Luminescent Hybrid Halides with Various Centering Metal Cations (Zn, Cd and Pb) and Diverse Structures
Fan, Liubing; Hao, Shiqiang; He, Shihui; Zhang, Xusheng; Li, Mingyang; Wolverton, Chris M.; Zhao, Jing; Liu, Quanlin; Dalton Transactions  (2023) –; doi:10.1039/D2DT04067K

data_7712578
_publ_section_title
;
 Luminescent Hybrid Halides with Various Centering Metal Cations (Zn, Cd
 and Pb) and Diverse Structures
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT04067K
_journal_year                    2023
_chemical_formula_moiety
'Br30 Pb11, 2(C10 H21 N), 2(C10 H18 N), 2(C10 H22 N), 2(C10 H17 N)'
_chemical_formula_sum            'C80 H144 Br30 N8 O Pb11'
_chemical_formula_weight         5910.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                74.55
_cell_angle_beta                 75.12
_cell_angle_gamma                86.03
_cell_formula_units_Z            1
_cell_length_a                   11.965
_cell_length_b                   16.476
_cell_length_c                   19.392
_cell_measurement_reflns_used    24999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8730
_cell_measurement_theta_min      1.8990
_cell_volume                     3561.138
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            75958
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    21.400
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27903
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         3.312
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         12535
_refine_ls_number_restraints     790
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+60.1359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                10578
_reflns_number_total             12535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2dt04067k2.cif
_cod_data_source_block           flb1025g_198k-jana
_cod_original_cell_volume        3561.2
_cod_database_code               7712578
_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. Restrained distances
 C1-C2
 1.54 with sigma of 0.02
 C34-C33
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C31, C32, C33, C34, C35, C36, C37, C38, C39, C40, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br11, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
C39 \\sim C40 \\sim N4: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim
C19 \\sim C20 \\sim N2: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) = Uanis(C18) = Uanis(C19) = Uanis(C17) = Uanis(C20) = Uanis(C16) =
Uanis(C15) = Uanis(C13) = Uanis(C14) = Uanis(C11) = Uanis(C12)
Uanis(N1) = Uanis(C9) = Uanis(C6) = Uanis(C5) = Uanis(C8) = Uanis(C7) =
Uanis(C10) = Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C1)
Uanis(N4) = Uanis(C37) = Uanis(C38) = Uanis(C36) = Uanis(C35) = Uanis(C39) =
Uanis(C34) = Uanis(C40) = Uanis(C31) = Uanis(C32) = Uanis(C33)
5. Others
 Sof(Br)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C32(H32A,H32B), C36(H36A,
 H36B), C39(H39A,H39B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C13(H13), C14(H14), C16(H16), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,
 H15C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C40(H40A,
 H40B,H40C)
;
_olex2_submission_special_instructions 'No special instructions were received'