Heterometallic Triiron-Oxo/Hydroxo Clusters: Effect of Redox-Inactive Metals
David E. Herbert; Davide Lionetti; Jonathan Rittle; Theodor Agapie; Journal of the American Chemical Society 135 (2013) 19075–19078; doi:10.1021/ja4104974

data_4121380
_publ_section_title
;
 Heterometallic Triiron-Oxo/Hydroxo Clusters: Effect of Redox-Inactive
 Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19075
_journal_page_last               19078
_journal_paper_doi               10.1021/ja4104974
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C82 H89 Ca F9 Fe3 N7 O24 S3'
_chemical_formula_weight         2031.41
_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                 103.928(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0308(6)
_cell_length_b                   25.1917(10)
_cell_length_c                   23.7066(10)
_cell_measurement_reflns_used    9261
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.03
_cell_measurement_theta_min      2.18
_cell_volume                     8712.6(6)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.886
_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  0.0956
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            311030
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         37.22
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.6684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             4196
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.049
_refine_diff_density_min         -1.835
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         39866
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+13.6955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                24672
_reflns_number_total             39866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4104974_Ca.cif
_cod_data_source_block           deh57_sad
_cod_database_code               4121380