#------------------------------------------------------------------------------
#$Date: 2020-03-05 02:02:26 +0200 (Thu, 05 Mar 2020) $
#$Revision: 248917 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/34/7703474.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_7703474
loop_
_publ_author_name
'Heitkemper, Tobias'
'Naß, Leonard'
'Sindlinger, Christian P.'
_publ_section_title
;
 2,5-Bis-trimethylsilyl substituted boroles.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2706
_journal_page_last               2714
_journal_paper_doi               10.1039/d0dt00393j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C57 H93 B Si2'
_chemical_formula_weight         845.30
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-01-10 deposited with the CCDC.	2020-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.605(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5775(17)
_cell_length_b                   21.320(2)
_cell_length_c                   16.318(3)
_cell_measurement_reflns_used    9639
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.35
_cell_volume                     5559.9(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            76308
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.068
_diffrn_reflns_theta_max         25.068
_diffrn_reflns_theta_min         1.592
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5816
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.010
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4929
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1401P)²+6.0168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4156
_reflns_number_total             4929
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00393j2.cif
_cod_data_source_block           sad_c2c_a
_cod_depositor_comments
'Adding full bibliography for 7703465--7703474.cif.'
_cod_original_cell_volume        5560.2(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7703474
_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.
;
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.991
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Si1 Si 0.32131(4) 0.37519(3) 0.74208(4) 0.0265(2) Uani 1 1 d . . . . .
C1 C 0.42907(13) 0.39551(10) 0.75408(14) 0.0245(5) Uani 1 1 d . . . . .
B1 B 0.500000 0.35125(16) 0.750000 0.0255(7) Uani 1 2 d S T P . .
C2 C 0.45831(13) 0.45444(10) 0.75494(13) 0.0226(5) Uani 1 1 d . . . . .
C003 C 0.40232(13) 0.56232(10) 0.70206(13) 0.0240(5) Uani 1 1 d . . . . .
H003 H 0.414251 0.556601 0.650879 0.029 Uiso 1 1 calc R U . . .
C3 C 0.32139(16) 0.36041(12) 0.85511(16) 0.0336(5) Uani 1 1 d . . . . .
H00P H 0.264449 0.350481 0.847704 0.050 Uiso 1 1 calc R U . . .
H00Q H 0.341272 0.397946 0.892706 0.050 Uiso 1 1 calc R U . . .
H00R H 0.358486 0.325060 0.884143 0.050 Uiso 1 1 calc R U . . .
C6 C 0.42012(13) 0.51407(10) 0.76500(13) 0.0225(5) Uani 1 1 d . . . . .
C5 C 0.28407(16) 0.30242(11) 0.67183(16) 0.0354(6) Uani 1 1 d . . . . .
H00A H 0.285323 0.309117 0.612996 0.053 Uiso 1 1 calc R U . . .
H00C H 0.226705 0.292936 0.663355 0.053 Uiso 1 1 calc R U . . .
H00F H 0.320725 0.267209 0.702477 0.053 Uiso 1 1 calc R U . . .
C4 C 0.24291(15) 0.43775(12) 0.68288(17) 0.0373(6) Uani 1 1 d . . . . .
H00G H 0.245595 0.447976 0.625592 0.056 Uiso 1 1 calc R U . . .
H4 H 0.255433 0.475344 0.720813 0.056 Uiso 1 1 calc R U . . .
H00I H 0.186658 0.422703 0.671241 0.056 Uiso 1 1 calc R U . . .
C8 C 0.36926(12) 0.57886(10) 0.85421(13) 0.0233(5) Uani 1 1 d . . . . .
C7 C 0.40323(13) 0.52326(10) 0.84124(14) 0.0228(5) Uani 1 1 d . . . . .
H7 H 0.415401 0.490662 0.884559 0.027 Uiso 1 1 calc R U . . .
C9 C 0.35173(14) 0.59142(10) 0.93778(14) 0.0257(5) Uani 1 1 d . . . . .
C10 C 0.40959(17) 0.64347(13) 0.99372(16) 0.0395(6) Uani 1 1 d . . . . .
H00V H 0.399284 0.681697 0.957299 0.059 Uiso 1 1 calc R U . . .
H00W H 0.467958 0.630457 1.012846 0.059 Uiso 1 1 calc R U . . .
H00X H 0.398702 0.651718 1.046944 0.059 Uiso 1 1 calc R U . . .
