# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_bk100-2
_database_code_depnum_ccdc_archive 'CCDC 2101114'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-08-03 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_audit_creation_date             2021-08-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H39 Cl3 N3 V'
_chemical_formula_sum            'C33 H39 Cl3 N3 V'
_chemical_formula_weight         634.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H39 Cl3 N3 V'
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'
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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.08899(15)
_cell_length_b                   19.34274(17)
_cell_length_c                   14.78739(17)
_cell_angle_alpha                90
_cell_angle_beta                 107.2322(12)
_cell_angle_gamma                90
_cell_volume                     3302.59(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31694
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      75.0050
_cell_measurement_theta_min      3.8450
_shelx_estimated_absorpt_T_max   0.866
_shelx_estimated_absorpt_T_min   0.638
_exptl_absorpt_coefficient_mu    4.933
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense green'
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0100
0 -1 0 0.0160
0 0 -1 0.0433
0 0 1 0.0433
1 0 -1 0.0194
-1 0 1 0.0482
-1 2 -2 0.0326
-2 -1 0 0.0426
-2 -2 1 0.0402
1 2 1 0.0441
-1 -2 -2 0.0411
0 1 -1 0.0276
-1 1 2 0.0419
-1 2 -1 0.0295

_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
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
0.0000 1.0000 -0.0000 -0.0246 0.0455 0.0605
-0.0000 -1.0000 0.0000 0.0246 -0.0455 -0.0605
0.0000 -0.0000 -1.0000 0.0959 -0.0146 0.0499
-0.0000 0.0000 1.0000 -0.0959 0.0146 -0.0499
1.0000 -0.0000 -1.0000 0.0148 -0.1126 0.0906
-1.0000 0.0000 1.0000 -0.0148 0.1126 -0.0906
-1.0000 2.0000 -2.0000 0.2234 0.1599 0.1801
-2.0000 -1.0000 0.0000 0.1867 0.1505 -0.1418
-2.0000 -2.0000 1.0000 0.1155 0.1196 -0.2522
1.0000 2.0000 1.0000 -0.2262 0.0076 0.1117
-1.0000 -2.0000 -2.0000 0.3220 -0.0222 -0.0618
0.0000 1.0000 -1.0000 0.0712 0.0309 0.1104
-1.0000 1.0000 2.0000 -0.1354 0.1727 -0.0800
-1.0000 2.0000 -1.0000 0.1276 0.1745 0.1302

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54724
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.658
_diffrn_reflns_theta_min         3.875
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     42.00  68.00   0.50    1.00    --   65.75-125.00-150.00   52
  2  ω     39.00  68.00   0.50    1.00    --   65.75-125.00 150.00   58
  3  ω     26.00  86.00   0.50    1.00    --   65.75-125.00   0.00  120
  4  ω     36.00  62.00   0.50    1.00    --   65.75-125.00 -30.00   52
  5  ω    -60.00 -33.00   0.50    1.00    --  -67.30 125.00-150.00   54
  6  ω    -78.00 -52.00   0.50    1.00    --  -67.30 -15.00 -60.00   52
  7  ω    -97.00 -46.00   0.50    1.00    --  -67.30   0.00 150.00  102
  8  ω    -92.00 -67.00   0.50    1.00    --  -67.30 125.00  30.00   50
  9  ω    -93.00 -36.00   0.50    1.00    --  -67.30   0.00 -90.00  114
 10  ω    -92.00 -32.00   0.50    1.00    --  -67.30 125.00 -60.00  120
 11  ω    -77.00 -40.00   0.50    1.00    --  -67.30   0.00-180.00   74
 12  ω    -73.00 -41.00   0.50    1.00    --  -67.30   0.00  30.00   64
 13  ω   -109.00 -54.00   0.50    1.00    --  -67.30 -15.00  90.00  110
 14  ω    -74.00 -35.00   0.50    1.00    --  -67.30 125.00   0.00   78
 15  ω     58.00  84.00   0.50    1.00    --   72.75  15.00 -60.00   52
 16  ω     51.00 110.00   0.50    1.00    --   72.75  15.00 120.00  118
 17  ω     36.00  98.00   0.50    1.00    --   72.75-125.00 120.00  124
 18  ω     50.00 112.00   0.50    1.00    --   72.75  15.00  60.00  124
 19  ω     64.00  97.00   0.50    1.00    --   72.75-125.00  30.00   66
 20  ω    -97.00 -36.00   0.50    1.00    --  -73.25 122.00-156.57  122
 21  ω    -97.00 -36.00   0.50    1.00    --  -73.25 123.00 165.23  122
 22  ω   -113.00 -45.00   0.50    1.00    --  -73.25 149.00 115.09  136
 23  ω   -111.00 -46.00   0.50    1.00    --  -73.25 146.00  53.23  130
 24  ω     74.00  99.00   0.50    4.00    --   76.90-118.00  -1.76   50
 25  ω     37.00  69.00   0.50    4.00    --   76.90-118.00  -1.76   64
 26  ω     38.00  99.00   0.50    4.00    --   76.90-118.00 -40.03  122
 27  ω     45.00 101.00   0.50    4.00    --   76.97-125.00  60.00  112
 28  ω     77.00 102.00   0.50    4.00    --   76.97-125.00 120.00   50
 29  ω     77.00 102.00   0.50    4.00    --   76.97-125.00  30.00   50
 30  ω     50.00 119.00   0.50    4.00    --   76.97  15.00-120.00  138
 31  ω     55.00 115.00   0.50    4.00    --   76.97  15.00 -30.00  120
 32  ω     72.00 102.00   0.50    4.00    --   76.97-125.00  90.00   60
 33  ω     49.00 111.00   0.50    4.00    --   76.97  15.00-180.00  124
 34  ω     54.00 101.00   0.50    4.00    --   76.97-125.00-150.00   94
 35  ω     77.00 102.00   0.50    4.00    --   76.97-125.00 150.00   50
 36  ω     38.00  63.00   0.50    4.00    --   76.97-125.00 150.00   50
 37  ω     77.00 102.00   0.50    4.00    --   76.97-125.00 -30.00   50
 38  ω     59.00 102.00   0.50    4.00    --   76.97-125.00 -60.00   86
 39  ω     69.00 102.00   0.50    4.00    --   76.97-125.00-120.00   66
 40  ω     41.00 102.00   0.50    4.00    --   76.97-125.00 -90.00  122
 41  ω     57.00 101.00   0.50    4.00    --   76.97-125.00-180.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0810140000
_diffrn_orient_matrix_UB_12      -0.0246464000
_diffrn_orient_matrix_UB_13      -0.0958635000
_diffrn_orient_matrix_UB_21      -0.0980040000
_diffrn_orient_matrix_UB_22      0.0455186000
_diffrn_orient_matrix_UB_23      0.0145905000
_diffrn_orient_matrix_UB_31      0.0406531000
_diffrn_orient_matrix_UB_32      0.0604776000
_diffrn_orient_matrix_UB_33      -0.0499162000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6266
_reflns_number_total             6754
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6754
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0345
_refine_ls_restrained_S_all      1.066
_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)+(0.0599P)²+1.4839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1027
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.62808(2) 0.87637(2) 0.34999(2) 0.02573(9) Uani 1 1 d . . . . .
Cl1 Cl 0.56296(4) 0.96063(2) 0.42038(3) 0.03849(12) Uani 1 1 d . . . . .
Cl2 Cl 0.58265(4) 0.89527(2) 0.19590(3) 0.03748(12) Uani 1 1 d . . . . .
Cl3 Cl 0.81372(4) 0.85574(3) 0.41611(4) 0.05490(15) Uani 1 1 d . . . . .
N1 N 0.38232(12) 0.65796(7) 0.39312(9) 0.0246(3) Uani 1 1 d . . . . .
N2 N 0.47823(13) 0.62711(7) 0.38823(10) 0.0271(3) Uani 1 1 d . . . . .
N3 N 0.54582(12) 0.67864(7) 0.37893(9) 0.0256(3) Uani 1 1 d . . . . .
C1 C 0.38661(14) 0.72869(8) 0.38758(10) 0.0236(3) Uani 1 1 d . . . . .
C2 C 0.49585(14) 0.74275(8) 0.37706(10) 0.0248(3) Uani 1 1 d . . . . .
C3 C 0.55353(14) 0.80472(9) 0.36524(11) 0.0277(3) Uani 1 1 d . . . . .
C4 C 0.29681(14) 0.77715(8) 0.39549(11) 0.0240(3) Uani 1 1 d . . . . .
C5 C 0.17846(15) 0.76160(9) 0.36581(12) 0.0298(3) Uani 1 1 d . . . . .
H5 H 0.153083 0.717803 0.338384 0.036 Uiso 1 1 calc R U . . .
C6 C 0.09813(15) 0.80955(10) 0.37610(12) 0.0327(4) Uani 1 1 d . . . . .
H6 H 0.017990 0.798449 0.356079 0.039 Uiso 1 1 calc R U . . .
C7 C 0.13420(17) 0.87371(9) 0.41553(13) 0.0326(4) Uani 1 1 d . . . . .
H7 H 0.078872 0.906650 0.422243 0.039 Uiso 1 1 calc R U . . .
C8 C 0.25098(17) 0.88970(9) 0.44510(13) 0.0337(4) Uani 1 1 d . . . . .
H8 H 0.275677 0.933561 0.472608 0.040 Uiso 1 1 calc R U . . .
C9 C 0.33241(15) 0.84200(9) 0.43484(12) 0.0294(3) Uani 1 1 d . . . . .
H9 H 0.412386 0.853545 0.454622 0.035 Uiso 1 1 calc R U . . .
C10 C 0.29110(15) 0.61348(8) 0.40557(12) 0.0267(3) Uani 1 1 d . . . . .
C11 C 0.20884(16) 0.58902(8) 0.32372(12) 0.0301(4) Uani 1 1 d . . . . .
C12 C 0.12292(16) 0.54587(9) 0.33755(14) 0.0352(4) Uani 1 1 d . . . . .
H12 H 0.064871 0.528128 0.284321 0.042 Uiso 1 1 calc R U . . .
C13 C 0.12125(17) 0.52860(9) 0.42796(15) 0.0384(4) Uani 1 1 d . . . . .
H13 H 0.061369 0.499640 0.435969 0.046 Uiso 1 1 calc R U . . .
C14 C 0.20552(17) 0.55288(10) 0.50691(14) 0.0372(4) Uani 1 1 d . . . . .
H14 H 0.203083 0.539925 0.568260 0.045 Uiso 1 1 calc R U . . .
C15 C 0.29417(16) 0.59619(9) 0.49773(12) 0.0299(4) Uani 1 1 d . . . . .
C16 C 0.21484(17) 0.60623(10) 0.22536(12) 0.0358(4) Uani 1 1 d . . . . .
H16 H 0.271873 0.644682 0.231449 0.043 Uiso 1 1 calc R U . . .
C17 C 0.2601(2) 0.54373(12) 0.18366(15) 0.0471(5) Uani 1 1 d . . . . .
H17A H 0.334885 0.529350 0.226775 0.071 Uiso 1 1 calc R U . . .
H17B H 0.269658 0.556243 0.122205 0.071 Uiso 1 1 calc R U . . .
H17C H 0.204608 0.505572 0.175293 0.071 Uiso 1 1 calc R U . . .
C18 C 0.0984(2) 0.63068(11) 0.15857(15) 0.0461(5) Uani 1 1 d . . . . .
H18A H 0.042958 0.592353 0.146186 0.069 Uiso 1 1 calc R U . . .
H18B H 0.109352 0.646375 0.098774 0.069 Uiso 1 1 calc R U . . .
H18C H 0.068710 0.668936 0.188100 0.069 Uiso 1 1 calc R U . . .
C19 C 0.38790(18) 0.62266(10) 0.58375(13) 0.0352(4) Uani 1 1 d . . . . .
H19 H 0.455902 0.636635 0.562537 0.042 Uiso 1 1 calc R U . . .
C20 C 0.4283(2) 0.56662(12) 0.65945(15) 0.0528(6) Uani 1 1 d . . . . .
H20A H 0.366575 0.556941 0.688177 0.079 Uiso 1 1 calc R U . . .
H20B H 0.497481 0.582660 0.708366 0.079 Uiso 1 1 calc R U . . .
H20C H 0.446744 0.524384 0.630262 0.079 Uiso 1 1 calc R U . . .
C21 C 0.3467(2) 0.68629(11) 0.62562(14) 0.0440(5) Uani 1 1 d . . . . .
H21A H 0.321508 0.721853 0.576611 0.066 Uiso 1 1 calc R U . . .
H21B H 0.410356 0.704332 0.677966 0.066 Uiso 1 1 calc R U . . .
H21C H 0.281750 0.673534 0.649163 0.066 Uiso 1 1 calc R U . . .
C22 C 0.66354(15) 0.66509(9) 0.37871(12) 0.0294(3) Uani 1 1 d . . . . .
C23 C 0.74965(16) 0.67019(9) 0.46572(13) 0.0330(4) Uani 1 1 d . . . . .
C24 C 0.86267(17) 0.65977(11) 0.46383(15) 0.0435(5) Uani 1 1 d . . . . .
H24 H 0.924611 0.662655 0.520945 0.052 Uiso 1 1 calc R U . . .
C25 C 0.8861(2) 0.64518(13) 0.37942(17) 0.0519(6) Uani 1 1 d . . . . .
H25 H 0.964044 0.639011 0.379422 0.062 Uiso 1 1 calc R U . . .
C26 C 0.7976(2) 0.63949(13) 0.29522(16) 0.0492(5) Uani 1 1 d . . . . .
H26 H 0.815628 0.628560 0.238562 0.059 Uiso 1 1 calc R U . . .
C27 C 0.68235(17) 0.64959(10) 0.29238(13) 0.0370(4) Uani 1 1 d . . . . .
C28 C 0.72146(16) 0.68409(10) 0.55764(12) 0.0355(4) Uani 1 1 d . . . . .
H28 H 0.643653 0.706718 0.541306 0.043 Uiso 1 1 calc R U . . .
C29 C 0.7141(2) 0.61650(11) 0.60905(16) 0.0473(5) Uani 1 1 d . . . . .
H29A H 0.657155 0.585885 0.566803 0.071 Uiso 1 1 calc R U . . .
H29B H 0.690415 0.626338 0.665620 0.071 Uiso 1 1 calc R U . . .
H29C H 0.790120 0.593934 0.627681 0.071 Uiso 1 1 calc R U . . .
C30 C 0.8083(2) 0.73254(12) 0.62363(15) 0.0486(5) Uani 1 1 d . . . . .
H30A H 0.813141 0.775669 0.590245 0.073 Uiso 1 1 calc R U . . .
H30B H 0.884601 0.710399 0.643739 0.073 Uiso 1 1 calc R U . . .
H30C H 0.782914 0.742676 0.679323 0.073 Uiso 1 1 calc R U . . .
C31 C 0.58532(18) 0.64506(11) 0.19955(13) 0.0404(4) Uani 1 1 d . . . . .
H31 H 0.510501 0.654082 0.213383 0.048 Uiso 1 1 calc R U . . .
C32 C 0.5997(2) 0.69974(11) 0.13016(14) 0.0437(5) Uani 1 1 d . . . . .
H32A H 0.605075 0.745464 0.159700 0.066 Uiso 1 1 calc R U . . .
H32B H 0.532715 0.698538 0.073240 0.066 Uiso 1 1 calc R U . . .
H32C H 0.670431 0.690491 0.112781 0.066 Uiso 1 1 calc R U . . .
C33 C 0.5782(3) 0.57322(12) 0.15504(17) 0.0602(7) Uani 1 1 d . . . . .
H33A H 0.651529 0.562624 0.142419 0.090 Uiso 1 1 calc R U . . .
H33B H 0.515020 0.572261 0.095506 0.090 Uiso 1 1 calc R U . . .
H33C H 0.563526 0.538730 0.198653 0.090 Uiso 1 1 calc R U . . .


_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 Cl1 2.2012(5) . ?
V1 Cl2 2.2104(5) . ?
V1 Cl3 2.2026(5) . ?
V1 C3 1.7042(17) . ?
N1 N2 1.325(2) . ?
N1 C1 1.372(2) . ?
N1 C10 1.453(2) . ?
N2 N3 1.322(2) . ?
N3 C2 1.376(2) . ?
N3 C22 1.448(2) . ?
C1 C2 1.401(2) . ?
C1 C4 1.465(2) . ?
C2 C3 1.423(2) . ?
C4 C5 1.399(2) . ?
C4 C9 1.396(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.384(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.390(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.402(2) . ?
C10 C15 1.393(2) . ?
C11 C12 1.394(3) . ?
C11 C16 1.515(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.398(3) . ?
C15 C19 1.520(3) . ?
C16 H16 1.0000 . ?
C16 C17 1.530(3) . ?
C16 C18 1.535(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 1.0000 . ?
C19 C20 1.531(3) . ?
C19 C21 1.526(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.398(2) . ?
C22 C27 1.394(2) . ?
C23 C24 1.390(3) . ?
C23 C28 1.520(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.388(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.385(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.395(3) . ?
C27 C31 1.521(3) . ?
C28 H28 1.0000 . ?
C28 C29 1.528(3) . ?
C28 C30 1.525(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 1.0000 . ?
C31 C32 1.519(3) . ?
C31 C33 1.529(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

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
Cl1 V1 Cl2 110.52(2) . . ?
Cl1 V1 Cl3 112.60(3) . . ?
Cl3 V1 Cl2 113.39(2) . . ?
C3 V1 Cl1 105.21(6) . . ?
C3 V1 Cl2 106.94(6) . . ?
C3 V1 Cl3 107.65(6) . . ?
N2 N1 C1 113.36(14) . . ?
N2 N1 C10 116.71(13) . . ?
C1 N1 C10 129.91(14) . . ?
N3 N2 N1 104.12(12) . . ?
N2 N3 C2 113.61(13) . . ?
N2 N3 C22 120.14(13) . . ?
C2 N3 C22 126.08(14) . . ?
N1 C1 C2 104.69(14) . . ?
N1 C1 C4 126.23(15) . . ?
C2 C1 C4 129.03(14) . . ?
N3 C2 C1 104.21(14) . . ?
N3 C2 C3 122.23(15) . . ?
C1 C2 C3 133.56(15) . . ?
C2 C3 V1 177.04(14) . . ?
C5 C4 C1 123.40(15) . . ?
C9 C4 C1 117.64(15) . . ?
C9 C4 C5 118.96(15) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.48(16) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.21(17) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.84(16) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.44(16) . . ?
C9 C8 H8 119.8 . . ?
C4 C9 H9 120.0 . . ?
C8 C9 C4 120.07(16) . . ?
C8 C9 H9 120.0 . . ?
C11 C10 N1 117.49(15) . . ?
C15 C10 N1 117.70(15) . . ?
C15 C10 C11 124.77(16) . . ?
C10 C11 C16 122.10(16) . . ?
C12 C11 C10 116.39(16) . . ?
C12 C11 C16 121.48(16) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.73(17) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 120.99(17) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.5 . . ?
C13 C14 C15 121.00(17) . . ?
C15 C14 H14 119.5 . . ?
C10 C15 C14 116.09(16) . . ?
C10 C15 C19 122.35(16) . . ?
C14 C15 C19 121.56(16) . . ?
C11 C16 H16 107.8 . . ?
C11 C16 C17 109.75(16) . . ?
C11 C16 C18 112.96(17) . . ?
C17 C16 H16 107.8 . . ?
C17 C16 C18 110.68(16) . . ?
C18 C16 H16 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19 107.9 . . ?
C15 C19 C20 111.76(16) . . ?
C15 C19 C21 111.05(16) . . ?
C20 C19 H19 107.9 . . ?
C21 C19 H19 107.9 . . ?
C21 C19 C20 110.26(17) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N3 116.71(15) . . ?
C27 C22 N3 117.91(15) . . ?
C27 C22 C23 125.37(17) . . ?
C22 C23 C28 122.16(16) . . ?
C24 C23 C22 116.08(17) . . ?
C24 C23 C28 121.73(17) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.75(19) . . ?
C25 C24 H24 119.6 . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 121.0(2) . . ?
C26 C25 H25 119.5 . . ?
C25 C26 H26 119.5 . . ?
C25 C26 C27 120.97(19) . . ?
C27 C26 H26 119.5 . . ?
C22 C27 C26 115.78(18) . . ?
C22 C27 C31 123.19(17) . . ?
C26 C27 C31 121.02(17) . . ?
C23 C28 H28 107.8 . . ?
C23 C28 C29 110.79(15) . . ?
C23 C28 C30 112.76(17) . . ?
C29 C28 H28 107.8 . . ?
C30 C28 H28 107.8 . . ?
C30 C28 C29 109.74(17) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 H31 107.9 . . ?
C27 C31 C33 111.76(18) . . ?
C32 C31 C27 110.96(17) . . ?
C32 C31 H31 107.9 . . ?
C32 C31 C33 110.19(17) . . ?
C33 C31 H31 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

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
N1 N2 N3 C2 -0.37(16) . . . . ?
N1 N2 N3 C22 175.16(13) . . . . ?
N1 C1 C2 N3 -0.89(16) . . . . ?
N1 C1 C2 C3 178.29(17) . . . . ?
N1 C1 C4 C5 -31.5(2) . . . . ?
N1 C1 C4 C9 148.46(16) . . . . ?
N1 C10 C11 C12 179.36(15) . . . . ?
N1 C10 C11 C16 1.5(2) . . . . ?
N1 C10 C15 C14 -179.53(15) . . . . ?
N1 C10 C15 C19 0.6(2) . . . . ?
N2 N1 C1 C2 0.76(17) . . . . ?
N2 N1 C1 C4 -176.83(14) . . . . ?
N2 N1 C10 C11 -90.13(18) . . . . ?
N2 N1 C10 C15 87.56(18) . . . . ?
N2 N3 C2 C1 0.82(17) . . . . ?
N2 N3 C2 C3 -178.47(14) . . . . ?
N2 N3 C22 C23 -93.45(19) . . . . ?
N2 N3 C22 C27 87.87(19) . . . . ?
N3 C22 C23 C24 -177.53(16) . . . . ?
N3 C22 C23 C28 4.3(3) . . . . ?
N3 C22 C27 C26 177.69(18) . . . . ?
N3 C22 C27 C31 -1.1(3) . . . . ?
C1 N1 N2 N3 -0.26(17) . . . . ?
C1 N1 C10 C11 91.6(2) . . . . ?
C1 N1 C10 C15 -90.8(2) . . . . ?
C1 C4 C5 C6 179.41(15) . . . . ?
C1 C4 C9 C8 -179.22(15) . . . . ?
C2 N3 C22 C23 81.5(2) . . . . ?
C2 N3 C22 C27 -97.2(2) . . . . ?
C2 C1 C4 C5 151.48(17) . . . . ?
C2 C1 C4 C9 -28.5(2) . . . . ?
C4 C1 C2 N3 176.60(15) . . . . ?
C4 C1 C2 C3 -4.2(3) . . . . ?
C4 C5 C6 C7 0.4(3) . . . . ?
C5 C4 C9 C8 0.8(2) . . . . ?
C5 C6 C7 C8 -0.3(3) . . . . ?
C6 C7 C8 C9 0.5(3) . . . . ?
C7 C8 C9 C4 -0.7(3) . . . . ?
C9 C4 C5 C6 -0.6(2) . . . . ?
C10 N1 N2 N3 -178.85(13) . . . . ?
C10 N1 C1 C2 179.11(15) . . . . ?
C10 N1 C1 C4 1.5(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C10 C11 C16 C17 103.66(19) . . . . ?
C10 C11 C16 C18 -132.31(18) . . . . ?
C10 C15 C19 C20 -139.58(19) . . . . ?
C10 C15 C19 C21 96.8(2) . . . . ?
C11 C10 C15 C14 -2.0(3) . . . . ?
C11 C10 C15 C19 178.06(16) . . . . ?
C11 C12 C13 C14 -0.9(3) . . . . ?
C12 C11 C16 C17 -74.1(2) . . . . ?
C12 C11 C16 C18 49.9(2) . . . . ?
C12 C13 C14 C15 0.7(3) . . . . ?
C13 C14 C15 C10 0.7(3) . . . . ?
C13 C14 C15 C19 -179.40(17) . . . . ?
C14 C15 C19 C20 40.5(2) . . . . ?
C14 C15 C19 C21 -83.1(2) . . . . ?
C15 C10 C11 C12 1.9(3) . . . . ?
C15 C10 C11 C16 -176.03(16) . . . . ?
C16 C11 C12 C13 177.56(17) . . . . ?
C22 N3 C2 C1 -174.40(14) . . . . ?
C22 N3 C2 C3 6.3(2) . . . . ?
C22 C23 C24 C25 0.0(3) . . . . ?
C22 C23 C28 C29 95.2(2) . . . . ?
C22 C23 C28 C30 -141.38(18) . . . . ?
C22 C27 C31 C32 117.0(2) . . . . ?
C22 C27 C31 C33 -119.5(2) . . . . ?
C23 C22 C27 C26 -0.9(3) . . . . ?
C23 C22 C27 C31 -179.67(18) . . . . ?
C23 C24 C25 C26 -1.1(4) . . . . ?
C24 C23 C28 C29 -82.9(2) . . . . ?
C24 C23 C28 C30 40.5(3) . . . . ?
C24 C25 C26 C27 1.3(4) . . . . ?
C25 C26 C27 C22 -0.3(3) . . . . ?
C25 C26 C27 C31 178.5(2) . . . . ?
C26 C27 C31 C32 -61.7(3) . . . . ?
C26 C27 C31 C33 61.7(3) . . . . ?
C27 C22 C23 C24 1.0(3) . . . . ?
C27 C22 C23 C28 -177.13(18) . . . . ?
C28 C23 C24 C25 178.1(2) . . . . ?

