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_4120258
_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
; 
C68 H31 B2 F30 Fe N2 Ni O P2 S2, C8 H20 N, C2 H4 Cl4 
;
_chemical_formula_sum            'C77 H53 B2 Cl2 F30 Fe N3 Ni O P2 S2'
_chemical_formula_weight         1939.36
_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                95.559(2)
_cell_angle_beta                 98.804(2)
_cell_angle_gamma                113.598(2)
_cell_formula_units_Z            2
_cell_length_a                   14.598(2)
_cell_length_b                   15.368(2)
_cell_length_c                   19.946(3)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.34
_cell_volume                     3990.0(10)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_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      183(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \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  bm59uasq-sr-p
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43992
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.8048
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       plate
_exptl_crystal_F_000             1948
_exptl_crystal_id                bm59uasq-sr-p
_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 -4 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.134
_platon_squeeze_details
; 
The unit cell was found to contain two solvent molecules of dichloromethane 
that were poorly resolved.  The electron count was found to be slightly 
higher than expected. 
;
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         14596
_refine_ls_number_restraints     1071
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.5820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                11524
_reflns_number_total             14596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404580r_si_002_2.cif
_cod_data_source_block           bm59uasq-sr-p
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4120258