#------------------------------------------------------------------------------
#$Date: 2017-03-05 06:12:29 +0100 (dom 05 de mar de 2017) $
#$Revision: 193812 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/16/7041616.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_7041616
loop_
_publ_author_name
'Wang, Yu-Ting'
'Gao, Bin-Bin'
'Wang, Fan'
'Liu, Shi-Yuan'
'Yu, Hong'
'Zhang, Wen-Hua'
'Lang, Jian-Ping'
_publ_section_title
;
 Palladium(ii) and palladium(ii)-silver(i) complexes with N-heterocyclic
 carbene and zwitterionic thiolate mixed ligands: synthesis, structural
 characterization and catalytic properties.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1832
_journal_page_last               1839
_journal_paper_doi               10.1039/c6dt04599e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C30 H42 F6 N6 O6 Pd S4'
_chemical_formula_sum            'C30 H42 F6 N6 O6 Pd S4'
_chemical_formula_weight         931.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-12-29 deposited with the CCDC.
2017-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.772(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.4841(14)
_cell_length_b                   10.5395(9)
_cell_length_c                   11.6208(10)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.33
_cell_volume                     1911.5(3)
_computing_cell_refinement       'Bruker D8 Quest'
_computing_data_collection       'Bruker D8 Quest'
_computing_data_reduction        'Bruker D8 Quest'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33954
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         2.332
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0226P)²+1.3203P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4051
_reflns_number_total             4395
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04599e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7041612--7041617.cif.'
_cod_database_code               7041616
_publcif_datablock.id            {23a3bb45-7e1b-4ee6-907e-d843b5454ada}
_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.
;
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.0000 1.0000 0.5000 0.01449(5) Uani 1 2 d S . P
S1 S 0.07269(2) 1.19262(4) 0.52724(4) 0.02421(9) Uani 1 1 d . . .
S2 S 0.39348(2) 0.69112(3) 0.30503(3) 0.01874(8) Uani 1 1 d . . .
F1 F 0.36732(8) 0.72730(11) 0.51173(10) 0.0423(3) Uani 1 1 d . . .
F2 F 0.41781(7) 0.54305(11) 0.49536(10) 0.0398(3) Uani 1 1 d . . .
F3 F 0.28578(7) 0.58528(12) 0.39981(11) 0.0438(3) Uani 1 1 d . . .
O1 O 0.48033(7) 0.73418(13) 0.36061(11) 0.0327(3) Uani 1 1 d . . .
O2 O 0.38432(9) 0.58200(11) 0.22801(11) 0.0330(3) Uani 1 1 d . . .
O3 O 0.33181(8) 0.79062(11) 0.25862(11) 0.0291(3) Uani 1 1 d . . .
N1 N -0.12335(8) 1.13966(12) 0.60333(11) 0.0183(2) Uani 1 1 d . . .
N2 N -0.03974(8) 1.01764(12) 0.73595(12) 0.0208(3) Uani 1 1 d . . .
N3 N 0.36459(8) 1.16096(11) 0.31699(11) 0.0182(2) Uani 1 1 d . . .
C1 C -0.05652(9) 1.05969(13) 0.62096(13) 0.0165(3) Uani 1 1 d . . .
C2 C -0.09693(11) 1.06885(16) 0.78791(15) 0.0269(3) Uani 1 1 d . . .
H2 H -0.0985 1.0529 0.8676 0.032 Uiso 1 1 calc R U .
C3 C -0.14953(10) 1.14494(16) 0.70510(15) 0.0248(3) Uani 1 1 d . . .
H3 H -0.1958 1.1932 0.7142 0.030 Uiso 1 1 calc R U .
C4 C 0.02700(11) 0.92664(18) 0.79523(16) 0.0308(4) Uani 1 1 d . . .
H4A H 0.0399 0.8743 0.7336 0.046 Uiso 1 1 calc R U .
H4B H 0.0073 0.8722 0.8493 0.046 Uiso 1 1 calc R U .
H4C H 0.0788 0.9721 0.8428 0.046 Uiso 1 1 calc R U .
C5 C -0.16534(10) 1.20638(16) 0.48988(15) 0.0257(3) Uani 1 1 d . . .
H5A H -0.1334 1.1921 0.4331 0.039 Uiso 1 1 calc R U .
H5B H -0.1669 1.2975 0.5060 0.039 Uiso 1 1 calc R U .
H5C H -0.2240 1.1745 0.4542 0.039 Uiso 1 1 calc R U .
C6 C 0.15821(9) 1.17981(14) 0.46700(14) 0.0200(3) Uani 1 1 d . . .
C7 C 0.22870(9) 1.10184(14) 0.51932(13) 0.0199(3) Uani 1 1 d . . .
H7 H 0.2304 1.0526 0.5886 0.024 Uiso 1 1 calc R U .
C8 C 0.29673(9) 1.09388(14) 0.47317(13) 0.0188(3) Uani 1 1 d . . .
H8 H 0.3440 1.0397 0.5101 0.023 Uiso 1 1 calc R U .
C9 C 0.29434(9) 1.16595(13) 0.37295(13) 0.0179(3) Uani 1 1 d . . .
C10 C 0.22523(10) 1.24459(15) 0.31919(15) 0.0247(3) Uani 1 1 d . . .
H10 H 0.2239 1.2941 0.2503 0.030 Uiso 1 1 calc R U .
C11 C 0.15790(10) 1.25102(16) 0.36604(15) 0.0252(3) Uani 1 1 d . . .