_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.810
####################################################################### 
# 
# 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_bk212
_database_code_depnum_ccdc_archive 'CCDC 2142648'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2022-01-17 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_audit_creation_date             2022-01-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H66 Cl3 N3 P V, 1[C4H8O]'
_chemical_formula_sum            'C45 H66 Cl3 N3 P V'
_chemical_formula_weight         837.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C49 H74 Cl3 N3 OP V'
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'
P P 0.2955 0.4335 '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                   11.3015(6)
_cell_length_b                   11.6166(3)
_cell_length_c                   20.8002(9)
_cell_angle_alpha                84.755(3)
_cell_angle_beta                 81.999(5)
_cell_angle_gamma                67.677(4)
_cell_volume                     2499.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9104
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      69.2520
_cell_measurement_theta_min      4.0910
_shelx_estimated_absorpt_T_max   0.930
_shelx_estimated_absorpt_T_min   0.487
_exptl_absorpt_coefficient_mu    3.658
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             892
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0078
0 0 1 0.0078
0 1 0 0.0773
0 -1 0 0.0773
-1 0 0 0.1147
1 0 0 0.1147
-1 -1 -1 0.0396
1 1 1 0.0453

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
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
-0.0009 -0.0001 -1.0001 -0.0031 -0.0726 0.0180
0.0009 0.0001 1.0001 0.0031 0.0726 -0.0180
0.0011 1.0001 -0.0001 -0.0744 0.0266 0.1197
-0.0011 -1.0001 0.0001 0.0744 -0.0266 -0.1197
-1.0000 -0.0001 0.0013 0.0884 0.0411 0.1118
1.0000 0.0001 -0.0013 -0.0884 -0.0411 -0.1118
-1.0019 -1.0003 -0.9988 0.1597 -0.0581 0.0101
1.0019 1.0003 0.9988 -0.1597 0.0581 -0.0101

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30255
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         4.118
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  59.00   0.50    4.00    --   59.56-107.00  39.00   68
  2  ω    -58.00 -22.00   0.50    4.00    --  -62.07 107.00 136.00   72
  3  ω    -84.00 -59.00   0.50    4.00    --  -71.26 107.00 136.00   50
  4  ω     52.00  93.00   0.50    4.00    --   73.45-107.00  39.00   82
  5  ω    -57.00 -32.00   0.50    4.00    --  -75.95 107.00 136.00   50
  6  ω    -95.00 -62.00   0.50    4.00    --  -75.95 107.00 136.00   66
  7  ω     69.00  96.00   0.50    4.00    --   81.22-107.00  39.00   54
  8  ω     11.00  37.00   0.50    4.00    --   59.56 -30.00  30.00   52
  9  ω     10.00  37.00   0.50    4.00    --   59.56 -30.00  90.00   54
 10  ω     10.00  35.00   0.50    4.00    --   59.56 -30.00-120.00   50
 11  ω     10.00  36.00   0.50    4.00    --   59.56 -30.00-150.00   52
 12  ω     10.00  36.00   0.50    4.00    --   59.56 -30.00-180.00   52
 13  ω     22.00  48.00   0.50    4.00    --   59.56 -95.00 -90.00   52
 14  ω   -111.00 -86.00   0.50    4.00    --  -62.07 -30.00-150.00   50
 15  ω   -100.00 -66.00   0.50    4.00    --  -62.07 -30.00  60.00   68
 16  ω   -111.00 -84.00   0.50    4.00    --  -71.26 -30.00 -60.00   54
 17  ω   -109.00 -75.00   0.50    4.00    --  -71.26 -30.00   0.00   68
 18  ω   -116.00 -72.00   0.50    4.00    --  -71.26 -30.00 120.00   88
 19  ω     35.00  74.00   0.50    4.00    --   71.88 -95.00 -90.00   78
 20  ω     34.00  70.00   0.50    4.00    --   71.88 -95.00  90.00   72
 21  ω     36.00  61.00   0.50    4.00    --   71.88-107.00  39.00   50
 22  ω     75.00 122.00   0.50    4.00    --   73.45  30.00  30.00   94
 23  ω     75.00 123.00   0.50    4.00    --   73.45  30.00 -30.00   96
 24  ω     35.00  83.00   0.50    4.00    --   73.45 -95.00 -30.00   96
 25  ω     28.00 104.00   0.50    4.00    --   73.45-125.00-180.00  152
 26  ω   -121.00 -77.00   0.50    4.00    --  -75.95-125.00  30.00   88
 27  ω   -107.00 -32.00   0.50    4.00    --  -75.95 125.00-180.00  150
 28  ω   -125.00-100.00   0.50    4.00    --  -75.95 -30.00  90.00   50
 29  ω   -122.00 -74.00   0.50    4.00    --  -75.95-125.00 120.00   96
 30  ω   -120.00 -74.00   0.50    4.00    --  -75.95-125.00 150.00   92
 31  ω   -125.00 -99.00   0.50    4.00    --  -75.95 -30.00-180.00   52
 32  ω     86.00 112.00   0.50    4.00    --   81.22-125.00 -90.00   52
 33  ω     90.00 131.00   0.50    4.00    --   81.22  30.00   0.00   82
 34  ω     86.00 112.00   0.50    4.00    --   81.22-125.00   0.00   52
 35  ω     38.00  64.00   0.50    4.00    --   81.22-125.00   0.00   52
 36  ω     87.00 128.00   0.50    4.00    --   81.22  30.00 -60.00   82
 37  ω     41.00  78.00   0.50    4.00    --   81.22 -95.00-150.00   74
 38  ω     91.00 122.00   0.50    4.00    --   81.22 125.00 -30.00   62
 39  ω     44.00 110.00   0.50    4.00    --   81.22-125.00  90.00  132
 40  ω     41.00  79.00   0.50    4.00    --   81.22 -95.00 -60.00   76
 41  ω     51.00 112.00   0.50    4.00    --   81.22-125.00 150.00  122
 42  ω     82.00 130.00   0.50    4.00    --   81.22  30.00  60.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0883858000
_diffrn_orient_matrix_UB_12      -0.0743124000
_diffrn_orient_matrix_UB_13      0.0032232000
_diffrn_orient_matrix_UB_21      -0.0410337000
_diffrn_orient_matrix_UB_22      0.0266669000
_diffrn_orient_matrix_UB_23      0.0726078000
_diffrn_orient_matrix_UB_31      -0.1118101000
_diffrn_orient_matrix_UB_32      0.1198149000
_diffrn_orient_matrix_UB_33      -0.0179333000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5416
_reflns_number_total             8894
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8894
_refine_ls_number_restraints     1141
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0931
_refine_ls_restrained_S_all      1.064
_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)+(0.1613P)²+2.0650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2637
_refine_ls_wR_factor_ref         0.2894
_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
 C45B-C44B
 1.52 with sigma of 0.02
 C35A-C34A = C35B-C34B = C36A-C35A = C35B-C36B = C36A-C37A = C37B-C36B
 1.52 with sigma of 0.02
 C38A-C39A = C38B-C39B = C40A-C39A = C39B-C40B = C40A-C41A = C40B-C41B
 1.52 with sigma of 0.02
 C42A-C43A = C42B-C43B = C44A-C43A = C44B-C43B = C45A-C44A
 1.52 with sigma of 0.02
 V1B-Cl2B = V1B-Cl1B = V1B-Cl3B
 2.3 with sigma of 0.02
 C34A-C36A = C35A-C37A
 2.5 with sigma of 0.04
 C38B-C40B = C39B-C41B
 2.5 with sigma of 0.04
 C38A-C40A = C39A-C41A
 2.5 with sigma of 0.04
 C34B-C36B = C35B-C37B
 2.5 with sigma of 0.04
 C42A-C44A = C43A-C45A
 2.5 with sigma of 0.04
 C42B-C44B = C45B-C43B
 2.5 with sigma of 0.04
 V1A-Cl3A \\sim V1A-Cl2A \\sim V1A-Cl1A
 with sigma of 0.02
 P1-C42A \\sim P1-C42B \\sim P1-C34A \\sim P1-C34B \\sim P1-C38A \\sim P1-C38B
 with sigma of 0.02
 V1A-P1 \\sim V1B-P1
 with sigma of 0.02
 V1A-C3 \\sim V1B-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(V1B)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(C34B)=Sof(H34C)=Sof(H34D)=
 Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=
 Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41D)=
 Sof(H41E)=Sof(H41F)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=
 Sof(H43D)=Sof(C44B)=Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=1-FVAR(1)
 Sof(V1A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=
 Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=
 Sof(H43B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(C45A)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C34A(H34A,H34B), C34B(H34C,H34D), C35A(H35A,H35B), C35B(H35C,H35D), C36A(H36A,
 H36B), C36B(H36C,H36D), C38A(H38A,H38B), C38B(H38C,H38D), C39A(H39A,H39B),
 C39B(H39C,H39D), C40A(H40A,H40B), C40B(H40C,H40D), C42A(H42A,H42B), C42B(H42C,
 H42D), C43A(H43A,H43B), C43B(H43C,H43D), C44A(H44A,H44B), C44B(H44C,H44D)
6.c Me refined with riding coordinates:
 C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F), C41A(H41A,H41B,H41C), C41B(H41D,
 H41E,H41F), C45A(H45A,H45B,H45C), C45B(H45D,H45E,H45F)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C24(H24), C25(H25), C26(H26)
6.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
V1A V 0.48912(16) 0.14681(17) 0.72931(9) 0.0502(5) Uani 0.857(3) 1 d D U P A 1
V1B V 0.5153(11) 0.1581(10) 0.7132(6) 0.0558(19) Uani 0.143(3) 1 d D U P A 2
Cl1A Cl 0.3779(2) 0.04871(18) 0.79717(11) 0.0793(6) Uani 0.857(3) 1 d D . P A 1
Cl1B Cl 0.608(2) 0.203(2) 0.6116(9) 0.149(8) Uani 0.143(3) 1 d D . P A 2
Cl2A Cl 0.54637(16) 0.00269(13) 0.65169(10) 0.0634(5) Uani 0.857(3) 1 d D U P A
1
Cl2B Cl 0.6907(11) 0.1281(12) 0.7598(8) 0.088(3) Uani 0.143(3) 1 d D U P A 2
Cl3A Cl 0.68255(14) 0.17647(13) 0.70569(10) 0.0557(5) Uani 0.857(3) 1 d D U P A
1
Cl3B Cl 0.4914(15) -0.0243(11) 0.7102(10) 0.102(4) Uani 0.143(3) 1 d D U P A 2
P1 P 0.4865(2) 0.24721(17) 0.83169(10) 0.0780(5) Uani 1 1 d D U . . .
N1 N 0.1797(4) 0.3651(3) 0.6485(2) 0.0491(9) Uani 1 1 d . U . . .
N2 N 0.0942(4) 0.4700(3) 0.6259(2) 0.0490(9) Uani 1 1 d . U . . .
N3 N 0.1386(4) 0.5566(3) 0.6378(2) 0.0456(9) Uani 1 1 d . U . . .
C1 C 0.2770(5) 0.3812(4) 0.6739(3) 0.0511(10) Uani 1 1 d . U . . .
C2 C 0.2518(5) 0.5092(4) 0.6656(3) 0.0482(10) Uani 1 1 d . U . . .
C3 C 0.3775(5) 0.2807(4) 0.7013(3) 0.0537(11) Uani 1 1 d D U . . .
C4 C 0.3296(5) 0.5792(4) 0.6769(3) 0.0513(11) Uani 1 1 d . U . . .
C5 C 0.4638(5) 0.5179(5) 0.6685(3) 0.0573(12) Uani 1 1 d . U . . .
H5 H 0.500849 0.432591 0.658026 0.069 Uiso 1 1 calc R U . . .
C6 C 0.5421(6) 0.5822(5) 0.6754(3) 0.0661(13) Uani 1 1 d . U . . .
H6 H 0.632972 0.540896 0.669181 0.079 Uiso 1 1 calc R U . . .
C7 C 0.4897(6) 0.7048(5) 0.6913(4) 0.0668(13) Uani 1 1 d . U . . .
H7 H 0.544419 0.748309 0.695098 0.080 Uiso 1 1 calc R U . . .
C8 C 0.3593(6) 0.7647(5) 0.7015(3) 0.0640(13) Uani 1 1 d . U . . .
H8 H 0.324081 0.848900 0.713797 0.077 Uiso 1 1 calc R U . . .
C9 C 0.2778(5) 0.7042(5) 0.6943(3) 0.0590(12) Uani 1 1 d . U . . .
H9 H 0.187151 0.746998 0.701003 0.071 Uiso 1 1 calc R U . . .
C10 C 0.1738(5) 0.2461(4) 0.6337(3) 0.0517(10) Uani 1 1 d . U . . .
C11 C 0.2386(5) 0.1972(4) 0.5748(3) 0.0529(11) Uani 1 1 d . U . . .
C12 C 0.2366(5) 0.0811(5) 0.5625(3) 0.0595(12) Uani 1 1 d . U . . .
H12 H 0.281111 0.041181 0.523595 0.071 Uiso 1 1 calc R U . . .
C13 C 0.1706(6) 0.0247(5) 0.6066(3) 0.0627(13) Uani 1 1 d . U . . .
H13 H 0.170485 -0.053746 0.597153 0.075 Uiso 1 1 calc R U . . .
C14 C 0.1057(6) 0.0773(5) 0.6631(3) 0.0640(13) Uani 1 1 d . U . . .
H14 H 0.059667 0.036055 0.691602 0.077 Uiso 1 1 calc R U . . .
C15 C 0.1054(6) 0.1930(5) 0.6802(3) 0.0589(11) Uani 1 1 d . U . . .
C16 C 0.3033(5) 0.2626(4) 0.5243(3) 0.0530(11) Uani 1 1 d . U . . .
H16 H 0.313039 0.331404 0.546030 0.064 Uiso 1 1 calc R U . . .
C17 C 0.2190(6) 0.3216(6) 0.4705(4) 0.0736(17) Uani 1 1 d . U . . .
H17A H 0.209833 0.256239 0.447328 0.110 Uiso 1 1 calc R U . . .
H17B H 0.258609 0.369831 0.440179 0.110 Uiso 1 1 calc R U . . .
H17C H 0.133927 0.376856 0.489237 0.110 Uiso 1 1 calc R U . . .
C18 C 0.4368(6) 0.1792(6) 0.4958(4) 0.0693(16) Uani 1 1 d . U . . .
H18A H 0.490948 0.142099 0.530955 0.104 Uiso 1 1 calc R U . . .
H18B H 0.475443 0.228786 0.465855 0.104 Uiso 1 1 calc R U . . .
H18C H 0.430102 0.113002 0.472301 0.104 Uiso 1 1 calc R U . . .
C19 C 0.0333(6) 0.2564(6) 0.7405(3) 0.0667(13) Uani 1 1 d . U . . .
H19 H 0.082250 0.304344 0.753855 0.080 Uiso 1 1 calc R U . . .
C20 C -0.0996(7) 0.3494(6) 0.7290(4) 0.0787(18) Uani 1 1 d . U . . .
H20A H -0.151734 0.305217 0.717464 0.118 Uiso 1 1 calc R U . . .
H20B H -0.091904 0.408595 0.693527 0.118 Uiso 1 1 calc R U . . .
H20C H -0.141040 0.394546 0.768712 0.118 Uiso 1 1 calc R U . . .
C21 C 0.0216(8) 0.1647(7) 0.7985(4) 0.091(2) Uani 1 1 d . U . . .
H21A H -0.008070 0.210050 0.838782 0.137 Uiso 1 1 calc R U . . .
H21B H 0.105880 0.098257 0.802209 0.137 Uiso 1 1 calc R U . . .
H21C H -0.040299 0.128383 0.790895 0.137 Uiso 1 1 calc R U . . .
C22 C 0.0635(5) 0.6843(4) 0.6178(3) 0.0469(10) Uani 1 1 d . U . . .
C23 C -0.0350(5) 0.7549(4) 0.6630(3) 0.0516(10) Uani 1 1 d . U . . .
C24 C -0.1090(5) 0.8757(5) 0.6418(3) 0.0570(12) Uani 1 1 d . U . . .
H24 H -0.177048 0.927753 0.670677 0.068 Uiso 1 1 calc R U . . .
C25 C -0.0851(5) 0.9195(5) 0.5807(3) 0.0615(13) Uani 1 1 d . U . . .
H25 H -0.135959 1.002185 0.567792 0.074 Uiso 1 1 calc R U . . .
C26 C 0.0108(5) 0.8470(4) 0.5372(3) 0.0582(12) Uani 1 1 d . U . . .
H26 H 0.023468 0.879592 0.494382 0.070 Uiso 1 1 calc R U . . .
C27 C 0.0904(5) 0.7261(4) 0.5547(3) 0.0519(10) Uani 1 1 d . U . . .
C28 C -0.0665(5) 0.7089(6) 0.7304(3) 0.0633(13) Uani 1 1 d . U . . .
H28 H 0.001180 0.625271 0.738677 0.076 Uiso 1 1 calc R U . . .
C29 C -0.1951(6) 0.6950(7) 0.7374(4) 0.0776(18) Uani 1 1 d . U . . .
H29A H -0.213066 0.663523 0.781481 0.116 Uiso 1 1 calc R U . . .
H29B H -0.193209 0.636360 0.705886 0.116 Uiso 1 1 calc R U . . .
H29C H -0.262645 0.776224 0.729235 0.116 Uiso 1 1 calc R U . . .
C30 C -0.0689(8) 0.7967(8) 0.7824(4) 0.096(2) Uani 1 1 d . U . . .
H30A H -0.130284 0.880785 0.773152 0.145 Uiso 1 1 calc R U . . .
H30B H 0.017162 0.798705 0.781632 0.145 Uiso 1 1 calc R U . . .
H30C H -0.095202 0.766301 0.825376 0.145 Uiso 1 1 calc R U . . .
C31 C 0.1973(6) 0.6491(5) 0.5067(3) 0.0606(13) Uani 1 1 d . U . . .
H31 H 0.225497 0.560242 0.523224 0.073 Uiso 1 1 calc R U . . .
C32 C 0.3123(6) 0.6897(7) 0.5028(4) 0.0783(18) Uani 1 1 d . U . . .
H32A H 0.384031 0.635395 0.473965 0.117 Uiso 1 1 calc R U . . .
H32B H 0.338710 0.683712 0.546275 0.117 Uiso 1 1 calc R U . . .
H32C H 0.287573 0.776003 0.485602 0.117 Uiso 1 1 calc R U . . .
C33 C 0.1545(7) 0.6563(6) 0.4393(3) 0.0719(16) Uani 1 1 d . U . . .
H33A H 0.129681 0.742094 0.421337 0.108 Uiso 1 1 calc R U . . .
H33B H 0.080770 0.630340 0.442837 0.108 Uiso 1 1 calc R U . . .
H33C H 0.225673 0.601047 0.410543 0.108 Uiso 1 1 calc R U . . .
C34A C 0.3433(8) 0.2875(9) 0.8873(4) 0.0892(17) Uani 0.857(3) 1 d D U P A 1
H34A H 0.328507 0.210182 0.902224 0.107 Uiso 0.857(3) 1 calc R U P A 1
H34B H 0.357736 0.322694 0.925734 0.107 Uiso 0.857(3) 1 calc R U P A 1
C34B C 0.349(3) 0.365(4) 0.809(2) 0.090(2) Uani 0.143(3) 1 d D U P A 2
H34C H 0.381999 0.412873 0.774068 0.107 Uiso 0.143(3) 1 calc R U P A 2
H34D H 0.307523 0.321303 0.786381 0.107 Uiso 0.143(3) 1 calc R U P A 2
C35A C 0.2237(9) 0.3783(10) 0.8617(5) 0.1012(18) Uani 0.857(3) 1 d D U P A 1
H35A H 0.212628 0.349484 0.820383 0.121 Uiso 0.857(3) 1 calc R U P A 1
H35B H 0.231107 0.460651 0.852895 0.121 Uiso 0.857(3) 1 calc R U P A 1
C35B C 0.237(4) 0.464(5) 0.844(3) 0.098(3) Uani 0.143(3) 1 d D U P A 2
H35C H 0.264442 0.472664 0.885590 0.118 Uiso 0.143(3) 1 calc R U P A 2
H35D H 0.225724 0.543036 0.818226 0.118 Uiso 0.143(3) 1 calc R U P A 2
C36A C 0.1062(9) 0.3900(11) 0.9118(5) 0.112(2) Uani 0.857(3) 1 d D U P A 1
H36A H 0.098009 0.307850 0.919143 0.134 Uiso 0.857(3) 1 calc R U P A 1
H36B H 0.120405 0.414378 0.953609 0.134 Uiso 0.857(3) 1 calc R U P A 1
C36B C 0.105(4) 0.461(6) 0.860(3) 0.106(3) Uani 0.143(3) 1 d D U P A 2
H36C H 0.111084 0.372910 0.864764 0.127 Uiso 0.143(3) 1 calc R U P A 2
H36D H 0.052594 0.501450 0.823646 0.127 Uiso 0.143(3) 1 calc R U P A 2
C37A C -0.0136(10) 0.4815(11) 0.8911(6) 0.113(3) Uani 0.857(3) 1 d D U P A 1
H37A H -0.085099 0.485413 0.924532 0.169 Uiso 0.857(3) 1 calc R U P A 1
H37B H -0.006780 0.563486 0.884688 0.169 Uiso 0.857(3) 1 calc R U P A 1
H37C H -0.029180 0.456937 0.850215 0.169 Uiso 0.857(3) 1 calc R U P A 1
C37B C 0.040(5) 0.527(6) 0.922(3) 0.109(5) Uani 0.143(3) 1 d D U P A 2
H37D H -0.045786 0.524286 0.932252 0.164 Uiso 0.143(3) 1 calc R U P A 2
H37E H 0.091993 0.485627 0.957695 0.164 Uiso 0.143(3) 1 calc R U P A 2
H37F H 0.033629 0.613890 0.916666 0.164 Uiso 0.143(3) 1 calc R U P A 2
C38A C 0.5155(10) 0.3916(8) 0.8211(5) 0.0845(16) Uani 0.857(3) 1 d D U P A 1
H38A H 0.592658 0.377766 0.789196 0.101 Uiso 0.857(3) 1 calc R U P A 1
H38B H 0.441828 0.454921 0.801234 0.101 Uiso 0.857(3) 1 calc R U P A 1
C38B C 0.557(6) 0.360(5) 0.832(2) 0.087(2) Uani 0.143(3) 1 d D U P A 2
H38C H 0.649914 0.321376 0.817439 0.105 Uiso 0.143(3) 1 calc R U P A 2
H38D H 0.518285 0.428539 0.800304 0.105 Uiso 0.143(3) 1 calc R U P A 2
C39A C 0.5349(12) 0.4474(10) 0.8795(5) 0.0944(18) Uani 0.857(3) 1 d D U P A 1
H39A H 0.605939 0.384217 0.901238 0.113 Uiso 0.857(3) 1 calc R U P A 1
H39B H 0.455766 0.468131 0.910664 0.113 Uiso 0.857(3) 1 calc R U P A 1
C39B C 0.541(6) 0.416(6) 0.897(3) 0.093(2) Uani 0.143(3) 1 d D U P A 2
H39C H 0.561442 0.350126 0.932269 0.111 Uiso 0.143(3) 1 calc R U P A 2
H39D H 0.451657 0.475514 0.907762 0.111 Uiso 0.143(3) 1 calc R U P A 2
C40A C 0.5661(11) 0.5648(9) 0.8635(5) 0.1012(19) Uani 0.857(3) 1 d D U P A 1
H40A H 0.497581 0.625837 0.839363 0.121 Uiso 0.857(3) 1 calc R U P A 1
H40B H 0.647863 0.542727 0.834353 0.121 Uiso 0.857(3) 1 calc R U P A 1
C40B C 0.635(6) 0.484(6) 0.891(2) 0.096(2) Uani 0.143(3) 1 d D U P A 2
H40C H 0.722413 0.426380 0.874213 0.116 Uiso 0.143(3) 1 calc R U P A 2
H40D H 0.607971 0.555653 0.859591 0.116 Uiso 0.143(3) 1 calc R U P A 2
C41A C 0.5785(12) 0.6273(11) 0.9226(6) 0.122(3) Uani 0.857(3) 1 d D U P A 1
H41A H 0.598463 0.701256 0.908026 0.183 Uiso 0.857(3) 1 calc R U P A 1
H41B H 0.497275 0.651991 0.951269 0.183 Uiso 0.857(3) 1 calc R U P A 1
H41C H 0.647851 0.568717 0.946249 0.183 Uiso 0.857(3) 1 calc R U P A 1
C41B C 0.640(6) 0.529(6) 0.957(2) 0.103(5) Uani 0.143(3) 1 d D U P A 2
H41D H 0.700526 0.571576 0.951993 0.154 Uiso 0.143(3) 1 calc R U P A 2
H41E H 0.553964 0.586075 0.972799 0.154 Uiso 0.143(3) 1 calc R U P A 2
H41F H 0.668185 0.457051 0.987394 0.154 Uiso 0.143(3) 1 calc R U P A 2
C42A C 0.6153(11) 0.1515(9) 0.8786(5) 0.1038(19) Uani 0.857(3) 1 d D U P A 1
H42A H 0.696971 0.153889 0.855287 0.125 Uiso 0.857(3) 1 calc R U P A 1
H42B H 0.601740 0.191227 0.920555 0.125 Uiso 0.857(3) 1 calc R U P A 1
C42B C 0.543(4) 0.133(5) 0.896(2) 0.100(2) Uani 0.143(3) 1 d D U P A 2
H42C H 0.526832 0.173002 0.938148 0.120 Uiso 0.143(3) 1 calc R U P A 2
H42D H 0.499969 0.072133 0.900236 0.120 Uiso 0.143(3) 1 calc R U P A 2
C43A C 0.6330(12) 0.0202(9) 0.8929(6) 0.113(2) Uani 0.857(3) 1 d D U P A 1
H43A H 0.653558 -0.022311 0.851392 0.135 Uiso 0.857(3) 1 calc R U P A 1
H43B H 0.550592 0.016244 0.914234 0.135 Uiso 0.857(3) 1 calc R U P A 1
C43B C 0.690(5) 0.067(6) 0.876(2) 0.110(2) Uani 0.143(3) 1 d D U P A 2
H43C H 0.704779 -0.002577 0.848146 0.132 Uiso 0.143(3) 1 calc R U P A 2
H43D H 0.722719 0.127092 0.850351 0.132 Uiso 0.143(3) 1 calc R U P A 2
C44A C 0.7372(12) -0.0502(10) 0.9358(6) 0.121(2) Uani 0.857(3) 1 d D U P A 1
H44A H 0.822693 -0.057453 0.913251 0.145 Uiso 0.857(3) 1 calc R U P A 1
H44B H 0.722553 -0.006421 0.976592 0.145 Uiso 0.857(3) 1 calc R U P A 1
C44B C 0.766(5) 0.017(5) 0.934(3) 0.116(3) Uani 0.143(3) 1 d D U P A 2
H44C H 0.705302 0.024952 0.974199 0.139 Uiso 0.143(3) 1 calc R U P A 2
H44D H 0.817984 0.067289 0.938291 0.139 Uiso 0.143(3) 1 calc R U P A 2
C45A C 0.7310(15) -0.1718(11) 0.9497(7) 0.156(4) Uani 0.857(3) 1 d D U P A 1
H45A H 0.797282 -0.221112 0.977561 0.233 Uiso 0.857(3) 1 calc R U P A 1
H45B H 0.645873 -0.163078 0.971948 0.233 Uiso 0.857(3) 1 calc R U P A 1
H45C H 0.745526 -0.213862 0.908915 0.233 Uiso 0.857(3) 1 calc R U P A 1
C45B C 0.854(7) -0.119(5) 0.927(3) 0.131(5) Uani 0.143(3) 1 d D U P A 2
H45D H 0.901456 -0.148158 0.965005 0.197 Uiso 0.143(3) 1 calc R U P A 2
H45E H 0.802472 -0.168721 0.923552 0.197 Uiso 0.143(3) 1 calc R U P A 2
H45F H 0.915061 -0.126419 0.887674 0.197 Uiso 0.143(3) 1 calc R U P A 2


