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_4309679
_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            'C72 H144 Co4 N4 O16 P4 Si8'
_chemical_formula_weight         1906.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.705(6)
_cell_length_b                   27.685(6)
_cell_length_c                   29.579(6)
_cell_measurement_temperature    133(2)
_cell_volume                     22549(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.778
_diffrn_measured_fraction_theta_max 0.778
_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  0.1441
_diffrn_reflns_av_sigmaI/netI    0.4750
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            60890
_diffrn_reflns_theta_full        24.92
_diffrn_reflns_theta_max         24.92
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.8614
_exptl_absorpt_correction_T_min  0.8021
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8096
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.697
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2032
_refine_ls_number_reflns         30611
_refine_ls_number_restraints     2771
_refine_ls_restrained_S_all      0.668
_refine_ls_R_factor_all          0.2562
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1844
_reflns_number_gt                7576
_reflns_number_total             30611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050859nsi20050527_102554.cif
_cod_data_source_block           r1173
_cod_original_cell_volume        22549(8)
_cod_database_code               4309679