Nickel‒iron‒sulfur complexes: approaching structural analogues of the active sites of NiFe-hydrogenase and carbon monoxide dehydrogenase/acetyl-CoA synthase
Smith, Matt C.; Barclay, J. Elaine; Cramer, Stephen P.; Davies, Sian C.; Gu, Wei-Wei; Hughes, David L.; Longhurst, Steven; Evans, David J.; Journal of the Chemical Society, Dalton Transactions  (2002) 2641–; doi:10.1039/b201578c

data_7011557
_publ_section_title
;
 Nickel--iron--sulfur complexes: approaching structural analogues of
 the active sites of NiFe-hydrogenase and carbon monoxide
 dehydrogenase/acetyl-CoA synthase
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2641
_journal_paper_doi               10.1039/b201578c
_journal_year                    2002
_chemical_formula_moiety         'C32 H36 Cl Fe N2 Ni O P2 S3, C2 H3 N'
_chemical_formula_structural     '[{Fe(NO)(N{CH2CH2S}3)-S,S'}NiCl(dppe)]'
_chemical_formula_sum            'C34 H39 Cl Fe N3 Ni O P2 S3'
_chemical_formula_weight         813.81
_chemical_name_common            'Complex 3'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.345(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9861(15)
_cell_length_b                   19.719(3)
_cell_length_c                   15.709(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     3612.6(9)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; \w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8511
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       'rhombic prisms'
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment
;
Hydrogen coordinates were initially located in idealised positions and 
subsequently refined freely except those of the disordered carbons, which
were set to ride on the parent atoms.  All isotropic thermal displacement
parameters were refined freely.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         7866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_obs          0.0347
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.1485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0843
_refine_ls_wR_factor_obs         0.0714
_reflns_number_observed          5425
_reflns_number_total             7866
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b201578c.txt
_cod_data_source_block           matt1
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.1485P] 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^)+(0.0310P)^2^+0.1485P] 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        3612.6(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7011557