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

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

data_complex2_110k
_database_code_depnum_ccdc_archive 'CCDC 2158535'
loop_
_audit_author_name
_audit_author_address
'Roxanna Martinez'
;Colorado State University
United States of America
;
_audit_update_record             
;
2023-07-08 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_audit_creation_date             2023-06-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H9 Cl3 O6 V, 2(C12 H28 N) 1.6[C4H8O]'
_chemical_formula_sum            'C42 H65 Cl3 N2 O6 V'
_chemical_formula_weight         851.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.0922(9)
_cell_length_b                   15.2744(8)
_cell_length_c                   17.8164(9)
_cell_angle_alpha                90
_cell_angle_beta                 105.925(2)
_cell_angle_gamma                90
_cell_volume                     5257.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9215
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.08
_cell_measurement_theta_min      2.50
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6353
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0651 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8510.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.158
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            335992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.268
_diffrn_reflns_theta_min         1.699
_diffrn_ambient_temperature      110.35
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10638
_reflns_number_total             13015
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         13015
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.117
_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)+(0.0712P)²+2.9250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1333
_refine_special_details          'Solvent mask in OLEX2,SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H00P)=Sof(Cl)=1-FVAR(1)
 Sof(Cl00)=Sof(H00Q)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N00B(H00B), N00C(H00L)
3.b Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00C), C00Q(H00D,H00E), C00T(H00F,H00G), C00U(H00M,H00N), C00W(H00H,
 H00I), C00Z(H00J,H00K), C011(H01D,H01E), C013(H01R,H01S), C014(H01F,H01G),
 C016(H01T,H01U), C018(H01V,H01W), C019(H01H,H01I), C01A(H01J,H01K), C01B(H01X,
 H01Y), C01C(H01Z,H), C01D(H01,HA), C01G(H2AA,HF), C01L(H4AA,HI)
3.c Aromatic/amide H refined with riding coordinates:
 C00J(H00O), C00K(H00P), C00N(H00Q), C00O(H00R), C00P(H00S), C00R(H00T),
 C00S(H00U), C00V(H00V), C012(H012), C015(H015)
3.d Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C01E(H0AA,HB,HC), C01F(H1AA,HD,HE), C01H(H01L,H01M,
 H01N), C01I(H01O,H01P,H01Q), C01K(H3AA,HG,HH)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V001 V 0.25466(2) 0.59512(2) 0.39339(2) 0.01536(7) Uani 1 1 d . . . . .
Cl00 Cl -0.01820(2) 0.59826(3) 0.07017(3) 0.02892(15) Uani 0.9045(17) 1 d . . P
A 1
Cl1 Cl 0.55701(2) 0.76828(4) 0.36430(3) 0.04125(13) Uani 1 1 d . . . . .
Cl2 Cl 0.27595(3) 0.32968(3) 0.70403(3) 0.04076(13) Uani 1 1 d . . . . .
O005 O 0.22172(6) 0.49662(7) 0.32397(7) 0.0190(2) Uani 1 1 d . . . . .
O006 O 0.17951(6) 0.65199(7) 0.31793(6) 0.0186(2) Uani 1 1 d . . . . .
O007 O 0.19458(6) 0.59835(7) 0.46348(7) 0.0188(2) Uani 1 1 d . . . . .
O008 O 0.33509(6) 0.59740(7) 0.35340(7) 0.0187(2) Uani 1 1 d . . . . .
O009 O 0.29474(6) 0.70435(7) 0.43722(7) 0.0197(2) Uani 1 1 d . . . . .
O00A O 0.30124(6) 0.50715(7) 0.46948(6) 0.0187(2) Uani 1 1 d . . . . .
N00B N 0.35554(7) 0.38805(9) 0.37395(8) 0.0202(3) Uani 1 1 d . . . . .
H00B H 0.324739 0.435439 0.384008 0.024 Uiso 1 1 calc R . . . .
N00C N 0.13728(7) 0.76049(9) 0.47155(8) 0.0207(3) Uani 1 1 d . . . . .
H00L H 0.157062 0.701948 0.464569 0.025 Uiso 1 1 calc R . . . .
C00D C 0.37804(8) 0.66464(10) 0.37693(9) 0.0186(3) Uani 1 1 d . . . . .
C00F C 0.35567(8) 0.72493(10) 0.42527(9) 0.0191(3) Uani 1 1 d . . . . .
C00G C 0.16796(8) 0.51387(10) 0.26282(9) 0.0190(3) Uani 1 1 d . . . . .
C00H C 0.14390(8) 0.60099(10) 0.26013(9) 0.0174(3) Uani 1 1 d . . . . .
C00I C 0.21038(8) 0.53991(10) 0.52205(9) 0.0187(3) Uani 1 1 d . . . . .
C00J C 0.08679(8) 0.62791(11) 0.20063(9) 0.0206(3) Uani 1 1 d . . . . .
H00O H 0.069896 0.686193 0.198596 0.025 Uiso 1 1 calc R . . . .
C00K C 0.05519(8) 0.56628(12) 0.14401(9) 0.0233(3) Uani 1 1 d . . . . .
H00P H 0.016023 0.583611 0.103276 0.028 Uiso 0.0955(17) 1 calc R . P A 2
C00L C 0.33198(8) 0.36837(11) 0.28786(10) 0.0233(3) Uani 1 1 d . . . . .
H00A H 0.281405 0.358013 0.272819 0.028 Uiso 1 1 calc R . . . .
H00C H 0.354517 0.313628 0.277878 0.028 Uiso 1 1 calc R . . . .
C00M C 0.26960(8) 0.48897(10) 0.52471(9) 0.0188(3) Uani 1 1 d . . . . .
C00N C 0.07867(9) 0.48127(12) 0.14500(10) 0.0282(4) Uani 1 1 d . . . . .
H00Q H 0.056204 0.441257 0.105289 0.034 Uiso 0.9045(17) 1 calc R . P A 1
C00O C 0.39658(9) 0.79637(11) 0.45574(10) 0.0255(3) Uani 1 1 d . . . . .
H00R H 0.381964 0.836645 0.488625 0.031 Uiso 1 1 calc R . . . .
C00P C 0.43961(9) 0.67757(11) 0.35731(10) 0.0240(3) Uani 1 1 d . . . . .
H00S H 0.454209 0.638206 0.323705 0.029 Uiso 1 1 calc R . . . .
C00Q C 0.34772(10) 0.44025(12) 0.23625(10) 0.0263(4) Uani 1 1 d . . . . .
H00D H 0.398048 0.441473 0.241461 0.032 Uiso 1 1 calc R . . . .
H00E H 0.334415 0.497673 0.253492 0.032 Uiso 1 1 calc R . . . .
C00R C 0.13591(9) 0.45457(12) 0.20505(10) 0.0256(3) Uani 1 1 d . . . . .
H00T H 0.152730 0.396307 0.206312 0.031 Uiso 1 1 calc R . . . .
C00S C 0.45942(9) 0.80904(12) 0.43796(11) 0.0294(4) Uani 1 1 d . . . . .
H00U H 0.488230 0.857280 0.459390 0.035 Uiso 1 1 calc R . . . .
C00T C 0.34596(9) 0.31005(11) 0.42170(10) 0.0248(3) Uani 1 1 d . . . . .
H00F H 0.368853 0.322001 0.477430 0.030 Uiso 1 1 calc R . . . .
H00G H 0.369063 0.258706 0.405991 0.030 Uiso 1 1 calc R . . . .
C00U C 0.16211(9) 0.82325(11) 0.42005(11) 0.0249(3) Uani 1 1 d . . . . .
H00M H 0.145715 0.802670 0.365371 0.030 Uiso 1 1 calc R . . . .
H00N H 0.213339 0.822480 0.435093 0.030 Uiso 1 1 calc R . . . .
C00V C 0.29083(9) 0.42501(11) 0.58198(10) 0.0233(3) Uani 1 1 d . . . . .
H00V H 0.331010 0.390762 0.585316 0.028 Uiso 1 1 calc R . . . .
C00W C 0.42865(8) 0.42230(11) 0.40058(10) 0.0218(3) Uani 1 1 d . . . . .
H00H H 0.440503 0.433287 0.457481 0.026 Uiso 1 1 calc R . . . .
H00I H 0.430841 0.479038 0.374508 0.026 Uiso 1 1 calc R . . . .
C00X C 0.25128(10) 0.41290(11) 0.63413(10) 0.0264(4) Uani 1 1 d . . . . .
C00Y C 0.47924(9) 0.75063(12) 0.38886(11) 0.0265(4) Uani 1 1 d . . . . .
C00Z C 0.48229(8) 0.36129(11) 0.38391(10) 0.0235(3) Uani 1 1 d . . . . .
H00J H 0.468091 0.344247 0.328164 0.028 Uiso 1 1 calc R . . . .
H00K H 0.485285 0.307480 0.415641 0.028 Uiso 1 1 calc R . . . .
C010 C 0.60423(9) 0.35296(13) 0.37202(12) 0.0311(4) Uani 1 1 d . . . . .
H01A H 0.585840 0.345281 0.315494 0.047 Uiso 1 1 calc GR . . . .
H01B H 0.611373 0.295488 0.397417 0.047 Uiso 1 1 calc GR . . . .
H01C H 0.648434 0.384291 0.383257 0.047 Uiso 1 1 calc GR . . . .
C011 C 0.27074(9) 0.28791(12) 0.41257(11) 0.0267(4) Uani 1 1 d . . . . .
H01D H 0.249295 0.266323 0.358985 0.032 Uiso 1 1 calc R . . . .
H01E H 0.245582 0.341205 0.420765 0.032 Uiso 1 1 calc R . . . .
C012 C 0.17264(9) 0.52688(11) 0.57551(10) 0.0242(3) Uani 1 1 d . . . . .
H012 H 0.133023 0.561736 0.573449 0.029 Uiso 1 1 calc R . . . .
C013 C 0.16259(9) 0.78184(12) 0.55738(10) 0.0259(3) Uani 1 1 d . . . . .
H01R H 0.143298 0.738703 0.587219 0.031 Uiso 1 1 calc R . . . .
H01S H 0.145344 0.840468 0.566592 0.031 Uiso 1 1 calc R . . . .
C014 C 0.55302(9) 0.40552(12) 0.40293(11) 0.0259(4) Uani 1 1 d . . . . .
H01F H 0.548022 0.464792 0.379573 0.031 Uiso 1 1 calc R . . . .
H01G H 0.571190 0.411975 0.460216 0.031 Uiso 1 1 calc R . . . .
C015 C 0.19336(10) 0.46193(12) 0.63260(11) 0.0274(4) Uani 1 1 d . . . . .
H015 H 0.167964 0.451852 0.669579 0.033 Uiso 1 1 calc R . . . .
C016 C 0.05998(9) 0.74931(12) 0.44994(10) 0.0254(3) Uani 1 1 d . . . . .
H01T H 0.039147 0.803152 0.464627 0.030 Uiso 1 1 calc R . . . .
H01U H 0.048767 0.700416 0.480861 0.030 Uiso 1 1 calc R . . . .
C018 C 0.02714(9) 0.73114(13) 0.36430(10) 0.0277(4) Uani 1 1 d . . . . .
H01V H 0.051123 0.681349 0.347447 0.033 Uiso 1 1 calc R . . . .
H01W H 0.032463 0.783083 0.333219 0.033 Uiso 1 1 calc R . . . .
C019 C 0.30839(11) 0.42507(14) 0.15107(11) 0.0341(4) Uani 1 1 d . . . . .
H01H H 0.258422 0.435540 0.144051 0.041 Uiso 1 1 calc R . . . .
H01I H 0.314262 0.363409 0.136982 0.041 Uiso 1 1 calc R . . . .
C01A C 0.26492(11) 0.21807(14) 0.47145(13) 0.0368(4) Uani 1 1 d . . . . .
H01J H 0.285629 0.162989 0.459047 0.044 Uiso 1 1 calc R . . . .
H01K H 0.291858 0.236906 0.524208 0.044 Uiso 1 1 calc R . . . .
C01B C 0.26609(10) 0.78885(13) 0.67624(11) 0.0312(4) Uani 1 1 d . . . . .
H01X H 0.316911 0.797090 0.691707 0.037 Uiso 1 1 calc R . . . .
