#------------------------------------------------------------------------------
#$Date: 2025-10-06 11:12:22 +0200 (Mon 06 de Oct de 2025) $
#$Revision: 302620 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/91/7719124.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_7719124
loop_
_publ_author_name
'Routh, Kousik'
'Kumar Swain, Rajesha'
'Kumar, Gaurav'
'Pradeep, Chullikkattil P.'
_publ_section_title
;
 Amine functionalized quinolinium polyoxometalates as highly active
 heterogeneous catalysts for solvent-free CO₂ cycloaddition and
 Knoevenagel condensation reactions.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12324
_journal_page_last               12339
_journal_paper_doi               10.1039/d5dt00934k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'O28 V10, 4(C10 H10 Cl N2), 2(C3 H7 N O), 2(O)'
_chemical_formula_sum            'C46 H60 Cl4 N10 O32 V10'
_chemical_formula_weight         1916.24
_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     iterative
_audit_creation_date             2024-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                114.428(5)
_cell_angle_beta                 99.672(4)
_cell_angle_gamma                99.647(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7219(4)
_cell_length_b                   12.6345(6)
_cell_length_c                   14.2538(10)
_cell_measurement_reflns_used    3466
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4030
_cell_measurement_theta_min      2.2080
_cell_volume                     1671.52(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 120.00   1.00   59.55    --   26.84 178.00  90.00   85
  2  ω     28.00 102.00   1.00   59.55    --   26.84  37.00 -60.00   74
  3  ω    -51.00  65.00   1.00   59.55    --   26.84 -77.00  60.00  116
  4  ω    -47.00  64.00   1.00   59.55    --   26.84 -57.00 150.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279178000
_diffrn_orient_matrix_UB_12      0.0111277000
_diffrn_orient_matrix_UB_13      0.0530526000
_diffrn_orient_matrix_UB_21      -0.0304922000
_diffrn_orient_matrix_UB_22      -0.0604714000
_diffrn_orient_matrix_UB_23      -0.0131288000
_diffrn_orient_matrix_UB_31      0.0559651000
_diffrn_orient_matrix_UB_32      -0.0175056000
_diffrn_orient_matrix_UB_33      -0.0149903000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9772
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.173
_diffrn_reflns_theta_min         1.835
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0687
_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)+(0.1076P)²+0.8086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4986
_reflns_number_total             7052
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt00934k2.cif
_cod_data_source_block           gk_114_1_rt_mo
_cod_depositor_comments
'Adding full bibliography for 7719124--7719126.cif.'
_cod_original_cell_volume        1671.50(17)
_cod_database_code               7719124
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C46  H58  Cl4  N10  O32  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.
;
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C15(H15), C12(H12), C5(H5), C2(H2), C11(H11), C16(H16), C8(H8),
 C6(H6), C23(H23), C1(H1)
2.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 8.919
_oxdiff_exptl_absorpt_empirical_full_min 0.590
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
V4 V 0.53026(6) 0.61068(6) 0.46799(6) 0.0255(2) Uani 1 1 d . . . . .
V5 V 0.68341(7) 0.41083(7) 0.40607(7) 0.0306(2) Uani 1 1 d . . . . .
V3 V 0.26145(7) 0.41937(7) 0.35982(7) 0.0313(2) Uani 1 1 d . . . . .
V1 V 0.47129(8) 0.41640(8) 0.23300(7) 0.0347(2) Uani 1 1 d . . . . .
V2 V 0.42258(9) 0.21275(7) 0.29740(7) 0.0390(2) Uani 1 1 d . . . . .
Cl2 Cl 1.3765(2) 0.7398(2) 0.0903(2) 0.1024(8) Uani 1 1 d . . . . .
Cl1 Cl 0.6876(3) 0.9644(3) 0.2469(3) 0.1440(13) Uani 1 1 d . . . . .
O8 O 0.7012(3) 0.5821(3) 0.4943(3) 0.0274(7) Uani 1 1 d . . . . .
O7 O 0.3448(3) 0.5864(3) 0.4578(3) 0.0290(7) Uani 1 1 d . . . . .
O14 O 0.5272(3) 0.5822(2) 0.6022(3) 0.0273(7) Uani 1 1 d . . . . .
O4 O 0.5210(3) 0.5944(3) 0.3431(3) 0.0309(7) Uani 1 1 d . . . . .
O5 O 0.6458(3) 0.4259(3) 0.2835(3) 0.0344(7) Uani 1 1 d . . . . .
O12 O 0.5746(3) 0.7597(3) 0.5502(3) 0.0350(8) Uani 1 1 d . . . . .
O9 O 0.5986(3) 0.2476(3) 0.3384(3) 0.0383(8) Uani 1 1 d . . . . .
O3 O 0.2990(3) 0.4291(3) 0.2494(3) 0.0365(8) Uani 1 1 d . . . . .
O6 O 0.2480(3) 0.2472(3) 0.3037(3) 0.0417(8) Uani 1 1 d . . . . .
O11 O 0.1083(3) 0.4173(3) 0.3417(3) 0.0433(9) Uani 1 1 d . . . . .
O13 O 0.8343(3) 0.4095(3) 0.4207(3) 0.0437(9) Uani 1 1 d . . . . .
O2 O 0.4209(3) 0.2560(3) 0.1885(3) 0.0426(8) Uani 1 1 d . . . . .
