#------------------------------------------------------------------------------
#$Date: 2024-12-07 19:01:34 +0200 (Sat, 07 Dec 2024) $
#$Revision: 296750 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312595.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2312595
loop_
_publ_author_name
'Chatkon, Aungkana'
'Haller, Kenneth J.'
'Haller, Joseph P.'
_publ_section_title
;
 Substitutional/positional disorder of biguanide and guanylurea in the
 structure of a decavanadate complex
 [(Bg)(HV₁₀O₂₈⁵⁻)]<sub>0.4</sub>[(HGU⁺)(V₁₀O₂₈⁶⁻)]<sub>0.6</sub>(H₂Met²⁺)₂(H₃O⁺)·8H₂O.
;
_journal_coeditor_code           AW5092SUP1
_journal_issue                   5
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              456
_journal_page_last               466
_journal_paper_doi               10.1107/S2052520624006929
_journal_volume                  80
_journal_year                    2024
_chemical_compound_source        'synthesized by authors, see text'
_chemical_formula_moiety
;
0.4(C2 H7 N5), 0.4(H V10 O28) 5-, 0.6(C2 H7 N4 O) 1+, 0.6(V10 O28) 6-,
2(C4 H13 N5) 2+, (H3 O) +, 8(H2 O)
;
_chemical_formula_sum            'C10 H53 N14.4 O37.6 V10'
_chemical_formula_weight         1486.26
_chemical_name_common
'[(Bg)(HV10O285-)]0.4/[(HGU+)(HV10O286-)]0.6(H2Met2+)2(H3O+) Octahydrate'
_chemical_name_systematic
;
imidodicarbonimidic diamide
bis(dihydro-3-(diaminomethylidene)-1,1-dimethylguanidine)
bis(μ₆-oxo)-tetrakis(μ₃-oxo)-tetradecakis(μ₂-oxo)-octa-oxo-
deca-vanadium(V) octahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2016/6 plus hand edits'
_audit_update_record
;

;
_cell_angle_alpha                90
_cell_angle_beta                 111.519(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4299(22)
_cell_length_b                   12.4338(22)
_cell_length_c                   14.4959(24)
_cell_measurement_reflns_used    14535
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.717
_cell_measurement_theta_min      3.001
_cell_volume                     2251.9(7)
_computing_cell_refinement       'APEX-II (Bruker, 2005)'
_computing_data_collection       'APEX-II (Bruker, 2005)'
_computing_data_reduction        'SAINT V8-34A (Bruker, 2001)'
_computing_molecular_graphics
'ORTEP-III (Burnett & Johnson, 1996), ORTEP3 (Farrugia, 2012)'
_computing_publication_material
;
  Chemdraw Ultra V7.0.1, (Evans, 2014), PUBLCIF (Westrip, 2010),
  PLATON (Spek, 2020), POV-Ray (Persistence of Vision)
;
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker SMART diffractometer with APEX-II CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            110394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.717
_diffrn_reflns_theta_min         3.071
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995), SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.192
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1489
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         14535
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0278P)²+1.5998P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12128
_reflns_number_total             14535
_reflns_threshold_expression     'I > 2σ(I)'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_cod_data_source_file            aw5092sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2312595.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312595
_cod_database_fobs_code          2312595
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_min   0.638
_shelx_estimated_absorpt_t_max   0.794
_publcif_funding_html            'Nakhon Ratchasima Rajabhat University (NRRU).'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.52664(2) -0.07422(2) 0.91896(2) 0.00868(3) Uani 1 1 d . . . . .
O1 O 0.60218(5) -0.00301(5) 1.05725(5) 0.00893(10) Uani 1 1 d . . . . .
O123 O 0.50667(5) 0.18266(5) 0.99753(5) 0.00986(10) Uani 1 1 d . . . . .
H123 H 0.507(6) 0.256(6) 1.014(6) 0.011 Uiso 0.2 1 d . U P A 1
O14 O 0.64618(5) -0.12654(6) 0.92949(5) 0.01015(10) Uani 1 1 d . . . . .
O15 O 0.56396(6) 0.11902(6) 1.18923(5) 0.01090(10) Uani 1 1 d . . . . .
V2 V 0.65101(2) 0.14300(2) 0.99104(2) 0.01040(3) Uani 1 1 d . . . . .
O2 O 0.67079(6) 0.24960(6) 0.93789(6) 0.01618(13) Uani 1 1 d . . . . .
O231 O 0.54466(5) 0.06701(5) 0.87506(5) 0.01014(10) Uani 1 1 d . . . . .
O24 O 0.75557(5) 0.05255(6) 0.98962(5) 0.01069(10) Uani 1 1 d . . . . .
O25 O 0.71289(6) 0.17673(6) 1.12298(5) 0.01138(11) Uani 1 1 d . . . . .
V3 V 0.40897(2) 0.14853(2) 0.85511(2) 0.00884(3) Uani 1 1 d . . . . .
O3 O 0.43254(6) 0.25250(6) 0.80137(6) 0.01459(12) Uani 1 1 d . . . . .
