#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:27:13 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179750 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/46/7004653.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_7004653
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 As B Cl2 N O5 W'
_chemical_formula_weight         541.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.14(3)
_cell_angle_beta                 100.66(3)
_cell_angle_gamma                103.98(3)
_cell_formula_units_Z            4
_cell_length_a                   8.9480(18)
_cell_length_b                   12.013(2)
_cell_length_c                   15.729(3)
_cell_measurement_reflns_used    5965
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      1.37
_cell_volume                     1545.4(7)
_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      100(1)
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'STOE-IPDS diffractometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11701
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.956
_exptl_absorpt_correction_T_max  0.6223
_exptl_absorpt_correction_T_min  0.2147
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'program faceit'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    2.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.884
_refine_diff_density_min         -6.328
_refine_diff_density_rms         0.458
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0626
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                5153
_reflns_number_total             6192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809773a.txt
_cod_data_source_block           acl1
_cod_original_cell_volume        1545.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004653
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.62500(5) 0.89796(3) 0.13820(2) 0.02579(15) Uani 1 1 d . . .
C1 C 0.8706(15) 0.9137(10) 0.1764(8) 0.035(3) Uani 1 1 d . . .
C2 C 0.6836(13) 1.0795(8) 0.1482(7) 0.027(2) Uani 1 1 d . . .
C3 C 0.3818(15) 0.8808(9) 0.0952(7) 0.032(2) Uani 1 1 d . . .
C4 C 0.5544(13) 0.7141(8) 0.1239(7) 0.027(2) Uani 1 1 d . . .
C5 C 0.6387(12) 0.8677(9) 0.0082(8) 0.031(2) Uani 1 1 d . . .
O1 O 0.9956(10) 0.9166(7) 0.1959(6) 0.041(2) Uani 1 1 d . . .
O2 O 0.7020(10) 1.1747(7) 0.1508(5) 0.0357(18) Uani 1 1 d . . .
O3 O 0.2608(10) 0.8779(7) 0.0689(5) 0.0370(19) Uani 1 1 d . . .
O4 O 0.5210(10) 0.6156(7) 0.1150(5) 0.0363(18) Uani 1 1 d . . .
O5 O 0.6460(11) 0.8493(7) -0.0640(5) 0.040(2) Uani 1 1 d . . .
As1 As 0.62181(13) 0.95307(8) 0.30471(7) 0.0262(2) Uani 1 1 d . . .
Cl1 Cl 0.8535(3) 0.9679(2) 0.39439(16) 0.0326(5) Uani 1 1 d . . .
Cl2 Cl 0.4784(3) 0.8009(2) 0.34167(16) 0.0342(6) Uani 1 1 d . . .
B1 B 0.6027(13) 1.1083(9) 0.3897(7) 0.026(2) Uani 1 1 d . . .
H1 H 0.707(13) 1.180(9) 0.378(6) 0.02(2) Uiso 1 1 d . . .
H2 H 0.620(11) 1.095(7) 0.458(5) 0.007(19) Uiso 1 1 d . . .
N1 N 0.4344(12) 1.1355(8) 0.3653(6) 0.0321(19) Uani 1 1 d . . .
C6 C 0.3886(15) 1.1394(10) 0.2688(7) 0.037(3) Uani 1 1 d . . .
H6A H 0.3646 1.0590 0.2277 0.056 Uiso 1 1 calc R . .
H6B H 0.4771 1.1941 0.2564 0.056 Uiso 1 1 calc R . .
H6C H 0.2945 1.1676 0.2596 0.056 Uiso 1 1 calc R . .
C7 C 0.4558(14) 1.2570(9) 0.4251(7) 0.033(2) Uani 1 1 d . . .
H7A H 0.5306 1.3170 0.4081 0.050 Uiso 1 1 calc R . .
H7B H 0.4981 1.2601 0.4880 0.050 Uiso 1 1 calc R . .
H7C H 0.3529 1.2735 0.4186 0.050 Uiso 1 1 calc R . .
C8 C 0.3032(15) 1.0494(11) 0.3832(8) 0.043(3) Uani 1 1 d . . .
H8A H 0.2057 1.0730 0.3714 0.065 Uiso 1 1 calc R . .
H8B H 0.3316 1.0492 0.4464 0.065 Uiso 1 1 calc R . .
