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_4303816
_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            'C36 H37 Fe2 N O4 P2 S2'
_chemical_formula_weight         785.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.316(5)
_cell_angle_beta                 100.308(5)
_cell_angle_gamma                97.616(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1157(9)
_cell_length_b                   11.4433(8)
_cell_length_c                   14.6215(11)
_cell_measurement_reflns_used    4998
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.12
_cell_volume                     1786.5(2)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15634
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  .8950
_exptl_absorpt_correction_T_min  .7250
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             812
_exptl_crystal_size_max          .54
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .11
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.464
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6220
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0514P)^2^+0.0104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                4147
_reflns_number_total             6220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901154m_si_002.cif
_cod_data_source_block           complex-1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4303816
_refine_ls_r_factor_ref          0.0796