O1 O 0.4683(3) 0.4276(4) 0.1255(3) 0.0480(9) Uani 1 1 d . . . . .
O10 O 0.3783(4) 0.0689(3) 0.2365(4) 0.0574(11) Uani 1 1 d . . . . .
N2 N 0.9663(4) 0.6890(4) 0.5047(4) 0.0518(12) Uani 1 1 d . . . . .
H2A H 0.883907 0.673182 0.501040 0.062 Uiso 1 1 calc R U . . .
H2B H 1.017387 0.660959 0.536039 0.062 Uiso 1 1 calc R U . . .
N3 N 0.8857(5) 0.6748(5) 0.0536(4) 0.0573(13) Uani 1 1 d . . . . .
N4 N 0.8853(5) 0.4893(4) 0.2347(4) 0.0526(12) Uani 1 1 d . . . . .
H4A H 0.961957 0.510803 0.278021 0.063 Uiso 1 1 d R U . . .
H4B H 0.828589 0.505950 0.271568 0.063 Uiso 1 1 d R U . . .
N1 N 1.1260(6) 0.9016(5) 0.3817(5) 0.0642(15) Uani 1 1 d . . . . .
C13 C 0.8878(5) 0.5499(5) 0.1772(5) 0.0445(12) Uani 1 1 d . . . . .
C14 C 1.0062(5) 0.5972(4) 0.1571(4) 0.0414(12) Uani 1 1 d . . . . .
C19 C 1.0028(6) 0.6594(5) 0.0953(4) 0.0444(12) Uani 1 1 d . . . . .
N5 N -0.1919(7) 0.1095(5) 0.1021(5) 0.0708(16) Uani 1 1 d . . . . .
C3 C 1.0137(6) 0.7556(5) 0.4628(5) 0.0551(15) Uani 1 1 d . . . . .
C18 C 1.1187(6) 0.7042(5) 0.0750(5) 0.0542(15) Uani 1 1 d . . . . .
H18 H 1.117086 0.745560 0.034091 0.065 Uiso 1 1 calc R U . . .
C15 C 1.1277(6) 0.5836(5) 0.1969(6) 0.0562(16) Uani 1 1 d . . . . .
H15 H 1.131744 0.543490 0.238833 0.067 Uiso 1 1 calc R U . . .
C9 C 0.9950(6) 0.8825(6) 0.3677(5) 0.0555(15) Uani 1 1 d . . . . .
C4 C 0.9368(6) 0.8039(5) 0.4110(5) 0.0521(14) Uani 1 1 d . . . . .
C12 C 0.7721(6) 0.5674(6) 0.1305(6) 0.0584(16) Uani 1 1 d . . . . .
H12 H 0.693047 0.536506 0.140293 0.070 Uiso 1 1 calc R U . . .
C5 C 0.8086(7) 0.7852(6) 0.3997(6) 0.0628(17) Uani 1 1 d . . . . .
H5 H 0.770361 0.739484 0.429531 0.075 Uiso 1 1 calc R U . . .
C2 C 1.1577(8) 0.7846(7) 0.4727(7) 0.077(2) Uani 1 1 d . . . . .
H2 H 1.213691 0.756966 0.509005 0.093 Uiso 1 1 calc R U . . .
C11 C 0.7729(6) 0.6289(6) 0.0710(6) 0.0623(17) Uani 1 1 d . . . . .
H11 H 0.694464 0.639428 0.041679 0.075 Uiso 1 1 calc R U . . .
O15 O 0.0193(6) 0.1003(6) 0.1653(5) 0.112(2) Uani 1 1 d . . . . .
C16 C 1.2378(7) 0.6256(6) 0.1775(7) 0.069(2) Uani 1 1 d . . . . .
H16 H 1.316433 0.613973 0.205025 0.083 Uiso 1 1 calc R U . . .
C8 C 0.9229(8) 0.9277(6) 0.3196(6) 0.073(2) Uani 1 1 d . . . . .
H8 H 0.961072 0.977457 0.293196 0.088 Uiso 1 1 calc R U . . .
C17 C 1.2346(7) 0.6866(6) 0.1159(6) 0.0636(18) Uani 1 1 d . . . . .
C20 C 0.8777(9) 0.7413(8) -0.0094(7) 0.088(3) Uani 1 1 d . . . . .
H20A H 0.928006 0.823479 0.034157 0.133 Uiso 1 1 calc R U . . .
H20B H 0.787780 0.738931 -0.033958 0.133 Uiso 1 1 calc R U . . .
H20C H 0.912059 0.704971 -0.069667 0.133 Uiso 1 1 calc R U . . .
C6 C 0.7286(7) 0.8287(7) 0.3473(7) 0.074(2) Uani 1 1 d . . . . .
H6 H 0.638457 0.810152 0.338730 0.088 Uiso 1 1 calc R U . . .
C7 C 0.7872(8) 0.9008(7) 0.3077(7) 0.075(2) Uani 1 1 d . . . . .
C10 C 1.1969(8) 0.9767(8) 0.3416(9) 0.100(3) Uani 1 1 d . . . . .
H10A H 1.156048 0.948092 0.267143 0.151 Uiso 1 1 calc R U . . .
H10B H 1.286366 0.972336 0.350587 0.151 Uiso 1 1 calc R U . . .
H10C H 1.194681 1.058780 0.380774 0.151 Uiso 1 1 calc R U . . .
