#------------------------------------------------------------------------------
#$Date: 2019-06-20 14:43:28 +0300 (Thu, 20 Jun 2019) $
#$Revision: 216302 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/16/1551691.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_1551691
loop_
_publ_author_name
'SHARMA, Neerupama'
'SINGH, Kuldeep'
'SACHAR, Renu'
'GUPTA, Vivek K.'
Rajnikant,
_publ_section_title
;
 Crystal Structure of
 Bis(O-propyldithiocarbonato-^|^kappa;2S,S^|^prime;)(3,5-lutidine-^|^kappa;N)nickel(II)
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              19
_journal_paper_doi               10.2116/xraystruct.29.19
_journal_volume                  29
_journal_year                    2013
_chemical_formula_moiety         'C22 H32 N2 Ni O2 S4'
_chemical_formula_sum            'C22 H32 N2 Ni O2 S4'
_chemical_formula_weight         543.45
_chemical_name_systematic
;
bis(O-propyldithiocarbonato-k2S,S?)(3,5-lutidine-kN)nickel(II)
;
_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_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                87.484(5)
_cell_angle_beta                 72.927(5)
_cell_angle_gamma                75.686(5)
_cell_formula_units_Z            1
_cell_length_a                   7.008(5)
_cell_length_b                   9.546(5)
_cell_length_c                   10.621(5)
_cell_measurement_reflns_used    5876
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0730
_cell_measurement_theta_min      3.4470
_cell_volume                     657.8(7)
_computing_cell_refinement       'CrysAlisPro, Diff.Ltd,Ver 1.171.34.40'
_computing_data_collection       'CrysAlisPro,Diff.Ltd,Ver 1.171.34.40'
_computing_data_reduction        'CrysAlisPro, Diff.Ltd,Ver 1.171.34.40'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'PLATON(Spek,2009)& PARST(Nardeli 1995'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1049
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'omega 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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12329
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Crys Alis RED'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'blocked shape'
_exptl_crystal_F_000             286
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0371
_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)+(0.0420P)²+0.3271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                2074
_reflns_number_total             2582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            29_19_1.txt
_cod_data_source_block           nirupama1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1551691
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 0.5000 0.5000 0.5000 0.03681(16) Uani 1 2 d S
S1 S 0.50009(11) 0.62585(7) 0.29257(7) 0.0471(2) Uani 1 1 d .
S2 S 0.85895(10) 0.49602(7) 0.38356(7) 0.04392(19) Uani 1 1 d .
O1 O 0.8686(3) 0.6299(2) 0.1586(2) 0.0541(5) Uani 1 1 d .
N1 N 0.5365(3) 0.3000(2) 0.4049(2) 0.0418(5) Uani 1 1 d .
C9 C 0.7565(4) 0.5851(3) 0.2694(3) 0.0423(6) Uani 1 1 d .
C2 C 0.4172(4) 0.2850(3) 0.3318(3) 0.0490(7) Uani 1 1 d .
H2 H 0.3195 0.3661 0.3197 0.059 Uiso 1 1 calc R
C3 C 0.4309(5) 0.1545(3) 0.2728(3) 0.0569(8) Uani 1 1 d .
C4 C 0.5742(5) 0.0356(3) 0.2934(3) 0.0587(8) Uani 1 1 d .
H4 H 0.5855 -0.0538 0.2567 0.070 Uiso 1 1 calc R
C5 C 0.7011(5) 0.0470(3) 0.3677(3) 0.0511(7) Uani 1 1 d .
C6 C 0.6769(4) 0.1828(3) 0.4208(3) 0.0469(6) Uani 1 1 d .
H6 H 0.7629 0.1927 0.4701 0.056 Uiso 1 1 calc R
C7 C 0.2923(6) 0.1464(4) 0.1899(4) 0.0934(13) Uani 1 1 d .
H7A H 0.2764 0.0494 0.1888 0.140 Uiso 1 1 calc R
H7B H 0.3522 0.1731 0.1016 0.140 Uiso 1 1 calc R
H7C H 0.1600 0.2115 0.2265 0.140 Uiso 1 1 calc R
C8 C 0.8592(6) -0.0807(3) 0.3929(4) 0.0743(10) Uani 1 1 d .
H8A H 0.8278 -0.1685 0.3743 0.111 Uiso 1 1 calc R
H8B H 0.8574 -0.0777 0.4834 0.111 Uiso 1 1 calc R
H8C H 0.9932 -0.0773 0.3370 0.111 Uiso 1 1 calc R
C10 C 1.0921(5) 0.5929(4) 0.1275(4) 0.0697(9) Uani 1 1 d .
H10A H 1.1460 0.4892 0.1130 0.084 Uiso 1 1 calc R
H10B H 1.1326 0.6226 0.2000 0.084 Uiso 1 1 calc R
C11 C 1.1760(7) 0.6704(5) 0.0045(4) 0.0928(13) Uani 1 1 d .
H11A H 1.3249 0.6368 -0.0241 0.111 Uiso 1 1 calc R
H11B H 1.1250 0.6452 -0.0649 0.111 Uiso 1 1 calc R
C12 C 1.1220(9) 0.8225(6) 0.0220(5) 0.137(2) Uani 1 1 d .
