data_sh4060 _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H106 B N Si5' _chemical_formula_sum 'C66 H106 B N Si5' _chemical_formula_weight 1064.77 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' 'B' 'B' 0.0013 0.0007 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5006(6) _cell_length_b 13.5798(6) _cell_length_c 18.9871(8) _cell_angle_alpha 98.387(2) _cell_angle_beta 92.938(2) _cell_angle_gamma 106.305(2) _cell_volume 3289.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 132(2) _cell_measurement_reflns_used 9672 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.76 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_F_000 1168 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.652 _exptl_crystal_size_mid 0.377 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 0.146 _shelx_estimated_absorpt_T_min 0.911 _shelx_estimated_absorpt_T_max 0.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7190 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 132(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 76421 _diffrn_reflns_av_unetI/netI 0.0359 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.089 _diffrn_reflns_theta_max 30.988 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 20730 _reflns_number_gt 16525 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.8406P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 20730 _refine_ls_number_parameters 1082 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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_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 Si1 Si 0.47547(2) 0.21690(2) 0.14532(2) 0.01490(6) Uani 1 1 d . . . . . Si2 Si 0.45467(2) 0.34646(2) 0.25405(2) 0.01449(6) Uani 1 1 d . . . . . Si3 Si 0.45793(2) 0.17473(2) 0.25941(2) 0.01214(6) Uani 1 1 d . . . . . Si4 Si 0.64045(2) 0.22941(2) 0.29085(2) 0.01138(6) Uani 1 1 d . . . . . Si5 Si 0.61475(2) 0.34532(2) 0.21534(2) 0.01332(6) Uani 1 1 d . . . . . N1 N 0.32273(8) 0.35262(7) 0.11095(5) 0.02045(19) Uani 1 1 d . . . . . B1 B 0.38580(10) 0.31494(9) 0.15198(6) 0.0179(2) Uani 1 1 d . . . . . C1 C 0.34594(8) 0.08310(8) 0.29605(5) 0.01325(18) Uani 1 1 d . . . . . C2 C 0.29357(8) -0.01678(8) 0.25733(5) 0.01497(19) Uani 1 1 d . . . . . C3 C 0.20448(8) -0.07724(8) 0.28160(6) 0.0186(2) Uani 1 1 d . . . . . C4 C 0.16518(8) -0.04425(9) 0.34407(6) 0.0196(2) Uani 1 1 d . . . . . C5 C 0.22065(9) 0.05179(9) 0.38393(6) 0.0196(2) Uani 1 1 d . . . . . C6 C 0.30904(8) 0.11585(8) 0.36136(5) 0.01557(19) Uani 1 1 d . . . . . C7 C 0.32961(8) -0.06015(8) 0.18822(6) 0.0168(2) Uani 1 1 d . . . . . C8 C 0.26470(11) -0.04941(11) 0.12320(6) 0.0260(2) Uani 1 1 d . . . . . C9 C 0.33057(10) -0.17252(9) 0.18643(7) 0.0246(2) Uani 1 1 d . . . . . C10 C 0.06372(9) -0.10848(10) 0.36598(7) 0.0247(2) Uani 1 1 d . . . . . C11 C -0.02137(11) -0.05592(13) 0.35801(9) 0.0375(3) Uani 1 1 d . . . . . C12 C 0.07371(12) -0.13157(13) 0.44173(8) 0.0369(3) Uani 1 1 d . . . . . C13 C 0.35942(9) 0.22144(8) 0.40717(6) 0.0175(2) Uani 1 1 d . . . . . C14 C 0.29040(11) 0.29244(10) 0.40081(7) 0.0268(2) Uani 1 1 d . . . . . C15 C 0.38610(11) 0.21499(10) 0.48517(6) 0.0267(3) Uani 1 1 d . . . . . C16 C 0.66096(8) 0.25455(8) 0.39304(5) 0.01356(18) Uani 1 1 d . . . . . C17 C 0.68023(8) 0.35238(8) 0.43773(5) 0.01591(19) Uani 1 1 d . . . . . C18 C 0.69071(9) 0.35892(9) 0.51177(6) 0.0192(2) Uani 1 1 d . . . . . C19 C 0.68401(8) 0.27282(9) 0.54450(6) 0.0185(2) Uani 1 1 d . . . . . C20 C 0.66546(8) 0.17708(9) 0.50075(6) 0.0173(2) Uani 1 1 d . . . . . C21 C 0.65342(8) 0.16647(8) 0.42626(5) 0.01447(19) Uani 1 1 d . . . . . C22 C 0.68808(9) 0.45302(8) 0.40931(6) 0.0188(2) Uani 1 1 d . . . . . C23 C 0.59395(10) 0.49071(10) 0.42573(7) 0.0246(2) Uani 1 1 d . . . . . C24 C 0.78869(11) 0.53855(9) 0.43791(7) 0.0267(2) Uani 1 1 d . . . . . C25 C 0.69595(10) 0.28353(10) 0.62540(6) 0.0239(2) Uani 1 1 d . . . . . C26 C 0.61267(13) 0.32568(12) 0.65898(7) 0.0336(3) Uani 1 1 d . . . . . C27 C 0.80371(13) 0.35126(14) 0.65696(8) 0.0395(3) Uani 1 1 d . . . . . C28 C 0.63252(8) 0.05733(8) 0.38350(6) 0.01617(19) Uani 1 1 d . . . . . C29 C 0.53308(10) -0.01806(9) 0.40110(7) 0.0225(2) Uani 1 1 d . . . . . C30 C 0.72517(10) 0.01522(10) 0.39346(7) 0.0251(2) Uani 1 1 d . . . . . C31 C 0.74608(8) 0.17065(8) 0.25570(5) 0.01328(18) Uani 1 1 d . . . . . C32 C 0.72908(8) 0.07391(8) 0.20994(5) 0.01464(19) Uani 1 1 d . . . . . C33 C 0.81330(8) 0.04184(8) 0.18743(6) 0.0172(2) Uani 1 1 d . . . . . C34 C 0.91548(8) 0.10032(8) 0.20811(6) 0.0174(2) Uani 1 1 d . . . . . C35 C 0.93186(8) 0.19440(9) 0.25304(6) 0.0180(2) Uani 1 1 d . . . . . C36 C 0.85005(8) 0.23102(8) 0.27636(5) 0.01557(19) Uani 1 1 d . . . . . C37 C 0.62193(8) 0.00093(8) 0.18286(6) 0.0175(2) Uani 1 1 d . . . . . C38 C 0.59737(10) -0.00171(10) 0.10316(7) 0.0250(2) Uani 1 1 d . . . . . C39 C 0.60977(10) -0.10936(9) 0.19784(8) 0.0260(2) Uani 1 1 d . . . . . C40 C 1.00278(9) 0.06097(9) 0.17949(6) 0.0214(2) Uani 1 1 d . . . . . C41 C 1.10917(10) 0.12113(11) 0.21732(8) 0.0287(3) Uani 1 1 d . . . . . C42 C 1.00196(11) 0.05915(12) 0.09886(7) 0.0319(3) Uani 1 1 d . . . . . C43 C 0.88093(8) 0.33680(8) 0.32474(6) 0.0190(2) Uani 1 1 d . . . . . C44 C 0.94958(10) 0.42241(10) 0.28924(8) 0.0281(3) Uani 1 1 d . . . . . C45 C 0.93303(11) 0.33122(12) 0.39688(7) 0.0306(3) Uani 1 1 d . . . . . C46 C 0.71476(8) 0.44218(8) 0.17356(5) 0.01484(19) Uani 1 1 d . . . . . C47 C 0.73956(8) 0.55103(8) 0.19653(6) 0.0174(2) Uani 1 1 d . . . . . C48 C 0.81769(9) 0.61817(8) 0.16636(6) 0.0199(2) Uani 1 1 d . . . . . C49 C 0.87210(8) 0.58205(8) 0.11338(6) 0.0191(2) Uani 1 1 d . . . . . C50 C 0.84554(9) 0.47526(9) 0.09009(6) 0.0192(2) Uani 1 1 d . . . . . C51 C 0.76995(8) 0.40489(8) 0.11930(5) 0.01611(19) Uani 1 1 d . . . . . C52 C 0.67888(10) 0.59672(8) 0.25078(6) 0.0213(2) Uani 1 1 d . . . . . C53 C 0.74129(14) 0.69991(10) 0.29668(8) 0.0347(3) Uani 1 1 d . . . . . C54 C 0.58170(11) 0.60905(11) 0.21274(8) 0.0295(3) Uani 1 1 d . . . . . C55 C 0.96141(9) 0.65241(9) 0.08236(7) 0.0227(2) Uani 1 1 d . . . . . C56 C 0.96904(11) 0.76727(11) 0.09835(10) 0.0379(3) Uani 1 1 d . . . . . C57 C 1.06307(10) 0.63536(12) 0.10783(9) 0.0320(3) Uani 1 1 d . . . . . C58 C 0.74620(9) 0.29011(8) 0.08916(6) 0.0180(2) Uani 1 1 d . . . . . C59 C 0.67548(10) 0.26485(10) 0.01936(6) 0.0240(2) Uani 1 1 d . . . . . C60 C 0.84232(10) 0.25382(10) 0.07810(7) 0.0256(2) Uani 1 1 d . . . . . C61 C 0.29851(10) 0.31684(11) 0.03241(6) 0.0279(3) Uani 1 1 d . . . . . C62 C 0.39229(15) 0.35605(19) -0.00709(9) 0.0535(5) Uani 1 1 d . . . . . C63 C 0.25494(13) 0.19906(12) 0.01435(8) 0.0391(3) Uani 1 1 d . . . . . C64 C 0.27765(11) 0.43488(10) 0.14264(7) 0.0289(3) Uani 1 1 d . . . . . C65 C 0.15988(13) 0.39457(13) 0.14026(10) 0.0409(4) Uani 1 1 d . . . . . C66 C 0.31054(14) 0.53234(12) 0.10856(11) 0.0421(4) Uani 1 1 d . . . . . H1 H 0.1653(10) -0.1454(11) 0.2532(7) 0.022(3) Uiso 1 1 d . . . . . H2 H 0.1952(11) 0.0761(11) 0.4273(8) 0.026(4) Uiso 1 1 d . . . . . H3 H 0.3995(10) -0.0183(10) 0.1856(7) 0.018(3) Uiso 1 1 d . . . . . H4 H 0.2873(12) -0.0752(12) 0.0781(9) 0.037(4) Uiso 1 1 d . . . . . H5 H 0.1928(13) -0.0873(12) 0.1236(8) 0.037(4) Uiso 1 1 d . . . . . H6 H 0.2690(11) 0.0239(12) 0.1224(8) 0.031(4) Uiso 1 1 d . . . . . H7 H 0.3735(12) -0.1783(11) 0.2300(8) 0.032(4) Uiso 1 1 d . . . . . H8 H 0.2611(13) -0.2192(13) 0.1847(8) 0.039(4) Uiso 1 1 d . . . . . H9 H 0.3622(11) -0.1961(11) 0.1424(8) 0.030(4) Uiso 1 1 d . . . . . H10 H 0.0434(11) -0.1760(12) 0.3330(8) 0.033(4) Uiso 1 1 d . . . . . H11 H -0.0353(15) -0.0470(15) 0.3077(11) 0.061(6) Uiso 1 1 d . . . . . H12 H -0.0861(14) -0.0957(13) 0.3719(9) 0.043(4) Uiso 1 1 d . . . . . H13 H 0.0008(14) 0.0146(15) 0.3870(10) 0.054(5) Uiso 1 1 d . . . . . H14 H 0.1275(14) -0.1653(13) 0.4498(9) 0.047(5) Uiso 1 1 d . . . . . H15 H 0.0073(14) -0.1793(13) 0.4506(9) 0.045(5) Uiso 1 1 d . . . . . H16 H 0.0876(14) -0.0646(15) 0.4768(10) 0.053(5) Uiso 1 1 d . . . . . H17 H 0.4253(10) 0.2528(10) 0.3888(7) 0.020(3) Uiso 1 1 d . . . . . H18 H 0.2734(12) 0.2961(12) 0.3501(9) 0.038(4) Uiso 1 1 d . . . . . H19 H 0.2267(13) 0.2670(12) 0.4215(8) 0.035(4) Uiso 1 1 d . . . . . H20 H 0.3228(12) 0.3613(12) 0.4249(8) 0.034(4) Uiso 1 1 d . . . . . H21 H 0.3229(13) 0.1895(12) 0.5085(9) 0.040(4) Uiso 1 1 d . . . . . H22 H 0.4231(11) 0.2826(12) 0.5103(8) 0.028(4) Uiso 1 1 d . . . . . H23 H 0.4300(13) 0.1694(13) 0.4891(9) 0.041(4) Uiso 1 1 d . . . . . H24 H 0.7043(10) 