# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1581481'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2018-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        (TBA)2_1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C24 H28 I2 O21 V6), 2(C16 H36 N), 1.5(C2 H3 N)'
_chemical_formula_sum            'C59 H102.50 I2 N3.50 O21 V6'
_chemical_formula_weight         1756.38

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'
I I -0.4742 1.8119 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   26.365(3)
_cell_length_b                   17.405(2)
_cell_length_c                   16.919(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.164(2)
_cell_angle_gamma                90
_cell_volume                     7493.4(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.34

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             3572
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.610
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1835 before and 0.1026 after correction. The Ratio of minimum to maximum transmission is 0.4855. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67274
_diffrn_reflns_av_unetI/netI     0.1057
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         0.800
_diffrn_reflns_theta_max         26.646
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15586
_reflns_number_gt                10061
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART V5.631 (?, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1490P)²+26.3270P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15586
_refine_ls_number_parameters     846
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2462
_refine_ls_wR_factor_gt          0.2127
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_restrained_S_all      0.942
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
I001 I 0.80113(3) 0.80629(4) 0.17863(4) 0.0531(2) Uani 1 1 d . . . . .
I002 I 0.33000(3) 0.55004(3) -0.02567(5) 0.0610(2) Uani 1 1 d . . . . .
V003 V 0.47737(5) 0.62355(6) 0.48732(6) 0.0153(2) Uani 1 1 d . . . . .
V004 V 0.43780(5) 0.48419(6) 0.38148(6) 0.0151(2) Uani 1 1 d . . . . .
V005 V 0.44417(5) 0.49192(6) 0.57948(6) 0.0153(2) Uani 1 1 d . . . . .
V006 V 0.06063(5) 0.92003(6) 0.07275(7) 0.0212(3) Uani 1 1 d . . . . .
V007 V 0.01592(5) 0.97191(7) -0.12043(7) 0.0224(3) Uani 1 1 d . . . . .
V008 V -0.05242(5) 0.89634(6) -0.02404(8) 0.0233(3) Uani 1 1 d . . . . .
O009 O 0.60287(18) 0.5311(2) 0.5292(3) 0.0154(9) Uani 1 1 d . . . . .
O00A O 0.5000 0.5000 0.5000 0.0126(13) Uani 1 2 d S . P . .
O00B O 0.53242(18) 0.6209(2) 0.4290(2) 0.0146(9) Uani 1 1 d . . . . .
O00C O 0.54046(18) 0.6223(2) 0.5897(2) 0.0153(9) Uani 1 1 d . . . . .
O00D O 0.43992(18) 0.5913(2) 0.5639(3) 0.0172(9) Uani 1 1 d . . . . .
O00E O 0.42901(18) 0.5902(2) 0.4033(2) 0.0159(9) Uani 1 1 d . . . . .
O00F O 0.0664(2) 1.0625(2) -0.0774(3) 0.0207(10) Uani 1 1 d . . . . .
O00G O 0.0000 1.0000 0.0000 0.0172(14) Uani 1 2 d S . P . .
O00H O 0.48981(19) 0.5024(2) 0.3385(3) 0.0181(10) Uani 1 1 d . . . . .
O00I O 0.1022(2) 1.0152(3) 0.0768(3) 0.0234(11) Uani 1 1 d . . . . .
O00J O 0.3885(2) 0.4663(2) 0.3056(3) 0.0211(10) Uani 1 1 d . . . . .
O00K O 0.46956(19) 0.7156(2) 0.4858(3) 0.0202(10) Uani 1 1 d . . . . .
O00L O 0.40303(19) 0.4746(3) 0.6332(3) 0.0208(10) Uani 1 1 d . . . . .
O00M O 0.00475(19) 0.8497(3) 0.0314(3) 0.0223(10) Uani 1 1 d . . . . .
O00N O 0.0711(2) 0.9131(3) -0.0440(3) 0.0219(10) Uani 1 1 d . . . . .
O00O O 0.0355(2) 0.9501(3) 0.1541(3) 0.0245(11) Uani 1 1 d . . . . .
O00P O -0.0312(2) 0.8999(3) -0.1226(3) 0.0277(12) Uani 1 1 d . . . . .
O00Q O 0.2315(2) 0.9233(3) -0.0052(3) 0.0271(11) Uani 1 1 d . . . . .
O00R O -0.0970(2) 0.8313(3) -0.0439(3) 0.0331(13) Uani 1 1 d . . . . .
O00S O 0.1090(2) 0.8653(3) 0.1145(3) 0.0275(12) Uani 1 1 d . . . . .
O00T O 0.0361(2) 0.9565(3) -0.2010(3) 0.0315(13) Uani 1 1 d . . . . .
O00U O 0.6749(2) 0.7418(3) 0.4809(3) 0.0291(12) Uani 1 1 d . . . . .
N00V N 0.4144(2) 0.7761(3) 0.2362(3) 0.0200(12) Uani 1 1 d . . . . .
N00W N 0.0116(3) 0.6854(3) -0.1644(4) 0.0271(14) Uani 1 1 d . . . . .
C00X C 0.3755(3) 0.8373(4) 0.1937(4) 0.0227(15) Uani 1 1 d . . . . .
H00A H 0.3462 0.8120 0.1557 0.027 Uiso 1 1 calc R U . . .
H00B H 0.3926 0.8697 0.1619 0.027 Uiso 1 1 calc R U . . .
C00Y C 0.2908(3) 0.8234(4) -0.0214(4) 0.0221(15) Uani 1 1 d . . . . .
C00Z C 0.3385(3) 0.7982(4) -0.0323(4) 0.0233(15) Uani 1 1 d . . . . .
H00Z H 0.3630 0.8340 -0.0402 0.028 Uiso 1 1 calc R U . . .
C010 C 0.3502(3) 0.7209(5) -0.0317(4) 0.0292(17) Uani 1 1 d . . . . .
