#------------------------------------------------------------------------------
#$Date: 2023-06-05 07:04:07 +0300 (Mon, 05 Jun 2023) $
#$Revision: 284229 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/89/1568959.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_1568959
loop_
_publ_author_name
'Salazar Marcano, David E.'
'Kalandia, Givi'
'Moussawi, Mhamad Aly'
'Van Hecke, Kristof'
'Parac-Vogt, Tatjana N'
_publ_section_title
;
 Rational synthesis of elusive organic-inorganic hybrid metal-oxo
 clusters: formation and post-functionalization of hexavanadates.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              5405
_journal_page_last               5414
_journal_paper_doi               10.1039/d3sc00038a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C12 H18 Cl2 N2 O21 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C44 H90 Cl2 N4 O21 V6'
_chemical_formula_weight         1387.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-18
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-07 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                112.102(6)
_cell_angle_beta                 97.669(5)
_cell_angle_gamma                93.798(5)
_cell_formula_units_Z            1
_cell_length_a                   10.7293(6)
_cell_length_b                   11.8938(8)
_cell_length_c                   12.7361(8)
_cell_measurement_reflns_used    3899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7340
_cell_measurement_theta_min      3.7750
_cell_volume                     1480.33(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    2.00    --  -41.68 -38.00  90.00   99
  2  ω    -66.00  33.00   1.00    2.00    --  -41.68  38.00 -90.00   99
  3  ω      7.00  34.00   1.00    2.00    --   41.68  83.00  96.38   27
  4  ω     27.00  98.00   1.00    2.00    --   41.68-125.00 -60.00   71
  5  ω    -30.00  70.00   1.00    2.00    --   41.68 -57.00 -30.00  100
  6  ω    103.00 178.00   1.00    6.00    --  106.01  77.00  30.00   75
  7  ω     33.00 132.00   1.00    6.00    --  106.01 -45.00 120.00   99
  8  ω    103.00 178.00   1.00    6.00    --  106.01  77.00-180.00   75
  9  ω     30.00 139.00   1.00    6.00    --  106.01 -77.00   0.00  109
 10  ω     33.00 112.00   1.00    6.00    --  106.01-125.00 -30.00   79
 11  ω     78.00 178.00   1.00    6.00    --  106.01  30.00 -30.00  100
 12  ω     33.00 132.00   1.00    6.00    --  106.01 -45.00-120.00   99
 13  ω     23.00 107.00   1.00    6.00    --  106.01 -94.00   0.00   84
 14  ω     78.00 178.00   1.00    6.00    --  106.01  30.00 120.00  100
 15  ω     33.00 112.00   1.00    6.00    --  106.01-125.00 120.00   79
 16  ω     23.00 107.00   1.00    6.00    --  106.01 -94.00 150.00   84
 17  ω     23.00 107.00   1.00    6.00    --  106.01 -94.00-150.00   84
 18  ω   -115.00 -14.00   1.00    2.00    --  -41.68 -57.00 -90.00  101
 19  ω   -116.00 -17.00   1.00    2.00    --  -41.68 -38.00 -30.00   99
 20  ω      8.00  42.00   1.00    2.00    --   41.68  82.00-130.74   34
 21  ω      9.00  42.00   1.00    2.00    --   41.68  80.00  31.74   33
 22  ω      7.00  34.00   1.00    2.00    --   41.68  83.00 -96.37   27
 23  ω     78.00 178.00   1.00    6.00    --  106.01  57.00  26.76  100
 24  ω     76.00 178.00   1.00    6.00    --  106.01  64.00-141.38  102
 25  ω     53.00 178.00   1.00    6.00    --  106.01  15.00-120.00  125
 26  ω     77.00 178.00   1.00    6.00    --  106.01  59.00  50.24  101
 27  ω     80.00 178.00   1.00    6.00    --  106.01  45.00   0.00   98
 28  ω     76.00 178.00   1.00    6.00    --  106.01  65.00 131.38  102
 29  ω     77.00 178.00   1.00    6.00    --  106.01  61.00-180.00  101
 30  ω     78.00 178.00   1.00    6.00    --  106.01  57.00 -41.30  100
 31  ω     77.00 178.00   1.00    6.00    --  106.01  61.00 120.00  101
 32  ω     77.00 178.00   1.00    6.00    --  106.01  60.00-101.64  101
 33  ω      6.00  83.00   1.00    2.00    --   41.68 -99.00 120.00   77
 34  ω      7.00  33.00   1.00    2.00    --   41.68  84.00 138.78   26
 35  ω      8.00  42.00   1.00    2.00    --   41.68  81.00-178.95   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0394903000
_diffrn_orient_matrix_UB_12      0.0873512000
_diffrn_orient_matrix_UB_13      -0.0585997000
_diffrn_orient_matrix_UB_21      -0.0146155000
_diffrn_orient_matrix_UB_22      0.0968309000
_diffrn_orient_matrix_UB_23      0.1172549000
_diffrn_orient_matrix_UB_31      0.1398579000
_diffrn_orient_matrix_UB_32      0.0534475000
_diffrn_orient_matrix_UB_33      0.0194125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27888
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.068
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.100
_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     356
_refine_ls_number_reflns         5919
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0784P)²+0.2053P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4169
_reflns_number_total             5919
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc00038a2.cif
_cod_data_source_block           exp_1670
_cod_depositor_comments
'Adding full bibliography for 1568959--1568960.cif.'
