# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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. 
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data_jz44_0m_0510
_database_code_depnum_ccdc_archive 'CCDC 1921675'
loop_
_audit_author_name
_audit_author_address
'Cassidy E. Jackson'
;Colorado State University
United States of America
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-05 downloaded from the CCDC.
;
_audit_creation_date             2019-05-15
_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            (n-Bu3NH)2[V(4-Br-C6H3O2)3]
_chemical_name_systematic        
'tris(4-bromocatecholato)vanadate(IV) bis-tri-n-butylammonium'
_chemical_formula_moiety         'C18 H9 Br3 O6 V, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H64 Br3 N2 O6 V'
_chemical_formula_weight         983.62
_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'
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'
Br Br -0.2901 2.4595 '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      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   14.6090(13)
_cell_length_b                   14.6090(13)
_cell_length_c                   21.144(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4512.6(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    116(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   0.654
_shelx_estimated_absorpt_T_min   0.614
_exptl_absorpt_coefficient_mu    2.921
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.4973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0783 before and 0.0610 after correction. The Ratio of minimum to maximum transmission is 0.6664. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.159
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16717
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.694
_diffrn_ambient_temperature      116.62
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.900
_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         0.651
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.784
_reflns_number_gt                4601
_reflns_number_total             5621
_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       '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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 
;
 Flack x determined using 1639 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5621
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.130
_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)+(0.0626P)²+2.3780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1261
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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. Restrained distances
 C00H-C00H_$1
 1.4 with sigma of 0.02
 C2B-H2B
 0.95 with sigma of 0.02
3. Same fragment restrains
{C1, C2A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1, C2A}
{C1A, C2B} sigma for 1-2: 0.02, 1-3: 0.04
as
{C2B, C1A}
4. Others
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(H2AC)=Sof(H2AD)=1-FVAR(1)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(H2AA)=Sof(H2AB)=FVAR(1)
 Sof(H00I)=Sof(H00J)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C00S)=Sof(H00Y)=Sof(H)=
 Sof(HA)=Sof(C00P)=Sof(H00Z)=Sof(HB)=1-FVAR(2)
 Sof(H00G)=Sof(H00H)=Sof(C00O)=Sof(H00R)=Sof(H00S)=Sof(C00Q)=Sof(H00T)=
 Sof(H00U)=Sof(C00R)=Sof(H00V)=Sof(H00W)=Sof(H00X)=FVAR(2)
 Fixed Sof: C1(0.5) H1(0.5) C2A(0.5) C2B(0.5) C1A(0.5) H1A(0.5) Br(0.5) H2B(0.5)
5.a Ternary CH refined with riding coordinates:
 N007(H007)
5.b Secondary CH2 refined with riding coordinates:
 C00C(H00A,H00B), C00D(H00C,H00D), C00F(H00E,H00F), C00I(H00G,H00H), C00I(H00I,
 H00J), C00J(H00K,H00L), C00L(H00P,H00Q), C00O(H00R,H00S), C00Q(H00T,H00U),
 C0AA(H0AA,H0AB), C00P(H00Z,HB), C2AA(H2AA,H2AB), C2AA(H2AC,H2AD)
5.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00), C00B(H1AA), C1(H1), C1A(H1A)
5.d Idealised Me refined as rotating group:
 C00K(H00M,H00N,H00O), C00R(H00V,H00W,H00X), C4(H4A,H4B,H4C), C4A(H4AA,H4AB,
 H4AC), C00S(H00Y,H,HA)
;
_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
Br01 Br -0.02578(4) 1.60100(4) 0.52751(3) 0.03444(17) Uani 1 1 d . . . . .
V002 V 0.17128(5) 1.17128(5) 0.500000 0.0205(2) Uani 1 2 d S T P . .
O004 O 0.1960(2) 1.2600(2) 0.56709(15) 0.0226(7) Uani 1 1 d . . . . .
O005 O 0.1016(2) 1.2751(2) 0.46767(15) 0.0217(7) Uani 1 1 d . . . . .
O006 O 0.1132(2) 1.0860(3) 0.44278(18) 0.0329(9) Uani 1 1 d . . . . .
N007 N 0.2997(3) 0.8331(3) 0.40244(19) 0.0242(9) Uani 1 1 d . . . . .
H007 H 0.293652 0.788619 0.366712 0.029 Uiso 1 1 calc R . . . .
C008 C 0.0954(3) 1.3461(3) 0.5073(2) 0.0211(9) Uani 1 1 d . . . . .
C009 C 0.1468(3) 1.4079(3) 0.6077(2) 0.0236(10) Uani 1 1 d . . . . .
H009 H 0.181184 1.401970 0.645637 0.028 Uiso 1 1 calc R . . . .
C00A C 0.0951(3) 1.4863(3) 0.5967(2) 0.0249(10) Uani 1 1 d . . . . .
H00 H 0.094719 1.534942 0.626491 0.030 Uiso 1 1 calc R . . . .
C00B C 0.0431(3) 1.4238(3) 0.4964(2) 0.0221(9) Uani 1 1 d . . . . .
H1AA H 0.007527 1.429853 0.459064 0.027 Uiso 1 1 calc R . . . .
C00C C 0.2893(3) 0.9270(3) 0.3744(2) 0.0243(10) Uani 1 1 d . . . . .
H00A H 0.349105 0.947232 0.357361 0.029 Uiso 1 1 calc R . . . .
H00B H 0.271338 0.970389 0.408177 0.029 Uiso 1 1 calc R . . . .
C00D C 0.2186(4) 0.9304(4) 0.3220(2) 0.0268(11) Uani 1 1 d . . . . .
H00C H 0.156538 0.924619 0.340344 0.032 Uiso 1 1 calc R . . . .
H00D H 0.228378 0.878575 0.292644 0.032 Uiso 1 1 calc R . . . .
C00E C 0.1478(3) 1.3382(3) 0.5629(2) 0.0220(10) Uani 1 1 d . . . . .
C00F C 0.2264(4) 1.0209(4) 0.2859(2) 0.0306(11) Uani 1 1 d . . . . .
H00E H 0.212428 1.072254 0.314893 0.037 Uiso 1 1 calc R . . . .
H00F H 0.289986 1.028642 0.270682 0.037 Uiso 1 1 calc R . . . .
C00G C 0.0443(4) 1.4922(3) 0.5418(2) 0.0260(11) Uani 1 1 d . . . . .
C00H C 0.0482(4) 1.0323(4) 0.4680(3) 0.0433(16) Uani 1 1 d D . . . .
C00I C 0.3943(4) 0.8211(4) 0.4288(2) 0.0315(11) Uani 1 1 d . . . . .
H00G H 0.439342 0.826254 0.393945 0.038 Uiso 0.607(14) 1 calc R . . A 1
H00H H 0.406882 0.870843 0.459339 0.038 Uiso 0.607(14) 1 calc R . . A 1
H00I H 0.398154 0.853045 0.469961 0.038 Uiso 0.393(14) 1 calc R . . A 2
H00J H 0.438725 0.850379 0.399749 0.038 Uiso 0.393(14) 1 calc R . . A 2
C00J C 0.2244(4) 0.8109(4) 0.4487(2) 0.0311(12) Uani 1 1 d . . . . .
H00K H 0.225251 0.744177 0.456986 0.037 Uiso 1 1 calc R . . . .
H00L H 0.164904 0.825653 0.428751 0.037 Uiso 1 1 calc R . . . .
C00K C 0.1615(5) 1.0244(4) 0.2299(3) 0.0413(14) Uani 1 1 d . . . . .
H00M H 0.172398 0.971353 0.202550 0.062 Uiso 1 1 calc GR . . . .
H00N H 0.172018 1.080785 0.205969 0.062 Uiso 1 1 calc GR . . . .
H00O H 0.098145 1.023134 0.245171 0.062 Uiso 1 1 calc GR . . . .
C00L C 0.2304(5) 0.8608(5) 0.5114(3) 0.0492(17) Uani 1 1 d . . . . .
H00P H 0.224320 0.927508 0.504274 0.059 Uiso 1 1 calc R . . . .
H00Q H 0.290821 0.849272 0.530999 0.059 Uiso 1 1 calc R . . . .
C00O C 0.4065(7) 0.7307(6) 0.4611(5) 0.030(2) Uiso 0.607(14) 1 d . . . A 1
H00R H 0.408998 0.681617 0.428812 0.036 Uiso 0.607(14) 1 calc R . . A 1
H00S H 0.352936 0.718797 0.488559 0.036 Uiso 0.607(14) 1 calc R . . A 1
C00Q C 0.4931(8) 0.7274(7) 0.5008(6) 0.037(3) Uani 0.607(14) 1 d . . . A 1
H00T H 0.543481 0.757652 0.477508 0.045 Uiso 0.607(14) 1 calc R . . A 1
H00U H 0.510708 0.662772 0.507891 0.045 Uiso 0.607(14) 1 calc R . . A 1
C00R C 0.4801(9) 0.7755(8) 0.5659(5) 0.052(3) Uani 0.607(14) 1 d . . . A 1
H00V H 0.456338 0.837524 0.559214 0.077 Uiso 0.607(14) 1 calc GR . . A 1
H00W H 0.539109 0.778910 0.587813 0.077 Uiso 0.607(14) 1 calc GR . . A 1
H00X H 0.436669 0.740492 0.591607 0.077 Uiso 0.607(14) 1 calc GR . . A 1
C4 C 0.1713(12) 0.8737(12) 0.6216(8) 0.068(5) Uiso 0.496(14) 1 d . . . B 1
H4A H 0.215565 0.837195 0.645607 0.103 Uiso 0.496(14) 1 calc GR . . B 1
H4B H 0.113398 0.876700 0.644843 0.103 Uiso 0.496(14) 1 calc GR . . B 1
H4C H 0.195409 0.935732 0.615616 0.103 Uiso 0.496(14) 1 calc GR . . B 1
C4A C 0.1802(11) 0.7357(10) 0.5824(8) 0.059(4) Uiso 0.504(14) 1 d . . . B 2
H4AA H 0.192421 0.693204 0.547487 0.089 Uiso 0.504(14) 1 calc GR . . B 2
H4AB H 0.129597 0.712228 0.608080 0.089 Uiso 0.504(14) 1 calc GR . . B 2
H4AC H 0.235166 0.741455 0.608682 0.089 Uiso 0.504(14) 1 calc GR . . B 2
C0AA C 0.5197(10) 0.7031(11) 0.4595(8) 0.037(4) Uani 0.393(14) 1 d . . . A 2
H0AA H 0.535680 0.637657 0.454386 0.045 Uiso 0.393(14) 1 calc R . . A 2
H0AB H 0.560521 0.738878 0.431477 0.045 Uiso 0.393(14) 1 calc R . . A 2
C00S C 0.5377(16) 0.7303(14) 0.5262(9) 0.058(6) Uani 0.393(14) 1 d . . . A 2
H00Y H 0.603931 0.733039 0.533486 0.086 Uiso 0.393(14) 1 calc GR . . A 2
H H 0.510371 0.685190 0.554857 0.086 Uiso 0.393(14) 1 calc GR . . A 2
HA H 0.510742 0.790609 0.534284 0.086 Uiso 0.393(14) 1 calc GR . . A 2
C00P C 0.4225(10) 0.7169(9) 0.4384(7) 0.025(3) Uiso 0.393(14) 1 d . . . A 2
H00Z H 0.381171 0.689267 0.470209 0.030 Uiso 0.393(14) 1 calc R . . A 2
HB H 0.413216 0.683914 0.398051 0.030 Uiso 0.393(14) 1 calc R . . A 2
C2AA C 0.1549(6) 0.8285(5) 0.5559(3) 0.060(2) Uani 1 1 d . . . . .
