#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/48/7054833.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_7054833
loop_
_publ_author_name
'Yadav, Manoj Kumar'
'Rajput, Gunjan'
'Prasad, Lal Bahadur'
'Drew, Michael G. B.'
'Singh, Nanhai'
_publ_section_title
;
 Rare intermolecular M⋯H--C anagostic interactions in homoleptic
 Ni(ii)--Pd(ii) dithiocarbamate complexes
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5493
_journal_paper_doi               10.1039/C5NJ00452G
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C32 H32 N2 Ni O2 S4'
_chemical_formula_weight         663.55
_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
_audit_update_record
;
2015-04-24 deposited with the CCDC.
2015-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.467(9)
_cell_angle_beta                 102.098(9)
_cell_angle_gamma                106.947(9)
_cell_formula_units_Z            1
_cell_length_a                   6.4945(7)
_cell_length_b                   11.1068(10)
_cell_length_c                   11.7301(13)
_cell_measurement_reflns_used    5443
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.07
_cell_volume                     760.24(15)
_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_publication_material  'SHELXL-97, PLATON, WINGX (Ferrugia, 2012)'
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5443
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.07
_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    0.946
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             346
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0431
_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)+(0.0619P)²+0.0183P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                2509
_reflns_number_total             3340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00452g2.cif
_cod_data_source_block           C1
_cod_depositor_comments
'Adding full bibliography for 7054833--7054836.cif.'
_cod_original_cell_volume        760.24(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054833
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
S11 S -0.07973(11) 0.54535(6) 0.17334(6) 0.0524(2) Uani 1 1 d . . .
S13 S -0.34025(11) 0.35677(6) -0.04681(6) 0.0509(2) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.5000 0.0000 0.04174(16) Uani 1 2 d S . .
C12 C -0.3368(4) 0.4238(2) 0.0992(2) 0.0442(6) Uani 1 1 d . . .
C21 C -0.4883(5) 0.4554(3) 0.2713(3) 0.0585(7) Uani 1 1 d . . .
H21A H -0.6277 0.4709 0.2712 0.070 Uiso 1 1 calc R . .
H21B H -0.3686 0.5400 0.2971 0.070 Uiso 1 1 calc R . .
C22 C -0.4447(5) 0.3800(3) 0.3617(3) 0.0550(7) Uani 1 1 d . E .
C23 C -0.2487(6) 0.3544(4) 0.3902(3) 0.0817(10) Uani 1 1 d . . .
H23 H -0.1381 0.3847 0.3532 0.098 Uiso 1 1 calc R . .
C24 C -0.2132(6) 0.2851(4) 0.4721(4) 0.0972(12) Uani 1 1 d . E .
H24 H -0.0797 0.2684 0.4911 0.117 Uiso 1 1 calc R . .
C25 C -0.3787(7) 0.2405(4) 0.5260(3) 0.0920(12) Uani 1 1 d . . .
H25 H -0.3561 0.1934 0.5818 0.110 Uiso 1 1 calc R A 1
C27 C -0.6023(5) 0.3329(3) 0.4189(3) 0.0651(8) Uani 1 1 d . . .
H27 H -0.7364 0.3491 0.4012 0.078 Uiso 1 1 calc R B 1
C31 C -0.7178(4) 0.2846(3) 0.0756(3) 0.0552(7) Uani 1 1 d . . .
H31A H -0.7207 0.2629 -0.0092 0.066 Uiso 1 1 calc R . .
H31B H -0.8393 0.3174 0.0818 0.066 Uiso 1 1 calc R . .
C32 C -0.7565(4) 0.1626(2) 0.1174(2) 0.0468(6) Uani 1 1 d . E .
C33 C -0.6074(5) 0.0967(3) 0.1198(3) 0.0658(8) Uani 1 1 d . . .
H33 H -0.4796 0.1277 0.0951 0.079 Uiso 1 1 calc R . .
C34 C -0.6451(7) -0.0136(3) 0.1580(3) 0.0818(10) Uani 1 1 d . E .
