# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_1670
_database_code_depnum_ccdc_archive 'CCDC 2217991'
loop_
_audit_author_name
_audit_author_address
'Kristof Van Hecke'
;Ghent University
Belgium
;
_audit_update_record             
;
2022-11-07 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_audit_creation_date             2021-03-18
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_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
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H10 N2 O2 Cl1 V10'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7293(6)
_cell_length_b                   11.8938(8)
_cell_length_c                   12.7361(8)
_cell_angle_alpha                112.102(6)
_cell_angle_beta                 97.669(5)
_cell_angle_gamma                93.798(5)
_cell_volume                     1480.33(18)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7340
_cell_measurement_theta_min      3.7750
_shelx_estimated_absorpt_T_max   0.736
_shelx_estimated_absorpt_T_min   0.435
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             722
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

_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.036
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

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4169
_reflns_number_total             5919
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0547
_refine_ls_restrained_S_all      1.025
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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_
_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) . . ?

_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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_am49
_database_code_depnum_ccdc_archive 'CCDC 2217992'
loop_
_audit_author_name
_audit_author_address
'Kristof Van Hecke'
;Ghent University
Belgium
;
_audit_update_record             
;
2022-11-07 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_audit_creation_date             2021-05-12
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H36 N2 O25 V6, 2(C16 H36 N), 2(C H Cl3)'
_chemical_formula_sum            'C56 H110 Cl6 N4 O25 V6'
_chemical_formula_weight         1757.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C56 H110 Cl6 N4 O25 V6'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   10.63100(10)
_cell_length_b                   19.7400(2)
_cell_length_c                   18.5098(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.0190(10)
_cell_angle_gamma                90
_cell_volume                     3884.39(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.5270
_cell_measurement_theta_min      3.2380
_shelx_estimated_absorpt_T_max   0.681
_shelx_estimated_absorpt_T_min   0.148
_exptl_absorpt_coefficient_mu    8.333
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.687
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1828
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 10 7 0.0410
0 -10 -7 0.0090
7 2 -1 0.1997
-7 -2 1 0.1617
0 -4 11 0.0308
1 10 -8 0.0480
2 9 8 0.0787
0 5 -11 0.0223

_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.05
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
-0.2990 10.0696 7.4218 -0.0665 -0.2810 -0.9574
0.2990 -10.0696 -7.4218 0.0665 0.2810 0.9574
6.8302 1.6563 -0.7085 0.5827 0.7600 -0.2879
-6.8302 -1.6563 0.7085 -0.5827 -0.7600 0.2879
0.2663 -3.7160 11.4864 -0.8133 0.3878 -0.4339
0.6960 9.6194 -7.8402 0.8955 -0.4264 -0.1278
1.6479 9.3824 7.6664 0.0273 -0.0120 -0.9996
-0.0263 5.3590 -10.9102 0.8604 -0.4101 0.3026

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19898
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.831
_diffrn_reflns_theta_min         3.273
_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 0.965
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -6.00   1.00    1.00    --  -41.68 125.00-120.00   81
  2  ω     27.00  98.00   1.00    1.00    --   41.68-125.00-150.00   71
  3  ω      6.00  83.00   1.00    1.00    --   41.68 -99.00-120.00   77
  4  ω    103.00 178.00   1.00    4.00    --  106.01  77.00-150.00   75
  5  ω    104.00 178.00   1.00    4.00    --  106.01 108.00 109.00   74
  6  ω     77.00 178.00   1.00    4.00    --  106.01  61.00   0.00  101
  7  ω     33.00 112.00   1.00    4.00    --  106.01-125.00-150.00   79
  8  ω     80.00 178.00   1.00    4.00    --  106.01  45.00 -60.00   98
  9  ω   -114.00 -12.00   1.00    1.00    --  -41.68 -65.00  94.00  102
 10  ω   -115.00 -86.00   1.00    1.00    --  -41.68 -57.00 -30.00   29
 11  ω   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00-150.00  101
;
_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      0.0695678000
_diffrn_orient_matrix_UB_12      0.0394353000
_diffrn_orient_matrix_UB_13      -0.0596577000
_diffrn_orient_matrix_UB_21      0.1224132000
_diffrn_orient_matrix_UB_22      -0.0379981000
_diffrn_orient_matrix_UB_23      0.0186265000
_diffrn_orient_matrix_UB_31      -0.0343650000
_diffrn_orient_matrix_UB_32      -0.0555903000
_diffrn_orient_matrix_UB_33      -0.0549610000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6027
_reflns_number_total             7301
_reflns_odcompleteness_completeness 96.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.095
_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)+(0.0267P)²+1.4836P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1057
_refine_special_details          ?
