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_4122465
_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
; 
2(C32 H31 Fe O3 P2 Pd S2), 2(B F4), 2(C4 H8 O), C4 H10 O 
;
_chemical_formula_sum            'C76 H88 B2 F8 Fe2 O9 P4 Pd2 S4'
_chemical_formula_weight         1895.70
_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                 97.4120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4661(8)
_cell_length_b                   20.6923(14)
_cell_length_c                   34.720(2)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.19
_cell_volume                     8168.8(9)
_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 V2008/2, 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  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      178(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  bm11yas
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            90489
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.8982
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3864
_exptl_crystal_id                bm11yas
_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, -3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1217
_refine_ls_number_reflns         15107
_refine_ls_number_restraints     1297
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+5.8634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                11178
_reflns_number_total             15107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja505783z_si_002.cif
_cod_data_source_block           '[(CO)3FeH(pdt)Pd(dppe)]BF4'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122464--4122465.cif.
;
_cod_original_cell_volume        8168.9(10)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               4122465