#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:44:47 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257530 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/47/7704792.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_7704792
loop_
_publ_author_name
'Yao, Zhi-Yuan'
'Zhang, Guo-Qin'
'Yao, Wan-Wan'
'Wang, Xiao-Zu'
'Qian, Yin'
'Ren, Xiao-Ming'
_publ_section_title
;
 Uniaxial thermal expansion behaviors and ionic conduction in a layered
 (NH₄)₂V₃O₈.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10638
_journal_page_last               10644
_journal_paper_doi               10.1039/d0dt01833c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '0.5(O16 V6), H8 N2'
_chemical_formula_sum            'H8 N2 O8 V3'
_chemical_formula_weight         316.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           100
_space_group_name_Hall           'P 4 -2ab'
_space_group_name_H-M_alt        'P 4 b m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2019-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-21 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8884(3)
_cell_length_b                   8.8884(3)
_cell_length_c                   5.5625(5)
_cell_measurement_reflns_used    2675
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      27.471
_cell_measurement_theta_min      4.587
_cell_volume                     439.46(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      240.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4362
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         3.241
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1184 before and 0.0756 after correction. The Ratio of minimum to maximum transmission is 0.7565. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 224 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         555
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0279
_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)+0.9736P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                525
_reflns_number_total             555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01833c2.cif
_cod_data_source_block           240k-1
_cod_depositor_comments
;Adding full bibliography for 7704781--7704792.cif.

 Adding full bibliography for 7704781--7704792.cif.
;
_cod_original_cell_volume        439.46(5)
_cod_database_code               7704792
_shelx_shelxl_version_number     2014/7
_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. Twinned data refinement
 Scales: 0.17(8)
 0.83(8)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
3. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
4.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D)
;
_shelx_res_file
;
    240k-1.res created by SHELXL-2014/7

TITL 240K-1 in P4bm
CELL 0.71073 8.8884 8.8884 5.5625 90 90 90
ZERR 2 0.0003 0.0003 0.0005 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,+Z
SYMM 0.5-Y,0.5-X,+Z
SYMM 0.5+Y,0.5+X,+Z
SFAC H N O V
UNIT 16 4 16 6

L.S. 20
PLAN  1
TEMP -33.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\240K-1.hkl">
REM </olex2.extras>

WGHT    0.000000    0.973600
BASF   0.82673
FVAR       0.26288
V2    4   -0.133511   -0.633510   -0.405561    10.50000    0.00732    0.00732 =
         0.01356    0.00088    0.00088    0.00053
N1    2   -0.330568   -0.830568   -0.935359    10.50000    0.02887    0.02887 =
         0.01591    0.00029    0.00029   -0.01185
AFIX   3
H1A   1   -0.328238   -0.828240   -1.097069    10.50000   -1.20000
H1B   1   -0.306628   -0.925020   -0.883938    10.50000   -1.20000
H1C   1   -0.423548   -0.808100   -0.883938    10.50000   -1.20000
AFIX   3
H1D   1   -0.262358   -0.762360   -0.875158    10.50000   -1.20000
AFIX   0

O4    3   -0.130497   -0.630497   -0.700090    10.50000    0.02212    0.02212 =
         0.01248   -0.00097   -0.00097   -0.00534
V1    4    0.000000   -1.000000   -0.401459    10.25000    0.00796    0.00796 =
         0.01570    0.00000    0.00000    0.00000
O1    3    0.000000   -1.000000   -0.687519    10.25000    0.03129    0.03129 =
         0.01630    0.00000    0.00000    0.00000
O3    3    0.000000   -0.500000   -0.291609    10.25000    0.01593    0.01593 =
         0.01566    0.00000    0.00000   -0.00454
O2    3   -0.085597   -0.807132   -0.298306    11.00000    0.01736    0.01035 =
         0.03000    0.00160    0.00205    0.00525
HKLF 4

REM  240K-1 in P4bm
REM R1 =  0.0279 for     525 Fo > 4sig(Fo)  and  0.0302 for all     555 data
REM     39 parameters refined using      1 restraints