_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
V1A Cl1A 2.274(2) . ?
V1A Cl2A 2.282(2) . ?
V1A Cl3A 2.320(2) . ?
V1A P1 2.511(3) . ?
V1A C3 1.703(5) . ?
V1B Cl1B 2.330(15) . ?
V1B Cl2B 2.222(14) . ?
V1B Cl3B 2.243(14) . ?
V1B P1 2.691(12) . ?
V1B C3 1.695(12) . ?
Cl2B P1 2.544(14) . ?
P1 C34A 1.783(8) . ?
P1 C34B 1.733(16) . ?
P1 C38A 1.816(7) . ?
P1 C38B 1.776(16) . ?
P1 C42A 1.810(9) . ?
P1 C42B 1.801(16) . ?
N1 N2 1.329(6) . ?
N1 C1 1.364(7) . ?
N1 C10 1.470(6) . ?
N2 N3 1.338(5) . ?
N3 C2 1.373(6) . ?
N3 C22 1.457(6) . ?
C1 C2 1.403(6) . ?
C1 C3 1.424(7) . ?
C2 C4 1.459(7) . ?
C4 C5 1.402(7) . ?
C4 C9 1.404(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.386(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.371(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.364(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.384(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(8) . ?
C10 C15 1.400(8) . ?
C11 C12 1.405(7) . ?
C11 C16 1.509(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.378(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.357(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.421(7) . ?
C15 C19 1.486(9) . ?
C16 H16 1.0000 . ?
C16 C17 1.514(9) . ?
C16 C18 1.521(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 1.0000 . ?
C19 C20 1.516(9) . ?
C19 C21 1.560(9) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.398(8) . ?
C22 C27 1.393(8) . ?
C23 C24 1.400(7) . ?
C23 C28 1.498(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.355(9) . ?
C25 H25 0.9500 . ?
C25 C26 1.369(9) . ?
C26 H26 0.9500 . ?
C26 C27 1.396(7) . ?
C27 C31 1.504(8) . ?
C28 H28 1.0000 . ?
C28 C29 1.509(9) . ?
C28 C30 1.543(10) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 1.0000 . ?
C31 C32 1.532(9) . ?
C31 C33 1.531(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34A H34A 0.9900 . ?
C34A H34B 0.9900 . ?
C34A C35A 1.496(11) . ?
C34B H34C 0.9900 . ?
C34B H34D 0.9900 . ?
C34B C35B 1.50(2) . ?
C35A H35A 0.9900 . ?
C35A H35B 0.9900 . ?
C35A C36A 1.540(12) . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C35B C36B 1.50(2) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C36A C37A 1.460(12) . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
C36B C37B 1.52(2) . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C38A C39A 1.507(10) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
C38B C39B 1.52(2) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C39A C40A 1.531(11) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C39B C40B 1.53(2) . ?
C40A H40A 0.9900 . ?
C40A H40B 0.9900 . ?
C40A C41A 1.532(12) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C40B C41B 1.52(2) . ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?
C41B H41D 0.9800 . ?
C41B H41E 0.9800 . ?
C41B H41F 0.9800 . ?
C42A H42A 0.9900 . ?
C42A H42B 0.9900 . ?
C42A C43A 1.469(12) . ?
C42B H42C 0.9900 . ?
C42B H42D 0.9900 . ?
C42B C43B 1.55(2) . ?
C43A H43A 0.9900 . ?
C43A H43B 0.9900 . ?
C43A C44A 1.509(12) . ?
C43B H43C 0.9900 . ?
C43B H43D 0.9900 . ?
C43B C44B 1.52(2) . ?
C44A H44A 0.9900 . ?
C44A H44B 0.9900 . ?
C44A C45A 1.442(13) . ?
C44B H44C 0.9900 . ?
C44B H44D 0.9900 . ?
C44B C45B 1.52(2) . ?
C45A H45A 0.9800 . ?
C45A H45B 0.9800 . ?
C45A H45C 0.9800 . ?
C45B H45D 0.9800 . ?
C45B H45E 0.9800 . ?
C45B H45F 0.9800 . ?

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
Cl1A V1A Cl2A 93.35(10) . . ?
Cl1A V1A Cl3A 145.24(11) . . ?
Cl1A V1A P1 82.76(9) . . ?
Cl2A V1A Cl3A 92.01(9) . . ?
Cl2A V1A P1 160.54(10) . . ?
Cl3A V1A P1 80.91(9) . . ?
C3 V1A Cl1A 106.4(2) . . ?
C3 V1A Cl2A 108.1(2) . . ?
C3 V1A Cl3A 104.5(2) . . ?
C3 V1A P1 91.3(2) . . ?
Cl1B V1B P1 133.1(8) . . ?
Cl2B V1B Cl1B 92.5(9) . . ?
Cl2B V1B Cl3B 109.4(7) . . ?
Cl2B V1B P1 61.5(5) . . ?
Cl3B V1B Cl1B 108.8(10) . . ?
Cl3B V1B P1 116.3(7) . . ?
C3 V1B Cl1B 89.5(8) . . ?
C3 V1B Cl2B 135.6(7) . . ?
C3 V1B Cl3B 111.8(7) . . ?
C3 V1B P1 85.5(5) . . ?
V1B Cl2B P1 68.4(4) . . ?
Cl2B P1 V1B 50.1(3) . . ?
C34A P1 V1A 117.5(3) . . ?
C34A P1 C38A 102.5(5) . . ?
C34A P1 C42A 105.6(5) . . ?
C34B P1 V1B 86.6(16) . . ?
C34B P1 Cl2B 128.1(16) . . ?
C34B P1 C38B 88(3) . . ?
C34B P1 C42B 142(2) . . ?
C38A P1 V1A 116.1(3) . . ?
C38B P1 V1B 112.7(17) . . ?
C38B P1 Cl2B 85(2) . . ?
C38B P1 C42B 108(3) . . ?
C42A P1 V1A 112.1(4) . . ?
C42A P1 C38A 101.3(5) . . ?
C42B P1 V1B 116(2) . . ?
C42B P1 Cl2B 88.5(17) . . ?
N2 N1 C1 113.9(4) . . ?
N2 N1 C10 118.3(4) . . ?
C1 N1 C10 126.8(4) . . ?
N1 N2 N3 103.2(4) . . ?
N2 N3 C2 113.8(4) . . ?
N2 N3 C22 116.2(4) . . ?
C2 N3 C22 130.1(4) . . ?
N1 C1 C2 105.0(4) . . ?
N1 C1 C3 122.7(4) . . ?
C2 C1 C3 132.3(5) . . ?
N3 C2 C1 104.1(4) . . ?
N3 C2 C4 125.7(4) . . ?
C1 C2 C4 130.0(5) . . ?
C1 C3 V1A 171.6(4) . . ?
C1 C3 V1B 164.8(7) . . ?
C5 C4 C2 117.5(5) . . ?
C5 C4 C9 118.8(5) . . ?
C9 C4 C2 123.7(5) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.7(5) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.7(5) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.3(5) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.8(5) . . ?
C9 C8 H8 119.6 . . ?
C4 C9 H9 120.1 . . ?
C8 C9 C4 119.7(5) . . ?
C8 C9 H9 120.1 . . ?
C11 C10 N1 116.0(5) . . ?
C11 C10 C15 126.6(5) . . ?
C15 C10 N1 117.4(5) . . ?
C10 C11 C12 115.4(5) . . ?
C10 C11 C16 124.4(4) . . ?
C12 C11 C16 120.2(5) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.5(6) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 118.9 . . ?
C14 C13 C12 122.3(5) . . ?
C14 C13 H13 118.9 . . ?
C13 C14 H14 119.5 . . ?
C13 C14 C15 121.0(6) . . ?
C15 C14 H14 119.5 . . ?
C10 C15 C14 114.3(6) . . ?
C10 C15 C19 122.4(5) . . ?
C14 C15 C19 123.3(5) . . ?
C11 C16 H16 107.4 . . ?
C11 C16 C17 110.4(5) . . ?
C11 C16 C18 113.8(5) . . ?
C17 C16 H16 107.4 . . ?
C17 C16 C18 110.0(6) . . ?
C18 C16 H16 107.4 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19 107.1 . . ?
C15 C19 C20 111.9(6) . . ?
C15 C19 C21 113.6(5) . . ?
C20 C19 H19 107.1 . . ?
C20 C19 C21 109.6(6) . . ?
C21 C19 H19 107.1 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N3 117.2(5) . . ?
C27 C22 N3 118.4(5) . . ?
C27 C22 C23 124.4(5) . . ?
C22 C23 C24 116.0(6) . . ?
C22 C23 C28 124.5(5) . . ?
C24 C23 C28 119.4(5) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.1(6) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.4(5) . . ?
C26 C25 H25 119.3 . . ?
C25 C26 H26 119.3 . . ?
C25 C26 C27 121.3(6) . . ?
C27 C26 H26 119.3 . . ?
C22 C27 C26 115.8(5) . . ?
C22 C27 C31 123.7(5) . . ?
C26 C27 C31 120.5(6) . . ?
C23 C28 H28 108.4 . . ?
C23 C28 C29 110.8(5) . . ?
C23 C28 C30 112.0(6) . . ?
C29 C28 H28 108.4 . . ?
C29 C28 C30 108.8(6) . . ?
C30 C28 H28 108.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 H31 108.0 . . ?
C27 C31 C32 109.6(5) . . ?
C27 C31 C33 112.5(5) . . ?
C32 C31 H31 108.0 . . ?
C33 C31 H31 108.0 . . ?
C33 C31 C32 110.7(6) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
P1 C34A H34A 108.3 . . ?
P1 C34A H34B 108.3 . . ?
H34A C34A H34B 107.4 . . ?
C35A C34A P1 116.0(7) . . ?
C35A C34A H34A 108.3 . . ?
C35A C34A H34B 108.3 . . ?
P1 C34B H34C 103.5 . . ?
P1 C34B H34D 103.5 . . ?
H34C C34B H34D 105.3 . . ?
C35B C34B P1 135(4) . . ?
C35B C34B H34C 103.5 . . ?
C35B C34B H34D 103.5 . . ?
C34A C35A H35A 109.7 . . ?
C34A C35A H35B 109.7 . . ?
C34A C35A C36A 109.7(8) . . ?
H35A C35A H35B 108.2 . . ?
C36A C35A H35A 109.7 . . ?
C36A C35A H35B 109.7 . . ?
C34B C35B H35C 106.2 . . ?
C34B C35B H35D 106.2 . . ?
H35C C35B H35D 106.4 . . ?
C36B C35B C34B 125(3) . . ?
C36B C35B H35C 106.2 . . ?
C36B C35B H35D 106.2 . . ?
C35A C36A H36A 109.1 . . ?
C35A C36A H36B 109.1 . . ?
H36A C36A H36B 107.8 . . ?
C37A C36A C35A 112.7(9) . . ?
C37A C36A H36A 109.1 . . ?
C37A C36A H36B 109.1 . . ?
C35B C36B H36C 109.7 . . ?
C35B C36B H36D 109.7 . . ?
C35B C36B C37B 110(3) . . ?
H36C C36B H36D 108.2 . . ?
C37B C36B H36C 109.7 . . ?
C37B C36B H36D 109.7 . . ?
C36A C37A H37A 109.5 . . ?
C36A C37A H37B 109.5 . . ?
C36A C37A H37C 109.5 . . ?
H37A C37A H37B 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
C36B C37B H37D 109.5 . . ?
C36B C37B H37E 109.5 . . ?
C36B C37B H37F 109.5 . . ?
H37D C37B H37E 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
P1 C38A H38A 107.5 . . ?
P1 C38A H38B 107.5 . . ?
H38A C38A H38B 107.0 . . ?
C39A C38A P1 119.2(7) . . ?
C39A C38A H38A 107.5 . . ?
C39A C38A H38B 107.5 . . ?
P1 C38B H38C 108.5 . . ?
P1 C38B H38D 108.5 . . ?
H38C C38B H38D 107.5 . . ?
C39B C38B P1 115(3) . . ?
C39B C38B H38C 108.5 . . ?
C39B C38B H38D 108.5 . . ?
C38A C39A H39A 108.8 . . ?
C38A C39A H39B 108.8 . . ?
C38A C39A C40A 114.0(8) . . ?
H39A C39A H39B 107.7 . . ?
C40A C39A H39A 108.8 . . ?
C40A C39A H39B 108.8 . . ?
C38B C39B H39C 110.5 . . ?
C38B C39B H39D 110.5 . . ?
C38B C39B C40B 106(2) . . ?
H39C C39B H39D 108.7 . . ?
C40B C39B H39C 110.5 . . ?
C40B C39B H39D 110.5 . . ?
C39A C40A H40A 108.6 . . ?
C39A C40A H40B 108.6 . . ?
C39A C40A C41A 114.8(9) . . ?
H40A C40A H40B 107.5 . . ?
C41A C40A H40A 108.6 . . ?
C41A C40A H40B 108.6 . . ?
C39B C40B H40C 109.6 . . ?
C39B C40B H40D 109.6 . . ?
H40C C40B H40D 108.2 . . ?
C41B C40B C39B 110(3) . . ?
C41B C40B H40C 109.6 . . ?
C41B C40B H40D 109.6 . . ?
C40A C41A H41A 109.5 . . ?
C40A C41A H41B 109.5 . . ?
C40A C41A H41C 109.5 . . ?
H41A C41A H41B 109.5 . . ?
H41A C41A H41C 109.5 . . ?
H41B C41A H41C 109.5 . . ?
C40B C41B H41D 109.5 . . ?
C40B C41B H41E 109.5 . . ?
C40B C41B H41F 109.5 . . ?
H41D C41B H41E 109.5 . . ?
H41D C41B H41F 109.5 . . ?
H41E C41B H41F 109.5 . . ?
P1 C42A H42A 107.7 . . ?
P1 C42A H42B 107.7 . . ?
H42A C42A H42B 107.1 . . ?
C43A C42A P1 118.6(8) . . ?
C43A C42A H42A 107.7 . . ?
C43A C42A H42B 107.7 . . ?
P1 C42B H42C 110.7 . . ?
P1 C42B H42D 110.7 . . ?
H42C C42B H42D 108.8 . . ?
C43B C42B P1 105(3) . . ?
C43B C42B H42C 110.7 . . ?
C43B C42B H42D 110.7 . . ?
C42A C43A H43A 108.6 . . ?
C42A C43A H43B 108.6 . . ?
C42A C43A C44A 114.8(10) . . ?
H43A C43A H43B 107.5 . . ?
C44A C43A H43A 108.6 . . ?
C44A C43A H43B 108.6 . . ?
C42B C43B H43C 109.0 . . ?
C42B C43B H43D 109.0 . . ?
H43C C43B H43D 107.8 . . ?
C44B C43B C42B 113(3) . . ?
C44B C43B H43C 109.0 . . ?
C44B C43B H43D 109.0 . . ?
C43A C44A H44A 110.4 . . ?
C43A C44A H44B 110.4 . . ?
H44A C44A H44B 108.6 . . ?
C45A C44A C43A 106.6(11) . . ?
C45A C44A H44A 110.4 . . ?
C45A C44A H44B 110.4 . . ?
C43B C44B H44C 109.3 . . ?
C43B C44B H44D 109.3 . . ?
C43B C44B C45B 111(3) . . ?
H44C C44B H44D 108.0 . . ?
C45B C44B H44C 109.3 . . ?
C45B C44B H44D 109.3 . . ?
C44A C45A H45A 109.5 . . ?
C44A C45A H45B 109.5 . . ?
C44A C45A H45C 109.5 . . ?
H45A C45A H45B 109.5 . . ?
H45A C45A H45C 109.5 . . ?
H45B C45A H45C 109.5 . . ?
C44B C45B H45D 109.5 . . ?
C44B C45B H45E 109.5 . . ?
C44B C45B H45F 109.5 . . ?
H45D C45B H45E 109.5 . . ?
H45D C45B H45F 109.5 . . ?
H45E C45B H45F 109.5 . . ?

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
V1A P1 C34A C35A -60.3(8) . . . . ?
V1A P1 C38A C39A -171.0(7) . . . . ?
V1A P1 C42A C43A -50.3(11) . . . . ?
V1B P1 C34B C35B 168(5) . . . . ?
V1B P1 C38B C39B 179(4) . . . . ?
V1B P1 C42B C43B 62(5) . . . . ?
Cl1B V1B C3 C1 16(2) . . . . ?
Cl2B V1B C3 C1 109(2) . . . . ?
Cl2B P1 C34B C35B -162(4) . . . . ?
Cl2B P1 C38B C39B -139(5) . . . . ?
Cl2B P1 C42B C43B 19(4) . . . . ?
Cl3B V1B C3 C1 -94(2) . . . . ?
P1 V1B C3 C1 149(2) . . . . ?
P1 C34A C35A C36A 172.4(8) . . . . ?
P1 C34B C35B C36B -105(7) . . . . ?
P1 C38A C39A C40A 176.7(8) . . . . ?
P1 C38B C39B C40B 166(5) . . . . ?
P1 C42A C43A C44A -176.3(9) . . . . ?
P1 C42B C43B C44B 152(4) . . . . ?
N1 N2 N3 C2 1.7(6) . . . . ?
N1 N2 N3 C22 179.8(4) . . . . ?
N1 C1 C2 N3 2.0(6) . . . . ?
N1 C1 C2 C4 -172.6(6) . . . . ?
N1 C1 C3 V1B 87(2) . . . . ?
N1 C10 C11 C12 177.5(4) . . . . ?
N1 C10 C11 C16 -5.2(8) . . . . ?
N1 C10 C15 C14 -179.0(5) . . . . ?
N1 C10 C15 C19 4.1(8) . . . . ?
N2 N1 C1 C2 -1.2(7) . . . . ?
N2 N1 C1 C3 179.3(5) . . . . ?
N2 N1 C10 C11 85.7(6) . . . . ?
N2 N1 C10 C15 -95.1(6) . . . . ?
N2 N3 C2 C1 -2.4(6) . . . . ?
N2 N3 C2 C4 172.5(5) . . . . ?
N2 N3 C22 C23 89.5(6) . . . . ?
N2 N3 C22 C27 -87.8(6) . . . . ?
N3 C2 C4 C5 -143.2(6) . . . . ?
N3 C2 C4 C9 35.4(10) . . . . ?
N3 C22 C23 C24 -177.6(4) . . . . ?
N3 C22 C23 C28 1.1(7) . . . . ?
N3 C22 C27 C26 176.7(4) . . . . ?
N3 C22 C27 C31 -3.3(7) . . . . ?
C1 N1 N2 N3 -0.3(6) . . . . ?
C1 N1 C10 C11 -82.4(7) . . . . ?
C1 N1 C10 C15 96.9(7) . . . . ?
C1 C2 C4 C5 30.4(10) . . . . ?
C1 C2 C4 C9 -151.0(6) . . . . ?
C2 N3 C22 C23 -92.8(6) . . . . ?
C2 N3 C22 C27 89.9(7) . . . . ?
C2 C1 C3 V1B -92(2) . . . . ?
C2 C4 C5 C6 176.7(6) . . . . ?
C2 C4 C9 C8 -177.4(6) . . . . ?
C3 C1 C2 N3 -178.4(6) . . . . ?
C3 C1 C2 C4 6.9(12) . . . . ?
C4 C5 C6 C7 0.8(10) . . . . ?
C5 C4 C9 C8 1.2(10) . . . . ?
C5 C6 C7 C8 1.2(11) . . . . ?
C6 C7 C8 C9 -2.0(11) . . . . ?
C7 C8 C9 C4 0.8(10) . . . . ?
C9 C4 C5 C6 -1.9(10) . . . . ?
C10 N1 N2 N3 -169.9(5) . . . . ?
C10 N1 C1 C2 167.4(5) . . . . ?
C10 N1 C1 C3 -12.2(9) . . . . ?
C10 C11 C12 C13 1.7(8) . . . . ?
C10 C11 C16 C17 -100.6(6) . . . . ?
C10 C11 C16 C18 135.1(6) . . . . ?
C10 C15 C19 C20 83.4(7) . . . . ?
C10 C15 C19 C21 -151.9(6) . . . . ?
C11 C10 C15 C14 0.2(8) . . . . ?
C11 C10 C15 C19 -176.7(6) . . . . ?
C11 C12 C13 C14 -0.2(9) . . . . ?
C12 C11 C16 C17 76.7(6) . . . . ?
C12 C11 C16 C18 -47.6(7) . . . . ?
C12 C13 C14 C15 -1.5(9) . . . . ?
C13 C14 C15 C10 1.5(8) . . . . ?
C13 C14 C15 C19 178.3(6) . . . . ?
C14 C15 C19 C20 -93.3(7) . . . . ?
C14 C15 C19 C21 31.5(9) . . . . ?
C15 C10 C11 C12 -1.7(8) . . . . ?
C15 C10 C11 C16 175.6(5) . . . . ?
C16 C11 C12 C13 -175.8(5) . . . . ?
C22 N3 C2 C1 179.8(5) . . . . ?
C22 N3 C2 C4 -5.3(10) . . . . ?
C22 C23 C24 C25 0.2(7) . . . . ?
C22 C23 C28 C29 -111.6(6) . . . . ?
C22 C23 C28 C30 126.6(6) . . . . ?
C22 C27 C31 C32 -101.3(6) . . . . ?
C22 C27 C31 C33 135.1(5) . . . . ?
C23 C22 C27 C26 -0.3(7) . . . . ?
C23 C22 C27 C31 179.7(5) . . . . ?
C23 C24 C25 C26 0.9(9) . . . . ?
C24 C23 C28 C29 67.1(7) . . . . ?
C24 C23 C28 C30 -54.6(7) . . . . ?
C24 C25 C26 C27 -1.9(8) . . . . ?
C25 C26 C27 C22 1.5(7) . . . . ?
C25 C26 C27 C31 -178.5(5) . . . . ?
C26 C27 C31 C32 78.7(7) . . . . ?
C26 C27 C31 C33 -44.9(7) . . . . ?
C27 C22 C23 C24 -0.5(7) . . . . ?
C27 C22 C23 C28 178.2(5) . . . . ?
C28 C23 C24 C25 -178.6(5) . . . . ?
C34A P1 C38A C39A 59.6(9) . . . . ?
C34A P1 C42A C43A 78.7(11) . . . . ?
C34A C35A C36A C37A 177.5(10) . . . . ?
C34B P1 C38B C39B 93(5) . . . . ?
C34B P1 C42B C43B -177(4) . . . . ?
C34B C35B C36B C37B 149(6) . . . . ?
C38A P1 C34A C35A 68.2(8) . . . . ?
C38A P1 C42A C43A -174.7(10) . . . . ?
C38A C39A C40A C41A 176.6(10) . . . . ?
C38B P1 C34B C35B -80(5) . . . . ?
C38B P1 C42B C43B -66(5) . . . . ?
C38B C39B C40B C41B -173(6) . . . . ?
C42A P1 C34A C35A 173.8(8) . . . . ?
C42A P1 C38A C39A -49.4(10) . . . . ?
C42A C43A C44A C45A 174.2(12) . . . . ?
C42B P1 C34B C35B 38(7) . . . . ?
C42B P1 C38B C39B -52(5) . . . . ?
C42B C43B C44B C45B 129(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 241.4 73.6 '2 THF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.909
_oxdiff_exptl_absorpt_empirical_full_min 0.278
####################################################################### 
# 
# 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_bk122
_database_code_depnum_ccdc_archive 'CCDC 2105986'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-08-27 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_audit_creation_date             2021-08-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H36 Cl3 N2 V, C6 H6'
_chemical_formula_sum            'C34 H42 Cl3 N2 V'
_chemical_formula_weight         635.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H42 Cl3 N2 V'
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'
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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.7785(3)
_cell_length_b                   9.29150(18)
_cell_length_c                   22.4036(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.312(2)
_cell_angle_gamma                90
_cell_volume                     3398.82(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7502
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5500
_cell_measurement_theta_min      3.6830
_shelx_estimated_absorpt_T_max   0.910
_shelx_estimated_absorpt_T_min   0.621
_exptl_absorpt_coefficient_mu    4.784
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -1 0.0270
-1 0 1 0.0489
0 1 0 0.0130
0 -1 0 0.0059
-1 0 0 0.0366
1 -2 2 0.0251
2 0 -1 0.0279
1 0 2 0.0543
-1 0 -2 0.0315

_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
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
1.0000 -0.0000 -0.9999 0.0238 -0.0989 0.0219
-1.0000 0.0000 0.9999 -0.0238 0.0989 -0.0219
0.0000 1.0000 -0.0001 -0.0838 0.0113 0.1426
-0.0000 -1.0000 0.0001 0.0838 -0.0113 -0.1426
-1.0000 0.0000 -0.0001 0.0357 0.0862 0.0141
0.9999 -2.0000 2.0002 0.0129 -0.0835 -0.3713
2.0000 -0.0000 -0.9999 -0.0118 -0.1851 0.0078
1.0000 0.0000 2.0000 -0.1546 -0.0609 -0.0861
-1.0000 -0.0000 -2.0000 0.1546 0.0609 0.0861