C13 C 0.35177(14) 0.62608(10) 0.78921(14) 0.0265(5) Uani 1 1 d . . . . .
H13 H 0.328449 0.664469 0.797497 0.032 Uiso 1 1 calc R U . . .
C12 C 0.26040(15) 0.61160(13) 0.90839(16) 0.0351(6) Uani 1 1 d . . . . .
H00J H 0.250888 0.651511 0.875819 0.053 Uiso 1 1 calc R U . . .
H00K H 0.248679 0.616720 0.961699 0.053 Uiso 1 1 calc R U . . .
H00L H 0.223273 0.579481 0.868873 0.053 Uiso 1 1 calc R U . . .
C11 C 0.36655(16) 0.53312(12) 0.99710(15) 0.0344(6) Uani 1 1 d . . . . .
H00M H 0.329200 0.499376 0.962310 0.052 Uiso 1 1 calc R U . . .
H00N H 0.355091 0.543085 1.049508 0.052 Uiso 1 1 calc R U . . .
H00O H 0.424836 0.519540 1.017497 0.052 Uiso 1 1 calc R U . . .
C16 C 0.3196(3) 0.73062(14) 0.6682(2) 0.0628(10) Uani 1 1 d . . . . .
H01A H 0.306348 0.761631 0.619878 0.094 Uiso 1 1 calc R U . . .
H01B H 0.365732 0.746183 0.722851 0.094 Uiso 1 1 calc R U . . .
H01C H 0.270230 0.723614 0.680486 0.094 Uiso 1 1 calc R U . . .
C20 C 0.51536(14) 0.24425(10) 0.68469(14) 0.0272(5) Uani 1 1 d . . . . .
H20 H 0.527628 0.266476 0.641181 0.033 Uiso 1 1 calc R U . . .
C21 C 0.51320(13) 0.17915(10) 0.68171(14) 0.0268(5) Uani 1 1 d . . . . .
C22 C 0.52409(15) 0.14129(10) 0.60718(15) 0.0299(5) Uani 1 1 d . . . . .
C23 C 0.54427(17) 0.18346(12) 0.54290(16) 0.0363(6) Uani 1 1 d . . . . .
H00S H 0.550321 0.157661 0.496264 0.054 Uiso 1 1 calc R U . . .
H00T H 0.596628 0.206040 0.576744 0.054 Uiso 1 1 calc R U . . .
H00U H 0.498784 0.213681 0.514541 0.054 Uiso 1 1 calc R U . . .
C24 C 0.59582(17) 0.09400(12) 0.64868(18) 0.0398(6) Uani 1 1 d . . . . .
H00Y H 0.601254 0.069473 0.600608 0.060 Uiso 1 1 calc R U . . .
H00Z H 0.583847 0.065791 0.689257 0.060 Uiso 1 1 calc R U . . .
H010 H 0.648183 0.116524 0.682699 0.060 Uiso 1 1 calc R U . . .
C25 C 0.44246(18) 0.10658(14) 0.55206(18) 0.0456(7) Uani 1 1 d . . . . .
H014 H 0.397560 0.137092 0.522770 0.068 Uiso 1 1 calc R U . . .
H015 H 0.427888 0.079628 0.592038 0.068 Uiso 1 1 calc R U . . .
H016 H 0.449637 0.080783 0.506076 0.068 Uiso 1 1 calc R U . . .
C26 C 0.500000 0.14782(14) 0.750000 0.0274(7) Uani 1 2 d S T P . .
H26 H 0.500001 0.103262 0.750000 0.033 Uiso 1 2 calc R U P . .
C15 C 0.34537(17) 0.66886(12) 0.63921(16) 0.0368(6) Uani 1 1 d . . . . .
C14 C 0.36747(14) 0.61862(10) 0.71257(14) 0.0264(5) Uani 1 1 d . . . . .
C18 C 0.27193(18) 0.64407(16) 0.55507(17) 0.0494(8) Uani 1 1 d . . . . .
H017 H 0.256701 0.675222 0.506673 0.074 Uiso 1 1 calc R U . . .
H018 H 0.223840 0.636264 0.569337 0.074 Uiso 1 1 calc R U . . .
H019 H 0.288352 0.604889 0.535455 0.074 Uiso 1 1 calc R U . . .
C19 C 0.500000 0.27834(14) 0.750000 0.0266(7) Uani 1 2 d S T P . .