C21 C -0.2072(10) 0.0185(8) -0.0013(6) 0.101(3) Uani 1 1 d . . . . .
H21A H -0.126652 0.028878 -0.021448 0.152 Uiso 1 1 calc R U . . .
H21B H -0.275986 0.023439 -0.050782 0.152 Uiso 1 1 calc R U . . .
H21C H -0.229451 -0.058898 -0.002429 0.152 Uiso 1 1 calc R U . . .
C23 C -0.0799(10) 0.1473(8) 0.1775(7) 0.093(3) Uani 1 1 d . . . . .
H23 H -0.071900 0.211614 0.243237 0.111 Uiso 1 1 calc R U . . .
C22 C -0.2991(12) 0.1575(10) 0.1265(10) 0.129(4) Uani 1 1 d . . . . .
H22A H -0.312070 0.207372 0.091931 0.194 Uiso 1 1 calc R U . . .
H22B H -0.281102 0.204935 0.202381 0.194 Uiso 1 1 calc R U . . .
H22C H -0.376854 0.092809 0.101633 0.194 Uiso 1 1 calc R U . . .
C1 C 1.2027(8) 0.8509(8) 0.4282(8) 0.089(3) Uani 1 1 d . . . . .
H1 H 1.290771 0.863698 0.428508 0.106 Uiso 1 1 calc R U . . .
O16 O 1.4790(7) 0.9845(10) 0.4114(10) 0.178(5) Uani 1 1 d . . . . .
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'
Cl Cl 0.1484 0.1585 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
14 2 -10 0.1217
-15 4 3 0.1209
0 8 11 0.0327
2 -8 19 0.0213
-8 -13 13 0.0433
6 -17 6 0.0414
-3 9 -19 0.0721
13 -3 -11 0.1002
-1 18 -7 0.0660
11 -12 10 0.0395
-1 -6 -13 0.0489
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
V1 V4 V3 60.19(3) . . ?
V2 V4 V3 116.42(3) 2_666 . ?
V2 V4 V1 175.72(3) 2_666 . ?
O8 V4 V3 127.16(9) . . ?
O8 V4 V1 88.69(10) . . ?
O8 V4 V2 91.81(10) . 2_666 ?
O8 V4 O7 156.33(13) . . ?
O8 V4 O14 80.80(12) . 2_666 ?
O8 V4 O14 80.74(12) . . ?
O7 V4 V3 36.46(10) . . ?
O7 V4 V1 90.58(10) . . ?
O7 V4 V2 87.26(10) . 2_666 ?
O7 V4 O14 80.94(12) . 2_666 ?
O7 V4 O14 80.93(12) . . ?
O14 V4 V3 86.20(8) . . ?
O14 V4 V3 46.39(7) 2_666 . ?
O14 V4 V1 48.91(9) 2_666 . ?
O14 V4 V1 127.25(8) . . ?
O14 V4 V2 127.00(9) 2_666 2_666 ?
O14 V4 V2 48.73(8) . 2_666 ?
O14 V4 O14 78.35(13) . 2_666 ?
O4 V4 V3 83.53(11) . . ?
O4 V4 V1 37.92(11) . . ?
O4 V4 V2 146.08(11) . 2_666 ?
O4 V4 O8 97.02(14) . . ?
O4 V4 O7 96.87(14) . . ?
O4 V4 O14 86.81(14) . 2_666 ?
O4 V4 O14 165.16(14) . . ?
O12 V4 V3 133.05(11) . . ?
O12 V4 V1 144.78(13) . . ?
O12 V4 V2 39.31(12) . 2_666 ?
O12 V4 O8 97.54(15) . . ?
O12 V4 O7 96.64(15) . . ?
O12 V4 O14 87.96(15) . . ?
O12 V4 O14 166.31(15) . 2_666 ?
O12 V4 O4 106.87(17) . . ?
V3 V5 V1 122.45(3) 2_666 . ?
V3 V5 V2 118.24(3) 2_666 . ?
V2 V5 V1 59.56(3) . . ?
O8 V5 V3 42.68(10) . 2_666 ?
O8 V5 V1 88.39(9) . . ?
O8 V5 V2 125.20(8) . . ?
O8 V5 O7 77.98(13) . 2_666 ?
O8 V5 O14 77.33(11) . 2_666 ?
O7 V5 V3 39.00(9) 2_666 2_666 ?
O7 V5 V1 124.25(8) 2_666 . ?
O7 V5 V2 85.30(9) 2_666 . ?
O7 V5 O14 75.45(12) 2_666 2_666 ?
O14 V5 V3 85.58(8) 2_666 2_666 ?
O14 V5 V1 48.81(8) 2_666 . ?
O14 V5 V2 47.92(7) 2_666 . ?
O5 V5 V3 134.50(11) . 2_666 ?
O5 V5 V1 32.93(10) . . ?
O5 V5 V2 83.18(11) . . ?
O5 V5 O8 91.85(14) . . ?
O5 V5 O7 156.23(13) . 2_666 ?
O5 V5 O14 81.41(13) . 2_666 ?
O5 V5 O9 93.35(16) . . ?
O9 V5 V3 126.73(12) . 2_666 ?
O9 V5 V1 82.92(12) . . ?
O9 V5 V2 32.02(10) . . ?
O9 V5 O8 155.12(14) . . ?
O9 V5 O7 87.74(15) . 2_666 ?
O9 V5 O14 79.43(13) . 2_666 ?
