#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316452.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_4316452
loop_
_publ_author_name
'José Vicente'
'María-Teresa Chicote'
'Eloísa Martínez-Viviente'
'Antonio-Jesús Martínez-Martínez'
'Nicolás Sánchez-Moya'
'Peter G. Jones'
_publ_section_title
;
 2-(Aminomethyl)phenyl Complexes of Au(III), Mixed Au(III)/Ag(I), and
 Pd(II) with the 2,2-Diacetyl-1,1-Ethylenedithiolato Ligand: Dancing of
 Palladacycles around a Juggler Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8099
_journal_page_last               8111
_journal_paper_doi               10.1021/ic101188z
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C25 H32 Cl2 N2 O2 Pd2 S2'
_chemical_formula_weight         740.35
_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
_cell_angle_alpha                101.931(3)
_cell_angle_beta                 92.169(3)
_cell_angle_gamma                108.554(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3598(12)
_cell_length_b                   11.6148(12)
_cell_length_c                   11.6365(12)
_cell_measurement_reflns_used    6140
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1415.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω-scan
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16952
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         8208
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0307P)²+0.1137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0543
_reflns_number_gt                7292
_reflns_number_total             8208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101188z_si_002_2.cif
_cod_data_source_block           oldnic
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (63 times).

'_geom_bond_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (37
times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4316452
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
Pd1 Pd 0.172872(10) 0.217652(10) 0.041381(9) 0.01614(3) Uani 1 1 d . . .
Pd2 Pd 0.257703(10) 0.382951(10) 0.425568(9) 0.01621(3) Uani 1 1 d . . .
S1 S 0.28718(4) 0.33468(3) 0.23422(3) 0.01847(7) Uani 1 1 d . . .
S2 S 0.35201(4) 0.16856(4) 0.05605(3) 0.02304(8) Uani 1 1 d . . .
N1 N -0.00331(12) 0.24086(12) 0.03382(12) 0.0193(2) Uani 1 1 d . . .
N2 N 0.24474(12) 0.44444(12) 0.60655(11) 0.0194(2) Uani 1 1 d . . .
O1 O 0.33811(11) 0.25621(11) 0.46770(10) 0.0255(2) Uani 1 1 d . . .
O2 O 0.41596(18) -0.03627(14) 0.24078(17) 0.0561(5) Uani 1 1 d . . .
C1 C 0.35852(14) 0.22032(14) 0.20903(14) 0.0196(3) Uani 1 1 d . . .
C2 C 0.40793(15) 0.17002(14) 0.28871(15) 0.0226(3) Uani 1 1 d . . .
C3 C 0.39790(16) 0.19188(15) 0.41310(16) 0.0256(3) Uani 1 1 d . . .
C4 C 0.4622(3) 0.1344(2) 0.4885(2) 0.0509(6) Uani 1 1 d . . .
H4A H 0.4597 0.1699 0.5721 0.061 Uiso 1 1 calc R . .
H4B H 0.5493 0.1519 0.4720 0.061 Uiso 1 1 calc R . .
H4C H 0.4194 0.0440 0.4708 0.061 Uiso 1 1 calc R . .
C5 C 0.46556(19) 0.07242(18) 0.23742(17) 0.0330(4) Uani 1 1 d . . .
C6 C 0.5871(2) 0.1148(2) 0.1871(2) 0.0427(5) Uani 1 1 d . . .
H6A H 0.6562 0.1437 0.2506 0.051 Uiso 1 1 calc R . .
H6B H 0.5890 0.1832 0.1494 0.051 Uiso 1 1 calc R . .
H6C H 0.5958 0.0450 0.1283 0.051 Uiso 1 1 calc R . .
C11 C 0.10962(15) 0.11801(14) -0.12271(13) 0.0196(3) Uani 1 1 d . . .
C12 C -0.02011(15) 0.08714(14) -0.14947(14) 0.0223(3) Uani 1 1 d . . .
C13 C -0.07905(17) 0.01840(16) -0.26157(15) 0.0296(4) Uani 1 1 d . . .
H13 H -0.1667 -0.0020 -0.2789 0.036 Uiso 1 1 calc R . .
C14 C -0.00927(19) -0.02028(17) -0.34789(15) 0.0333(4) Uani 1 1 d . . .
H14 H -0.0494 -0.0685 -0.4237 0.040 Uiso 1 1 calc R . .
C15 C 0.11888(19) 0.01181(16) -0.32278(15) 0.0299(4) Uani 1 1 d . . .
H15 H 0.1666 -0.0130 -0.3823 0.036 Uiso 1 1 calc R . .
C16 C 0.17864(17) 0.08026(15) -0.21084(14) 0.0242(3) Uani 1 1 d . . .
H16 H 0.2665 0.1012 -0.1946 0.029 Uiso 1 1 calc R . .