H010 H 0.3823 0.7046 -0.0389 0.035 Uiso 1 1 calc R U . . .
C011 C 0.5724(3) 0.6796(3) 0.4445(4) 0.0185(14) Uani 1 1 d . . . . .
H4AA H 0.5558 0.7297 0.4388 0.022 Uiso 1 1 calc R U . . .
H H 0.5924 0.6757 0.4041 0.022 Uiso 1 1 calc R U . . .
C012 C 0.6098(3) 0.6725(3) 0.5301(4) 0.0187(14) Uani 1 1 d . . . . .
C013 C 0.4575(3) 0.8102(4) 0.3044(4) 0.0244(16) Uani 1 1 d . . . . .
H01Q H 0.4816 0.7694 0.3290 0.029 Uiso 1 1 calc R U . . .
H01R H 0.4419 0.8299 0.3462 0.029 Uiso 1 1 calc R U . . .
C014 C 0.4380(3) 0.7392(4) 0.1722(4) 0.0213(15) Uani 1 1 d . . . . .
H01S H 0.4103 0.7120 0.1330 0.026 Uiso 1 1 calc R U . . .
H01T H 0.4506 0.7797 0.1428 0.026 Uiso 1 1 calc R U . . .
C015 C 0.3865(3) 0.7160(4) 0.2750(4) 0.0251(16) Uani 1 1 d . . . . .
H01U H 0.3669 0.7424 0.3081 0.030 Uiso 1 1 calc R U . . .
H01V H 0.4130 0.6848 0.3117 0.030 Uiso 1 1 calc R U . . .
C016 C 0.4826(3) 0.6838(4) 0.2052(4) 0.0253(16) Uani 1 1 d . . . . .
H01W H 0.4735 0.6498 0.2449 0.030 Uiso 1 1 calc R U . . .
H01X H 0.5139 0.7122 0.2328 0.030 Uiso 1 1 calc R U . . .
C017 C 0.6388(3) 0.5940(3) 0.5387(4) 0.0197(14) Uani 1 1 d . . . . .
H5AA H 0.6583 0.5904 0.4977 0.024 Uiso 1 1 calc R U . . .
HA H 0.6636 0.5910 0.5922 0.024 Uiso 1 1 calc R U . . .
C018 C 0.1235(3) 0.9164(4) -0.0514(4) 0.0229(15) Uani 1 1 d . . . . .
H1BA H 0.1233 0.9054 -0.1077 0.028 Uiso 1 1 calc R U . . .
HB H 0.1440 0.8768 -0.0172 0.028 Uiso 1 1 calc R U . . .
C019 C 0.2789(3) 0.9087(4) -0.0272(5) 0.0272(16) Uani 1 1 d . . . . .
H2BA H 0.3075 0.9366 0.0091 0.033 Uiso 1 1 calc R U . . .
HC H 0.2757 0.9263 -0.0827 0.033 Uiso 1 1 calc R U . . .
C01A C 0.3128(3) 0.6227(4) 0.2610(4) 0.0241(15) Uani 1 1 d . . . . .
H01Y H 0.3340 0.5937 0.3067 0.029 Uiso 1 1 calc R U . . .
HD H 0.2936 0.6614 0.2829 0.029 Uiso 1 1 calc R U . . .
C01B C 0.7297(3) 0.8116(4) 0.4165(5) 0.0270(17) Uani 1 1 d . . . . .
C01C C 0.1502(3) 0.9942(4) -0.0271(4) 0.0230(15) Uani 1 1 d . . . . .
C01D C 0.3489(3) 0.6626(4) 0.2157(4) 0.0225(15) Uani 1 1 d . . . . .
H01Z H 0.3687 0.6245 0.1945 0.027 Uiso 1 1 calc R U . . .
HE H 0.3280 0.6920 0.1699 0.027 Uiso 1 1 calc R U . . .
C01E C 0.4890(3) 0.8746(4) 0.2784(4) 0.0251(16) Uani 1 1 d . . . . .
H01 H 0.4680 0.9211 0.2690 0.030 Uiso 1 1 calc R U . . .
HF H 0.4968 0.8606 0.2274 0.030 Uiso 1 1 calc R U . . .
C01F C 0.1196(3) 1.0569(4) -0.0828(4) 0.0238(16) Uani 1 1 d . . . . .
H3BA H 0.1370 1.1058 -0.0678 0.029 Uiso 1 1 calc R U . . .
HG H 0.1197 1.0459 -0.1390 0.029 Uiso 1 1 calc R U . . .
C01G C 0.5802(3) 0.6804(4) 0.5967(4) 0.0179(14) Uani 1 1 d . . . . .
H6AA H 0.6051 0.6765 0.6501 0.021 Uiso 1 1 calc R U . . .
HH H 0.5639 0.7307 0.5927 0.021 Uiso 1 1 calc R U . . .
C01H C 0.6490(3) 0.7387(4) 0.5450(4) 0.0221(15) Uani 1 1 d . . . . .
H7AA H 0.6308 0.7868 0.5472 0.027 Uiso 1 1 calc R U . . .
HI H 0.6747 0.7316 0.5972 0.027 Uiso 1 1 calc R U . . .
C01I C -0.0169(3) 0.6082(4) -0.1779(5) 0.0266(16) Uani 1 1 d . . . . .
H01A H 0.0062 0.5693 -0.1466 0.032 Uiso 1 1 calc R U . . .
H01B H -0.0238 0.5947 -0.2353 0.032 Uiso 1 1 calc R U . . .
C01J C 0.1529(3) 1.0118(4) 0.0625(4) 0.0256(16) Uani 1 1 d . . . . .
H4BA H 0.1734 0.9723 0.0970 0.031 Uiso 1 1 calc R U . . .
HJ H 0.1706 1.0606 0.0775 0.031 Uiso 1 1 calc R U . . .
