Small iron‒carbonyl clusters bearing imidazolium-2-trithioperoxycarboxylate ligands
Beltrán Álvarez, Tomás Francisco F.; Zaragoza, Guillermo; Delaude, Lionel; Dalton Trans.  (2017) –; doi:10.1039/C7DT03202A

data_7044248
_publ_section_title
;
 Small iron--carbonyl clusters bearing
 imidazolium-2-trithioperoxycarboxylate ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03202A
_journal_year                    2017
_chemical_formula_moiety         'C28 H24 Fe2 N2 O6 S3'
_chemical_formula_sum            'C28 H24 Fe2 N2 O6 S3'
_chemical_formula_weight         692.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'direct - structure invariant direct methods'
_atom_sites_solution_secondary   'direct - structure invariant direct methods'
_audit_block_doi                 10.5517/ccdc.csd.cc1pdx33
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2017-07-10T12:50:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-07-11 deposited with the CCDC.
2017-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.563(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8189(3)
_cell_length_b                   14.3858(7)
_cell_length_c                   23.8316(12)
_cell_measurement_reflns_used    1955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      2.83
_cell_measurement_wavelength     0.71073
_cell_volume                     3020.4(2)
_computing_cell_refinement       'APPEX2v2014.11-0 (BRUKER AXS, 2005)'
_computing_data_collection       'APPEX2v2014.11-0 (BRUKER AXS, 2005)'
_computing_data_reduction        'APEX3 v2017.3-0 (BRUKER AXS, 2005)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            61786
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.131
_diffrn_reflns_theta_min         2.221
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  0.8373
_exptl_absorpt_correction_T_min  0.7676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS-2016/2'
_exptl_crystal_colour            Blue-Green
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     376
_refine_ls_number_reflns         8125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+1.3626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0
_reflns_number_gt                6276
_reflns_number_total             8125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03202a2.cif
_cod_data_source_block           TOBE72
_cod_database_code               7044248
_shelx_estimated_absorpt_t_min   0.728
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              73419