O34 O 0.70562(5) -0.18813(5) 1.11338(5) 0.01002(10) Uani 1 1 d . . . . .
O35 O 0.33536(6) 0.06158(6) 0.75339(5) 0.01088(10) Uani 1 1 d . . . . .
V4 V 0.76162(2) -0.07668(2) 1.05869(2) 0.00884(3) Uani 1 1 d . . . . .
O4 O 0.86260(6) -0.13630(6) 1.04831(6) 0.01307(11) Uani 1 1 d . . . . .
V5 V 0.71366(2) 0.06736(2) 1.20940(2) 0.01013(3) Uani 1 1 d . . . . .
O5 O 0.78110(6) 0.11850(6) 1.31570(5) 0.01481(12) Uani 1 1 d . . . . .
O54 O 0.81563(5) -0.00795(5) 1.17830(5) 0.01010(10) Uani 1 1 d . . . . .
N1M N 0.72400(8) -0.35972(7) 0.94069(6) 0.01562(14) Uani 1 1 d D . . . .
H1M1 H 0.7004(13) -0.3887(13) 0.8835(9) 0.017 Uiso 1 1 d D U . . .
H1M2 H 0.7096(13) -0.2946(9) 0.9468(12) 0.017 Uiso 1 1 d D U . . .
C1M C 0.77943(8) -0.41860(8) 1.01807(7) 0.01195(14) Uani 1 1 d . . . . .
N2M N 0.80756(8) -0.51846(7) 1.00901(7) 0.01768(16) Uani 1 1 d D . . . .
H2M1 H 0.7946(14) -0.5432(13) 0.9510(9) 0.019 Uiso 1 1 d D U . . .
H2M2 H 0.8306(13) -0.5571(13) 1.0618(10) 0.019 Uiso 1 1 d D U . . .
N3M N 0.80330(7) -0.37537(7) 1.11015(6) 0.01154(12) Uani 1 1 d D . . . .
H3M H 0.7691(12) -0.3191(10) 1.1137(12) 0.013 Uiso 1 1 d D U . . .
C2M C 0.89056(7) -0.40637(7) 1.19314(6) 0.01024(13) Uani 1 1 d . . . . .
N5M N 0.98278(7) -0.42517(7) 1.18313(6) 0.01324(13) Uani 1 1 d D . . . .
H5M1 H 1.0373(10) -0.4492(13) 1.2299(10) 0.015 Uiso 1 1 d D U . . .
H5M2 H 0.9913(13) -0.4061(13) 1.1314(9) 0.015 Uiso 1 1 d D U . . .
N4M N 0.87763(7) -0.41228(7) 1.27850(6) 0.01163(12) Uani 1 1 d . . . . .
C3M C 0.77359(9) -0.39938(10) 1.28800(8) 0.01795(18) Uani 1 1 d D . . . .
H3M1 H 0.7183(11) -0.4106(14) 1.2265(9) 0.020 Uiso 1 1 d D U . . .
H3M2 H 0.7668(14) -0.4488(12) 1.3341(11) 0.020 Uiso 1 1 d D U . . .
H3M3 H 0.7655(14) -0.3311(10) 1.3126(12) 0.020 Uiso 1 1 d D U . . .
C4M C 0.97077(8) -0.42442(9) 1.37028(7) 0.01565(16) Uani 1 1 d D . . . .
H4M1 H 1.0276(11) -0.3803(12) 1.3672(12) 0.017 Uiso 1 1 d D U . . .
H4M2 H 0.9528(13) -0.4025(13) 1.4258(10) 0.017 Uiso 1 1 d D U . . .
H4M3 H 0.9910(13) -0.4977(9) 1.3783(12) 0.017 Uiso 1 1 d D U . . .
O1W O 0.92933(8) -0.17924(8) 1.31343(7) 0.02381(17) Uani 1 1 d D . . . .
H1W1 H 0.9865(9) -0.1697(15) 1.3044(13) 0.026 Uiso 1 1 d D U . . .
H1W2 H 0.8851(11) -0.1374(13) 1.2754(12) 0.026 Uiso 1 1 d D U . . .
O2W O 1.13944(8) -0.15685(7) 1.31415(6) 0.02118(16) Uani 1 1 d D . . . .
H2W1 H 1.1391(14) -0.1489(14) 1.2561(8) 0.023 Uiso 1 1 d D U . . .
H2W2 H 1.1837(12) -0.2057(11) 1.3374(11) 0.023 Uiso 1 1 d D U . . .
O3W O 1.14241(8) -0.16341(8) 1.12021(7) 0.02163(16) Uani 1 1 d D . . . .
H3W1 H 1.1700(13) -0.1229(11) 1.0917(12) 0.024 Uiso 1 1 d D U . . .
H3W2 H 1.1764(13) -0.2201(9) 1.1309(13) 0.024 Uiso 1 1 d D U . . .
O4W O 0.99909(9) -0.33545(9) 1.01557(7) 0.0278(2) Uani 1 1 d D . . . .
H4W1 H 0.9659(14) -0.3312(14) 0.9544(7) 0.031 Uiso 1 1 d D U . . .
