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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/7/01/09/7010952.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_7010952
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_moiety         'Pd C6 S10 (N C7 H18 )2'
_chemical_formula_sum            'C20 H36 N2 Pd S10'
_chemical_formula_weight         731.51
_chemical_name_common            (MeNEt3)2[Pd(dmit)2]
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.410(2)
_cell_length_b                   12.937(3)
_cell_length_c                   23.445(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3157.4(12)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8289
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_T_max  1.153
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0567
_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)+(0.0610P)²+1.6674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                2416
_reflns_number_total             2746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105854c.txt
_cod_data_source_block           me32.pd
_cod_original_cell_volume        3157.4(11)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7010952
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.0000 0.0000 0.0000 0.0670(2) Uani 1 2 d S . .
S1 S 0.03102(13) -0.11908(11) 0.07237(6) 0.0807(4) Uani 1 1 d . . .
S2 S 0.17204(13) 0.09659(11) 0.03261(6) 0.0786(4) Uani 1 1 d . . .
S3 S 0.22083(14) -0.12010(11) 0.17001(6) 0.0818(4) Uani 1 1 d . . .
S4 S 0.34164(14) 0.06800(11) 0.13591(6) 0.0831(4) Uani 1 1 d . . .
S5 S 0.43994(18) -0.04116(13) 0.23961(7) 0.0973(5) Uani 1 1 d . . .
C1 C 0.1580(4) -0.0628(4) 0.1085(2) 0.0688(12) Uani 1 1 d . . .
C2 C 0.2161(5) 0.0261(4) 0.0921(2) 0.0693(12) Uani 1 1 d . . .
C3 C 0.3385(5) -0.0318(4) 0.1851(2) 0.0772(13) Uani 1 1 d . . .
N1 N 0.8425(4) 0.2359(3) 0.13088(16) 0.0767(11) Uani 1 1 d . . .
C4 C 0.9642(6) 0.2087(5) 0.1635(3) 0.106(2) Uani 1 1 d . . .
H4A H 1.0314 0.1919 0.1371 0.160 Uiso 1 1 calc R . .
H4B H 0.9480 0.1504 0.1878 0.160 Uiso 1 1 calc R . .
H4C H 0.9900 0.2667 0.1864 0.160 Uiso 1 1 calc R . .
C5 C 0.8645(6) 0.3373(5) 0.0993(3) 0.1017(18) Uani 1 1 d . . .
H5A H 0.7853 0.3561 0.0801 0.122 Uiso 1 1 calc R . .
H5B H 0.8824 0.3906 0.1272 0.122 Uiso 1 1 calc R . .
C6 C 0.9689(6) 0.3376(6) 0.0568(3) 0.111(2) Uani 1 1 d . . .
H6A H 0.9742 0.4045 0.0393 0.167 Uiso 1 1 calc R . .
H6B H 0.9515 0.2865 0.0281 0.167 Uiso 1 1 calc R . .
H6C H 1.0488 0.3218 0.0753 0.167 Uiso 1 1 calc R . .
C7 C 0.7362(6) 0.2611(5) 0.1721(2) 0.0981(18) Uani 1 1 d . . .
H7A H 0.7646 0.3177 0.1962 0.118 Uiso 1 1 calc R . .
H7B H 0.6628 0.2855 0.1505 0.118 Uiso 1 1 calc R . .
C8 C 0.6929(7) 0.1754(7) 0.2096(3) 0.138(3) Uani 1 1 d . . .
H8A H 0.6267 0.2000 0.2347 0.207 Uiso 1 1 calc R . .
H8B H 0.7641 0.1506 0.2317 0.207 Uiso 1 1 calc R . .
H8C H 0.6596 0.1201 0.1865 0.207 Uiso 1 1 calc R . .
C9 C 0.8122(6) 0.1448(5) 0.0949(3) 0.1022(19) Uani 1 1 d . . .
H9A H 0.8848 0.1321 0.0700 0.123 Uiso 1 1 calc R . .
H9B H 0.8034 0.0851 0.1196 0.123 Uiso 1 1 calc R . .
C10 C 0.6953(6) 0.1524(6) 0.0593(3) 0.121(2) Uani 1 1 d . . .
H10A H 0.6857 0.0903 0.0373 0.182 Uiso 1 1 calc R . .
H10B H 0.7027 0.2105 0.0341 0.182 Uiso 1 1 calc R . .
H10C H 0.6216 0.1613 0.0835 0.182 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
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 S2 180.00(10) . 5 ?
S2 Pd1 S1 90.53(5) . . ?
S2 Pd1 S1 89.47(5) 5 . ?
S2 Pd1 S1 89.47(5) . 5 ?
S2 Pd1 S1 90.53(5) 5 5 ?
S1 Pd1 S1 180.00(7) . 5 ?
C1 S1 Pd1 100.70(17) . . ?
C2 S2 Pd1 100.77(17) . . ?
C3 S3 C1 98.9(2) . . ?
C3 S4 C2 98.4(2) . . ?
C2 C1 S1 123.9(4) . . ?
C2 C1 S3 115.3(4) . . ?
S1 C1 S3 120.8(3) . . ?
C1 C2 S2 124.0(4) . . ?
C1 C2 S4 115.4(4) . . ?
S2 C2 S4 120.6(3) . . ?
S5 C3 S3 124.3(3) . . ?
S5 C3 S4 123.7(3) . . ?
S3 C3 S4 112.0(3) . . ?
C9 N1 C7 112.4(4) . . ?
C9 N1 C4 106.3(5) . . ?
C7 N1 C4 109.8(4) . . ?
C9 N1 C5 116.1(4) . . ?
C7 N1 C5 103.7(4) . . ?
C4 N1 C5 108.6(4) . . ?
C6 C5 N1 116.2(5) . . ?
C8 C7 N1 116.2(5) . . ?
C10 C9 N1 116.3(5) . . ?
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 2.3138(14) . ?
Pd1 S2 2.3138(14) 5 ?
Pd1 S1 2.3143(14) . ?
Pd1 S1 2.3143(14) 5 ?
S1 C1 1.731(5) . ?
S2 C2 1.728(5) . ?
S3 C3 1.712(5) . ?
S3 C1 1.748(5) . ?
S4 C3 1.730(6) . ?
S4 C2 1.749(5) . ?
S5 C3 1.663(5) . ?
C1 C2 1.355(7) . ?
N1 C9 1.482(7) . ?
N1 C7 1.506(6) . ?
N1 C4 1.521(7) . ?
N1 C5 1.524(7) . ?
C5 C6 1.474(8) . ?
C7 C8 1.484(8) . ?
C9 C10 1.479(8) . ?