_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 Ternary CH refined with riding coordinates:
 C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.44947(4) 0.43594(3) 0.90477(3) 0.01737(12) Uani 1 1 d . . . . .
V2 V 0.53593(4) 0.40134(3) 1.05665(3) 0.01794(12) Uani 1 1 d . . . . .
V3 V 0.69033(4) 0.50500(3) 0.94850(3) 0.01651(11) Uani 1 1 d . . . . .
O1 O 0.40754(17) 0.52826(10) 0.87018(11) 0.0179(4) Uani 1 1 d . . . . .
O2 O 0.28235(17) 0.44564(10) 0.95720(10) 0.0156(4) Uani 1 1 d . . . . .
O3 O 0.29623(17) 0.57807(10) 0.98645(11) 0.0167(4) Uani 1 1 d . . . . .
O4 O 0.1087(2) 0.60564(12) 0.74683(13) 0.0309(5) Uani 1 1 d . . . . .
O5 O -0.1285(2) 0.59816(11) 0.69610(12) 0.0265(5) Uani 1 1 d . . . . .
O6 O -0.1057(3) 0.48820(13) 0.66857(14) 0.0412(6) Uani 1 1 d . . . . .
O7 O 0.500000 0.500000 1.000000 0.0153(6) Uani 1 2 d S T P . .
O8 O 0.61217(18) 0.44939(11) 0.88253(11) 0.0197(4) Uani 1 1 d . . . . .
O9 O 0.62771(18) 0.58194(10) 0.91167(11) 0.0201(4) Uani 1 1 d . . . . .
O10 O 0.83551(19) 0.50330(11) 0.92331(11) 0.0216(4) Uani 1 1 d . . . . .
O11 O 0.39522(19) 0.39486(11) 0.83705(12) 0.0229(5) Uani 1 1 d . . . . .
O12 O 0.48498(18) 0.36767(10) 0.97106(12) 0.0194(4) Uani 1 1 d . . . . .
O13 O 0.57830(19) 0.33594(10) 1.10171(12) 0.0229(4) Uani 1 1 d . . . . .
N1 N 0.0595(2) 0.54095(14) 0.84512(14) 0.0199(5) Uani 1 1 d D . . . .
C1 C 0.1799(3) 0.53239(14) 0.88255(15) 0.0161(6) Uani 1 1 d . . . . .
C2 C 0.1874(3) 0.58562(15) 0.94242(16) 0.0183(6) Uani 1 1 d . . . . .
H2A H 0.188095 0.631285 0.920313 0.022 Uiso 1 1 calc R . . . .
H2B H 0.111515 0.582160 0.973145 0.022 Uiso 1 1 calc R . . . .
C3 C 0.2925(2) 0.53925(16) 0.83092(15) 0.0180(6) Uani 1 1 d . . . . .
H3A H 0.285142 0.505617 0.791473 0.022 Uiso 1 1 calc R . . . .
H3B H 0.293038 0.585058 0.809154 0.022 Uiso 1 1 calc R . . . .
C4 C 0.1742(2) 0.46114(14) 0.91493(15) 0.0164(6) Uani 1 1 d . . . . .
