Broadband Emission with a Massive Stokes Shift from Sulfonium Pb‒Br Hybrids
Smith, Matthew D.; Watson, Brian L.; Dauskardt, Reinhold H.; Karunadasa, Hemamala I.; Chemistry of Materials 29 (2017) 7083–; doi:10.1021/acs.chemmater.7b02594

data_4002856
_publ_section_title
;
 Broadband Emission with a Massive Stokes Shift from Sulfonium Pb--Br
 Hybrids
;
_journal_issue                   17
_journal_name_full               'Chemistry of Materials'
_journal_page_first              7083
_journal_paper_doi               10.1021/acs.chemmater.7b02594
_journal_volume                  29
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Br12 Pb3, 3(C8 H20 S2)'
_chemical_formula_sum            'C24 H60 Br12 Pb3 S6'
_chemical_formula_weight         2121.57
_chemical_name_systematic
'tris(butane-1,4-bis(dimethylsulfonium)) dodecabromotriplumbate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1968(11)
_cell_length_b                   11.2070(6)
_cell_length_c                   21.0031(11)
_cell_measurement_reflns_used    9552
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.221
_cell_measurement_theta_min      3.009
_cell_volume                     5224.7(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            115262
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         30.210
_diffrn_reflns_theta_min         1.455
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.557
_exptl_absorpt_correction_T_max  0.6480
_exptl_absorpt_correction_T_min  0.2929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
 wR2(int) was 0.1677 before and 0.0877 after correction. 
The Ratio of minimum to maximum transmission is 0.4520. 
The \l/2 correction factor is Not present.'
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.697
_exptl_crystal_description       plate
_exptl_crystal_F_000             3864
_exptl_crystal_recrystallization_method
'Crystallized from a vapor diffusion of acetone into dimethylsulfoxide.'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.916
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.213
_refine_ls_abs_structure_details
;
 Flack x determined using 5375 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         11959
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0309P)^2^+32.0438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11512
_reflns_number_total             11959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b02594_si_003.cif
_cod_data_source_block           g1_orthop_0p77_a
_cod_database_code               4002856
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              37915
_shelx_hkl_checksum              87731