H34 H -0.5437 -0.0580 0.1597 0.098 Uiso 1 1 calc R . .
C35 C -0.8324(7) -0.0579(3) 0.1934(3) 0.0861(12) Uani 1 1 d . . .
H35 H -0.8575 -0.1333 0.2194 0.103 Uiso 1 1 calc R C 1
C37 C -0.9430(5) 0.1138(3) 0.1535(3) 0.0631(8) Uani 1 1 d . . .
H37 H -1.0463 0.1569 0.1517 0.076 Uiso 1 1 calc R D 1
N14 N -0.5030(4) 0.3883(2) 0.1465(2) 0.0474(5) Uani 1 1 d . . .
C36A C -0.9821(6) 0.0030(3) 0.1922(3) 0.0753(10) Uani 0.519(5) 1 d P E 1
H36A H -1.1094 -0.0290 0.2169 0.090 Uiso 0.519(5) 1 calc PR E 1
C26A C -0.5706(6) 0.2639(4) 0.4997(3) 0.0733(9) Uani 0.519(5) 1 d P E 1
O28 O -0.7550(8) 0.1992(5) 0.5367(4) 0.0901(18) Uani 0.519(5) 1 d PD E 1
C29 C -0.7277(17) 0.1202(10) 0.6180(9) 0.112(3) Uani 0.519(5) 1 d PD E 1
H29A H -0.7272 0.0377 0.5738 0.168 Uiso 0.519(5) 1 calc PR E 1
H29B H -0.8496 0.1053 0.6539 0.168 Uiso 0.519(5) 1 calc PR E 1
H29C H -0.5882 0.1647 0.6807 0.168 Uiso 0.519(5) 1 calc PR E 1
C36B C -0.9821(6) 0.0030(3) 0.1922(3) 0.0753(10) Uani 0.481(5) 1 d P E 2
C26B C -0.5706(6) 0.2639(4) 0.4997(3) 0.0733(9) Uani 0.481(5) 1 d P E 2
H26B H -0.6813 0.2331 0.5364 0.088 Uiso 0.481(5) 1 calc PR E 2
O38 O -1.1385(10) -0.0163(6) 0.2539(7) 0.118(3) Uani 0.481(5) 1 d PD E 2
C39 C -1.1516(19) -0.1101(11) 0.3252(11) 0.128(4) Uani 0.481(5) 1 d PD E 2
H39A H -1.1889 -0.1962 0.2725 0.192 Uiso 0.481(5) 1 calc PR E 2
H39B H -1.2652 -0.1094 0.3658 0.192 Uiso 0.481(5) 1 calc PR E 2
H39C H -1.0092 -0.0865 0.3842 0.192 Uiso 0.481(5) 1 calc PR E 2
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 S11 Ni1 85.57(9) . .
C12 S13 Ni1 85.96(9) . .
S13 Ni1 S13 180.0 2_565 .
S13 Ni1 S11 100.64(3) 2_565 .
S13 Ni1 S11 79.36(3) . .
S13 Ni1 S11 79.36(3) 2_565 2_565
S13 Ni1 S11 100.64(3) . 2_565
S11 Ni1 S11 180.00(4) . 2_565
N14 C12 S13 125.4(2) . .
N14 C12 S11 125.5(2) . .
S13 C12 S11 109.09(14) . .
N14 C21 C22 113.8(2) . .
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 . .
C23 C22 C27 117.0(3) . .
C23 C22 C21 122.1(3) . .
C27 C22 C21 120.9(3) . .
C24 C23 C22 121.1(3) . .
C24 C23 H23 119.4 . .
C22 C23 H23 119.4 . .
C23 C24 C25 118.8(4) . .
C23 C24 H24 120.6 . .
C25 C24 H24 120.6 . .
C26B C25 C26A 0.00(11) . .
C26B C25 C24 121.1(4) . .
C26A C25 C24 121.1(4) . .
C26B C25 H25 119.4 . .
C26A C25 H25 119.4 . .
C24 C25 H25 119.4 . .
