Preparation, Facile Deprotonation, and Rapid H/D Exchange of the μ-Hydride Diiron Model Complexes of the [FeFe]-Hydrogenase Containing a Pendant Amine in a Chelating Diphosphine Ligand
Ning Wang; Mei Wang; Jihong Liu; Kun Jin; Lin Chen; Licheng Sun; Inorganic Chemistry 48 (2009) 11551–11558; doi:10.1021/ic901154m

data_4303818
_publ_section_title
;
Preparation, Facile Deprotonation, and Rapid H/D Exchange of the \m-Hydride
Diiron Model Complexes of the [FeFe]-Hydrogenase Containing a Pendant Amine
in a Chelating Diphosphine Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11551
_journal_page_last               11558
_journal_paper_doi               10.1021/ic901154m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C47 H47 Cl4 Fe4 N O10 P2 S4'
_chemical_formula_weight         1341.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.833(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.8118(9)
_cell_length_b                   10.2078(4)
_cell_length_c                   22.6200(7)
_cell_measurement_reflns_used    2166
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.16
_cell_volume                     5694.3(4)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17268
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  .853
_exptl_absorpt_correction_T_min  .743
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
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_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .11
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4982
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_gt           0.0598
_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^)+(0.1215P)^2^+0.0120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1925
_reflns_number_gt                3242
_reflns_number_total             4982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901154m_si_004.cif
_cod_data_source_block           complex-3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4303818
_refine_ls_r_factor_ref          0.0958