053(2) 0.0349(17) 0.077(3) 0.0233(18) 0.041(2) 0.0181(15) C28 0.0415(18) 0.052(2) 0.084(3) 0.039(2) 0.0266(19) 0.0267(16) C29 0.0367(17) 0.0485(18) 0.0501(19) 0.0234(16) 0.0084(14) 0.0191(14) _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 Li N5 2.051(5) 2_666 ? Li N1 2.092(5) . ? Li N4 2.109(5) 2_666 ? Li N3 2.131(5) . ? Li C17 2.432(6) 2_666 ? Li Li 3.094(10) 2_666 ? N1 C7 1.302(3) . ? N1 C1 1.413(4) . ? N2 C7 1.362(4) . ? N2 Si 1.765(3) . ? N2 H2A 0.8600 . ? N3 C16 1.466(4) . ? N3 C15 1.468(4) . ? N3 Si 1.740(3) . ? N4 C17 1.339(3) . ? N4 Si 1.687(2) . ? N4 Li 2.109(5) 2_666 ? N5 C17 1.321(3) . ? N5 C24 1.403(4) . ? N5 Li 2.051(5) 2_666 ? Si C14 1.860(3) . ? C1 C6 1.393(4) . ? C1 C2 1.395(4) . ? C2 C3 1.377(4) . ? C2 H2 0.9300 . ? C3 C4 1.370(5) . ? C3 H3 0.9300 . ? C4 C5 1.380(5) . ? C4 H4 0.9300 . ? C5 C6 1.382(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.492(4) . ? C8 C13 1.388(4) . ? C8 C9 1.398(4) . ? C9 C10 1.373(4) . ? C9 H9 0.9300 . ? C10 C11 1.373(5) . ? C10 H10 0.9300 . ? C11 C12 1.383(5) . ? C11 H11 0.9300 . ? C12 C13 1.374(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.505(4) . ? C17 Li 2.432(6) 2_666 ? C18 C19 1.379(4) . ? C18 C23 1.386(4) . ? C19 C20 1.384(5) . ? C19 H19 0.9300 . ? C20 C21 1.387(6) . ? C20 H20 0.9300 . ? C21 C22 1.367(6) . ? C21 H21 0.9300 . ? C22 C23 1.393(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.390(4) . ? C24 C25 1.398(4) . ? C25 C26 1.384(4) . ? C25 H25 0.9300 . ? C26 C27 1.371(5) . ? C26 H26 0.9300 . ? C27 C28 1.369(5) . ? C27 H27 0.9300 . ? C28 C29 1.393(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? 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 N5 Li N1 123.1(3) 2_666 . ? N5 Li N4 66.18(17) 2_666 2_666 ? N1 Li N4 128.9(3) . 2_666 ? N5 Li N3 102.6(2) 2_666 . ? N1 Li N3 100.2(2) . . ? N4 Li N3 128.3(3) 2_666 . ? N5 Li C17 32.90(11) 2_666 2_666 ? N1 Li C17 136.1(3) . 2_666 ? N4 Li C17 33.35(11) 2_666 2_666 ? N3 Li C17 118.5(2) . 2_666 ? N5 Li Li 123.3(3) 2_666 2_666 ? N1 Li Li 107.1(3) . 2_666 ? N4 Li Li 62.32(17) 2_666 2_666 ? N3 Li Li 91.6(2) . 2_666 ? C17 Li Li 92.5(2) 2_666 2_666 ? C7 N1 C1 121.1(2) . . ? C7 N1 Li 125.9(2) . . ? C1 N1 Li 112.8(2) . . ? C7 N2 Si 127.16(19) . . ? C7 N2 H2A 116.4 . . ? Si N2 H2A 116.4 . . ? C16 N3 C15 110.1(2) . . ? C16 N3 Si 117.6(2) . . ? C15 N3 Si 116.7(2) . . ? C16 N3 Li 108.3(2) . . ? C15 N3 Li 107.5(2) . . ? Si N3 Li 94.78(17) . . ? C17 N4 Si 129.89(19) . . ? C17 N4 Li 86.7(2) . 2_666 ? Si N4 Li 142.62(19) . 2_666 ? C17 N5 C24 124.9(2) . . ? C17 N5 Li 89.6(2) . 2_666 ? C24 N5 Li 141.4(2) . 2_666 ? N4 Si N3 103.99(12) . . ? N4 Si N2 114.90(12) . . ? N3 Si N2 102.90(12) . . ? N4 Si C14 117.91(14) . . ? N3 Si C14 112.30(14) . . ? N2 Si C14 104.03(14) . . ? C6 C1 C2 118.7(3) . . ? C6 C1 N1 122.7(3) . . ? C2 C1 N1 118.3(3) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? N1 C7 N2 118.0(2) . . ? N1 C7 C8 126.0(2) . . ? N2 C7 C8 116.0(2) . . ? C13 C8 C9 118.5(3) . . ? C13 C8 C7 120.9(3) . . ? C9 C8 C7 120.5(2) . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 121.0(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C12 119.2(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 120.7(3) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? Si C14 H14A 109.5 . . ? Si C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 N4 117.2(2) . . ? N5 C17 C18 123.2(2) . . ? N4 C17 C18 119.4(2) . . ? N5 C17 Li 57.47(18) . 2_666 ? N4 C17 Li 59.94(18) . 2_666 ? C18 C17 Li 179.3(2) . 2_666 ? C19 C18 C23 118.9(3) . . ? C19 C18 C17 121.3(3) . . ? C23 C18 C17 119.6(3) . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 119.5(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 120.2(3) . . ? C18 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C29 C24 C25 117.4(3) . . ? C29 C24 N5 118.5(3) . . ? C25 C24 N5 123.7(3) . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C27 C26 C25 120.6(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 119.4(3) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 120.6(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C24 C29 C28 120.8(3) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? 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 N5 Li N1 C7 -113.5(3) 2_666 . . . ? N4 Li N1 C7 161.8(3) 2_666 . . . ? N3 Li N1 C7 -1.0(3) . . . . ? C17 Li N1 C7 -153.4(3) 2_666 . . . ? Li Li N1 C7 93.9(3) 2_666 . . . ? N5 Li N1 C1 61.1(3) 2_666 . . . ? N4 Li N1 C1 -23.6(4) 2_666 . . . ? N3 Li N1 C1 173.6(2) . . . . ? C17 Li N1 C1 21.2(4) 2_666 . . . ? Li Li N1 C1 -91.5(3) 2_666 . . . ? N5 Li N3 C16 53.2(3) 2_666 . . . ? N1 Li N3 C16 -74.3(3) . . . . ? N4 Li N3 C16 122.7(3) 2_666 . . . ? C17 Li N3 C16 84.2(3) 2_666 . . . ? Li Li N3 C16 177.9(2) 2_666 . . . ? N5 Li N3 C15 -65.7(3) 2_666 . . . ? N1 Li N3 C15 166.8(2) . . . . ? N4 Li N3 C15 3.8(4) 2_666 . . . ? C17 Li N3 C15 -34.7(3) 2_666 . . . ? Li Li N3 C15 59.0(3) 2_666 . . . ? N5 Li N3 Si 174.36(18) 2_666 . . . ? N1 Li N3 Si 46.8(2) . . . . ? N4 Li N3 Si -116.2(3) 2_666 . . . ? C17 Li N3 Si -154.7(2) 2_666 . . . ? Li Li N3 Si -60.9(2) 2_666 . . . ? C17 N4 Si N3 169.0(2) . . . . ? Li N4 Si N3 2.9(3) 2_666 . . . ? C17 N4 Si N2 -79.3(3) . . . . ? Li N4 Si N2 114.6(3) 2_666 . . . ? C17 N4 Si C14 43.9(3) . . . . ? Li N4 Si C14 -122.2(3) 2_666 . . . ? C16 N3 Si N4 161.7(2) . . . . ? C15 N3 Si N4 -64.2(2) . . . . ? Li N3 Si N4 48.15(18) . . . . ? C16 N3 Si N2 41.5(2) . . . . ? C15 N3 Si N2 175.7(2) . . . . ? Li N3 Si N2 -72.00(17) . . . . ? C16 N3 Si C14 -69.8(3) . . . . ? C15 N3 Si C14 64.4(2) . . . . ? Li N3 Si C14 176.74(18) . . . . ? C7 N2 Si N4 -44.1(3) . . . . ? C7 N2 Si N3 68.2(2) . . . . ? C7 N2 Si C14 -174.5(2) . . . . ? C7 N1 C1 C6 -48.7(4) . . . . ? Li N1 C1 C6 136.5(3) . . . . ? C7 N1 C1 C2 136.7(3) . . . . ? Li N1 C1 C2 -38.2(3) . . . . ? C6 C1 C2 C3 1.8(4) . . . . ? N1 C1 C2 C3 176.6(3) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C4 C5 C6 C1 1.3(4) . . . . ? C2 C1 C6 C5 -2.1(4) . . . . ? N1 C1 C6 C5 -176.7(3) . . . . ? C1 N1 C7 N2 165.2(2) . . . . ? Li N1 C7 N2 -20.6(4) . . . . ? C1 N1 C7 C8 -16.7(4) . . . . ? Li N1 C7 C8 157.4(3) . . . . ? Si N2 C7 N1 -10.4(4) . . . . ? Si N2 C7 C8 171.36(18) . . . . ? N1 C7 C8 C13 148.4(3) . . . . ? N2 C7 C8 C13 -33.5(4) . . . . ? N1 C7 C8 C9 -35.0(4) . . . . ? N2 C7 C8 C9 143.1(3) . . . . ? C13 C8 C9 C10 -0.5(4) . . . . ? C7 C8 C9 C10 -177.2(3) . . . . ? C8 C9 C10 C11 0.0(5) . . . . ? C9 C10 C11 C12 0.9(5) . . . . ? C10 C11 C12 C13 -1.2(5) . . . . ? C11 C12 C13 C8 0.7(5) . . . . ? C9 C8 C13 C12 0.1(4) . . . . ? C7 C8 C13 C12 176.8(3) . . . . ? C24 N5 C17 N4 -166.3(3) . . . . ? Li N5 C17 N4 -4.8(3) 2_666 . . . ? C24 N5 C17 C18 18.1(4) . . . . ? Li N5 C17 C18 179.7(3) 2_666 . . . ? C24 N5 C17 Li -161.5(3) . . . 2_666 ? Si N4 C17 N5 -167.0(2) . . . . ? Li N4 C17 N5 4.7(3) 2_666 . . . ? Si N4 C17 C18 8.8(4) . . . . ? Li N4 C17 C18 -179.6(3) 2_666 . . . ? Si N4 C17 Li -171.6(3) . . . 2_666 ? N5 C17 C18 C19 -124.7(3) . . . . ? N4 C17 C18 C19 59.9(4) . . . . ? Li C17 C18 C19 32(19) 2_666 . . . ? N5 C17 C18 C23 60.3(4) . . . . ? N4 C17 C18 C23 -115.1(3) . . . . ? Li C17 C18 C23 -143(19) 2_666 . . . ? C23 C18 C19 C20 1.4(4) . . . . ? C17 C18 C19 C20 -173.6(3) . . . . ? C18 C19 C20 C21 1.1(5) . . . . ? C19 C20 C21 C22 -2.1(5) . . . . ? C20 C21 C22 C23 0.7(6) . . . . ? C19 C18 C23 C22 -2.9(5) . . . . ? C17 C18 C23 C22 172.2(3) . . . . ? C21 C22 C23 C18 1.9(5) . . . . ? C17 N5 C24 C29 -143.8(3) . . . . ? Li N5 C24 C29 66.7(5) 2_666 . . . ? C17 N5 C24 C25 43.8(4) . . . . ? Li N5 C24 C25 -105.7(4) 2_666 . . . ? C29 C24 C25 C26 0.3(4) . . . . ? N5 C24 C25 C26 172.8(3) . . . . ? C24 C25 C26 C27 0.1(4) . . . . ? C25 C26 C27 C28 -0.5(5) . . . . ? C26 C27 C28 C29 0.5(5) . . . . ? C25 C24 C29 C28 -0.3(4) . . . . ? N5 C24 C29 C28 -173.1(3) . . . . ? C27 C28 C29 C24 -0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.451 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.057 #END data_hs0303p _database_code_depnum_ccdc_archive 'CCDC 761271' #TrackingRef '- 2 3 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H46 Cl3 N5 O2 Si Zr' _chemical_formula_weight 818.45 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7016(17) _cell_length_b 20.676(2) _cell_length_c 26.029(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.506(2) _cell_angle_gamma 90.00 _cell_volume 7911.6(16) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6050 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 22.79 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8102 _exptl_absorpt_correction_T_max 0.8981 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32332 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13925 _reflns_number_gt 10269 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+1.9467P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13925 _refine_ls_number_parameters 887 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1438 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.31535(3) 0.84400(3) 0.07973(2) 0.02688(15) Uani 1 1 d . . . Cl1 Cl 0.36177(10) 0.79544(9) -0.00181(6) 0.0471(4) Uani 1 1 d . . . Cl2 Cl 0.28742(11) 0.94909(8) 0.03109(7) 0.0521(5) Uani 1 1 d . . . Cl3 Cl 0.27098(10) 0.89117(8) 0.16237(6) 0.0396(4) Uani 1 1 d . . . O1 O 0.4483(2) 0.90059(18) 0.08927(14) 0.0323(9) Uani 1 1 d . . . N1 N 0.1652(3) 0.8430(2) 0.05733(17) 0.0305(11) Uani 1 1 d . . . H1 H 0.1565 0.8538 0.0254 0.037 Uiso 1 1 calc R . . N2 N 0.0869(3) 0.7841(2) 0.11773(17) 0.0283(11) Uani 1 1 d . . . N3 N 0.1490(3) 0.6777(2) 0.17342(18) 0.0355(12) Uani 1 1 d . . . N4 N 0.2670(3) 0.7489(2) 0.10854(17) 0.0280(11) Uani 1 1 d . . . N5 N 0.4118(3) 0.7739(2) 0.11661(17) 0.0304(11) Uani 1 1 d . . . Si1 Si 0.16152(10) 0.71525(8) 0.11678(6) 0.0300(4) Uani 1 1 d . . . C1 C 0.0894(4) 0.8302(3) 0.0805(2) 0.0287(13) Uani 1 1 d . . . C2 C 0.0044(4) 0.8647(3) 0.06575(19) 0.0273(13) Uani 1 1 d . . . C3 