Chiral organic hybrids for nonlinear optical applications and solvent-induced reversible red-yellow color change.
Yu, Hongli; Hao, Ruibin; Zhao, Dong; Chi, Lingyu; Zhao, Xianlong; Cui, Yibo; Liu, Kunjie; Zhao, Jing; Liu, Quanlin; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11638–11643; doi:10.1039/d5dt00391a

data_7719217
_publ_section_title
;
 Chiral organic hybrids for nonlinear optical applications and
 solvent-induced reversible red-yellow color change.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11638
_journal_page_last               11643
_journal_paper_doi               10.1039/d5dt00391a
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration rm
_chemical_formula_moiety         '0.5(I12 Pb4), C12 H20 N2, 2(H2 O)'
_chemical_formula_sum            'C12 H24 I6 N2 O2 Pb2'
_chemical_formula_weight         1404.11
_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   mixed
_audit_creation_date             2025-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-04-21 deposited with the CCDC.	2025-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.828(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9964(2)
_cell_length_b                   20.7634(6)
_cell_length_c                   17.0445(5)
_cell_measurement_reflns_used    11339
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.6250
_cell_measurement_theta_min      2.3160
_cell_volume                     2759.31(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.140a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     -6.00  66.00   0.50    0.77    --    3.13  57.00 -60.00  144
  2  \w      4.00  73.00   0.50    0.77    --    3.13  38.00-150.00  138
  3  \w    -14.00  34.00   0.50    0.77    --    3.13 -99.00 120.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15481
_diffrn_reflns_point_group_measured_fraction_full 0.879
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.313
_exptl_absorpt_coefficient_mu    18.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.140a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.380
_exptl_crystal_description       cube
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8557
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0481
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    0.751
_reflns_Friedel_fraction_max     0.751
_reflns_number_gt                7530
_reflns_number_total             8557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00391a2.cif
_cod_data_source_block           s-pbi3_auto
_cod_database_code               7719217
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.281
_shelx_estimated_absorpt_t_min   0.164
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.987(7)
 0.013(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H4B-H3E
 2.2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C6) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4)
Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12)
Uanis(C19) = Uanis(C16)
Uanis(C8) = Uanis(C9) = Uanis(C12)
5.a Free rotating group:
 O4(H4B,H4C), O2(H2B,H2C), O1(H1D,H1E), O3(H3D,H3E)
5.b Ternary CH refined with riding coordinates:
 N4(H4), N2(H2A), C11(H11), C23(H23)
5.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C12(H12A,H12B), C8(H8A,H8B), C10(H10A,H10B), C9(H9A,H9B),
 C24(H24A,H24B), C21(H21A,H21B), C20(H20A,H20B), C19(H19A,H19B), C22(H22A,H22B)
5.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C6(H6), C1(H1), C3(H3), C4(H4A), C14(H14), C18(H18),
 C13(H13), C17(H17)
5.e Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_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
;