Order‒disorder transformation of intercalated cations triggering huge negative thermal expansion, switchable dielectrics and ion conduction near room temperature in a 2D vanadium oxide hybrid
Yao, Zhi-Yuan; Qian, Yin; Ren, Qiu; Zhang, Guo-Qin; Zhang, Jin; Liu, Wen-Long; Luo, Hong-Bin; Ren, Xiao-Ming; Journal of Materials Chemistry C 7 (2019) 13243–; doi:10.1039/C9TC04911H

data_7238026
_publ_section_title
;
 Order--disorder transformation of intercalated cations triggering huge
 negative thermal expansion, switchable dielectrics and ion conduction
 near room temperature in a 2D vanadium oxide hybrid
;
_journal_issue                   42
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              13243
_journal_paper_doi               10.1039/C9TC04911H
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         '0.5(O20 V8), C3 H12 N2'
_chemical_formula_sum            'C3 H12 N2 O10 V4'
_chemical_formula_weight         439.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-04 deposited with the CCDC.	2019-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.935(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9959(11)
_cell_length_b                   10.0451(11)
_cell_length_c                   15.538(2)
_cell_measurement_reflns_used    1510
_cell_measurement_temperature    330(2)
_cell_measurement_theta_max      27.405
_cell_measurement_theta_min      3.317
_cell_volume                     1211.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      330.15
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2939
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         3.317
_exptl_absorpt_coefficient_mu    3.040
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1145 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.7888.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1359
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0338P)^2^+8.9582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1083
_reflns_number_total             1359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc04911h2.cif
_cod_data_source_block           1_CCDC1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7238026
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Rigid bond restraints
 N1, N2, C1A, C1B, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C1A \\sim C1B \\sim C2: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(N2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H2AA)=1-
 FVAR(1)
 Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H2BB)=
 FVAR(1)
 Fixed Sof: C2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2BB), C2(H2AA)
5.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              55446
_olex2_submission_special_instructions 'No special instructions were received'