END

WGHT      0.0000      0.9734

REM Highest difference peak  0.414,  deepest hole -0.491,  1-sigma level  0.088
Q1    1  -0.0443 -0.6364 -0.4042  11.00000  0.05    0.41
;
_shelx_res_checksum              62099
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
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
V2 V -0.13351(7) -0.63351(7) -0.4056(3) 0.0094(2) Uani 1 2 d S T P . .
N1 N -0.3306(4) -0.8306(4) -0.9354(14) 0.0245(15) Uani 1 2 d S T P . .
H1A H -0.3282 -0.8282 -1.0971 0.029 Uiso 1 2 d RS T P . .
H1B H -0.3066 -0.9250 -0.8839 0.029 Uiso 0.5 1 d R . . . .
H1C H -0.4235 -0.8081 -0.8839 0.029 Uiso 0.5 1 d R . . . .
H1D H -0.2624 -0.7624 -0.8752 0.029 Uiso 1 2 d RS T P . .
O4 O -0.1305(4) -0.6305(4) -0.7001(9) 0.0189(10) Uani 1 2 d S T P . .
V1 V 0.0000 -1.0000 -0.4015(4) 0.0105(3) Uani 1 4 d S T P . .
O1 O 0.0000 -1.0000 -0.6875(14) 0.0263(17) Uani 1 4 d S T P . .
O3 O 0.0000 -0.5000 -0.2916(12) 0.0158(14) Uani 1 4 d S T P . .
O2 O -0.0856(4) -0.8071(4) -0.2983(8) 0.0192(7) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V2 0.0073(3) 0.0073(3) 0.0136(4) 0.0009(5) 0.0009(5) 0.0005(3)
N1 0.0289(18) 0.0289(18) 0.016(4) 0.0003(19) 0.0003(19) -0.012(2)
O4 0.0221(16) 0.0221(16) 0.012(2) -0.0010(14) -0.0010(14) -0.005(2)
V1 0.0080(4) 0.0080(4) 0.0157(6) 0.000 0.000 0.000
O1 0.031(3) 0.031(3) 0.016(4) 0.000 0.000 0.000
O3 0.016(2) 0.016(2) 0.016(3) 0.000 0.000 -0.005(3)
O2 0.0174(17) 0.0103(16) 0.0300(17) 0.0016(14) 0.0021(15) 0.0053(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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
_geom_angle_publ_flag
O4 V2 O3 109.4(3) . . ?
O4 V2 O2 111.09(18) . 8_545 ?
O4 V2 O2 111.09(18) . . ?
O2 V2 O3 108.01(18) 8_545 . ?
O2 V2 O3 108.01(19) . . ?
O2 V2 O2 109.2(2) 8_545 . ?
H1A N1 H1B 109.2 . . ?
H1A N1 H1C 109.6 . . ?
H1A N1 H1D 109.5 . . ?
H1B N1 H1C 108.7 . . ?
H1B N1 H1D 109.8 . . ?
H1C N1 H1D 110.1 . . ?
O1 V1 O2 107.01(13) . . ?
O1 V1 O2 107.01(13) . 2_535 ?
O1 V1 O2 107.01(13) . 4_645 ?
O1 V1 O2 107.01(13) . 3_445 ?
O2 V1 O2 85.09(7) 3_445 2_535 ?
O2 V1 O2 146.0(3) . 2_535 ?
O2 V1 O2 85.09(7) 4_645 2_535 ?
O2 V1 O2 85.09(8) . 4_645 ?
O2 V1 O2 85.09(8) . 3_445 ?
O2 V1 O2 146.0(3) 4_645 3_445 ?
V2 O3 V2 138.6(4) 2_545 . ?
V2 O2 V1 141.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V2 O4 1.639(5) . ?
V2 O3 1.794(3) . ?
V2 O2 1.708(3) 8_545 ?
V2 O2 1.708(3) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9121 . ?
N1 H1C 0.8971 . ?
N1 H1D 0.9205 . ?
V1 O1 1.591(8) . ?
V1 O2 1.961(3) 2_535 ?
V1 O2 1.961(3) 3_445 ?
V1 O2 1.961(3) . ?
V1 O2 1.961(3) 4_645 ?
O3 V2 1.794(3) 2_545 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 V2 O3 V2 0.000(1) . . . 2_545 ?
O4 V2 O2 V1 11.9(4) . . . . ?
O3 V2 O2 V1 -108.0(4) . . . . ?
O2 V2 O3 V2 -121.02(16) 8_545 . . 2_545 ?
O2 V2 O3 V2 121.02(16) . . . 2_545 ?
O2 V2 O2 V1 134.8(2) 8_545 . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.17(8)
2 0.83(8)