H8C H 0.2856 0.9691 0.3437 0.065 Uiso 1 1 calc R . .
W2 W 0.10246(5) 0.38909(3) 0.12837(2) 0.02581(15) Uani 1 1 d . . .
C9 C 0.3401(14) 0.4018(9) 0.1777(8) 0.034(2) Uani 1 1 d . . .
C10 C 0.1705(13) 0.5722(9) 0.1473(7) 0.029(2) Uani 1 1 d . . .
C11 C -0.1394(14) 0.3775(9) 0.0824(7) 0.032(2) Uani 1 1 d . . .
C12 C 0.0331(12) 0.2032(8) 0.1031(7) 0.028(2) Uani 1 1 d . . .
C13 C 0.1317(14) 0.3669(8) 0.0004(8) 0.031(2) Uani 1 1 d . . .
O9 O 0.4654(10) 0.4069(7) 0.2047(6) 0.0387(19) Uani 1 1 d . . .
O10 O 0.1990(10) 0.6711(7) 0.1549(5) 0.0353(18) Uani 1 1 d . . .
O11 O -0.2606(10) 0.3774(7) 0.0572(5) 0.0363(18) Uani 1 1 d . . .
O12 O 0.0046(10) 0.1028(7) 0.0872(5) 0.0368(18) Uani 1 1 d . . .
O13 O 0.1501(11) 0.3524(7) -0.0690(5) 0.0398(19) Uani 1 1 d . . .
As2 As 0.06386(13) 0.41625(8) 0.28765(7) 0.0256(2) Uani 1 1 d . . .
Cl3 Cl 0.2971(3) 0.5102(2) 0.38877(16) 0.0332(5) Uani 1 1 d . . .
Cl4 Cl 0.0231(3) 0.24559(19) 0.32572(16) 0.0303(5) Uani 1 1 d . . .
B2 B -0.1035(15) 0.4722(10) 0.3519(8) 0.032(2) Uani 1 1 d . . .
H3 H -0.059(15) 0.475(10) 0.416(7) 0.04(3) Uiso 1 1 d . . .
H4 H -0.213(11) 0.406(7) 0.316(5) 0.006(19) Uiso 1 1 d . . .
N2 N -0.1064(11) 0.6059(7) 0.3625(5) 0.033(2) Uani 1 1 d . . .
C14 C 0.0445(14) 0.6957(9) 0.4190(8) 0.038(3) Uani 1 1 d . . .
H14A H 0.0297 0.7755 0.4316 0.057 Uiso 1 1 calc R . .
H14B H 0.1283 0.6941 0.3869 0.057 Uiso 1 1 calc R . .
H14C H 0.0753 0.6769 0.4760 0.057 Uiso 1 1 calc R . .
C15 C -0.1423(17) 0.6299(10) 0.2701(8) 0.043(3) Uani 1 1 d . . .
H15A H -0.2485 0.5784 0.2345 0.064 Uiso 1 1 calc R . .
H15B H -0.0626 0.6125 0.2381 0.064 Uiso 1 1 calc R . .
H15C H -0.1385 0.7140 0.2787 0.064 Uiso 1 1 calc R . .
C16 C -0.2345(16) 0.6232(10) 0.4050(7) 0.042(3) Uani 1 1 d . . .
H16A H -0.2124 0.6111 0.4651 0.062 Uiso 1 1 calc R . .
H16B H -0.3357 0.5654 0.3678 0.062 Uiso 1 1 calc R . .
H16C H -0.2411 0.7047 0.4105 0.062 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'
O O 0.0106 0.0060 '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'
As As 0.0499 2.0058 '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'
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
C5 W1 C2 87.9(4) . . ?
C5 W1 C4 91.1(4) . . ?
C2 W1 C4 177.0(4) . . ?
C5 W1 C3 89.4(4) . . ?
C2 W1 C3 90.7(4) . . ?
C4 W1 C3 86.5(4) . . ?
C5 W1 C1 88.5(4) . . ?
C2 W1 C1 89.4(4) . . ?
C4 W1 C1 93.5(4) . . ?
C3 W1 C1 177.9(4) . . ?
C5 W1 As1 175.5(3) . . ?
C2 W1 As1 87.9(3) . . ?
