Band Gap-Tunable, Chiral Hybrid Metal Halides Displaying Second-Harmonic Generation
Dehnhardt, Natalie; Axt, Marleen; Zimmermann, Jonas; Yang, Meng; Mette, Gerson; Heine, Johanna; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c01605

data_4003544
_publ_section_title
;
 Band Gap-Tunable, Chiral Hybrid Metal Halides Displaying Second-Harmonic
 Generation
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01605
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'I10 Sb2, 4(C8 H11 F N)'
_chemical_formula_sum            'C32 H44 F4 I10 N4 Sb2'
_chemical_formula_weight         2073.21
_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   geom
_audit_creation_date             2020-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.966(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9520(7)
_cell_length_b                   14.3430(7)
_cell_length_c                   14.3389(7)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.48
_cell_volume                     2653.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43870
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.309
_diffrn_reflns_theta_min         2.123
_exptl_absorpt_coefficient_mu    6.875
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0772 before and 0.0543 after correction. The Ratio of minimum to maximum transmission is 0.7287. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.595
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details
;
 Flack x determined using 4241 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9664
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0172
_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^)+(0.0095P)^2^+0.1431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0381
_refine_ls_wR_factor_ref         0.0385
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                9284
_reflns_number_total             9664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01605_si_004.cif
_cod_data_source_block           compound3
_cod_database_code               4003544
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.349
_shelx_estimated_absorpt_t_min   0.276
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C3 \\sim C8-C3 \\sim C8-C7 \\sim C7-C6 \\sim C5-C4 \\sim C6-C5
 with sigma of 0.02
 C12-C11 \\sim C13-C12 \\sim C14-C13 \\sim C15-C14 \\sim C16-C15 \\sim C16-C11
 with sigma of 0.02
 C24-C19 \\sim C24-C23 \\sim C23-C22 \\sim C22-C21 \\sim C21-C20 \\sim C20-C19
 with sigma of 0.02
3. Others
 Sof(C32B)=Sof(H32B)=Sof(C31B)=Sof(H31B)=Sof(C30B)=Sof(C29B)=Sof(H29B)=
 Sof(C28B)=Sof(H28B)=Sof(F4B)=1-FVAR(1)
 Sof(F4A)=Sof(C32A)=Sof(H32A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(C29A)=
 Sof(H29A)=Sof(C28A)=Sof(H28A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C18(H18), C26(H26), C2(H2)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C32B(H32B), C31B(H31B), C29B(H29B), C28B(H28B), C32A(H32A),
 C31A(H31A), C29A(H29A), C28A(H28A), C13(H13), C5(H5), C12(H12), C4(H4),
 C20(H20), C21(H21), C23(H23), C8(H8), C15(H15), C16(H16), C24(H24)
4.c Fitted hexagon refined as free rotating group:
 C27(C32B,C31B,C30B,C29B,C28B)
4.d Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), C9(H9A,
 H9B,H9C), C1(H1D,H1E,H1F), C25(H25A,H25B,H25C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              75228
_shelx_hkl_checksum              29775
_olex2_submission_special_instructions 'No special instructions were received'