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_4127466
_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, C F3 O3 S, 3(C4 H8 O)'
_chemical_formula_sum            'C91 H99 F3 Fe4 N15 O11 S'
_chemical_formula_weight         1891.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-14
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.122(9)
_cell_length_b                   18.204(5)
_cell_length_c                   24.698(6)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.16
_cell_measurement_theta_min      3.01
_cell_volume                     8597(5)
_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      100.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0952
_diffrn_reflns_av_unetI/netI     0.0944
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67468
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        65.360
_diffrn_reflns_theta_max         65.360
_diffrn_reflns_theta_min         3.016
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.172
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1572 before and 0.1108 after correction. The Ratio of minimum to maximum transmission is 0.6335. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       needle
_exptl_crystal_F_000             3940
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.128(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         13153
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+44.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                10506
_reflns_number_total             13153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03157_si_001.cif
_cod_data_source_block           v19070
_cod_database_code               4127466
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.872(8)
 0.128(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 H25-N25
 0.9 with sigma of 0.02
4. Rigid bond restraints
 O11, C11
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C42, C43
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C11 \\sim C12 \\sim C44 \\sim C45: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C44) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
6.a Secondary CH2 refined with riding coordinates:
 C200(H20A,H20B), C201(H20C,H20D), C202(H20E,H20F), C203(H20G,H20H), C208(H20I,
 H20J), C209(H20K,H20L), C210(H21A,H21B), C211(H21C,H21D), C204(H20M,H20N),
 C205(H20O,H20P), C206(H20Q,H20R), C207(H20S,H20T)
6.b Aromatic/amide H refined with riding coordinates:
 N35(H35), C2(H2), C4(H4), C6(H6), C13(H13), C14(H14), C15(H15A), C16(H16),
 C23(H23), C24(H24), C25(H25A), C26(H26), C33(H33), C34(H34), C35(H35A),
 C36(H36), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C56(H56), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67),
  C68(H68), C69(H69), C70(H70), C71(H71), C80(H80), C81(H81), C90(H90), C91(H91)
6.c Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C84(H84A,H84B,
 H84C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C94(H94A,H94B,H94C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C)
;
_shelx_res_checksum              39837
_shelx_hkl_checksum              91086
_olex2_submission_special_instructions 'No special instructions were received'