A mono-oxo-bridged binuclear iron(iii) complex with a Fe–O–Fe angle of 180.0° and its catalytic activity for hydrogen evolution
Sun, Xia-Xing; Du, Juan; Tan, Jie-Jie; Zhan, Shu-Zhong; New Journal of Chemistry 46 (2022) 3794–3799; doi:10.1039/D1NJ05904A

data_7061271
_publ_section_title
;
 A mono-oxo-bridged binuclear iron(iii) complex with a Fe--O--Fe angle of
 180.0\% and its catalytic activity for hydrogen evolution
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3794
_journal_page_last               3799
_journal_paper_doi               10.1039/D1NJ05904A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C18 H12 Cl2 Fe N4 O3.5, H2 O, C3 H7 N O'
_chemical_formula_sum            'C21 H21 Cl2 Fe N5 O5.5'
_chemical_formula_weight         558.18
_chemical_name_systematic        Fe-bpc
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-13 deposited with the CCDC.	2022-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                70.037(4)
_cell_angle_beta                 71.256(4)
_cell_angle_gamma                81.851(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6244(5)
_cell_length_b                   10.9915(5)
_cell_length_c                   12.4372(6)
_cell_measurement_reflns_used    5254
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.6350
_cell_measurement_theta_min      4.7960
_cell_volume                     1170.29(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     59.00  86.00   1.00    2.00    --    0.00  19.00 -90.00   27
  2  \w      6.00  39.00   1.00    2.00    --    0.00  82.00   0.00   33
  3  \w    -27.00   4.00   1.00    2.00    --    0.00  82.00   0.00   31
  4  \w    -26.00  39.00   1.00    2.00    --    0.00  19.00 -90.00   65
  5  \w    -39.00  31.00   1.00    2.00    --    0.00 -82.00  60.00   70
  6  \w     54.00  88.00   1.00    5.00    --  101.30 -82.00 -30.00   34
  7  \w     12.00  39.00   1.00    5.00    --  101.30 -82.00 -30.00   27
  8  \w     17.00 100.00   1.00    5.00    --  101.30 -38.00-120.00   83
  9  \w     42.00 136.00   1.00    5.00    --  101.30 -82.00 -90.00   94
 10  \w     13.00 122.00   1.00    5.00    --  101.30 -57.00 120.00  109
 11  \w     16.00  41.00   1.00    5.00    --  101.30 -82.00 -90.00   25
 12  \w     13.00 128.00   1.00    5.00    --  101.30 -82.00 120.00  115
 13  \w     13.00 126.00   1.00    5.00    --  101.30 -19.00 -60.00  113
 14  \w     95.00 136.00   1.00    5.00    --  101.30 -82.00 -30.00   41
 15  \w    112.00 189.00   1.00    5.00    --  101.30   0.00  30.00   77
 16  \w     12.00  85.00   1.00    5.00    --  101.30   0.00  30.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0017121000
_diffrn_orient_matrix_UB_12      -0.1032795000
_diffrn_orient_matrix_UB_13      0.1208843000
_diffrn_orient_matrix_UB_21      0.1338872000
_diffrn_orient_matrix_UB_22      -0.0707694000
_diffrn_orient_matrix_UB_23      -0.0636767000
_diffrn_orient_matrix_UB_31      0.1033468000
_diffrn_orient_matrix_UB_32      0.0811823000
_diffrn_orient_matrix_UB_33      0.0183095000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9172
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.020
_diffrn_reflns_theta_min         3.956
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.677
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1396P)^2^+0.7104P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4158
_reflns_number_total             4584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05904a2.cif
_cod_data_source_block           4225
_cod_depositor_comments          'Adding full bibliography for 7061271.cif.'
_cod_original_formula_sum        'C21 H21 Cl2 Fe N5 O5.50'
_cod_database_code               7061271
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Rotating group:
 O1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C16(H16), C13(H13), C12(H12), C11(H11), C15(H15), C6(H6), C10(H10),
 C14(H14), C3(H3), C19(H19)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              10469
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.776
_oxdiff_exptl_absorpt_empirical_full_min 0.566