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_4003545
_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         'Br4 Sb, Br5 Sb, Br, 4(C8 H11 F N)'
_chemical_formula_sum            'C32 H44 Br10 F4 N4 Sb2'
_chemical_formula_weight         1603.31
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5638(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3557(5)
_cell_length_b                   13.4134(6)
_cell_length_c                   14.4815(6)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.25
_cell_volume                     2388.74(17)
_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    'XS (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  0.0352
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26419
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.326
_diffrn_reflns_theta_min         2.247
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.538
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1168 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.6651. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 3462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         8554
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0200
_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          0.0372
_refine_ls_wR_factor_ref         0.0383
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                7881
_reflns_number_total             8554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01605_si_003.cif
_cod_data_source_block           compound2
_cod_database_code               4003545
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.420
_shelx_estimated_absorpt_t_min   0.191
_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.a Ternary CH refined with riding coordinates:
 C10(H10), C18(H18), C26(H26), C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C28(H28), C8(H8), C7(H7), C15(H15), C20(H20), C21(H21), C5(H5),
 C13(H13), C12(H12), C29(H29), C32(H32), C24(H24), C31(H31), C4(H4), C23(H23)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N4(H4A,H4B,H4C), N3(H3A,H3B,H3C), C17(H17A,
 H17B,H17C), C9(H9A,H9B,H9C), C1(H1D,H1E,H1F), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              53892
_shelx_hkl_checksum              95430
_olex2_submission_special_instructions 'No special instructions were received'