#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:21:41 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180431 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/00/7210097.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_7210097
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            'C26 H24 N2 Ni O2 S4'
_chemical_formula_weight         583.42
_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                80.996(6)
_cell_angle_beta                 82.990(6)
_cell_angle_gamma                89.460(5)
_cell_formula_units_Z            1
_cell_length_a                   6.2494(4)
_cell_length_b                   6.9702(5)
_cell_length_c                   15.3641(13)
_cell_measurement_reflns_used    4914
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.96
_cell_volume                     656.03(9)
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4914
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.96
_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    1.085
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.96102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.477
_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         0.815
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0569
_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)+(0.0733P)²+0.3197P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                1993
_reflns_number_total             2857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce27096c.txt
_cod_data_source_block           6
_cod_original_cell_volume        656.03(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210097
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 -0.0521(5) -0.2178(5) 0.1365(2) 0.0502(8) Uani 1 1 d . . .
S11 S 0.28433(16) -0.25201(17) 0.01205(7) 0.0579(3) Uani 1 1 d . . .
S13 S 0.25081(16) 0.06654(16) 0.10459(7) 0.0579(3) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.0000 0.0000 0.0489(3) Uani 1 2 d S . .
C12 C 0.1289(6) -0.1463(6) 0.0923(2) 0.0489(9) Uani 1 1 d . . .
C21 C -0.1849(6) -0.1087(6) 0.1973(3) 0.0534(10) Uani 1 1 d . . .
H21A H -0.3352 -0.1233 0.1894 0.064 Uiso 1 1 calc R . .
H21B H -0.1474 0.0281 0.1814 0.064 Uiso 1 1 calc R . .
C22 C -0.1590(7) -0.1724(6) 0.2937(3) 0.0579(11) Uani 1 1 d . . .
C23 C 0.0320(8) -0.1691(10) 0.3262(3) 0.0912(18) Uani 1 1 d . . .
H23 H 0.1568 -0.1304 0.2882 0.109 Uiso 1 1 calc R . .
C24 C 0.0410(13) -0.2223(15) 0.4140(5) 0.148(4) Uani 1 1 d . . .
H24 H 0.1726 -0.2240 0.4366 0.178 Uiso 1 1 calc R . .
C25 C -0.1291(16) -0.2695(15) 0.4650(6) 0.153(3) Uani 1 1 d . . .
H25 H -0.1180 -0.3026 0.5253 0.184 Uiso 1 1 calc R . .
C26 C -0.3142(13) -0.2755(11) 0.4404(5) 0.111(2) Uani 1 1 d . . .
H26 H -0.4347 -0.3115 0.4814 0.133 Uiso 1 1 calc R . .
C27 C -0.3320(7) -0.2284(6) 0.3536(3) 0.0629(12) Uani 1 1 d . . .
H27 H -0.4667 -0.2344 0.3342 0.076 Uiso 1 1 calc R . .
C31 C -0.1447(7) -0.3985(7) 0.1166(3) 0.0636(12) Uani 1 1 d . A .
H31A H -0.0292 -0.4740 0.0911 0.076 Uiso 1 1 calc R . .
H31B H -0.2429 -0.3645 0.0725 0.076 Uiso 1 1 calc R . .
C32 C -0.2621(7) -0.5208(6) 0.1955(3) 0.0519(10) Uani 1 1 d . . .
O33 O -0.1488(6) -0.6118(5) 0.2594(3) 0.0786(14) Uani 1 1 d . . .
C34 C -0.2996(15) -0.7229(8) 0.3259(4) 0.120(3) Uani 1 1 d . . .
H34 H -0.2670 -0.7976 0.3781 0.144 Uiso 1 1 calc R A 1
C35 C -0.5115(12) -0.6979(10) 0.2971(5) 0.119(3) Uani 1 1 d . A .
H35 H -0.6415 -0.7529 0.3255 0.143 Uiso 1 1 calc R B 1
C36 C -0.4734(7) -0.5658(8) 0.2127(3) 0.086(2) Uani 1 1 d . . .