_cod_database_code               1568959
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N2 O2 Cl1 V10'
_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.
;
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.435
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.88 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C22(H22A,H22B,
 H22C)
;
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.489
_oxdiff_exptl_absorpt_empirical_full_min 0.673
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -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_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 0.49873(7) 0.97034(7) 0.31499(6) 0.02816(18) Uani 1 1 d . . . . .
V2 V 0.44767(7) 1.18518(7) 0.52024(6) 0.02797(18) Uani 1 1 d . . . . .
V3 V 0.30087(7) 0.90575(7) 0.43881(6) 0.02787(18) Uani 1 1 d . . . . .
Cl1 Cl 1.03705(13) 0.66457(14) -0.00820(11) 0.0523(3) Uani 1 1 d . . . . .
O1 O 0.500000 1.000000 0.500000 0.0258(8) Uani 1 2 d S T P . .
O2 O 0.4599(3) 1.1293(3) 0.3698(3) 0.0329(7) Uani 1 1 d . . . . .
O3 O 0.3371(3) 0.9036(3) 0.3012(3) 0.0326(7) Uani 1 1 d . . . . .
O4 O 0.3788(3) 0.7739(3) 0.4304(3) 0.0340(7) Uani 1 1 d . . . . .
O5 O 0.1513(3) 0.8547(3) 0.4087(3) 0.0340(7) Uani 1 1 d . . . . .
O6 O 0.3983(3) 1.3167(3) 0.5456(3) 0.0339(7) Uani 1 1 d . . . . .
O7 O 0.5166(3) 0.9443(3) 0.1860(3) 0.0351(7) Uani 1 1 d . . . . .
O8 O 0.5613(3) 0.8187(3) 0.3234(3) 0.0287(6) Uani 1 1 d . . . . .
O9 O 0.7234(3) 0.9153(3) 0.5206(2) 0.0274(6) Uani 1 1 d . . . . .
O10 O 0.6808(3) 1.0439(3) 0.3894(3) 0.0286(6) Uani 1 1 d . . . . .
O11 O 0.8254(3) 0.7840(3) 0.0920(3) 0.0391(8) Uani 1 1 d . . . . .
N1 N 0.8964(4) 0.8101(4) 0.2774(3) 0.0319(8) Uani 1 1 d D . . . .
C1 C 0.7891(4) 0.8613(4) 0.3320(4) 0.0300(9) Uani 1 1 d . . . . .
C2 C 0.7808(4) 0.9893(4) 0.3324(4) 0.0298(9) Uani 1 1 d . . . . .
H2A H 0.862376 1.041556 0.371775 0.036 Uiso 1 1 calc R . . . .
H2B H 0.765647 0.984002 0.252142 0.036 Uiso 1 1 calc R . . . .
C3 C 0.8195(4) 0.8677(4) 0.4557(4) 0.0301(9) Uani 1 1 d . . . . .
H3A H 0.829051 0.784594 0.453389 0.036 Uiso 1 1 calc R . . . .
H3B H 0.901174 0.920063 0.494212 0.036 Uiso 1 1 calc R . . . .
C4 C 0.6668(4) 0.7747(4) 0.2683(4) 0.0288(9) Uani 1 1 d . . . . .
H4A H 0.650245 0.768210 0.187741 0.035 Uiso 1 1 calc R . . . .
