Tetrabutylammonium isobutyl silsesquioxane monochloroferrate(III)
Hay, Michael T.; Geib, Steven J.; Acta Crystallographica Section E 63 (2007) m445–m446; doi:10.1107/S1600536807000360

data_2212054
_publ_section_title
;
 Tetrabutylammonium isobutyl silsesquioxane monochloroferrate(III)
;
_journal_coeditor_code           BT2233
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m445
_journal_page_last               m446
_journal_paper_doi               10.1107/S1600536807000360
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C16 H36 N) [Fe Si7 Cl O12 (C4 H9)7]'
_chemical_formula_moiety         'C16 H36 N +, C28 H63 Cl Fe O12 Si7 -'
_chemical_formula_sum            'C44 H99 Cl Fe N O12 Si7'
_chemical_formula_weight         1122.17
_chemical_name_systematic
;
tetrabutylammonium chloroheptaisobutyldodeca-\m-oxo-heptasiliconferrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.5860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.6451(11)
_cell_length_b                   32.1149(15)
_cell_length_c                   18.3528(9)
_cell_measurement_reflns_used    8154
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.17
_cell_volume                     12462.8(10)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54262
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  0.9372
_exptl_absorpt_correction_T_min  0.8491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         12260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.078P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                8887
_reflns_number_total             12260
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2233.cif
_cod_data_source_block           I
_cod_database_code               2212054
_cod_database_fobs_code          2212054