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_7720464
_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         'C16 H15 Fe2 O5 P S2'
_chemical_formula_sum            'C16 H15 Fe2 O5 P S2'
_chemical_formula_weight         494.07
_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             2022-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-05-16 deposited with the CCDC.	2025-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.887(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5053(3)
_cell_length_b                   9.6893(3)
_cell_length_c                   21.8776(7)
_cell_measurement_reflns_used    6646
_cell_measurement_temperature    170
_cell_measurement_theta_max      28.7010
_cell_measurement_theta_min      2.3130
_cell_volume                     1971.71(11)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_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 0.864
_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    -49.00  49.25   0.75   40.00    --  -17.01  77.00 150.00  131
  2  \w    -45.00 -15.75   0.75   40.00    --  -17.01  77.00 120.00   39
  3  \w     -9.00  96.00   0.75   40.00    --   17.79  77.00 -90.00  140
  4  \w     -7.00 101.00   0.75   40.00    --   17.79  77.00  30.00  144
;
_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      0.0062246000
_diffrn_orient_matrix_UB_12      -0.0683068000
_diffrn_orient_matrix_UB_13      0.0119426000
_diffrn_orient_matrix_UB_21      0.0069752000
_diffrn_orient_matrix_UB_22      0.0262000000
_diffrn_orient_matrix_UB_23      0.0307429000
_diffrn_orient_matrix_UB_31      -0.0756736000
_diffrn_orient_matrix_UB_32      -0.0031988000
_diffrn_orient_matrix_UB_33      -0.0030486000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.163
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.789
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.649
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.7360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4009
_reflns_number_total             4597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02885j2.cif
_cod_data_source_block           ib71bis
_cod_database_code               7720464
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C16 H15 Fe2 S2 P1 O5'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              12840
_olex2_date_sample_data_collection 2022-03-08
_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 2.015
_oxdiff_exptl_absorpt_empirical_full_min 0.751