C01K C 0.4938(3) 0.6362(4) 0.1353(5) 0.0305(17) Uani 1 1 d . . . . .
H1AA H 0.4662 0.5984 0.1170 0.037 Uiso 1 1 calc R U . . .
HK H 0.4940 0.6696 0.0895 0.037 Uiso 1 1 calc R U . . .
C01L C 0.3137(3) 0.6679(4) -0.0201(4) 0.0315(18) Uani 1 1 d . . . . .
C01M C 0.0626(3) 0.6758(4) -0.1902(4) 0.0272(16) Uani 1 1 d . . . . .
H01C H 0.0858 0.6422 -0.1513 0.033 Uiso 1 1 calc R U . . .
H01D H 0.0546 0.6507 -0.2432 0.033 Uiso 1 1 calc R U . . .
C01N C 0.1453(3) 0.7338(4) -0.2081(5) 0.0332(18) Uani 1 1 d . . . . .
H01E H 0.1411 0.7037 -0.2577 0.040 Uiso 1 1 calc R U . . .
H01F H 0.1651 0.7031 -0.1626 0.040 Uiso 1 1 calc R U . . .
C01O C 0.2659(3) 0.6908(4) -0.0098(5) 0.0306(17) Uani 1 1 d . . . . .
H5BA H 0.2414 0.6545 -0.0035 0.037 Uiso 1 1 calc R U . . .
C01P C 0.2053(3) 0.9919(4) -0.0403(5) 0.0274(16) Uani 1 1 d . . . . .
H6BA H 0.2030 0.9933 -0.0984 0.033 Uiso 1 1 calc R U . . .
HL H 0.2252 1.0364 -0.0149 0.033 Uiso 1 1 calc R U . . .
C01Q C 0.5406(3) 0.8899(5) 0.3441(5) 0.0344(19) Uani 1 1 d . . . . .
H3AA H 0.5627 0.8447 0.3492 0.041 Uiso 1 1 calc R U . . .
HM H 0.5589 0.9319 0.3258 0.041 Uiso 1 1 calc R U . . .
C01R C 0.0827(3) 0.6812(4) 0.0643(5) 0.0295(17) Uani 1 1 d . . . . .
H01G H 0.0661 0.7268 0.0790 0.035 Uiso 1 1 calc R U . . .
H01H H 0.0870 0.6445 0.1087 0.035 Uiso 1 1 calc R U . . .
C01S C -0.0687(3) 0.6068(4) -0.1536(5) 0.0308(17) Uani 1 1 d . . . . .
H01I H -0.0642 0.6326 -0.1014 0.037 Uiso 1 1 calc R U . . .
H01J H -0.0953 0.6345 -0.1942 0.037 Uiso 1 1 calc R U . . .
C01T C 0.7701(4) 0.8077(5) 0.2818(5) 0.037(2) Uani 1 1 d . . . . .
C01U C 0.0234(3) 0.7097(4) -0.0758(4) 0.0307(18) Uani 1 1 d . . . . .
H01K H -0.0088 0.7275 -0.0645 0.037 Uiso 1 1 calc R U . . .
H01L H 0.0477 0.7526 -0.0673 0.037 Uiso 1 1 calc R U . . .
C01V C -0.0232(3) 0.7480(4) -0.2148(5) 0.0311(17) Uani 1 1 d . . . . .
H01M H -0.0555 0.7513 -0.1977 0.037 Uiso 1 1 calc R U . . .
H01N H -0.0052 0.7970 -0.2024 0.037 Uiso 1 1 calc R U . . .
C01W C 0.2546(3) 0.7697(4) -0.0089(5) 0.0295(17) Uani 1 1 d . . . . .
H7BA H 0.2230 0.7860 0.0001 0.035 Uiso 1 1 calc R U . . .
C01X C 0.7249(4) 0.8483(5) 0.2777(5) 0.0357(19) Uani 1 1 d . . . . .
H8AA H 0.7083 0.8750 0.2304 0.043 Uiso 1 1 calc R U . . .
C01Y C 0.0471(4) 0.6463(4) -0.0141(5) 0.0353(19) Uani 1 1 d . . . . .
H01O H 0.0191 0.6172 -0.0007 0.042 Uiso 1 1 calc R U . . .
H01P H 0.0674 0.6113 -0.0384 0.042 Uiso 1 1 calc R U . . .
C01Z C 0.7770(3) 0.7725(4) 0.4195(5) 0.0314(18) Uani 1 1 d . . . . .
H9AA H 0.7947 0.7476 0.4675 0.038 Uiso 1 1 calc R U . . .
C020 C 0.7059(4) 0.8107(4) 0.4874(5) 0.0334(19) Uani 1 1 d . . . . .
H0BA H 0.7332 0.8110 0.5385 0.040 Uiso 1 1 calc R U . . .
HN H 0.6839 0.8556 0.4860 0.040 Uiso 1 1 calc R U . . .
C021 C 0.2970(3) 0.9127(4) 0.2118(5) 0.0326(18) Uani 1 1 d . . . . .
H02Q H 0.2938 0.9288 0.1558 0.039 Uiso 1 1 calc R U . . .
H02R H 0.2884 0.9564 0.2414 0.039 Uiso 1 1 calc R U . . .
C022 C 0.3535(3) 0.8887(4) 0.2507(4) 0.0283(17) Uani 1 1 d . . . . .
H02S H 0.3551 0.8612 0.3012 0.034 Uiso 1 1 calc R U . . .
H02T H 0.3752 0.9343 0.2643 0.034 Uiso 1 1 calc R U . . .
C023 C 0.0915(3) 0.7504(5) -0.1957(5) 0.0333(18) Uani 1 1 d . . . . .
H02A H 0.0713 0.7809 -0.2411 0.040 Uiso 1 1 calc R U . . .
H02B H 0.0953 0.7797 -0.1458 0.040 Uiso 1 1 calc R U . . .
