Synthesis, Characterization, and Calculated Electronic Structure of the Crystalline Metal-Organic Polymers [Hg(SC6H4S)(en)]n and [Pb(SC6H4S)(dien)]n
Dayna L. Turner; Kevin H. Stone; Peter W. Stephens; Aron Walsh; Mayank Pratap Singh; Thomas P. Vaid; Inorganic Chemistry 51 (2012) 370–376; doi:10.1021/ic201779a

data_4327813
_publ_contact_author_email       tpvaid@ua.edu
_publ_contact_author_name        'Thomas P. Vaid'
_publ_section_title
;
 Synthesis, Characterization, and Calculated Electronic Structure of the
 Crystalline Metal-Organic Polymers [Hg(SC6H4S)(en)]n and
 [Pb(SC6H4S)(dien)]n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              370
_journal_page_last               376
_journal_paper_doi               10.1021/ic201779a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_structural     Pb(SC6H4S)(N3C4H13)
_chemical_formula_sum            'C10 H17 N3 Pb S2'
_chemical_formula_weight         450.61
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                61.186(3)
_cell_angle_beta                 86.117(3)
_cell_angle_gamma                86.053(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3106(3)
_cell_length_b                   10.2825(4)
_cell_length_c                   10.2809(4)
_cell_measurement_temperature    298
_cell_volume                     675.01(5)
_computing_cell_refinement       'TOPAS Academic'
_computing_data_collection       EPICS
_computing_publication_material  enCIFer
_computing_structure_refinement  'TOPAS Academic'
_computing_structure_solution    'TOPAS Academic'
_diffrn_ambient_temperature      298
_diffrn_detector                 'NaI scintillation counter'
_diffrn_measurement_device_type  'Huber diffractometer'
_diffrn_radiation_monochromator  'double Si(111)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69702
_diffrn_source                   synchrotron
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_density_method    'Not Measured'
_pd_block_diffractogram_id       Pb(SC6H4S)(dien)
_pd_instr_location
; 
X16C, National Synchrotron Light Source, Brookhaven National Laboratory
;
_pd_meas_2theta_range_inc        0.005
_pd_meas_2theta_range_max        40
_pd_meas_2theta_range_min        1
_pd_meas_number_of_points        7800
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.005
_pd_proc_2theta_range_max        40
_pd_proc_2theta_range_min        3
_pd_proc_info_excluded_regions
;
1 to 3 degrees due to high low angle 
background and no diffraction peaks in that region
;
_pd_proc_ls_background_function
;
Chebyshev polynomial with 12 coeffecients
;
_pd_proc_ls_pref_orient_corr
; 
none 
;
_pd_proc_ls_profile_function
;
Simple_Axial_Model(9.07(3)) function with Rp=9999,Rs=300 in TOPAS-Academic
;
_pd_proc_ls_prof_R_factor        3.667
_pd_proc_ls_prof_wR_expected     2.680
_pd_proc_ls_prof_wR_factor       4.678
_pd_proc_wavelength              0.69702
_pd_spec_mounting
;Sample was loaded into a thin walled glass capillary of nominal 0.7mm
 diameter
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              4
_pd_spec_size_thick              0.7
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.746
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     64
_refine_ls_R_I_factor            1.872
_refine_ls_shift/su_max          0.0001
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            ic201779a_si_002_2.cif
_cod_data_source_block           Pb(SC6H4S)(dien)_x-ray
_cod_depositor_comments          'Adding Fobs data.'
_cod_original_cell_volume        675.01(4)
_cod_database_code               4327813
_cod_database_fobs_code          4327813