#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/28/7012891.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_7012891
loop_
_publ_author_name
'Jörg Haberecht'
'Anja Krummland'
'Frank Breher'
'Björn Gebhardt'
'Heinz Rüegger'
'Reinhard Nesper'
'Hansjörg Grützmacher'
_publ_section_title
;
 Functionalized borazines as precursors for new silica gels
;
_journal_issue                   11
_journal_name_full               'Dalton Trans.'
_journal_page_first              2126
_journal_page_last               2132
_journal_paper_doi               10.1039/b302275g
_journal_year                    2003
_chemical_formula_sum            'C6 H9 B3 Cl9 N3 Si3'
_chemical_formula_weight         558.91
_chemical_name_common            B-tris(E-trichlorosilylvinyl)borazine&#x00A0;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.250(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2678(16)
_cell_length_b                   11.1725(13)
_cell_length_c                   15.6744(17)
_cell_measurement_temperature    233(2)
_cell_volume                     2321.7(5)
_computing_molecular_graphics    'ORTEP31, POVRAY for Windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART with CCD Area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22017
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  0.8657
_exptl_absorpt_correction_T_min  0.2141
_exptl_absorpt_correction_type   'empirical (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          1.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         7068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          1.240
_refine_ls_shift/su_mean         0.219
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0657P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                3893
_reflns_number_total             7068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302275g.txt
_cod_data_source_block           B-tris(E-trichlorosilylvinyl)borazine_(beta-5):
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012891
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl33 Cl 0.61983(6) 0.05365(7) 0.28387(4) 0.0596(2) Uani 1 1 d . . .
Si1 Si 0.89043(6) 0.78056(6) -0.07910(5) 0.04425(18) Uani 1 1 d . . .
Si2 Si 0.97451(6) 0.08156(7) -0.35024(4) 0.04400(18) Uani 1 1 d . . .
Cl13 Cl 0.76161(6) 0.85248(6) -0.13221(6) 0.0627(2) Uani 1 1 d . . .
Cl23 Cl 0.88615(6) -0.06455(8) -0.36267(5) 0.0694(2) Uani 1 1 d . . .
Si3 Si 0.60871(6) -0.03630(6) 0.17119(4) 0.04223(18) Uani 1 1 d . . .
Cl12 Cl 0.90095(7) 0.83698(7) 0.04310(5) 0.0697(2) Uani 1 1 d . . .
Cl22 Cl 1.11888(6) 0.02473(8) -0.33313(6) 0.0708(2) Uani 1 1 d . . .
Cl21 Cl 0.96585(9) 0.17734(9) -0.45926(5) 0.0888(3) Uani 1 1 d . . .
Cl32 Cl 0.67035(8) -0.19999(7) 0.18944(6) 0.0767(3) Uani 1 1 d . . .
Cl11 Cl 1.00743(7) 0.84892(8) -0.14230(6) 0.0728(2) Uani 1 1 d . . .
Cl31 Cl 0.46018(7) -0.06032(12) 0.14320(7) 0.0974(4) Uani 1 1 d . . .
N3 N 0.79374(16) 0.15995(16) -0.05637(12) 0.0382(5) Uani 1 1 d . . .
H3A H 0.7763 0.0863 -0.0630 0.046 Uiso 1 1 calc R . .
N2 N 0.86982(16) 0.34028(16) -0.11083(12) 0.0390(5) Uani 1 1 d . . .
H2A H 0.9014 0.3769 -0.1500 0.047 Uiso 1 1 calc R . .
N1 N 0.79929(17) 0.33958(17) 0.02911(12) 0.0413(5) Uani 1 1 d . . .
H1A H 0.7881 0.3761 0.0761 0.050 Uiso 1 1 calc R . .
C32 C 0.6713(2) 0.0448(2) 0.08727(15) 0.0425(6) Uani 1 1 d . . .
H32A H 0.6714 0.0085 0.0339 0.051 Uiso 1 1 calc R . .
C31 C 0.7164(2) 0.1494(2) 0.09451(15) 0.0404(6) Uani 1 1 d . . .
H31A H 0.7161 0.1864 0.1477 0.048 Uiso 1 1 calc R . .
C22 C 0.9401(2) 0.1721(2) -0.25940(15) 0.0443(6) Uani 1 1 d . . .
