#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:19:13 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179104 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/66/4306663.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_4306663
loop_
_publ_author_name
'Daniel J. Harrison'
'Antonio G. De Crisci'
'Alan J. Lough'
'Mitchell J. Kerr'
'Ulrich Fekl'
_publ_section_title
;
Nickel Dithiolene Chelate Rings in a New Role as η5-Coordinating Ligands:
Synthesis, Structural Characterization, and Redox Reactivity of an
"Fe2Ni" Bis-Double-Decker
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10199
_journal_page_last               10201
_journal_paper_doi               10.1021/ic801487f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C28 H42 Fe2 Ni S4, B F4'
_chemical_formula_sum            'C28 H42 B F4 Fe2 Ni S4'
_chemical_formula_weight         764.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.1233(17)
_cell_angle_beta                 101.2840(19)
_cell_angle_gamma                104.741(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2743(2)
_cell_length_b                   8.3071(3)
_cell_length_c                   12.9787(5)
_cell_measurement_reflns_used    10562
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.7
_cell_volume                     799.37(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'ω scans and ω scans with κ offsets'
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10562
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.781
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             395
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0369
_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)+(0.0473P)²+0.6597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                2902
_reflns_number_total             3599
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic801487f_si_002.cif
_cod_data_source_block           k08209
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4306663
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54858(4) 0.74926(4) 0.19370(3) 0.01641(12) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.5000 0.0000 0.01886(13) Uani 1 2 d S . .
S1 S 0.67608(8) 0.53717(9) 0.15788(6) 0.02231(16) Uani 1 1 d . . .
S2 S 0.58839(9) 0.78095(9) 0.03104(6) 0.02285(16) Uani 1 1 d . . .
C1 C 0.8061(3) 0.7605(4) 0.2097(2) 0.0238(6) Uani 1 1 d . . .
C2 C 0.7659(3) 0.8727(4) 0.1522(2) 0.0242(6) Uani 1 1 d . . .
C3 C 0.9550(3) 0.8180(4) 0.3130(2) 0.0322(7) Uani 1 1 d . . .
H3A H 1.0589 0.8019 0.2922 0.048 Uiso 1 1 calc R . .
H3B H 0.9243 0.7471 0.3602 0.048 Uiso 1 1 calc R . .
H3C H 0.9787 0.9426 0.3538 0.048 Uiso 1 1 calc R . .
C4 C 0.8660(4) 1.0649(4) 0.1838(3) 0.0367(8) Uani 1 1 d . . .
H4A H 0.9654 1.0781 0.1525 0.055 Uiso 1 1 calc R . .
H4B H 0.9081 1.1165 0.2650 0.055 Uiso 1 1 calc R . .
H4C H 0.7899 1.1253 0.1545 0.055 Uiso 1 1 calc R . .
C5 C 0.5417(3) 0.8936(3) 0.3490(2) 0.0210(5) Uani 1 1 d . . .
C6 C 0.4517(4) 0.9451(4) 0.2635(2) 0.0235(6) Uani 1 1 d . . .
C7 C 0.3126(3) 0.7914(4) 0.1882(2) 0.0261(6) Uani 1 1 d . . .
C8 C 0.3157(3) 0.6477(4) 0.2282(2) 0.0236(6) Uani 1 1 d . . .
C9 C 0.4576(3) 0.7113(4) 0.3275(2) 0.0223(6) Uani 1 1 d . . .
C10 C 0.6923(4) 1.0124(4) 0.4468(3) 0.0360(8) Uani 1 1 d . . .
H10A H 0.6489 1.0679 0.5071 0.054 Uiso 1 1 calc R . .
H10B H 0.7648 1.1038 0.4251 0.054 Uiso 1 1 calc R . .
H10C H 0.7619 0.9435 0.4722 0.054 Uiso 1 1 calc R . .
C11 C 0.4870(5) 1.1270(4) 0.2581(3) 0.0461(9) Uani 1 1 d . . .
H11A H 0.4077 1.1807 0.2900 0.069 Uiso 1 1 calc R . .
H11B H 0.4690 1.1228 0.1804 0.069 Uiso 1 1 calc R . .
H11C H 0.6076 1.1974 0.3004 0.069 Uiso 1 1 calc R . .
C12 C 0.1853(4) 0.7842(6) 0.0865(3) 0.0463(9) Uani 1 1 d . . .
H12A H 0.0736 0.7819 0.1019 0.069 Uiso 1 1 calc R . .
H12B H 0.1688 0.6777 0.0254 0.069 Uiso 1 1 calc R . .
H12C H 0.2302 0.8884 0.0654 0.069 Uiso 1 1 calc R . .
