#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:21:41 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180431 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/00/7210096.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_7210096
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            'C24 H22 N4 Ni O2 S4'
_chemical_formula_weight         585.41
_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                78.834(11)
_cell_angle_beta                 76.312(12)
_cell_angle_gamma                83.671(13)
_cell_formula_units_Z            1
_cell_length_a                   6.1216(11)
_cell_length_b                   10.3788(16)
_cell_length_c                   10.7918(9)
_cell_measurement_reflns_used    4843
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.43
_cell_volume                     652.08(17)
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4830
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.43
_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    1.094
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.83180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details
w=1/[σ²(Fo²)+(0.0955P)²+0.0980P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                1887
_reflns_number_total             2842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce27096c.txt
_cod_data_source_block           5
_cod_original_cell_volume        652.08(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210096
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
Ni1 Ni 0.0000 0.0000 0.0000 0.0530(3) Uani 1 2 d S .
S11 S -0.21132(19) 0.04360(10) -0.14394(10) 0.0603(3) Uani 1 1 d . .
C12 C -0.2857(6) -0.1159(4) -0.0921(4) 0.0532(9) Uani 1 1 d . .
S13 S -0.14333(19) -0.19138(11) 0.02560(11) 0.0615(3) Uani 1 1 d . .
N14 N -0.4310(6) -0.1707(3) -0.1334(3) 0.0568(8) Uani 1 1 d . .
C21 C -0.5467(7) -0.0989(4) -0.2333(4) 0.0653(11) Uani 1 1 d . .
H21A H -0.5260 -0.0057 -0.2442 0.078 Uiso 1 1 calc R .
H21B H -0.7069 -0.1106 -0.2041 0.078 Uiso 1 1 calc R .
C22 C -0.4639(8) -0.1429(4) -0.3621(4) 0.0632(11) Uani 1 1 d . .
C23 C -0.2444(9) -0.1316(5) -0.4234(5) 0.0758(13) Uani 1 1 d . .
H23 H -0.1445 -0.0972 -0.3875 0.091 Uiso 1 1 calc R .
N24 N -0.1777(15) -0.1724(8) -0.5384(8) 0.153(3) Uani 1 1 d . .
C25 C -0.3416(19) -0.2123(8) -0.5807(8) 0.134(4) Uani 1 1 d . .
H25 H -0.2958 -0.2330 -0.6634 0.160 Uiso 1 1 calc R .
C26 C -0.553(2) -0.2279(8) -0.5287(9) 0.149(3) Uani 1 1 d . .
H26 H -0.6555 -0.2610 -0.5641 0.179 Uiso 1 1 calc R .
C27 C -0.5934(13) -0.1899(6) -0.4221(6) 0.109(2) Uani 1 1 d . .
H27 H -0.7423 -0.1959 -0.3765 0.131 Uiso 1 1 calc R .
C31 C -0.4893(8) -0.3063(5) -0.0782(5) 0.0695(12) Uani 1 1 d . A
H31A H -0.6514 -0.3100 -0.0625 0.083 Uiso 1 1 calc R .
H31B H -0.4464 -0.3312 0.0046 0.083 Uiso 1 1 calc R .
C32 C -0.3787(9) -0.4026(5) -0.1627(5) 0.0756(13) Uani 1 1 d . .
C33 C -0.1538(10) -0.4296(6) -0.1901(7) 0.140(3) Uani 1 1 d . .
H33 H -0.0481 -0.3962 -0.1576 0.168 Uiso 1 1 calc R .
C34 C -0.1108(17) -0.5189(8) -0.2781(9) 0.166(4) Uani 1 1 d . .
H34 H 0.0334 -0.5507 -0.3149 0.199 Uiso 1 1 calc R .
C35 C -0.305(3) -0.5544(7) -0.3042(9) 0.198(6) Uani 1 1 d . .
H35 H -0.3240 -0.6136 -0.3548 0.238 Uiso 1 1 calc R .
O36 O -0.4751(13) -0.4688(6) -0.2263(5) 0.137(3) 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'
N N 0.0061 0.0033 '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'
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
S11 Ni1 S11 180.0 . 2
S11 Ni1 S13 79.22(4) . .
S11 Ni1 S13 100.78(4) 2 .