H4B H 0.676942 0.692144 0.267136 0.035 Uiso 1 1 calc R . . . .
C5 C 0.9057(4) 0.7772(4) 0.1658(4) 0.0327(9) Uani 1 1 d . . . . .
C6 C 1.0305(5) 0.7240(5) 0.1403(4) 0.0418(11) Uani 1 1 d . . . . .
H6A H 1.039040 0.658124 0.169491 0.050 Uiso 1 1 calc R . . . .
H6B H 1.102700 0.788965 0.181623 0.050 Uiso 1 1 calc R . . . .
N2 N 0.3124(4) 0.3865(4) 0.2523(3) 0.0368(9) Uani 1 1 d . . . . .
C7 C 0.3071(5) 0.4765(4) 0.3728(4) 0.0363(10) Uani 1 1 d . . . . .
H7A H 0.321094 0.433568 0.425713 0.044 Uiso 1 1 calc R . . . .
H7B H 0.378728 0.542520 0.395530 0.044 Uiso 1 1 calc R . . . .
C8 C 0.1868(5) 0.5354(5) 0.3914(4) 0.0389(11) Uani 1 1 d . . . . .
H8A H 0.112205 0.471732 0.360542 0.047 Uiso 1 1 calc R . . . .
H8B H 0.178469 0.591457 0.350535 0.047 Uiso 1 1 calc R . . . .
C9 C 0.1922(6) 0.6063(5) 0.5196(5) 0.0453(12) Uani 1 1 d . . . . .
H9A H 0.200392 0.549025 0.559219 0.054 Uiso 1 1 calc R . . . .
H9B H 0.268803 0.667589 0.549695 0.054 Uiso 1 1 calc R . . . .
C10 C 0.0763(6) 0.6713(5) 0.5480(6) 0.0542(14) Uani 1 1 d . . . . .
H10A H 0.067120 0.727678 0.508643 0.081 Uiso 1 1 calc GR . . . .
H10B H 0.086637 0.717284 0.631302 0.081 Uiso 1 1 calc GR . . . .
H10C H 0.000583 0.610750 0.522470 0.081 Uiso 1 1 calc GR . . . .
C11 C 0.2044(5) 0.2817(5) 0.2077(4) 0.0395(11) Uani 1 1 d . . . . .
H11A H 0.123704 0.315650 0.199072 0.047 Uiso 1 1 calc R . . . .
H11B H 0.215062 0.225234 0.130212 0.047 Uiso 1 1 calc R . . . .
C12 C 0.1929(5) 0.2077(5) 0.2816(5) 0.0423(11) Uani 1 1 d . . . . .
H12A H 0.171910 0.260294 0.356592 0.051 Uiso 1 1 calc R . . . .
H12B H 0.274680 0.177788 0.296187 0.051 Uiso 1 1 calc R . . . .
C13 C 0.0881(5) 0.0983(5) 0.2196(5) 0.0468(12) Uani 1 1 d . . . . .
H13A H 0.070033 0.060021 0.273724 0.056 Uiso 1 1 calc R . . . .
H13B H 0.009553 0.128102 0.195851 0.056 Uiso 1 1 calc R . . . .
C14 C 0.1256(6) 0.0035(6) 0.1150(6) 0.0590(15) Uani 1 1 d . . . . .
H14A H 0.145775 0.041524 0.062139 0.089 Uiso 1 1 calc GR . . . .
H14B H 0.055164 -0.062476 0.076197 0.089 Uiso 1 1 calc GR . . . .
H14C H 0.200106 -0.030190 0.138793 0.089 Uiso 1 1 calc GR . . . .
H1 H 0.966(4) 0.808(7) 0.320(5) 0.071 Uiso 1 1 d DR . . . .
C15 C 0.4416(5) 0.3422(4) 0.2607(4) 0.0382(10) Uani 1 1 d . . . . .
H15A H 0.506832 0.414646 0.289069 0.046 Uiso 1 1 calc R . . . .
H15B H 0.447753 0.306815 0.319889 0.046 Uiso 1 1 calc R . . . .
C16 C 0.4757(5) 0.2489(5) 0.1525(4) 0.0429(12) Uani 1 1 d . . . . .
H16A H 0.464679 0.278813 0.089522 0.051 Uiso 1 1 calc R . . . .
