Tetrabutylammonium tetrakis(trimethylsilanolato-κ<i>O</i>)ferrate(III)
Hay, Michael; Staples, Richard; Lee, Andre; Acta Crystallographica Section E 68 (2012) m1186–; doi:10.1107/S1600536812035337

data_2236680
_publ_section_title
;
 Tetrabutylammonium tetrakis(trimethylsilanolato-\k<i>O</i>)ferrate(III)
;
_journal_coeditor_code           VN2048
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1186
_journal_paper_doi               10.1107/S1600536812035337
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C16 H36 N) [Fe (C3 H9 O Si)4]'
_chemical_formula_moiety         'C16 H36 N +, C12 H36 Fe O4 Si4 -'
_chemical_formula_sum            'C28 H72 Fe N O4 Si4'
_chemical_formula_weight         655.08
_chemical_name_systematic
;
Tetrabutylammonium tetrakis(trimethylsilanolato-\k<i>O</i>)ferrate(III)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.7220(10)
_cell_angle_beta                 82.8340(10)
_cell_angle_gamma                81.6580(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4952(5)
_cell_length_b                   10.5143(5)
_cell_length_c                   19.3506(9)
_cell_measurement_reflns_used    7900
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.34
_cell_volume                     2083.37(17)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w and \f 0.5 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0890
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18068
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.8718
_exptl_absorpt_correction_T_min  0.7667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                6223
_reflns_number_total             9424
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            vn2048.cif
_cod_data_source_block           I
_cod_database_code               2236680
_cod_database_fobs_code          2236680