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.529
_diffrn_reflns_theta_min         3.737
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  30.00   1.00   12.50    --  -43.50  81.00-130.00   46
  2  ω      3.00  28.00   1.00   12.50    --   43.68 -81.00 106.00   25
  3  ω     52.00 101.00   1.00   50.00    --  103.26 -81.00 106.00   49
  4  ω    106.00 178.00   1.00   50.00    --  103.26  81.00-130.00   72
  5  ω    -59.00  -6.00   1.00   12.50    --  -43.50 125.00 -60.00   53
  6  ω   -103.00 -18.00   1.00   12.50    --  -43.50 -57.00  60.00   85
  7  ω      7.00  84.00   1.00   12.50    --   43.68 -99.00 -90.00   77
  8  ω    103.00 175.00   1.00   50.00    --  103.26  77.00  90.00   72
  9  ω    116.00 148.00   1.00   50.00    --  103.26 125.00 -90.00   32
 10  ω     34.00  84.00   1.00   50.00    --  103.26 -61.00 -30.00   50
 11  ω    115.00 176.00   1.00   50.00    --  103.26  77.00 -60.00   61
 12  ω    116.00 143.00   1.00   50.00    --  103.26 125.00  30.00   27
 13  ω     86.00 166.00   1.00   50.00    --  103.26  45.00-150.00   80
 14  ω    134.00 159.00   1.00   50.00    --  103.26  77.00 120.00   25
 15  ω     40.00  67.00   1.00   50.00    --  103.26-125.00  90.00   27
 16  ω     99.00 125.00   1.00   50.00    --  103.26 -77.00 -90.00   26
;
_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      -0.0356587000
_diffrn_orient_matrix_UB_12      -0.0837573000
_diffrn_orient_matrix_UB_13      -0.0594811000
_diffrn_orient_matrix_UB_21      -0.0862235000
_diffrn_orient_matrix_UB_22      0.0112881000
_diffrn_orient_matrix_UB_23      0.0126685000
_diffrn_orient_matrix_UB_31      -0.0140823000
_diffrn_orient_matrix_UB_32      0.1425767000
_diffrn_orient_matrix_UB_33      -0.0360194000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                5506
_reflns_number_total             6581
_reflns_odcompleteness_completeness 99.95
_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 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6581
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0387
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0484P)²+1.9668P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1017
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C31A \\sim C31B \\sim C32A \\sim C32B \\sim C33A \\sim C33B \\sim C34A \\sim
C34B \\sim C35A \\sim C35B \\sim C36A \\sim C36B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33B)=Sof(C34B)=
 Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=
 Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A),
 C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B)
4.c Fitted hexagon refined as free rotating group:
 C31A(C32A,C33A,C34A,C35A,C36A), C31B(C32B,C33B,C34B,C35B,C36B)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.28092(2) 0.43353(4) 0.58258(2) 0.01938(10) Uani 1 1 d . . . . .
Cl1 Cl 0.40611(3) 0.37415(6) 0.63150(3) 0.03454(14) Uani 1 1 d . . . . .
Cl2 Cl 0.25178(3) 0.34303(6) 0.48888(2) 0.02816(13) Uani 1 1 d . . . . .
Cl3 Cl 0.18572(3) 0.36975(6) 0.63092(3) 0.03010(13) Uani 1 1 d . . . . .
N1 N 0.20902(10) 0.85148(19) 0.56531(8) 0.0216(4) Uani 1 1 d . . . . .
N2 N 0.34052(11) 0.85878(19) 0.57310(8) 0.0222(4) Uani 1 1 d . . . . .
C2 C 0.27667(12) 0.7680(2) 0.57167(9) 0.0202(4) Uani 1 1 d . . . . .
C4 C 0.31239(14) 0.9983(2) 0.56685(11) 0.0286(5) Uani 1 1 d . . . . .
H4 H 0.344501 1.082227 0.566055 0.034 Uiso 1 1 calc R U . . .
C5 C 0.23044(14) 0.9940(2) 0.56206(11) 0.0279(5) Uani 1 1 d . . . . .
H5 H 0.194447 1.074259 0.557329 0.033 Uiso 1 1 calc R U . . .
C6 C 0.27923(12) 0.6165(2) 0.57601(10) 0.0220(4) Uani 1 1 d . . . . .
C7 C 0.12810(12) 0.7947(2) 0.56278(10) 0.0236(4) Uani 1 1 d . . . . .
C8 C 0.10823(13) 0.7582(2) 0.61813(11) 0.0255(5) Uani 1 1 d . . . . .
C9 C 0.03082(14) 0.6988(3) 0.61365(12) 0.0340(5) Uani 1 1 d . . . . .
H9 H 0.014446 0.671939 0.649965 0.041 Uiso 1 1 calc R U . . .
C10 C -0.02257(15) 0.6782(3) 0.55732(14) 0.0412(6) Uani 1 1 d . . . . .
H10 H -0.074822 0.636699 0.555451 0.049 Uiso 1 1 calc R U . . .
C11 C -0.00110(15) 0.7169(3) 0.50431(13) 0.0384(6) Uani 1 1 d . . . . .
H11 H -0.038948 0.702258 0.466151 0.046 Uiso 1 1 calc R U . . .
C12 C 0.07527(14) 0.7775(3) 0.50499(11) 0.0300(5) Uani 1 1 d . . . . .
C13 C 0.16643(14) 0.7865(3) 0.67986(11) 0.0296(5) Uani 1 1 d . . . . .
H13 H 0.223693 0.775808 0.674520 0.036 Uiso 1 1 calc R U . . .
C14 C 0.15606(19) 0.9406(3) 0.70021(13) 0.0429(6) Uani 1 1 d . . . . .
H14A H 0.099805 0.954600 0.704609 0.064 Uiso 1 1 calc R U . . .
H14B H 0.167366 1.007730 0.669434 0.064 Uiso 1 1 calc R U . . .
H14C H 0.194355 0.958586 0.739664 0.064 Uiso 1 1 calc R U . . .
C15 C 0.15549(17) 0.6824(3) 0.73019(12) 0.0382(6) Uani 1 1 d . . . . .
H15A H 0.200125 0.696046 0.766579 0.057 Uiso 1 1 calc R U . . .
H15B H 0.156398 0.583201 0.715488 0.057 Uiso 1 1 calc R U . . .
H15C H 0.102945 0.701193 0.740771 0.057 Uiso 1 1 calc R U . . .
C16 C 0.09925(17) 0.8177(3) 0.44599(11) 0.0368(6) Uani 1 1 d . . . . .
H16 H 0.148853 0.880619 0.456725 0.044 Uiso 1 1 calc R U . . .
C17 C 0.0316(2) 0.9024(4) 0.40333(15) 0.0575(8) Uani 1 1 d . . . . .
H17A H -0.016838 0.841015 0.390287 0.086 Uiso 1 1 calc R U . . .
H17B H 0.050639 0.933852 0.367257 0.086 Uiso 1 1 calc R U . . .
H17C H 0.017322 0.986714 0.425012 0.086 Uiso 1 1 calc R U . . .
C18 C 0.1212(3) 0.6853(4) 0.41329(16) 0.0727(12) Uani 1 1 d . . . . .
H18A H 0.165880 0.633205 0.440693 0.109 Uiso 1 1 calc R U . . .
H18B H 0.138781 0.714955 0.376330 0.109 Uiso 1 1 calc R U . . .
H18C H 0.073262 0.622447 0.401780 0.109 Uiso 1 1 calc R U . . .
C19 C 0.42435(13) 0.8125(2) 0.57912(11) 0.0230(4) Uani 1 1 d . . . . .
C20 C 0.47582(14) 0.8093(2) 0.63773(11) 0.0258(5) Uani 1 1 d . . . . .
C21 C 0.55500(15) 0.7596(3) 0.64197(12) 0.0324(5) Uani 1 1 d . . . . .
H21 H 0.592085 0.755141 0.680984 0.039 Uiso 1 1 calc R U . . .
C22 C 0.58086(15) 0.7165(3) 0.59040(12) 0.0339(5) Uani 1 1 d . . . . .
H22 H 0.634993 0.681158 0.594538 0.041 Uiso 1 1 calc R U . . .
C23 C 0.52888(15) 0.7242(3) 0.53316(12) 0.0322(5) Uani 1 1 d . . . . .
H23 H 0.547686 0.694388 0.498231 0.039 Uiso 1 1 calc R U . . .
C24 C 0.44927(14) 0.7750(2) 0.52575(11) 0.0254(5) Uani 1 1 d . . . . .
C25 C 0.44776(15) 0.8541(3) 0.69479(11) 0.0309(5) Uani 1 1 d . . . . .
H25 H 0.397308 0.913998 0.681210 0.037 Uiso 1 1 calc R U . . .
C26 C 0.4250(2) 0.7243(3) 0.72812(14) 0.0507(8) Uani 1 1 d . . . . .
H26A H 0.402862 0.756333 0.762744 0.076 Uiso 1 1 calc R U . . .
H26B H 0.473769 0.665113 0.743336 0.076 Uiso 1 1 calc R U . . .
H26C H 0.383554 0.667433 0.699874 0.076 Uiso 1 1 calc R U . . .
C27 C 0.5115(2) 0.9463(4) 0.73723(16) 0.0577(9) Uani 1 1 d . . . . .
H27A H 0.561750 0.890219 0.751509 0.087 Uiso 1 1 calc R U . . .
H27B H 0.490343 0.976550 0.772547 0.087 Uiso 1 1 calc R U . . .
H27C H 0.523449 1.031400 0.714987 0.087 Uiso 1 1 calc R U . . .
C28 C 0.39334(15) 0.7882(3) 0.46207(11) 0.0309(5) Uani 1 1 d . . . . .
H28 H 0.341859 0.837963 0.465798 0.037 Uiso 1 1 calc R U . . .
C29 C 0.43437(18) 0.8781(3) 0.42056(13) 0.0428(6) Uani 1 1 d . . . . .
H29A H 0.450039 0.971888 0.439689 0.064 Uiso 1 1 calc R U . . .
H29B H 0.396068 0.892100 0.380780 0.064 Uiso 1 1 calc R U . . .
H29C H 0.483330 0.827994 0.414567 0.064 Uiso 1 1 calc R U . . .
C30 C 0.3710(2) 0.6404(3) 0.43370(14) 0.0538(8) Uani 1 1 d . . . . .
H30A H 0.420517 0.592278 0.427733 0.081 Uiso 1 1 calc R U . . .
H30B H 0.332014 0.651433 0.394024 0.081 Uiso 1 1 calc R U . . .
H30C H 0.345995 0.582532 0.461104 0.081 Uiso 1 1 calc R U . . .
C31A C 0.60478(18) 0.3429(4) 0.77810(16) 0.0724(11) Uani 0.785(5) 1 d G U P A 1
H31A H 0.554944 0.290940 0.773439 0.087 Uiso 0.785(5) 1 calc R U P A 1
C32A C 0.6614(2) 0.3429(5) 0.83421(14) 0.0770(11) Uani 0.785(5) 1 d G U P A 1
H32A H 0.650186 0.291009 0.867909 0.092 Uiso 0.785(5) 1 calc R U P A 1
C33A C 0.73427(19) 0.4189(5) 0.84103(12) 0.0807(12) Uani 0.785(5) 1 d G U P A 1
H33A H 0.772934 0.418880 0.879385 0.097 Uiso 0.785(5) 1 calc R U P A 1
C34A C 0.75061(16) 0.4948(4) 0.79173(16) 0.0825(13) Uani 0.785(5) 1 d G U P A 1
H34A H 0.800441 0.546684 0.796391 0.099 Uiso 0.785(5) 1 calc R U P A 1
C35A C 0.69403(18) 0.4947(5) 0.73561(13) 0.0702(12) Uani 0.785(5) 1 d G U P A 1
H35A H 0.705201 0.546617 0.701920 0.084 Uiso 0.785(5) 1 calc R U P A 1
C36A C 0.62112(17) 0.4188(5) 0.72880(11) 0.0702(11) Uani 0.785(5) 1 d G U P A 1
H36A H 0.582452 0.418746 0.690443 0.084 Uiso 0.785(5) 1 calc R U P A 1
C31B C 0.6180(8) 0.3356(15) 0.7527(6) 0.0761(16) Uani 0.215(5) 1 d G U P A 2
H31B H 0.581869 0.273506 0.725448 0.091 Uiso 0.215(5) 1 calc R U P A 2
C32B C 0.6517(9) 0.2919(13) 0.8125(6) 0.0770(16) Uani 0.215(5) 1 d G U P A 2
H32B H 0.638618 0.199928 0.826160 0.092 Uiso 0.215(5) 1 calc R U P A 2
C33B C 0.7046(9) 0.3827(16) 0.8524(4) 0.0778(18) Uani 0.215(5) 1 d G U P A 2
H33B H 0.727632 0.352828 0.893274 0.093 Uiso 0.215(5) 1 calc R U P A 2
C34B C 0.7238(8) 0.5172(15) 0.8324(6) 0.0793(16) Uani 0.215(5) 1 d G U P A 2
H34B H 0.759897 0.579309 0.859676 0.095 Uiso 0.215(5) 1 calc R U P A 2
C35B C 0.6901(8) 0.5609(13) 0.7726(6) 0.0773(16) Uani 0.215(5) 1 d G U P A 2
H35B H 0.703150 0.652890 0.758965 0.093 Uiso 0.215(5) 1 calc R U P A 2
C36B C 0.6372(9) 0.4701(16) 0.7327(4) 0.0749(16) Uani 0.215(5) 1 d G U P A 2
H36B H 0.614136 0.499991 0.691850 0.090 Uiso 0.215(5) 1 calc R U P A 2


_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 Cl1 2.2040(6) . ?
V1 Cl2 2.2090(6) . ?
V1 Cl3 2.2073(6) . ?
V1 C6 1.706(2) . ?
N1 C2 1.355(3) . ?
N1 C5 1.379(3) . ?
N1 C7 1.445(3) . ?
N2 C2 1.358(3) . ?
N2 C4 1.376(3) . ?
N2 C19 1.447(3) . ?
C2 C6 1.412(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.355(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.398(3) . ?
C7 C12 1.400(3) . ?
C8 C9 1.394(3) . ?
C8 C13 1.521(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.366(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.397(4) . ?
C12 C16 1.514(4) . ?
C13 H13 1.0000 . ?
C13 C14 1.525(4) . ?
C13 C15 1.528(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 1.0000 . ?
C16 C17 1.524(4) . ?
C16 C18 1.520(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.396(3) . ?
C19 C24 1.399(3) . ?
C20 C21 1.389(3) . ?
C20 C25 1.519(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.377(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.390(3) . ?
C24 C28 1.521(3) . ?
C25 H25 1.0000 . ?
C25 C26 1.513(4) . ?
C25 C27 1.521(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 1.0000 . ?
C28 C29 1.527(3) . ?
C28 C30 1.523(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31A H31A 0.9500 . ?
C31A C32A 1.3900 . ?
C31A C36A 1.3900 . ?
C32A H32A 0.9500 . ?
C32A C33A 1.3900 . ?
C33A H33A 0.9500 . ?
C33A C34A 1.3900 . ?
C34A H34A 0.9500 . ?
C34A C35A 1.3900 . ?
C35A H35A 0.9500 . ?
C35A C36A 1.3900 . ?
C36A H36A 0.9500 . ?
C31B H31B 0.9500 . ?
C31B C32B 1.3900 . ?
C31B C36B 1.3900 . ?
C32B H32B 0.9500 . ?
C32B C33B 1.3900 . ?
C33B H33B 0.9500 . ?
C33B C34B 1.3900 . ?
C34B H34B 0.9500 . ?
C34B C35B 1.3900 . ?
C35B H35B 0.9500 . ?
C35B C36B 1.3900 . ?
C36B H36B 0.9500 . ?

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
Cl1 V1 Cl2 110.75(3) . . ?
Cl1 V1 Cl3 113.78(3) . . ?
Cl3 V1 Cl2 109.71(3) . . ?
C6 V1 Cl1 106.70(7) . . ?
C6 V1 Cl2 107.55(8) . . ?
C6 V1 Cl3 108.08(7) . . ?
C2 N1 C5 109.45(18) . . ?
C2 N1 C7 123.51(18) . . ?
C5 N1 C7 127.04(18) . . ?
C2 N2 C4 109.42(18) . . ?
C2 N2 C19 124.21(18) . . ?
C4 N2 C19 126.36(18) . . ?
N1 C2 N2 106.53(18) . . ?
N1 C2 C6 126.13(19) . . ?
N2 C2 C6 127.34(19) . . ?
N2 C4 H4 126.3 . . ?
C5 C4 N2 107.35(19) . . ?
C5 C4 H4 126.3 . . ?
N1 C5 H5 126.4 . . ?
C4 C5 N1 107.25(19) . . ?
C4 C5 H5 126.4 . . ?
C2 C6 V1 178.59(19) . . ?
C8 C7 N1 117.87(19) . . ?
C8 C7 C12 124.3(2) . . ?
C12 C7 N1 117.8(2) . . ?
C7 C8 C13 122.0(2) . . ?
C9 C8 C7 116.2(2) . . ?
C9 C8 C13 121.8(2) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.2(2) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.4(2) . . ?
C12 C11 H11 119.3 . . ?
C7 C12 C16 122.7(2) . . ?
C11 C12 C7 116.1(2) . . ?
C11 C12 C16 121.2(2) . . ?
C8 C13 H13 107.9 . . ?
C8 C13 C14 109.9(2) . . ?
C8 C13 C15 113.6(2) . . ?
C14 C13 H13 107.9 . . ?
C14 C13 C15 109.4(2) . . ?
C15 C13 H13 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 H16 107.9 . . ?
C12 C16 C17 111.4(2) . . ?
C12 C16 C18 111.3(2) . . ?
C17 C16 H16 107.9 . . ?
C18 C16 H16 107.9 . . ?
C18 C16 C17 110.1(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 N2 118.13(19) . . ?
C20 C19 C24 123.8(2) . . ?
C24 C19 N2 118.0(2) . . ?
C19 C20 C25 122.8(2) . . ?
C21 C20 C19 116.5(2) . . ?
C21 C20 C25 120.7(2) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.2(2) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.6(2) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 120.9(2) . . ?
C24 C23 H23 119.5 . . ?
C19 C24 C28 122.7(2) . . ?
C23 C24 C19 116.8(2) . . ?
C23 C24 C28 120.5(2) . . ?
C20 C25 H25 107.5 . . ?
C20 C25 C27 111.8(2) . . ?
C26 C25 C20 111.1(2) . . ?
C26 C25 H25 107.5 . . ?
C26 C25 C27 111.2(3) . . ?
C27 C25 H25 107.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28 108.5 . . ?
C24 C28 C29 110.4(2) . . ?
C24 C28 C30 111.0(2) . . ?
C29 C28 H28 108.5 . . ?
C30 C28 H28 108.5 . . ?
C30 C28 C29 110.0(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32A C31A H31A 120.0 . . ?
C32A C31A C36A 120.0 . . ?
C36A C31A H31A 120.0 . . ?
C31A C32A H32A 120.0 . . ?
C33A C32A C31A 120.0 . . ?
C33A C32A H32A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C32A C33A C34A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C33A C34A H34A 120.0 . . ?
C33A C34A C35A 120.0 . . ?
C35A C34A H34A 120.0 . . ?
C34A C35A H35A 120.0 . . ?
C36A C35A C34A 120.0 . . ?
C36A C35A H35A 120.0 . . ?
C31A C36A H36A 120.0 . . ?
C35A C36A C31A 120.0 . . ?
C35A C36A H36A 120.0 . . ?
C32B C31B H31B 120.0 . . ?
C32B C31B C36B 120.0 . . ?
C36B C31B H31B 120.0 . . ?
C31B C32B H32B 120.0 . . ?
C33B C32B C31B 120.0 . . ?
C33B C32B H32B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C34B C33B C32B 120.0 . . ?
C34B C33B H33B 120.0 . . ?
C33B C34B H34B 120.0 . . ?
C35B C34B C33B 120.0 . . ?
C35B C34B H34B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C34B C35B C36B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C31B C36B H36B 120.0 . . ?
C35B C36B C31B 120.0 . . ?
C35B C36B H36B 120.0 . . ?

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
N1 C7 C8 C9 -177.6(2) . . . . ?
N1 C7 C8 C13 4.4(3) . . . . ?
N1 C7 C12 C11 177.4(2) . . . . ?
N1 C7 C12 C16 -0.9(3) . . . . ?
N2 C4 C5 N1 -0.1(3) . . . . ?
N2 C19 C20 C21 177.85(19) . . . . ?
N2 C19 C20 C25 -0.8(3) . . . . ?
N2 C19 C24 C23 -176.92(19) . . . . ?
N2 C19 C24 C28 3.1(3) . . . . ?
C2 N1 C5 C4 -0.4(3) . . . . ?
C2 N1 C7 C8 80.2(3) . . . . ?
C2 N1 C7 C12 -98.6(3) . . . . ?
C2 N2 C4 C5 0.5(3) . . . . ?
C2 N2 C19 C20 -94.6(3) . . . . ?
C2 N2 C19 C24 86.1(3) . . . . ?
C4 N2 C2 N1 -0.8(2) . . . . ?
C4 N2 C2 C6 179.4(2) . . . . ?
C4 N2 C19 C20 86.7(3) . . . . ?
C4 N2 C19 C24 -92.6(3) . . . . ?
C5 N1 C2 N2 0.7(2) . . . . ?
C5 N1 C2 C6 -179.4(2) . . . . ?
C5 N1 C7 C8 -99.5(3) . . . . ?
C5 N1 C7 C12 81.6(3) . . . . ?
C7 N1 C2 N2 -179.10(18) . . . . ?
C7 N1 C2 C6 0.8(3) . . . . ?
C7 N1 C5 C4 179.4(2) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C7 C8 C13 C14 84.5(3) . . . . ?
C7 C8 C13 C15 -152.5(2) . . . . ?
C7 C12 C16 C17 -134.1(3) . . . . ?
C7 C12 C16 C18 102.5(3) . . . . ?
C8 C7 C12 C11 -1.3(3) . . . . ?
C8 C7 C12 C16 -179.7(2) . . . . ?
C8 C9 C10 C11 -0.6(4) . . . . ?
C9 C8 C13 C14 -93.3(3) . . . . ?
C9 C8 C13 C15 29.7(3) . . . . ?
C9 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 C7 0.5(4) . . . . ?
C10 C11 C12 C16 178.9(3) . . . . ?
C11 C12 C16 C17 47.6(3) . . . . ?
C11 C12 C16 C18 -75.8(3) . . . . ?
C12 C7 C8 C9 1.2(3) . . . . ?
C12 C7 C8 C13 -176.8(2) . . . . ?
C13 C8 C9 C10 177.8(2) . . . . ?
C19 N2 C2 N1 -179.67(19) . . . . ?
C19 N2 C2 C6 0.4(3) . . . . ?
C19 N2 C4 C5 179.4(2) . . . . ?
C19 C20 C21 C22 0.3(4) . . . . ?
C19 C20 C25 C26 98.4(3) . . . . ?
C19 C20 C25 C27 -136.8(3) . . . . ?
C19 C24 C28 C29 125.9(2) . . . . ?
C19 C24 C28 C30 -112.0(3) . . . . ?
C20 C19 C24 C23 3.8(3) . . . . ?
C20 C19 C24 C28 -176.2(2) . . . . ?
C20 C21 C22 C23 1.2(4) . . . . ?
C21 C20 C25 C26 -80.2(3) . . . . ?
C21 C20 C25 C27 44.6(3) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C22 C23 C24 C19 -2.2(3) . . . . ?
C22 C23 C24 C28 177.8(2) . . . . ?
C23 C24 C28 C29 -54.1(3) . . . . ?
C23 C24 C28 C30 68.1(3) . . . . ?
C24 C19 C20 C21 -2.9(3) . . . . ?
C24 C19 C20 C25 178.4(2) . . . . ?
C25 C20 C21 C22 179.0(2) . . . . ?
C31A C32A C33A C34A 0.0 . . . . ?
C32A C31A C36A C35A 0.0 . . . . ?
C32A C33A C34A C35A 0.0 . . . . ?
C33A C34A C35A C36A 0.0 . . . . ?
C34A C35A C36A C31A 0.0 . . . . ?
C36A C31A C32A C33A 0.0 . . . . ?
C31B C32B C33B C34B 0.0 . . . . ?
C32B C31B C36B C35B 0.0 . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C33B C34B C35B C36B 0.0 . . . . ?
C34B C35B C36B C31B 0.0 . . . . ?
C36B C31B C32B C33B 0.0 . . . . ?

