#------------------------------------------------------------------------------
#$Date: 2022-06-26 01:45:49 +0300 (Sun, 26 Jun 2022) $
#$Revision: 276270 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/05/7710598.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_7710598
loop_
_publ_author_name
'Roesky, Herbert W.'
'Nazish, Mohd'
'Ding, Yi'
'Legendre, Christina M.'
'Kumar, Arun'
'Graw, Nico'
'Schwederski, Brigitte'
'Herbst-Irmer, Regine'
'P, Parvathy'
'Parameswaran, Pattiyil'
'Stalke, Dietmar'
'Kaim, Wolfgang'
_publ_section_title
;
 High yield of a variety of silicon-boron radicals and their reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01318E
_journal_year                    2022
_chemical_formula_moiety         'C34 H55 B Br2 N2 Si'
_chemical_formula_sum            'C34 H55 B Br2 N2 Si'
_chemical_formula_weight         690.52
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-10-05 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.12(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.079(3)
_cell_length_b                   12.497(2)
_cell_length_c                   17.886(3)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.413
_cell_measurement_theta_min      2.2205
_cell_volume                     3452.7(11)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.37A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            147210
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         1.508
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    2.408
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.127
_refine_diff_density_max         2.088
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0448
_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/[σ²(Fo²)+(0.0499P)²+8.8000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6483
_reflns_number_total             7978
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01318e2.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710598
_shelx_shelxl_version_number     2018/3
_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+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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.73305(2) 0.53159(2) 0.54157(2) 0.01901(9) Uani 1 1 d . . . . .
Si1 Si 0.70847(5) 0.35341(7) 0.41467(5) 0.01297(17) Uani 1 1 d . . . . .
N1 N 0.65549(16) 0.2956(2) 0.48326(15) 0.0148(5) Uani 1 1 d . . . . .
C1 C 0.7324(2) 0.2678(2) 0.53124(17) 0.0147(6) Uani 1 1 d . . . . .
B1 B 0.7197(2) 0.5205(3) 0.4213(2) 0.0153(7) Uani 1 1 d . . . . .
Br2 Br 0.83935(2) 0.53684(3) 0.39788(2) 0.01920(9) Uani 1 1 d . . . . .
N2 N 0.79264(16) 0.2930(2) 0.49561(15) 0.0141(5) Uani 1 1 d . . . . .
C2 C 0.7472(2) 0.2200(3) 0.60997(19) 0.0194(6) Uani 1 1 d . . . . .
C3 C 0.7757(2) 0.2841(3) 0.6753(2) 0.0264(7) Uani 1 1 d . . . . .
H3 H 0.786152 0.358084 0.669872 0.032 Uiso 1 1 calc R U . . .
C4 C 0.7890(3) 0.2393(4) 0.7490(2) 0.0365(10) Uani 1 1 d . . . . .
H4 H 0.809048 0.282795 0.793912 0.044 Uiso 1 1 calc R U . . .
C5 C 0.7732(3) 0.1324(4) 0.7570(2) 0.0389(11) Uani 1 1 d . . . . .
H5 H 0.781235 0.102559 0.807370 0.047 Uiso 1 1 calc R U . . .
C6 C 0.7456(2) 0.0683(3) 0.6920(3) 0.0348(10) Uani 1 1 d . . . . .
H6 H 0.736153 -0.005899 0.697751 0.042 Uiso 1 1 calc R U . . .
C7 C 0.7317(2) 0.1117(3) 0.6183(2) 0.0251(7) Uani 1 1 d . . . . .
H7 H 0.711674 0.067726 0.573560 0.030 Uiso 1 1 calc R U . . .
C8 C 0.5677(2) 0.2962(3) 0.49632(19) 0.0179(6) Uani 1 1 d . . . . .
C9 C 0.5685(2) 0.3325(3) 0.5780(2) 0.0234(7) Uani 1 1 d . . . . .
H9A H 0.508955 0.343256 0.580353 0.035 Uiso 1 1 calc R U . . .
H9B H 0.600659 0.399865 0.590243 0.035 Uiso 1 1 calc R U . . .
H9C H 0.596550 0.277713 0.615841 0.035 Uiso 1 1 calc R U . . .
C10 C 0.5276(2) 0.1841(3) 0.4810(2) 0.0252(7) Uani 1 1 d . . . . .
H10A H 0.469700 0.184995 0.488869 0.038 Uiso 1 1 calc R U . . .