C17 C 0.42007(19) 0.68167(12) 0.61600(18) 0.0425(6) Uani 1 1 d . . . . .
H011 H 0.437891 0.642387 0.598158 0.064 Uiso 1 1 calc R U . . .
H012 H 0.466435 0.699057 0.668873 0.064 Uiso 1 1 calc R U . . .
H013 H 0.403578 0.711749 0.566165 0.064 Uiso 1 1 calc R U . . .
C105 C -0.1171(11) 0.5539(8) 0.1474(13) 0.058(5) Uani 0.338(5) 1 d D U P A -1
H10A H -0.161072 0.548399 0.168894 0.087 Uiso 0.338(5) 1 calc R U P A -1
H10B H -0.077961 0.518577 0.167772 0.087 Uiso 0.338(5) 1 calc R U P A -1
H10C H -0.142394 0.555515 0.081372 0.087 Uiso 0.338(5) 1 calc R U P A -1
C104 C -0.0742(8) 0.6097(5) 0.1817(8) 0.073(3) Uani 0.338(5) 1 d D U P A -1
H10D H -0.115821 0.641954 0.178622 0.087 Uiso 0.338(5) 1 calc R U P A -1
H10E H -0.048258 0.623480 0.141271 0.087 Uiso 0.338(5) 1 calc R U P A -1
C103 C -0.0115(11) 0.6088(6) 0.2703(9) 0.096(5) Uani 0.338(5) 1 d D U P A -1
H10F H 0.031388 0.638201 0.268382 0.115 Uiso 0.338(5) 1 calc R U P A -1
H10G H -0.037488 0.630566 0.305824 0.115 Uiso 0.338(5) 1 calc R U P A -1
C102 C 0.0343(9) 0.5617(6) 0.3261(10) 0.089(4) Uani 0.338(5) 1 d D U P A -1
H12A H 0.004065 0.551010 0.363617 0.107 Uiso 0.338(5) 1 calc R U P A -1
H12B H 0.027321 0.525174 0.286164 0.107 Uiso 0.338(5) 1 calc R U P A -1
C101 C 0.1150(11) 0.5618(11) 0.3828(11) 0.084(5) Uani 0.338(5) 1 d D U P A -1
H10H H 0.136750 0.604706 0.389889 0.101 Uiso 0.338(5) 1 calc R U P A -1
H10I H 0.146245 0.535117 0.358583 0.101 Uiso 0.338(5) 1 calc R U P A -1
H10J H 0.121391 0.545545 0.441454 0.101 Uiso 0.338(5) 1 calc R U P A -1
C1A C 0.1176(17) 0.5630(16) 0.322(3) 0.059(7) Uani 0.162(5) 1 d D U P A -2
H1AA H 0.090094 0.562661 0.363048 0.071 Uiso 0.162(5) 1 calc R U P A -2
H1AB H 0.175951 0.576313 0.354337 0.071 Uiso 0.162(5) 1 calc R U P A -2
H1AC H 0.115976 0.520808 0.297294 0.071 Uiso 0.162(5) 1 calc R U P A -2
C2A C 0.0761(19) 0.6047(15) 0.251(2) 0.068(5) Uani 0.162(5) 1 d D U P A -2
H2AA H 0.054365 0.581424 0.193566 0.082 Uiso 0.162(5) 1 calc R U P A -2
H2AB H 0.116470 0.636338 0.249116 0.082 Uiso 0.162(5) 1 calc R U P A -2
C3A C 0.007(2) 0.6365(10) 0.261(3) 0.073(4) Uani 0.162(5) 1 d D U P A -2
H3AA H -0.020219 0.663296 0.206710 0.087 Uiso 0.162(5) 1 calc R U P A -2
H3AB H 0.031753 0.664914 0.313164 0.087 Uiso 0.162(5) 1 calc R U P A -2
C4A C -0.057(2) 0.6000(15) 0.272(2) 0.070(4) Uani 0.162(5) 1 d D U P A -2
H4AA H -0.034191 0.580890 0.332421 0.084 Uiso 0.162(5) 1 calc R U P A -2
H4AB H -0.103823 0.627997 0.266674 0.084 Uiso 0.162(5) 1 calc R U P A -2
C5A C -0.088(2) 0.5530(13) 0.207(2) 0.073(6) Uani 0.162(5) 1 d D U P A -2
H5AA H -0.071895 0.562070 0.157473 0.109 Uiso 0.162(5) 1 calc R U P A -2
H5AB H -0.148646 0.551127 0.184396 0.109 Uiso 0.162(5) 1 calc R U P A -2
H5AC H -0.063550 0.512645 0.234570 0.109 Uiso 0.162(5) 1 calc R U P A -2
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'
Si Si 0.0817 0.0704 '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
C3 Si1 C4 109.09(12) . .
