#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/48/7054835.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_7054835
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            'C34 H38 N4 Ni O6 S4'
_chemical_formula_weight         785.63
_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                104.768(12)
_cell_angle_beta                 103.014(11)
_cell_angle_gamma                105.644(14)
_cell_formula_units_Z            1
_cell_length_a                   7.0268(10)
_cell_length_b                   10.6267(18)
_cell_length_c                   13.7577(16)
_cell_measurement_reflns_used    6893
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.06
_cell_volume                     907.7(3)
_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(Farrugia,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 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6893
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.06
_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    0.814
_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    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0573
_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)+(0.0461P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                2465
_reflns_number_total             3961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00452g2.cif
_cod_data_source_block           C3
_cod_depositor_comments
'Adding full bibliography for 7054833--7054836.cif.'
_cod_original_cell_volume        907.7(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054835
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
S11 S 0.20016(12) -0.12123(10) -0.03763(7) 0.0456(3) Uani 1 1 d .
S13 S 0.19794(14) 0.03701(12) 0.15930(7) 0.0540(3) Uani 1 1 d .
Ni1 Ni 0.0000 0.0000 0.0000 0.0410(2) Uani 1 2 d S
C12 C 0.3101(5) -0.0698(4) 0.0974(3) 0.0381(8) Uani 1 1 d .
N44 N 0.4568(4) -0.1077(3) 0.1463(2) 0.0387(7) Uani 1 1 d .
O24 O 1.1029(4) 0.3836(3) 0.3780(3) 0.0811(10) Uani 1 1 d .
O25 O 1.3825(3) 0.2762(3) 0.4533(2) 0.0665(8) Uani 1 1 d .
C21 C 0.5338(4) -0.0644(4) 0.2625(2) 0.0439(9) Uani 1 1 d .
H21A H 0.5129 -0.1464 0.2834 0.053 Uiso 1 1 calc R
H21B H 0.4523 -0.0134 0.2916 0.053 Uiso 1 1 calc R
C22 C 0.7607(4) 0.0251(4) 0.3094(2) 0.0394(8) Uani 1 1 d .
C23 C 0.8213(5) 0.1615(4) 0.3163(3) 0.0495(10) Uani 1 1 d .
H23 H 0.7233 0.1971 0.2878 0.059 Uiso 1 1 calc R
C24 C 1.0282(6) 0.2474(4) 0.3657(3) 0.0548(10) Uani 1 1 d .
C25 C 1.1745(5) 0.1934(4) 0.4073(3) 0.0456(9) Uani 1 1 d .
C26 C 1.1143(5) 0.0552(4) 0.3984(2) 0.0397(9) Uani 1 1 d .
C27 C 0.9059(4) -0.0301(4) 0.3491(2) 0.0394(8) Uani 1 1 d .
H27 H 0.8648 -0.1234 0.3431 0.047 Uiso 1 1 calc R
O28 O 1.2690(3) 0.0098(3) 0.43864(18) 0.0501(7) Uani 1 1 d .
C241 C 0.9579(7) 0.4456(5) 0.3421(5) 0.120(2) Uani 1 1 d .
H24A H 0.8816 0.3954 0.2686 0.180 Uiso 1 1 calc R
H24B H 1.0313 0.5402 0.3508 0.180 Uiso 1 1 calc R
H24C H 0.8630 0.4432 0.3826 0.180 Uiso 1 1 calc R
C251 C 1.4303(6) 0.3581(5) 0.5600(3) 0.0804(15) Uani 1 1 d .
H25A H 1.3305 0.4038 0.5658 0.121 Uiso 1 1 calc R
H25B H 1.5673 0.4264 0.5835 0.121 Uiso 1 1 calc R
H25C H 1.4254 0.2999 0.6032 0.121 Uiso 1 1 calc R
C281 C 1.2138(5) -0.1335(4) 0.4251(3) 0.0522(10) Uani 1 1 d .
H28A H 1.1143 -0.1579 0.4609 0.078 Uiso 1 1 calc R
H28B H 1.3358 -0.1529 0.4542 0.078 Uiso 1 1 calc R
H28C H 1.1537 -0.1867 0.3510 0.078 Uiso 1 1 calc R
C51 C 0.5429(5) -0.2020(4) 0.0884(3) 0.0450(9) Uani 1 1 d .
H51A H 0.6928 -0.1579 0.1089 0.054 Uiso 1 1 calc R
H51B H 0.4859 -0.2204 0.0130 0.054 Uiso 1 1 calc R
C52 C 0.4941(5) -0.3358(3) 0.1100(2) 0.0558(11) Uani 1 1 d G
C53 C 0.2929(4) -0.4092(4) 0.1038(3) 0.0916(17) Uani 1 1 d G
H53 H 0.1855 -0.3760 0.0844 0.110 Uiso 1 1 calc R
C54 C 0.2522(6) -0.5321(4) 0.1265(3) 0.144(3) Uani 1 1 d G
H54 H 0.1175 -0.5812 0.1224 0.172 Uiso 1 1 calc R
C55 C 0.4127(9) -0.5816(3) 0.1554(3) 0.160(4) Uani 1 1 d G
H55 H 0.3854 -0.6638 0.1706 0.192 Uiso 1 1 calc R
N56 N 0.6139(7) -0.5082(4) 0.1616(2) 0.132(2) Uani 1 1 d G
C57 C 0.6546(4) -0.3853(4) 0.1389(2) 0.0872(16) Uani 1 1 d G
H57 H 0.7893 -0.3362 0.1430 0.105 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
C12 S11 Ni1 84.93(12) . .