H10B H 0.564187 0.132891 0.517089 0.038 Uiso 1 1 calc R U . . .
H10C H 0.523433 0.162846 0.427363 0.038 Uiso 1 1 calc R U . . .
C11 C 0.5142(2) 0.3753(3) 0.4374(2) 0.0217(7) Uani 1 1 d . . . . .
H11A H 0.455390 0.378925 0.443226 0.033 Uiso 1 1 calc R U . . .
H11B H 0.511643 0.351491 0.384616 0.033 Uiso 1 1 calc R U . . .
H11C H 0.541008 0.446239 0.446535 0.033 Uiso 1 1 calc R U . . .
C12 C 0.8881(2) 0.2714(3) 0.52254(19) 0.0202(7) Uani 1 1 d . . . . .
C13 C 0.9325(2) 0.3570(3) 0.5810(2) 0.0288(8) Uani 1 1 d . . . . .
H13A H 0.995123 0.344574 0.596713 0.043 Uiso 1 1 calc R U . . .
H13B H 0.910515 0.353610 0.626844 0.043 Uiso 1 1 calc R U . . .
H13C H 0.920334 0.427859 0.556890 0.043 Uiso 1 1 calc R U . . .
C14 C 0.9249(2) 0.2762(3) 0.4525(2) 0.0229(7) Uani 1 1 d . . . . .
H14A H 0.988196 0.271349 0.470381 0.034 Uiso 1 1 calc R U . . .
H14B H 0.908174 0.343942 0.424778 0.034 Uiso 1 1 calc R U . . .
H14C H 0.902026 0.216387 0.417364 0.034 Uiso 1 1 calc R U . . .
C15 C 0.9069(2) 0.1597(3) 0.5586(2) 0.0295(8) Uani 1 1 d . . . . .
H15A H 0.967839 0.141704 0.564951 0.044 Uiso 1 1 calc R U . . .
H15B H 0.869877 0.107096 0.524277 0.044 Uiso 1 1 calc R U . . .
H15C H 0.895177 0.158875 0.609454 0.044 Uiso 1 1 calc R U . . .
C16 C 0.6921(2) 0.2527(3) 0.32999(18) 0.0171(6) Uani 1 1 d . . . . .
C17 C 0.7194(2) 0.1399(3) 0.3639(2) 0.0210(7) Uani 1 1 d . . . . .
H17A H 0.709389 0.087787 0.321432 0.032 Uiso 1 1 calc R U . . .
H17B H 0.685150 0.120191 0.399375 0.032 Uiso 1 1 calc R U . . .
H17C H 0.781007 0.140478 0.392456 0.032 Uiso 1 1 calc R U . . .
C18 C 0.5969(2) 0.2398(3) 0.28113(19) 0.0209(7) Uani 1 1 d . . . . .
H18A H 0.592749 0.181733 0.243455 0.031 Uiso 1 1 calc R U . . .
H18B H 0.576768 0.306683 0.253368 0.031 Uiso 1 1 calc R U . . .
H18C H 0.560792 0.222851 0.315594 0.031 Uiso 1 1 calc R U . . .
C19 C 0.7469(2) 0.2842(3) 0.27534(19) 0.0215(7) Uani 1 1 d . . . . .
H19A H 0.740472 0.229879 0.234635 0.032 Uiso 1 1 calc R U . . .
H19B H 0.807924 0.289287 0.305222 0.032 Uiso 1 1 calc R U . . .
H19C H 0.727317 0.353629 0.251362 0.032 Uiso 1 1 calc R U . . .
C20 C 0.66348(19) 0.6231(2) 0.37947(18) 0.0151(6) Uani 1 1 d . . . . .
C21 C 0.59197(19) 0.6151(3) 0.31243(18) 0.0158(6) Uani 1 1 d . . . . .
C22 C 0.5466(2) 0.7057(3) 0.27658(19) 0.0185(6) Uani 1 1 d . . . . .
H22 H 0.498941 0.696397 0.231780 0.022 Uiso 1 1 calc R U . . .
C23 C 0.5687(2) 0.8075(3) 0.30391(19) 0.0186(6) Uani 1 1 d . . . . .
C24 C 0.6404(2) 0.8164(3) 0.3690(2) 0.0190(6) Uani 1 1 d . . . . .
H24 H 0.657326 0.885933 0.389069 0.023 Uiso 1 1 calc R U . . .
C25 C 0.6885(2) 0.7296(3) 0.40628(18) 0.0165(6) Uani 1 1 d . . . . .
