#------------------------------------------------------------------------------
#$Date: 2017-09-08 05:44:08 +0300 (Fri, 08 Sep 2017) $
#$Revision: 200362 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/41/7044140.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_7044140
loop_
_publ_author_name
'Singh, Ajai kumar'
'Dubey, Pooja'
'Gupta, Sonu'
_publ_section_title
;
 Trinuclear complexes of palladium(II) with chalcogenated N-heterocyclic
 carbenes: catalysis of selective nitrile-primary amide interconversion
 and Sonogashira coupling
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02592K
_journal_year                    2017
_chemical_formula_moiety         'C36 H38 Cl6 N6 Pd3 S2, 2(C2 H3 N)'
_chemical_formula_sum            'C40 H44 Cl6 N8 Pd3 S2'
_chemical_formula_weight         1232.85
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1n441z
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-19 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.804(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.797(3)
_cell_length_b                   10.941(3)
_cell_length_c                   19.404(6)
_cell_measurement_reflns_used    2116
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.40
_cell_measurement_theta_min      2.14
_cell_volume                     2481.3(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23279
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.912
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014/7)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224.0
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0707P)²+1.9086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3091
_reflns_number_total             4353
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02592k2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group_crystal_system' value 'Monoclinic' changed to
'monoclinic' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7044140
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 1.0000 0.5000 0.5000 0.0363(2) Uani 1 2 d S . P
Pd2 Pd 0.70553(5) 0.12694(6) 0.68257(3) 0.0540(2) Uani 1 1 d . . .
S1 S 0.84485(16) 0.37898(16) 0.51684(10) 0.0429(4) Uani 1 1 d . . .
Cl3 Cl 0.8000(2) 0.1275(2) 0.79349(12) 0.0764(7) Uani 1 1 d . . .
Cl2 Cl 0.6237(2) 0.1252(2) 0.56814(12) 0.0776(7) Uani 1 1 d . . .
Cl1 Cl 1.0020(2) 0.38979(18) 0.40054(11) 0.0629(6) Uani 1 1 d . . .
N1 N 0.9254(5) 0.1991(5) 0.6387(3) 0.0461(15) Uani 1 1 d . . .
N2 N 0.8980(6) 0.0037(6) 0.6317(3) 0.0576(17) Uani 1 1 d . . .
C9 C 0.8554(7) 0.1096(7) 0.6498(4) 0.051(2) Uani 1 1 d . . .
C15 C 1.0011(7) 0.0265(7) 0.6071(4) 0.052(2) Uani 1 1 d . . .
C1 C 0.7280(6) 0.4614(7) 0.4718(5) 0.053(2) Uani 1 1 d . . .
C7 C 0.8155(7) 0.3896(6) 0.6061(4) 0.050(2) Uani 1 1 d . . .
H7A H 0.8102 0.4750 0.6189 0.060 Uiso 1 1 calc R U .
H7B H 0.7426 0.3512 0.6100 0.060 Uiso 1 1 calc R U .
C10 C 1.0190(6) 0.1507(7) 0.6113(4) 0.0468(18) Uani 1 1 d . . .
N3 N 0.5455(7) 0.1454(7) 0.7143(4) 0.077(2) Uani 1 1 d . . .
C13 C 1.1694(9) 0.0004(10) 0.5581(5) 0.081(3) Uani 1 1 d . . .
H13 H 1.2210 -0.0491 0.5388 0.097 Uiso 1 1 calc R U .
C8 C 0.9085(7) 0.3282(7) 0.6555(4) 0.054(2) Uani 1 1 d . . .
H8A H 0.9798 0.3719 0.6545 0.065 Uiso 1 1 calc R U .
H8B H 0.8891 0.3337 0.7024 0.065 Uiso 1 1 calc R U .
C12 C 1.1889(8) 0.1244(10) 0.5626(5) 0.075(3) Uani 1 1 d . . .
H12 H 1.2542 0.1559 0.5472 0.090 Uiso 1 1 calc R U .
C11 C 1.1146(7) 0.2036(8) 0.5892(4) 0.062(2) Uani 1 1 d . . .
H11 H 1.1280 0.2873 0.5921 0.074 Uiso 1 1 calc R U .
C14 C 1.0775(7) -0.0513(8) 0.5808(5) 0.064(2) Uani 1 1 d . . .
H14 H 1.0659 -0.1353 0.5789 0.077 Uiso 1 1 calc R U .
C16 C 0.8464(9) -0.1168(7) 0.6367(5) 0.080(3) Uani 1 1 d . . .
H16A H 0.8480 -0.1383 0.6848 0.120 Uiso 1 1 calc R U .
H16B H 0.8888 -0.1762 0.6142 0.120 Uiso 1 1 calc R U .
H16C H 0.7686 -0.1150 0.6144 0.120 Uiso 1 1 calc R U .
C6 C 0.6775(8) 0.5614(9) 0.4977(6) 0.086(3) Uani 1 1 d . . .
H5 H 0.7042 0.5894 0.5422 0.103 Uiso 1 1 calc R U .
C2 C 0.6878(9) 0.4222(11) 0.4069(6) 0.094(3) Uani 1 1 d . . .
H1 H 0.7215 0.3552 0.3884 0.113 Uiso 1 1 calc R U .
C17 C 0.4555(10) 0.1558(11) 0.7272(5) 0.091(4) Uani 1 1 d . . .