O13 V5 V3 90.64(15) . 2_666 ?
O13 V5 V1 134.88(15) . . ?
O13 V5 V2 133.82(14) . . ?
O13 V5 O8 100.66(16) . . ?
O13 V5 O7 100.84(17) . 2_666 ?
O13 V5 O14 176.04(17) . 2_666 ?
O13 V5 O5 102.14(18) . . ?
O13 V5 O9 101.98(17) . . ?
V4 V3 V1 59.90(2) . . ?
V5 V3 V4 62.69(3) 2_666 . ?
V5 V3 V1 122.36(3) 2_666 . ?
O8 V3 V4 81.12(8) 2_666 . ?
O8 V3 V5 40.14(8) 2_666 2_666 ?
O8 V3 V1 123.06(8) 2_666 . ?
O8 V3 O14 74.49(11) 2_666 2_666 ?
O7 V3 V4 36.57(8) . . ?
O7 V3 V5 40.79(10) . 2_666 ?
O7 V3 V1 90.40(9) . . ?
O7 V3 O8 77.27(13) . 2_666 ?
O7 V3 O14 78.43(11) . 2_666 ?
O7 V3 O6 152.98(14) . . ?
O14 V3 V4 43.70(7) 2_666 . ?
O14 V3 V5 85.64(8) 2_666 2_666 ?
O14 V3 V1 48.57(8) 2_666 . ?
O3 V3 V4 79.71(11) . . ?
O3 V3 V5 135.82(12) . 2_666 ?
O3 V3 V1 33.73(10) . . ?
O3 V3 O8 156.37(13) . 2_666 ?
O3 V3 O7 95.08(15) . . ?
O3 V3 O14 82.10(13) . 2_666 ?
O3 V3 O6 94.69(17) . . ?
O6 V3 V4 121.76(11) . . ?
O6 V3 V5 123.91(12) . 2_666 ?
O6 V3 V1 83.93(11) . . ?
O6 V3 O8 83.78(14) . 2_666 ?
O6 V3 O14 78.06(13) . 2_666 ?
O11 V3 V4 137.57(14) . . ?
O11 V3 V5 91.01(14) . 2_666 ?
O11 V3 V1 136.71(14) . . ?
O11 V3 O8 100.19(16) . 2_666 ?
O11 V3 O7 101.78(17) . . ?
O11 V3 O14 174.55(16) . 2_666 ?
O11 V3 O3 103.27(17) . . ?
O11 V3 O6 100.38(17) . . ?
V4 V1 V3 59.91(2) . . ?
V5 V1 V4 61.00(2) . . ?
V5 V1 V3 92.65(3) . . ?
V2 V1 V4 91.54(3) . . ?
V2 V1 V5 59.96(3) . . ?
V2 V1 V3 63.95(3) . . ?
O14 V1 V4 43.66(7) 2_666 . ?
O14 V1 V5 46.63(7) 2_666 . ?
O14 V1 V3 46.03(7) 2_666 . ?
O14 V1 V2 47.92(7) 2_666 . ?
O4 V1 V4 30.41(9) . . ?
O4 V1 V5 80.88(9) . . ?
O4 V1 V3 78.30(9) . . ?
O4 V1 V2 121.95(10) . . ?
O4 V1 O14 74.06(12) . 2_666 ?
O5 V1 V4 79.15(11) . . ?
O5 V1 V5 32.30(10) . . ?
O5 V1 V3 124.53(11) . . ?
O5 V1 V2 83.06(11) . . ?
O5 V1 O14 78.61(13) . 2_666 ?
O5 V1 O4 84.31(14) . . ?
O5 V1 O3 153.42(15) . . ?
O3 V1 V4 77.34(11) . . ?
O3 V1 V5 122.47(11) . . ?
O3 V1 V3 30.02(10) . . ?
O3 V1 V2 85.35(10) . . ?
O3 V1 O14 75.88(12) . 2_666 ?
O3 V1 O4 81.70(14) . . ?
O2 V1 V4 124.65(12) . . ?
O2 V1 V5 83.52(12) . . ?
O2 V1 V3 83.02(12) . . ?
O2 V1 V2 33.26(12) . . ?
O2 V1 O14 81.00(14) . 2_666 ?
O2 V1 O4 154.98(15) . . ?
O2 V1 O5 92.85(16) . . ?
O2 V1 O3 90.42(16) . . ?
O1 V1 V4 131.46(15) . . ?
O1 V1 V5 135.42(13) . . ?
O1 V1 V3 131.66(14) . . ?
O1 V1 V2 137.00(15) . . ?
O1 V1 O14 174.70(17) . 2_666 ?
O1 V1 O4 101.04(18) . . ?
O1 V1 O5 103.15(17) . . ?
O1 V1 O3 101.64(17) . . ?
O1 V1 O2 103.80(19) . . ?
V4 V2 V5 62.55(3) 2_666 . ?
V4 V2 V1 92.49(3) 2_666 . ?
V1 V2 V5 60.48(3) . . ?
O14 V2 V4 43.29(8) 2_666 2_666 ?
O14 V2 V5 46.99(7) 2_666 . ?
O14 V2 V1 49.20(8) 2_666 . ?
O12 V2 V4 31.39(9) 2_666 2_666 ?
O12 V2 V5 84.11(9) 2_666 . ?
O12 V2 V1 123.81(9) 2_666 . ?
