Connecting [NiFe]- and [FeFe]-Hydrogenases: Mixed-Valence Nickel-Iron Dithiolates with Rotated Structures
David Schilter; Thomas B. Rauchfuss; Matthias Stein; Inorganic Chemistry 51 (2012) 8931–8941; doi:10.1021/ic300910r

data_4330050
_publ_section_title
;
 Connecting [NiFe]- and [FeFe]-Hydrogenases: Mixed-Valence Nickel-Iron
 Dithiolates with Rotated Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8931
_journal_page_last               8941
_journal_paper_doi               10.1021/ic300910r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
; 
C49 H87 Fe Ni O2 P3 S2, C H2 Cl2, 0.5(C5 H12), B F4 
;
_chemical_formula_sum            'C52.5 H95 B Cl2 F4 Fe Ni O2 P3 S2'
_chemical_formula_weight         1187.58
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.627(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8734(13)
_cell_length_b                   10.7843(7)
_cell_length_c                   26.3625(14)
_cell_measurement_reflns_used    3186
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      65.64
_cell_measurement_theta_min      2.31
_cell_volume                     5926.7(6)
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  bc71pasq
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37216
_diffrn_reflns_theta_full        68.02
_diffrn_reflns_theta_max         68.02
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    5.011
_exptl_absorpt_correction_T_max  0.8382
_exptl_absorpt_correction_T_min  0.1690
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_id                bc71pasq
_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 0 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.042
_platon_squeeze_details
; 
The electron count from the "squeeze" model converged in good agreement 
with the number of solvate molecules predicted by the complete refinement. 
;
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         10341
_refine_ls_number_restraints     466
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                6709
_reflns_number_total             10341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300910r_si_002_2.cif
_cod_data_source_block           bc71pasq
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C52.50 H95 B Cl2 F4 Fe Ni O2 P3 S2'
_cod_database_code               4330050