Temperature-Controlled Syntheses of Substituted 1,2,4-Triazolelead(II) Complexes: Active Lone Pair and N-H...X (X = Cl, Br, I) Hydrogen Bonds
Jian-Kai Cheng; Jian Zhang; Pei-Xiu Yin; Qi-Pu Lin; Zhao-Ji Li; Yuan-Gen Yao; Inorganic Chemistry 48 (2009) 9992–9994; doi:10.1021/ic901653y

data_4303530
_publ_section_title
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Temperature-Controlled Syntheses of Substituted 1,2,4-Triazolelead(II)
Complexes: Active Lone Pair and N-H...X (X = Cl, Br, I) Hydrogen Bonds
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9992
_journal_page_last               9994
_journal_paper_doi               10.1021/ic901653y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C2 H N3 Pb S '
_chemical_formula_sum            'C2 H N3 Pb S'
_chemical_formula_weight         306.33
_chemical_name_systematic
;
 ?
;
_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
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.8582(13)
_cell_length_b                   8.4826(9)
_cell_length_c                   13.0291(15)
_cell_measurement_reflns_used    919
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.13
_cell_volume                     979.0(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury CCD diffractometer'
_diffrn_measurement_method       '\w 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  0.1099
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_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6923
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    34.741
_exptl_absorpt_correction_T_max  .124
_exptl_absorpt_correction_T_min  .05
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .08
_exptl_crystal_size_min          .06
_refine_diff_density_max         3.375
_refine_diff_density_min         -3.245
_refine_diff_density_rms         0.547
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0830P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                1012
_reflns_number_total             1125
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic901653y_si_001_4.cif
_cod_data_source_block           4
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
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_cod_database_code               4303530
_refine_ls_r_factor_ref          0.0510