#------------------------------------------------------------------------------ #$Date: 2019-03-20 01:18:38 +0200 (Wed, 20 Mar 2019) $ #$Revision: 214197 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/07/1550755.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1550755 loop_ _publ_author_name 'Liu, Siyuan' 'L\'egar\'e, Marc-Andr\'e' 'Hofmann, Alexander' 'Rempel, Anna' 'Hagspiel, Stephan' 'Braunschweig, Holger' _publ_section_title ; Synthesis of Unsymmetrical B2E2 and B2E3 Heterocycles by Borylene Insertion into Boradichalcogeniranes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC00657E _journal_year 2019 _chemical_formula_moiety 'C15 H35 B2 N3 Se2 Si2' _chemical_formula_sum 'C15 H35 B2 N3 Se2 Si2' _chemical_formula_weight 493.18 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2018-12-20 deposited with the CCDC. 2019-03-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.60(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.500(5) _cell_length_b 12.544(6) _cell_length_c 16.944(7) _cell_measurement_reflns_used 2992 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.33 _cell_measurement_theta_min 2.48 _cell_volume 2302.6(18) _computing_cell_refinement 'Saint+ ver. V8.37A (Bruker AXS)' _computing_data_collection 'APEX2 ver. 2014.9 (Bruker AXS)' _computing_data_reduction 'Saint+ ver. V8.37A (Bruker AXS)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD area detector (Apex2)' _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker X8-APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_unetI/netI 0.0713 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 27381 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.017 _diffrn_reflns_theta_min 1.885 _diffrn_source 'rotating-anode (Nonius FR-591)' _exptl_absorpt_coefficient_mu 3.319 _exptl_absorpt_correction_T_max 0.5256 _exptl_absorpt_correction_T_min 0.3432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SadAbs 2016/2 (Bruker AXS)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.423 _exptl_crystal_description plate _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.412 _exptl_crystal_size_mid 0.388 _exptl_crystal_size_min 0.146 _refine_diff_density_max 0.671 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.119 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 228 _refine_ls_number_reflns 4531 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0394 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.2246P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.0956 