#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:30:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178568 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/77/4067784.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4067784
loop_
_publ_author_name
'Rose-Munch, Françoise'
'Li, Ming'
'Rose, Eric'
'Daran, Jean Claude'
'Bossi, Alberto'
'Licandro, Emanuela'
'Mussini, Patrizia Romana'
_publ_section_title
;
 Tetrathia[7]helicene-Based Complexes of Ferrocene and
 (η5-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       'ω and φ'
_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/[σ²(Fo²)+(0.0659P)²+0.0000P] where P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.622287(19) 0.01870(4) 0.260161(16) 0.02636(11) Uani 1 1 d .
S3 S 0.92176(4) 0.08386(7) 0.03964(3) 0.03107(16) Uani 1 1 d .
S6 S 0.90454(4) 0.66273(7) -0.08050(3) 0.03880(18) Uani 1 1 d .
C1 C 0.80813(13) 0.2557(2) 0.05916(10) 0.0251(5) Uani 1 1 d .
H1 H 0.7619 0.2983 0.0758 0.030 Uiso 1 1 calc R
C2 C 0.83587(13) 0.1333(2) 0.08091(11) 0.0266(5) Uani 1 1 d .
C3A C 0.92098(14) 0.2333(3) -0.00644(11) 0.0266(5) Uani 1 1 d .
C3B C 0.85497(13) 0.3150(2) 0.00866(10) 0.0245(5) Uani 1 1 d .
C4 C 0.98032(14) 0.2761(3) -0.04996(11) 0.0318(6) Uani 1 1 d .
H4 H 1.0226 0.2163 -0.0610 0.038 Uiso 1 1 calc R
C5 C 0.97575(14) 0.4047(3) -0.07578(11) 0.0348(6) Uani 1 1 d .
H5 H 1.0162 0.4372 -0.1037 0.042 Uiso 1 1 calc R
C5A C 0.91092(15) 0.4890(3) -0.06088(12) 0.0310(5) Uani 1 1 d .
C5B C 0.84712(14) 0.4449(3) -0.02267(11) 0.0265(5) Uani 1 1 d .
C6A C 0.81772(16) 0.6801(3) -0.03578(12) 0.0353(6) Uani 1 1 d .
C6B C 0.78853(14) 0.5526(3) -0.01404(11) 0.0289(5) Uani 1 1 d .
C7 C 0.78244(17) 0.8073(3) -0.02024(14) 0.0436(7) Uani 1 1 d .
C8 C 0.80309(14) 0.0529(3) 0.13243(12) 0.0289(5) Uani 1 1 d .
C9 C 0.77057(15) -0.0003(2) 0.17670(12) 0.0307(5) Uani 1 1 d .
C10 C 0.72912(14) -0.0552(3) 0.23174(11) 0.0287(5) Uani 1 1 d .
C11 C 0.73353(15) -0.0039(3) 0.29639(12) 0.0337(6) Uani 1 1 d .
H11 H 0.7671 0.0680 0.3112 0.040 Uiso 1 1 calc R
C12 C 0.67869(15) -0.0798(3) 0.33489(12) 0.0355(6) Uani 1 1 d .
H12 H 0.6698 -0.0670 0.3799 0.043 Uiso 1 1 calc R
C13 C 0.64047(15) -0.1757(3) 0.29547(12) 0.0333(6) Uani 1 1 d .
H13 H 0.6009 -0.2390 0.3089 0.040 Uiso 1 1 calc R
C14 C 0.67116(15) -0.1624(3) 0.23139(12) 0.0314(5) Uani 1 1 d .
H14 H 0.6557 -0.2156 0.1949 0.038 Uiso 1 1 calc R
C15 C 0.59116(19) 0.1575(3) 0.19105(15) 0.0502(8) Uani 1 1 d .
H15 H 0.6196 0.1761 0.1524 0.060 Uiso 1 1 calc R
C16 C 0.60093(19) 0.2239(3) 0.25050(16) 0.0499(8) Uani 1 1 d .
H16 H 0.6375 0.2959 0.2594 0.060 Uiso 1 1 calc R
C17 C 0.54758(17) 0.1665(3) 0.29506(14) 0.0426(7) Uani 1 1 d .
H17 H 0.5419 0.1932 0.3390 0.051 Uiso 1 1 calc R
C18 C 0.50436(16) 0.0631(3) 0.26357(14) 0.0424(7) Uani 1 1 d .
H18 H 0.4644 0.0072 0.2823 0.051 Uiso 1 1 calc R
C19 C 0.53082(18) 0.0568(3) 0.19890(15) 0.0483(8) Uani 1 1 d .
H19 H 0.5117 -0.0040 0.1663 0.058 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C19 Fe1 C15 41.06(13) . .
C19 Fe1 C11 162.00(12) . .
C15 Fe1 C11 124.52(12) . .
C19 Fe1 C10 124.07(11) . .
C15 Fe1 C10 105.01(11) . .
C11 Fe1 C10 41.09(10) . .
C19 Fe1 C14 106.57(12) . .
C15 Fe1 C14 118.25(12) . .
C11 Fe1 C14 68.74(11) . .
C10 Fe1 C14 41.18(10) . .
C19 Fe1 C16 68.02(14) . .
C15 Fe1 C16 40.15(13) . .
C11 Fe1 C16 107.78(13) . .
C10 Fe1 C16 118.35(11) . .
C14 Fe1 C16 152.96(11) . .
C19 Fe1 C18 40.62(12) . .
C15 Fe1 C18 68.55(12) . .
C11 Fe1 C18 155.81(11) . .
C10 Fe1 C18 162.52(11) . .
C14 Fe1 C18 126.23(11) . .