H16B H 0.419775 0.170657 0.127904 0.051 Uiso 1 1 calc R . . . .
C17 C 0.6141(5) 0.2297(5) 0.1796(5) 0.0452(12) Uani 1 1 d . . . . .
H17A H 0.667969 0.309446 0.207074 0.054 Uiso 1 1 calc R . . . .
H17B H 0.623102 0.199934 0.242773 0.054 Uiso 1 1 calc R . . . .
C18 C 0.6620(6) 0.1392(6) 0.0771(5) 0.0541(14) Uani 1 1 d . . . . .
H18A H 0.648869 0.165356 0.012533 0.081 Uiso 1 1 calc GR . . . .
H18B H 0.615347 0.057740 0.054594 0.081 Uiso 1 1 calc GR . . . .
H18C H 0.752617 0.136401 0.098331 0.081 Uiso 1 1 calc GR . . . .
C19 C 0.2943(5) 0.4456(5) 0.1652(4) 0.0415(11) Uani 1 1 d . . . . .
H19A H 0.286057 0.380717 0.087233 0.050 Uiso 1 1 calc R . . . .
H19B H 0.213334 0.481137 0.170241 0.050 Uiso 1 1 calc R . . . .
C20 C 0.3962(5) 0.5425(5) 0.1780(4) 0.0421(11) Uani 1 1 d . . . . .
H20A H 0.474592 0.505431 0.159803 0.051 Uiso 1 1 calc R . . . .
H20B H 0.414000 0.602185 0.258842 0.051 Uiso 1 1 calc R . . . .
C21 C 0.3593(5) 0.6105(5) 0.0977(5) 0.0424(11) Uani 1 1 d . . . . .
H21A H 0.289706 0.658680 0.124534 0.051 Uiso 1 1 calc R . . . .
H21B H 0.432979 0.668432 0.103545 0.051 Uiso 1 1 calc R . . . .
C22 C 0.3175(5) 0.5257(5) -0.0265(5) 0.0459(12) Uani 1 1 d . . . . .
H22A H 0.309606 0.573714 -0.074358 0.069 Uiso 1 1 calc GR . . . .
H22B H 0.235403 0.478885 -0.035350 0.069 Uiso 1 1 calc GR . . . .
H22C H 0.380501 0.469286 -0.050502 0.069 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -5 -4 0.0254
-1 5 4 0.0134
-5 3 4 0.0338
-5 -4 0 0.0347
6 3 0 0.0370
6 -2 -4 0.0459
-3 7 -4 0.0346
3 -7 4 0.0010
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
V3 V1 V2 65.92(3) . . ?
O1 V1 V2 47.31(2) . . ?
O1 V1 V3 47.41(2) . . ?
O2 V1 V2 33.35(10) . . ?
O2 V1 V3 88.54(10) . . ?
O2 V1 O1 80.64(10) . . ?
O2 V1 O8 156.98(13) . . ?
O2 V1 O10 86.19(14) . . ?
O3 V1 V2 87.20(10) . . ?
O3 V1 V3 34.21(10) . . ?
O3 V1 O1 81.59(10) . . ?
O3 V1 O2 93.77(15) . . ?
O3 V1 O8 89.52(14) . . ?
O3 V1 O10 158.61(13) . . ?
O7 V1 V2 137.00(12) . . ?
O7 V1 V3 138.05(13) . . ?
O7 V1 O1 172.28(12) . . ?
O7 V1 O2 103.80(16) . . ?
O7 V1 O3 104.20(16) . . ?
O7 V1 O8 97.42(15) . . ?
O7 V1 O10 96.55(15) . . ?
O8 V1 V2 124.41(9) . . ?
O8 V1 V3 81.45(9) . . ?
O8 V1 O1 77.32(9) . . ?
O8 V1 O10 82.59(12) . . ?
O10 V1 V2 81.04(9) . . ?
O10 V1 V3 124.52(9) . . ?
O10 V1 O1 77.29(9) . . ?
V3 V2 V1 66.13(3) 2_676 . ?
O1 V2 V1 47.52(2) . . ?
O1 V2 V3 47.47(2) . 2_676 ?
O2 V2 V1 34.36(10) . . ?
O2 V2 V3 87.54(10) . 2_676 ?
O2 V2 O1 81.86(10) . . ?
O2 V2 O4 93.97(15) . 2_676 ?
O2 V2 O8 158.53(13) . 2_676 ?