0.4261(10) 0.5415(7) 0.021(3) Uiso 1 1 d . . . . . H25 H 0.6618(10) 0.1154(10) 0.5225(7) 0.020(3) Uiso 1 1 d . . . . . H26 H 0.6886(10) 0.4394(10) 0.3585(7) 0.017(3) Uiso 1 1 d . . . . . H27 H 0.5967(12) 0.5548(12) 0.4061(8) 0.036(4) Uiso 1 1 d . . . . . H28 H 0.5902(11) 0.5049(11) 0.4776(8) 0.029(4) Uiso 1 1 d . . . . . H29 H 0.5305(12) 0.4395(12) 0.4073(8) 0.033(4) Uiso 1 1 d . . . . . H30 H 0.7958(11) 0.5547(11) 0.4899(8) 0.032(4) Uiso 1 1 d . . . . . H31 H 0.8495(13) 0.5201(12) 0.4249(9) 0.040(4) Uiso 1 1 d . . . . . H32 H 0.7933(12) 0.6046(13) 0.4183(8) 0.040(4) Uiso 1 1 d . . . . . H33 H 0.6867(10) 0.2140(11) 0.6369(7) 0.023(3) Uiso 1 1 d . . . . . H34 H 0.6182(13) 0.3944(14) 0.6504(9) 0.043(5) Uiso 1 1 d . . . . . H35 H 0.6204(12) 0.3286(12) 0.7118(9) 0.041(4) Uiso 1 1 d . . . . . H36 H 0.5423(13) 0.2827(13) 0.6394(9) 0.041(4) Uiso 1 1 d . . . . . H37 H 0.8581(15) 0.3251(14) 0.6354(10) 0.054(5) Uiso 1 1 d . . . . . H38 H 0.8147(13) 0.4216(14) 0.6492(9) 0.043(5) Uiso 1 1 d . . . . . H39 H 0.8101(14) 0.3558(14) 0.7112(10) 0.053(5) Uiso 1 1 d . . . . . H40 H 0.6236(9) 0.0616(9) 0.3331(7) 0.013(3) Uiso 1 1 d . . . . . H41 H 0.5176(12) -0.0850(13) 0.3685(9) 0.039(4) Uiso 1 1 d . . . . . H42 H 0.5404(11) -0.0300(11) 0.4499(8) 0.026(4) Uiso 1 1 d . . . . . H43 H 0.4752(11) 0.0079(11) 0.3943(8) 0.027(4) Uiso 1 1 d . . . . . H44 H 0.7872(12) 0.0613(11) 0.3775(8) 0.029(4) Uiso 1 1 d . . . . . H45 H 0.7112(12) -0.0537(12) 0.3649(8) 0.035(4) Uiso 1 1 d . . . . . H46 H 0.7392(12) 0.0098(11) 0.4430(8) 0.033(4) Uiso 1 1 d . . . . . H47 H 0.8002(10) -0.0237(10) 0.1558(7) 0.020(3) Uiso 1 1 d . . . . . H48 H 1.0007(11) 0.2361(10) 0.2690(7) 0.020(3) Uiso 1 1 d . . . . . H49 H 0.5726(10) 0.0273(10) 0.2072(7) 0.017(3) Uiso 1 1 d . . . . . H50 H 0.6030(12) 0.0666(12) 0.0935(8) 0.035(4) Uiso 1 1 d . . . . . H51 H 0.5268(12) -0.0488(12) 0.0852(8) 0.034(4) Uiso 1 1 d . . . . . H52 H 0.6476(12) -0.0278(12) 0.0749(9) 0.039(4) Uiso 1 1 d . . . . . H53 H 0.5422(12) -0.1544(12) 0.1811(8) 0.033(4) Uiso 1 1 d . . . . . H54 H 0.6229(13) -0.1124(13) 0.2482(10) 0.045(5) Uiso 1 1 d . . . . . H55 H 0.6592(13) -0.1407(13) 0.1729(9) 0.041(4) Uiso 1 1 d . . . . . H56 H 0.9881(10) -0.0106(11) 0.1869(7) 0.022(3) Uiso 1 1 d . . . . . H57 H 1.1300(12) 0.1944(13) 0.2085(8) 0.036(4) Uiso 1 1 d . . . . . H58 H 1.1100(12) 0.1209(12) 0.2700(9) 0.035(4) Uiso 1 1 d . . . . . H59 H 1.1603(13) 0.0890(13) 0.2000(9) 0.045(5) Uiso 1 1 d . . . . . H60 H 1.0154(12) 0.1297(13) 0.0874(8) 0.037(4) Uiso 1 1 d . . . . . H61 H 0.9364(13) 0.0195(13) 0.0724(9) 0.041(4) Uiso 1 1 d . . . . . H62 H 1.0551(13) 0.0340(12) 0.0804(8) 0.038(4) Uiso 1 1 d . . . . . H63 H 0.8190(10) 0.3556(10) 0.3340(7) 0.018(3) Uiso 1 1 d . . . . . H64 H 0.9632(12) 0.4893(13) 0.3201(9) 0.039(4) Uiso 1 1 d . . . . . H65 H 0.9165(12) 0.4259(12) 0.2429(9) 0.039(4) Uiso 1 1 d . . . . . H66 H 1.0155(13) 0.4083(12) 0.2830(9) 0.041(4) Uiso 1 1 d . . . . . H67 H 0.9983(13) 0.3112(12) 0.3914(8) 0.040(4) Uiso 1 1 d . . . . . H68 H 0.9549(14) 0.3991(14) 0.4272(10) 0.053(5) Uiso 1 1 d . . . . . H69 H 0.8871(13) 0.2801(13) 0.4228(9) 0.039(4) Uiso 1 1 d . . . . . H70 H 0.8331(10) 0.6904(11) 0.1828(7) 0.024(3) Uiso 1 1 d . . . . . H71 H 0.8842(11) 0.4494(11) 0.0534(7) 0.024(3) Uiso 1 1 d . . . . . H72 H 0.7079(10) 0.2510(10) 0.1237(7) 0.018(3) Uiso 1 1 d . . . . . H73 H 0.6157(12) 0.2887(11) 0.0263(8) 0.032(4) Uiso 1 1 d . . . . . H74 H 0.6488(11) 0.1880(12) 0.0030(8) 0.032(4) Uiso 1 1 d . . . . . H75 H 0.7105(12) 0.3000(12) -0.0162(9) 0.036(4) Uiso 1 1 d . . . . . H76 H 0.8877(12) 0.2708(12) 0.1217(9) 0.035(4) Uiso 1 1 d . . . . . H77 H 0.8231(11) 0.1773(12) 0.0635(8) 0.028(4) Uiso 1 1 d . . . . . H78 H 0.8827(12) 0.2860(12) 0.0422(8) 0.033(4) Uiso 1 1 d . . . . . H79 H 0.9512(12) 0.6310(12) 0.0295(8) 0.034(4) Uiso 1 1 d . . . . . H80 H 0.9892(14) 0.7941(14) 0.1490(10) 0.052(5) Uiso 1 1 d . . . . . H81 H 0.9038(14) 0.7802(13) 0.0860(9) 0.046(5) Uiso 1 1 d . . . . . H82 H 1.0225(14) 0.8060(14) 0.0674(9) 0.050(5) Uiso 1 1 d . . . . . H83 H 1.1239(13) 0.6822(12) 0.0889(9) 0.040(4) Uiso 1 1 d . . . . . H84 H 1.0603(13) 0.5611(14) 0.0932(9) 0.045(5) Uiso 1 1 d . . . . . H85 H 1.0734(13) 0.6529(13) 0.1601(9) 0.042(4) Uiso 1 1 d . . . . . H86 H 0.6563(10) 0.5482(10) 0.2832(7) 0.018(3) Uiso 1 1 d . . . . . H87 H 0.7003(13) 0.7188(13) 0.3340(9) 0.042(4) Uiso 1 1 d . . . . . H88 H 0.8065(13) 0.6958(12) 0.3183(8) 0.036(4) Uiso 1 1 d . . . . . H89 H 0.7543(12) 0.7569(13) 0.2696(9) 0.038(4) Uiso 1 1 d . . . . . H90 H 0.5994(12) 0.6617(12) 0.1821(8) 0.036(4) Uiso 1 1 d . . . . . H91 H 0.5404(12) 0.5461(13) 0.1843(8) 0.035(4) Uiso 1 1 d . . . . . H92 H 0.5392(13) 0.6316(13) 0.2465(9) 0.045(5) Uiso 1 1 d . . . . . H93 H 0.2451(11) 0.3470(11) 0.0181(8) 0.030(4) Uiso 1 1 d . . . . . H94 H 0.4456(15) 0.3276(14) 0.0061(10) 0.054(5) Uiso 1 1 d . . . . . H95 H 0.4203(16) 0.4338(17) 0.0048(11) 0.064(6) Uiso 1 1 d . . . . . H96 H 0.3758(17) 0.3362(17) -0.0588(13) 0.082(7) Uiso 1 1 d . . . . . H97 H 0.3060(13) 0.1642(13) 0.0299(9) 0.045(5) Uiso 1 1 d . . . . . H98 H 0.1938(15) 0.1762(14) 0.0376(10) 0.050(5) Uiso 1 1 d . . . . . H99 H 0.2350(15) 0.1780(15) -0.0372(11) 0.062(6) Uiso 1 1 d . . . . . H100 H 0.3072(12) 0.4548(12) 0.1918(9) 0.037(4) Uiso 1 1 d . . . . . H101 H 0.1415(16) 0.3379(17) 0.1647(11) 0.070(6) Uiso 1 1 d . . . . . H102 H 0.1340(13) 0.4485(13) 0.1658(9) 0.046(5) Uiso 1 1 d . . . . . H103 H 0.1269(15) 0.3773(15) 0.0889(11) 0.059(6) Uiso 1 1 d . . . . . H104 H 0.2834(14) 0.5846(15) 0.1340(10) 0.052(5) Uiso 1 1 d . . . . . H105 H 0.3838(14) 0.5574(13) 0.1106(9) 0.046(5) Uiso 1 1 d . . . . . H106 H 0.2800(14) 0.5206(14) 0.0593(10) 0.052(5) Uiso 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 Si1 0.01764(14) 0.01436(13) 0.01256(12) 0.00045(10) 0.00174(10) 0.00528(11) Si2 0.01713(14) 0.01322(13) 0.01435(13) 0.00108(10) 0.00263(10) 0.00682(11) Si3 0.01173(13) 0.01130(12) 0.01315(12) 0.00121(9) 0.00176(10) 0.00328(10) Si4 0.01179(13) 0.01029(12) 0.01191(12) 0.00058(9) 0.00246(9) 0.00338(10) Si5 0.01550(13) 0.01065(12) 0.01397(12) 0.00205(10) 0.00338(10) 0.00372(10) N1 0.0237(5) 0.0199(4) 0.0193(4) 0.0050(4) -0.0007(4) 0.0085(4) B1 0.0196(6) 0.0166(5) 0.0178(5) 0.0039(4) 0.0027(4) 0.0051(5) C1 0.0118(4) 0.0129(4) 0.0145(4) 0.0010(3) 0.0013(3) 0.0034(4) C2 0.0136(5) 0.0140(4) 0.0165(5) 0.0002(4) 0.0006(4) 0.0041(4) C3 0.0159(5) 0.0157(5) 0.0205(5) -0.0005(4) 0.0011(4) 0.0005(4) C4 0.0152(5) 0.0196(5) 0.0225(5) 0.0041(4) 0.0044(4) 0.0017(4) C5 0.0186(5) 0.0210(5) 0.0180(5) 0.0010(4) 0.0060(4) 0.0043(4) C6 0.0152(5) 0.0153(5) 0.0155(4) 0.0004(4) 0.0019(4) 0.0043(4) C7 0.0151(5) 0.0149(5) 0.0179(5) -0.0027(4) 0.0020(4) 0.0031(4) C8 0.0285(7) 0.0303(6) 0.0191(5) -0.0034(5) -0.0007(5) 0.0125(5) C9 0.0257(6) 0.0164(5) 0.0307(6) -0.0013(4) 0.0054(5) 0.0067(5) C10 0.0187(5) 0.0252(6) 0.0258(6) 0.0036(5) 0.0056(4) -0.0009(5) C11 0.0177(6) 0.0459(9) 0.0497(9) 0.0184(7) 0.0083(6) 0.0041(6) C12 0.0263(7) 0.0467(9) 0.0363(7) 0.0190(7) 0.0084(6) 0.0011(7) C13 0.0190(5) 0.0162(5) 0.0149(5) -0.0017(4) 0.0032(4) 0.0030(4) C14 0.0291(7) 0.0218(6) 0.0288(6) -0.0033(5) 0.0033(5) 0.0103(5) C15 0.0330(7) 0.0259(6) 0.0163(5) -0.0013(4) 0.0000(5) 0.0037(5) C16 0.0122(4) 0.0151(4) 0.0130(4) 0.0006(3) 0.0028(3) 0.0040(4) C17 0.0160(5) 0.0153(5) 0.0155(5) -0.0003(4) 0.0027(4) 0.0043(4) C18 0.0221(5) 0.0178(5) 0.0154(5) -0.0027(4) 0.0018(4) 0.0050(4) C19 0.0171(5) 0.0239(5) 0.0136(4) 0.0006(4) 0.0016(4) 0.0056(4) C20 0.0170(5) 0.0199(5) 0.0157(5) 0.0040(4) 0.0025(4) 0.0057(4) C21 0.0123(4) 0.0156(5) 0.0152(4) 0.0017(4) 0.0026(3) 0.0037(4) C22 0.0267(6) 0.0132(5) 0.0151(5) -0.0012(4) 0.0034(4) 0.0052(4) C23 0.0311(7) 0.0197(5) 0.0231(6) -0.0033(4) 0.0012(5) 0.0114(5) C24 0.0298(7) 0.0179(5) 0.0284(6) -0.0014(5) 0.0064(5) 0.0026(5) C25 0.0308(6) 0.0271(6) 0.0128(5) 0.0013(4) 0.0003(4) 0.0083(5) C26 0.0474(9) 0.0405(8) 0.0187(6) 0.0052(5) 0.0105(6) 0.0208(7) C27 0.0405(8) 0.0468(9) 0.0232(6) 0.0001(6) -0.0095(6) 0.0051(7) C28 0.0196(5) 0.0139(4) 0.0153(5) 0.0027(4) 0.0023(4) 0.0050(4) C29 0.0244(6) 0.0176(5) 0.0232(5) 0.0039(4) 0.0039(4) 0.0017(5) C30 0.0272(6) 0.0227(6) 0.0283(6) 0.0017(5) 0.0027(5) 0.0136(5) C31 0.0141(5) 0.0132(4) 0.0133(4) 0.0025(3) 0.0037(3) 0.0048(4) C32 0.0157(5) 0.0133(4) 0.0153(4) 0.0018(4) 0.0028(4) 0.0050(4) C33 0.0188(5) 0.0138(5) 0.0195(5) -0.0004(4) 0.0039(4) 0.0069(4) C34 0.0168(5) 0.0186(5) 0.0199(5) 0.0050(4) 0.0055(4) 0.0089(4) C35 