#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:29:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178784 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/38/4103836.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_4103836
loop_
_publ_author_name
'Vivian Wing-Wah Yam'
'Jason Ka-Wai Lee'
'Chi-Chiu Ko'
'Nianyong Zhu'
_publ_section_title
;
 Photochromic Diarylethene-Containing Ionic Liquids and N-Heterocyclic
 Carbenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              912
_journal_page_last               913
_journal_paper_doi               10.1021/ja808791e
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C34 H40 I2 N4 Pd S4'
_chemical_formula_sum            'C34 H40 I2 N4 Pd S4'
_chemical_formula_weight         993.14
_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                103.03(3)
_cell_angle_beta                 91.32(3)
_cell_angle_gamma                103.46(3)
_cell_formula_units_Z            1
_cell_length_a                   7.9510(16)
_cell_length_b                   11.154(2)
_cell_length_c                   11.492(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    263(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     962.6(4)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      263(2)
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5372
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.331
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    ride-on
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0356P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2455
_reflns_number_total             3068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808791e_si_006.cif
_cod_data_source_block           complex_5
_cod_original_cell_volume        962.6(3)
_cod_database_code               4103836
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
Pd1 Pd 0.0000 0.0000 0.0000 0.02432(15) Uani 1 2 d S
I1 I -0.25992(4) -0.11167(3) -0.15816(3) 0.04453(15) Uani 1 1 d .
S1 S 0.31630(19) 0.62874(12) -0.24823(14) 0.0484(4) Uani 1 1 d .
S2 S 0.61058(18) 0.21257(13) -0.49670(13) 0.0436(3) Uani 1 1 d .
N1 N 0.0978(5) 0.2332(3) -0.1063(3) 0.0287(9) Uani 1 1 d .
N2 N 0.2324(5) 0.0910(3) -0.1820(3) 0.0276(9) Uani 1 1 d .
C1 C 0.1125(6) 0.1144(4) -0.1046(4) 0.0277(10) Uani 1 1 d .
C2 C 0.2110(6) 0.2848(4) -0.1837(4) 0.0269(10) Uani 1 1 d .
C3 C 0.2970(6) 0.1950(4) -0.2322(4) 0.0279(10) Uani 1 1 d .
C4 C -0.0125(7) 0.2978(5) -0.0302(5) 0.0425(13) Uani 1 1 d .
H4A H -0.0047 0.3797 -0.0461 0.064 Uiso 1 1 calc R
H4B H 0.0246 0.3079 0.0523 0.064 Uiso 1 1 calc R
H4C H -0.1304 0.2485 -0.0462 0.064 Uiso 1 1 calc R
C5 C 0.2785(7) -0.0301(4) -0.2087(5) 0.0445(14) Uani 1 1 d .
H5A H 0.3650 -0.0290 -0.2656 0.067 Uiso 1 1 calc R
H5B H 0.1773 -0.0965 -0.2417 0.067 Uiso 1 1 calc R
H5C H 0.3237 -0.0449 -0.1364 0.067 Uiso 1 1 calc R
C6 C 0.5451(7) 0.5098(6) -0.1572(6) 0.0575(17) Uani 1 1 d .
H6A H 0.6180 0.5908 -0.1595 0.086 Uiso 1 1 calc R
H6B H 0.5845 0.4437 -0.2098 0.086 Uiso 1 1 calc R
H6C H 0.5502 0.4985 -0.0769 0.086 Uiso 1 1 calc R
C7 C 0.3626(7) 0.5038(5) -0.1966(5) 0.0379(12) Uani 1 1 d .
C8 C 0.2164(6) 0.4089(4) -0.2081(4) 0.0290(11) Uani 1 1 d .
C9 C 0.0675(7) 0.4382(4) -0.2562(4) 0.0345(12) Uani 1 1 d .
H9 H -0.0426 0.3836 -0.2671 0.041 Uiso 1 1 calc R
C10 C 0.1011(7) 0.5528(5) -0.2847(5) 0.0392(12) Uani 1 1 d .
C11 C -0.0195(8) 0.6117(5) -0.3414(6) 0.0537(16) Uani 1 1 d .
H11A H 0.0422 0.6937 -0.3501 0.081 Uiso 1 1 calc R
H11B H -0.1134 0.6208 -0.2917 0.081 Uiso 1 1 calc R
H11C H -0.0649 0.5585 -0.4188 0.081 Uiso 1 1 calc R
C12 C 0.3038(7) 0.2901(6) -0.4773(5) 0.0487(14) Uani 1 1 d .
