Spectroscopic identification of an Fe(III) center, not Fe(IV), in the crystalline Sc-O-Fe adduct derived from [Fe(IV)(O)(TMC)]²⁺.
Prakash, Jai; Rohde, Gregory T.; Meier, Katlyn K.; Jasniewski, Andrew J.; Van Heuvelen, Katherine M.; Münck, Eckard; Que, Jr, Lawrence; Journal of the American Chemical Society 137 (2015) 3478–3481; doi:10.1021/jacs.5b00535

data_4129325
_publ_section_title
;
 Spectroscopic identification of an Fe(III) center, not Fe(IV), in the
 crystalline Sc-O-Fe adduct derived from [Fe(IV)(O)(TMC)]&#x00B2;&#x207A;.
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_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3478
_journal_page_last               3481
_journal_paper_doi               10.1021/jacs.5b00535
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C20 H35 F12 Fe N5 O13 S4 Sc, 2(C2 H3 N)'
_chemical_formula_sum            'C24 H41 F12 Fe N7 O13 S4 Sc'
_chemical_formula_weight         1092.69
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b a m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0006(13)
_cell_length_b                   22.0279(15)
_cell_length_c                   11.4933(8)
_cell_measurement_reflns_used    5457
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      20.58
_cell_measurement_theta_min      2.17
_cell_volume                     4557.3(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      102(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43189
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         4399
_refine_ls_number_restraints     547
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+19.7278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2196
_reflns_number_gt                3154
_reflns_number_total             4399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b00535_si_002.cif
_cod_data_source_block           13053g
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      Pbam
_cod_database_code               4129325