0.0134(5) 0.0192(5) 0.0209(5) 0.0016(4) 0.0028(4) 0.0045(4) C36 0.0147(5) 0.0155(5) 0.0164(5) 0.0012(4) 0.0028(4) 0.0046(4) C37 0.0156(5) 0.0135(5) 0.0223(5) -0.0024(4) 0.0026(4) 0.0051(4) C38 0.0261(6) 0.0227(6) 0.0239(6) -0.0031(5) -0.0025(5) 0.0078(5) C39 0.0239(6) 0.0144(5) 0.0366(7) 0.0018(5) 0.0034(5) 0.0020(5) C40 0.0194(5) 0.0207(5) 0.0275(6) 0.0035(4) 0.0072(4) 0.0110(4) C41 0.0182(6) 0.0323(7) 0.0402(7) 0.0054(6) 0.0049(5) 0.0149(5) C42 0.0283(7) 0.0429(8) 0.0287(6) 0.0012(6) 0.0113(5) 0.0180(6) C43 0.0134(5) 0.0178(5) 0.0223(5) -0.0040(4) 0.0024(4) 0.0022(4) C44 0.0225(6) 0.0185(5) 0.0370(7) -0.0028(5) 0.0080(5) -0.0012(5) C45 0.0269(7) 0.0355(7) 0.0241(6) -0.0073(5) -0.0040(5) 0.0078(6) C46 0.0163(5) 0.0125(4) 0.0157(4) 0.0028(4) 0.0028(4) 0.0038(4) C47 0.0196(5) 0.0136(5) 0.0192(5) 0.0017(4) 0.0018(4) 0.0056(4) C48 0.0204(5) 0.0121(5) 0.0258(5) 0.0040(4) 0.0012(4) 0.0023(4) C49 0.0155(5) 0.0185(5) 0.0226(5) 0.0079(4) 0.0007(4) 0.0016(4) C50 0.0189(5) 0.0192(5) 0.0202(5) 0.0053(4) 0.0062(4) 0.0051(4) C51 0.0176(5) 0.0152(5) 0.0162(5) 0.0036(4) 0.0033(4) 0.0051(4) C52 0.0310(6) 0.0116(5) 0.0218(5) 0.0018(4) 0.0085(4) 0.0066(4) C53 0.0548(10) 0.0157(6) 0.0300(7) -0.0024(5) 0.0099(6) 0.0068(6) C54 0.0344(7) 0.0259(6) 0.0358(7) 0.0086(5) 0.0142(6) 0.0175(6) C55 0.0170(5) 0.0231(5) 0.0259(6) 0.0098(5) 0.0014(4) -0.0004(4) C56 0.0229(7) 0.0243(6) 0.0670(11) 0.0211(7) 0.0057(7) 0.0005(5) C57 0.0175(6) 0.0357(7) 0.0445(8) 0.0155(6) 0.0058(5) 0.0054(5) C58 0.0238(5) 0.0141(5) 0.0177(5) 0.0035(4) 0.0088(4) 0.0066(4) C59 0.0300(6) 0.0213(6) 0.0191(5) -0.0001(4) 0.0047(5) 0.0062(5) C60 0.0312(7) 0.0237(6) 0.0282(6) 0.0072(5) 0.0124(5) 0.0151(5) C61 0.0297(6) 0.0383(7) 0.0186(5) 0.0077(5) -0.0027(5) 0.0137(6) C62 0.0493(10) 0.0864(15) 0.0296(8) 0.0262(9) 0.0122(7) 0.0179(10) C63 0.0422(9) 0.0404(8) 0.0318(7) -0.0077(6) -0.0122(6) 0.0167(7) C64 0.0368(7) 0.0257(6) 0.0296(6) 0.0053(5) -0.0036(5) 0.0187(5) C65 0.0411(8) 0.0420(8) 0.0546(10) 0.0216(8) 0.0167(7) 0.0273(7) C66 0.0394(9) 0.0257(7) 0.0642(11) 0.0139(7) -0.0075(8) 0.0131(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 B1 2.0311(13) . ? Si1 Si3 2.3270(4) . ? Si1 Si5 2.3602(4) . ? Si1 Si2 2.5911(4) . ? Si2 B1 2.0379(12) . ? Si2 Si5 2.3215(4) . ? Si2 Si3 2.3617(4) . ? Si3 C1 1.9032(10) . ? Si3 Si4 2.3816(4) . ? Si4 C16 1.9123(10) . ? Si4 C31 1.9228(10) . ? Si4 Si5 2.3594(4) . ? Si5 C46 1.8972(10) . ? N1 B1 1.3735(15) . ? N1 C64 1.4844(16) . ? N1 C61 1.4888(15) . ? C1 C2 1.4133(14) . ? C1 C6 1.4179(14) . ? C2 C3 1.3949(15) . ? C2 C7 1.5187(14) . ? C3 C4 1.3900(15) . ? C3 H1 0.989(14) . ? C4 C5 1.3928(15) . ? C4 C10 1.5177(15) . ? C5 C6 1.3938(15) . ? C5 H2 0.958(14) . ? C6 C13 1.5176(14) . ? C7 C9 1.5251(16) . ? C7 C8 1.5254(16) . ? C7 H3 0.963(13) . ? C8 H4 0.973(16) . ? C8 H5 0.963(16) . ? C8 H6 0.983(15) . ? C9 H7 1.011(15) . ? C9 H8 0.969(16) . ? C9 H9 1.009(15) . ? C10 C12 1.5233(18) . ? C10 C11 1.5250(19) . ? C10 H10 0.991(15) . ? C11 H11 1.00(2) . ? C11 H12 0.962(17) . ? C11 H13 0.989(19) . ? C12 H14 0.978(18) . ? C12 H15 0.986(17) . ? C12 H16 1.010(19) . ? C13 C15 1.5270(16) . ? C13 C14 1.5295(17) . ? C13 H17 0.979(14) . ? C14 H18 0.989(16) . ? C14 H19 0.960(16) . ? C14 H20 0.949(16) . ? C15 H21 0.980(17) . ? C15 H22 0.955(15) . ? C15 H23 0.978(17) . ? C16 C21 1.4132(14) . ? C16 C17 1.4167(14) . ? C17 C18 1.3929(14) . ? C17 C22 1.5199(15) . ? C18 C19 1.3856(15) . ? C18 H24 0.964(13) . ? C19 C20 1.3872(15) . ? C19 C25 1.5175(15) . ? C20 C21 1.3968(14) . ? C20 H25 0.977(13) . ? C21 C28 1.5252(14) . ? C22 C23 1.5276(17) . ? C22 C24 1.5308(17) . ? C22 H26 0.957(13) . ? C23 H27 0.988(16) . ? C23 H28 0.983(15) . ? C23 H29 0.951(16) . ? C24 H30 0.974(15) . ? C24 H31 0.957(17) . ? C24 H32 1.008(16) . ? C25 C27 1.5232(19) . ? C25 C26 1.5254(19) . ? C25 H33 0.975(14) . ? C26 H34 0.954(17) . ? C26 H35 0.996(17) . ? C26 H36 0.985(17) . ? C27 H37 0.985(19) . ? C27 H38 0.959(18) . ? C27 H39 1.020(19) . ? C28 C29 1.5284(16) . ? C28 C30 1.5285(16) . ? C28 H40 0.971(12) . ? C29 H41 0.985(16) . ? C29 H42 0.969(14) . ? C29 H43 0.954(15) . ? C30 H44 0.986(15) . ? C30 H45 0.974(16) . ? C30 H46 0.968(15) . ? C31 C36 1.4142(14) . ? C31 C32 1.4179(14) . ? C32 C33 1.3923(14) . ? C32 C37 1.5197(15) . ? C33 C34 1.3879(15) . ? C33 H47 0.964(13) . ? C34 C35 1.3831(15) . ? C34 C40 1.5181(15) . ? C35 C36 1.3991(15) . ? C35 H48 0.949(13) . ? C36 C43 1.5234(14) . ? C37 C38 1.5255(16) . ? C37 C39 1.5304(16) . ? C37 H49 0.950(13) . ? C38 H50 0.955(16) . ? C38 H51 0.996(15) . ? C38 H52 0.995(17) . ? C39 H53 0.953(16) . ? C39 H54 0.973(18) . ? C39 H55 0.991(17) . ? C40 C41 1.5200(18) . ? C40 C42 1.5268(18) . ? C40 H56 0.969(14) . ? C41 H57 0.997(16) . ? C41 H58 1.000(16) . ? C41 H59 0.961(18) . ? C42 H60 0.982(16) . ? C42 H61 0.966(17) . ? C42 H62 0.940(17) . ? C43 C45 1.5290(17) . ? C43 C44 1.5337(17) . ? C43 H63 0.958(13) . ? C44 H64 0.971(16) . ? C44 H65 0.981(16) . ? C44 H66 0.971(17) . ? C45 H67 0.999(17) . ? C45 H68 0.971(19) . ? C45 H69 0.999(16) . ? C46 C47 1.4164(14) . ? C46 C51 1.4182(14) . ? C47 C48 1.3951(15) . ? C47 C52 1.5173(15) . ? C48 C49 1.3880(16) . ? C48 H70 0.945(14) . ? C49 C50 1.3899(15) . ? C49 C55 1.5178(15) . ? C50 C51 1.3883(15) . ? C50 H71 0.975(14) . ? C51 C58 1.5166(14) . ? C52 C54 1.5272(18) . ? C52 C53 1.5293(17) . ? C52 H86 0.965(13) . ? C53 H87 0.971(17) . ? C53 H88 0.972(16) . ? C53 H89 0.971(16) . ? C54 H90 0.972(16) . ? C54 H91 0.949(16) . ? C54 H92 0.956(18) . ? C55 C56 1.5180(19) . ? C55 C57 1.5213(17) . ? C55 H79 0.995(15) . ? C56 H80 0.973(19) . ? C56 H81 0.969(18) . ? C56 H82 1.031(18) . ? C57 H83 1.006(17) . ? C57 H84 0.996(17) . ? C57 H85 0.979(17) . ? C58 C60 1.5258(16) . ? C58 C59 1.5296(16) . ? C58 H72 0.982(13) . ? C59 H73 0.958(16) . ? C59 H74 0.999(15) . ? C59 H75 0.952(16) . ? C60 H76 0.962(16) . ? C60 H77 0.990(15) . ? C60 H78 0.972(16) . ? C61 C62 1.511(2) . ? C61 C63 1.521(2) . ? C61 H93 0.969(15) . ? C62 H94 0.95(2) . ? C62 H95 1.00(2) . ? C62 H96 0.98(2) . ? C63 H97 0.995(18) . ? C63 H98 0.952(19) . ? C63 H99 0.98(2) . ? C64 C66 1.522(2) . ? C64 C65 1.525(2) . ? C64 H100 0.964(16) . ? C65 H101 0.94(2) . ? C65 H102 0.975(18) . ? C65 H103 1.02(2) . ? C66 H104 0.968(19) . ? C66 H105 0.949(18) . ? C66 H106 0.975(19) . ? 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 B1 Si1 Si3 97.08(4) . . ? B1 Si1 Si5 91.39(4) . . ? Si3 Si1 Si5 77.147(13) . . ? B1 Si1 Si2 50.56(4) . . ? Si3 Si1 Si2 57.095(11) . . ? Si5 Si1 Si2 55.687(11) . . ? B1 Si2 Si5 92.34(4) . . ? B1 Si2 Si3 95.81(4) . . ? Si5 Si2 Si3 77.223(13) . . ? B1 Si2 Si1 50.33(4) . . ? Si5 Si2 Si1 57.113(12) . . ? Si3 Si2 Si1 55.816(11) . . ? C1 Si3 Si1 130.55(3) . . ? C1 Si3 Si2 119.20(3) . . ? Si1 Si3 Si2 67.089(12) . . ? C1 Si3 Si4 132.58(3) . . ? Si1 Si3 Si4 92.884(14) . . ? Si2 Si3 Si4 92.236(14) . . ? C16 Si4 C31 107.74(4) . . ? C16 Si4 Si5 127.54(3) . . ? C31 Si4 Si5 108.27(3) . . ? C16 Si4 Si3 106.67(3) . . ? C31 Si4 Si3 130.27(3) . . ? Si5 Si4 Si3 76.116(13) . . ? C46 Si5 Si2 132.33(3) . . ? C46 Si5 Si4 128.93(3) . . ? Si2 Si5 Si4 93.831(14) . . ? C46 Si5 Si1 121.72(3) . . ? Si2 Si5 Si1 67.200(13) . . ? Si4 Si5 Si1 92.608(14) . . ? B1 N1 C64 121.31(10) . . ? B1 N1 C61 122.55(10) . . ? C64 N1 C61 116.10(9) . . ? N1 B1 Si1 142.21(9) . . ? N1 B1 Si2 138.23(9) . . ? Si1 B1 Si2 79.10(4) . . ? C2 C1 C6 118.13(9) . . ? C2 C1 Si3 121.24(7) . . ? C6 C1 Si3 120.54(7) . . ? C3 C2 C1 119.77(9) . . ? C3 C2 C7 118.26(9) . . ? C1 C2 C7 121.96(9) . . ? C4 C3 C2 122.56(10) . . ? C4 C3 H1 117.3(8) . . ? C2 C3 H1 120.1(8) . . ? C3 C4 C5 117.19(10) . . ? C3 C4 C10 121.11(10) . . ? C5 C4 C10 121.65(10) . . ? C4 C5 C6 122.38(10) . . ? C4 C5 H2 118.7(8) . . ? C6 C5 H2 118.8(8) . . ? C5 C6 C1 119.82(10) . . ? C5 C6 C13 117.63(9) . . ? C1 C6 C13 122.50(9) . . ? C2 C7 C9 111.99(9) . . ? C2 C7 C8 111.18(9) . . ? C9 C7 C8 111.24(9) . . ? C2 C7 H3 107.4(8) . . ? C9 C7 H3 108.2(8) . . ? C8 C7 H3 106.6(8) . . ? C7 C8 H4 112.8(9) . . ? C7 C8 H5 111.0(9) . . ? H4 C8 H5 107.4(13) . . ? C7 C8 H6 111.0(9) . . ? H4 C8 H6 106.4(12) . . ? H5 C8 H6 107.9(13) . . ? C7 C9 H7 110.2(8) . . ? C7 C9 H8 111.7(9) . . ? H7 C9 H8 109.2(13) . . ? C7 C9 H9 109.8(8) . . ? H7 C9 H9 108.3(12) . . ? H8 C9 H9 107.6(12) . . ? C4 C10 C12 112.89(10) . . ? C4 C10 C11 111.08(10) . . ? C12 C10 C11 110.02(12) . . ? C4 C10 H10 106.7(9) . . ? C12 C10 H10 107.4(9) . . ? C11 C10 H10 108.5(9) . . ? C10 C11 H11 112.0(11) . . ? C10 C11 H12 