C16 Fe1 C18 67.90(13) . .
C19 Fe1 C17 67.76(13) . .
C15 Fe1 C17 67.87(12) . .
C11 Fe1 C17 121.19(12) . .
C10 Fe1 C17 154.22(11) . .
C14 Fe1 C17 164.26(11) . .
C16 Fe1 C17 40.33(11) . .
C18 Fe1 C17 40.08(12) . .
C19 Fe1 C12 155.05(12) . .
C15 Fe1 C12 163.37(13) . .
C11 Fe1 C12 41.01(10) . .
C10 Fe1 C12 68.99(10) . .
C14 Fe1 C12 68.12(11) . .
C16 Fe1 C12 127.84(13) . .
C18 Fe1 C12 121.59(11) . .
C17 Fe1 C12 110.40(12) . .
C19 Fe1 C13 120.23(12) . .
C15 Fe1 C13 154.25(12) . .
C11 Fe1 C13 68.41(11) . .
C10 Fe1 C13 69.21(10) . .
C14 Fe1 C13 41.01(10) . .
C16 Fe1 C13 164.73(12) . .
C18 Fe1 C13 109.12(11) . .
C17 Fe1 C13 127.88(11) . .
C12 Fe1 C13 39.80(11) . .
C3A S3 C2 91.89(11) . .
C5A S6 C6A 91.27(12) . .
C2 C1 C3B 113.8(2) . .
C1 C2 C8 126.2(2) . .
C1 C2 S3 111.44(17) . .
C8 C2 S3 122.33(18) . .
C3B C3A C4 122.8(2) . .
C3B C3A S3 110.78(17) . .
C4 C3A S3 126.3(2) . .
C3A C3B C5B 118.2(2) . .
C3A C3B C1 112.1(2) . .
C5B C3B C1 129.5(2) . .
C5 C4 C3A 118.7(2) . .
C4 C5 C5A 119.5(2) . .
C5 C5A C5B 123.2(2) . .
C5 C5A S6 124.26(19) . .
C5B C5A S6 112.3(2) . .
C5A C5B C3B 117.1(2) . .
C5A C5B C6B 112.0(2) . .
C3B C5B C6B 130.2(2) . .
C6B C6A C7 123.3(3) . .
C6B C6A S6 112.4(2) . .
C7 C6A S6 124.3(2) . .
C6A C6B C6B 116.83(16) . 2_655
C6A C6B C5B 110.8(2) . .
C6B C6B C5B 132.32(14) 2_655 .
C7 C7 C6A 118.39(17) 2_655 .
C9 C8 C2 172.1(3) . .
C8 C9 C10 175.9(3) . .
C11 C10 C14 107.0(2) . .
C11 C10 C9 125.9(2) . .
C14 C10 C9 127.0(2) . .
C11 C10 Fe1 69.44(14) . .
C14 C10 Fe1 69.47(14) . .
C9 C10 Fe1 122.24(17) . .
C10 C11 C12 108.0(2) . .
C10 C11 Fe1 69.47(14) . .
C12 C11 Fe1 70.08(14) . .
C13 C12 C11 108.7(2) . .
C13 C12 Fe1 70.12(14) . .
C11 C12 Fe1 68.91(14) . .
C12 C13 C14 108.1(2) . .
C12 C13 Fe1 70.08(15) . .
C14 C13 Fe1 68.97(14) . .
C13 C14 C10 108.2(2) . .
C13 C14 Fe1 70.02(14) . .
C10 C14 Fe1 69.35(14) . .
C16 C15 C19 107.4(3) . .
C16 C15 Fe1 70.13(17) . .
C19 C15 Fe1 69.31(15) . .
C15 C16 C17 108.5(3) . .
C15 C16 Fe1 69.72(17) . .
C17 C16 Fe1 70.19(17) . .
C18 C17 C16 108.4(3) . .
C18 C17 Fe1 69.78(16) . .
C16 C17 Fe1 69.48(16) . .
C17 C18 C19 107.6(3) . .
C17 C18 Fe1 70.14(16) . .
C19 C18 Fe1 69.16(16) . .
C18 C19 C15 108.0(3) . .
C18 C19 Fe1 70.22(16) . .
C15 C19 Fe1 69.63(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C19 2.027(3) .
Fe1 C15 2.031(3) .
Fe1 C11 2.032(3) .
Fe1 C10 2.032(2) .
Fe1 C14 2.034(3) .
Fe1 C16 2.036(3) .
Fe1 C18 2.041(3) .
Fe1 C17 2.045(3) .
Fe1 C12 2.047(2) .
Fe1 C13 2.048(2) .
S3 C3A 1.736(2) .
S3 C2 1.754(2) .
S6 C5A 1.740(3) .
S6 C6A 1.746(3) .
C1 C2 1.354(3) .
C1 C3B 1.433(3) .
C2 C8 1.434(3) .
C3A C3B 1.406(3) .
C3A C4 1.413(3) .
C3B C5B 1.424(3) .
C4 C5 1.360(4) .
C5 C5A 1.403(4) .
C5A C5B 1.406(3) .
C5B C6B 1.453(3) .
C6A C6B 1.408(3) .
C6A C7 1.410(4) .
C6B C6B 1.428(5) 2_655
C7 C7 1.382(6) 2_655
C8 C9 1.187(3) .
C9 C10 1.440(3) .
C10 C11 1.426(3) .
C10 C14 1.430(3) .
C11 C12 1.429(3) .
C12 C13 1.394(4) .
C13 C14 1.430(3) .
C15 C16 1.396(5) .
C15 C19 1.423(4) .
C16 C17 1.407(4) .
C17 C18 1.400(4) .
C18 C19 1.412(4) .