O12 V2 O14 74.62(12) 2_666 2_666 ?
O9 V2 V4 80.67(12) . 2_666 ?
O9 V2 V5 33.17(10) . . ?
O9 V2 V1 84.63(11) . . ?
O9 V2 O14 79.64(12) . 2_666 ?
O9 V2 O12 86.94(15) . 2_666 ?
O9 V2 O6 154.79(15) . . ?
O9 V2 O2 93.92(17) . . ?
O6 V2 V4 77.22(11) . 2_666 ?
O6 V2 V5 122.99(10) . . ?
O6 V2 V1 84.37(11) . . ?
O6 V2 O14 76.00(12) . 2_666 ?
O6 V2 O12 80.50(15) . 2_666 ?
O2 V2 V4 124.69(11) . 2_666 ?
O2 V2 V5 83.38(11) . . ?
O2 V2 V1 32.43(11) . . ?
O2 V2 O14 81.46(14) . 2_666 ?
O2 V2 O12 155.52(15) . 2_666 ?
O2 V2 O6 88.83(16) . . ?
O10 V2 V4 131.29(17) . 2_666 ?
O10 V2 V5 136.66(17) . . ?
O10 V2 V1 136.07(17) . . ?
O10 V2 O14 173.62(18) . 2_666 ?
O10 V2 O12 99.89(19) . 2_666 ?
O10 V2 O9 103.6(2) . . ?
O10 V2 O6 100.09(19) . . ?
O10 V2 O2 103.7(2) . . ?
V4 O8 V5 107.87(14) . . ?
V4 O8 V3 107.56(14) . 2_666 ?
V5 O8 V3 97.18(13) . 2_666 ?
V4 O7 V5 108.01(15) . 2_666 ?
V3 O7 V4 106.96(14) . . ?
V3 O7 V5 100.20(14) . 2_666 ?
V4 O14 V4 101.65(13) . 2_666 ?
V4 O14 V5 93.87(11) . 2_666 ?
V4 O14 V5 91.12(10) 2_666 2_666 ?
V4 O14 V3 95.80(11) . 2_666 ?
V4 O14 V3 89.91(10) 2_666 2_666 ?
V4 O14 V1 87.44(10) 2_666 2_666 ?
V4 O14 V1 170.83(15) . 2_666 ?
V4 O14 V2 169.89(16) 2_666 2_666 ?
V4 O14 V2 87.98(10) . 2_666 ?
V5 O14 V1 84.57(10) 2_666 2_666 ?
V5 O14 V2 85.08(10) 2_666 2_666 ?
V3 O14 V5 169.86(16) 2_666 2_666 ?
V3 O14 V1 85.40(10) 2_666 2_666 ?
V3 O14 V2 92.21(10) 2_666 2_666 ?
V2 O14 V1 82.88(11) 2_666 2_666 ?
V4 O4 V1 111.67(16) . . ?
V5 O5 V1 114.77(17) . . ?
V4 O12 V2 109.30(17) . 2_666 ?
V2 O9 V5 114.81(17) . . ?
V3 O3 V1 116.25(17) . . ?
V3 O6 V2 111.74(16) . . ?
V1 O2 V2 114.31(19) . . ?
H2A N2 H2B 120.0 . . ?
C3 N2 H2A 120.0 . . ?
C3 N2 H2B 120.0 . . ?
C19 N3 C20 121.9(6) . . ?
C11 N3 C19 120.4(5) . . ?
C11 N3 C20 117.7(6) . . ?
H4A N4 H4B 108.9 . . ?
C13 N4 H4A 109.0 . . ?
C13 N4 H4B 109.7 . . ?
C9 N1 C10 120.9(7) . . ?
C9 N1 C1 124.7(6) . . ?
C1 N1 C10 114.4(7) . . ?
N4 C13 C14 122.5(5) . . ?
N4 C13 C12 120.8(5) . . ?
C12 C13 C14 116.7(5) . . ?
C19 C14 C13 120.0(5) . . ?
C15 C14 C13 122.4(5) . . ?
C15 C14 C19 117.5(5) . . ?
N3 C19 C14 119.9(5) . . ?
N3 C19 C18 120.3(5) . . ?
C18 C19 C14 119.7(5) . . ?
C21 N5 C22 119.0(8) . . ?
C23 N5 C21 120.8(7) . . ?
C23 N5 C22 120.2(8) . . ?
N2 C3 C4 123.1(6) . . ?
N2 C3 C2 119.0(6) . . ?
C4 C3 C2 117.9(5) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 C19 119.6(6) . . ?
C17 C18 H18 120.2 . . ?
C14 C15 H15 118.5 . . ?
C16 C15 C14 122.9(6) . . ?
C16 C15 H15 118.5 . . ?
N1 C9 C4 114.8(6) . . ?
C8 C9 N1 123.9(7) . . ?
C8 C9 C4 121.3(6) . . ?
C3 C4 C9 121.4(5) . . ?
C5 C4 C3 122.5(6) . . ?
C5 C4 C9 116.1(6) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 C13 121.5(6) . . ?
C11 C12 H12 119.2 . . ?
C4 C5 H5 117.7 . . ?
C4 C5 C6 124.5(7) . . ?
C6 C5 H5 117.7 . . ?
C3 C2 H2 121.2 . . ?
C1 C2 C3 117.7(7) . . ?
C1 C2 H2 121.2 . . ?
