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_4323627
_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            'C53 H66 B Cu N6 O2'
_chemical_formula_weight         893.47
_chemical_name_systematic
; Hydrotris(3-cumenyl-5-methyl-pyrazol-1-yl)-
borato-copper(II)-3,5-di-tert-butylsemiquinone
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90.00
_cell_angle_beta                 102.8420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.3081(3)
_cell_length_b                   13.0291(2)
_cell_length_c                   21.4783(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      0
_cell_volume                     5268.08(15)
_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      293(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  0.1067
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45805
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.933627
_exptl_absorpt_correction_T_min  0.763986
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.127
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9061
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_obs          0.0707
_refine_ls_shift/esd_max         0.414
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+4.0896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2146
_refine_ls_wR_factor_obs         0.1568
_reflns_number_observed          4945
_reflns_number_total             9263
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970244t_3.cif
_cod_data_source_block           TpCum,MeCu(3,5-DBSQ)
_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 (77 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 (129
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^)+(0.0898P)^2^+4.0896P] 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^)+(0.0898P)^2^+4.0896P] 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        5268.1(2)
_cod_database_code               4323627