Tetradecanuclear Iron(III)-Oxo Nanoclusters Stabilized by Trilacunary Heteropolyanions.
Ibrahim, Masooma; Haider, Ali; Xiang, Yixian; Bassil, Bassem S.; Carey, Akina M.; Rullik, Lisa; Jameson, Geoffrey B.; Doungmene, Floriant; Mbomekallé, Israël M; Oliveira, Pedro de; Mereacre, Valeriu; Kostakis, George E.; Powell, Annie K.; Kortz, Ulrich; Inorganic chemistry 54 (2015) 6136–6146; doi:10.1021/acs.inorgchem.5b00124

data_4343324
_publ_section_title
;
 Tetradecanuclear Iron(III)-Oxo Nanoclusters Stabilized by Trilacunary
 Heteropolyanions.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6136
_journal_page_last               6146
_journal_paper_doi               10.1021/acs.inorgchem.5b00124
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'Fe14 Ge4 H290 Na24 O311 P6 Rb4 W36'
_chemical_formula_weight         14038.7
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n'
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.690(2)
_cell_length_b                   27.943(3)
_cell_length_c                   18.793(2)
_cell_measurement_reflns_used    9611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      2.17
_cell_volume                     11915(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            338779
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    19.660
_exptl_absorpt_correction_T_max  0.440
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.875
_exptl_crystal_description       block
_exptl_crystal_F_000             12740
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.440
_exptl_transmission_factor_min   0.088
_refine_diff_density_max         2.958
_refine_diff_density_min         -2.528
_refine_diff_density_rms         0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         9936
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+1176.7366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                9015
_reflns_number_total             9936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00124_si_004.cif
_cod_data_source_block           try
_cod_depositor_comments
'Adding full bibliography for 4343322--4343324.cif.'
_cod_original_formula_sum        'Fe14 H290 Ge4 Na24 O311 P6 Rb4 W36'
_cod_database_code               4343324
_shelx_estimated_absorpt_t_min   0.088
_shelx_estimated_absorpt_t_max   0.440