N3 C11 C12 121.4(6) . . ?
N3 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.7(7) . . ?
C17 C16 H16 120.1 . . ?
C9 C8 H8 120.3 . . ?
C9 C8 C7 119.5(6) . . ?
C7 C8 H8 120.3 . . ?
C18 C17 Cl2 119.9(5) . . ?
C18 C17 C16 120.5(6) . . ?
C16 C17 Cl2 119.6(6) . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C5 C6 H6 121.4 . . ?
C5 C6 C7 117.3(7) . . ?
C7 C6 H6 121.4 . . ?
C8 C7 Cl1 120.6(6) . . ?
C6 C7 Cl1 117.9(6) . . ?
C6 C7 C8 121.4(7) . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C21 H21A 109.5 . . ?
N5 C21 H21B 109.5 . . ?
N5 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N5 C23 H23 117.8 . . ?
O15 C23 N5 124.4(7) . . ?
O15 C23 H23 117.8 . . ?
N5 C22 H22A 109.5 . . ?
N5 C22 H22B 109.5 . . ?
N5 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C1 H1 118.4 . . ?
C2 C1 N1 123.2(7) . . ?
C2 C1 H1 118.4 . . ?
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
V4 V3 3.1010(10) . ?
V4 V1 3.1004(12) . ?
V4 V2 3.0494(12) 2_666 ?
V4 O8 1.931(3) . ?
V4 O7 1.932(3) . ?
V4 O14 2.092(3) . ?
V4 O14 2.142(3) 2_666 ?
V4 O4 1.689(3) . ?
V4 O12 1.683(3) . ?
V5 V3 3.0130(12) 2_666 ?
V5 V1 3.0945(11) . ?
V5 V2 3.0783(12) . ?
V5 O8 1.958(3) . ?
V5 O7 2.000(3) 2_666 ?
V5 O14 2.259(3) 2_666 ?
V5 O5 1.821(3) . ?
V5 O9 1.855(3) . ?
V5 O13 1.600(3) . ?
V3 V1 3.1096(11) . ?
V3 O8 2.059(3) 2_666 ?
V3 O7 1.927(3) . ?
V3 O14 2.245(3) 2_666 ?
V3 O3 1.735(4) . ?
V3 O6 1.952(4) . ?
V3 O11 1.613(3) . ?
V1 V2 3.0660(12) . ?
V1 O14 2.339(3) 2_666 ?
V1 O4 2.050(3) . ?
V1 O5 1.853(3) . ?
V1 O3 1.925(3) . ?
V1 O2 1.804(4) . ?
V1 O1 1.592(4) . ?
V2 O14 2.293(3) 2_666 ?
V2 O12 2.047(4) 2_666 ?
V2 O9 1.798(4) . ?
V2 O6 1.999(4) . ?
V2 O2 1.845(4) . ?
V2 O10 1.597(4) . ?
Cl2 C17 1.716(6) . ?
Cl1 C7 1.758(8) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C3 1.302(7) . ?
N3 C19 1.376(7) . ?
N3 C11 1.358(9) . ?
N3 C20 1.463(8) . ?
N4 H4A 0.8642 . ?
N4 H4B 0.8649 . ?
N4 C13 1.335(7) . ?
N1 C9 1.351(8) . ?
N1 C10 1.469(10) . ?
N1 C1 1.368(10) . ?
C13 C14 1.435(7) . ?
C13 C12 1.402(8) . ?
C14 C19 1.403(7) . ?
C14 C15 1.398(8) . ?
C19 C18 1.402(8) . ?
N5 C21 1.406(9) . ?
N5 C23 1.331(11) . ?
N5 C22 1.416(10) . ?
C3 C4 1.391(9) . ?
C3 C2 1.494(10) . ?
C18 H18 0.9300 . ?
C18 C17 1.375(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.331(8) . ?
C9 C4 1.478(9) . ?
C9 C8 1.299(10) . ?
C4 C5 1.325(9) . ?
C12 H12 0.9300 . ?
C12 C11 1.367(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.371(9) . ?
C2 H2 0.9300 . ?
C2 C1 1.320(10) . ?
C11 H11 0.9300 . ?
O15 C23 1.305(11) . ?
C16 H16 0.9300 . ?
C16 C17 1.387(10) . ?
C8 H8 0.9300 . ?
C8 C7 1.403(10) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C6 H6 0.9300 . ?
C6 C7 1.377(10) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C23 H23 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C1 H1 0.9300 . ?
