[FeFe]-Hydrogenase Synthetic Mimics Based onPeri-Substituted Dichalcogenides
Figliola, Carlotta; Male, Louise; Horton, Peter N.; Pitak, Mateusz B.; Coles, Simon J.; Horswell, Sarah L.; Grainger, Richard S.; Organometallics 33 (2014) 4449–; doi:10.1021/om500683p

data_4084250
_publ_section_title
;
 [FeFe]-Hydrogenase Synthetic Mimics Based onPeri-Substituted
 Dichalcogenides
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4449
_journal_paper_doi               10.1021/om500683p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H22 Fe2 O6 S Se'
_chemical_formula_sum            'C24 H22 Fe2 O6 S Se'
_chemical_formula_weight         629.13
_chemical_name_systematic
;
[{Fe(CO)~3~}~2~(\m~2~-1,8-SeS-2,7-di-<i>tert</i>-butyl-naph)]
;
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                79.877(8)
_cell_angle_beta                 87.581(9)
_cell_angle_gamma                87.026(9)
_cell_formula_units_Z            4
_cell_length_a                   7.4178(5)
_cell_length_b                   14.1007(10)
_cell_length_c                   24.3025(17)
_cell_measurement_reflns_used    10675
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.4
_cell_volume                     2497.6(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov, O.V., Bourhis, L.J., Gildea, R.J., Howard, J.A.K,
& Puschmann, H., 2009)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_radiation_monochromator  Mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_av_unetI/netI     0.1384
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23769
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.435
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    2.740
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.573
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         8494
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.1000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1268P)^2^+39.5065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2357
_refine_ls_wR_factor_ref         0.2862
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5059
_reflns_number_total             8494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500683p_si_002.cif
_cod_data_source_block           7b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4084250
_publ_secton_comment
;
The structure contains two crystallographically-independent molecules.
The sulphur and selenium atoms in both molecules are both disordered 
over two positions, with the refined percentage occupancy ratio between 
the major and minor positions (labelled Se/S and S'/Se' in molecule 1 
and Se1/S1 and S1'/Se1' in molecule 2 respectively), being 
51.1 (8) : 48.9 (8) (molecule 1) and 53.0 (8) : 47.0 (8) (molecule 2).
The hydrogen atoms were added at calculated positions and 
refined by use of a riding model with the isotropic 
displacement parameters based on the equivalent isotropic 
displacement parameter (Ueq) of the parent atom.
;
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.973
_shelxl_version_number           2013-4
_shelx_res_checksum              99220
_shelx_hkl_checksum              18442