#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/09/7010955.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_7010955
loop_
_publ_author_name
'Fang Qi'
'Thomas C. W. Mak'
'Zhou Zhong-Yuan'
'Yang Qing-Chuan'
'Liu Zhi'
'Yu Wen-Tao'
'Zhu Dao-Ben'
'Jiang Min-Hua'
_publ_section_title
;
 Syntheses and crystal structures of the molecular conductors
 Z[Pd(dmit)2]2{Z = (Me3NEt)+, (MeNEt3)+, (NEt4)+} and their precursors
 Z2[Pd(dmit)2]
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1377
_journal_page_last               1385
_journal_paper_doi               10.1039/b105854c
_journal_year                    2002
_chemical_formula_sum            'C20 H20 N Pd2 S20'
_chemical_formula_weight         1128.37
_chemical_name_common            (NEt4)[Pd(dmit)2]2
_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                83.947(4)
_cell_angle_beta                 83.301(4)
_cell_angle_gamma                72.741(4)
_cell_formula_units_Z            1
_cell_length_a                   6.297(1)
_cell_length_b                   7.875(1)
_cell_length_c                   18.885(3)
_cell_measurement_temperature    294(2)
_cell_volume                     885.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker 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      294(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4364
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    2.215
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3959
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             559
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.368
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4364
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1219P)²+0.8260P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.2144
_reflns_number_gt                2865
_reflns_number_total             4364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105854c.txt
_cod_data_source_block           e4pd2
_cod_original_cell_volume        885.8(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010955
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 0.51275(4) -0.18986(3) 0.536828(13) 0.02833(6) Uani 1 1 d . . .
S1 S 0.22781(13) -0.19009(13) 0.47054(5) 0.0343(2) Uani 1 1 d . . .
S2 S 0.76930(14) -0.34651(13) 0.45321(5) 0.0372(2) Uani 1 1 d . . .
S3 S 0.23918(16) -0.33916(13) 0.32990(5) 0.0422(3) Uani 1 1 d . . .
S4 S 0.71981(17) -0.48370(13) 0.31796(5) 0.0420(3) Uani 1 1 d . . .
S5 S 0.4681(2) -0.53336(16) 0.20274(6) 0.0628(4) Uani 1 1 d . . .
S6 S 0.26101(13) -0.05416(12) 0.62714(4) 0.0318(2) Uani 1 1 d . . .
S7 S 0.80409(14) -0.20920(12) 0.60298(5) 0.0349(2) Uani 1 1 d . . .
S8 S 0.33281(16) 0.03162(13) 0.77108(5) 0.0419(3) Uani 1 1 d . . .
S9 S 0.81102(15) -0.11083(13) 0.75140(5) 0.0402(3) Uani 1 1 d . . .
S10 S 0.6053(2) 0.03941(19) 0.88897(6) 0.0663(4) Uani 1 1 d . . .
N1 N 0.0000 0.5000 1.0000 0.0478(15) Uani 1 2 d SD . .
C1 C 0.3736(5) -0.3017(4) 0.39926(16) 0.0307(8) Uani 1 1 d . . .
C2 C 0.6021(6) -0.3686(4) 0.39396(17) 0.0307(9) Uani 1 1 d . . .
C3 C 0.4771(6) -0.4546(4) 0.27909(18) 0.0369(10) Uani 1 1 d . . .
C4 C 0.4386(6) -0.0556(4) 0.68910(17) 0.0332(9) Uani 1 1 d . . .
C5 C 0.6674(5) -0.1242(4) 0.67957(18) 0.0312(9) Uani 1 1 d . . .
C6 C 0.5870(7) -0.0109(5) 0.8077(2) 0.0427(11) Uani 1 1 d . . .