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
N2 H2A O8 0.86 2.06 2.887(5) 159.8 . yes
N2 H2A O6 0.86 3.20 3.781(6) 127.0 2_666 yes
N2 H2B O13 0.86 2.07 2.911(6) 164.4 2_766 yes
N4 H4A O11 0.86 2.39 3.085(6) 137.9 1_655 yes
N4 H4B O5 0.86 2.12 2.844(5) 141.3 . yes
C15 H15 O3 0.93 2.51 3.114(6) 123.1 1_655 yes
C15 H15 O11 0.93 2.58 3.507(7) 171.9 1_655 yes
C12 H12 O5 0.93 2.97 3.632(8) 129.0 . yes
C12 H12 O1 0.93 2.49 3.410(7) 168.1 . yes
C5 H5 O8 0.93 2.57 3.482(7) 166.4 . yes
C5 H5 O4 0.93 2.72 3.322(8) 123.1 . yes
C5 H5 O12 0.93 2.91 3.621(8) 134.4 . yes
C2 H2 O7 0.93 2.69 3.425(8) 137.0 1_655 yes
C2 H2 O9 0.93 2.73 3.625(9) 161.5 2_766 yes
C2 H2 O13 0.93 2.69 3.382(8) 131.6 2_766 yes
C11 H11 O1 0.93 2.42 3.214(7) 142.8 2_665 yes
C16 H16 O4 0.93 2.81 3.703(8) 162.1 1_655 yes
C16 H16 O1 0.93 3.03 3.751(7) 135.6 1_655 yes
C8 H8 O15 0.93 2.92 3.825(10) 165.2 1_665 yes
C20 H20B O2 0.96 2.89 3.759(8) 150.6 2_665 yes
C20 H20B O1 0.96 2.87 3.663(9) 140.2 2_665 yes
C6 H6 O16 0.93 2.97 3.602(11) 126.6 1_455 yes
C10 H10A O15 0.96 3.24 3.874(14) 125.3 1_665 yes
C10 H10B O16 0.96 2.05 2.993(12) 165.0 . yes
C10 H10C O6 0.96 3.02 3.642(10) 123.8 1_665 yes
C21 H21A O15 0.96 2.62 3.387(12) 137.4 2 yes
C21 H21B O10 0.96 2.37 3.164(10) 139.9 2 yes
C23 H23 O11 0.93 2.62 3.269(9) 127.7 . yes
C23 H23 N2 0.93 3.19 3.979(10) 143.5 2_666 yes
C22 H22A Cl2 0.96 2.94 3.839(11) 155.9 2_665 yes
C22 H22B O9 0.96 2.43 3.211(11) 137.9 1_455 yes
C22 H22B O13 0.96 2.98 3.897(14) 160.3 1_455 yes
C1 H1 O16 0.93 2.81 3.502(13) 132.4 2_876 yes
C1 H1 O16 0.93 2.43 3.253(10) 147.5 . 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
V4 V3 O3 V1 49.75(16) . . . . ?
V4 V1 O5 V5 51.63(15) . . . . ?
V4 V1 O2 V2 -6.0(3) . . . . ?
V4 V2 O9 V5 -52.95(17) 2_666 . . . ?
V4 V2 O2 V1 7.8(3) 2_666 . . . ?
V5 V3 O3 V1 80.9(2) 2_666 . . . ?
V5 V1 O2 V2 41.79(17) . . . . ?
V5 V2 O2 V1 -42.07(17) . . . . ?
V3 V4 O4 V1 -48.05(12) . . . . ?
V3 V4 O12 V2 79.7(2) . . . 2_666 ?
V3 V5 O5 V1 -82.3(2) 2_666 . . . ?
V3 V5 O9 V2 85.4(2) 2_666 . . . ?
V3 V1 O5 V5 10.4(2) . . . . ?
V3 V1 O2 V2 -51.69(17) . . . . ?
V1 V4 O12 V2 177.92(6) . . . 2_666 ?
V1 V5 O9 V2 -40.17(18) . . . . ?
V1 V2 O9 V5 40.46(17) . . . . ?
V2 V4 O4 V1 -177.39(6) 2_666 . . . ?
V2 V5 O5 V1 41.07(15) . . . . ?
V2 V1 O5 V5 -41.28(16) . . . . ?
O8 V4 O4 V1 78.72(16) . . . . ?
O8 V4 O12 V2 -83.60(17) . . . 2_666 ?
O8 V5 O5 V1 -84.17(18) . . . . ?
O8 V5 O9 V2 30.2(5) . . . . ?
O8 V3 O3 V1 13.5(5) 2_666 . . . ?
O7 V4 O4 V1 -82.06(16) . . . . ?
O7 V4 O12 V2 77.40(17) . . . 2_666 ?
O7 V5 O5 V1 -20.5(5) 2_666 . . . ?
O7 V5 O9 V2 84.8(2) 2_666 . . . ?
O7 V3 O3 V1 83.08(19) . . . . ?
O14 V4 O4 V1 -1.6(6) . . . . ?
O14 V4 O4 V1 -1.59(14) 2_666 . . . ?
O14 V4 O12 V2 -1.5(7) 2_666 . . 2_666 ?
O14 V4 O12 V2 -3.22(15) . . . 2_666 ?
O14 V5 O5 V1 -7.28(17) 2_666 . . . ?
O14 V5 O9 V2 9.14(19) 2_666 . . . ?
O14 V3 O3 V1 5.53(18) 2_666 . . . ?
O14 V1 O5 V5 7.10(16) 2_666 . . . ?
O14 V1 O2 V2 -5.22(18) 2_666 . . . ?
O14 V2 O9 V5 -8.99(18) 2_666 . . . ?
O14 V2 O2 V1 5.32(19) 2_666 . . . ?
O4 V4 O12 V2 176.67(14) . . . 2_666 ?
O4 V1 O5 V5 81.94(19) . . . . ?
O4 V1 O2 V2 -9.9(5) . . . . ?
O5 V5 O9 V2 -71.5(2) . . . . ?
O5 V1 O2 V2 72.8(2) . . . . ?
O12 V4 O4 V1 178.84(14) . . . . ?
O12 V2 O9 V5 -83.9(2) 2_666 . . . ?
O12 V2 O2 V1 17.7(5) 2_666 . . . ?
