2-Pyrrolyloximes in High-Nuclearity Transition-Metal Cluster Chemistry: Fe10 and Fe12
Evangelia S. Koumousi; Anastasia Routzomani; Tu N. Nguyen; Dimosthenis P. Giannopoulos; Catherine P. Raptopoulou; Vassilis Psycharis; George Christou; Theocharis C. Stamatatos; Inorganic Chemistry 52 (2013) 1176–1178; doi:10.1021/ic3023908

data_4333735
_publ_section_title
;
 2-Pyrrolyloximes in High-Nuclearity Transition-Metal Cluster Chemistry:
 Fe10 and Fe12
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1176
_journal_page_last               1178
_journal_paper_doi               10.1021/ic3023908
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C92 H146.4 Cl2 Fe12 N13 O40.7'
_chemical_formula_weight         2826.92
_chemical_name_systematic
;
 ?
;
_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                116.8700(10)
_cell_angle_beta                 105.8740(10)
_cell_angle_gamma                98.7320(10)
_cell_formula_units_Z            1
_cell_length_a                   15.4735(2)
_cell_length_b                   16.0289(2)
_cell_length_c                   16.9333(3)
_cell_measurement_reflns_used    40314
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.99
_cell_measurement_theta_min      6.54
_cell_volume                     3412.82(10)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47154
_diffrn_reflns_theta_full        63.00
_diffrn_reflns_theta_max         63.00
_diffrn_reflns_theta_min         6.54
_exptl_absorpt_coefficient_mu    10.885
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1461
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1003P)^2^+1.2738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                8005
_reflns_number_total             10443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3023908_si_004.cif
_cod_data_source_block           xsar29
_cod_original_cell_volume        3412.82(9)
_cod_original_formula_sum        'C92 H146.40 Cl2 Fe12 N13 O40.70'
_cod_database_code               4333735