A mixed-anion compound based upon a [Pb<sub>4</sub>O<sub>4</sub>] heterocubane unit: synthesis, structure and electronic properties of Pb<sub>8</sub>O<sub>4</sub>I<sub>6</sub>(CN<sub>2</sub>).
Schwarz, Albert T.; Petersen, Nele; Ströbele, Markus; Enseling, David; Jüstel, Thomas; Slabon, Adam; Meyer, H-Jürgen; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15169–15175; doi:10.1039/d5dt01979f

data_7719482
_publ_section_title
;
 A mixed-anion compound based upon a [Pb<sub>4</sub>O<sub>4</sub>]
 heterocubane unit: synthesis, structure and electronic properties of
 Pb<sub>8</sub>O<sub>4</sub>I<sub>6</sub>(CN<sub>2</sub>).
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15169
_journal_page_last               15175
_journal_paper_doi               10.1039/d5dt01979f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C I6 N2 O4 Pb8'
_chemical_formula_sum            'C I6 N2 O4 Pb8'
_chemical_formula_weight         2522.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-07 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.053(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8050(5)
_cell_length_b                   8.13080(10)
_cell_length_c                   16.1378(4)
_cell_measurement_reflns_used    11589
_cell_measurement_temperature    150.00(11)
_cell_measurement_theta_max      45.2740
_cell_measurement_theta_min      2.7420
_cell_volume                     2253.21(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  -9.00   0.50   38.00    --  -39.27  93.00 164.00  114
  2  \w     28.00  62.00   0.50   38.00    --   40.83 -93.00  52.00   68
  3  \w    -49.00 -24.00   0.50   38.00    --  -39.27 -67.00  93.67   50
  4  \w    -42.00 -17.00   0.50   38.00    --  -39.27 -85.00  68.13   50
  5  \w   -111.00 -34.00   0.50   38.00    --  -39.27 -19.00 -30.00  154
  6  \w   -110.00 -69.00   0.50   38.00    --  -39.27 -57.00  90.00   82
  7  \w    -74.00 -34.00   0.50   38.00    --  -39.27   0.00-180.00   80
  8  \w    -88.00 -63.00   0.50   38.00    --  -39.27   0.00 -30.00   50
  9  \w    -96.00 -68.00   0.50   38.00    --  -39.27-178.00-180.00   56
 10  \w   -105.00 -78.00   0.50   38.00    --  -39.27-178.00 -60.00   54
 11  \w   -108.00 -50.00   0.50   38.00    --  -39.27 -19.00  90.00  116
 12  \w    -85.00 -59.00   0.50   38.00    --  -39.27 -67.00  93.67   52
 13  \w    -29.00   5.00   0.50   38.00    --   40.83 -19.00 -30.00   68
 14  \w    -22.00   5.00   0.50   38.00    --   40.83 -19.00 -60.00   54
 15  \w    -28.00  -2.00   0.50   38.00    --   40.83 -19.00-120.00   52
 16  \w    -90.00 -41.00   0.50   38.00    --  -39.27 136.00  99.93   98
 17  \w    -59.00 -33.00   0.50   38.00    --  -39.27 -45.00 -11.60   52
 18  \w    -83.00 -37.00   0.50   38.00    --  -39.27 130.00  81.15   92
 19  \w    -99.00 -20.00   0.50   38.00    --  -39.27 -77.00-120.00  158
 20  \w    -90.00 -45.00   0.50   38.00    --  -39.27 137.00-119.45   90
 21  \w    -91.00 -41.00   0.50   38.00    --  -39.27 138.00  41.14  100
 22  \w    -87.00 -28.00   0.50   38.00    --  -39.27 -57.00-120.00  118
 23  \w    -64.00 -33.00   0.50   38.00    --  -39.27   0.00-120.00   62
 24  \w    -84.00 -32.00   0.50   38.00    --  -39.27 -43.00 136.51  104
 25  \w   -110.00 -32.00   0.50   38.00    --  -39.27 -57.00 -30.00  156
 26  \w   -109.00 -34.00   0.50   38.00    --  -39.27 -19.00 150.00  150
 27  \w   -110.00 -77.00   0.50   38.00    --  -39.27 -77.00 -60.00   66
 28  \w    -65.00 -20.00   0.50   38.00    --  -39.27 -77.00 -60.00   90
 29  \w    -65.00 -20.00   0.50   38.00    --  -39.27 -77.00-180.00   90
 30  \w    -99.00 -57.00   0.50   38.00    --  -39.27 -77.00 120.00   84
 31  \w    -51.00 -20.00   0.50   38.00    --  -39.27 -77.00 120.00   62
 32  \w    -42.00  30.00   0.50   38.00    --  -39.27  19.00  60.00  144
 33  \w    -57.00  19.00   0.50   38.00    --  -39.27  77.00-120.00  152
 34  \w   -106.00 -36.00   0.50   38.00    --  -39.27  -7.00-139.79  140
 35  \w    -88.00 -59.00   0.50   38.00    --  -39.27 -57.00  60.00   58
 36  \w    -53.00 -28.00   0.50   38.00    --  -39.27 -57.00  60.00   50
 37  \w   -106.00 -80.00   0.50   38.00    --  -39.27 -77.00   0.00   52
 38  \w    -48.00 -22.00   0.50   38.00    --  -39.27 -77.00   0.00   52
 39  \w     29.00  70.00   0.50   38.00    --   40.83 -99.00   0.00   82
 40  \w      1.00  70.00   0.50   38.00    --   40.83 -99.00 -90.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0376187000
_diffrn_orient_matrix_UB_12      -0.0257847000
_diffrn_orient_matrix_UB_13      -0.0051943000
_diffrn_orient_matrix_UB_21      -0.0156260000
_diffrn_orient_matrix_UB_22      0.0765493000
_diffrn_orient_matrix_UB_23      -0.0203899000
_diffrn_orient_matrix_UB_31      -0.0068415000
_diffrn_orient_matrix_UB_32      -0.0329456000
_diffrn_orient_matrix_UB_33      -0.0432879000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29157
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.372
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    67.772
_exptl_absorpt_correction_T_max  0.433
_exptl_absorpt_correction_T_min  0.155
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    7.437
_exptl_crystal_description       plate
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0113
_refine_ls_R_factor_gt           0.0108
_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^)+15.8450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0214
_refine_ls_wR_factor_ref         0.0215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2033
_reflns_number_total             2070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01979f2.cif
_cod_data_source_block           asp275_v1
_cod_depositor_comments          'Adding full bibliography for 7719482.cif.'
_cod_database_code               7719482
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Pb8 O4 I6 C N2'
_shelx_estimated_absorpt_t_max   0.359
_shelx_estimated_absorpt_t_min   0.150
_olex2_refinement_description
;
;
_shelx_res_checksum              7316
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.542
_oxdiff_exptl_absorpt_empirical_full_min 0.619