C26B C27 C26A 0.0(3) . .
C26B C27 C22 122.7(3) . .
C26A C27 C22 122.7(3) . .
C26B C27 H27 118.6 . .
C26A C27 H27 118.6 . .
C22 C27 H27 118.6 . .
N14 C31 C32 112.8(2) . .
N14 C31 H31A 109.0 . .
C32 C31 H31A 109.0 . .
N14 C31 H31B 109.0 . .
C32 C31 H31B 109.0 . .
H31A C31 H31B 107.8 . .
C37 C32 C33 118.1(3) . .
C37 C32 C31 120.6(2) . .
C33 C32 C31 121.3(2) . .
C34 C33 C32 120.5(3) . .
C34 C33 H33 119.7 . .
C32 C33 H33 119.7 . .
C35 C34 C33 119.1(3) . .
C35 C34 H34 120.4 . .
C33 C34 H34 120.4 . .
C36B C35 C36A 0.0(3) . .
C36B C35 C34 122.3(3) . .
C36A C35 C34 122.3(3) . .
C36B C35 H35 118.8 . .
C36A C35 H35 118.8 . .
C34 C35 H35 118.8 . .
C32 C37 C36B 121.7(3) . .
C32 C37 C36A 121.7(3) . .
C36B C37 C36A 0.0(3) . .
C32 C37 H37 119.1 . .
C36B C37 H37 119.1 . .
C36A C37 H37 119.1 . .
C12 N14 C31 121.6(2) . .
C12 N14 C21 121.6(2) . .
C31 N14 C21 116.6(2) . .
C35 C36A C37 118.2(3) . .
C35 C36A H36A 120.9 . .
C37 C36A H36A 120.9 . .
C25 C26A C27 119.2(3) . .
C25 C26A O28 121.2(4) . .
C27 C26A O28 118.7(4) . .
C26A O28 C29 119.6(5) . .
C35 C36B O38 124.1(4) . .
C35 C36B C37 118.2(3) . .
O38 C36B C37 115.6(4) . .
C25 C26B C27 119.2(3) . .
C25 C26B H26B 120.4 . .
C27 C26B H26B 120.4 . .
C36B O38 C39 119.7(7) . .
O38 C39 H39A 109.5 . .
O38 C39 H39B 109.5 . .
H39A C39 H39B 109.5 . .
O38 C39 H39C 109.5 . .
H39A C39 H39C 109.5 . .
H39B C39 H39C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S11 C12 1.725(3) .
S11 Ni1 2.2006(7) .
S13 C12 1.719(3) .
S13 Ni1 2.1932(7) .
Ni1 S13 2.1932(7) 2_565
Ni1 S11 2.2006(7) 2_565
C12 N14 1.311(3) .
C21 N14 1.473(3) .
C21 C22 1.508(4) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C23 1.372(4) .
C22 C27 1.373(4) .
C23 C24 1.369(5) .
C23 H23 0.9300 .
C24 C25 1.378(5) .
C24 H24 0.9300 .
C25 C26B 1.332(5) .
C25 C26A 1.332(5) .
C25 H25 0.9300 .
C27 C26B 1.352(4) .
C27 C26A 1.352(4) .
C27 H27 0.9300 .
C31 N14 1.470(3) .
C31 C32 1.503(3) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 C37 1.365(4) .
C32 C33 1.373(4) .
C33 C34 1.360(4) .
C33 H33 0.9300 .
C34 C35 1.356(5) .
C34 H34 0.9300 .
C35 C36B 1.336(5) .
C35 C36A 1.336(5) .
C35 H35 0.9300 .
C37 C36B 1.368(4) .
C37 C36A 1.368(4) .
C37 H37 0.9300 .
C36A H36A 0.9300 .
C26A O28 1.407(5) .
O28 C29 1.436(7) .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C36B O38 1.359(6) .
C26B H26B 0.9300 .
O38 C39 1.454(7) .
C39 H39A 0.9600 .
C39 H39B 0.9600 .
C39 H39C 0.9600 .
