Effect of porphyrin ligands on the catalytic CH<sub>4</sub> oxidation activity of monocationic μ-nitrido-bridged iron porphyrinoid dimers by using H<sub>2</sub>O<sub>2</sub> as an oxidant.
Yamada, Yasuyuki; Miwa, Yusuke; Toyoda, Yuka; Uno, Yoshiki; Phung, Quan Manh; Tanaka, Kentaro; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6556–6567; doi:10.1039/d3dt04313d

data_7715472
_publ_section_title
;
 Effect of porphyrin ligands on the catalytic CH<sub>4</sub> oxidation
 activity of monocationic &#x3bc;-nitrido-bridged iron porphyrinoid dimers
 by using H<sub>2</sub>O<sub>2</sub> as an oxidant.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6556
_journal_page_last               6567
_journal_paper_doi               10.1039/d3dt04313d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '4(I3), 4(C93 H61 Fe2 N10), 16(C H Cl3)'
_chemical_formula_sum            'C388 H260 Cl48 Fe8 I12 N40'
_chemical_formula_weight         9153.994
_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_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-18 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   20.2412(6)
_cell_length_b                   15.9489(5)
_cell_length_c                   27.7869(8)
_cell_measurement_reflns_used    145933
_cell_measurement_temperature    173
_cell_measurement_theta_max      13.31
_cell_measurement_theta_min      0.725
_cell_volume                     8970.3(5)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9996
_diffrn_measurement_device_type  'SPring-8/BL02B1 PILATUS3 X CdTe 1M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4129
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            164406
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9996
_diffrn_reflns_theta_full        13.2608
_diffrn_reflns_theta_max         13.26
_diffrn_reflns_theta_min         0.43
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8129
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'blackish green'
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             4503.729
_refine_diff_density_max         2.0771
_refine_diff_density_min         -1.4065
_refine_diff_density_rms         0.0937
_refine_ls_d_res_high            0.9000
_refine_ls_d_res_low             27.7869
_refine_ls_goodness_of_fit_ref   1.2997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    272
_refine_ls_number_parameters     2387
_refine_ls_number_reflns         25785
_refine_ls_number_restraints     491
_refine_ls_restrained_S_all      1.2863
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                22741
_reflns_number_total             25785
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt04313d2.cif
_cod_data_source_block           texray_a
_cod_depositor_comments
'Adding full bibliography for 7715472--7715473.cif.'
_cod_database_code               7715472
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-Cl1
 1.78 with sigma of 0.02
 Cl1-Cl2
 2.9 with sigma of 0.02
 C2-Cl4
 1.78 with sigma of 0.02
 C11-Cl4A
 1.78 with sigma of 0.02
 Cl4-Cl5
 2.9 with sigma of 0.02
 Cl4A-Cl5A
 2.9 with sigma of 0.02
 C3-Cl7
 1.78 with sigma of 0.02
 C9-Cl7A
 1.78 with sigma of 0.02
 Cl7-Cl9
 2.9 with sigma of 0.02