H2AA H 0.156430 0.760967 0.559847 0.072 Uiso 0.496(14) 1 calc R . . B 1
H2AB H 0.094223 0.846545 0.539150 0.072 Uiso 0.496(14) 1 calc R . . B 1
H2AC H 0.147169 0.872914 0.590842 0.072 Uiso 0.504(14) 1 calc R . . B 2
H2AD H 0.096207 0.824206 0.532645 0.072 Uiso 0.504(14) 1 calc R . . B 2
C1 C 0.0015(7) 0.9596(8) 0.4483(6) 0.030(2) Uiso 0.5 1 d D . . C -1
H1 H 0.011264 0.939159 0.406181 0.036 Uiso 0.5 1 calc R . . C -1
C2A C -0.0619(7) 0.9105(7) 0.4862(5) 0.029(2) Uiso 0.5 1 d D . . C -1
C2B C -0.0715(8) 0.9263(8) 0.4510(6) 0.035(2) Uiso 0.5 1 d D . . C 1
C1A C -0.0044(7) 0.9767(7) 0.4221(6) 0.028(2) Uiso 0.5 1 d D . . C 1
H1A H 0.007060 0.976123 0.377836 0.034 Uiso 0.5 1 calc R . . C 1
Br Br -0.18312(10) 0.86712(11) 0.55240(7) 0.0526(4) Uani 0.5 1 d . . . C -1
H2B H -0.096(13) 0.884(11) 0.421(7) 0.10(7) Uiso 0.5 1 d D . . 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
Br01 C00G 1.914(5) . ?
V002 O004 1.955(3) . ?
V002 O004 1.955(3) 7_466 ?
V002 O005 1.950(3) . ?
V002 O005 1.950(3) 7_466 ?
V002 O006 1.933(4) 7_466 ?
V002 O006 1.933(4) . ?
O004 C00E 1.346(6) . ?
O005 C008 1.336(5) . ?
O006 C00H 1.342(7) . ?
N007 H007 1.0000 . ?
N007 C00C 1.503(6) . ?
N007 C00I 1.500(6) . ?
N007 C00J 1.507(6) . ?
C008 C00B 1.387(7) . ?
C008 C00E 1.408(7) . ?
C009 H009 0.9500 . ?
C009 C00A 1.392(7) . ?
C009 C00E 1.390(7) . ?
C00A H00 0.9500 . ?
C00A C00G 1.380(7) . ?
C00B H1AA 0.9500 . ?
C00B C00G 1.386(7) . ?
C00C H00A 0.9900 . ?
C00C H00B 0.9900 . ?
C00C C00D 1.514(7) . ?
C00D H00C 0.9900 . ?
C00D H00D 0.9900 . ?
C00D C00F 1.531(7) . ?
C00F H00E 0.9900 . ?
C00F H00F 0.9900 . ?
C00F C00K 1.516(7) . ?
C00H C00H 1.391(13) 7_466 ?
C00H C1 1.330(12) . ?
C00H C1A 1.481(12) . ?
C00I H00G 0.9900 . ?
C00I H00H 0.9900 . ?
C00I H00I 0.9900 . ?
C00I H00J 0.9900 . ?
C00I C00O 1.498(10) . ?
C00I C00P 1.589(15) . ?
C00J H00K 0.9900 . ?
C00J H00L 0.9900 . ?
C00J C00L 1.516(7) . ?
C00K H00M 0.9800 . ?
C00K H00N 0.9800 . ?
C00K H00O 0.9800 . ?
C00L H00P 0.9900 . ?
C00L H00Q 0.9900 . ?
C00L C2AA 1.524(9) . ?
C00O H00R 0.9900 . ?
C00O H00S 0.9900 . ?
C00O C00Q 1.520(15) . ?
C00Q H00T 0.9900 . ?
C00Q H00U 0.9900 . ?
C00Q C00R 1.556(15) . ?
C00R H00V 0.9800 . ?
C00R H00W 0.9800 . ?
C00R H00X 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 C2AA 1.557(18) . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C4A C2AA 1.513(17) . ?
C0AA H0AA 0.9900 . ?
C0AA H0AB 0.9900 . ?
C0AA C00S 1.49(2) . ?
C0AA C00P 1.502(19) . ?
C00S H00Y 0.9800 . ?
C00S H 0.9800 . ?
C00S HA 0.9800 . ?
C00P H00Z 0.9900 . ?
C00P HB 0.9900 . ?
C2AA H2AA 0.9900 . ?
C2AA H2AB 0.9900 . ?
C2AA H2AC 0.9900 . ?
C2AA H2AD 0.9900 . ?
C1 H1 0.9500 . ?
C1 C2A 1.420(16) . ?
C1 C2B 1.174(16) . ?
C1 C1A 0.615(13) . ?
C2A C2B 0.793(13) . ?
C2A C1A 1.866(16) . ?
C2A Br 1.900(11) 7_466 ?
C2A Br 2.344(10) . ?
C2B C1A 1.371(16) . ?
C2B H2B 0.96(3) . ?
C1A H1A 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
O004 V002 O004 106.4(2) . 7_466 ?
O005 V002 O004 80.52(13) . . ?
O005 V002 O004 87.00(13) . 7_466 ?
O005 V002 O004 80.52(13) 7_466 7_466 ?
O005 V002 O004 86.99(13) 7_466 . ?
O005 V002 O005 159.1(2) . 7_466 ?
O006 V002 O004 164.27(15) . . ?
O006 V002 O004 87.47(15) . 7_466 ?
O006 V002 O004 87.47(15) 7_466 . ?
O006 V002 O004 164.27(15) 7_466 7_466 ?
O006 V002 O005 102.99(15) 7_466 . ?
O006 V002 O005 93.03(15) . . ?
O006 V002 O005 102.99(15) . 7_466 ?
O006 V002 O005 93.02(15) 7_466 7_466 ?
O006 V002 O006 80.0(2) 7_466 . ?
C00E O004 V002 114.8(3) . . ?
C008 O005 V002 114.8(3) . . ?
C00H O006 V002 116.0(3) . . ?
C00C N007 H007 106.6 . . ?
C00C N007 C00J 112.2(4) . . ?
C00I N007 H007 106.6 . . ?
C00I N007 C00C 110.2(4) . . ?
C00I N007 C00J 114.0(4) . . ?
C00J N007 H007 106.6 . . ?
O005 C008 C00B 124.6(4) . . ?
O005 C008 C00E 115.1(4) . . ?
C00B C008 C00E 120.3(4) . . ?
C00A C009 H009 120.2 . . ?
C00E C009 H009 120.2 . . ?
C00E C009 C00A 119.6(4) . . ?
C009 C00A H00 120.5 . . ?
C00G C00A C009 119.0(4) . . ?
C00G C00A H00 120.5 . . ?
C008 C00B H1AA 121.0 . . ?
C00G C00B C008 117.9(4) . . ?
C00G C00B H1AA 121.0 . . ?
N007 C00C H00A 109.0 . . ?
N007 C00C H00B 109.0 . . ?
N007 C00C C00D 112.8(4) . . ?
H00A C00C H00B 107.8 . . ?
C00D C00C H00A 109.0 . . ?
C00D C00C H00B 109.0 . . ?
C00C C00D H00C 109.7 . . ?
C00C C00D H00D 109.7 . . ?
C00C C00D C00F 110.0(4) . . ?
H00C C00D H00D 108.2 . . ?
C00F C00D H00C 109.7 . . ?
C00F C00D H00D 109.7 . . ?
O004 C00E C008 114.1(4) . . ?
O004 C00E C009 125.6(4) . . ?
C009 C00E C008 120.2(4) . . ?
C00D C00F H00E 109.2 . . ?
C00D C00F H00F 109.2 . . ?
H00E C00F H00F 107.9 . . ?
C00K C00F C00D 111.8(5) . . ?
C00K C00F H00E 109.2 . . ?
C00K C00F H00F 109.2 . . ?
C00A C00G Br01 118.2(4) . . ?
C00A C00G C00B 122.9(5) . . ?
C00B C00G Br01 118.9(4) . . ?
O006 C00H C00H 114.0(3) . 7_466 ?
O006 C00H C1A 115.2(7) . . ?
C00H C00H C1A 130.0(5) 7_466 . ?
C1 C00H O006 134.8(7) . . ?
C1 C00H C00H 110.7(6) . 7_466 ?
C1 C00H C1A 24.5(6) . . ?
N007 C00I H00G 109.1 . . ?
N007 C00I H00H 109.1 . . ?
N007 C00I H00I 108.9 . . ?
N007 C00I H00J 108.9 . . ?
N007 C00I C00P 113.5(6) . . ?
H00G C00I H00H 107.9 . . ?
H00I C00I H00J 107.7 . . ?
C00O C00I N007 112.4(5) . . ?
C00O C00I H00G 109.1 . . ?
C00O C00I H00H 109.1 . . ?
C00P C00I H00I 108.9 . . ?
C00P C00I H00J 108.9 . . ?
N007 C00J H00K 108.5 . . ?
N007 C00J H00L 108.5 . . ?
N007 C00J C00L 115.0(4) . . ?
H00K C00J H00L 107.5 . . ?
C00L C00J H00K 108.5 . . ?
C00L C00J H00L 108.5 . . ?
C00F C00K H00M 109.5 . . ?
C00F C00K H00N 109.5 . . ?
C00F C00K H00O 109.5 . . ?
H00M C00K H00N 109.5 . . ?
H00M C00K H00O 109.5 . . ?
H00N C00K H00O 109.5 . . ?
C00J C00L H00P 109.6 . . ?
C00J C00L H00Q 109.6 . . ?
C00J C00L C2AA 110.4(5) . . ?
H00P C00L H00Q 108.1 . . ?
C2AA C00L H00P 109.6 . . ?
C2AA C00L H00Q 109.6 . . ?
C00I C00O H00R 109.2 . . ?
C00I C00O H00S 109.2 . . ?
C00I C00O C00Q 112.3(7) . . ?
H00R C00O H00S 107.9 . . ?
C00Q C00O H00R 109.2 . . ?
C00Q C00O H00S 109.2 . . ?
C00O C00Q H00T 109.2 . . ?
C00O C00Q H00U 109.2 . . ?
C00O C00Q C00R 111.9(9) . . ?
H00T C00Q H00U 107.9 . . ?
C00R C00Q H00T 109.2 . . ?
C00R C00Q H00U 109.2 . . ?
C00Q C00R H00V 109.5 . . ?
C00Q C00R H00W 109.5 . . ?
C00Q C00R H00X 109.5 . . ?
H00V C00R H00W 109.5 . . ?
H00V C00R H00X 109.5 . . ?
H00W C00R H00X 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2AA C4 H4A 109.5 . . ?
C2AA C4 H4B 109.5 . . ?
C2AA C4 H4C 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
C2AA C4A H4AA 109.5 . . ?
C2AA C4A H4AB 109.5 . . ?
C2AA C4A H4AC 109.5 . . ?
H0AA C0AA H0AB 107.6 . . ?
C00S C0AA H0AA 108.7 . . ?
C00S C0AA H0AB 108.7 . . ?