H12A H 0.3463 0.3104 -0.5497 0.073 Uiso 1 1 calc R
H12B H 0.2909 0.3658 -0.4226 0.073 Uiso 1 1 calc R
H12C H 0.1934 0.2296 -0.4955 0.073 Uiso 1 1 calc R
C13 C 0.4298(7) 0.2346(4) -0.4209(4) 0.0343(11) Uani 1 1 d .
C14 C 0.4316(6) 0.1945(4) -0.3180(4) 0.0303(11) Uani 1 1 d .
C15 C 0.5806(6) 0.1453(4) -0.3014(5) 0.0349(12) Uani 1 1 d .
H15 H 0.6013 0.1149 -0.2348 0.042 Uiso 1 1 calc R
C16 C 0.6869(6) 0.1472(5) -0.3903(5) 0.0385(12) Uani 1 1 d .
C17 C 0.8456(7) 0.0941(5) -0.4101(6) 0.0489(14) Uani 1 1 d .
H17A H 0.8909 0.1075 -0.4841 0.073 Uiso 1 1 calc R
H17B H 0.8141 0.0048 -0.4136 0.073 Uiso 1 1 calc R
H17C H 0.9324 0.1362 -0.3451 0.073 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
S S 0.1246 0.1234 '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'
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'
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 180.0(2) . 2
C1 Pd1 I1 87.65(13) . 2
C1 Pd1 I1 92.35(13) 2 2
C1 Pd1 I1 92.35(13) . .
C1 Pd1 I1 87.65(13) 2 .
I1 Pd1 I1 180.000(17) 2 .
C10 S1 C7 93.3(2) . .
C16 S2 C13 93.1(2) . .
C1 N1 C2 110.9(4) . .
C1 N1 C4 122.9(4) . .
C2 N1 C4 126.0(4) . .
C1 N2 C3 111.5(3) . .
C1 N2 C5 121.5(4) . .
C3 N2 C5 127.0(4) . .
N2 C1 N1 105.1(4) . .
N2 C1 Pd1 125.7(3) . .
N1 C1 Pd1 129.0(3) . .
C3 C2 N1 106.7(4) . .
C3 C2 C8 130.4(4) . .
N1 C2 C8 122.7(4) . .
C2 C3 N2 105.8(4) . .
C2 C3 C14 131.9(4) . .
N2 C3 C14 122.3(4) . .
C8 C7 C6 130.4(4) . .
C8 C7 S1 109.7(4) . .
C6 C7 S1 119.7(4) . .
C7 C8 C9 113.0(4) . .
C7 C8 C2 124.4(4) . .
C9 C8 C2 122.4(4) . .
C10 C9 C8 114.1(5) . .
C9 C10 C11 128.9(5) . .
C9 C10 S1 109.8(4) . .
C11 C10 S1 121.3(4) . .
C14 C13 C12 132.2(5) . .
C14 C13 S2 110.1(4) . .
C12 C13 S2 117.6(4) . .
C13 C14 C15 112.4(4) . .
C13 C14 C3 125.7(4) . .
C15 C14 C3 121.9(4) . .
C16 C15 C14 114.2(4) . .
C15 C16 C17 129.6(5) . .
C15 C16 S2 110.1(4) . .
C17 C16 S2 120.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 2.020(4) .
Pd1 C1 2.020(4) 2
Pd1 I1 2.5950(11) 2
Pd1 I1 2.5950(11) .
S1 C10 1.719(6) .
S1 C7 1.741(5) .
S2 C16 1.723(5) .
S2 C13 1.735(5) .
N1 C1 1.362(5) .
N1 C2 1.399(6) .
N1 C4 1.449(6) .
N2 C1 1.349(6) .
N2 C3 1.407(5) .
N2 C5 1.449(5) .
C2 C3 1.366(6) .
C2 C8 1.465(6) .
C3 C14 1.472(6) .
C6 C7 1.492(7) .
C7 C8 1.359(7) .
C8 C9 1.430(7) .
C9 C10 1.359(6) .
C10 C11 1.494(7) .
C12 C13 1.499(7) .
C13 C14 1.356(6) .
C14 C15 1.442(6) .
C15 C16 1.342(7) .
C16 C17 1.515(7) .