C 0.0056(4) 0.9312(3) 0.0597(2) 0.0436(17) Uani 1 1 d . . . H3 H 0.0599 0.9543 0.0651 0.052 Uiso 1 1 calc R . . C4 C -0.0734(5) 0.9640(4) 0.0456(3) 0.058(2) Uani 1 1 d . . . H4 H -0.0730 1.0092 0.0418 0.070 Uiso 1 1 calc R . . C5 C -0.1533(5) 0.9291(4) 0.0372(3) 0.066(2) Uani 1 1 d . . . H5 H -0.2071 0.9508 0.0279 0.079 Uiso 1 1 calc R . . C6 C -0.1534(4) 0.8632(4) 0.0425(2) 0.058(2) Uani 1 1 d . . . H6 H -0.2074 0.8400 0.0366 0.070 Uiso 1 1 calc R . . C7 C -0.0760(4) 0.8311(3) 0.0564(2) 0.0388(16) Uani 1 1 d . . . H7 H -0.0770 0.7858 0.0596 0.047 Uiso 1 1 calc R . . C8 C 0.0171(3) 0.7888(3) 0.1569(2) 0.0299(14) Uani 1 1 d . . . C9 C 0.0130(4) 0.8436(3) 0.1867(2) 0.0379(15) Uani 1 1 d . . . H9 H 0.0554 0.8770 0.1821 0.045 Uiso 1 1 calc R . . C10 C -0.0536(4) 0.8492(3) 0.2235(2) 0.0452(17) Uani 1 1 d . . . H10 H -0.0575 0.8869 0.2435 0.054 Uiso 1 1 calc R . . C11 C -0.1137(4) 0.7998(4) 0.2309(2) 0.0477(18) Uani 1 1 d . . . H11 H -0.1585 0.8036 0.2563 0.057 Uiso 1 1 calc R . . C12 C -0.1097(4) 0.7448(3) 0.2018(2) 0.0447(17) Uani 1 1 d . . . H12 H -0.1506 0.7107 0.2077 0.054 Uiso 1 1 calc R . . C13 C -0.0454(4) 0.7397(3) 0.1637(2) 0.0336(14) Uani 1 1 d . . . H13 H -0.0441 0.7029 0.1425 0.040 Uiso 1 1 calc R . . C14 C 0.1241(4) 0.6664(3) 0.0609(2) 0.0395(16) Uani 1 1 d . . . H14A H 0.1552 0.6251 0.0615 0.059 Uiso 1 1 calc R . . H14B H 0.1385 0.6892 0.0295 0.059 Uiso 1 1 calc R . . H14C H 0.0590 0.6594 0.0626 0.059 Uiso 1 1 calc R . . C15 C 0.1734(4) 0.7099(3) 0.2216(2) 0.0481(18) Uani 1 1 d . . . H15A H 0.1203 0.7124 0.2434 0.072 Uiso 1 1 calc R . . H15B H 0.1952 0.7533 0.2144 0.072 Uiso 1 1 calc R . . H15C H 0.2208 0.6855 0.2390 0.072 Uiso 1 1 calc R . . C16 C 0.1129(5) 0.6129(3) 0.1800(3) 0.058(2) Uani 1 1 d . . . H16A H 0.1577 0.5862 0.1975 0.086 Uiso 1 1 calc R . . H16B H 0.0990 0.5944 0.1466 0.086 Uiso 1 1 calc R . . H16C H 0.0579 0.6148 0.2003 0.086 Uiso 1 1 calc R . . C17 C 0.3504(4) 0.7288(3) 0.1239(2) 0.0281(13) Uani 1 1 d . . . C18 C 0.3676(3) 0.6651(3) 0.1485(2) 0.0301(14) Uani 1 1 d . . . C19 C 0.3307(4) 0.6084(3) 0.1300(2) 0.0362(15) Uani 1 1 d . . . H19 H 0.2987 0.6089 0.0985 0.043 Uiso 1 1 calc R . . C20 C 0.3396(4) 0.5513(3) 0.1562(3) 0.0463(17) Uani 1 1 d . . . H20 H 0.3136 0.5133 0.1429 0.056 Uiso 1 1 calc R . . C21 C 0.3863(5) 0.5496(3) 0.2021(3) 0.0546(19) Uani 1 1 d . . . H21 H 0.3907 0.5108 0.2207 0.066 Uiso 1 1 calc R . . C22 C 0.4269(5) 0.6051(4) 0.2208(3) 0.0536(19) Uani 1 1 d . . . H22 H 0.4610 0.6037 0.2515 0.064 Uiso 1 1 calc R . . C23 C 0.4176(4) 0.6625(3) 0.1946(2) 0.0412(16) Uani 1 1 d . . . H23 H 0.4450 0.7002 0.2077 0.049 Uiso 1 1 calc R . . C24 C 0.5077(4) 0.7607(3) 0.1169(2) 0.0316(14) Uani 1 1 d . . . C25 C 0.5661(4) 0.7944(3) 0.1487(2) 0.0412(16) Uani 1 1 d . . . H25 H 0.5428 0.8246 0.1722 0.049 Uiso 1 1 calc R . . C26 C 0.6586(4) 0.7840(4) 0.1462(3) 0.0523(19) Uani 1 1 d . . . H26 H 0.6980 0.8071 0.1681 0.063 Uiso 1 1 calc R . . C27 C 0.6939(4) 0.7403(4) 0.1122(3) 0.056(2) Uani 1 1 d . . . H27 H 0.7570 0.7336 0.1108 0.067 Uiso 1 1 calc R . . C28 C 0.6364(4) 0.7062(4) 0.0802(3) 0.0521(19) Uani 1 1 d . . . H28 H 0.6603 0.6764 0.0566 0.062 Uiso 1 1 calc R . . C29 C 0.5424(4) 0.7159(3) 0.0827(2) 0.0416(16) Uani 1 1 d . . . H29 H 0.5029 0.6921 0.0613 0.050 Uiso 1 1 calc R . . C30 C 0.4579(4) 0.9606(3) 0.1186(3) 0.0471(17) Uani 1 1 d . . . H30A H 0.4798 0.9516 0.1536 0.057 Uiso 1 1 calc R . . H30B H 0.3997 0.9834 0.1205 0.057 Uiso 1 1 calc R . . C31 C 0.5258(5) 0.9995(4) 0.0898(3) 0.066(2) Uani 1 1 d . . . H31A H 0.5614 1.0270 0.1131 0.080 Uiso 1 1 calc R . . H31B H 0.4958 1.0269 0.0640 0.080 Uiso 1 1 calc R . . C32 C 0.5853(4) 0.9494(4) 0.0647(3) 0.060(2) Uani 1 1 d . . . H32A H 0.6169 0.9672 0.0349 0.072 Uiso 1 1 calc R . . H32B H 0.6301 0.9317 0.0890 0.072 Uiso 1 1 calc R . . C33 C 0.5166(4) 0.8996(3) 0.0491(2) 0.0430(16) Uani 1 1 d . . . H33A H 0.4892 0.9106 0.0157 0.052 Uiso 1 1 calc R . . H33B H 0.5449 0.8568 0.0467 0.052 Uiso 1 1 calc R . . C34 C 0.5968(4) 0.8571(3) 0.4205(2) 0.0343(15) Uani 1 1 d . . . C35 C 0.5148(4) 0.8962(3) 0.4316(2) 0.0337(15) Uani 1 1 d . . . C36 C 0.5191(4) 0.9627(3) 0.4302(2) 0.0470(17) Uani 1 1 d . . . H36 H 0.5745 0.9829 0.4222 0.056 Uiso 1 1 calc R . . C37 C 0.4427(5) 1.0008(4) 0.4403(3) 0.066(2) Uani 1 1 d . . . H37 H 0.4452 1.0461 0.4375 0.079 Uiso 1 1 calc R . . Zr2 Zr 0.82293(4) 0.86518(3) 0.41992(2) 0.02917(16) Uani 1 1 d . . . Cl4 Cl 0.78142(10) 0.89466(8) 0.33121(6) 0.0391(4) Uani 1 1 d . . . Cl5 Cl 0.79931(10) 0.98248(7) 0.44738(6) 0.0417(4) Uani 1 1 d . . . Cl6 Cl 0.86289(10) 0.83540(9) 0.50825(6) 0.0475(4) Uani 1 1 d . . . O2 O 0.9608(2) 0.91311(19) 0.40888(14) 0.0349(10) Uani 1 1 d . . . N6 N 0.6740(3) 0.8717(2) 0.44223(18) 0.0383(13) Uani 1 1 d . . . H6A H 0.6670 0.8880 0.4728 0.046 Uiso 1 1 calc R . . N7 N 0.5895(3) 0.8045(2) 0.38894(18) 0.0327(12) Uani 1 1 d . . . N8 N 0.6476(3) 0.6899(3) 0.3440(2) 0.0451(14) Uani 1 1 d . . . N9 N 