Dual-Band Luminescent Lead-Free Antimony Chloride Halides with Near-Unity Photoluminescence Quantum Efficiency
Li, Zhongyuan; Li, Ye; Liang, Pei; Zhou, Tianliang; Wang, Le; Xie, Rong-Jun; Chemistry of Materials  (2019) –; doi:10.1021/acs.chemmater.9b02935

data_4003088
_publ_section_title
;
 Dual-Band Luminescent Lead-Free Antimony Chloride Halides with Near-Unity
 Photoluminescence Quantum Efficiency
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b02935
_journal_year                    2019
_chemical_formula_moiety         'Cl5 Sb, 2(C8 H20 N)'
_chemical_formula_sum            'C16 H40 Cl5 N2 Sb'
_chemical_formula_weight         559.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6371(10)
_cell_length_b                   13.9398(10)
_cell_length_c                   14.1728(12)
_cell_measurement_reflns_used    7979
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3600
_cell_measurement_theta_min      4.6740
_cell_volume                     2496.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -71.00 -21.00   0.50    0.05    --  -42.80 -37.00-120.00  100
  2  \w   -118.00  36.00   0.50    0.05    --  -42.80   0.00 -90.00  308
  3  \w   -115.00 -75.00   0.50    0.05    --  -42.80-125.00   0.00   80
  4  \w    -63.00  23.00   0.50    0.05    --  -42.80  57.00-150.00  172
  5  \w   -116.00 -90.00   0.50    0.05    --  -42.80 -37.00-120.00   52
  6  \w    -28.00  64.00   0.50    0.05    --   42.80 -37.00   0.00  184
  7  \w   -155.00-129.00   0.50    0.13    --  -90.25-125.00 150.00   52
  8  \w   -109.00 -83.00   0.50    0.13    --  -90.25  77.00-180.00   52
  9  \w    -72.00 -46.00   0.50    0.13    --  -90.25  77.00-180.00   52
 10  \w   -101.00 -19.00   0.50    0.13    --  -90.25  77.00-120.00  164
 11  \w   -104.00 -78.00   0.50    0.13    --  -90.25-125.00 150.00   52
 12  \w    -90.00 -25.00   0.50    0.13    --  -90.25 125.00-120.00  130
 13  \w     49.00  93.00   0.50    0.13    --  110.18 -94.00  90.00   88
 14  \w     83.00 116.00   0.50    0.13    --  110.18-125.00 -60.00   66
 15  \w     36.00 105.00   0.50    0.13    --  110.18 -45.00-180.00  138
 16  \w     62.00 115.00   0.50    0.13    --  110.18-125.00-150.00  106
 17  \w     83.00 132.00   0.50    0.13    --  110.18 -45.00 -90.00   98
 18  \w     39.00  99.00   0.50    0.13    --  110.18 -94.00   0.00  120
 19  \w     38.00  64.00   0.50    0.13    --  110.18 -45.00 -90.00   52
 20  \w     44.00 108.00   0.50    0.13    --  110.18 -94.00  30.00  128
 21  \w     64.00 178.00   0.50    0.13    --  110.18  15.00 150.00  228
 22  \w     42.00  87.00   0.50    0.13    --  110.18 -94.00 -30.00   90
 23  \w     29.00 153.00   0.50    0.13    --  110.18 -15.00 -90.00  248
 24  \w     84.00 117.00   0.50    0.13    --  110.18-125.00 -90.00   66
 25  \w     48.00 125.00   0.50    0.13    --  110.18 -45.00  90.00  154
 26  \w     54.00  80.00   0.50    0.13    --  110.18-125.00 -90.00   52
 27  \w    112.00 175.00   0.50    0.13    --  110.18 125.00 -60.00  126
 28  \w     37.00  63.00   0.50    0.13    --  110.18-125.00 -30.00   52
 29  \w     33.00 133.00   0.50    0.13    --  110.18 -30.00   0.00  200
;
_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      -0.0325418000
_diffrn_orient_matrix_UB_12      -0.1004125000
_diffrn_orient_matrix_UB_13      -0.0344737000
_diffrn_orient_matrix_UB_21      0.1071185000
_diffrn_orient_matrix_UB_22      -0.0107537000
_diffrn_orient_matrix_UB_23      -0.0509763000
_diffrn_orient_matrix_UB_31      0.0482695000
_diffrn_orient_matrix_UB_32      -0.0447460000
_diffrn_orient_matrix_UB_33      0.0896657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24210
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.674
_diffrn_reflns_theta_min         4.449
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.700
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.582
_refine_diff_density_min         -3.324
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2608
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0735
_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^)+(0.1062P)^2^+26.8423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2388
_reflns_number_total             2608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (TTA)2SbCl5-001.cif
_cod_data_source_block           exp_1956
_cod_database_code               4003088
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.547
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N2-C5 \\sim N2-C5A \\sim N2-C7A \\sim N2-C7
 with sigma of 0.02
 C8A-C7A \\sim C8-C7 \\sim C6-C5 \\sim C6-C5A
 with sigma of 0.02
3. Rigid bond restraints
 C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C7A)=Sof(H7AA)=
 Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(1)
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7A(H7AA,H7AB), C5A(H5AA,H5AB), C7(H7A,
 H7B)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6BD,H6BE,H6BF), C6(H6AA,H6AB,H6AC),
 C8A(H8AA,H8AB,H8AC), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              20456
_shelx_hkl_checksum              18696
_shelx_fab_checksum              60248
_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 1.767
_oxdiff_exptl_absorpt_empirical_full_min 0.693