C00S C0AA C00P 114.4(15) . . ?
C00P C0AA H0AA 108.7 . . ?
C00P C0AA H0AB 108.7 . . ?
C0AA C00S H00Y 109.5 . . ?
C0AA C00S H 109.5 . . ?
C0AA C00S HA 109.5 . . ?
H00Y C00S H 109.5 . . ?
H00Y C00S HA 109.5 . . ?
H C00S HA 109.5 . . ?
C00I C00P H00Z 108.7 . . ?
C00I C00P HB 108.7 . . ?
C0AA C00P C00I 114.3(11) . . ?
C0AA C00P H00Z 108.7 . . ?
C0AA C00P HB 108.7 . . ?
H00Z C00P HB 107.6 . . ?
C00L C2AA C4 107.9(8) . . ?
C00L C2AA H2AA 110.1 . . ?
C00L C2AA H2AB 110.1 . . ?
C00L C2AA H2AC 109.8 . . ?
C00L C2AA H2AD 109.8 . . ?
C4 C2AA H2AA 110.1 . . ?
C4 C2AA H2AB 110.1 . . ?
C4A C2AA C00L 109.2(9) . . ?
C4A C2AA H2AC 109.8 . . ?
C4A C2AA H2AD 109.8 . . ?
H2AA C2AA H2AB 108.4 . . ?
H2AC C2AA H2AD 108.3 . . ?
C00H C1 H1 117.9 . . ?
C00H C1 C2A 124.1(10) . . ?
C2A C1 H1 117.9 . . ?
C2B C1 C00H 141.4(12) . . ?
C2B C1 H1 92.9 . . ?
C2B C1 C2A 33.9(7) . . ?
C1A C1 C00H 91.7(17) . . ?
C1A C1 H1 45.8 . . ?
C1A C1 C2A 129(2) . . ?
C1A C1 C2B 94.9(19) . . ?
C1 C2A C1A 14.9(6) . . ?
C1 C2A Br 165.2(8) . . ?
C1 C2A Br 118.5(8) . 7_466 ?
C2B C2A C1 55.8(13) . . ?
C2B C2A C1A 41.0(12) . . ?
C2B C2A Br 73.1(12) . 7_466 ?
C2B C2A Br 120.4(14) . . ?
C1A C2A Br 156.1(7) . . ?
C1A C2A Br 107.9(6) . 7_466 ?
Br C2A Br 69.5(3) 7_466 . ?
C1 C2B C1A 26.6(7) . . ?
C1 C2B H2B 125(10) . . ?
C2A C2B C1 90.3(16) . . ?
C2A C2B C1A 116.7(16) . . ?
C2A C2B H2B 120(10) . . ?
C1A C2B H2B 109(10) . . ?
C00H C1A C2A 92.3(7) . . ?
C00H C1A H1A 124.1 . . ?
C1 C1A C00H 63.8(15) . . ?
C1 C1A C2A 36.5(15) . . ?
C1 C1A C2B 58.6(16) . . ?
C1 C1A H1A 149.3 . . ?
C2A C1A H1A 142.2 . . ?
C2B C1A C00H 111.9(10) . . ?
C2B C1A C2A 22.3(6) . . ?
C2B C1A H1A 124.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'slow evaporation'
_chemical_properties_physical    Air-sensitive,Heat-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_jz25_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1921677'
loop_
_audit_author_name
_audit_author_address
'Cassidy E. Jackson'
;Colorado State University
United States of America
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-05 downloaded from the CCDC.
;
_audit_creation_date             2019-05-15
_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            (n-Bu3NH)2[V(C6Br4O2)3]
_chemical_name_systematic        
'tris(tetrabromocatecholato)vanadate(IV) bis-tri-n-butylammonium'
_chemical_formula_moiety         'Br12 C18 O6 V, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H56 Br12 N2 O6 V'
_chemical_formula_weight         1694.63
_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'
Br Br -0.2901 2.4595 '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'
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'
H H 0.0000 0.0000 '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                   12.039(5)
_cell_length_b                   12.432(6)
_cell_length_c                   37.11(2)
_cell_angle_alpha                83.93(3)
_cell_angle_beta                 89.04(2)
_cell_angle_gamma                84.219(19)
_cell_volume                     5495(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      26.484
_cell_measurement_theta_min      2.277
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.950
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1344 before and 0.0554 after correction. The Ratio of minimum to maximum transmission is 0.4797. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             51
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.142
_exptl_special_details           
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1344 before and 0.0554 after correction.
The Ratio of minimum to maximum transmission is 0.4797.
The λ/2 correction factor is Not present.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            46089
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_min         3.783
_diffrn_ambient_temperature      145.03
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17019
_reflns_number_total             21824
_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       '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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         21824
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0653
_refine_ls_restrained_S_all      1.154
_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)+83.8435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1685
_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. Others
 Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N014(H014), N01G(H01G), N01Q(H01Q), N025(H025)
3.b Secondary CH2 refined with riding coordinates:
 C01X(H01A,H01B), C021(H02I,H02J), C022(H02,H), C026(H02K,H02L), C029(H02M,
 H02N), C02C(H02R,H02S), C02E(H02T,H02U), C02F(H0AA,HA), C02G(H3AA,HB),
 C02H(H1BA,HC), C02I(H02A,H02B), C02J(H02V,H02W), C02K(H4AA,HD), C02L(H02X,
 H02Y), C02N(H02C,H02D), C02O(H6AA,HG), C02P(H7AA,HH), C02Q(H2BA,HI), C02S(H3BA,
 HL), C02T(H02E,H02F), C02U(H8AA,HM), C02V(H9AA,HN), C02W(H4BA,HO), C02Y(H02G,
 H02H), C02Z(H0BA,HR), C030(H03A,H03B), C031(H03Z,HS), C032(H03O,H03P),
 C033(H03,HT), C034(H6BA,HU), C036(H7BA,HV), C037(H03C,H03D), C038(H8BA,HW),
 C039(H03E,H03F), C03A(H03G,H03H), C1(H1AA,H1AB), C1(H1BC,H1BD)
3.c Idealised Me refined as rotating group:
 C02B(H02O,H02P,H02Q), C02M(H5AA,HE,HF), C02R(H02Z,HJ,HK), C02X(H5BA,HP,HQ),
 C035(H03T,H03U,H03V), C03B(H03I,H03J,H03K), C03C(H03L,H03M,H03N), C03D(H9BA,HX,
 HY), C03E(H0CA,HZ,H1CA), C03G(H03W,H03X,H03Y), C03H(H03Q,H03R,H03S), C2(H2A,
 H2B,H2C), C2A(H2AA,H2AB,H2AC)
;
_atom_sites_solution_hydrogens   geom
_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
Br01 Br 0.59497(7) 0.69931(7) 0.37484(3) 0.0250(2) Uani 1 1 d . . . . .
Br02 Br 0.36263(8) 0.32499(7) 0.29971(3) 0.0266(2) Uani 1 1 d . . . . .
Br03 Br 1.22880(7) 0.42811(8) 0.20951(3) 0.0264(2) Uani 1 1 d . . . . .
Br04 Br 1.10101(8) 0.67862(7) 0.20447(3) 0.0264(2) Uani 1 1 d . . . . .
Br05 Br 0.24317(7) 0.57978(8) 0.29133(3) 0.0275(2) Uani 1 1 d . . . . .
Br06 Br 0.87904(8) 0.30253(7) 0.12710(3) 0.0318(2) Uani 1 1 d . . . . .
Br08 Br 1.00164(8) 0.27994(9) 0.46923(3) 0.0321(2) Uani 1 1 d . . . . .
Br09 Br 1.02975(9) 0.34536(8) 0.28127(3) 0.0334(2) Uani 1 1 d . . . . .
Br0A Br 0.35701(8) 0.76576(8) 0.33069(3) 0.0358(2) Uani 1 1 d . . . . .
Br0B Br 1.11829(8) 0.24170(8) 0.16982(3) 0.0374(3) Uani 1 1 d . . . . .
Br0C Br 0.62293(9) 1.09986(8) 0.13229(3) 0.0391(3) Uani 1 1 d . . . . .
Br0D Br 0.84619(9) -0.09666(8) 0.36334(3) 0.0377(3) Uani 1 1 d . . . . .
Br0E Br 0.38595(9) 1.12150(9) 0.17810(3) 0.0406(3) Uani 1 1 d . . . . .
Br0F Br 1.02381(9) 0.74579(10) 0.02323(3) 0.0387(3) Uani 1 1 d . . . . .
Br0G Br 0.28863(8) 0.90111(10) 0.21901(3) 0.0409(3) Uani 1 1 d . . . . .
Br0H Br 0.48152(9) 0.73313(10) 0.02573(3) 0.0370(2) Uani 1 1 d . . . . .
Br0I Br 1.08009(9) -0.11566(9) 0.31511(3) 0.0415(3) Uani 1 1 d . . . . .
Br0J Br 0.45908(9) 0.28054(10) 0.48115(3) 0.0405(3) Uani 1 1 d . . . . .
Br0K Br 0.60588(11) 0.26284(10) 0.55614(3) 0.0420(3) Uani 1 1 d . . . . .
Br0L Br 1.17349(9) 0.10708(10) 0.27460(3) 0.0420(3) Uani 1 1 d . . . . .
Br0M Br 0.88070(11) 0.25526(10) 0.55069(3) 0.0425(3) Uani 1 1 d . . . . .
Br0N Br 0.88801(12) 0.76390(10) -0.05488(3) 0.0469(3) Uani 1 1 d . . . . .
Br0O Br 0.61290(12) 0.76721(10) -0.05359(3) 0.0470(3) Uani 1 1 d . . . . .
V0P V 0.75560(11) 0.70244(11) 0.12789(4) 0.0147(3) Uani 1 1 d . . . . .
V0Q V 0.71590(11) 0.29885(11) 0.37127(4) 0.0153(3) Uani 1 1 d . . . . .
O00R O 0.8233(5) 0.2962(5) 0.40976(16) 0.0195(12) Uani 1 1 d . . . . .
O00S O 0.8835(5) 0.6935(5) 0.15934(16) 0.0188(12) Uani 1 1 d . . . . .
O00T O 0.8345(5) 0.3183(5) 0.33655(16) 0.0184(12) Uani 1 1 d . . . . .
O00U O 0.7195(5) 0.8556(5) 0.13529(16) 0.0183(12) Uani 1 1 d . . . . .
O00V O 0.6322(5) 0.6857(5) 0.16096(16) 0.0175(12) Uani 1 1 d . . . . .
O00W O 0.8573(5) 0.7273(5) 0.08713(16) 0.0196(12) Uani 1 1 d . . . . .
O00X O 0.7514(5) 0.1469(5) 0.36287(16) 0.0195(12) Uani 1 1 d . . . . .
O00Y O 0.6195(5) 0.2696(5) 0.41376(16) 0.0197(12) Uani 1 1 d . . . . .
O00Z O 0.6816(5) 0.4568(5) 0.36701(16) 0.0182(12) Uani 1 1 d . . . . .
O010 O 0.5825(5) 0.3104(5) 0.34272(17) 0.0216(13) Uani 1 1 d . . . . .
O011 O 0.7885(5) 0.5443(5) 0.13371(16) 0.0188(12) Uani 1 1 d . . . . .
O012 O 0.6526(5) 0.7068(5) 0.08826(16) 0.0196(12) Uani 1 1 d . . . . .
