#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:21:41 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180431 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/00/7210099.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_7210099
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 H32 N2 Ni O2 S4'
_chemical_formula_weight         591.49
_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                98.677(8)
_cell_angle_beta                 97.771(8)
_cell_angle_gamma                106.057(9)
_cell_formula_units_Z            1
_cell_length_a                   6.4140(6)
_cell_length_b                   7.9477(8)
_cell_length_c                   14.5825(13)
_cell_measurement_reflns_used    5170
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.32
_cell_volume                     693.83(12)
_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 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.1568
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5170
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.32
_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    1.026
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             310
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.0669
_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)+(0.0274P)²+0.0000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                1423
_reflns_number_total             3039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce27096c.txt
_cod_data_source_block           3
_cod_original_cell_volume        693.83(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7210099
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 1.0000 1.0000 0.0411(3) Uani 1 2 d S
S11 S 0.2198(2) 0.84009(18) 0.96331(9) 0.0485(4) Uani 1 1 d .
C12 C 0.0057(8) 0.7292(6) 0.8732(3) 0.0408(12) Uani 1 1 d .
S13 S -0.2083(2) 0.8125(2) 0.87283(9) 0.0570(4) Uani 1 1 d .
O14 O -0.0034(5) 0.5922(4) 0.8091(2) 0.0480(9) Uani 1 1 d .
C15 C 0.1850(8) 0.5181(6) 0.8115(3) 0.0415(13) Uani 1 1 d .
H15 H 0.3242 0.6155 0.8313 0.050 Uiso 1 1 calc R
C16 C 0.1692(9) 0.4240(7) 0.7115(3) 0.0516(15) Uani 1 1 d .
H16A H 0.0236 0.3385 0.6889 0.062 Uiso 1 1 calc R
H16B H 0.1913 0.5103 0.6705 0.062 Uiso 1 1 calc R
C17 C 0.3432(8) 0.3283(7) 0.7089(3) 0.0510(15) Uani 1 1 d .
H17A H 0.3314 0.2661 0.6450 0.061 Uiso 1 1 calc R
H17B H 0.4890 0.4147 0.7283 0.061 Uiso 1 1 calc R
N18 N 0.3143(7) 0.2003(5) 0.7720(2) 0.0436(11) Uani 1 1 d .
C19 C 0.3470(8) 0.2974(7) 0.8688(3) 0.0510(14) Uani 1 1 d .
H19A H 0.4921 0.3852 0.8854 0.061 Uiso 1 1 calc R
H19B H 0.3391 0.2149 0.9118 0.061 Uiso 1 1 calc R
C20 C 0.1711(8) 0.3904(7) 0.8783(3) 0.0470(14) Uani 1 1 d .
H20A H 0.0259 0.3027 0.8636 0.056 Uiso 1 1 calc R
H20B H 0.1937 0.4549 0.9426 0.056 Uiso 1 1 calc R
C21 C 0.4683(9) 0.0959(7) 0.7650(3) 0.0582(15) Uani 1 1 d .
H21A H 0.4665 0.0318 0.8166 0.070 Uiso 1 1 calc R
H21B H 0.6163 0.1769 0.7722 0.070 Uiso 1 1 calc R
C22 C 0.4176(9) -0.0362(7) 0.6733(3) 0.0446(13) Uani 1 1 d .
C23 C 0.5838(9) -0.0856(8) 0.6378(3) 0.0648(17) Uani 1 1 d .
H23 H 0.7295 -0.0333 0.6689 0.078 Uiso 1 1 calc R
C24 C 0.5354(11) -0.2137(9) 0.5554(4) 0.079(2) Uani 1 1 d .
H24 H 0.6492 -0.2481 0.5327 0.094 Uiso 1 1 calc R
C25 C 0.3257(11) -0.2894(8) 0.5076(4) 0.0724(19) Uani 1 1 d .
H25 H 0.2962 -0.3720 0.4515 0.087 Uiso 1 1 calc R
C26 C 0.1585(10) -0.2438(8) 0.5423(4) 0.0660(17) Uani 1 1 d .
H26 H 0.0135 -0.2963 0.5105 0.079 Uiso 1 1 calc R
C27 C 0.2053(9) -0.1184(7) 0.6254(4) 0.0624(16) Uani 1 1 d .