H4W2 H 1.0168(15) -0.2751(9) 1.0356(12) 0.031 Uiso 1 1 d D U . . .
O1HB O 0.4025(10) 0.6481(10) 0.7766(9) 0.0594(13) Uiso 0.2 1 d . U P B 1
O1HG O 0.3722(6) 0.6547(7) 0.7596(6) 0.0594(13) Uiso 0.3 1 d . U P C 2
N1B N 0.5076(4) 0.5210(3) 1.1606(4) 0.0114(4) Uiso 0.2 1 d D U P D 1
H1B1 H 0.488881 0.584669 1.133181 0.012 Uiso 0.2 1 calc R U P D 1
H1B2 H 0.518186 0.511443 1.223595 0.012 Uiso 0.2 1 calc R U P D 1
N5B N 0.5081(4) 0.5984(5) 0.9881(5) 0.0210(6) Uiso 0.2 1 d D U P D 1
HDUM H 0.495537 0.606918 1.043103 0.023 Uiso 0 1 calc R U P D 1
H5B1 H 0.512385 0.654967 0.953191 0.023 Uiso 0.2 1 calc R U P D 1
C3B C 0.5201(3) 0.5045(5) 0.9590(5) 0.0308(6) Uiso 0.2 1 d D U P D 1
N4B N 0.5402(7) 0.4504(9) 0.8826(7) 0.0495(17) Uiso 0.2 1 d D U P D 1
H4B1 H 0.548618 0.487117 0.834134 0.054 Uiso 0.2 1 calc R U P D 1
H4B2 H 0.544265 0.379755 0.883264 0.054 Uiso 0.2 1 calc R U P D 1
N3B N 0.5131(5) 0.4179(6) 1.0147(4) 0.0195(6) Uiso 0.2 1 d D U P D 1
C1B C 0.5200(3) 0.4395(4) 1.1068(3) 0.0147(4) Uiso 0.2 1 d D U P D 1
N2B N 0.5474(6) 0.3634(6) 1.1775(6) 0.0259(6) Uiso 0.2 1 d D U P D 1
H2B1 H 0.551560 0.379308 1.237911 0.028 Uiso 0.2 1 calc R U P D 1
H2B2 H 0.561281 0.297563 1.163308 0.028 Uiso 0.2 1 calc R U P D 1
O3G O 0.4871(3) 0.5272(3) 1.1344(3) 0.0114(4) Uiso 0.3 1 d D U P E 2
N1G N 0.4805(4) 0.5953(4) 0.9639(3) 0.0210(6) Uiso 0.3 1 d D U P E 2
H1G1 H 0.461240 0.638386 0.912074 0.023 Uiso 0.3 1 calc R U P E 2
H1G2 H 0.482554 0.619503 1.021573 0.023 Uiso 0.3 1 calc R U P E 2
C1G C 0.5058(2) 0.4970(4) 0.9552(4) 0.0308(6) Uiso 0.3 1 d D U P E 2
N2G N 0.5000(7) 0.4697(8) 0.8662(6) 0.0495(17) Uiso 0.3 1 d D U P E 2
H2G1 H 0.480001 0.517344 0.817928 0.054 Uiso 0.3 1 calc R U P E 2
H2G2 H 0.516118 0.403762 0.854605 0.054 Uiso 0.3 1 calc R U P E 2
N3G N 0.5376(3) 0.4226(3) 1.0338(3) 0.0195(6) Uiso 0.3 1 d D U P E 2
H3G H 0.565654 0.362069 1.023257 0.021 Uiso 0.3 1 calc R U P E 2
C3G C 0.52967(19) 0.4337(3) 1.1260(2) 0.0147(4) Uiso 0.3 1 d D U P E 2
N4G N 0.5646(4) 0.3525(4) 1.1842(4) 0.0259(6) Uiso 0.3 1 d D U P E 2
H4G1 H 0.562335 0.353369 1.244117 0.028 Uiso 0.3 1 calc R U P E 2
H4G2 H 0.590747 0.296136 1.164071 0.028 Uiso 0.3 1 calc R U P E 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
_geom_angle_publ_flag
O14 V1 O15 107.13(4) . 3_657 ?
O14 V1 O231 98.73(3) . . ?
O15 V1 O231 97.46(3) 3_657 . ?
O14 V1 O123 95.95(3) . 3_657 ?
O15 V1 O123 95.52(3) 3_657 3_657 ?
O231 V1 O123 156.57(3) . 3_657 ?
O14 V1 O1 88.02(3) . . ?
O15 V1 O1 164.74(3) 3_657 . ?
O231 V1 O1 81.58(3) . . ?
O123 V1 O1 80.78(3) 3_657 . ?
O14 V1 O1 165.70(3) . 3_657 ?
O15 V1 O1 86.98(3) 3_657 3_657 ?
O231 V1 O1 81.27(3) . 3_657 ?
O123 V1 O1 80.02(3) 3_657 3_657 ?
O1 V1 O1 77.81(3) . 3_657 ?