H01Y H 0.245205 0.841873 0.692321 0.037 Uiso 1 1 calc R . . . .
C01C C -0.04973(10) 0.70956(14) 0.34917(12) 0.0328(4) Uani 1 1 d . . . . .
H01Z H -0.054680 0.655869 0.378304 0.039 Uiso 1 1 calc R . . . .
H H -0.072947 0.757988 0.369004 0.039 Uiso 1 1 calc R . . . .
C01D C 0.24099(9) 0.78089(13) 0.58715(11) 0.0296(4) Uani 1 1 d . . . . .
H01 H 0.260025 0.830035 0.563272 0.036 Uiso 1 1 calc R . . . .
HA H 0.258753 0.725660 0.570853 0.036 Uiso 1 1 calc R . . . .
C01E C 0.24888(11) 0.71059(14) 0.72024(12) 0.0365(4) Uani 1 1 d . . . . .
H0AA H 0.265417 0.656872 0.701215 0.055 Uiso 1 1 calc GR . . . .
HB H 0.198651 0.707096 0.711729 0.055 Uiso 1 1 calc GR . . . .
HC H 0.271481 0.717374 0.776130 0.055 Uiso 1 1 calc GR . . . .
C01F C -0.08512(11) 0.69578(18) 0.26314(13) 0.0448(5) Uani 1 1 d . . . . .
H1AA H -0.081991 0.749576 0.234328 0.067 Uiso 1 1 calc GR . . . .
HD H -0.133892 0.681015 0.256287 0.067 Uiso 1 1 calc GR . . . .
HE H -0.062339 0.647849 0.243235 0.067 Uiso 1 1 calc GR . . . .
C01G C 0.13786(12) 0.91688(13) 0.42412(17) 0.0459(6) Uani 1 1 d . . . . .
H2AA H 0.162371 0.942711 0.475192 0.055 Uiso 1 1 calc R . . . .
HF H 0.087656 0.917199 0.419702 0.055 Uiso 1 1 calc R . . . .
C01H C 0.33431(15) 0.48570(16) 0.09698(13) 0.0493(6) Uani 1 1 d . . . . .
H01L H 0.304881 0.479161 0.043429 0.074 Uiso 1 1 calc GR . . . .
H01M H 0.382107 0.470342 0.098908 0.074 Uiso 1 1 calc GR . . . .
H01N H 0.332575 0.546499 0.113915 0.074 Uiso 1 1 calc GR . . . .
C01I C 0.19116(12) 0.20054(19) 0.47223(15) 0.0519(6) Uani 1 1 d . . . . .
H01O H 0.163686 0.184207 0.419663 0.078 Uiso 1 1 calc GR . . . .
H01P H 0.171609 0.253415 0.489003 0.078 Uiso 1 1 calc GR . . . .
H01Q H 0.190317 0.152616 0.508530 0.078 Uiso 1 1 calc GR . . . .
C01K C 0.22577(16) 0.98017(18) 0.36039(15) 0.0565(7) Uani 1 1 d . . . . .
H3AA H 0.230482 1.021471 0.320071 0.085 Uiso 1 1 calc GR . . . .
HG H 0.243548 0.922760 0.350681 0.085 Uiso 1 1 calc GR . . . .
HH H 0.252192 1.001587 0.411779 0.085 Uiso 1 1 calc GR . . . .
C01L C 0.15190(15) 0.97214(17) 0.35835(19) 0.0610(8) Uani 1 1 d . . . . .
H4AA H 0.126530 0.946029 0.307723 0.073 Uiso 1 1 calc R . . . .
HI H 0.132955 1.031582 0.360777 0.073 Uiso 1 1 calc R . . . .
Cl Cl 0.0594(3) 0.4192(4) 0.0639(3) 0.0348(14) Uani 0.0955(17) 1 d . . 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
V001 O005 1.9448(11) . ?
V001 O006 1.9307(11) . ?
V001 O007 1.9612(11) . ?
V001 O008 1.9371(11) . ?
V001 O009 1.9227(11) . ?
V001 O00A 1.9552(11) . ?
Cl00 C00K 1.7547(17) . ?
Cl1 C00Y 1.7554(18) . ?
Cl2 C00X 1.7532(17) . ?
O005 C00G 1.3333(19) . ?
O006 C00H 1.3324(19) . ?
O007 C00I 1.3434(19) . ?
O008 C00D 1.3329(19) . ?
O009 C00F 1.3362(19) . ?
O00A C00M 1.339(2) . ?
N00B C00L 1.506(2) . ?
N00B C00T 1.507(2) . ?
N00B C00W 1.508(2) . ?
N00C C00U 1.504(2) . ?
N00C C013 1.509(2) . ?
N00C C016 1.504(2) . ?
C00D C00F 1.416(2) . ?
C00D C00P 1.389(2) . ?
C00F C00O 1.384(2) . ?
C00G C00H 1.412(2) . ?
C00G C00R 1.390(2) . ?
C00H C00J 1.393(2) . ?
C00I C00M 1.412(2) . ?
C00I C012 1.385(2) . ?
C00J C00K 1.398(2) . ?
C00K C00N 1.380(3) . ?
C00L C00Q 1.520(3) . ?
C00M C00V 1.392(2) . ?
C00N C00R 1.399(2) . ?
C00N Cl 1.682(5) . ?
C00O C00S 1.397(3) . ?
C00P C00Y 1.396(2) . ?
C00Q C019 1.524(2) . ?
C00S C00Y 1.382(3) . ?
C00T C011 1.513(2) . ?
C00U C01G 1.519(3) . ?
C00V C00X 1.391(3) . ?
C00W C00Z 1.515(2) . ?
C00X C015 1.378(3) . ?
C00Z C014 1.525(2) . ?
C010 C014 1.522(3) . ?
C011 C01A 1.523(3) . ?
C012 C015 1.400(2) . ?
C013 C01D 1.518(2) . ?
C016 C018 1.513(2) . ?
C018 C01C 1.529(3) . ?
C019 C01H 1.527(3) . ?
C01A C01I 1.510(3) . ?
C01B C01D 1.533(2) . ?
C01B C01E 1.520(3) . ?
C01C C01F 1.517(3) . ?
C01G C01L 1.532(4) . ?
C01K C01L 1.480(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O005 V001 O007 105.24(5) . . ?
O005 V001 O00A 85.63(5) . . ?
O006 V001 O005 80.83(5) . . ?
O006 V001 O007 86.08(5) . . ?
O006 V001 O008 107.92(5) . . ?
O006 V001 O00A 157.83(5) . . ?
O008 V001 O005 87.29(5) . . ?
O008 V001 O007 162.77(5) . . ?
O008 V001 O00A 88.76(5) . . ?
O009 V001 O005 163.97(5) . . ?
O009 V001 O006 93.02(5) . . ?
O009 V001 O007 88.97(5) . . ?
O009 V001 O008 80.50(5) . . ?
O009 V001 O00A 104.32(5) . . ?
O00A V001 O007 80.62(5) . . ?
C00G O005 V001 115.14(10) . . ?
C00H O006 V001 115.26(10) . . ?
C00I O007 V001 114.98(10) . . ?
C00D O008 V001 115.57(10) . . ?
C00F O009 V001 116.06(10) . . ?
C00M O00A V001 114.74(10) . . ?
C00L N00B C00T 111.35(13) . . ?
C00L N00B C00W 113.36(13) . . ?
C00T N00B C00W 111.16(13) . . ?
C00U N00C C013 113.87(13) . . ?
C00U N00C C016 114.10(13) . . ?
C016 N00C C013 108.73(13) . . ?
O008 C00D C00F 113.97(14) . . ?
O008 C00D C00P 125.09(15) . . ?
C00P C00D C00F 120.93(15) . . ?
O009 C00F C00D 113.68(14) . . ?
O009 C00F C00O 126.47(15) . . ?
C00O C00F C00D 119.85(15) . . ?
O005 C00G C00H 114.02(14) . . ?
O005 C00G C00R 125.69(15) . . ?
C00R C00G C00H 120.29(15) . . ?
O006 C00H C00G 114.74(13) . . ?
O006 C00H C00J 124.82(14) . . ?
C00J C00H C00G 120.44(15) . . ?
O007 C00I C00M 114.18(14) . . ?
O007 C00I C012 124.92(15) . . ?
C012 C00I C00M 120.88(15) . . ?
C00H C00J C00K 117.80(15) . . ?
C00J C00K Cl00 118.39(13) . . ?
C00N C00K Cl00 119.05(13) . . ?
C00N C00K C00J 122.56(15) . . ?
N00B C00L C00Q 114.36(13) . . ?
O00A C00M C00I 115.27(14) . . ?
O00A C00M C00V 124.91(15) . . ?
C00V C00M C00I 119.82(15) . . ?
C00K C00N C00R 119.36(16) . . ?
C00K C00N Cl 121.5(2) . . ?
C00R C00N Cl 116.1(2) . . ?
C00F C00O C00S 119.79(17) . . ?
C00D C00P C00Y 117.47(16) . . ?
C00L C00Q C019 110.82(15) . . ?
C00G C00R C00N 119.54(16) . . ?
C00Y C00S C00O 119.29(16) . . ?
N00B C00T C011 113.24(14) . . ?
N00C C00U C01G 113.99(16) . . ?
C00X C00V C00M 117.81(15) . . ?
N00B C00W C00Z 114.14(13) . . ?
C00V C00X Cl2 117.97(14) . . ?
C015 C00X Cl2 118.73(14) . . ?
C015 C00X C00V 123.29(16) . . ?
C00P C00Y Cl1 118.08(15) . . ?
C00S C00Y Cl1 119.29(14) . . ?
C00S C00Y C00P 122.62(16) . . ?
C00W C00Z C014 110.71(14) . . ?
C00T C011 C01A 110.22(15) . . ?
C00I C012 C015 119.46(16) . . ?
N00C C013 C01D 112.39(14) . . ?
C010 C014 C00Z 111.53(15) . . ?
C00X C015 C012 118.73(16) . . ?
N00C C016 C018 114.40(14) . . ?
C016 C018 C01C 110.93(15) . . ?
C00Q C019 C01H 111.25(18) . . ?
C01I C01A C011 113.05(18) . . ?
C01E C01B C01D 114.51(16) . . ?
C01F C01C C018 112.26(17) . . ?
C013 C01D C01B 112.09(15) . . ?
C00U C01G C01L 110.7(2) . . ?
C01K C01L C01G 114.9(2) . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 67.2 electrons were 
found in a volume of 263.0Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1.6[C4H8O] per Formula Unit 
which account for 64 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 0.000 263.0 67.2 ?
2 0.000 0.500 0.500 263.0 67.2 ?
3 0.500 0.000 0.500 311.1 126.2 ?