_olex2_date_sample_data_collection 2021-08-26
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.891
####################################################################### 
# 
# 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_bk183
_database_code_depnum_ccdc_archive 'CCDC 2130296'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-12-21 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_audit_creation_date             2021-12-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H57 Cl2 N4 Si2 V'
_chemical_formula_sum            'C39 H57 Cl2 N4 Si2 V'
_chemical_formula_weight         759.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C39 H57 Cl2 N4 Si2 V'
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'
Si Si 0.2541 0.3302 '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           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   15.1641(2)
_cell_length_b                   12.35741(14)
_cell_length_c                   24.0239(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.8825(14)
_cell_angle_gamma                90
_cell_volume                     4284.32(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18924
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.8440
_cell_measurement_theta_min      3.0670
_shelx_estimated_absorpt_T_max   0.927
_shelx_estimated_absorpt_T_min   0.485
_exptl_absorpt_coefficient_mu    3.842
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0119
0 0 1 0.0078
0 -1 0 0.0793
1 -1 0 0.0615
-1 1 0 0.1418
-2 0 1 0.0955
-1 -1 1 0.0630
1 1 -1 0.0461
2 0 -1 0.0764
-2 -1 1 0.0667

_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
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
-0.0005 0.0008 -1.0002 0.0009 -0.0648 -0.0186
0.0005 -0.0008 1.0002 -0.0009 0.0648 0.0186
-0.0004 -0.9996 -0.0011 -0.0675 -0.0296 0.1005
0.9997 -0.9998 -0.0008 0.0175 -0.0122 0.1626
-0.9997 0.9998 0.0008 -0.0175 0.0122 -0.1626
-1.9998 -0.0006 0.9997 -0.1709 0.0298 -0.1057
-1.0001 -1.0004 0.9989 -0.1534 0.0177 0.0570
1.0001 1.0004 -0.9989 0.1534 -0.0177 -0.0570
1.9998 0.0006 -0.9997 0.1709 -0.0298 0.1057
-2.0002 -1.0002 0.9986 -0.2384 0.0002 -0.0052

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            56762
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.496
_diffrn_reflns_theta_min         3.079
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     22.00  65.00   0.50    1.00    --   59.87-104.00-139.00   86
  2  ω    -54.00 -21.00   0.50    1.00    --  -62.28 104.00 -39.00   66
  3  ω    -63.00 -28.00   0.50    1.00    --  -71.26 104.00 -39.00   70
  4  ω     35.00  60.00   0.50    2.00    --   71.88-104.00-139.00   50
  5  ω     57.00  91.00   0.50    2.00    --   73.64-104.00-139.00   68
  6  ω    -83.00 -35.00   0.50    2.00    --  -76.11 104.00 -39.00   96
  7  ω     73.00  98.00   0.50    2.00    --   81.22-104.00-139.00   50
  8  ω     11.00  36.00   0.50    1.00    --   59.87 -30.00-180.00   50
  9  ω     11.00  36.00   0.50    1.00    --   59.87 -30.00 -60.00   50
 10  ω     61.00 104.00   0.50    1.00    --   59.87  30.00 120.00   86
 11  ω   -112.00 -63.00   0.50    1.00    --  -62.28 -30.00-150.00   98
 12  ω   -112.00 -69.00   0.50    1.00    --  -62.28 -30.00 -90.00   86
 13  ω   -110.00 -45.00   0.50    1.00    --  -71.26   0.00 -90.00  130
 14  ω   -102.00 -76.00   0.50    1.00    --  -71.26 -30.00 120.00   52
 15  ω   -111.00 -85.00   0.50    1.00    --  -71.26 -30.00-180.00   52
 16  ω   -119.00 -75.00   0.50    1.00    --  -71.26 -30.00-120.00   88
 17  ω     76.00 113.00   0.50    2.00    --   71.88  30.00 -90.00   74
 18  ω     74.00 111.00   0.50    2.00    --   71.88  30.00 150.00   74
 19  ω     35.00  67.00   0.50    2.00    --   73.64 -95.00 -90.00   64
 20  ω     34.00  80.00   0.50    2.00    --   73.64 -95.00 150.00   92
 21  ω     36.00  82.00   0.50    2.00    --   73.64 -95.00  90.00   92
 22  ω   -125.00 -81.00   0.50    2.00    --  -76.11 -30.00   0.00   88
 23  ω   -105.00 -33.00   0.50    2.00    --  -76.11 125.00 -90.00  144
 24  ω   -107.00 -34.00   0.50    2.00    --  -76.11 125.00   0.00  146
 25  ω   -122.00 -97.00   0.50    2.00    --  -76.11-125.00 -60.00   50
 26  ω     84.00 110.00   0.50    2.00    --   81.22-125.00 150.00   52
 27  ω     37.00  80.00   0.50    2.00    --   81.22-125.00 150.00   86
 28  ω     41.00  73.00   0.50    2.00    --   81.22 -95.00  30.00   64
 29  ω     52.00  77.00   0.50    2.00    --   81.22-125.00 -60.00   50
 30  ω    100.00 125.00   0.50    2.00    --   81.22 125.00 150.00   50
 31  ω     97.00 131.00   0.50    2.00    --   81.22  30.00-150.00   68
 32  ω     99.00 126.00   0.50    2.00    --   81.22 125.00-180.00   54
 33  ω     44.00 116.00   0.50    2.00    --   81.22   0.00-180.00  144
 34  ω     80.00 112.00   0.50    2.00    --   81.22-125.00 -60.00   64
 35  ω     87.00 112.00   0.50    2.00    --   81.22-125.00  30.00   50
 36  ω     38.00 111.00   0.50    2.00    --   81.22-125.00-150.00  146
 37  ω     54.00  79.00   0.50    2.00    --   81.22-125.00-180.00   50
 38  ω     87.00 129.00   0.50    2.00    --   81.22  30.00-180.00   84
 39  ω     65.00  90.00   0.50    2.00    --   81.22 -95.00-150.00   50
 40  ω     87.00 112.00   0.50    2.00    --   81.22-125.00-180.00   50
 41  ω     52.00  81.00   0.50    2.00    --   81.22-125.00 -30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0850139000
_diffrn_orient_matrix_UB_12      0.0674935000
_diffrn_orient_matrix_UB_13      -0.0008493000
_diffrn_orient_matrix_UB_21      0.0174642000
_diffrn_orient_matrix_UB_22      0.0295626000
_diffrn_orient_matrix_UB_23      0.0648019000
_diffrn_orient_matrix_UB_31      0.0620933000
_diffrn_orient_matrix_UB_32      -0.1005872000
_diffrn_orient_matrix_UB_33      0.0184605000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7129
_reflns_number_total             8625
_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 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8625
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.037
_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)+(0.0802P)²+1.9346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1372
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.46406(3) 0.72113(3) 0.65767(2) 0.03150(12) Uani 1 1 d . . . . .
Cl1 Cl 0.57507(4) 0.73571(6) 0.61451(3) 0.05154(18) Uani 1 1 d . . . . .
Cl2 Cl 0.47541(5) 0.56755(6) 0.70888(3) 0.05307(18) Uani 1 1 d . . . . .
Si1 Si 0.36212(5) 0.94449(5) 0.66399(3) 0.04120(17) Uani 1 1 d . . . . .
Si2 Si 0.54871(5) 0.88787(7) 0.75342(3) 0.0499(2) Uani 1 1 d . . . . .
N1 N 0.17727(13) 0.67304(16) 0.46707(8) 0.0334(4) Uani 1 1 d . . . . .
N2 N 0.16182(13) 0.58826(15) 0.49703(8) 0.0327(4) Uani 1 1 d . . . . .
N3 N 0.22971(12) 0.59388(14) 0.54740(8) 0.0293(4) Uani 1 1 d . . . . .
N4 N 0.45023(14) 0.85179(17) 0.69484(9) 0.0391(4) Uani 1 1 d . . . . .
C1 C 0.25298(16) 0.73146(19) 0.49675(10) 0.0345(5) Uani 1 1 d . . . . .
C2 C 0.28890(15) 0.67989(18) 0.55086(9) 0.0307(4) Uani 1 1 d . . . . .
C3 C 0.36558(16) 0.70497(18) 0.60024(10) 0.0327(5) Uani 1 1 d . . . . .
C4 C 0.11621(16) 0.68882(19) 0.40770(10) 0.0363(5) Uani 1 1 d . . . . .
C5 C 0.03283(17) 0.74199(19) 0.40084(11) 0.0385(5) Uani 1 1 d . . . . .
C6 C -0.02551(18) 0.7525(2) 0.34281(12) 0.0443(6) Uani 1 1 d . . . . .
H6 H -0.083434 0.788326 0.335220 0.053 Uiso 1 1 calc R U . . .
C7 C 0.00072(19) 0.7113(2) 0.29691(11) 0.0464(6) Uani 1 1 d . . . . .
H7 H -0.040051 0.718076 0.258158 0.056 Uiso 1 1 calc R U . . .
C8 C 0.08421(19) 0.6608(2) 0.30606(11) 0.0464(6) Uani 1 1 d . . . . .
H8 H 0.100602 0.633522 0.273598 0.056 Uiso 1 1 calc R U . . .
C9 C 0.14597(17) 0.6486(2) 0.36263(10) 0.0427(6) Uani 1 1 d . . . . .
C10 C 0.00415(18) 0.7848(2) 0.45175(12) 0.0443(6) Uani 1 1 d . . . . .
H10 H 0.061902 0.798624 0.484823 0.053 Uiso 1 1 calc R U . . .
C11 C -0.0494(3) 0.8914(3) 0.43786(18) 0.0807(11) Uani 1 1 d . . . . .
H11A H -0.012804 0.944606 0.424204 0.121 Uiso 1 1 calc R U . . .
H11B H -0.061299 0.918626 0.473201 0.121 Uiso 1 1 calc R U . . .
H11C H -0.108486 0.879222 0.407282 0.121 Uiso 1 1 calc R U . . .
C12 C -0.0534(2) 0.7028(3) 0.47268(14) 0.0617(8) Uani 1 1 d . . . . .
H12A H -0.065337 0.730179 0.507971 0.093 Uiso 1 1 calc R U . . .
H12B H -0.019554 0.634197 0.481581 0.093 Uiso 1 1 calc R U . . .
H12C H -0.112422 0.691155 0.441972 0.093 Uiso 1 1 calc R U . . .
C13 C 0.2378(2) 0.5932(3) 0.37107(12) 0.0627(9) Uani 1 1 d . . . . .
H13 H 0.271154 0.591288 0.414010 0.075 Uiso 1 1 calc R U . . .
C14 C 0.2974(3) 0.6601(5) 0.34167(16) 0.1034(17) Uani 1 1 d . . . . .
H14A H 0.260805 0.676944 0.301327 0.155 Uiso 1 1 calc R U . . .
H14B H 0.352198 0.618159 0.341602 0.155 Uiso 1 1 calc R U . . .
H14C H 0.316849 0.727490 0.363454 0.155 Uiso 1 1 calc R U . . .
C15 C 0.2232(3) 0.4769(4) 0.34961(19) 0.1010(16) Uani 1 1 d . . . . .
H15A H 0.185936 0.475942 0.308282 0.152 Uiso 1 1 calc R U . . .
H15B H 0.190807 0.436720 0.372644 0.152 Uiso 1 1 calc R U . . .
H15C H 0.283382 0.442949 0.354055 0.152 Uiso 1 1 calc R U . . .
C16 C 0.23977(15) 0.50812(17) 0.58988(9) 0.0303(4) Uani 1 1 d . . . . .
C17 C 0.19063(16) 0.51593(18) 0.63016(10) 0.0329(5) Uani 1 1 d . . . . .
C18 C 0.20461(18) 0.4334(2) 0.67148(10) 0.0394(5) Uani 1 1 d . . . . .
H18 H 0.172513 0.435363 0.699768 0.047 Uiso 1 1 calc R U . . .
C19 C 0.26417(18) 0.3492(2) 0.67195(11) 0.0428(6) Uani 1 1 d . . . . .
H19 H 0.273423 0.294438 0.700919 0.051 Uiso 1 1 calc R U . . .
C20 C 0.31064(18) 0.3434(2) 0.63085(12) 0.0441(6) Uani 1 1 d . . . . .
H20 H 0.350848 0.284108 0.631590 0.053 Uiso 1 1 calc R U . . .
C21 C 0.29945(17) 0.4232(2) 0.58826(11) 0.0395(5) Uani 1 1 d . . . . .
C22 C 0.12328(19) 0.6062(2) 0.63012(12) 0.0431(6) Uani 1 1 d . . . . .
H22 H 0.126001 0.660721 0.599940 0.052 Uiso 1 1 calc R U . . .
C23 C 0.1527(3) 0.6614(3) 0.69042(16) 0.0853(13) Uani 1 1 d . . . . .
H23A H 0.109055 0.719775 0.690758 0.128 Uiso 1 1 calc R U . . .
H23B H 0.215083 0.691520 0.698289 0.128 Uiso 1 1 calc R U . . .
H23C H 0.152530 0.608163 0.720619 0.128 Uiso 1 1 calc R U . . .
C24 C 0.0254(2) 0.5640(3) 0.61540(19) 0.0709(10) Uani 1 1 d . . . . .
H24A H 0.022402 0.508050 0.643640 0.106 Uiso 1 1 calc R U . . .
H24B H 0.006714 0.533125 0.575929 0.106 Uiso 1 1 calc R U . . .
H24C H -0.016373 0.623581 0.617063 0.106 Uiso 1 1 calc R U . . .
C25 C 0.3465(2) 0.4134(2) 0.54119(14) 0.0531(7) Uani 1 1 d . . . . .
H25 H 0.336750 0.483159 0.519011 0.064 Uiso 1 1 calc R U . . .
C26 C 0.4504(2) 0.3955(4) 0.56614(19) 0.0833(12) Uani 1 1 d . . . . .
H26A H 0.462242 0.324352 0.584956 0.125 Uiso 1 1 calc R U . . .
H26B H 0.477425 0.451881 0.595052 0.125 Uiso 1 1 calc R U . . .
H26C H 0.478538 0.398826 0.534504 0.125 Uiso 1 1 calc R U . . .
C27 C 0.3007(3) 0.3240(4) 0.49825(17) 0.0900(13) Uani 1 1 d . . . . .
H27A H 0.310476 0.254186 0.518564 0.135 Uiso 1 1 calc R U . . .
H27B H 0.328195 0.322057 0.466273 0.135 Uiso 1 1 calc R U . . .
H27C H 0.234148 0.338375 0.482327 0.135 Uiso 1 1 calc R U . . .
C28 C 0.29246(18) 0.8211(2) 0.47237(10) 0.0411(6) Uani 1 1 d . . . . .
C29 C 0.2398(2) 0.9045(2) 0.44100(13) 0.0588(8) Uani 1 1 d . . . . .
H29 H 0.174670 0.905690 0.434056 0.071 Uiso 1 1 calc R U . . .
C30 C 0.2829(3) 0.9871(3) 0.41953(15) 0.0749(11) Uani 1 1 d . . . . .
H30 H 0.247363 1.045866 0.398779 0.090 Uiso 1 1 calc R U . . .
C31 C 0.3770(3) 0.9836(3) 0.42834(14) 0.0705(10) Uani 1 1 d . . . . .
H31 H 0.405699 1.039141 0.412655 0.085 Uiso 1 1 calc R U . . .
C32 C 0.4294(2) 0.9011(3) 0.45940(13) 0.0596(8) Uani 1 1 d . . . . .
H32 H 0.494398 0.900023 0.465619 0.072 Uiso 1 1 calc R U . . .
C33 C 0.38818(19) 0.8188(2) 0.48193(11) 0.0453(6) Uani 1 1 d . . . . .
H33 H 0.424639 0.761513 0.503641 0.054 Uiso 1 1 calc R U . . .
C34 C 0.2434(2) 0.8870(3) 0.6376(2) 0.0739(11) Uani 1 1 d . . . . .
H34A H 0.235100 0.849198 0.600464 0.111 Uiso 1 1 calc R U . . .
H34B H 0.197846 0.945603 0.631682 0.111 Uiso 1 1 calc R U . . .
H34C H 0.234510 0.836009 0.666616 0.111 Uiso 1 1 calc R U . . .
C35 C 0.3864(3) 1.0171(3) 0.60273(15) 0.0664(9) Uani 1 1 d . . . . .
H35A H 0.442779 1.060594 0.617891 0.100 Uiso 1 1 calc R U . . .
H35B H 0.334163 1.064621 0.583572 0.100 Uiso 1 1 calc R U . . .
H35C H 0.395174 0.964518 0.574351 0.100 Uiso 1 1 calc R U . . .
C36 C 0.3540(2) 1.0503(2) 0.71777(16) 0.0626(8) Uani 1 1 d . . . . .
H36A H 0.339278 1.016026 0.750613 0.094 Uiso 1 1 calc R U . . .
H36B H 0.305085 1.102070 0.698635 0.094 Uiso 1 1 calc R U . . .
H36C H 0.413338 1.088446 0.732249 0.094 Uiso 1 1 calc R U . . .
C37 C 0.6069(3) 1.0086(4) 0.73453(17) 0.0806(12) Uani 1 1 d . . . . .
H37A H 0.627916 0.991998 0.700764 0.121 Uiso 1 1 calc R U . . .
H37B H 0.660314 1.028228 0.767964 0.121 Uiso 1 1 calc R U . . .
H37C H 0.563161 1.069219 0.724908 0.121 Uiso 1 1 calc R U . . .
C38 C 0.5187(2) 0.9187(3) 0.82163(14) 0.0681(9) Uani 1 1 d . . . . .
H38A H 0.517935 0.997250 0.826994 0.102 Uiso 1 1 calc R U . . .
H38B H 0.565109 0.886107 0.855270 0.102 Uiso 1 1 calc R U . . .
H38C H 0.457496 0.888840 0.818393 0.102 Uiso 1 1 calc R U . . .
C39 C 0.6327(3) 0.7756(4) 0.77209(19) 0.0910(14) Uani 1 1 d . . . . .
H39A H 0.603593 0.712250 0.783690 0.136 Uiso 1 1 calc R U . . .
H39B H 0.686745 0.797438 0.804530 0.136 Uiso 1 1 calc R U . . .
H39C H 0.652272 0.757440 0.737971 0.136 Uiso 1 1 calc R U . . .


_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 Cl1 2.2390(7) . ?
V1 Cl2 2.2395(7) . ?
V1 N4 1.888(2) . ?
V1 C3 1.705(2) . ?
Si1 N4 1.743(2) . ?
Si1 C34 1.857(3) . ?
Si1 C35 1.855(3) . ?
Si1 C36 1.869(3) . ?
Si2 N4 1.766(2) . ?
Si2 C37 1.859(4) . ?
Si2 C38 1.869(3) . ?
Si2 C39 1.843(4) . ?
N1 N2 1.332(3) . ?
N1 C1 1.358(3) . ?
N1 C4 1.456(3) . ?
N2 N3 1.328(2) . ?
N3 C2 1.377(3) . ?
N3 C16 1.446(3) . ?
C1 C2 1.399(3) . ?
C1 C28 1.464(3) . ?
C2 C3 1.417(3) . ?
C4 C5 1.389(3) . ?
C4 C9 1.387(4) . ?
C5 C6 1.409(3) . ?
C5 C10 1.514(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.380(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.367(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.402(3) . ?
C9 C13 1.509(4) . ?
C10 H10 1.0000 . ?
C10 C11 1.530(4) . ?
C10 C12 1.520(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.546(5) . ?
C13 C15 1.520(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.394(3) . ?
C16 C21 1.394(3) . ?
C17 C18 1.393(3) . ?
C17 C22 1.512(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.376(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.380(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.394(3) . ?
C21 C25 1.516(3) . ?
C22 H22 1.0000 . ?
C22 C23 1.538(4) . ?
C22 C24 1.508(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 1.0000 . ?
C25 C26 1.520(5) . ?
C25 C27 1.525(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.378(4) . ?
C28 C33 1.399(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.394(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.377(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.365(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.388(4) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?

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
Cl1 V1 Cl2 112.38(3) . . ?
N4 V1 Cl1 111.03(7) . . ?
N4 V1 Cl2 117.77(7) . . ?
C3 V1 Cl1 103.35(8) . . ?
C3 V1 Cl2 104.22(8) . . ?
C3 V1 N4 106.62(10) . . ?
N4 Si1 C34 115.49(13) . . ?
N4 Si1 C35 110.01(14) . . ?
N4 Si1 C36 111.76(14) . . ?
C34 Si1 C36 103.95(16) . . ?
C35 Si1 C34 108.78(19) . . ?
C35 Si1 C36 106.33(16) . . ?
N4 Si2 C37 110.90(14) . . ?
N4 Si2 C38 112.11(13) . . ?
N4 Si2 C39 110.85(14) . . ?
C37 Si2 C38 108.17(17) . . ?
C39 Si2 C37 108.6(2) . . ?
C39 Si2 C38 106.0(2) . . ?
N2 N1 C1 113.26(18) . . ?
N2 N1 C4 118.06(18) . . ?
C1 N1 C4 128.61(19) . . ?
N3 N2 N1 103.62(17) . . ?
N2 N3 C2 113.82(17) . . ?
N2 N3 C16 119.26(17) . . ?
C2 N3 C16 126.68(18) . . ?
Si1 N4 V1 122.89(11) . . ?
Si1 N4 Si2 121.54(12) . . ?
Si2 N4 V1 113.78(11) . . ?
N1 C1 C2 105.71(19) . . ?
N1 C1 C28 125.1(2) . . ?
C2 C1 C28 128.8(2) . . ?
N3 C2 C1 103.58(19) . . ?
N3 C2 C3 124.8(2) . . ?
C1 C2 C3 131.6(2) . . ?
C2 C3 V1 172.95(19) . . ?
C5 C4 N1 117.5(2) . . ?
C9 C4 N1 117.1(2) . . ?
C9 C4 C5 125.4(2) . . ?
C4 C5 C6 115.7(2) . . ?
C4 C5 C10 123.1(2) . . ?
C6 C5 C10 121.2(2) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.3 . . ?
C8 C7 C6 121.3(2) . . ?
C8 C7 H7 119.3 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C8 116.0(2) . . ?
C4 C9 C13 124.5(2) . . ?
C8 C9 C13 119.6(2) . . ?
C5 C10 H10 107.6 . . ?
C5 C10 C11 112.9(2) . . ?
C5 C10 C12 111.8(2) . . ?
C11 C10 H10 107.6 . . ?
C12 C10 H10 107.6 . . ?
C12 C10 C11 109.0(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C13 H13 107.6 . . ?
C9 C13 C14 109.9(3) . . ?
C9 C13 C15 110.6(3) . . ?
C14 C13 H13 107.6 . . ?
C15 C13 H13 107.6 . . ?
C15 C13 C14 113.3(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N3 118.42(19) . . ?
C21 C16 N3 117.42(19) . . ?
C21 C16 C17 124.2(2) . . ?
C16 C17 C22 123.7(2) . . ?
C18 C17 C16 116.6(2) . . ?
C18 C17 C22 119.7(2) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 121.0(2) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.8(2) . . ?
C20 C19 H19 119.6 . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 121.0(2) . . ?
C21 C20 H20 119.5 . . ?
C16 C21 C25 122.6(2) . . ?
C20 C21 C16 116.5(2) . . ?
C20 C21 C25 120.8(2) . . ?
C17 C22 H22 108.6 . . ?
C17 C22 C23 109.1(3) . . ?
C23 C22 H22 108.6 . . ?
C24 C22 C17 111.2(2) . . ?
C24 C22 H22 108.6 . . ?
C24 C22 C23 110.7(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25 107.6 . . ?
C21 C25 C26 112.7(3) . . ?
C21 C25 C27 110.0(2) . . ?
C26 C25 H25 107.6 . . ?
C26 C25 C27 111.3(3) . . ?
C27 C25 H25 107.6 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C1 123.0(2) . . ?
C29 C28 C33 120.2(2) . . ?
C33 C28 C1 116.8(2) . . ?
C28 C29 H29 120.3 . . ?
C28 C29 C30 119.4(3) . . ?
C30 C29 H29 120.3 . . ?
C29 C30 H30 119.9 . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 119.7 . . ?
C32 C31 C30 120.6(3) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 119.9 . . ?
C31 C32 C33 120.2(3) . . ?
C33 C32 H32 119.9 . . ?
C28 C33 H33 120.3 . . ?
C32 C33 C28 119.4(3) . . ?
C32 C33 H33 120.3 . . ?
Si1 C34 H34A 109.5 . . ?
Si1 C34 H34B 109.5 . . ?
Si1 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
Si1 C35 H35A 109.5 . . ?
Si1 C35 H35B 109.5 . . ?
Si1 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Si2 C37 H37A 109.5 . . ?
Si2 C37 H37B 109.5 . . ?
Si2 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Si2 C38 H38A 109.5 . . ?
Si2 C38 H38B 109.5 . . ?
Si2 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
Si2 C39 H39A 109.5 . . ?
Si2 C39 H39B 109.5 . . ?
Si2 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

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
Cl1 V1 N4 Si1 100.48(12) . . . . ?
Cl1 V1 N4 Si2 -64.48(12) . . . . ?
Cl2 V1 N4 Si1 -127.96(11) . . . . ?
Cl2 V1 N4 Si2 67.08(12) . . . . ?
N1 N2 N3 C2 -0.1(2) . . . . ?
N1 N2 N3 C16 -174.90(18) . . . . ?
N1 C1 C2 N3 0.4(2) . . . . ?
N1 C1 C2 C3 -178.4(2) . . . . ?
N1 C1 C28 C29 48.1(4) . . . . ?
N1 C1 C28 C33 -131.5(3) . . . . ?
N1 C4 C5 C6 -178.0(2) . . . . ?
N1 C4 C5 C10 0.9(3) . . . . ?
N1 C4 C9 C8 177.4(2) . . . . ?
N1 C4 C9 C13 -1.9(4) . . . . ?
N2 N1 C1 C2 -0.5(3) . . . . ?
N2 N1 C1 C28 172.8(2) . . . . ?
N2 N1 C4 C5 83.7(3) . . . . ?
N2 N1 C4 C9 -95.8(3) . . . . ?
N2 N3 C2 C1 -0.1(2) . . . . ?
N2 N3 C2 C3 178.7(2) . . . . ?
N2 N3 C16 C17 -88.0(3) . . . . ?
N2 N3 C16 C21 92.8(2) . . . . ?
N3 C16 C17 C18 -177.98(19) . . . . ?
N3 C16 C17 C22 3.3(3) . . . . ?
N3 C16 C21 C20 177.8(2) . . . . ?
N3 C16 C21 C25 -5.3(3) . . . . ?
C1 N1 N2 N3 0.4(2) . . . . ?
C1 N1 C4 C5 -99.5(3) . . . . ?
C1 N1 C4 C9 81.0(3) . . . . ?
C1 C28 C29 C30 179.7(3) . . . . ?
C1 C28 C33 C32 179.4(2) . . . . ?
C2 N3 C16 C17 98.0(3) . . . . ?
C2 N3 C16 C21 -81.2(3) . . . . ?
C2 C1 C28 C29 -140.2(3) . . . . ?
C2 C1 C28 C33 40.2(4) . . . . ?
C3 V1 N4 Si1 -11.41(16) . . . . ?
C3 V1 N4 Si2 -176.37(12) . . . . ?
C4 N1 N2 N3 177.65(19) . . . . ?
C4 N1 C1 C2 -177.4(2) . . . . ?
C4 N1 C1 C28 -4.1(4) . . . . ?
C4 C5 C6 C7 0.2(4) . . . . ?
C4 C5 C10 C11 143.9(3) . . . . ?
C4 C5 C10 C12 -92.7(3) . . . . ?
C4 C9 C13 C14 -116.7(3) . . . . ?
C4 C9 C13 C15 117.5(3) . . . . ?
C5 C4 C9 C8 -2.1(4) . . . . ?
C5 C4 C9 C13 178.6(3) . . . . ?
C5 C6 C7 C8 -1.1(4) . . . . ?
C6 C5 C10 C11 -37.2(4) . . . . ?
C6 C5 C10 C12 86.1(3) . . . . ?
C6 C7 C8 C9 0.4(4) . . . . ?
C7 C8 C9 C4 1.1(4) . . . . ?
C7 C8 C9 C13 -179.6(3) . . . . ?
C8 C9 C13 C14 64.0(4) . . . . ?
C8 C9 C13 C15 -61.8(4) . . . . ?
C9 C4 C5 C6 1.4(4) . . . . ?
C9 C4 C5 C10 -179.7(2) . . . . ?
C10 C5 C6 C7 -178.7(2) . . . . ?
C16 N3 C2 C1 174.1(2) . . . . ?
C16 N3 C2 C3 -7.0(3) . . . . ?
C16 C17 C18 C19 0.1(3) . . . . ?
C16 C17 C22 C23 -124.1(3) . . . . ?
C16 C17 C22 C24 113.5(3) . . . . ?
C16 C21 C25 C26 129.5(3) . . . . ?
C16 C21 C25 C27 -105.8(3) . . . . ?
C17 C16 C21 C20 -1.3(4) . . . . ?
C17 C16 C21 C25 175.6(2) . . . . ?
C17 C18 C19 C20 -1.0(4) . . . . ?
C18 C17 C22 C23 57.2(3) . . . . ?
C18 C17 C22 C24 -65.1(3) . . . . ?
C18 C19 C20 C21 0.8(4) . . . . ?
C19 C20 C21 C16 0.3(4) . . . . ?
C19 C20 C21 C25 -176.6(3) . . . . ?
C20 C21 C25 C26 -53.8(4) . . . . ?
C20 C21 C25 C27 70.9(4) . . . . ?
C21 C16 C17 C18 1.1(3) . . . . ?
C21 C16 C17 C22 -177.6(2) . . . . ?
C22 C17 C18 C19 178.8(2) . . . . ?
C28 C1 C2 N3 -172.6(2) . . . . ?
C28 C1 C2 C3 8.7(4) . . . . ?
C28 C29 C30 C31 1.7(5) . . . . ?
C29 C28 C33 C32 -0.2(4) . . . . ?
C29 C30 C31 C32 -1.7(6) . . . . ?
C30 C31 C32 C33 0.8(5) . . . . ?
C31 C32 C33 C28 0.2(4) . . . . ?
C33 C28 C29 C30 -0.8(5) . . . . ?
C34 Si1 N4 V1 50.2(2) . . . . ?
C34 Si1 N4 Si2 -146.01(18) . . . . ?
C35 Si1 N4 V1 -73.41(18) . . . . ?
C35 Si1 N4 Si2 90.41(18) . . . . ?
C36 Si1 N4 V1 168.71(15) . . . . ?
C36 Si1 N4 Si2 -27.47(19) . . . . ?
C37 Si2 N4 V1 110.34(18) . . . . ?
C37 Si2 N4 Si1 -54.8(2) . . . . ?
C38 Si2 N4 V1 -128.64(16) . . . . ?
C38 Si2 N4 Si1 66.18(19) . . . . ?
C39 Si2 N4 V1 -10.4(2) . . . . ?
C39 Si2 N4 Si1 -175.6(2) . . . . ?