S11 Ni1 S13 100.78(4) . 2
S11 Ni1 S13 79.22(4) 2 2
S13 Ni1 S13 180.00(2) . 2
C12 S11 Ni1 85.85(14) . .
N14 C12 S11 125.4(3) . .
N14 C12 S13 125.3(3) . .
S11 C12 S13 109.3(2) . .
C12 S13 Ni1 85.61(14) . .
C12 N14 C31 120.8(4) . .
C12 N14 C21 121.9(4) . .
C31 N14 C21 117.3(4) . .
N14 C21 C22 113.4(3) . .
N14 C21 H21A 108.9 . .
C22 C21 H21A 108.9 . .
N14 C21 H21B 108.9 . .
C22 C21 H21B 108.9 . .
H21A C21 H21B 107.7 . .
C27 C22 C23 117.0(5) . .
C27 C22 C21 123.9(5) . .
C23 C22 C21 119.1(4) . .
N24 C23 C22 117.0(6) . .
N24 C23 H23 121.5 . .
C22 C23 H23 121.5 . .
C25 N24 C23 114.7(8) . .
C26 C25 N24 132.4(9) . .
C26 C25 H25 113.8 . .
N24 C25 H25 113.8 . .
C27 C26 C25 106.7(9) . .
C27 C26 H26 126.6 . .
C25 C26 H26 126.6 . .
C26 C27 C22 132.0(9) . .
C26 C27 H27 114.0 . .
C22 C27 H27 114.0 . .
N14 C31 C32 113.3(4) . .
N14 C31 H31A 108.9 . .
C32 C31 H31A 108.9 . .
N14 C31 H31B 108.9 . .
C32 C31 H31B 108.9 . .
H31A C31 H31B 107.7 . .
O36 C32 C36 0.0(5) . .
O36 C32 C33 110.0(6) . .
C36 C32 C33 110.0(6) . .
O36 C32 O33 110.0(6) . .
C36 C32 O33 110.0(6) . .
C33 C32 O33 0.0 . .
O36 C32 C31 127.5(6) . .
C36 C32 C31 127.5(6) . .
C33 C32 C31 122.4(5) . .
O33 C32 C31 122.4(5) . .
C32 C33 C34 106.2(6) . .
C32 C33 H33 126.9 . .
C34 C33 H33 126.9 . .
C32 O33 C34 106.2(6) . .
C35 C34 C33 113.3(8) . .
C35 C34 O33 113.3(8) . .
C33 C34 O33 0.0(4) . .
C35 C34 H34 123.4 . .
C33 C34 H34 123.4 . .
O33 C34 H34 123.4 . .
C34 C35 O36 99.0(6) . .
C34 C35 C36 99.0(6) . .
O36 C35 C36 0.0(5) . .
C34 C35 H35 130.5 . .
O36 C35 H35 130.5 . .
C36 C35 H35 130.5 . .
C32 C36 C35 111.5(8) . .
C32 C36 H36 124.2 . .
C35 C36 H36 124.2 . .
C32 O36 C35 111.5(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S11 2.2002(11) .
Ni1 S11 2.2002(11) 2
Ni1 S13 2.2019(11) .
Ni1 S13 2.2020(11) 2
S11 C12 1.717(4) .
C12 N14 1.308(5) .
C12 S13 1.724(4) .
N14 C31 1.465(5) .
N14 C21 1.467(5) .
C21 C22 1.503(6) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C27 1.318(7) .
C22 C23 1.357(6) .
C23 N24 1.347(9) .
C23 H23 0.9300 .
N24 C25 1.329(11) .
C25 C26 1.300(11) .
C25 H25 0.9300 .
C26 C27 1.250(9) .
C26 H26 0.9300 .
C27 H27 0.9300 .
C31 C32 1.484(7) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 O36 1.325(7) .
C32 C36 1.325(7) .
C32 C33 1.347(7) .
C32 O33 1.347(7) .
C33 C34 1.414(9) .
C33 H33 0.9300 .
O33 C34 1.414(9) .
C34 C35 1.387(14) .
C34 H34 0.9300 .
C35 O36 1.501(13) .
C35 C36 1.501(13) .
C35 H35 0.9300 .
C36 H36 0.9300 .