C013 C 0.9404(7) 0.4081(7) 0.1518(2) 0.0196(17) Uani 1 1 d . . . . .
N014 N 0.9173(6) 0.5324(6) 0.36449(19) 0.0195(15) Uani 1 1 d . . . . .
H014 H 0.852908 0.488897 0.362077 0.023 Uiso 1 1 calc R . . . .
C015 C 0.5297(7) 0.5968(6) 0.3500(2) 0.0163(16) Uani 1 1 d . . . . .
C016 C 0.3791(7) 0.5432(7) 0.3162(2) 0.0207(18) Uani 1 1 d . . . . .
C017 C 0.9835(7) 0.2175(7) 0.3068(2) 0.0222(18) Uani 1 1 d . . . . .
C018 C 0.6960(7) 0.7249(7) 0.0552(2) 0.0191(17) Uani 1 1 d . . . . .
C019 C 0.5841(7) 0.4903(6) 0.3519(2) 0.0164(16) Uani 1 1 d . . . . .
C01A C 1.0912(7) 0.4614(7) 0.1855(2) 0.0201(18) Uani 1 1 d . . . . .
C01B C 1.0424(7) 0.3827(7) 0.1695(2) 0.0204(18) Uani 1 1 d . . . . .
C01C C 0.8898(7) 0.2250(7) 0.3288(2) 0.0184(17) Uani 1 1 d . . . . .
C01D C 0.6370(8) 0.7364(7) 0.0227(2) 0.0220(18) Uani 1 1 d . . . . .
C01E C 0.9384(7) 0.5954(6) 0.1644(2) 0.0150(16) Uani 1 1 d . . . . .
C01F C 0.8457(7) 0.1301(7) 0.3446(2) 0.0185(17) Uani 1 1 d . . . . .
N01G N 0.5481(6) 0.4772(6) 0.1310(2) 0.0244(16) Uani 1 1 d . . . . .
H01G H 0.608831 0.524155 0.134698 0.029 Uiso 1 1 calc R . . . .
C01H C 0.8463(8) 0.2769(7) 0.4739(3) 0.026(2) Uani 1 1 d . . . . .
C01I C 0.6687(7) 0.2742(7) 0.4456(2) 0.0220(18) Uani 1 1 d . . . . .
C01J C 0.4224(7) 0.8915(8) 0.1920(3) 0.026(2) Uani 1 1 d . . . . .
C01K C 0.6228(7) 0.8739(7) 0.1528(2) 0.0198(18) Uani 1 1 d . . . . .
C01L C 0.5748(7) 0.7785(7) 0.1679(2) 0.0195(17) Uani 1 1 d . . . . .
C01M C 0.5303(7) 0.4104(7) 0.3373(2) 0.0210(18) Uani 1 1 d . . . . .
C01N C 0.6171(7) 0.2717(7) 0.4793(2) 0.0213(18) Uani 1 1 d . . . . .
C01O C 1.0363(7) 0.5680(7) 0.1834(2) 0.0179(17) Uani 1 1 d . . . . .
C01P C 0.7843(8) 0.2822(7) 0.4429(2) 0.0211(18) Uani 1 1 d . . . . .
N01Q N 0.9670(8) 0.9236(7) 0.1301(2) 0.033(2) Uani 1 1 d . . . . .
H01Q H 0.909977 0.870147 0.133475 0.039 Uiso 1 1 calc R . . . .
C01R C 1.0006(8) 0.0216(8) 0.3190(3) 0.0248(19) Uani 1 1 d . . . . .
C01S C 0.4292(7) 0.6234(7) 0.3317(2) 0.0221(18) Uani 1 1 d . . . . .
C01T C 0.8691(8) 0.7439(8) 0.0220(3) 0.028(2) Uani 1 1 d . . . . .
C01U C 0.4649(8) 0.9828(7) 0.1752(3) 0.027(2) Uani 1 1 d . . . . .
C01V C 0.5655(8) 0.9755(7) 0.1560(3) 0.0250(19) Uani 1 1 d . . . . .
C01W C 0.8869(7) 0.5119(7) 0.1496(2) 0.0165(16) Uani 1 1 d . . . . .
C01X C 0.8846(8) 0.6084(8) 0.3921(3) 0.026(2) Uani 1 1 d . . . . .
H01A H 0.822294 0.660993 0.382426 0.032 Uiso 1 1 calc R . . . .
H01B H 0.948512 0.649949 0.396091 0.032 Uiso 1 1 calc R . . . .
C01Y C 0.4301(7) 0.4352(7) 0.3192(2) 0.0210(18) Uani 1 1 d . . . . .
C01Z C 0.8093(9) 0.7513(8) -0.0103(2) 0.030(2) Uani 1 1 d . . . . .
C020 C 0.9025(8) 0.0275(7) 0.3399(3) 0.025(2) Uani 1 1 d . . . . .
C021 C 0.8138(8) 0.6332(8) 0.4548(3) 0.030(2) Uani 1 1 d . . . . .
H02I H 0.744837 0.678101 0.446231 0.036 Uiso 1 1 calc R . . . .
H02J H 0.872843 0.682214 0.456730 0.036 Uiso 1 1 calc R . . . .
C022 C 0.5914(8) 0.4005(8) 0.1039(3) 0.027(2) Uani 1 1 d . . . . .
H02 H 0.654187 0.350820 0.114765 0.032 Uiso 1 1 calc R . . . .
H H 0.531416 0.355731 0.098481 0.032 Uiso 1 1 calc R . . . .
C023 C 0.7940(8) 0.2676(7) 0.5078(2) 0.0245(19) Uani 1 1 d . . . . .
C024 C 1.0413(7) 0.1141(8) 0.3025(3) 0.026(2) Uani 1 1 d . . . . .
N025 N 0.5069(7) 1.0790(7) 0.3985(2) 0.0328(19) Uani 1 1 d . . . . .
H025 H 0.556268 1.138971 0.393438 0.039 Uiso 1 1 calc R . . . .
C026 C 1.0171(8) 0.4519(7) 0.3764(2) 0.0226(18) Uani 1 1 d . . . . .
H02K H 0.994137 0.400605 0.396694 0.027 Uiso 1 1 calc R . . . .
H02L H 1.041147 0.409385 0.356016 0.027 Uiso 1 1 calc R . . . .
C027 C 0.4794(7) 0.7887(7) 0.1880(3) 0.0239(19) Uani 1 1 d . . . . .
C028 C 0.8109(7) 0.7322(7) 0.0549(2) 0.0200(17) Uani 1 1 d . . . . .
C029 C 1.1144(7) 0.5069(7) 0.3881(2) 0.0225(18) Uani 1 1 d . . . . .
H02M H 1.095157 0.539430 0.410936 0.027 Uiso 1 1 calc R . . . .
H02N H 1.130862 0.565965 0.369382 0.027 Uiso 1 1 calc R . . . .
C02A C 0.6953(10) 0.7510(8) -0.0101(2) 0.031(2) Uani 1 1 d . . . . .
C02B C 1.3157(9) 0.4764(10) 0.4087(3) 0.039(3) Uani 1 1 d . . . . .
H02O H 1.315434 0.551449 0.397448 0.058 Uiso 1 1 calc GR . . . .
H02P H 1.386128 0.434863 0.402862 0.058 Uiso 1 1 calc GR . . . .
H02Q H 1.308240 0.476221 0.435000 0.058 Uiso 1 1 calc GR . . . .
C02C C 0.8493(8) 0.5532(8) 0.4281(3) 0.026(2) Uani 1 1 d . . . . .
H02R H 0.786538 0.510085 0.424185 0.032 Uiso 1 1 calc R . . . .
H02S H 0.912256 0.502366 0.438311 0.032 Uiso 1 1 calc R . . . .
C02D C 0.6792(9) 0.2677(8) 0.5105(3) 0.029(2) Uani 1 1 d . . . . .
C02E C 0.8258(9) 0.6222(10) 0.3070(3) 0.036(2) Uani 1 1 d . . . . .
H02T H 0.788868 0.554998 0.305866 0.043 Uiso 1 1 calc R . . . .
H02U H 0.775675 0.672601 0.320303 0.043 Uiso 1 1 calc R . . . .
C02F C 0.3515(8) 0.4917(8) 0.1066(3) 0.026(2) Uani 1 1 d . . . . .
H0AA H 0.338722 0.431909 0.125521 0.031 Uiso 1 1 calc R . . . .
HA H 0.371772 0.459393 0.083778 0.031 Uiso 1 1 calc R . . . .
C02G C 0.5282(8) 0.4137(8) 0.1671(3) 0.030(2) Uani 1 1 d . . . . .
H3AA H 0.463706 0.450467 0.179463 0.036 Uiso 1 1 calc R . . . .
HB H 0.509744 0.340072 0.163184 0.036 Uiso 1 1 calc R . . . .
C02H C 0.5357(9) 1.0012(8) 0.3705(3) 0.031(2) Uani 1 1 d . . . . .
H1BA H 0.494866 0.936193 0.376229 0.037 Uiso 1 1 calc R . . . .
HC H 0.616598 0.977121 0.371701 0.037 Uiso 1 1 calc R . . . .
C02I C 0.9157(9) 1.0205(8) 0.1042(3) 0.031(2) Uani 1 1 d . . . . .
H02A H 0.852084 1.058353 0.116506 0.038 Uiso 1 1 calc R . . . .
H02B H 0.972324 1.072498 0.098718 0.038 Uiso 1 1 calc R . . . .
C02J C 0.9351(8) 0.5947(8) 0.3272(2) 0.027(2) Uani 1 1 d . . . . .
H02V H 0.968515 0.662667 0.330392 0.032 Uiso 1 1 calc R . . . .
H02W H 0.987792 0.549990 0.312781 0.032 Uiso 1 1 calc R . . . .
C02K C 0.6825(9) 0.3797(8) 0.0434(3) 0.032(2) Uani 1 1 d . . . . .
H4AA H 0.748906 0.337277 0.054968 0.038 Uiso 1 1 calc R . . . .
HD H 0.628317 0.327972 0.038745 0.038 Uiso 1 1 calc R . . . .
C02L C 1.2177(9) 0.4243(9) 0.3940(3) 0.035(2) Uani 1 1 d . . . . .
H02X H 1.239756 0.395609 0.370782 0.042 Uiso 1 1 calc R . . . .
H02Y H 1.199188 0.362534 0.411414 0.042 Uiso 1 1 calc R . . . .
C02M C 0.7166(11) 0.4371(10) 0.0081(3) 0.047(3) Uani 1 1 d . . . . .
H5AA H 0.745944 0.383522 -0.008101 0.070 Uiso 1 1 calc GR . . . .
HE H 0.774428 0.484354 0.012347 0.070 Uiso 1 1 calc GR . . . .
HF H 0.651626 0.481205 -0.003108 0.070 Uiso 1 1 calc GR . . . .
C02N C 1.0692(10) 0.8659(8) 0.1153(3) 0.037(3) Uani 1 1 d . . . . .
H02C H 1.048919 0.833604 0.093349 0.044 Uiso 1 1 calc R . . . .
H02D H 1.097303 0.805484 0.133440 0.044 Uiso 1 1 calc R . . . .
C02O C 0.6303(8) 0.4577(8) 0.0691(3) 0.031(2) Uani 1 1 d . . . . .
H6AA H 0.685763 0.507246 0.074610 0.037 Uiso 1 1 calc R . . . .
