#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:27:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179750 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004650.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_7004650
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 Cl2 N O5 P W'
_chemical_formula_weight         497.71
_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                 132.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.459(6)
_cell_length_b                   7.1490(14)
_cell_length_c                   20.408(4)
_cell_measurement_reflns_used    847
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.00
_cell_volume                     3146.9(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 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       rotation
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9146
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    7.792
_exptl_absorpt_correction_T_max  0.6321
_exptl_absorpt_correction_T_min  0.4602
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.770
_refine_diff_density_min         -4.214
_refine_diff_density_rms         0.307
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.104
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0902P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                2624
_reflns_number_total             2974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809773a.txt
_cod_data_source_block           li
_cod_original_cell_volume        3147.0(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7004650
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
W1 W 0.142512(9) 0.12732(4) 0.457296(14) 0.02785(16) Uani 1 1 d . . .
Cl1 Cl 0.12345(8) -0.2076(3) 0.58402(12) 0.0416(4) Uani 1 1 d . . .
Cl2 Cl 0.23577(8) 0.0752(3) 0.70163(11) 0.0462(4) Uani 1 1 d . . .
P1 P 0.14535(7) 0.0649(3) 0.57949(10) 0.0277(3) Uani 1 1 d . . .
O1 O 0.2125(3) 0.5050(9) 0.5644(4) 0.0510(14) Uani 1 1 d . . .
O2 O 0.0095(2) 0.3166(11) 0.3378(4) 0.0578(16) Uani 1 1 d . . .
O3 O 0.0742(3) -0.2564(12) 0.3586(5) 0.075(2) Uani 1 1 d . . .
O4 O 0.2708(2) -0.0896(9) 0.5673(4) 0.0464(13) Uani 1 1 d . . .
O5 O 0.1451(3) 0.2464(8) 0.3110(4) 0.0474(13) Uani 1 1 d . . .
N1 N 0.0914(3) 0.2149(9) 0.6575(4) 0.0351(13) Uani 1 1 d . . .
C1 C 0.1878(4) 0.3737(11) 0.5264(5) 0.0398(18) Uani 1 1 d . . .
C2 C 0.0576(3) 0.2551(12) 0.3823(5) 0.0391(16) Uani 1 1 d . . .
C3 C 0.0985(4) -0.1206(10) 0.3939(5) 0.0382(17) Uani 1 1 d . . .
C4 C 0.2251(3) -0.0110(11) 0.5287(4) 0.0333(14) Uani 1 1 d . . .
C5 C 0.1441(3) 0.2021(11) 0.3639(4) 0.0341(14) Uani 1 1 d . . .
C6 C 0.0496(3) 0.0592(12) 0.6353(5) 0.0395(15) Uani 1 1 d . . .
H6A H 0.0650 -0.0570 0.6321 0.059 Uiso 1 1 calc R . .
H6B H 0.0082 0.0836 0.5779 0.059 Uiso 1 1 calc R . .
H6C H 0.0481 0.0494 0.6812 0.059 Uiso 1 1 calc R . .
C7 C 0.1523(4) 0.1858(17) 0.7507(5) 0.061(3) Uani 1 1 d . . .
H7A H 0.1467 0.1958 0.7923 0.092 Uiso 1 1 calc R . .
H7B H 0.1815 0.2801 0.7649 0.092 Uiso 1 1 calc R . .
H7C H 0.1681 0.0625 0.7556 0.092 Uiso 1 1 calc R . .
C8 C 0.0620(7) 0.3895(14) 0.6534(10) 0.076(4) Uani 1 1 d . . .
H8A H 0.0184 0.3899 0.5988 0.114 Uiso 1 1 calc R . .
H8B H 0.0822 0.4971 0.6538 0.114 Uiso 1 1 calc R . .
H8C H 0.0661 0.3951 0.7047 0.114 Uiso 1 1 calc R . .
B1 B 0.0975(3) 0.2385(11) 0.5864(5) 0.0311(14) Uani 1 1 d . . .
H1A H 0.1148 0.3634 0.5956 0.037 Uiso 1 1 calc R . .
H1B H 0.0553 0.2395 0.5272 0.037 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
W W -0.8490 6.8722 '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 W1 C2 88.8(3) . . ?
C5 W1 C4 91.1(3) . . ?
C2 W1 C4 177.4(3) . . ?
C5 W1 C3 92.6(3) . . ?
C2 W1 C3 89.3(3) . . ?
C4 W1 C3 88.1(3) . . ?
C5 W1 C1 89.9(3) . . ?
C2 W1 C1 91.3(3) . . ?
C4 W1 C1 91.3(3) . . ?
C3 W1 C1 177.4(3) . . ?
C5 W1 P1 174.4(2) . . ?
C2 W1 P1 91.07(19) . . ?
C4 W1 P1 89.28(18) . . ?
C3 W1 P1 93.0(2) . . ?
C1 W1 P1 84.5(2) . . ?
B1 P1 Cl2 106.9(2) . . ?
B1 P1 Cl1 109.4(2) . . ?
Cl2 P1 Cl1 99.47(11) . . ?
B1 P1 W1 115.2(2) . . ?
Cl2 P1 W1 109.86(9) . . ?
Cl1 P1 W1 114.57(9) . . ?
C6 N1 C7 108.1(6) . . ?
C6 N1 C8 106.3(7) . . ?
C7 N1 C8 109.7(8) . . ?
C6 N1 B1 112.8(5) . . ?
C7 N1 B1 113.2(5) . . ?
C8 N1 B1 106.5(6) . . ?
O1 C1 W1 179.2(7) . . ?
O2 C2 W1 176.0(7) . . ?
O3 C3 W1 179.7(8) . . ?
O4 C4 W1 178.8(6) . . ?
O5 C5 W1 179.4(7) . . ?
N1 B1 P1 122.3(5) . . ?
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
W1 C5 2.009(6) . ?
W1 C2 2.055(7) . ?
W1 C4 2.047(7) . ?
W1 C3 2.053(7) . ?
W1 C1 2.076(8) . ?
W1 P1 2.4780(16) . ?
Cl1 P1 2.074(3) . ?
Cl2 P1 2.066(3) . ?
P1 B1 1.953(7) . ?
O1 C1 1.115(9) . ?
O2 C2 1.129(9) . ?
O3 C3 1.127(10) . ?
O4 C4 1.143(8) . ?
O5 C5 1.145(8) . ?
N1 C6 1.484(9) . ?
N1 C7 1.493(10) . ?
N1 C8 1.489(11) . ?
N1 B1 1.588(8) . ?
