#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:27:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179750 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004651.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_7004651
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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.178(2)
_cell_length_b                   9.5430(19)
_cell_length_c                   33.348(7)
_cell_measurement_reflns_used    1129
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      24.30
_cell_measurement_theta_min      1.80
_cell_volume                     3233.1(11)
_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 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            16144
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    4.073
_exptl_absorpt_correction_T_max  0.8346
_exptl_absorpt_correction_T_min  0.3706
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.051
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0315
_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)+(0.0450P)²+5.4064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                6326
_reflns_number_total             7398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809773a.txt
_cod_data_source_block           abs
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7004651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.76950(2) 0.182924(18) 0.136625(5) 0.02740(6) Uani 1 1 d . . .
P1 P 0.80310(12) -0.04554(12) 0.17062(4) 0.0275(2) Uani 1 1 d . . .
Cl1 Cl 0.81050(17) -0.21279(13) 0.13118(4) 0.0465(3) Uani 1 1 d . . .
Cl2 Cl 0.98940(15) -0.06308(17) 0.19894(5) 0.0508(3) Uani 1 1 d . . .
B1 B 0.6718(8) -0.0974(7) 0.2080(2) 0.0455(16) Uani 1 1 d . . .
H1 H 0.567(12) -0.137(13) 0.184(3) 0.13(4) Uiso 1 1 d . . .
H2 H 0.677(7) -0.008(8) 0.231(2) 0.06(2) Uiso 1 1 d . . .
N1 N 0.6973(5) -0.2233(5) 0.23963(14) 0.0388(10) Uani 1 1 d . . .
C1 C 0.9684(6) 0.2074(6) 0.13331(18) 0.0418(12) Uani 1 1 d . . .
O1 O 1.0784(5) 0.2190(6) 0.13154(17) 0.0654(14) Uani 1 1 d . . .
C2 C 0.7594(6) 0.0917(5) 0.08091(15) 0.0367(11) Uani 1 1 d . . .
O2 O 0.7529(5) 0.0404(5) 0.04998(12) 0.0559(12) Uani 1 1 d . . .
C3 C 0.5716(6) 0.1562(5) 0.14012(16) 0.0369(11) Uani 1 1 d . . .
O3 O 0.4603(4) 0.1420(5) 0.14110(14) 0.0513(10) Uani 1 1 d . . .
C4 C 0.7839(7) 0.2662(6) 0.19329(19) 0.0465(14) Uani 1 1 d . . .
O4 O 0.7947(8) 0.3108(7) 0.22482(18) 0.086(2) Uani 1 1 d . . .
C5 C 0.7369(6) 0.3730(5) 0.11137(16) 0.0387(11) Uani 1 1 d . . .
O5 O 0.7148(5) 0.4809(4) 0.09690(15) 0.0597(13) Uani 1 1 d . . .
C6 C 0.5610(8) -0.2619(9) 0.2536(2) 0.0643(19) Uani 1 1 d . . .
H6A H 0.5695 -0.3388 0.2726 0.096 Uiso 1 1 calc R . .
H6B H 0.5042 -0.2899 0.2306 0.096 Uiso 1 1 calc R . .
H6C H 0.5232 -0.1814 0.2664 0.096 Uiso 1 1 calc R . .
C7 C 0.7803(9) -0.1838(9) 0.2752(2) 0.069(2) Uani 1 1 d . . .
H7A H 0.7747 -0.2554 0.2957 0.104 Uiso 1 1 calc R . .
H7B H 0.7505 -0.0950 0.2855 0.104 Uiso 1 1 calc R . .
H7C H 0.8709 -0.1749 0.2680 0.104 Uiso 1 1 calc R . .
C8 C 0.7503(9) -0.3529(7) 0.2213(2) 0.0628(19) Uani 1 1 d . . .
H8A H 0.8384 -0.3348 0.2130 0.094 Uiso 1 1 calc R . .
H8B H 0.6937 -0.3798 0.1982 0.094 Uiso 1 1 calc R . .
H8C H 0.7532 -0.4280 0.2410 0.094 Uiso 1 1 calc R . .