112.0(10) . . ? H11 C11 H12 106.5(14) . . ? C10 C11 H13 109.5(11) . . ? H11 C11 H13 106.6(15) . . ? H12 C11 H13 110.1(15) . . ? C10 C12 H14 113.4(10) . . ? C10 C12 H15 108.6(10) . . ? H14 C12 H15 107.1(14) . . ? C10 C12 H16 109.0(10) . . ? H14 C12 H16 110.2(14) . . ? H15 C12 H16 108.3(14) . . ? C6 C13 C15 113.20(9) . . ? C6 C13 C14 109.72(9) . . ? C15 C13 C14 111.51(10) . . ? C6 C13 H17 108.2(8) . . ? C15 C13 H17 106.0(8) . . ? C14 C13 H17 107.9(8) . . ? C13 C14 H18 111.0(9) . . ? C13 C14 H19 110.6(9) . . ? H18 C14 H19 108.2(13) . . ? C13 C14 H20 111.9(9) . . ? H18 C14 H20 107.6(13) . . ? H19 C14 H20 107.3(13) . . ? C13 C15 H21 110.7(9) . . ? C13 C15 H22 109.5(9) . . ? H21 C15 H22 108.0(13) . . ? C13 C15 H23 111.4(10) . . ? H21 C15 H23 109.2(13) . . ? H22 C15 H23 107.9(13) . . ? C21 C16 C17 117.78(9) . . ? C21 C16 Si4 116.33(7) . . ? C17 C16 Si4 125.88(8) . . ? C18 C17 C16 119.78(9) . . ? C18 C17 C22 116.85(9) . . ? C16 C17 C22 123.36(9) . . ? C19 C18 C17 122.59(10) . . ? C19 C18 H24 118.5(8) . . ? C17 C18 H24 118.9(8) . . ? C18 C19 C20 117.64(10) . . ? C18 C19 C25 120.83(10) . . ? C20 C19 C25 121.53(10) . . ? C19 C20 C21 121.86(10) . . ? C19 C20 H25 119.2(8) . . ? C21 C20 H25 119.0(8) . . ? C20 C21 C16 120.36(9) . . ? C20 C21 C28 117.34(9) . . ? C16 C21 C28 122.30(9) . . ? C17 C22 C23 110.43(9) . . ? C17 C22 C24 112.77(10) . . ? C23 C22 C24 110.61(9) . . ? C17 C22 H26 108.3(8) . . ? C23 C22 H26 108.1(8) . . ? C24 C22 H26 106.5(8) . . ? C22 C23 H27 111.4(9) . . ? C22 C23 H28 110.7(8) . . ? H27 C23 H28 108.5(12) . . ? C22 C23 H29 112.2(9) . . ? H27 C23 H29 108.6(13) . . ? H28 C23 H29 105.2(12) . . ? C22 C24 H30 111.7(9) . . ? C22 C24 H31 113.1(10) . . ? H30 C24 H31 106.2(13) . . ? C22 C24 H32 112.0(9) . . ? H30 C24 H32 108.5(12) . . ? H31 C24 H32 104.9(13) . . ? C19 C25 C27 111.56(11) . . ? C19 C25 C26 111.35(10) . . ? C27 C25 C26 110.64(12) . . ? C19 C25 H33 107.3(8) . . ? C27 C25 H33 108.1(8) . . ? C26 C25 H33 107.7(8) . . ? C25 C26 H34 111.9(10) . . ? C25 C26 H35 109.5(9) . . ? H34 C26 H35 107.5(13) . . ? C25 C26 H36 111.9(10) . . ? H34 C26 H36 106.3(14) . . ? H35 C26 H36 109.6(13) . . ? C25 C27 H37 111.3(11) . . ? C25 C27 H38 110.9(10) . . ? H37 C27 H38 108.1(15) . . ? C25 C27 H39 109.9(10) . . ? H37 C27 H39 111.3(15) . . ? H38 C27 H39 105.1(14) . . ? C21 C28 C29 112.31(9) . . ? C21 C28 C30 111.23(9) . . ? C29 C28 C30 111.05(9) . . ? C21 C28 H40 108.1(7) . . ? C29 C28 H40 107.2(7) . . ? C30 C28 H40 106.6(7) . . ? C28 C29 H41 110.0(9) . . ? C28 C29 H42 110.5(8) . . ? H41 C29 H42 109.0(12) . . ? C28 C29 H43 110.9(9) . . ? H41 C29 H43 106.5(12) . . ? H42 C29 H43 109.8(12) . . ? C28 C30 H44 110.0(8) . . ? C28 C30 H45 110.2(9) . . ? H44 C30 H45 108.1(12) . . ? C28 C30 H46 111.1(9) . . ? H44 C30 H46 109.3(12) . . ? H45 C30 H46 108.1(12) . . ? C36 C31 C32 117.42(9) . . ? C36 C31 Si4 116.58(7) . . ? C32 C31 Si4 125.99(8) . . ? C33 C32 C31 119.84(9) . . ? C33 C32 C37 116.69(9) . . ? C31 C32 C37 123.47(9) . . ? C34 C33 C32 122.98(10) . . ? C34 C33 H47 118.4(8) . . ? C32 C33 H47 118.6(8) . . ? C35 C34 C33 117.08(9) . . ? C35 C34 C40 123.31(10) . . ? C33 C34 C40 119.59(10) . . ? C34 C35 C36 122.26(10) . . ? C34 C35 H48 119.6(8) . . ? C36 C35 H48 118.2(8) . . ? C35 C36 C31 120.41(9) . . ? C35 C36 C43 115.90(9) . . ? C31 C36 C43 123.68(9) . . ? C32 C37 C38 111.35(9) . . ? C32 C37 C39 111.89(9) . . ? C38 C37 C39 110.05(10) . . ? C32 C37 H49 107.8(8) . . ? C38 C37 H49 107.2(8) . . ? C39 C37 H49 108.4(8) . . ? C37 C38 H50 110.7(9) . . ? C37 C38 H51 111.8(9) . . ? H50 C38 H51 109.6(13) . . ? C37 C38 H52 110.7(9) . . ? H50 C38 H52 106.8(13) . . ? H51 C38 H52 107.1(12) . . ? C37 C39 H53 111.3(9) . . ? C37 C39 H54 113.5(10) . . ? H53 C39 H54 108.2(13) . . ? C37 C39 H55 111.4(9) . . ? H53 C39 H55 106.3(13) . . ? H54 C39 H55 105.6(13) . . ? C34 C40 C41 113.72(10) . . ? C34 C40 C42 110.44(10) . . ? C41 C40 C42 110.82(11) . . ? C34 C40 H56 106.6(8) . . ? C41 C40 H56 108.1(8) . . ? C42 C40 H56 106.7(8) . . ? C40 C41 H57 111.2(9) . . ? C40 C41 H58 110.7(9) . . ? H57 C41 H58 109.4(12) . . ? C40 C41 H59 110.0(10) . . ? H57 C41 H59 108.0(13) . . ? H58 C41 H59 107.5(13) . . ? C40 C42 H60 111.1(9) . . ? C40 C42 H61 113.7(10) . . ? H60 C42 H61 105.5(13) . . ? C40 C42 H62 111.2(10) . . ? H60 C42 H62 105.5(13) . . ? H61 C42 H62 109.4(14) . . ? C36 C43 C45 110.84(10) . . ? C36 C43 C44 112.22(9) . . ? C45 C43 C44 111.25(10) . . ? C36 C43 H63 108.0(8) . . ? C45 C43 H63 107.2(8) . . ? C44 C43 H63 107.1(8) . . ? C43 C44 H64 109.8(10) . . ? C43 C44 H65 111.4(9) . . ? H64 C44 H65 108.9(13) . . ? C43 C44 H66 108.8(9) . . ? H64 C44 H66 108.0(13) . . ? H65 C44 H66 109.9(13) . . ? C43 C45 H67 111.7(9) . . ? C43 C45 H68 111.0(11) . . ? H67 C45 H68 104.5(14) . . ? C43 C45 H69 112.5(9) . . ? H67 C45 H69 107.5(13) . . ? H68 C45 H69 109.3(14) . . ? C47 C46 C51 118.37(9) . . ? C47 C46 Si5 122.33(8) . . ? C51 C46 Si5 119.25(7) . . ? C48 C47 C46 119.71(10) . . ? C48 C47 C52 119.03(9) . . ? C46 C47 C52 121.19(9) . . ? C49 C48 C47 122.13(10) . . ? C49 C48 H70 119.7(8) . . ? C47 C48 H70 118.1(8) . . ? C48 C49 C50 117.68(10) . . ? C48 C49 C55 123.45(10) . . ? C50 C49 C55 118.82(10) . . ? C51 C50 C49 122.53(10) . . ? C51 C50 H71 119.4(8) . . ? C49 C50 H71 118.0(8) . . ? C50 C51 C46 119.54(10) . . ? C50 C51 C58 118.12(9) . . ? C46 C51 C58 122.29(9) . . ? C47 C52 C54 109.69(10) . . ? C47 C52 C53 114.31(11) . . ? C54 C52 C53 110.23(11) . . ? C47 C52 H86 108.4(8) . . ? C54 C52 H86 107.3(8) . . ? C53 C52 H86 106.6(8) . . ? C52 C53 H87 109.1(10) . . ? C52 C53 H88 111.9(9) . . ? H87 C53 H88 109.3(13) . . ? C52 C53 H89 111.9(9) . . ? H87 C53 H89 104.6(13) . . ? H88 C53 H89 109.8(13) . . ? C52 C54 H90 111.2(9) . . ? C52 C54 H91 112.5(9) . . ? H90 C54 H91 108.2(13) . . ? C52 C54 H92 110.8(10) . . ? H90 C54 H92 106.4(13) . . ? H91 C54 H92 107.4(14) . . ? C49 C55 C56 114.51(11) . . ? C49 C55 C57 109.83(10) . . ? C56 C55 C57 110.03(11) . . ? C49 C55 H79 107.6(9) . . ? C56 C55 H79 107.6(9) . . ? C57 C55 H79 107.0(9) . . ? C55 C56 H80 110.4(11) . . ? C55 C56 H81 112.1(10) . . ? H80 C56 H81 107.9(15) . . ? C55 C56 H82 108.1(10) . . ? H80 C56 H82 111.1(14) . . ? H81 C56 H82 107.3(14) . . ? C55 C57 H83 111.5(9) . . ? C55 C57 H84 109.9(10) . . ? H83 C57 H84 110.4(13) . . ? C55 C57 H85 108.6(10) . . ? H83 C57 H85 107.1(13) . . ? H84 C57 H85 109.2(14) . . ? C51 C58 C60 114.01(10) . . ? C51 C58 C59 109.41(9) . . ? C60 C58 C59 110.74(9) . . ? C51 C58 H72 107.4(8) . . ? C60 C58 H72 107.2(8) . . ? C59 C58 H72 107.8(8) . . ? C58 C59 H73 110.6(9) . . ? C58 C59 H74 110.8(8) . . ? H73 C59 H74 106.2(12) . . ? C58 C59 H75 110.5(9) . . ? H73 C59 H75 106.5(13) . . ? H74 C59 H75 112.2(13) . . ? C58 C60 H76 111.0(9) . . ? C58 C60 H77 111.0(8) . . ? H76 C60 H77 107.0(12) . . ? C58 C60 H78 112.5(9) . . ? H76 C60 H78 106.9(13) . . ? H77 C60 H78 108.3(12) . . ? N1 C61 C62 111.21(12) . . ? N1 C61 C63 111.53(11) . . ? C62 C61 C63 111.21(15) . . ? N1 C61 H93 105.8(9) . . ? C62 C61 H93 108.8(9) . . ? C63 C61 H93 108.1(9) . . ? C61 C62 H94 110.4(11) . . ? C61 C62 H95 110.8(12) . . ? H94 C62 H95 107.9(16) . . ? C61 C62 H96 111.5(13) . . ? H94 C62 H96 107.5(17) . . ? H95 C62 H96 108.7(17) . . ? C61 C63 H97 111.2(10) . . ? C61 C63 H98 110.0(11) . . ? H97 C63 H98 108.5(14) . . ? C61 C63 H99 109.9(11) . . ? H97 C63 H99 110.2(15) . . ? H98 C63 H99 107.0(15) . . ? N1 C64 C66 112.41(12) . . ? N1 C64 C65 111.69(11) . . ? C66 C64 C65 111.13(11) . . ? N1 C64 H100 105.5(9) . . ? C66 C64 H100 106.4(9) . . ? C65 C64 H100 109.4(9) . . ? C64 C65 H101 109.7(13) . . ? C64 C65 H102 109.2(10) . . ? H101 C65 H102 106.3(16) . . ? C64 C65 H103 110.7(11) . . ? H101 C65 H103 112.9(17) . . ? H102 C65 H103 107.9(15) . . ? C64 C66 H104 108.3(11) . . ? C64 C66 H105 110.8(10) . . ? H104 C66 H105 110.2(15) . . ? C64 C66 H106 112.0(11) . . ? H104 C66 H106 105.3(15) . . ? H105 C66 H106 110.1(15) . . ? _refine_diff_density_max 0.402 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.049 _shelx_res_file ; TITL sh4060 in P-1 sh4060.res created by SHELXL-2018/3 at 15:52:26 on 09-Sep-2019 CELL 0.71073 13.5006 13.5798 18.9871 98.387 92.938 106.305 ZERR 2.000 0.0006 0.0006 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H N B Si UNIT 132 212 2 2 10 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 8 BOND $H FMAP 2 PLAN -5 SIZE 0.12 0.377 0.652 ACTA TEMP -140.500 WGHT 0.044000 0.840600 FVAR 0.38461 SI1 5 0.475466 0.216898 0.145319 11.00000 0.01764 0.01436 = 