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_4003087
_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(C13 H22 N)'
_chemical_formula_sum            'C26 H44 Cl5 N2 Sb'
_chemical_formula_weight         683.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-23
_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                   9.25420(10)
_cell_length_b                   13.6419(2)
_cell_length_c                   24.1148(3)
_cell_measurement_reflns_used    27815
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.2830
_cell_measurement_theta_min      3.3970
_cell_volume                     3044.37(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.910
_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     46.00  74.00   0.50    0.50    --   11.81 178.00   0.00   56
  2  \w     46.00  83.00   0.50    0.50    --   11.81 178.00 120.00   74
  3  \w     45.00  78.00   0.50    0.50    --   11.81 178.00 -30.00   66
  4  \w     46.00  76.00   0.50    0.50    --   11.81-178.00  90.00   60
  5  \w     44.00  78.00   0.50    0.50    --   11.81-178.00-120.00   68
  6  \w    -86.00  10.00   0.50    0.50    --  -12.05 -57.00 -30.00  192
  7  \w      6.00  32.00   0.50    0.50    --  -12.05  57.00  90.00   52
  8  \w    -86.00  10.00   0.50    0.50    --  -12.05 -57.00  90.00  192
  9  \w     -5.00  20.00   0.50    0.50    --  -12.05 -99.00  90.00   50
 10  \w    -80.00   8.00   0.50    0.50    --  -12.05 -57.00-150.00  176
;
_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      -0.0227669000
_diffrn_orient_matrix_UB_12      0.0340518000
_diffrn_orient_matrix_UB_13      0.0204356000
_diffrn_orient_matrix_UB_21      0.0664203000
_diffrn_orient_matrix_UB_22      0.0255363000
_diffrn_orient_matrix_UB_23      -0.0027064000
_diffrn_orient_matrix_UB_31      -0.0307370000
_diffrn_orient_matrix_UB_32      0.0298709000
_diffrn_orient_matrix_UB_33      -0.0209768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42287
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.319
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80337
_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    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 3409 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         8645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0172P)^2^+0.5459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0437
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                8395
_reflns_number_total             8645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (TEBA)2SbCl5-002.cif
_cod_data_source_block           exp_2365
_cod_database_code               4003087
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B),
 C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              10881
_shelx_hkl_checksum              16925
_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 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.828