#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/48/7054834.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_7054834
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            'C29 H29 N3 Pd S4'
_chemical_formula_weight         654.19
_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                74.967(12)
_cell_angle_beta                 84.813(10)
_cell_angle_gamma                72.281(14)
_cell_formula_units_Z            1
_cell_length_a                   6.7086(10)
_cell_length_b                   10.3187(18)
_cell_length_c                   10.8136(12)
_cell_measurement_reflns_used    4823
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.23
_cell_volume                     688.59(19)
_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      150(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_device_type  'CCD diffractometer'
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4823
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.23
_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    1.002
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             334
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.079
_refine_diff_density_min         -1.631
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0931
_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)+(0.1412P)²+0.1098P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2176
_refine_ls_wR_factor_ref         0.2487
_reflns_number_gt                2704
_reflns_number_total             3838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00452g2.cif
_cod_data_source_block           C2
_cod_depositor_comments
'Adding full bibliography for 7054833--7054836.cif.'
_cod_original_cell_volume        688.59(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054834
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 0.4087(8) 0.1335(6) 0.1643(5) 0.0413(12) Uani 1 1 d . B .
Pd1 Pd 0.0000 0.0000 0.0000 0.0373(3) Uani 1 2 d S . .
S11 S 0.1551(3) -0.03163(17) 0.19325(14) 0.0423(4) Uani 1 1 d . . .
S13 S 0.2123(3) 0.14774(17) -0.04666(14) 0.0401(4) Uani 1 1 d . . .
C12 C 0.2811(9) 0.0876(7) 0.1131(6) 0.0373(12) Uani 1 1 d . . .
C21 C 0.4754(11) 0.0697(8) 0.2983(6) 0.0506(17) Uani 1 1 d . . .
H21A H 0.6242 0.0565 0.3028 0.061 Uiso 1 1 calc R . .
H21B H 0.4529 -0.0221 0.3249 0.061 Uiso 1 1 calc R . .
C22 C 0.3622(12) 0.1551(7) 0.3898(6) 0.0499(16) Uani 1 1 d . . .
C23 C 0.4559(14) 0.2342(9) 0.4403(7) 0.062(2) Uani 1 1 d . . .
H23 H 0.5928 0.2342 0.4169 0.075 Uiso 1 1 calc R . .
C25 C 0.1581(12) 0.1569(9) 0.4293(7) 0.0558(18) Uani 1 1 d . . .
H25 H 0.0927 0.1043 0.3984 0.067 Uiso 1 1 calc R . .
C26 C 0.0502(13) 0.2358(10) 0.5140(8) 0.063(2) Uani 1 1 d . . .
H26 H -0.0859 0.2357 0.5395 0.076 Uiso 1 1 calc R . .
C27 C 0.1432(15) 0.3116(9) 0.5583(7) 0.067(2) Uani 1 1 d . . .
H27 H 0.0692 0.3656 0.6135 0.081 Uiso 1 1 calc R . .
C28 C 0.3476(15) 0.3122(9) 0.5243(7) 0.065(2) Uani 1 1 d . . .
H28 H 0.4105 0.3644 0.5576 0.079 Uiso 1 1 calc R . .
C31 C 0.5213(10) 0.2301(8) 0.0844(7) 0.0487(16) Uani 1 1 d . . .
H31A H 0.4462 0.2751 0.0046 0.058 Uiso 1 1 calc R A 1
H31B H 0.6581 0.1734 0.0633 0.058 Uiso 1 1 calc R A 1
C32A C 0.5531(19) 0.3423(12) 0.1366(14) 0.032(3) Uani 0.50 1 d PG B 1
C33A C 0.7430(13) 0.3543(15) 0.1740(17) 0.037(3) Uani 0.50 1 d PG B 1
H33A H 0.8760 0.2940 0.1666 0.044 Uiso 0.50 1 calc PR B 1
C34A C 0.694(2) 0.4743(15) 0.2247(18) 0.055(6) Uani 0.50 1 d PG B 1
H34A H 0.7894 0.5065 0.2564 0.066 Uiso 0.50 1 calc PR B 1
C35A C 0.474(2) 0.5366(9) 0.2186(13) 0.054(5) Uani 0.50 1 d PG B 1
H35A H 0.3997 0.6168 0.2456 0.065 Uiso 0.50 1 calc PR B 1
N36A N 0.3868(13) 0.4551(10) 0.1641(9) 0.041(3) Uani 0.50 1 d PG B 1
C37A C 0.168(2) 0.4755(15) 0.1484(14) 0.054(4) Uani 0.50 1 d P B 1
H37A H 0.1106 0.4320 0.2271 0.082 Uiso 0.50 1 calc PR B 1
H37B H 0.1510 0.4341 0.0816 0.082 Uiso 0.50 1 calc PR B 1
H37C H 0.0961 0.5742 0.1259 0.082 Uiso 0.50 1 calc PR B 1
C32B C 0.493(2) 0.3466(14) 0.1417(17) 0.049(5) Uani 0.50 1 d PG B 2
C33B C 0.6660(15) 0.3747(16) 0.1777(18) 0.047(4) Uani 0.50 1 d PG B 2
H33B H 0.7985 0.3118 0.1757 0.056 Uiso 0.50 1 calc PR B 2
C34B C 0.641(2) 0.4969(17) 0.2168(19) 0.060(6) Uani 0.50 1 d PG B 2
H34B H 0.7571 0.5157 0.2409 0.072 Uiso 0.50 1 calc PR B 2
C35B C 0.443(3) 0.5910(11) 0.2198(16) 0.082(8) Uani 0.50 1 d PG B 2
H35B H 0.4265 0.6727 0.2460 0.098 Uiso 0.50 1 calc PR B 2
C36B C 0.2700(19) 0.5629(12) 0.1838(12) 0.078(6) Uani 0.50 1 d PG B 2
H36B H 0.1375 0.6258 0.1858 0.093 Uiso 0.50 1 calc PR B 2
C37B C 0.2948(17) 0.4406(16) 0.1447(13) 0.059(5) Uani 0.50 1 d PG B 2
H37D H 0.1789 0.4218 0.1206 0.071 Uiso 0.50 1 calc PR B 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'
Pd Pd -0.9988 1.0072 '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'
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 120.5(6) . .