V1 O1 V1 102.19(3) . 3_657 ?
V1 O1 V3 95.27(3) . 3_657 ?
V1 O1 V3 92.59(3) 3_657 3_657 ?
V1 O1 V2 92.73(3) . . ?
V1 O1 V2 94.97(3) 3_657 . ?
V3 O1 V2 167.60(3) 3_657 . ?
V1 O1 V4 87.88(3) . . ?
V1 O1 V4 169.92(3) 3_657 . ?
V3 O1 V4 85.97(2) 3_657 . ?
V2 O1 V4 84.87(2) . . ?
V1 O1 V5 170.29(3) . . ?
V1 O1 V5 87.43(3) 3_657 . ?
V3 O1 V5 85.43(2) 3_657 . ?
V2 O1 V5 85.11(2) . . ?
V4 O1 V5 82.51(2) . . ?
V1 O123 V2 107.30(3) 3_657 . ?
V1 O123 V3 105.80(3) 3_657 . ?
V2 O123 V3 99.93(3) . . ?
V1 O123 H123 119(5) 3_657 . ?
V2 O123 H123 109(5) . . ?
V3 O123 H123 114(5) . . ?
V1 O14 V4 110.08(4) . . ?
V1 O15 V5 111.60(4) 3_657 . ?
O2 V2 O24 104.05(4) . . ?
O2 V2 O25 102.75(4) . . ?
O24 V2 O25 95.60(3) . . ?
O2 V2 O231 100.35(4) . . ?
O24 V2 O231 90.85(3) . . ?
O25 V2 O231 153.68(3) . . ?
O2 V2 O123 98.65(4) . . ?
O24 V2 O123 155.43(3) . . ?
O25 V2 O123 88.36(3) . . ?
O231 V2 O123 75.80(3) . . ?
O2 V2 O1 173.21(3) . . ?
O24 V2 O1 81.52(3) . . ?
O25 V2 O1 80.32(3) . . ?
O231 V2 O1 75.43(3) . . ?
O123 V2 O1 75.25(3) . . ?
V1 O231 V2 107.01(3) . . ?
V1 O231 V3 106.98(3) . . ?
V2 O231 V3 102.29(3) . . ?
V2 O24 V4 114.11(4) . . ?
V2 O25 V5 115.28(4) . . ?
O3 V3 O35 103.49(4) . . ?
O3 V3 O34 103.84(4) . 3_657 ?
O35 V3 O34 96.12(3) . 3_657 ?
O3 V3 O231 98.43(4) . . ?
O35 V3 O231 90.66(3) . . ?
O34 V3 O231 154.44(3) 3_657 . ?
O3 V3 O123 98.96(4) . . ?
O35 V3 O123 155.08(3) . . ?
O34 V3 O123 88.80(3) 3_657 . ?
O231 V3 O123 75.36(3) . . ?
O3 V3 O1 172.79(3) . 3_657 ?
O35 V3 O1 81.33(3) . 3_657 ?
O34 V3 O1 80.72(3) 3_657 3_657 ?
O231 V3 O1 75.98(3) . 3_657 ?
O123 V3 O1 75.36(3) . 3_657 ?
V3 O34 V4 114.20(4) 3_657 . ?
V3 O35 V5 114.84(4) . 3_657 ?
O4 V4 O54 104.52(4) . . ?
O4 V4 O24 102.62(4) . . ?
O54 V4 O24 91.73(3) . . ?
O4 V4 O34 100.47(4) . . ?
O54 V4 O34 91.46(3) . . ?
O24 V4 O34 155.08(3) . . ?
O4 V4 O14 99.07(4) . . ?
O54 V4 O14 156.37(3) . . ?
O24 V4 O14 84.32(3) . . ?
O34 V4 O14 82.92(3) . . ?
O4 V4 O1 172.91(3) . . ?
O54 V4 O1 82.41(3) . . ?
O24 V4 O1 78.37(3) . . ?
O34 V4 O1 77.58(3) . . ?
O14 V4 O1 73.97(3) . . ?
O5 V5 O54 103.15(4) . . ?
O5 V5 O25 102.73(4) . . ?
O54 V5 O25 91.60(3) . . ?
O5 V5 O35 101.27(4) . 3_657 ?
O54 V5 O35 90.39(3) . 3_657 ?
O25 V5 O35 154.78(3) . 3_657 ?
O5 V5 O15 101.16(4) . . ?
O54 V5 O15 155.62(3) . . ?
O25 V5 O15 84.86(3) . . ?
O35 V5 O15 83.04(3) 3_657 . ?
O5 V5 O1 175.04(3) . . ?
O54 V5 O1 81.68(3) . . ?
O25 V5 O1 78.05(3) . . ?
O35 V5 O1 77.37(3) 3_657 . ?
O15 V5 O1 73.98(3) . . ?
V4 O54 V5 113.39(4) . . ?
C1M N1M H1M1 119.0(12) . . ?
C1M N1M H1M2 121.6(11) . . ?
H1M1 N1M H1M2 119.4(16) . . ?
N1M C1M N2M 122.11(9) . . ?