4 0.500 0.500 1.000 311.1 126.2 ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: HMDSO, THF'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_Complex6_99K
_database_code_depnum_ccdc_archive 'CCDC 2159051'
loop_
_audit_author_name
_audit_author_address
'Roxanna Martinez'
;Colorado State University
United States of America
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_audit_creation_date             2021-12-15
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 Cl12 O6 V, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Cl12 N2 O6 V'
_chemical_formula_weight         1161.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         C41H51Cl12N3O6V
_chemical_oxdiff_usercomment     'Crystallized from THF/HMDSO.'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.54130(10)
_cell_length_b                   12.30200(10)
_cell_length_c                   19.1790(2)
_cell_angle_alpha                95.5380(10)
_cell_angle_beta                 106.4910(10)
_cell_angle_gamma                95.7900(10)
_cell_volume                     2575.27(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    37794
_cell_measurement_temperature    99.9(7)
_cell_measurement_theta_max      77.9070
_cell_measurement_theta_min      3.6320
_shelx_estimated_absorpt_T_max   0.681
_shelx_estimated_absorpt_T_min   0.443
_exptl_absorpt_coefficient_mu    7.717
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.588
_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            'dark blue'
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1194
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 4 6 0.0167
-1 7 -6 0.0190
-7 0 7 0.0514
3 -7 3 0.0388
7 -2 -6 0.0554
0 -3 -10 0.0145
-7 -3 4 0.0497

_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.054
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
3.7138 3.7235 5.6765 0.2218 0.9253 0.3076
-0.9273 7.2381 -5.9532 0.9062 -0.2172 0.3628
-7.0701 0.0046 7.2320 0.2584 -0.0621 -0.9640
3.2442 -7.0812 3.4322 -0.9718 0.2330 -0.0362
7.2593 -1.8515 -5.6642 -0.4880 0.1171 0.8650
-0.3015 -2.7468 -10.3861 -0.2266 -0.9455 0.2338
-6.5165 -3.2128 3.5283 -0.1060 -0.4408 -0.8913

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60728
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.171
_diffrn_reflns_theta_min         2.424
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  23.00   0.50    1.60    --  -48.30  90.00 152.00  194
  2  ω      6.00  56.00   0.50    1.60    --   48.30 -90.00  38.00  100
  3  ω   -143.00-118.00   0.50    6.41    --  -86.25 -90.00  38.00   50
  4  ω    -71.00 -46.00   0.50    6.41    --  -86.25  90.00 152.00   50
  5  ω     37.00  86.00   0.50    6.41    --  107.75 -90.00  38.00   98
  6  ω    132.00 157.00   0.50    6.41    --  107.75  90.00 152.00   50
  7  ω    -18.00   8.00   0.50    1.60    --  -48.30  19.00  60.00   52
  8  ω    -41.00  19.00   0.50    1.60    --  -48.30  37.00 150.00  120
  9  ω   -119.00 -75.00   0.50    1.60    --  -48.30-125.00 150.00   88
 10  ω    -42.00  24.00   0.50    1.60    --  -48.30  37.00  90.00  132
 11  ω   -118.00 -89.00   0.50    1.60    --  -48.30-125.00 120.00   58
 12  ω    -24.00  19.00   0.50    1.60    --   48.30 -19.00 120.00   86
 13  ω     38.00 117.00   0.50    1.60    --   48.30  57.00   0.00  158
 14  ω    -50.00 -18.00   0.50    6.41    --  -86.25  45.00 -30.00   64
 15  ω    -50.00 -17.00   0.50    6.41    --  -86.25  45.00   0.00   66
 16  ω     39.00  69.00   0.50    6.41    --  107.75 -77.00  60.00   60
 17  ω     37.00  66.00   0.50    6.41    --  107.75 -61.00 150.00   58
 18  ω     60.00  95.00   0.50    6.41    --  107.75 -75.00  76.87   70
 19  ω    130.00 167.00   0.50    6.41    --  107.75 125.00  30.00   74
 20  ω     50.00  76.00   0.50    6.41    --  107.75 -94.00  90.00   52
 21  ω     38.00  72.00   0.50    6.41    --  107.75 -94.00  30.00   68
 22  ω     43.00  69.00   0.50    6.41    --  107.75-104.00  -6.58   52
 23  ω     46.00 101.00   0.50    6.41    --  107.75 -94.00-120.00  110
 24  ω    136.00 168.00   0.50    6.41    --  107.75  77.00 -90.00   64
 25  ω    146.00 175.00   0.50    6.41    --  107.75  61.00-150.00   58
 26  ω     88.00 132.00   0.50    6.41    --  107.75  77.00 -90.00   88
 27  ω    126.00 167.00   0.50    6.41    --  107.75  30.00-150.00   82
 28  ω     65.00  98.00   0.50    6.41    --  107.75 -94.00-150.00   66
 29  ω     64.00  96.00   0.50    6.41    --  107.75 -77.00 -60.00   64
 30  ω     80.00 106.00   0.50    6.41    --  107.75 -94.00  30.00   52
 31  ω     93.00 119.00   0.50    6.41    --  107.75  63.00-112.50   52
 32  ω    126.00 176.00   0.50    6.41    --  107.75  63.00-112.50  100
 33  ω    104.00 130.00   0.50    6.41    --  107.75  61.00 -30.00   52
 34  ω     39.00  65.00   0.50    6.41    --  107.75 -77.00-150.00   52
 35  ω     81.00 107.00   0.50    6.41    --  107.75-106.00 124.27   52
 36  ω     38.00 108.00   0.50    6.41    --  107.75-107.00 -29.29  140
 37  ω    105.00 155.00   0.50    6.41    --  107.75  30.00 120.00  100
 38  ω     81.00 106.00   0.50    6.41    --  107.75 -94.00 120.00   50
 39  ω    145.00 178.00   0.50    6.41    --  107.75  80.00 -48.49   66
 40  ω    117.00 142.00   0.50    6.41    --  107.75  80.00 -48.49   50
 41  ω     42.00  68.00   0.50    6.41    --  107.75 -94.00 120.00   52
 42  ω     40.00  69.00   0.50    6.41    --  107.75 -61.00 -90.00   58
 43  ω    102.00 128.00   0.50    6.41    --  107.75  81.00 -66.32   52
 44  ω     95.00 141.00   0.50    6.41    --  107.75  61.00-150.00   92
 45  ω    102.00 128.00   0.50    6.41    --  107.75 -85.00 118.70   52
 46  ω     73.00 106.00   0.50    6.41    --  107.75 -94.00-180.00   66
 47  ω     93.00 143.00   0.50    6.41    --  107.75  76.00  98.11  100
 48  ω     72.00 118.00   0.50    6.41    --  107.75 -85.00  -3.28   92
 49  ω    105.00 177.00   0.50    6.41    --  107.75  77.00  30.00  144
 50  ω    103.00 132.00   0.50    6.41    --  107.75  30.00 -90.00   58
 51  ω    139.00 167.00   0.50    6.41    --  107.75  30.00 -90.00   56
 52  ω    110.00 154.00   0.50    6.41    --  107.75  77.00 -60.00   88
 53  ω     86.00 178.00   0.50    6.41    --  107.75  77.00-180.00  184
 54  ω    151.00 177.00   0.50    6.41    --  107.75  30.00-180.00   52
 55  ω     71.00 104.00   0.50    6.41    --  107.75 -94.00  60.00   66
 56  ω     62.00 107.00   0.50    6.41    --  107.75-100.00 -96.83   90
 57  ω     79.00 111.00   0.50    6.41    --  107.75-125.00-180.00   64
 58  ω     66.00  92.00   0.50    6.41    --  107.75-130.00  91.03   52
 59  ω    126.00 173.00   0.50    6.41    --  107.75  45.00  30.00   94
 60  ω    149.00 175.00   0.50    6.41    --  107.75 125.00-180.00   52
 61  ω     82.00 108.00   0.50    6.41    --  107.75-125.00-150.00   52
 62  ω    136.00 162.00   0.50    6.41    --  107.75 104.00  12.49   52
 63  ω    148.00 174.00   0.50    6.41    --  107.75  61.00 -30.00   52
 64  ω     45.00  72.00   0.50    6.41    --  107.75 -83.00 -25.02   54
 65  ω    101.00 131.00   0.50    6.41    --  107.75 -83.00 -25.02   60
 66  ω     37.00  89.00   0.50    6.41    --  107.75 -94.00 -60.00  104
 67  ω     64.00 106.00   0.50    6.41    --  107.75 -94.00 -30.00   84
 68  ω     39.00 106.00   0.50    6.41    --  107.75 -98.00  10.83  134
 69  ω     97.00 132.00   0.50    6.41    --  107.75  30.00-180.00   70
 70  ω    126.00 177.00   0.50    6.41    --  107.75  97.00 132.32  102
 71  ω     77.00 111.00   0.50    6.41    --  107.75-125.00-120.00   68
 72  ω     79.00 108.00   0.50    6.41    --  107.75-125.00 -30.00   58
 73  ω    105.00 138.00   0.50    6.41    --  107.75  45.00  90.00   66
 74  ω    105.00 136.00   0.50    6.41    --  107.75 125.00-150.00   62
 75  ω    142.00 174.00   0.50    6.41    --  107.75 125.00-150.00   64
 76  ω     95.00 154.00   0.50    6.41    --  107.75 125.00-120.00  118
 77  ω    153.00 178.00   0.50    6.41    --  107.75 125.00   0.00   50
 78  ω    101.00 146.00   0.50    6.41    --  107.75 125.00  90.00   90
 79  ω     96.00 136.00   0.50    6.41    --  107.75 125.00 120.00   80
 80  ω    139.00 165.00   0.50    6.41    --  107.75 125.00 150.00   52
 81  ω    143.00 169.00   0.50    6.41    --  107.75  55.00 -71.34   52
 82  ω     94.00 119.00   0.50    6.41    --  107.75  61.00-120.00   50
 83  ω     87.00 113.00   0.50    6.41    --  107.75  77.00 120.00   52
 84  ω     87.00 122.00   0.50    6.41    --  107.75  77.00 150.00   70
 85  ω     42.00  67.00   0.50    6.41    --  107.75 -77.00 150.00   50
 86  ω     36.00  66.00   0.50    6.41    --  107.75 -94.00 150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0436631000
_diffrn_orient_matrix_UB_12      0.1138314000
_diffrn_orient_matrix_UB_13      -0.0070220000
_diffrn_orient_matrix_UB_21      0.0873508000
_diffrn_orient_matrix_UB_22      0.0443348000
_diffrn_orient_matrix_UB_23      0.0767768000
_diffrn_orient_matrix_UB_31      0.1009907000
_diffrn_orient_matrix_UB_32      0.0346075000
_diffrn_orient_matrix_UB_33      -0.0345916000
_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              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9766
_reflns_number_total             10949
_reflns_odcompleteness_completeness 98.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.89
_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 1.171.41.117a (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 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         10949
_refine_ls_number_restraints     876
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      1.063
_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)+(0.0399P)²+2.8170P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1123
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C38, C37B}
3. Restrained distances
 N1-H1
 0.88 with sigma of 0.02
 N2-H2
 0.83 with sigma of 0.02
 N2B-H2B
 0.83 with sigma of 0.02
 N2-C35 \\sim N2-C31 \\sim N2-C40B \\sim N2B-C39B \\sim N2B-C35B \\sim N2B-C31B
 with sigma of 0.02
 C40-C40B \\sim C39B-C40B \\sim C41-C40 \\sim C31-C32 \\sim C32B-C31B \\sim
C32B-C33 \\sim C32-C33 ~
 C37-C36 \\sim C35B-C36B \\sim C36B-C37B \\sim C37B-C37
 with sigma of 0.02
 C38B-C37B \\sim C33-C34 \\sim C42B-C41B \\sim C41-C42
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C42) = Uanis(C38B)
Uanis(C38) = Uanis(C37B)
5. Rigid body (RIGU) restrains
 C33, C34, C40B, N2, C31, C32, C35, C36, C37, C40, C41, C42, N2B, C31B, C32B,
 C35B, C36B, C37B, C38B, C39B, C41B, C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=
 Sof(H29D)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(H33C)=Sof(H33D)=Sof(H40C)=Sof(H40D)=Sof(N2B)=Sof(H2B)=Sof(C31B)=Sof(H31C)=
 Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C35B)=Sof(H35C)=Sof(H35D)=
 Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(C38B)=
 Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39B)=Sof(H39A)=Sof(H39B)=Sof(C41B)=
 Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(H33A)=Sof(H33B)=Sof(H40A)=Sof(H40B)=Sof(N2)=Sof(H2)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=
 Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H38C)=Sof(C40)=Sof(H40E)=Sof(H40F)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(H42C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C27(H27A,H27B), C27(H27C,H27D), C28(H28A,H28B),
 C29(H29A,H29B), C28B(H28C,H28D), C29B(H29C,H29D), C33(H33A,H33B), C33(H33C,
 H33D), C40B(H40A,H40B), C40B(H40C,H40D), C31(H31A,H31B), C32(H32A,H32B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C40(H40E,H40F), C41(H41A,H41B),
  C31B(H31C,H31D), C32B(H32C,H32D), C35B(H35C,H35D), C36B(H36C,H36D), C37B(H37C,
 H37D), C39B(H39A,H39B), C41B(H41C,H41D)
7.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C30B(H30D,H30E,
 H30F), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C),
 C38B(H38D,H38E,H38F), C42B(H42D,H42E,H42F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V V 0.61214(4) 0.70568(3) 0.24511(2) 0.03163(10) Uani 1 1 d . U . . .
Cl1 Cl 0.73572(7) 1.09728(5) 0.22393(4) 0.04766(16) Uani 1 1 d . U . . .
