Disphenoidal Zero-Dimensional Lead, Tin, and Germanium Halides: Highly Emissive Singlet and Triplet Self-Trapped Excitons and X-ray Scintillation.
Morad, Viktoriia; Shynkarenko, Yevhen; Yakunin, Sergii; Brumberg, Alexandra; Schaller, Richard D.; Kovalenko, Maksym V.; Journal of the American Chemical Society 141 (2019) 9764–9768; doi:10.1021/jacs.9b02365

data_4128269
_publ_section_title
;
 Disphenoidal Zero-Dimensional Lead, Tin, and Germanium Halides: Highly
 Emissive Singlet and Triplet Self-Trapped Excitons and X-ray
 Scintillation.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9764
_journal_page_last               9768
_journal_paper_doi               10.1021/jacs.9b02365
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '2(Br), Br2 Ge, 2(C10 H22 N)'
_chemical_formula_sum            'C20 H44 Br4 Ge N2'
_chemical_formula_weight         704.80
_chemical_name_systematic
'1-butyl-1-methylpiperidinium tetrabromogermanate(II)'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 121.862(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0807(7)
_cell_length_b                   8.42480(10)
_cell_length_c                   18.3778(5)
_cell_measurement_reflns_used    7545
_cell_measurement_temperature    122(3)
_cell_measurement_theta_max      30.1690
_cell_measurement_theta_min      2.3830
_cell_volume                     2640.61(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.921
_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    -25.00  20.00   1.00   65.44    --  -20.55 -99.00 120.00   45
  2  \w    -25.00  20.00   1.00   65.44    --  -20.55 -99.00  60.00   45
  3  \w    -47.00  40.00   1.00   65.44    --   21.02 -57.00  90.00   87
  4  \w    -17.00  93.00   1.00   65.44    --   21.02  19.00 -90.00  110
  5  \w     34.00  95.00   1.00   65.44    --   21.02 179.00 120.00   61
  6  \w    -25.00  61.00   1.00   65.44    --   21.02 -99.00 -30.00   86
  7  \w    -48.00  50.00   1.00   65.44    --   21.02 -77.00-150.00   98
  8  \w      3.00  42.00   1.00   65.44    --   21.02  57.00 120.00   39
  9  \w      3.00  89.00   1.00   65.44    --   21.02  57.00   0.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0058775000
_diffrn_orient_matrix_UB_12      0.0818092000
_diffrn_orient_matrix_UB_13      0.0039589000
_diffrn_orient_matrix_UB_21      -0.0388009000
_diffrn_orient_matrix_UB_22      -0.0164086000
_diffrn_orient_matrix_UB_23      -0.0106838000
_diffrn_orient_matrix_UB_31      0.0137589000
_diffrn_orient_matrix_UB_32      -0.0112923000
_diffrn_orient_matrix_UB_33      0.0439746000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20153
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.911
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method 'Crystalized from EtOH'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         3856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+0.5175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3269
_reflns_number_total             3856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02365_si_001.cif
_cod_data_source_block           vmd325
_cod_original_cell_volume        2640.61(16)
_cod_database_code               4128269
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H44 N2 Ge Br4'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C005(H00A,H00B), C006(H00C,H00D), C007(H00E,H00F), C008(H00G,H00H), C009(H00I,
 H00J), C00A(H00K,H00L), C00C(H00P,H00Q), C00D(H00R,H00S)
2.b Idealised Me refined as rotating group:
 C00B(H00M,H00N,H00O), C00E(H00T,H00U,H00V)
;
_shelx_res_checksum              8140
_shelx_hkl_checksum              12737
_olex2_submission_original_sample_id a
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.735
_oxdiff_exptl_absorpt_empirical_full_min 0.824