N1M C1M N3M 118.10(9) . . ?
N2M C1M N3M 119.71(9) . . ?
C1M N2M H2M1 118.5(12) . . ?
C1M N2M H2M2 117.4(12) . . ?
H2M1 N2M H2M2 123.7(16) . . ?
C1M N3M C2M 123.94(8) . . ?
C1M N3M H3M 116.5(11) . . ?
C2M N3M H3M 118.6(11) . . ?
N4M C2M N5M 123.20(8) . . ?
N4M C2M N3M 118.02(8) . . ?
N5M C2M N3M 118.74(8) . . ?
C2M N5M H5M1 122.9(11) . . ?
C2M N5M H5M2 119.5(11) . . ?
H5M1 N5M H5M2 117.2(16) . . ?
C2M N4M C4M 119.91(8) . . ?
C2M N4M C3M 122.95(8) . . ?
C4M N4M C3M 116.99(8) . . ?
N4M C3M H3M1 110.2(11) . . ?
N4M C3M H3M2 110.0(11) . . ?
H3M1 C3M H3M2 109.3(15) . . ?
N4M C3M H3M3 112.4(11) . . ?
H3M1 C3M H3M3 109.5(15) . . ?
H3M2 C3M H3M3 105.4(15) . . ?
N4M C4M H4M1 109.2(10) . . ?
N4M C4M H4M2 109.8(10) . . ?
H4M1 C4M H4M2 109.1(14) . . ?
N4M C4M H4M3 108.8(11) . . ?
H4M1 C4M H4M3 111.2(14) . . ?
H4M2 C4M H4M3 108.6(14) . . ?
H1W1 O1W H1W2 106.4(14) . . ?
H2W1 O2W H2W2 103.3(13) . . ?
H3W1 O3W H3W2 107.4(14) . . ?
H4W1 O4W H4W2 107.2(15) . . ?
C1B N1B H1B1 120.0 . . ?
C1B N1B H1B2 120.0 . . ?
H1B1 N1B H1B2 120.0 . . ?
C3B N5B HDUM 120.0 . . ?
C3B N5B H5B1 120.0 . . ?
N5B C3B N3B 118.8(7) . . ?
N5B C3B N4B 141.8(8) . . ?
N3B C3B N4B 99.4(6) . . ?
C3B N4B H4B1 120.0 . . ?
C3B N4B H4B2 120.0 . . ?
H4B1 N4B H4B2 120.0 . . ?
C1B N3B C3B 116.0(6) . . ?
N1B C1B N3B 140.0(6) . . ?
N1B C1B N2B 98.6(5) . . ?
N3B C1B N2B 121.4(6) . . ?
C1B N2B H2B1 120.0 . . ?
C1B N2B H2B2 120.0 . . ?
H2B1 N2B H2B2 120.0 . . ?
C1G N1G H1G1 120.0 . . ?
C1G N1G H1G2 120.0 . . ?
H1G1 N1G H1G2 120.0 . . ?
N1G C1G N2G 114.8(6) . . ?
N1G C1G N3G 123.9(5) . . ?
N2G C1G N3G 121.3(6) . . ?
C1G N2G H2G1 120.0 . . ?
C1G N2G H2G2 120.0 . . ?
H2G1 N2G H2G2 120.0 . . ?
C3G N3G C1G 127.4(4) . . ?
C3G N3G H3G 116.3 . . ?
C1G N3G H3G 116.3 . . ?
N4G C3G O3G 134.0(4) . . ?
N4G C3G N3G 114.5(4) . . ?
O3G C3G N3G 111.5(3) . . ?
C3G N4G H4G1 120.0 . . ?
C3G N4G H4G2 120.0 . . ?
H4G1 N4G H4G2 120.0 . . ?
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
V1 O14 1.6863(7) . ?
V1 O15 1.6884(7) 3_657 ?
V1 O231 1.9132(7) . ?
V1 O123 1.9700(7) 3_657 ?
V1 O1 2.0832(7) . ?
V1 O1 2.1147(7) 3_657 ?
O1 V3 2.2472(7) 3_657 ?
O1 V2 2.2602(7) . ?
O1 V4 2.3220(7) . ?
O1 V5 2.3343(7) . ?
O123 V2 2.0354(8) . ?
O123 V3 2.0436(8) . ?
O123 H123 0.94(8) . ?
O14 V4 2.0410(7) . ?
O15 V5 2.0270(8) . ?
V2 O2 1.6034(8) . ?
V2 O24 1.8051(7) . ?
V2 O25 1.8326(8) . ?
V2 O231 1.9995(8) . ?
O231 V3 2.0112(7) . ?
O24 V4 1.8792(7) . ?
O25 V5 1.8464(8) . ?
V3 O3 1.5997(7) . ?
V3 O35 1.8030(7) . ?
V3 O34 1.8262(7) 3_657 ?
O34 V4 1.8847(7) . ?
O35 V5 1.8856(8) 3_657 ?
V4 O4 1.6003(7) . ?
V4 O54 1.8276(7) . ?