C7 C 0.1549(9) 0.3812(10) 0.9513(2) 0.055(3) Uani 0.50 1 d PD A 1
H7A H 0.1952 0.2613 0.9741 0.066 Uiso 0.50 1 calc PR A 1
H7B H 0.2900 0.4181 0.9411 0.066 Uiso 0.50 1 calc PR A 1
C8 C 0.0557(8) 0.3800(6) 0.88014(18) 0.088(2) Uani 0.50 1 d PD A 1
H8A H 0.1623 0.2977 0.8501 0.132 Uiso 0.50 1 calc PR A 1
H8B H 0.0217 0.4974 0.8563 0.132 Uiso 0.50 1 calc PR A 1
H8C H -0.0783 0.3439 0.8899 0.132 Uiso 0.50 1 calc PR A 1
C7' C -0.1007(11) 0.5180(8) 0.9271(3) 0.054(3) Uani 0.50 1 d PD . 2
H7'A H -0.2469 0.4984 0.9346 0.065 Uiso 0.50 1 calc PR . 2
H7'B H -0.1168 0.6367 0.9042 0.065 Uiso 0.50 1 calc PR . 2
C8' C 0.0557(8) 0.3800(6) 0.88014(18) 0.088(2) Uani 0.50 1 d P B 2
H8'A H -0.0051 0.3874 0.8352 0.132 Uiso 0.50 1 calc PR B 2
H8'B H 0.0725 0.2630 0.9035 0.132 Uiso 0.50 1 calc PR B 2
H8'C H 0.1988 0.4021 0.8720 0.132 Uiso 0.50 1 calc PR B 2
C9 C -0.0450(6) 0.6952(6) 0.9732(4) 0.050(3) Uani 0.50 1 d PD A 1
H9A H -0.1408 0.7693 1.0090 0.060 Uiso 0.50 1 calc PR A 1
H9B H -0.1218 0.7171 0.9301 0.060 Uiso 0.50 1 calc PR A 1
C10 C 0.1744(6) 0.7450(4) 0.9575(4) 0.099(2) Uani 0.50 1 d PD A 1
H10A H 0.1428 0.8690 0.9413 0.148 Uiso 0.50 1 calc PR A 1
H10B H 0.2673 0.6741 0.9211 0.148 Uiso 0.50 1 calc PR A 1
H10C H 0.2502 0.7233 1.0002 0.148 Uiso 0.50 1 calc PR A 1
C9' C 0.2158(9) 0.5450(5) 0.9797(4) 0.044(2) Uani 0.50 1 d PD . 2
H9'A H 0.2978 0.4762 0.9404 0.053 Uiso 0.50 1 calc PR . 2
H9'B H 0.3061 0.5128 1.0200 0.053 Uiso 0.50 1 calc PR . 2
C10' C 0.1744(6) 0.7450(4) 0.9575(4) 0.099(2) Uani 0.50 1 d P C 2
H10D H 0.3148 0.7698 0.9445 0.148 Uiso 0.50 1 calc PR C 2
H10E H 0.0964 0.8132 0.9968 0.148 Uiso 0.50 1 calc PR C 2
H10F H 0.0861 0.7769 0.9174 0.148 Uiso 0.50 1 calc PR C 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'
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
_geom_angle_publ_flag
S2 Pd1 S7 87.88(3) . . ?
S2 Pd1 S6 175.17(3) . . ?
S7 Pd1 S6 90.43(3) . . ?
S2 Pd1 S1 90.06(4) . . ?
S7 Pd1 S1 176.33(4) . . ?
S6 Pd1 S1 91.38(3) . . ?
S2 Pd1 Pd1 96.48(3) . 2_656 ?
S7 Pd1 Pd1 96.05(3) . 2_656 ?
S6 Pd1 Pd1 88.19(3) . 2_656 ?
S1 Pd1 Pd1 87.20(3) . 2_656 ?
C1 S1 Pd1 101.30(12) . . ?
C2 S2 Pd1 101.09(11) . . ?
C1 S3 C3 97.14(17) . . ?
C3 S4 C2 97.71(17) . . ?
C4 S6 Pd1 100.35(11) . . ?
C5 S7 Pd1 101.57(12) . . ?
C4 S8 C6 97.50(18) . . ?
C6 S9 C5 98.28(18) . . ?
C7 N1 C7 180.0(3) 2_567 . ?
C7 N1 C9' 66.0(4) 2_567 2_567 ?
C7 N1 C9' 114.0(4) . 2_567 ?
