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_4322242
_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
'Pyrolysis of cesium dibromoamino-tris(trifluoromethyl)borate'
_chemical_formula_moiety         'Cs 1+, C3 B F9 Br 1-'
_chemical_formula_structural     'Cs B (C F3)3 Br'
_chemical_formula_sum            'C3 B Br Cs F9'
_chemical_formula_weight         430.66
_chemical_name_systematic
;
 Cesium bromo-tris(trifluoromethyl)borate
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9001(14)
_cell_length_b                   9.9001(14)
_cell_length_c                   9.9001(14)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      13.3
_cell_volume                     970.3(2)
_computing_cell_refinement       'Siemens P3/PC Version 4.27'
_computing_data_collection       'Siemens P3/PC Version 4.27'
_computing_data_reduction        'Siemens XDISK, Siemens SHELXTL,Version 5.03'
_computing_molecular_graphics    'Siemens SHELXTL, XP, Version 5.03'
_computing_publication_material  'Siemens SHELXTL, XL, Version 5.03'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Siemens P3 four-circle diffractometer'
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3143
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.032
_exptl_absorpt_correction_T_max  0.4907
_exptl_absorpt_correction_T_min  0.1830
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.948
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.547
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.279
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_coef       0
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.200
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_restrained_S_obs      1.200
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         0.028
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1490
_refine_ls_wR_factor_obs         0.1445
_reflns_number_observed          671
_reflns_number_total             965
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990352a_1.cif
_cod_data_source_block           bbr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=3D(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=3D1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322242