#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:40:27 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234898 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/95/4349587.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_4349587
loop_
_publ_author_name
'Andrade, Marta M.'
'Silva, Rafaela A. L.'
'Santos, Isabel C.'
'Lopes, Elsa B.'
'Rabaça, Sandra'
'Pereira, Laura C. J.'
'Coutinho, Joana T.'
'Telo, João P.'
'Rovira, Concepció'
'Almeida, Manuel'
'Belo, Dulce'
_publ_section_title
;
 Gold and nickel alkyl substituted bis-thiophenedithiolene complexes:
 anionic and neutral forms
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              270
_journal_paper_doi               10.1039/C6QI00447D
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C20 H28 Ni S6'
_chemical_formula_sum            'C20 H28 Ni S6'
_chemical_formula_weight         519.49
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_audit_update_record
;
2016-09-21 deposited with the CCDC.
2016-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                97.787(2)
_cell_angle_beta                 97.987(2)
_cell_angle_gamma                100.485(2)
_cell_formula_units_Z            1
_cell_length_a                   5.6359(2)
_cell_length_b                   8.3540(4)
_cell_length_c                   12.3983(5)
_cell_measurement_reflns_used    2937
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.51
_cell_volume                     560.62(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5873
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  0.9720
_exptl_absorpt_correction_T_min  0.5988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0279
_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)+(0.0302P)²+0.2631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                1830
_reflns_number_total             2107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00447d2.cif
_cod_data_source_block           compound_8
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4349587
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
Ni1 Ni 0.0000 0.0000 0.0000 0.01687(12) Uani 1 2 d S
S1 S 0.20258(10) 0.03883(7) 0.16453(4) 0.01903(14) Uani 1 1 d .
S2 S 0.27367(10) 0.16691(7) -0.05561(4) 0.01941(14) Uani 1 1 d .
S3 S 0.73902(10) 0.39327(7) 0.07415(4) 0.01976(15) Uani 1 1 d .
C1 C 0.4824(4) 0.2396(3) 0.06104(18) 0.0169(5) Uani 1 1 d .
C2 C 0.4579(4) 0.1833(3) 0.16070(17) 0.0159(4) Uani 1 1 d .
C3 C 0.6562(4) 0.2646(3) 0.24914(17) 0.0164(5) Uani 1 1 d .
C4 C 0.8151(4) 0.3822(3) 0.21398(17) 0.0169(5) Uani 1 1 d .
C5 C 0.6833(4) 0.2265(3) 0.36525(17) 0.0186(5) Uani 1 1 d .
H5 H 0.8385 0.2994 0.4071 0.022 Uiso 1 1 calc R
C6 C 1.0284(4) 0.5091(3) 0.28247(18) 0.0197(5) Uani 1 1 d .
H6 H 1.1072 0.4554 0.3412 0.024 Uiso 1 1 calc R
C7 C 0.4754(4) 0.2678(3) 0.42493(19) 0.0251(5) Uani 1 1 d .
H7A H 0.4668 0.3838 0.4243 0.038 Uiso 1 1 calc R
H7C H 0.5070 0.2489 0.5014 0.038 Uiso 1 1 calc R
H7B H 0.3197 0.1971 0.3872 0.038 Uiso 1 1 calc R
C10 C 1.2227(4) 0.5709(3) 0.2152(2) 0.0250(5) Uani 1 1 d .
H10B H 1.3628 0.6440 0.2646 0.037 Uiso 1 1 calc R
H10A H 1.1535 0.6317 0.1606 0.037 Uiso 1 1 calc R
H10C H 1.2766 0.4766 0.1772 0.037 Uiso 1 1 calc R
C8 C 0.7100(4) 0.0479(3) 0.36906(19) 0.0239(5) Uani 1 1 d .
H8B H 0.7407 0.0314 0.4461 0.036 Uiso 1 1 calc R
H8A H 0.8474 0.0259 0.3329 0.036 Uiso 1 1 calc R
H8C H 0.5591 -0.0277 0.3306 0.036 Uiso 1 1 calc R
C9 C 0.9363(4) 0.6528(3) 0.33924(19) 0.0259(5) Uani 1 1 d .
H9B H 0.8248 0.6128 0.3883 0.039 Uiso 1 1 calc R
H9C H 0.8491 0.7037 0.2835 0.039 Uiso 1 1 calc R
H9A H 1.0754 0.7348 0.3826 0.039 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'
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
S2 Ni1 S2 180.00(3) . 2
S2 Ni1 S1 86.79(2) . 2
S2 Ni1 S1 93.21(2) 2 2
S2 Ni1 S1 93.21(2) . .
S2 Ni1 S1 86.79(2) 2 .
S1 Ni1 S1 180.000(15) 2 .
C2 S1 Ni1 103.69(7) . .
C1 S2 Ni1 102.45(8) . .
C1 S3 C4 90.95(10) . .
C2 C1 S2 122.49(17) . .
C2 C1 S3 111.88(16) . .
S2 C1 S3 125.59(13) . .
C1 C2 C3 112.68(19) . .
C1 C2 S1 118.07(17) . .
C3 C2 S1 129.20(17) . .
C4 C3 C2 110.92(19) . .
C4 C3 C5 124.27(19) . .
C2 C3 C5 124.80(19) . .
C3 C4 C6 128.11(19) . .
C3 C4 S3 113.51(16) . .
C6 C4 S3 118.15(16) . .
C3 C5 C8 112.29(18) . .
C3 C5 C7 112.40(18) . .
C8 C5 C7 111.02(19) . .
C3 C5 H5 106.9 . .
C8 C5 H5 106.9 . .
C7 C5 H5 106.9 . .
C4 C6 C9 110.01(18) . .
C4 C6 C10 112.95(19) . .
C9 C6 C10 110.40(19) . .
C4 C6 H6 107.8 . .
C9 C6 H6 107.8 . .
C10 C6 H6 107.8 . .
C5 C7 H7A 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
H7C C7 H7B 109.5 . .
C6 C10 H10B 109.5 . .
C6 C10 H10A 109.5 . .
H10B C10 H10A 109.5 . .
C6 C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
C5 C8 H8B 109.5 . .
C5 C8 H8A 109.5 . .
H8B C8 H8A 109.5 . .
C5 C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
C6 C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C6 C9 H9A 109.5 . .
H9B C9 H9A 109.5 . .
H9C C9 H9A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S2 2.1382(5) .
Ni1 S2 2.1382(5) 2
Ni1 S1 2.1468(5) 2
Ni1 S1 2.1468(5) .
S1 C2 1.712(2) .
S2 C1 1.695(2) .
S3 C1 1.723(2) .
S3 C4 1.746(2) .
C1 C2 1.396(3) .
C2 C3 1.447(3) .
C3 C4 1.364(3) .
C3 C5 1.509(3) .
C4 C6 1.516(3) .
C5 C8 1.533(3) .
C5 C7 1.535(3) .
C5 H5 1.0000 .
C6 C9 1.519(3) .
C6 C10 1.525(3) .
C6 H6 1.0000 .
C7 H7A 0.9800 .
C7 H7C 0.9800 .
C7 H7B 0.9800 .
C10 H10B 0.9800 .
C10 H10A 0.9800 .
C10 H10C 0.9800 .
C8 H8B 0.9800 .
C8 H8A 0.9800 .
C8 H8C 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C9 H9A 0.9800 .
