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_4323696
_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 I N9 O Zn'
_chemical_formula_weight         724.71
_chemical_melting_point          261
_chemical_name_systematic
Hydrotris(5-methyl-3-3'-pyridyl-pyrazole-1-yl)borato-zinc-iodide
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.99(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.922(1)
_cell_length_b                   10.476(4)
_cell_length_c                   31.444(1)
_cell_measurement_temperature    293(2)
_cell_volume                     6097(3)
_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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            6097
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.39
_diffrn_standards_interval_count 'ICR every 3600s, OCR every 200 refl.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   'empirical (XEMP)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      1.52
_exptl_crystal_description       isometric
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.071
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_hydrogen_treatment    Riding-Model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_obs          0.0337
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+9.2828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1023
_refine_ls_wR_factor_obs         0.0896
_reflns_number_observed          4963
_reflns_number_total             5980
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970628j_1.cif
_cod_data_source_block           w29
_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 (50 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 (80
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^)+(0.0567P)^2^+9.2828P] 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^)+(0.0567P)^2^+9.2828P] 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        6097.1(5)
_cod_database_code               4323696