C17 C -0.08997(15) 0.12675(15) -0.05051(15) 0.0234(3) Uani 1 1 d . . .
H17A H -0.1622 0.1453 -0.0824 0.028 Uiso 1 1 calc R . .
H17B H -0.1218 0.0586 -0.0089 0.028 Uiso 1 1 calc R . .
C18 C -0.05107(16) 0.25324(17) 0.15067(15) 0.0285(3) Uani 1 1 d . . .
H18A H 0.0031 0.3303 0.2045 0.034 Uiso 1 1 calc R . .
H18B H -0.0517 0.1816 0.1830 0.034 Uiso 1 1 calc R . .
H18C H -0.1362 0.2560 0.1420 0.034 Uiso 1 1 calc R . .
C19 C 0.00390(17) 0.35246(16) -0.01156(17) 0.0287(4) Uani 1 1 d . . .
H19A H -0.0785 0.3626 -0.0147 0.034 Uiso 1 1 calc R . .
H19B H 0.0305 0.3423 -0.0911 0.034 Uiso 1 1 calc R . .
H19C H 0.0644 0.4264 0.0410 0.034 Uiso 1 1 calc R . .
C21 C 0.20231(14) 0.52594(14) 0.41154(13) 0.0183(3) Uani 1 1 d . . .
C22 C 0.16946(15) 0.58482(14) 0.51804(13) 0.0200(3) Uani 1 1 d . . .
C23 C 0.14374(17) 0.69586(15) 0.52727(14) 0.0253(3) Uani 1 1 d . . .
H23 H 0.1220 0.7345 0.5997 0.030 Uiso 1 1 calc R . .
C24 C 0.14979(17) 0.75029(15) 0.43103(15) 0.0265(3) Uani 1 1 d . . .
H24 H 0.1332 0.8265 0.4378 0.032 Uiso 1 1 calc R . .
C25 C 0.18006(18) 0.69298(16) 0.32510(15) 0.0271(3) Uani 1 1 d . . .
H25 H 0.1828 0.7292 0.2587 0.032 Uiso 1 1 calc R . .
C26 C 0.20671(16) 0.58183(15) 0.31552(14) 0.0227(3) Uani 1 1 d . . .
H26 H 0.2281 0.5438 0.2426 0.027 Uiso 1 1 calc R . .
C27 C 0.15933(16) 0.51975(16) 0.61795(14) 0.0239(3) Uani 1 1 d . . .
H27A H 0.1823 0.5821 0.6944 0.029 Uiso 1 1 calc R . .
H27B H 0.0722 0.4646 0.6159 0.029 Uiso 1 1 calc R . .
C28 C 0.37395(16) 0.52551(17) 0.65685(15) 0.0276(3) Uani 1 1 d . . .
H28A H 0.3759 0.5566 0.7421 0.033 Uiso 1 1 calc R . .
H28B H 0.4003 0.5962 0.6190 0.033 Uiso 1 1 calc R . .
H28C H 0.4308 0.4771 0.6426 0.033 Uiso 1 1 calc R . .
C29 C 0.20242(16) 0.34302(16) 0.67012(15) 0.0260(3) Uani 1 1 d . . .
H29A H 0.2017 0.3791 0.7539 0.031 Uiso 1 1 calc R . .
H29B H 0.2595 0.2946 0.6623 0.031 Uiso 1 1 calc R . .
H29C H 0.1180 0.2882 0.6362 0.031 Uiso 1 1 calc R . .
