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_4323695
_publ_section_title
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 Two New Pyridyl-Substituted Tris(pyrazolyl)borate Ligands and Their
 Potassium Salts
;
_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            'C30 H35 B K N9 O2'
_chemical_formula_weight         603.58
_chemical_melting_point          198
_chemical_name_systematic
;
Diaqua-Potassium-
hydrotris(5-methyl-3-3'(4'-methyl)-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                76.680(9)
_cell_angle_beta                 75.130(9)
_cell_angle_gamma                89.600(11)
_cell_formula_units_Z            2
_cell_length_a                   9.4810(15)
_cell_length_b                   11.6130(14)
_cell_length_c                   15.5160(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1604.3(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
_diffrn_reflns_av_R_equivalents  0.0107
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5735
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.79
_diffrn_standards_interval_count 'ICR every 3600 s, OCR every 200 refl.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      1.35
_exptl_crystal_description       isometric
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.058
_refine_ls_hydrogen_treatment    Riding-Modell
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_obs          0.0445
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.9287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1440
_refine_ls_wR_factor_obs         0.1140
_reflns_number_observed          3807
_reflns_number_total             5514
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970627r_2.cif
_cod_data_source_block           w24
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.9287P] 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^)+(0.0592P)^2^+0.9287P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323695