Synthesis, characterization, and H/D exchange of μ-hydride-containing [FeFe]-hydrogenase subsite models formed by protonation reactions of (μ-TDT)Fe2(CO)4(PMe3)2 (TDT = SCH2SCH2S) with protic acids.
Song, Li-Cheng; Zhu, An-Guo; Guo, Yuan-Qiang; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5021–5029; doi:10.1039/c5dt04297f

data_7037839
_publ_section_title
;
 Synthesis, characterization, and H/D exchange of \m-hydride-containing
 [FeFe]-hydrogenase subsite models formed by protonation reactions of
 (\m-TDT)Fe2(CO)4(PMe3)2 (TDT = SCH2SCH2S) with protic acids.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5021
_journal_page_last               5029
_journal_paper_doi               10.1039/c5dt04297f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C12 H23 B F4 Fe2 O4 P2 S3'
_chemical_formula_weight         587.93
_chemical_name_systematic        'compound 5'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-25 deposited with the CCDC.
2016-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.970(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.2814(7)
_cell_length_b                   17.4609(9)
_cell_length_c                   21.0295(9)
_cell_measurement_temperature    296(2)
_cell_volume                     4522.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25853
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  0.7671
_exptl_absorpt_correction_T_min  0.7436
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         7967
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+46.8455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                6118
_reflns_number_total             7967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04297f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7037836--7037840.cif.'
_cod_original_sg_symbol_H-M      p21/c
_cod_database_code               7037839