C024 C 0.7976(3) 0.7705(4) 0.3518(5) 0.0301(17) Uani 1 1 d . . . . .
H024 H 0.8288 0.7449 0.3537 0.036 Uiso 1 1 calc R U . . .
C025 C 0.1366(4) 0.7025(4) 0.0533(5) 0.037(2) Uani 1 1 d . . . . .
H02C H 0.1324 0.7367 0.0076 0.055 Uiso 1 1 calc R U . . .
H02D H 0.1544 0.6568 0.0435 0.055 Uiso 1 1 calc R U . . .
H02E H 0.1570 0.7273 0.1020 0.055 Uiso 1 1 calc R U . . .
C026 C -0.0872(4) 0.5254(4) -0.1470(6) 0.038(2) Uani 1 1 d . . . . .
H02F H -0.0905 0.4993 -0.1988 0.046 Uiso 1 1 calc R U . . .
H02G H -0.0609 0.4983 -0.1054 0.046 Uiso 1 1 calc R U . . .
C027 C 0.5467(4) 0.5958(4) 0.1638(5) 0.036(2) Uani 1 1 d . . . . .
H02U H 0.5542 0.5689 0.1185 0.054 Uiso 1 1 calc R U . . .
H02V H 0.5456 0.5598 0.2063 0.054 Uiso 1 1 calc R U . . .
H02W H 0.5738 0.6331 0.1845 0.054 Uiso 1 1 calc R U . . .
C028 C 0.5334(4) 0.9095(5) 0.4268(5) 0.038(2) Uani 1 1 d . . . . .
H02X H 0.5114 0.9541 0.4224 0.057 Uiso 1 1 calc R U . . .
H02Y H 0.5670 0.9200 0.4639 0.057 Uiso 1 1 calc R U . . .
HO H 0.5172 0.8671 0.4470 0.057 Uiso 1 1 calc R U . . .
C029 C 0.7047(3) 0.8490(4) 0.3445(5) 0.0332(18) Uani 1 1 d . . . . .
H029 H 0.6735 0.8751 0.3415 0.040 Uiso 1 1 calc R U . . .
C02A C 0.1768(4) 0.8067(5) -0.2147(5) 0.042(2) Uani 1 1 d . . . . .
H02H H 0.1575 0.8374 -0.2597 0.063 Uiso 1 1 calc R U . . .
H02I H 0.2100 0.7927 -0.2237 0.063 Uiso 1 1 calc R U . . .
H02J H 0.1825 0.8357 -0.1649 0.063 Uiso 1 1 calc R U . . .
C02B C -0.0370(4) 0.7355(5) -0.3070(5) 0.044(2) Uani 1 1 d . . . . .
C02C C 0.2577(4) 0.8482(5) 0.2118(6) 0.043(2) Uani 1 1 d . . . . .
H02Z H 0.2655 0.8051 0.1815 0.065 Uiso 1 1 calc R U . . .
HP H 0.2228 0.8661 0.1867 0.065 Uiso 1 1 calc R U . . .
HQ H 0.2601 0.8327 0.2671 0.065 Uiso 1 1 calc R U . . .
C02D C 0.2739(4) 0.5690(5) 0.2053(5) 0.040(2) Uani 1 1 d . . . . .
H02 H 0.2490 0.5986 0.1652 0.060 Uiso 1 1 calc R U . . .
HR H 0.2556 0.5397 0.2373 0.060 Uiso 1 1 calc R U . . .
HS H 0.2924 0.5348 0.1781 0.060 Uiso 1 1 calc R U . . .
C02E C 0.3032(4) 1.1214(5) 0.2632(6) 0.050(3) Uani 1 1 d . . . . .
C02F C -0.1391(4) 0.5218(5) -0.1254(7) 0.050(2) Uani 1 1 d . . . . .
H02K H -0.1664 0.5401 -0.1707 0.074 Uiso 1 1 calc R U . . .
H02L H -0.1375 0.5533 -0.0782 0.074 Uiso 1 1 calc R U . . .
H02M H -0.1463 0.4696 -0.1135 0.074 Uiso 1 1 calc R U . . .
C02G C 0.3113(5) 1.1268(6) 0.1825(6) 0.061(3) Uani 1 1 d . . . . .
H8BA H 0.3361 1.0883 0.1763 0.091 Uiso 1 1 calc R U . . .
HT H 0.3247 1.1768 0.1750 0.091 Uiso 1 1 calc R U . . .
HU H 0.2785 1.1187 0.1423 0.091 Uiso 1 1 calc R U . . .
N02H N 0.2965(5) 1.1155(5) 0.3257(7) 0.090(4) Uani 1 1 d . . . . .
C0 C -0.0714(9) 0.7971(12) -0.3639(14) 0.044(5) Uiso 0.49(2) 1 d . . P A 1
H0A H -0.0814 0.7780 -0.4197 0.052 Uiso 0.49(2) 1 calc R U P A 1
H0B H -0.1033 0.8058 -0.3468 0.052 Uiso 0.49(2) 1 calc R U P A 1
C02L C -0.0803(8) 0.8156(11) -0.4278(9) 0.044(6) Uani 0.51(2) 1 d . . P A 2
H02N H -0.0543 0.7949 -0.4523 0.065 Uiso 0.51(2) 1 calc R U P A 2
H02O H -0.0893 0.8668 -0.4479 0.065 Uiso 0.51(2) 1 calc R U P A 2
H02P H -0.1112 0.7839 -0.4417 0.065 Uiso 0.51(2) 1 calc R U P A 2
C0AA C -0.0438(9) 0.8686(13) -0.3615(13) 0.060(7) Uani 0.49(2) 1 d . . P A 1
H0AA H -0.0622 0.9007 -0.4059 0.090 Uiso 0.49(2) 1 calc R U P A 1
H0AB H -0.0089 0.8588 -0.3665 0.090 Uiso 0.49(2) 1 calc R U P A 1
H0AC H -0.0418 0.8941 -0.3105 0.090 Uiso 0.49(2) 1 calc R U P A 1
C2AA C -0.0589(8) 0.8177(10) -0.3367(12) 0.031(5) Uiso 0.51(2) 1 d . . P A 2
H2AA H -0.0864 0.8319 -0.3110 0.037 Uiso 0.51(2) 1 calc R U P A 2
H2AB H -0.0310 0.8555 -0.3217 0.037 Uiso 0.51(2) 1 calc R U P A 2
C1 C 0.1518(7) 0.4936(10) -0.1499(10) 0.038(4) Uiso 0.5 1 d . . P . .