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3357 _reflns_number_total 4531 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc00657e2.cif _cod_data_source_block AlHo054_a _cod_original_cell_volume 2302.8(18) _cod_database_code 1550755 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.342 _shelx_estimated_absorpt_t_max 0.643 _shelx_res_file ; TITL AlHo054_a.res in P2(1)/n AlHo054_a.res created by SHELXL-2016/6 at 12:44:05 on 27-Feb-2018 REM Old TITL AlHo054 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.098, Rweak 0.005, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C16 B2 N2 Si2 Se2 CELL 0.71073 11.50041 12.54360 16.94425 90.0000 109.5954 90.0000 ZERR 4.000 0.00476 0.00626 0.00695 0.0000 0.0241 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H B N SI SE UNIT 60 140 8 12 8 8 TEMP -173.15 SIZE 0.146 0.388 0.412 L.S. 10 BOND $H LIST 4 Acta 52 Shel 999. 0.81 Conf FMAP 2 PLAN 20 WGHT 0.040500 0.224600 FVAR 0.30601 SE1 6 0.591011 0.362920 0.722974 11.00000 0.01366 0.01567 = 0.01232 -0.00200 0.00548 -0.00284 B1 3 0.561058 0.263898 0.616932 11.00000 0.00939 0.01991 = 0.01271 -0.00143 0.00466 -0.00099 SE2 6 0.378478 0.227751 0.609852 11.00000 0.01200 0.02190 = 0.01510 -0.00423 0.00467 -0.00329 RESI 1 TBU C1 1 0.655157 0.162664 0.637484 11.00000 0.01141 0.01772 = 0.01520 0.00105 0.00711 -0.00087 C2 1 0.788502 0.197835 0.654699 11.00000 0.01576 0.02724 = 0.02049 -0.00517 0.00573 0.00202 AFIX 137 H2A 2 0.794963 0.235176 0.605536 11.00000 -1.50000 H2B 2 0.842419 0.135108 0.666456 11.00000 -1.50000 H2C 2 0.813707 0.245793 0.703155 11.00000 -1.50000 AFIX 0 C3 1 0.620621 0.084406 0.563315 11.00000 0.02043 0.02028 = 0.02255 -0.00272 0.00078 0.00522 AFIX 137 H3A 2 0.624048 0.121251 0.513141 11.00000 -1.50000 H3B 2 0.536878 0.057427 0.553143 11.00000 -1.50000 H3C 2 0.678933 0.024681 0.576407 11.00000 -1.50000 AFIX 0 C4 1 0.652315 0.098760 0.714124 11.00000 0.02573 0.02011 = 0.02571 0.00462 0.00832 0.00521 AFIX 137 H4A 2 0.567257 0.077292 0.706364 11.00000 -1.50000 H4B 2 0.683783 0.143087 0.764454 11.00000 -1.50000 H4C 2 0.704090 0.035122 0.720459 11.00000 -1.50000 AFIX 0 RESI 0 RESI 2 IME C1 1 0.561029 0.329359 0.533726 11.00000 0.01486 0.01371 = 0.01685 0.00012 0.00683 0.00229 N1 4 0.633274 0.411698 0.527663 11.00000 0.01997 0.01747 = 0.01578 -0.00108 0.00871 -0.00260 C2 1 0.604742 0.444498 0.446163 11.00000 0.03047 0.02017 = 0.02233 0.00667 0.01446 0.00118 AFIX 43 H2 2 0.641872 