HG H 0.566075 0.502447 0.057079 0.037 Uiso 1 1 calc R . . . .
C02P C 0.4469(8) 0.5524(8) 0.1178(3) 0.028(2) Uani 1 1 d . . . . .
H7AA H 0.468964 0.602184 0.096935 0.033 Uiso 1 1 calc R . . . .
HH H 0.420279 0.597244 0.137385 0.033 Uiso 1 1 calc R . . . .
C02Q C 0.2995(9) 1.0527(8) 0.4025(3) 0.038(3) Uani 1 1 d . . . . .
H2BA H 0.306782 1.001219 0.383823 0.045 Uiso 1 1 calc R . . . .
HI H 0.309214 1.010214 0.426597 0.045 Uiso 1 1 calc R . . . .
C02R C 0.7923(9) 0.5730(10) 0.4924(3) 0.037(2) Uani 1 1 d . . . . .
H02Z H 0.728062 0.531012 0.491090 0.055 Uiso 1 1 calc GR . . . .
HJ H 0.776748 0.625959 0.510057 0.055 Uiso 1 1 calc GR . . . .
HK H 0.858417 0.523686 0.499934 0.055 Uiso 1 1 calc GR . . . .
C02S C 0.5071(10) 1.0508(9) 0.3322(3) 0.038(2) Uani 1 1 d . . . . .
H3BA H 0.529190 1.125774 0.328658 0.045 Uiso 1 1 calc R . . . .
HL H 0.425410 1.054608 0.328666 0.045 Uiso 1 1 calc R . . . .
C02T C 0.8171(10) 1.0836(9) 0.0459(3) 0.040(3) Uani 1 1 d . . . . .
H02E H 0.868034 1.141437 0.041699 0.047 Uiso 1 1 calc R . . . .
H02F H 0.750736 1.113018 0.059143 0.047 Uiso 1 1 calc R . . . .
C02U C 0.2446(9) 0.5691(9) 0.1010(3) 0.034(2) Uani 1 1 d . . . . .
H8AA H 0.222229 0.598247 0.124097 0.041 Uiso 1 1 calc R . . . .
HM H 0.258774 0.631025 0.083005 0.041 Uiso 1 1 calc R . . . .
C02V C 0.6056(11) 0.3454(11) 0.2280(3) 0.047(3) Uani 1 1 d . . . . .
H9AA H 0.538669 0.383205 0.238718 0.056 Uiso 1 1 calc R . . . .
HN H 0.588889 0.270592 0.224931 0.056 Uiso 1 1 calc R . . . .
C02W C 0.6601(10) 0.9927(9) 0.4404(3) 0.037(2) Uani 1 1 d . . . . .
H4BA H 0.701645 1.049722 0.427260 0.045 Uiso 1 1 calc R . . . .
HO H 0.679872 0.924501 0.429141 0.045 Uiso 1 1 calc R . . . .
C02X C 0.0928(9) 1.0419(11) 0.4086(3) 0.045(3) Uani 1 1 d . . . . .
H5BA H 0.085421 0.999181 0.388164 0.068 Uiso 1 1 calc GR . . . .
HP H 0.022019 1.085697 0.412356 0.068 Uiso 1 1 calc GR . . . .
HQ H 0.111660 0.992805 0.430510 0.068 Uiso 1 1 calc GR . . . .
C02Y C 1.2722(10) 0.8697(10) 0.0999(3) 0.045(3) Uani 1 1 d . . . . .
H02G H 1.293941 0.824635 0.122773 0.054 Uiso 1 1 calc R . . . .
H02H H 1.262231 0.819974 0.081333 0.054 Uiso 1 1 calc R . . . .
C02Z C 0.6289(9) 0.4046(9) 0.1908(3) 0.033(2) Uani 1 1 d . . . . .
H0BA H 0.649801 0.478150 0.193770 0.040 Uiso 1 1 calc R . . . .
HR H 0.692410 0.364269 0.179151 0.040 Uiso 1 1 calc R . . . .
C030 C 0.8757(10) 0.9877(8) 0.0691(3) 0.036(2) Uani 1 1 d . . . . .
H03A H 0.823708 0.931141 0.074398 0.043 Uiso 1 1 calc R . . . .
H03B H 0.940257 0.956018 0.055514 0.043 Uiso 1 1 calc R . . . .
C031 C 0.5668(11) 0.9837(10) 0.3041(3) 0.045(3) Uani 1 1 d . . . . .
H03Z H 0.648328 0.986981 0.305842 0.054 Uiso 1 1 calc R . . . .
HS H 0.551816 0.906748 0.309521 0.054 Uiso 1 1 calc R . . . .
C032 C 0.8443(11) 0.6741(12) 0.2690(3) 0.051(3) Uani 1 1 d . . . . .
H03O H 0.892130 0.622527 0.255437 0.061 Uiso 1 1 calc R . . . .
H03P H 0.884063 0.739629 0.270138 0.061 Uiso 1 1 calc R . . . .
C033 C 0.6976(12) 0.9756(10) 0.4799(3) 0.046(3) Uani 1 1 d . . . . .
H03 H 0.664790 0.911752 0.492389 0.056 Uiso 1 1 calc R . . . .
HT H 0.669706 1.040057 0.492228 0.056 Uiso 1 1 calc R . . . .
C034 C 0.3894(9) 1.1315(9) 0.3967(3) 0.039(3) Uani 1 1 d . . . . .
H6BA H 0.377855 1.173610 0.372632 0.046 Uiso 1 1 calc R . . . .
HU H 0.379419 1.183471 0.415177 0.046 Uiso 1 1 calc R . . . .
C035 C 0.1507(9) 0.5110(10) 0.0877(3) 0.044(3) Uani 1 1 d . . . . .
H03T H 0.176662 0.473110 0.066818 0.065 Uiso 1 1 calc GR . . . .
H03U H 0.087177 0.564183 0.080574 0.065 Uiso 1 1 calc GR . . . .
H03V H 0.127665 0.458199 0.107192 0.065 Uiso 1 1 calc GR . . . .
C036 C 0.1844(9) 1.1162(9) 0.4004(4) 0.042(3) Uani 1 1 d . . . . .
H7BA H 0.179713 1.171334 0.417873 0.050 Uiso 1 1 calc R . . . .
HV H 0.173456 1.154859 0.375756 0.050 Uiso 1 1 calc R . . . .
C037 C 0.8867(11) 0.9566(13) 0.1907(4) 0.056(4) Uani 1 1 d . . . . .
H03C H 0.871961 0.879926 0.197104 0.067 Uiso 1 1 calc R . . . .
H03D H 0.821003 0.994822 0.177474 0.067 Uiso 1 1 calc R . . . .
C038 C 0.5364(9) 1.0253(9) 0.4358(3) 0.036(2) Uani 1 1 d . . . . .
H8BA H 0.495844 0.959833 0.440673 0.043 Uiso 1 1 calc R . . . .
HW H 0.511163 1.075891 0.453815 0.043 Uiso 1 1 calc R . . . .
C039 C 1.1614(10) 0.9365(8) 0.1058(3) 0.040(3) Uani 1 1 d . . . . .
H03E H 1.169656 0.982783 0.125485 0.047 Uiso 1 1 calc R . . . .
H03F H 1.141498 0.984856 0.083394 0.047 Uiso 1 1 calc R . . . .
C03A C 0.9860(10) 0.9604(9) 0.1671(3) 0.042(3) Uani 1 1 d . . . . .
H03G H 1.048881 0.913199 0.179031 0.050 Uiso 1 1 calc R . . . .
H03H H 1.007317 1.035672 0.163870 0.050 Uiso 1 1 calc R . . . .
C03B C 1.3653(11) 0.9382(11) 0.0880(4) 0.050(3) Uani 1 1 d . . . . .
H03I H 1.350056 0.974193 0.063574 0.076 Uiso 1 1 calc GR . . . .
H03J H 1.436042 0.891790 0.087945 0.076 Uiso 1 1 calc GR . . . .
H03K H 1.370226 0.993257 0.104838 0.076 Uiso 1 1 calc GR . . . .
C03C C 0.7804(12) 1.0537(11) 0.0095(4) 0.057(3) Uani 1 1 d . . . . .
H03L H 0.846415 1.034793 -0.005268 0.085 Uiso 1 1 calc GR . . . .
H03M H 0.734982 1.115791 -0.003135 0.085 Uiso 1 1 calc GR . . . .
H03N H 0.736272 0.991403 0.013345 0.085 Uiso 1 1 calc GR . . . .
C03D C 0.5288(16) 1.0245(13) 0.2656(4) 0.074(5) Uani 1 1 d . . . . .
H9BA H 0.567715 0.978582 0.248467 0.112 Uiso 1 1 calc GR . . . .
HX H 0.546354 1.099742 0.259733 0.112 Uiso 1 1 calc GR . . . .
HY H 0.448121 1.021539 0.263738 0.112 Uiso 1 1 calc GR . . . .
C03E C 0.8251(14) 0.9578(13) 0.4829(4) 0.071(5) Uani 1 1 d . . . . .
H0CA H 0.853104 0.895009 0.470322 0.107 Uiso 1 1 calc GR . . . .
HZ H 0.846147 0.944231 0.508529 0.107 Uiso 1 1 calc GR . . . .
H1CA H 0.857599 1.022658 0.471869 0.107 Uiso 1 1 calc GR . . . .
C03G C 0.7017(14) 0.3397(16) 0.2540(4) 0.075(5) Uani 1 1 d . . . . .
H03W H 0.771483 0.316960 0.241673 0.112 Uiso 1 1 calc GR . . . .
H03X H 0.689824 0.286973 0.274888 0.112 Uiso 1 1 calc GR . . . .
H03Y H 0.706254 0.411479 0.262202 0.112 Uiso 1 1 calc GR . . . .
C03H C 0.7340(12) 0.7063(13) 0.2488(4) 0.062(4) Uani 1 1 d . . . . .
H03Q H 0.749490 0.730607 0.223418 0.093 Uiso 1 1 calc GR . . . .
H03R H 0.691270 0.765344 0.260089 0.093 Uiso 1 1 calc GR . . . .
H03S H 0.690570 0.643354 0.250043 0.093 Uiso 1 1 calc GR . . . .
Br1 Br 0.42930(9) 0.66058(8) 0.21265(3) 0.0337(2) Uani 1 1 d . . . . .
C1 C 0.9028(13) 1.0102(14) 0.2258(4) 0.068(5) Uani 1 1 d . . . . .
H1AA H 0.960371 0.964045 0.240727 0.082 Uiso 0.66(3) 1 calc R . P A 1
H1AB H 0.932035 1.081335 0.219106 0.082 Uiso 0.66(3) 1 calc R . P A 1
H1BC H 0.871476 0.964622 0.246242 0.082 Uiso 0.34(3) 1 calc R . P A 2
H1BD H 0.984090 1.007755 0.230063 0.082 Uiso 0.34(3) 1 calc R . P A 2
C2 C 0.8113(18) 1.0262(18) 0.2462(6) 0.057(6) Uiso 0.66(3) 1 d . . P A 1
H2A H 0.752474 1.069607 0.231638 0.085 Uiso 0.66(3) 1 calc GR . P A 1
H2B H 0.828678 1.064902 0.266799 0.085 Uiso 0.66(3) 1 calc GR . P A 1
H2C H 0.785685 0.955884 0.255223 0.085 Uiso 0.66(3) 1 calc GR . P A 1
C2A C 0.859(3) 1.113(3) 0.2274(9) 0.040(10) Uiso 0.34(3) 1 d . . P A 2
H2AA H 0.890936 1.160159 0.208137 0.060 Uiso 0.34(3) 1 calc GR . P A 2
H2AB H 0.874945 1.135855 0.251021 0.060 Uiso 0.34(3) 1 calc GR . P A 2
H2AC H 0.777618 1.116836 0.224241 0.060 Uiso 0.34(3) 1 calc GR . 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
Br01 C015 1.889(8) . ?
