#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/28/7012889.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_7012889
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 H6 B3 N3'
_chemical_formula_weight         152.57
_chemical_melting_point          405
_chemical_name_common            triethynylborazine
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 116.641(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.792(3)
_cell_length_b                   3.9345(5)
_cell_length_c                   23.671(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1897.3(4)
_computing_molecular_graphics    ORTEP32
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            8798
_diffrn_reflns_theta_full        32.89
_diffrn_reflns_theta_max         32.89
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   empirical(SADABS)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0832P)²+0.0949P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1641
_reflns_number_gt                2127
_reflns_number_total             3156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302275g.txt
_cod_data_source_block           B-triethynylborazine_(4a)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7012889
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N 0.28327(4) 0.0592(2) 0.67616(4) 0.0470(2) Uani 1 1 d . . .
H2A H 0.2519 0.1495 0.6818 0.056 Uiso 1 1 calc R . .
N3 N 0.32630(4) -0.1499(2) 0.60554(4) 0.0486(2) Uani 1 1 d . . .
H3A H 0.3211 -0.1920 0.5679 0.058 Uiso 1 1 calc R . .
N1 N 0.39450(4) -0.1608(3) 0.71916(4) 0.0478(2) Uani 1 1 d . . .
H1A H 0.4313 -0.2063 0.7511 0.057 Uiso 1 1 calc R . .
C21 C 0.20734(6) 0.0807(3) 0.55596(5) 0.0518(3) Uani 1 1 d . . .
B3 B 0.38763(6) -0.2283(3) 0.65774(6) 0.0456(3) Uani 1 1 d . . .
B1 B 0.34293(6) -0.0207(3) 0.73011(5) 0.0438(3) Uani 1 1 d . . .
C11 C 0.35113(5) 0.0395(3) 0.79778(5) 0.0493(3) Uani 1 1 d . . .
B2 B 0.27327(6) -0.0041(3) 0.61343(6) 0.0448(3) Uani 1 1 d . . .
C22 C 0.15676(6) 0.1453(4) 0.51242(6) 0.0666(4) Uani 1 1 d . . .
H22 H 0.1169 0.1963 0.4781 0.080 Uiso 1 1 calc R . .
C31 C 0.44485(5) -0.3854(3) 0.64827(5) 0.0543(3) Uani 1 1 d . . .
C12 C 0.35681(6) 0.0845(4) 0.84936(6) 0.0628(3) Uani 1 1 d . . .
H12 H 0.3613 0.1198 0.8899 0.075 Uiso 1 1 calc R . .
C32 C 0.48901(6) -0.5097(5) 0.64264(7) 0.0735(4) Uani 1 1 d . . .
H32 H 0.5238 -0.6077 0.6382 0.088 Uiso 1 1 calc R . .
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
N2 0.0372(4) 0.0589(5) 0.0467(5) -0.0001(4) 0.0204(4) 0.0073(4)
N3 0.0421(4) 0.0627(6) 0.0425(4) -0.0022(4) 0.0202(3) 0.0064(4)
N1 0.0356(4) 0.0611(5) 0.0440(4) 0.0009(4) 0.0155(3) 0.0065(4)
C21 0.0453(5) 0.0629(7) 0.0464(5) 0.0001(5) 0.0199(4) 0.0085(5)
B3 0.0382(5) 0.0504(6) 0.0504(6) -0.0020(5) 0.0217(4) 0.0018(5)
B1 0.0392(6) 0.0491(6) 0.0444(5) -0.0001(5) 0.0198(4) -0.0021(5)
C11 0.0406(5) 0.0602(6) 0.0489(5) -0.0006(5) 0.0217(4) -0.0016(5)
B2 0.0385(5) 0.0496(6) 0.0457(6) 0.0025(5) 0.0184(4) 0.0021(5)
C22 0.0538(7) 0.0880(10) 0.0488(6) 0.0010(6) 0.0146(5) 0.0164(6)
C31 0.0411(5) 0.0677(7) 0.0514(6) -0.0095(5) 0.0183(4) 0.0035(5)
C12 0.0574(7) 0.0849(9) 0.0523(6) -0.0063(6) 0.0301(5) -0.0056(6)
C32 0.0438(6) 0.1020(11) 0.0708(8) -0.0243(8) 0.0222(6) 0.0106(7)
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'
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
B2 N2 B1 122.77(9) . . ?
B3 N3 B2 122.30(9) . . ?
B3 N1 B1 122.65(9) . . ?
C22 C21 B2 179.43(12) . . ?
N1 B3 N3 117.65(9) . . ?
N1 B3 C31 120.75(9) . . ?
N3 B3 C31 121.60(10) . . ?
N2 B1 N1 117.21(9) . . ?
N2 B1 C11 121.31(9) . . ?
N1 B1 C11 121.47(9) . . ?
C12 C11 B1 179.37(11) . . ?
N2 B2 N3 117.40(9) . . ?
N2 B2 C21 121.32(9) . . ?
N3 B2 C21 121.28(9) . . ?
C32 C31 B3 178.15(14) . . ?
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
N2 B2 1.4195(14) . ?
N2 B1 1.4216(15) . ?
N3 B3 1.4236(15) . ?
N3 B2 1.4239(14) . ?
N1 B3 1.4157(15) . ?
N1 B1 1.4235(14) . ?
C21 C22 1.1791(16) . ?
C21 B2 1.5449(16) . ?
B3 C31 1.5479(15) . ?
B1 C11 1.5454(15) . ?
C11 C12 1.1820(16) . ?
C31 C32 1.1791(16) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21146212