C7 N1 C9' 114.0(4) 2_567 . ?
C7 N1 C9' 66.0(4) . . ?
C9' N1 C9' 180.0(6) 2_567 . ?
C7 N1 C9 67.3(4) 2_567 . ?
C7 N1 C9 112.7(4) . . ?
C9' N1 C9 110.4(2) 2_567 . ?
C9' N1 C9 69.6(2) . . ?
C7 N1 C9 112.7(4) 2_567 2_567 ?
C7 N1 C9 67.3(4) . 2_567 ?
C9' N1 C9 69.6(2) 2_567 2_567 ?
C9' N1 C9 110.4(2) . 2_567 ?
C9 N1 C9 180.000(2) . 2_567 ?
C7 N1 C7' 109.8(3) 2_567 . ?
C7 N1 C7' 70.2(3) . . ?
C9' N1 C7' 76.6(4) 2_567 . ?
C9' N1 C7' 103.4(4) . . ?
C9 N1 C7' 74.2(4) . . ?
C9 N1 C7' 105.8(4) 2_567 . ?
C7 N1 C7' 70.2(3) 2_567 2_567 ?
C7 N1 C7' 109.8(3) . 2_567 ?
C9' N1 C7' 103.4(4) 2_567 2_567 ?
C9' N1 C7' 76.6(4) . 2_567 ?
C9 N1 C7' 105.8(4) . 2_567 ?
C9 N1 C7' 74.2(4) 2_567 2_567 ?
C7' N1 C7' 180.000(3) . 2_567 ?
C2 C1 S1 122.2(3) . . ?
C2 C1 S3 116.4(2) . . ?
S1 C1 S3 121.40(18) . . ?
C1 C2 S2 125.3(3) . . ?
C1 C2 S4 115.2(3) . . ?
S2 C2 S4 119.4(2) . . ?
S5 C3 S4 123.5(2) . . ?
S5 C3 S3 123.0(2) . . ?
S4 C3 S3 113.5(2) . . ?
C5 C4 S6 124.4(3) . . ?
C5 C4 S8 115.6(3) . . ?
S6 C4 S8 119.96(19) . . ?
C4 C5 S7 123.1(3) . . ?
C4 C5 S9 115.4(3) . . ?
S7 C5 S9 121.41(19) . . ?
S10 C6 S9 124.0(3) . . ?
S10 C6 S8 122.8(2) . . ?
S9 C6 S8 113.2(2) . . ?
N1 C7 C8 112.4(4) . . ?
N1 C7' C9' 50.3(2) . 2_567 ?
N1 C9 C10 110.6(3) . . ?
N1 C9' C7' 53.0(3) . 2_567 ?
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 S2 2.2931(9) . ?
Pd1 S7 2.2975(10) . ?
Pd1 S6 2.3048(9) . ?
Pd1 S1 2.3051(10) . ?
Pd1 Pd1 3.1295(7) 2_656 ?
S1 C1 1.706(3) . ?
S2 C2 1.678(4) . ?
S3 C1 1.734(4) . ?
S3 C3 1.741(3) . ?
S4 C3 1.716(4) . ?
S4 C2 1.749(3) . ?
S5 C3 1.642(4) . ?
S6 C4 1.708(4) . ?
S7 C5 1.689(3) . ?
S8 C4 1.739(3) . ?
S8 C6 1.744(4) . ?
S9 C6 1.705(4) . ?
S9 C5 1.744(4) . ?
S10 C6 1.651(4) . ?
N1 C7 1.451(5) 2_567 ?
N1 C7 1.451(5) . ?
N1 C9' 1.501(6) 2_567 ?
N1 C9' 1.501(6) . ?
N1 C9 1.520(5) . ?
N1 C9 1.520(5) 2_567 ?
N1 C7' 1.558(5) . ?
N1 C7' 1.558(5) 2_567 ?
C1 C2 1.373(5) . ?
C4 C5 1.378(5) . ?
C7 C8 1.548(6) . ?
C7' C9' 1.897(9) 2_567 ?
C9 C10 1.533(5) . ?
C9' C7' 1.897(9) 2_567 ?