H36 H -0.5784 -0.5203 0.1768 0.103 Uiso 1 1 calc PR A 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'
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
C12 N14 C21 121.4(3) . .
C12 N14 C31 120.3(3) . .
C21 N14 C31 117.7(3) . .
C12 S11 Ni1 85.59(13) . .
C12 S13 Ni1 85.65(13) . .
S11 Ni1 S11 180.0 . 2_655
S11 Ni1 S13 79.57(4) . .
S11 Ni1 S13 100.43(4) 2_655 .
S11 Ni1 S13 100.43(4) . 2_655
S11 Ni1 S13 79.57(4) 2_655 2_655
S13 Ni1 S13 180.0 . 2_655
N14 C12 S13 125.7(3) . .
N14 C12 S11 125.1(3) . .
S13 C12 S11 109.2(2) . .
N14 C21 C22 113.9(3) . .
N14 C21 H21A 108.8 . .
C22 C21 H21A 108.8 . .
N14 C21 H21B 108.8 . .
C22 C21 H21B 108.8 . .
H21A C21 H21B 107.7 . .
C27 C22 C23 116.2(4) . .
C27 C22 C21 120.6(4) . .
C23 C22 C21 123.2(4) . .
C24 C23 C22 119.7(5) . .
C24 C23 H23 120.1 . .
C22 C23 H23 120.1 . .
C25 C24 C23 119.7(8) . .
C25 C24 H24 120.2 . .
C23 C24 H24 120.2 . .
C24 C25 C26 124.7(10) . .
C24 C25 H25 117.6 . .
C26 C25 H25 117.6 . .
C25 C26 C27 118.1(8) . .
C25 C26 H26 120.9 . .
C27 C26 H26 120.9 . .
C26 C27 C22 121.5(5) . .
C26 C27 H27 119.2 . .
C22 C27 H27 119.2 . .
N14 C31 C32 113.8(3) . .
N14 C31 H31A 108.8 . .
C32 C31 H31A 108.8 . .
N14 C31 H31B 108.8 . .
C32 C31 H31B 108.8 . .
H31A C31 H31B 107.7 . .
O36 C32 C36 0.0(7) . .
O36 C32 C33 111.9(4) . .
C36 C32 C33 111.9(4) . .
O36 C32 O33 111.9(4) . .
C36 C32 O33 111.9(4) . .
C33 C32 O33 0.0(4) . .
O36 C32 C31 129.0(5) . .
C36 C32 C31 129.0(5) . .
C33 C32 C31 119.0(4) . .
O33 C32 C31 119.0(4) . .
C32 C33 C34 107.4(5) . .
C32 C33 H33 126.3 . .
C34 C33 H33 126.3 . .
C32 O33 C34 107.4(5) . .
O33 C34 C33 0.0(4) . .
O33 C34 C35 107.8(6) . .
C33 C34 C35 107.8(6) . .
O33 C34 H34 126.1 . .
C33 C34 H34 126.1 . .
C35 C34 H34 126.1 . .
C34 C35 O36 103.8(5) . .
C34 C35 C36 103.8(5) . .
O36 C35 C36 0.0(3) . .
C34 C35 H35 128.1 . .
O36 C35 H35 128.1 . .
C36 C35 H35 128.1 . .
C32 C36 C35 109.0(5) . .
C32 C36 H36 125.5 . .
C35 C36 H36 125.5 . .
C32 O36 C35 109.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N14 C12 1.306(4) .
N14 C21 1.469(5) .
N14 C31 1.480(5) .
S11 C12 1.728(4) .
S11 Ni1 2.1951(10) .
S13 C12 1.721(4) .
S13 Ni1 2.1980(10) .
Ni1 S11 2.1951(10) 2_655
Ni1 S13 2.1980(10) 2_655
C21 C22 1.506(6) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C27 1.349(5) .