V5 O5 1.6048(8) . ?
V5 O54 1.8462(7) . ?
N1M C1M 1.3175(13) . ?
N1M H1M1 0.851(10) . ?
N1M H1M2 0.845(10) . ?
C1M N2M 1.3184(13) . ?
C1M N3M 1.3635(12) . ?
N2M H2M1 0.851(10) . ?
N2M H2M2 0.859(10) . ?
N3M C2M 1.3910(12) . ?
N3M H3M 0.849(10) . ?
C2M N4M 1.3132(12) . ?
C2M N5M 1.3197(12) . ?
N5M H5M1 0.849(10) . ?
N5M H5M2 0.833(10) . ?
N4M C4M 1.4617(13) . ?
N4M C3M 1.4622(13) . ?
C3M H3M1 0.939(11) . ?
C3M H3M2 0.937(10) . ?
C3M H3M3 0.942(11) . ?
C4M H4M1 0.954(11) . ?
C4M H4M2 0.961(10) . ?
C4M H4M3 0.946(10) . ?
O1W H1W1 0.833(9) . ?
O1W H1W2 0.829(9) . ?
O2W H2W1 0.846(9) . ?
O2W H2W2 0.830(9) . ?
O3W H3W1 0.822(9) . ?
O3W H3W2 0.823(9) . ?
O4W H4W1 0.835(9) . ?
O4W H4W2 0.809(9) . ?
N1B C1B 1.325(5) . ?
N1B H1B1 0.8800 . ?
N1B H1B2 0.8800 . ?
N5B C3B 1.272(6) . ?
N5B HDUM 0.8800 . ?
N5B H5B1 0.8800 . ?
C3B N3B 1.369(6) . ?
C3B N4B 1.403(6) . ?
N4B H4B1 0.8800 . ?
N4B H4B2 0.8800 . ?
N3B C1B 1.332(5) . ?
C1B N2B 1.343(6) . ?
N2B H2B1 0.8800 . ?
N2B H2B2 0.8800 . ?
O3G C3G 1.321(4) . ?
N1G C1G 1.287(5) . ?
N1G H1G1 0.8800 . ?
N1G H1G2 0.8800 . ?
C1G N2G 1.308(6) . ?
C1G N3G 1.408(5) . ?
N2G H2G1 0.8800 . ?
N2G H2G2 0.8800 . ?
N3G C3G 1.385(4) . ?
N3G H3G 0.8800 . ?
C3G N4G 1.290(5) . ?
N4G H4G1 0.8800 . ?
N4G H4G2 0.8800 . ?
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
_geom_hbond_publ_flag
O123 H123 N3B 0.94(8) 2.02(8) 2.935(7) 165(7) . yes
O1W H1W1 O2W 0.833(9) 2.013(9) 2.8316(15) 167.3(17) . yes
O1W H1W2 O54 0.829(9) 2.116(10) 2.9173(12) 162.5(17) . yes
O1W H1W2 O34 0.829(9) 2.751(15) 3.3251(13) 127.9(16) . yes
O2W H2W1 O3W 0.846(9) 1.994(10) 2.8274(13) 168.0(16) . yes
O2W H2W2 O25 0.830(9) 1.952(9) 2.7783(11) 173.6(16) 2_747 yes
O3W H3W1 O24 0.822(9) 2.004(10) 2.8129(11) 168.0(17) 3_757 yes
O3W H3W2 O5 0.823(9) 2.152(10) 2.9277(13) 157.3(16) 2_747 yes
O3W H3W2 O2 0.823(9) 2.616(16) 3.1147(13) 120.4(13) 3_757 yes
O4W H4W2 O4 0.809(9) 2.753(18) 3.2178(14) 118.5(16) . yes
O4W H4W2 O3W 0.809(9) 2.181(12) 2.9050(15) 149.1(19) . yes
O4W H4W1 O1W 0.835(9) 1.923(10) 2.7356(14) 164(2) 4 yes
C3M H3M3 O1W 0.942(11) 2.896(17) 3.3818(17) 113.3(12) . yes
C3M H3M1 O34 0.939(11) 3.188(17) 3.5277(14) 103.5(11) . yes
C3M H3M2 O3W 0.937(10) 2.907(15) 3.5664(16) 128.5(13) 2_747 yes
C3M H3M1 O3 0.939(11) 2.744(17) 3.1695(14) 108.5(12) 3_657 yes
C3M H3M2 O14 0.937(10) 2.656(17) 3.1326(13) 112.2(12) 4_556 yes
C3M H3M1 O3G 0.939(11) 2.996(14) 3.783(4) 142.3(13) 1_545 yes
C3M H3M2 O24 0.937(10) 2.649(11) 3.5703(14) 167.8(14) 4_556 yes
C3M H3M2 O4 0.937(10) 3.080(17) 3.5433(15) 112.3(12) 4_556 yes
C4M H4M1 O1W 0.954(11) 2.800(17) 3.1537(15) 102.9(11) . yes
C4M H4M2 O4 0.961(10) 2.536(11) 3.4772(14) 166.4(14) 4_556 yes
C4M H4M3 O4 0.946(10) 2.536(13) 3.3770(13) 148.2(14) 2_747 yes
C4M H4M1 O54 0.954(11) 2.899(16) 3.3594(13) 110.8(12) 2_747 yes
C4M H4M1 O24 0.954(11) 3.009(16) 3.4983(14) 113.3(12) 2_747 yes
