Dielectric and optical properties of a new organic–inorganic hybrid phase transition material
Zhang, Yinan; Cai, Zhuoer; Zhang, Xinyi; Xiao, Shiyue; Liu, Xianmin; Zhao, Yingyi; Hua, Xiu-Ni; Sun, Baiwang; CrystEngComm 25 (2023) 4284–4289; doi:10.1039/D3CE00454F

data_7246928
_publ_section_title
;
 Dielectric and optical properties of a new organic--inorganic hybrid
 phase transition material
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              4284
_journal_page_last               4289
_journal_paper_doi               10.1039/D3CE00454F
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Cl4 Mn, 2(C7 H17 Cl N)'
_chemical_formula_sum            'C14 H33.52 Cl6 Mn N2'
_chemical_formula_weight         497.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-05
_audit_creation_method
;FinalCif V118 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-04-07 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                110.169(2)
_cell_angle_beta                 113.276(2)
_cell_angle_gamma                90.899(3)
_cell_formula_units_Z            4
_cell_length_a                   12.9520(9)
_cell_length_b                   13.4792(10)
_cell_length_c                   15.8481(12)
_cell_measurement_reflns_used    5751
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.369
_cell_measurement_theta_min      2.5755
_cell_volume                     2348.4(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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    'SHELXD-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9578
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.449
_diffrn_reflns_theta_min         2.167
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.260237
_exptl_absorpt_correction_T_min  0.220953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 45763 reflections, Rint = 0.0641
 (24369 with I > 3sig(I), Rint = 0.0503)
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.710
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9578
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0780
_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^)+(0.0940P)^2^+12.0537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6830
_reflns_number_total             9578
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  0.01151
_twin_individual_twin_matrix_12  0.01979
_twin_individual_twin_matrix_13  -0.99002
_twin_individual_twin_matrix_21  -0.91385
_twin_individual_twin_matrix_22  0.17251
_twin_individual_twin_matrix_23  0.08495
_twin_individual_twin_matrix_31  0.95026
_twin_individual_twin_matrix_32  0.90388
_twin_individual_twin_matrix_33  0.95758
_cod_data_source_file            d3ce00454f2.cif
_cod_data_source_block           n4_0m_4
_cod_depositor_comments
'Adding full bibliography for 7246928--7246929.cif.'
_cod_database_code               7246928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C30A = C3-C29
 1.5 with sigma of 0.02
 Cl14-C3 = Cl15-C4
 1.77 with sigma of 0.02
 C3-C29 = C4-C30A
 1.5 with sigma of 0.02
 Cl15-C4 = Cl14-C3
 1.7 with sigma of 0.02
3. Rigid bond restraints
 Cl13, C14, N3, C15, C16, C13, C25, C24, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C29, C3, N1, Cl14, C4, C1, C2, C30A, Cl15, C28, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C14 \\sim Cl13 \\sim N3 \\sim C15 \\sim C16 \\sim C13 \\sim C25 \\sim C24 \\sim
C23: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C29 \\sim C3 \\sim N1 \\sim Cl14 \\sim C4 \\sim C1 \\sim C2 \\sim C30A \\sim
Cl15 \\sim C28 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C30A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Cl13, C14, N3, C15, C16, C13, C25, C24, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C29, C3, N1, Cl14, C4, C1, C2, C30A, Cl15, C28, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(Cl15)=Sof(H4BC)=Sof(H4BD)=
 Sof(H3BC)=Sof(H3BD)=1-FVAR(1)
 Sof(H4AA)=Sof(H4AB)=Sof(H3AA)=Sof(H3AB)=Sof(Cl14)=Sof(C30A)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C6(H6A,H6B), C11(H11A,H11B), C8(H8A,H8B), C5(H5A,
 H5B), C4(H4AA,H4AB), C4(H4BC,H4BD), C7(H7A,H7B), C1(H1A,H1B), C12(H12A,H12B),
 C2(H2A,H2B), C15(H15A,H15B), C3(H3BC,H3BD), C3(H3AA,H3AB), C14(H14A,H14B),
 C16(H16A,H16B), C13(H13A,H13B)
7.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C22(H22A,H22B,
 H22C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C25(H25A,
 H25B,H25C), C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C),
 C26(H26A,H26B,H26C), C30A(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.964