#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:44:47 +0200 (mar 06 de oct de 2020) $
#$Revision: 257530 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/47/7704787.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_7704787
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         'O8 V3, 0.5(H16 N4)'
_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             2019-11-25
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-05-19 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                   8.8572(3)
_cell_length_b                   8.8572(3)
_cell_length_c                   5.5653(5)
_cell_measurement_reflns_used    2549
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.511
_cell_measurement_theta_min      4.603
_cell_volume                     436.60(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_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  0.0561
_diffrn_reflns_av_unetI/netI     0.0383
_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            4273
_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         27.574
_diffrn_reflns_theta_min         3.253
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1228 before and 0.0802 after correction. The Ratio of minimum to maximum transmission is 0.7359. 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    2.411
_exptl_crystal_description       plate
_exptl_crystal_F_000             310
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 217 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0335
_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)+1.2576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                531
_reflns_number_total             555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01833c2.cif
_cod_data_source_block           120k
_cod_depositor_comments
;Adding full bibliography for 7704781--7704792.cif.

 Adding full bibliography for 7704781--7704792.cif.
;
_cod_original_cell_volume        436.60(5)
_cod_database_code               7704787
_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: 0.20(9)
 0.80(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
3. Restrained distances
 N1-H1D
 0.9 with sigma of 0.02
4. Others
 Fixed Sof: H1B(0.5) H1C(0.5)
5.a Riding coordinates:
 N1(H1A,H1B,H1C)
;
_shelx_res_file
;
    120k.res created by SHELXL-2014/7

TITL 120K in P4bm
CELL 0.71073 8.8572 8.8572 5.5653 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
DFIX 0.9 N1 H1d

L.S. 20
PLAN  1
TEMP -153.15
CONF
MORE -1
BOND $H
fmap 2
acta
TWIN 1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%120K.hkl">
REM </olex2.extras>

WGHT    0.000000    1.257600
BASF   0.79626
FVAR       0.24763
V2    4   -0.133351   -0.366649   -0.461809    10.50000    0.00916    0.00916 =
         0.01053   -0.00249    0.00249   -0.00185
V1    4    0.000000    0.000000   -0.458552    10.25000    0.00863    0.00863 =
         0.01948    0.00000    0.00000    0.00000
O2    3   -0.085640   -0.192927   -0.354666    11.00000    0.03666    0.01559 =
         0.02677   -0.00768    0.01352   -0.01372
O4    3   -0.129713   -0.370287   -0.756234    10.50000    0.01802    0.01802 =
         0.00771   -0.00002    0.00002    0.00787
O1    3    0.000000    0.000000   -0.743988    10.25000    0.02607    0.02607 =
         0.01871    0.00000    0.00000    0.00000
O3    3    0.000000   -0.500000   -0.347634    10.25000    0.02826    0.02826 =
         0.01013    0.00000    0.00000    0.00789
N1    2   -0.329732   -0.170268   -0.991546    10.50000    0.02137    0.02137 =
         0.01248   -0.00294    0.00294    0.00514
AFIX   3
H1A   1   -0.319222   -0.180780   -1.153346    10.50000   -1.20000
H1B   1   -0.426432   -0.192920   -0.948776    10.50000   -1.20000
H1C   1   -0.307812   -0.074290   -0.948776    10.50000   -1.20000
AFIX   0
H1D   1   -0.259584   -0.240416   -0.955774    10.50000    0.09103
HKLF 4

REM  120K in P4bm
REM R1 =  0.0335 for     531 Fo > 4sig(Fo)  and  0.0367 for all     555 data
REM     42 parameters refined using      2 restraints