0.7693(3) 0.7670(2) 0.40213(18) 0.0325(12) Uani 1 1 d . . . N10 N 0.9146(3) 0.7870(2) 0.39156(18) 0.0337(12) Uani 1 1 d . . . Si2 Si 0.66180(11) 0.73457(9) 0.39625(7) 0.0399(5) Uani 1 1 d . . . C38 C 0.3646(5) 0.9704(5) 0.4545(3) 0.071(3) Uani 1 1 d . . . H38 H 0.3130 0.9955 0.4619 0.085 Uiso 1 1 calc R . . C39 C 0.3585(5) 0.9051(5) 0.4582(3) 0.066(2) Uani 1 1 d . . . H39 H 0.3037 0.8859 0.4685 0.079 Uiso 1 1 calc R . . C40 C 0.4330(4) 0.8664(4) 0.4469(2) 0.0507(18) Uani 1 1 d . . . H40 H 0.4290 0.8211 0.4493 0.061 Uiso 1 1 calc R . . C41 C 0.5191(4) 0.8054(3) 0.3491(2) 0.0322(14) Uani 1 1 d . . . C42 C 0.5191(4) 0.8540(3) 0.3131(2) 0.0397(16) Uani 1 1 d . . . H42 H 0.5644 0.8860 0.3144 0.048 Uiso 1 1 calc R . . C43 C 0.4532(5) 0.8562(3) 0.2751(2) 0.0495(18) Uani 1 1 d . . . H43 H 0.4513 0.8906 0.2515 0.059 Uiso 1 1 calc R . . C44 C 0.3900(5) 0.8068(4) 0.2725(3) 0.057(2) Uani 1 1 d . . . H44 H 0.3463 0.8068 0.2459 0.068 Uiso 1 1 calc R . . C45 C 0.3899(4) 0.7581(3) 0.3080(3) 0.0468(18) Uani 1 1 d . . . H45 H 0.3455 0.7255 0.3061 0.056 Uiso 1 1 calc R . . C46 C 0.4550(4) 0.7567(3) 0.3468(2) 0.0396(16) Uani 1 1 d . . . H46 H 0.4556 0.7231 0.3711 0.047 Uiso 1 1 calc R . . C47 C 0.6227(4) 0.6915(3) 0.4550(2) 0.0530(19) Uani 1 1 d . . . H47A H 0.5586 0.6814 0.4515 0.079 Uiso 1 1 calc R . . H47B H 0.6322 0.7190 0.4848 0.079 Uiso 1 1 calc R . . H47C H 0.6572 0.6518 0.4593 0.079 Uiso 1 1 calc R . . C48 C 0.6716(5) 0.7165(4) 0.2925(2) 0.058(2) Uani 1 1 d . . . H48A H 0.7172 0.6892 0.2768 0.087 Uiso 1 1 calc R . . H48B H 0.6955 0.7600 0.2965 0.087 Uiso 1 1 calc R . . H48C H 0.6177 0.7177 0.2708 0.087 Uiso 1 1 calc R . . C49 C 0.6108(5) 0.6230(4) 0.3434(3) 0.076(3) Uani 1 1 d . . . H49A H 0.5556 0.6218 0.3227 0.115 Uiso 1 1 calc R . . H49B H 0.5973 0.6097 0.3782 0.115 Uiso 1 1 calc R . . H49C H 0.6555 0.5939 0.3288 0.115 Uiso 1 1 calc R . . C50 C 0.8500(4) 0.7426(3) 0.3889(2) 0.0343(15) Uani 1 1 d . . . C51 C 0.8647(4) 0.6750(3) 0.3713(2) 0.0325(14) Uani 1 1 d . . . C52 C 0.8304(4) 0.6227(3) 0.3980(3) 0.0493(18) Uani 1 1 d . . . H52 H 0.8005 0.6298 0.4293 0.059 Uiso 1 1 calc R . . C53 C 0.8389(5) 0.5615(4) 0.3801(3) 0.070(2) Uani 1 1 d . . . H53 H 0.8149 0.5269 0.3991 0.084 Uiso 1 1 calc R . . C54 C 0.8808(6) 0.5495(4) 0.3357(4) 0.078(3) Uani 1 1 d . . . H54 H 0.8851 0.5070 0.3231 0.093 Uiso 1 1 calc R . . C55 C 0.9185(5) 0.6011(4) 0.3082(3) 0.067(2) Uani 1 1 d . . . H55 H 0.9497 0.5932 0.2775 0.080 Uiso 1 1 calc R . . C56 C 0.9098(4) 0.6630(3) 0.3260(2) 0.0464(17) Uani 1 1 d . . . H56 H 0.9346 0.6976 0.3074 0.056 Uiso 1 1 calc R . . C57 C 1.0106(4) 0.7728(3) 0.3908(2) 0.0334(14) Uani 1 1 d . . . C58 C 1.0623(4) 0.8009(3) 0.3528(2) 0.0413(16) Uani 1 1 d . . . H58 H 1.0345 0.8251 0.3264 0.050 Uiso 1 1 calc R . . C59 C 1.1561(4) 0.7929(3) 0.3542(3) 0.0486(18) Uani 1 1 d . . . H59 H 1.1921 0.8124 0.3289 0.058 Uiso 1 1 calc R . . C60 C 1.1966(4) 0.7568(4) 0.3921(3) 0.058(2) Uani 1 1 d . . . H60 H 1.2602 0.7520 0.3932 0.069 Uiso 1 1 calc R . . C61 C 1.1434(4) 0.7276(4) 0.4285(3) 0.056(2) Uani 1 1 d . . . H61 H 1.1707 0.7019 0.4541 0.067 Uiso 1 1 calc R . . C62 C 1.0504(4) 0.7356(3) 0.4276(2) 0.0440(17) Uani 1 1 d . . . H62 H 1.0144 0.7153 0.4526 0.053 Uiso 1 1 calc R . . C63 C 1.0300(4) 0.9176(3) 0.4491(2) 0.0429(17) Uani 1 1 d . . . H63A H 1.0567 0.8750 0.4560 0.051 Uiso 1 1 calc R . . H63B H 1.0039 0.9344 0.4809 0.051 Uiso 1 1 calc R . . C64 C 1.1005(4) 0.9630(4) 0.4287(3) 0.056(2) Uani 1 1 d . . . H64A H 1.1439 0.9406 0.4066 0.067 Uiso 1 1 calc R . . H64B H 1.1336 0.9848 0.4566 0.067 Uiso 1 1 calc R . . C65 C 1.0420(4) 1.0102(3) 0.3983(3) 0.058(2) Uani 1 1 d . . . H65A H 1.0783 1.0351 0.3738 0.070 Uiso 1 1 calc R . . H65B H 1.0095 1.0400 0.4209 0.070 Uiso 1 1 calc R . . C66 C 0.9771(4) 0.9639(3) 0.3710(3) 0.0453(17) Uani 1 1 d . . . H66A H 0.9203 0.9858 0.3615 0.054 Uiso 1 1 calc R . . H66B H 1.0049 0.9461 0.3400 0.054 Uiso 1 1 calc R . . O3 O 0.3007(6) 0.5211(6) 0.3275(3) 0.158(4) Uani 1 1 d . . . C67 C 0.2616(10) 0.5741(7) 0.3531(7) 0.179(8) Uani 1 1 d D . . H67A H 0.2733 0.5708 0.3902 0.214 Uiso 1 1 calc R . . H67B H 0.2884 0.6146 0.3408 0.214 Uiso 1 1 calc R . . C68 C 0.1612(8) 0.5739(6) 0.3427(5) 0.138(5) Uani 1 1 d D . . H68A H 0.1434 0.6105 0.3210 0.166 Uiso 1 1 calc R . . H68B H 0.1269 0.5758 0.3748 0.166 Uiso 1 1 calc R . . C69 C 0.1454(9) 0.5116(6) 0.3158(4) 0.123(4) Uani 1 1 d . . . H69A H 0.1001 0.4858 0.3341 0.147 Uiso 1 1 calc R . . H69B H 0.1230 0.5194 0.2807 0.147 Uiso 1 1 calc R . . C70 C 0.2321(10) 0.4778(7) 0.3147(5) 0.138(5) Uani 1 1 d . . . H70A H 0.2317 0.4418 0.3392 0.166 Uiso 1 1 calc R . . H70B H 0.2425 0.4601 0.2803 0.166 Uiso 1 1 calc R . . O4 O 0.2310(10) 0.0732(7) 0.3233(7) 0.295(9) Uani 1 1 d . . . C71 C 0.3308(11) 0.0754(6) 0.3174(5) 0.147(5) Uani 1 1 d . . . H71A H 0.3489 0.1110 0.2949 0.176 Uiso 1 1 calc R . . H71B H 0.3614 0.0804 0.3508 0.176 Uiso 1 1 calc R . . C72 C 0.3519(9) 0.0136(7) 