Chalcogenide substitution in the [2Fe] cluster of [FeFe]-hydrogenases conserves high enzymatic activity
Kertess, L.; Wittkamp, F.; Sommer, C.; Esselborn, J.; Rüdiger, O.; Reijerse, E. J.; Hofmann, E.; Lubitz, W.; Winkler, M.; Happe, T.; Apfel, U.-P.; Dalton Transactions  (2017) –; doi:10.1039/C7DT03785F

data_7044863
_publ_section_title
;
 Chalcogenide substitution in the [2Fe] cluster of [FeFe]-hydrogenases
 conserves high enzymatic activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03785F
_journal_year                    2017
_chemical_formula_moiety         'C16 H11 Fe2 N O8 Se2'
_chemical_formula_sum            'C16 H11 Fe2 N O8 Se2'
_chemical_formula_weight         614.88
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2017-08-23 deposited with the CCDC.
2017-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                100.188(2)
_cell_angle_beta                 100.216(2)
_cell_angle_gamma                100.918(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8537(2)
_cell_length_b                   9.3351(2)
_cell_length_c                   14.4434(4)
_cell_measurement_reflns_used    12916
_cell_measurement_temperature    114(4)
_cell_measurement_theta_max      76.0130
_cell_measurement_theta_min      4.9160
_cell_volume                     998.70(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      114(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9854
_diffrn_measurement_details
;
  1 omega  -37.00   75.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552  -77.0000  120.0000 112

  2 omega  -33.00   71.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552  -57.0000 -150.0000 104

  3 omega  -33.00   71.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552  -57.0000  -30.0000 104

  4 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000   30.0000 79

  5 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -30.0000 34

  6 omega   82.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  120.0000 76

  7 omega   29.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000   30.0000 80

  8 omega   35.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -60.0000 81

  9 omega   29.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -120.0000 80

 10 omega   85.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -150.0000 73

 11 omega   39.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   60.0000 104

 12 omega   35.00  150.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000   60.0000 115

 13 omega   35.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -150.0000 81

 14 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 34

 15 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -120.0000 34

 16 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  150.0000 79

 17 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -57.0000 -150.0000 103

 18 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000  -90.0000 112

 19 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000    0.0000 112

 20 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -57.0000   90.0000 103

 21 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 34

 22 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -120.0000 79

 23 omega   82.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   30.0000 76

 24 omega   83.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 75

 25 omega   85.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -60.0000 73

 26 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 79

 27 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   30.0000 79

 28 omega   85.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -30.0000 73

 29 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -57.0000   30.0000 103

 30 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000 -120.0000 112

 31 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000  150.0000 112

 32 omega    2.00   99.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3552 -125.0000   90.0000 97

 33 omega   83.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 75

 34 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 34

 35 omega   83.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   60.0000 75

 36 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  120.0000 79

 37 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000    0.0000 79

 38 omega   83.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -150.0000 75

 39 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   90.0000 79

 40 omega   83.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 75

 41 omega  -99.00   -2.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  125.0000 -180.0000 97

 42 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3552  -77.0000   30.0000 112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1882198000
_diffrn_orient_matrix_UB_12      -0.0419819000
_diffrn_orient_matrix_UB_13      0.0188173000
_diffrn_orient_matrix_UB_21      0.0049363000
_diffrn_orient_matrix_UB_22      -0.1665850000
_diffrn_orient_matrix_UB_23      -0.0220952000
_diffrn_orient_matrix_UB_31      0.0803335000
_diffrn_orient_matrix_UB_32      0.0118873000
_diffrn_orient_matrix_UB_33      0.1071869000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19974
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.180
_diffrn_reflns_theta_min         4.944
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.231
_exptl_absorpt_correction_T_max  0.390
_exptl_absorpt_correction_T_min  0.195
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.1744
_exptl_crystal_size_mid          0.1349
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0398P)^2^+0.5444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4007
_reflns_number_total             4101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03785f2.cif
_cod_data_source_block           2a
_cod_database_code               7044863
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C16 H11 N1 O8 Fe2 Se2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C12(H12), C16(H16), C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'