A Terminal Fe<sup>III</sup>-Oxo in a Tetranuclear Cluster: Effects of Distal Metal Centers on Structure and Reactivity.
Reed, Christopher J.; Agapie, Theodor; Journal of the American Chemical Society 141 (2019) 9479–9484; doi:10.1021/jacs.9b03157

data_4127468
_publ_section_title
;
 A Terminal Fe<sup>III</sup>-Oxo in a Tetranuclear Cluster: Effects of
 Distal Metal Centers on Structure and Reactivity.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9479
_journal_page_last               9484
_journal_paper_doi               10.1021/jacs.9b03157
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C78 H75 Fe4 N15 O5, 4(C3 H3)'
_chemical_formula_sum            'C90 H87 Fe4 N15 O5'
_chemical_formula_weight         1682.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-14 deposited with the CCDC.    2019-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                102.370(6)
_cell_angle_beta                 94.445(4)
_cell_angle_gamma                102.897(9)
_cell_formula_units_Z            2
_cell_length_a                   12.3162(13)
_cell_length_b                   15.5743(15)
_cell_length_c                   21.6599(15)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.41
_cell_measurement_theta_min      3.23
_cell_volume                     3921.5(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            82816
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.094
_diffrn_reflns_theta_min         3.227
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.338
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1072 before and 0.0612 after correction.
The Ratio of minimum to maximum transmission is 0.6557.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         15385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+3.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13148
_reflns_number_total             15385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03157_si_001.cif
_cod_data_source_block           v18489_a
_cod_original_cell_volume        3921.5(6)
_cod_database_code               4127468
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.665
_shelx_estimated_absorpt_t_min   0.279
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N00S) = Uanis(N13)
3. Others
 Sof(C5AA)=Sof(H5AA)=Sof(C6AA)=Sof(H6AA)=Sof(C7AA)=Sof(H7AA)=Sof(C8AA)=
 Sof(H8AA)=Sof(C18)=Sof(H18)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(C3)=Sof(H3)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C1)=Sof(H1)=Sof(C3AA)=
 Sof(H3AA)=Sof(C4AA)=Sof(H4AA)=FVAR(1)
 Sof(N13)=1-FVAR(2)
 Sof(N00S)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00L(H00L), C00M(H00M), C00O(H00O), C00R(H00R), C00T(H00T),
 C00U(H00U), C00V(H00V), C00Y(H00Y), C00Z(H00Z), C015(H015), C016(H016),
 C019(H019), C01H(H01H), C01J(H01J), C01L(H01L), C01P(H01P), C01Q(H01Q),
 C01R(H01R), C01S(H01S), C01V(H01V), C01Y(H01Y), C01Z(H01Z), C022(H022),
 C025(H025), C026(H026), C027(H027), C028(H028), C02A(H02D), C02B(H02E),
 C02C(H02F), C02D(H02G), C02F(H02H), C02G(H02I), C02H(H02J), C02I(H02K),
 C02J(H02L), C02L(H02M), C02M(H02N), C02Q(H02R), C02R(H02S), C02S(H02T),
 C02U(H02X), C02V(H1AA), C02X(H02Y), C02Y(H02Z), C2(H2), C3(H3), C4(H4), C5(H5),
  C6(H6), C1(H1), C32(H32), C1AA(H1AB), C2AA(H2AA), C3AA(H3AA), C4AA(H4AA),
 C5AA(H5AA), C6AA(H6AA), C7AA(H7AA), C8AA(H8AA), C18(H18), C6A(H6A)
4.b Idealised Me refined as rotating group:
 C012(H01A,H01B,H01C), C01E(H01D,H01E,H01F), C01N(H01G,H01I,H01K), C020(H02A,
 H02B,H02C), C02P(H02O,H02P,H02Q), C02T(H02U,H02V,H02W), C02Z(H02,H,HA),
 C030(H03A,H03B,H03C), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              71591
_shelx_hkl_checksum              99467
_olex2_submission_special_instructions 'No special instructions were received'