#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:35:27 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179755 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/51/7005126.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_7005126
loop_
_publ_author_name
'Chang, Xiaohong'
'Kim, Mi-Young'
'Kim, Yong-Joo'
'Huh, Hyun Sue'
'Lee, Soon W.'
_publ_section_title
;
 Dinuclear palladium-azido complexes containing thiophene derivatives:
 reactivity toward organic isocyanides and isothiocyanates.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              792
_journal_page_last               801
_journal_paper_doi               10.1039/b616901e
_journal_year                    2007
_chemical_formula_sum            'C40 H62 Cl4 N4 P4 Pd2 S2'
_chemical_formula_weight         1141.54
_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                87.887(17)
_cell_angle_beta                 76.69(2)
_cell_angle_gamma                81.063(16)
_cell_formula_units_Z            1
_cell_length_a                   8.5056(17)
_cell_length_b                   12.325(2)
_cell_length_c                   13.107(4)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      5.02
_cell_volume                     1320.9(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4962
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.31
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.8289
_exptl_absorpt_correction_T_min  0.4721
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'yellow '
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'block '
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0620P)²+1.1307P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                3598
_reflns_number_total             4624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b616901e.txt
_cod_data_source_block           465
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7005126
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 0.67451(5) 0.67646(3) 0.80055(3) 0.04785(15) Uani 1 1 d . . .
P1 P 0.49329(19) 0.83311(11) 0.78454(11) 0.0591(4) Uani 1 1 d . . .
P2 P 0.83752(17) 0.51140(12) 0.81741(11) 0.0591(4) Uani 1 1 d . . .
S1 S 0.63647(16) 0.60225(11) 0.57226(10) 0.0537(3) Uani 1 1 d . . .
N1 N 0.7810(7) 0.7535(5) 0.8973(4) 0.0874(17) Uani 1 1 d . . .
N2 N 0.9117(7) 0.8002(5) 1.0307(4) 0.0816(16) Uani 1 1 d . . .
C1 C 0.5727(6) 0.5994(4) 0.7074(4) 0.0472(11) Uani 1 1 d . . .
C2 C 0.4546(6) 0.5345(4) 0.7318(4) 0.0564(13) Uani 1 1 d . . .
H2 H 0.4025 0.5220 0.8008 0.068 Uiso 1 1 calc R . .
C3 C 0.4155(7) 0.4874(4) 0.6469(4) 0.0566(13) Uani 1 1 d . . .
H3 H 0.3368 0.4413 0.6548 0.068 Uiso 1 1 calc R . .
C4 C 0.5034(6) 0.5155(4) 0.5524(4) 0.0455(11) Uani 1 1 d . . .
C5 C 0.8346(7) 0.7758(4) 0.9658(4) 0.0621(14) Uani 1 1 d . . .
C6 C 0.8597(7) 0.8197(4) 1.1377(4) 0.0578(13) Uani 1 1 d . . .
C7 C 0.7171(7) 0.7886(4) 1.2022(5) 0.0682(15) Uani 1 1 d . . .
C8 C 0.6884(10) 0.8062(6) 1.3116(6) 0.089(2) Uani 1 1 d . . .
H8 H 0.5957 0.7856 1.3561 0.107 Uiso 1 1 calc R . .
C9 C 0.7957(12) 0.8533(7) 1.3524(6) 0.101(2) Uani 1 1 d . . .
H9 H 0.7764 0.8628 1.4245 0.121 Uiso 1 1 calc R . .
C10 C 0.9299(10) 0.8862(5) 1.2893(6) 0.084(2) Uani 1 1 d . . .
H10 H 0.9993 0.9203 1.3185 0.101 Uiso 1 1 calc R . .
C11 C 0.9652(7) 0.8699(4) 1.1825(5) 0.0647(15) Uani 1 1 d . . .
C12 C 0.5964(9) 0.7400(6) 1.1585(7) 0.094(2) Uani 1 1 d . . .
H12A H 0.5454 0.7941 1.1169 0.142 Uiso 1 1 calc R . .
H12B H 0.5146 0.7169 1.2150 0.142 Uiso 1 1 calc R . .
H12C H 0.6515 0.6779 1.1156 0.142 Uiso 1 1 calc R . .
C13 C 1.1142(8) 0.9069(6) 1.1151(6) 0.091(2) Uani 1 1 d . . .
H13A H 1.1655 0.9460 1.1571 0.137 Uiso 1 1 calc R . .
H13B H 1.0838 0.9543 1.0608 0.137 Uiso 1 1 calc R . .
H13C H 1.1891 0.8441 1.0840 0.137 Uiso 1 1 calc R . .
C14 C 0.5420(12) 0.8993(7) 0.6610(6) 0.128(3) Uani 1 1 d . . .
H14A H 0.5507 0.8479 0.6060 0.191 Uiso 1 1 calc R . .
H14B H 0.6441 0.9262 0.6533 0.191 Uiso 1 1 calc R . .
H14C H 0.4574 0.9597 0.6570 0.191 Uiso 1 1 calc R . .
C15 C 0.2822(9) 0.8168(6) 0.7994(7) 0.104(3) Uani 1 1 d . . .
H15A H 0.2452 0.7807 0.8647 0.157 Uiso 1 1 calc R . .
H15B H 0.2719 0.7733 0.7427 0.157 Uiso 1 1 calc R . .
H15C H 0.2170 0.8877 0.7987 0.157 Uiso 1 1 calc R . .
C16 C 0.4798(9) 0.9368(5) 0.8819(6) 0.095(2) Uani 1 1 d . . .
