Explorations of the nonheme high-valent iron-oxo landscape: crystal structure of a synthetic complex with an [FeIV2(μ-O)<sub>2</sub>] diamond core relevant to the chemistry of sMMOH.
Rohde, Gregory T.; Xue, Genqiang; Que, Jr, Lawrence; Faraday discussions 234 (2022) 109–128; doi:10.1039/d1fd00066g

data_1566368
_publ_section_title
;
 Explorations of the nonheme high-valent iron-oxo landscape: crystal
 structure of a synthetic complex with an [FeIV2(\m-O)<sub>2</sub>]
 diamond core relevant to the chemistry of sMMOH.
;
_journal_issue                   0
_journal_name_full               'Faraday discussions'
_journal_page_first              109
_journal_page_last               128
_journal_paper_doi               10.1039/d1fd00066g
_journal_volume                  234
_journal_year                    2022
_chemical_formula_moiety
'C54 H72 Fe2 N8 O8, 3(Cl O4), 2(C4 H7 N), 2(H2 O)'
_chemical_formula_sum            'C62 H90 Cl3 Fe2 N10 O22'
_chemical_formula_weight         1545.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-09-24 deposited with the CCDC.	2021-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.110(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.9262(12)
_cell_length_b                   11.1080(4)
_cell_length_c                   22.8446(10)
_cell_measurement_reflns_used    3170
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      65.93
_cell_measurement_theta_min      3.28
_cell_volume                     6841.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXP'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14758
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.664
_diffrn_reflns_theta_max         66.664
_diffrn_reflns_theta_min         3.278
_exptl_absorpt_coefficient_mu    5.190
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             3244
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6021
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.0870
_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^)+(0.1548P)^2^+6.3536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2250
_refine_ls_wR_factor_ref         0.2707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3441
_reflns_number_total             6021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1fd00066g2.cif
_cod_data_source_block           13307_0m
_cod_depositor_comments
'Adding full bibliography for 1566366--1566368.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1566368
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              21770