Cl2 Cl 0.92340(7) 1.11418(6) 0.13387(4) 0.05237(18) Uani 1 1 d . U . . .
Cl3 Cl 0.98420(7) 0.90028(7) 0.05785(5) 0.05423(19) Uani 1 1 d . U . . .
Cl4 Cl 0.86206(6) 0.66957(5) 0.07534(4) 0.04245(15) Uani 1 1 d . U . . .
Cl5 Cl 0.98583(7) 0.70807(6) 0.45078(4) 0.04834(16) Uani 1 1 d . U . . .
Cl6 Cl 0.93169(10) 0.73998(7) 0.60317(4) 0.0678(2) Uani 1 1 d . U . . .
Cl7 Cl 0.66517(12) 0.75672(8) 0.60791(6) 0.0809(3) Uani 1 1 d . U . . .
Cl8 Cl 0.45726(9) 0.76099(7) 0.46137(6) 0.0738(3) Uani 1 1 d . U . . .
Cl9 Cl 0.18116(6) 0.67238(5) 0.09546(5) 0.05010(17) Uani 1 1 d . U . . .
Cl10 Cl 0.05029(6) 0.43000(5) 0.07732(4) 0.04436(15) Uani 1 1 d . U . . .
Cl11 Cl 0.19541(6) 0.24929(5) 0.14908(5) 0.05073(18) Uani 1 1 d . U . . .
Cl12 Cl 0.47317(6) 0.30705(5) 0.23584(5) 0.04920(17) Uani 1 1 d . U . . .
O1 O 0.64055(15) 0.85925(13) 0.22986(10) 0.0342(4) Uani 1 1 d . U . . .
O2 O 0.70625(14) 0.68630(13) 0.17748(9) 0.0308(3) Uani 1 1 d . U . . .
O3 O 0.75958(15) 0.70508(13) 0.32446(10) 0.0338(3) Uani 1 1 d . U . . .
O4 O 0.54939(17) 0.73679(14) 0.32847(12) 0.0420(4) Uani 1 1 d . U . . .
O5 O 0.44674(15) 0.69624(14) 0.18301(12) 0.0401(4) Uani 1 1 d . U . . .
O6 O 0.57028(15) 0.54546(13) 0.23287(11) 0.0385(4) Uani 1 1 d . U . . .
C1 C 0.7207(2) 0.87681(19) 0.19280(13) 0.0307(5) Uani 1 1 d . U . . .
C2 C 0.7717(2) 0.9795(2) 0.18281(14) 0.0350(5) Uani 1 1 d . U . . .
C3 C 0.8552(2) 0.9866(2) 0.14242(15) 0.0382(5) Uani 1 1 d . U . . .
C4 C 0.8846(2) 0.8920(2) 0.10989(14) 0.0368(5) Uani 1 1 d . U . . .
C5 C 0.8324(2) 0.7880(2) 0.11880(13) 0.0321(5) Uani 1 1 d . U . . .
C6 C 0.7549(2) 0.78055(19) 0.16218(13) 0.0291(4) Uani 1 1 d . U . . .
C7 C 0.7481(3) 0.72062(19) 0.39132(15) 0.0373(5) Uani 1 1 d . U . . .
C8 C 0.8407(3) 0.7233(2) 0.45558(16) 0.0433(6) Uani 1 1 d . U . . .
C9 C 0.8160(3) 0.7366(2) 0.52318(17) 0.0517(7) Uani 1 1 d . U . . .
C10 C 0.6976(4) 0.7465(2) 0.52496(19) 0.0566(9) Uani 1 1 d . U . . .
C11 C 0.6046(3) 0.7464(2) 0.46019(19) 0.0505(8) Uani 1 1 d . U . . .
C12 C 0.6290(3) 0.73538(19) 0.39344(17) 0.0416(6) Uani 1 1 d . U . . .
C13 C 0.3840(2) 0.59538(19) 0.16989(15) 0.0357(5) Uani 1 1 d . U . . .
C14 C 0.2617(2) 0.5697(2) 0.13145(15) 0.0376(5) Uani 1 1 d . U . . .
C15 C 0.2036(2) 0.4614(2) 0.12371(15) 0.0370(5) Uani 1 1 d . U . . .
C16 C 0.2691(2) 0.3803(2) 0.15426(16) 0.0378(5) Uani 1 1 d . U . . .
C17 C 0.3935(2) 0.4056(2) 0.19192(16) 0.0376(5) Uani 1 1 d . U . . .
C18 C 0.4526(2) 0.51233(19) 0.19909(16) 0.0359(5) Uani 1 1 d . U . . .
N1 N 0.8105(2) 0.46904(18) 0.22814(13) 0.0394(5) Uani 1 1 d D U . . .
H1 H 0.749(2) 0.507(2) 0.2232(18) 0.047 Uiso 1 1 d D U . . .
C19 C 0.7936(2) 0.3894(2) 0.28033(15) 0.0369(5) Uani 1 1 d . U . . .
H19A H 0.859985 0.342755 0.287979 0.044 Uiso 1 1 calc R U . . .
H19B H 0.715438 0.340532 0.257892 0.044 Uiso 1 1 calc R U . . .
C20 C 0.7932(3) 0.4458(2) 0.35393(17) 0.0442(6) Uani 1 1 d . U . . .
H20A H 0.733978 0.499556 0.346084 0.053 Uiso 1 1 calc R U . . .
H20B H 0.875006 0.486907 0.379374 0.053 Uiso 1 1 calc R U . . .
C21 C 0.7600(3) 0.3643(3) 0.40244(17) 0.0498(7) Uani 1 1 d . U . . .
H21A H 0.677923 0.323465 0.377371 0.060 Uiso 1 1 calc R U . . .
H21B H 0.819017 0.310343 0.410399 0.060 Uiso 1 1 calc R U . . .
C22 C 0.7609(4) 0.4232(3) 0.4762(2) 0.0641(9) Uani 1 1 d . U . . .
H22A H 0.840998 0.466468 0.500056 0.096 Uiso 1 1 calc R U . . .
H22B H 0.744469 0.368617 0.507390 0.096 Uiso 1 1 calc R U . . .
H22C H 0.697953 0.472292 0.468667 0.096 Uiso 1 1 calc R U . . .
C23 C 0.9279(3) 0.5474(2) 0.25626(16) 0.0401(6) Uani 1 1 d . U . . .
H23A H 0.923496 0.598427 0.298373 0.048 Uiso 1 1 calc R U . . .
H23B H 0.935757 0.592117 0.217186 0.048 Uiso 1 1 calc R U . . .
C24 C 1.0404(2) 0.4912(2) 0.28013(14) 0.0375(5) Uani 1 1 d . U . . .
H24A H 1.041502 0.434913 0.239890 0.045 Uiso 1 1 calc R U . . .
H24B H 1.037890 0.453370 0.323036 0.045 Uiso 1 1 calc R U . . .
C25 C 1.1566(3) 0.5742(3) 0.30036(16) 0.0497(7) Uani 1 1 d . U . . .
H25A H 1.161984 0.607704 0.256289 0.060 Uiso 1 1 calc R U . . .
H25B H 1.151975 0.633841 0.337597 0.060 Uiso 1 1 calc R U . . .
C26 C 1.2703(3) 0.5215(3) 0.33020(17) 0.0579(8) Uani 1 1 d . U . . .
H26A H 1.269897 0.495719 0.376903 0.087 Uiso 1 1 calc R U . . .
H26B H 1.342530 0.575836 0.338002 0.087 Uiso 1 1 calc R U . . .
H26C H 1.272307 0.458934 0.295036 0.087 Uiso 1 1 calc R U . . .
C27 C 0.7957(2) 0.4095(2) 0.15350(15) 0.0433(6) Uani 1 1 d . U . . .
H27A H 0.835546 0.341798 0.157918 0.052 Uiso 0.688(8) 1 calc R U P A 1
H27B H 0.833832 0.457157 0.125106 0.052 Uiso 0.688(8) 1 calc R U P A 1
H27C H 0.852234 0.353357 0.161649 0.052 Uiso 0.312(8) 1 calc R U P A 2
H27D H 0.829568 0.463927 0.127214 0.052 Uiso 0.312(8) 1 calc R U P A 2
C28 C 0.6605(6) 0.3802(8) 0.1152(4) 0.064(2) Uani 0.688(8) 1 d . U P A 1
H28A H 0.619372 0.446620 0.117743 0.077 Uiso 0.688(8) 1 calc R U P A 1
H28B H 0.625183 0.324556 0.140125 0.077 Uiso 0.688(8) 1 calc R U P A 1
C29 C 0.6399(4) 0.3346(5) 0.0357(2) 0.0570(14) Uani 0.688(8) 1 d . U P A 1
H29A H 0.687051 0.272039 0.033568 0.068 Uiso 0.688(8) 1 calc R U P A 1
H29B H 0.670365 0.392378 0.010319 0.068 Uiso 0.688(8) 1 calc R U P A 1
C30 C 0.5034(6) 0.2951(10) -0.0044(4) 0.105(4) Uani 0.688(8) 1 d . U P A 1
H30A H 0.474107 0.235086 0.019073 0.158 Uiso 0.688(8) 1 calc R U P A 1
H30B H 0.493327 0.268582 -0.055858 0.158 Uiso 0.688(8) 1 calc R U P A 1
H30C H 0.456321 0.356496 -0.001654 0.158 Uiso 0.688(8) 1 calc R U P A 1
C28B C 0.6732(14) 0.3482(9) 0.0959(8) 0.048(3) Uani 0.312(8) 1 d . U P A 2
H28C H 0.691532 0.289276 0.063286 0.057 Uiso 0.312(8) 1 calc R U P A 2
H28D H 0.618534 0.314435 0.121681 0.057 Uiso 0.312(8) 1 calc R U P A 2
C29B C 0.6109(8) 0.4353(8) 0.0502(5) 0.045(2) Uani 0.312(8) 1 d . U P A 2
H29C H 0.596982 0.495926 0.083535 0.054 Uiso 0.312(8) 1 calc R U P A 2
H29D H 0.665141 0.466917 0.023398 0.054 Uiso 0.312(8) 1 calc R U P A 2
C30B C 0.4912(10) 0.3840(10) -0.0035(6) 0.057(3) Uani 0.312(8) 1 d . U P A 2
H30D H 0.506087 0.332763 -0.041471 0.086 Uiso 0.312(8) 1 calc R U P A 2
H30E H 0.447425 0.441809 -0.026396 0.086 Uiso 0.312(8) 1 calc R U P A 2
H30F H 0.441923 0.343843 0.022222 0.086 Uiso 0.312(8) 1 calc R U P A 2
C33 C 0.1053(3) 0.8809(3) 0.31049(19) 0.0547(7) Uani 1 1 d D U . . .
H33A H 0.055425 0.827191 0.268226 0.066 Uiso 0.503(4) 1 calc R U P B 1
H33B H 0.141013 0.838706 0.350896 0.066 Uiso 0.503(4) 1 calc R U P B 1
H33C H 0.064276 0.842150 0.260474 0.066 Uiso 0.497(4) 1 calc R U P B 2
H33D H 0.126634 0.825172 0.344261 0.066 Uiso 0.497(4) 1 calc R U P B 2
C34 C 0.0222(3) 0.9533(3) 0.3347(2) 0.0667(9) Uani 1 1 d D U . . .
H34A H 0.065852 0.995446 0.382698 0.100 Uiso 1 1 calc R U . . .
H34B H -0.049688 0.907353 0.338461 0.100 Uiso 1 1 calc R U . . .
H34C H -0.003516 1.004292 0.298816 0.100 Uiso 1 1 calc R U . . .
C40B C 0.3389(4) 0.9597(3) 0.16412(19) 0.0675(10) Uani 1 1 d D U . . .
