Polyhedral Cobalt(II) and Iron(II) Siloxanes: Synthesis and X-ray Crystal Structure of [(RSi(OH)O2)Co(OPMe3)]4 and [(RSiO3)2(RSi(OH)O2)4(μ3-OH)2Fe8(THF)4] (R = (2,6-iPr2C6H3)N(SiMe3))
Umesh N. Nehete; Herbert W. Roesky; Hongping Zhu; Sharanappa Nembenna; Hans-Georg Schmidt; Mathias Noltemeyer; Dmitrij Bogdanov; Konrad Samwer; Inorganic Chemistry 44 (2005) 7243–7248; doi:10.1021/ic050859n

data_4309680
_publ_section_title
;
Polyhedral Cobalt(II) and Iron(II) Siloxanes: Synthesis and X-ray Crystal
Structure of [(RSi(OH)O2)Co(OPMe3)]4 and
[(RSiO3)2(RSi(OH)O2)4(\m3-OH)2Fe8(THF)4] (R = (2,6-iPr2C6H3)N(SiMe3))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7243
_journal_page_last               7248
_journal_paper_doi               10.1021/ic050859n
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C148 H236 Fe8 N6 O24 Si12'
_chemical_formula_weight         3267.31
_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                61.551(4)
_cell_angle_beta                 81.352(5)
_cell_angle_gamma                86.545(5)
_cell_formula_units_Z            1
_cell_length_a                   16.1290(13)
_cell_length_b                   16.7869(13)
_cell_length_c                   17.4643(14)
_cell_measurement_temperature    133(2)
_cell_volume                     4109.9(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  IPDS2
_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  0.1561
_diffrn_reflns_av_sigmaI/netI    0.1662
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            76145
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.8505
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1734
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         13591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                7331
_reflns_number_total             13591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050859nsi20050527_102613.cif
_cod_data_source_block           r1186
_cod_database_code               4309680