#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:19:13 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179104 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/66/4306664.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_4306664
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, F6 P'
_chemical_formula_sum            'C28 H42 F6 Fe2 Ni P S4'
_chemical_formula_weight         822.24
_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                105.575(5)
_cell_angle_beta                 101.908(4)
_cell_angle_gamma                103.120(4)
_cell_formula_units_Z            1
_cell_length_a                   8.3214(7)
_cell_length_b                   8.4045(6)
_cell_length_c                   13.0294(11)
_cell_measurement_reflns_used    7216
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.6
_cell_volume                     819.43(12)
_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, 2001)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ 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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0760
_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       -14
_diffrn_reflns_number            7216
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.717
_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    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             423
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0492
_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)+(0.0626P)²+0.0359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1308
_reflns_number_gt                2493
_reflns_number_total             3646
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic801487f_si_003.cif
_cod_data_source_block           k0828
_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_original_cell_volume        819.43(11)
_cod_database_code               4306664
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
Ni1 Ni 0.5000 1.0000 0.5000 0.0261(2) Uani 1 2 d S . .
Fe1 Fe 0.45773(7) 0.75289(6) 0.30867(4) 0.02296(18) Uani 1 1 d . . .
S1 S 0.31747(13) 0.95436(12) 0.34271(8) 0.0283(3) Uani 1 1 d . . .
S2 S 0.42858(13) 0.72472(12) 0.47264(8) 0.0290(3) Uani 1 1 d . . .
C1 C 0.2006(5) 0.7328(5) 0.2937(3) 0.0301(9) Uani 1 1 d . . .
C2 C 0.2517(5) 0.6283(5) 0.3527(3) 0.0301(9) Uani 1 1 d . . .
C3 C 0.0499(5) 0.6706(6) 0.1910(3) 0.0359(10) Uani 1 1 d . . .
H3A H -0.0531 0.6870 0.2122 0.054 Uiso 1 1 calc R . .
H3B H 0.0299 0.5475 0.1522 0.054 Uiso 1 1 calc R . .
H3C H 0.0748 0.7369 0.1417 0.054 Uiso 1 1 calc R . .
C4 C 0.1612(6) 0.4376(5) 0.3242(4) 0.0386(11) Uani 1 1 d . . .
H4A H 0.0659 0.4238 0.3577 0.058 Uiso 1 1 calc R . .
H4B H 0.2429 0.3816 0.3531 0.058 Uiso 1 1 calc R . .
H4C H 0.1161 0.3837 0.2433 0.058 Uiso 1 1 calc R . .
C5 C 0.6835(5) 0.8580(5) 0.2725(3) 0.0281(9) Uani 1 1 d . . .
C6 C 0.6954(5) 0.7162(5) 0.3123(3) 0.0298(9) Uani 1 1 d . . .
C7 C 0.5615(5) 0.5638(5) 0.2369(3) 0.0302(9) Uani 1 1 d . . .
C8 C 0.4657(5) 0.6143(5) 0.1532(3) 0.0282(9) Uani 1 1 d . . .
C9 C 0.5413(5) 0.7938(5) 0.1748(3) 0.0247(8) Uani 1 1 d . . .
C10 C 0.8045(6) 1.0370(5) 0.3222(4) 0.0482(13) Uani 1 1 d . . .
H10A H 0.9001 1.0455 0.2889 0.072 Uiso 1 1 calc R . .
H10B H 0.8494 1.0640 0.4026 0.072 Uiso 1 1 calc R . .
H10C H 0.7435 1.1193 0.3078 0.072 Uiso 1 1 calc R . .
C11 C 0.8269(6) 0.7253(7) 0.4137(4) 0.0518(13) Uani 1 1 d . . .
H11A H 0.9387 0.7356 0.3986 0.078 Uiso 1 1 calc R . .
H11B H 0.7912 0.6200 0.4325 0.078 Uiso 1 1 calc R . .
H11C H 0.8366 0.8264 0.4761 0.078 Uiso 1 1 calc R . .
C12 C 0.5355(7) 0.3852(5) 0.2422(4) 0.0512(14) Uani 1 1 d . . .
H12A H 0.6108 0.3314 0.2056 0.077 Uiso 1 1 calc R . .
H12B H 0.4152 0.3163 0.2045 0.077 Uiso 1 1 calc R . .
H12C H 0.5635 0.3903 0.3201 0.077 Uiso 1 1 calc R . .
C13 C 0.3173(6) 0.4972(6) 0.0562(3) 0.0428(11) Uani 1 1 d . . .
H13A H 0.3602 0.4333 -0.0014 0.064 Uiso 1 1 calc R . .
H13B H 0.2519 0.5661 0.0263 0.064 Uiso 1 1 calc R . .
H13C H 0.2424 0.4152 0.0801 0.064 Uiso 1 1 calc R . .
