#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:06:09 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180003 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/97/7029754.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_7029754
loop_
_publ_author_name
'Kořenková, Monika'
'Mairychová, Barbora'
'R°užička, Aleš'
'Jambor, Roman'
'Dostál, Libor'
_publ_section_title
;
 Synthesis of heteroboroxines with MB2O3 core (M = Sb, Bi, Sn)-an
 influence of the substitution of parent boronic acids.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7096
_journal_page_last               7108
_journal_paper_doi               10.1039/c3dt53012d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C24 H27 B2 Bi Br2 N2 O3'
_chemical_formula_sum            'C24 H27 B2 Bi Br2 N2 O3'
_chemical_formula_weight         781.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5821(7)
_cell_length_b                   23.4640(6)
_cell_length_c                   9.1219(17)
_cell_measurement_reflns_used    24099
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      1
_cell_volume                     2693.0(5)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23911
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.542
_exptl_absorpt_correction_T_max  0.341
_exptl_absorpt_correction_T_min  0.145
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0127P)²+5.4686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                3023
_reflns_number_total             3453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53012d2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-12899/cifs/7029754.cif.
;
_cod_database_code               7029754
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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
Bi1 Bi 0.353968(12) 0.2500 0.960500(17) 0.01840(5) Uani 1 2 d S
O2 O 0.0950(2) 0.2500 1.0968(4) 0.0227(7) Uani 1 2 d S
O1 O 0.24338(17) 0.18778(10) 1.0491(2) 0.0233(5) Uani 1 1 d .
C10 C -0.1065(3) 0.11031(15) 1.2023(4) 0.0254(7) Uani 1 1 d .
H10 H -0.1767 0.1172 1.2289 0.030 Uiso 1 1 d R
C11 C -0.0681(3) 0.05534(14) 1.1929(4) 0.0248(7) Uani 1 1 d .
C12 C 0.0357(3) 0.04393(15) 1.1543(4) 0.0275(7) Uani 1 1 d .
H12 H 0.0604 0.0067 1.1481 0.033 Uiso 1 1 d R
C13 C 0.1025(2) 0.08960(14) 1.1247(3) 0.0218(7) Uani 1 1 d .
H13 H 0.1727 0.0824 1.0991 0.026 Uiso 1 1 d R
B1 B 0.1430(3) 0.19696(15) 1.0885(4) 0.0190(7) Uani 1 1 d .
C9 C -0.0379(2) 0.15485(14) 1.1728(4) 0.0221(6) Uani 1 1 d .
H9 H -0.0630 0.1920 1.1805 0.026 Uiso 1 1 d R
C8 C 0.0684(2) 0.14563(14) 1.1324(3) 0.0187(6) Uani 1 1 d .
N1 N 0.3912(2) 0.34843(13) 0.8210(3) 0.0239(6) Uani 1 1 d .
C2 C 0.2572(2) 0.30163(15) 0.6699(4) 0.0234(7) Uani 1 1 d .
C1 C 0.2777(3) 0.2500 0.7389(5) 0.0205(9) Uani 1 2 d S
C3 C 0.2076(3) 0.30131(18) 0.5321(4) 0.0310(8) Uani 1 1 d .
H3 H 0.1942 0.3356 0.4843 0.037 Uiso 1 1 d R
C4 C 0.1805(4) 0.2500 0.4671(6) 0.0352(13) Uani 1 2 d S
H4 H 0.1428 0.2500 0.3794 0.042 Uiso 1 2 d SR
C6 C 0.4804(3) 0.34064(18) 0.7194(4) 0.0327(8) Uani 1 1 d .
H6A H 0.4869 0.3738 0.6584 0.039 Uiso 1 1 d R
H6B H 0.4676 0.3078 0.6592 0.039 Uiso 1 1 d R
H6C H 0.5449 0.3353 0.7739 0.039 Uiso 1 1 d R
C5 C 0.2914(3) 0.35670(15) 0.7403(4) 0.0261(7) Uani 1 1 d .
H5A H 0.3021 0.3853 0.6649 0.031 Uiso 1 1 d R
H5B H 0.2365 0.3702 0.8063 0.031 Uiso 1 1 d R
C7 C 0.4127(3) 0.39748(17) 0.9168(4) 0.0334(8) Uani 1 1 d .
H7A H 0.4773 0.3913 0.9705 0.040 Uiso 1 1 d R
H7B H 0.3548 0.4023 0.9843 0.040 Uiso 1 1 d R
H7C H 0.4197 0.4311 0.8576 0.040 Uiso 1 1 d R
Br1 Br -0.16098(3) -0.006269(16) 1.23575(5) 0.04339(11) Uani 1 1 d .