0.01256 0.00045 0.00174 0.00528 SI2 5 0.454672 0.346465 0.254046 11.00000 0.01713 0.01322 = 0.01435 0.00108 0.00263 0.00682 SI3 5 0.457932 0.174730 0.259409 11.00000 0.01173 0.01130 = 0.01315 0.00121 0.00176 0.00328 SI4 5 0.640449 0.229412 0.290846 11.00000 0.01179 0.01029 = 0.01191 0.00058 0.00246 0.00338 SI5 5 0.614752 0.345316 0.215338 11.00000 0.01550 0.01065 = 0.01397 0.00205 0.00338 0.00372 N1 3 0.322727 0.352620 0.110955 11.00000 0.02370 0.01990 = 0.01927 0.00497 -0.00072 0.00849 B1 4 0.385803 0.314942 0.151979 11.00000 0.01962 0.01657 = 0.01776 0.00387 0.00273 0.00507 C1 1 0.345944 0.083105 0.296054 11.00000 0.01182 0.01294 = 0.01448 0.00097 0.00131 0.00342 C2 1 0.293572 -0.016777 0.257332 11.00000 0.01361 0.01401 = 0.01649 0.00020 0.00063 0.00408 C3 1 0.204484 -0.077241 0.281604 11.00000 0.01595 0.01565 = 0.02048 -0.00054 0.00109 0.00054 C4 1 0.165182 -0.044250 0.344074 11.00000 0.01519 0.01960 = 0.02249 0.00414 0.00439 0.00173 C5 1 0.220651 0.051786 0.383930 11.00000 0.01857 0.02100 = 0.01800 0.00101 0.00602 0.00430 C6 1 0.309037 0.115854 0.361357 11.00000 0.01516 0.01527 = 0.01555 0.00037 0.00191 0.00430 C7 1 0.329607 -0.060152 0.188221 11.00000 0.01514 0.01494 = 0.01790 -0.00266 0.00202 0.00309 C8 1 0.264705 -0.049414 0.123195 11.00000 0.02848 0.03026 = 0.01910 -0.00340 -0.00065 0.01247 C9 1 0.330572 -0.172519 0.186428 11.00000 0.02573 0.01642 = 0.03070 -0.00132 0.00544 0.00674 C10 1 0.063717 -0.108482 0.365978 11.00000 0.01869 0.02515 = 0.02579 0.00364 0.00557 -0.00091 C11 1 -0.021365 -0.055924 0.358015 11.00000 0.01770 0.04586 = 0.04966 0.01839 0.00833 0.00411 C12 1 0.073710 -0.131569 0.441726 11.00000 0.02631 0.04670 = 0.03625 0.01904 0.00840 0.00112 C13 1 0.359425 0.221442 0.407172 11.00000 0.01896 0.01618 = 0.01489 -0.00168 0.00319 0.00303 C14 1 0.290397 0.292437 0.400810 11.00000 0.02910 0.02179 = 0.02883 -0.00333 0.00335 0.01028 C15 1 0.386104 0.214988 0.485175 11.00000 0.03302 0.02588 = 0.01632 -0.00127 -0.00003 0.00372 C16 1 0.660955 0.254551 0.393041 11.00000 0.01221 0.01507 = 0.01302 0.00060 0.00283 0.00395 C17 1 0.680229 0.352381 0.437733 11.00000 0.01603 0.01526 = 0.01550 -0.00035 0.00274 0.00433 C18 1 0.690705 0.358923 0.511768 11.00000 0.02214 0.01782 = 0.01542 -0.00267 0.00180 0.00504 C19 1 0.684005 0.272824 0.544502 11.00000 0.01707 0.02394 = 0.01361 0.00059 0.00156 0.00564 C20 1 0.665461 0.177079 0.500747 11.00000 0.01695 0.01992 = 0.01575 0.00404 0.00255 0.00572 C21 1 0.653416 0.166474 0.426265 11.00000 0.01228 0.01562 = 0.01520 0.00174 0.00264 0.00375 C22 1 0.688077 0.453025 0.409313 11.00000 0.02666 0.01317 = 0.01512 -0.00118 0.00340 0.00519 C23 1 0.593946 0.490713 0.425731 11.00000 0.03108 0.01971 = 0.02313 -0.00326 0.00118 0.01140 C24 1 0.788686 0.538551 0.437908 11.00000 0.02984 0.01788 = 0.02840 -0.00139 0.00636 0.00262 C25 1 0.695951 0.283525 0.625399 11.00000 0.03082 0.02708 = 0.01275 0.00126 0.00034 0.00828 C26 1 0.612669 0.325679 0.658983 11.00000 0.04743 0.04054 = 0.01870 0.00523 0.01053 0.02080 C27 1 0.803709 0.351261 0.656956 11.00000 0.04052 0.04683 = 0.02317 0.00011 -0.00948 0.00511 C28 1 0.632516 0.057329 0.383498 11.00000 0.01959 0.01390 = 0.01527 0.00275 0.00231 0.00502 C29 1 0.533083 -0.018057 0.401098 11.00000 0.02438 0.01757 = 0.02324 0.00393 0.00393 0.00168 C30 1 0.725165 0.015223 0.393457 11.00000 0.02724 0.02271 = 0.02835 0.00168 0.00269 0.01360 C31 1 0.746080 0.170646 0.255696 11.00000 0.01412 0.01323 = 0.01334 0.00255 0.00374 0.00477 C32 1 0.729084 0.073906 0.209942 11.00000 0.01570 0.01331 = 0.01534 0.00182 0.00281 0.00499 C33 1 0.813299 0.041845 0.187429 11.00000 0.01883 0.01381 = 0.01949 -0.00039 0.00395 0.00689 C34 1 0.915485 0.100323 0.208112 11.00000 0.01684 0.01863 = 0.01995 0.00502 0.00554 0.00892 C35 1 0.931864 0.194401 0.253045 11.00000 0.01340 0.01921 = 0.02093 0.00156 0.00281 0.00450 C36 1 0.850054 0.231024 0.276359 11.00000 0.01469 0.01546 = 0.01638 0.00115 0.00283 0.00464 C37 1 0.621926 0.000932 0.182860 11.00000 0.01561 0.01352 = 0.02235 -0.00238 0.00261 0.00510 C38 1 0.597365 -0.001710 0.103162 11.00000 0.02613 0.02266 = 0.02393 -0.00307 -0.00247 0.00777 C39 1 0.609767 -0.109362 0.197840 11.00000 0.02388 0.01444 = 0.03664 0.00181 0.00338 0.00204 C40 1 1.002783 0.060969 0.179485 11.00000 0.01938 0.02073 = 0.02753 0.00352 0.00722 0.01098 C41 1 1.109169 0.121128 0.217315 11.00000 0.01819 0.03234 = 0.04019 0.00541 0.00486 0.01486 C42 1 1.001963 0.059147 0.098865 11.00000 0.02827 0.04289 = 0.02869 0.00125 0.01134 0.01798 C43 1 0.880934 0.336804 0.324743 11.00000 0.01335 0.01777 = 0.02227 -0.00402 0.00239 0.00219 C44 1 0.949576 0.422407 0.289241 11.00000 0.02251 0.01848 = 0.03704 -0.00276 0.00799 -0.00115 C45 1 0.933028 0.331224 0.396882 11.00000 0.02685 0.03555 = 0.02408 -0.00728 -0.00403 0.00777 C46 1 0.714759 0.442182 0.173564 11.00000 0.01633 0.01253 = 0.01569 0.00282 0.00284 0.00381 C47 1 0.739556 0.551029 0.196534 11.00000 0.01957 0.01363 = 0.01915 0.00167 0.00185 0.00556 C48 1 0.817686 0.618172 0.166364 11.00000 0.02045 0.01215 = 0.02578 0.00396 0.00123 0.00226 C49 1 0.872104 0.582052 0.113380 11.00000 0.01549 0.01847 = 0.02261 0.00792 0.00075 0.00164 C50 1 0.845536 0.475265 0.090087 11.00000 0.01890 0.01917 = 0.02023 0.00528 0.00622 0.00509 C51 1 0.769947 0.404891 0.119301 11.00000 0.01763 0.01518 = 0.01623 0.00360 0.00329 0.00514 C52 1 0.678883 0.596723 0.250778 11.00000 0.03103 0.01159 = 0.02178 0.00184 0.00850 0.00657 C53 1 0.741292 0.699914 0.296679 11.00000 0.05484 0.01571 = 0.03004 -0.00242 0.00992 0.00677 C54 1 0.581704 0.609054 0.212740 11.00000 0.03443 0.02588 = 0.03579 0.00863 0.01421 0.01747 C55 1 0.961412 0.652407 0.082356 11.00000 0.01702 0.02308 = 0.02594 0.00982 0.00137 -0.00042 C56 1 0.969038 0.767271 0.098355 11.00000 0.02290 0.02426 = 0.06705 0.02112 0.00571 0.00052 C57 1 1.063074 0.635356 0.107834 11.00000 0.01745 0.03569 = 0.04453 0.01546 0.00585 0.00538 C58 1 0.746198 0.290113 0.089160 11.00000 0.02382 0.01414 = 0.01766 0.00355 0.00884 0.00663 C59 1 0.675481 0.264846 0.019356 11.00000 0.02998 0.02130 = 0.01910 -0.00006 0.00466 0.00625 C60 1 0.842323 0.253823 0.078097 11.00000 0.03119 0.02373 = 0.02823 0.00717 0.01241 0.01506 C61 1 0.298507 0.316838 0.032411 11.00000 0.02967 0.03827 = 0.01855 0.00773 -0.00265 0.01374 C62 1 0.392290 0.356051 -0.007089 11.00000 0.04926 0.08640 = 0.02965 0.02624 0.01223 0.01789 C63 1 0.254937 0.199062 0.014347 11.00000 0.04220 0.04036 = 0.03175 -0.00771 -0.01225 0.01672 C64 1 0.277651 0.434884 0.142642 11.00000 0.03683 0.02572 = 0.02962 0.00525 -0.00357 0.01867 C65 1 0.159883 0.394567 0.140258 11.00000 0.04107 0.04204 = 0.05458 0.02163 0.01668 0.02728 C66 1 0.310540 0.532340 0.108565 11.00000 0.03940 0.02571 = 0.06423 0.01394 -0.00746 0.01310 H1 2 0.165256 -0.145394 0.253214 11.00000 0.02170 H2 2 0.195157 0.076105 0.427283 11.00000 0.02565 H3 2 0.399457 -0.018291 0.185552 11.00000 0.01754 H4 2 0.287286 -0.075168 0.078129 11.00000 0.03676 H5 2 0.192817 -0.087280 0.123577 11.00000 0.03741 H6 2 0.269009 0.023886 0.122407 11.00000 0.03062 H7 2 0.373540 -0.178283 0.229972 11.00000 0.03228 H8 2 0.261131 -0.219227 0.184716 11.00000 0.03858 H9 2 0.362179 -0.196131 0.142422 11.00000 0.03035 H10 2 0.043392 -0.175975 0.332985 11.00000 0.03257 H11 2 -0.035335 -0.046989 0.307699 11.00000 0.06148 H12 2 -0.086138 -0.095678 0.371893 11.00000 0.04314 H13 2 0.000808 0.014586 0.386974 11.00000 0.05387 H14 2 0.127488 -0.165305 0.449802 11.00000 0.04691 H15 2 0.007338 -0.179289 0.450627 11.00000 0.04493 H16 2 0.087583 -0.064635 0.476786 11.00000 0.05296 H17 2 0.425333 0.252827 0.388774 11.00000 0.01968 H18 2 0.273369 0.296143 0.350136 11.00000 0.03775 H19 2 0.226683 0.266967 0.421481 11.00000 0.03531 H20 2 0.322795 0.361307 0.424906 11.00000 0.03375 H21 2 0.322930 0.189504 0.508454 11.00000 0.04016 H22 2 0.423063 0.282646 0.510342 11.00000 0.02839 H23 2 0.430041 0.169390 0.489145 11.00000 0.04129 H24 2 0.704276 0.426064 0.541493 11.00000 0.02090 H25 2 0.661767 0.115437 0.522533 11.00000 0.01984 H26 2 0.688557 0.439430 0.358464 11.00000 0.01693 H27 2 0.596693 0.554812 0.406118 11.00000 0.03643 H28 2 0.590159 0.504912 0.477638 11.00000 0.02928 H29 2 0.530456 0.439539 0.407343 11.00000 0.03324 H30 2 0.795805 0.554653 0.489922 11.00000 0.03248 H31 2 0.849540 0.520149 0.424886 11.00000 0.04004 H32 2 0.793256 0.604634 0.418306 11.00000 0.04021 H33 2 0.686692 0.214018 0.636853 11.00000 0.02331 H34 2 0.618198 0.394400 0.650363 11.00000 