Br02 C01Y 1.875(9) . ?
Br03 C01A 1.882(8) . ?
Br04 C01O 1.890(8) . ?
Br05 C016 1.883(8) . ?
Br06 C013 1.892(9) . ?
Br08 C01H 1.880(10) . ?
Br09 C017 1.891(9) . ?
Br0A C01S 1.888(9) . ?
Br0B C01B 1.892(9) . ?
Br0C C01V 1.884(9) . ?
Br0D C020 1.872(10) . ?
Br0E C01U 1.896(9) . ?
Br0F C01T 1.866(10) . ?
Br0G C01J 1.883(9) . ?
Br0H C01D 1.877(9) . ?
Br0I C01R 1.888(9) . ?
Br0J C01N 1.896(9) . ?
Br0K C02D 1.896(10) . ?
Br0L C024 1.883(9) . ?
Br0M C023 1.904(9) . ?
Br0N C01Z 1.892(10) . ?
Br0O C02A 1.892(9) . ?
V0P O00S 1.935(6) . ?
V0P O00U 1.957(6) . ?
V0P O00V 1.925(6) . ?
V0P O00W 1.949(6) . ?
V0P O011 1.955(6) . ?
V0P O012 1.932(6) . ?
V0Q O00R 1.938(6) . ?
V0Q O00T 1.923(6) . ?
V0Q O00X 1.951(6) . ?
V0Q O00Y 1.967(6) . ?
V0Q O00Z 1.956(6) . ?
V0Q O010 1.923(6) . ?
O00R C01P 1.310(11) . ?
O00S C01E 1.324(10) . ?
O00T C01C 1.334(10) . ?
O00U C01K 1.335(11) . ?
O00V C01L 1.331(10) . ?
O00W C028 1.321(10) . ?
O00X C01F 1.323(10) . ?
O00Y C01I 1.341(11) . ?
O00Z C019 1.319(10) . ?
O010 C01M 1.331(11) . ?
O011 C01W 1.338(10) . ?
O012 C018 1.333(10) . ?
C013 C01B 1.395(12) . ?
C013 C01W 1.378(12) . ?
N014 C01X 1.487(12) . ?
N014 C026 1.524(11) . ?
N014 C02J 1.535(11) . ?
C015 C019 1.413(11) . ?
C015 C01S 1.391(12) . ?
C016 C01S 1.394(12) . ?
C016 C01Y 1.413(12) . ?
C017 C01C 1.381(12) . ?
C017 C024 1.423(13) . ?
C018 C01D 1.396(12) . ?
C018 C028 1.396(12) . ?
C019 C01M 1.398(12) . ?
C01A C01B 1.381(13) . ?
C01A C01O 1.415(12) . ?
C01C C01F 1.410(12) . ?
C01D C02A 1.398(14) . ?
C01E C01O 1.379(11) . ?
C01E C01W 1.422(11) . ?
C01F C020 1.412(12) . ?
N01G C022 1.511(12) . ?
N01G C02G 1.510(12) . ?
N01G C02P 1.514(12) . ?
C01H C01P 1.374(13) . ?
C01H C023 1.394(14) . ?
C01I C01N 1.386(13) . ?
C01I C01P 1.407(13) . ?
C01J C01U 1.376(14) . ?
C01J C027 1.409(13) . ?
C01K C01L 1.428(12) . ?
C01K C01V 1.392(12) . ?
C01L C027 1.360(13) . ?
C01M C01Y 1.382(12) . ?
C01N C02D 1.380(13) . ?
N01Q C02I 1.543(13) . ?
N01Q C02N 1.488(15) . ?
N01Q C03A 1.520(14) . ?
C01R C020 1.402(14) . ?
C01R C024 1.376(14) . ?
C01T C01Z 1.400(14) . ?
C01T C028 1.398(13) . ?
C01U C01V 1.396(14) . ?
C01X C02C 1.511(13) . ?
C01Z C02A 1.373(16) . ?
C021 C02C 1.506(14) . ?
C021 C02R 1.542(14) . ?
C022 C02O 1.497(14) . ?
C023 C02D 1.384(14) . ?
N025 C02H 1.507(13) . ?
N025 C034 1.497(14) . ?
N025 C038 1.502(13) . ?
C026 C029 1.507(12) . ?
C027 Br1 1.899(9) . ?
C029 C02L 1.534(13) . ?
C02B C02L 1.536(15) . ?
C02E C02J 1.516(14) . ?
C02E C032 1.510(15) . ?
C02F C02P 1.524(13) . ?
C02F C02U 1.531(13) . ?
C02G C02Z 1.498(14) . ?
C02H C02S 1.519(15) . ?
C02I C030 1.505(14) . ?
C02K C02M 1.496(15) . ?
C02K C02O 1.517(14) . ?
C02N C039 1.499(16) . ?
C02Q C034 1.529(15) . ?
C02Q C036 1.524(15) . ?
C02S C031 1.528(17) . ?
C02T C030 1.515(15) . ?
C02T C03C 1.523(18) . ?
C02U C035 1.515(15) . ?
C02V C02Z 1.530(14) . ?
C02V C03G 1.509(17) . ?
C02W C033 1.530(15) . ?
C02W C038 1.512(16) . ?
C02X C036 1.516(16) . ?
C02Y C039 1.524(16) . ?
C02Y C03B 1.507(18) . ?
C031 C03D 1.528(17) . ?
C032 C03H 1.533(17) . ?
C033 C03E 1.53(2) . ?
C037 C03A 1.473(19) . ?
C037 C1 1.550(16) . ?
C1 C2 1.34(3) . ?
C1 C2A 1.34(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
O00S V0P O00U 90.5(2) . . ?
O00S V0P O00W 87.5(3) . . ?
O00S V0P O011 81.8(2) . . ?
O00V V0P O00S 103.8(3) . . ?
O00V V0P O00U 81.8(2) . . ?
O00V V0P O00W 168.5(3) . . ?
O00V V0P O011 88.2(3) . . ?
O00V V0P O012 88.5(3) . . ?
O00W V0P O00U 96.3(3) . . ?
O00W V0P O011 95.5(3) . . ?
O011 V0P O00U 165.6(3) . . ?
O012 V0P O00S 167.3(3) . . ?
O012 V0P O00U 94.4(3) . . ?
O012 V0P O00W 80.3(3) . . ?
O012 V0P O011 95.7(2) . . ?
O00R V0Q O00X 95.4(3) . . ?
O00R V0Q O00Y 79.9(3) . . ?
O00R V0Q O00Z 94.3(2) . . ?
O00T V0Q O00R 88.9(3) . . ?
O00T V0Q O00X 81.9(2) . . ?
O00T V0Q O00Y 168.3(3) . . ?
O00T V0Q O00Z 88.5(2) . . ?
O00X V0Q O00Y 95.7(3) . . ?
O00X V0Q O00Z 166.2(3) . . ?
O00Z V0Q O00Y 95.6(3) . . ?
O010 V0Q O00R 165.3(3) . . ?
O010 V0Q O00T 104.9(3) . . ?
O010 V0Q O00X 91.7(3) . . ?
O010 V0Q O00Y 86.6(3) . . ?
O010 V0Q O00Z 81.2(2) . . ?
C01P O00R V0Q 116.2(6) . . ?
C01E O00S V0P 113.9(5) . . ?
C01C O00T V0Q 113.5(5) . . ?
C01K O00U V0P 112.8(5) . . ?
C01L O00V V0P 114.6(5) . . ?
C028 O00W V0P 114.7(5) . . ?
C01F O00X V0Q 112.7(5) . . ?
C01I O00Y V0Q 114.3(5) . . ?
C019 O00Z V0Q 113.4(5) . . ?
C01M O010 V0Q 114.6(5) . . ?
C01W O011 V0P 112.8(5) . . ?
C018 O012 V0P 115.7(5) . . ?
C01B C013 Br06 120.1(7) . . ?
C01W C013 Br06 118.8(6) . . ?
C01W C013 C01B 120.9(8) . . ?
C01X N014 C026 112.3(7) . . ?
C01X N014 C02J 111.1(7) . . ?
C026 N014 C02J 112.6(7) . . ?
C019 C015 Br01 117.6(6) . . ?
C01S C015 Br01 121.5(6) . . ?
C01S C015 C019 120.9(8) . . ?
C01S C016 Br05 119.6(7) . . ?
C01S C016 C01Y 120.0(8) . . ?
C01Y C016 Br05 120.4(6) . . ?
C01C C017 Br09 119.2(7) . . ?
C01C C017 C024 120.0(8) . . ?
C024 C017 Br09 120.7(7) . . ?
O012 C018 C01D 125.9(8) . . ?
O012 C018 C028 113.8(7) . . ?
C01D C018 C028 120.4(8) . . ?
O00Z C019 C015 126.3(7) . . ?
O00Z C019 C01M 115.5(7) . . ?
C01M C019 C015 118.2(7) . . ?
C01B C01A Br03 120.7(7) . . ?
C01B C01A C01O 118.9(7) . . ?
C01O C01A Br03 120.4(6) . . ?
C013 C01B Br0B 120.2(7) . . ?
C01A C01B Br0B 119.5(6) . . ?
C01A C01B C013 120.3(8) . . ?
O00T C01C C017 124.5(8) . . ?
O00T C01C C01F 115.2(7) . . ?
C017 C01C C01F 120.3(8) . . ?
C018 C01D Br0H 117.4(7) . . ?
C018 C01D C02A 119.1(9) . . ?
C02A C01D Br0H 123.5(7) . . ?
O00S C01E C01O 125.9(7) . . ?
O00S C01E C01W 115.3(7) . . ?
C01O C01E C01W 118.8(7) . . ?
O00X C01F C01C 115.1(7) . . ?
O00X C01F C020 125.4(8) . . ?
C01C C01F C020 119.5(8) . . ?
C022 N01G C02P 113.2(7) . . ?
C02G N01G C022 109.9(7) . . ?
C02G N01G C02P 112.6(8) . . ?
C01P C01H Br08 118.2(7) . . ?
C01P C01H C023 120.1(9) . . ?
C023 C01H Br08 121.7(7) . . ?
O00Y C01I C01N 126.6(8) . . ?
O00Y C01I C01P 113.9(8) . . ?
C01N C01I C01P 119.5(8) . . ?
C01U C01J Br0G 121.4(7) . . ?
C01U C01J C027 118.8(8) . . ?
C027 C01J Br0G 119.7(7) . . ?
O00U C01K C01L 115.1(7) . . ?
O00U C01K C01V 125.6(8) . . ?
C01V C01K C01L 119.3(8) . . ?
O00V C01L C01K 114.3(7) . . ?
O00V C01L C027 126.2(8) . . ?
C027 C01L C01K 119.5(8) . . ?
O010 C01M C019 114.7(7) . . ?
O010 C01M C01Y 123.7(8) . . ?
