#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/89/2208912.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2208912
loop_
_publ_author_name
'Ling-Qian Kong'
'Jian-Min Dou'
'Cheng-Juan Li'
'Da-Cheng Li'
'Da-Qi Wang'
_publ_section_title
;
 Bis[(18-crown-6)isothiocyanatolead(II)] tetrathiocyanatopalladate(II)
;
_journal_coeditor_code           HY2001
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1030
_journal_page_last               m1032
_journal_paper_doi               10.1107/S1600536806012530
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Pb (N C S) (C12 H24 O6)]2 [Pd (N C S)4]'
_chemical_formula_moiety         '2C13 H24 N O6 Pb S + , C4 N4 Pd S4 2-'
_chemical_formula_sum            'C30 H48 N6 O12 Pb2 Pd S6'
_chemical_formula_weight         1397.88
_chemical_name_systematic
;
bis[(1,4,7,10,13,16-hexaoxacyclooctadecane-κ⁶O)(isothiocyanato-
κN)lead(II)] tetrakis(thiocyanato-κS)palladium(II)
;
_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           SHELXL97
_cell_angle_alpha                92.043(4)
_cell_angle_beta                 105.979(3)
_cell_angle_gamma                101.316(4)
_cell_formula_units_Z            1
_cell_length_a                   8.336(2)
_cell_length_b                   11.958(3)
_cell_length_c                   12.464(3)
_cell_measurement_reflns_used    2559
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.5
_cell_volume                     1165.9(5)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6061
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    7.911
_exptl_absorpt_correction_T_max  0.1799
_exptl_absorpt_correction_T_min  0.1484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.541
_refine_diff_density_min         -1.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0369
_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)+(0.0542P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                3276
_reflns_number_total             4040
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2001.cif
_cod_data_source_block           I
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2208912
_cod_database_fobs_code          2208912
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Pb Pb1 0.33163(3) 0.21010(2) 0.74201(2) 0.04404(13) Uani d . 1
Pd Pd1 0.5000 0.5000 1.0000 0.03721(19) Uani d S 1
N N1 0.8441(11) 0.8176(7) 1.0319(9) 0.097(3) Uani d . 1
N N2 0.1144(10) 0.6239(7) 0.7647(7) 0.080(3) Uani d . 1
N N3 0.3864(9) 0.1284(6) 0.5848(6) 0.0574(18) Uani d DU 1
O O1 0.6585(6) 0.1889(5) 0.8419(4) 0.0531(14) Uani d . 1
O O2 0.6003(6) 0.3896(5) 0.7636(5) 0.0567(14) Uani d . 1
O O3 0.3021(7) 0.3809(5) 0.6021(5) 0.0602(15) Uani d . 1
O O4 0.0161(7) 0.2255(5) 0.6065(5) 0.0618(16) Uani d . 1
O O5 0.0684(7) 0.0279(5) 0.7002(5) 0.0589(15) Uani d . 1
O O6 0.3855(7) 0.0111(4) 0.8302(4) 0.0520(13) Uani d . 1
S S1 0.5323(3) 0.67377(19) 0.9214(2) 0.0693(7) Uani d . 1
S S2 0.2177(2) 0.44691(17) 0.89047(18) 0.0546(5) Uani d . 1
S S3 0.4577(4) 0.2157(2) 0.4011(2) 0.0882(8) Uani d . 1
C C1 0.7707(11) 0.2941(8) 0.8959(8) 0.071(3) Uani d . 1
H H1A 0.8853 0.2821 0.9277 0.085 Uiso calc R 1
H H1B 0.7319 0.3229 0.9559 0.085 Uiso calc R 1
C C2 0.7705(10) 0.3767(9) 0.8117(9) 0.074(3) Uani d . 1
