Phase Transition and Switchable Dielectric Properties of a Three-Dimensional Hydrogen-Bonding Framework Based on Cobalt (Ⅲ), o-Bromoaniline, and 18-Crown-6
Hu, Hong-Zhi; Yan, Yi-Bo; Wang, Na; Adila, Abuduheni; Liu, Yang; Liu, Zun-Qi; Crystals 14 (2024) 87–; doi:10.3390/cryst14010087

data_1570897
_publ_section_title
;
 Phase Transition and Switchable Dielectric Properties of a
 Three-Dimensional Hydrogen-Bonding Framework Based on Cobalt (&#x2162;),
 o-Bromoaniline, and 18-Crown-6
;
_journal_issue                   1
_journal_name_full               Crystals
_journal_page_first              87
_journal_paper_doi               10.3390/cryst14010087
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety
'2(C6 H7 Br N), C6 H Co N6, C12 H24 O6, 2(H2 O)'
_chemical_formula_sum            'C30 H43 Br2 Co N8 O8'
_chemical_formula_weight         862.45
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-04
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5465)
;
_cell_angle_alpha                77.799(4)
_cell_angle_beta                 78.954(4)
_cell_angle_gamma                88.451(4)
_cell_formula_units_Z            1
_cell_length_a                   8.724(3)
_cell_length_b                   9.687(3)
_cell_length_c                   11.556(4)
_cell_measurement_reflns_used    3808
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.818
_cell_measurement_theta_min      2.379
_cell_volume                     936.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7666
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.738
_diffrn_reflns_theta_min         2.518
_exptl_absorpt_coefficient_mu    2.647
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.1294 before and 0.0489 after correction. The Ratio of minimum to maximum transmission is 0.4205. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_refine_diff_density_max         1.253
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.112(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+3.5138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3013
_reflns_number_total             3968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            RT.cif
_cod_data_source_block           180204ly2_0m
_cod_database_code               1570897
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C12-C13
 1.5 with sigma of 0.02
 C11-C12
 2.4 with sigma of 0.02
 C11-C10
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O2, O1, C10, C15, C11, C12, C13, O3, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H3A(0.5)
5.a Riding coordinates:
 N3(H3A), O4(H4A,H4B)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C15(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
5.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              77612
_shelx_hkl_checksum              50996
_olex2_submission_special_instructions 'No special instructions were received'