O9 V5 O5 V1 71.49(19) . . . . ?
O9 V2 O2 V1 -73.6(2) . . . . ?
O3 V1 O5 V5 23.5(4) . . . . ?
O3 V1 O2 V2 -80.9(2) . . . . ?
O6 V3 O3 V1 -71.7(2) . . . . ?
O6 V2 O9 V5 -24.0(5) . . . . ?
O6 V2 O2 V1 81.3(2) . . . . ?
O11 V3 O3 V1 -173.5(2) . . . . ?
O13 V5 O5 V1 174.51(19) . . . . ?
O13 V5 O9 V2 -174.6(2) . . . . ?
O2 V1 O5 V5 -73.1(2) . . . . ?
O2 V2 O9 V5 71.6(2) . . . . ?
O1 V1 O5 V5 -178.0(2) . . . . ?
O1 V1 O2 V2 177.0(2) . . . . ?
O10 V2 O9 V5 176.6(2) . . . . ?
O10 V2 O2 V1 -178.6(2) . . . . ?
N2 C3 C4 C9 177.8(6) . . . . ?
N2 C3 C4 C5 -0.4(10) . . . . ?
N2 C3 C2 C1 179.1(8) . . . . ?
N3 C19 C18 C17 -179.1(6) . . . . ?
N4 C13 C14 C19 179.5(5) . . . . ?
N4 C13 C14 C15 -0.4(9) . . . . ?
N4 C13 C12 C11 -179.7(6) . . . . ?
N1 C9 C4 C3 0.7(9) . . . . ?
N1 C9 C4 C5 179.0(6) . . . . ?
N1 C9 C8 C7 179.0(7) . . . . ?
C13 C14 C19 N3 -0.2(8) . . . . ?
C13 C14 C19 C18 -179.3(5) . . . . ?
C13 C14 C15 C16 179.0(6) . . . . ?
C13 C12 C11 N3 0.6(11) . . . . ?
C14 C13 C12 C11 -1.5(9) . . . . ?
C14 C19 C18 C17 0.0(9) . . . . ?
C14 C15 C16 C17 0.5(11) . . . . ?
C19 N3 C11 C12 0.6(10) . . . . ?
C19 C14 C15 C16 -0.8(9) . . . . ?
C19 C18 C17 Cl2 179.4(5) . . . . ?
C19 C18 C17 C16 -0.3(10) . . . . ?
C3 C4 C5 C6 -178.4(7) . . . . ?
C3 C2 C1 N1 5.5(14) . . . . ?
C15 C14 C19 N3 179.7(5) . . . . ?
C15 C14 C19 C18 0.5(8) . . . . ?
C15 C16 C17 Cl2 -179.6(5) . . . . ?
C15 C16 C17 C18 0.1(11) . . . . ?
C9 N1 C1 C2 -5.7(14) . . . . ?
C9 C4 C5 C6 3.2(10) . . . . ?
C9 C8 C7 Cl1 177.9(6) . . . . ?
C9 C8 C7 C6 0.9(12) . . . . ?
C4 C3 C2 C1 -2.4(11) . . . . ?
C4 C9 C8 C7 -0.4(11) . . . . ?
C4 C5 C6 C7 -2.9(12) . . . . ?
C12 C13 C14 C19 1.3(8) . . . . ?
C12 C13 C14 C15 -178.6(6) . . . . ?
C5 C6 C7 Cl1 -176.4(6) . . . . ?
C5 C6 C7 C8 0.7(12) . . . . ?
C2 C3 C4 C9 -0.5(9) . . . . ?
C2 C3 C4 C5 -178.8(6) . . . . ?
C11 N3 C19 C14 -0.8(8) . . . . ?
C11 N3 C19 C18 178.3(6) . . . . ?
C8 C9 C4 C3 -179.9(7) . . . . ?
C8 C9 C4 C5 -1.5(9) . . . . ?
C20 N3 C19 C14 178.7(6) . . . . ?
C20 N3 C19 C18 -2.2(9) . . . . ?
C20 N3 C11 C12 -178.9(7) . . . . ?
C10 N1 C9 C4 179.2(6) . . . . ?
C10 N1 C9 C8 -0.2(11) . . . . ?
C10 N1 C1 C2 177.2(9) . . . . ?
C21 N5 C23 O15 -4.5(14) . . . . ?
C22 N5 C23 O15 173.1(9) . . . . ?
C1 N1 C9 C4 2.3(10) . . . . ?
C1 N1 C9 C8 -177.2(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
14.0000 2.0000 -10.0000 -0.1174 -0.4165 0.8984
-15.0000 4.0000 3.0000 -0.2151 0.1761 -0.9545
0.0000 8.0000 11.0000 0.6726 -0.6282 -0.3049
2.0000 -8.0000 19.0000 0.9748 0.1733 -0.0328
-8.0000 -13.0000 13.0000 0.3217 0.8594 -0.4150
6.0000 -17.0000 6.0000 0.2967 0.7663 0.5434
-3.0000 9.0000 -19.0000 -0.9916 -0.2033 -0.0406
13.0000 -3.0000 -11.0000 -0.2540 -0.0706 0.9450
-1.0000 18.0000 -7.0000 -0.1990 -0.9661 -0.2661
11.0000 -12.0000 10.0000 0.7041 0.2590 0.6758
-1.0000 -6.0000 -13.0000 -0.7844 0.5640 0.2439