H12A H 0.9749 0.8563 0.0543 0.205 Uiso 1 1 calc R
H12B H 1.1713 0.8656 -0.0607 0.205 Uiso 1 1 calc R
H12C H 1.1831 0.8489 0.0845 0.205 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'
N N 0.0061 0.0033 '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'
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'
H H 0.0000 0.0000 '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
N1 Ni1 N1 180.000(1) . 2_666
N1 Ni1 S2 90.46(6) . 2_666
N1 Ni1 S2 89.54(6) 2_666 2_666
N1 Ni1 S2 89.54(6) . .
N1 Ni1 S2 90.46(6) 2_666 .
S2 Ni1 S2 180.0 2_666 .
N1 Ni1 S1 89.71(7) . 2_666
N1 Ni1 S1 90.29(7) 2_666 2_666
S2 Ni1 S1 73.23(3) 2_666 2_666
S2 Ni1 S1 106.77(3) . 2_666
N1 Ni1 S1 90.29(7) . .
N1 Ni1 S1 89.71(7) 2_666 .
S2 Ni1 S1 106.77(3) 2_666 .
S2 Ni1 S1 73.23(3) . .
S1 Ni1 S1 180.0 2_666 .
C9 S1 Ni1 82.70(9) . .
C9 S2 Ni1 83.27(10) . .
C9 O1 C10 119.8(2) . .
C2 N1 C6 117.7(2) . .
C2 N1 Ni1 121.84(17) . .
C6 N1 Ni1 120.46(18) . .
O1 C9 S2 123.0(2) . .
O1 C9 S1 116.2(2) . .
S2 C9 S1 120.79(17) . .
N1 C2 C3 123.4(3) . .
N1 C2 H2 118.3 . .
C3 C2 H2 118.3 . .
C4 C3 C2 117.4(3) . .
C4 C3 C7 122.3(3) . .
C2 C3 C7 120.3(3) . .
C3 C4 C5 120.9(3) . .
C3 C4 H4 119.5 . .
C5 C4 H4 119.5 . .
C4 C5 C6 117.1(3) . .
C4 C5 C8 122.5(3) . .
C6 C5 C8 120.4(3) . .
N1 C6 C5 123.5(3) . .
N1 C6 H6 118.2 . .
C5 C6 H6 118.2 . .
C3 C7 H7A 109.5 . .
C3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C3 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O1 C10 C11 108.0(3) . .
O1 C10 H10A 110.1 . .
C11 C10 H10A 110.1 . .
O1 C10 H10B 110.1 . .
C11 C10 H10B 110.1 . .
H10A C10 H10B 108.4 . .
C12 C11 C10 113.5(4) . .
C12 C11 H11A 108.9 . .
C10 C11 H11A 108.9 . .
C12 C11 H11B 108.9 . .
C10 C11 H11B 108.9 . .
H11A C11 H11B 107.7 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.123(2) .
Ni1 N1 2.123(2) 2_666
Ni1 S2 2.4472(17) 2_666
Ni1 S2 2.4472(17) .
Ni1 S1 2.4626(12) 2_666
Ni1 S1 2.4626(12) .
S1 C9 1.686(3) .
S2 C9 1.682(3) .
O1 C9 1.328(3) .
O1 C10 1.456(4) .
N1 C2 1.331(3) .
N1 C6 1.336(3) .
C2 C3 1.388(4) .
C2 H2 0.9300 .
C3 C4 1.374(4) .
C3 C7 1.507(5) .
C4 C5 1.376(4) .
C4 H4 0.9300 .
C5 C6 1.388(4) .
C5 C8 1.504(4) .
C6 H6 0.9300 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C10 C11 1.510(5) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.413(6) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
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_1
N1 Ni1 S1 C9 91.00(10) 2_666
S2 Ni1 S1 C9 -179.56(8) 2_666
S2 Ni1 S1 C9 0.44(8) .
S1 Ni1 S1 C9 -9(100) 2_666
N1 Ni1 S2 C9 90.00(11) .
N1 Ni1 S2 C9 -90.00(11) 2_666
S1 Ni1 S2 C9 179.56(8) 2_666
S1 Ni1 S2 C9 -0.44(8) .
S2 Ni1 N1 C2 57.3(2) 2_666
S2 Ni1 N1 C2 -122.7(2) .
S1 Ni1 N1 C2 130.5(2) 2_666
S1 Ni1 N1 C2 -49.5(2) .
S2 Ni1 N1 C6 -120.2(2) 2_666
S2 Ni1 N1 C6 59.8(2) .
S1 Ni1 N1 C6 -47.0(2) 2_666
S1 Ni1 N1 C6 133.0(2) .
C10 O1 C9 S2 4.5(3) .
C10 O1 C9 S1 -176.8(2) .
Ni1 S2 C9 O1 179.3(2) .
Ni1 S2 C9 S1 0.71(13) .
Ni1 S1 C9 O1 -179.38(19) .
Ni1 S1 C9 S2 -0.71(13) .
C6 N1 C2 C3 0.4(4) .
Ni1 N1 C2 C3 -177.2(2) .
N1 C2 C3 C4 0.9(4) .
N1 C2 C3 C7 -179.2(3) .
C2 C3 C4 C5 -1.2(4) .
C7 C3 C4 C5 178.8(3) .
C3 C4 C5 C6 0.3(4) .
C3 C4 C5 C8 179.8(3) .
C2 N1 C6 C5 -1.4(4) .
Ni1 N1 C6 C5 176.3(2) .
C4 C5 C6 N1 1.0(4) .
C8 C5 C6 N1 -178.4(3) .
C9 O1 C10 C11 -174.2(3) .
O1 C10 C11 C12 66.1(5) .
