Bis[(18-crown-6)isothiocyanatolead(II)] tetrathiocyanatopalladate(II)
Ling-Qian Kong; Jian-Min Dou; Cheng-Juan Li; Da-Cheng Li; Da-Qi Wang; Acta Crystallographica Section E 62 (2006) m1030–m1032; doi:10.1107/S1600536806012530

data_2208912
_publ_section_title
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 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-\k^6^<i>O</i>)(isothiocyanato-
\k<i>N</i>)lead(II)] tetrakis(thiocyanato-\k<i>S</i>)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       '\f and \w'
_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/[\s^2^(Fo^2^)+(0.0542P)^2^] where P=(Fo^2^+2Fc^2^)/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>2\s(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