H27 H 0.0897 -0.0894 0.6493 0.075 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'
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
S13 Ni1 S13 180.00(9) . 2_577
S13 Ni1 S11 79.38(5) . .
S13 Ni1 S11 100.62(5) 2_577 .
S13 Ni1 S11 100.62(5) . 2_577
S13 Ni1 S11 79.38(5) 2_577 2_577
S11 Ni1 S11 179.999(1) . 2_577
C12 S11 Ni1 83.52(16) . .
O14 C12 S13 120.7(4) . .
O14 C12 S11 126.4(4) . .
S13 C12 S11 112.9(3) . .
C12 S13 Ni1 84.19(18) . .
C12 O14 C15 120.0(4) . .
O14 C15 C20 110.5(3) . .
O14 C15 C16 105.9(4) . .
C20 C15 C16 111.1(4) . .
O14 C15 H15 109.8 . .
C20 C15 H15 109.8 . .
C16 C15 H15 109.8 . .
C17 C16 C15 109.6(4) . .
C17 C16 H16A 109.8 . .
C15 C16 H16A 109.8 . .
C17 C16 H16B 109.8 . .
C15 C16 H16B 109.8 . .
H16A C16 H16B 108.2 . .
N18 C17 C16 110.3(4) . .
N18 C17 H17A 109.6 . .
C16 C17 H17A 109.6 . .
N18 C17 H17B 109.6 . .
C16 C17 H17B 109.6 . .
H17A C17 H17B 108.1 . .
C21 N18 C19 110.3(4) . .
C21 N18 C17 111.3(4) . .
C19 N18 C17 108.9(4) . .
N18 C19 C20 110.2(4) . .
N18 C19 H19A 109.6 . .
C20 C19 H19A 109.6 . .
N18 C19 H19B 109.6 . .
C20 C19 H19B 109.6 . .
H19A C19 H19B 108.1 . .
C15 C20 C19 109.2(4) . .
C15 C20 H20A 109.8 . .
C19 C20 H20A 109.8 . .
C15 C20 H20B 109.8 . .
C19 C20 H20B 109.8 . .
H20A C20 H20B 108.3 . .
N18 C21 C22 113.9(4) . .
N18 C21 H21A 108.8 . .
C22 C21 H21A 108.8 . .
N18 C21 H21B 108.8 . .
C22 C21 H21B 108.8 . .
H21A C21 H21B 107.7 . .
C27 C22 C23 117.7(5) . .
C27 C22 C21 121.8(5) . .
C23 C22 C21 120.3(5) . .
C22 C23 C24 120.2(6) . .
C22 C23 H23 119.9 . .
C24 C23 H23 119.9 . .
C25 C24 C23 121.2(5) . .
C25 C24 H24 119.4 . .
C23 C24 H24 119.4 . .
C24 C25 C26 119.5(6) . .
C24 C25 H25 120.3 . .
C26 C25 H25 120.3 . .
C25 C26 C27 119.6(6) . .
C25 C26 H26 120.2 . .
C27 C26 H26 120.2 . .
C22 C27 C26 121.7(5) . .
C22 C27 H27 119.1 . .
C26 C27 H27 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S13 2.1999(14) .
Ni1 S13 2.1999(14) 2_577
Ni1 S11 2.2089(12) .
Ni1 S11 2.2089(12) 2_577
S11 C12 1.698(5) .
C12 O14 1.306(5) .
C12 S13 1.680(5) .
O14 C15 1.482(5) .
C15 C20 1.502(6) .
C15 C16 1.512(5) .
C15 H15 0.9800 .
C16 C17 1.516(6) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 N18 1.462(5) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
N18 C21 1.460(6) .
N18 C19 1.460(5) .
C19 C20 1.520(6) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 C22 1.505(6) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C27 1.372(7) .
C22 C23 1.371(6) .
C23 C24 1.389(7) .
C23 H23 0.9300 .
C24 C25 1.352(7) .
C24 H24 0.9300 .
C25 C26 1.357(7) .
C25 H25 0.9300 .
C26 C27 1.387(7) .
C26 H26 0.9300 .
C27 H27 0.9300 .