0.04275 H35 2 0.620368 0.328564 0.711753 11.00000 0.04080 H36 2 0.542322 0.282720 0.639378 11.00000 0.04073 H37 2 0.858143 0.325065 0.635371 11.00000 0.05405 H38 2 0.814733 0.421581 0.649192 11.00000 0.04277 H39 2 0.810068 0.355754 0.711185 11.00000 0.05323 H40 2 0.623553 0.061602 0.333071 11.00000 0.01338 H41 2 0.517556 -0.085001 0.368472 11.00000 0.03875 H42 2 0.540411 -0.029999 0.449922 11.00000 0.02624 H43 2 0.475214 0.007927 0.394305 11.00000 0.02721 H44 2 0.787220 0.061297 0.377495 11.00000 0.02910 H45 2 0.711218 -0.053738 0.364931 11.00000 0.03540 H46 2 0.739195 0.009793 0.443047 11.00000 0.03290 H47 2 0.800208 -0.023729 0.155788 11.00000 0.02011 H48 2 1.000666 0.236117 0.268957 11.00000 0.02010 H49 2 0.572587 0.027274 0.207242 11.00000 0.01713 H50 2 0.602997 0.066615 0.093464 11.00000 0.03503 H51 2 0.526843 -0.048760 0.085161 11.00000 0.03373 H52 2 0.647607 -0.027753 0.074889 11.00000 0.03884 H53 2 0.542163 -0.154440 0.181082 11.00000 0.03313 H54 2 0.622921 -0.112424 0.248217 11.00000 0.04483 H55 2 0.659168 -0.140660 0.172934 11.00000 0.04127 H56 2 0.988115 -0.010595 0.186914 11.00000 0.02227 H57 2 1.129969 0.194423 0.208467 11.00000 0.03618 H58 2 1.109983 0.120857 0.269968 11.00000 0.03546 H59 2 1.160264 0.089010 0.200050 11.00000 0.04462 H60 2 1.015422 0.129671 0.087378 11.00000 0.03695 H61 2 0.936422 0.019545 0.072381 11.00000 0.04086 H62 2 1.055097 0.033970 0.080397 11.00000 0.03819 H63 2 0.818983 0.355640 0.333977 11.00000 0.01778 H64 2 0.963164 0.489328 0.320108 11.00000 0.03933 H65 2 0.916465 0.425904 0.242854 11.00000 0.03939 H66 2 1.015547 0.408343 0.282974 11.00000 0.04063 H67 2 0.998344 0.311152 0.391409 11.00000 0.03972 H68 2 0.954932 0.399109 0.427185 11.00000 0.05264 H69 2 0.887096 0.280054 0.422763 11.00000 0.03886 H70 2 0.833078 0.690416 0.182750 11.00000 0.02399 H71 2 0.884247 0.449387 0.053394 11.00000 0.02420 H72 2 0.707868 0.250963 0.123746 11.00000 0.01800 H73 2 0.615739 0.288749 0.026279 11.00000 0.03209 H74 2 0.648773 0.188021 0.003049 11.00000 0.03200 H75 2 0.710539 0.299993 -0.016153 11.00000 0.03646 H76 2 0.887678 0.270819 0.121653 11.00000 0.03507 H77 2 0.823126 0.177336 0.063517 11.00000 0.02762 H78 2 0.882686 0.285995 0.042189 11.00000 0.03287 H79 2 0.951221 0.630955 0.029463 11.00000 0.03444 H80 2 0.989220 0.794068 0.148972 11.00000 0.05216 H81 2 0.903757 0.780158 0.086042 11.00000 0.04601 H82 2 1.022451 0.805986 0.067413 11.00000 0.05034 H83 2 1.123880 0.682156 0.088869 11.00000 0.03993 H84 2 1.060282 0.561069 0.093165 11.00000 0.04537 H85 2 1.073352 0.652948 0.160068 11.00000 0.04171 H86 2 0.656349 0.548229 0.283208 11.00000 0.01839 H87 2 0.700313 0.718848 0.334043 11.00000 0.04166 H88 2 0.806515 0.695771 0.318325 11.00000 0.03587 H89 2 0.754264 0.756878 0.269614 11.00000 0.03784 H90 2 0.599353 0.661689 0.182137 11.00000 0.03550 H91 2 0.540450 0.546065 0.184300 11.00000 0.03547 H92 2 0.539185 0.631561 0.246522 11.00000 0.04522 H93 2 0.245138 0.346952 0.018052 11.00000 0.03032 H94 2 0.445619 0.327618 0.006071 11.00000 0.05363 H95 2 0.420272 0.433838 0.004751 11.00000 0.06446 H96 2 0.375777 0.336176 -0.058751 11.00000 0.08153 H97 2 0.306031 0.164212 0.029893 11.00000 0.04466 H98 2 0.193842 0.176241 0.037623 11.00000 0.04973 H99 2 0.234958 0.177956 -0.037236 11.00000 0.06176 H100 2 0.307220 0.454774 0.191764 11.00000 0.03664 H101 2 0.141527 0.337935 0.164736 11.00000 0.07021 H102 2 0.133987 0.448516 0.165774 11.00000 0.04550 H103 2 0.126894 0.377342 0.088947 11.00000 0.05932 H104 2 0.283387 0.584602 0.134046 11.00000 0.05236 H105 2 0.383839 0.557445 0.110570 11.00000 0.04610 H106 2 0.280010 0.520567 0.059280 11.00000 0.05166 HKLF 4 REM sh4060 in P-1 REM wR2 = 0.096503, GooF = S = 1.02761, Restrained GooF = 1.02761 for all data REM R1 = 0.037286 for 16525 Fo > 4sig(Fo) and 0.052714 for all 20730 data REM 1082 parameters refined using 0 restraints END WGHT 0.0441 0.8408 REM Highest difference peak 0.402, deepest hole -0.228, 1-sigma level 0.049 Q1 1 0.3218 0.0314 0.2764 11.00000 0.05 0.40 Q2 1 0.7773 0.0724 0.1949 11.00000 0.05 0.40 Q3 1 0.2774 0.0734 0.3773 11.00000 0.05 0.39 Q4 1 0.8000 0.2072 0.2612 11.00000 0.05 0.39 Q5 1 0.1988 0.0019 0.3638 11.00000 0.05 0.39 ; _shelx_res_checksum 27151 _shelx_hkl_file ; -1 0 0 1750.12 35.5005 1 1 0 0 1782.20 35.2161 9 1 0 0 1755.43 34.4778 1 1 0 0 1668.09 35.2049 2 1 0 0 1795.97 36.2908 1 1 0 0 1758.60 35.3968 8 -2 0 0 2094.30 41.2285 2 -2 0 0 1955.01 41.0963 2 -2 0 0 2088.71 41.7300 1 -2 0 0 2072.41 41.3752 8 -2 0 0 2154.40 41.1520 9 2 0 0 2031.72 41.3720 8 2 0 0 2106.39 42.2881 9 2 0 0 2116.45 41.9053 2 2 0 0 2145.52 41.3815 1 -3 0 0 4494.29 91.3351 9 -3 0 0 4406.69 90.9072 2 -3 0 0 4709.84 89.9483 8 -3 0 0 4572.07 90.7849 1 -3 0 0 4572.73 90.8379 2 3 0 0 4386.58 92.4605 2 3 0 0 4652.11 92.2753 9 3 0 0 4664.24 92.4215 8 -4 0 0 161.534 4.34867 1 -4 0 0 160.807 4.53550 8 -4 0 0 166.770 4.16464 9 -4 0 0 157.643 4.10903 2 -4 0 0 166.313 4.30060 2 4 0 0 153.415 4.47970 1 4 0 0 158.027 4.55741 8 4 0 0 160.819 4.12231 2 4 0 0 158.709 4.18959 9 -5 0 0 143.580 4.47131 8 -5 0 0 138.557 4.03327 2 -5 0 0 140.657 3.93223 9 -5 0 0 133.402 4.11595 1 -5 0 0 137.849 3.90726 2 5 0 0 136.705 4.37375 1 5 0 0 139.532 4.40276 8 5 0 0 138.481 4.10300 2 5 0 0 137.755 3.92033 2 -6 0 0 290.158 7.24311 9 -6 0 0 291.465 7.21056 2 -6 0 0 301.027 7.61200 1 -6 0 0 293.093 7.90147 8 -6 0 0 298.304 7.43956 2 6 0 0 282.358 7.80334 1 6 0 0 290.148 7.26126 2 6 0 0 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9 6 2 -3 151.325 4.91190 4 -6 -2 3 149.004 5.08322 8 -6 -2 3 151.392 4.38456 2 -6 -2 3 160.021 4.64448 9 -6 -2 3 150.340 4.81842 1 -6 -2 3 148.207 4.76684 4 5 2 -3 1603.79 34.4869 1 5 2 -3 1662.96 33.9980 9 5 2 -3 1638.82 34.2564 4 5 2 -3 1740.43 34.0857 2 5 2 -3 1680.31 34.2145 2 -5 -2 3 1670.42 33.6678 2 -5 -2 3 1667.26 33.9394 9 -5 -2 3 1658.74 34.1721 4 -5 -2 3 1652.39 33.6332 2 -5 -2 3 1613.13 34.1658 1 -5 -2 3 1696.31 34.6315 8 4 2 -3 59.3874 2.27219 9 4 2 -3 59.3405 2.42370 4 4 2 -3 55.5334 2.26016 2 4 2 -3 55.6044 2.49921 1 4 2 -3 61.5733 2.33327 2 -4 -2 3 60.7354 2.06453 2 -4 -2 3 59.9851 2.27083 9 -4 -2 3 62.0256 2.42205 4 -4 -2 3 58.5149 2.05971 2 -4 -2 3 59.3043 2.35828 1 3 2 -3 27.7498 1.36736 2 3 2 -3 25.3737 1.34454 2 3 2 -3 24.7711 1.41132 4 3 2 -3 24.9426 1.37374 9 3 2 -3 25.2588 1.51760 1 -3 -2 3 26.3726 1.35969 9 -3 -2 3 28.6175 1.16712 2 -3 -2 3 26.3871 1.45556 1 -3 -2 3 27.4846 1.20025 2 2 2 -3 1980.67 39.3440 2 2 2 -3 2031.93 39.4751 9 2 2 -3 2002.72 39.5188 4 2 2 -3 1880.91 39.5786 1 2 2 -3 1971.45 39.3348 2 -2 -2 3 1956.02 39.0048 2 -2 -2 3 2074.46 39.0813 2 -2 -2 3 1962.84 39.5138 1 -2 -2 3 1922.41 39.3094 9 1 2 -3 2651.89 55.0399 2 1 2 -3 2752.09 54.3206 1 1 2 -3 2687.81 54.1637 9 1 2 -3 2790.80 54.0578 2 1 2 -3 2805.68 54.3042 1 1 2 -3 2744.86 53.8870 7 -1 -2 3 2768.44 54.2597 1 -1 -2 3 2648.81 54.3806 2 -1 -2 3 2704.66 54.0319 9 -1 -2 3 2861.49 54.6976 6 0 2 -3 1803.00 36.0392 2 0 2 -3 1861.13 36.3519 1 0 2 -3 1778.72 36.6448 5 0 2 -3 1784.20 36.3366 1 0 2 -3 1854.32 35.9958 7 0 2 -3 1795.24 36.0735 2 0 2 -3 1851.41 36.2334 9 0 -2 3 1876.18 36.1301 7 0 -2 3 1757.50 36.0674 9 0 -2 3 1869.72 36.7009 6 0 -2 3 1855.58 36.3206 1 0 -2 3 1808.12 36.5714 8 0 -2 3 1826.58 36.4188 2 0 -2 3 1807.16 36.0620 2 -1 2 -3 1098.90 22.3554 7 -1 2 -3 1132.34 22.4563 2 -1 2 -3 1138.28 23.0677 1 -1 2 -3 1112.92 22.7120 1 -1 2 -3 1066.64 22.8765 8 -1 2 -3 1116.84 22.4682 2 -1 2 -3 1127.88 22.9407 5 -1 2 -3 1115.12 22.6037 9 1 -2 3 1095.85 22.8877 5 1 -2 3 1125.35 22.9085 8 1 -2 3 1125.49 22.6800 1 1 -2 3 1089.27 22.2768 2 1 -2 3 1150.89 22.2441 7 1 -2 3 1140.12 22.9543 6 1 -2 3 1148.46 22.3065 2 -2 2 -3 1324.94 26.6756 5 -2 2 -3 1306.70 26.2921 2 -2 2 -3 1268.97 26.3092 2 -2 2 -3 1329.32 26.1916 7 -2 2 -3 1285.02 26.7434 8 -2 2 -3 1254.39 26.4513 1 2 -2 3 1317.92 26.7057 8 2 -2 3 1343.77 26.2005 2 2 -2 3 1296.22 26.1628 2 2 -2 3 1306.40 26.6695 5 2 -2 3 1330.25 26.0912 7 2 -2 3 1297.23 26.5196 1 -3 2 -3 161.805 4.36250 1 -3 2 -3 161.273 4.57746 8 -3 2 -3 165.845 4.29015 2 3 -2 3 163.765 4.12473 2 3 -2 3 156.740 4.39725 1 3 -2 3 163.451 4.13198 2 3 -2 3 159.595 4.50855 8 -4 2 -3 33.8884 1.72772 2 -4 2 -3 31.6710 1.79340 1 -4 2 -3 32.2257 1.90779 8 4 -2 3 33.5635 1.91561 3 4 -2 3 38.0004 1.68510 2 4 -2 3 33.0558 1.86327 1 4 -2 3 32.5113 1.59615 2 4 -2 3 34.6326 1.91178 8 -5 2 -3 9.49200 1.33573 3 -5 2 -3 10.7767 1.46254 8 -5 2 -3 11.5496 1.23196 2 -5 2 -3 13.5266 