C4M H4M2 O3W 0.961(10) 3.136(16) 3.6750(15) 117.2(12) 4_556 yes
C4M H4M3 O3W 0.946(10) 2.736(15) 3.3635(16) 124.5(12) 2_747 yes
N1M H1M2 O4 0.845(10) 2.836(15) 3.3890(13) 124.7(14) . yes
N1M H1M2 O34 0.845(10) 2.772(14) 3.3665(12) 128.8(14) . yes
N1M H1M2 O14 0.845(10) 2.236(11) 3.0660(12) 167.6(16) . yes
N1M H1M1 O3G 0.851(10) 2.982(17) 3.361(4) 109.3(13) 3_657 yes
N1M H1M1 O35 0.851(10) 1.963(11) 2.8040(12) 169.6(16) 2_646 yes
N2M H2M2 O2W 0.859(10) 2.099(11) 2.9496(14) 170.6(17) 2_747 yes
N2M H2M1 O4W 0.851(10) 3.034(17) 3.2936(16) 100.2(12) 3_747 yes
N2M H2M1 O2 0.851(10) 3.034(17) 3.3711(13) 106.2(13) 1_545 yes
N2M H2M1 O5 0.851(10) 2.121(11) 2.9657(13) 172.0(17) 4 yes
N3M H3M O34 0.849(10) 1.837(10) 2.6811(11) 172.4(16) . yes
N3M H3M O4 0.849(10) 2.918(15) 3.2859(12) 108.4(12) . yes
N5M H5M1 O1W 0.849(10) 2.997(16) 3.3663(14) 108.7(12) 2_747 yes
N5M H5M1 O54 0.849(10) 2.068(10) 2.9041(12) 168.0(15) 2_747 yes
N5M H5M2 O5 0.833(10) 2.882(16) 3.2110(13) 105.8(12) 2_747 yes
N5M H5M2 O4W 0.833(10) 1.931(10) 2.7535(13) 168.7(16) . yes
N1B H1B1 N5B 0.88 2.22 2.681(9) 112.5 . yes
N1B H1B1 O3 0.88 2.32 2.925(4) 126.1 3_667 yes
N1B H1B2 O15 0.88 2.37 2.948(4) 123.2 2_657 yes
N1B H1B2 O35 0.88 2.80 3.241(5) 112.9 4_566 yes
N1B H1B2 O231 0.88 2.31 3.159(5) 162.7 4_566 yes
N2B H2B2 O25 0.88 2.76 3.498(8) 142.3 . yes
N2B H2B2 O15 0.88 2.25 3.047(7) 150.5 . yes
N2B H2B2 O123 0.88 2.66 3.333(9) 134.4 . yes
N2B H2B1 O3 0.88 2.68 3.117(7) 112.1 4_566 yes
N2B H2B1 O231 0.88 2.13 3.005(8) 172.3 4_566 yes
N2B H2B1 O35 0.88 3.08 3.535(8) 114.2 4_566 yes
N4B H4B1 O1HB 0.88 2.71 3.121(16) 109.7 . yes
N4B H4B2 O2 0.88 2.27 2.987(10) 138.7 . yes
N4B H4B2 O3 0.88 2.20 2.878(10) 133.1 . yes
N4B H4B2 O123 0.88 3.10 3.822(12) 140.6 . yes
N4B H4B1 O35 0.88 2.52 3.319(10) 151.4 2_656 yes
N4B H4B1 O15 0.88 2.55 3.060(8) 117.5 4_565 yes
N5B H5B1 O1HB 0.88 2.44 2.933(14) 115.6 . yes
N5B H5B1 O123 0.88 2.19 2.742(6) 120.6 3_667 yes
N1G H1G2 O3G 0.88 1.98 2.584(6) 124.6 . yes
N1G H1G1 O1HG 0.88 2.10 2.875(9) 146.3 . yes
N1G H1G2 O123 0.88 2.49 2.809(5) 102.4 3_667 yes
N1G H1G2 O2 0.88 2.85 3.464(4) 128.2 3_667 yes
N2G H2G1 O1HG 0.88 2.20 2.946(13) 142.6 . yes
N2G H2G2 O3 0.88 2.18 2.894(9) 137.8 . yes
N2G H2G2 O2 0.88 2.76 3.476(11) 139.7 . yes
N2G H2G1 O35 0.88 3.07 3.465(8) 109.9 2_656 yes
N2G H2G1 O231 0.88 2.76 3.538(9) 147.5 2_656 yes
N2G H2G2 O15 0.88 2.71 3.186(7) 114.9 4_565 yes
N3G H3G O2 0.88 2.60 3.404(4) 152.2 . yes
N3G H3G O123 0.88 2.35 3.031(4) 134.3 . yes
N3G H3G O25 0.88 3.04 3.785(4) 144.3 . yes
N4G H4G2 O123 0.88 2.66 3.293(6) 129.4 . yes
N4G H4G2 O25 0.88 2.44 3.290(6) 161.8 . yes
N4G H4G2 O15 0.88 2.28 2.904(5) 127.6 . yes
N4G H4G1 O3 0.88 2.55 3.153(5) 126.1 4_566 yes
N4G H4G1 O231 0.88 2.23 3.045(6) 154.0 4_566 yes
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
O15 V1 O14 V4 179.98(3) 3_657 . . . ?