_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.825
_oxdiff_exptl_absorpt_empirical_full_min 0.564
####################################################################### 
# 
# 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_bk142
_database_code_depnum_ccdc_archive 'CCDC 2114605'
loop_
_audit_author_name
_audit_author_address
'Farzaneh Fadaei Tirani'
;Institute of Chemical Sciences and Engineering, Ecole Polytechnique Federale de Lausanne
Switzerland
;
_audit_update_record             
;
2021-10-08 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_audit_creation_date             2021-10-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_shelx_SHELXL_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H78 Cl4 N6 V2, 2(C6 H6)'
_chemical_formula_sum            'C78 H90 Cl4 N6 V2'
_chemical_formula_weight         1355.23
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C78 H90 Cl4 N6 V2'
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'
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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.2710(5)
_cell_length_b                   23.7721(4)
_cell_length_c                   13.68963(17)
_cell_angle_alpha                90
_cell_angle_beta                 98.8968(15)
_cell_angle_gamma                90
_cell_volume                     7482.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17787
_cell_measurement_temperature    229.99(10)
_cell_measurement_theta_max      75.8710
_cell_measurement_theta_min      3.8260
_shelx_estimated_absorpt_T_max   0.865
_shelx_estimated_absorpt_T_min   0.507
_exptl_absorpt_coefficient_mu    3.746
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2856
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0187
1 0 0 0.0247
1 1 1 0.0812
1 2 0 0.0901
0 -1 1 0.0674
0 1 -1 0.0701
1 -2 -1 0.1080
-1 2 1 0.0848
-1 1 0 0.0756
1 -1 0 0.0734
-1 2 2 0.0802
0 -1 -2 0.1070
1 -2 -2 0.1072
-2 1 1 0.0589
-2 0 1 0.0367
-2 -1 1 0.0415
2 1 -1 0.0457
0 -1 0 0.0903
0 1 0 0.0940

_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
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
-1.0000 0.0000 -0.0000 0.0073 0.0610 -0.0267
1.0000 -0.0000 0.0000 -0.0073 -0.0610 0.0267
1.0000 1.0000 1.0000 0.0422 -0.0342 0.1451
1.0000 2.0000 0.0000 0.1207 -0.0677 0.0457
0.0000 -1.0000 1.0000 -0.0785 0.0334 0.0994
-0.0000 1.0000 -1.0000 0.0785 -0.0334 -0.0994
1.0000 -2.0000 -1.0000 -0.1209 -0.0844 -0.1012
-1.0000 2.0000 1.0000 0.1209 0.0844 0.1012
-1.0000 1.0000 0.0000 0.0713 0.0577 -0.0172
1.0000 -1.0000 -0.0000 -0.0713 -0.0577 0.0172
-1.0000 2.0000 2.0000 0.1065 0.1145 0.2101
-0.0000 -1.0000 -2.0000 -0.0351 -0.0569 -0.2273
1.0000 -2.0000 -2.0000 -0.1065 -0.1145 -0.2101
-2.0000 1.0000 1.0000 0.0642 0.1488 0.0650
-2.0000 0.0000 1.0000 0.0002 0.1521 0.0555
-2.0000 -1.0000 1.0000 -0.0638 0.1554 0.0460
2.0000 1.0000 -1.0000 0.0638 -0.1554 -0.0460
0.0000 -1.0000 -0.0000 -0.0640 0.0033 -0.0095
-0.0000 1.0000 0.0000 0.0640 -0.0033 0.0095

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            45562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.061
_diffrn_reflns_theta_min         3.719
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      229.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -95.00 -52.00   1.00    4.00    --  -40.91-162.00 -17.00   43
  2  ω    -93.00 -68.00   1.00    4.00    --  -40.91 162.00  11.00   25
  3  ω    -66.00 -41.00   1.00    4.00    --  -40.91 117.00-139.00   25
  4  ω     32.00  57.00   1.00    4.00    --   40.91-117.00 133.00   25
  5  ω     70.00  95.00   1.00    4.00    --   40.91-162.00 -17.00   25
  6  ω     92.00 117.00   1.00   16.00    --  112.00-162.00 -17.00   25
  7  ω     54.00  80.00   1.00   16.00    --  112.00-117.00 133.00   26
  8  ω    115.00 140.00   1.00   16.00    --  112.00 117.00-139.00   25
  9  ω     91.00 116.00   1.00   16.00    --  112.00 162.00  11.00   25
 10  ω   -113.00 -17.00   1.00    4.00    --  -40.91 -57.00-120.00   96
 11  ω    -86.00  -6.00   1.00    4.00    --  -40.91 125.00 120.00   80
 12  ω   -104.00 -14.00   1.00    4.00    --  -40.91 -57.00 -60.00   90
 13  ω   -105.00 -16.00   1.00    4.00    --  -40.91 -38.00 -30.00   89
 14  ω     28.00  96.00   1.00    4.00    --   40.91-125.00 150.00   68
 15  ω    142.00 168.00   1.00   16.00    --  112.00  61.00  60.00   26
 16  ω    107.00 175.00   1.00   16.00    --  112.00 111.00-150.00   68
 17  ω    103.00 176.00   1.00   16.00    --  112.00  77.00 -90.00   73
 18  ω     57.00  84.00   1.00   16.00    --  112.00 -94.00 150.00   27
 19  ω     70.00 109.00   1.00   16.00    --  112.00-111.00-150.00   39
 20  ω     87.00 154.00   1.00   16.00    --  112.00  45.00-180.00   67
 21  ω    107.00 157.00   1.00   16.00    --  112.00  77.00-150.00   50
 22  ω     54.00 109.00   1.00   16.00    --  112.00-111.00 -30.00   55
 23  ω    108.00 139.00   1.00   16.00    --  112.00 111.00 120.00   31
 24  ω     54.00 138.00   1.00   16.00    --  112.00 -45.00 120.00   84
 25  ω    108.00 165.00   1.00   16.00    --  112.00 111.00-180.00   57
 26  ω     42.00 109.00   1.00   16.00    --  112.00-111.00 150.00   67
 27  ω     77.00 104.00   1.00   16.00    --  112.00 -94.00  30.00   27
 28  ω     59.00 108.00   1.00   16.00    --  112.00-111.00  30.00   49
 29  ω     43.00 109.00   1.00   16.00    --  112.00-111.00 -60.00   66
 30  ω    119.00 150.00   1.00   16.00    --  112.00 111.00  90.00   31
 31  ω     36.00  84.00   1.00   16.00    --  112.00-111.00  60.00   48
 32  ω    104.00 165.00   1.00   16.00    --  112.00  77.00-180.00   61
 33  ω     72.00 109.00   1.00   16.00    --  112.00-111.00-120.00   37
 34  ω     46.00 104.00   1.00   16.00    --  112.00-111.00 -90.00   58
 35  ω    104.00 133.00   1.00   16.00    --  112.00 111.00  60.00   29
 36  ω     45.00  72.00   1.00   16.00    --  112.00 -77.00 -30.00   27
 37  ω    103.00 129.00   1.00   16.00    --  112.00  77.00-120.00   26
 38  ω    142.00 167.00   1.00   16.00    --  112.00  77.00-120.00   25
 39  ω     71.00 109.00   1.00   16.00    --  112.00-111.00-180.00   38
 40  ω     30.00  70.00   1.00   16.00    --  112.00 -94.00  30.00   40
 41  ω     31.00 102.00   1.00   16.00    --  112.00 -94.00 -30.00   71
 42  ω    140.00 177.00   1.00   16.00    --  112.00  77.00 120.00   37
 43  ω     53.00 109.00   1.00   16.00    --  112.00-111.00  90.00   56
 44  ω     49.00  75.00   1.00   16.00    --  112.00 -94.00 -60.00   26
 45  ω    103.00 135.00   1.00   16.00    --  112.00  77.00 120.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073294000
_diffrn_orient_matrix_UB_12      0.0640178000
_diffrn_orient_matrix_UB_13      -0.0144526000
_diffrn_orient_matrix_UB_21      -0.0609982000
_diffrn_orient_matrix_UB_22      -0.0033469000
_diffrn_orient_matrix_UB_23      0.0301027000
_diffrn_orient_matrix_UB_31      0.0267250000
_diffrn_orient_matrix_UB_32      0.0094857000
_diffrn_orient_matrix_UB_33      0.1089227000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                6691
_reflns_number_total             7784
_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 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7784
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.076
_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)+(0.0700P)²+1.3624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1153
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37-C36_$1 = C36-C35 = C34-C35_$1 = C34-C35 = C36-C35 = C37-C36
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C42(0.5) H42(0.5) C41(0.5) H41(0.5) C40(0.5) H40(0.5) C39(0.5)
 H39(0.5) C38(0.5) H38(0.5) C43(0.5) H43(0.5)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C24(H24), C25(H25), C26(H26), C34(H34), C35(H35), C36(H36), C37(H37), C42(H42),
  C41(H41), C40(H40), C39(H39), C38(H38), C43(H43)
5.c Fitted hexagon refined as free rotating group:
 C42(C41,C40,C39,C38,C43)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.51174(2) 0.73037(2) 0.84114(2) 0.03828(9) Uani 1 1 d . . . . .
Cl1 Cl 0.52553(2) 0.64819(2) 0.92048(3) 0.05679(13) Uani 1 1 d . . . . .
Cl2 Cl 0.51712(2) 0.80496(2) 0.94087(3) 0.05991(13) Uani 1 1 d . . . . .
N1 N 0.65490(6) 0.72433(5) 0.68466(9) 0.0359(3) Uani 1 1 d . . . . .
N2 N 0.70744(6) 0.74662(6) 0.68559(9) 0.0386(3) Uani 1 1 d . . . . .
N3 N 0.70491(6) 0.79449(6) 0.73456(8) 0.0367(3) Uani 1 1 d . . . . .
C1 C 0.61828(7) 0.75622(6) 0.73323(10) 0.0355(3) Uani 1 1 d . . . . .
C2 C 0.65286(7) 0.80310(7) 0.76567(10) 0.0368(3) Uani 1 1 d . . . . .
C3 C 0.56028(7) 0.74160(7) 0.74286(11) 0.0383(3) Uani 1 1 d . . . . .
C4 C 0.63806(8) 0.85415(7) 0.81692(11) 0.0421(3) Uani 1 1 d . . . . .
C5 C 0.67800(10) 0.87901(9) 0.89110(14) 0.0563(5) Uani 1 1 d . . . . .
H5 H 0.714566 0.862302 0.910801 0.068 Uiso 1 1 calc R U . . .
C6 C 0.66367(12) 0.92820(10) 0.93546(17) 0.0762(7) Uani 1 1 d . . . . .
H6 H 0.690815 0.945183 0.984635 0.091 Uiso 1 1 calc R U . . .
C7 C 0.60993(13) 0.95246(11) 0.90809(19) 0.0815(8) Uani 1 1 d . . . . .
H7 H 0.600441 0.985877 0.938663 0.098 Uiso 1 1 calc R U . . .
C8 C 0.56991(11) 0.92781(10) 0.83582(19) 0.0724(7) Uani 1 1 d . . . . .
H8 H 0.533027 0.944192 0.817838 0.087 Uiso 1 1 calc R U . . .
C9 C 0.58404(9) 0.87895(8) 0.78973(14) 0.0531(4) Uani 1 1 d . . . . .
H9 H 0.556904 0.862561 0.739847 0.064 Uiso 1 1 calc R U . . .
C10 C 0.64261(7) 0.67114(7) 0.63350(11) 0.0401(3) Uani 1 1 d . . . . .
C11 C 0.65573(9) 0.62165(8) 0.68691(13) 0.0507(4) Uani 1 1 d . . . . .
C12 C 0.64483(11) 0.57127(9) 0.63493(16) 0.0630(5) Uani 1 1 d . . . . .
H12 H 0.652285 0.536856 0.668305 0.076 Uiso 1 1 calc R U . . .
C13 C 0.62322(11) 0.57133(9) 0.53511(16) 0.0634(5) Uani 1 1 d . . . . .
H13 H 0.616402 0.536985 0.501286 0.076 Uiso 1 1 calc R U . . .
C14 C 0.61162(9) 0.62089(9) 0.48485(13) 0.0558(5) Uani 1 1 d . . . . .
H14 H 0.597323 0.619929 0.416782 0.067 Uiso 1 1 calc R U . . .
C15 C 0.62059(8) 0.67290(8) 0.53262(11) 0.0448(4) Uani 1 1 d . . . . .
C16 C 0.68400(12) 0.62204(9) 0.79442(15) 0.0669(6) Uani 1 1 d . . . . .
H16 H 0.677363 0.659590 0.821906 0.080 Uiso 1 1 calc R U . . .
C17 C 0.74916(15) 0.61430(16) 0.7997(2) 0.1011(11) Uani 1 1 d . . . . .
H17A H 0.756996 0.577199 0.775373 0.152 Uiso 1 1 calc R U . . .
H17B H 0.767952 0.618075 0.867760 0.152 Uiso 1 1 calc R U . . .
H17C H 0.764170 0.642668 0.759415 0.152 Uiso 1 1 calc R U . . .
C18 C 0.65898(15) 0.57833(11) 0.85732(18) 0.0820(8) Uani 1 1 d . . . . .
H18A H 0.617390 0.584087 0.852857 0.123 Uiso 1 1 calc R U . . .
H18B H 0.677301 0.582066 0.925633 0.123 Uiso 1 1 calc R U . . .
H18C H 0.666296 0.540959 0.833568 0.123 Uiso 1 1 calc R U . . .
C19 C 0.60896(9) 0.72784(8) 0.47654(12) 0.0504(4) Uani 1 1 d . . . . .
H19 H 0.598980 0.756555 0.523545 0.061 Uiso 1 1 calc R U . . .
C20 C 0.55829(11) 0.72445(11) 0.39041(14) 0.0644(6) Uani 1 1 d . . . . .
H20A H 0.549430 0.761822 0.363841 0.097 Uiso 1 1 calc R U . . .
H20B H 0.524332 0.709042 0.413914 0.097 Uiso 1 1 calc R U . . .
H20C H 0.569102 0.700339 0.339042 0.097 Uiso 1 1 calc R U . . .
C21 C 0.66388(11) 0.74725(12) 0.43865(15) 0.0670(6) Uani 1 1 d . . . . .
H21A H 0.674621 0.719765 0.392315 0.100 Uiso 1 1 calc R U . . .
H21B H 0.695243 0.751087 0.493812 0.100 Uiso 1 1 calc R U . . .
H21C H 0.656734 0.783265 0.405692 0.100 Uiso 1 1 calc R U . . .
C22 C 0.75454(7) 0.83233(7) 0.74338(11) 0.0412(3) Uani 1 1 d . . . . .
C23 C 0.75006(9) 0.87916(8) 0.68114(14) 0.0502(4) Uani 1 1 d . . . . .
C24 C 0.79702(10) 0.91612(9) 0.69393(17) 0.0619(5) Uani 1 1 d . . . . .
H24 H 0.795800 0.948267 0.653679 0.074 Uiso 1 1 calc R U . . .
C25 C 0.84501(10) 0.90681(10) 0.76375(18) 0.0638(5) Uani 1 1 d . . . . .
H25 H 0.875784 0.932845 0.771590 0.077 Uiso 1 1 calc R U . . .
C26 C 0.84839(9) 0.85923(9) 0.82282(14) 0.0565(5) Uani 1 1 d . . . . .
H26 H 0.881735 0.853164 0.869892 0.068 Uiso 1 1 calc R U . . .
C27 C 0.80314(8) 0.82020(8) 0.81363(12) 0.0450(4) Uani 1 1 d . . . . .
C28 C 0.69816(10) 0.89122(10) 0.60201(16) 0.0629(5) Uani 1 1 d . . . . .
H28 H 0.669845 0.860164 0.602383 0.075 Uiso 1 1 calc R U . . .
C29 C 0.66830(13) 0.94610(12) 0.6240(2) 0.0881(9) Uani 1 1 d . . . . .
H29A H 0.694269 0.977473 0.618607 0.132 Uiso 1 1 calc R U . . .
H29B H 0.658728 0.944737 0.690468 0.132 Uiso 1 1 calc R U . . .
H29C H 0.632959 0.950883 0.576915 0.132 Uiso 1 1 calc R U . . .
C30 C 0.71724(13) 0.89294(13) 0.49994(18) 0.0824(8) Uani 1 1 d . . . . .
H30A H 0.683249 0.896138 0.449406 0.124 Uiso 1 1 calc R U . . .
H30B H 0.738117 0.858669 0.489594 0.124 Uiso 1 1 calc R U . . .
H30C H 0.742459 0.925097 0.496138 0.124 Uiso 1 1 calc R U . . .
C31 C 0.80860(9) 0.76751(8) 0.87758(12) 0.0502(4) Uani 1 1 d . . . . .
H31 H 0.771564 0.746405 0.863749 0.060 Uiso 1 1 calc R U . . .
C32 C 0.81996(11) 0.78205(11) 0.98833(14) 0.0653(6) Uani 1 1 d . . . . .
H32A H 0.821217 0.747713 1.026872 0.098 Uiso 1 1 calc R U . . .
H32B H 0.788979 0.806035 1.004250 0.098 Uiso 1 1 calc R U . . .
H32C H 0.856847 0.801585 1.003731 0.098 Uiso 1 1 calc R U . . .
C33 C 0.85725(12) 0.72994(11) 0.85179(17) 0.0692(6) Uani 1 1 d . . . . .
H33A H 0.894012 0.749826 0.865590 0.104 Uiso 1 1 calc R U . . .
H33B H 0.849422 0.720229 0.782181 0.104 Uiso 1 1 calc R U . . .
H33C H 0.859252 0.695889 0.891206 0.104 Uiso 1 1 calc R U . . .
C34 C 0.500000 0.41308(15) 0.750000 0.0807(11) Uani 1 2 d DS T P . .
H34 H 0.500000 0.373538 0.750000 0.097 Uiso 1 2 calc R U P . .
C35 C 0.50458(11) 0.44221(12) 0.66389(18) 0.0757(7) Uani 1 1 d D . . . .
H35 H 0.507885 0.422592 0.605401 0.091 Uiso 1 1 calc R U . . .
C36 C 0.50427(13) 0.49937(12) 0.66465(19) 0.0839(8) Uani 1 1 d D . . . .
H36 H 0.507000 0.519385 0.606326 0.101 Uiso 1 1 calc R U . . .
C37 C 0.500000 0.52786(17) 0.750000 0.0986(15) Uani 1 2 d DS T P . .
H37 H 0.500000 0.567401 0.750000 0.118 Uiso 1 2 calc R U P . .
C42 C 0.5213(7) 0.8942(6) 0.1827(13) 0.199(5) Uani 0.5 1 d G U P A -1
H42 H 0.543819 0.888709 0.132110 0.239 Uiso 0.5 1 calc R U P A -1
C41 C 0.4610(7) 0.8962(6) 0.1602(12) 0.198(5) Uani 0.5 1 d G U P A -1
H41 H 0.442758 0.892174 0.094339 0.237 Uiso 0.5 1 calc R U P A -1
C40 C 0.4277(7) 0.9043(6) 0.2350(14) 0.201(5) Uani 0.5 1 d G U P A -1
H40 H 0.386934 0.905685 0.219763 0.241 Uiso 0.5 1 calc R U P A -1
C39 C 0.4547(7) 0.9103(5) 0.3324(13) 0.198(4) Uani 0.5 1 d G U P A -1
H39 H 0.432169 0.915731 0.382958 0.237 Uiso 0.5 1 calc R U P A -1
C38 C 0.5150(7) 0.9082(6) 0.3549(13) 0.200(5) Uani 0.5 1 d G U P A -1
H38 H 0.533229 0.912266 0.420731 0.240 Uiso 0.5 1 calc R U P A -1
C43 C 0.5483(7) 0.9002(6) 0.2801(14) 0.204(5) Uani 0.5 1 d G U P A -1
H43 H 0.589054 0.898755 0.295308 0.245 Uiso 0.5 1 calc R U P A -1


_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 V1 2.4706(5) 2_656 ?
V1 Cl1 2.2341(5) . ?
V1 Cl2 2.2295(5) . ?
V1 C3 1.9045(16) . ?
V1 C3 1.8991(16) 2_656 ?
N1 N2 1.331(2) . ?
N1 C1 1.385(2) . ?
N1 C10 1.4524(19) . ?
N2 N3 1.3268(19) . ?
N3 C2 1.360(2) . ?
N3 C22 1.454(2) . ?
C1 C2 1.406(2) . ?
C1 C3 1.419(2) . ?
C2 C4 1.469(2) . ?
C4 C5 1.397(2) . ?
C4 C9 1.386(3) . ?
C5 H5 0.9400 . ?
C5 C6 1.382(3) . ?
C6 H6 0.9400 . ?
C6 C7 1.376(4) . ?
C7 H7 0.9400 . ?
C7 C8 1.380(3) . ?
C8 H8 0.9400 . ?
C8 C9 1.385(3) . ?
C9 H9 0.9400 . ?
C10 C11 1.394(2) . ?
C10 C15 1.397(2) . ?
C11 C12 1.396(3) . ?
C11 C16 1.516(3) . ?
C12 H12 0.9400 . ?
C12 C13 1.381(3) . ?
C13 H13 0.9400 . ?
C13 C14 1.370(3) . ?
C14 H14 0.9400 . ?
C14 C15 1.399(3) . ?
C15 C19 1.518(3) . ?
C16 H16 0.9900 . ?
C16 C17 1.518(4) . ?
C16 C18 1.522(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 H19 0.9900 . ?
C19 C20 1.535(3) . ?
C19 C21 1.523(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 C23 1.396(2) . ?
C22 C27 1.397(2) . ?
C23 C24 1.392(3) . ?
C23 C28 1.520(3) . ?
C24 H24 0.9400 . ?
C24 C25 1.371(3) . ?
C25 H25 0.9400 . ?
C25 C26 1.386(3) . ?
C26 H26 0.9400 . ?
C26 C27 1.394(3) . ?
C27 C31 1.522(3) . ?
C28 H28 0.9900 . ?
C28 C29 1.530(4) . ?
C28 C30 1.531(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 H30C 0.9700 . ?
C31 H31 0.9900 . ?
C31 C32 1.538(2) . ?
C31 C33 1.526(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C34 H34 0.9400 . ?
C34 C35 1.385(3) . ?
C34 C35 1.385(3) 2_656 ?
C35 H35 0.9400 . ?
C35 C36 1.359(4) . ?
C36 H36 0.9400 . ?
C36 C37 1.367(3) . ?
C37 H37 0.9400 . ?
C42 H42 0.9400 . ?
C42 C41 1.3900 . ?
C42 C43 1.3900 . ?
C41 H41 0.9400 . ?
C41 C40 1.3900 . ?
C40 H40 0.9400 . ?
C40 C39 1.3900 . ?
C39 H39 0.9400 . ?
C39 C38 1.3900 . ?
C38 H38 0.9400 . ?
C38 C43 1.3900 . ?
C43 H43 0.9400 . ?

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
Cl1 V1 V1 118.930(14) . 2_656 ?
Cl2 V1 V1 126.955(15) . 2_656 ?
Cl2 V1 Cl1 114.05(2) . . ?
C3 V1 V1 49.59(5) 2_656 2_656 ?
C3 V1 V1 49.40(5) . 2_656 ?
C3 V1 Cl1 117.66(5) 2_656 . ?
C3 V1 Cl1 114.19(5) . . ?
C3 V1 Cl2 102.69(5) 2_656 . ?
C3 V1 Cl2 109.74(5) . . ?
C3 V1 C3 96.71(7) 2_656 . ?
N2 N1 C1 114.21(13) . . ?
N2 N1 C10 117.60(13) . . ?
C1 N1 C10 128.18(14) . . ?
N3 N2 N1 103.52(13) . . ?
N2 N3 C2 113.48(13) . . ?
N2 N3 C22 118.41(14) . . ?
C2 N3 C22 127.98(14) . . ?
N1 C1 C2 102.76(14) . . ?
N1 C1 C3 125.10(14) . . ?
C2 C1 C3 132.13(15) . . ?
N3 C2 C1 106.01(13) . . ?
N3 C2 C4 124.03(15) . . ?
C1 C2 C4 129.85(16) . . ?
V1 C3 V1 81.01(7) 2_656 . ?
C1 C3 V1 137.81(11) . 2_656 ?
C1 C3 V1 140.92(11) . . ?
C5 C4 C2 121.18(16) . . ?
C9 C4 C2 119.54(14) . . ?
C9 C4 C5 119.27(16) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 119.91(19) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.40(19) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.1(2) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.1(2) . . ?
C9 C8 H8 120.0 . . ?
C4 C9 H9 119.9 . . ?
C8 C9 C4 120.24(18) . . ?
C8 C9 H9 119.9 . . ?
C11 C10 N1 118.10(13) . . ?
C11 C10 C15 124.12(15) . . ?
C15 C10 N1 117.72(15) . . ?
C10 C11 C12 116.67(17) . . ?
C10 C11 C16 122.07(16) . . ?
C12 C11 C16 121.15(18) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.9(2) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 119.6 . . ?
C14 C13 C12 120.74(18) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 H14 119.3 . . ?
C13 C14 C15 121.44(17) . . ?
C15 C14 H14 119.3 . . ?
C10 C15 C14 116.15(17) . . ?
C10 C15 C19 122.35(15) . . ?
C14 C15 C19 121.46(15) . . ?
C11 C16 H16 107.7 . . ?
C11 C16 C17 109.0(2) . . ?
C11 C16 C18 113.5(2) . . ?
C17 C16 H16 107.7 . . ?
C17 C16 C18 110.9(2) . . ?
C18 C16 H16 107.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19 107.8 . . ?
C15 C19 C20 113.51(17) . . ?
C15 C19 C21 109.85(18) . . ?
C20 C19 H19 107.8 . . ?
C21 C19 H19 107.8 . . ?
C21 C19 C20 109.84(16) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N3 117.34(14) . . ?
C23 C22 C27 124.12(16) . . ?
C27 C22 N3 118.54(15) . . ?
C22 C23 C28 124.16(17) . . ?
C24 C23 C22 116.33(17) . . ?
C24 C23 C28 119.50(18) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 C23 121.7(2) . . ?
C25 C24 H24 119.2 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.35(19) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 119.4 . . ?
C25 C26 C27 121.11(18) . . ?
C27 C26 H26 119.4 . . ?
C22 C27 C31 123.54(16) . . ?
C26 C27 C22 116.39(17) . . ?
C26 C27 C31 120.06(16) . . ?
C23 C28 H28 108.2 . . ?
C23 C28 C29 110.8(2) . . ?
C23 C28 C30 110.2(2) . . ?
C29 C28 H28 108.2 . . ?
C29 C28 C30 111.2(2) . . ?
C30 C28 H28 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 H31 108.3 . . ?
C27 C31 C32 111.63(17) . . ?
C27 C31 C33 110.33(17) . . ?
C32 C31 H31 108.3 . . ?
C33 C31 H31 108.3 . . ?
C33 C31 C32 109.83(17) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34 120.0 2_656 . ?
C35 C34 H34 120.0 . . ?
C35 C34 C35 120.0(3) 2_656 . ?
C34 C35 H35 120.3 . . ?
C36 C35 C34 119.5(3) . . ?
C36 C35 H35 120.3 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.2(3) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 C36 120.6(4) . 2_656 ?
C36 C37 H37 119.7 . . ?
C36 C37 H37 119.7 2_656 . ?
C41 C42 H42 120.0 . . ?
C41 C42 C43 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C41 H41 120.0 . . ?
C42 C41 C40 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C40 H40 120.0 . . ?
C39 C40 C41 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C39 H39 120.0 . . ?
C40 C39 C38 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C38 H38 120.0 . . ?
C43 C38 C39 120.0 . . ?
C43 C38 H38 120.0 . . ?
C42 C43 H43 120.0 . . ?
C38 C43 C42 120.0 . . ?
C38 C43 H43 120.0 . . ?