C3 Si1 C1 110.52(10) . .
C4 Si1 C1 112.61(11) . .
C3 Si1 C5 108.65(11) . .
C4 Si1 C5 106.21(12) . .
C1 Si1 C5 109.61(10) . .
C2 C1 B1 104.51(19) . .
C2 C1 Si1 125.34(16) . .
B1 C1 Si1 129.51(16) . .
C19 B1 C1 126.49(13) . .
C19 B1 C1 126.49(13) . 2_656
C1 B1 C1 107.0(3) . 2_656
C1 C2 C6 127.63(19) . .
C1 C2 C2 111.86(12) . 2_656
C6 C2 C2 120.51(11) . 2_656
C14 C003 C6 121.43(19) . .
C003 C6 C7 118.90(19) . .
C003 C6 C2 121.72(18) . .
C7 C6 C2 119.36(18) . .
C7 C8 C13 118.22(19) . .
C7 C8 C9 122.85(18) . .
C13 C8 C9 118.91(19) . .
C8 C7 C6 121.19(19) . .
C10 C9 C11 108.49(19) . .
C10 C9 C12 109.5(2) . .
C11 C9 C12 107.83(19) . .
C10 C9 C8 109.07(17) . .
C11 C9 C8 112.00(18) . .
C12 C9 C8 109.94(17) . .
C14 C13 C8 122.2(2) . .
C21 C20 C19 122.1(2) . .
C20 C21 C26 117.4(2) . .
C20 C21 C22 122.82(19) . .
C26 C21 C22 119.8(2) . .
C25 C22 C23 108.0(2) . .
C25 C22 C24 109.8(2) . .
C23 C22 C24 107.8(2) . .
C25 C22 C21 108.90(19) . .
C23 C22 C21 112.00(18) . .
C24 C22 C21 110.25(18) . .
C21 C26 C21 123.0(3) . 2_656
C16 C15 C14 111.81(19) . .
C16 C15 C18 109.0(2) . .
C14 C15 C18 107.7(2) . .
C16 C15 C17 108.5(2) . .
C14 C15 C17 110.7(2) . .
C18 C15 C17 109.1(2) . .
C003 C14 C13 118.03(19) . .
C003 C14 C15 119.27(19) . .
C13 C14 C15 122.68(19) . .
C20 C19 C20 117.7(3) 2_656 .
C20 C19 B1 121.13(14) 2_656 .
C20 C19 B1 121.13(14) . .
C105 C104 C103 117.6(12) . .
C102 C103 C104 133.2(13) . .
C101 C102 C103 128.4(15) . .
C1A C2A C3A 113(2) . .
C2A C3A C4A 119.5(17) . .
C5A C4A C3A 111.6(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C3 1.871(2) .
Si1 C4 1.872(3) .
Si1 C1 1.872(2) .
Si1 C5 1.878(2) .
C1 C2 1.355(3) .
C1 B1 1.587(3) .
B1 C19 1.554(5) .
C2 C6 1.478(3) .
C2 C2 1.540(4) 2_656
C003 C14 1.390(3) .
C003 C6 1.394(3) .
C6 C7 1.408(3) .
C8 C7 1.383(3) .
C8 C13 1.401(3) .
C8 C9 1.542(3) .
C9 C10 1.525(3) .
C9 C11 1.530(3) .
C9 C12 1.533(3) .
C13 C14 1.397(3) .
C16 C15 1.530(4) .
C20 C21 1.389(3) .
C20 C19 1.406(3) .
C21 C26 1.399(3) .
C21 C22 1.537(3) .
C22 C25 1.530(3) .
C22 C23 1.531(3) .
C22 C24 1.534(3) .
C15 C14 1.531(3) .
C15 C18 1.535(4) .
C15 C17 1.535(4) .
C105 C104 1.395(15) .
C104 C103 1.407(13) .
C103 C102 1.370(12) .
C102 C101 1.332(16) .
C1A C2A 1.395(18) .
C2A C3A 1.446(16) .
C3A C4A 1.449(15) .
C4A C5A 1.386(19) .