O2 V2 O9 89.58(14) . 2_676 ?
O4 V2 V1 88.80(10) 2_676 . ?
O4 V2 V3 33.52(10) 2_676 2_676 ?
O4 V2 O1 80.98(10) 2_676 . ?
O4 V2 O8 86.66(13) 2_676 2_676 ?
O4 V2 O9 157.91(13) 2_676 2_676 ?
O6 V2 V1 137.94(12) . . ?
O6 V2 V3 136.17(13) . 2_676 ?
O6 V2 O1 172.77(12) . . ?
O6 V2 O2 103.86(15) . . ?
O6 V2 O4 102.79(16) . 2_676 ?
O6 V2 O8 96.90(14) . 2_676 ?
O6 V2 O9 97.48(15) . 2_676 ?
O8 V2 V1 124.34(9) 2_676 . ?
O8 V2 V3 81.17(9) 2_676 2_676 ?
O8 V2 O1 77.04(8) 2_676 . ?
O9 V2 V1 81.88(8) 2_676 . ?
O9 V2 V3 125.19(9) 2_676 2_676 ?
O9 V2 O1 77.95(8) 2_676 . ?
O9 V2 O8 82.24(12) 2_676 2_676 ?
V2 V3 V1 66.07(3) 2_676 . ?
O1 V3 V1 47.61(2) . . ?
O1 V3 V2 47.46(2) . 2_676 ?
O3 V3 V1 33.78(10) . . ?
O3 V3 V2 89.06(10) . 2_676 ?
O3 V3 O1 81.37(10) . . ?
O3 V3 O9 86.87(13) . 2_676 ?
O3 V3 O10 158.23(14) . 2_676 ?
O4 V3 V1 87.65(11) . . ?
O4 V3 V2 34.66(11) . 2_676 ?
O4 V3 O1 82.10(11) . . ?
O4 V3 O3 94.15(15) . . ?
O4 V3 O9 159.17(14) . 2_676 ?
O4 V3 O10 89.17(14) . 2_676 ?
O5 V3 V1 136.89(12) . . ?
O5 V3 V2 138.42(12) . 2_676 ?
O5 V3 O1 171.75(12) . . ?
O5 V3 O3 103.29(16) . . ?
O5 V3 O4 104.13(16) . . ?
O5 V3 O9 95.84(14) . 2_676 ?
O5 V3 O10 96.71(15) . 2_676 ?
O9 V3 V1 81.67(9) 2_676 . ?
O9 V3 V2 124.71(9) 2_676 2_676 ?
O9 V3 O1 77.48(9) 2_676 . ?
O10 V3 V1 125.21(9) 2_676 . ?
O10 V3 V2 81.49(9) 2_676 2_676 ?
O10 V3 O1 77.79(9) 2_676 . ?
O10 V3 O9 82.58(12) 2_676 2_676 ?
V1 O1 V1 180.00(4) . 2_676 ?
V2 O1 V1 85.17(3) 2_676 2_676 ?
V2 O1 V1 94.83(3) . 2_676 ?
V2 O1 V1 94.83(3) 2_676 . ?
V2 O1 V1 85.17(3) . . ?
V2 O1 V2 180.0 . 2_676 ?
V2 O1 V3 94.94(3) 2_676 2_676 ?
V2 O1 V3 85.07(3) . 2_676 ?
V2 O1 V3 94.93(3) . . ?
V2 O1 V3 85.07(3) 2_676 . ?
V3 O1 V1 84.99(3) 2_676 2_676 ?
V3 O1 V1 95.01(3) . 2_676 ?
V3 O1 V1 95.01(3) 2_676 . ?
V3 O1 V1 84.99(3) . . ?
V3 O1 V3 180.0 2_676 . ?
V2 O2 V1 112.29(15) . . ?
V1 O3 V3 112.01(16) . . ?
V3 O4 V2 111.82(16) . 2_676 ?
V1 O8 V2 110.24(14) . 2_676 ?
C4 O8 V1 118.7(3) . . ?
C4 O8 V2 119.1(2) . 2_676 ?
V2 O9 V3 109.06(13) 2_676 2_676 ?
C3 O9 V2 119.0(3) . 2_676 ?
C3 O9 V3 118.6(3) . 2_676 ?
V3 O10 V1 109.43(14) 2_676 . ?
C2 O10 V1 118.4(3) . . ?
