#------------------------------------------------------------------------------
#$Date: 2024-08-07 14:09:54 +0200 (Wed 07 de Aug de 2024) $
#$Revision: 294029 $
#$URL: svn://www.crystallography.net/cod/cif/9/01/43/9014304.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the American Mineralogist Crystal Structure Database,
# http://rruff.geo.arizona.edu/AMS/amcsd.php
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_9014304
loop_
_publ_author_name
'Yoshida, H.'
'Yamaura, J.'
'Isobe, M.'
'Nilsen, G. J.'
'Hiroi, Z.'
_publ_section_title
;
Orbital Switching in a Frustrated Magnet
;
_journal_name_full               'Nature Communications'
_journal_page_first              860
_journal_page_last               865
_journal_paper_doi               10.1038/ncomms1875
_journal_volume                  3
_journal_year                    2012
_chemical_compound_source        Synthetic
_chemical_formula_moiety         'Cu3 H2 O9 V2, 2(H2O)'
_chemical_formula_sum            'Cu3 H6 O11 V2'
_chemical_formula_weight         474.56
_chemical_name_mineral           Volborthite
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_audit_creation_method           teXsan
_cell_angle_alpha                90
_cell_angle_beta                 95.035(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.657(3)
_cell_length_b                   5.887(1)
_cell_length_c                   7.228(2)
_cell_measurement_reflns_used    1895
_cell_measurement_temperature    323.0
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      3.82
_cell_volume                     451.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'APEX (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'Crystal Maker'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus, 2007)'
_database_code_amcsd             0019038
_diffrn_ambient_temperature      323.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1895
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    8.988
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_correction_T_min  0.5501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.28
_refine_diff_density_min         -0.75
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.407
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_parameters     49
_refine_ls_number_reflns         586
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          -0.2390
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²) + (0.0399P)²+8.7052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                586
_reflns_number_total             598
_reflns_threshold_expression     >2.0sigma(I)
_cod_original_formula_sum        'Cu3 V2 O11 H6'
_cod_database_code               9014304
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 1/2+x,1/2+y,z
3 x,-y,z
4 1/2+x,1/2-y,z
5 -x,y,-z
6 1/2-x,1/2+y,-z
7 -x,-y,-z
8 1/2-x,1/2-y,-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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.0000 0.0000 0.0000 0.0123(1) Uani 1.00 d S . . 0
Cu2 Cu 0.2500 0.2500 0.0000 0.01265(7) Uani 1.00 d S . . 0
V1 V -0.00337(4) 0.5000 0.25375(6) 0.0168(1) Uani 1.00 d S . . 0
O1 O 0.0000 0.5000 0.5000 0.043(1) Uani 1.00 d S . . 0
O2 O 0.3422(2) 0.5000 0.1168(2) 0.0112(4) Uani 1.00 d S . . 0
O3 O 0.0723(1) 0.2699(3) 0.1866(2) 0.0296(4) Uani 1.00 d . . . 0
O4 O 0.3416(2) 0.0000 0.1524(3) 0.0148(4) Uani 1.00 d S . . 0
Wat5 O 0.1758(3) 0.0000 0.5205(4) 0.0525(9) Uani 1.00 d S . . 2
H1 H 0.3500 0.5000 0.2529 0.0134 Uiso 1.00 calc S . . 0
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cu1 0.0114(2) 0.0076(2) 0.0185(2) 0.0000 0.0037(2) 0.0000
Cu2 0.0127(1) 0.0054(1) 0.0195(1) -0.0008(1) -0.0008(1) 0.0001(1)
V1 0.0113(2) 0.0270(2) 0.0122(2) 0.0000 0.0023(2) 0.0000