END

WGHT      0.0000      1.2576

REM Highest difference peak  0.515,  deepest hole -0.530,  1-sigma level  0.103
Q1    1  -0.0353 -0.3820 -0.4615  11.00000  0.05    0.51
;
_shelx_res_checksum              24415
_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 -0.13335(8) -0.36665(8) -0.4618(3) 0.0096(3) Uani 1 2 d S T P . .
V1 V 0.0000 0.0000 -0.4586(5) 0.0122(4) Uani 1 4 d S T P . .
O2 O -0.0856(5) -0.1929(5) -0.3547(9) 0.0263(10) Uani 1 1 d . . . . .
O4 O -0.1297(4) -0.3703(4) -0.7562(10) 0.0146(11) Uani 1 2 d S T P . .
O1 O 0.0000 0.0000 -0.7440(17) 0.0236(19) Uani 1 4 d S T P . .
O3 O 0.0000 -0.5000 -0.3476(14) 0.022(2) Uani 1 4 d S T P . .
N1 N -0.3297(5) -0.1703(5) -0.9915(17) 0.0184(16) Uani 1 2 d DS T P . .
H1A H -0.3192 -0.1808 -1.1533 0.022 Uiso 1 2 d R U P . .
H1B H -0.4264 -0.1929 -0.9488 0.022 Uiso 0.5 1 d R U P . .
H1C H -0.3078 -0.0743 -0.9488 0.022 Uiso 0.5 1 d R U P . .
H1D H -0.260(4) -0.240(4) -0.96(4) 0.09(4) Uiso 1 2 d DS . P . .
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 0.0092(3) 0.0092(3) 0.0105(5) -0.0025(7) 0.0025(7) -0.0019(4)
V1 0.0086(4) 0.0086(4) 0.0195(8) 0.000 0.000 0.000
O2 0.037(3) 0.016(2) 0.027(2) -0.0077(18) 0.014(2) -0.014(2)
O4 0.0180(18) 0.0180(18) 0.008(2) 0.0000(15) 0.0000(15) 0.008(2)
O1 0.026(3) 0.026(3) 0.019(5) 0.000 0.000 0.000
O3 0.028(3) 0.028(3) 0.010(4) 0.000 0.000 0.008(4)
N1 0.0214(19) 0.0214(19) 0.012(4) -0.003(2) 0.003(2) 0.005(2)
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
O2 V2 O2 109.0(3) 7_445 . ?
O2 V2 O3 108.0(2) 7_445 . ?
O2 V2 O3 108.0(2) . . ?
O4 V2 O2 111.3(2) . . ?
O4 V2 O2 111.3(2) . 7_445 ?
O4 V2 O3 109.2(3) . . ?
O2 V1 O2 145.6(3) . 2 ?
O2 V1 O2 84.99(9) 2 3 ?
O2 V1 O2 84.99(9) . 3 ?
O2 V1 O2 84.99(9) . 4 ?
O2 V1 O2 84.99(9) 2 4 ?
O2 V1 O2 145.6(3) 3 4 ?
O1 V1 O2 107.18(17) . 4 ?
O1 V1 O2 107.18(16) . 3 ?
O1 V1 O2 107.18(17) . . ?
O1 V1 O2 107.18(17) . 2 ?
V2 O2 V1 141.4(3) . . ?
V2 O3 V2 138.3(5) 2_545 . ?
H1A N1 H1B 109.4 . . ?
H1A N1 H1C 109.6 . . ?
H1A N1 H1D 94.4 . . ?
H1B N1 H1C 109.9 . . ?
H1B N1 H1D 116.0 . . ?
H1C N1 H1D 116.2 . . ?
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 O2 1.703(4) . ?
V2 O2 1.703(4) 7_445 ?
V2 O4 1.639(6) . ?
V2 O3 1.787(3) . ?
V1 O2 1.957(4) . ?
V1 O2 1.957(4) 4 ?
V1 O2 1.957(4) 3 ?
V1 O2 1.957(4) 2 ?
V1 O1 1.589(9) . ?
O3 V2 1.787(3) 2_545 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9113 . ?
N1 H1C 0.9039 . ?
N1 H1D 0.90(3) . ?
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
O2 V2 O2 V1 -134.8(3) 7_445 . . . ?
O2 V2 O3 V2 -121.14(19) . . . 2_545 ?
O2 V2 O3 V2 121.14(19) 7_445 . . 2_545 ?
O4 V2 O2 V1 -11.7(6) . . . . ?
O4 V2 O3 V2 0.000(1) . . . 2_545 ?
O3 V2 O2 V1 108.1(5) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.20(9)
2 0.80(9)