C99 C 0.5550(4) 0.4328(4) -0.0454(4) 0.0390(11) Uani 0.508(5) 1 d PDU A 1
H99A H 0.5768 0.5209 -0.0509 0.047 Uiso 0.508(5) 1 calc PR A 1
H99B H 0.4923 0.4181 0.0115 0.047 Uiso 0.508(5) 1 calc PR A 1
Cl1 Cl 0.6880(4) 0.4093(5) 0.0087(4) 0.0560(12) Uani 0.508(5) 1 d PDU A 1
Cl2 Cl 0.4883(5) 0.3362(5) -0.1837(4) 0.0445(8) Uani 0.508(5) 1 d PDU A 1
C99' C 0.5955(4) 0.2916(3) -0.1055(3) 0.0327(10) Uani 0.492(5) 1 d PDU A 2
H99C H 0.6532 0.2616 -0.1554 0.039 Uiso 0.492(5) 1 calc PR A 2
H99D H 0.5477 0.2229 -0.0701 0.039 Uiso 0.492(5) 1 calc PR A 2
Cl1' Cl 0.6841(4) 0.4202(5) 0.0092(4) 0.0475(10) Uani 0.492(5) 1 d PDU A 2
Cl2' Cl 0.4965(6) 0.3265(6) -0.1904(5) 0.0592(11) Uani 0.492(5) 1 d PDU A 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'
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C11 Pd1 N1 82.35(6) . . y
C11 Pd1 S2 96.83(5) . . y
N1 Pd1 S2 172.62(4) . . y
C11 Pd1 S1 169.38(5) . . y
N1 Pd1 S1 108.16(4) . . y
S2 Pd1 S1 72.940(14) . . y
C21 Pd2 O1 169.22(5) . . y
C21 Pd2 N2 83.06(6) . . y
O1 Pd2 N2 89.11(5) . . y
C21 Pd2 S1 94.79(4) . . y
O1 Pd2 S1 92.33(3) . . y
N2 Pd2 S1 174.42(4) . . y
C1 S1 Pd2 110.63(6) . . y
C1 S1 Pd1 82.34(5) . . y
Pd2 S1 Pd1 141.128(19) . . y
C1 S2 Pd1 86.95(5) . . y
C19 N1 C18 109.22(13) . . y
C19 N1 C17 109.46(13) . . y
C18 N1 C17 109.55(12) . . y
C19 N1 Pd1 110.00(10) . . y
C18 N1 Pd1 112.11(10) . . y
C17 N1 Pd1 106.44(9) . . y
C29 N2 C28 109.07(13) . . y
C29 N2 C27 110.33(12) . . y
C28 N2 C27 109.98(13) . . y
C29 N2 Pd2 114.38(10) . . y
C28 N2 Pd2 104.60(10) . . y
C27 N2 Pd2 108.29(9) . . y
C3 O1 Pd2 134.33(11) . . y
C2 C1 S1 129.79(12) . . y
C2 C1 S2 122.75(12) . . y
S1 C1 S2 107.40(9) . . y
C1 C2 C3 125.97(14) . . y
C1 C2 C5 116.57(15) . . y
C3 C2 C5 117.11(14) . . y
O1 C3 C2 125.71(15) . . y
O1 C3 C4 114.99(16) . . y
C2 C3 C4 119.30(16) . . y
O2 C5 C6 121.44(17) . . y
O2 C5 C2 120.60(18) . . y
C6 C5 C2 117.92(17) . . y
C16 C11 C12 118.80(14) . . y
C16 C11 Pd1 127.75(12) . . y
C12 C11 Pd1 113.43(11) . . y
C13 C12 C11 120.58(16) . . y
C13 C12 C17 122.89(15) . . y
C11 C12 C17 116.47(14) . . y
C14 C13 C12 119.94(17) . . y
C15 C14 C13 119.76(16) . . y
C14 C15 C16 120.71(16) . . y
C15 C16 C11 120.19(17) . . y
N1 C17 C12 108.86(13) . . y
C26 C21 C22 117.79(13) . . y
C26 C21 Pd2 128.02(11) . . y
C22 C21 Pd2 113.70(11) . . y
C23 C22 C21 120.90(14) . . y
C23 C22 C27 122.31(14) . . y
C21 C22 C27 116.76(13) . . y
C24 C23 C22 120.30(14) . . y
C25 C24 C23 119.70(15) . . y
C24 C25 C26 120.24(15) . . y
C21 C26 C25 121.05(14) . . y
N2 C27 C22 109.36(12) . . y
Cl1 C99 Cl2 113.6(3) . . ?
Cl2' C99' Cl1' 113.0(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C11 1.9887(15) . y
Pd1 N1 2.1037(13) . y
Pd1 S2 2.2908(4) . y
Pd1 S1 2.4422(4) . y
Pd2 C21 1.9875(15) . y
Pd2 O1 2.0886(11) . y
Pd2 N2 2.1061(13) . y
Pd2 S1 2.2459(4) . y
S1 C1 1.7462(15) . y
S2 C1 1.7479(16) . y
N1 C19 1.478(2) . y
N1 C18 1.479(2) . y
N1 C17 1.499(2) . y
N2 C29 1.481(2) . y
N2 C28 1.487(2) . y
N2 C27 1.492(2) . y
O1 C3 1.258(2) . y
O2 C5 1.217(2) . y
C1 C2 1.382(2) . y
C2 C3 1.432(2) . y
C2 C5 1.514(2) . y
C3 C4 1.501(2) . y
C5 C6 1.497(3) . y
C11 C16 1.397(2) . y
C11 C12 1.407(2) . y
C12 C13 1.397(2) . y
C12 C17 1.500(2) . y
C13 C14 1.393(3) . y
C14 C15 1.386(3) . y
C15 C16 1.397(2) . y
C21 C26 1.398(2) . y
C21 C22 1.411(2) . y
C22 C23 1.395(2) . y
C22 C27 1.501(2) . y
C23 C24 1.389(2) . y
C24 C25 1.385(2) . y
C25 C26 1.401(2) . y
C99 Cl1 1.736(7) . ?
C99 Cl2 1.744(6) . ?
C99' Cl2' 1.666(6) . ?
C99' Cl1' 1.772(5) . ?