H40A H 0.324798 1.037588 0.170811 0.081 Uiso 0.503(4) 1 calc R U P B 1
H40B H 0.257665 0.915612 0.142269 0.081 Uiso 0.503(4) 1 calc R U P B 1
H40C H 0.338648 0.879229 0.154069 0.081 Uiso 0.497(4) 1 calc R U P B 2
H40D H 0.254472 0.974541 0.159355 0.081 Uiso 0.497(4) 1 calc R U P B 2
N2 N 0.3859(4) 0.9297(3) 0.2359(2) 0.0353(10) Uani 0.503(4) 1 d D U P B 1
H2 H 0.430(5) 0.887(4) 0.224(3) 0.042 Uiso 0.503(4) 1 d D U P B 1
C31 C 0.2962(7) 0.8702(6) 0.2654(4) 0.0392(15) Uani 0.503(4) 1 d D U P B 1
H31A H 0.340689 0.836764 0.308335 0.047 Uiso 0.503(4) 1 calc R U P B 1
H31B H 0.247256 0.809500 0.227554 0.047 Uiso 0.503(4) 1 calc R U P B 1
C32 C 0.2101(9) 0.9421(9) 0.2883(6) 0.042(2) Uani 0.503(4) 1 d D U P B 1
H32A H 0.174089 0.982988 0.247173 0.050 Uiso 0.503(4) 1 calc R U P B 1
H32B H 0.258566 0.997129 0.330191 0.050 Uiso 0.503(4) 1 calc R U P B 1
C35 C 0.4680(5) 1.0266(4) 0.2874(3) 0.0350(11) Uani 0.503(4) 1 d D U P B 1
H35A H 0.522961 1.061527 0.262208 0.042 Uiso 0.503(4) 1 calc R U P B 1
H35B H 0.416868 1.081866 0.298435 0.042 Uiso 0.503(4) 1 calc R U P B 1
C36 C 0.5439(6) 0.9954(5) 0.3584(4) 0.0361(14) Uani 0.503(4) 1 d D U P B 1
H36A H 0.582194 0.929792 0.347554 0.043 Uiso 0.503(4) 1 calc R U P B 1
H36B H 0.489948 0.974822 0.388270 0.043 Uiso 0.503(4) 1 calc R U P B 1
C37 C 0.6437(5) 1.0876(5) 0.4030(3) 0.0368(12) Uani 0.503(4) 1 d D U P B 1
H37A H 0.695301 1.112162 0.372574 0.044 Uiso 0.503(4) 1 calc R U P B 1
H37B H 0.606279 1.151353 0.417977 0.044 Uiso 0.503(4) 1 calc R U P B 1
C38 C 0.7188(3) 1.0475(3) 0.46808(18) 0.0535(7) Uani 0.503(4) 1 d . U P B 1
H38A H 0.668760 1.029070 0.500016 0.080 Uiso 0.503(4) 1 calc R U P B 1
H38B H 0.786261 1.104912 0.494719 0.080 Uiso 0.503(4) 1 calc R U P B 1
H38C H 0.751479 0.981602 0.453094 0.080 Uiso 0.503(4) 1 calc R U P B 1
C40 C 0.4023(6) 0.9509(8) 0.1090(4) 0.0656(19) Uani 0.503(4) 1 d D U P B 1
H40E H 0.413033 0.873443 0.096045 0.079 Uiso 0.503(4) 1 calc R U P B 1
H40F H 0.483202 0.996571 0.126057 0.079 Uiso 0.503(4) 1 calc R U P B 1
C41 C 0.3154(9) 0.9951(10) 0.0423(5) 0.074(3) Uani 0.503(4) 1 d D U P B 1
H41A H 0.296061 0.941224 -0.002526 0.089 Uiso 0.503(4) 1 calc R U P B 1
H41B H 0.238370 1.008969 0.052431 0.089 Uiso 0.503(4) 1 calc R U P B 1
C42 C 0.3859(8) 1.1039(7) 0.0326(5) 0.0748(14) Uani 0.503(4) 1 d D U P B 1
H42A H 0.432680 1.143290 0.080923 0.112 Uiso 0.503(4) 1 calc R U P B 1
H42B H 0.327946 1.150125 0.006706 0.112 Uiso 0.503(4) 1 calc R U P B 1
H42C H 0.441727 1.087169 0.004153 0.112 Uiso 0.503(4) 1 calc R U P B 1
N2B N 0.4307(5) 0.9351(4) 0.3016(3) 0.0473(12) Uani 0.497(4) 1 d D U P B 2
H2B H 0.474(6) 0.888(5) 0.290(4) 0.057 Uiso 0.497(4) 1 d D U P B 2
C31B C 0.3072(7) 0.8768(7) 0.2977(5) 0.0485(19) Uani 0.497(4) 1 d D U P B 2
H31C H 0.317649 0.824650 0.334478 0.058 Uiso 0.497(4) 1 calc R U P B 2
H31D H 0.270904 0.833480 0.248589 0.058 Uiso 0.497(4) 1 calc R U P B 2
C32B C 0.2199(9) 0.9553(10) 0.3113(7) 0.047(3) Uani 0.497(4) 1 d D U P B 2
H32C H 0.201216 1.003657 0.272337 0.057 Uiso 0.497(4) 1 calc R U P B 2
H32D H 0.255257 1.001826 0.359336 0.057 Uiso 0.497(4) 1 calc R U P B 2
C35B C 0.5037(7) 0.9932(6) 0.3758(4) 0.0462(16) Uani 0.497(4) 1 d D U P B 2
H35C H 0.494750 0.945499 0.413182 0.055 Uiso 0.497(4) 1 calc R U P B 2
H35D H 0.468933 1.061508 0.385437 0.055 Uiso 0.497(4) 1 calc R U P B 2
C36B C 0.6373(6) 1.0231(7) 0.3853(3) 0.0499(14) Uani 0.497(4) 1 d D U P B 2
H36C H 0.648367 1.089130 0.360881 0.060 Uiso 0.497(4) 1 calc R U P B 2
H36D H 0.666312 0.961923 0.360294 0.060 Uiso 0.497(4) 1 calc R U P B 2
C37B C 0.7188(3) 1.0475(3) 0.46808(18) 0.0535(7) Uani 0.497(4) 1 d D U P B 2
H37C H 0.710666 1.121311 0.490285 0.064 Uiso 0.497(4) 1 calc R U P B 2
H37D H 0.694748 0.991540 0.496991 0.064 Uiso 0.497(4) 1 calc R U P B 2
C38B C 0.8501(7) 1.0421(7) 0.4656(5) 0.0748(14) Uani 0.497(4) 1 d D U P B 2
H38D H 0.858879 0.966115 0.449533 0.112 Uiso 0.497(4) 1 calc R U P B 2
H38E H 0.907010 1.066442 0.514629 0.112 Uiso 0.497(4) 1 calc R U P B 2
H38F H 0.867996 1.090268 0.431130 0.112 Uiso 0.497(4) 1 calc R U P B 2
C39B C 0.4264(6) 1.0066(6) 0.2436(4) 0.0511(14) Uani 0.497(4) 1 d D U P B 2
H39A H 0.510165 1.023226 0.240011 0.061 Uiso 0.497(4) 1 calc R U P B 2
H39B H 0.401199 1.077263 0.259212 0.061 Uiso 0.497(4) 1 calc R U P B 2
C41B C 0.3897(7) 1.0189(6) 0.1126(4) 0.0534(15) Uani 0.497(4) 1 d D U P B 2
H41C H 0.479108 1.018446 0.129308 0.064 Uiso 0.497(4) 1 calc R U P B 2
H41D H 0.376017 1.096664 0.120387 0.064 Uiso 0.497(4) 1 calc R U P B 2
C42B C 0.3486(10) 0.9841(9) 0.0293(5) 0.062(2) Uani 0.497(4) 1 d D U P B 2
H42D H 0.343620 0.903839 0.019095 0.094 Uiso 0.497(4) 1 calc R U P B 2
H42E H 0.407580 1.019707 0.007829 0.094 Uiso 0.497(4) 1 calc R U P B 2
H42F H 0.268262 1.006373 0.007938 0.094 Uiso 0.497(4) 1 calc R U P B 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
V O1 1.9489(16) . ?
V O2 1.9264(16) . ?
V O3 1.9355(19) . ?
V O4 1.9549(19) . ?
V O5 1.9272(19) . ?
V O6 1.9564(16) . ?
Cl1 C2 1.726(3) . ?
Cl2 C3 1.727(2) . ?
Cl3 C4 1.725(2) . ?
Cl4 C5 1.721(3) . ?
Cl5 C8 1.731(3) . ?
Cl6 C9 1.718(4) . ?
Cl7 C10 1.731(3) . ?
Cl8 C11 1.734(3) . ?
Cl9 C14 1.726(3) . ?
Cl10 C15 1.725(3) . ?
Cl11 C16 1.724(2) . ?
Cl12 C17 1.734(3) . ?
O1 C1 1.330(3) . ?
O2 C6 1.332(3) . ?
O3 C7 1.324(3) . ?
O4 C12 1.324(4) . ?
O5 C13 1.335(3) . ?
O6 C18 1.330(3) . ?
C1 C2 1.393(3) . ?
C1 C6 1.413(3) . ?
C2 C3 1.399(4) . ?
C3 C4 1.385(4) . ?
C4 C5 1.404(3) . ?
C5 C6 1.386(3) . ?
C7 C8 1.378(4) . ?
C7 C12 1.416(4) . ?
C8 C9 1.403(4) . ?
C9 C10 1.393(5) . ?
C10 C11 1.392(5) . ?
C11 C12 1.384(4) . ?
C13 C14 1.382(4) . ?
C13 C18 1.416(4) . ?
C14 C15 1.404(3) . ?
C15 C16 1.387(4) . ?
C16 C17 1.400(4) . ?
C17 C18 1.392(3) . ?
N1 H1 0.879(18) . ?
N1 C19 1.504(3) . ?
N1 C23 1.509(4) . ?
N1 C27 1.500(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.513(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.523(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.522(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.509(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.530(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.512(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 H27C 0.9900 . ?
C27 H27D 0.9900 . ?
C27 C28 1.512(8) . ?
C27 C28B 1.590(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.516(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.548(8) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C28B H28C 0.9900 . ?
C28B H28D 0.9900 . ?
C28B C29B 1.552(16) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C29B C30B 1.504(12) . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 H33C 0.9900 . ?
C33 H33D 0.9900 . ?
C33 C34 1.508(5) . ?
C33 C32 1.543(10) . ?
C33 C32B 1.526(10) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C40B H40A 0.9900 . ?
C40B H40B 0.9900 . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C40B N2 1.429(5) . ?
C40B C40 1.449(8) . ?
C40B C39B 1.585(8) . ?
C40B C41B 1.494(8) . ?
N2 H2 0.82(2) . ?
N2 C31 1.479(8) . ?
N2 C35 1.518(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.521(9) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.502(9) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.528(7) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.465(6) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C40 H40E 0.9900 . ?
C40 H40F 0.9900 . ?
C40 C41 1.566(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.550(12) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
N2B H2B 0.85(2) . ?
N2B C31B 1.508(8) . ?
N2B C35B 1.500(8) . ?
N2B C39B 1.477(8) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C31B C32B 1.521(10) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
C35B H35C 0.9900 . ?
C35B H35D 0.9900 . ?
C35B C36B 1.504(8) . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
C36B C37B 1.581(7) . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C37B C38B 1.537(8) . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
C39B H39A 0.9900 . ?
C39B H39B 0.9900 . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C41B C42B 1.534(10) . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 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
O1 V O4 95.22(7) . . ?
O1 V O6 165.25(8) . . ?
O2 V O1 81.94(7) . . ?
O2 V O3 88.32(7) . . ?
O2 V O4 168.13(8) . . ?
O2 V O5 104.22(8) . . ?
O2 V O6 88.54(7) . . ?
O3 V O1 97.67(7) . . ?
O3 V O4 80.62(8) . . ?
O3 V O6 93.26(7) . . ?
O4 V O6 96.32(8) . . ?
O5 V O1 89.44(7) . . ?
O5 V O3 166.40(8) . . ?
O5 V O4 87.22(9) . . ?
O5 V O6 81.98(7) . . ?
C1 O1 V 113.04(14) . . ?
C6 O2 V 113.82(14) . . ?
C7 O3 V 115.48(16) . . ?
C12 O4 V 114.64(15) . . ?
C13 O5 V 114.13(16) . . ?
C18 O6 V 112.84(14) . . ?
O1 C1 C2 125.8(2) . . ?
O1 C1 C6 114.99(19) . . ?
C2 C1 C6 119.3(2) . . ?
C1 C2 Cl1 119.35(19) . . ?
C1 C2 C3 120.1(2) . . ?
