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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/09/7010950.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_7010950
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            'C16 H28 N2 Pd S10'
_chemical_formula_weight         675.40
_chemical_name_common            (Me3NEt)2[Pd(dmit)2]
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.760(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.471(3)
_cell_length_b                   10.522(3)
_cell_length_c                   12.358(2)
_cell_measurement_temperature    294(2)
_cell_volume                     1385.3(6)
_computing_cell_refinement       'BIOTEX Rigaku'
_computing_data_collection       'RAXIS Rigaku'
_computing_data_reduction        'BIOTEX Rigaku'
_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 0.837
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device_type  'IP Rigaku'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2047
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.432
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.565
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0066(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0941P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.2004
_reflns_number_gt                1741
_reflns_number_total             2047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105854c.txt
_cod_data_source_block           fa1
_cod_original_cell_volume        1385.3(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010950
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.0000 0.5000 0.06213(11) Uani 1 2 d S . .
N1 N 0.2698(2) 0.7857(3) 0.4122(2) 0.0796(10) Uani 1 1 d . . .
C1 C 0.2128(3) 0.1906(3) 0.6463(3) 0.0629(10) Uani 1 1 d . . .
C2 C 0.1922(3) 0.2255(3) 0.5337(2) 0.0629(10) Uani 1 1 d . . .
C3 C 0.3602(3) 0.3891(3) 0.6618(2) 0.0631(10) Uani 1 1 d . . .
C4 C 0.1961(3) 0.7306(4) 0.4798(3) 0.1070(16) Uani 1 1 d . . .
H4A H 0.2539 0.6844 0.5459 0.128 Uiso 1 1 calc R . .
H4B H 0.1625 0.8004 0.5105 0.128 Uiso 1 1 calc R . .
C5 C 0.1884(3) 0.8467(4) 0.3018(3) 0.0953(15) Uani 1 1 d . . .
H5A H 0.1366 0.9098 0.3181 0.143 Uiso 1 1 calc R . .
H5B H 0.1361 0.7835 0.2505 0.143 Uiso 1 1 calc R . .
H5C H 0.2398 0.8864 0.2653 0.143 Uiso 1 1 calc R . .
C6 C 0.3498(3) 0.6852(4) 0.3875(3) 0.0945(14) Uani 1 1 d . . .
H6A H 0.3953 0.7217 0.3438 0.142 Uiso 1 1 calc R . .
H6B H 0.2971 0.6178 0.3432 0.142 Uiso 1 1 calc R . .
H6C H 0.4079 0.6519 0.4597 0.142 Uiso 1 1 calc R . .
C7 C 0.3574(4) 0.8883(4) 0.4873(4) 0.137(2) Uani 1 1 d . . .
H7A H 0.3086 0.9528 0.5059 0.206 Uiso 1 1 calc R . .
H7B H 0.4042 0.9257 0.4452 0.206 Uiso 1 1 calc R . .
H7C H 0.4143 0.8508 0.5579 0.206 Uiso 1 1 calc R . .
C8 C 0.0922(4) 0.6454(4) 0.4164(3) 0.1094(17) Uani 1 1 d . . .
H8A H 0.0491 0.6205 0.4664 0.164 Uiso 1 1 calc R . .
H8B H 0.1245 0.5713 0.3918 0.164 Uiso 1 1 calc R . .
H8C H 0.0349 0.6886 0.3493 0.164 Uiso 1 1 calc R . .
S1 S 0.13545(8) 0.06594(9) 0.68191(7) 0.0735(3) Uani 1 1 d . . .
S2 S 0.08296(8) 0.15118(8) 0.41217(7) 0.0727(3) Uani 1 1 d . . .
S3 S 0.32099(8) 0.28566(9) 0.75126(7) 0.0756(3) Uani 1 1 d . . .
S4 S 0.28139(9) 0.35390(9) 0.51720(7) 0.0754(3) Uani 1 1 d . . .
S5 S 0.46101(10) 0.51038(8) 0.70904(9) 0.0816(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'
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
S1 Pd1 S1 180.0 . 3_556 ?
S1 Pd1 S2 89.73(3) . 3_556 ?
S1 Pd1 S2 90.27(3) 3_556 3_556 ?
S1 Pd1 S2 90.27(3) . . ?
S1 Pd1 S2 89.73(3) 3_556 . ?
S2 Pd1 S2 180.0 3_556 . ?
C5 N1 C6 109.9(3) . . ?
C5 N1 C4 112.6(3) . . ?
C6 N1 C4 110.6(3) . . ?
C5 N1 C7 107.5(3) . . ?
C6 N1 C7 107.8(3) . . ?
C4 N1 C7 108.2(3) . . ?
C2 C1 S1 123.3(2) . . ?
C2 C1 S3 114.2(2) . . ?
S1 C1 S3 122.50(18) . . ?
C1 C2 S2 123.5(2) . . ?
C1 C2 S4 115.8(2) . . ?
S2 C2 S4 120.66(17) . . ?
S5 C3 S4 123.8(2) . . ?
S5 C3 S3 124.55(17) . . ?
S4 C3 S3 111.66(16) . . ?
C8 C4 N1 116.8(3) . . ?
C1 S1 Pd1 101.72(10) . . ?
C2 S2 Pd1 101.14(11) . . ?
C3 S3 C1 99.65(15) . . ?
C3 S4 C2 98.63(15) . . ?
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 S1 2.3151(9) . ?
Pd1 S1 2.3151(9) 3_556 ?
Pd1 S2 2.3195(10) 3_556 ?
Pd1 S2 2.3195(10) . ?
N1 C5 1.484(4) . ?
N1 C6 1.504(5) . ?
N1 C4 1.508(5) . ?
N1 C7 1.531(5) . ?
C1 C2 1.372(4) . ?
C1 S1 1.730(3) . ?
C1 S3 1.740(3) . ?
C2 S2 1.744(3) . ?
C2 S4 1.751(3) . ?
C3 S5 1.675(3) . ?
C3 S4 1.717(3) . ?
C3 S3 1.726(3) . ?
C4 C8 1.465(5) . ?