C1AA C 0.1536(7) 0.4682(10) -0.2259(11) 0.042(4) Uiso 0.5 1 d . . P . .
H1AB H 0.1642 0.5096 -0.2556 0.062 Uiso 0.5 1 calc R U P . .
H1AC H 0.1194 0.4503 -0.2554 0.062 Uiso 0.5 1 calc R U P . .
H1AD H 0.1784 0.4268 -0.2200 0.062 Uiso 0.5 1 calc R U P . .
N2 N 0.1506(8) 0.5285(11) -0.0863(12) 0.068(5) Uiso 0.5 1 d . . P . .


_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
I001 C01T 2.113(8) . ?
I002 C01L 2.103(8) . ?
V003 O00K 1.614(4) . ?
V003 O00E 1.742(4) . ?
V003 O00D 1.908(4) . ?
V003 O00B 1.958(4) . ?
V003 O00C 2.064(5) . ?
V003 O00A 2.2270(10) . ?
V003 V005 3.0265(15) . ?
V003 V004 3.0333(15) . ?
V004 O00J 1.600(5) . ?
V004 O00H 1.741(5) . ?
V004 O00E 1.908(4) . ?
V004 O00C 1.964(4) 3_666 ?
V004 O009 2.086(4) 3_666 ?
V004 O00A 2.2507(11) . ?
V004 V005 3.0361(17) 3_666 ?
V005 O00L 1.616(5) . ?
V005 O00D 1.748(4) . ?
V005 O00H 1.924(5) 3_666 ?
V005 O009 1.971(4) 3_666 ?
V005 O00B 2.074(4) 3_666 ?
V005 O00A 2.2428(11) . ?
V005 V004 3.0360(17) 3_666 ?
V006 O00S 1.600(5) . ?
V006 O00O 1.757(5) . ?
V006 O00M 1.903(5) . ?
V006 O00I 1.976(5) . ?
V006 O00N 2.068(5) . ?
V006 O00G 2.2311(12) . ?
V006 V007 3.0188(17) 3_575 ?
V006 V008 3.0301(19) . ?
V007 O00T 1.610(5) . ?
V007 O00P 1.758(5) . ?
V007 O00O 1.898(5) 3_575 ?
V007 O00N 1.962(5) . ?
V007 O00F 2.069(5) . ?
V007 O00G 2.2392(11) . ?
V007 V006 3.0188(17) 3_575 ?
V007 V008 3.0286(17) . ?
V008 O00R 1.602(5) . ?
V008 O00M 1.753(5) . ?
V008 O00P 1.894(5) . ?
V008 O00F 1.982(5) 3_575 ?
V008 O00I 2.068(5) 3_575 ?
V008 O00G 2.2442(12) . ?
O009 C017 1.429(8) . ?
O009 V005 1.971(4) 3_666 ?
O009 V004 2.086(4) 3_666 ?
O00A V003 2.2270(10) 3_666 ?
O00A V005 2.2428(11) 3_666 ?
O00A V004 2.2507(11) 3_666 ?
O00B C011 1.442(8) . ?
O00B V005 2.074(4) 3_666 ?
O00C C01G 1.439(8) . ?
O00C V004 1.964(4) 3_666 ?
O00F C01F 1.432(9) . ?
O00F V008 1.982(5) 3_575 ?
O00G V006 2.2312(12) 3_575 ?
O00G V007 2.2392(11) 3_575 ?
O00G V008 2.2442(12) 3_575 ?
O00H V005 1.924(5) 3_666 ?
O00I C01J 1.420(9) . ?
O00I V008 2.068(5) 3_575 ?
O00N C018 1.420(8) . ?
O00O V007 1.898(5) 3_575 ?
O00Q C019 1.419(8) . ?
O00Q C01P 1.428(8) . ?
O00U C01H 1.426(8) . ?
O00U C020 1.438(8) . ?
N00V C013 1.513(9) . ?
N00V C00X 1.522(9) . ?
N00V C015 1.522(8) . ?
N00V C014 1.526(8) . ?
N00W C01U 1.511(9) . ?
N00W C01I 1.525(8) . ?
N00W C01M 1.528(10) . ?
N00W C01V 1.531(10) . ?
C00X C022 1.537(10) . ?
C00X H00A 0.9700 . ?
C00X H00B 0.9700 . ?
C00Y C00Z 1.390(10) . ?
C00Y C01W 1.391(10) . ?
C00Y C019 1.516(9) . ?
C00Z C010 1.379(11) . ?
C00Z H00Z 0.9300 . ?
C010 C01L 1.382(11) . ?
C010 H010 0.9300 . ?
C011 C012 1.527(9) . ?
C011 H4AA 0.9700 . ?
C011 H 0.9700 . ?
C012 C01H 1.525(9) . ?
C012 C01G 1.535(9) . ?
C012 C017 1.554(9) . ?
C013 C01E 1.526(9) . ?
C013 H01Q 0.9700 . ?
C013 H01R 0.9700 . ?
C014 C016 1.510(10) . ?
C014 H01S 0.9700 . ?
C014 H01T 0.9700 . ?
C015 C01D 1.528(10) . ?
C015 H01U 0.9700 . ?
C015 H01V 0.9700 . ?
C016 C01K 1.534(10) . ?
