Hydrogen Activation by Biomimetic [NiFe]-Hydrogenase Model Containing Protected Cyanide Cofactors
Brian C. Manor; Thomas B. Rauchfuss; Journal of the American Chemical Society 135 (2013) 11895–11900; doi:10.1021/ja404580r

data_4120257
_publ_contact_author
;
Thomas B. Rauchfuss
University of Illinois
School of Chemical Sciences, Box 12-6
600 South Mathews Avenue
Urbana, Illinois  61801
USA
;
_publ_contact_author_email       rauchfuz@illinois.edu
_publ_contact_author_fax         '1  217 244 3186'
_publ_contact_author_phone       '1  217 333 7355'
_publ_section_title
;
 Hydrogen Activation by Biomimetic [NiFe]-Hydrogenase Model Containing
 Protected Cyanide Cofactors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11895
_journal_page_last               11900
_journal_paper_doi               10.1021/ja404580r
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C69 H30 B2 F30 Fe N2 Ni O2 P2 S2, C4H8O, C5H12'
_chemical_formula_sum            'C78 H50 B2 F30 Fe N2 Ni O3 P2 S2'
_chemical_formula_weight         1895.44
_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-97
_audit_update_record
;
?
;
_cell_angle_alpha                102.1330(10)
_cell_angle_beta                 107.4610(10)
_cell_angle_gamma                100.6930(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7927(16)
_cell_length_b                   17.481(2)
_cell_length_c                   18.899(2)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.27
_cell_volume                     4095.9(8)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm08sasq-sr
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16168
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.9089
_exptl_absorpt_correction_T_min  0.8307
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_id                bm08sasq-sr
_exptl_crystal_preparation
;
The data crystal was mounted using oil (Parantone-N, Exxon) to a
0.3 mm cryo-loop (Hampton Research) with the (0 1 0) scattering
planes roughly normal to the spindle axis.
;
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.241
_platon_squeeze_details
;
One solvent molecule of THF and pentane were found
in the unit cell but were poorly resolved.  The
found electron count matches the expected for
one THF and pentane.
;
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1559
_refine_ls_number_reflns         16164
_refine_ls_number_restraints     2681
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                12345
_reflns_number_total             16164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404580r_si_002_1.cif
_cod_data_source_block           bm08sasq-sr
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4120257