H4A H 0.098171 0.457294 0.945563 0.020 Uiso 1 1 calc R . . . .
H4B H 0.166636 0.427628 0.875370 0.020 Uiso 1 1 calc R . . . .
C5 C 0.0330(3) 0.57712(15) 0.78536(16) 0.0205(6) Uani 1 1 d . . . . .
C6 C -0.1080(3) 0.58152(17) 0.77013(17) 0.0242(7) Uani 1 1 d . . . . .
H6A H -0.148408 0.537556 0.781304 0.029 Uiso 1 1 calc R . . . .
H6B H -0.146455 0.616589 0.801342 0.029 Uiso 1 1 calc R . . . .
C7 C -0.1218(3) 0.54551(17) 0.64935(19) 0.0267(7) Uani 1 1 d . . . . .
C8 C -0.1346(3) 0.56943(18) 0.57287(19) 0.0323(8) Uani 1 1 d . . . . .
H8A H -0.052180 0.586940 0.556365 0.039 Uiso 1 1 calc R . . . .
H8B H -0.195187 0.607485 0.571514 0.039 Uiso 1 1 calc R . . . .
C9 C -0.1780(4) 0.51535(19) 0.5210(2) 0.0354(8) Uani 1 1 d . . . . .
H9A H -0.264006 0.500957 0.534687 0.042 Uiso 1 1 calc R . . . .
H9B H -0.122108 0.475487 0.525689 0.042 Uiso 1 1 calc R . . . .
C10 C -0.1790(4) 0.5381(2) 0.4428(2) 0.0409(9) Uani 1 1 d . . . . .
H10A H -0.092411 0.550534 0.428285 0.049 Uiso 1 1 calc R . . . .
H10B H -0.232182 0.579087 0.438295 0.049 Uiso 1 1 calc R . . . .
C11 C -0.2286(5) 0.4835(2) 0.3916(2) 0.0516(11) Uani 1 1 d . . . . .
H11A H -0.225997 0.500361 0.341801 0.077 Uiso 1 1 calc GR . . . .
H11B H -0.315581 0.472277 0.404479 0.077 Uiso 1 1 calc GR . . . .
H11C H -0.176158 0.442864 0.395622 0.077 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.30422(12) 0.22989(6) 1.04942(9) 0.0704(4) Uani 1 1 d . . . . .
Cl2 Cl 0.18253(11) 0.26601(5) 0.91517(6) 0.0528(3) Uani 1 1 d . . . . .
Cl3 Cl 0.09936(8) 0.32513(5) 1.04942(5) 0.0408(2) Uani 1 1 d . . . . .
C28 C 0.2296(3) 0.29458(17) 1.0016(2) 0.0308(8) Uani 1 1 d . . . . .
H28 H 0.290705 0.332626 0.995139 0.037 Uiso 1 1 calc R . . . .
N2 N 0.7077(2) 0.28256(14) 0.77928(15) 0.0251(6) Uani 1 1 d . . . . .
C12 C 0.7254(3) 0.29255(17) 0.85988(19) 0.0291(7) Uani 1 1 d . . . . .
H12A H 0.642388 0.302094 0.881831 0.035 Uiso 1 1 calc R . . . .
H12B H 0.779030 0.332923 0.867573 0.035 Uiso 1 1 calc R . . . .
C13 C 0.7843(4) 0.23287(17) 0.8993(2) 0.0331(8) Uani 1 1 d . . . . .
H13A H 0.730500 0.192338 0.893259 0.040 Uiso 1 1 calc R . . . .
H13B H 0.867717 0.222781 0.878053 0.040 Uiso 1 1 calc R . . . .
C14 C 0.7992(3) 0.24839(19) 0.9786(2) 0.0364(8) Uani 1 1 d . . . . .
H14A H 0.714989 0.255652 1.000134 0.044 Uiso 1 1 calc R . . . .
H14B H 0.847621 0.290902 0.984140 0.044 Uiso 1 1 calc R . . . .