0.501667 0.426531 11.00000 -1.20000 AFIX 0 N2 4 0.488999 0.310026 0.453447 11.00000 0.02122 0.01725 = 0.01067 -0.00002 0.00543 -0.00080 C3 1 0.514952 0.380862 0.399716 11.00000 0.02834 0.02563 = 0.01610 0.00483 0.01280 0.00456 AFIX 43 H3 2 0.476227 0.383900 0.340649 11.00000 -1.20000 AFIX 0 C4 1 0.732979 0.462002 0.595715 11.00000 0.02928 0.02043 = 0.02738 -0.00575 0.01372 -0.01307 AFIX 137 H4A 2 0.800161 0.482090 0.575249 11.00000 -1.50000 H4B 2 0.764020 0.411664 0.642309 11.00000 -1.50000 H4C 2 0.701307 0.525828 0.615009 11.00000 -1.50000 AFIX 0 C5 1 0.395230 0.226358 0.421610 11.00000 0.02015 0.02759 = 0.01216 -0.00152 0.00153 -0.00299 AFIX 137 H5A 2 0.312928 0.256751 0.411212 11.00000 -1.50000 H5B 2 0.409526 0.169128 0.463160 11.00000 -1.50000 H5C 2 0.400784 0.197472 0.369253 11.00000 -1.50000 AFIX 0 RESI 0 RESI 3 NTMS B1 3 0.428055 0.308060 0.715047 11.00000 0.01408 0.01727 = 0.01716 0.00354 0.00697 0.00549 C1 1 0.147099 0.405260 0.637755 11.00000 0.02258 0.03986 = 0.02787 0.00231 0.00621 0.01144 AFIX 137 H1A 2 0.176116 0.375151 0.594319 11.00000 -1.50000 H1B 2 0.180428 0.477373 0.651747 11.00000 -1.50000 H1C 2 0.056712 0.408232 0.617054 11.00000 -1.50000 AFIX 0 SI1 5 0.455051 0.312389 0.880612 11.00000 0.01759 0.02070 = 0.01554 0.00036 0.00769 -0.00029 C2 1 0.143716 0.181663 0.708886 11.00000 0.02268 0.03842 = 0.05653 -0.01176 0.02015 -0.00651 AFIX 137 H2A 2 0.053403 0.182037 0.685123 11.00000 -1.50000 H2B 2 0.169722 0.139091 0.760362 11.00000 -1.50000 H2C 2 0.177939 0.150630 0.668319 11.00000 -1.50000 AFIX 0 SI2 5 0.200429 0.319723 0.733121 11.00000 0.01413 0.02811 = 0.02380 -0.00413 0.00786 -0.00036 C3 1 0.126321 0.378516 0.804852 11.00000 0.01863 0.05360 = 0.03310 -0.00437 0.01333 0.00574 AFIX 137 H3A 2 0.039121 0.392766 0.773825 11.00000 -1.50000 H3B 2 0.167929 0.445355 0.828070 11.00000 -1.50000 H3C 2 0.132771 0.328480 0.850547 11.00000 -1.50000 AFIX 0 C4 1 0.553676 0.191479 0.897064 11.00000 0.02498 0.02509 = 0.02182 0.00358 0.00644 0.00090 AFIX 137 H4A 2 0.501898 0.127679 0.889556 11.00000 -1.50000 H4B 2 0.613801 0.192252 0.953957 11.00000 -1.50000 H4C 2 0.597347 0.190733 0.856359 11.00000 -1.50000 AFIX 0 C5 1 0.551593 0.433158 0.915564 11.00000 0.03134 0.02971 = 0.02352 -0.00246 0.00759 -0.00750 AFIX 137 H5A 2 0.603147 0.443482 0.880394 11.00000 -1.50000 H5B 2 0.604469 0.424385 0.974074 11.00000 -1.50000 H5C 2 0.498196 0.495446 0.910700 11.00000 -1.50000 AFIX 0 C6 1 0.362573 0.294390 0.951676 11.00000 0.02388 0.04762 = 0.01921 0.00121 0.01077 0.00322 AFIX 137 H6A 2 0.315152 0.359369 0.951453 11.00000 -1.50000 H6B 2 0.418186 0.280180 1.008719 11.00000 -1.50000 H6C 2 0.305875 0.234180 0.932129 11.00000 -1.50000 AFIX 0 N1 4 0.362987 0.320782 0.773840 11.00000 0.01513 0.01659 = 0.01851 -0.00032 0.00525 0.00144 RESI 0 HKLF 4 REM AlHo054_a.res in P2(1)/n REM R1 = 0.0394 for 3357 Fo > 4sig(Fo) and 0.0668 for all 4531 data REM 228 parameters refined using 0 restraints END WGHT 0.0405 0.2246 REM Highest difference peak 0.671, deepest hole -0.519, 1-sigma level 0.119 Q1 1 0.3810 0.1277 0.6123 11.00000 0.05 0.67 Q2 1 0.3774 0.3306 0.6101 11.00000 0.05 0.63 Q3 1 0.5009 0.3092 0.7274 11.00000 0.05 0.62 Q4 1 0.6145 0.2189 0.6245 11.00000 0.05 0.59 Q5 1 0.2977 0.3065 0.6213 11.00000 0.05 0.54 Q6 1 0.2982 0.1627 0.6211 11.00000 0.05 0.53 Q7 1 0.3414 0.2983 0.6561 11.00000 0.05 0.51 Q8 1 0.6808 0.2787 0.7236 11.00000 0.05 0.51 Q9 1 0.4230 0.2614 0.6789 11.00000 0.05 0.51 Q10 1 0.4043 0.2984 0.9192 11.00000 0.05 0.51 Q11 1 0.5935 0.4608 0.7268 11.00000 0.05 0.50 Q12 1 0.6783 0.3527 0.7459 11.00000 0.05 0.50 Q13 1 0.5771 0.3253 0.7771 11.00000 0.05 0.50 Q14 1 0.4588 0.3044 0.5958 11.00000 0.05 0.48 Q15 1 0.2951 0.1074 0.6311 11.00000 0.05 0.48 Q16 1 0.6735 0.4476 0.7136 11.00000 0.05 0.48 Q17 1 0.3595 0.1620 0.6751 11.00000 0.05 0.47 Q18 1 0.4547 0.3367 0.9384 11.00000 0.05 0.47 Q19 1 0.4295 0.3139 0.9309 11.00000 0.05 0.46 Q20 1 0.1805 0.2427 0.7233 11.00000 0.05 0.45 ; _shelx_res_checksum 89545 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Se1 Se 0.59101(4) 0.36292(3) 0.72297(2) 0.01360(12) Uani 1 1 d . . B1 B 0.5611(4) 0.2639(4) 0.6169(3) 0.0138(10) Uani 1 1 d . . Se2 Se 0.37848(4) 0.22775(4) 0.60985(2) 0.01630(12) Uani 1 1 d . . C1_1 C 0.6552(4) 0.1627(3) 0.6375(2) 0.0141(9) Uani 1 1 d . . C2_1 C 0.7885(4) 0.1978(4) 0.6547(2) 0.0213(10) Uani 1 1 d . . H2A_1 H 0.794963 0.235176 0.605536 0.032 Uiso 1 1 calc R U H2B_1 H 0.842419 0.135108 0.666456 0.032 Uiso 1 1 calc R U H2C_1 H 0.813707 0.245793 0.703155 0.032 Uiso 1 1 calc R U C3_1 C 0.6206(4) 0.0844(4) 0.5633(2) 0.0227(10) Uani 1 1 d . . H3A_1 H 0.624048 0.121251 0.513141 0.034 Uiso 1 1 calc R U H3B_1 H 0.536878 0.057427 0.553143 0.034 Uiso 1 1 calc R U H3C_1 H 0.678933 0.024681 0.576407 0.034 Uiso 1 1 calc R U C4_1 C 0.6523(4) 0.0988(4) 0.7141(2) 0.0239(10) Uani 1 1 d . . H4A_1 H 0.567257 0.077292 0.706364 0.036 Uiso 1 1 calc R U H4B_1 H 0.683783 0.143087 0.764454 0.036 Uiso 1 1 calc R U H4C_1 H 