Synthesis and Characterization of Fluorinated Tris(pyrazolyl)borate Complexes. Observation of an (η5-Pyrazole)-K+ Interaction in the Solid State
Zhengbo Hu; Sergiu M. Gorun; Inorganic Chemistry 40 (2001) 667–671; doi:10.1021/ic000860g

data_4319241
_publ_section_title
;
 Synthesis and Characterization of Fluorinated Tris(pyrazolyl)borate
 Complexes. Observation of an (\h5-Pyrazole)-K+ Interaction in the Solid
 State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              667
_journal_page_last               671
_journal_paper_doi               10.1021/ic000860g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C15.5 H13 B Cu0.5 F9 K N6 O1.5'
_chemical_formula_weight         560.00
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                71.3010(10)
_cell_angle_beta                 69.7850(10)
_cell_angle_gamma                66.5390(10)
_cell_formula_units_Z            4
_cell_length_a                   12.0411(2)
_cell_length_b                   14.9791(2)
_cell_length_c                   16.0567(3)
_cell_measurement_temperature    298(2)
_cell_volume                     2436.01(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23858
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       boulder
_exptl_crystal_F_000             1118
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         9718
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         0.306
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.7068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1397
_refine_ls_wR_factor_obs         0.1149
_reflns_number_observed          6563
_reflns_number_total             9720
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000860g_1.cif
_cod_data_source_block           smg57
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.7068P] 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^)+(0.0678P)^2^+0.7068P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C15.50 H13 B Cu0.50 F9 K N6 O1.50'
_cod_database_code               4319241