#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/28/7052847.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_7052847
loop_
_publ_author_name
'Famengo, Alessia'
'Pinero, Dalice'
'Jeannin, Olivier'
'Guizouarn, Thierry'
'Piekara-Sady, Lidia'
'Fourmigué, Marc'
_publ_section_title
;
 Dithiolene complexes as metallo-ligands: a crown-ether approach
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              638
_journal_paper_doi               10.1039/c1nj20870e
_journal_volume                  36
_journal_year                    2012
_chemical_formula_moiety         'C24 H40 Ni O8 S8'
_chemical_formula_sum            'C24 H40 Ni O8 S8'
_chemical_formula_weight         771.75
_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                67.4590(10)
_cell_angle_beta                 74.151(2)
_cell_angle_gamma                84.463(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1918(4)
_cell_length_b                   9.5486(4)
_cell_length_c                   10.6697(4)
_cell_measurement_reflns_used    6645
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.30
_cell_volume                     832.01(6)
_computing_cell_refinement       'Bruker SMART (Bruker, 2002)'
_computing_data_collection       'Bruker SAINT (Bruker, 2002)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2002)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10148
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0233
_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)+(0.0407P)²+0.1129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                3498
_reflns_number_total             3777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20870e.txt
_cod_data_source_block           import3
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052847
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
Ni Ni 1.0000 0.0000 1.0000 0.01349(9) Uani 1 2 d S
S1 S 1.17741(4) 0.03250(4) 1.08034(4) 0.01672(10) Uani 1 1 d .
S2 S 1.07717(4) -0.22157(4) 1.01078(4) 0.01644(10) Uani 1 1 d .
S3 S 1.43548(4) -0.16531(5) 1.17611(4) 0.01903(11) Uani 1 1 d .
S4 S 1.34466(4) -0.41019(4) 1.09677(4) 0.01868(11) Uani 1 1 d .
O1 O 1.39488(13) -0.13100(12) 1.46127(11) 0.0197(2) Uani 1 1 d .
O2 O 1.28106(13) -0.41272(13) 1.72339(12) 0.0234(3) Uani 1 1 d .
O3 O 1.18330(13) -0.60502(13) 1.58317(12) 0.0239(3) Uani 1 1 d .
O4 O 1.16122(13) -0.67208(13) 1.34473(11) 0.0235(3) Uani 1 1 d .
C1 C 1.27536(16) -0.13347(17) 1.11060(15) 0.0143(3) Uani 1 1 d .
C2 C 1.23180(16) -0.24856(17) 1.07729(15) 0.0141(3) Uani 1 1 d .
C3 C 1.44929(18) 0.00171(18) 1.21406(16) 0.0188(3) Uani 1 1 d .
H3A H 1.5535 0.0148 1.2117 0.023 Uiso 1 1 calc R
H3B H 1.4222 0.0899 1.1411 0.023 Uiso 1 1 calc R
C4 C 1.34893(18) -0.00575(18) 1.35519(16) 0.0192(3) Uani 1 1 d .
H4A H 1.3585 0.0874 1.3689 0.023 Uiso 1 1 calc R
H4B H 1.2440 -0.0183 1.3594 0.023 Uiso 1 1 calc R
C5 C 1.31667(18) -0.13759(18) 1.59869(16) 0.0205(3) Uani 1 1 d .
H5A H 1.2085 -0.1344 1.6082 0.025 Uiso 1 1 calc R
H5B H 1.3445 -0.0503 1.6128 0.025 Uiso 1 1 calc R
C6 C 1.35501(19) -0.28063(19) 1.70808(17) 0.0226(3) Uani 1 1 d .
H6A H 1.4635 -0.2954 1.6836 0.027 Uiso 1 1 calc R
H6B H 1.3279 -0.2683 1.7977 0.027 Uiso 1 1 calc R
C7 C 1.36729(18) -0.48493(18) 1.63191(17) 0.0208(3) Uani 1 1 d .
H7A H 1.4686 -0.5043 1.6454 0.025 Uiso 1 1 calc R
H7B H 1.3755 -0.4182 1.5351 0.025 Uiso 1 1 calc R
C8 C 1.29383(18) -0.63188(18) 1.66070(17) 0.0210(3) Uani 1 1 d .
H8A H 1.3700 -0.7002 1.6342 0.025 Uiso 1 1 calc R
H8B H 1.2462 -0.6794 1.7603 0.025 Uiso 1 1 calc R
C9 C 1.1276(2) -0.74215(19) 1.59023(18) 0.0251(4) Uani 1 1 d .
H9A H 1.0573 -0.7904 1.6809 0.030 Uiso 1 1 calc R
H9B H 1.2108 -0.8110 1.5801 0.030 Uiso 1 1 calc R
C10 C 1.04918(19) -0.7099(2) 1.47548(17) 0.0246(4) Uani 1 1 d .
H10A H 0.9919 -0.7985 1.4924 0.030 Uiso 1 1 calc R
H10B H 0.9797 -0.6264 1.4734 0.030 Uiso 1 1 calc R
C11 C 1.09802(18) -0.60895(19) 1.22777(16) 0.0214(3) Uani 1 1 d .
H11A H 1.0312 -0.5264 1.2368 0.026 Uiso 1 1 calc R
H11B H 1.0397 -0.6854 1.2231 0.026 Uiso 1 1 calc R
C12 C 1.22579(18) -0.55105(18) 1.09607(16) 0.0198(3) Uani 1 1 d .
H12A H 1.1835 -0.5070 1.0155 0.024 Uiso 1 1 calc R
H12B H 1.2879 -0.6360 1.0856 0.024 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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
S1 Ni S1 180.0 2_757 .
