Synthesis with Structural and Electronic Characterization of Homoleptic Fe(II)- and Fe(III)-Fluorinated Phenolate Complexes
Stefanie A. Cantalupo; Helen E. Ferreira; Eman Bataineh; Annie J. King; Montana V. Petersen; Teresa Wojtasiewicz; Antonio G. DiPasquale; Arnold L. Rheingold; Linda H. Doerrer; Inorganic Chemistry 50 (2011) 6584–6596; doi:10.1021/ic2003782

data_4325595
_publ_section_title
;
 Synthesis with Structural and Electronic Characterization of Homoleptic
 Fe(II)- and Fe(III)-Fluorinated Phenolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6584
_journal_page_last               6596
_journal_paper_doi               10.1021/ic2003782
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C52 H58 F20 Fe K2 O17'
_chemical_formula_weight         1469.03
_chemical_name_common            'SAC-I-95 (yellow)'
_chemical_name_systematic
;
 ?
;
_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                 97.334(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.792(2)
_cell_length_b                   25.567(4)
_cell_length_c                   16.529(2)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.36
_cell_volume                     6199.9(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_refln_scan_rate          20
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44702
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.9060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.887
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         10952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1351P)^2^+18.6766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2361
_refine_ls_wR_factor_ref         0.2595
_reflns_number_gt                8354
_reflns_number_total             10952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2003782_si_002_7.cif
_cod_data_source_block           lhd76_compound_6
_cod_original_cell_volume        6200.3(15)
_cod_database_code               4325595