New BDH-TTP/[MIII(C5O5)3]3- (M = Fe, Ga) Isostructural Molecular Metals
Luca Pilia; Elisa Sessini; Flavia Artizzu; Masahiro Yamashita; Angela Serpe; Kazuya Kubo; Hiroshi Ito; Hisaaki Tanaka; Shin-ichi Kuroda; Jun-ichi Yamada; Paola Deplano; Carlos J. Gómez-García; Maria Laura Mercuri; Inorganic Chemistry 52 (2013) 423–430; doi:10.1021/ic302234j

data_4331739
_publ_section_title
;
 New BDH-TTP/[MIII(C5O5)3]3- (M = Fe, Ga) Isostructural Molecular Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              423
_journal_page_last               430
_journal_paper_doi               10.1021/ic302234j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C76 H50 Cl2 Fe O15 S48'
_chemical_formula_weight         2868.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 123.738(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   44.603(7)
_cell_length_b                   10.6036(16)
_cell_length_c                   25.964(4)
_cell_measurement_temperature    100(2)
_cell_volume                     10212(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            59684
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_description       prism
_exptl_crystal_F_000             5816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         14836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+27.8482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                11720
_reflns_number_total             14836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302234j_si_001_1.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        10211(3)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4331739