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_4325592
_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            'C70 H77 F30 Fe K2 O17'
_chemical_formula_weight         1894.37
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
SHELXL-97

Platon program Squeeze used to account for void volume of 492 A3 with
electron count of 108 e. Associated with two hexanes (100 e/unit cell)
and placed into the unit card to adjust molecular weight, denisty, and
F000 value.
;
_cell_angle_alpha                88.796(2)
_cell_angle_beta                 74.063(2)
_cell_angle_gamma                89.938(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0618(15)
_cell_length_b                   14.3821(15)
_cell_length_c                   21.326(2)
_cell_measurement_reflns_used    9072
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.45
_cell_volume                     4146.2(7)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.953
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63123
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  0.9221
_exptl_absorpt_correction_T_min  0.8864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1934
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.810
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         18350
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1433P)^2^+5.0823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2340
_refine_ls_wR_factor_ref         0.2561
_reflns_number_gt                13684
_reflns_number_total             18350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2003782_si_002_4.cif
_cod_data_source_block           lhd257_compound_3b
_cod_original_cell_volume        4146.1(8)
_cod_database_code               4325592