C13 C 0.1888(4) 0.4656(4) 0.1796(3) 0.0445(9) Uani 1 1 d . . .
H13A H 0.0944 0.4569 0.2153 0.067 Uiso 1 1 calc R . .
H13B H 0.2481 0.3813 0.1919 0.067 Uiso 1 1 calc R . .
H13C H 0.1405 0.4391 0.0995 0.067 Uiso 1 1 calc R . .
C14 C 0.5041(5) 0.6058(5) 0.3998(3) 0.0389(8) Uani 1 1 d . . .
H14A H 0.4327 0.6053 0.4517 0.058 Uiso 1 1 calc R . .
H14B H 0.6275 0.6587 0.4416 0.058 Uiso 1 1 calc R . .
H14C H 0.4826 0.4846 0.3531 0.058 Uiso 1 1 calc R . .
F1 F 0.0609(5) 0.3115(5) 0.4621(3) 0.0500(10) Uani 0.50 1 d PD A -1
F2 F 0.0915(14) 0.5567(9) 0.5964(4) 0.105(4) Uani 0.50 1 d PD A -1
F3 F 0.1143(10) 0.5687(7) 0.4309(6) 0.095(2) Uani 0.50 1 d PD A -1
F4 F -0.1437(6) 0.4405(9) 0.4502(9) 0.142(6) Uani 0.50 1 d PD A -1
B1 B 0.0303(6) 0.4709(9) 0.4850(4) 0.0388(19) Uani 0.50 1 d PD A -1
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
_geom_angle_publ_flag
C7 Fe1 C6 40.77(11) . . ?
C7 Fe1 C2 132.29(12) . . ?
C6 Fe1 C2 106.40(11) . . ?
C7 Fe1 C1 168.70(12) . . ?
C6 Fe1 C1 128.67(11) . . ?
C2 Fe1 C1 39.44(12) . . ?
C7 Fe1 C5 68.12(11) . . ?
C6 Fe1 C5 40.40(11) . . ?
C2 Fe1 C5 111.46(11) . . ?
C1 Fe1 C5 106.02(10) . . ?
C7 Fe1 C8 40.21(12) . . ?
C6 Fe1 C8 67.86(11) . . ?
C2 Fe1 C8 172.49(11) . . ?
C1 Fe1 C8 147.96(12) . . ?
C5 Fe1 C8 67.66(10) . . ?
C7 Fe1 C9 67.67(11) . . ?
C6 Fe1 C9 67.50(11) . . ?
C2 Fe1 C9 143.26(11) . . ?
C1 Fe1 C9 114.56(11) . . ?
C5 Fe1 C9 39.92(10) . . ?
C8 Fe1 C9 40.24(11) . . ?
C7 Fe1 S1 143.69(9) . . ?
C6 Fe1 S1 166.93(8) . . ?
C2 Fe1 S1 77.44(8) . . ?
C1 Fe1 S1 47.59(8) . . ?
C5 Fe1 S1 126.53(8) . . ?
C8 Fe1 S1 109.26(8) . . ?
C9 Fe1 S1 101.76(8) . . ?
C7 Fe1 S2 101.14(8) . . ?
C6 Fe1 S2 107.16(8) . . ?
C2 Fe1 S2 47.65(8) . . ?
C1 Fe1 S2 77.24(8) . . ?
C5 Fe1 S2 141.36(8) . . ?
C8 Fe1 S2 128.20(8) . . ?
C9 Fe1 S2 168.05(8) . . ?
S1 Fe1 S2 84.77(3) . . ?
C7 Fe1 Ni1 106.02(8) . . ?
C6 Fe1 Ni1 141.30(8) . . ?
C2 Fe1 Ni1 81.93(8) . . ?
C1 Fe1 Ni1 81.79(7) . . ?
C5 Fe1 Ni1 166.13(8) . . ?
C8 Fe1 Ni1 99.56(8) . . ?
C9 Fe1 Ni1 126.52(8) . . ?
S1 Fe1 Ni1 50.937(18) . . ?
S2 Fe1 Ni1 50.803(18) . . ?
S2 Ni1 S2 180.000(12) 2_665 . ?
S2 Ni1 S1 90.01(3) 2_665 . ?
S2 Ni1 S1 89.99(3) . . ?
S2 Ni1 S1 89.99(3) 2_665 2_665 ?
S2 Ni1 S1 90.01(3) . 2_665 ?
S1 Ni1 S1 180.0 . 2_665 ?
S2 Ni1 Fe1 54.49(2) 2_665 2_665 ?
S2 Ni1 Fe1 125.51(2) . 2_665 ?
S1 Ni1 Fe1 125.591(19) . 2_665 ?
S1 Ni1 Fe1 54.409(19) 2_665 2_665 ?