S1 Ni S2 92.227(13) 2_757 2_757
S1 Ni S2 87.773(13) . 2_757
S1 Ni S2 87.773(14) 2_757 .
S1 Ni S2 92.227(13) . .
S2 Ni S2 180.0 2_757 .
C1 S1 Ni 104.34(5) . .
C2 S2 Ni 104.61(5) . .
C1 S3 C3 104.14(7) . .
C2 S4 C12 104.61(7) . .
C4 O1 C5 112.02(12) . .
C6 O2 C7 112.10(12) . .
C9 O3 C8 111.92(12) . .
C11 O4 C10 112.53(12) . .
C2 C1 S1 119.85(11) . .
C2 C1 S3 117.25(11) . .
S1 C1 S3 122.85(9) . .
C1 C2 S2 118.94(11) . .
C1 C2 S4 118.16(11) . .
S2 C2 S4 122.81(9) . .
C4 C3 S3 113.52(11) . .
C4 C3 H3A 108.9 . .
S3 C3 H3A 108.9 . .
C4 C3 H3B 108.9 . .
S3 C3 H3B 108.9 . .
H3A C3 H3B 107.7 . .
O1 C4 C3 108.17(12) . .
O1 C4 H4A 110.1 . .
C3 C4 H4A 110.1 . .
O1 C4 H4B 110.1 . .
C3 C4 H4B 110.1 . .
H4A C4 H4B 108.4 . .
O1 C5 C6 110.55(13) . .
O1 C5 H5A 109.5 . .
C6 C5 H5A 109.5 . .
O1 C5 H5B 109.5 . .
C6 C5 H5B 109.5 . .
H5A C5 H5B 108.1 . .
O2 C6 C5 113.97(13) . .
O2 C6 H6A 108.8 . .
C5 C6 H6A 108.8 . .
O2 C6 H6B 108.8 . .
C5 C6 H6B 108.8 . .
H6A C6 H6B 107.7 . .
O2 C7 C8 110.73(13) . .
O2 C7 H7A 109.5 . .
C8 C7 H7A 109.5 . .
O2 C7 H7B 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 108.1 . .
O3 C8 C7 110.10(13) . .
O3 C8 H8A 109.6 . .
C7 C8 H8A 109.6 . .
O3 C8 H8B 109.6 . .
C7 C8 H8B 109.6 . .
H8A C8 H8B 108.2 . .
O3 C9 C10 109.97(14) . .
O3 C9 H9A 109.7 . .
C10 C9 H9A 109.7 . .
O3 C9 H9B 109.7 . .
C10 C9 H9B 109.7 . .
H9A C9 H9B 108.2 . .
O4 C10 C9 108.40(14) . .
O4 C10 H10A 110.0 . .
C9 C10 H10A 110.0 . .
O4 C10 H10B 110.0 . .
C9 C10 H10B 110.0 . .
H10A C10 H10B 108.4 . .
O4 C11 C12 108.36(13) . .
O4 C11 H11A 110.0 . .
C12 C11 H11A 110.0 . .
O4 C11 H11B 110.0 . .
C12 C11 H11B 110.0 . .
H11A C11 H11B 108.4 . .
C11 C12 S4 113.31(11) . .
C11 C12 H12A 108.9 . .
S4 C12 H12A 108.9 . .
C11 C12 H12B 108.9 . .
S4 C12 H12B 108.9 . .
H12A C12 H12B 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni S1 2.1344(4) 2_757
Ni S1 2.1344(4) .
Ni S2 2.1356(4) 2_757
Ni S2 2.1356(4) .
S1 C1 1.7081(15) .
S2 C2 1.7117(15) .
S3 C1 1.7492(14) .
S3 C3 1.8127(16) .
S4 C2 1.7505(15) .
S4 C12 1.8163(16) .
O1 C4 1.4197(18) .
O1 C5 1.4258(18) .
O2 C6 1.4236(19) .
O2 C7 1.4297(19) .
O3 C9 1.419(2) .
O3 C8 1.4242(19) .
O4 C11 1.4177(18) .
O4 C10 1.4276(19) .
C1 C2 1.399(2) .
C3 C4 1.515(2) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.504(2) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.503(2) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.505(2) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.512(2) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
S2 Ni S1 C1 178.74(5) 2_757
S2 Ni S1 C1 -1.26(5) .
S1 Ni S2 C2 -179.43(5) 2_757
S1 Ni S2 C2 0.57(5) .
Ni S1 C1 C2 1.95(13) .
Ni S1 C1 S3 179.31(8) .
C3 S3 C1 C2 -177.27(12) .
C3 S3 C1 S1 5.31(11) .
S1 C1 C2 S2 -1.69(18) .
S3 C1 C2 S2 -179.19(7) .
S1 C1 C2 S4 174.89(8) .
S3 C1 C2 S4 -2.61(17) .
Ni S2 C2 C1 0.48(13) .
Ni S2 C2 S4 -175.94(8) .
C12 S4 C2 C1 163.40(12) .
C12 S4 C2 S2 -20.16(11) .
C1 S3 C3 C4 82.92(12) .
C5 O1 C4 C3 173.97(12) .
S3 C3 C4 O1 61.40(15) .
C4 O1 C5 C6 173.64(12) .
C7 O2 C6 C5 89.58(17) .
O1 C5 C6 O2 -76.43(17) .
C6 O2 C7 C8 174.36(13) .
C9 O3 C8 C7 171.00(13) .
O2 C7 C8 O3 86.13(16) .
C8 O3 C9 C10 -163.09(14) .
C11 O4 C10 C9 -167.43(14) .
O3 C9 C10 O4 72.45(18) .
C10 O4 C11 C12 171.45(13) .
O4 C11 C12 S4 -58.25(15) .
C2 S4 C12 C11 -71.11(12) .