C15 C 0.8659(4) 0.1920(2) 1.0196(2) 0.0428(9) Uani 1 1 d . . . . .
H15A H 0.947453 0.182866 0.996933 0.064 Uiso 1 1 calc GR . . . .
H15B H 0.814264 0.150834 1.018274 0.064 Uiso 1 1 calc GR . . . .
H15C H 0.878799 0.205845 1.069856 0.064 Uiso 1 1 calc GR . . . .
C16 C 0.8326(3) 0.26651(17) 0.74283(19) 0.0278(7) Uani 1 1 d . . . . .
H16A H 0.863351 0.222624 0.761790 0.033 Uiso 1 1 calc R . . . .
H16B H 0.817072 0.260563 0.690476 0.033 Uiso 1 1 calc R . . . .
C17 C 0.9363(3) 0.31850(18) 0.7521(2) 0.0316(8) Uani 1 1 d . . . . .
H17A H 0.950411 0.327245 0.804154 0.038 Uiso 1 1 calc R . . . .
H17B H 0.911334 0.361634 0.728904 0.038 Uiso 1 1 calc R . . . .
C18 C 1.0568(3) 0.2923(2) 0.7179(2) 0.0474(11) Uani 1 1 d . . . . .
H18A H 1.040469 0.281680 0.666471 0.057 Uiso 1 1 calc R . . . .
H18B H 1.081917 0.249798 0.742290 0.057 Uiso 1 1 calc R . . . .
C19 C 1.1646(4) 0.3429(3) 0.7226(2) 0.0523(12) Uani 1 1 d . . . . .
H19A H 1.237377 0.325288 0.696079 0.078 Uiso 1 1 calc GR . . . .
H19B H 1.187624 0.349737 0.773391 0.078 Uiso 1 1 calc GR . . . .
H19C H 1.138356 0.386137 0.701497 0.078 Uiso 1 1 calc GR . . . .
C20 C 0.6218(3) 0.22253(17) 0.76484(19) 0.0284(7) Uani 1 1 d . . . . .
H20A H 0.662551 0.181181 0.784072 0.034 Uiso 1 1 calc R . . . .
H20B H 0.613422 0.216792 0.711919 0.034 Uiso 1 1 calc R . . . .
C21 C 0.4906(3) 0.22812(18) 0.7974(2) 0.0356(8) Uani 1 1 d . . . . .
H21A H 0.452465 0.272016 0.783648 0.043 Uiso 1 1 calc R . . . .
H21B H 0.496362 0.226467 0.850792 0.043 Uiso 1 1 calc R . . . .
C22 C 0.4075(3) 0.17010(18) 0.7706(2) 0.0373(9) Uani 1 1 d . . . . .
H22A H 0.319644 0.179050 0.785448 0.045 Uiso 1 1 calc R . . . .
H22B H 0.409703 0.169492 0.717100 0.045 Uiso 1 1 calc R . . . .
C23 C 0.4458(4) 0.1010(2) 0.7982(3) 0.0568(13) Uani 1 1 d . . . . .
H23A H 0.528030 0.088793 0.778128 0.085 Uiso 1 1 calc GR . . . .
H23B H 0.383139 0.067352 0.783309 0.085 Uiso 1 1 calc GR . . . .
H23C H 0.451016 0.102050 0.851042 0.085 Uiso 1 1 calc GR . . . .
C24 C 0.6520(3) 0.34764(16) 0.7491(2) 0.0301(7) Uani 1 1 d . . . . .
H24A H 0.576495 0.359355 0.777752 0.036 Uiso 1 1 calc R . . . .
H24B H 0.714023 0.384523 0.755898 0.036 Uiso 1 1 calc R . . . .
C25 C 0.6153(4) 0.3454(2) 0.6700(2) 0.0417(9) Uani 1 1 d . . . . .
H25A H 0.689629 0.333052 0.640537 0.050 Uiso 1 1 calc R . . . .