H22A H 0.9748 0.2436 -0.2504 0.053 Uiso 1 1 calc R . .
B2 B 0.8440(2) 0.2168(2) -0.12365(17) 0.0367(6) Uani 1 1 d . . .
B1 B 0.8455(2) 0.4045(2) -0.03667(17) 0.0387(6) Uani 1 1 d . . .
B3 B 0.7706(2) 0.2177(2) 0.02146(16) 0.0364(6) Uani 1 1 d . . .
C11 C 0.8654(2) 0.5433(2) -0.02800(16) 0.0494(7) Uani 1 1 d . . .
H11A H 0.8631 0.5749 0.0268 0.059 Uiso 1 1 calc R . .
C21 C 0.8707(2) 0.1450(2) -0.20580(15) 0.0421(6) Uani 1 1 d . . .
H21A H 0.8334 0.0761 -0.2175 0.050 Uiso 1 1 calc R . .
C12 C 0.8844(2) 0.6179(2) -0.08769(17) 0.0526(7) Uani 1 1 d . . .
H12A H 0.8964 0.5854 -0.1410 0.063 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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
C12 Si1 Cl12 112.52(10) . . ?
C12 Si1 Cl11 111.85(10) . . ?
Cl12 Si1 Cl11 108.74(5) . . ?
C12 Si1 Cl13 109.23(11) . . ?
Cl12 Si1 Cl13 106.90(5) . . ?
Cl11 Si1 Cl13 107.37(5) . . ?
C22 Si2 Cl23 111.29(9) . . ?
C22 Si2 Cl21 111.14(9) . . ?
Cl23 Si2 Cl21 109.55(6) . . ?
C22 Si2 Cl22 109.62(10) . . ?
Cl23 Si2 Cl22 107.60(5) . . ?
Cl21 Si2 Cl22 107.51(5) . . ?
C32 Si3 Cl32 111.02(9) . . ?
C32 Si3 Cl31 112.18(9) . . ?
Cl32 Si3 Cl31 107.26(6) . . ?
C32 Si3 Cl33 111.19(9) . . ?
Cl32 Si3 Cl33 108.03(5) . . ?
Cl31 Si3 Cl33 106.93(5) . . ?
B2 N3 B3 123.9(2) . . ?
B1 N2 B2 122.9(2) . . ?
B3 N1 B1 123.5(2) . . ?
C31 C32 Si3 126.7(2) . . ?
C32 C31 B3 125.9(2) . . ?
C21 C22 Si2 125.4(2) . . ?
N3 B2 N2 116.3(2) . . ?
N3 B2 C21 120.6(2) . . ?
N2 B2 C21 123.1(2) . . ?
N2 B1 N1 117.2(2) . . ?
N2 B1 C11 121.8(2) . . ?
N1 B1 C11 121.0(2) . . ?
N1 B3 N3 116.2(2) . . ?
N1 B3 C31 122.2(2) . . ?
N3 B3 C31 121.6(2) . . ?
C12 C11 B1 127.7(2) . . ?
C22 C21 B2 126.7(2) . . ?
C11 C12 Si1 127.0(2) . . ?
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
Cl33 Si3 2.0325(10) . ?
Si1 C12 1.824(3) . ?
Si1 Cl12 2.0160(11) . ?
Si1 Cl11 2.0238(11) . ?
Si1 Cl13 2.0367(10) . ?
Si2 C22 1.819(2) . ?
Si2 Cl23 2.0148(11) . ?
Si2 Cl21 2.0157(11) . ?
Si2 Cl22 2.0258(11) . ?
Si3 C32 1.824(2) . ?
Si3 Cl32 2.0190(11) . ?
Si3 Cl31 2.0200(12) . ?
N3 B2 1.420(3) . ?
N3 B3 1.424(3) . ?
N2 B1 1.414(3) . ?
N2 B2 1.434(3) . ?
N1 B3 1.418(3) . ?
N1 B1 1.419(3) . ?
C32 C31 1.316(3) . ?
C31 B3 1.573(3) . ?
C22 C21 1.306(3) . ?
B2 C21 1.569(3) . ?
B1 C11 1.578(4) . ?
C11 C12 1.285(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 28549248