 Cl7A-Cl8A = Cl8A-Cl9A = Cl9A-Cl7A
 2.9 with sigma of 0.02
 C4-Cl10
 1.78 with sigma of 0.02
 Cl10-Cl12
 2.9 with sigma of 0.02
 C5-Cl13
 1.78 with sigma of 0.02
 Cl13-Cl14
 2.9 with sigma of 0.02
 C6-Cl16
 1.78 with sigma of 0.02
 C10-Cl1D
 1.78 with sigma of 0.02
 Cl16-Cl17
 2.9 with sigma of 0.02
 Cl1D-Cl1E
 2.9 with sigma of 0.02
 C7-Cl19
 1.78 with sigma of 0.02
 Cl19-Cl20
 2.9 with sigma of 0.02
 C8-Cl22
 1.78 with sigma of 0.02
 C8C-Cl1A
 1.78 with sigma of 0.02
 Cl22-Cl23
 2.9 with sigma of 0.02
 Cl1A-Cl1B
 2.9 with sigma of 0.02
 C1-Cl1 \\sim C1-Cl2 \\sim C1-Cl3
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl2-Cl3 \\sim Cl3-Cl1
 with sigma of 0.02
 C2-Cl4 \\sim C2-Cl5 \\sim C2-Cl6
 with sigma of 0.02
 C11-Cl4A \\sim C11-Cl5A \\sim C11-Cl6A
 with sigma of 0.02
 Cl4-Cl5 \\sim Cl5-Cl6 \\sim Cl6-Cl4
 with sigma of 0.02
 Cl4A-Cl5A \\sim Cl5A-Cl6A \\sim Cl6A-Cl4A
 with sigma of 0.02
 C3-Cl7 \\sim C3-Cl8 \\sim C3-Cl9
 with sigma of 0.02
 C9-Cl7A \\sim C9-Cl8A \\sim C9-Cl9A
 with sigma of 0.02
 Cl7-Cl8 \\sim Cl8-Cl9 \\sim Cl9-Cl7
 with sigma of 0.02
 C4-Cl10 \\sim C4-Cl11 \\sim C4-Cl12
 with sigma of 0.02
 Cl10-Cl11 \\sim Cl11-Cl12 \\sim Cl12-Cl10
 with sigma of 0.02
 C5-Cl13 \\sim C5-Cl14 \\sim C5-Cl15
 with sigma of 0.02
 Cl13-Cl14 \\sim Cl14-Cl15 \\sim Cl15-Cl13
 with sigma of 0.02
 C6-Cl16 \\sim C6-Cl17 \\sim C6-Cl18
 with sigma of 0.02
 C10-Cl1D \\sim C10-Cl1E \\sim C10-Cl
 with sigma of 0.02
 Cl16-Cl17 \\sim Cl17-Cl18 \\sim Cl18-Cl16
 with sigma of 0.02
 Cl1D-Cl1E \\sim Cl1E-Cl \\sim Cl-Cl1D
 with sigma of 0.02
 C7-Cl19 \\sim C7-Cl20 \\sim C7-Cl21
 with sigma of 0.02
 Cl19-Cl20 \\sim Cl20-Cl21 \\sim Cl21-Cl19
 with sigma of 0.02
 C8-Cl22 \\sim C8-Cl23 \\sim C8-Cl24
 with sigma of 0.02
 C8C-Cl1A \\sim C8C-Cl1B \\sim C8C-Cl1C
 with sigma of 0.02
 Cl22-Cl23 \\sim Cl23-Cl24 \\sim Cl24-Cl22
 with sigma of 0.02
 Cl1A-Cl1B \\sim Cl1B-Cl1C \\sim Cl1C-Cl1A
 with sigma of 0.02
3. Rigid bond restraints
 C1, Cl1, Cl2, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, Cl4A, Cl5A, Cl6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, Cl7, Cl8, Cl9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, Cl7A, Cl8A, Cl9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, Cl10, Cl11, Cl12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, Cl13, Cl14, Cl15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, Cl19, Cl20, Cl21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, Cl22, Cl23, Cl24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8C, Cl1A, Cl1B, Cl1C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl3)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(Cl5) \\sim Ueq, Uanis(Cl6)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C11) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(Cl5A) \\sim Ueq, Uanis(Cl6A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C3) \\sim Ueq, Uanis(Cl7) \\sim Ueq, Uanis(Cl8) \\sim Ueq, Uanis(Cl9)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq, Uanis(Cl7A) \\sim Ueq, Uanis(Cl8A) \\sim Ueq, Uanis(Cl9A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C4) \\sim Ueq, Uanis(Cl10) \\sim Ueq, Uanis(Cl11) \\sim Ueq, Uanis(Cl12)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5) \\sim