#------------------------------------------------------------------------------
#$Date: 2019-11-24 16:33:09 +0100 (dom 24 de nov de 2019) $
#$Revision: 238849 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/80/7238026.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7238026
loop_
_publ_author_name
'Yao, Zhi-Yuan'
'Qian, Yin'
'Ren, Qiu'
'Zhang, Guo-Qin'
'Zhang, Jin'
'Liu, Wen-Long'
'Luo, Hong-Bin'
'Ren, Xiao-Ming'
_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 λ/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/[σ²(Fo²)+(0.0338P)²+8.9582P] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.79095(10) 0.55149(7) 0.52843(6) 0.0143(2) Uani 1 1 d . . . . .
V2 V 0.44050(10) 0.74052(7) 0.55009(5) 0.0140(2) Uani 1 1 d . . . . .
O1 O 0.8932(5) 0.5798(4) 0.6310(2) 0.0280(8) Uani 1 1 d . . . . .
O2 O 0.7543(4) 0.3719(3) 0.5117(2) 0.0198(8) Uani 1 1 d . . . . .
O3 O 0.8989(4) 0.6154(3) 0.4537(2) 0.0195(7) Uani 1 1 d . . . . .
O4 O 0.5942(4) 0.6243(3) 0.5075(3) 0.0249(8) Uani 1 1 d . . . . .
O5 O 0.4605(5) 0.7110(4) 0.6534(2) 0.0312(9) Uani 1 1 d . . . . .
N1 N 0.7460(8) 0.4858(7) 0.2783(4) 0.0288(16) Uani 0.761(11) 1 d . U P A -1
H1A H 0.8093 0.5241 0.3270 0.043 Uiso 0.761(11) 1 calc GR . P A -1
H1B H 0.8150 0.4516 0.2468 0.043 Uiso 0.761(11) 1 calc GR . P A -1
H1C H 0.6825 0.4212 0.2935 0.043 Uiso 0.761(11) 1 calc GR . P A -1
C1A C 0.6330(13) 0.5852(11) 0.2250(8) 0.053(2) Uani 0.761(11) 1 d . U P A -1
H1AA H 0.5701 0.5461 0.1696 0.064 Uiso 0.761(11) 1 calc R . P A -1
H1AB H 0.7006 0.6592 0.2117 0.064 Uiso 0.761(11) 1 calc R . P A -1
N2 N 0.810(3) 0.569(3) 0.2649(18) 0.056(5) Uani 0.239(11) 1 d . U P A -2
H2A H 0.8857 0.5718 0.3172 0.084 Uiso 0.239(11) 1 calc GR . P A -2
H2B H 0.8556 0.6067 0.2239 0.084 Uiso 0.239(11) 1 calc GR . P A -2
H2C H 0.7828 0.4849 0.2500 0.084 Uiso 0.239(11) 1 calc GR . P A -2
C1B C 0.685(4) 0.627(3) 0.269(2) 0.046(4) Uani 0.239(11) 1 d . U P A -2
H1BA H 0.6727 0.6815 0.2165 0.055 Uiso 0.239(11) 1 calc R . P A -2
H1BB H 0.7369 0.6875 0.3173 0.055 Uiso 0.239(11) 1 calc R . P A -2
C2 C 0.509(2) 0.6332(14) 0.2778(9) 0.057(3) Uani 0.5 1 d . U P . .
H2BB H 0.4776 0.6499 0.3306 0.068 Uiso 0.761(11) 1 calc R . P A -1
H2AA H 0.4481 0.6357 0.3217 0.068 Uiso 0.239(11) 1 calc R . P A -2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 V1 O2 109.58(18) . .
O1 V1 O3 112.17(18) . .
O1 V1 O4 109.62(18) . .
O3 V1 O2 110.98(16) . .
O4 V1 O2 106.74(15) . .
O4 V1 O3 107.57(17) . .
O2 V2 V2 38.86(9) 3_455 7_566
O2 V2 V2 38.76(9) 5_666 7_566
O2 V2 O2 77.62(14) 3_455 5_666
O3 V2 V2 121.28(11) 7_666 7_566
O3 V2 O2 87.07(13) 7_666 3_455
O3 V2 O2 149.27(15) 7_666 5_666
O4 V2 V2 120.03(11) . 7_566
O4 V2 O2 88.88(14) . 5_666
O4 V2 O2 143.16(16) . 3_455
O4 V2 O3 87.71(14) . 7_666
O5 V2 V2 111.49(15) . 7_566
O5 V2 O2 104.94(17) . 5_666
O5 V2 O2 108.24(18) . 3_455
O5 V2 O3 105.12(17) . 7_666
O5 V2 O4 108.33(18) . .
V1 O2 V2 122.12(17) . 3_545
V1 O2 V2 135.28(18) . 5_666
V2 O2 V2 102.38(14) 3_545 5_666
V1 O3 V2 137.5(2) . 7_666
V1 O4 V2 146.8(2) . .
H1A N1 H1B 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C1A N1 H1A 109.5 . .
C1A N1 H1B 109.5 . .
C1A N1 H1C 109.5 . .
N1 C1A H1AA 110.1 . .
N1 C1A H1AB 110.1 . .
N1 C1A C2 108.0(9) . .
H1AA C1A H1AB 108.4 . .
C2 C1A H1AA 110.1 . .
C2 C1A H1AB 110.1 . .
H2A N2 H2B 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
C1B N2 H2A 109.5 . .
C1B N2 H2B 109.5 . .
C1B N2 H2C 109.5 . .
N2 C1B H1BA 98.5 . .
N2 C1B H1BB 98.5 . .
N2 C1B C2 152(3) . .
H1BA C1B H1BB 103.8 . .
C2 C1B H1BA 98.5 . .
C2 C1B H1BB 98.5 . .
C1A C2 H2BB 152.8 . .
C1B C2 H2AA 139.6 . .
C2 C2 C1A 54.3(19) 2_655 .
C2 C2 C1B 81(3) 2_655 .
C2 C2 H2BB 152.8 2_655 .
C2 C2 H2AA 139.6 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.632(4) .
V1 O2 1.837(3) .
V1 O3 1.728(3) .
V1 O4 1.694(3) .
V2 V2 3.0751(16) 7_566
V2 O2 1.975(3) 5_666
V2 O2 1.971(3) 3_455
V2 O3 1.945(3) 7_666
V2 O4 1.924(3) .
V2 O5 1.602(4) .
O2 V2 1.975(3) 5_666
O2 V2 1.971(3) 3_545
O3 V2 1.945(3) 7_666
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
N1 C1A 1.462(12) .
C1A H1AA 0.9700 .
C1A H1AB 0.9700 .
C1A C2 1.509(19) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N2 C1B 1.17(3) .
C1B H1BA 0.9700 .
C1B H1BB 0.9700 .
C1B C2 1.45(3) .
C2 C2 0.84(3) 2_655
C2 H2BB 0.9300 .
C2 H2AA 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O3 0.89 2.13 3.003(7) 165.1 .
N1 H1B O1 0.89 2.07 2.890(7) 153.5 6_565
N1 H1C O5 0.89 2.05 2.934(8) 171.0 5_666
N2 H2A O1 0.89 2.33 2.94(3) 126.3 5_766
N2 H2A O3 0.89 2.14 2.89(3) 140.4 .
N2 H2A O5 0.89 2.49 2.96(3) 113.0 7_666
N2 H2B O5 0.89 2.39 3.21(3) 154.5 8_565
N2 H2C O1 0.89 2.33 2.77(3) 110.9 6_565