C14 C 0.4863(6) 0.8973(5) 0.1045(4) 0.0399(11) Uani 1 1 d . . .
H14A H 0.5599 0.9069 0.0553 0.060 Uiso 1 1 calc R . .
H14B H 0.4966 1.0133 0.1525 0.060 Uiso 1 1 calc R . .
H14C H 0.3663 0.8396 0.0597 0.060 Uiso 1 1 calc R . .
P1 P 0.0000 1.0000 0.0000 0.0323(4) Uani 1 2 d S . .
F1 F 0.1477(4) 1.0676(4) 0.1131(3) 0.0731(10) Uani 1 1 d . . .
F2 F -0.1318(4) 0.9199(4) 0.0574(3) 0.0704(10) Uani 1 1 d . . .
F3 F -0.0463(3) 1.1793(3) 0.0342(2) 0.0436(7) Uani 1 1 d . . .
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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
S2 Ni1 S2 180.00(6) . 2_676 ?
S2 Ni1 S1 89.98(4) . 2_676 ?
S2 Ni1 S1 90.02(4) 2_676 2_676 ?
S2 Ni1 S1 90.02(4) . . ?
S2 Ni1 S1 89.98(4) 2_676 . ?
S1 Ni1 S1 180.0 2_676 . ?
S2 Ni1 Fe1 54.57(3) . . ?
S2 Ni1 Fe1 125.43(3) 2_676 . ?
S1 Ni1 Fe1 125.46(3) 2_676 . ?
S1 Ni1 Fe1 54.54(3) . . ?
S2 Ni1 Fe1 125.43(3) . 2_676 ?
S2 Ni1 Fe1 54.57(3) 2_676 2_676 ?
S1 Ni1 Fe1 54.54(3) 2_676 2_676 ?
S1 Ni1 Fe1 125.46(3) . 2_676 ?
Fe1 Ni1 Fe1 180.0 . 2_676 ?
C6 Fe1 C2 131.86(16) . . ?
C6 Fe1 C8 68.08(16) . . ?
C2 Fe1 C8 112.05(16) . . ?
C6 Fe1 C1 167.81(16) . . ?
C2 Fe1 C1 39.33(16) . . ?
C8 Fe1 C1 105.65(15) . . ?
C6 Fe1 C7 40.72(16) . . ?
C2 Fe1 C7 106.48(15) . . ?
C8 Fe1 C7 40.39(15) . . ?
C1 Fe1 C7 127.89(16) . . ?
C6 Fe1 C9 67.65(15) . . ?
C2 Fe1 C9 144.07(15) . . ?
C8 Fe1 C9 39.96(14) . . ?
C1 Fe1 C9 114.82(15) . . ?
C7 Fe1 C9 67.51(14) . . ?
C6 Fe1 C5 40.45(15) . . ?
C2 Fe1 C5 172.28(16) . . ?
C8 Fe1 C5 67.47(15) . . ?
C1 Fe1 C5 148.32(16) . . ?
C7 Fe1 C5 67.89(15) . . ?
C9 Fe1 C5 39.91(15) . . ?
C6 Fe1 S1 144.52(12) . . ?
C2 Fe1 S1 77.40(12) . . ?
C8 Fe1 S1 125.37(11) . . ?
C1 Fe1 S1 47.67(11) . . ?
C7 Fe1 S1 165.76(12) . . ?
C9 Fe1 S1 101.10(10) . . ?
C5 Fe1 S1 109.38(11) . . ?
C6 Fe1 S2 101.18(11) . . ?
C2 Fe1 S2 47.60(11) . . ?
C8 Fe1 S2 142.42(11) . . ?
C1 Fe1 S2 77.25(12) . . ?
C7 Fe1 S2 107.94(11) . . ?
C9 Fe1 S2 167.61(11) . . ?
C5 Fe1 S2 127.90(11) . . ?
S1 Fe1 S2 84.93(4) . . ?
C6 Fe1 Ni1 106.56(11) . . ?
C2 Fe1 Ni1 82.06(11) . . ?
C8 Fe1 Ni1 165.12(11) . . ?
C1 Fe1 Ni1 82.03(11) . . ?
C7 Fe1 Ni1 142.33(12) . . ?
C9 Fe1 Ni1 125.32(10) . . ?
C5 Fe1 Ni1 99.21(11) . . ?
S1 Fe1 Ni1 51.07(3) . . ?
S2 Fe1 Ni1 51.04(3) . . ?
C1 S1 Ni1 106.33(14) . . ?
C1 S1 Fe1 60.38(13) . . ?
Ni1 S1 Fe1 74.39(3) . . ?
C2 S2 Ni1 106.44(14) . . ?
C2 S2 Fe1 60.30(13) . . ?
