Two New Pyridyl-Substituted Tris(pyrazolyl)borate Ligands and Their Potassium Salts
Karl Weis; Heinrich Vahrenkamp; Inorganic Chemistry 36 (1997) 5589–5591; doi:10.1021/ic970627r

data_4323694
_publ_section_title
;
 Two New Pyridyl-Substituted Tris(pyrazolyl)borate Ligands and Their
 Potassium Salts
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5589
_journal_page_last               5591
_journal_paper_doi               10.1021/ic970627r
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        Acetonitrile
_chemical_formula_sum            'C27 H27 B K N9 O'
_chemical_formula_weight         543.49
_chemical_melting_point          263
_chemical_name_systematic
Aqua-potassium-hydrotris(5-methyl-3-3'-pyridyl-pyrazole-1-yl)borate
_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                75.480(13)
_cell_angle_beta                 82.93(2)
_cell_angle_gamma                88.43(2)
_cell_formula_units_Z            2
_cell_length_a                   8.893(2)
_cell_length_b                   11.733(2)
_cell_length_c                   13.272(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1330.4(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Nonius-Turbo-CAD4
_diffrn_measurement_method       Omega-2Theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
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_diffrn_reflns_theta_min         2.64
_diffrn_standards_interval_count 'ICR every 3600 s, OCR every 200 refl.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      1.37
_exptl_crystal_description       isometric
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.022
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.022
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_obs          0.0452
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_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+1.2211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1351
_refine_ls_wR_factor_obs         0.1058
_reflns_number_observed          4006
_reflns_number_total             5784
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970627r_1.cif
_cod_data_source_block           w17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (55 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (123
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+1.2211P] 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^)+(0.0492P)^2^+1.2211P] 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               4323694