Synthesis and structure of a thiolate-bridged nickel‒iron complex: towards a mimic of the active site of NiFe-hydrogenase
Davies, Sian C.; Evans, David J.; Hughes, David L.; Longhurst, Steven; Roger Sanders, J.; Chemical Communications  (1999) 1935–; doi:10.1039/a905353k

data_7115239
_publ_section_title
;
 Synthesis and structure of a thiolate-bridged nickel--iron complex:
 towards a mimic of the active site of NiFe-hydrogenase
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1935
_journal_paper_doi               10.1039/a905353k
_journal_year                    1999
_chemical_formula_moiety         'C34 H36 Cl Fe N Ni O2 P2 S3'
_chemical_formula_structural     '[{Fe(NS3)(CO)2-S,S'}NiCl(dppe)]'
_chemical_formula_sum            'C34 H36 Cl Fe N Ni O2 P2 S3'
_chemical_formula_weight         798.77
_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
_cell_angle_alpha                91.563(13)
_cell_angle_beta                 91.289(10)
_cell_angle_gamma                92.839(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5630(11)
_cell_length_b                   12.068(2)
_cell_length_c                   12.348(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      8
_cell_volume                     1719.8(4)
_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  0.061
_diffrn_reflns_av_sigmaI/netI    0.1265
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5687
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        6.2
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_T_max  0.31
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       'square plates'
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.966
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment
;
 Hydrogen atom coordinates were of idealised positions and set to ride 
on the
 parent carbon atoms.  Isotropic thermal displacement parameters of all 
H atoms
 were free to refine.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         4782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_obs          0.0584
_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^)+(0.0493P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1513
_refine_ls_wR_factor_obs         0.1125
_reflns_number_observed          '2254 to theta=23 (2325 to theta=24)'
_reflns_number_total             '4782 to theta=23 (5382 to theta=24)'
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905353k.txt
_cod_data_source_block           s17c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_site_calc_flag' value 'Calc' changed to 'calc'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (36
times).

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0493P)^2^] 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^)+(0.0493P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

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

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1719.9(4)
_cod_original_sg_symbol_H-M      'P -1   (no. 2)'
_cod_database_code               7115239