Selective halogenation at the pnictogen atom in Lewis-acid/base-stabilised phosphanylboranes and arsanylboranes
Schwan, Karl-Christian; Adolf, Ariane; Thoms, Christine; Zabel, Manfred; Timoshkin, Alexey Y.; Scheer, Manfred; Dalton Transactions  (2008) 5054–5058; doi:10.1039/b809773a

data_7004654
_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_compound_source        'see text'
_chemical_formula_moiety         'C8 H11 As B Br2 N O5 W'
_chemical_formula_structural     'C8 H11 As B Br2 N O5 W'
_chemical_formula_sum            'C8 H11 As B Br2 N O5 W'
_chemical_formula_weight         630.55
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                84.206(4)
_cell_angle_beta                 89.154(3)
_cell_angle_gamma                75.918(3)
_cell_formula_units_Z            4
_cell_length_a                   9.0879(3)
_cell_length_b                   12.1395(6)
_cell_length_c                   14.9688(6)
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    123
_cell_measurement_theta_max      62.0662
_cell_measurement_theta_min      2.9605
_cell_volume                     1593.50(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
1 omega 22.00 71.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -1.2571 45.0000 0.0000 0.0000 0.0000 49

2 phi -149.00 -91.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -1.2571 0.0000 - 0.0000 0.0000 58

3 omega -23.00 31.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -1.2571 -75.0000 240.0000 0.0000 0.0000 54

4 omega -78.00 -22.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -1.2571 -75.0000 240.0000 0.0000 0.0000 56

5 phi -179.00 -119.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -83.1433 0.0000 - 0.0000 0.0000 60

6 omega -115.00 -59.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 75.0000 240.0000 0.0000 0.0000 56

7 omega -111.00 -56.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 102.0000 206.0000 0.0000 0.0000 55

8 phi -61.00 1.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -83.1433 0.0000 - 0.0000 0.0000 62

9 omega -114.00 -59.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 109.0000 83.0000 0.0000 0.0000 55

10 omega -105.00 -53.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 -65.0000 214.0000 0.0000 0.0000 52

11 omega -110.00 -58.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 45.0000 120.0000 0.0000 0.0000 52

12 omega -114.00 -59.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 75.0000 0.0000 0.0000 0.0000 55

13 phi -121.00 -59.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -83.1433 0.0000 - 0.0000 0.0000 62

14 omega -61.00 -6.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 109.0000 83.0000 0.0000 0.0000 55

15 omega -61.00 -6.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 75.0000 0.0000 0.0000 0.0000 55

16 omega -133.00 -105.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 -65.0000 214.0000 0.0000 0.0000 28

17 omega -60.00 -9.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -83.1433 45.0000 120.0000 0.0000 0.0000 51

18 omega 57.00 109.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 49.0000 -39.0000 0.0000 0.0000 52

19 omega 11.00 62.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 -45.0000 120.0000 0.0000 0.0000 51

20 omega 11.00 62.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 -45.0000 240.0000 0.0000 0.0000 51

21 omega 58.00 109.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 45.0000 0.0000 0.0000 0.0000 51

22 omega 58.00 86.00 1.0000 4.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 84.3933 45.0000 240.0000 0.0000 0.0000 28

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10477
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        62.16
_diffrn_reflns_theta_max         62.16
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.628
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.076
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                4146
_reflns_number_total             4876
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b809773a.txt
_cod_data_source_block           thc1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7004654