C12 S13 Ni1 85.74(11) . .
S13 Ni1 S13 180.00(6) 2 .
S13 Ni1 S11 79.39(4) 2 2
S13 Ni1 S11 100.61(4) . 2
S13 Ni1 S11 100.61(4) 2 .
S13 Ni1 S11 79.39(4) . .
S11 Ni1 S11 180.00(2) 2 .
N44 C12 S13 124.8(2) . .
N44 C12 S11 125.3(3) . .
S13 C12 S11 109.88(19) . .
C12 N44 C51 122.0(3) . .
C12 N44 C21 121.5(3) . .
C51 N44 C21 116.4(3) . .
C24 O24 C241 117.7(3) . .
C25 O25 C251 112.9(3) . .
N44 C21 C22 113.3(2) . .
N44 C21 H21A 108.9 . .
C22 C21 H21A 108.9 . .
N44 C21 H21B 108.9 . .
C22 C21 H21B 108.9 . .
H21A C21 H21B 107.7 . .
C23 C22 C27 120.4(3) . .
C23 C22 C21 119.9(3) . .
C27 C22 C21 119.6(3) . .
C22 C23 C24 120.5(4) . .
C22 C23 H23 119.8 . .
C24 C23 H23 119.8 . .
O24 C24 C23 125.0(4) . .
O24 C24 C25 115.4(3) . .
C23 C24 C25 119.5(4) . .
C26 C25 C24 120.0(3) . .
C26 C25 O25 119.6(3) . .
C24 C25 O25 120.3(4) . .
C25 C26 O28 116.2(3) . .
C25 C26 C27 120.0(3) . .
O28 C26 C27 123.8(3) . .
C22 C27 C26 119.5(3) . .
C22 C27 H27 120.2 . .
C26 C27 H27 120.2 . .
C26 O28 C281 117.4(3) . .
O24 C241 H24A 109.5 . .
O24 C241 H24B 109.5 . .
H24A C241 H24B 109.5 . .
O24 C241 H24C 109.5 . .
H24A C241 H24C 109.5 . .
H24B C241 H24C 109.5 . .
O25 C251 H25A 109.5 . .
O25 C251 H25B 109.5 . .
H25A C251 H25B 109.5 . .
O25 C251 H25C 109.5 . .
H25A C251 H25C 109.5 . .
H25B C251 H25C 109.5 . .
O28 C281 H28A 109.5 . .
O28 C281 H28B 109.5 . .
H28A C281 H28B 109.5 . .
O28 C281 H28C 109.5 . .
H28A C281 H28C 109.5 . .
H28B C281 H28C 109.5 . .
N44 C51 C52 111.6(3) . .
N44 C51 H51A 109.3 . .
C52 C51 H51A 109.3 . .
N44 C51 H51B 109.3 . .
C52 C51 H51B 109.3 . .
H51A C51 H51B 108.0 . .
C53 C52 C57 120.0 . .
C53 C52 C51 121.1(3) . .
C57 C52 C51 118.9(3) . .
C54 C53 C52 120.0 . .
C54 C53 H53 120.0 . .
C52 C53 H53 120.0 . .
C55 C54 C53 120.0 . .
C55 C54 H54 120.0 . .
C53 C54 H54 120.0 . .
C54 C55 N56 120.0 . .
C54 C55 H55 120.0 . .
N56 C55 H55 120.0 . .
C57 N56 C55 120.0 . .
N56 C57 C52 120.0 . .
N56 C57 H57 120.0 . .
C52 C57 H57 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S11 C12 1.719(3) .
S11 Ni1 2.2070(10) .
S13 C12 1.710(3) .
S13 Ni1 2.1875(10) .
Ni1 S13 2.1875(10) 2
Ni1 S11 2.2070(10) 2
C12 N44 1.315(4) .
N44 C51 1.463(4) .
N44 C21 1.471(4) .
O24 C24 1.350(5) .
O24 C241 1.421(5) .
O25 C25 1.384(4) .
O25 C251 1.413(5) .
C21 C22 1.506(4) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C23 1.368(5) .
C22 C27 1.385(4) .
C23 C24 1.390(5) .
C23 H23 0.9300 .
C24 C25 1.391(5) .
C25 C26 1.379(5) .
C26 O28 1.367(4) .
C26 C27 1.396(4) .
C27 H27 0.9300 .
O28 C281 1.416(4) .
C241 H24A 0.9600 .
C241 H24B 0.9600 .
C241 H24C 0.9600 .
C251 H25A 0.9600 .
C251 H25B 0.9600 .
C251 H25C 0.9600 .
C281 H28A 0.9600 .
C281 H28B 0.9600 .
C281 H28C 0.9600 .
C51 C52 1.492(4) .
C51 H51A 0.9700 .
C51 H51B 0.9700 .
C52 C53 1.3900 .
C52 C57 1.3900 .
C53 C54 1.3900 .
C53 H53 0.9300 .
C54 C55 1.3900 .
C54 H54 0.9300 .
C55 N56 1.3900 .
C55 H55 0.9300 .
N56 C57 1.3900 .
C57 H57 0.9300 .
