0D Chiral Hybrid Indium(III) Halides for Second Harmonic Generation
Qi, Siming; Ge, Fei; Han, Xiao; Cheng, Puxin; Shi, Rongchao; Liu, Chao; Zheng, Yongshen; Xin, Mingyang; Xu, Jialiang; Dalton Transactions  (2022) –; doi:10.1039/D2DT00925K

data_7710249
_publ_section_title
;
 0D Chiral Hybrid Indium(III) Halides for Second Harmonic Generation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00925K
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety         'Cl6 In, 3(Cl), 6(C9 H14 N)'
_chemical_formula_sum            'C54 H84 Cl9 In N6'
_chemical_formula_weight         1251.14
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-03-26 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.0073(2)
_cell_length_b                   17.0073(2)
_cell_length_c                   39.2070(6)
_cell_measurement_reflns_used    42488
_cell_measurement_temperature    100.3(8)
_cell_measurement_theta_max      29.7440
_cell_measurement_theta_min      3.6300
_cell_volume                     9821.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.3(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.930
_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    -76.00 -40.00   0.50    1.69    --    9.20  19.00-180.00   72
  2  \w      0.00  91.00   0.50    1.69    --    9.20  19.00-180.00  182
  3  \w    -36.00  36.00   0.50    1.69    --   -9.40 -82.00 120.00  144
  4  \w    -17.00  34.00   0.50    1.69    --   -9.40 -82.00-180.00  102
  5  \w     -1.00  26.00   0.50    1.69    --   -9.40 -38.00 -90.00   54
  6  \w    -85.00 -23.00   0.50    1.69    --   -9.40 -38.00 -90.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0013070000
_diffrn_orient_matrix_UB_12      0.0149419000
_diffrn_orient_matrix_UB_13      0.0167687000
_diffrn_orient_matrix_UB_21      -0.0046226000
_diffrn_orient_matrix_UB_22      0.0361739000
_diffrn_orient_matrix_UB_23      -0.0067841000
_diffrn_orient_matrix_UB_31      -0.0478911000
_diffrn_orient_matrix_UB_32      -0.0280750000
_diffrn_orient_matrix_UB_33      0.0001871000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            89782
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.041
_diffrn_reflns_theta_min         3.411
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
TITL s-in-cl   P 31 2 1     R = 0.04
CELL   17.0073   17.0073   39.2070     90.00     90.00    120.00
SPGR P3121
C101 0.251 0.920 0.837 !       5.11 eA-3
C102 0.958 0.300 0.195 !       4.32 eA-3
C103 0.719 0.723 0.521 !       3.01 eA-3
C104 0.998 0.388 0.195 !       2.96 eA-3
C105 0.929 0.359 0.162 !       2.62 eA-3
C106 0.991 0.441 0.159 !       1.42 eA-3
C107 0.104 0.395 0.124 !       0.81 eA-3
Q108 0.138 0.670 0.080 !       0.78 eA-3
Q109 0.013 0.411 0.218 !       0.69 eA-3
C110 0.049 0.487 0.139 !       0.66 eA-3
C111 0.238 0.950 0.876 !       0.64 eA-3
C112 0.091 0.469 0.146 !       0.63 eA-3
Q113 0.356 0.519 0.439 !       0.53 eA-3
C114 0.120 0.453 0.142 !       0.53 eA-3
Q115 0.425 0.546 0.454 !       0.52 eA-3
C116 0.779 0.784 0.482 !       0.50 eA-3
;
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 6273 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         17211
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+10.2938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                15431
_reflns_number_total             17211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00925k2.cif
_cod_data_source_block           S-MPEA-In-Cl
_cod_original_cell_volume        9821.2(3)
_cod_database_code               7710249
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.803
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C8 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C9: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
3.a Ternary CH refined with riding coordinates:
 C3(H3), C21(H21), C30(H30), C12(H12), C39(H39), C01O(H01O)
3.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C10(H10A,H10B), C28(H28A,H28B), C37(H37A,H37B), C1(H1A,H1B),
 C014(H01A,H01B)
3.c Aromatic/amide H refined with riding coordinates:
 C45(H45), C27(H27), C44(H44), C35(H35), C00V(H00V), C26(H26), C36(H36),
 C23(H23), C33(H33), C24(H24), C25(H25), C34(H34), C01B(H01C), C01E(H01E),
 C32(H32), C18(H18), C14(H14), C5(H5), C43(H43), C16(H16), C01N(H01N),
 C01P(H01P), C9(H9), C41(H41), C17(H17), C8(H8), C15(H15), C42(H42), C7(H7),
 C6(H6)
3.d Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N6(H6A,H6B,H6C), N1(H1C,H1D,H1E), N2(H2D,H2E,H2F), N5(H5A,
 H5B,H5C), N3(H3A,H3B,H3C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C11(H11A,
 H11B,H11C), C38(H38A,H38B,H38C), C2(H2A,H2B,H2C), C01R(H01D,H01F,H01G)
;
_platon_squeeze_void_probe_radius 1.20
_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 2.227
_oxdiff_exptl_absorpt_empirical_full_min 0.453