#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:27:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179750 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004652.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_7004652
loop_
_publ_author_name
'Schwan, Karl-Christian'
'Adolf, Ariane'
'Thoms, Christine'
'Zabel, Manfred'
'Timoshkin, Alexey Y.'
'Scheer, Manfred'
_publ_section_title
;
 Selective halogenation at the pnictogen atom in
 Lewis-acid/base-stabilised phosphanylboranes and arsanylboranes
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              5054
_journal_page_last               5058
_journal_paper_doi               10.1039/b809773a
_journal_year                    2008
_chemical_formula_sum            'C8 H11 B Br2 N O5 P W'
_chemical_formula_weight         586.63
_chemical_name_systematic
;
?
;
_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                 131.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.639(6)
_cell_length_b                   7.3060(15)
_cell_length_c                   20.260(4)
_cell_measurement_reflns_used    1335
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      2.75
_cell_volume                     3262.3(19)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software'
_computing_molecular_graphics    SIEMENS-XP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9641
_diffrn_reflns_theta_full        22.35
_diffrn_reflns_theta_max         22.35
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    6.493
_exptl_absorpt_correction_T_max  0.3448
_exptl_absorpt_correction_T_min  0.2258
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0359P)²+7.0264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                3654
_reflns_number_total             4062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809773a.txt
_cod_data_source_block           br6a
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7004652
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
W W 0.141376(6) 0.632170(19) 0.456442(9) 0.02637(6) Uani 1 1 d . . .
C1 C 0.22186(19) 0.4915(6) 0.5248(3) 0.0331(8) Uani 1 1 d . . .
O1 O 0.26601(16) 0.4109(5) 0.5629(2) 0.0479(8) Uani 1 1 d . . .
C2 C 0.1876(2) 0.8681(5) 0.5261(3) 0.0349(9) Uani 1 1 d . . .
O2 O 0.2136(2) 0.9965(5) 0.5653(3) 0.0567(10) Uani 1 1 d . . .
C3 C 0.0591(2) 0.7601(6) 0.3850(3) 0.0389(9) Uani 1 1 d . . .
O3 O 0.01201(19) 0.8255(7) 0.3415(3) 0.0639(11) Uani 1 1 d . . .
C4 C 0.0965(2) 0.3944(7) 0.3905(3) 0.0422(10) Uani 1 1 d . . .
O4 O 0.0720(2) 0.2626(6) 0.3543(3) 0.0709(12) Uani 1 1 d . . .
C5 C 0.1434(2) 0.7098(6) 0.3632(3) 0.0347(8) Uani 1 1 d . . .
O5 O 0.14435(19) 0.7552(5) 0.3103(2) 0.0526(9) Uani 1 1 d . . .
P P 0.14342(4) 0.56629(12) 0.57867(6) 0.02462(17) Uani 1 1 d . . .
Br2 Br 0.120372(19) 0.27362(5) 0.58148(3) 0.03595(10) Uani 1 1 d . . .
Br1 Br 0.239805(19) 0.57894(7) 0.70886(3) 0.04003(11) Uani 1 1 d . . .
B B 0.0959(2) 0.7337(6) 0.5875(3) 0.0295(8) Uani 1 1 d . . .
H1 H 0.048(2) 0.736(7) 0.522(3) 0.037(13) Uiso 1 1 d . . .
H2 H 0.113(4) 0.857(10) 0.598(5) 0.08(2) Uiso 1 1 d . . .
N N 0.09016(17) 0.7103(5) 0.6602(2) 0.0326(7) Uani 1 1 d . . .
C6 C 0.0494(2) 0.5549(7) 0.6394(3) 0.0401(9) Uani 1 1 d . . .
H6A H 0.0670 0.4405 0.6416 0.060 Uiso 1 1 calc R . .
H6B H 0.0100 0.5716 0.5805 0.060 Uiso 1 1 calc R . .
H6C H 0.0449 0.5520 0.6826 0.060 Uiso 1 1 calc R . .
C7 C 0.0599(4) 0.8828(7) 0.6552(6) 0.072(2) Uani 1 1 d . . .
H7A H 0.0548 0.8759 0.6977 0.108 Uiso 1 1 calc R . .
H7B H 0.0204 0.8956 0.5958 0.108 Uiso 1 1 calc R . .
H7C H 0.0849 0.9878 0.6687 0.108 Uiso 1 1 calc R . .
C8 C 0.1494(3) 0.6840(10) 0.7522(3) 0.0587(15) Uani 1 1 d . . .
H8A H 0.1437 0.6937 0.7939 0.088 Uiso 1 1 calc R . .
H8B H 0.1777 0.7773 0.7654 0.088 Uiso 1 1 calc R . .
H8C H 0.1655 0.5640 0.7572 0.088 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 0.0015 0.0009 '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 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.1811 1.6452 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.4201 4.6430 '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
C5 W C4 92.30(18) . . ?
C5 W C3 88.70(18) . . ?
C4 W C3 88.8(2) . . ?
C5 W C1 91.36(17) . . ?
C4 W C1 88.29(19) . . ?
C3 W C1 177.10(18) . . ?
C5 W C2 89.10(17) . . ?
C4 W C2 178.42(18) . . ?
C3 W C2 91.96(19) . . ?
C1 W C2 90.94(18) . . ?
C5 W P 174.32(12) . . ?
C4 W P 93.35(14) . . ?
C3 W P 90.93(13) . . ?
C1 W P 89.30(12) . . ?
C2 W P 85.25(12) . . ?
O1 C1 W 178.7(4) . . ?
O2 C2 W 179.1(6) . . ?
O3 C3 W 176.3(4) . . ?
O4 C4 W 179.7(5) . . ?
O5 C5 W 179.4(4) . . ?
B P Br1 107.09(15) . . ?
B P Br2 109.93(14) . . ?
Br1 P Br2 100.25(4) . . ?
B P W 115.45(14) . . ?
Br1 P W 109.07(5) . . ?
Br2 P W 113.75(4) . . ?
N B P 122.8(3) . . ?
C8 N C6 108.0(4) . . ?
C8 N C7 110.1(5) . . ?
C6 N C7 106.4(4) . . ?
C8 N B 113.7(4) . . ?
C6 N B 112.5(3) . . ?
C7 N B 105.8(4) . . ?
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
W C5 2.012(4) . ?
W C4 2.048(5) . ?
W C3 2.049(5) . ?
W C1 2.061(4) . ?
W C2 2.063(4) . ?
W P 2.4835(11) . ?
C1 O1 1.142(5) . ?
C2 O2 1.134(5) . ?
C3 O3 1.143(6) . ?
C4 O4 1.131(6) . ?
C5 O5 1.140(5) . ?
P B 1.961(4) . ?
P Br1 2.2474(17) . ?
P Br2 2.2569(10) . ?
B N 1.602(5) . ?
N C8 1.489(7) . ?
N C6 1.498(5) . ?
N C7 1.511(6) . ?