C01Y C01M C019 121.5(8) . . ?
C01I C01N Br0J 118.0(7) . . ?
C02D C01N Br0J 121.1(7) . . ?
C02D C01N C01I 120.7(8) . . ?
C01A C01O Br04 120.2(6) . . ?
C01E C01O Br04 118.4(6) . . ?
C01E C01O C01A 121.3(7) . . ?
O00R C01P C01H 125.5(9) . . ?
O00R C01P C01I 115.0(8) . . ?
C01H C01P C01I 119.5(9) . . ?
C02N N01Q C02I 113.5(8) . . ?
C02N N01Q C03A 112.4(8) . . ?
C03A N01Q C02I 110.0(8) . . ?
C020 C01R Br0I 119.0(7) . . ?
C024 C01R Br0I 119.9(7) . . ?
C024 C01R C020 121.1(8) . . ?
C015 C01S Br0A 119.6(6) . . ?
C015 C01S C016 119.8(8) . . ?
C016 C01S Br0A 120.5(6) . . ?
C01Z C01T Br0F 122.9(7) . . ?
C028 C01T Br0F 118.4(7) . . ?
C028 C01T C01Z 118.7(9) . . ?
C01J C01U Br0E 119.7(7) . . ?
C01J C01U C01V 121.3(8) . . ?
C01V C01U Br0E 119.0(7) . . ?
C01K C01V Br0C 118.9(7) . . ?
C01K C01V C01U 119.6(9) . . ?
C01U C01V Br0C 121.5(7) . . ?
O011 C01W C013 125.7(7) . . ?
O011 C01W C01E 114.7(7) . . ?
C013 C01W C01E 119.6(7) . . ?
N014 C01X C02C 114.1(7) . . ?
C016 C01Y Br02 120.9(6) . . ?
C01M C01Y Br02 119.7(7) . . ?
C01M C01Y C016 119.5(8) . . ?
C01T C01Z Br0N 118.9(8) . . ?
C02A C01Z Br0N 120.0(7) . . ?
C02A C01Z C01T 121.1(9) . . ?
C01F C020 Br0D 118.5(7) . . ?
C01R C020 Br0D 122.1(7) . . ?
C01R C020 C01F 119.4(9) . . ?
C02C C021 C02R 110.4(8) . . ?
C02O C022 N01G 113.3(8) . . ?
C01H C023 Br0M 119.9(7) . . ?
C02D C023 Br0M 119.5(7) . . ?
C02D C023 C01H 120.6(8) . . ?
C017 C024 Br0L 119.0(7) . . ?
C01R C024 Br0L 121.4(7) . . ?
C01R C024 C017 119.6(8) . . ?
C034 N025 C02H 114.4(8) . . ?
C034 N025 C038 112.1(9) . . ?
C038 N025 C02H 110.5(8) . . ?
C029 C026 N014 112.6(7) . . ?
C01J C027 Br1 120.6(7) . . ?
C01L C027 C01J 121.3(9) . . ?
C01L C027 Br1 118.0(7) . . ?
O00W C028 C018 115.4(8) . . ?
O00W C028 C01T 124.4(8) . . ?
C018 C028 C01T 120.2(8) . . ?
C026 C029 C02L 110.2(8) . . ?
C01D C02A Br0O 118.1(8) . . ?
C01Z C02A Br0O 121.5(7) . . ?
C01Z C02A C01D 120.4(8) . . ?
C021 C02C C01X 112.3(8) . . ?
C01N C02D Br0K 119.6(8) . . ?
C01N C02D C023 119.3(9) . . ?
C023 C02D Br0K 121.1(7) . . ?
C032 C02E C02J 111.3(9) . . ?
C02P C02F C02U 110.4(8) . . ?
C02Z C02G N01G 111.2(8) . . ?
N025 C02H C02S 113.0(8) . . ?
C030 C02I N01Q 113.4(8) . . ?
C02E C02J N014 111.2(7) . . ?
C02M C02K C02O 112.3(9) . . ?
C029 C02L C02B 111.2(9) . . ?
N01Q C02N C039 114.3(8) . . ?
C022 C02O C02K 112.6(8) . . ?
N01G C02P C02F 112.9(8) . . ?
C036 C02Q C034 109.6(9) . . ?
C02H C02S C031 111.2(9) . . ?
C030 C02T C03C 112.8(10) . . ?
C035 C02U C02F 110.9(9) . . ?
C03G C02V C02Z 113.2(10) . . ?
C038 C02W C033 113.8(10) . . ?
C03B C02Y C039 113.3(10) . . ?
C02G C02Z C02V 110.7(9) . . ?
C02I C030 C02T 111.7(9) . . ?
C03D C031 C02S 112.0(11) . . ?
C02E C032 C03H 111.8(11) . . ?
C02W C033 C03E 111.6(11) . . ?
N025 C034 C02Q 114.9(9) . . ?
C02X C036 C02Q 111.4(10) . . ?
C03A C037 C1 111.3(11) . . ?
N025 C038 C02W 113.0(9) . . ?
C02N C039 C02Y 111.9(9) . . ?
C037 C03A N01Q 112.7(9) . . ?
C2 C1 C037 115.6(15) . . ?
C2A C1 C037 118.2(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method layering
_chemical_properties_physical    Air-sensitive,Heat-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_jz29
_database_code_depnum_ccdc_archive 'CCDC 1921676'
loop_
_audit_author_name
_audit_author_address
'Cassidy E. Jackson'
;Colorado State University
United States of America
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-05 downloaded from the CCDC.
;
_audit_creation_date             2019-05-15
_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            (n-Bu3NH)2[V(4,5-Br2-C6H2O2)3]
_chemical_name_systematic        
'tris(4,5-dibromo-catecholato)vanadate(IV) bis-tri-n-butylammonium'
_chemical_formula_moiety         'C18 H6 Br6 O6 V, 2(C12 H28 N)'
_chemical_formula_sum            'C42 H62 Br6 N2 O6 V'
_chemical_formula_weight         1221.33
_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'
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'
Br Br -0.2901 2.4595 '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      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+3/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+1/4'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   10.7250(6)
_cell_length_b                   10.7250(6)
_cell_length_c                   42.298(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4865.3(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.69
_shelx_estimated_absorpt_T_max   0.519
_shelx_estimated_absorpt_T_min   0.499
_exptl_absorpt_coefficient_mu    5.176
_exptl_absorpt_correction_T_max  0.7043
_exptl_absorpt_correction_T_min  0.6083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1220 before and 0.1131 after correction. The Ratio of minimum to maximum transmission is 0.8637. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.146
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            408403
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         1.926
_diffrn_ambient_temperature      119.76
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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         0.666
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4495
_reflns_number_total             4625
_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       '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 (Sheldrick, 2015)'
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 
;
 Flack x determined using 1744 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.059(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.148
_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)+(0.0689P)²+16.3328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1500
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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. Restrained distances
 C20-C18
 1.52 with sigma of 0.02
 C20-C18A
 1.52 with sigma of 0.02
3. Others
 Sof(H20C)=Sof(H20D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(H1AC)=Sof(H1AD)=
 Sof(C1A)=Sof(H1AE)=Sof(H1AF)=Sof(H1AG)=Sof(C5AB)=Sof(H5AD)=Sof(H5AE)=Sof(H5AF)=
 Sof(C4AB)=Sof(H4AC)=Sof(H4AD)=Sof(C2AB)=Sof(H2AC)=Sof(H2AD)=1-FVAR(1)
 Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H20A)=
 Sof(H20B)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=
 Sof(H5AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C0AA(H0AA,H0AB), C2AA(H2AA,H2AB), C15(H15A,H15B), C18(H18A,
 H18B), C20(H20A,H20B), C20(H20C,H20D), C4AA(H4AA,H4AB), C6AA(H6AA,H6AB),
 C18A(H18C,H18D), C1AB(H1AA,H1AB), C1AB(H1AC,H1AD), C4AB(H4AC,H4AD), C2AB(H2AC,
 H2AD)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C21(H21)
4.d Idealised Me refined as rotating group:
 C5AA(H5AA,H5AB,H5AC), C7AA(H7AA,H7AB,H7AC), C1(H1A,H1B,H1C), C1A(H1AE,H1AF,
 H1AG), C5AB(H5AD,H5AE,H5AF)
;
_atom_sites_solution_hydrogens   geom
_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
Br1 Br 0.23775(9) 1.65556(10) 0.28474(3) 0.0552(3) Uani 1 1 d . . . . .
V2 V 0.73355(12) 1.26645(12) 0.250000 0.0311(4) Uani 1 2 d S T P . .
Br3 Br 1.20082(10) 1.40962(15) 0.35577(3) 0.0702(4) Uani 1 1 d . . . . .
Br4 Br 1.04937(16) 1.16806(12) 0.39013(3) 0.0828(5) Uani 1 1 d . . . . .
O1 O 0.7753(5) 1.1685(5) 0.28738(14) 0.0387(13) Uani 1 1 d . . . . .
O2 O 0.5943(5) 1.3226(5) 0.27555(13) 0.0343(12) Uani 1 1 d . . . . .
O3 O 0.8792(5) 1.3560(5) 0.26424(13) 0.0366(12) Uani 1 1 d . . . . .
C4 C 0.4303(8) 1.4759(8) 0.2794(2) 0.0396(19) Uani 1 1 d . . . . .
H4 H 0.398984 1.444721 0.298838 0.048 Uiso 1 1 calc R . . . .
C5 C 1.0604(9) 1.3303(10) 0.3362(2) 0.048(2) Uani 1 1 d . . . . .
C6 C 0.9231(8) 1.3214(8) 0.29219(19) 0.0385(18) Uani 1 1 d . . . . .
C7 C 0.5331(7) 1.4208(7) 0.26429(19) 0.0341(16) Uani 1 1 d . . . . .
C8 C 1.0235(8) 1.3778(9) 0.3076(2) 0.0420(19) Uani 1 1 d . . . . .
H8 H 1.065266 1.447158 0.298502 0.050 Uiso 1 1 calc R . . . .
C9 C 0.3761(8) 1.5793(7) 0.2643(2) 0.0392(18) Uani 1 1 d . . . . .
C10 C 1.0004(10) 1.2340(10) 0.3499(2) 0.051(3) Uani 1 1 d . . . . .
C11 C 0.8645(8) 1.2180(8) 0.3054(2) 0.0384(18) Uani 1 1 d . . . . .
C21 C 0.8997(10) 1.1742(9) 0.3352(2) 0.048(2) Uani 1 1 d . . . . .
H21 H 0.857198 1.106966 0.345085 0.058 Uiso 1 1 calc R . . . .
N3 N 1.4667(8) 1.0436(9) 0.0502(2) 0.057(2) Uani 1 1 d . . . . .
H3 H 1.413958 1.111982 0.041313 0.068 Uiso 1 1 calc R . . . .
C3AA C 1.6531(9) 1.1876(11) 0.0478(3) 0.058(3) Uani 1 1 d . . . . .
H3AA H 1.660072 1.193128 0.071133 0.069 Uiso 1 1 calc R . . . .
H3AB H 1.597356 1.255313 0.040510 0.069 Uiso 1 1 calc R . . . .
C0AA C 1.6009(9) 1.0659(10) 0.0388(2) 0.052(2) Uani 1 1 d . . . . .
H0AA H 1.654969 0.999466 0.047520 0.063 Uiso 1 1 calc R . . . .