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'
O O 0.0106 0.0060 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 '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
0 0 1 0.039
0 0 -1 0.082
-1 1 0 0.065
1 -1 0 0.175
1 1 0 0.168
-1 -1 0 0.116
0 1 0 0.177
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
O1 Bi1 O1 84.44(12) . 8_565
O1 Bi1 C1 93.52(10) . .
O1 Bi1 C1 93.52(10) 8_565 .
O1 Bi1 N1 73.09(8) . 8_565
O1 Bi1 N1 150.25(8) 8_565 8_565
C1 Bi1 N1 69.26(7) . 8_565
O1 Bi1 N1 150.25(8) . .
O1 Bi1 N1 73.09(8) 8_565 .
C1 Bi1 N1 69.26(7) . .
N1 Bi1 N1 119.18(12) 8_565 .
B1 O2 B1 127.9(4) . 8_565
B1 O1 Bi1 126.8(2) . .
C11 C10 C9 118.4(3) . .
C11 C10 H10 120.7 . .
C9 C10 H10 120.9 . .
C12 C11 C10 121.9(3) . .
C12 C11 Br1 119.2(3) . .
C10 C11 Br1 118.9(2) . .
C11 C12 C13 118.2(3) . .
C11 C12 H12 121.0 . .
C13 C12 H12 120.8 . .
C8 C13 C12 122.4(3) . .
C8 C13 H13 118.7 . .
C12 C13 H13 118.9 . .
O1 B1 O2 125.0(3) . .
O1 B1 C8 120.6(3) . .
O2 B1 C8 114.4(3) . .
C10 C9 C8 122.0(3) . .
C10 C9 H9 118.8 . .
C8 C9 H9 119.2 . .
C13 C8 C9 117.0(3) . .
C13 C8 B1 121.9(3) . .
C9 C8 B1 121.0(3) . .
C6 N1 C5 110.7(3) . .
C6 N1 C7 109.4(3) . .
C5 N1 C7 110.6(3) . .
C6 N1 Bi1 109.1(2) . .
C5 N1 Bi1 101.69(19) . .
C7 N1 Bi1 115.2(2) . .
C1 C2 C3 118.9(3) . .
C1 C2 C5 120.1(3) . .
C3 C2 C5 120.9(3) . .
C2 C1 C2 121.3(4) 8_565 .
C2 C1 Bi1 119.3(2) 8_565 .
C2 C1 Bi1 119.3(2) . .
C4 C3 C2 119.9(4) . .
C4 C3 H3 120.4 . .
C2 C3 H3 119.7 . .
C3 C4 C3 120.8(5) 8_565 .
C3 C4 H4 119.6 8_565 .
C3 C4 H4 119.6 . .
N1 C6 H6A 109.3 . .
N1 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N1 C6 H6C 109.6 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N1 C5 C2 110.2(3) . .
N1 C5 H5A 109.2 . .
C2 C5 H5A 109.3 . .
N1 C5 H5B 110.0 . .
C2 C5 H5B 109.9 . .
H5A C5 H5B 108.2 . .
N1 C7 H7A 109.9 . .
N1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N1 C7 H7C 109.0 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 O1 2.173(2) .
Bi1 O1 2.173(2) 8_565
Bi1 C1 2.237(4) .
Bi1 N1 2.678(3) 8_565
Bi1 N1 2.678(3) .
O2 B1 1.385(4) .
O2 B1 1.385(4) 8_565
O1 B1 1.331(4) .
C10 C11 1.380(5) .
C10 C9 1.381(5) .
C10 H10 0.9300 .
C11 C12 1.378(5) .
C11 Br1 1.900(3) .
C12 C13 1.388(5) .
C12 H12 0.9300 .
C13 C8 1.384(5) .
C13 H13 0.9300 .
B1 C8 1.578(5) .
C9 C8 1.405(4) .
C9 H9 0.9301 .
N1 C6 1.467(4) .
N1 C5 1.468(4) .
N1 C7 1.470(5) .
C2 C1 1.390(4) .
C2 C3 1.403(5) .
C2 C5 1.506(5) .
C1 C2 1.389(4) 8_565
C3 C4 1.385(5) .
C3 H3 0.9299 .
C4 C3 1.385(5) 8_565
C4 H4 0.9300 .
C6 H6A 0.9600 .
C6 H6B 0.9599 .
C6 H6C 0.9600 .
C5 H5A 0.9699 .
C5 H5B 0.9700 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
