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_4325590
_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            'C38 H24 F25 Fe N2 O5'
_chemical_formula_weight         1119.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 98.504(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.466(3)
_cell_length_b                   11.1062(15)
_cell_length_c                   33.506(5)
_cell_measurement_reflns_used    5646
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.32
_cell_volume                     8268(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            28704
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       blade
_exptl_crystal_F_000             4456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         7271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1623
_reflns_number_gt                6143
_reflns_number_total             7271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2003782_si_002_2.cif
_cod_data_source_block           lhd36a-compound_2
_cod_original_cell_volume        8268.1(19)
_cod_database_code               4325590