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_4127465
_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 H76 Fe4 N15 O5, F6 P, 0.5(C4 O), 1.5(C2.5)'
_chemical_formula_sum            'C83.75 H76 F6 Fe4 N15 O5.5 P'
_chemical_formula_weight         1748.96
_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             2018-12-24
_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                89.286(4)
_cell_angle_beta                 87.757(4)
_cell_angle_gamma                79.589(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9919(11)
_cell_length_b                   13.7630(9)
_cell_length_c                   25.905(2)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.38
_cell_measurement_theta_min      3.26
_cell_volume                     4201.8(6)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.970
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            115990
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.814
_diffrn_reflns_theta_min         3.265
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.222
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       plate
_exptl_crystal_F_000             1801
_refine_diff_density_max         1.747
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_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1060
_refine_ls_number_reflns         16721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+16.7068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14182
_reflns_number_total             16721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03157_si_001.cif
_cod_data_source_block           v18533-copy
_cod_original_formula_sum        'C83.75 H76 F6 Fe4 N15 O5.50 P'
_cod_database_code               4127465
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Others
 Sof(H02P)=Sof(H02Q)=Sof(H02R)=Sof(H02V)=Sof(H02W)=Sof(H02X)=Sof(C4AA)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C0BA)=1-FVAR(1)
 Sof(H02F)=Sof(H02L)=Sof(H02O)=Sof(H02S)=Sof(H02T)=Sof(H02U)=Sof(C8AA)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9AA)=FVAR(1)
 Fixed Sof: H02E(0.5) H02H(0.5) O2(0.5) C3AA(0.5) C5(0.5) C5AA(0.5) C4(0.5)
 C6AA(0.5) C2BA(0.5) C7AA(0.5) C1BA(0.25)
3.a Riding coordinates:
 N01V(H01V)
3.b Rotating group:
 O00M(H00M)
3.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00R(H00R), C00X(H00X), C00Z(H00Z), C011(H011), C012(H012),
 C018(H018), C01A(H01A), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F),
 C01I(H01I), C01J(H01J), C01K(H01K), N01L(H01L), C01M(H01M), C01O(H01O),
 C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01U(H01U), C01W(H01W),
 C01X(H01X), C020(H020), C021(H021), C023(H023), C024(H024), C025(H025),
 C026(H026), C027(H027), C028(H028), C029(H029), C02A(H02A), C02B(H02B),
 C02C(H02C), C02D(H02D), C02G(H02G), N02H(H02E), N02H(H02H), C02I(H02I),
 C02J(H02J), C02K(H02K), C02M(H02M), C02N(H02N), C1AA(H1AA)
3.d Idealised Me refined as rotating group:
 C02Q(H02P,H02Q,H02R), C02Q(H02F,H02L,H02O), C02T(H02V,H02W,H02X), C02T(H02S,
 H02T,H02U), C02U(H02Y,H,HA), C02V(H02Z,HB,HC), C02W(H02,HD,HE), C3(H3A,H3B,
 H3C), C9(H9A,H9B,H9C), C2AA(H2AA,H2AB,H2AC), C4AA(H4AA,H4AB,H4AC), C8AA(H8AA,
 H8AB,H8AC)
;
_shelx_res_checksum              66596
_shelx_hkl_checksum              49661
_olex2_submission_special_instructions 'No special instructions were received'