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_4319242
_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            'C17 H16 B Cu F9 N6 O2'
_chemical_formula_weight         581.71
_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                 99.0870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1931(2)
_cell_length_b                   8.93000(10)
_cell_length_c                   19.136
_cell_measurement_temperature    293(2)
_cell_volume                     2394.94(4)
_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      293(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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22121
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.973
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4807
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.974
_refine_ls_restrained_S_obs      1.035
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_obs          0.0388
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1058
_refine_ls_wR_factor_obs         0.0928
_reflns_number_observed          3369
_reflns_number_total             4808
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000860g_2.cif
_cod_data_source_block           smg36
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0578P)^2^+0.0000P] 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^)+(0.0578P)^2^+0.0000P] 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        2394.97(4)
_cod_database_code               4319242