C4 C 0.5476(10) 0.5786(14) 0.3954(8) 0.106(5) Uani 1 1 d . . .
H3 H 0.4849 0.6173 0.3703 0.127 Uiso 1 1 calc R U .
C5 C 0.5896(11) 0.6195(11) 0.4594(8) 0.106(4) Uani 1 1 d . . .
H4 H 0.5577 0.6884 0.4773 0.127 Uiso 1 1 calc R U .
C3 C 0.5959(11) 0.4818(14) 0.3675(7) 0.120(5) Uani 1 1 d . . .
H2 H 0.5685 0.4551 0.3228 0.144 Uiso 1 1 calc R U .
C18 C 0.3380(9) 0.1684(17) 0.7420(6) 0.166(7) Uani 1 1 d . . .
H18A H 0.3211 0.2533 0.7480 0.249 Uiso 1 1 calc R U .
H18B H 0.3292 0.1246 0.7839 0.249 Uiso 1 1 calc R U .
H18C H 0.2864 0.1357 0.7040 0.249 Uiso 1 1 calc R U .
C20 C 0.5852(13) 0.1508(15) 0.3252(8) 0.129(6) Uani 1 1 d . . .
C19 C 0.5154(13) 0.1530(14) 0.3818(7) 0.144(6) Uani 1 1 d . . .
H19A H 0.4492 0.2033 0.3688 0.216 Uiso 1 1 calc R U .
H19B H 0.5594 0.1857 0.4229 0.216 Uiso 1 1 calc R U .
H19C H 0.4915 0.0714 0.3910 0.216 Uiso 1 1 calc R U .
N7 N 0.6386(14) 0.1501(15) 0.2799(8) 0.176(6) Uani 1 1 d . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
I I -0.4742 1.8119 '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
Cl1 Pd1 Cl1 180.0 3_766 .
Cl1 Pd1 S1 94.80(7) 3_766 .
Cl1 Pd1 S1 85.20(7) . .
Cl1 Pd1 S1 85.20(7) 3_766 3_766
Cl1 Pd1 S1 94.80(7) . 3_766
S1 Pd1 S1 180.0 . 3_766
C9 Pd2 N3 178.4(3) . .
C9 Pd2 Cl3 87.7(2) . .
N3 Pd2 Cl3 93.9(2) . .
C9 Pd2 Cl2 88.0(2) . .
N3 Pd2 Cl2 90.4(2) . .
Cl3 Pd2 Cl2 175.70(9) . .
C1 S1 C7 101.6(4) . .
C1 S1 Pd1 102.5(2) . .
C7 S1 Pd1 110.7(3) . .
C9 N1 C10 109.1(6) . .
C9 N1 C8 124.8(6) . .
C10 N1 C8 126.1(6) . .
C9 N2 C15 108.3(7) . .
C9 N2 C16 126.4(7) . .
C15 N2 C16 125.3(7) . .
N1 C9 N2 109.6(7) . .
N1 C9 Pd2 126.3(6) . .
N2 C9 Pd2 123.9(6) . .
C10 C15 C14 121.7(8) . .
C10 C15 N2 107.0(7) . .
C14 C15 N2 131.3(8) . .
C2 C1 C6 118.6(9) . .
C2 C1 S1 116.6(7) . .
C6 C1 S1 124.8(7) . .
C8 C7 S1 111.1(5) . .
C15 C10 C11 121.3(7) . .
C15 C10 N1 105.9(6) . .
C11 C10 N1 132.8(7) . .
C17 N3 Pd2 175.7(8) . .
C14 C13 C12 121.8(9) . .
N1 C8 C7 113.3(7) . .
C13 C12 C11 122.2(9) . .
C12 C11 C10 116.0(8) . .
C13 C14 C15 117.1(9) . .
C5 C6 C1 120.8(11) . .
C1 C2 C3 120.6(11) . .
N3 C17 C18 178.4(12) . .
C5 C4 C3 120.5(12) . .
C4 C5 C6 120.6(12) . .
C4 C3 C2 118.9(13) . .
N7 C20 C19 179(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl1 2.2784(19) 3_766
Pd1 Cl1 2.2784(19) .
Pd1 S1 2.3179(19) .
Pd1 S1 2.3179(19) 3_766
Pd2 C9 1.968(7) .
Pd2 N3 2.073(8) .
Pd2 Cl3 2.285(2) .
Pd2 Cl2 2.298(2) .
S1 C1 1.775(8) .
S1 C7 1.816(7) .
N1 C9 1.317(9) .
N1 C10 1.393(9) .
N1 C8 1.470(9) .
N2 C9 1.329(9) .
N2 C15 1.387(9) .
N2 C16 1.461(10) .
C15 C10 1.376(10) .
C15 C14 1.387(11) .
C1 C2 1.353(13) .
C1 C6 1.373(12) .
C7 C8 1.512(10) .
C10 C11 1.386(11) .
N3 C17 1.130(11) .
C13 C14 1.349(12) .
C13 C12 1.377(12) .
C12 C11 1.381(12) .
C6 C5 1.350(14) .
C2 C3 1.400(15) .
C17 C18 1.460(14) .
C4 C5 1.350(17) .
C4 C3 1.350(17) .
C20 N7 1.149(19) .
C20 C19 1.46(2) .