C016 H01W 0.9700 . ?
C016 H01X 0.9700 . ?
C017 H5AA 0.9700 . ?
C017 HA 0.9700 . ?
C018 C01C 1.532(9) . ?
C018 H1BA 0.9700 . ?
C018 HB 0.9700 . ?
C019 H2BA 0.9700 . ?
C019 HC 0.9700 . ?
C01A C02D 1.519(11) . ?
C01A C01D 1.537(10) . ?
C01A H01Y 0.9700 . ?
C01A HD 0.9700 . ?
C01B C029 1.386(11) . ?
C01B C01Z 1.410(11) . ?
C01B C020 1.493(10) . ?
C01C C01J 1.529(10) . ?
C01C C01F 1.526(10) . ?
C01C C01P 1.528(10) . ?
C01D H01Z 0.9700 . ?
C01D HE 0.9700 . ?
C01E C01Q 1.538(11) . ?
C01E H01 0.9700 . ?
C01E HF 0.9700 . ?
C01F H3BA 0.9700 . ?
C01F HG 0.9700 . ?
C01G H6AA 0.9700 . ?
C01G HH 0.9700 . ?
C01H H7AA 0.9700 . ?
C01H HI 0.9700 . ?
C01I C01S 1.526(10) . ?
C01I H01A 0.9700 . ?
C01I H01B 0.9700 . ?
C01J H4BA 0.9700 . ?
C01J HJ 0.9700 . ?
C01K C027 1.524(11) . ?
C01K H1AA 0.9700 . ?
C01K HK 0.9700 . ?
C01L C01O 1.377(11) . ?
C01M C023 1.520(10) . ?
C01M H01C 0.9700 . ?
C01M H01D 0.9700 . ?
C01N C023 1.514(11) . ?
C01N C02A 1.537(11) . ?
C01N H01E 0.9700 . ?
C01N H01F 0.9700 . ?
C01O C01W 1.407(10) . ?
C01O H5BA 0.9300 . ?
C01P H6BA 0.9700 . ?
C01P HL 0.9700 . ?
C01Q C028 1.500(11) . ?
C01Q H3AA 0.9700 . ?
C01Q HM 0.9700 . ?
C01R C025 1.527(11) . ?
C01R C01Y 1.536(11) . ?
C01R H01G 0.9700 . ?
C01R H01H 0.9700 . ?
C01S C026 1.512(10) . ?
C01S H01I 0.9700 . ?
C01S H01J 0.9700 . ?
C01T C01X 1.371(12) . ?
C01T C024 1.376(12) . ?
C01U C01Y 1.534(11) . ?
C01U H01K 0.9700 . ?
C01U H01L 0.9700 . ?
C01V C02B 1.522(11) . ?
C01V H01M 0.9700 . ?
C01V H01N 0.9700 . ?
C01W H7BA 0.9300 . ?
C01X C029 1.370(11) . ?
C01X H8AA 0.9300 . ?
C01Y H01O 0.9700 . ?
C01Y H01P 0.9700 . ?
C01Z C024 1.390(10) . ?
C01Z H9AA 0.9300 . ?
C020 H0BA 0.9700 . ?
C020 HN 0.9700 . ?
C021 C022 1.521(11) . ?
C021 C02C 1.527(11) . ?
C021 H02Q 0.9700 . ?
C021 H02R 0.9700 . ?
C022 H02S 0.9700 . ?
C022 H02T 0.9700 . ?
C023 H02A 0.9700 . ?
C023 H02B 0.9700 . ?
C024 H024 0.9300 . ?
C025 H02C 0.9600 . ?
C025 H02D 0.9600 . ?
C025 H02E 0.9600 . ?
C026 C02F 1.506(12) . ?
C026 H02F 0.9700 . ?
C026 H02G 0.9700 . ?
C027 H02U 0.9600 . ?
C027 H02V 0.9600 . ?
C027 H02W 0.9600 . ?
C028 H02X 0.9600 . ?
C028 H02Y 0.9600 . ?
C028 HO 0.9600 . ?
C029 H029 0.9300 . ?
C02A H02H 0.9600 . ?
C02A H02I 0.9600 . ?
C02A H02J 0.9600 . ?
C02B C0 1.56(2) . ?
C02B C2AA 1.576(19) . ?
C02C H02Z 0.9600 . ?
C02C HP 0.9600 . ?
C02C HQ 0.9600 . ?
C02D H02 0.9600 . ?
C02D HR 0.9600 . ?
C02D HS 0.9600 . ?
C02E N02H 1.122(13) . ?
C02E C02G 1.439(13) . ?
C02F H02K 0.9600 . ?
C02F H02L 0.9600 . ?
C02F H02M 0.9600 . ?
C02G H8BA 0.9600 . ?
C02G HT 0.9600 . ?
C02G HU 0.9600 . ?
C0 C0AA 1.44(3) . ?
C0 H0A 0.9700 . ?
C0 H0B 0.9700 . ?
C02L C2AA 1.50(2) . ?
C02L H02N 0.9600 . ?
C02L H02O 0.9600 . ?
C02L H02P 0.9600 . ?
C0AA H0AA 0.9600 . ?
C0AA H0AB 0.9600 . ?
C0AA H0AC 0.9600 . ?
C2AA H2AA 0.9700 . ?
C2AA H2AB 0.9700 . ?
C1 N2 1.24(2) . ?
C1 C1AA 1.37(2) . ?
C1AA H1AB 0.9600 . ?
C1AA H1AC 0.9600 . ?
C1AA H1AD 0.9600 . ?

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
O00K V003 O00E 104.7(2) . . ?
O00K V003 O00D 102.5(2) . . ?
O00E V003 O00D 93.3(2) . . ?
O00K V003 O00B 97.1(2) . . ?
O00E V003 O00B 93.5(2) . . ?
O00D V003 O00B 156.81(19) . . ?