S2 Ni1 Fe1 125.505(19) 2_665 . ?
S2 Ni1 Fe1 54.49(2) . . ?
S1 Ni1 Fe1 54.409(19) . . ?
S1 Ni1 Fe1 125.591(19) 2_665 . ?
Fe1 Ni1 Fe1 180.00(2) 2_665 . ?
C1 S1 Ni1 106.42(10) . . ?
C1 S1 Fe1 60.48(9) . . ?
Ni1 S1 Fe1 74.65(2) . . ?
C2 S2 Ni1 106.69(10) . . ?
C2 S2 Fe1 60.37(9) . . ?
Ni1 S2 Fe1 74.70(2) . . ?
C2 C1 C3 124.2(3) . . ?
C2 C1 S1 118.3(2) . . ?
C3 C1 S1 117.6(2) . . ?
C2 C1 Fe1 70.24(15) . . ?
C3 C1 Fe1 129.7(2) . . ?
S1 C1 Fe1 71.94(9) . . ?
C1 C2 C4 124.9(3) . . ?
C1 C2 S2 117.8(2) . . ?
C4 C2 S2 117.2(2) . . ?
C1 C2 Fe1 70.31(15) . . ?
C4 C2 Fe1 130.3(2) . . ?
S2 C2 Fe1 71.98(9) . . ?
C9 C5 C6 108.0(2) . . ?
C9 C5 C10 125.8(3) . . ?
C6 C5 C10 126.1(3) . . ?
C9 C5 Fe1 70.37(15) . . ?
C6 C5 Fe1 69.49(15) . . ?
C10 C5 Fe1 127.90(19) . . ?
C5 C6 C7 107.7(2) . . ?
C5 C6 C11 126.2(3) . . ?
C7 C6 C11 126.0(3) . . ?
C5 C6 Fe1 70.10(15) . . ?
C7 C6 Fe1 69.26(15) . . ?
C11 C6 Fe1 129.5(2) . . ?
C8 C7 C6 108.1(2) . . ?
C8 C7 C12 125.9(3) . . ?
C6 C7 C12 126.0(3) . . ?
C8 C7 Fe1 70.67(15) . . ?
C6 C7 Fe1 69.97(15) . . ?
C12 C7 Fe1 125.5(2) . . ?
C7 C8 C9 107.8(2) . . ?
C7 C8 C13 126.4(3) . . ?
C9 C8 C13 125.7(3) . . ?
C7 C8 Fe1 69.13(15) . . ?
C9 C8 Fe1 70.10(15) . . ?
C13 C8 Fe1 128.7(2) . . ?
C5 C9 C8 108.4(2) . . ?
C5 C9 C14 125.7(3) . . ?
C8 C9 C14 125.9(3) . . ?
C5 C9 Fe1 69.71(15) . . ?
C8 C9 Fe1 69.66(15) . . ?
C14 C9 Fe1 128.7(2) . . ?
F3 B1 F4 110.1(4) . . ?
F3 B1 F2 109.6(4) . . ?
F4 B1 F2 110.3(4) . . ?
F3 B1 F1 109.2(4) . . ?
F4 B1 F1 108.8(4) . . ?
F2 B1 F1 108.9(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C7 2.061(3) . ?
Fe1 C6 2.071(3) . ?
Fe1 C2 2.075(3) . ?
Fe1 C1 2.076(2) . ?
Fe1 C5 2.079(3) . ?
Fe1 C8 2.081(3) . ?
Fe1 C9 2.087(3) . ?
Fe1 S1 2.2680(7) . ?
Fe1 S2 2.2699(8) . ?
Fe1 Ni1 2.6896(4) . ?
Ni1 S2 2.1609(7) 2_665 ?
Ni1 S2 2.1609(7) . ?
Ni1 S1 2.1655(7) . ?
Ni1 S1 2.1655(7) 2_665 ?
Ni1 Fe1 2.6896(4) 2_665 ?
S1 C1 1.761(3) . ?
S2 C2 1.764(3) . ?
C1 C2 1.401(4) . ?
C1 C3 1.503(4) . ?
C2 C4 1.501(4) . ?
C5 C9 1.422(4) . ?
C5 C6 1.433(4) . ?
C5 C10 1.497(4) . ?
C6 C7 1.439(4) . ?
C6 C11 1.488(4) . ?
C7 C8 1.424(4) . ?
C7 C12 1.496(4) . ?
C8 C9 1.434(4) . ?
C8 C13 1.491(4) . ?
C9 C14 1.502(4) . ?
F1 B1 1.379(9) . ?
F2 B1 1.358(5) . ?
F3 B1 1.356(5) . ?
F4 B1 1.356(5) . ?
