Nickel-iron dithiolates related to the deactivated [NiFe]-hydrogenases.
Schilter, David; Rauchfuss, Thomas B.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 13324–13329; doi:10.1039/c2dt31895d

data_7020587
_publ_section_title
;
 Nickel-iron dithiolates related to the deactivated [NiFe]-hydrogenases.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13324
_journal_page_last               13329
_journal_paper_doi               10.1039/c2dt31895d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety
'C32 H30 Fe I Ni O3 P2 S2, 2(C H2 Cl2), 1(B F4)'
_chemical_formula_sum            'C34 H34 B Cl4 F4 Fe I Ni O3 P2 S2'
_chemical_formula_weight         1086.74
_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-97
_audit_update_record
;
?
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.871(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.9159(6)
_cell_length_b                   17.9577(5)
_cell_length_c                   21.4995(6)
_cell_measurement_reflns_used    5113
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      67.00
_cell_measurement_theta_min      3.19
_cell_volume                     8420.5(4)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
;
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5
(Bruker, 2005 & 2007)
;
_computing_molecular_graphics
;
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994)
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  bc59q2as
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31074
_diffrn_reflns_theta_full        68.01
_diffrn_reflns_theta_max         68.01
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    13.505
_exptl_absorpt_correction_T_max  0.5187
_exptl_absorpt_correction_T_min  0.1329
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4320
_exptl_crystal_id                bc59q2as
_exptl_crystal_preparation
;
The data crystal was mounted using oil (Parantone-N, Exxon) to a
0.3 mm cryo-loop (Hampton Research) with the (1 1 -2) scattering
planes roughly normal to the spindle axis.
;
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         7275
_refine_ls_number_restraints     640
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0469P)^2^+4.7077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                5687
_reflns_number_total             7275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31895d.txt
_cod_data_source_block           bc59q2as
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C2/c '
_cod_database_code               7020587