Ueq, Uanis(Cl13) \\sim Ueq, Uanis(Cl14) \\sim Ueq, Uanis(Cl15)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C6) \\sim Ueq, Uanis(Cl16) \\sim Ueq, Uanis(Cl17) \\sim Ueq, Uanis(Cl18)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C10) \\sim Ueq, Uanis(Cl1D) \\sim Ueq, Uanis(Cl1E) \\sim Ueq, Uanis(Cl)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C7) \\sim Ueq, Uanis(Cl19) \\sim Ueq, Uanis(Cl20) \\sim Ueq, Uanis(Cl21)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C8) \\sim Ueq, Uanis(Cl22) \\sim Ueq, Uanis(Cl23) \\sim Ueq, Uanis(Cl24)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C8C) \\sim Ueq, Uanis(Cl1A) \\sim Ueq, Uanis(Cl1B) \\sim Ueq, Uanis(Cl1C)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C2, Cl4, Cl5, Cl6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, Cl16, Cl17, Cl18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, Cl1D, Cl1E, Cl
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C8C)=Sof(H8C)=Sof(Cl1A)=Sof(Cl1B)=Sof(Cl1C)=1-FVAR(1)
 Sof(Cl22)=Sof(Cl23)=Sof(Cl24)=Sof(C8)=Sof(H8)=FVAR(1)
 Sof(C9)=Sof(H9)=Sof(Cl9A)=Sof(Cl8A)=Sof(Cl7A)=1-FVAR(2)
 Sof(Cl8)=Sof(Cl9)=Sof(C3)=Sof(H3)=Sof(Cl7)=FVAR(2)
 Sof(C10)=Sof(H10)=Sof(Cl)=Sof(Cl1D)=Sof(Cl1E)=1-FVAR(3)
 Sof(Cl16)=Sof(Cl18)=Sof(Cl17)=Sof(C6)=Sof(H6)=FVAR(3)
 Sof(Cl4A)=Sof(C11)=Sof(H11)=Sof(Cl6A)=Sof(Cl5A)=1-FVAR(4)
 Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=Sof(C2)=Sof(H2)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C4(H4), C1(H1), C5(H5), C7(H7), C3(H3), C2(H2), C6(H6), C8(H8), C8C(H8C),
 C9(H9), C10(H10), C11(H11)
7.b Aromatic/amide H refined with riding coordinates:
 C14B(H14B), C57B(H57B), C4B(H4B), C47B(H47B), C58A(H58A), C63A(H63A),
 C18B(H18B), C48A(H48A), C8B(H8B), C53A(H53A), C47A(H47A), C17A(H17A),
 C52B(H52B), C57A(H57A), C7A(H7A), C13B(H13B), C62B(H62B), C12A(H12A),
 C13A(H13A), C58B(H58B), C43A(H43A), C44A(H44A), C9B(H9B), C48B(H48B),
 C23B(H23B), C62A(H62A), C76B(H76B), C3A(H3A), C66B(H66B), C76A(H76A),
 C82A(H82A), C22B(H22B), C78B(H78B), C19B(H19B), C34B(H34B), C53B(H53B),
 C31A(H31A), C8A(H8A), C3B(H3B), C2A(H2A), C35B(H35B), C63B(H63B), C32A(H32A),
 C69B(H69B), C37B(H37B), C26B(H26B), C87A(H87A), C18A(H18A), C70A(H70A),
 C88A(H88A), C82B(H82B), C25B(H25B), C73A(H73A), C34A(H34A), C22A(H22A),
 C36B(H36B), C38B(H38B), C86A(H86A), C70B(H70B), C52A(H52A), C28A(H28A),
 C84A(H84A), C85A(H85A), C40A(H40A), C72A(H72A), C88B(H88B), C24B(H24B),
 C78A(H78A), C74A(H74A), C81B(H81B), C75A(H75A), C67B(H67B), C40B(H40B),
 C29A(H29A), C79B(H79B), C66A(H66A), C41A(H41A), C84B(H84B), C28B(H28B),
 C80B(H80B), C42A(H42A), C72B(H72B), C68B(H68B), C30A(H30A), C38A(H38A),
 C26A(H26A), C35A(H35A), C32B(H32B), C29B(H29B), C44B(H44B), C23A(H23A),
 C41B(H41B), C85B(H85B), C73B(H73B), C36A(H36A), C67A(H67A), C75B(H75B),
 C74B(H74B), C81A(H81A), C86B(H86B), C25A(H25A), C30B(H30B), C69A(H69A),
 C37A(H37A), C24A(H24A), C79A(H79A), C87B(H87B), C42B(H42B), C68A(H68A),
 C80A(H80A), C31B(H31B), C43B(H43B), C89B(H89B), C89A(H89A), C93B(H93B),
 C93A(H93A), C91B(H91B), C91A(H91A), C92B(H92B), C90B(H90B), C92A(H92A),
 C90A(H90A)
;
_olex2_submission_original_sample_id FePor2NI3
_olex2_submission_special_instructions 'No special instructions were received'