One-dimensional silver iodide homo-helical chains induced by achiral ammonium featuring second-order optical nonlinearity.
Liu, Tong; Zheng, Yong-Shen; Liang, Xiao-Wen; Yao, Zhao-Quan; Zhao, Jiong-Peng; Liu, Fu-Chen; Chemical communications (Cambridge, England) 61 (2025) 10327–10330; doi:10.1039/d5cc03059e

data_7134657
_publ_section_title
;
 One-dimensional silver iodide homo-helical chains induced by achiral
 ammonium featuring second-order optical nonlinearity.
;
_journal_issue                   56
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10327
_journal_page_last               10330
_journal_paper_doi               10.1039/d5cc03059e
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'Ag5 I7, 2(C6 H16 N1)'
_chemical_formula_sum            'C12 H32 Ag5 I7 N2'
_chemical_formula_weight         1632.04
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-03
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-06-03 deposited with the CCDC.	2025-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.1737(12)
_cell_length_b                   12.1737(12)
_cell_length_c                   19.4498(19)
_cell_measurement_reflns_used    2872
_cell_measurement_temperature    294.2(5)
_cell_measurement_theta_max      29.7900
_cell_measurement_theta_min      3.5170
_cell_volume                     2496.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.102a 64-bit (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.2(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.902
_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    -17.00  14.00   0.50    8.00    --    0.00  77.00 -90.00   62
  2  \w    -19.00  88.00   0.50    8.00    --    0.00  57.00 -30.00  214
  3  \w    -89.00 -64.00   0.50    8.00    --    0.00 -57.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0549594000
_diffrn_orient_matrix_UB_12      -0.0061384000
_diffrn_orient_matrix_UB_13      0.0003073000
_diffrn_orient_matrix_UB_21      0.0383061000
_diffrn_orient_matrix_UB_22      0.0663158000
_diffrn_orient_matrix_UB_23      0.0051670000
_diffrn_orient_matrix_UB_31      -0.0060370000
_diffrn_orient_matrix_UB_32      -0.0093799000
_diffrn_orient_matrix_UB_33      0.0361054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16476
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.783
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.090
_diffrn_reflns_theta_min         3.142
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.387
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.257
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.337
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details
;
 Flack x determined using 1767 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_coef       0.0316(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7669
_refine_ls_number_restraints     433
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.811
_reflns_Friedel_fraction_max     0.664
_reflns_number_gt                5216
_reflns_number_total             7669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03059e2.cif
_cod_data_source_block           exp_11891
_cod_depositor_comments
'Adding full bibliography for 7134657--7134659.cif.'
_cod_original_cell_volume        2496.3(5)
_cod_database_code               7134657
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.315
_shelx_estimated_absorpt_t_min   0.048
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C4-C3 \\sim C6-C5 \\sim C1-C2 \\sim C8-C7 \\sim C12-C11 \\sim C10-C9 \\sim
N1-C3 \\sim N1-C5 \\sim N1-C1 \\sim N2-
 C7 \\sim N2-C11 \\sim N2-C9
 with sigma of 0.01
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 N1-C4 \\sim N1A-C4A
 with sigma of 0.04
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 N1-C6 \\sim N1A-C6A
 with sigma of 0.04
 N1-C2 \\sim N1A-C2A
 with sigma of 0.04
 C12-C11 \\sim C12A-C11A
 with sigma of 0.02
 N1-C3 \\sim N1A-C3A
 with sigma of 0.02
 N1-C5 \\sim N1A-C5A
 with sigma of 0.02
 N1-C1 \\sim N1A-C1A
 with sigma of 0.02
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C3-C1 \\sim C3A-C1A
 with sigma of 0.04
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C5-C1 \\sim C5A-C1A
 with sigma of 0.04
 N2-C12 \\sim N2A-C12A
 with sigma of 0.04
 N2-C8 \\sim N2A-C8A
 with sigma of 0.04
 N2-C10 \\sim N2A-C10A
 with sigma of 0.04
 N2-C7 \\sim N2A-C7A
 with sigma of 0.02
 N2-C11 \\sim N2A-C11A
 with sigma of 0.02
 N2-C9 \\sim N2A-C9A
 with sigma of 0.02
 C7-C11 \\sim C7A-C11A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C11-C9 \\sim C11A-C9A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N1 \\sim C4 \\sim C3 \\sim C5 \\sim C6 \\sim C1 \\sim C2 \\sim N2 \\sim C7
\\sim C12 \\sim C11 \\sim C9 \\sim C8 \\sim C10: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
N1 \\sim C4 \\sim C3 \\sim C5 \\sim C6 \\sim C1 \\sim C2 \\sim N1A \\sim C4A
\\sim C3A \\sim C5A \\sim C6A \\sim C1A \\sim C2A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
N2 \\sim C7 \\sim C9 \\sim C8 \\sim C10 \\sim N2A \\sim C7A \\sim C9A \\sim C8A
\\sim C10A \\sim C12 \\sim C11 \\sim C11A \\sim C12A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Ag7) = Uanis(Ag1)
Uanis(Ag5) = Uanis(Ag6)
Uanis(C4) = Uanis(C4A)
Uanis(C8A) = Uanis(C8)
4. Others
 Sof(Ag7)=1-FVAR(1)
 Sof(Ag1)=FVAR(1)
 Sof(Ag5)=1-FVAR(2)
 Sof(Ag6)=FVAR(2)
 Sof(N2A)=Sof(H2AA)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C11A)=Sof(H11C)=Sof(H11D)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C10A)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(N1A)=
 Sof(H1AA)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C1A)=
 Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AB)=Sof(H2AC)=Sof(H2AD)=1-FVAR(3)
 Sof(N1)=Sof(H1)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(N2)=Sof(H2)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N2A(H2AA), N1A(H1AA)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B), C7(H7A,H7B), C11(H11A,H11B), C9(H9A,
 H9B), C7A(H7AA,H7AB), C11A(H11C,H11D), C9A(H9AA,H9AB), C3A(H3AA,H3AB),
 C5A(H5AA,H5AB), C1A(H1AB,H1AC)
5.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C),
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C8A(H8AA,H8AB,H8AC), C10A(H10D,H10E,
 H10F), C12A(H12D,H12E,H12F), C4A(H4AA,H4AB,H4AC), C6A(H6AA,H6AB,H6AC),
 C2A(H2AB,H2AC,H2AD)
;
_shelx_res_checksum              67760
_shelx_hkl_checksum              8066
_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 2.162
_oxdiff_exptl_absorpt_empirical_full_min 0.594