Design of boron-decorated bimetallic iron complexes related to the active site of [FeFe]-hydrogenases and reactivity with hydride donors.
Bennour, Ines; Monnot, Victor; Schollhammer, Philippe; Chatelain, Lucile; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1915–1922; doi:10.1039/d5dt02885j

data_7720465
_publ_section_title
;
 Design of boron-decorated bimetallic iron complexes related to the active
 site of [FeFe]-hydrogenases and reactivity with hydride donors.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1915
_journal_page_last               1922
_journal_paper_doi               10.1039/d5dt02885j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C38 H32 B F10 Fe2 Na O9 S2'
_chemical_formula_sum            'C38 H32 B F10 Fe2 Na O9 S2'
_chemical_formula_weight         1032.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-16 deposited with the CCDC.	2025-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.553(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4643(9)
_cell_length_b                   19.6751(16)
_cell_length_c                   11.7454(10)
_cell_measurement_reflns_used    5770
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.1950
_cell_measurement_theta_min      2.2530
_cell_volume                     2096.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -48.00  48.00   1.00  120.00    --  -17.01  77.00-150.00   96
  2  \w     -1.00  95.00   1.00  120.00    --   17.79  77.00 -30.00   96
  3  \w      0.00  96.00   1.00  120.00    --   17.79  77.00  90.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0729412000
_diffrn_orient_matrix_UB_12      -0.0066143000
_diffrn_orient_matrix_UB_13      0.0354054000
_diffrn_orient_matrix_UB_21      0.0267722000
_diffrn_orient_matrix_UB_22      0.0070264000
_diffrn_orient_matrix_UB_23      -0.0493468000
_diffrn_orient_matrix_UB_31      0.0085507000
_diffrn_orient_matrix_UB_32      0.0347348000
_diffrn_orient_matrix_UB_33      0.0167628000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12255
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.809
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.087
_refine_diff_density_max         4.043
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.246
_refine_ls_abs_structure_details
;
 Flack x determined using 2405 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8000
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.1345
_refine_ls_shift/su_max          0.103
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1800P)^2^+54.2276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3651
_refine_ls_wR_factor_ref         0.3701
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.890
_reflns_Friedel_fraction_max     0.862
_reflns_number_gt                7225
_reflns_number_total             8000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02885j2.cif
_cod_data_source_block           ib169-150k
_cod_database_code               7720465
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C40 H40 B1 F10 Fe2 O6 S2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), B1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14)
;
_shelx_res_checksum              5058
_olex2_date_sample_data_collection 2023-03-28
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.941
_oxdiff_exptl_absorpt_empirical_full_min 0.674