Bulk Assembly of Zero-Dimensional Organic Lead Bromide Hybrid with Efficient Blue Emission
Lin, Haoran; Zhou, Chenkun; Chaaban, Maya; Xu, Liang-Jin; Zhou, Yan; Neu, Jennifer; Worku, Michael; Berkwits, Ella; He, Qingquan; Lee, Sujin; Lin, Xinsong; Siegrist, Theo; Du, Mao-Hua; Ma, Biwu; ACS Materials Letters  (2019) 594–; doi:10.1021/acsmaterialslett.9b00333

data_4515188
_publ_section_title
;
 Bulk Assembly of Zero-Dimensional Organic Lead Bromide Hybrid with
 Efficient Blue Emission
;
_journal_name_full               'ACS Materials Letters'
_journal_page_first              594
_journal_paper_doi               10.1021/acsmaterialslett.9b00333
_journal_year                    2019
_chemical_formula_moiety         'Br4 Pb, 2(C13 H19 N4)'
_chemical_formula_sum            'C26 H38 Br4 N8 Pb'
_chemical_formula_weight         989.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.488(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9526(3)
_cell_length_b                   16.0859(5)
_cell_length_c                   21.5605(8)
_cell_measurement_reflns_used    6508
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      29.3800
_cell_measurement_theta_min      1.8910
_cell_volume                     3104.83(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.796
_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    -28.00  10.00   0.50   27.58    --    4.71 -37.00 -60.00   76
  2  \w    -22.00  21.00   0.50   27.58    --   -5.81 -99.00 -60.00   86
  3  \w    -68.00 -31.00   0.50   27.58    --    4.71 -37.00 -60.00   74
  4  \w     -7.00  37.00   0.50   27.58    --    4.71  27.00 157.00   88
;
_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      0.0779036000
_diffrn_orient_matrix_UB_12      -0.0034440000
_diffrn_orient_matrix_UB_13      -0.0051730000
_diffrn_orient_matrix_UB_21      -0.0144408000
_diffrn_orient_matrix_UB_22      -0.0150915000
_diffrn_orient_matrix_UB_23      -0.0303405000
_diffrn_orient_matrix_UB_31      0.0010894000
_diffrn_orient_matrix_UB_32      0.0413151000
_diffrn_orient_matrix_UB_33      -0.0115602000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15687
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.854
_diffrn_reflns_theta_min         1.889
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_F_000             1888
_refine_diff_density_max         3.336
_refine_diff_density_min         -2.514
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+82.0157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4980
_reflns_number_total             6552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz9b00333_si_002.cif
_cod_data_source_block           lhr-hmta-blue1
_cod_database_code               4515188
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H38 N8 Pb Br4'
_chemical_oxdiff_usercomment     'transparent irregular,150 K'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8070(14)
 0.1930(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16)
;
_shelx_res_checksum              80664
_shelx_hkl_checksum              20103
_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 2.317
_oxdiff_exptl_absorpt_empirical_full_min 0.689