C3 C2 Cl1 120.52(19) . . ?
C2 C3 Cl2 119.8(2) . . ?
C4 C3 Cl2 119.74(19) . . ?
C4 C3 C2 120.5(2) . . ?
C3 C4 Cl3 120.69(19) . . ?
C3 C4 C5 119.9(2) . . ?
C5 C4 Cl3 119.4(2) . . ?
C4 C5 Cl4 120.67(19) . . ?
C6 C5 Cl4 119.54(18) . . ?
C6 C5 C4 119.8(2) . . ?
O2 C6 C1 115.1(2) . . ?
O2 C6 C5 124.5(2) . . ?
C5 C6 C1 120.3(2) . . ?
O3 C7 C8 125.3(2) . . ?
O3 C7 C12 114.5(3) . . ?
C8 C7 C12 120.2(3) . . ?
C7 C8 Cl5 118.8(2) . . ?
C7 C8 C9 119.9(3) . . ?
C9 C8 Cl5 121.3(3) . . ?
C8 C9 Cl6 119.8(3) . . ?
C10 C9 Cl6 120.5(2) . . ?
C10 C9 C8 119.8(3) . . ?
C9 C10 Cl7 120.0(3) . . ?
C11 C10 Cl7 119.7(3) . . ?
C11 C10 C9 120.4(3) . . ?
C10 C11 Cl8 121.0(2) . . ?
C12 C11 Cl8 118.8(3) . . ?
C12 C11 C10 120.1(3) . . ?
O4 C12 C7 114.6(2) . . ?
O4 C12 C11 125.8(3) . . ?
C11 C12 C7 119.6(3) . . ?
O5 C13 C14 124.8(2) . . ?
O5 C13 C18 114.8(2) . . ?
C14 C13 C18 120.5(2) . . ?
C13 C14 Cl9 119.34(19) . . ?
C13 C14 C15 119.9(2) . . ?
C15 C14 Cl9 120.8(2) . . ?
C14 C15 Cl10 119.8(2) . . ?
C16 C15 Cl10 120.12(19) . . ?
C16 C15 C14 120.0(2) . . ?
C15 C16 Cl11 119.8(2) . . ?
C15 C16 C17 120.2(2) . . ?
C17 C16 Cl11 120.0(2) . . ?
C16 C17 Cl12 120.29(19) . . ?
C18 C17 Cl12 119.2(2) . . ?
C18 C17 C16 120.4(2) . . ?
O6 C18 C13 115.4(2) . . ?
O6 C18 C17 125.5(2) . . ?
C17 C18 C13 119.0(2) . . ?
C19 N1 H1 105(2) . . ?
C19 N1 C23 113.7(2) . . ?
C23 N1 H1 109(2) . . ?
C27 N1 H1 106(2) . . ?
C27 N1 C19 111.0(2) . . ?
C27 N1 C23 111.9(2) . . ?
N1 C19 H19A 108.9 . . ?
N1 C19 H19B 108.9 . . ?
N1 C19 C20 113.1(2) . . ?
H19A C19 H19B 107.8 . . ?
C20 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
C19 C20 C21 112.3(2) . . ?
H20A C20 H20B 107.9 . . ?
C21 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 C20 111.2(3) . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
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 . . ?
N1 C23 H23A 108.8 . . ?
N1 C23 H23B 108.8 . . ?
N1 C23 C24 114.0(2) . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C23 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
C23 C24 C25 111.3(2) . . ?
H24A C24 H24B 108.0 . . ?
C25 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C24 C25 H25A 109.1 . . ?
C24 C25 H25B 109.1 . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 C24 112.3(3) . . ?
C26 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
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 . . ?
N1 C27 H27A 110.2 . . ?
N1 C27 H27B 110.2 . . ?
N1 C27 H27C 105.5 . . ?
N1 C27 H27D 105.5 . . ?
N1 C27 C28 107.7(3) . . ?
N1 C27 C28B 127.4(6) . . ?
H27A C27 H27B 108.5 . . ?
H27C C27 H27D 106.0 . . ?
C28 C27 H27A 110.2 . . ?
C28 C27 H27B 110.2 . . ?
C28B C27 H27C 105.5 . . ?
C28B C27 H27D 105.5 . . ?
C27 C28 H28A 109.7 . . ?
C27 C28 H28B 109.7 . . ?
C27 C28 C29 109.8(5) . . ?
H28A C28 H28B 108.2 . . ?
C29 C28 H28A 109.7 . . ?
C29 C28 H28B 109.7 . . ?
C28 C29 H29A 109.3 . . ?
C28 C29 H29B 109.3 . . ?
C28 C29 C30 111.8(5) . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C28B H28C 110.2 . . ?
C27 C28B H28D 110.2 . . ?
H28C C28B H28D 108.5 . . ?
C29B C28B C27 107.7(7) . . ?
C29B C28B H28C 110.2 . . ?
C29B C28B H28D 110.2 . . ?
C28B C29B H29C 109.5 . . ?
C28B C29B H29D 109.5 . . ?
H29C C29B H29D 108.1 . . ?
C30B C29B C28B 110.6(9) . . ?
C30B C29B H29C 109.5 . . ?
C30B C29B H29D 109.5 . . ?
C29B C30B H30D 109.5 . . ?
C29B C30B H30E 109.5 . . ?
C29B C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
H33A C33 H33B 107.5 . . ?
H33C C33 H33D 108.5 . . ?
C34 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
C34 C33 H33C 110.2 . . ?
C34 C33 H33D 110.2 . . ?
C34 C33 C32 115.3(5) . . ?
C34 C33 C32B 107.4(5) . . ?
C32 C33 H33A 108.4 . . ?
C32 C33 H33B 108.4 . . ?
C32B C33 H33C 110.2 . . ?
C32B C33 H33D 110.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
H40A C40B H40B 106.5 . . ?
H40C C40B H40D 108.8 . . ?
N2 C40B H40A 106.5 . . ?
N2 C40B H40B 106.5 . . ?
N2 C40B C40 123.2(5) . . ?
C40 C40B H40A 106.5 . . ?
C40 C40B H40B 106.5 . . ?
C39B C40B H40C 110.7 . . ?
C39B C40B H40D 110.7 . . ?
C41B C40B H40C 110.7 . . ?
C41B C40B H40D 110.7 . . ?
C41B C40B C39B 105.3(4) . . ?
C40B N2 H2 95(5) . . ?
C40B N2 C31 115.9(4) . . ?
C40B N2 C35 110.5(4) . . ?
C31 N2 H2 110(5) . . ?
C31 N2 C35 115.3(4) . . ?
C35 N2 H2 108(5) . . ?
N2 C31 H31A 108.7 . . ?
N2 C31 H31B 108.7 . . ?
N2 C31 C32 114.2(6) . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C33 C32 H32A 108.3 . . ?
C33 C32 H32B 108.3 . . ?
C31 C32 C33 115.8(8) . . ?
C31 C32 H32A 108.3 . . ?
C31 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
N2 C35 H35A 108.8 . . ?
N2 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C36 C35 N2 113.7(4) . . ?
C36 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
C35 C36 H36A 108.9 . . ?
C35 C36 H36B 108.9 . . ?
C35 C36 C37 113.3(5) . . ?
H36A C36 H36B 107.7 . . ?
C37 C36 H36A 108.9 . . ?
C37 C36 H36B 108.9 . . ?
C36 C37 H37A 109.8 . . ?
C36 C37 H37B 109.8 . . ?
H37A C37 H37B 108.2 . . ?
C38 C37 C36 109.6(4) . . ?
C38 C37 H37A 109.8 . . ?
C38 C37 H37B 109.8 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40B C40 H40E 111.1 . . ?
C40B C40 H40F 111.1 . . ?
C40B C40 C41 103.1(6) . . ?
H40E C40 H40F 109.1 . . ?
C41 C40 H40E 111.1 . . ?
C41 C40 H40F 111.1 . . ?
C40 C41 H41A 110.6 . . ?
C40 C41 H41B 110.6 . . ?
H41A C41 H41B 108.7 . . ?
C42 C41 C40 105.7(8) . . ?
C42 C41 H41A 110.6 . . ?
C42 C41 H41B 110.6 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C31B N2B H2B 109(5) . . ?
C35B N2B H2B 106(5) . . ?
C35B N2B C31B 115.1(6) . . ?
C39B N2B H2B 101(5) . . ?
C39B N2B C31B 113.2(6) . . ?
C39B N2B C35B 111.9(5) . . ?
N2B C31B H31C 109.0 . . ?
N2B C31B H31D 109.0 . . ?
N2B C31B C32B 113.1(6) . . ?
H31C C31B H31D 107.8 . . ?
C32B C31B H31C 109.0 . . ?
C32B C31B H31D 109.0 . . ?
C33 C32B H32C 110.7 . . ?
C33 C32B H32D 110.7 . . ?
C31B C32B C33 105.0(8) . . ?
C31B C32B H32C 110.7 . . ?
C31B C32B H32D 110.7 . . ?
H32C C32B H32D 108.8 . . ?
N2B C35B H35C 108.6 . . ?
N2B C35B H35D 108.6 . . ?
N2B C35B C36B 114.8(6) . . ?
H35C C35B H35D 107.5 . . ?
C36B C35B H35C 108.6 . . ?
C36B C35B H35D 108.6 . . ?
C35B C36B H36C 108.8 . . ?
C35B C36B H36D 108.8 . . ?
C35B C36B C37B 113.8(5) . . ?
H36C C36B H36D 107.7 . . ?
C37B C36B H36C 108.8 . . ?
C37B C36B H36D 108.8 . . ?
C36B C37B H37C 110.7 . . ?
C36B C37B H37D 110.7 . . ?
H37C C37B H37D 108.8 . . ?
C38B C37B C36B 105.0(5) . . ?
C38B C37B H37C 110.7 . . ?
C38B C37B H37D 110.7 . . ?
C37B C38B H38D 109.5 . . ?
C37B C38B H38E 109.5 . . ?
C37B C38B H38F 109.5 . . ?
H38D C38B H38E 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C40B C39B H39A 108.1 . . ?
C40B C39B H39B 108.1 . . ?
N2B C39B C40B 116.7(5) . . ?
N2B C39B H39A 108.1 . . ?
N2B C39B H39B 108.1 . . ?
H39A C39B H39B 107.3 . . ?
C40B C41B H41C 106.6 . . ?
C40B C41B H41D 106.6 . . ?
C40B C41B C42B 123.1(6) . . ?
H41C C41B H41D 106.5 . . ?
C42B C41B H41C 106.6 . . ?
C42B C41B H41D 106.6 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42E 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O2 0.879(18) 2.49(3) 3.166(3) 134(3) .
N1 H1 O6 0.879(18) 2.22(2) 3.038(3) 156(3) .
N2 H2 O1 0.82(2) 2.46(4) 3.176(4) 145(6) .
N2 H2 O5 0.82(2) 2.45(4) 3.166(4) 146(6) .
N2B H2B O4 0.85(2) 2.23(5) 2.935(5) 140(7) .

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
V O1 C1 C2 -170.3(2) . . . . ?
V O1 C1 C6 9.3(3) . . . . ?
V O2 C6 C1 -5.2(2) . . . . ?
V O2 C6 C5 175.72(18) . . . . ?
V O3 C7 C8 179.98(19) . . . . ?
V O3 C7 C12 -0.1(2) . . . . ?
V O4 C12 C7 5.0(3) . . . . ?
V O4 C12 C11 -174.8(2) . . . . ?
V O5 C13 C14 175.1(2) . . . . ?
V O5 C13 C18 -4.6(3) . . . . ?
V O6 C18 C13 8.2(3) . . . . ?
V O6 C18 C17 -170.6(2) . . . . ?
Cl1 C2 C3 Cl2 0.3(3) . . . . ?
Cl1 C2 C3 C4 179.5(2) . . . . ?
Cl2 C3 C4 Cl3 -2.6(3) . . . . ?
Cl2 C3 C4 C5 177.85(19) . . . . ?
Cl3 C4 C5 Cl4 -2.7(3) . . . . ?
Cl3 C4 C5 C6 178.23(18) . . . . ?
Cl4 C5 C6 O2 4.8(3) . . . . ?
Cl4 C5 C6 C1 -174.18(18) . . . . ?