0.2946(5) 0.143(5) Uani 1 1 d . . . H72A H 0.4051 -0.0053 0.3118 0.171 Uiso 1 1 calc R . . H72B H 0.3663 0.0194 0.2582 0.171 Uiso 1 1 calc R . . C73 C 0.2746(10) -0.0295(6) 0.2996(5) 0.151(5) Uani 1 1 d D . . H73A H 0.2675 -0.0576 0.2695 0.181 Uiso 1 1 calc R . . H73B H 0.2790 -0.0560 0.3307 0.181 Uiso 1 1 calc R . . C74 C 0.2007(7) 0.0182(7) 0.3028(4) 0.119(4) Uani 1 1 d D . . H74A H 0.1760 0.0266 0.2684 0.143 Uiso 1 1 calc R . . H74B H 0.1516 0.0007 0.3240 0.143 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 Zr1 0.0230(3) 0.0277(3) 0.0300(3) 0.0028(2) 0.0034(2) 0.0039(2) Cl1 0.0322(9) 0.0708(13) 0.0383(10) -0.0145(8) 0.0014(7) 0.0032(8) Cl2 0.0412(10) 0.0490(11) 0.0664(12) 0.0293(9) 0.0096(8) 0.0067(8) Cl3 0.0424(9) 0.0408(10) 0.0357(9) -0.0013(7) 0.0086(7) 0.0036(7) O1 0.030(2) 0.030(2) 0.036(2) 0.0014(18) 0.0076(18) -0.0021(18) N1 0.027(3) 0.041(3) 0.023(3) 0.006(2) -0.001(2) 0.004(2) N2 0.023(3) 0.032(3) 0.030(3) 0.007(2) 0.002(2) 0.004(2) N3 0.036(3) 0.036(3) 0.035(3) 0.003(2) 0.000(2) 0.000(2) N4 0.023(2) 0.023(3) 0.038(3) 0.004(2) 0.002(2) 0.007(2) N5 0.021(3) 0.029(3) 0.040(3) -0.001(2) -0.006(2) 0.004(2) Si1 0.0252(9) 0.0283(10) 0.0366(10) 0.0023(7) -0.0005(7) 0.0022(7) C1 0.029(3) 0.031(4) 0.025(3) -0.002(3) -0.001(3) 0.002(3) C2 0.025(3) 0.035(4) 0.021(3) 0.003(3) -0.003(2) -0.002(3) C3 0.039(4) 0.044(4) 0.047(4) 0.010(3) 0.009(3) 0.004(3) C4 0.062(5) 0.052(5) 0.061(5) 0.031(4) 0.017(4) 0.026(4) C5 0.038(4) 0.101(7) 0.057(5) 0.036(5) 0.005(4) 0.029(5) C6 0.032(4) 0.100(7) 0.043(4) 0.029(4) -0.011(3) 0.007(4) C7 0.040(4) 0.045(4) 0.032(4) 0.008(3) -0.002(3) -0.005(3) C8 0.019(3) 0.039(4) 0.032(4) 0.006(3) -0.004(2) 0.010(3) C9 0.035(4) 0.036(4) 0.042(4) 0.004(3) 0.004(3) 0.004(3) C10 0.051(4) 0.046(4) 0.039(4) -0.008(3) 0.001(3) 0.012(4) C11 0.042(4) 0.072(6) 0.029(4) 0.010(4) 0.010(3) 0.013(4) C12 0.034(4) 0.055(5) 0.045(4) 0.010(3) 0.006(3) -0.006(3) C13 0.029(3) 0.043(4) 0.029(4) -0.001(3) -0.003(3) 0.001(3) C14 0.037(4) 0.043(4) 0.038(4) -0.004(3) -0.008(3) 0.000(3) C15 0.049(4) 0.056(5) 0.039(4) 0.006(3) -0.003(3) -0.002(3) C16 0.060(5) 0.041(5) 0.071(5) 0.014(4) 0.003(4) -0.012(4) C17 0.026(3) 0.024(3) 0.034(4) -0.005(3) 0.004(3) -0.001(3) C18 0.022(3) 0.033(4) 0.035(4) 0.000(3) 0.001(3) 0.001(3) C19 0.033(3) 0.029(4) 0.046(4) 0.000(3) -0.006(3) 0.004(3) C20 0.046(4) 0.028(4) 0.065(5) 0.000(3) 0.010(4) 0.007(3) C21 0.060(5) 0.039(5) 0.065(5) 0.015(4) 0.000(4) 0.010(4) C22 0.064(5) 0.055(5) 0.042(4) 0.008(4) -0.013(3) 0.007(4) C23 0.044(4) 0.037(4) 0.042(4) -0.004(3) -0.007(3) 0.002(3) C24 0.026(3) 0.034(4) 0.035(4) 0.004(3) -0.003(3) 0.006(3) C25 0.029(3) 0.048(4) 0.046(4) -0.003(3) -0.007(3) -0.004(3) C26 0.034(4) 0.061(5) 0.062(5) 0.008(4) -0.015(3) -0.005(4) C27 0.019(3) 0.083(6) 0.066(5) 0.021(4) 0.001(3) 0.009(4) C28 0.044(4) 0.070(5) 0.042(4) 0.003(4) 0.005(3) 0.017(4) C29 0.031(4) 0.048(4) 0.045(4) 0.003(3) 0.001(3) 0.008(3) C30 0.047(4) 0.037(4) 0.058(5) -0.004(3) 0.002(3) -0.014(3) C31 0.062(5) 0.043(5) 0.094(6) 0.002(4) 0.011(4) -0.016(4) C32 0.035(4) 0.066(6) 0.078(6) 0.021(4) 0.008(4) -0.014(4) C33 0.038(4) 0.051(4) 0.041(4) 0.007(3) 0.013(3) -0.003(3) C34 0.023(3) 0.045(4) 0.035(4) 0.004(3) 0.003(3) -0.002(3) C35 0.021(3) 0.052(4) 0.028(3) -0.004(3) -0.001(2) 0.008(3) C36 0.043(4) 0.054(5) 0.044(4) -0.010(3) 0.001(3) 0.013(3) C37 0.056(5) 0.080(6) 0.061(5) -0.025(4) -0.012(4) 0.026(5) Zr2 0.0204(3) 0.0311(3) 0.0360(4) -0.0045(3) -0.0037(2) 0.0021(2) Cl4 0.0405(9) 0.0419(10) 0.0350(9) -0.0070(7) -0.0047(7) 0.0063(7) Cl5 0.0380(9) 0.0374(9) 0.0495(10) -0.0143(7) -0.0031(7) 0.0019(7) Cl6 0.0373(9) 0.0618(12) 0.0433(10) 0.0098(8) -0.0049(7) -0.0012(8) O2 0.027(2) 0.038(3) 0.040(3) -0.005(2) -0.0087(18) 0.0041(18) N6 0.024(3) 0.055(4) 0.036(3) -0.017(3) -0.003(2) 0.004(2) N7 0.020(3) 0.036(3) 0.043(3) -0.004(2) -0.005(2) -0.003(2) N8 0.037(3) 0.043(4) 0.055(4) 0.001(3) -0.005(3) -0.001(3) N9 0.024(3) 0.029(3) 0.044(3) -0.004(2) 0.000(2) 0.001(2) N10 0.020(3) 0.032(3) 0.049(3) -0.004(2) 0.002(2) 0.006(2) Si2 0.0276(9) 0.0411(11) 0.0510(12) 0.0006(9) -0.0042(8) -0.0028(8) C38 0.036(5) 0.117(8) 0.060(5) -0.047(5) -0.006(4) 0.025(5) C39 0.027(4) 0.113(8) 0.058(5) -0.023(5) 0.008(3) -0.003(5) C40 0.038(4) 0.074(5) 0.040(4) -0.005(4) 0.003(3) -0.006(4) C41 0.021(3) 0.044(4) 0.031(4) -0.010(3) 0.002(3) 0.007(3) C42 0.040(4) 0.038(4) 0.041(4) -0.009(3) 0.011(3) 0.003(3) C43 0.056(5) 0.055(5) 0.038(4) -0.002(3) -0.006(3) 0.012(4) C44 0.048(5) 0.086(6) 0.035(4) -0.017(4) -0.013(3) 0.019(4) C45 0.032(4) 0.059(5) 0.049(5) -0.019(4) -0.007(3) -0.002(3) C46 0.034(4) 0.049(4) 0.035(4) -0.001(3) 0.001(3) 0.001(3) C47 0.036(4) 0.070(5) 0.053(5) 0.024(4) 0.003(3) -0.003(3) C48 0.056(5) 0.080(6) 0.037(4) -0.009(4) 0.010(3) 0.011(4) C49 0.081(6) 0.052(5) 0.096(7) -0.003(4) -0.029(5) -0.013(4) C50 0.032(3) 0.036(4) 0.035(4) 0.009(3) -0.008(3) 0.000(3) C51 0.026(3) 0.036(4) 0.035(4) 0.004(3) -0.003(3) 