H0AB H 1.602792 1.058749 0.015492 0.063 Uiso 1 1 calc R . . . .
C2AA C 1.4805(16) 0.8010(16) 0.0467(4) 0.045(4) Uiso 0.69(3) 1 d . . . A 1
H2AA H 1.466883 0.790350 0.069722 0.054 Uiso 0.69(3) 1 calc R . . A 1
H2AB H 1.571442 0.808831 0.043282 0.054 Uiso 0.69(3) 1 calc R . . A 1
C15 C 1.4567(11) 1.0503(12) 0.0848(3) 0.062(3) Uani 1 1 d . . . . .
H15A H 1.484111 1.133441 0.092229 0.074 Uiso 1 1 calc R . . B 1
H15B H 1.511330 0.986649 0.094568 0.074 Uiso 1 1 calc R . . B 1
C18 C 1.3098(17) 1.0665(17) 0.1284(4) 0.063(5) Uiso 0.69(3) 1 d D . . A 1
H18A H 1.362979 1.013669 0.142045 0.076 Uiso 0.69(3) 1 calc R . . A 1
H18B H 1.336061 1.154288 0.131123 0.076 Uiso 0.69(3) 1 calc R . . A 1
C20 C 1.3259(14) 1.0284(15) 0.0943(3) 0.077(4) Uani 1 1 d D . . . .
H20A H 1.304922 0.939095 0.091788 0.093 Uiso 0.69(3) 1 calc R . . A 1
H20B H 1.269200 1.077712 0.080742 0.093 Uiso 0.69(3) 1 calc R . . A 1
H20C H 1.327809 0.959274 0.109833 0.093 Uiso 0.31(3) 1 calc R . . A 2
H20D H 1.282611 0.995940 0.075377 0.093 Uiso 0.31(3) 1 calc R . . A 2
C4AA C 1.435(2) 0.684(2) 0.0299(6) 0.063(6) Uiso 0.69(3) 1 d . . . A 1
H4AA H 1.347601 0.666296 0.035871 0.076 Uiso 0.69(3) 1 calc R . . A 1
H4AB H 1.438899 0.695833 0.006761 0.076 Uiso 0.69(3) 1 calc R . . A 1
C6AA C 1.7802(10) 1.2022(12) 0.0330(3) 0.062(3) Uani 1 1 d . . . . .
H6AA H 1.826139 1.122543 0.035051 0.074 Uiso 1 1 calc R . . . .
H6AB H 1.769843 1.219653 0.010167 0.074 Uiso 1 1 calc R . . . .
C5AA C 1.5163(17) 0.5762(17) 0.0393(5) 0.057(4) Uiso 0.69(3) 1 d . . . A 1
H5AA H 1.486535 0.500133 0.028941 0.086 Uiso 0.69(3) 1 calc GR . . A 1
H5AB H 1.513151 0.565398 0.062289 0.086 Uiso 0.69(3) 1 calc GR . . A 1
H5AC H 1.602435 0.592882 0.032786 0.086 Uiso 0.69(3) 1 calc GR . . A 1
C7AA C 1.8547(14) 1.3022(17) 0.0473(4) 0.096(5) Uani 1 1 d . . . . .
H7AA H 1.925853 1.321285 0.033541 0.144 Uiso 1 1 calc GR . . . .
H7AB H 1.885065 1.275248 0.068012 0.144 Uiso 1 1 calc GR . . . .
H7AC H 1.803002 1.376909 0.049735 0.144 Uiso 1 1 calc GR . . . .
C1 C 1.177(2) 1.053(3) 0.1379(6) 0.084(6) Uiso 0.69(3) 1 d . . . A 1
H1A H 1.162052 0.966504 0.144607 0.126 Uiso 0.69(3) 1 calc GR . . A 1
H1B H 1.123348 1.072809 0.119937 0.126 Uiso 0.69(3) 1 calc GR . . A 1
H1C H 1.159253 1.109411 0.155468 0.126 Uiso 0.69(3) 1 calc GR . . A 1
C18A C 1.243(7) 1.126(6) 0.108(2) 0.15(3) Uiso 0.31(3) 1 d D . . A 2
H18C H 1.294928 1.184895 0.120214 0.174 Uiso 0.31(3) 1 calc R . . A 2
H18D H 1.204941 1.173262 0.090351 0.174 Uiso 0.31(3) 1 calc R . . A 2
C1AB C 1.4190(10) 0.9215(10) 0.0365(3) 0.059(3) Uani 1 1 d . . . . .
H1AA H 1.329174 0.915246 0.041645 0.071 Uiso 0.69(3) 1 calc R . . A 1
H1AB H 1.425799 0.927069 0.013222 0.071 Uiso 0.69(3) 1 calc R . . A 1
H1AC H 1.327809 0.913274 0.039438 0.071 Uiso 0.31(3) 1 calc R . . A 2
H1AD H 1.438971 0.914666 0.013737 0.071 Uiso 0.31(3) 1 calc R . . A 2
C1A C 1.141(4) 1.083(4) 0.1287(10) 0.059(10) Uiso 0.31(3) 1 d . . . A 2
H1AE H 1.080742 1.035271 0.116252 0.089 Uiso 0.31(3) 1 calc GR . . A 2
H1AF H 1.100019 1.154810 0.138363 0.089 Uiso 0.31(3) 1 calc GR . . A 2
H1AG H 1.175855 1.029305 0.145365 0.089 Uiso 0.31(3) 1 calc GR . . A 2
C5AB C 1.524(4) 0.590(4) 0.0520(12) 0.065(11) Uiso 0.31(3) 1 d . . . A 2
H5AD H 1.579381 0.556886 0.035586 0.097 Uiso 0.31(3) 1 calc GR . . A 2
H5AE H 1.466264 0.525071 0.058905 0.097 Uiso 0.31(3) 1 calc GR . . A 2
H5AF H 1.573884 0.618730 0.069990 0.097 Uiso 0.31(3) 1 calc GR . . A 2
C4AB C 1.453(5) 0.696(4) 0.0390(12) 0.060(12) Uiso 0.31(3) 1 d . . . A 2
H4AC H 1.362419 0.680642 0.041948 0.073 Uiso 0.31(3) 1 calc R . . A 2
H4AD H 1.468784 0.702887 0.015995 0.073 Uiso 0.31(3) 1 calc R . . A 2
C2AB C 1.489(3) 0.825(3) 0.0557(9) 0.042(8) Uiso 0.31(3) 1 d . . . A 2
H2AC H 1.462158 0.825797 0.078067 0.050 Uiso 0.31(3) 1 calc R . . A 2
H2AD H 1.580217 0.839454 0.054721 0.050 Uiso 0.31(3) 1 calc R . . 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
Br1 C9 1.901(9) . ?
V2 O1 1.950(6) 8_775 ?
V2 O1 1.950(6) . ?
V2 O2 1.939(6) . ?
V2 O2 1.939(6) 8_775 ?
V2 O3 1.930(6) . ?
V2 O3 1.930(6) 8_775 ?
Br3 C5 1.917(10) . ?
Br4 C10 1.917(9) . ?
O1 C11 1.333(10) . ?
O2 C7 1.330(10) . ?
O3 C6 1.325(10) . ?
C4 C7 1.404(11) . ?
C4 C9 1.405(12) . ?
C5 C8 1.371(13) . ?
C5 C10 1.348(16) . ?
C6 C8 1.397(12) . ?
C6 C11 1.392(13) . ?
C7 C7 1.397(17) 8_775 ?
C9 C9 1.389(19) 8_775 ?
C10 C21 1.400(15) . ?
C11 C21 1.397(12) . ?
N3 C0AA 1.536(13) . ?
N3 C15 1.469(14) . ?
N3 C1AB 1.520(15) . ?
C3AA C0AA 1.471(15) . ?
C3AA C6AA 1.509(14) . ?
C2AA C4AA 1.52(3) . ?
C2AA C1AB 1.514(18) . ?
C15 C20 1.478(17) . ?
C18 C20 1.507(17) . ?
C18 C1 1.48(3) . ?
C20 C18A 1.49(3) . ?
C4AA C5AA 1.50(3) . ?
C6AA C7AA 1.467(19) . ?
C18A C1A 1.47(8) . ?
C1AB C2AB 1.52(3) . ?
C5AB C4AB 1.48(6) . ?
C4AB C2AB 1.60(6) . ?

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 V2 O1 114.2(4) . 8_775 ?
O2 V2 O1 83.8(2) . . ?
O2 V2 O1 159.7(2) 8_775 . ?
O2 V2 O1 159.7(2) . 8_775 ?
O2 V2 O1 83.8(2) 8_775 8_775 ?
O2 V2 O2 80.4(3) . 8_775 ?
O3 V2 O1 86.1(2) 8_775 . ?
O3 V2 O1 80.2(2) 8_775 8_775 ?
O3 V2 O1 86.1(2) . 8_775 ?
O3 V2 O1 80.2(2) . . ?
O3 V2 O2 107.2(2) 8_775 8_775 ?
O3 V2 O2 92.4(2) . 8_775 ?
O3 V2 O2 107.2(2) . . ?
O3 V2 O2 92.4(2) 8_775 . ?
O3 V2 O3 154.5(4) 8_775 . ?
C11 O1 V2 114.5(5) . . ?
C7 O2 V2 115.3(5) . . ?
C6 O3 V2 115.3(5) . . ?
C7 C4 C9 116.9(8) . . ?
C8 C5 Br3 116.3(8) . . ?
C10 C5 Br3 122.1(7) . . ?
C10 C5 C8 121.7(9) . . ?
O3 C6 C8 124.7(9) . . ?
O3 C6 C11 114.9(7) . . ?
C11 C6 C8 120.3(8) . . ?
O2 C7 C4 123.9(8) . . ?
O2 C7 C7 114.6(4) . 8_775 ?
C7 C7 C4 121.5(5) 8_775 . ?
C5 C8 C6 118.3(9) . . ?
C4 C9 Br1 117.2(7) . . ?
C9 C9 Br1 121.1(3) 8_775 . ?
C9 C9 C4 121.6(5) 8_775 . ?
C5 C10 Br4 122.1(7) . . ?
C5 C10 C21 122.0(8) . . ?
C21 C10 Br4 115.8(8) . . ?
O1 C11 C6 114.3(7) . . ?
O1 C11 C21 125.2(9) . . ?
C6 C11 C21 120.5(8) . . ?
C11 C21 C10 117.0(10) . . ?
C15 N3 C0AA 111.9(8) . . ?
C15 N3 C1AB 113.4(9) . . ?
C1AB N3 C0AA 109.3(8) . . ?
C0AA C3AA C6AA 109.1(9) . . ?
C3AA C0AA N3 114.4(8) . . ?
C1AB C2AA C4AA 115.7(14) . . ?
N3 C15 C20 109.5(10) . . ?
C1 C18 C20 110.0(16) . . ?
C15 C20 C18 109.1(12) . . ?
C15 C20 C18A 124(4) . . ?
C5AA C4AA C2AA 109.1(17) . . ?
C7AA C6AA C3AA 113.4(11) . . ?
C1A C18A C20 117(5) . . ?
C2AA C1AB N3 118.7(11) . . ?
C2AB C1AB N3 102.6(18) . . ?
C5AB C4AB C2AB 112(4) . . ?
C1AB C2AB C4AB 103(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'slow evaporation'
_chemical_properties_physical    Air-sensitive,Heat-sensitive
