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_4333734
_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            'C94.4 H159.8 Fe10 N10.2 O41.6'
_chemical_formula_weight         2661.82
_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                105.1950(10)
_cell_angle_beta                 92.8840(10)
_cell_angle_gamma                113.1850(10)
_cell_formula_units_Z            1
_cell_length_a                   13.5678(3)
_cell_length_b                   15.6628(3)
_cell_length_c                   18.6330(3)
_cell_measurement_reflns_used    32983
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      6.50
_cell_volume                     3459.66(12)
_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 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42033
_diffrn_reflns_theta_full        60.99
_diffrn_reflns_theta_max         60.99
_diffrn_reflns_theta_min         6.50
_exptl_absorpt_coefficient_mu    8.758
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_type   'empirical and numerical'
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     744
_refine_ls_number_reflns         10090
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0934
_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^)+(0.1801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2449
_refine_ls_wR_factor_ref         0.2966
_reflns_number_gt                5941
_reflns_number_total             10090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3023908_si_002.cif
_cod_data_source_block           xsar88c
_cod_original_formula_sum        'C94.40 H159.80 Fe10 N10.20 O41.60'
_cod_database_code               4333734