Iron in a Trigonal Tris(alkoxide) Ligand Environment
Matthew B. Chambers; Stanislav Groysman; Dino Villagrán; Daniel G. Nocera; Inorganic Chemistry 52 (2013) 3159–3169; doi:10.1021/ic302634q

data_4334200
_publ_section_title
;
 Iron in a Trigonal Tris(alkoxide) Ligand Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3159
_journal_page_last               3169
_journal_paper_doi               10.1021/ic302634q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C30 H63 Fe O3, C20 H40 K O10'
_chemical_formula_sum            'C50 H103 Fe K O13'
_chemical_formula_weight         1007.27
_chemical_name_common            Fe(Ditox)3K(15C5)2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.295(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.381(3)
_cell_length_b                   17.218(5)
_cell_length_c                   29.190(9)
_cell_measurement_temperature    100(2)
_cell_volume                     5719(3)
_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 1.000
_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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            95450
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.9257
_exptl_absorpt_correction_T_min  0.9257
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       Block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         10479
_refine_ls_number_restraints     601
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+6.1178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                7808
_reflns_number_total             10479
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302634q_si_002_04.cif
_cod_data_source_block           cmpd_5_Fe(Ditox)3K(15C5)2
_cod_database_code               4334200