O1 0.020(1) 0.099(3) 0.010(1) 0.0000 0.004(1) 0.0000
O2 0.0125(7) 0.0028(7) 0.0186(8) 0.0000 0.0024(6) 0.0000
O3 0.0197(6) 0.0326(8) 0.0372(7) 0.0057(6) 0.0069(6) 0.0172(6)
O4 0.0164(8) 0.0078(7) 0.0200(8) 0.0000 0.0009(7) 0.0000
Wat5 0.072(2) 0.064(2) 0.022(1) 0.0000 0.004(1) 0.0000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.320 1.265
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
V V 0.300 0.529
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 7_555 . 5_445 yes
O2 Cu1 O3 89.81(5) 7_555 . . yes
O2 Cu1 O3 89.81(5) 7_555 . 2_555 yes
O2 Cu1 O3 90.19(5) 7_555 . 3_555 yes
O2 Cu1 O3 90.19(5) 7_555 . 4_555 yes
O2 Cu1 O3 90.19(5) 5_445 . . yes
O2 Cu1 O3 90.19(5) 5_445 . 2_555 yes
O2 Cu1 O3 89.81(5) 5_445 . 3_555 yes
O2 Cu1 O3 89.81(5) 5_445 . 4_555 yes
O3 Cu1 O3 93.54(8) . . 2_555 yes
O3 Cu1 O3 180.0 . . 3_555 yes
O3 Cu1 O3 86.46(8) . . 4_555 yes
O3 Cu1 O3 86.46(8) 2_555 . 3_555 yes
O3 Cu1 O3 180.0 2_555 . 4_555 yes
O3 Cu1 O3 93.54(8) 3_555 . 4_555 yes
O2 Cu2 O2 180.0 . . 7_555 yes
O2 Cu2 O3 96.48(7) . . . yes
O2 Cu2 O3 83.52(7) . . 7_555 yes
O2 Cu2 O4 96.51(5) . . . yes
O2 Cu2 O4 83.49(5) . . 7_555 yes
O2 Cu2 O3 83.52(7) 7_555 . . yes
O2 Cu2 O3 96.48(7) 7_555 . 7_555 yes
O2 Cu2 O4 83.49(5) 7_555 . . yes
O2 Cu2 O4 96.51(5) 7_555 . 7_555 yes
O3 Cu2 O3 180.0 . . 7_555 yes
O3 Cu2 O4 95.44(7) . . . yes
O3 Cu2 O4 84.56(7) . . 7_555 yes
O3 Cu2 O4 84.56(7) 7_555 . . yes
O3 Cu2 O4 95.44(7) 7_555 . 7_555 yes
O4 Cu2 O4 180.0 . . 7_555 yes
O1 V1 O3 108.85(6) . . . yes
O1 V1 O3 108.85(6) . . 2_565 yes
O1 V1 O4 110.80(7) . . 5_455 yes
O3 V1 O3 108.4(1) . . 2_565 yes
O3 V1 O4 109.94(6) . . 5_455 yes
O3 V1 O4 109.94(6) 2_565 . 5_455 yes
V1 O1 V1 180.0000(1) . . 3_566 yes
Cu1 O2 Cu2 103.71(7) 5_555 . . yes
Cu1 O2 Cu2 103.71(7) 5_555 . 2_565 yes
Cu2 O2 Cu2 99.85(8) . . 2_565 yes
Cu1 O3 Cu2 82.60(5) . . . yes
Cu1 O3 V1 128.13(8) . . . yes
Cu2 O3 V1 128.45(9) . . . yes
Cu2 O4 Cu2 92.60(7) . . 2_555 yes
Cu2 O4 V1 128.15(6) . . 5_545 yes
Cu2 O4 V1 128.15(6) 2_555 . 5_545 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.947(2) . 7_555 yes
Cu1 O2 1.947(2) . 5_445 yes
Cu1 O3 2.181(2) . . yes
Cu1 O3 2.181(2) . 2_555 yes
Cu1 O3 2.181(2) . 3_555 yes
Cu1 O3 2.181(2) . 4_555 yes
Cu2 O2 1.923(1) . . yes
Cu2 O2 1.923(1) . 7_555 yes
Cu2 O3 2.423(2) . . yes
Cu2 O3 2.423(2) . 7_555 yes
Cu2 O4 2.036(1) . . yes
Cu2 O4 2.036(1) . 7_555 yes
V1 O1 1.7771(4) . . yes
V1 O3 1.670(2) . . yes
V1 O3 1.670(2) . 2_565 yes
V1 O4 1.747(2) . 5_455 yes
O2 H1 0.980 . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cu1 Cu2 3.0437(7) . . ?
Cu1 Cu2 3.0437(7) . 2_555 ?
Cu1 Cu2 3.0437(7) . 3_555 ?
Cu1 Cu2 3.0437(7) . 4_555 ?
O1 O3 2.804(2) . . ?
O1 O3 2.804(2) . 4_556 ?
O1 O3 2.804(2) . 2_565 ?
O1 O3 2.804(2) . 3_566 ?
O1 O4 2.901(2) . 5_455 ?
O1 O4 2.901(2) . 7_556 ?
O2 O3 2.928(2) . 5_555 ?
O2 O3 2.928(2) . 6_555 ?
O2 O3 2.918(2) . 7_555 ?
O2 O3 2.918(2) . 8_555 ?
O2 O4 2.9548(9) . . ?
O2 O4 2.637(2) . 7_555 ?
O2 O4 2.9548(9) . 1_565 ?
O2 Wat5 2.645(3) . 7_556 ?
O3 O3 3.178(3) . 2_555 ?
O3 O3 2.987(3) . 4_555 ?
O3 O3 2.709(3) . 2_565 ?
O3 O4 3.013(2) . 7_555 ?
O3 O4 2.799(2) . 5_455 ?
O3 Wat5 3.016(3) . . ?
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1
;cod-tools version 3.8.0
Id: cif_guess_AMCSD_atom_types 9574 2023-05-10 09:00:05Z saulius
;
2023-05-10T18:55:04+03:00
;Derived hydrogen counts
from atom names that follow the AMCSD naming convention
(Wat == water, O-H == hydroxyl).
;
2 'Vaitkus, Antanas' 2024-08-07T15:10:00+03:00
;
 Updated atom labels in the GEOM_ANGLE, GEOM_BOND and GEOM_CONTACT data loops
 to establish relationships between loop packets from different data loops.
;
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0019038
