Smallest molecular chalcogenidometalate anions of the heaviest metals: syntheses, structures, and their interconversion.
Thiele, G.; Donsbach, C.; Riedel, R.; Marsch, M.; Harms, K.; Dehnen, S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5958–5967; doi:10.1039/c5dt03996g

data_7037271
_publ_section_title
;
 Smallest molecular chalcogenidometalate anions of the heaviest metals:
 syntheses, structures, and their interconversion.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5958
_journal_page_last               5967
_journal_paper_doi               10.1039/c5dt03996g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C2 H10 K4 N2 O Pb Se4'
_chemical_formula_sum            'C2 H10 K4 N2 O Pb Se4'
_chemical_formula_weight         757.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                92.602(2)
_cell_angle_beta                 102.770(2)
_cell_angle_gamma                93.193(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0377(5)
_cell_length_b                   8.1958(5)
_cell_length_c                   12.6944(7)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.49
_cell_volume                     812.87(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34849
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.158
_diffrn_reflns_theta_min         2.493
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.333
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.2086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1606 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.2798.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.095
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+1.6923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3464
_reflns_number_total             3613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03996g2.cif
_cod_data_source_block           Compound9
_cod_depositor_comments
'Adding full bibliography for 7037263--7037272.cif.'
_cod_database_code               7037271
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Others
 Uiso(H1A)=Uiso(H1B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C1(H1E,H1F), C2(H2C,H2D)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'