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_4323626
_publ_contact_author
;
 Cortlandt G. Pierpont
;
_publ_contact_author_email       cortlandt.pierpont@colorado.edu
_publ_contact_author_fax         3034920951
_publ_contact_author_phone       3034928420
_publ_section_title
;
 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/Methanol
_chemical_formula_sum            'C110 H140 B2 Cl8 N12 O4 Zn2'
_chemical_formula_weight         2130.30
_chemical_name_systematic
;
Hydrotris(3-cumenyl-5-methyl-pyrazol-1-yl)borato
-zinc-3,5-di-tert.butyl-semiquinone
;
_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     'Patterson heavy atom method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                80.049(12)
_cell_angle_beta                 89.853(8)
_cell_angle_gamma                85.542(12)
_cell_formula_units_Z            2
_cell_length_a                   14.261(3)
_cell_length_b                   18.760(7)
_cell_length_c                   21.710(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      0
_cell_volume                     5703(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_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      145(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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39839
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.863409
_exptl_absorpt_correction_T_min  0.725044
_exptl_absorpt_correction_type   semi-impirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1344
_refine_ls_number_reflns         26100
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.140
_refine_ls_restrained_S_obs      1.149
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_obs          0.0644
_refine_ls_shift/esd_max         0.328
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+10.1829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1739
_refine_ls_wR_factor_obs         0.1567
_reflns_number_observed          21409
_reflns_number_total             26114
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970244t_2.cif
_cod_data_source_block           TpCum,MeZn(3,5-DBSQ)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+10.1829P] 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^)+(0.0630P)^2^+10.1829P] 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        5703.0(27)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4323626