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_4002855
_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_formula_moiety         '0.5(Br20 Pb6), 4(C3 H9 S)'
_chemical_formula_sum            'C12 H36 Br10 Pb3 S4'
_chemical_formula_weight         1729.32
_chemical_name_systematic
'tetrakis(trimethylsulfonium) decabromotriplumbate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.622(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4104(5)
_cell_length_b                   9.2728(4)
_cell_length_c                   18.5164(8)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    298
_cell_measurement_theta_max      33.389
_cell_measurement_theta_min      2.420
_cell_volume                     1941.84(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      298
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24062
_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         27.822
_diffrn_reflns_theta_min         2.165
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    28.993
_exptl_absorpt_correction_T_max  0.3405
_exptl_absorpt_correction_T_min  0.1454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1476 before and 0.0568 after correction. 
The Ratio of minimum to maximum transmission is 0.4270. 
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    2.958
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_preparation       'Crystallized from commerical reagents'
_exptl_crystal_recrystallization_method
;
'Vapor diffusion of diethylether into a 
mixture of dimethylformamide and dimethylsulfoxide.'
;
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3555
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0398P)^2^+9.2025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2832
_reflns_number_total             3555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b02594_si_002.cif
_cod_data_source_block           g1_0p83_a
_cod_database_code               4002855
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              56758
_shelx_hkl_checksum              32161