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
N1 N2 N3 C2 0.67(15) . . . . ?
N1 N2 N3 C22 -175.55(12) . . . . ?
N1 C1 C2 N3 -0.28(14) . . . . ?
N1 C1 C2 C4 175.94(14) . . . . ?
N1 C1 C3 V1 -63.8(2) . . . 2_656 ?
N1 C1 C3 V1 124.51(17) . . . . ?
N1 C10 C11 C12 -178.36(19) . . . . ?
N1 C10 C11 C16 -2.1(3) . . . . ?
N1 C10 C15 C14 177.35(16) . . . . ?
N1 C10 C15 C19 -0.5(3) . . . . ?
N2 N1 C1 C2 0.74(15) . . . . ?
N2 N1 C1 C3 -179.83(13) . . . . ?
N2 N1 C10 C11 89.00(19) . . . . ?
N2 N1 C10 C15 -88.39(18) . . . . ?
N2 N3 C2 C1 -0.25(16) . . . . ?
N2 N3 C2 C4 -176.74(13) . . . . ?
N2 N3 C22 C23 101.98(18) . . . . ?
N2 N3 C22 C27 -78.73(18) . . . . ?
N3 C2 C4 C5 -42.5(2) . . . . ?
N3 C2 C4 C9 135.98(18) . . . . ?
N3 C22 C23 C24 177.21(18) . . . . ?
N3 C22 C23 C28 -3.2(3) . . . . ?
N3 C22 C27 C26 -176.78(16) . . . . ?
N3 C22 C27 C31 3.8(3) . . . . ?
C1 N1 N2 N3 -0.88(15) . . . . ?
C1 N1 C10 C11 -91.7(2) . . . . ?
C1 N1 C10 C15 90.9(2) . . . . ?
C1 C2 C4 C5 141.93(18) . . . . ?
C1 C2 C4 C9 -39.6(2) . . . . ?
C2 N3 C22 C23 -73.6(2) . . . . ?
C2 N3 C22 C27 105.67(19) . . . . ?
C2 C1 C3 V1 115.47(18) . . . 2_656 ?
C2 C1 C3 V1 -56.2(3) . . . . ?
C2 C4 C5 C6 177.6(2) . . . . ?
C2 C4 C9 C8 -178.6(2) . . . . ?
C3 C1 C2 N3 -179.65(14) . . . . ?
C3 C1 C2 C4 -3.4(3) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C5 C4 C9 C8 -0.1(3) . . . . ?
C5 C6 C7 C8 -0.1(5) . . . . ?
C6 C7 C8 C9 -0.8(5) . . . . ?
C7 C8 C9 C4 0.9(4) . . . . ?
C9 C4 C5 C6 -0.9(3) . . . . ?
C10 N1 N2 N3 178.55(12) . . . . ?
C10 N1 C1 C2 -178.62(13) . . . . ?
C10 N1 C1 C3 0.8(2) . . . . ?
C10 C11 C12 C13 1.3(3) . . . . ?
C10 C11 C16 C17 -96.5(3) . . . . ?
C10 C11 C16 C18 139.4(2) . . . . ?
C10 C15 C19 C20 -149.11(18) . . . . ?
C10 C15 C19 C21 87.5(2) . . . . ?
C11 C10 C15 C14 0.1(3) . . . . ?
C11 C10 C15 C19 -177.73(18) . . . . ?
C11 C12 C13 C14 -0.4(4) . . . . ?
C12 C11 C16 C17 79.5(3) . . . . ?
C12 C11 C16 C18 -44.6(3) . . . . ?
C12 C13 C14 C15 -0.7(4) . . . . ?
C13 C14 C15 C10 0.8(3) . . . . ?
C13 C14 C15 C19 178.7(2) . . . . ?
C14 C15 C19 C20 33.1(3) . . . . ?
C14 C15 C19 C21 -90.3(2) . . . . ?
C15 C10 C11 C12 -1.1(3) . . . . ?
C15 C10 C11 C16 175.1(2) . . . . ?
C16 C11 C12 C13 -175.0(2) . . . . ?
C22 N3 C2 C1 175.53(13) . . . . ?
C22 N3 C2 C4 -1.0(2) . . . . ?
C22 C23 C24 C25 0.1(3) . . . . ?
C22 C23 C28 C29 117.2(2) . . . . ?
C22 C23 C28 C30 -119.3(2) . . . . ?
C22 C27 C31 C32 -123.4(2) . . . . ?
C22 C27 C31 C33 114.2(2) . . . . ?
C23 C22 C27 C26 2.5(3) . . . . ?
C23 C22 C27 C31 -176.95(18) . . . . ?
C23 C24 C25 C26 1.2(4) . . . . ?
C24 C23 C28 C29 -63.2(3) . . . . ?
C24 C23 C28 C30 60.3(3) . . . . ?
C24 C25 C26 C27 -0.7(4) . . . . ?
C25 C26 C27 C22 -1.0(3) . . . . ?
C25 C26 C27 C31 178.4(2) . . . . ?
C26 C27 C31 C32 57.2(2) . . . . ?
C26 C27 C31 C33 -65.2(2) . . . . ?
C27 C22 C23 C24 -2.0(3) . . . . ?
C27 C22 C23 C28 177.6(2) . . . . ?
C28 C23 C24 C25 -179.5(2) . . . . ?
C34 C35 C36 C37 0.6(4) . . . . ?
C35 C34 C35 C36 -0.30(19) 2_656 . . . ?
C35 C36 C37 C36 -0.30(19) . . . 2_656 ?
C42 C41 C40 C39 0.0 . . . . ?
C41 C42 C43 C38 0.0 . . . . ?
C41 C40 C39 C38 0.0 . . . . ?
C40 C39 C38 C43 0.0 . . . . ?
C39 C38 C43 C42 0.0 . . . . ?
C43 C42 C41 C40 0.0 . . . . ?

_olex2_date_sample_data_collection 2021-10-07
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.664
####################################################################### 
# 
# 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_bk135
_database_code_depnum_ccdc_archive 'CCDC 2148180'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;EPFL
Switzerland
;
_audit_update_record             
;
2022-01-31 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_audit_creation_date             2021-09-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H66 N3 O3 V'
_chemical_formula_sum            'C45 H66 N3 O3 V'
_chemical_formula_weight         747.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H78 N3 O3 V1'
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'
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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9179(4)
_cell_length_b                   19.6672(5)
_cell_length_c                   24.8242(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.425(3)
_cell_angle_gamma                90
_cell_volume                     5272.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4612
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      72.1220
_cell_measurement_theta_min      3.5600
_shelx_estimated_absorpt_T_max   0.869
_shelx_estimated_absorpt_T_min   0.636
_exptl_absorpt_coefficient_mu    1.822
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
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 dark orange'
_exptl_crystal_density_diffrn    0.942
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 1 0.0399
0 1 -2 0.1290
0 2 1 0.1029
0 1 1 0.0999
0 1 0 0.1021
0 -1 2 0.1000
0 0 1 0.0979
0 0 -1 0.1436
6 4 -7 0.0382
-1 3 -15 0.1327
0 -12 -6 0.0894
-5 -9 1 0.0507
4 6 9 0.0876
-7 0 8 0.0289
5 8 -5 0.0467
5 7 4 0.0691
6 -5 -10 0.0774

_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.079
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
-1.0000 -1.0000 1.0000 0.1494 0.0184 -0.0716
0.0000 1.0000 -2.0000 -0.0114 0.0331 0.1437
0.0000 2.0000 1.0000 -0.0871 0.1443 -0.0095
0.0000 1.0000 1.0000 -0.0500 0.0800 -0.0344
0.0000 1.0000 0.0000 -0.0371 0.0644 0.0249
-0.0000 -1.0000 2.0000 0.0114 -0.0331 -0.1437
-0.0000 0.0000 1.0000 -0.0129 0.0156 -0.0594
0.0000 -0.0000 -1.0000 0.0129 -0.0156 0.0594
6.2680 4.3552 -7.1782 -0.8536 -0.2529 0.4553
-1.2849 3.2953 -14.7003 0.2278 0.0687 0.9713
-0.4250 -11.8314 -5.7462 0.5661 -0.8227 0.0515
-5.0176 -8.9928 0.9337 0.9496 -0.2271 -0.2161
4.4368 5.8366 8.5837 -0.8823 0.2117 -0.4204
-6.5789 0.4879 8.1041 0.7010 0.6000 -0.3856
5.1011 8.3991 -5.2307 -0.8827 0.1162 0.4553
5.4571 6.7633 3.8401 -0.9833 0.1287 -0.1286
5.5257 -4.6054 -10.0069 -0.3919 -0.8240 0.4093

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25540
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.644
_diffrn_reflns_theta_min         3.600
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00  14.00   1.00   12.50    --  -40.91  99.00  -7.00   68
  2  ω     11.00  57.00   1.00   12.50    --   40.91 -99.00-112.00   46
  3  ω    105.00 137.00   1.00   50.00    --  105.15  99.00  -7.00   32
  4  ω     38.00  73.00   1.00   50.00    --  105.15 -99.00-112.00   35
  5  ω    -91.00 -14.00   1.00   12.50    --  -40.91 -57.00 -90.00   77
  6  ω    -31.00  65.00   1.00   12.50    --   40.91 -38.00 120.00   96
  7  ω    -20.00   6.00   1.00   12.50    --   40.91 -77.00-150.00   26
  8  ω    131.00 177.00   1.00   50.00    --  105.15 111.00 -60.00   46
  9  ω     79.00 178.00   1.00   50.00    --  105.15  45.00 150.00   99
 10  ω    127.00 178.00   1.00   50.00    --  105.15  77.00 -30.00   51
 11  ω    121.00 148.00   1.00   50.00    --  105.15 111.00-180.00   27
 12  ω     55.00 106.00   1.00   50.00    --  105.15-111.00 -60.00   51
 13  ω     34.00 134.00   1.00   50.00    --  105.15 -61.00 -90.00  100
 14  ω     53.00 127.00   1.00   50.00    --  105.15 -61.00  30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1251529000
_diffrn_orient_matrix_UB_12      -0.0371008000
_diffrn_orient_matrix_UB_13      -0.0128706000
_diffrn_orient_matrix_UB_21      -0.0671747000
_diffrn_orient_matrix_UB_22      0.0643616000
_diffrn_orient_matrix_UB_23      0.0156254000
_diffrn_orient_matrix_UB_31      -0.0126794000
_diffrn_orient_matrix_UB_32      0.0249356000
_diffrn_orient_matrix_UB_33      -0.0593752000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                6724
_reflns_number_total             10235
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10235
_refine_ls_number_restraints     1102
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0611
_refine_ls_restrained_S_all      1.102
_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)+(0.1065P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1880
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-C2 \\sim C57-C2
 with sigma of 0.02
 C47-C46 \\sim C46-C45 \\sim C45-C47 \\sim C48-C49 \\sim C49-C50 \\sim C48-C50
 with sigma of 0.02
 C49-C44 \\sim C47-C44 \\sim C48-C44 \\sim C46-C44 \\sim C50-C44 \\sim C45-C44
 with sigma of 0.02
 C38-C36 \\sim C39-C36 \\sim C37-C36 \\sim C41-C40 \\sim C42-C40 \\sim C43-C40
 with sigma of 0.02
 C41-C42 \\sim C42-C43 \\sim C41-C43 \\sim C38-C37 \\sim C37-C39 \\sim C38-C39
 with sigma of 0.02
 O1-C32 \\sim O1-C28
 with sigma of 0.02
 C29-C30 \\sim C30-C31 \\sim C29-C31 \\sim C33-C34 \\sim C34-C35 \\sim C33-C35
 with sigma of 0.02
 C33-C32 \\sim C34-C32 \\sim C35-C32 \\sim C31-C28 \\sim C29-C28 \\sim C30-C28
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C38 \\sim C36 \\sim C39 \\sim C37 \\sim C41 \\sim C40 \\sim C43 \\sim C42 \\sim
C32 \\sim C33 \\sim C29 \\sim C28 \\sim C30 \\sim C34 \\sim C31 \\sim C35 \\sim
C49 \\sim C47 \\sim C48 \\sim C46 \\sim C50 \\sim C45 \\sim C44: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C51 \\sim C60 \\sim C62 \\sim C53 \\sim C58 \\sim C54 \\sim C61 \\sim C56 \\sim
C59 \\sim C52 \\sim C57 \\sim C55: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=1-FVAR(1)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(1)
 Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=
 Sof(H55)=Sof(C56)=Sof(H56)=1-FVAR(2)
 Sof(C57)=Sof(C62)=Sof(H62)=Sof(C61)=Sof(H61)=Sof(C60)=Sof(H60)=Sof(C59)=
 Sof(H59)=Sof(C58)=Sof(H58)=FVAR(2)
 Sof(C40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(3)
 Sof(C36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(3)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(4)
 Sof(C28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C62(H62), C61(H61), C60(H60), C59(H59), C58(H58)
6.c Fitted hexagon refined as free rotating group:
 C57(C62,C61,C60,C59,C58)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.25629(4) 0.25933(2) 0.26582(2) 0.04813(15) Uani 1 1 d . . . . .
O1 O 0.2098(2) 0.31207(11) 0.20729(8) 0.0692(6) Uani 1 1 d D . . . .
O2 O 0.3922(2) 0.21376(12) 0.25360(9) 0.0684(6) Uani 1 1 d . . . . .
O3 O 0.13386(19) 0.20083(10) 0.27333(8) 0.0583(5) Uani 1 1 d . . . . .
N1 N 0.32020(19) 0.38734(10) 0.40186(8) 0.0395(4) Uani 1 1 d . . . . .
N2 N 0.3532(2) 0.39192(10) 0.45563(8) 0.0428(4) Uani 1 1 d . . . . .
N3 N 0.38086(19) 0.32835(10) 0.47051(8) 0.0419(4) Uani 1 1 d . . . . .
C1 C 0.3261(2) 0.32219(12) 0.38119(9) 0.0404(5) Uani 1 1 d . . . . .
C2 C 0.3682(2) 0.28306(12) 0.42858(10) 0.0429(5) Uani 1 1 d D . . . .
C3 C 0.2849(2) 0.44904(12) 0.37175(9) 0.0431(5) Uani 1 1 d . . . . .
C4 C 0.3785(3) 0.48709(13) 0.35327(10) 0.0495(5) Uani 1 1 d . . . . .
C5 C 0.3422(3) 0.54691(15) 0.32512(12) 0.0596(6) Uani 1 1 d . . . . .
H5 H 0.402188 0.574437 0.312331 0.071 Uiso 1 1 calc R U . . .
C6 C 0.2192(3) 0.56617(16) 0.31581(13) 0.0651(7) Uani 1 1 d . . . . .
H6 H 0.196380 0.606297 0.296310 0.078 Uiso 1 1 calc R U . . .
C7 C 0.1301(3) 0.52753(16) 0.33463(12) 0.0633(7) Uani 1 1 d . . . . .
H7 H 0.047090 0.541859 0.328210 0.076 Uiso 1 1 calc R U . . .
C8 C 0.1604(3) 0.46711(14) 0.36323(11) 0.0508(5) Uani 1 1 d . . . . .
C9 C 0.5127(3) 0.46610(15) 0.36464(13) 0.0602(6) Uani 1 1 d . . . . .
H9 H 0.515130 0.416619 0.372049 0.072 Uiso 1 1 calc R U . . .
C10 C 0.5816(4) 0.4787(3) 0.31671(17) 0.0939(12) Uani 1 1 d . . . . .
H10A H 0.532437 0.462111 0.283588 0.141 Uiso 1 1 calc R U . . .
H10B H 0.660268 0.454881 0.322578 0.141 Uiso 1 1 calc R U . . .
H10C H 0.596150 0.527030 0.313342 0.141 Uiso 1 1 calc R U . . .
C11 C 0.5768(4) 0.5018(2) 0.41543(17) 0.0890(11) Uani 1 1 d . . . . .
H11A H 0.576681 0.550455 0.409193 0.134 Uiso 1 1 calc R U . . .
H11B H 0.661467 0.485729 0.423670 0.134 Uiso 1 1 calc R U . . .
H11C H 0.533047 0.491864 0.445832 0.134 Uiso 1 1 calc R U . . .
C12 C 0.0631(3) 0.42588(17) 0.38635(14) 0.0649(7) Uani 1 1 d . . . . .
H12 H 0.093499 0.378557 0.391360 0.078 Uiso 1 1 calc R U . . .
C13 C -0.0607(4) 0.4243(3) 0.3500(2) 0.1144(16) Uani 1 1 d . . . . .
H13A H -0.092754 0.470181 0.344885 0.172 Uiso 1 1 calc R U . . .
H13B H -0.118211 0.396698 0.366901 0.172 Uiso 1 1 calc R U . . .
H13C H -0.050535 0.404924 0.315029 0.172 Uiso 1 1 calc R U . . .
C14 C 0.0465(5) 0.4542(2) 0.44240(18) 0.0974(12) Uani 1 1 d . . . . .
H14A H 0.124866 0.452067 0.466492 0.146 Uiso 1 1 calc R U . . .
H14B H -0.014743 0.427386 0.457534 0.146 Uiso 1 1 calc R U . . .
H14C H 0.019054 0.501096 0.438614 0.146 Uiso 1 1 calc R U . . .
C15 C 0.4210(2) 0.31660(13) 0.52815(10) 0.0461(5) Uani 1 1 d . . . . .
C16 C 0.3299(3) 0.30655(15) 0.56104(11) 0.0545(6) Uani 1 1 d . . . . .
C17 C 0.3727(3) 0.29205(18) 0.61582(12) 0.0661(8) Uani 1 1 d . . . . .
H17 H 0.315204 0.285040 0.639984 0.079 Uiso 1 1 calc R U . . .
C18 C 0.4965(3) 0.28789(18) 0.63482(12) 0.0689(8) Uani 1 1 d . . . . .
H18 H 0.522391 0.277184 0.671635 0.083 Uiso 1 1 calc R U . . .
C19 C 0.5836(3) 0.29902(17) 0.60126(12) 0.0654(7) Uani 1 1 d . . . . .
H19 H 0.668222 0.296207 0.615369 0.079 Uiso 1 1 calc R U . . .
C20 C 0.5477(3) 0.31456(15) 0.54608(11) 0.0533(6) Uani 1 1 d . . . . .
C21 C 0.1926(3) 0.3103(2) 0.54055(13) 0.0715(8) Uani 1 1 d . . . . .
H21 H 0.182783 0.324729 0.501943 0.086 Uiso 1 1 calc R U . . .
C22 C 0.1314(4) 0.3648(2) 0.57215(18) 0.0931(11) Uani 1 1 d . . . . .
H22A H 0.145979 0.354208 0.610722 0.140 Uiso 1 1 calc R U . . .
H22B H 0.042971 0.365567 0.559562 0.140 Uiso 1 1 calc R U . . .
H22C H 0.166498 0.408950 0.566099 0.140 Uiso 1 1 calc R U . . .
C23 C 0.1292(4) 0.2417(3) 0.5426(2) 0.1119(15) Uani 1 1 d . . . . .
H23A H 0.168421 0.208900 0.521533 0.168 Uiso 1 1 calc R U . . .
H23B H 0.042431 0.246050 0.527584 0.168 Uiso 1 1 calc R U . . .
H23C H 0.136355 0.226541 0.580143 0.168 Uiso 1 1 calc R U . . .
C24 C 0.6439(3) 0.32818(19) 0.50939(13) 0.0676(7) Uani 1 1 d . . . . .
H24 H 0.599397 0.340206 0.472980 0.081 Uiso 1 1 calc R U . . .
C25 C 0.7269(4) 0.3883(3) 0.52951(17) 0.0948(12) Uani 1 1 d . . . . .
H25A H 0.676694 0.428769 0.530647 0.142 Uiso 1 1 calc R U . . .
H25B H 0.787019 0.395619 0.504923 0.142 Uiso 1 1 calc R U . . .
H25C H 0.769854 0.378543 0.565727 0.142 Uiso 1 1 calc R U . . .
C26 C 0.7211(5) 0.2635(3) 0.5028(2) 0.1162(16) Uani 1 1 d . . . . .
H26A H 0.776009 0.254675 0.536466 0.174 Uiso 1 1 calc R U . . .
H26B H 0.769764 0.270257 0.473519 0.174 Uiso 1 1 calc R U . . .
H26C H 0.666041 0.225061 0.494278 0.174 Uiso 1 1 calc R U . . .
C27 C 0.2919(2) 0.30428(13) 0.32639(10) 0.0462(5) Uani 1 1 d . . . . .
C28 C 0.1863(10) 0.3813(4) 0.1912(4) 0.0976(13) Uani 0.611(10) 1 d D U P A 1
C29 C 0.1382(11) 0.3818(4) 0.1308(3) 0.111(2) Uani 0.611(10) 1 d D U P A 1
H29A H 0.196210 0.358159 0.111295 0.166 Uiso 0.611(10) 1 calc R U P A 1
H29B H 0.128963 0.428359 0.118029 0.166 Uiso 0.611(10) 1 calc R U P A 1
H29C H 0.058472 0.359070 0.124330 0.166 Uiso 0.611(10) 1 calc R U P A 1
C30 C 0.0886(9) 0.4099(4) 0.2226(4) 0.117(2) Uani 0.611(10) 1 d D U P A 1
H30A H 0.018489 0.379108 0.219469 0.175 Uiso 0.611(10) 1 calc R U P A 1
H30B H 0.061513 0.453894 0.207728 0.175 Uiso 0.611(10) 1 calc R U P A 1
H30C H 0.123394 0.414916 0.260635 0.175 Uiso 0.611(10) 1 calc R U P A 1
C31 C 0.3110(12) 0.4142(8) 0.2033(6) 0.111(2) Uani 0.389(10) 1 d D U P A 1
H31A H 0.341622 0.409916 0.241902 0.166 Uiso 0.389(10) 1 calc R U P A 1
H31B H 0.304160 0.461916 0.193567 0.166 Uiso 0.389(10) 1 calc R U P A 1
H31C H 0.367995 0.391996 0.182459 0.166 Uiso 0.389(10) 1 calc R U P A 1
C32 C 0.1983(14) 0.3791(6) 0.1868(5) 0.0981(15) Uani 0.389(10) 1 d D U P A 2
C33 C 0.2189(16) 0.3756(6) 0.1271(4) 0.101(2) Uani 0.389(10) 1 d D U P A 2
H33A H 0.298749 0.355020 0.124873 0.152 Uiso 0.389(10) 1 calc R U P A 2
H33B H 0.216988 0.421198 0.112033 0.152 Uiso 0.389(10) 1 calc R U P A 2
H33C H 0.154044 0.348474 0.106533 0.152 Uiso 0.389(10) 1 calc R U P A 2
C34 C 0.0670(12) 0.3990(7) 0.1923(6) 0.116(2) Uani 0.389(10) 1 d D U P A 2
H34A H 0.049264 0.385884 0.228023 0.174 Uiso 0.389(10) 1 calc R U P A 2
H34B H 0.010014 0.376021 0.164511 0.174 Uiso 0.389(10) 1 calc R U P A 2
H34C H 0.057503 0.447780 0.187884 0.174 Uiso 0.389(10) 1 calc R U P A 2
C35 C 0.2854(10) 0.4301(5) 0.2161(4) 0.115(2) Uani 0.611(10) 1 d D U P A 2
H35A H 0.316987 0.413130 0.252197 0.173 Uiso 0.611(10) 1 calc R U P A 2
H35B H 0.241893 0.472577 0.219321 0.173 Uiso 0.611(10) 1 calc R U P A 2
H35C H 0.353799 0.437658 0.195939 0.173 Uiso 0.611(10) 1 calc R U P A 2
C36 C 0.5153(8) 0.2308(5) 0.2414(4) 0.0948(17) Uani 0.635(10) 1 d D U P B 1
C37 C 0.5906(7) 0.1670(5) 0.2462(4) 0.107(2) Uani 0.635(10) 1 d D U P B 1
H37A H 0.588620 0.146674 0.281698 0.160 Uiso 0.635(10) 1 calc R U P B 1
H37B H 0.675501 0.177670 0.242132 0.160 Uiso 0.635(10) 1 calc R U P B 1
H37C H 0.556608 0.135329 0.218017 0.160 Uiso 0.635(10) 1 calc R U P B 1
C38 C 0.4972(10) 0.2536(6) 0.1822(4) 0.125(2) Uani 0.635(10) 1 d D U P B 1
H38A H 0.473570 0.214916 0.158750 0.188 Uiso 0.635(10) 1 calc R U P B 1
H38B H 0.574004 0.272655 0.173572 0.188 Uiso 0.635(10) 1 calc R U P B 1
H38C H 0.432664 0.287841 0.176530 0.188 Uiso 0.635(10) 1 calc R U P B 1
C39 C 0.5707(8) 0.2874(5) 0.2765(4) 0.112(2) Uani 0.635(10) 1 d D U P B 1
H39A H 0.521536 0.328207 0.268371 0.168 Uiso 0.635(10) 1 calc R U P B 1
H39B H 0.654533 0.295575 0.269510 0.168 Uiso 0.635(10) 1 calc R U P B 1
H39C H 0.572046 0.275351 0.314464 0.168 Uiso 0.635(10) 1 calc R U P B 1
C40 C 0.5252(13) 0.2120(8) 0.2602(6) 0.0958(19) Uani 0.365(10) 1 d D U P B 2
C41 C 0.5504(14) 0.2280(9) 0.2046(6) 0.113(2) Uani 0.365(10) 1 d D U P B 2
H41A H 0.489112 0.205846 0.178139 0.170 Uiso 0.365(10) 1 calc R U P B 2
H41B H 0.632308 0.211814 0.200329 0.170 Uiso 0.365(10) 1 calc R U P B 2
H41C H 0.546185 0.276786 0.199029 0.170 Uiso 0.365(10) 1 calc R U P B 2
C42 C 0.5755(13) 0.1414(8) 0.2747(7) 0.105(3) Uani 0.365(10) 1 d D U P B 2
H42A H 0.560044 0.129592 0.311081 0.158 Uiso 0.365(10) 1 calc R U P B 2
H42B H 0.663945 0.140646 0.273600 0.158 Uiso 0.365(10) 1 calc R U P B 2
H42C H 0.534729 0.108706 0.248816 0.158 Uiso 0.365(10) 1 calc R U P B 2
C43 C 0.5841(14) 0.2594(8) 0.3037(7) 0.109(3) Uani 0.365(10) 1 d D U P B 2
H43A H 0.541085 0.302701 0.300416 0.163 Uiso 0.365(10) 1 calc R U P B 2
H43B H 0.670308 0.266340 0.299741 0.163 Uiso 0.365(10) 1 calc R U P B 2
H43C H 0.579114 0.239911 0.339241 0.163 Uiso 0.365(10) 1 calc R U P B 2
C44 C 0.0465(4) 0.1808(2) 0.30644(15) 0.0829(9) Uani 1 1 d D U . . .
C45 C 0.0563(9) 0.2210(4) 0.3585(3) 0.0895(18) Uani 0.540(5) 1 d D U P C 1
H45A H 0.134763 0.211160 0.380872 0.134 Uiso 0.540(5) 1 calc R U P C 1
H45B H -0.011041 0.208475 0.378048 0.134 Uiso 0.540(5) 1 calc R U P C 1
H45C H 0.051402 0.269139 0.350078 0.134 Uiso 0.540(5) 1 calc R U P C 1
C46 C 0.0984(8) 0.1056(4) 0.3255(3) 0.1022(18) Uani 0.540(5) 1 d D U P C 1
H46A H 0.110953 0.079203 0.293764 0.153 Uiso 0.540(5) 1 calc R U P C 1
H46B H 0.038752 0.082670 0.344585 0.153 Uiso 0.540(5) 1 calc R U P C 1
H46C H 0.176410 0.110030 0.349597 0.153 Uiso 0.540(5) 1 calc R U P C 1
C47 C -0.0733(7) 0.1724(5) 0.2766(3) 0.0971(19) Uani 0.540(5) 1 d D U P C 1
H47A H -0.105781 0.216390 0.263778 0.146 Uiso 0.540(5) 1 calc R U P C 1
H47B H -0.127504 0.152251 0.299796 0.146 Uiso 0.540(5) 1 calc R U P C 1
H47C H -0.068651 0.142922 0.245611 0.146 Uiso 0.540(5) 1 calc R U P C 1
C48 C -0.0389(9) 0.1254(5) 0.2808(4) 0.090(2) Uani 0.460(5) 1 d D U P C 2
H48A H -0.072605 0.138386 0.243903 0.135 Uiso 0.460(5) 1 calc R U P C 2
H48B H -0.106031 0.119067 0.301964 0.135 Uiso 0.460(5) 1 calc R U P C 2
H48C H 0.007075 0.083322 0.280129 0.135 Uiso 0.460(5) 1 calc R U P C 2
C49 C -0.0479(9) 0.2470(4) 0.2959(4) 0.0986(19) Uani 0.460(5) 1 d D U P C 2
H49A H -0.001666 0.288505 0.305400 0.148 Uiso 0.460(5) 1 calc R U P C 2
H49B H -0.113161 0.242747 0.318324 0.148 Uiso 0.460(5) 1 calc R U P C 2
H49C H -0.084056 0.248574 0.257831 0.148 Uiso 0.460(5) 1 calc R U P C 2
C50 C 0.0836(11) 0.1786(6) 0.3644(3) 0.105(2) Uani 0.460(5) 1 d D U P C 2
H50A H 0.134163 0.138604 0.373896 0.158 Uiso 0.460(5) 1 calc R U P C 2
H50B H 0.010630 0.176666 0.382481 0.158 Uiso 0.460(5) 1 calc R U P C 2
H50C H 0.131006 0.219069 0.376085 0.158 Uiso 0.460(5) 1 calc R U P C 2
C51 C 0.3947(5) 0.21008(17) 0.43362(19) 0.0562(7) Uani 0.872(6) 1 d D U P D 2
C52 C 0.4224(5) 0.1759(2) 0.38792(17) 0.0799(12) Uani 0.872(6) 1 d . U P D 2
H52 H 0.425342 0.199917 0.355390 0.096 Uiso 0.872(6) 1 calc R U P D 2
C53 C 0.4457(6) 0.1062(2) 0.3901(2) 0.1037(15) Uani 0.872(6) 1 d . U P D 2
H53 H 0.462126 0.083373 0.358690 0.124 Uiso 0.872(6) 1 calc R U P D 2
C54 C 0.4449(6) 0.0709(2) 0.4372(2) 0.1071(15) Uani 0.872(6) 1 d . U P D 2
H54 H 0.462993 0.024170 0.438541 0.129 Uiso 0.872(6) 1 calc R U P D 2
C55 C 0.4177(6) 0.1038(2) 0.4827(2) 0.0977(14) Uani 0.872(6) 1 d . U P D 2
H55 H 0.415549 0.079167 0.514954 0.117 Uiso 0.872(6) 1 calc R U P D 2
C56 C 0.3934(5) 0.1731(2) 0.48148(18) 0.0751(11) Uani 0.872(6) 1 d . U P D 2
H56 H 0.375884 0.195215 0.513057 0.090 Uiso 0.872(6) 1 calc R U P D 2
C57 C 0.394(3) 0.2085(6) 0.4340(10) 0.069(2) Uani 0.128(6) 1 d DG U P D 1
C62 C 0.456(3) 0.1802(10) 0.4816(10) 0.077(2) Uani 0.128(6) 1 d G U P D 1
H62 H 0.495762 0.208515 0.509218 0.093 Uiso 0.128(6) 1 calc R U P D 1
C61 C 0.459(3) 0.1100(10) 0.4883(9) 0.089(2) Uani 0.128(6) 1 d G U P D 1
H61 H 0.500745 0.090888 0.520515 0.107 Uiso 0.128(6) 1 calc R U P D 1
C60 C 0.399(3) 0.0682(7) 0.4475(11) 0.096(3) Uani 0.128(6) 1 d G U P D 1
H60 H 0.401471 0.020730 0.452032 0.115 Uiso 0.128(6) 1 calc R U P D 1
C59 C 0.337(3) 0.0965(8) 0.3999(9) 0.092(2) Uani 0.128(6) 1 d G U P D 1
H59 H 0.297212 0.068197 0.372252 0.110 Uiso 0.128(6) 1 calc R U P D 1
C58 C 0.334(3) 0.1667(9) 0.3931(8) 0.080(2) Uani 0.128(6) 1 d G U P D 1
H58 H 0.292228 0.185823 0.360955 0.097 Uiso 0.128(6) 1 calc R U P D 1