0.704090 0.035122 0.720459 0.036 Uiso 1 1 calc R U C1_2 C 0.5610(4) 0.3294(3) 0.5337(2) 0.0148(9) Uani 1 1 d . . N1_2 N 0.6333(3) 0.4117(3) 0.52766(19) 0.0171(8) Uani 1 1 d . . C2_2 C 0.6047(4) 0.4445(4) 0.4462(2) 0.0229(10) Uani 1 1 d . . H2_2 H 0.641872 0.501667 0.426531 0.027 Uiso 1 1 calc R U N2_2 N 0.4890(3) 0.3100(3) 0.45345(18) 0.0164(8) Uani 1 1 d . . C3_2 C 0.5150(4) 0.3809(4) 0.3997(2) 0.0220(10) Uani 1 1 d . . H3_2 H 0.476227 0.383900 0.340649 0.026 Uiso 1 1 calc R U C4_2 C 0.7330(4) 0.4620(4) 0.5957(2) 0.0246(11) Uani 1 1 d . . H4A_2 H 0.800161 0.482090 0.575249 0.037 Uiso 1 1 calc R U H4B_2 H 0.764020 0.411664 0.642309 0.037 Uiso 1 1 calc R U H4C_2 H 0.701307 0.525828 0.615009 0.037 Uiso 1 1 calc R U C5_2 C 0.3952(4) 0.2264(4) 0.4216(2) 0.0209(10) Uani 1 1 d . . H5A_2 H 0.312928 0.256751 0.411212 0.031 Uiso 1 1 calc R U H5B_2 H 0.409526 0.169128 0.463160 0.031 Uiso 1 1 calc R U H5C_2 H 0.400784 0.197472 0.369253 0.031 Uiso 1 1 calc R U B1_3 B 0.4281(4) 0.3081(4) 0.7150(3) 0.0157(10) Uani 1 1 d . . C1_3 C 0.1471(4) 0.4053(4) 0.6378(3) 0.0307(12) Uani 1 1 d . . H1A_3 H 0.176116 0.375151 0.594319 0.046 Uiso 1 1 calc R U H1B_3 H 0.180428 0.477373 0.651747 0.046 Uiso 1 1 calc R U H1C_3 H 0.056712 0.408232 0.617054 0.046 Uiso 1 1 calc R U Si1_3 Si 0.45505(11) 0.31239(10) 0.88061(6) 0.0174(3) Uani 1 1 d . . C2_3 C 0.1437(4) 0.1817(4) 0.7089(3) 0.0375(13) Uani 1 1 d . . H2A_3 H 0.053403 0.182037 0.685123 0.056 Uiso 1 1 calc R U H2B_3 H 0.169722 0.139091 0.760362 0.056 Uiso 1 1 calc R U H2C_3 H 0.177939 0.150630 0.668319 0.056 Uiso 1 1 calc R U Si2_3 Si 0.20043(11) 0.31972(11) 0.73312(7) 0.0216(3) Uani 1 1 d . . C3_3 C 0.1263(4) 0.3785(5) 0.8049(3) 0.0339(13) Uani 1 1 d . . H3A_3 H 0.039121 0.392766 0.773825 0.051 Uiso 1 1 calc R U H3B_3 H 0.167929 0.445355 0.828070 0.051 Uiso 1 1 calc R U H3C_3 H 0.132771 0.328480 0.850547 0.051 Uiso 1 1 calc R U C4_3 C 0.5537(4) 0.1915(4) 0.8971(3) 0.0243(10) Uani 1 1 d . . H4A_3 H 0.501898 0.127679 0.889556 0.036 Uiso 1 1 calc R U H4B_3 H 0.613801 0.192252 0.953957 0.036 Uiso 1 1 calc R U H4C_3 H 0.597347 0.190733 0.856359 0.036 Uiso 1 1 calc R U C5_3 C 0.5516(4) 0.4332(4) 0.9156(2) 0.0286(12) Uani 1 1 d . . H5A_3 H 0.603147 0.443482 0.880394 0.043 Uiso 1 1 calc R U H5B_3 H 0.604469 0.424385 0.974074 0.043 Uiso 1 1 calc R U H5C_3 H 0.498196 0.495446 0.910700 0.043 Uiso 1 1 calc R U C6_3 C 0.3626(4) 0.2944(4) 0.9517(2) 0.0293(12) Uani 1 1 d . . H6A_3 H 0.315152 0.359369 0.951453 0.044 Uiso 1 1 