Tris(trifluoromethyl)borane Carbonyl, (CF3)3BCO Synthesis, Physical, Chemical and Spectroscopic Properties, Gas Phase, and Solid State Structure
Maik Finze; Eduard Bernhardt; Annegret Terheiden; Michael Berkei; Helge Willner; Dines Christen; Heinz Oberhammer; Friedhelm Aubke; Journal of the American Chemical Society 124 (2002) 15385–15398; doi:10.1021/ja0209924

data_4115394
_publ_section_title
;
 Tris(trifluoromethyl)borane Carbonyl, (CF3)3BCO Synthesis, Physical,
 Chemical and Spectroscopic Properties, Gas Phase, and Solid State
 Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15385
_journal_page_last               15398
_journal_paper_doi               10.1021/ja0209924
_journal_volume                  124
_journal_year                    2002
_chemical_formula_structural     (CF~3~)~3~BCO
_chemical_formula_sum            'C4 B F9 O'
_chemical_formula_weight         245.85
_chemical_melting_point          282(1)
_chemical_name_common            Tris(trifluoromethyl)_Borane_Carbonyl
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.254(1)
_cell_length_b                   9.959(2)
_cell_length_c                   10.793(2)
_cell_measurement_reflns_used    3216
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      3.5
_cell_volume                     779.5(2)
_computing_cell_refinement       'DENZO SCALEPACK'
_computing_data_collection       KappaCCD
_computing_data_reduction        'DENZO SCALEPACK'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_publication_material
;SHELXL-93 (Sheldrick, 1993), Parst 
(Nardelli, 1983), Platon (Spek, 1982) & Missym (Le Page, 1987) 
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measurement_device       'KappaCCD NONIUS'
_diffrn_measurement_method       w--2q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3216
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.1230(383)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.137
_refine_ls_goodness_of_fit_obs   1.337
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_restrained_S_obs      1.337
_refine_ls_R_factor_all          0.1651
_refine_ls_R_factor_obs          0.1271
_refine_ls_shift/su_max          -0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+(0.1823P)^2^+8.1774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3937
_refine_ls_wR_factor_obs         0.3641
_reflns_number_observed          676
_reflns_number_total             1012
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0209924.cif
_cod_data_source_block           1537
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[s^2^(Fo^2^)+(0.1823P)^2^+8.1774P] 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^)+(0.1823P)^2^+8.1774P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115394