C26 C 0.5629(2) 0.5108(3) 0.27046(18) 0.0162(6) Uani 1 1 d . . . . .
H26 H 0.592873 0.451326 0.304972 0.019 Uiso 1 1 calc R U . . .
C27 C 0.5920(2) 0.5071(3) 0.19557(19) 0.0219(7) Uani 1 1 d . . . . .
H27A H 0.577094 0.437314 0.170365 0.033 Uiso 1 1 calc R U . . .
H27B H 0.654740 0.517749 0.208470 0.033 Uiso 1 1 calc R U . . .
H27C H 0.562613 0.563761 0.160142 0.033 Uiso 1 1 calc R U . . .
C28 C 0.4656(2) 0.4917(3) 0.2524(2) 0.0209(7) Uani 1 1 d . . . . .
H28A H 0.452578 0.417156 0.236354 0.031 Uiso 1 1 calc R U . . .
H28B H 0.435008 0.539491 0.210307 0.031 Uiso 1 1 calc R U . . .
H28C H 0.446680 0.506148 0.299018 0.031 Uiso 1 1 calc R U . . .
C29 C 0.5211(2) 0.9075(3) 0.2654(2) 0.0245(7) Uani 1 1 d . . . . .
H29 H 0.563941 0.953870 0.249438 0.029 Uiso 1 1 calc R U . . .
C30 C 0.4861(3) 0.9707(3) 0.3231(2) 0.0307(8) Uani 1 1 d . . . . .
H30A H 0.458071 1.036117 0.298140 0.046 Uiso 1 1 calc R U . . .
H30B H 0.533988 0.989494 0.368525 0.046 Uiso 1 1 calc R U . . .
H30C H 0.443895 0.926918 0.339705 0.046 Uiso 1 1 calc R U . . .
C31 C 0.4476(3) 0.8832(3) 0.1928(2) 0.0327(9) Uani 1 1 d . . . . .
H31A H 0.419808 0.950215 0.170599 0.049 Uiso 1 1 calc R U . . .
H31B H 0.404983 0.836943 0.206623 0.049 Uiso 1 1 calc R U . . .
H31C H 0.470867 0.846799 0.154360 0.049 Uiso 1 1 calc R U . . .
C32 C 0.7682(2) 0.7598(3) 0.47293(19) 0.0183(6) Uani 1 1 d . . . . .
H32 H 0.800177 0.692459 0.493201 0.022 Uiso 1 1 calc R U . . .
C33 C 0.7412(3) 0.8128(3) 0.5399(2) 0.0273(8) Uani 1 1 d . . . . .
H33A H 0.792937 0.829854 0.582234 0.041 Uiso 1 1 calc R U . . .
H33B H 0.704247 0.763679 0.559093 0.041 Uiso 1 1 calc R U . . .
H33C H 0.709158 0.878742 0.521276 0.041 Uiso 1 1 calc R U . . .
C34 C 0.8300(2) 0.8335(3) 0.4450(2) 0.0245(7) Uani 1 1 d . . . . .
H34A H 0.879094 0.852694 0.489267 0.037 Uiso 1 1 calc R U . . .
H34B H 0.799105 0.898543 0.422321 0.037 Uiso 1 1 calc R U . . .
H34C H 0.851146 0.796250 0.405690 0.037 Uiso 1 1 calc R U . . .
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 Si1 N2 71.85(12) . . ?
N1 Si1 C16 106.37(13) . . ?
N2 Si1 C16 105.01(13) . . ?
N1 Si1 B1 113.87(13) . . ?
N2 Si1 B1 109.28(13) . . ?
C16 Si1 B1 133.22(14) . . ?
N1 Si1 C1 36.04(11) . . ?
N2 Si1 C1 35.89(11) . . ?
C16 Si1 C1 111.29(13) . . ?
B1 Si1 C1 115.20(13) . . ?
C1 N1 C8 130.2(3) . . ?
C1 N1 Si1 90.75(19) . . ?
C8 N1 Si1 137.8(2) . . ?
N2 C1 N1 107.2(3) . . ?
N2 C1 C2 126.9(3) . . ?
N1 C1 C2 125.9(3) . . ?
N2 C1 Si1 54.12(15) . . ?
N1 C1 Si1 53.21(15) . . ?
C2 C1 Si1 175.6(2) . . ?
C20 B1 Br2 104.8(2) . . ?
C20 B1 Si1 137.0(2) . . ?
Br2 B1 Si1 98.95(15) . . ?
