#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:23:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/01/7210100.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_7210100
loop_
_publ_author_name
'Rajput, Gunjan'
'Singh, Vikram'
'Gupta, Ajit N.'
'Yadav, Manoj Kumar'
'Kumar, Vinod'
'Singh, Santosh Kumar'
'Prasad, Akhilesh'
'Drew, Michael G. B.'
'Singh, Nanhai'
_publ_section_title
;
 Unusual C--H⋯Ni anagostic interactions in new homoleptic Ni(ii)
 dithio complexes
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4676
_journal_paper_doi               10.1039/c3ce27096c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C28 H26 N4 Ni S4'
_chemical_formula_weight         605.48
_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                76.000(19)
_cell_angle_beta                 80.634(19)
_cell_angle_gamma                73.41(2)
_cell_formula_units_Z            1
_cell_length_a                   6.4456(14)
_cell_length_b                   10.110(2)
_cell_length_c                   11.407(3)
_cell_measurement_reflns_used    5137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.11
_cell_volume                     687.7(3)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5137
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.59515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1171P)²+0.6119P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2541
_refine_ls_wR_factor_ref         0.2835
_reflns_number_gt                1792
_reflns_number_total             3018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce27096c.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210100
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
N14 N 0.3980(9) 0.1405(6) 0.1449(5) 0.0472(14) Uani 1 1 d . . .
S11 S 0.1845(3) 0.1613(2) -0.04560(18) 0.0550(5) Uani 1 1 d . . .
S13 S 0.1328(3) -0.0313(2) 0.17324(19) 0.0550(6) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.0000 0.0000 0.0486(5) Uani 1 2 d S . .
C12 C 0.2632(11) 0.0983(7) 0.0983(7) 0.0459(16) Uani 1 1 d . . .
C21 C 0.4702(12) 0.0698(8) 0.2655(8) 0.0574(19) Uani 1 1 d . . .
H21A H 0.6262 0.0567 0.2607 0.069 Uiso 1 1 calc R . .
H21B H 0.4430 -0.0230 0.2862 0.069 Uiso 1 1 calc R . .
C22 C 0.3633(12) 0.1463(8) 0.3667(7) 0.0555(19) Uani 1 1 d . B .
C23 C 0.4864(16) 0.1840(10) 0.4325(8) 0.072(2) Uani 1 1 d . . .
H23 H 0.6362 0.1630 0.4122 0.086 Uiso 1 1 calc R A 1
N24 N 0.4039(19) 0.2498(12) 0.5251(8) 0.100(3) Uani 1 1 d . . .
C25 C 0.189(2) 0.2796(13) 0.5513(10) 0.107(4) Uani 1 1 d . . .
H25 H 0.1289 0.3237 0.6162 0.129 Uiso 1 1 calc R B 1
C26 C 0.0509(19) 0.2493(14) 0.4886(11) 0.112(4) Uani 1 1 d . B .
H26 H -0.0990 0.2759 0.5075 0.135 Uiso 1 1 calc R . .
C27 C 0.1413(14) 0.1786(11) 0.3973(9) 0.085(3) Uani 1 1 d . . .
H27 H 0.0526 0.1521 0.3554 0.101 Uiso 1 1 calc R B .
C31 C 0.5059(13) 0.2495(9) 0.0719(7) 0.060(2) Uani 1 1 d . . .
H31A H 0.4374 0.2910 -0.0028 0.072 Uiso 1 1 calc R . .
H31B H 0.6570 0.2042 0.0502 0.072 Uiso 1 1 calc R . .
C32 C 0.4976(11) 0.3648(7) 0.1352(6) 0.0462(16) Uani 1 1 d . D .
C33 C 0.2976(13) 0.4612(9) 0.1573(8) 0.068(2) Uani 1 1 d . . .
H33 H 0.1718 0.4543 0.1319 0.081 Uiso 1 1 calc R C 1
C34 C 0.2894(17) 0.5651(9) 0.2161(10) 0.090(3) Uani 1 1 d . . .
