Synthesis, structural and theoretical studies of dithiodiglycolamide compounds of palladium(ii).
Vats, Balgovind; Kannan, S.; Sundararajan, Mahesh; Kumar, Mukesh; Drew, M. G. B.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11867–11876; doi:10.1039/c4dt03814b

data_7035388
_publ_section_title
;
 Synthesis, structural and theoretical studies of dithiodiglycolamide
 compounds of palladium(ii).
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11867
_journal_page_last               11876
_journal_paper_doi               10.1039/c4dt03814b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C36 H72 N4 O4 Pd S4, 2(N O3)'
_chemical_formula_sum            'C36 H72 N6 O10 Pd S4'
_chemical_formula_weight         983.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-18
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2014-06-24 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                107.383(9)
_cell_angle_beta                 90.550(8)
_cell_angle_gamma                90.063(8)
_cell_formula_units_Z            1
_cell_length_a                   7.3801(7)
_cell_length_b                   11.9176(13)
_cell_length_c                   14.8102(14)
_cell_measurement_reflns_used    2926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.8110
_cell_measurement_theta_min      3.8740
_cell_volume                     1243.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3200
_diffrn_measured_fraction_theta_full 0.9835
_diffrn_measured_fraction_theta_max 0.9461
_diffrn_measurement_details
;
  1 omega  -16.00   28.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 44

  2 omega   31.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -180.0000 37

  3 omega  -47.00   10.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -180.0000 57

  4 omega -155.00   30.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -30.0000  -60.0000 185

  5 omega -100.00  -37.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  126.0000 -180.0000 63

  6 omega -157.00 -122.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000   30.0000 35

  7 omega -155.00  -99.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000  -30.0000 56

  8 omega -132.00 -100.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000    0.0000 32

  9 omega   97.00  154.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289   77.0000  -30.0000 57

 10 omega   -1.00   68.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289  -30.0000 -180.0000 69

 11 omega  119.00  149.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289  126.0000  150.0000 30

 12 omega    7.00   62.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289   77.0000  -30.0000 55

 13 omega   12.00   71.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000    0.0000 59

 14 omega   25.00   71.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000  -60.0000 46

 15 omega   42.00  102.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -116.0000  -86.0000 60

 16 omega   10.00   69.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -25.0000 -150.0000 59

 17 omega   34.00   62.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000 -180.0000 28

 18 omega   15.00   65.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000  -90.0000 50

 19 omega   24.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000  -90.0000 85

 20 omega  122.00  151.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000  120.0000 29

 21 omega   58.00  154.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   50.0000 -150.0000 96

 22 omega   47.00   72.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000  120.0000 25

 23 omega  113.00  141.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -92.0000   30.0000 28

 24 omega   43.00   77.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000  120.0000 34

 25 omega   81.00  110.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000 -180.0000 29

 26 omega   18.00   69.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000   60.0000 51

 27 omega   39.00  108.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -92.0000   30.0000 69

 28 omega   62.00  158.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000   90.0000 96

 29 omega    9.00  151.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -12.0000   30.0000 142
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0238277000
_diffrn_orient_matrix_UB_12      -0.0567655000
_diffrn_orient_matrix_UB_13      0.0801507000
_diffrn_orient_matrix_UB_21      -0.0295570000
_diffrn_orient_matrix_UB_22      -0.1225283000
_diffrn_orient_matrix_UB_23      -0.0715384000
_diffrn_orient_matrix_UB_31      0.2052774000
_diffrn_orient_matrix_UB_32      -0.0104962000
_diffrn_orient_matrix_UB_33      -0.0184463000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_laue_measured_fraction_full 0.981
_diffrn_reflns_laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6637
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.27
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.023
_exptl_absorpt_correction_T_max  0.377
_exptl_absorpt_correction_T_min  0.057
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.5482
_exptl_crystal_size_mid          0.2102
_exptl_crystal_size_min          0.0938
_refine_diff_density_max         1.244
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0010(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1888P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3983
_reflns_number_total             4525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03814b3.cif
_cod_data_source_block           exp_29
_cod_depositor_comments
'Adding full bibliography for 7035386--7035388.cif.'
_cod_database_code               7035388
_chemical_oxdiff_formula         c18h36ns24o8pdcl
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C41(H41), C24(H24), C51(H51)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C13(H13A,H13B), C21(H21A,H21B), C12(H12A,H12B)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
;
_shelxl_version_number           2013-4