C2 O10 V3 119.0(3) . 2_676 ?
C5 N1 C1 126.4(4) . . ?
N1 C1 C2 109.7(4) . . ?
N1 C1 C3 105.1(3) . . ?
N1 C1 C4 109.3(4) . . ?
C2 C1 C3 110.5(4) . . ?
C2 C1 C4 111.8(4) . . ?
C4 C1 C3 110.1(4) . . ?
O10 C2 C1 111.2(3) . . ?
O9 C3 C1 112.1(3) . . ?
O8 C4 C1 110.7(3) . . ?
O11 C5 N1 125.4(4) . . ?
O11 C5 C6 123.2(4) . . ?
N1 C5 C6 111.4(4) . . ?
C5 C6 Cl1 112.2(3) . . ?
C7 N2 C11 112.4(4) . . ?
C7 N2 C15 105.1(4) . . ?
C7 N2 C19 111.7(4) . . ?
C15 N2 C11 112.2(4) . . ?
C19 N2 C11 103.5(4) . . ?
C19 N2 C15 112.1(4) . . ?
C8 C7 N2 117.1(4) . . ?
C7 C8 C9 108.9(4) . . ?
C10 C9 C8 113.3(5) . . ?
C12 C11 N2 116.1(4) . . ?
C11 C12 C13 109.8(4) . . ?
C14 C13 C12 112.1(5) . . ?
C16 C15 N2 117.9(4) . . ?
C15 C16 C17 108.0(4) . . ?
C18 C17 C16 113.6(5) . . ?
C20 C19 N2 116.0(4) . . ?
C19 C20 C21 111.8(4) . . ?
C22 C21 C20 113.3(4) . . ?
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 V2 3.0338(11) . ?
V1 V3 3.0288(11) . ?
V1 O1 2.2454(7) . ?
V1 O2 1.851(3) . ?
V1 O3 1.816(3) . ?
V1 O7 1.594(3) . ?
V1 O8 2.000(3) . ?
V1 O10 2.033(3) . ?
V2 V3 3.0258(11) 2_676 ?
V2 O1 2.2378(7) . ?
V2 O2 1.802(3) . ?
V2 O4 1.854(3) 2_676 ?
V2 O6 1.614(3) . ?
V2 O8 2.024(3) 2_676 ?
V2 O9 2.014(3) 2_676 ?
V3 O1 2.2383(8) . ?
V3 O3 1.837(3) . ?
V3 O4 1.800(3) . ?
V3 O5 1.619(3) . ?
V3 O9 2.036(3) 2_676 ?
V3 O10 2.017(3) 2_676 ?
Cl1 C6 1.766(5) . ?
O8 C4 1.437(5) . ?
O9 C3 1.421(5) . ?
O10 C2 1.431(5) . ?
O11 C5 1.217(6) . ?
N1 C1 1.472(6) . ?
N1 C5 1.344(6) . ?
C1 C2 1.530(6) . ?
C1 C3 1.537(6) . ?
C1 C4 1.532(6) . ?
C5 C6 1.541(7) . ?
N2 C7 1.516(6) . ?
N2 C11 1.523(7) . ?
N2 C15 1.521(6) . ?
N2 C19 1.519(6) . ?
C7 C8 1.513(7) . ?
C8 C9 1.520(7) . ?
C9 C10 1.520(8) . ?
C11 C12 1.520(7) . ?
C12 C13 1.541(7) . ?
C13 C14 1.511(9) . ?
C15 C16 1.517(7) . ?
C16 C17 1.531(8) . ?
C17 C18 1.524(7) . ?
C19 C20 1.482(8) . ?
C20 C21 1.552(7) . ?
C21 C22 1.507(8) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.6379 -4.9082 -3.9007 -0.2254 -0.9420 -0.2488
-0.6379 4.9082 3.9007 0.2254 0.9420 0.2488
-4.6801 3.2507 4.3458 0.2141 0.8927 -0.3964
-5.2793 -3.6101 -0.4895 -0.0782 -0.3298 -0.9408
5.7383 3.1938 -0.0089 0.0529 0.2244 0.9731
5.6167 -2.3865 -4.0932 -0.1904 -0.7931 0.5785
-2.8044 7.1133 -3.8051 0.9551 0.2836 -0.0859
2.8044 -7.1133 3.8051 -0.9551 -0.2836 0.0859