H H2A 0.8429 0.4499 0.8464 0.088 Uiso calc R 1
H H2B 0.8150 0.3495 0.7538 0.088 Uiso calc R 1
C C3 0.5935(12) 0.4663(8) 0.6781(9) 0.071(3) Uani d . 1
H H3A 0.6236 0.4335 0.6159 0.086 Uiso calc R 1
H H3B 0.6743 0.5382 0.7074 0.086 Uiso calc R 1
C C4 0.4182(12) 0.4865(7) 0.6393(8) 0.067(3) Uani d . 1
H H4A 0.3914 0.5245 0.7003 0.080 Uiso calc R 1
H H4B 0.4096 0.5357 0.5786 0.080 Uiso calc R 1
C C5 0.1353(12) 0.3945(9) 0.5431(8) 0.074(3) Uani d . 1
H H5A 0.1403 0.4351 0.4777 0.089 Uiso calc R 1
H H5B 0.0930 0.4395 0.5912 0.089 Uiso calc R 1
C C6 0.0186(13) 0.2819(9) 0.5081(8) 0.076(3) Uani d . 1
H H6A -0.0953 0.2910 0.4689 0.092 Uiso calc R 1
H H6B 0.0579 0.2371 0.4580 0.092 Uiso calc R 1
C C7 -0.1176(11) 0.1231(9) 0.5807(9) 0.083(3) Uani d . 1
H H7A -0.1101 0.0760 0.5180 0.099 Uiso calc R 1
H H7B -0.2289 0.1428 0.5612 0.099 Uiso calc R 1
C C8 -0.0931(11) 0.0606(9) 0.6825(9) 0.073(3) Uani d . 1
H H8A -0.0923 0.1096 0.7465 0.088 Uiso calc R 1
H H8B -0.1846 -0.0066 0.6717 0.088 Uiso calc R 1
C C9 0.0905(12) -0.0638(7) 0.7706(7) 0.068(3) Uani d . 1
H H9A 0.0012 -0.1314 0.7391 0.081 Uiso calc R 1
H H9B 0.0852 -0.0415 0.8449 0.081 Uiso calc R 1
C C10 0.2587(12) -0.0881(7) 0.7766(7) 0.059(2) Uani d . 1
H H10A 0.2759 -0.1533 0.8191 0.071 Uiso calc R 1
H H10B 0.2661 -0.1059 0.7018 0.071 Uiso calc R 1
C C11 0.5546(11) -0.0057(8) 0.8484(8) 0.067(3) Uani d . 1
H H11A 0.5753 -0.0214 0.7771 0.080 Uiso calc R 1
H H11B 0.5693 -0.0709 0.8914 0.080 Uiso calc R 1
C C12 0.6743(11) 0.0959(8) 0.9086(7) 0.063(2) Uani d . 1
H H12A 0.6510 0.1131 0.9788 0.076 Uiso calc R 1
H H12B 0.7898 0.0834 0.9255 0.076 Uiso calc R 1
C C13 0.7203(11) 0.7552(7) 0.9872(8) 0.054(2) Uani d . 1
C C14 0.1620(10) 0.5550(7) 0.8173(7) 0.055(2) Uani d . 1
C C15 0.4150(11) 0.1668(7) 0.5127(7) 0.056(2) Uani d DU 1
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'
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Pb1 O5 . . 84.3(2) ?
N3 Pb1 O6 . . 84.2(2) ?
O5 Pb1 O6 . . 60.90(16) ?
N3 Pb1 O2 . . 90.3(2) ?
O5 Pb1 O2 . . 174.34(16) ?
O6 Pb1 O2 . . 120.10(16) ?
N3 Pb1 O1 . . 81.6(2) ?
O5 Pb1 O1 . . 120.97(17) ?
O6 Pb1 O1 . . 60.80(16) ?
O2 Pb1 O1 . . 59.39(16) ?
N3 Pb1 O3 . . 78.8(2) ?
O5 Pb1 O3 . . 117.61(17) ?
O6 Pb1 O3 . . 162.98(17) ?
O2 Pb1 O3 . . 59.58(16) ?
O1 Pb1 O3 . . 115.16(17) ?
N3 Pb1 O4 . . 88.6(2) ?
O5 Pb1 O4 . . 60.22(17) ?
O6 Pb1 O4 . . 121.09(17) ?
O2 Pb1 O4 . . 118.31(17) ?
O1 Pb1 O4 . . 169.88(17) ?
O3 Pb1 O4 . . 59.78(17) ?
S2 Pd1 S2 . 2_667 180.00(10) yes
S2 Pd1 S1 . 2_667 89.19(7) yes
S2 Pd1 S1 2_667 2_667 90.81(7) ?
S2 Pd1 S1 . . 90.81(7) yes
S2 Pd1 S1 2_667 . 89.19(7) ?
S1 Pd1 S1 2_667 . 180.0 ?
C15 N3 Pb1 . . 130.7(7) ?
C12 O1 C1 . . 113.1(6) ?
C12 O1 Pb1 . . 115.4(4) ?
C1 O1 Pb1 . . 113.6(5) ?
C2 O2 C3 . . 110.7(7) ?
C2 O2 Pb1 . . 120.3(5) ?
C3 O2 Pb1 . . 119.4(5) ?
C4 O3 C5 . . 112.4(6) ?
C4 O3 Pb1 . . 117.0(4) ?
C5 O3 Pb1 . . 118.6(5) ?
C6 O4 C7 . . 110.6(7) ?
C6 O4 Pb1 . . 115.1(5) ?
C7 O4 Pb1 . . 117.5(5) ?
C8 O5 C9 . . 114.7(7) ?
C8 O5 Pb1 . . 112.4(5) ?
C9 O5 Pb1 . . 116.7(5) ?
C11 O6 C10 . . 112.8(6) ?
C11 O6 Pb1 . . 114.6(4) ?
C10 O6 Pb1 . . 114.6(4) ?
C13 S1 Pd1 . . 109.6(3) ?
C14 S2 Pd1 . . 110.0(3) ?
O1 C1 C2 . . 108.0(7) ?
O1 C1 H1A . . 110.1 ?
C2 C1 H1A . . 110.1 ?
