Models of the Ni-L and Ni-SIa States of the [NiFe]-Hydrogenase Active Site.
Chambers, Geoffrey M.; Huynh, Mioy T.; Li, Yulong; Hammes-Schiffer, Sharon; Rauchfuss, Thomas B.; Reijerse, Edward; Lubitz, Wolfgang; Inorganic chemistry 55 (2016) 419–431; doi:10.1021/acs.inorgchem.5b01662

data_4346547
_publ_section_title
;
 Models of the Ni-L and Ni-SIa States of the [NiFe]-Hydrogenase Active
 Site.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              419
_journal_page_last               431
_journal_paper_doi               10.1021/acs.inorgchem.5b01662
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C35 H35 Fe Ni O P2 S2, C7 H8'
_chemical_formula_sum            'C42 H43 Fe Ni O P2 S2'
_chemical_formula_weight         804.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-12-12
_audit_creation_method
; 
Olex2 1.2 
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959) 
;
_cell_angle_alpha                90
_cell_angle_beta                 112.4382(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6228(3)
_cell_length_b                   23.8083(9)
_cell_length_c                   9.7696(4)
_cell_measurement_reflns_used    5406
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.416
_cell_measurement_theta_min      2.256
_cell_volume                     1853.80(12)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      183.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm73a
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.514
_diffrn_reflns_theta_min         2.255
_exptl_absorpt_coefficient_mu    1.131
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9322
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0708 before and 0.0444 after correction. 
The Ratio of minimum to maximum transmission is 0.9336. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       prism
_exptl_crystal_F_000             838
_exptl_crystal_id                MeCpNiFe
_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 3 face scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3937
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.000
_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^+0.6504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3282
_reflns_number_total             3937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01662_si_002.cif
_cod_data_source_block           mo_cd73a_0m
_cod_database_code               4346547
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.826
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Uiso/Uaniso restraints and constraints 
P1 \\sim P2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim 
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim 
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim 
C31 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of 
0.02 
3. Others 
 Fixed Sof: P1(0.5) P2(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) 
 H8B(0.5) C9(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) 
 C13(0.5) H13(0.5) C14(0.5) H14(0.5) C15(0.5) C16(0.5) H16(0.5) C17(0.5) 
 H17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5) H20(0.5) C21(0.5) 
 C22(0.5) H22(0.5) C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) 
 C26(0.5) H26(0.5) C27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) 
 H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5) C100(0.5) C101(0.5) H101(0.5) 
 C102(0.5) H102(0.5) C103(0.5) H103(0.5) C104(0.5) H104(0.5) C105(0.5) 
 H105(0.5) C106(0.5) H10A(0.5) H10B(0.5) H10C(0.5) 
4.a Ternary CH refined with riding coordinates: 
 C1(H1), C2(H2), C3(H3) 
4.b Secondary CH2 refined with riding coordinates: 
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B) 
4.c Aromatic/amide H refined with riding coordinates: 
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), 
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), 
 C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105) 
4.d Fitted hexagon refined as free rotating group: 
 C9(C10,C11,C12,C13,C14), C15(C16,C17,C18,C19,C20), C21(C22,C23,C24,C25,C26), 
 C27(C28,C29,C30,C31,C32), C100(C101,C102,C103,C104,C105) 
4.e Idealised Me refined as rotating group: 
 C106(H10A,H10B,H10C) 
;
_olex2_submission_special_instructions 'No special instructions were received'