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_4346546
_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_absolute_configuration ad
_chemical_formula_moiety         'C35 H35 Fe Ni O P2 S2, C4 H8 O, B F4'
_chemical_formula_sum            'C39 H43 B F4 Fe Ni O2 P2 S2'
_chemical_formula_weight         871.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-12-13
_audit_creation_method
; 
Olex2 1.2 
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959) 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8768(5)
_cell_length_b                   14.4157(5)
_cell_length_c                   18.7392(7)
_cell_measurement_reflns_used    9610
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.59
_cell_volume                     3748.7(2)
_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      99.99
_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  c42f
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41146
_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         25.410
_diffrn_reflns_theta_min         2.309
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.865053
_exptl_absorpt_correction_T_min  0.738368
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction. 
 
For component 1: 
 wR2(int) was 0.0859 before and 0.0661 after correction. 
 The Ratio of minimum to maximum transmission not present. 
 The \l/2 correction factor is Not present 
 
For component 2: 
 wR2(int) was 0.0863 before and 0.0625 after correction. 
 The Ratio of minimum to maximum transmission is 0.85. 
 The \l/2 correction factor is Not present 
 
Final HKLF 4 output contains 122217 reflections, Rint = 0.0563 
 (93237 with I > 3sig(I), Rint = 0.0474) 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       prism
_exptl_crystal_F_000             1800
_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          0.121
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
; 
 Flack x determined using 2714 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         41146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0326P)^2^+2.6598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                36564
_reflns_number_total             41146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01662_si_002.cif
_cod_data_source_block           mo_cd42f_0m_a
_cod_database_code               4346546
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
; 
1. Twinned data refinement 
 Scales: 0.5337(18) 0.4663(18) 
2. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
3.a Secondary CH2 refined with riding coordinates: 
 C39(H39A,H39B), C36(H36A,H36B), C37(H37A,H37B), C7(H7A,H7B), C38(H38A,H38B), 
 C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B), C6(H6A,H6B) 
3.b Aromatic/amide H refined with riding coordinates: 
 C27(H27), C26(H26), C21(H21), C34(H34), C20(H20), C5(H5), C19(H19), C24(H24), 
 C1(H1), C32(H32), C25(H25), C18(H18), C2(H2), C31(H31), C28(H28), C4(H4), 
 C3(H3), C33(H33), C22(H22), C30(H30), C12(H12), C16(H16), C14(H14), C15(H15), 
 C13(H13) 
;
_olex2_submission_special_instructions 'No special instructions were received'