[FeFe]-Hydrogenase H-Cluster Mimics Mediated by Naphthalene Monoimide Derivatives of Peri-Substituted Dichalcogenides
Weigand, Wolfgang; Abul-Futouh, Hassan; Zagranyarski, Yulian; Müller, Carolin; Schulz, Martin; Kupfer, Stephan; Görls, Helmar; El-khateeb, Mohammad Yaseen; Gräfe, Stefanie; Dietzek, Benjamin; Peneva, Kalina; Dalton Trans.  (2017) –; doi:10.1039/C7DT02079A

data_7043441
_publ_section_title
;
 [FeFe]-Hydrogenase H-Cluster Mimics Mediated by Naphthalene Monoimide
 Derivatives of Peri-Substituted Dichalcogenides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02079A
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H19 Br2 Fe2 N O8 S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C32 H23 Br2 Cl4 Fe2 N O8 S2'
_chemical_formula_weight         1026.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-01-30 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9262(3)
_cell_length_b                   14.1295(3)
_cell_length_c                   19.6116(3)
_cell_measurement_reflns_used    23620
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.78
_cell_volume                     3858.98(13)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23620
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    3.257
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.422
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.473(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+17.2269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                7849
_reflns_number_total             8839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02079a2.cif
_cod_data_source_block           FO6138
_cod_database_code               7043441