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_4346551
_publ_section_title
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 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         'C44 H37 Fe Ni O P2 S2'
_chemical_formula_sum            'C44 H37 Fe Ni O P2 S2'
_chemical_formula_weight         822.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-06
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 99.419(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0127(7)
_cell_length_b                   21.3183(14)
_cell_length_c                   18.3474(12)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.44
_cell_volume                     4249.4(5)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd82s_0m
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            122795
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.334
_diffrn_reflns_theta_min         2.217
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.9661
_exptl_absorpt_correction_T_min  0.7846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.1455 before and 0.0674 after correction. 
The Ratio of minimum to maximum transmission is 0.8121. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       plate
_exptl_crystal_F_000             1700
_exptl_crystal_id                CpNiFeSPh0
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the 2 3 -3 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0474P)^2^+2.4414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9147
_reflns_number_total             10581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01662_si_002.cif
_cod_data_source_block           mo_cd82s_0m
_cod_database_code               4346551
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.731
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
2.a Aromatic/amide H refined with riding coordinates: 
 C7(H7), C1(H1), C5(H5), C9(H9), C28(H28), C43(H43), C18(H18), C27(H27), 
 C11(H11), C17(H17), C23(H23), C8(H8), C19(H19), C25(H25), C13(H13), C16(H16), 
 C40(H40), C29(H29), C10(H10), C4(H4), C34(H34), C3(H3), C24(H24), C31(H31), 
 C33(H33), C42(H42), C41(H41), C2(H2), C39(H39), C35(H35), C36(H36), C37(H37), 
 C30(H30), C15(H15), C21(H21), C14(H14), C22(H22) 
;
_smtbx_masks_special_details
; 
Solvent was present in the unit cell. The solvent was partially occupied and by 
two different species, which were disordered. These species were determined to b 
pentane and toluene. The residual electron density equated to 30.3, indicating a 
greater occupancy than 0.5, but less than 0.75. Attempts to model this disorder 
preliminarily yielded an approximately 50:50 ratio of pentane to toluene. 
;
_olex2_submission_special_instructions 'No special instructions were received'