H34 H 0.1574 0.6292 0.2311 0.108 Uiso 1 1 calc R B 1
C35 C 0.472(2) 0.5754(10) 0.2529(10) 0.088(3) Uani 1 1 d . . .
H35 H 0.4636 0.6462 0.2940 0.106 Uiso 1 1 calc R D 1
C36 C 0.6707(16) 0.4835(10) 0.2309(10) 0.084(3) Uani 1 1 d . . .
H36 H 0.7963 0.4914 0.2557 0.101 Uiso 1 1 calc R B 1
C37 C 0.6768(12) 0.3810(9) 0.1719(8) 0.061(2) Uani 1 1 d . . .
H37 H 0.8103 0.3188 0.1558 0.073 Uiso 1 1 calc R D 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'
N N 0.0061 0.0033 '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
C12 N14 C21 121.3(6) . .
C12 N14 C31 120.9(6) . .
C21 N14 C31 117.4(6) . .
C12 S11 Ni1 85.9(3) . .
C12 S13 Ni1 85.5(2) . .
S13 Ni1 S13 180.00(4) . 2
S13 Ni1 S11 79.35(7) . .
S13 Ni1 S11 100.65(7) 2 .
S13 Ni1 S11 100.65(7) . 2
S13 Ni1 S11 79.35(7) 2 2
S11 Ni1 S11 180.00(6) . 2
N14 C12 S11 125.9(6) . .
N14 C12 S13 125.0(6) . .
S11 C12 S13 109.0(4) . .
N14 C21 C22 115.3(6) . .
C23 C22 C27 117.6(8) . .
C23 C22 C21 120.1(7) . .
C27 C22 C21 122.3(7) . .
N24 C23 C24 0.0(12) . .
N24 C23 C22 123.6(9) . .
C24 C23 C22 123.6(9) . .
C25 C24 C23 116.8(9) . .
C25 N24 C23 116.8(9) . .
N24 C25 C24 0.0(11) . .
N24 C25 C26 124.0(10) . .
C24 C25 C26 124.0(10) . .
C27 C26 C25 117.5(11) . .
C26 C27 C22 120.4(9) . .
N14 C31 C32 114.1(6) . .
C37 C32 C33 118.1(8) . .
C37 C32 C31 122.5(7) . .
C33 C32 C31 119.4(7) . .
N34 C33 C34 0.0(8) . .
N34 C33 C32 119.4(8) . .
C34 C33 C32 119.4(8) . .
C35 C34 C33 120.3(9) . .
C35 N34 C33 120.3(9) . .
N34 C35 C34 0.0(11) . .
N34 C35 N36 121.4(9) . .
C34 C35 N36 121.4(9) . .
N34 C35 C36 121.4(9) . .
C34 C35 C36 121.4(9) . .
N36 C35 C36 0.0(10) . .
C37 C36 C35 117.7(9) . .
C37 N36 C35 117.7(9) . .
N36 C37 C36 0.0(7) . .
N36 C37 C32 123.1(8) . .
C36 C37 C32 123.1(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N14 C12 1.300(9) .
N14 C21 1.471(9) .
N14 C31 1.481(9) .
S11 C12 1.714(7) .
S11 Ni1 2.2004(19) .
S13 C12 1.735(7) .
S13 Ni1 2.198(2) .
Ni1 S13 2.198(2) 2
Ni1 S11 2.2004(19) 2
C21 C22 1.508(11) .
C22 C23 1.358(11) .
C22 C27 1.379(11) .
C23 N24 1.341(13) .
C23 C24 1.341(13) .
C24 C25 1.331(15) .
N24 C25 1.331(15) .
C25 C26 1.365(16) .
C26 C27 1.364(14) .
C31 C32 1.498(10) .
C32 C37 1.355(9) .
C32 C33 1.404(11) .
C33 N34 1.361(13) .
C33 C34 1.361(13) .
C34 C35 1.352(14) .
N34 C35 1.352(14) .
C35 N36 1.376(14) .
C35 C36 1.376(14) .
C36 C37 1.354(12) .
N36 C37 1.354(12) .