W2 W 0.73194(2) 0.216476(19) 0.378064(6) 0.02902(6) Uani 1 1 d . . .
P2 P 0.77806(13) 0.06303(12) 0.43712(4) 0.0287(2) Uani 1 1 d . . .
Cl4 Cl 0.77322(19) 0.17599(15) 0.49054(4) 0.0509(4) Uani 1 1 d . . .
Cl3 Cl 0.97419(15) 0.00475(18) 0.44167(5) 0.0524(4) Uani 1 1 d . . .
B2 B 0.6689(7) -0.1020(6) 0.44132(19) 0.0400(13) Uani 1 1 d . . .
H3 H 0.573(7) -0.058(7) 0.444(2) 0.049(18) Uiso 1 1 d . . .
H4 H 0.685(7) -0.152(8) 0.413(2) 0.06(2) Uiso 1 1 d . . .
N2 N 0.6946(5) -0.2193(5) 0.47567(14) 0.0391(10) Uani 1 1 d . . .
C9 C 0.5868(6) 0.3138(6) 0.40716(18) 0.0386(11) Uani 1 1 d . . .
O9 O 0.5063(5) 0.3681(5) 0.42372(16) 0.0612(13) Uani 1 1 d . . .
C10 C 0.5963(6) 0.0778(6) 0.35348(16) 0.0403(12) Uani 1 1 d . . .
O10 O 0.5227(5) 0.0011(6) 0.33940(15) 0.0621(13) Uani 1 1 d . . .
C11 C 0.8678(6) 0.3509(6) 0.40527(19) 0.0431(13) Uani 1 1 d . . .
O11 O 0.9401(5) 0.4273(5) 0.42064(18) 0.0664(14) Uani 1 1 d . . .
C12 C 0.8754(6) 0.1145(6) 0.34823(17) 0.0390(11) Uani 1 1 d . . .
O12 O 0.9508(5) 0.0559(5) 0.33120(16) 0.0583(12) Uani 1 1 d . . .
C13 C 0.7021(6) 0.3493(6) 0.33070(17) 0.0405(12) Uani 1 1 d . . .
O13 O 0.6879(5) 0.4260(5) 0.30488(14) 0.0533(11) Uani 1 1 d . . .
C14 C 0.6976(9) -0.1619(8) 0.51728(19) 0.064(2) Uani 1 1 d . . .
H14A H 0.7064 -0.2383 0.5364 0.096 Uiso 1 1 calc R . .
H14B H 0.6166 -0.1113 0.5211 0.096 Uiso 1 1 calc R . .
H14C H 0.7719 -0.0987 0.5214 0.096 Uiso 1 1 calc R . .
C15 C 0.5838(12) -0.3199(10) 0.4715(3) 0.104(4) Uani 1 1 d . . .
H15A H 0.5871 -0.3822 0.4945 0.156 Uiso 1 1 calc R . .
H15B H 0.5906 -0.3742 0.4471 0.156 Uiso 1 1 calc R . .
H15C H 0.5011 -0.2690 0.4701 0.156 Uiso 1 1 calc R . .
C16 C 0.8172(13) -0.2944(11) 0.4712(4) 0.127(6) Uani 1 1 d . . .
H16A H 0.8904 -0.2293 0.4739 0.190 Uiso 1 1 calc R . .
H16B H 0.8151 -0.3381 0.4449 0.190 Uiso 1 1 calc R . .
H16C H 0.8278 -0.3659 0.4918 0.190 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'
Cl Cl 0.0998 0.0984 '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 W1 C3 89.9(2) . . ?
C5 W1 C4 92.1(2) . . ?
C3 W1 C4 90.7(3) . . ?
C5 W1 C1 90.8(2) . . ?
C3 W1 C1 179.3(2) . . ?
C4 W1 C1 89.4(3) . . ?
C5 W1 C2 90.3(2) . . ?
C3 W1 C2 90.2(2) . . ?
C4 W1 C2 177.4(2) . . ?
C1 W1 C2 89.7(2) . . ?
C5 W1 P1 176.96(17) . . ?
C3 W1 P1 88.48(14) . . ?
C4 W1 P1 85.34(18) . . ?
C1 W1 P1 90.88(16) . . ?
