Dinuclear and Mononuclear Iron(II)-Thiolate Complexes with Mixed CO/CN-Ligands: Synthetic Advances for Iron Sites of [Fe]-Only Hydrogenases
Wen-Feng Liaw; Nan-Hung Lee; Chien-Hong Chen; Chien-Ming Lee; Gene-Hsiang Lee; Shie-Ming Peng; Journal of the American Chemical Society 122 (2000) 488–494; doi:10.1021/ja992300q

data_4115889
_publ_section_title
;
 Dinuclear and Mononuclear Iron(II)-Thiolate Complexes with Mixed
 CO/CN-Ligands: Synthetic Advances for Iron Sites of [Fe]-Only
 Hydrogenases
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              488
_journal_page_last               494
_journal_paper_doi               10.1021/ja992300q
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C50 H45 Fe N6 O2 P2 S2'
_chemical_formula_weight         943.83
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.737(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.4494(3)
_cell_length_b                   12.2321(2)
_cell_length_c                   31.6646(3)
_cell_measurement_reflns_used    8292
_cell_measurement_temperature    295(2)
_cell_volume                     9404.5(2)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method       '\w 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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            33954
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   ' empirical used sadabs'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.00004(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         10107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_obs          0.0578
_refine_ls_shift/esd_max         0.023
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+17.9139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1484
_refine_ls_wR_factor_obs         0.1323
_reflns_number_observed          7872
_reflns_number_total             10762
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja992300q_2.cif
_cod_data_source_block           ic6075
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' 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^)+(0.0532P)^2^+17.9139P] 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^)+(0.0532P)^2^+17.9139P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115889