Crystal structure of [μ~2~-3,3-dimethyl-4-(propan-2-ylidene)thietane-2,2-dithiolato-κ^4^<i>S</i>:<i>S</i>':<i>S</i>:<i>S</i>']bis[tricarbonyliron(I)](<i>Fe</i>—<i>Fe</i>)
Zhao, Peihua; Bertke, Jeffery A.; Rauchfuss, Thomas B.; Acta Crystallographica Section E 71 (2015) 1296–1299; doi:10.1107/S2056989015018496

data_2241191
_publ_contact_author
;
Jeffery A. Bertke
School of Chemical Sciences
University of Illinois at Urbana-Champaign
Urbana, Illinois  61801
USA
;
_publ_section_title
;
 Crystal structure of
 [\m~2~-3,3-dimethyl-4-(propan-2-ylidene)thietane-2,2-dithiolato-\k^4^<i>S</i>:<i>S</i>':<i>S</i>:<i>S</i>']bis[tricarbonyliron(I)](<i>Fe</i>---<i>Fe</i>)
;
_journal_coeditor_code           WM5218
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1296
_journal_page_last               1299
_journal_paper_doi               10.1107/S2056989015018496
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Fe2 (C8 H12 S3) (C O)6]'
_chemical_formula_moiety         'C14 H12 Fe2 O6 S3'
_chemical_formula_sum            'C14 H12 Fe2 O6 S3'
_chemical_formula_weight         484.12
_chemical_name_systematic
'[\m~2~-3,3-Dimethyl-4-(propan-2-ylidene)thietane-2,2-dithiolato-\k^4^<i>S</i>,<i>S</i>':<i>S</i>,<i>S</i>]bis[tricarbonyliron(I)](<i>Fe</i>---<i>Fe</i>)'
_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-2014/6
_cell_angle_alpha                88.092(6)
_cell_angle_beta                 78.668(6)
_cell_angle_gamma                76.559(6)
_cell_formula_units_Z            2
_cell_length_a                   9.3619(10)
_cell_length_b                   9.7681(11)
_cell_length_c                   10.6249(12)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.28
_cell_volume                     926.51(18)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014) and SHELXTL (Sheldrick, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008), <i>CrystalMaker</i> (CrystalMaker,
1994)
;
_computing_publication_material
;
XCIF (Bruker, 2014), publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_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  0.0335
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26313
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.171
_diffrn_reflns_theta_min         2.700
_exptl_absorpt_coefficient_mu    1.930
_exptl_absorpt_correction_T_max  0.93493
_exptl_absorpt_correction_T_min  0.75166
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0274P)^2^+0.4094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                3603
_reflns_number_total             4095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5218sup1.cif
_cod_data_source_block           I
_cod_database_code               2241191
_shelx_estimated_absorpt_t_min   0.628
_shelx_estimated_absorpt_t_max   0.903
_shelx_hkl_checksum              57549
_shelx_res_checksum              65819
_shelxl_version_number           2014/6
_cod_database_fobs_code 2241191