calc R U H6B_3 H 0.418186 0.280180 1.008719 0.044 Uiso 1 1 calc R U H6C_3 H 0.305875 0.234180 0.932129 0.044 Uiso 1 1 calc R U N1_3 N 0.3630(3) 0.3208(3) 0.77384(19) 0.0168(8) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0137(2) 0.0157(2) 0.01232(19) -0.00200(16) 0.00548(15) -0.00284(18) B1 0.009(2) 0.020(3) 0.013(2) -0.0014(19) 0.0047(17) -0.001(2) Se2 0.0120(2) 0.0219(3) 0.0151(2) -0.00423(17) 0.00467(16) -0.00329(18) C1_1 0.011(2) 0.018(3) 0.0152(18) 0.0010(16) 0.0071(16) -0.0009(17) C2_1 0.016(2) 0.027(3) 0.020(2) -0.0052(19) 0.0057(17) 0.002(2) C3_1 0.020(2) 0.020(3) 0.023(2) -0.0027(19) 0.0008(18) 0.005(2) C4_1 0.026(2) 0.020(3) 0.026(2) 0.005(2) 0.0083(19) 0.005(2) C1_2 0.015(2) 0.014(2) 0.0169(19) 0.0001(17) 0.0068(16) 0.0023(18) N1_2 0.0200(19) 0.017(2) 0.0158(16) -0.0011(15) 0.0087(14) -0.0026(16) C2_2 0.030(3) 0.020(3) 0.022(2) 0.0067(19) 0.0145(19) 0.001(2) N2_2 0.0212(19) 0.017(2) 0.0107(15) 0.0000(14) 0.0054(14) -0.0008(16) C3_2 0.028(3) 0.026(3) 0.0161(19) 0.0048(19) 0.0128(18) 0.005(2) C4_2 0.029(3) 0.020(3) 0.027(2) -0.006(2) 0.014(2) -0.013(2) C5_2 0.020(2) 0.028(3) 0.0122(18) -0.0015(18) 0.0015(17) -0.003(2) B1_3 0.014(2) 0.017(3) 0.017(2) 0.004(2) 0.0070(19) 0.005(2) C1_3 0.023(3) 0.040(3) 0.028(2) 0.002(2) 0.006(2) 0.011(2) Si1_3 0.0176(6) 0.0207(7) 0.0155(5) 0.0004(5) 0.0077(5) -0.0003(5) C2_3 0.023(3) 0.038(3) 0.057(3) -0.012(3) 0.020(2) -0.007(2) Si2_3 0.0141(6) 0.0281(8) 0.0238(6) -0.0041(6) 0.0079(5) -0.0004(6) C3_3 0.019(2) 0.054(4) 0.033(2) -0.004(2) 0.013(2) 0.006(2) C4_3 0.025(2) 0.025(3) 0.022(2) 0.004(2) 0.0064(19) 0.001(2) C5_3 0.031(3) 0.030(3) 0.024(2) -0.002(2) 0.008(2) -0.007(2) C6_3 0.024(2) 0.048(4) 0.019(2) 0.001(2) 0.0108(19) 0.003(2) N1_3 0.0151(18) 0.017(2) 0.0185(16) -0.0003(15) 0.0053(14) 0.0014(16) 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' B B 0.0013 0.0007 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2.00 1.00 2.00 0.0750 -1.00 0.00 -2.00 0.1660 1.00 0.00 2.00 0.1220 1.00 1.00 -1.00 0.0400 1.00 1.00 -2.00 0.0630 -1.00 -1.00 2.00 0.1550 2.00 1.00 -1.00 0.0340 2.00 1.00 -2.00 0.0260 1.00 0.00 1.00 0.1130 1.00 0.00 -1.00 0.0200 -1.00 0.00 1.00 0.0730 2.00 -1.00 -2.00 0.0750 2.00 -2.00 -1.00 0.1420 1.00 -2.00 0.00 0.1810 -1.00 2.00 0.00 0.1520 -1.00 1.00 -2.00 0.1490 -1.00 -1.00 -2.00 0.1910 0.00 -2.00 1.00 0.2070 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle B1_3 Se1 B1 81.72(19) C1_1 B1 C1_2 112.6(3) C1_1 B1 Se2 114.9(3) C1_2 B1 Se2 110.3(3) C1_1 B1 