Tetrathia[7]helicene-Based Complexes of Ferrocene and (η5-Cyclohexadienyl)tricarbonylmanganese: Synthesis and Electrochemical Studies
Rose-Munch, Françoise; Li, Ming; Rose, Eric; Daran, Jean Claude; Bossi, Alberto; Licandro, Emanuela; Mussini, Patrizia Romana; Organometallics 31 (2012) 92–; doi:10.1021/om200571a

data_4067784
_publ_section_title
;
 Tetrathia[7]helicene-Based Complexes of Ferrocene and
 (\h5-Cyclohexadienyl)tricarbonylmanganese: Synthesis and Electrochemical
 Studies
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              92
_journal_paper_doi               10.1021/om200571a
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46 H24 Fe2 S4'
_chemical_formula_sum            'C23 H12 Fe S2'
_chemical_formula_weight         408.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.286(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.8995(4)
_cell_length_b                   9.7167(3)
_cell_length_c                   20.6494(5)
_cell_measurement_reflns_used    3568
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.1
_cell_measurement_theta_min      2.6
_cell_volume                     3390.74(16)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -54.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000    0.0000    0.0000    0.0000 115

  2 omega  -54.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000   90.0000    0.0000    0.0000 115

  3 omega  -54.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  180.0000    0.0000    0.0000 115

  4 omega  -54.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  270.0000    0.0000    0.0000 115

;
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       '\w and \f'
_diffrn_orient_matrix_UB_11      -0.0137079710
_diffrn_orient_matrix_UB_12      0.0454696382
_diffrn_orient_matrix_UB_13      0.0244856025
_diffrn_orient_matrix_UB_21      0.0178068567
_diffrn_orient_matrix_UB_22      0.0560991904
_diffrn_orient_matrix_UB_23      -0.0164916963
_diffrn_orient_matrix_UB_31      -0.0354265391
_diffrn_orient_matrix_UB_32      0.0106163906
_diffrn_orient_matrix_UB_33      -0.0175917312
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16757
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2006)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                3125
_reflns_number_total             4955
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200571a_si_002.cif
_cod_data_source_block           lm033
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4067784