Cl5 C8 C9 Cl6 0.9(3) . . . . ?
Cl5 C8 C9 C10 -178.7(2) . . . . ?
Cl6 C9 C10 Cl7 -2.5(3) . . . . ?
Cl6 C9 C10 C11 178.4(2) . . . . ?
Cl7 C10 C11 Cl8 2.1(3) . . . . ?
Cl7 C10 C11 C12 -178.3(2) . . . . ?
Cl8 C11 C12 O4 1.3(4) . . . . ?
Cl8 C11 C12 C7 -178.41(18) . . . . ?
Cl9 C14 C15 Cl10 0.4(3) . . . . ?
Cl9 C14 C15 C16 -178.7(2) . . . . ?
Cl10 C15 C16 Cl11 -2.7(3) . . . . ?
Cl10 C15 C16 C17 180.0(2) . . . . ?
Cl11 C16 C17 Cl12 -2.0(3) . . . . ?
Cl11 C16 C17 C18 -177.2(2) . . . . ?
Cl12 C17 C18 O6 5.4(4) . . . . ?
Cl12 C17 C18 C13 -173.2(2) . . . . ?
O1 C1 C2 Cl1 2.8(4) . . . . ?
O1 C1 C2 C3 -179.9(2) . . . . ?
O1 C1 C6 O2 -2.8(3) . . . . ?
O1 C1 C6 C5 176.3(2) . . . . ?
O3 C7 C8 Cl5 1.4(3) . . . . ?
O3 C7 C8 C9 -177.8(2) . . . . ?
O3 C7 C12 O4 -3.2(3) . . . . ?
O3 C7 C12 C11 176.6(2) . . . . ?
O5 C13 C14 Cl9 1.2(4) . . . . ?
O5 C13 C14 C15 -177.2(2) . . . . ?
O5 C13 C18 O6 -2.5(3) . . . . ?
O5 C13 C18 C17 176.3(2) . . . . ?
C1 C2 C3 Cl2 -177.00(19) . . . . ?
C1 C2 C3 C4 2.3(4) . . . . ?
C2 C1 C6 O2 176.8(2) . . . . ?
C2 C1 C6 C5 -4.1(3) . . . . ?
C2 C3 C4 Cl3 178.2(2) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
C3 C4 C5 Cl4 176.92(19) . . . . ?
C3 C4 C5 C6 -2.2(4) . . . . ?
C4 C5 C6 O2 -176.1(2) . . . . ?
C4 C5 C6 C1 4.9(3) . . . . ?
C6 C1 C2 Cl1 -176.85(18) . . . . ?
C6 C1 C2 C3 0.4(4) . . . . ?
C7 C8 C9 Cl6 -179.97(19) . . . . ?
C7 C8 C9 C10 0.4(4) . . . . ?
C8 C7 C12 O4 176.7(2) . . . . ?
C8 C7 C12 C11 -3.5(4) . . . . ?
C8 C9 C10 Cl7 177.1(2) . . . . ?
C8 C9 C10 C11 -2.0(4) . . . . ?
C9 C10 C11 Cl8 -178.9(2) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 O4 -178.3(2) . . . . ?
C10 C11 C12 C7 2.0(4) . . . . ?
C12 C7 C8 Cl5 -178.53(18) . . . . ?
C12 C7 C8 C9 2.3(4) . . . . ?
C13 C14 C15 Cl10 178.7(2) . . . . ?
C13 C14 C15 C16 -0.3(4) . . . . ?
C14 C13 C18 O6 177.8(2) . . . . ?
C14 C13 C18 C17 -3.4(4) . . . . ?
C14 C15 C16 Cl11 176.3(2) . . . . ?
C14 C15 C16 C17 -1.0(4) . . . . ?
C15 C16 C17 Cl12 175.3(2) . . . . ?
C15 C16 C17 C18 0.1(4) . . . . ?
C16 C17 C18 O6 -179.2(2) . . . . ?
C16 C17 C18 C13 2.1(4) . . . . ?
C18 C13 C14 Cl9 -179.1(2) . . . . ?
C18 C13 C14 C15 2.5(4) . . . . ?
N1 C19 C20 C21 172.7(2) . . . . ?
N1 C23 C24 C25 174.1(2) . . . . ?
N1 C27 C28 C29 171.9(5) . . . . ?
N1 C27 C28B C29B 86.0(11) . . . . ?
C19 N1 C23 C24 53.3(3) . . . . ?
C19 N1 C27 C28 79.3(5) . . . . ?
C19 N1 C27 C28B 70.8(6) . . . . ?
C19 C20 C21 C22 179.7(3) . . . . ?
C23 N1 C19 C20 59.3(3) . . . . ?
C23 N1 C27 C28 -152.5(4) . . . . ?
C23 N1 C27 C28B -160.9(6) . . . . ?
C23 C24 C25 C26 175.4(2) . . . . ?
C27 N1 C19 C20 -173.4(2) . . . . ?
C27 N1 C23 C24 -73.5(3) . . . . ?
C27 C28 C29 C30 175.7(7) . . . . ?
C27 C28B C29B C30B -177.6(10) . . . . ?
C34 C33 C32 C31 178.7(6) . . . . ?
C34 C33 C32B C31B 171.8(6) . . . . ?
C40B N2 C31 C32 -73.2(7) . . . . ?
C40B N2 C35 C36 -166.4(5) . . . . ?
C40B C40 C41 C42 113.4(7) . . . . ?
N2 C40B C40 C41 -179.0(6) . . . . ?
N2 C31 C32 C33 172.9(6) . . . . ?
N2 C35 C36 C37 168.5(5) . . . . ?
C31 N2 C35 C36 59.9(7) . . . . ?
C35 N2 C31 C32 58.0(7) . . . . ?
C35 C36 C37 C38 -175.7(5) . . . . ?
C40 C40B N2 C31 -139.0(6) . . . . ?
C40 C40B N2 C35 87.6(6) . . . . ?
N2B C31B C32B C33 -176.1(7) . . . . ?
N2B C35B C36B C37B -161.0(5) . . . . ?
C31B N2B C35B C36B 163.4(6) . . . . ?
C31B N2B C39B C40B -40.8(7) . . . . ?
C35B N2B C31B C32B 65.8(9) . . . . ?
C35B N2B C39B C40B -172.8(5) . . . . ?
C35B C36B C37B C38B 163.9(6) . . . . ?
C39B C40B C41B C42B 168.0(8) . . . . ?
C39B N2B C31B C32B -64.6(9) . . . . ?
C39B N2B C35B C36B -65.6(8) . . . . ?
C41B C40B C39B N2B -155.8(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.777
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexanes, THF'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_Complex5_104K
_database_code_depnum_ccdc_archive 'CCDC 2159088'
loop_
_audit_author_name
_audit_author_address
'Roxanna Martinez'
;Colorado State University
United States of America
;
_audit_update_record             
;
2023-07-07 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_audit_creation_date             2022-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H6 Cl6 O6 V, 2(C12 H28 N) 1.7[C4H8O]'
_chemical_formula_sum            'C42 H62 Cl6 N2 O6 V'
_chemical_formula_weight         954.57
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      trigonal
_space_group_IT_number           152
_space_group_name_H-M_alt        'P 31 2 1'
_space_group_name_Hall           'P 31 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'

_cell_length_a                   15.2509(4)
_cell_length_b                   15.2509(4)
_cell_length_c                   18.9173(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3810.5(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9044
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      2.65
_shelx_estimated_absorpt_T_max   0.954
_shelx_estimated_absorpt_T_min   0.925
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1562 before and 0.0977 after correction.
The Ratio of minimum to maximum transmission is 0.8543.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1503
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.086
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            227182
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         1.542
_diffrn_ambient_temperature      104.52
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5400
_reflns_number_total             5840
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 
;
 Flack x determined using 2302 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5840
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0304
_refine_ls_restrained_S_all      1.120
_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)+(0.0482P)²+1.6329P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0892
_refine_special_details          'Solvent mask in Olex2,SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N008(H008)
2.b Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B), C00J(H00C,H00D), C00K(H00E,H00F), C00L(H00G,H00H), C00M(H00I,
 H00J), C00N(H00K,H00L), C00O(H00M,H00N), C00P(H00O,H00P), C00R(H00T,H00U)
2.c Aromatic/amide H refined with riding coordinates:
 C00B(H00Z), C00C(H00), C00F(H0AA)
2.d Idealised Me refined as rotating group:
 C00Q(H00Q,H00R,H00S), C00S(H00V,H00W,H00X), C00T(H00Y,H,HA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V001 V 0.000000 0.36163(4) 0.666667 0.01424(14) Uani 1 2 d S T P . .
Cl02 Cl 0.45581(5) 0.77856(6) 0.60662(4) 0.02688(17) Uani 1 1 d . . . . .
Cl03 Cl -0.02913(7) -0.08614(6) 0.58662(4) 0.02936(18) Uani 1 1 d . . . . .
Cl04 Cl 0.40814(6) 0.80509(6) 0.76463(4) 0.02954(18) Uani 1 1 d . . . . .
O005 O 0.11761(14) 0.44526(15) 0.60904(10) 0.0173(4) Uani 1 1 d . . . . .
O006 O -0.02513(15) 0.25096(15) 0.60268(10) 0.0179(4) Uani 1 1 d . . . . .
O007 O 0.07697(15) 0.47057(15) 0.73308(10) 0.0178(4) Uani 1 1 d . . . . .
N008 N -0.01948(19) 0.32314(19) 0.46264(12) 0.0206(5) Uani 1 1 d . . . . .
H008 H -0.016554 0.313430 0.514689 0.025 Uiso 1 1 calc R . . . .
C009 C 0.1656(2) 0.5446(2) 0.70957(14) 0.0162(5) Uani 1 1 d . . . . .
C00A C 0.1870(2) 0.5309(2) 0.63869(14) 0.0158(5) Uani 1 1 d . . . . .
C00B C 0.2757(2) 0.6045(2) 0.60669(14) 0.0166(5) Uani 1 1 d . . . . .
H00Z H 0.289997 0.597212 0.558868 0.020 Uiso 1 1 calc R . . . .
C00C C -0.0251(2) 0.0926(2) 0.59432(14) 0.0187(5) Uani 1 1 d . . . . .
H00 H -0.041717 0.083852 0.545458 0.022 Uiso 1 1 calc R . . . .
C00D C -0.0131(2) 0.1776(2) 0.63056(14) 0.0171(5) Uani 1 1 d . . . . .
C00E C 0.3431(2) 0.6889(2) 0.64569(15) 0.0195(6) Uani 1 1 d . . . . .
C00F C 0.2329(2) 0.6288(2) 0.74774(15) 0.0197(5) Uani 1 1 d . . . . .
H0AA H 0.218644 0.637460 0.795280 0.024 Uiso 1 1 calc R . . . .
C00G C -0.0122(2) 0.0210(2) 0.63116(14) 0.0182(5) Uani 1 1 d . . . . .
C00H C 0.3225(2) 0.7011(2) 0.71529(15) 0.0200(6) Uani 1 1 d . . . . .
C00I C 0.0364(2) 0.2775(2) 0.42775(16) 0.0213(6) Uani 1 1 d . . . . .
H00A H 0.032474 0.283056 0.375845 0.026 Uiso 1 1 calc R . . . .
H00B H 0.002655 0.204564 0.439765 0.026 Uiso 1 1 calc R . . . .
C00J C 0.0388(3) 0.4652(2) 0.37276(16) 0.0254(6) Uani 1 1 d . . . . .
H00C H 0.083728 0.444614 0.349256 0.030 Uiso 1 1 calc R . . . .
H00D H -0.028412 0.428432 0.349733 0.030 Uiso 1 1 calc R . . . .
C00K C 0.0818(2) 0.5776(2) 0.36335(17) 0.0264(7) Uani 1 1 d . . . . .
H00E H 0.152335 0.613979 0.381076 0.032 Uiso 1 1 calc R . . . .
H00F H 0.041715 0.599629 0.391653 0.032 Uiso 1 1 calc R . . . .
C00L C -0.2980(2) 0.1087(3) 0.4427(2) 0.0347(8) Uani 1 1 d . . . . .
H00G H -0.330212 0.135816 0.474693 0.042 Uiso 1 1 calc R . . . .