0.003(3) C52 0.049(4) 0.044(5) 0.056(5) 0.013(3) 0.013(3) 0.008(3) C53 0.059(5) 0.032(5) 0.119(8) 0.019(4) 0.025(5) 0.005(4) C54 0.067(6) 0.034(5) 0.133(9) -0.015(5) 0.013(5) -0.003(4) C55 0.078(6) 0.053(5) 0.070(6) -0.017(4) 0.028(4) 0.003(4) C56 0.053(4) 0.035(4) 0.051(5) 0.001(3) 0.003(3) 0.007(3) C57 0.025(3) 0.037(4) 0.038(4) -0.012(3) -0.003(3) 0.002(3) C58 0.034(4) 0.049(4) 0.041(4) 0.000(3) -0.004(3) 0.000(3) C59 0.029(4) 0.064(5) 0.053(5) 0.003(4) 0.013(3) -0.001(3) C60 0.017(3) 0.102(7) 0.055(5) -0.007(4) -0.003(3) 0.012(4) C61 0.035(4) 0.092(6) 0.040(4) 0.015(4) -0.007(3) 0.015(4) C62 0.033(4) 0.063(5) 0.036(4) 0.010(3) 0.004(3) 0.002(3) C63 0.035(4) 0.056(5) 0.037(4) -0.009(3) -0.010(3) 0.003(3) C64 0.037(4) 0.084(6) 0.047(5) -0.012(4) -0.003(3) -0.014(4) C65 0.050(4) 0.057(5) 0.067(5) -0.005(4) 0.000(4) -0.011(4) C66 0.042(4) 0.037(4) 0.056(5) 0.005(3) -0.007(3) -0.005(3) O3 0.137(8) 0.216(12) 0.121(7) -0.009(7) -0.008(6) -0.049(8) C67 0.193(18) 0.102(11) 0.239(19) -0.031(11) -0.105(15) 0.011(11) C68 0.127(11) 0.106(11) 0.180(13) 0.021(9) -0.010(9) -0.024(9) C69 0.140(12) 0.119(11) 0.110(10) 0.000(8) 0.004(8) -0.002(9) C70 0.128(12) 0.164(14) 0.121(11) -0.037(9) 0.008(9) 0.002(11) O4 0.205(15) 0.165(13) 0.52(3) 0.008(14) 0.174(16) -0.004(11) C71 0.196(16) 0.100(11) 0.144(12) -0.014(8) 0.000(10) 0.019(11) C72 0.135(12) 0.102(11) 0.191(14) -0.020(10) 0.028(9) -0.014(9) C73 0.165(14) 0.115(11) 0.173(13) -0.054(9) 0.063(10) 0.008(11) C74 0.076(8) 0.143(13) 0.139(10) 0.012(9) 0.017(7) -0.021(9) _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 Zr1 N4 2.223(4) . ? Zr1 N5 2.238(4) . ? Zr1 N1 2.278(4) . ? Zr1 O1 2.289(4) . ? Zr1 Cl1 2.4501(16) . ? Zr1 Cl3 2.4555(16) . ? Zr1 Cl2 2.5461(16) . ? Zr1 C17 2.693(6) . ? O1 C33 1.457(6) . ? O1 C30 1.463(7) . ? N1 C1 1.299(7) . ? N1 H1 0.8700 . ? N2 C1 1.360(7) . ? N2 C8 1.456(7) . ? N2 Si1 1.798(5) . ? N3 C16 1.452(7) . ? N3 C15 1.462(7) . ? N3 Si1 1.677(5) . ? N4 C17 1.353(6) . ? N4 Si1 1.714(5) . ? N5 C17 1.314(7) . ? N5 C24 1.437(6) . ? Si1 C14 1.849(6) . ? C1 C2 1.487(7) . ? C2 C3 1.384(8) . ? C2 C7 1.391(7) . ? C3 C4 1.391(8) . ? C3 H3 0.9400 . ? C4 C5 1.394(10) . ? C4 H4 0.9400 . ? C5 C6 1.368(10) . ? C5 H5 0.9400 . ? C6 C7 1.364(8) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C9 1.375(8) . ? C8 C13 1.381(8) . ? C9 C10 1.380(8) . ? C9 H9 0.9400 . ? C10 C11 1.365(9) . ? C10 H10 0.9400 . ? C11 C12 1.367(9) . ? C11 H11 0.9400 . ? C12 C13 1.381(8) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.484(8) . ? C18 C19 1.377(8) . ? C18 C23 1.403(7) . ? C19 C20 1.370(8) . ? C19 H19 0.9400 . ? C20 C21 1.373(9) . ? C20 H20 0.9400 . ? C21 C22 1.380(9) . ? C21 H21 0.9400 . ? C22 C23 1.373(9) . ? C22 H22 0.9400 . ? C23 H23 0.9400 . ? C24 C25 1.377(8) . ? C24 C29 1.384(8) . ? C25 C26 1.379(8) . ? C25 H25 0.9400 . ? C26 C27 1.369(10) . ? C26 H26 0.9400 . ? C27 C28 1.375(9) . ? C27 H27 0.9400 . ? C28 C29 1.399(8) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C30 C31 1.489(9) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.508(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.496(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 N6 1.299(7) . ? C34 N7 1.368(7) . ? C34 C35 1.481(8) . ? C35 C36 1.378(8) . ? C35 C40 1.411(8) . ? C36 C37 1.399(9) . ? C36 H36 0.9400 . ? C37 C38 1.363(11) . ? C37 H37 0.9400 . ? Zr2 N9 2.225(5) . ? Zr2 N10 2.234(4) . ? Zr2 N6 2.274(5) . ? Zr2 O2 2.276(4) . ? Zr2 Cl6 2.4467(16) . ? Zr2 Cl4 2.4598(16) . ? Zr2 Cl5 2.5530(16) . ? Zr2 C50 2.690(6) . ? O2 C63 1.456(6) . ? O2 C66 1.463(7) . ? N6 H6A 0.8700 . ? N7 C41 1.459(7) . ? N7 Si2 1.803(5) . ? N8 C49 1.484(8) . ? N8 C48 1.494(8) . ? N8 Si2 1.657(6) . ? N9 C50 1.338(7) . ? N9 Si2 1.722(5) . ? N10 C50 1.323(7) . ? N10 C57 1.441(7) . ? Si2 C47 1.864(6) . ? C38 C39 1.357(11) . ? C38 H38 0.9400 . ? C39 C40 1.391(9) . ? C39 H39 0.9400 . ? C40 H40 0.9400 . ? C41 C42 1.373(8) . ? C41 C46 1.380(8) . ? C42 C43 1.380(8) . ? C42 H42 0.9400 . ? C43 C44 1.382(10) . ? C43 H43 0.9400 . ? C44 C45 1.366(9) . ? C44 H44 0.9400 . ? C45 C46 1.386(8) . ? C45 H45 0.9400 . ? C46 H46 0.9400 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C50 C51 1.487(8) . ? C51 C56 1.379(8) . ? C51 C52 1.383(8) . ? C52 C53 1.356(9) . ? C52 H52 0.9400 . ? C53 C54 1.337(11) . ? C53 H53 0.9400 . ? C54 C55 1.401(10) . ? C54 H54 0.9400 . ? C55 C56 1.368(9) . ? C55 H55 0.9400 . ? C56 H56 0.9400 . ? C57 C62 1.357(8) . ? C57 C58 1.382(8) . ? C58 C59 1.388(8) . ? C58 H58 0.9400 . ? C59 C60 1.369(9) . ? C59 H59 0.9400 . ? C60 C61 1.374(9) . ? C60 H60 0.9400 . ? C61 C62 1.378(8) . ? C61 H61 0.9400 . ? C62 H62 0.9400 . ? C63 C64 1.499(9) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C64 C65 1.518(9) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C65 C66 1.523(8) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? O3 C70 1.388(13) . ? O3 C67 1.409(14) . ? C67 C68 1.499(9) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C68 C69 1.483(14) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C69 C70 1.455(14) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? O4 C74 1.332(16) . ? O4 C71 1.478(16) . ? C71 C72 1.444(14) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C72 C73 1.450(14) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C73 C74 1.469(9) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? 