Se1 111.7(2) C1_2 B1 Se1 113.0(3) Se2 B1 Se1 92.86(18) B1_3 Se2 B1 81.80(19) C2_1 C1_1 C4_1 107.1(3) C2_1 C1_1 C3_1 107.9(3) C4_1 C1_1 C3_1 106.6(4) C2_1 C1_1 B1 111.6(4) C4_1 C1_1 B1 112.8(3) C3_1 C1_1 B1 110.6(3) C1_1 C2_1 H2A_1 109.5 C1_1 C2_1 H2B_1 109.5 H2A_1 C2_1 H2B_1 109.5 C1_1 C2_1 H2C_1 109.5 H2A_1 C2_1 H2C_1 109.5 H2B_1 C2_1 H2C_1 109.5 C1_1 C3_1 H3A_1 109.5 C1_1 C3_1 H3B_1 109.5 H3A_1 C3_1 H3B_1 109.5 C1_1 C3_1 H3C_1 109.5 H3A_1 C3_1 H3C_1 109.5 H3B_1 C3_1 H3C_1 109.5 C1_1 C4_1 H4A_1 109.5 C1_1 C4_1 H4B_1 109.5 H4A_1 C4_1 H4B_1 109.5 C1_1 C4_1 H4C_1 109.5 H4A_1 C4_1 H4C_1 109.5 H4B_1 C4_1 H4C_1 109.5 N1_2 C1_2 N2_2 104.2(3) N1_2 C1_2 B1 129.0(3) N2_2 C1_2 B1 126.9(4) C1_2 N1_2 C2_2 111.1(3) C1_2 N1_2 C4_2 127.4(3) C2_2 N1_2 C4_2 121.5(4) C3_2 C2_2 N1_2 106.9(4) C3_2 C2_2 H2_2 126.5 N1_2 C2_2 H2_2 126.5 C1_2 N2_2 C3_2 110.7(4) C1_2 N2_2 C5_2 128.4(3) C3_2 N2_2 C5_2 120.9(3) C2_2 C3_2 N2_2 107.1(3) C2_2 C3_2 H3_2 126.5 N2_2 C3_2 H3_2 126.5 N1_2 C4_2 H4A_2 109.5 N1_2 C4_2 H4B_2 109.5 H4A_2 C4_2 H4B_2 109.5 N1_2 C4_2 H4C_2 109.5 H4A_2 C4_2 H4C_2 109.5 H4B_2 C4_2 H4C_2 109.5 N2_2 C5_2 H5A_2 109.5 N2_2 C5_2 H5B_2 109.5 H5A_2 C5_2 H5B_2 109.5 N2_2 C5_2 H5C_2 109.5 H5A_2 C5_2 H5C_2 109.5 H5B_2 C5_2 H5C_2 109.5 N1_3 B1_3 Se1 128.3(3) N1_3 B1_3 Se2 128.7(3) Se1 B1_3 Se2 102.9(2) Si2_3 C1_3 H1A_3 109.5 Si2_3 C1_3 H1B_3 109.5 H1A_3 C1_3 H1B_3 109.5 Si2_3 C1_3 H1C_3 109.5 H1A_3 C1_3 H1C_3 109.5 H1B_3 C1_3 H1C_3 109.5 N1_3 Si1_3 C5_3 111.56(19) N1_3 Si1_3 C4_3 109.17(18) C5_3 Si1_3 C4_3 110.4(2) N1_3 Si1_3 C6_3 113.08(18) C5_3 Si1_3 C6_3 107.6(2) C4_3 Si1_3 C6_3 104.8(2) Si2_3 C2_3 H2A_3 109.5 Si2_3 C2_3 H2B_3 109.5 H2A_3 C2_3 H2B_3 109.5 Si2_3 C2_3 H2C_3 109.5 H2A_3 C2_3 H2C_3 109.5 H2B_3 C2_3 H2C_3 109.5 N1_3 Si2_3 C2_3 110.1(2) N1_3 Si2_3 C3_3 113.61(19) C2_3 Si2_3 C3_3 108.2(3) N1_3 Si2_3 C1_3 109.4(2) C2_3 Si2_3 C1_3 111.0(2) C3_3 Si2_3 C1_3 104.4(2) Si2_3 C3_3 H3A_3 109.5 Si2_3 C3_3 H3B_3 109.5 H3A_3 C3_3 H3B_3 109.5 Si2_3 C3_3 H3C_3 109.5 H3A_3 C3_3 H3C_3 109.5 H3B_3 C3_3 H3C_3 109.5 Si1_3 C4_3 H4A_3 109.5 Si1_3 C4_3 H4B_3 109.5 H4A_3 C4_3 H4B_3 109.5 Si1_3 C4_3 H4C_3 109.5 H4A_3 C4_3 H4C_3 109.5 H4B_3 C4_3 H4C_3 109.5 Si1_3 C5_3 H5A_3 109.5 Si1_3 C5_3 H5B_3 109.5 H5A_3 C5_3 H5B_3 109.5 Si1_3 C5_3 H5C_3 109.5 H5A_3 C5_3 H5C_3 109.5 H5B_3 C5_3 H5C_3 109.5 Si1_3 C6_3 H6A_3 109.5 Si1_3 C6_3 H6B_3 109.5 H6A_3 C6_3 H6B_3 109.5 Si1_3 C6_3 H6C_3 109.5 H6A_3 C6_3 H6C_3 109.5 H6B_3 C6_3 H6C_3 109.5 B1_3 N1_3 Si2_3 117.2(3) B1_3 N1_3 