Ni1 S2 Fe1 74.39(3) . . ?
C2 C1 C3 124.7(4) . . ?
C2 C1 S1 118.2(3) . . ?
C3 C1 S1 117.1(3) . . ?
C2 C1 Fe1 70.2(2) . . ?
C3 C1 Fe1 129.9(3) . . ?
S1 C1 Fe1 71.94(14) . . ?
C1 C2 C4 124.7(4) . . ?
C1 C2 S2 118.3(3) . . ?
C4 C2 S2 116.9(3) . . ?
C1 C2 Fe1 70.4(2) . . ?
C4 C2 Fe1 131.0(3) . . ?
S2 C2 Fe1 72.10(14) . . ?
C9 C5 C6 107.7(3) . . ?
C9 C5 C10 126.7(4) . . ?
C6 C5 C10 125.5(4) . . ?
C9 C5 Fe1 70.0(2) . . ?
C6 C5 Fe1 68.8(2) . . ?
C10 C5 Fe1 128.9(3) . . ?
C5 C6 C7 107.9(3) . . ?
C5 C6 C11 125.8(4) . . ?
C7 C6 C11 126.2(4) . . ?
C5 C6 Fe1 70.8(2) . . ?
C7 C6 Fe1 70.1(2) . . ?
C11 C6 Fe1 125.6(3) . . ?
C8 C7 C6 107.4(3) . . ?
C8 C7 C12 126.7(4) . . ?
C6 C7 C12 125.7(4) . . ?
C8 C7 Fe1 69.7(2) . . ?
C6 C7 Fe1 69.2(2) . . ?
C12 C7 Fe1 129.1(3) . . ?
C9 C8 C7 108.4(3) . . ?
C9 C8 C13 125.6(4) . . ?
C7 C8 C13 126.0(4) . . ?
C9 C8 Fe1 70.6(2) . . ?
C7 C8 Fe1 69.9(2) . . ?
C13 C8 Fe1 127.6(3) . . ?
C8 C9 C5 108.6(3) . . ?
C8 C9 C14 126.0(4) . . ?
C5 C9 C14 125.4(3) . . ?
C8 C9 Fe1 69.4(2) . . ?
C5 C9 Fe1 70.1(2) . . ?
C14 C9 Fe1 128.3(3) . . ?
F1 P1 F1 180.0 . 2_575 ?
F1 P1 F2 90.06(18) . . ?
F1 P1 F2 89.94(18) 2_575 . ?
F1 P1 F2 89.94(18) . 2_575 ?
F1 P1 F2 90.06(18) 2_575 2_575 ?
F2 P1 F2 180.000(1) . 2_575 ?
F1 P1 F3 90.18(13) . 2_575 ?
F1 P1 F3 89.82(13) 2_575 2_575 ?
F2 P1 F3 89.90(13) . 2_575 ?
F2 P1 F3 90.10(13) 2_575 2_575 ?
F1 P1 F3 89.82(13) . . ?
F1 P1 F3 90.18(13) 2_575 . ?
F2 P1 F3 90.10(13) . . ?
F2 P1 F3 89.90(13) 2_575 . ?
F3 P1 F3 180.000(1) 2_575 . ?
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
Ni1 S2 2.1630(10) . ?
Ni1 S2 2.1630(10) 2_676 ?
Ni1 S1 2.1639(10) 2_676 ?
Ni1 S1 2.1639(10) . ?
Ni1 Fe1 2.6791(6) . ?
Ni1 Fe1 2.6791(6) 2_676 ?
Fe1 C6 2.063(4) . ?
Fe1 C2 2.069(4) . ?
Fe1 C8 2.071(4) . ?
Fe1 C1 2.072(4) . ?
Fe1 C7 2.074(4) . ?
Fe1 C9 2.087(4) . ?
Fe1 C5 2.090(4) . ?
Fe1 S1 2.2657(11) . ?
Fe1 S2 2.2668(11) . ?
S1 C1 1.762(4) . ?
S2 C2 1.759(4) . ?
C1 C2 1.394(6) . ?
C1 C3 1.507(5) . ?
C2 C4 1.513(5) . ?
C5 C9 1.425(5) . ?
C5 C6 1.436(5) . ?
C5 C10 1.489(5) . ?
C6 C7 1.439(6) . ?
C6 C11 1.503(6) . ?
C7 C8 1.431(5) . ?
C7 C12 1.490(5) . ?
C8 C9 1.421(5) . ?
C8 C13 1.492(5) . ?
C9 C14 1.497(5) . ?
P1 F1 1.578(3) . ?
P1 F1 1.578(3) 2_575 ?
P1 F2 1.578(3) . ?
P1 F2 1.578(3) 2_575 ?
P1 F3 1.610(2) 2_575 ?
P1 F3 1.610(2) . ?