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 N4 Zr1 N5 59.09(16) . . ? N4 Zr1 N1 76.45(16) . . ? N5 Zr1 N1 135.45(17) . . ? N4 Zr1 O1 133.69(14) . . ? N5 Zr1 O1 75.36(15) . . ? N1 Zr1 O1 148.96(15) . . ? N4 Zr1 Cl1 91.28(12) . . ? N5 Zr1 Cl1 85.76(12) . . ? N1 Zr1 Cl1 92.93(12) . . ? O1 Zr1 Cl1 93.40(10) . . ? N4 Zr1 Cl3 88.13(12) . . ? N5 Zr1 Cl3 93.07(12) . . ? N1 Zr1 Cl3 87.91(12) . . ? O1 Zr1 Cl3 86.28(10) . . ? Cl1 Zr1 Cl3 178.83(6) . . ? N4 Zr1 Cl2 150.65(11) . . ? N5 Zr1 Cl2 149.83(13) . . ? N1 Zr1 Cl2 74.29(12) . . ? O1 Zr1 Cl2 75.61(10) . . ? Cl1 Zr1 Cl2 87.93(6) . . ? Cl3 Zr1 Cl2 93.08(6) . . ? N4 Zr1 C17 30.04(15) . . ? N5 Zr1 C17 29.08(15) . . ? N1 Zr1 C17 106.39(16) . . ? O1 Zr1 C17 104.24(15) . . ? Cl1 Zr1 C17 87.36(12) . . ? Cl3 Zr1 C17 91.63(12) . . ? Cl2 Zr1 C17 175.27(12) . . ? C33 O1 C30 108.8(4) . . ? C33 O1 Zr1 120.6(3) . . ? C30 O1 Zr1 124.7(3) . . ? C1 N1 Zr1 135.8(4) . . ? C1 N1 H1 112.1 . . ? Zr1 N1 H1 112.1 . . ? C1 N2 C8 118.5(4) . . ? C1 N2 Si1 121.6(4) . . ? C8 N2 Si1 119.7(3) . . ? C16 N3 C15 114.0(5) . . ? C16 N3 Si1 125.0(4) . . ? C15 N3 Si1 121.0(4) . . ? C17 N4 Si1 131.0(4) . . ? C17 N4 Zr1 94.6(3) . . ? Si1 N4 Zr1 133.9(2) . . ? C17 N5 C24 122.7(5) . . ? C17 N5 Zr1 95.1(3) . . ? C24 N5 Zr1 138.1(4) . . ? N3 Si1 N4 113.8(2) . . ? N3 Si1 N2 106.4(2) . . ? N4 Si1 N2 103.4(2) . . ? N3 Si1 C14 113.8(3) . . ? N4 Si1 C14 112.7(3) . . ? N2 Si1 C14 105.4(2) . . ? N1 C1 N2 120.1(5) . . ? N1 C1 C2 120.4(5) . . ? N2 C1 C2 119.5(5) . . ? C3 C2 C7 119.2(5) . . ? C3 C2 C1 119.6(5) . . ? C7 C2 C1 121.1(5) . . ? C2 C3 C4 120.2(6) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 119.2(7) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.1(6) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C7 C6 C5 120.7(7) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C2 120.5(6) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C9 C8 C13 120.1(5) . . ? C9 C8 N2 119.0(5) . . ? C13 C8 N2 121.0(5) . . ? C8 C9 C10 119.7(6) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 119.9(6) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.9(6) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C13 119.6(6) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C8 119.7(6) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 N4 111.2(5) . . ? N5 C17 C18 125.3(5) . . ? N4 C17 C18 123.4(5) . . ? N5 C17 Zr1 55.9(3) . . ? N4 C17 Zr1 55.4(3) . . ? C18 C17 Zr1 178.8(4) . . ? C19 C18 C23 117.9(5) . . ? C19 C18 C17 122.6(5) . . ? C23 C18 C17 119.3(5) . . ? C20 C19 C18 121.6(6) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 120.0(6) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 119.8(6) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 120.2(6) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 120.5(6) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? C25 C24 C29 119.6(5) . . ? C25 C24 N5 120.8(5) . . ? C29 C24 N5 119.5(5) . . ? C26 C25 C24 120.1(6) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.8(6) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 119.7(6) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C29 120.1(6) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 119.6(6) . . ? C24 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? O1 C30 C31 105.0(5) . . ? O1 C30 H30A 110.8 . . ? C31 C30 H30A 110.8 . . ? O1 C30 H30B 110.8 . . ? C31 C30 H30B 110.8 . . ? H30A C30 H30B 108.8 . . ? C30 C31 C32 103.9(6) . . ? C30 C31 H31A 111.0 . . ? C32 C31 H31A 111.0 . . ? C30 C31 H31B 111.0 . . ? C32 C31 H31B 111.0 . . ? H31A C31 H31B 109.0 . . ? C33 C32 C31 101.4(5) . . ? C33 C32 H32A 111.5 . . ? C31 C32 H32A 111.5 . . ? C33 C32 H32B 111.5 . . ? C31 C32 H32B 111.5 . . ? H32A C32 H32B 109.3 . . ? O1 C33 C32 105.3(5) . . ? O1 C33 H33A 110.7 . . ? C32 C33 H33A 110.7 . . ? O1 C33 H33B 110.7 . . ? C32 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? N6 C34 N7 120.6(5) . . ? N6 C34 C35 119.9(5) . . ? N7 C34 C35 119.4(5) . . ? C36 C35 C40 118.9(6) . . ? C36 C35 C34 120.1(6) . . ? C40 C35 C34 120.9(6) . . ? C35 C36 C37 121.3(7) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C38 C37 C36 118.1(8) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? N9 Zr2 N10 59.03(16) . . ? N9 Zr2 N6 76.52(17) . . ? N10 Zr2 N6 135.44(18) . . ? N9 Zr2 O2 133.27(15) . . ? N10 Zr2 O2 74.50(15) . . ? N6 Zr2 O2 150.05(16) . . ? N9 Zr2 Cl6 92.74(13) . . ? N10 Zr2 Cl6 89.31(13) . . ? N6 Zr2 Cl6 89.92(13) . . ? O2 Zr2 Cl6 91.24(10) . . ? N9 Zr2 Cl4 86.91(13) . . ? N10 Zr2 Cl4 90.83(13) . . ? N6 