C12 N14 C31 121.3(6) . .
C21 N14 C31 117.2(6) . .
S11 Pd1 S11 180.00(8) 2 .
S11 Pd1 S13 75.38(6) 2 2
S11 Pd1 S13 104.62(6) . 2
S11 Pd1 S13 104.62(6) 2 .
S11 Pd1 S13 75.38(6) . .
S13 Pd1 S13 180.0 2 .
C12 S11 Pd1 87.0(2) . .
C12 S13 Pd1 86.4(2) . .
N14 C12 S11 125.7(5) . .
N14 C12 S13 123.0(5) . .
S11 C12 S13 111.2(4) . .
N14 C21 C22 113.7(6) . .
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 . .
C25 C22 C23 117.4(7) . .
C25 C22 C21 120.5(7) . .
C23 C22 C21 122.1(7) . .
C28 C23 C22 120.8(8) . .
C28 C23 H23 119.6 . .
C22 C23 H23 119.6 . .
C26 C25 C22 121.4(7) . .
C26 C25 H25 119.3 . .
C22 C25 H25 119.3 . .
C27 C26 C25 119.5(8) . .
C27 C26 H26 120.2 . .
C25 C26 H26 120.2 . .
C26 C27 C28 121.8(8) . .
C26 C27 H27 119.1 . .
C28 C27 H27 119.1 . .
C23 C28 C27 119.1(8) . .
C23 C28 H28 120.5 . .
C27 C28 H28 120.5 . .
C32B C31 N14 108.6(8) . .
C32B C31 C32A 15.3(8) . .
N14 C31 C32A 118.9(7) . .
C32B C31 H31A 102.3 . .
N14 C31 H31A 107.6 . .
C32A C31 H31A 107.6 . .
C32B C31 H31B 122.8 . .
N14 C31 H31B 107.6 . .
C32A C31 H31B 107.6 . .
H31A C31 H31B 107.0 . .
C33A C32A N36A 108.0 . .
C33A C32A C31 128.4(9) . .
N36A C32A C31 123.5(9) . .
C34A C33A C32A 108.0 . .
C34A C33A H33A 126.0 . .
C32A C33A H33A 126.0 . .
C33A C34A C35A 108.0 . .
C33A C34A H34A 126.0 . .
C35A C34A H34A 126.0 . .
N36A C35A C34A 108.0 . .
N36A C35A H35A 126.0 . .
C34A C35A H35A 126.0 . .
C35A N36A C32A 108.0 . .
C35A N36A C37A 126.4(11) . .
C32A N36A C37A 125.5(11) . .
C33B C32B C37B 120.0 . .
C33B C32B C31 120.0(11) . .
C37B C32B C31 119.5(11) . .
C34B C33B C32B 120.0 . .
C34B C33B H33B 120.0 . .
C32B C33B H33B 120.0 . .
C35B C34B C33B 120.0 . .
C35B C34B H34B 120.0 . .
C33B C34B H34B 120.0 . .
C34B C35B C36B 120.0 . .
C34B C35B H35B 120.0 . .
C36B C35B H35B 120.0 . .
C37B C36B C35B 120.0 . .
C37B C36B H36B 120.0 . .
C35B C36B H36B 120.0 . .
C36B C37B C32B 120.0 . .
C36B C37B H37D 120.0 . .
C32B C37B H37D 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N14 C12 1.316(8) .
N14 C21 1.475(8) .
N14 C31 1.485(9) .
Pd1 S11 2.3213(16) 2
Pd1 S11 2.3213(16) .
Pd1 S13 2.3239(16) 2
Pd1 S13 2.3239(16) .
S11 C12 1.711(7) .
S13 C12 1.731(6) .
C21 C22 1.497(9) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C25 1.393(10) .
C22 C23 1.402(10) .
C23 C28 1.380(11) .
C23 H23 0.9300 .
C25 C26 1.390(10) .
C25 H25 0.9300 .
C26 C27 1.333(12) .
C26 H26 0.9300 .
C27 C28 1.388(12) .
C27 H27 0.9300 .
C28 H28 0.9300 .
C31 C32B 1.446(11) .
C31 C32A 1.489(11) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32A C33A 1.4200 .
C32A N36A 1.4200 .
C33A C34A 1.4200 .
C33A H33A 0.9300 .
C34A C35A 1.4200 .
C34A H34A 0.9300 .
C35A N36A 1.4200 .
C35A H35A 0.9300 .
N36A C37A 1.437(16) .
C37A H37A 0.9600 .
C37A H37B 0.9600 .
C37A H37C 0.9600 .
C32B C33B 1.3900 .
C32B C37B 1.3900 .
C33B C34B 1.3900 .
C33B H33B 0.9300 .
C34B C35B 1.3900 .
C34B H34B 0.9300 .
C35B C36B 1.3900 .
C35B H35B 0.9300 .
C36B C37B 1.3900 .
C36B H36B 0.9300 .
C37B H37D 0.9300 .
