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_7134659
_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 N)'
_chemical_formula_sum            'C12 H32 Ag5 I7 N2'
_chemical_formula_weight         1632.04
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-29
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-05-29 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                   12.0456(6)
_cell_length_b                   12.0456(6)
_cell_length_c                   19.1296(10)
_cell_measurement_reflns_used    6516
_cell_measurement_temperature    80.0(10)
_cell_measurement_theta_max      29.1700
_cell_measurement_theta_min      3.3980
_cell_volume                     2403.8(2)
_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      N~2~
_diffrn_ambient_temperature      80.0(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_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    -96.00   7.00   0.50   35.00    --   -7.70 -77.00 150.00  206
  2  \w    -52.00  22.00   0.50   35.00    --    7.70 -57.00 -60.00  148
;
_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      0.0620666000
_diffrn_orient_matrix_UB_12      0.0544918000
_diffrn_orient_matrix_UB_13      -0.0028438000
_diffrn_orient_matrix_UB_21      -0.0276072000
_diffrn_orient_matrix_UB_22      0.0397141000
_diffrn_orient_matrix_UB_23      -0.0037157000
_diffrn_orient_matrix_UB_31      0.0020417000
_diffrn_orient_matrix_UB_32      0.0082197000
_diffrn_orient_matrix_UB_33      0.0368040000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10225
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.068
_diffrn_reflns_theta_min         3.195
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.748
_exptl_absorpt_correction_T_max  0.646
_exptl_absorpt_correction_T_min  0.028
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    3.382
_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          0.17
_refine_diff_density_max         2.328
_refine_diff_density_min         -2.194
_refine_diff_density_rms         0.354
_refine_ls_abs_structure_details
;
 Flack x determined using 2188 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_coef       0.0067(3)
_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   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5870
_refine_ls_number_restraints     703
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0789P)^2^+58.3948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_full    0.751
_reflns_Friedel_fraction_max     0.676
_reflns_number_gt                5746
_reflns_number_total             5870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03059e2.cif
_cod_data_source_block           1oxsg
_cod_depositor_comments
'Adding full bibliography for 7134657--7134659.cif.'
_cod_original_cell_volume        2403.8(3)
_cod_database_code               7134659
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         Ag5C11I7N2H32
_shelx_estimated_absorpt_t_max   0.288
_shelx_estimated_absorpt_t_min   0.046
_olex2_refinement_description
;
1. Restrained distances
 C9-C10 \\sim C8-C7 \\sim C12-C11 \\sim C2-C1A \\sim C2-C1 \\sim C4-C3 \\sim
C16-C15 \\sim C6-C5 \\sim C14-C13
 with sigma of 0.02
 N2-C7 \\sim N2-C9 \\sim N2-C11 \\sim N1-C1 \\sim N11-C1A \\sim N1-C3 \\sim
N11-C15 \\sim N1-C5 \\sim N11-C13
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C13 \\sim C2 \\sim C1 \\sim N1 \\sim N11 \\sim C3 \\sim C5 \\sim C15 \\sim C4
\\sim C6 \\sim C16 \\sim C14 \\sim C1A \\sim C8 \\sim N2 \\sim C9 \\sim C7
\\sim C11 \\sim C10 \\sim C12: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 3.8A
Uanis(N11) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim
Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C12) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C15) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(N11) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: H2BD(0.5) H2BE(0.5) H2BF(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5)
 C1(0.5) H1A(0.5) H1B(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) N1(0.5) H1(0.5)
 N11(0.5) H11(0.5) C3(0.5) H3A(0.5) H3B(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C13(0.5) H13A(0.5) H13B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) H6C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
4.a Riding coordinates:
 C2(H2BD,H2BE,H2BF), C2(H2AA,H2AB,H2AC)
4.b Ternary CH refined with riding coordinates:
 N2(H2), N1(H1), N11(H11)
4.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C7(H7A,H7B), C11(H11A,H11B), C1(H1A,H1B), C1A(H1AA,H1AB), C3(H3A,
 H3B), C13(H13A,H13B), C5(H5A,H5B), C15(H15A,H15B)
4.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C16(H16A,H16B,
 H16C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              29326
_shelx_hkl_checksum              84395
_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 3.881
_oxdiff_exptl_absorpt_empirical_full_min 0.419