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_7710248
_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           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-25
_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                   17.05090(10)
_cell_length_b                   17.05090(10)
_cell_length_c                   39.5214(4)
_cell_measurement_reflns_used    36540
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.1850
_cell_measurement_theta_min      3.1730
_cell_volume                     9950.79(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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     32.00  80.00   0.50    0.50    --    0.00  82.00-180.00   96
  2  \w    -35.00  20.00   0.50    0.50    --    0.00  82.00-180.00  110
  3  \w    -66.00  40.00   0.50    0.50    --    0.00 -77.00  90.00  212
  4  \w     59.00 188.00   0.50    0.68    --   98.20  45.00   0.00  258
  5  \w     78.00 187.00   0.50    0.68    --   98.20  45.00  30.00  218
  6  \w     11.00  54.00   0.50    0.68    --   98.20 -45.00 -30.00   86
  7  \w     84.00 133.00   0.50    0.68    --   98.20  77.00 -90.00   98
  8  \w     14.00 141.00   0.50    0.68    --   98.20 -82.00-180.00  254
  9  \w     60.00 138.00   0.50    0.68    --   98.20 -45.00 -30.00  156
 10  \w     47.00 153.00   0.50    0.68    --   98.20  30.00-120.00  212
 11  \w    142.00 167.00   0.50    0.68    --   98.20 -15.00-150.00   50
 12  \w     12.00  48.00   0.50    0.68    --   98.20 -61.00 -60.00   72
 13  \w     76.00 101.00   0.50    0.68    --   98.20 -61.00 -60.00   50
 14  \w     15.00  85.00   0.50    0.68    --   98.20 -15.00-150.00  140
;
_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      -0.0838361000
_diffrn_orient_matrix_UB_12      -0.0245313000
_diffrn_orient_matrix_UB_13      -0.0219276000
_diffrn_orient_matrix_UB_21      -0.0547236000
_diffrn_orient_matrix_UB_22      -0.0077709000
_diffrn_orient_matrix_UB_23      0.0320904000
_diffrn_orient_matrix_UB_31      0.0293035000
_diffrn_orient_matrix_UB_32      0.1011525000
_diffrn_orient_matrix_UB_33      -0.0028582000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            67549
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.608
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    6.458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
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    1.253
_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
_refine_diff_density_max         1.430
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 5196 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         13247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+3.1625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                12481
_reflns_number_total             13247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00925k2.cif
_cod_data_source_block           R-MPEA-InCl
_cod_original_cell_volume        9950.79(15)
_cod_database_code               7710248
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.358
_shelx_estimated_absorpt_t_min   0.247
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C21(H21), C48(H48), C39(H39), C2(H2), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C19(H19A,H19B), C28(H28A,H28B), C10(H10A,H10B), C46(H46A,
 H46B), C1(H1D,H1E)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C23(H23), C9(H9), C18(H18), C14(H14), C33(H33), C17(H17), C24(H24),
 C15(H15), C41(H41), C25(H25), C27(H27), C7(H7), C16(H16), C8(H8), C6(H6),
 C54(H54), C50(H50), C26(H26), C34(H34), C43(H43), C5(H5), C42(H42), C45(H45),
 C53(H53), C52(H52), C36(H36), C51(H51), C44(H44), C35(H35)
2.d Idealised Me refined as rotating group:
 N6(H6A,H6B,H6C), N4(H4A,H4B,H4C), N5(H5A,H5B,H5C), N1(H1A,H1B,H1C), N2(H2A,
 H2B,H2C), N3(H3D,H3E,H3F), C38(H38A,H38B,H38C), C11(H11A,H11B,H11C), C29(H29A,
 H29B,H29C), C20(H20A,H20B,H20C), C47(H47A,H47B,H47C), C3(H3A,H3B,H3C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 3.978
_oxdiff_exptl_absorpt_empirical_full_min 0.552