O00K V003 O00C 95.5(2) . . ?
O00E V003 O00C 159.80(19) . . ?
O00D V003 O00C 82.74(19) . . ?
O00B V003 O00C 83.21(18) . . ?
O00K V003 O00A 171.69(19) . . ?
O00E V003 O00A 82.97(14) . . ?
O00D V003 O00A 79.83(13) . . ?
O00B V003 O00A 79.07(12) . . ?
O00C V003 O00A 76.83(12) . . ?
O00K V003 V005 134.96(17) . . ?
O00E V003 V005 85.40(14) . . ?
O00D V003 V005 32.46(13) . . ?
O00B V003 V005 126.46(13) . . ?
O00C V003 V005 80.67(12) . . ?
O00A V003 V005 47.60(3) . . ?
O00K V003 V004 139.57(18) . . ?
O00E V003 V004 35.59(14) . . ?
O00D V003 V004 90.36(14) . . ?
O00B V003 V004 82.49(13) . . ?
O00C V003 V004 124.35(12) . . ?
O00A V003 V004 47.69(3) . . ?
V005 V003 V004 66.28(4) . . ?
O00J V004 O00H 105.3(2) . . ?
O00J V004 O00E 103.3(2) . . ?
O00H V004 O00E 93.1(2) . . ?
O00J V004 O00C 97.9(2) . 3_666 ?
O00H V004 O00C 93.7(2) . 3_666 ?
O00E V004 O00C 155.13(18) . 3_666 ?
O00J V004 O009 95.3(2) . 3_666 ?
O00H V004 O009 159.4(2) . 3_666 ?
O00E V004 O009 82.61(17) . 3_666 ?
O00C V004 O009 82.64(17) 3_666 3_666 ?
O00J V004 O00A 171.10(18) . . ?
O00H V004 O00A 83.13(15) . . ?
O00E V004 O00A 78.84(14) . . ?
O00C V004 O00A 78.28(13) 3_666 . ?
O009 V004 O00A 76.28(13) 3_666 . ?
O00J V004 V003 135.33(16) . . ?
O00H V004 V003 85.11(15) . . ?
O00E V004 V003 32.09(14) . . ?
O00C V004 V003 125.12(13) 3_666 . ?
O009 V004 V003 80.60(12) 3_666 . ?
O00A V004 V003 47.03(3) . . ?
O00J V004 V005 140.57(18) . 3_666 ?
O00H V004 V005 36.07(15) . 3_666 ?
O00E V004 V005 89.71(15) . 3_666 ?
O00C V004 V005 81.91(14) 3_666 3_666 ?
O009 V004 V005 123.48(13) 3_666 3_666 ?
O00A V004 V005 47.38(3) . 3_666 ?
V003 V004 V005 65.63(4) . 3_666 ?
O00L V005 O00D 104.1(2) . . ?
O00L V005 O00H 102.5(2) . 3_666 ?
O00D V005 O00H 93.9(2) . 3_666 ?
O00L V005 O009 97.8(2) . 3_666 ?
O00D V005 O009 93.46(19) . 3_666 ?
O00H V005 O009 155.95(19) 3_666 3_666 ?
O00L V005 O00B 96.8(2) . 3_666 ?
O00D V005 O00B 159.12(19) . 3_666 ?
O00H V005 O00B 82.50(18) 3_666 3_666 ?
O009 V005 O00B 82.51(17) 3_666 3_666 ?
O00L V005 O00A 172.63(17) . . ?
O00D V005 O00A 82.76(15) . . ?
O00H V005 O00A 79.50(14) 3_666 . ?
O009 V005 O00A 78.75(13) 3_666 . ?
O00B V005 O00A 76.36(12) 3_666 . ?
O00L V005 V003 139.30(17) . . ?
O00D V005 V003 35.86(14) . . ?
O00H V005 V003 90.21(14) 3_666 . ?
O009 V005 V003 82.49(13) 3_666 . ?
O00B V005 V003 123.34(12) 3_666 . ?
O00A V005 V003 47.16(3) . . ?
O00L V005 V004 134.74(18) . 3_666 ?
O00D V005 V004 85.35(16) . 3_666 ?
O00H V005 V004 32.19(13) 3_666 3_666 ?
O009 V005 V004 126.14(14) 3_666 3_666 ?
O00B V005 V004 80.68(13) 3_666 3_666 ?
O00A V005 V004 47.61(3) . 3_666 ?
V003 V005 V004 65.82(4) . 3_666 ?
O00S V006 O00O 104.5(2) . . ?
O00S V006 O00M 103.3(2) . . ?
O00O V006 O00M 93.7(2) . . ?
O00S V006 O00I 96.5(2) . . ?
O00O V006 O00I 92.5(2) . . ?
O00M V006 O00I 157.0(2) . . ?
O00S V006 O00N 95.6(2) . . ?
O00O V006 O00N 159.7(2) . . ?
O00M V006 O00N 83.97(19) . . ?
O00I V006 O00N 82.56(19) . . ?
O00S V006 O00G 171.15(18) . . ?
O00O V006 O00G 83.34(16) . . ?
O00M V006 O00G 79.90(15) . . ?
O00I V006 O00G 78.88(15) . . ?
O00N V006 O00G 76.38(14) . . ?
O00S V006 V007 139.80(19) . 3_575 ?
O00O V006 V007 35.85(16) . 3_575 ?
O00M V006 V007 89.54(15) . 3_575 ?
O00I V006 V007 82.65(15) . 3_575 ?
O00N V006 V007 123.83(14) . 3_575 ?
O00G V006 V007 47.64(3) . 3_575 ?
O00S V006 V008 135.6(2) . . ?
O00O V006 V008 86.82(18) . . ?
O00M V006 V008 32.45(14) . . ?
O00I V006 V008 126.19(15) . . ?
O00N V006 V008 80.43(15) . . ?
O00G V006 V008 47.57(3) . . ?
