Halogenation of (CF3)3B.NH3: N,N-Dihaloamino- and Halo-tris(trifluoromethyl)borates [(CF3)3B-NX2]- and [(CF3)3B-X]-, X = F, Cl, Br
David J. Brauer; Hans Bürger; Yonas Chebude; Gottfried Pawelke; Inorganic Chemistry 38 (1999) 3972–3977; doi:10.1021/ic990352a

data_4322244
_publ_section_title
;
 Halogenation of (CF3)3B.NH3: N,N-Dihaloamino- and
 Halo-tris(trifluoromethyl)borates [(CF3)3B-NX2]- and [(CF3)3B-X]-, X = F,
 Cl, Br
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3972
_journal_page_last               3977
_journal_paper_doi               10.1021/ic990352a
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source
;
 Reaction of Cs[B(CF3)3NBr2] with fluorine in the presence
 of H2O and CH3CN
;
_chemical_formula_structural     'Cs B (C F3)3 N H C (O) C Br3'
_chemical_formula_sum            'C5 H B Br3 Cs F9 N O'
_chemical_formula_weight         645.52
_chemical_name_systematic
;
 Cesium tribromoacetamido-tris(trifluoromethyl)borate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 118.416(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.121(4)
_cell_length_b                   16.765(3)
_cell_length_c                   10.005(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      34.9
_cell_measurement_theta_min      25.5
_cell_volume                     2968.3(10)
_computing_cell_refinement       'Siemens P3/PC Version 4.27'
_computing_data_collection       'Siemens P3/PC Version 4.27'
_computing_data_reduction        'Siemens XDISK,SHELXTL, Version 5.03'
_computing_molecular_graphics    'Siemens SHELXTL, XP, Version 5.03'
_computing_publication_material  'Siemens SHELXTL, XCIF, Version 5.03'
_computing_structure_refinement  'Siemens SHELXTL, XL, Version 5.03'
_computing_structure_solution    'Siemens SHELXTL, XS, Version 5.03'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       'profile fitted \w 2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1219
_diffrn_reflns_av_sigmaI/netI    0.1166
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6331
_diffrn_reflns_theta_max         69.28
_diffrn_reflns_theta_min         3.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    29.875
_exptl_absorpt_correction_T_max  0.1157
_exptl_absorpt_correction_T_min  0.0097
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.889
_exptl_crystal_density_method    none
_exptl_crystal_description       'monoclinic plate'
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.543
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.00029(4)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_obs          0.0589
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1766
_refine_ls_wR_factor_obs         0.1678
_reflns_number_observed          2349
_reflns_number_total             2770
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990352a_3.cif
_cod_data_source_block           yon5p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2968.4(9)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4322244