H25B H 0.550213 0.310168 0.662604 0.050 Uiso 1 1 calc R . . . .
C26 C 0.5653(4) 0.4130(2) 0.6455(3) 0.0494(11) Uani 1 1 d . . . . .
H26A H 0.630893 0.447878 0.652952 0.059 Uiso 1 1 calc R . . . .
H26B H 0.491873 0.425277 0.675638 0.059 Uiso 1 1 calc R . . . .
C27 C 0.5262(4) 0.4129(2) 0.5664(3) 0.0605(14) Uani 1 1 d . . . . .
H27A H 0.599666 0.403534 0.536113 0.091 Uiso 1 1 calc GR . . . .
H27B H 0.491357 0.457343 0.553765 0.091 Uiso 1 1 calc GR . . . .
H27C H 0.462290 0.377925 0.558531 0.091 Uiso 1 1 calc GR . . . .
H1 H -0.005(3) 0.526(2) 0.870(2) 0.073 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 3.0353(7) . ?
V1 V3 3.0114(7) . ?
V1 O1 1.982(2) . ?
V1 O2 2.0338(19) . ?
V1 O7 2.2347(5) . ?
V1 O8 1.798(2) . ?
V1 O11 1.600(2) . ?
V1 O12 1.861(2) . ?
V2 V3 3.0354(7) 3_667 ?
V2 O1 2.031(2) 3_667 ?
V2 O3 1.997(2) 3_667 ?
V2 O7 2.2446(5) . ?
V2 O9 1.866(2) 3_667 ?
V2 O12 1.801(2) . ?
V2 O13 1.602(2) . ?
V3 O2 2.020(2) 3_667 ?
V3 O3 2.039(2) 3_667 ?
V3 O7 2.2392(5) . ?
V3 O8 1.840(2) . ?
V3 O9 1.793(2) . ?
V3 O10 1.613(2) . ?
O1 C3 1.439(3) . ?
O2 C4 1.424(3) . ?
O3 C2 1.422(3) . ?
O4 C5 1.214(4) . ?
O5 C6 1.426(4) . ?
O5 C7 1.354(4) . ?
O6 C7 1.198(4) . ?
N1 C1 1.465(4) . ?
N1 C5 1.346(4) . ?
C1 C2 1.529(4) . ?
C1 C3 1.537(4) . ?
C1 C4 1.530(4) . ?
C5 C6 1.528(4) . ?
C7 C8 1.498(5) . ?
C8 C9 1.508(5) . ?
C9 C10 1.516(5) . ?
C10 C11 1.530(5) . ?
Cl1 C28 1.744(4) . ?
Cl2 C28 1.768(4) . ?
Cl3 C28 1.751(4) . ?
N2 C12 1.517(4) . ?
N2 C16 1.524(4) . ?
N2 C20 1.519(4) . ?
N2 C24 1.520(4) . ?
C12 C13 1.521(5) . ?
C13 C14 1.508(5) . ?
C14 C15 1.522(5) . ?
C16 C17 1.516(4) . ?
C17 C18 1.519(5) . ?
C18 C19 1.523(5) . ?
C20 C21 1.525(4) . ?
C21 C22 1.529(5) . ?
C22 C23 1.513(6) . ?
C24 C25 1.516(5) . ?
C25 C26 1.506(5) . ?
C26 C27 1.521(7) . ?

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 66.153(16) . . ?
O1 V1 V2 125.04(6) . . ?
O1 V1 V3 82.06(6) . . ?
O1 V1 O2 82.60(8) . . ?
O1 V1 O7 77.80(6) . . ?
O2 V1 V2 81.00(6) . . ?
O2 V1 V3 124.89(6) . . ?
O2 V1 O7 77.30(6) . . ?
O7 V1 V2 47.479(13) . . ?
O7 V1 V3 47.755(13) . . ?
O8 V1 V2 87.38(7) . . ?
O8 V1 V3 34.58(7) . . ?
O8 V1 O1 90.37(9) . . ?
