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_4127469
_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(C F3 O3 S)'
_chemical_formula_sum            'C80 H76 F6 Fe4 N15 O11 S2'
_chemical_formula_weight         1825.07
_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             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                95.271(14)
_cell_angle_beta                 90.124(12)
_cell_angle_gamma                104.174(19)
_cell_formula_units_Z            2
_cell_length_a                   12.150(2)
_cell_length_b                   14.975(5)
_cell_length_c                   23.386(6)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.13
_cell_measurement_theta_min      3.06
_cell_volume                     4106.7(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.961
_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  0.0491
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            93135
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.371
_diffrn_reflns_theta_min         3.057
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.726
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1041 before and 0.0644 after correction. The Ratio of minimum to maximum transmission is 0.6790. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             1878
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         16109
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0470P)^2^+3.1559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14516
_reflns_number_total             16109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03157_si_001.cif
_cod_data_source_block           v19078
_cod_original_cell_volume        4106.5(18)
_cod_database_code               4127469
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.237
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Same fragment restrains
{S100, F100, F102, F101, O100, O102, O101, C100} sigma for 1-2: 0.02, 1-3: 0.04
as
{S101, F103, F104, F105, O103, O104, O105, C101}
{S100, F101, F100, F102, O102, O100, O101, C100} sigma for 1-2: 0.01, 1-3: 0.02
as
{S102, F106, F107, F108, O106, O107, O108, C102}
3. Others
 Sof(S102)=Sof(F106)=Sof(F107)=Sof(F108)=Sof(O106)=Sof(O107)=Sof(O108)=
 Sof(C102)=1-FVAR(1)
 Sof(S101)=Sof(F103)=Sof(F104)=Sof(F105)=Sof(O103)=Sof(O104)=Sof(O105)=
 Sof(C101)=FVAR(1)
4.a Rotating group:
 O2(H2)
4.b Aromatic/amide H refined with riding coordinates:
 N25(H25), N35(H35), C2(H2A), 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)
4.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              66035
_shelx_hkl_checksum              54629
_shelx_fab_checksum              13908
_olex2_submission_special_instructions 'No special instructions were received'