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_7720462
_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         '2(C28 H10 B F10 Fe2 N O6 S2), 5(C7 H8)'
_chemical_formula_sum            'C91 H60 B2 F20 Fe4 N2 O12 S4'
_chemical_formula_weight         2126.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-15
_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                 91.854(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7611(4)
_cell_length_b                   31.1858(12)
_cell_length_c                   12.1671(5)
_cell_measurement_reflns_used    8584
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.3890
_cell_measurement_theta_min      2.4290
_cell_volume                     4460.3(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 0.994
_diffrn_measured_fraction_theta_max 0.824
_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    -42.00  67.00   0.50   15.00    --  -17.09  19.00-120.00  218
  2  \w    -25.00  58.00   0.50   15.00    --   17.95 -99.00   0.00  166
;
_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      -0.0087416000
_diffrn_orient_matrix_UB_12      0.0086338000
_diffrn_orient_matrix_UB_13      0.0530180000
_diffrn_orient_matrix_UB_21      0.0479844000
_diffrn_orient_matrix_UB_22      0.0135237000
_diffrn_orient_matrix_UB_23      -0.0055439000
_diffrn_orient_matrix_UB_31      -0.0355237000
_diffrn_orient_matrix_UB_32      0.0161212000
_diffrn_orient_matrix_UB_33      -0.0236702000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18560
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.378
_diffrn_reflns_theta_min         1.797
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.931
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.549
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.233
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         10114
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.4383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7605
_reflns_number_total             10114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02885j2.cif
_cod_data_source_block           ib122-b-150k
_cod_database_code               7720462
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C42 H26 B1 F10 Fe2 N1 O6 S2'
_olex2_refinement_description
;
1. Restrained distances
 C50-C51
 1.51 with sigma of 0.02
 C51-C56 = C51-C52 = C55-C54
 1.39 with sigma of 0.02
 C56-C55 = C54-C53 = C53-C52
 1.38 with sigma of 0.02
 C43-C44
 1.51 with sigma of 0.02
 C44-C49 = C44-C45 = C48-C47
 1.39 with sigma of 0.02
 C49-C48 = C47-C46 = C46-C45
 1.38 with sigma of 0.02
 C29-C30
 1.51 with sigma of 0.02
 C30-C35 = C30-C31 = C34-C33
 1.39 with sigma of 0.02
 C35-C34 = C33-C32 = C32-C31
 1.38 with sigma of 0.02
 C30-C35
 1.39 with sigma of 0.02
 C35-C30 = C31-C32 = C33-C34
 1.41 with sigma of 0.02
 C50-C56 = C50-C52
 2.52 with sigma of 0.04
 C51-C55
 2.42 with sigma of 0.04
 C51-C53
 2.41 with sigma of 0.04
 C56-C54
 2.39 with sigma of 0.04
 C55-C53 = C54-C52
 2.4 with sigma of 0.04
 C43-C49 = C43-C45
 2.52 with sigma of 0.04
 C44-C48
 2.42 with sigma of 0.04
 C44-C46
 2.41 with sigma of 0.04
 C49-C47
 2.39 with sigma of 0.04
 C48-C46 = C47-C45
 2.4 with sigma of 0.04
 C29-C35 = C29-C31
 2.52 with sigma of 0.04
 C30-C34
 2.42 with sigma of 0.04
 C30-C32
 2.41 with sigma of 0.04
 C35-C33
 2.39 with sigma of 0.04
 C34-C32 = C33-C31
 2.4 with sigma of 0.04
 C51-C56 \\sim C56-C55 \\sim C55-C54 \\sim C54-C53 \\sim C53-C52 \\sim C52-C51
 with sigma of 0.02
 C51-C53 \\sim C51-C55 \\sim C52-C54 \\sim C56-C52 \\sim C55-C53 \\sim C56-C54
 with sigma of 0.04
 C50-C52 \\sim C50-C56
 with sigma of 0.04
 C44-C49 \\sim C49-C48 \\sim C48-C47 \\sim C47-C46 \\sim C46-C45 \\sim C45-C44
 with sigma of 0.02
 C44-C46 \\sim C44-C48 \\sim C45-C47 \\sim C49-C45 \\sim C48-C46 \\sim C49-C47
 with sigma of 0.04
 C43-C45 \\sim C43-C49
 with sigma of 0.04
 C30-C35 \\sim C35-C34 \\sim C34-C33 \\sim C33-C32 \\sim C32-C31 \\sim C31-C30
 with sigma of 0.02
 C30-C32 \\sim C30-C34 \\sim C31-C33 \\sim C35-C31 \\sim C34-C32 \\sim C35-C33
 with sigma of 0.04
 C29-C31 \\sim C29-C35
 with sigma of 0.04
2. Restrained planarity
 C50, C51, C52, C53, C54, C55, C56
 with sigma of 0.1
 C43, C44, C45, C46, C47, C48, C49
 with sigma of 0.1
 C29, C30, C31, C32, C33, C34, C35
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C29) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C50, C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, C44, C45, C46, C47, C48, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=
 Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=1-FVAR(1)
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=
 Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56)=FVAR(1)
 Fixed Sof: C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) C31(0.5) H31(0.5)
 C32(0.5) H32(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35)
6.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C36(H36A,H36B,H36C), C50(H50A,H50B,H50C), C43(H43A,H43B,
 H43C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              92266
_olex2_date_sample_data_collection 2023-03-21
_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 2.945
_oxdiff_exptl_absorpt_empirical_full_min 0.704