O8 V1 O2 159.40(9) . . ?
O8 V1 O7 82.30(7) . . ?
O8 V1 O12 93.61(9) . . ?
O11 V1 V2 136.09(9) . . ?
O11 V1 V3 138.25(8) . . ?
O11 V1 O1 97.58(10) . . ?
O11 V1 O2 96.13(9) . . ?
O11 V1 O7 172.32(8) . . ?
O11 V1 O8 104.00(10) . . ?
O11 V1 O12 102.85(11) . . ?
O12 V1 V2 33.40(6) . . ?
O12 V1 V3 88.75(6) . . ?
O12 V1 O1 157.54(9) . . ?
O12 V1 O2 86.02(8) . . ?
O12 V1 O7 80.85(7) . . ?
V1 V2 V3 66.052(16) . 3_667 ?
O1 V2 V1 123.57(6) 3_667 . ?
O1 V2 V3 80.70(6) 3_667 3_667 ?
O1 V2 O7 76.59(6) 3_667 . ?
O3 V2 V1 81.63(6) 3_667 . ?
O3 V2 V3 124.87(6) 3_667 3_667 ?
O3 V2 O1 82.12(8) 3_667 3_667 ?
O3 V2 O7 77.80(6) 3_667 . ?
O7 V2 V1 47.205(14) . . ?
O7 V2 V3 47.317(13) . 3_667 ?
O9 V2 V1 88.24(7) 3_667 . ?
O9 V2 V3 33.18(6) 3_667 3_667 ?
O9 V2 O1 86.85(9) 3_667 3_667 ?
O9 V2 O3 157.40(9) 3_667 3_667 ?
O9 V2 O7 80.49(6) 3_667 . ?
O12 V2 V1 34.66(6) . . ?
O12 V2 V3 87.65(6) . 3_667 ?
O12 V2 O1 158.08(9) . 3_667 ?
O12 V2 O3 89.55(9) . 3_667 ?
O12 V2 O7 81.85(7) . . ?
O12 V2 O9 93.53(9) . 3_667 ?
O13 V2 V1 138.49(9) . . ?
O13 V2 V3 136.89(8) . 3_667 ?
O13 V2 O1 96.96(10) . 3_667 ?
O13 V2 O3 96.95(10) . 3_667 ?
O13 V2 O7 172.10(8) . . ?
O13 V2 O9 103.94(10) . 3_667 ?
O13 V2 O12 104.19(11) . . ?
V1 V3 V2 66.018(16) . 3_667 ?
O2 V3 V1 124.93(6) 3_667 . ?
O2 V3 V2 81.20(6) 3_667 3_667 ?
O2 V3 O3 82.40(8) 3_667 3_667 ?
O2 V3 O7 77.47(5) 3_667 . ?
O3 V3 V1 81.61(6) 3_667 . ?
O3 V3 V2 124.31(6) 3_667 3_667 ?
O3 V3 O7 77.08(5) 3_667 . ?
O7 V3 V1 47.630(13) . . ?
O7 V3 V2 47.468(13) . 3_667 ?
O8 V3 V1 33.68(6) . . ?
O8 V3 V2 89.13(6) . 3_667 ?
O8 V3 O2 157.82(9) . 3_667 ?
O8 V3 O3 86.77(9) . 3_667 ?
O8 V3 O7 81.28(6) . . ?
O9 V3 V1 88.03(7) . . ?
O9 V3 V2 34.71(6) . 3_667 ?
O9 V3 O2 88.46(9) . 3_667 ?
O9 V3 O3 158.69(9) . 3_667 ?
O9 V3 O7 82.17(6) . . ?
O9 V3 O8 94.90(10) . . ?
O10 V3 V1 136.60(8) . . ?
O10 V3 V2 139.64(8) . 3_667 ?
O10 V3 O2 97.04(10) . 3_667 ?
O10 V3 O3 94.99(9) . 3_667 ?
O10 V3 O7 170.80(8) . . ?
