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_4128270
_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         'Br4 Sn, 2(C10 H22 N)'
_chemical_formula_sum            'C20 H44 Br4 N2 Sn'
_chemical_formula_weight         750.90
_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             2018-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 123.374(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.122(3)
_cell_length_b                   8.4218(6)
_cell_length_c                   18.801(2)
_cell_measurement_reflns_used    10353
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.2640
_cell_measurement_theta_min      2.3490
_cell_volume                     2660.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28c (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_temperature      293(2)
_diffrn_detector                 'Bruker Apex I'
_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 0.924
_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      2.18 182.14   0.30   10.08    --   28.00  73.93 -25.82  600
  2  \w      2.18 182.14   0.30   10.06    --   28.00  73.93  94.18  600
  3  \w      2.18 182.14   0.30   10.07    --   28.00  73.93-145.82  600
;
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0418063000
_diffrn_orient_matrix_UB_12      0.0007218000
_diffrn_orient_matrix_UB_13      0.0295868000
_diffrn_orient_matrix_UB_21      -0.0049145000
_diffrn_orient_matrix_UB_22      -0.0344319000
_diffrn_orient_matrix_UB_23      0.0312233000
_diffrn_orient_matrix_UB_31      0.0026187000
_diffrn_orient_matrix_UB_32      -0.0769966000
_diffrn_orient_matrix_UB_33      -0.0137154000
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14448
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.419
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    6.977
_exptl_absorpt_correction_T_max  0.09706
_exptl_absorpt_correction_T_min  0.06737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28c (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         4061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0352P)^2^+7.0867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3695
_reflns_number_total             4061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02365_si_003.cif
_cod_data_source_block           a
_cod_database_code               4128270
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C120H120Br24Sn6
_shelx_estimated_absorpt_t_max   0.367
_shelx_estimated_absorpt_t_min   0.351
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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), C00A(H00M,H00N), C00B(H00O,
 H00P), C00C(H00Q,H00R), C00D(H00S,H00T), C00E(H00U,H00V)
2.b Idealised Me refined as rotating group:
 C008(H00G,H00H,H00I), C009(H00J,H00K,H00L)
;
_shelx_res_checksum              88556
_shelx_hkl_checksum              80403
_olex2_exptl_crystal_mounting_method tip-mounted
_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 1.908
_oxdiff_exptl_absorpt_empirical_full_min 0.697