Simple Zinc Complexes of Pyridyl-Substituted Tris(pyrazolyl)borate Ligands
Karl Weis; Heinrich Vahrenkamp; Inorganic Chemistry 36 (1997) 5592–5596; doi:10.1021/ic970628j

data_4323697
_publ_section_title
;
 Simple Zinc Complexes of Pyridyl-Substituted Tris(pyrazolyl)borate
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5592
_journal_page_last               5596
_journal_paper_doi               10.1021/ic970628j
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        Ethanol
_chemical_formula_sum            'C29 H31 B F N9 O Zn'
_chemical_formula_weight         616.81
_chemical_melting_point          151
_chemical_name_systematic
Hydrotris(5-methyl-3-3'-pyridyl-pyrazole-1-yl)borato-zinc-fluoride
_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                72.34(3)
_cell_angle_beta                 75.32(3)
_cell_angle_gamma                73.09(5)
_cell_formula_units_Z            2
_cell_length_a                   11.123(5)
_cell_length_b                   11.638(7)
_cell_length_c                   13.793(4)
_cell_measurement_temperature    200(2)
_cell_volume                     1600.8(14)
_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-2-Theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6539
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.01
_diffrn_standards_interval_count 'ICR every 3600 s, OCR every 200 refl.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   'empirical (XEMP)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_meas      1.19
_exptl_crystal_description       isometric
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.039
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_restrained_S_obs      1.039
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_obs          0.0662
_refine_ls_shift/esd_max         -0.057
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1407P)^2^+3.3016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2213
_refine_ls_wR_factor_obs         0.1946
_reflns_number_observed          5593
_reflns_number_total             6264
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970628j_2.cif
_cod_data_source_block           w36
_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 (54 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 (85
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^)+(0.1407P)^2^+3.3016P] 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^)+(0.1407P)^2^+3.3016P] 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        1600.9(13)
_cod_database_code               4323697