1.50262 1 5 -2 3 14.6779 1.36219 2 5 -2 3 11.8136 1.50207 1 5 -2 3 11.3089 1.44665 3 5 -2 3 12.9870 1.48345 8 -6 2 -3 142.206 4.28927 2 -6 2 -3 135.376 4.69565 3 -6 2 -3 144.068 4.67082 1 -6 2 -3 147.251 4.64156 2 -6 2 -3 150.270 5.11107 8 6 -2 3 136.765 4.81997 8 6 -2 3 130.848 4.74234 3 6 -2 3 145.789 4.46135 2 6 -2 3 137.929 4.76988 1 -7 2 -3 163.590 5.41047 1 -7 2 -3 163.491 4.98731 2 -7 2 -3 176.021 5.43359 2 -7 2 -3 175.380 5.97267 8 7 -2 3 166.785 5.65820 3 7 -2 3 177.455 5.78989 8 7 -2 3 169.587 5.71249 1 7 -2 3 175.563 5.28916 2 -8 2 -3 2.70807 0.97066 2 -8 2 -3 0.87108 0.86766 2 -8 2 -3 0.89962 1.07486 1 -8 2 -3 1.64005 1.28487 8 8 -2 3 1.18070 1.06332 3 8 -2 3 2.63162 0.94251 2 8 -2 3 1.46166 1.08728 8 8 -2 3 3.52815 1.32441 1 -9 2 -3 38.5295 3.15530 8 -9 2 -3 33.1834 2.64935 1 -9 2 -3 32.3008 2.27084 2 -9 2 -3 32.0906 2.44840 2 9 -2 3 31.3583 2.96623 3 9 -2 3 26.3574 2.60606 1 9 -2 3 33.3633 2.40640 2 9 -2 3 28.5632 2.78266 8 -10 2 -3 49.1724 3.31937 1 -10 2 -3 48.0200 3.06399 2 -10 2 -3 55.5230 3.78403 8 -10 2 -3 47.5531 2.92111 2 10 -2 3 53.8304 3.59000 3 10 -2 3 48.0103 3.02446 2 10 -2 3 49.7259 3.47837 8 10 -2 3 48.4570 3.59831 1 -11 2 -3 65.4543 3.75585 2 -11 2 -3 62.4956 4.27419 8 -11 2 -3 63.9271 3.85184 1 11 -2 3 65.7590 4.20707 3 11 -2 3 70.8961 4.40795 1 11 -2 3 67.8318 4.27904 8 -12 2 -3 91.3782 4.90581 1 12 -2 3 87.0331 5.04469 8 12 -2 3 83.5165 4.88674 1 -13 2 -3 20.9667 2.99627 9 -13 2 -3 18.1572 2.74192 1 13 -2 3 13.4766 2.68872 8 13 -2 3 14.7128 3.04497 1 -14 2 -3 111.972 5.84690 1 -14 2 -3 108.499 5.77393 4 -14 2 -3 104.185 5.94416 9 14 -2 3 109.447 6.33277 1 -15 2 -3 27.2769 3.77618 9 -15 2 -3 28.4605 3.62435 4 -15 2 -3 30.7537 3.82249 1 15 -2 3 23.0499 3.74043 1 -16 2 -3 16.8660 3.00362 1 -16 2 -3 10.6460 2.73387 9 16 -2 3 18.7147 3.61223 1 -17 2 -3 16.7651 3.29986 9 17 -2 3 17.5890 3.77573 1 -18 2 -3 5.06698 2.65088 9 18 -2 3 13.5746 3.67058 1 18 1 -3 1.90275 3.30719 1 -18 -1 3 4.30617 1.98964 9 17 1 -3 28.6891 4.72689 1 -17 -1 3 32.9048 3.65105 9 16 1 -3 48.6440 5.42991 1 -16 -1 3 39.8166 3.87488 9 15 1 -3 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31.4842 2.41814 8 -8 -1 3 32.5334 1.90521 2 -8 -1 3 33.9419 2.31748 4 -8 -1 3 31.6846 2.23567 1 -8 -1 3 30.0469 2.00922 9 7 1 -3 13.8865 1.85429 1 7 1 -3 13.5711 1.49247 2 7 1 -3 14.6935 1.53607 9 7 1 -3 14.6766 1.63109 2 -7 -1 3 13.9734 1.58376 1 -7 -1 3 12.9802 1.38910 9 -7 -1 3 16.6290 1.67664 4 -7 -1 3 14.1988 1.32106 2 -7 -1 3 15.0024 1.75303 8 6 1 -3 552.033 12.7152 2 6 1 -3 557.585 12.5934 2 6 1 -3 560.292 12.5700 9 6 1 -3 554.533 13.1748 1 -6 -1 3 557.472 12.7210 1 -6 -1 3 568.997 12.7476 4 -6 -1 3 550.304 13.0812 8 -6 -1 3 569.574 12.1824 2 -6 -1 3 556.979 12.3831 9 5 1 -3 79.4296 2.80928 2 5 1 -3 83.3798 3.18272 1 5 1 -3 78.4328 2.77550 9 5 1 -3 78.7544 2.82424 2 5 1 -3 77.6776 2.95439 4 -5 -1 3 82.0822 2.44182 2 -5 -1 3 77.3097 3.02873 8 -5 -1 3 81.8768 2.90468 4 -5 -1 3 79.2999 2.46949 2 -5 -1 3 78.6629 2.67811 9 -5 -1 3 79.7118 2.88136 1 4 1 -3 542.036 11.7846 9 4 1 -3 552.596 11.7947 2 4 1 -3 542.031 11.8735 2 4 1 -3 542.109 12.1925 1 4 1 -3 556.417 12.0432 4 -4 -1 3 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2 -6 -2 -3 46.6510 2.66732 4 6 2 3 42.9848 2.33762 2 6 2 3 46.9600 2.29045 2 6 2 3 40.6215 2.67083 1 6 2 3 41.2765 2.24173 7 -7 -2 -3 231.495 7.01108 2 -7 -2 -3 234.255 7.20274 4 -7 -2 -3 238.804 7.51090 8 -7 -2 -3 249.054 7.37452 1 -7 -2 -3 240.076 6.88534 2 7 2 3 236.934 6.87988 2 7 2 3 246.085 7.55022 1 7 2 3 236.081 6.77540 7 7 2 3 236.231 6.62267 2 -8 -2 -3 3.87344 1.23319 4 -8 -2 -3 4.33507 1.45296 8 -8 -2 -3 3.18002 1.37238 1 -8 -2 -3 2.00365 0.96074 2 -8 -2 -3 2.83426 1.16116 2 8 2 3 1.42438 0.84649 2 8 2 3 6.12247 1.71505 1 8 2 3 2.19925 0.88210 7 -9 -2 -3 21.9199 2.34018 2 -9 -2 -3 15.3219 1.80816 2 -9 -2 -3 14.7005 2.11641 4 -9 -2 -3 17.9610 2.48303 1 -9 -2 -3 17.6036 2.41185 8 9 2 3 14.5431 1.76840 7 9 2 3 17.9621 1.89148 2 9 2 3 15.5980 2.30290 3 9 2 3 17.6572 2.55987 1 -10 -2 -3 147.281 6.42145 8 -10 -2 -3 148.728 6.09165 4 -10 -2 -3 151.837 6.26107 1 -10 -2 -3 152.799 8.23474 2 -10 -2 -3 141.725 6.12885 2 10 2 3 150.170 6.39427 1 10 2 3 149.937 5.58738 7 -11 -2 -3 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3.07558 3 -12 3 3 38.5334 2.42657 9 -12 3 3 38.8406 2.92623 9 -12 3 3 41.7320 3.08631 1 -12 3 3 42.3859 3.03214 4 11 -3 -3 193.933 6.38387 2 11 -3 -3 207.408 7.48082 1 11 -3 -3 187.821 6.35211 3 11 -3 -3 199.713 7.08927 8 11 -3 -3 191.499 6.65986 2 -11 3 3 197.372 6.37570 4 -11 3 3 186.547 5.56741 9 -11 3 3 200.867 6.41763 1 -11 3 3 191.327 6.21054 9 -11 3 3 190.981 7.30935 8 10 -3 -3 0.93648 0.91673 3 10 -3 -3 1.72854 1.00707 2 10 -3 -3 -0.1002 0.82865 2 10 -3 -3 0.87849 1.10951 8 10 -3 -3 -1.8592 1.05460 1 -10 3 3 0.97822 1.03647 1 -10 3 3 -0.2864 1.08719 8 -10 3 3 0.74712 0.97341 9 -10 3 3 1.50498 0.92880 4 -10 3 3 2.21089 0.78249 9 9 -3 -3 2.52157 1.06834 2 9 -3 -3 2.54344 0.96577 3 9 -3 -3 2.98064 0.89910 2 9 -3 -3 0.47418 1.12998 1 9 -3 -3 1.92018 1.03157 8 -9 3 3 2.04209 0.96867 9 -9 3 3 1.20879 1.09347 8 -9 3 3 1.31447 0.69129 9 -9 3 3 1.86317 0.94970 1 8 -3 -3 21.0864 1.68907 3 8 -3 -3 23.7561 1.80617 2 8 -3 -3 23.3227 2.35663 1 8 -3 -3 19.1056 1.86029 2 8 -3 -3 26.3179 2.33176 8 -8 3 3 23.4036 1.82548 9 -8 3 3 22.1348 1.82146 1 -8 3 3 21.0339 1.44581 9 7 -3 -3 17.8045 1.83131 8 7 -3 -3 15.9893 1.86173 1 7 -3 -3 12.0465 1.37482 2 7 -3 -3 14.3292 1.29921 2 7 -3 -3 14.4580 1.33413 3 -7 3 3 14.0338 1.34486 9 -7 3 3 15.9276 1.47828 1 -7 3 3 13.9417 1.11848 9 6 -3 -3 134.036 4.47178 8 6 -3 -3 138.107 3.84209 3 6 -3 -3 135.392 3.84579 2 6 -3 -3 136.119 4.16814 2 6 -3 -3 133.582 4.53273 1 -6 3 3 135.346 3.47421 9 -6 3 3 141.546 3.77654 9 -6 3 3 131.421 3.93023 1 -6 3 3 132.250 4.58561 8 5 -3 -3 2067.51 41.1332 8 5 -3 -3 1962.01 40.5025 2 5 -3 -3 1982.95 40.2031 2 5 -3 -3 2009.13 41.0715 1 -5 3 3 1993.92 41.2338 8 -5 3 3 2039.61 39.8255 9 -5 3 3 2000.82 40.1047 3 -5 3 3 2069.43 40.4204 1 -5 3 3 2012.91 40.0085 9 4 -3 -3 57.8203 2.33629 1 4 -3 -3 59.2799 2.35518 8 4 -3 -3 59.6720 1.78906 2 4 -3 -3 61.2624 1.96193 2 -4 3 3 60.2123 1.44771 9 -4 3 3 59.4082 1.75894 3 -4 3 3 58.7214 2.48117 8 -4 3 3 59.9581 1.95239 1 -4 3 3 59.2458 1.49971 9 3 -3 -3 118.489 2.84022 2 3 -3 -3 121.103 3.45062 1 3 -3 -3 125.806 3.31803 1 3 -3 -3 126.080 2.79330 2 3 -3 -3 120.911 3.60143 8 3 -3 -3 123.679 3.66090 5 -3 3 3 119.450 3.61808 8 2 -3 -3 437.892 9.79239 5 2 -3 -3 437.762 9.86990 8 2 -3 -3 441.389 9.59501 1 2 -3 -3 457.773 9.56349 1 -2 3 3 440.200 9.24108 4 1 -3 -3 235.429 4.91498 2 1 -3 -3 234.405 5.41874 1 1 -3 -3 236.911 5.50187 1 1 -3 -3 231.275 5.55014 5 -1 3 3 234.306 5.55915 5 -1 3 3 232.036 5.18800 4 -1 3 3 229.623 5.37048 6 0 -3 -3 430.200 9.92364 1 0 -3 -3 432.289 9.01978 2 0 -3 -3 438.060 9.00142 7 0 -3 -3 440.032 9.41558 1 0 -3 -3 427.344 9.36982 4 0 -3 -3 414.148 9.09233 2 0 3 3 430.568 9.32671 6 0 3 3 441.475 9.39075 1 0 3 3 437.357 9.37097 1 0 3 3 420.544 9.44529 5 0 3 3 429.508 9.21612 4 -1 -3 -3 24.0145 1.16883 7 -1 -3 -3 25.5020 1.26800 2 -1 -3 -3 24.6799 1.37007 1 -1 -3 -3 23.5109 1.20044 2 -1 -3 -3 25.4074 1.36056 4 1 3 3 24.2936 1.41425 1 1 3 3 24.9466 0.89768 2 1 3 3 24.3583 0.95071 2 1 3 3 23.4691 0.85887 7 1 3 3 23.5598 1.07010 9 -2 -3 -3 851.011 18.0814 2 -2 -3 -3 825.608 18.1363 4 -2 -3 -3 847.736 18.1574 1 -2 -3 -3 866.227 17.8958 2 -2 -3 -3 858.863 17.9278 7 2 3 3 852.286 17.5350 7 2 3 3 859.860 17.4723 2 2 3 3 861.055 18.2451 1 2 3 3 881.471 17.6780 2 -3 -3 -3 422.627 9.74830 4 -3 -3 -3 422.042 9.53226 7 -3 -3 -3 389.220 9.66105 1 -3 -3 -3 390.285 9.57618 2 -3 -3 -3 422.185 9.47336 2 3 3 3 418.672 9.05349 2 3 3 3 407.085 9.79098 1 3 3 3 401.229 9.13303 7 3 3 3 401.160 9.25663 2 -4 -3 -3 17.8405 1.75535 1 -4 -3 -3 23.1444 1.86242 7 -4 -3 -3 18.8061 1.83435 4 4 3 3 19.4315 1.50908 2 4 3 3 18.3218 1.44889 7 4 3 3 19.6614 1.88931 1 4 3 3 18.9538 1.43381 2 -5 -3 -3 -0.1771 0.75478 2 -5 -3 -3 0.02664 0.61375 7 -5 -3 -3 0.31843 0.79223 4 -5 -3 -3 -0.7286 0.78028 8 -5 -3 -3 0.17698 0.88703 1 -5 -3 -3 0.48272 0.58565 2 5 3 3 0.45403 0.60896 7 5 3 3 0.98363 0.66664 2 5 3 3 -1.0309 0.79360 1 5 3 3 0.51864 0.61102 2 -6 -3 -3 54.7995 3.19433 8 -6 -3 -3 53.3689 2.80450 2 -6 -3 -3 47.7871 2.92914 1 -6 -3 -3 50.5537 2.92821 4 6 3 3 52.9138 2.63176 2 6 3 3 50.9107 2.46198 2 6 3 3 49.5791 2.52825 7 6 3 3 50.9507 3.06168 1 -7 -3 -3 8.62128 1.56764 1 -7 -3 -3 11.0040 1.57998 2 -7 -3 -3 10.2761 