Multifunctional molecular ferroelectric with Chiral feature, High Curie Temperature, Large Spontaneous Polarization and Photoluminescence: (C9H14N)2CdBr4
Li, Yu-Kong; Lai, Yuan Yuan; Ying, Ting-Ting; Han, Ding-Chong; Tan, Yu-Hui; Tang, Yun Zhi; Du, Peng-Kang; Zhang, Hao; Chemical Science  (2021) –; doi:10.1039/D1SC03964D

data_1564606
_publ_section_title
;
 Multifunctional molecular ferroelectric with Chiral feature, High Curie
 Temperature, Large Spontaneous Polarization and Photoluminescence:
 (C9H14N)2CdBr4
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03964D
_journal_year                    2021
_chemical_formula_moiety         'Br4 Cd, 2(C9 H14 N)'
_chemical_formula_sum            'C18 H28 Br4 Cd N2'
_chemical_formula_weight         704.46
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2021-07-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-18 deposited with the CCDC.	2021-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.514(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2525(5)
_cell_length_b                   7.9861(3)
_cell_length_c                   13.9703(6)
_cell_measurement_reflns_used    5995
_cell_measurement_temperature    373.0
_cell_measurement_theta_max      24.7010
_cell_measurement_theta_min      2.1790
_cell_volume                     1244.64(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      373.0
_diffrn_detector                 'CCD plate'
_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    -61.00  11.00   0.50    0.35    --    8.30 -57.00-120.00  144
  2  \w    -18.00  43.00   0.50    0.35    --    8.30 -99.00 150.00  122
  3  \w    -13.00  56.00   0.50    0.35    --    8.30  77.00-120.00  138
  4  \w     14.00  39.00   0.50    0.35    --    8.30 -99.00  30.00   50
  5  \w    -76.00 -46.00   0.50    0.35    --   -8.69 -57.00-180.00   60
  6  \w    -82.00   2.00   0.50    0.35    --   -8.69 -37.00  60.00  168
  7  \w    -82.00  -3.00   0.50    0.35    --   -8.69 -57.00 -30.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0236765000
_diffrn_orient_matrix_UB_12      0.0549167000
_diffrn_orient_matrix_UB_13      -0.0376221000
_diffrn_orient_matrix_UB_21      -0.0130198000
_diffrn_orient_matrix_UB_22      -0.0694732000
_diffrn_orient_matrix_UB_23      -0.0312440000
_diffrn_orient_matrix_UB_31      -0.0575615000
_diffrn_orient_matrix_UB_32      -0.0068364000
_diffrn_orient_matrix_UB_33      0.0151656000
_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  0.0659
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15582
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1159 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(13)
_refine_ls_extinction_coef       0.0139(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5135
_refine_ls_number_restraints     442
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0242P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3337
_reflns_number_total             5135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03964d2.cif
_cod_data_source_block           1-ITP
_cod_original_cell_volume        1244.64(10)
_cod_database_code               1564606
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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
2. Restrained distances
 C16A-C17A \\sim C16B-C17B \\sim C16B-C15B \\sim C16A-C15A \\sim C17B-C18B
\\sim C17A-C18A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1A \\sim C17B \\sim C15B \\sim C10B \\sim C11B \\sim C14B \\sim C18A \\sim
C16A \\sim C13B \\sim C12B \\sim C15A \\sim C14A \\sim C13A \\sim C11A \\sim
C10A \\sim N1B \\sim C18B \\sim C17A \\sim C16B \\sim C12A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Br4A \\sim Br4C \\sim Br4B \\sim Br3A \\sim Br3B \\sim Br3C \\sim Br1B \\sim
Br1A \\sim Br1C \\sim Br2C \\sim Br2B \\sim Br2A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(C15B) \\sim Ueq, Uanis(C10B) \\sim Ueq, Uanis(C11B) \\sim Ueq,
Uanis(C14B) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C12B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cd1A(0.15) Br4A(0.15) Br3A(0.15) Br2C(0.15) Br1B(0.7) Br1A(0.15)
 Cd1B(0.7) Br4C(0.15) Cd1C(0.15) Br4B(0.7) Br1C(0.15) Br3B(0.7) Br3C(0.15)
 Br2B(0.7) Br2A(0.15) N1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C17B(0.5)
 H17C(0.5) H17D(0.5) C15B(0.5) C10B(0.5) H10B(0.5) C11B(0.5) H11B(0.5)
 C14B(0.5) H14B(0.5) C18A(0.5) H18A(0.5) H18B(0.5) C16A(0.5) H16A(0.5)
 H16B(0.5) C13B(0.5) H13B(0.5) C12B(0.5) H12B(0.5) C15A(0.5) C14A(0.5)
 H14A(0.5) C13A(0.5) H13A(0.5) C12A(0.5) H12A(0.5) C11A(0.5) H11A(0.5)
 C10A(0.5) H10A(0.5) N1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C18B(0.5) H18C(0.5)
 H18D(0.5) C17A(0.5) H17A(0.5) H17B(0.5) C16B(0.5) H16C(0.5) H16D(0.5)
5.a Riding coordinates:
 C16A(H16A,H16B)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C7(H7A,H7B), C17B(H17C,H17D), C18A(H18A,H18B),
 C18B(H18C,H18D), C17A(H17A,H17B), C16B(H16C,H16D)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C2(H2), C3(H3), C4(H4), C10B(H10B), C11B(H11B), C14B(H14B),
 C13B(H13B), C12B(H12B), C14A(H14A), C13A(H13A), C12A(H12A), C11A(H11A),
 C10A(H10A)
5.d Fitted hexagon refined as free rotating group:
 C15A(C14A,C13A,C12A,C11A,C10A)
5.e Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1A(H1AA,H1AB,H1AC), N1B(H1BA,H1BB,H1BC)
;
_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 8.294
_oxdiff_exptl_absorpt_empirical_full_min 0.513