C2 W1 P1 92.25(14) . . ?
B1 P1 Cl1 105.2(2) . . ?
B1 P1 Cl2 109.4(2) . . ?
Cl1 P1 Cl2 99.19(8) . . ?
B1 P1 W1 115.90(19) . . ?
Cl1 P1 W1 113.43(7) . . ?
Cl2 P1 W1 112.18(7) . . ?
N1 B1 P1 121.4(4) . . ?
C7 N1 C8 109.8(6) . . ?
C7 N1 C6 107.8(6) . . ?
C8 N1 C6 106.3(6) . . ?
C7 N1 B1 113.7(6) . . ?
C8 N1 B1 113.4(5) . . ?
C6 N1 B1 105.4(5) . . ?
O1 C1 W1 179.1(6) . . ?
O2 C2 W1 179.4(5) . . ?
O3 C3 W1 178.3(5) . . ?
O4 C4 W1 178.4(7) . . ?
O5 C5 W1 178.2(5) . . ?
C13 W2 C9 90.4(2) . . ?
C13 W2 C10 91.5(2) . . ?
C9 W2 C10 89.7(2) . . ?
C13 W2 C11 91.1(3) . . ?
C9 W2 C11 89.6(2) . . ?
C10 W2 C11 177.3(2) . . ?
C13 W2 C12 89.8(2) . . ?
C9 W2 C12 178.6(2) . . ?
C10 W2 C12 89.0(2) . . ?
C11 W2 C12 91.7(2) . . ?
C13 W2 P2 176.92(18) . . ?
C9 W2 P2 89.93(15) . . ?
C10 W2 P2 91.55(15) . . ?
C11 W2 P2 85.87(17) . . ?
C12 W2 P2 89.93(16) . . ?
B2 P2 Cl3 109.3(2) . . ?
B2 P2 Cl4 108.4(2) . . ?
Cl3 P2 Cl4 98.56(9) . . ?
B2 P2 W2 117.14(18) . . ?
Cl3 P2 W2 110.67(8) . . ?
Cl4 P2 W2 111.14(7) . . ?
N2 B2 P2 123.2(4) . . ?
C16 N2 C15 108.9(8) . . ?
C16 N2 C14 107.9(7) . . ?
C15 N2 C14 107.4(6) . . ?
C16 N2 B2 111.8(5) . . ?
C15 N2 B2 107.1(5) . . ?
C14 N2 B2 113.6(5) . . ?
O9 C9 W2 179.4(6) . . ?
O10 C10 W2 178.9(6) . . ?
O11 C11 W2 178.1(6) . . ?
O12 C12 W2 177.6(5) . . ?
O13 C13 W2 178.0(6) . . ?
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 2.019(5) . ?
W1 C3 2.040(6) . ?
W1 C4 2.047(6) . ?
W1 C1 2.047(6) . ?
W1 C2 2.049(5) . ?
W1 P1 2.4717(12) . ?
P1 B1 1.945(7) . ?
P1 Cl1 2.0723(18) . ?
P1 Cl2 2.073(2) . ?
B1 N1 1.610(7) . ?
N1 C7 1.463(9) . ?
N1 C8 1.494(9) . ?
N1 C6 1.534(9) . ?
C1 O1 1.130(8) . ?
C2 O2 1.140(7) . ?
C3 O3 1.143(7) . ?
C4 O4 1.134(8) . ?
C5 O5 1.153(7) . ?
W2 C13 2.033(5) . ?
W2 C9 2.040(6) . ?
W2 C10 2.048(6) . ?
W2 C11 2.057(6) . ?
W2 C12 2.060(6) . ?
W2 P2 2.4762(13) . ?
P2 B2 1.937(6) . ?
P2 Cl3 2.069(2) . ?
P2 Cl4 2.0853(19) . ?
B2 N2 1.612(7) . ?
N2 C16 1.455(10) . ?
N2 C15 1.481(9) . ?
N2 C14 1.490(8) . ?
C9 O9 1.140(7) . ?
C10 O10 1.129(7) . ?
C11 O11 1.135(8) . ?
C12 O12 1.130(7) . ?
C13 O13 1.133(7) . ?