O10 V3 O8 103.16(10) . . ?
O10 V3 O9 105.24(10) . . ?
V1 O1 V2 110.31(9) . 3_667 ?
C3 O1 V1 119.52(17) . . ?
C3 O1 V2 118.99(17) . 3_667 ?
V3 O2 V1 109.41(9) 3_667 . ?
C4 O2 V1 117.61(16) . . ?
C4 O2 V3 119.14(16) . 3_667 ?
V2 O3 V3 109.70(9) 3_667 3_667 ?
C2 O3 V2 118.44(17) . 3_667 ?
C2 O3 V3 118.65(17) . 3_667 ?
C7 O5 C6 115.4(3) . . ?
V1 O7 V1 180.0 3_667 . ?
V1 O7 V2 94.686(19) . 3_667 ?
V1 O7 V2 85.316(19) 3_667 3_667 ?
V1 O7 V2 85.316(19) . . ?
V1 O7 V2 94.682(19) 3_667 . ?
V1 O7 V3 95.385(18) 3_667 . ?
V1 O7 V3 95.385(18) . 3_667 ?
V1 O7 V3 84.615(18) . . ?
V1 O7 V3 84.614(18) 3_667 3_667 ?
V2 O7 V2 180.0 . 3_667 ?
V3 O7 V2 85.217(18) 3_667 . ?
V3 O7 V2 85.215(18) . 3_667 ?
V3 O7 V2 94.785(18) . . ?
V3 O7 V2 94.783(18) 3_667 3_667 ?
V3 O7 V3 180.0 3_667 . ?
V1 O8 V3 111.74(11) . . ?
V3 O9 V2 112.11(10) . 3_667 ?
V2 O12 V1 111.94(10) . . ?
C5 N1 C1 129.2(2) . . ?
N1 C1 C2 108.0(2) . . ?
N1 C1 C3 112.1(2) . . ?
N1 C1 C4 104.8(2) . . ?
C2 C1 C3 110.4(2) . . ?
C2 C1 C4 110.5(2) . . ?
C4 C1 C3 110.8(2) . . ?
O3 C2 C1 112.7(2) . . ?
O1 C3 C1 109.5(2) . . ?
O2 C4 C1 112.3(2) . . ?
O4 C5 N1 126.2(3) . . ?
O4 C5 C6 121.0(3) . . ?
N1 C5 C6 112.8(3) . . ?
O5 C6 C5 109.9(2) . . ?
O5 C7 C8 110.9(3) . . ?
O6 C7 O5 122.8(3) . . ?
O6 C7 C8 126.2(3) . . ?
C7 C8 C9 113.9(3) . . ?
C8 C9 C10 113.6(3) . . ?
C9 C10 C11 112.7(4) . . ?
Cl1 C28 Cl2 110.7(2) . . ?
Cl1 C28 Cl3 110.8(2) . . ?
Cl3 C28 Cl2 110.09(18) . . ?
C12 N2 C16 110.7(2) . . ?
C12 N2 C20 110.4(3) . . ?
C12 N2 C24 107.5(2) . . ?
C20 N2 C16 106.5(2) . . ?
C20 N2 C24 111.2(3) . . ?
C24 N2 C16 110.6(3) . . ?
N2 C12 C13 115.0(3) . . ?
C14 C13 C12 110.6(3) . . ?
C13 C14 C15 112.6(3) . . ?
C17 C16 N2 116.3(3) . . ?
C16 C17 C18 109.6(3) . . ?
C17 C18 C19 112.8(4) . . ?
N2 C20 C21 115.1(3) . . ?
C20 C21 C22 110.2(3) . . ?
C23 C22 C21 114.2(3) . . ?
C25 C24 N2 115.5(3) . . ?
C26 C25 C24 110.8(3) . . ?
C25 C26 C27 112.7(4) . . ?

_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 2.374
_oxdiff_exptl_absorpt_empirical_full_min 0.670

