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_7044862
_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         'C11 H9 Fe2 N O8 Se2'
_chemical_formula_sum            'C11 H9 Fe2 N O8 Se2'
_chemical_formula_weight         552.81
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-08-23 deposited with the CCDC.
2017-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8436(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.78531(10)
_cell_length_b                   8.65801(11)
_cell_length_c                   20.60799(20)
_cell_measurement_reflns_used    15388
_cell_measurement_temperature    111(1)
_cell_measurement_theta_max      75.9370
_cell_measurement_theta_min      4.3770
_cell_volume                     1702.25(3)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      111(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -71.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302   57.0000   60.0000 104

  2 omega -124.00  -79.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000   60.0000 45

  3 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000  -90.0000 103

  4 omega  -20.00   83.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2302  -99.0000 -180.0000 103

  5 omega   35.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -90.0000 81

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

  7 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 34

  8 omega   35.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -30.0000 81

  9 omega   39.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   90.0000 104

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

 11 omega   52.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000   60.0000 106

 12 omega   35.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  120.0000 81

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

 14 omega   35.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 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   52.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000 -180.0000 106

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

 18 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000  120.0000 103

 19 omega -124.00  -79.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -99.0000  120.0000 45

 20 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000 -180.0000 103

 21 omega -115.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -57.0000    0.0000 103

 22 omega    4.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2302   88.0000   97.1606 29

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

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

 25 omega   82.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -60.0000 76

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

 27 omega   83.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 75

 28 omega   79.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -60.0000 79

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

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

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

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

 33 omega -120.00  -32.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000  -60.0000 88

 34 omega -120.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302  -77.0000   90.0000 112

 35 omega -114.00  -66.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302 -137.0000 -170.0000 48

 36 omega    2.00   99.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2302 -125.0000  150.0000 97

 37 omega    2.00   99.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2302 -125.0000  -60.0000 97
;
_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      -0.0696429000
_diffrn_orient_matrix_UB_12      0.0413224000
_diffrn_orient_matrix_UB_13      0.0578364000
_diffrn_orient_matrix_UB_21      0.1363995000
_diffrn_orient_matrix_UB_22      -0.0419698000
_diffrn_orient_matrix_UB_23      0.0503537000
_diffrn_orient_matrix_UB_31      0.0511781000
_diffrn_orient_matrix_UB_32      0.1678423000
_diffrn_orient_matrix_UB_33      -0.0016614000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25880
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.407
_diffrn_reflns_theta_min         4.401
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.940
_exptl_absorpt_correction_T_max  0.412
_exptl_absorpt_correction_T_min  0.078
_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    2.157
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1027
_exptl_crystal_size_min          0.0791
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0171
_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^)+(0.0235P)^2^+0.8683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3437
_reflns_number_total             3540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03785f2.cif
_cod_data_source_block           2b
_cod_database_code               7044862
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe2 Se2 C11 H20 N2 O4 '
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C19(H19A,H19B)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'