H16A H 0.4517 0.9057 0.9508 0.143 Uiso 1 1 calc R . .
H16B H 0.3973 0.9972 0.8744 0.143 Uiso 1 1 calc R . .
H16C H 0.5833 0.9623 0.8723 0.143 Uiso 1 1 calc R . .
C17 C 0.9014(10) 0.4193(6) 0.7065(6) 0.113(3) Uani 1 1 d . . .
H17A H 0.8073 0.4067 0.6825 0.170 Uiso 1 1 calc R . .
H17B H 0.9561 0.3508 0.7270 0.170 Uiso 1 1 calc R . .
H17C H 0.9746 0.4516 0.6510 0.170 Uiso 1 1 calc R . .
C18 C 0.7380(9) 0.4290(6) 0.9238(7) 0.097(2) Uani 1 1 d . . .
H18A H 0.6998 0.4727 0.9863 0.145 Uiso 1 1 calc R . .
H18B H 0.8146 0.3669 0.9362 0.145 Uiso 1 1 calc R . .
H18C H 0.6470 0.4039 0.9051 0.145 Uiso 1 1 calc R . .
C19 C 1.0284(7) 0.5240(6) 0.8504(6) 0.0809(19) Uani 1 1 d . . .
H19A H 1.0079 0.5713 0.9101 0.121 Uiso 1 1 calc R . .
H19B H 1.0984 0.5546 0.7919 0.121 Uiso 1 1 calc R . .
H19C H 1.0806 0.4528 0.8667 0.121 Uiso 1 1 calc R . .
C20 C 0.1822(18) 0.7405(12) 0.5058(12) 0.211(8) Uani 1 1 d . . .
H20A H 0.2763 0.6938 0.5217 0.253 Uiso 1 1 calc R . .
H20B H 0.1607 0.7130 0.4428 0.253 Uiso 1 1 calc R . .
Cl1 Cl 0.0080(5) 0.7376(5) 0.6127(4) 0.240(2) Uani 1 1 d . . .
Cl2 Cl 0.2205(5) 0.8674(4) 0.4866(4) 0.2073(18) 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'
P P 0.1023 0.0942 '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
C1 Pd1 N1 179.1(2) . . ?
C1 Pd1 P2 87.75(14) . . ?
N1 Pd1 P2 91.37(16) . . ?
C1 Pd1 P1 88.50(14) . . ?
N1 Pd1 P1 92.37(16) . . ?
P2 Pd1 P1 175.11(6) . . ?
C14 P1 C15 103.7(5) . . ?
C14 P1 C16 105.8(4) . . ?
C15 P1 C16 102.2(4) . . ?
C14 P1 Pd1 113.5(3) . . ?
C15 P1 Pd1 116.8(3) . . ?
C16 P1 Pd1 113.5(2) . . ?
C19 P2 C17 102.6(4) . . ?
C19 P2 C18 103.7(3) . . ?
C17 P2 C18 104.4(4) . . ?
C19 P2 Pd1 114.7(2) . . ?
C17 P2 Pd1 118.4(2) . . ?
C18 P2 Pd1 111.5(2) . . ?
C1 S1 C4 94.1(2) . . ?
C5 N1 Pd1 164.3(6) . . ?
C5 N2 C6 130.3(6) . . ?
C2 C1 S1 107.6(3) . . ?
C2 C1 Pd1 130.1(4) . . ?
S1 C1 Pd1 122.2(3) . . ?
C1 C2 C3 116.1(5) . . ?
C4 C3 C2 113.6(5) . . ?
C3 C4 C4 129.7(6) . 2_666 ?
C3 C4 S1 108.7(3) . . ?
C4 C4 S1 121.6(5) 2_666 . ?
N1 C5 N2 171.9(7) . . ?
N2 C6 C11 115.3(5) . . ?
N2 C6 C7 125.0(5) . . ?
C11 C6 C7 119.6(5) . . ?
C6 C7 C8 118.1(6) . . ?
C6 C7 C12 122.0(6) . . ?
C8 C7 C12 119.9(6) . . ?
C9 C8 C7 120.5(7) . . ?
C10 C9 C8 121.0(7) . . ?
C9 C10 C11 121.1(7) . . ?
C10 C11 C6 119.7(6) . . ?
C10 C11 C13 119.8(6) . . ?
C6 C11 C13 120.5(5) . . ?
Cl2 C20 Cl1 109.4(6) . . ?
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 C1 1.992(4) . ?
Pd1 N1 2.053(5) . ?
Pd1 P2 2.3111(15) . ?
Pd1 P1 2.3113(15) . ?
P1 C14 1.777(8) . ?
P1 C15 1.803(7) . ?
P1 C16 1.812(6) . ?
P2 C19 1.804(6) . ?
P2 C17 1.807(6) . ?
P2 C18 1.820(8) . ?
S1 C1 1.730(5) . ?
S1 C4 1.739(4) . ?
N1 C5 1.155(6) . ?
N2 C5 1.258(6) . ?
N2 C6 1.387(7) . ?
C1 C2 1.354(7) . ?
C2 C3 1.401(6) . ?
C3 C4 1.355(7) . ?
C4 C4 1.455(9) 2_666 ?
C6 C11 1.405(7) . ?
C6 C7 1.408(8) . ?
C7 C8 1.417(10) . ?
C7 C12 1.493(9) . ?
C8 C9 1.366(11) . ?
C9 C10 1.355(11) . ?
C10 C11 1.378(9) . ?
C11 C13 1.493(9) . ?
C20 Cl2 1.645(15) . ?
C20 Cl1 1.794(17) . ?
