Tetraphenylphosphonium tetrakis(trimethylsilanolato)ferrate(III)
Hay, Michael T.; Yennawar, Hemant P.; IUCrData 3 (2018) x171823–; doi:10.1107/S2414314617018235

data_1548666
_publ_section_title
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 Tetraphenylphosphonium tetrakis(trimethylsilanolato)ferrate(III)
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_journal_coeditor_code           SJ4151
_journal_issue                   1
_journal_name_full               IUCrData
_journal_page_first              x171823
_journal_paper_doi               10.1107/S2414314617018235
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          '(C24 H20 P) [Fe (C3 H9 O1 Si1)4]'
_chemical_formula_moiety         'C24 H20 P +, C12 H36 Fe O4 Si4 -'
_chemical_formula_sum            'C36 H56 Fe O4 P Si4'
_chemical_formula_weight         751.98
_chemical_name_systematic
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Tetraphenylphosphonium tetrakis(trimethylsilanolato)ferrate(III)
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.589(7)
_cell_length_b                   12.589(7)
_cell_length_c                   13.689(7)
_cell_measurement_reflns_used    3702
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.014
_cell_measurement_theta_min      2.191
_cell_volume                     2169(2)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.723
_diffrn_reflns_theta_min         2.198
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.599979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.226
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
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_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                2258
_reflns_number_total             2712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj4151sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1548666.cif.'
_cod_original_cell_volume        2169(3)
_cod_database_code               1548666
_cod_database_fobs_code          1548666
_shelx_hkl_checksum              43709
_shelx_res_checksum              66967