Pocket Semiquinonate Complexes of Cobalt(II), Copper(II), and Zinc(II) Prepared with the Hydrotris(cumenylmethylpyrazolyl)borate Ligand
Michael Ruf; Bruce C. Noll; Markus D. Groner; Gordon T. Yee; Cortlandt G. Pierpont; Inorganic Chemistry 36 (1997) 4860–4865; doi:10.1021/ic970244t

data_4323625
_publ_contact_author
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 Cortlandt G. Pierpont
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_publ_contact_author_email       cortlandt.pierpont@colorado.edu
_publ_contact_author_fax         3034920951
_publ_contact_author_phone       3034928420
_publ_section_title
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 Pocket Semiquinonate Complexes of Cobalt(II), Copper(II), and Zinc(II)
 Prepared with the Hydrotris(cumenylmethylpyrazolyl)borate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4860
_journal_page_last               4865
_journal_paper_doi               10.1021/ic970244t
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        Dichloromethane/Acetonitrile
_chemical_formula_sum            'C81.5 H96 B2 Cl5 Co N13'
_chemical_formula_weight         1508.50
_chemical_name_systematic
;
 Bis[hydrotris(3-cumenyl-5-methyl-pyrazol-1-yl)borato]cobalt(II)
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7189(4)
_cell_length_b                   17.4806(3)
_cell_length_c                   25.7123(6)
_cell_measurement_reflns_used    8129
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      0
_cell_volume                     7964.1(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens XSCANS'
_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      148(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50964
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.831162
_exptl_absorpt_correction_T_min  0.747864
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       'Pyramid   '
_exptl_crystal_F_000             3178
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.062
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_obs          0.0538
_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^)+(0.0757P)^2^+9.4458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1577
_refine_ls_wR_factor_obs         0.1438
_reflns_number_observed          8203
_reflns_number_total             9817
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970244t_1.cif
_cod_data_source_block           (TpCum,Me)2Co
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+9.4458P] 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^)+(0.0757P)^2^+9.4458P] 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_original_formula_sum        'C81.50 H96 B2 Cl5 Co N13'
_cod_database_code               4323625