Syntheses of Tricyanofluoroborates M[BF(CN)3] (M = Na, K): (CH3)3SiCl Catalysis, Countercation Effect, and Reaction Intermediates.
Sprenger, Jan A. P.; Landmann, Johannes; Drisch, Michael; Ignat'ev, Nikolai; Finze, Maik; Inorganic chemistry 54 (2015) 3403–3412; doi:10.1021/ic503077c

data_4342698
_publ_section_title
;
 Syntheses of Tricyanofluoroborates M[BF(CN)3] (M = Na, K): (CH3)3SiCl
 Catalysis, Countercation Effect, and Reaction Intermediates.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3403
_journal_page_last               3412
_journal_paper_doi               10.1021/ic503077c
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C7 H9 B F N4 Na Si'
_chemical_formula_sum            'C7 H9 B F N4 Na Si'
_chemical_formula_weight         230.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6004(9)
_cell_length_b                   8.8498(7)
_cell_length_c                   10.0689(10)
_cell_measurement_reflns_used    8510
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.8615
_cell_measurement_theta_min      2.787
_cell_volume                     1301.01(18)
_computing_cell_refinement       'Saint+ ver. 8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.34A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14585
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         2.457
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Sadabs 2014/4 (Bruker 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.4535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1272
_reflns_number_total             1364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic503077c_si_002.cif
_cod_data_source_block           NaBFCN3TMSCN
_cod_depositor_comments          'Adding full bibliography for 4342698.cif.'
_cod_database_code               4342698
_shelxl_version_number           2013-4
_shelx_res_checksum              32376
_shelx_hkl_checksum              60508