C20 B1 Br1 107.7(2) . . ?
Br2 B1 Br1 111.09(16) . . ?
Si1 B1 Br1 96.11(15) . . ?
C1 N2 C12 128.1(3) . . ?
C1 N2 Si1 89.99(19) . . ?
C12 N2 Si1 141.9(2) . . ?
C3 C2 C7 120.0(3) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 120.4(3) . . ?
C2 C3 C4 119.6(4) . . ?
C5 C4 C3 120.4(4) . . ?
C4 C5 C6 120.1(4) . . ?
C5 C6 C7 120.3(4) . . ?
C6 C7 C2 119.8(4) . . ?
N1 C8 C11 105.8(2) . . ?
N1 C8 C9 113.2(3) . . ?
C11 C8 C9 108.7(3) . . ?
N1 C8 C10 109.7(3) . . ?
C11 C8 C10 109.9(3) . . ?
C9 C8 C10 109.5(3) . . ?
N2 C12 C13 109.7(3) . . ?
N2 C12 C14 108.9(3) . . ?
C13 C12 C14 108.6(3) . . ?
N2 C12 C15 111.4(3) . . ?
C13 C12 C15 110.5(3) . . ?
C14 C12 C15 107.7(3) . . ?
C19 C16 C18 108.6(3) . . ?
C19 C16 C17 109.4(3) . . ?
C18 C16 C17 104.8(3) . . ?
C19 C16 Si1 110.7(2) . . ?
C18 C16 Si1 114.2(2) . . ?
C17 C16 Si1 108.9(2) . . ?
C21 C20 C25 115.8(3) . . ?
C21 C20 B1 123.4(3) . . ?
C25 C20 B1 120.6(3) . . ?
C22 C21 C20 121.8(3) . . ?
C22 C21 C26 114.8(3) . . ?
C20 C21 C26 123.2(3) . . ?
C23 C22 C21 122.4(3) . . ?
C22 C23 C24 116.2(3) . . ?
C22 C23 C29 123.4(3) . . ?
C24 C23 C29 120.4(3) . . ?
C25 C24 C23 123.9(3) . . ?
C24 C25 C20 119.8(3) . . ?
C24 C25 C32 114.4(3) . . ?
C20 C25 C32 125.8(3) . . ?
C21 C26 C28 113.4(3) . . ?
C21 C26 C27 109.4(3) . . ?
C28 C26 C27 110.7(3) . . ?
C31 C29 C23 113.3(3) . . ?
C31 C29 C30 109.6(3) . . ?
C23 C29 C30 110.5(3) . . ?
C33 C32 C25 110.9(3) . . ?
C33 C32 C34 110.1(3) . . ?
C25 C32 C34 111.7(3) . . ?
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
Br1 B1 2.106(4) . ?
Si1 N1 1.826(3) . ?
Si1 N2 1.847(3) . ?
Si1 C16 1.930(3) . ?
Si1 B1 2.096(4) . ?
Si1 C1 2.279(3) . ?
N1 C1 1.341(4) . ?
N1 C8 1.493(4) . ?
C1 N2 1.336(4) . ?
C1 C2 1.487(4) . ?
B1 C20 1.627(5) . ?
B1 Br2 2.090(3) . ?
N2 C12 1.499(4) . ?
C2 C3 1.385(5) . ?
C2 C7 1.391(5) . ?
C3 C4 1.392(5) . ?
C4 C5 1.375(7) . ?
C5 C6 1.380(7) . ?
C6 C7 1.385(5) . ?
C8 C11 1.525(5) . ?
C8 C9 1.527(4) . ?
C8 C10 1.534(5) . ?
C12 C13 1.527(5) . ?
C12 C14 1.529(5) . ?
C12 C15 1.532(5) . ?
C16 C19 1.538(4) . ?
C16 C18 1.546(4) . ?
C16 C17 1.549(4) . ?
C20 C21 1.416(4) . ?
C20 C25 1.434(4) . ?
C21 C22 1.402(4) . ?
C21 C26 1.513(4) . ?
C22 C23 1.374(5) . ?
C23 C24 1.398(5) . ?
C23 C29 1.526(4) . ?
C24 C25 1.391(5) . ?
C25 C32 1.535(4) . ?
C26 C28 1.526(4) . ?
C26 C27 1.537(4) . ?
C29 C31 1.524(5) . ?
C29 C30 1.526(5) . ?
C32 C33 1.534(5) . ?
C32 C34 1.536(5) . ?
