3,3'-Bis(triphenylsilyl)biphenoxide as a Sterically Hindered Ligand on Fe(II), Fe(III), and Cr(II)
Ajay Kayal; Sonny C. Lee; Inorganic Chemistry 41 (2002) 321–330; doi:10.1021/ic010909y

data_4317446
_publ_contact_author_address
;
Department of Chemistry
Princeton University
Princeton
NJ 08544
USA
;
_publ_contact_author_email       sclee@chemvax.princeton.edu
_publ_contact_author_fax         '1 609 258 6746'
_publ_contact_author_name        'Sonny C. Lee'
_publ_contact_author_phone       '1 609 258 3879'
_publ_section_title
;
 3,3'-Bis(triphenylsilyl)biphenoxide as a Sterically Hindered Ligand on
 Fe(II), Fe(III), and Cr(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              321
_journal_page_last               330
_journal_paper_doi               10.1021/ic010909y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C58 H44 Cl Fe N2 O2. C4 H10 O. C4 H8 O'
_chemical_formula_sum            'C66 H62 Cl Fe N2 O4 Si2'
_chemical_formula_weight         1094.66
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.158(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8214(6)
_cell_length_b                   29.735(2)
_cell_length_c                   15.7349(9)
_cell_measurement_reflns_used    17028
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.48
_cell_measurement_theta_min      1.48
_cell_volume                     5922.4(6)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17028
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         7341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_restrained_S_obs      1.212
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_obs          0.0497
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1249
_refine_ls_wR_factor_obs         0.1154
_reflns_number_observed          4948
_reflns_number_total             7341
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic010909y_1.cif
_cod_data_source_block           10.Et2O.THF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+0.0000P] 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^)+(0.0649P)^2^+0.0000P] 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        5922.3(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4317446