C4 W1 As1 93.1(3) . . ?
C3 W1 As1 92.4(3) . . ?
C1 W1 As1 89.8(3) . . ?
O1 C1 W1 176.8(10) . . ?
O2 C2 W1 174.3(10) . . ?
O3 C3 W1 174.0(11) . . ?
O4 C4 W1 177.6(10) . . ?
O5 C5 W1 179.1(9) . . ?
B1 As1 Cl1 92.3(3) . . ?
B1 As1 Cl2 105.7(3) . . ?
Cl1 As1 Cl2 96.03(10) . . ?
B1 As1 W1 131.5(3) . . ?
Cl1 As1 W1 111.74(8) . . ?
Cl2 As1 W1 112.37(8) . . ?
N1 B1 As1 115.8(7) . . ?
C8 N1 C7 108.1(9) . . ?
C8 N1 C6 109.6(9) . . ?
C7 N1 C6 107.5(7) . . ?
C8 N1 B1 112.7(8) . . ?
C7 N1 B1 106.3(8) . . ?
C6 N1 B1 112.4(9) . . ?
C13 W2 C10 88.5(4) . . ?
C13 W2 C9 90.6(5) . . ?
C10 W2 C9 88.6(4) . . ?
C13 W2 C12 89.0(4) . . ?
C10 W2 C12 177.4(4) . . ?
C9 W2 C12 91.9(4) . . ?
C13 W2 C11 91.1(4) . . ?
C10 W2 C11 91.3(4) . . ?
C9 W2 C11 178.3(4) . . ?
C12 W2 C11 88.3(4) . . ?
C13 W2 As2 179.6(3) . . ?
C10 W2 As2 91.6(3) . . ?
C9 W2 As2 89.7(3) . . ?
C12 W2 As2 90.9(3) . . ?
C11 W2 As2 88.5(3) . . ?
O9 C9 W2 178.6(11) . . ?
O10 C10 W2 176.1(9) . . ?
O11 C11 W2 175.7(10) . . ?
O12 C12 W2 175.3(10) . . ?
O13 C13 W2 177.9(8) . . ?
B2 As2 Cl4 93.6(3) . . ?
B2 As2 Cl3 104.0(3) . . ?
Cl4 As2 Cl3 96.06(10) . . ?
B2 As2 W2 134.1(3) . . ?
Cl4 As2 W2 112.15(8) . . ?
Cl3 As2 W2 109.89(9) . . ?
N2 B2 As2 117.2(8) . . ?
C16 N2 C14 108.3(8) . . ?
C16 N2 C15 107.9(8) . . ?
C14 N2 C15 108.2(9) . . ?
C16 N2 B2 107.8(8) . . ?
C14 N2 B2 113.3(7) . . ?
C15 N2 B2 111.2(8) . . ?
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 2.026(13) . ?
W1 C2 2.078(9) . ?
W1 C4 2.092(9) . ?
W1 C3 2.100(12) . ?
W1 C1 2.118(12) . ?
W1 As1 2.5587(12) . ?
C1 O1 1.094(15) . ?
C2 O2 1.106(12) . ?
C3 O3 1.074(14) . ?
C4 O4 1.117(12) . ?
C5 O5 1.125(14) . ?
As1 B1 2.097(10) . ?
As1 Cl1 2.224(3) . ?
As1 Cl2 2.225(3) . ?
B1 N1 1.614(13) . ?
N1 C8 1.482(16) . ?
N1 C7 1.491(12) . ?
N1 C6 1.512(13) . ?
W2 C13 2.043(12) . ?
W2 C10 2.070(10) . ?
W2 C9 2.079(11) . ?
W2 C12 2.090(9) . ?
W2 C11 2.110(11) . ?
W2 As2 2.5505(12) . ?
C9 O9 1.105(14) . ?
C10 O10 1.126(12) . ?
C11 O11 1.083(14) . ?
C12 O12 1.128(12) . ?
C13 O13 1.116(14) . ?
As2 B2 2.110(11) . ?
As2 Cl4 2.230(2) . ?
As2 Cl3 2.231(3) . ?
B2 N2 1.583(12) . ?
N2 C16 1.462(14) . ?
N2 C14 1.481(14) . ?
N2 C15 1.536(13) . ?