O231 V1 O14 V4 79.33(4) . . . . ?
O123 V1 O14 V4 -82.35(4) 3_657 . . . ?
O1 V1 O14 V4 -1.84(3) . . . . ?
O1 V1 O14 V4 -9.59(15) 3_657 . . . ?
O2 V2 O24 V4 174.40(4) . . . . ?
O25 V2 O24 V4 69.74(4) . . . . ?
O231 V2 O24 V4 -84.71(4) . . . . ?
O123 V2 O24 V4 -28.62(9) . . . . ?
O1 V2 O24 V4 -9.58(4) . . . . ?
O2 V2 O25 V5 -176.09(4) . . . . ?
O24 V2 O25 V5 -70.29(4) . . . . ?
O231 V2 O25 V5 33.10(9) . . . . ?
O123 V2 O25 V5 85.41(4) . . . . ?
O1 V2 O25 V5 10.09(4) . . . . ?
O3 V3 O35 V5 -176.32(4) . . . 3_657 ?
O34 V3 O35 V5 -70.46(4) 3_657 . . 3_657 ?
O231 V3 O35 V5 84.85(4) . . . 3_657 ?
O123 V3 O35 V5 29.97(9) . . . 3_657 ?
O1 V3 O35 V5 9.14(4) 3_657 . . 3_657 ?
V2 O24 V4 O4 -177.77(4) . . . . ?
V2 O24 V4 O54 -72.47(4) . . . . ?
V2 O24 V4 O34 24.73(10) . . . . ?
V2 O24 V4 O14 84.18(4) . . . . ?
V2 O24 V4 O1 9.41(3) . . . . ?
V3 O34 V4 O4 176.10(4) 3_657 . . . ?
V3 O34 V4 O54 71.05(4) 3_657 . . . ?
V3 O34 V4 O24 -26.22(9) 3_657 . . . ?
V3 O34 V4 O14 -85.93(4) 3_657 . . . ?
V3 O34 V4 O1 -10.85(3) 3_657 . . . ?
V2 O25 V5 O5 175.17(4) . . . . ?
V2 O25 V5 O54 71.31(4) . . . . ?
V2 O25 V5 O35 -23.00(10) . . . 3_657 ?
V2 O25 V5 O15 -84.53(4) . . . . ?
V2 O25 V5 O1 -9.84(4) . . . . ?
O4 V4 O54 V5 -179.50(4) . . . . ?
O24 V4 O54 V5 76.99(4) . . . . ?
O34 V4 O54 V5 -78.29(4) . . . . ?
O14 V4 O54 V5 -2.74(10) . . . . ?
O1 V4 O54 V5 -1.03(3) . . . . ?
O5 V5 O54 V4 179.88(4) . . . . ?
O25 V5 O54 V4 -76.65(4) . . . . ?
O35 V5 O54 V4 78.21(4) 3_657 . . . ?
O15 V5 O54 V4 4.39(10) . . . . ?
O1 V5 O54 V4 1.03(3) . . . . ?
N1M C1M N3M C2M -154.59(10) . . . . ?
N2M C1M N3M C2M 28.55(15) . . . . ?
C1M N3M C2M N4M -141.50(10) . . . . ?
C1M N3M C2M N5M 40.53(14) . . . . ?
N5M C2M N4M C4M 9.40(14) . . . . ?
N3M C2M N4M C4M -168.47(9) . . . . ?
N5M C2M N4M C3M -175.22(10) . . . . ?
N3M C2M N4M C3M 6.90(14) . . . . ?
N5B C3B N3B C1B -15.8(5) . . . . ?
N4B C3B N3B C1B 164.2(5) . . . . ?
C3B N3B C1B N1B 21.0(5) . . . . ?
C3B N3B C1B N2B -159.0(5) . . . . ?
N1G C1G N3G C3G 12.2(5) . . . . ?
N2G C1G N3G C3G -167.8(5) . . . . ?
C1G N3G C3G N4G 179.7(3) . . . . ?
C1G N3G C3G O3G -0.3(3) . . . . ?
loop_
_publcif_info_cif.paper_type
CB
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{b27542d7-25ad-45f8-a1bb-4c82666715fb} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_exptl_table_header_item
?
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{b27542d7-25ad-45f8-a1bb-4c82666715fb} '_geom_hbond_atom_site_label_D'
{b27542d7-25ad-45f8-a1bb-4c82666715fb} '_publcif_info_datablock.publ_exptl'