_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 O1 1.797(2) . ?
V1 O2 1.797(2) . ?
V1 O3 1.794(2) . ?
V1 C27 1.739(2) . ?
O1 C28 1.431(8) . ?
O1 C32 1.412(12) . ?
O2 C36 1.459(9) . ?
O2 C40 1.438(15) . ?
O3 C44 1.404(4) . ?
N1 N2 1.333(3) . ?
N1 C1 1.385(3) . ?
N1 C3 1.448(3) . ?
N2 N3 1.326(3) . ?
N3 C2 1.362(3) . ?
N3 C15 1.452(3) . ?
C1 C2 1.425(3) . ?
C1 C27 1.402(3) . ?
C2 C51 1.466(4) . ?
C2 C57 1.494(13) . ?
C3 C4 1.397(4) . ?
C3 C8 1.391(4) . ?
C4 C5 1.396(4) . ?
C4 C9 1.509(4) . ?
C5 H5 0.9400 . ?
C5 C6 1.382(5) . ?
C6 H6 0.9400 . ?
C6 C7 1.369(5) . ?
C7 H7 0.9400 . ?
C7 C8 1.399(4) . ?
C8 C12 1.515(4) . ?
C9 H9 0.9900 . ?
C9 C10 1.518(5) . ?
C9 C11 1.521(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 H12 0.9900 . ?
C12 C13 1.511(5) . ?
C12 C14 1.534(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C15 C16 1.391(4) . ?
C15 C20 1.390(4) . ?
C16 C17 1.401(4) . ?
C16 C21 1.512(4) . ?
C17 H17 0.9400 . ?
C17 C18 1.367(5) . ?
C18 H18 0.9400 . ?
C18 C19 1.371(5) . ?
C19 H19 0.9400 . ?
C19 C20 1.402(4) . ?
C20 C24 1.511(5) . ?
C21 H21 0.9900 . ?
C21 C22 1.537(6) . ?
C21 C23 1.521(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C24 H24 0.9900 . ?
C24 C25 1.528(5) . ?
C24 C26 1.548(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C28 C29 1.515(9) . ?
C28 C30 1.519(10) . ?
C28 C31 1.498(11) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 H30C 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C32 C33 1.533(12) . ?
C32 C34 1.511(12) . ?
C32 C35 1.497(12) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 H34C 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 H35C 0.9700 . ?
C36 C37 1.495(9) . ?
C36 C38 1.522(9) . ?
C36 C39 1.486(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 H39C 0.9700 . ?
C40 C41 1.479(12) . ?
C40 C42 1.517(12) . ?
C40 C43 1.500(12) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 H42C 0.9700 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 H43C 0.9700 . ?
C44 C45 1.505(7) . ?
C44 C46 1.630(8) . ?
C44 C47 1.415(7) . ?
C44 C48 1.512(7) . ?
C44 C49 1.657(9) . ?
C44 C50 1.438(8) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 H45C 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 H46C 0.9700 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C47 H47C 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 H48C 0.9700 . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C49 H49C 0.9700 . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C50 H50C 0.9700 . ?
C51 C52 1.389(6) . ?
C51 C56 1.395(6) . ?
C52 H52 0.9400 . ?
C52 C53 1.394(5) . ?
C53 H53 0.9400 . ?
C53 C54 1.361(7) . ?
C54 H54 0.9400 . ?
C54 C55 1.370(8) . ?
C55 H55 0.9400 . ?
C55 C56 1.389(5) . ?
C56 H56 0.9400 . ?
C57 C62 1.3900 . ?
C57 C58 1.3900 . ?
C62 H62 0.9400 . ?
C62 C61 1.3900 . ?
C61 H61 0.9400 . ?
C61 C60 1.3900 . ?
C60 H60 0.9400 . ?
C60 C59 1.3900 . ?
C59 H59 0.9400 . ?
C59 C58 1.3900 . ?
C58 H58 0.9400 . ?

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
O2 V1 O1 107.10(12) . . ?
O3 V1 O1 109.13(10) . . ?
O3 V1 O2 110.11(11) . . ?
C27 V1 O1 114.00(11) . . ?
C27 V1 O2 108.30(11) . . ?
C27 V1 O3 108.17(11) . . ?
C28 O1 V1 142.4(4) . . ?
C32 O1 V1 146.1(5) . . ?
C36 O2 V1 136.8(4) . . ?
C40 O2 V1 146.9(6) . . ?
C44 O3 V1 145.24(19) . . ?
N2 N1 C1 114.39(18) . . ?
N2 N1 C3 118.21(18) . . ?
C1 N1 C3 127.39(19) . . ?
N3 N2 N1 103.44(18) . . ?
N2 N3 C2 114.22(19) . . ?
N2 N3 C15 116.63(19) . . ?
C2 N3 C15 129.2(2) . . ?
N1 C1 C2 102.74(19) . . ?
N1 C1 C27 124.9(2) . . ?
C27 C1 C2 132.3(2) . . ?
N3 C2 C1 105.2(2) . . ?
N3 C2 C51 125.4(3) . . ?
N3 C2 C57 125.2(9) . . ?
C1 C2 C51 129.4(3) . . ?
C1 C2 C57 129.6(9) . . ?
C4 C3 N1 117.8(2) . . ?
C8 C3 N1 118.2(2) . . ?
C8 C3 C4 124.0(2) . . ?
C3 C4 C9 121.9(2) . . ?
C5 C4 C3 116.7(3) . . ?
C5 C4 C9 121.4(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.8(3) . . ?
C7 C6 H6 119.6 . . ?
C6 C7 H7 119.4 . . ?
C6 C7 C8 121.2(3) . . ?
C8 C7 H7 119.4 . . ?
C3 C8 C7 116.6(3) . . ?
C3 C8 C12 122.0(2) . . ?
C7 C8 C12 121.3(3) . . ?
C4 C9 H9 107.6 . . ?
C4 C9 C10 112.8(3) . . ?
C4 C9 C11 110.2(3) . . ?
C10 C9 H9 107.6 . . ?
C10 C9 C11 110.7(3) . . ?
C11 C9 H9 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12 108.0 . . ?
C8 C12 C14 109.4(3) . . ?
C13 C12 C8 113.6(3) . . ?
C13 C12 H12 108.0 . . ?
C13 C12 C14 109.6(4) . . ?
C14 C12 H12 108.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N3 117.5(2) . . ?
C20 C15 N3 117.5(2) . . ?
C20 C15 C16 124.9(2) . . ?
C15 C16 C17 115.6(3) . . ?
C15 C16 C21 123.7(2) . . ?
C17 C16 C21 120.7(3) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.3(3) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 H18 119.3 . . ?
C17 C18 C19 121.3(3) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 C19 116.2(3) . . ?
C15 C20 C24 123.3(2) . . ?
C19 C20 C24 120.5(3) . . ?
C16 C21 H21 107.5 . . ?
C16 C21 C22 110.3(3) . . ?
C16 C21 C23 112.2(3) . . ?
C22 C21 H21 107.5 . . ?
C23 C21 H21 107.5 . . ?
C23 C21 C22 111.5(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 H24 107.6 . . ?
C20 C24 C25 111.8(3) . . ?
C20 C24 C26 110.8(3) . . ?
C25 C24 H24 107.6 . . ?
C25 C24 C26 111.3(4) . . ?
C26 C24 H24 107.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C1 C27 V1 164.0(2) . . ?
O1 C28 C29 107.7(6) . . ?
O1 C28 C30 108.6(7) . . ?
O1 C28 C31 103.6(9) . . ?
C29 C28 C30 109.8(7) . . ?
C31 C28 C29 111.7(8) . . ?
C31 C28 C30 115.0(8) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O1 C32 C33 106.8(9) . . ?
O1 C32 C34 104.1(10) . . ?
O1 C32 C35 115.7(10) . . ?
C34 C32 C33 112.0(10) . . ?
C35 C32 C33 109.1(9) . . ?
C35 C32 C34 109.0(9) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O2 C36 C37 107.7(6) . . ?
O2 C36 C38 106.0(6) . . ?
O2 C36 C39 111.0(6) . . ?
C37 C36 C38 108.5(6) . . ?
C39 C36 C37 114.2(7) . . ?
C39 C36 C38 109.2(7) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O2 C40 C41 102.2(10) . . ?
O2 C40 C42 111.9(10) . . ?
O2 C40 C43 112.7(10) . . ?
C41 C40 C42 107.8(9) . . ?
C41 C40 C43 114.9(10) . . ?
C43 C40 C42 107.2(9) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O3 C44 C45 112.7(4) . . ?
O3 C44 C46 100.8(4) . . ?
O3 C44 C47 112.4(5) . . ?
O3 C44 C48 112.7(5) . . ?
O3 C44 C49 98.5(4) . . ?
O3 C44 C50 118.6(5) . . ?
C45 C44 C46 104.4(5) . . ?
C47 C44 C45 117.1(6) . . ?
C47 C44 C46 107.6(5) . . ?
C48 C44 C49 99.7(5) . . ?
C50 C44 C48 117.7(6) . . ?
C50 C44 C49 105.0(6) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44 C49 H49A 109.5 . . ?
C44 C49 H49B 109.5 . . ?
C44 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C50 H50A 109.5 . . ?
C44 C50 H50B 109.5 . . ?
C44 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 C2 117.9(4) . . ?
C52 C51 C56 118.3(3) . . ?
C56 C51 C2 123.8(4) . . ?
C51 C52 H52 119.9 . . ?
C51 C52 C53 120.3(4) . . ?
C53 C52 H52 119.9 . . ?
C52 C53 H53 119.6 . . ?
C54 C53 C52 120.7(5) . . ?
C54 C53 H53 119.6 . . ?
C53 C54 H54 120.1 . . ?
C53 C54 C55 119.7(4) . . ?
C55 C54 H54 120.1 . . ?
C54 C55 H55 119.7 . . ?
C54 C55 C56 120.7(5) . . ?
C56 C55 H55 119.7 . . ?
C51 C56 H56 119.9 . . ?
C55 C56 C51 120.2(4) . . ?
C55 C56 H56 119.9 . . ?
C62 C57 C2 122.0(14) . . ?
C62 C57 C58 120.0 . . ?
C58 C57 C2 117.1(13) . . ?
C57 C62 H62 120.0 . . ?
C61 C62 C57 120.0 . . ?
C61 C62 H62 120.0 . . ?
C62 C61 H61 120.0 . . ?
C62 C61 C60 120.0 . . ?
C60 C61 H61 120.0 . . ?
C61 C60 H60 120.0 . . ?
C61 C60 C59 120.0 . . ?
C59 C60 H60 120.0 . . ?
C60 C59 H59 120.0 . . ?
C58 C59 C60 120.0 . . ?
C58 C59 H59 120.0 . . ?
C57 C58 H58 120.0 . . ?
C59 C58 C57 120.0 . . ?
C59 C58 H58 120.0 . . ?

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
V1 O1 C28 C29 -175.4(6) . . . . ?
V1 O1 C28 C30 -56.6(11) . . . . ?
V1 O1 C28 C31 66.1(10) . . . . ?
V1 O1 C32 C33 147.8(9) . . . . ?
V1 O1 C32 C34 -93.5(13) . . . . ?
V1 O1 C32 C35 26.1(18) . . . . ?
V1 O2 C36 C37 169.8(4) . . . . ?
V1 O2 C36 C38 -74.3(7) . . . . ?
V1 O2 C36 C39 44.1(9) . . . . ?
V1 O2 C40 C41 -105.8(12) . . . . ?
V1 O2 C40 C42 139.1(10) . . . . ?
V1 O2 C40 C43 18.1(17) . . . . ?
V1 O3 C44 C45 -3.0(7) . . . . ?
V1 O3 C44 C46 -113.8(5) . . . . ?
V1 O3 C44 C47 132.0(5) . . . . ?
V1 O3 C44 C48 175.1(5) . . . . ?
V1 O3 C44 C49 70.8(5) . . . . ?
V1 O3 C44 C50 -41.5(8) . . . . ?
O1 V1 O2 C36 57.2(6) . . . . ?
O1 V1 O2 C40 92.3(12) . . . . ?
O1 V1 O3 C44 -115.3(4) . . . . ?
O1 V1 C27 C1 178.5(8) . . . . ?
O2 V1 O1 C28 -122.5(8) . . . . ?
O2 V1 O1 C32 -111.2(12) . . . . ?
O2 V1 O3 C44 127.4(4) . . . . ?
O2 V1 C27 C1 -62.4(8) . . . . ?
O3 V1 O1 C28 118.4(8) . . . . ?
O3 V1 O1 C32 129.6(11) . . . . ?
O3 V1 O2 C36 175.7(6) . . . . ?
O3 V1 O2 C40 -149.2(12) . . . . ?
O3 V1 C27 C1 56.9(8) . . . . ?
N1 N2 N3 C2 0.6(3) . . . . ?
N1 N2 N3 C15 180.0(2) . . . . ?
N1 C1 C2 N3 0.5(3) . . . . ?
N1 C1 C2 C51 -179.1(4) . . . . ?
N1 C1 C2 C57 179.9(19) . . . . ?
N1 C1 C27 V1 -172.4(7) . . . . ?
N1 C3 C4 C5 -179.0(2) . . . . ?
N1 C3 C4 C9 -1.0(4) . . . . ?
N1 C3 C8 C7 179.1(2) . . . . ?
N1 C3 C8 C12 2.5(4) . . . . ?
N2 N1 C1 C2 -0.2(3) . . . . ?
N2 N1 C1 C27 177.7(2) . . . . ?
N2 N1 C3 C4 87.7(3) . . . . ?
N2 N1 C3 C8 -91.9(3) . . . . ?
N2 N3 C2 C1 -0.7(3) . . . . ?
N2 N3 C2 C51 178.9(3) . . . . ?
N2 N3 C2 C57 179.9(17) . . . . ?
N2 N3 C15 C16 85.4(3) . . . . ?
N2 N3 C15 C20 -96.1(3) . . . . ?
N3 C2 C51 C52 -156.3(4) . . . . ?
N3 C2 C51 C56 23.9(7) . . . . ?
N3 C2 C57 C62 -13(3) . . . . ?
N3 C2 C57 C58 156.5(14) . . . . ?
N3 C15 C16 C17 176.9(3) . . . . ?
N3 C15 C16 C21 -2.8(4) . . . . ?
N3 C15 C20 C19 -176.2(3) . . . . ?
N3 C15 C20 C24 3.9(4) . . . . ?
C1 N1 N2 N3 -0.2(3) . . . . ?
C1 N1 C3 C4 -91.2(3) . . . . ?
C1 N1 C3 C8 89.2(3) . . . . ?
C1 C2 C51 C52 23.2(7) . . . . ?
C1 C2 C51 C56 -156.7(4) . . . . ?
C1 C2 C57 C62 167.9(13) . . . . ?
C1 C2 C57 C58 -23(3) . . . . ?
C2 N3 C15 C16 -95.2(3) . . . . ?
C2 N3 C15 C20 83.2(3) . . . . ?
C2 C1 C27 V1 4.7(10) . . . . ?
C2 C51 C52 C53 -178.6(4) . . . . ?
C2 C51 C56 C55 179.0(4) . . . . ?
C2 C57 C62 C61 169(3) . . . . ?
C2 C57 C58 C59 -169(3) . . . . ?
C3 N1 N2 N3 -179.2(2) . . . . ?
C3 N1 C1 C2 178.7(2) . . . . ?
C3 N1 C1 C27 -3.4(4) . . . . ?
C3 C4 C5 C6 -0.8(4) . . . . ?
C3 C4 C9 C10 141.2(3) . . . . ?
C3 C4 C9 C11 -94.5(3) . . . . ?
C3 C8 C12 C13 -145.7(4) . . . . ?
C3 C8 C12 C14 91.5(4) . . . . ?
C4 C3 C8 C7 -0.4(4) . . . . ?
C4 C3 C8 C12 -177.1(3) . . . . ?
C4 C5 C6 C7 0.9(5) . . . . ?
C5 C4 C9 C10 -40.9(4) . . . . ?
C5 C4 C9 C11 83.5(4) . . . . ?
C5 C6 C7 C8 -0.8(5) . . . . ?
C6 C7 C8 C3 0.5(4) . . . . ?
C6 C7 C8 C12 177.2(3) . . . . ?
C7 C8 C12 C13 37.8(5) . . . . ?
C7 C8 C12 C14 -84.9(4) . . . . ?
C8 C3 C4 C5 0.6(4) . . . . ?
C8 C3 C4 C9 178.6(3) . . . . ?
C9 C4 C5 C6 -178.9(3) . . . . ?
C15 N3 C2 C1 180.0(2) . . . . ?
C15 N3 C2 C51 -0.4(5) . . . . ?
C15 N3 C2 C57 0.5(18) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
C15 C16 C21 C22 -121.7(3) . . . . ?
C15 C16 C21 C23 113.3(4) . . . . ?
C15 C20 C24 C25 120.5(3) . . . . ?
C15 C20 C24 C26 -114.7(4) . . . . ?
C16 C15 C20 C19 2.1(4) . . . . ?
C16 C15 C20 C24 -177.8(3) . . . . ?
C16 C17 C18 C19 1.3(6) . . . . ?
C17 C16 C21 C22 58.5(4) . . . . ?
C17 C16 C21 C23 -66.5(5) . . . . ?
C17 C18 C19 C20 -0.5(6) . . . . ?
C18 C19 C20 C15 -1.1(5) . . . . ?
C18 C19 C20 C24 178.8(3) . . . . ?
C19 C20 C24 C25 -59.4(4) . . . . ?
C19 C20 C24 C26 65.4(4) . . . . ?
C20 C15 C16 C17 -1.4(4) . . . . ?
C20 C15 C16 C21 178.9(3) . . . . ?
C21 C16 C17 C18 179.4(3) . . . . ?
C27 V1 O1 C28 -2.7(8) . . . . ?
C27 V1 O1 C32 8.6(12) . . . . ?
C27 V1 O2 C36 -66.2(6) . . . . ?
C27 V1 O2 C40 -31.1(12) . . . . ?
C27 V1 O3 C44 9.2(4) . . . . ?
C27 C1 C2 N3 -177.1(3) . . . . ?
C27 C1 C2 C51 3.3(5) . . . . ?
C27 C1 C2 C57 2.3(19) . . . . ?
C51 C52 C53 C54 -1.7(9) . . . . ?
C52 C51 C56 C55 -0.8(8) . . . . ?
C52 C53 C54 C55 1.7(10) . . . . ?
C53 C54 C55 C56 -1.3(10) . . . . ?
C54 C55 C56 C51 0.8(9) . . . . ?
C56 C51 C52 C53 1.2(9) . . . . ?
C57 C62 C61 C60 0.0 . . . . ?
C62 C57 C58 C59 0.0 . . . . ?
C62 C61 C60 C59 0.0 . . . . ?
C61 C60 C59 C58 0.0 . . . . ?
C60 C59 C58 C57 0.0 . . . . ?
C58 C57 C62 C61 0.0 . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 144 electrons were 
found in a volume of 1154Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.85[C5H12] per Asymmetric Unit 
which account for 143 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 577.1 72.3 '1.7 C5H12'
2 -0.500 0.500 0.000 577.1 72.3 '1.7 C5H12'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2021-09-15
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.557
