Protonation of nickel-iron hydrogenase models proceeds after isomerization at nickel.
Huynh, Mioy T.; Schilter, David; Hammes-Schiffer, Sharon; Rauchfuss, Thomas B.; Journal of the American Chemical Society 136 (2014) 12385–12395; doi:10.1021/ja505783z

data_4122464
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Protonation of nickel-iron hydrogenase models proceeds after
 isomerization at nickel.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12385
_journal_page_last               12395
_journal_paper_doi               10.1021/ja505783z
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C32 H30 Fe O3 P2 Pd S2'
_chemical_formula_sum            'C32 H30 Fe O3 P2 Pd S2'
_chemical_formula_weight         750.87
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_audit_update_record
; 
? 
;
_cell_angle_alpha                104.6390(10)
_cell_angle_beta                 106.7250(10)
_cell_angle_gamma                90.9840(10)
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_cell_length_a                   8.8996(8)
_cell_length_b                   12.8830(11)
_cell_length_c                   14.7781(13)
_cell_measurement_reflns_used    6798
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.40
_cell_volume                     1562.6(2)
_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 V2008/1, TWINABS V2008/2 
(Bruker, 2005 & 2008) 
;
_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  'SHELX-2012/9 (Sheldrick, 2012)'
_computing_structure_solution    'SHELX-2012/9 (Sheldrick, 2012)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
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_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  bm51xas
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19155
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.112
_diffrn_reflns_theta_min         1.494
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_exptl_absorpt_correction_T_max  0.9393
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_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_id                bm51xas
_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 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.4918P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5656
_reflns_number_total             6763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505783z_si_002.cif
_cod_data_source_block           (CO)3Fe(pdt)Pd(dppe)
_cod_depositor_comments
'Adding full bibliography for 4122464--4122465.cif.'
_cod_database_code               4122464
_shelx_estimated_absorpt_t_min   0.638
_shelx_estimated_absorpt_t_max   0.928
_shelxl_version_number           2012-9
_shelx_res_checksum              12009
_shelx_hkl_checksum              7253