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_4330049
_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 H63 Fe Ni O2 P3 S2, B F4'
_chemical_formula_sum            'C51 H67 B Cl4 F4 Fe Ni O2 P3 S2'
_chemical_formula_weight         1212.25
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.7681(8)
_cell_length_b                   20.7681(8)
_cell_length_c                   27.296(2)
_cell_measurement_reflns_used    5773
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.58
_cell_measurement_theta_min      2.24
_cell_volume                     10195.8(9)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, 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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ba47matsq
_diffrn_reflns_av_R_equivalents  0.1292
_diffrn_reflns_av_sigmaI/netI    0.1140
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            86061
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.9497
_exptl_absorpt_correction_T_min  0.7651
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3774
_exptl_crystal_id                ba47matsq
_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 2 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.054
_platon_squeeze_details
; 
The electron count from the "squeeze" model was lower than the 
number of solvate molecules predicted by the complete refinement. 
This is due to the disorder in the anion. The "squeeze" data are 
reported here. This model converged with wR2 = 0.1684 and 
R1 = 0.1201 for 889 parameters with 1562 restraints against 12418 data. 
;
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         12418
_refine_ls_number_restraints     1562
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                6647
_reflns_number_total             12418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300910r_si_002_1.cif
_cod_data_source_block           ba47matsq
_cod_original_cell_volume        10195.9(10)
_cod_database_code               4330049