H11 H 0.1107 1.3051 0.3285 0.030 Uiso 1 1 calc R U .
C12 C 0.43698(10) 1.07614(15) 0.38517(15) 0.0238(3) Uani 1 1 d . . .
H12A H 0.4156 0.9894 0.3857 0.036 Uiso 1 1 calc R U .
H12B H 0.4615 1.1066 0.4689 0.036 Uiso 1 1 calc R U .
H12C H 0.4812 1.0769 0.3455 0.036 Uiso 1 1 calc R U .
C13 C 0.33029(11) 1.11159(16) 0.18884(14) 0.0259(3) Uani 1 1 d . . .
H13A H 0.3101 1.0243 0.1899 0.039 Uiso 1 1 calc R U .
H13B H 0.3759 1.1132 0.1517 0.039 Uiso 1 1 calc R U .
H13C H 0.2826 1.1652 0.1416 0.039 Uiso 1 1 calc R U .
C14 C 0.40083(10) 1.29250(14) 0.31677(16) 0.0245(3) Uani 1 1 d . . .
H14A H 0.4459 1.2899 0.2787 0.037 Uiso 1 1 calc R U .
H14B H 0.4250 1.3229 0.4006 0.037 Uiso 1 1 calc R U .
H14C H 0.3551 1.3500 0.2709 0.037 Uiso 1 1 calc R U .
C15 C 0.36506(10) 0.63316(16) 0.43469(15) 0.0257(3) 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pd Pd -0.9988 1.0072 '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
C1 Pd1 C1 180.00(9) 3_576 .
C1 Pd1 S1 91.93(4) 3_576 .
C1 Pd1 S1 88.07(4) . .
C1 Pd1 S1 88.07(4) 3_576 3_576
C1 Pd1 S1 91.93(4) . 3_576
S1 Pd1 S1 180.00(2) . 3_576
C6 S1 Pd1 108.70(5) . .
O2 S2 O3 115.49(8) . .
O2 S2 O1 114.95(8) . .
O3 S2 O1 114.74(8) . .
O2 S2 C15 104.10(8) . .
O3 S2 C15 102.45(7) . .
O1 S2 C15 102.57(8) . .
C1 N1 C3 111.04(13) . .
C1 N1 C5 124.45(12) . .
C3 N1 C5 124.44(13) . .
C1 N2 C2 110.67(13) . .
C1 N2 C4 124.63(13) . .
C2 N2 C4 124.65(14) . .
C12 N3 C9 112.73(11) . .
C12 N3 C13 107.38(12) . .
C9 N3 C13 110.15(11) . .
C12 N3 C14 107.49(12) . .
C9 N3 C14 109.24(11) . .
C13 N3 C14 109.78(12) . .
N1 C1 N2 104.64(12) . .
N1 C1 Pd1 128.72(11) . .
N2 C1 Pd1 126.38(11) . .
C3 C2 N2 107.19(14) . .
C3 C2 H2 126.4 . .
N2 C2 H2 126.4 . .
C2 C3 N1 106.43(13) . .
C2 C3 H3 126.8 . .
N1 C3 H3 126.8 . .
N2 C4 H4A 109.5 . .
N2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N1 C5 H5A 109.5 . .
N1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
N1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C11 C6 C7 117.54(13) . .
C11 C6 S1 120.35(12) . .
C7 C6 S1 122.08(12) . .
C8 C7 C6 121.96(14) . .
C8 C7 H7 119.0 . .
C6 C7 H7 119.0 . .
C9 C8 C7 118.94(14) . .
C9 C8 H8 120.5 . .
C7 C8 H8 120.5 . .
C8 C9 C10 120.40(13) . .
C8 C9 N3 122.00(13) . .
C10 C9 N3 117.59(13) . .
C9 C10 C11 119.90(14) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C10 C11 C6 121.25(14) . .
C10 C11 H11 119.4 . .
C6 C11 H11 119.4 . .
N3 C12 H12A 109.5 . .
N3 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N3 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N3 C13 H13A 109.5 . .
N3 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N3 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N3 C14 H14A 109.5 . .
N3 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N3 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
F2 C15 F1 107.75(14) . .
F2 C15 F3 107.49(14) . .
F1 C15 F3 107.40(13) . .
F2 C15 S2 112.37(11) . .
F1 C15 S2 110.36(11) . .
F3 C15 S2 111.25(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 2.0205(14) 3_576
Pd1 C1 2.0206(14) .
Pd1 S1 2.3266(4) .
Pd1 S1 2.3267(4) 3_576
S1 C6 1.7694(15) .
S2 O2 1.4351(12) .
S2 O3 1.4392(12) .
S2 O1 1.4413(12) .
S2 C15 1.8214(16) .
F1 C15 1.3289(19) .
F2 C15 1.3268(19) .
F3 C15 1.3363(19) .
N1 C1 1.3493(18) .
N1 C3 1.3844(19) .
N1 C5 1.458(2) .
N2 C1 1.3493(19) .
N2 C2 1.3824(19) .
N2 C4 1.455(2) .
N3 C12 1.4975(19) .
N3 C9 1.5004(18) .
N3 C13 1.505(2) .
N3 C14 1.5100(18) .
C2 C3 1.336(2) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C11 1.391(2) .
C6 C7 1.393(2) .
C7 C8 1.393(2) .
C7 H7 0.9500 .
C8 C9 1.380(2) .
C8 H8 0.9500 .
C9 C10 1.385(2) .
C10 C11 1.386(2) .
C10 H10 0.9500 .
C11 H11 0.9500 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
