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_4319243
_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 F9 K N7'
_chemical_formula_weight         539.28
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                73.7650(10)
_cell_angle_beta                 83.0730(10)
_cell_angle_gamma                64.8460(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7152(2)
_cell_length_b                   11.1235(2)
_cell_length_c                   12.2161(2)
_cell_measurement_temperature    298(2)
_cell_volume                     1265.41(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\f 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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -15
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_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   'Empirical (SADABS) '
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       'Irreg. cut'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.146
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4932
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_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.1532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1422
_refine_ls_wR_factor_obs         0.1266
_reflns_number_observed          3392
_reflns_number_total             4932
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000860g_3.cif
_cod_data_source_block           smg03
_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^)+(0.0647P)^2^+0.1532P] 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^)+(0.0647P)^2^+0.1532P] 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               4319243