Si1_3 115.4(3) Si2_3 N1_3 Si1_3 126.4(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Se1 B1_3 1.958(5) Se1 B1 2.115(5) B1 C1_1 1.629(6) B1 C1_2 1.631(6) B1 Se2 2.112(5) Se2 B1_3 1.958(5) C1_1 C2_1 1.527(5) C1_1 C4_1 1.536(5) C1_1 C3_1 1.538(5) C2_1 H2A_1 0.9800 C2_1 H2B_1 0.9800 C2_1 H2C_1 0.9800 C3_1 H3A_1 0.9800 C3_1 H3B_1 0.9800 C3_1 H3C_1 0.9800 C4_1 H4A_1 0.9800 C4_1 H4B_1 0.9800 C4_1 H4C_1 0.9800 C1_2 N1_2 1.351(5) C1_2 N2_2 1.356(5) N1_2 C2_2 1.371(5) N1_2 C4_2 1.468(5) C2_2 C3_2 1.333(6) C2_2 H2_2 0.9500 N2_2 C3_2 1.375(5) N2_2 C5_2 1.471(5) C3_2 H3_2 0.9500 C4_2 H4A_2 0.9800 C4_2 H4B_2 0.9800 C4_2 H4C_2 0.9800 C5_2 H5A_2 0.9800 C5_2 H5B_2 0.9800 C5_2 H5C_2 0.9800 B1_3 N1_3 1.441(6) C1_3 Si2_3 1.864(5) C1_3 H1A_3 0.9800 C1_3 H1B_3 0.9800 C1_3 H1C_3 0.9800 Si1_3 N1_3 1.766(3) Si1_3 C5_3 1.854(5) Si1_3 C4_3 1.858(5) Si1_3 C6_3 1.868(4) C2_3 Si2_3 1.848(5) C2_3 H2A_3 0.9800 C2_3 H2B_3 0.9800 C2_3 H2C_3 0.9800 Si2_3 N1_3 1.762(4) Si2_3 C3_3 1.855(5) C3_3 H3A_3 0.9800 C3_3 H3B_3 0.9800 C3_3 H3C_3 0.9800 C4_3 H4A_3 0.9800 C4_3 H4B_3 0.9800 C4_3 H4C_3 0.9800 C5_3 H5A_3 0.9800 C5_3 H5B_3 0.9800 C5_3 H5C_3 0.9800 C6_3 H6A_3 0.9800 C6_3 H6B_3 0.9800 C6_3 H6C_3 0.9800 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 C1_2 B1 C1_1 C2_1 61.2(4) Se2 B1 C1_1 C2_1 -171.3(3) Se1 B1 C1_1 C2_1 -67.2(4) C1_2 B1 C1_1 C4_1 -178.2(3) Se2 B1 C1_1 C4_1 -50.7(4) Se1 B1 C1_1 C4_1 53.4(4) C1_2 B1 C1_1 C3_1 -59.0(4) Se2 B1 C1_1 C3_1 68.5(4) Se1 B1 C1_1 C3_1 172.6(3) C1_1 B1 C1_2 N1_2 -89.1(5) Se2 B1 C1_2 N1_2 141.0(4) Se1 B1 C1_2 N1_2 38.6(5) C1_1 B1 C1_2 N2_2 88.7(5) Se2 B1 C1_2 N2_2 -41.2(5) Se1 B1 C1_2 N2_2 -143.6(4) N2_2 C1_2 N1_2 C2_2 1.6(5) B1 C1_2 N1_2 C2_2 179.7(4) N2_2 C1_2 N1_2 C4_2 -176.9(4) B1 C1_2 N1_2 C4_2 1.3(7) C1_2 N1_2 C2_2 C3_2 -1.2(5) C4_2 N1_2 C2_2 C3_2 177.4(4) N1_2 C1_2 N2_2 C3_2 -1.4(5) B1 C1_2 N2_2 C3_2 -179.6(4) N1_2 C1_2 N2_2 C5_2 177.7(4) B1 C1_2 N2_2 C5_2 -0.5(7) N1_2 C2_2 C3_2 N2_2 0.3(5) C1_2 N2_2 C3_2 C2_2 0.7(5) C5_2 N2_2 C3_2 C2_2 -178.5(4) Se1 B1_3 N1_3 Si2_3 151.2(3) Se2 B1_3 N1_3 Si2_3 -31.3(5) Se1 B1_3 N1_3 Si1_3 -39.5(5) Se2 B1_3 N1_3 Si1_3 138.1(3) C2_3 Si2_3 N1_3 B1_3 77.0(4) C3_3 Si2_3 N1_3 B1_3 -161.5(4) C1_3 Si2_3 N1_3 B1_3 -45.2(4) C2_3 Si2_3 N1_3 Si1_3 -91.1(3) C3_3 Si2_3 N1_3 Si1_3 30.5(4) C1_3 Si2_3 N1_3 Si1_3 146.8(3) C5_3 Si1_3 N1_3 B1_3 73.3(4) C4_3 Si1_3 N1_3 B1_3 -49.0(4) C6_3 Si1_3 N1_3 B1_3 -165.2(3) C5_3 Si1_3 N1_3 Si2_3 -118.4(3) C4_3 Si1_3 N1_3 Si2_3 119.3(3) C6_3 Si1_3 N1_3 Si2_3 3.0(4)