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_7712579
_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
'1.01(Br4 Cd), 0.5(C10 H21 N), C10 H20 N, 0.5(C10 H10 N)'
_chemical_formula_sum            'C20 H34 Br4.03 Cd N2'
_chemical_formula_weight         736.73
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-12-06
_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                90
_cell_angle_beta                 102.820(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5329(5)
_cell_length_b                   9.9301(2)
_cell_length_c                   33.1666(6)
_cell_measurement_reflns_used    8934
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.44
_cell_measurement_theta_min      3.18
_cell_volume                     5630.5(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            41042
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         5.151
_exptl_absorpt_coefficient_mu    12.957
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.074
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1499P)^2^+16.9217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2365
_refine_ls_wR_factor_ref         0.2526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6854
_reflns_number_total             8804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04067k2.cif
_cod_data_source_block           cu_0721_10_
_cod_database_code               7712579
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.357
_shelx_estimated_absorpt_t_min   0.284
_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
 C58-C1
 1.52 with sigma of 0.02
 C70-C29
 1.52 with sigma of 0.01
 C58-C41
 1.52 with sigma of 0.02
 N4-C64
 1.48 with sigma of 0.02
 N4-C59
 1.54 with sigma of 0.02
 N4-C65
 1.54 with sigma of 0.02
 C65-C66
 1.54 with sigma of 0.02
 C67-C68
 1.54 with sigma of 0.02
 C61-C60
 1.47 with sigma of 0.02
 C61-C62
 1.47 with sigma of 0.02
 C62-C63
 1.47 with sigma of 0.02
 C63-N4
 1.47 with sigma of 0.02
 C60-C59
 1.47 with sigma of 0.02
 C59-N4
 1.47 with sigma of 0.02
 C28-C23 \\sim C23-C12 \\sim C17-C15 \\sim C24-C15 \\sim C16-C10 \\sim C9-C10
 with sigma of 0.0001
 N4-C63 \\sim C61-C60
 with sigma of 0.02
 N4-C63 \\sim C61-C60 \\sim C59-C65
 with sigma of 0.02
 C62-C61 \\sim C60-C59
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim N3 \\sim C30 \\sim C32 \\sim C42 \\sim C45 \\sim C12 \\sim C28 \\sim
C41 \\sim C23 \\sim C58: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C15 \\sim N2 \\sim C11 \\sim C18 \\sim C31 \\sim C36 \\sim C17 \\sim C39 \\sim
C24 \\sim C29 \\sim C70: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N1 \\sim C1AA \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C16 \\sim C14
\\sim C10 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C30 \\sim N3 \\sim C32 \\sim C42 \\sim C45 \\sim C12 \\sim C28 \\sim C41 \\sim
C23 \\sim C58: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C58 \\sim N3 \\sim C30 \\sim C32 \\sim C42 \\sim C45 \\sim C12 \\sim C28 \\sim
C41 \\sim C23: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cd \\sim Br10: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(Br2) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Cd) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(BrB) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C65) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C61) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C29) = Uanis(C70)
Uanis(C59) = Uanis(C60)
Uanis(C63) = Uanis(N4) = Uanis(C65)
Uanis(C23) = Uanis(C12)
Uanis(C9) = Uanis(C10)
Uanis(C61) = Uanis(C60)
Uanis(C60) = Uanis(C59) = Uanis(C61)
Uanis(C62) = Uanis(C63) = Uanis(C61)
Uanis(C63) = Uanis(C65) = Uanis(N4)
Uanis(C64) = Uanis(N4)
Uanis(C68) = Uanis(C67)
Uanis(C66) = Uanis(C65) = Uanis(C67)
4. Others
 Sof(Br11)=Sof(Br13)=1-FVAR(1)
 Sof(Br4)=Sof(Br5)=Sof(Br2)=Sof(Br3)=Sof(Br9)=Sof(Br10)=FVAR(1)
 Sof(BrB)=1-FVAR(2)
 Sof(BrA)=FVAR(2)
 Sof(Br6B)=1-FVAR(3)
 Sof(Br6A)=FVAR(3)
 Sof(Br7B)=1-FVAR(4)
 Sof(Br7A)=FVAR(4)
5.a Riding coordinates:
 C70(H70A,H70B,H70C), C1(H1A,H1B,H1C)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C23(H23A,
 H23B), C24(H24A,H24B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C36(H36A,H36B), C39(H39A,H39B), C58(H58A,H58B), C1AA(H1AA,
 H1AB), C8(H8A,H8B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C14(H14A,H14B),
 C66(H66A,H66B)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C41(H41), C42(H42), C16(H16), C10(H10), C63(H63), C60(H60),
 C61(H61), C62(H62)
5.d X=CH2 refined with riding coordinates:
 C64(H64A,H64B)
5.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C45(H45A,H45B,H45C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C)
5.f :
 C67(H67), C68(H68)
;
_shelx_res_checksum              84301
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'