Non-centrosymmetric phase of [C4N2H14][CdBr4] for Solar-Blind Ultraviolet Detection
Ma, Li; Wen, Jinrong; Liu, Zhanqiang; Hou, Jingshan; Miao, Xuyan; Fang, Yongzheng; Huang, Yanwei; Zhang, Ganghua; CrystEngComm  (2025) –; doi:10.1039/D5CE00884K

data_7251193
_publ_section_title
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 Non-centrosymmetric phase of [C4N2H14][CdBr4] for Solar-Blind Ultraviolet
 Detection
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00884K
_journal_year                    2025
_chemical_formula_moiety         '2(Br2 Cd0.5), C4 H14 N2'
_chemical_formula_sum            'C4 H14 Br4 Cd N2'
_chemical_formula_weight         522.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2p8112
_audit_creation_date             2024-12-24
_audit_creation_method
; 
Olex2 1.5 
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) 
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_audit_update_record
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2025-08-13 deposited with the CCDC.	2025-10-30 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 94.813(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.958(2)
_cell_length_b                   7.807(2)
_cell_length_c                   19.790(7)
_cell_measurement_reflns_used    6511
_cell_measurement_temperature    293.00
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.75
_cell_volume                     1225.2(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8600
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         2.569
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.781
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1325 before and 0.0719 after correction. 
The Ratio of minimum to maximum transmission is 0.5194. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.831
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.240
_refine_diff_density_min         -2.785
_refine_diff_density_rms         0.382
_refine_ls_abs_structure_details
; 
 Twinning involves inversion, so Flack parameter cannot be determined 
;
_refine_ls_extinction_coef       0.211(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.1121
_refine_ls_shift/su_max          0.087
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2369
_refine_ls_wR_factor_ref         0.2423
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                3088
_reflns_number_total             3487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00884k2.cif
_cod_data_source_block           p21c_1
_cod_database_code               7251193
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.215
_shelx_estimated_absorpt_t_min   0.176
_olex2_refinement_description
; 
1. Twinned data refinement 
 Scales: 0.73(11) 
 -0.00(3) 0.27(10) 0.00(3) 
2. Fixed Uiso 
 At 1.2 times of: 
  All C(H,H) groups, All N(H,H,H) groups 
3. Restrained distances 
 N2-C34 = N9-C2 = N1-C15 = N8-C11 
 1.48 with sigma of 0.0001 
 N8-C11 
 1.47 with sigma of 0.01 
 C34-C33 = C33-C16 = C2-C16 = C22-C15 = C22-C17 = C17-C11 
 1.53 with sigma of 0.0001 
 Br1C-Cd1 
 2.7 with sigma of 0.02 
 Cd2-Br3 \\sim Cd2A-Br3A 
 with sigma of 0.02 
 Cd2-Br6 \\sim Cd2A-Br6A 
 with sigma of 0.02 
 Cd2-Br5 \\sim Cd2A-Br5A 
 with sigma of 0.02 
 Cd2-Br8 \\sim Cd2A-Br8A 
 with sigma of 0.02 
 Br3-Br6 \\sim Br3A-Br6A 
 with sigma of 0.04 
 Br3-Br5 \\sim Br3A-Br5A 
 with sigma of 0.04 
 Br3-Br8 \\sim Br3A-Br8A 
 with sigma of 0.04 
 Br6-Br5 \\sim Br6A-Br5A 
 with sigma of 0.04 
 Br6-Br8 \\sim Br6A-Br8A 
 with sigma of 0.04 
 Br5-Br8 \\sim Br5A-Br8A 
 with sigma of 0.04 
 Cd1-Br4 \\sim Cd1A-Br4A 
 with sigma of 0.02 
 Cd1-Br2 \\sim Cd1A-Br2A 
 with sigma of 0.02 
 Cd1-Br7 \\sim Cd1A-Br7A 
 with sigma of 0.02 
 Cd1-Br1B \\sim Cd1A-Br1C 
 with sigma of 0.02 
 Br4-Br2 \\sim Br4A-Br2A 
 with sigma of 0.04 
 Br4-Br7 \\sim Br4A-Br7A 
 with sigma of 0.04 
 Br4-Br1B \\sim Br4A-Br1C 
 with sigma of 0.04 
 Br2-Br7 \\sim Br2A-Br7A 
 with sigma of 0.04 
 Br2-Br1B \\sim Br2A-Br1C 
 with sigma of 0.04 
 Br7-Br1B \\sim Br7A-Br1C 
 with sigma of 0.04 
4. Rigid bond restraints 
 All non-hydrogen atoms 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 
5. Uiso/Uaniso restraints and constraints 
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma 
for terminal atoms of 0.02 within 2A 
Uanis(N2) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C16) 
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N9) \\sim Ueq: with sigma of 0.005 and 
sigma for terminal atoms of 0.01 
Uanis(N1) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C17) 
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.003 and 
sigma for terminal atoms of 0.006 
Uanis(Br5) \\sim Ueq, Uanis(Cd2) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br6) 
\\sim Ueq, Uanis(Br8) \\sim Ueq: with sigma of 0.003 and sigma for terminal 
atoms of 0.006 
Uanis(Br1C) \\sim Ueq, Uanis(Cd1) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Br4) 
\\sim Ueq, Uanis(Br7) \\sim Ueq: with sigma of 0.005 and sigma for terminal 
atoms of 0.01 
Uanis(Cd2) = Uanis(Cd2A) 
Uanis(Cd1A) = Uanis(Cd1) 
6. Others 
 Sof(Br6A)=Sof(Cd2A)=Sof(Br3A)=Sof(Br5A)=Sof(Br8A)=1-FVAR(1) 
 Sof(Cd2)=Sof(Br3)=Sof(Br6)=Sof(Br5)=Sof(Br8)=FVAR(1) 
 Sof(Cd1)=Sof(Br4)=Sof(Br2)=Sof(Br7)=Sof(Br1C)=1-FVAR(2) 
 Sof(Br1B)=Sof(Cd1A)=Sof(Br2A)=Sof(Br4A)=Sof(Br7A)=FVAR(2) 
7.a Secondary CH2 refined with riding coordinates: 
 C11(H11A,H11B), C16(H16A,H16B), C22(H22A,H22B), C15(H15A,H15B), C17(H17A, 
 H17B), C2(H2A,H2B), C34(H34A,H34B), C33(H33A,H33B) 
7.b Me refined with riding coordinates: 
 N8(H8A,H8B,H8C), N1(H1A,H1B,H1C) 
7.c Idealised Me refined as rotating group: 
 N9(H9A,H9B,H9C), N2(H2C,H2D,H2E) 
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_shelx_res_checksum              92701
_olex2_submission_special_instructions 'No special instructions were received'