1.50322 2 -7 -3 -3 11.8108 1.88106 8 -7 -3 -3 12.3553 1.82484 4 7 3 3 14.1396 1.67835 7 7 3 3 12.4778 1.53064 2 7 3 3 10.7252 1.85237 1 -8 -3 -3 54.2397 3.17413 2 -8 -3 -3 49.3352 3.41112 1 -8 -3 -3 57.6203 3.43579 4 -8 -3 -3 47.8177 3.37778 8 -8 -3 -3 57.4379 3.21696 2 8 3 3 61.7547 3.77824 1 8 3 3 54.9487 2.90798 2 8 3 3 59.0286 3.06922 7 -9 -3 -3 9.05326 1.82287 2 -9 -3 -3 8.19505 1.90123 4 -9 -3 -3 9.31587 2.06896 8 -9 -3 -3 9.81843 1.82013 2 -9 -3 -3 7.47810 1.96338 1 9 3 3 9.58120 1.70994 2 9 3 3 6.14192 1.86510 1 9 3 3 11.2715 1.80957 7 -10 -3 -3 13.6939 2.33719 1 -10 -3 -3 11.1230 2.10353 4 10 3 3 10.4032 1.60310 7 10 3 3 12.8155 2.54230 1 -11 -3 -3 19.2891 2.78566 4 -11 -3 -3 21.1107 2.91478 1 11 3 3 20.0170 3.06962 1 -12 -3 -3 14.7011 2.66184 4 -12 -3 -3 13.0324 2.74112 1 12 3 3 15.4976 2.88439 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3.64509 7 10 -5 9 93.3390 4.87542 1 10 -5 9 93.0887 5.02865 8 -11 5 -9 238.286 9.08177 3 -11 5 -9 232.594 8.59196 1 -11 5 -9 248.049 9.09389 9 11 -5 9 236.374 8.59492 1 11 -5 9 240.017 7.05659 7 11 -5 9 236.174 7.08758 7 11 -5 9 253.046 9.09439 8 -12 5 -9 19.3576 3.19812 9 -12 5 -9 12.1535 2.72528 1 12 -5 9 11.2871 1.65770 7 12 -5 9 13.4810 2.78550 8 12 -5 9 16.4473 1.91653 7 12 -5 9 13.9118 2.63291 1 -13 5 -9 164.879 7.77197 9 -13 5 -9 163.602 7.32778 1 13 -5 9 149.795 7.41792 8 13 -5 9 155.079 5.74165 7 13 -5 9 151.848 5.75874 7 13 -5 9 157.841 7.22480 1 -14 5 -9 49.6631 5.02317 9 -14 5 -9 40.7595 4.32876 1 14 -5 9 43.2133 3.15153 7 14 -5 9 38.1291 3.01007 7 14 -5 9 37.4681 4.26261 8 -15 5 -9 12.1480 3.02164 9 -15 5 -9 13.9601 2.95396 1 15 -5 9 9.65540 3.15712 8 15 -5 9 9.23557 1.74944 7 15 -5 9 13.7794 2.22200 7 -16 5 -9 34.2007 4.55339 1 -16 5 -9 32.8456 4.81139 9 16 -5 9 27.5801 2.96733 7 -17 5 -9 0.94178 2.76426 1 -17 5 -9 1.34059 2.48689 9 17 -5 9 1.62866 1.48318 7 -18 5 -9 8.52752 3.26353 1 -18 5 -9 9.42124 3.48739 9 18 -5 9 6.59802 1.85052 7 16 4 -9 16.5910 3.89395 1 15 4 -9 2.03504 2.42470 1 14 4 -9 16.8463 3.61191 1 13 4 -9 2.39549 2.29411 1 12 4 -9 -2.1539 1.59280 1 11 4 -9 43.4199 4.31024 1 11 4 -9 45.5124 3.54700 2 10 4 -9 13.2752 2.47613 1 10 4 -9 18.4467 2.20110 2 9 4 -9 184.865 6.61508 2 9 4 -9 201.152 7.39573 1 9 4 -9 187.942 6.53089 2 8 4 -9 33.3054 2.58141 2 8 4 -9 32.9425 2.64667 2 8 4 -9 36.3129 3.32017 1 -8 -4 9 35.5400 2.78502 8 7 4 -9 50.3961 2.86277 9 7 4 -9 49.3307 3.27827 1 7 4 -9 51.5081 2.88221 2 7 4 -9 55.2274 3.01982 2 -7 -4 9 52.3104 3.10687 8 6 4 -9 99.5228 3.86229 9 6 4 -9 96.2556 3.74156 2 6 4 -9 92.6678 4.18513 1 6 4 -9 96.2183 3.77929 2 5 4 -9 24.4786 1.76336 2 5 4 -9 25.6350 1.98544 9 5 4 -9 25.5441 1.92654 2 5 4 -9 18.8678 1.82040 4 5 4 -9 28.4689 2.17165 1 -5 -4 9 27.0830 1.75476 1 4 4 -9 3.67992 0.95136 9 4 4 -9 4.96611 1.14494 1 4 4 -9 3.41240 0.80560 2 4 4 -9 2.25408 0.84117 2 -4 -4 9 4.67513 0.85898 1 3 4 -9 72.4863 2.70488 2 3 4 -9 73.1026 2.90560 9 3 4 -9 69.0630 2.51681 2 3 4 -9 71.8183 3.06369 1 -3 -4 9 75.1708 4.03052 6 2 4 -9 13.5473 1.34717 9 2 4 -9 11.7936 1.36742 1 2 4 -9 12.1005 1.05461 2 2 4 -9 12.1759 1.09609 2 -2 -4 9 10.4473 1.42058 8 -2 -4 9 12.6350 2.04491 6 1 4 -9 484.047 11.5199 1 1 4 -9 501.969 12.3923 5 1 4 -9 510.704 11.2513 9 1 4 -9 516.586 10.8155 2 1 4 -9 493.120 10.6981 2 -1 -4 9 493.945 12.9012 6 -1 -4 9 492.105 11.8467 8 0 4 -9 1985.61 41.3646 5 0 4 -9 1997.97 39.8086 2 0 4 -9 2019.75 40.2718 9 0 4 -9 2026.73 39.7791 2 0 4 -9 2000.68 40.6686 1 0 -4 9 1981.48 40.9525 8 0 -4 9 1964.34 42.1765 6 0 -4 9 1936.99 40.8548 1 -1 4 -9 308.364 8.33193 8 -1 4 -9 321.030 8.50610 5 -1 4 -9 309.468 7.35753 2 -1 4 -9 322.269 8.08491 1 -1 4 -9 320.268 8.07057 1 -1 4 -9 321.228 7.74081 9 -1 4 -9 321.536 7.34697 2 1 -4 9 319.613 7.32493 1 1 -4 9 309.435 9.07408 6 1 -4 9 317.353 8.24091 8 -2 4 -9 -0.1851 0.55623 2 -2 4 -9 -0.7872 0.73347 5 -2 4 -9 0.62641 0.91164 8 -2 4 -9 0.86023 0.80093 1 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4.19295 8 13 -4 9 47.0000 3.03800 7 13 -4 9 41.2997 4.28741 1 13 -4 9 41.9860 2.96112 7 -14 4 -9 14.2601 2.90306 1 -14 4 -9 20.9266 3.55651 9 14 -4 9 15.5212 2.13949 7 14 -4 9 12.0176 2.88945 8 14 -4 9 18.8359 2.32445 7 -15 4 -9 98.3436 6.72688 9 -15 4 -9 95.2347 6.26301 1 15 -4 9 108.140 4.83905 7 15 -4 9 92.4247 6.39136 8 15 -4 9 98.7567 4.75485 7 -16 4 -9 4.77486 2.61945 1 -16 4 -9 2.02807 2.46096 9 16 -4 9 5.74351 1.61617 7 -17 4 -9 6.69488 3.07129 9 -17 4 -9 8.07978 3.20435 1 17 -4 9 3.26297 1.58330 7 17 3 -9 10.3149 3.82637 1 16 3 -9 8.13351 3.19570 1 15 3 -9 12.4518 3.24171 1 14 3 -9 10.1112 3.03239 1 13 3 -9 0.43328 1.88424 1 12 3 -9 3.45512 1.67930 2 12 3 -9 0.09044 1.68749 1 11 3 -9 82.9358 4.36547 2 11 3 -9 83.5345 5.07264 1 10 3 -9 105.203 4.67582 2 10 3 -9 103.608 5.13957 2 10 3 -9 100.670 5.20295 1 9 3 -9 5.85296 1.48280 2 9 3 -9 7.61365 1.86933 1 9 3 -9 3.39788 1.14490 2 -9 -3 9 6.12970 1.57994 8 8 3 -9 97.5022 4.05692 2 8 3 -9 109.439 4.74576 1 8 3 -9 94.1603 4.02721 2 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12.1291 2 5 -6 11 470.806 11.7569 1 5 -6 11 483.310 12.7136 8 5 -6 11 455.184 13.3753 6 -6 6 -11 32.9116 2.72223 2 -6 6 -11 37.1341 2.76201 2 -6 6 -11 34.4311 3.13268 9 -6 6 -11 38.0153 3.04929 1 -6 6 -11 32.2794 3.30050 3 6 -6 11 37.6726 3.78409 6 6 -6 11 31.3360 3.03287 8 6 -6 11 39.0744 2.71356 1 -7 6 -11 1.60755 1.40414 1 -7 6 -11 2.60324 1.40656 2 -7 6 -11 -0.1467 1.20708 9 -7 6 -11 -0.9010 1.27018 3 7 -6 11 0.23589 1.64492 6 7 -6 11 0.29273 1.32533 8 7 -6 11 0.10329 1.11283 1 -8 6 -11 228.055 8.41042 3 -8 6 -11 238.451 8.18923 9 -8 6 -11 224.783 7.89804 1 -8 6 -11 228.107 7.82369 2 8 -6 11 223.063 5.27607 7 8 -6 11 226.564 8.78472 6 8 -6 11 221.160 7.42919 1 8 -6 11 218.759 5.25927 7 8 -6 11 226.101 8.00092 8 -9 6 -11 63.9133 4.13765 2 -9 6 -11 58.5624 4.26320 3 -9 6 -11 57.0050 4.27156 9 -9 6 -11 65.5933 4.17156 1 9 -6 11 55.7509 2.31352 7 9 -6 11 55.4104 4.51019 6 9 -6 11 58.9569 3.86208 1 9 -6 11 62.2594 4.32456 8 9 -6 11 60.5777 2.38574 7 -10 6 -11 69.9840 4.86024 9 -10 6 -11 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3.55279 6 -3 1 26 13.7772 4.16929 6 -2 1 26 28.1185 5.42234 6 -1 1 26 16.7385 4.41590 6 0 -1 -26 33.9523 4.03884 1 0 1 26 36.9098 6.04571 6 -1 -1 -26 125.982 5.12840 1 1 1 26 146.845 9.85012 6 -2 -1 -26 15.7537 2.46683 1 2 1 26 19.5037 4.75062 6 -5 2 26 65.5332 7.25032 6 -4 2 26 37.7060 5.94135 6 -3 2 26 2.70152 3.49268 6 -2 2 26 0.56461 3.07589 6 -1 2 26 3.12284 3.20306 6 0 2 26 32.0230 5.56629 6 -1 -2 -26 1.41132 1.69231 1 1 2 26 0.35664 2.72730 6 -5 3 26 13.6419 4.08774 6 -4 3 26 12.0350 4.06693 6 -3 3 26 23.3936 5.09195 6 -2 3 26 18.4404 4.55823 6 -1 3 26 16.2885 4.32975 6 1 6 -27 -0.7239 1.67054 1 -1 -6 27 -4.3494 2.80271 6 0 6 -27 1.84635 1.88658 1 0 -6 27 -0.6555 3.65751 6 -1 6 -27 21.3667 3.07123 1 1 -6 27 21.0527 5.44981 6 -3 -5 27 4.85764 4.22068 6 2 5 -27 -1.8939 1.44795 1 -2 -5 27 1.46369 3.57563 6 1 5 -27 14.2117 2.43455 1 -1 -5 27 11.9097 4.78181 6 0 5 -27 65.7954 4.23191 1 0 -5 27 57.7907 7.62992 6 -1 5 -27 37.8276 3.64975 1 1 -5 27 33.9613 6.18863 6 -2 5 -27 54.0258 4.19037 1 2 -5 27 59.2598 7.70214 6 3 4 -27 3.69068 1.63379 1 -3 -4 27 0.68848 3.47115 6 2 4 -27 2.21015 1.67387 1 -2 -4 27 -1.3319 2.92018 6 1 4 -27 -0.1314 1.38019 1 -1 -4 27 -5.9091 2.41146 6 0 4 -27 30.4773 3.12987 1 0 -4 27 27.3427 5.78003 6 -1 4 -27 0.94368 1.57953 1 1 -4 27 -1.6067 3.51413 6 -2 4 -27 3.64597 1.94511 1 2 -4 27 11.1967 4.20545 6 -4 -3 27 17.8822 4.84931 6 -3 -3 27 28.8725 5.63672 6 -2 -3 27 20.8974 5.21659 6 1 3 -27 -1.2229 1.30565 1 -1 -3 27 -0.9338 3.33780 6 0 3 -27 2.85689 1.58272 1 0 -3 27 -2.6238 2.99127 6 -1 3 -27 35.3507 3.34208 1 1 -3 27 40.8845 6.32326 6 -2 3 -27 0.15568 1.62465 1 2 -3 27 -3.4671 3.47942 6 -4 -2 27 17.5747 5.07781 6 -3 -2 27 3.02856 3.44198 6 -2 -2 27 7.49870 4.24499 6 -1 -2 27 -4.4176 2.79682 6 0 2 -27 -0.1759 1.38684 1 0 -2 27 -1.6196 3.31842 6 -1 2 -27 20.6409 2.57706 1 1 -2 27 22.5402 5.18743 6 2 -2 27 45.4739 7.07908 6 -4 -1 27 5.42191 3.87714 6 -3 -1 27 82.5572 8.53811 6 -2 -1 27 43.7484 6.34713 6 -1 -1 27 4.88767 4.02419 6 0 -1 27 94.8326 9.19535 6 -1 1 -27 29.9966 2.95267 1 1 -1 27 37.2143 6.43035 6 -3 0 27 4.74209 3.52412 6 -2 0 27 2.79942 3.71496 6 -1 0 27 1.44443 3.18595 6 0 0 27 99.4603 8.41043 6 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.7190 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71091 13.524 13.598 19.011 98.348 92.953 106.302 ) ; _shelx_hkl_checksum 67735