Syntheses and X-ray characterization of metal complexes with the pentadentate thiosemicarbazone ligand bis(4-N-methylthiosemicarbazone)-2,6-diacetylpyridine. The first pentacoordinate lead(II) complex with a pentagonal geometry.
Pedrido, Rosa; Bermejo, Manuel R.; Romero, M José; Vázquez, Miguel; González-Noya, Ana M; Maneiro, Marcelino; Rodríguez, M Jesús; Fernández, M Isabel; Dalton transactions (Cambridge, England : 2003)  (2005) 572–579; doi:10.1039/b416296j

data_7008064
_publ_section_title
;
 Syntheses and X-ray characterization of metal complexes with the
 pentadentate thiosemicarbazone ligand
 bis(4-N-methylthiosemicarbazone)-2,6-diacetylpyridine. The first
 pentacoordinate lead(II) complex with a pentagonal geometry.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              572
_journal_page_last               579
_journal_paper_doi               10.1039/b416296j
_journal_year                    2005
_chemical_formula_sum            'C28 H44 N14 O3 S4 Zn2'
_chemical_formula_weight         883.76
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                92.21(3)
_cell_angle_beta                 107.08(3)
_cell_angle_gamma                90.75(4)
_cell_formula_units_Z            2
_cell_length_a                   11.008(4)
_cell_length_b                   11.763(4)
_cell_length_c                   15.946(6)
_cell_measurement_temperature    298(2)
_cell_volume                     1971.6(13)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.1644
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8315
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    1.478
_exptl_absorpt_correction_T_max  0.963581
_exptl_absorpt_correction_T_min  0.699924
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       Blocklike
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_hydrogen_treatment    'riding mode'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6793
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.130
_refine_ls_R_factor_all          0.1912
_refine_ls_R_factor_obs          0.0874
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.0715P)^2^+9.7371P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2329
_refine_ls_wR_factor_obs         0.1720
_reflns_number_observed          3359
_reflns_number_total             6793
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b416296j.txt
_cod_data_source_block           zndapt
_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:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.0715P)^2^+9.7371P] where P==(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w==1/[\s^2^(Fo^2^)+(0.0715P)^2^+9.7371P] where P==(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1971.6(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008064