O1 C1 H1B . . 110.1 ?
C2 C1 H1B . . 110.1 ?
H1A C1 H1B . . 108.4 ?
O2 C2 C1 . . 108.9(7) ?
O2 C2 H2A . . 109.9 ?
C1 C2 H2A . . 109.9 ?
O2 C2 H2B . . 109.9 ?
C1 C2 H2B . . 109.9 ?
H2A C2 H2B . . 108.3 ?
O2 C3 C4 . . 108.6(7) ?
O2 C3 H3A . . 110.0 ?
C4 C3 H3A . . 110.0 ?
O2 C3 H3B . . 110.0 ?
C4 C3 H3B . . 110.0 ?
H3A C3 H3B . . 108.3 ?
O3 C4 C3 . . 109.2(7) ?
O3 C4 H4A . . 109.8 ?
C3 C4 H4A . . 109.8 ?
O3 C4 H4B . . 109.8 ?
C3 C4 H4B . . 109.8 ?
H4A C4 H4B . . 108.3 ?
O3 C5 C6 . . 110.1(8) ?
O3 C5 H5A . . 109.6 ?
C6 C5 H5A . . 109.6 ?
O3 C5 H5B . . 109.6 ?
C6 C5 H5B . . 109.6 ?
H5A C5 H5B . . 108.1 ?
O4 C6 C5 . . 107.6(7) ?
O4 C6 H6A . . 110.2 ?
C5 C6 H6A . . 110.2 ?
O4 C6 H6B . . 110.2 ?
C5 C6 H6B . . 110.2 ?
H6A C6 H6B . . 108.5 ?
O4 C7 C8 . . 106.8(8) ?
O4 C7 H7A . . 110.4 ?
C8 C7 H7A . . 110.4 ?
O4 C7 H7B . . 110.4 ?
C8 C7 H7B . . 110.4 ?
H7A C7 H7B . . 108.6 ?
O5 C8 C7 . . 106.5(7) ?
O5 C8 H8A . . 110.4 ?
C7 C8 H8A . . 110.4 ?
O5 C8 H8B . . 110.4 ?
C7 C8 H8B . . 110.4 ?
H8A C8 H8B . . 108.6 ?
O5 C9 C10 . . 107.2(7) ?
O5 C9 H9A . . 110.3 ?
C10 C9 H9A . . 110.3 ?
O5 C9 H9B . . 110.3 ?
C10 C9 H9B . . 110.3 ?
H9A C9 H9B . . 108.5 ?
O6 C10 C9 . . 107.9(7) ?
O6 C10 H10A . . 110.1 ?
C9 C10 H10A . . 110.1 ?
O6 C10 H10B . . 110.1 ?
C9 C10 H10B . . 110.1 ?
H10A C10 H10B . . 108.4 ?
O6 C11 C12 . . 109.3(7) ?
O6 C11 H11A . . 109.8 ?
C12 C11 H11A . . 109.8 ?
O6 C11 H11B . . 109.8 ?
C12 C11 H11B . . 109.8 ?
H11A C11 H11B . . 108.3 ?
O1 C12 C11 . . 109.2(7) ?
O1 C12 H12A . . 109.8 ?
C11 C12 H12A . . 109.8 ?
O1 C12 H12B . . 109.8 ?
C11 C12 H12B . . 109.8 ?
H12A C12 H12B . . 108.3 ?
N1 C13 S1 . . 175.2(8) ?
N2 C14 S2 . . 175.7(8) ?
N3 C15 S3 . . 176.0(9) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 N3 . 2.353(7) yes
Pb1 O5 . 2.692(5) yes
Pb1 O6 . 2.721(5) yes
Pb1 O2 . 2.727(5) yes
Pb1 O1 . 2.733(5) yes
Pb1 O3 . 2.736(5) yes
Pb1 O4 . 2.752(5) yes
Pd1 S2 . 2.3214(19) yes
Pd1 S2 2_667 2.3214(19) ?
Pd1 S1 2_667 2.329(2) ?
Pd1 S1 . 2.329(2) yes
N1 C13 . 1.133(11) ?
N2 C14 . 1.136(10) ?
N3 C15 . 1.086(9) ?
O1 C12 . 1.417(9) ?
O1 C1 . 1.429(10) ?
O2 C2 . 1.422(10) ?
O2 C3 . 1.427(10) ?
O3 C4 . 1.407(10) ?
O3 C5 . 1.426(10) ?
O4 C6 . 1.423(10) ?
O4 C7 . 1.444(11) ?
O5 C8 . 1.437(10) ?
O5 C9 . 1.437(10) ?
O6 C11 . 1.420(9) ?
O6 C10 . 1.427(10) ?
S1 C13 . 1.648(9) ?
S2 C14 . 1.675(8) ?
S3 C15 . 1.629(9) ?
C1 C2 . 1.466(13) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.478(12) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 C6 . 1.470(13) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C8 . 1.481(13) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C10 . 1.469(13) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 C12 . 1.443(12) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