H00H H -0.305414 0.126821 0.393690 0.042 Uiso 1 1 calc R . . . .
C00M C -0.1305(2) 0.2686(2) 0.44245(16) 0.0228(6) Uani 1 1 d . . . . .
H00I H -0.163895 0.301578 0.466741 0.027 Uiso 1 1 calc R . . . .
H00J H -0.136057 0.276023 0.390917 0.027 Uiso 1 1 calc R . . . .
C00N C 0.0281(2) 0.4357(2) 0.45042(15) 0.0228(6) Uani 1 1 d . . . . .
H00K H 0.095940 0.470464 0.472620 0.027 Uiso 1 1 calc R . . . .
H00L H -0.013706 0.459990 0.474163 0.027 Uiso 1 1 calc R . . . .
C00O C 0.1470(2) 0.3274(3) 0.44944(17) 0.0281(7) Uani 1 1 d . . . . .
H00M H 0.151953 0.330620 0.501655 0.034 Uiso 1 1 calc R . . . .
H00N H 0.183666 0.397532 0.431022 0.034 Uiso 1 1 calc R . . . .
C00P C 0.1959(3) 0.2688(3) 0.42111(19) 0.0307(7) Uani 1 1 d . . . . .
H00O H 0.264817 0.297934 0.441268 0.037 Uiso 1 1 calc R . . . .
H00P H 0.156158 0.197667 0.437348 0.037 Uiso 1 1 calc R . . . .
C00Q C 0.0805(3) 0.6049(3) 0.28605(19) 0.0326(8) Uani 1 1 d . . . . .
H00Q H 0.113435 0.576341 0.257159 0.049 Uiso 1 1 calc GR . . . .
H00R H 0.116944 0.678775 0.280875 0.049 Uiso 1 1 calc GR . . . .
H00S H 0.010306 0.577352 0.270413 0.049 Uiso 1 1 calc GR . . . .
C00R C -0.1858(2) 0.1578(3) 0.4607(2) 0.0337(8) Uani 1 1 d . . . . .
H00T H -0.178024 0.149513 0.511782 0.040 Uiso 1 1 calc R . . . .
H00U H -0.155674 0.123358 0.434186 0.040 Uiso 1 1 calc R . . . .
C00S C 0.2033(3) 0.2698(3) 0.34112(19) 0.0326(7) Uani 1 1 d . . . . .
H00V H 0.135179 0.237810 0.320691 0.049 Uiso 1 1 calc GR . . . .
H00W H 0.237059 0.232406 0.326501 0.049 Uiso 1 1 calc GR . . . .
H00X H 0.242517 0.339933 0.324498 0.049 Uiso 1 1 calc GR . . . .
C00T C -0.3515(3) -0.0041(4) 0.4495(3) 0.0588(13) Uani 1 1 d . . . . .
H00Y H -0.320736 -0.031370 0.417301 0.088 Uiso 1 1 calc GR . . . .
H H -0.423159 -0.032384 0.437428 0.088 Uiso 1 1 calc GR . . . .
HA H -0.345737 -0.022389 0.498245 0.088 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V001 O005 1.9351(19) 6_556 ?
V001 O005 1.9351(19) . ?
V001 O006 1.953(2) . ?
V001 O006 1.953(2) 6_556 ?
V001 O007 1.941(2) . ?
V001 O007 1.9408(19) 6_556 ?
Cl02 C00E 1.738(3) . ?
Cl03 C00G 1.740(3) . ?
Cl04 C00H 1.738(3) . ?
O005 C00A 1.326(3) . ?
O006 C00D 1.330(3) . ?
O007 C009 1.332(3) . ?
N008 H008 1.0000 . ?
N008 C00I 1.497(4) . ?
N008 C00M 1.515(4) . ?
N008 C00N 1.511(4) . ?
C009 C00A 1.420(4) . ?
C009 C00F 1.381(4) . ?
C00A C00B 1.392(4) . ?
C00B H00Z 0.9500 . ?
C00B C00E 1.391(4) . ?
C00C H00 0.9500 . ?
C00C C00D 1.395(4) . ?
C00C C00G 1.389(4) . ?
C00D C00D 1.410(5) 6_556 ?
C00E C00H 1.388(4) . ?
C00F H0AA 0.9500 . ?
C00F C00H 1.397(4) . ?
C00G C00G 1.382(6) 6_556 ?
C00I H00A 0.9900 . ?
C00I H00B 0.9900 . ?
C00I C00O 1.519(4) . ?
C00J H00C 0.9900 . ?
C00J H00D 0.9900 . ?
C00J C00K 1.509(4) . ?
C00J C00N 1.521(4) . ?
C00K H00E 0.9900 . ?
C00K H00F 0.9900 . ?
C00K C00Q 1.524(5) . ?
C00L H00G 0.9900 . ?
C00L H00H 0.9900 . ?
C00L C00R 1.524(4) . ?
C00L C00T 1.496(6) . ?
C00M H00I 0.9900 . ?
C00M H00J 0.9900 . ?
C00M C00R 1.503(4) . ?
C00N H00K 0.9900 . ?
C00N H00L 0.9900 . ?
C00O H00M 0.9900 . ?
C00O H00N 0.9900 . ?
C00O C00P 1.520(5) . ?
C00P H00O 0.9900 . ?
C00P H00P 0.9900 . ?
C00P C00S 1.517(5) . ?
C00Q H00Q 0.9800 . ?
C00Q H00R 0.9800 . ?
C00Q H00S 0.9800 . ?
C00R H00T 0.9900 . ?
C00R H00U 0.9900 . ?
C00S H00V 0.9800 . ?
C00S H00W 0.9800 . ?
C00S H00X 0.9800 . ?
C00T H00Y 0.9800 . ?
C00T H 0.9800 . ?
C00T HA 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
O005 V001 O005 157.44(13) 6_556 . ?
O005 V001 O006 111.26(9) 6_556 . ?
O005 V001 O006 86.39(8) . . ?
O005 V001 O006 86.39(8) 6_556 6_556 ?
O005 V001 O006 111.26(9) . 6_556 ?
O005 V001 O007 86.99(8) 6_556 . ?
O005 V001 O007 80.56(8) 6_556 6_556 ?
O005 V001 O007 80.56(8) . . ?
O005 V001 O007 86.99(8) . 6_556 ?
O006 V001 O006 79.99(11) 6_556 . ?
O007 V001 O006 156.12(9) . . ?
O007 V001 O006 86.21(8) 6_556 . ?
O007 V001 O006 86.21(8) . 6_556 ?
O007 V001 O006 156.13(9) 6_556 6_556 ?
O007 V001 O007 112.77(12) . 6_556 ?
C00A O005 V001 115.55(16) . . ?
C00D O006 V001 115.54(17) . . ?
C009 O007 V001 115.65(17) . . ?
C00I N008 H008 106.7 . . ?
C00I N008 C00M 111.9(2) . . ?
C00I N008 C00N 113.6(2) . . ?
C00M N008 H008 106.7 . . ?
C00N N008 H008 106.7 . . ?
C00N N008 C00M 110.8(2) . . ?
O007 C009 C00A 113.6(2) . . ?
O007 C009 C00F 125.6(3) . . ?
C00F C009 C00A 120.8(2) . . ?
O005 C00A C009 114.5(2) . . ?
O005 C00A C00B 125.9(2) . . ?
C00B C00A C009 119.6(2) . . ?
C00A C00B H00Z 120.5 . . ?
C00E C00B C00A 119.1(2) . . ?
C00E C00B H00Z 120.5 . . ?
C00D C00C H00 120.7 . . ?
C00G C00C H00 120.7 . . ?
C00G C00C C00D 118.6(3) . . ?
O006 C00D C00C 125.3(2) . . ?
O006 C00D C00D 114.44(14) . 6_556 ?
C00C C00D C00D 120.27(16) . 6_556 ?
C00B C00E Cl02 119.0(2) . . ?
C00H C00E Cl02 119.9(2) . . ?
C00H C00E C00B 121.0(3) . . ?
C009 C00F H0AA 120.5 . . ?
C009 C00F C00H 118.9(3) . . ?
C00H C00F H0AA 120.5 . . ?
C00C C00G Cl03 118.8(2) . . ?
C00G C00G Cl03 120.06(10) 6_556 . ?
C00G C00G C00C 121.09(16) 6_556 . ?
C00E C00H Cl04 121.0(2) . . ?
C00E C00H C00F 120.6(3) . . ?
C00F C00H Cl04 118.4(2) . . ?
N008 C00I H00A 108.9 . . ?
N008 C00I H00B 108.9 . . ?
N008 C00I C00O 113.3(2) . . ?
H00A C00I H00B 107.7 . . ?
C00O C00I H00A 108.9 . . ?
C00O C00I H00B 108.9 . . ?
H00C C00J H00D 107.9 . . ?
C00K C00J H00C 109.3 . . ?
C00K C00J H00D 109.3 . . ?
C00K C00J C00N 111.8(3) . . ?
C00N C00J H00C 109.3 . . ?
C00N C00J H00D 109.3 . . ?
C00J C00K H00E 109.3 . . ?
C00J C00K H00F 109.3 . . ?
C00J C00K C00Q 111.5(3) . . ?
H00E C00K H00F 108.0 . . ?
C00Q C00K H00E 109.3 . . ?
C00Q C00K H00F 109.3 . . ?
H00G C00L H00H 107.9 . . ?
C00R C00L H00G 109.2 . . ?
C00R C00L H00H 109.2 . . ?
C00T C00L H00G 109.2 . . ?
C00T C00L H00H 109.2 . . ?
C00T C00L C00R 112.2(3) . . ?
N008 C00M H00I 108.8 . . ?
N008 C00M H00J 108.8 . . ?
H00I C00M H00J 107.7 . . ?
C00R C00M N008 113.9(2) . . ?
C00R C00M H00I 108.8 . . ?
C00R C00M H00J 108.8 . . ?
N008 C00N C00J 113.8(2) . . ?
N008 C00N H00K 108.8 . . ?
N008 C00N H00L 108.8 . . ?
C00J C00N H00K 108.8 . . ?
C00J C00N H00L 108.8 . . ?
H00K C00N H00L 107.7 . . ?
C00I C00O H00M 109.4 . . ?
C00I C00O H00N 109.4 . . ?
C00I C00O C00P 111.0(3) . . ?
H00M C00O H00N 108.0 . . ?
C00P C00O H00M 109.4 . . ?
C00P C00O H00N 109.4 . . ?
C00O C00P H00O 108.8 . . ?
C00O C00P H00P 108.8 . . ?
H00O C00P H00P 107.7 . . ?
C00S C00P C00O 113.7(3) . . ?
C00S C00P H00O 108.8 . . ?
C00S C00P H00P 108.8 . . ?
C00K C00Q H00Q 109.5 . . ?
C00K C00Q H00R 109.5 . . ?
C00K C00Q H00S 109.5 . . ?
H00Q C00Q H00R 109.5 . . ?
H00Q C00Q H00S 109.5 . . ?
H00R C00Q H00S 109.5 . . ?
C00L C00R H00T 109.4 . . ?
C00L C00R H00U 109.4 . . ?
C00M C00R C00L 111.3(3) . . ?
C00M C00R H00T 109.4 . . ?
C00M C00R H00U 109.4 . . ?
H00T C00R H00U 108.0 . . ?
C00P C00S H00V 109.5 . . ?
C00P C00S H00W 109.5 . . ?
C00P C00S H00X 109.5 . . ?
H00V C00S H00W 109.5 . . ?
H00V C00S H00X 109.5 . . ?
H00W C00S H00X 109.5 . . ?
C00L C00T H00Y 109.5 . . ?
C00L C00T H 109.5 . . ?
C00L C00T HA 109.5 . . ?
H00Y C00T H 109.5 . . ?
H00Y C00T HA 109.5 . . ?
H C00T HA 109.5 . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 71.3 electrons were 
found in a volume of 153.0Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1.7[C4H8O] per Formula Unit 
which account for 68 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 0.294 0.167 153.0 71.3 '0.5 C4H8O'
2 0.294 0.000 0.833 153.0 71.3 ?
3 0.706 0.706 0.500 153.0 71.3 ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: HMDSO, THF'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Air-sensitive,Moisture-sensitive