Zr2 Cl4 89.63(13) . . ? O2 Zr2 Cl4 89.28(10) . . ? Cl6 Zr2 Cl4 179.49(6) . . ? N9 Zr2 Cl5 151.17(12) . . ? N10 Zr2 Cl5 149.72(13) . . ? N6 Zr2 Cl5 74.83(13) . . ? O2 Zr2 Cl5 75.24(10) . . ? Cl6 Zr2 Cl5 90.46(6) . . ? Cl4 Zr2 Cl5 89.67(5) . . ? N9 Zr2 C50 29.70(16) . . ? N10 Zr2 C50 29.33(16) . . ? N6 Zr2 C50 106.14(18) . . ? O2 Zr2 C50 103.76(16) . . ? Cl6 Zr2 C50 90.61(12) . . ? Cl4 Zr2 C50 89.27(12) . . ? Cl5 Zr2 C50 178.55(13) . . ? C63 O2 C66 108.7(4) . . ? C63 O2 Zr2 123.7(4) . . ? C66 O2 Zr2 123.4(3) . . ? C34 N6 Zr2 135.6(4) . . ? C34 N6 H6A 112.2 . . ? Zr2 N6 H6A 112.2 . . ? C34 N7 C41 117.8(5) . . ? C34 N7 Si2 122.1(4) . . ? C41 N7 Si2 120.0(4) . . ? C49 N8 C48 115.0(6) . . ? C49 N8 Si2 124.8(5) . . ? C48 N8 Si2 120.2(5) . . ? C50 N9 Si2 130.2(4) . . ? C50 N9 Zr2 94.8(4) . . ? Si2 N9 Zr2 134.2(3) . . ? C50 N10 C57 124.1(5) . . ? C50 N10 Zr2 94.8(4) . . ? C57 N10 Zr2 138.2(4) . . ? N8 Si2 N9 113.5(3) . . ? N8 Si2 N7 106.9(2) . . ? N9 Si2 N7 103.7(2) . . ? N8 Si2 C47 111.7(3) . . ? N9 Si2 C47 113.7(3) . . ? N7 Si2 C47 106.5(3) . . ? C39 C38 C37 122.3(7) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C38 C39 C40 120.4(7) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C39 C40 C35 118.9(7) . . ? C39 C40 H40 120.6 . . ? C35 C40 H40 120.6 . . ? C42 C41 C46 120.5(6) . . ? C42 C41 N7 119.4(5) . . ? C46 C41 N7 120.1(5) . . ? C41 C42 C43 120.7(6) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 118.5(7) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? C45 C44 C43 121.1(6) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 120.2(7) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 119.0(6) . . ? C41 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N8 C48 H48A 109.5 . . ? N8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N8 C49 H49A 109.5 . . ? N8 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N8 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N10 C50 N9 111.3(5) . . ? N10 C50 C51 124.2(5) . . ? N9 C50 C51 124.4(5) . . ? N10 C50 Zr2 55.8(3) . . ? N9 C50 Zr2 55.5(3) . . ? C51 C50 Zr2 179.6(4) . . ? C56 C51 C52 117.9(6) . . ? C56 C51 C50 120.2(6) . . ? C52 C51 C50 121.8(6) . . ? C53 C52 C51 121.6(7) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C54 C53 C52 120.9(7) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 119.2(7) . . ? C53 C54 H54 120.4 . . ? C55 C54 H54 120.4 . . ? C56 C55 C54 120.0(7) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.3(7) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? C62 C57 C58 120.5(6) . . ? C62 C57 N10 121.4(6) . . ? C58 C57 N10 118.0(5) . . ? C57 C58 C59 118.9(6) . . ? C57 C58 H58 120.6 . . ? C59 C58 H58 120.6 . . ? C60 C59 C58 120.6(6) . . ? C60 C59 H59 119.7 . . ? C58 C59 H59 119.7 . . ? C59 C60 C61 119.4(6) . . ? C59 C60 H60 120.3 . . ? C61 C60 H60 120.3 . . ? C60 C61 C62 120.4(6) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? C57 C62 C61 120.1(6) . . ? C57 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? O2 C63 C64 105.5(5) . . ? O2 C63 H63A 110.6 . . ? C64 C63 H63A 110.6 . . ? O2 C63 H63B 110.6 . . ? C64 C63 H63B 110.6 . . ? H63A C63 H63B 108.8 . . ? C63 C64 C65 101.4(5) . . ? C63 C64 H64A 111.5 . . ? C65 C64 H64A 111.5 . . ? C63 C64 H64B 111.5 . . ? C65 C64 H64B 111.5 . . ? H64A C64 H64B 109.3 . . ? C64 C65 C66 100.9(6) . . ? C64 C65 H65A 111.6 . . ? C66 C65 H65A 111.6 . . ? C64 C65 H65B 111.6 . . ? C66 C65 H65B 111.6 . . ? H65A C65 H65B 109.4 . . ? O2 C66 C65 104.1(5) . . ? O2 C66 H66A 110.9 . . ? C65 C66 H66A 110.9 . . ? O2 C66 H66B 110.9 . . ? C65 C66 H66B 110.9 . . ? H66A C66 H66B 109.0 . . ? C70 O3 C67 108.5(11) . . ? C68 C67 O3 108.5(11) . . ? C68 C67 H67A 110.0 . . ? O3 C67 H67A 110.0 . . ? C68 C67 H67B 110.0 . . ? O3 C67 H67B 110.0 . . ? H67A C67 H67B 108.4 . . ? C67 C68 C69 103.8(11) . . ? C67 C68 H68A 111.0 . . ? C69 C68 H68A 111.0 . . ? C67 C68 H68B 111.0 . . ? C69 C68 H68B 111.0 . . ? H68A C68 H68B 109.0 . . ? C70 C69 C68 107.1(11) . . ? C70 C69 H69A 110.3 . . ? C68 C69 H69A 110.3 . . ? C70 C69 H69B 110.3 . . ? C68 C69 H69B 110.3 . . ? H69A C69 H69B 108.6 . . ? O3 C70 C69 108.7(12) . . ? O3 C70 H70A 110.0 . . ? C69 C70 H70A 110.0 . . ? O3 C70 H70B 110.0 . . ? C69 C70 H70B 110.0 . . ? H70A C70 H70B 108.3 . . ? C74 O4 C71 108.3(12) . . ? C72 C71 O4 103.4(12) . . ? C72 C71 H71A 111.1 . . ? O4 C71 H71A 111.1 . . ? C72 C71 H71B 111.1 . . ? O4 C71 H71B 111.1 . . ? H71A C71 H71B 109.0 . . ? C71 C72 C73 109.6(11) . . ? C71 C72 H72A 109.8 . . ? C73 C72 H72A 109.8 . . ? C71 C72 H72B 109.8 . . ? C73 C72 H72B 109.8 . . ? H72A C72 H72B 108.2 . . ? C74 C73 C72 100.0(11) . . ? C74 C73 H73A 111.8 . . ? C72 C73 H73A 111.8 . . ? C74 C73 H73B 111.8 . . ? C72 C73 H73B 111.8 . . ? H73A C73 H73B 109.5 . . ? O4 C74 C73 110.6(11) . . ? O4 C74 H74A 109.5 . . ? C73 C74 H74A 109.5 . . ? O4 C74 H74B 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.407 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.084