C22 C23 1.351(6) .
C23 C24 1.350(8) .
C23 H23 0.9300 .
C24 C25 1.255(10) .
C24 H24 0.9300 .
C25 C26 1.263(10) .
C25 H25 0.9300 .
C26 C27 1.341(8) .
C26 H26 0.9300 .
C27 H27 0.9300 .
C31 C32 1.484(5) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 O36 1.345(6) .
C32 C36 1.345(6) .
C32 C33 1.355(6) .
C32 O33 1.355(6) .
C33 C34 1.436(7) .
C33 H33 0.9300 .
O33 C34 1.436(7) .
C34 C35 1.447(10) .
C34 H34 0.9300 .
C35 O36 1.462(9) .
C35 C36 1.462(9) .
C35 H35 0.9300 .
C36 H36 0.9300 .
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_4
C12 S11 Ni1 S11 -122(6) 2_655
C12 S11 Ni1 S13 0.45(14) .
C12 S11 Ni1 S13 -179.55(14) 2_655
C12 S13 Ni1 S11 -0.45(14) .
C12 S13 Ni1 S11 179.55(14) 2_655
C12 S13 Ni1 S13 38(2) 2_655
C21 N14 C12 S13 6.3(6) .
C31 N14 C12 S13 177.3(3) .
C21 N14 C12 S11 -173.8(3) .
C31 N14 C12 S11 -2.9(6) .
Ni1 S13 C12 N14 -179.6(4) .
Ni1 S13 C12 S11 0.60(19) .
Ni1 S11 C12 N14 179.6(4) .
Ni1 S11 C12 S13 -0.60(19) .
C12 N14 C21 C22 -100.5(4) .
C31 N14 C21 C22 88.3(4) .
N14 C21 C22 C27 -124.4(4) .
N14 C21 C22 C23 58.6(6) .
C27 C22 C23 C24 0.7(10) .
C21 C22 C23 C24 177.8(6) .
C22 C23 C24 C25 -1.8(14) .
C23 C24 C25 C26 1.5(18) .
C24 C25 C26 C27 0.1(17) .
C25 C26 C27 C22 -1.3(11) .
C23 C22 C27 C26 0.8(8) .
C21 C22 C27 C26 -176.3(5) .
C12 N14 C31 C32 146.8(4) .
C21 N14 C31 C32 -41.9(6) .
N14 C31 C32 O36 114.3(5) .
N14 C31 C32 C36 114.3(5) .
N14 C31 C32 C33 -69.3(5) .
N14 C31 C32 O33 -69.3(5) .
O36 C32 C33 C34 -1.6(5) .
C36 C32 C33 C34 -1.6(5) .
O33 C32 C33 C34 0(100) .
C31 C32 C33 C34 -178.5(4) .
O36 C32 O33 C34 -1.6(5) .
C36 C32 O33 C34 -1.6(5) .
C33 C32 O33 C34 0(100) .
C31 C32 O33 C34 -178.5(4) .
C32 O33 C34 C33 0(100) .
C32 O33 C34 C35 1.6(6) .
C32 C33 C34 O33 0(100) .
C32 C33 C34 C35 1.6(6) .
O33 C34 C35 O36 -1.0(6) .
C33 C34 C35 O36 -1.0(6) .
O33 C34 C35 C36 -1.0(6) .
C33 C34 C35 C36 -1.0(6) .
O36 C32 C36 C35 0(100) .
C33 C32 C36 C35 1.0(6) .
O33 C32 C36 C35 1.0(6) .
C31 C32 C36 C35 177.5(4) .
C34 C35 C36 C32 0.0(6) .
O36 C35 C36 C32 0(100) .
C36 C32 O36 C35 0(100) .
C33 C32 O36 C35 1.0(6) .
O33 C32 O36 C35 1.0(6) .
C31 C32 O36 C35 177.5(4) .
C34 C35 O36 C32 0.0(6) .
C36 C35 O36 C32 0(100) .
