Characterisation of a triply thiolate-bridged Ni‒Fe amine‒thiolate complex: insights into the electronic structure of the active site of [NiFe] hydrogenase
Steinfeld, Gunther; Kersting, Berthold; Chemical Communications  (2000) 205–; doi:10.1039/a908201h

data_7110765
_publ_section_title
;
 Characterisation of a triply thiolate-bridged Ni--Fe amine--thiolate
 complex: insights into the electronic structure of the active site of
 [NiFe] hydrogenase
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              205
_journal_paper_doi               10.1039/a908201h
_journal_year                    2000
_chemical_compound_source
;

 Crystals were grown by recrystallization from CH3CN

;
_chemical_formula_sum            'C178 H224 B3 Cl Fe2 N24 Ni2 O S6'
_chemical_formula_weight         3205.17
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.849(3)
_cell_length_b                   19.849(3)
_cell_length_c                   79.082(16)
_cell_measurement_temperature    180(2)
_cell_volume                     26983(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       'BRUKER AXS'
_diffrn_measurement_method       multirun
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1943
_diffrn_reflns_av_sigmaI/netI    0.1523
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       104
_diffrn_reflns_limit_l_min       -95
_diffrn_reflns_number            54984
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_meas      ?
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             10224
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.917
_refine_ls_goodness_of_fit_obs   1.130
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         7429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_obs          0.0686
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2165
_refine_ls_wR_factor_obs         0.1675
_reflns_number_observed          3045
_reflns_number_total             7430
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908201hsup1.cif
_cod_data_source_block           nife
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not determined' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        26982.7(79)
_cod_original_sg_symbol_H-M      'R3(bar)c, No. 167'
_cod_database_code               7110765