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_4127467
_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, 2(C6 H6)'
_chemical_formula_sum            'C90 H88 Fe4 N15 O5'
_chemical_formula_weight         1683.15
_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                70.794(3)
_cell_angle_beta                 86.911(3)
_cell_angle_gamma                70.570(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1115(11)
_cell_length_b                   15.0509(11)
_cell_length_c                   21.1556(16)
_cell_measurement_reflns_used    9443
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.31
_cell_measurement_theta_min      2.37
_cell_volume                     3993.7(5)
_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_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            143926
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.534
_diffrn_reflns_theta_min         2.370
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0732 before and 0.0502 after correction.
The Ratio of minimum to maximum transmission is 0.9354.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         41418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0456P)^2^+1.7735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32203
_reflns_number_total             41418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03157_si_001.cif
_cod_data_source_block           v18485
_cod_database_code               4127467
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.818
_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.a Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00Q(H00Q), C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V),
 C00W(H00W), C00X(H00X), C00Z(H00Z), C01A(H01A), C01B(H01B), C01D(H01D),
 C01E(H01E), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01N(H01N),
 C01P(H01P), C01R(H01R), C01T(H01T), C01U(H01U), C01V(H01V), C01Y(H01Y),
 C01Z(H01Z), C02C(H02C), C02D(H02D), C02F(H02F), C02H(H02H), C02I(H02I),
 C02J(H02J), C02K(H02K), C02O(H02O), C02Q(H02S), C02S(H02T), C011(H011),
 C013(H013), C015(H015), C016(H016), C017(H017), C023(H023), C024(H024),
 C026(H026), C027(H027), C028(H028), C1(H1), C2(H2), C02Z(H1AA), C031(H031),
 C032(H032), C034(H034), C02E(H2AA), C02M(H3AA), C02R(H4AA), C02U(H5AA),
 C02W(H6AA), C02Y(H7AA)
2.b Idealised Me refined as rotating group:
 C02G(H02B,H02E,H02G), C02N(H02L,H02M,H02N), C02P(H02P,H02Q,H02R), C02T(H02U,
 H02V,H02W), C02V(H02X,H02Y,H), C02X(H02Z,HA,HB), C021(H02,HC,HD), C029(H0AA,HE,
 HF), C033(H03A,H03B,H03C)
;
_shelx_res_checksum              49716
_shelx_hkl_checksum              16323
_olex2_submission_special_instructions 'No special instructions were received'