V007 V006 V008 66.26(4) 3_575 . ?
O00T V007 O00P 104.6(3) . . ?
O00T V007 O00O 103.4(2) . 3_575 ?
O00P V007 O00O 93.4(2) . 3_575 ?
O00T V007 O00N 96.8(2) . . ?
O00P V007 O00N 92.3(2) . . ?
O00O V007 O00N 156.8(2) 3_575 . ?
O00T V007 O00F 95.7(2) . . ?
O00P V007 O00F 159.5(2) . . ?
O00O V007 O00F 84.5(2) 3_575 . ?
O00N V007 O00F 82.4(2) . . ?
O00T V007 O00G 171.4(2) . . ?
O00P V007 O00G 82.83(16) . . ?
O00O V007 O00G 80.11(14) 3_575 . ?
O00N V007 O00G 78.30(13) . . ?
O00F V007 O00G 76.72(13) . . ?
O00T V007 V006 136.2(2) . 3_575 ?
O00P V007 V006 86.08(17) . 3_575 ?
O00O V007 V006 32.84(14) 3_575 3_575 ?
O00N V007 V006 125.51(14) . 3_575 ?
O00F V007 V006 81.08(13) . 3_575 ?
O00G V007 V006 47.41(3) . 3_575 ?
O00T V007 V008 139.4(2) . . ?
O00P V007 V008 35.43(16) . . ?
O00O V007 V008 89.67(15) 3_575 . ?
O00N V007 V008 82.04(14) . . ?
O00F V007 V008 124.08(13) . . ?
O00G V007 V008 47.58(3) . . ?
V006 V007 V008 66.00(4) 3_575 . ?
O00R V008 O00M 105.4(3) . . ?
O00R V008 O00P 102.0(3) . . ?
O00M V008 O00P 94.3(2) . . ?
O00R V008 O00F 98.3(2) . 3_575 ?
O00M V008 O00F 91.9(2) . 3_575 ?
O00P V008 O00F 156.3(2) . 3_575 ?
O00R V008 O00I 95.1(2) . 3_575 ?
O00M V008 O00I 159.3(2) . 3_575 ?
O00P V008 O00I 84.0(2) . 3_575 ?
O00F V008 O00I 82.16(19) 3_575 3_575 ?
O00R V008 O00G 171.4(2) . . ?
O00M V008 O00G 82.70(16) . . ?
O00P V008 O00G 79.84(16) . . ?
O00F V008 O00G 78.33(14) 3_575 . ?
O00I V008 O00G 76.73(14) 3_575 . ?
O00R V008 V007 134.5(2) . . ?
O00M V008 V007 86.55(15) . . ?
O00P V008 V007 32.57(16) . . ?
O00F V008 V007 125.53(14) 3_575 . ?
O00I V008 V007 81.01(14) 3_575 . ?
O00G V008 V007 47.44(3) . . ?
O00R V008 V006 140.6(2) . . ?
O00M V008 V006 35.63(15) . . ?
O00P V008 V006 89.78(17) . . ?
O00F V008 V006 82.09(15) 3_575 . ?
O00I V008 V006 123.71(14) 3_575 . ?
O00G V008 V006 47.20(3) . . ?
V007 V008 V006 65.94(4) . . ?
C017 O009 V005 119.8(4) . 3_666 ?
C017 O009 V004 117.8(4) . 3_666 ?
V005 O009 V004 109.4(2) 3_666 3_666 ?
V003 O00A V003 179.998(13) . 3_666 ?
V003 O00A V005 85.24(4) . . ?
V003 O00A V005 94.76(4) 3_666 . ?
V003 O00A V005 94.76(4) . 3_666 ?
V003 O00A V005 85.24(4) 3_666 3_666 ?
V005 O00A V005 180.0 . 3_666 ?
V003 O00A V004 85.29(4) . . ?
V003 O00A V004 94.71(4) 3_666 . ?
V005 O00A V004 94.99(4) . . ?
V005 O00A V004 85.01(4) 3_666 . ?
V003 O00A V004 94.71(4) . 3_666 ?
V003 O00A V004 85.29(4) 3_666 3_666 ?
V005 O00A V004 85.01(4) . 3_666 ?
V005 O00A V004 94.99(4) 3_666 3_666 ?
V004 O00A V004 180.0 . 3_666 ?
C011 O00B V003 119.6(3) . . ?
C011 O00B V005 117.8(4) . 3_666 ?
V003 O00B V005 109.30(19) . 3_666 ?
C01G O00C V004 118.9(4) . 3_666 ?
C01G O00C V003 118.2(3) . . ?
V004 O00C V003 109.7(2) 3_666 . ?
V005 O00D V003 111.7(2) . . ?
V003 O00E V004 112.3(2) . . ?
C01F O00F V008 119.1(4) . 3_575 ?
C01F O00F V007 118.4(4) . . ?
V008 O00F V007 109.4(2) 3_575 . ?
V006 O00G V006 180.00(6) . 3_575 ?
V006 O00G V007 95.05(4) . . ?
V006 O00G V007 84.95(4) 3_575 . ?
V006 O00G V007 84.95(4) . 3_575 ?
V006 O00G V007 95.05(4) 3_575 3_575 ?
V007 O00G V007 180.0 . 3_575 ?
V006 O00G V008 94.77(5) . 3_575 ?
V006 O00G V008 85.23(5) 3_575 3_575 ?
V007 O00G V008 95.01(4) . 3_575 ?
V007 O00G V008 84.99(4) 3_575 3_575 ?
V006 O00G V008 85.23(5) . . ?
V006 O00G V008 94.77(5) 3_575 . ?
V007 O00G V008 84.99(4) . . ?
V007 O00G V008 95.01(4) 3_575 . ?
V008 O00G V008 180.0 3_575 . ?
V004 O00H V005 111.7(2) . 3_666 ?
C01J O00I V006 119.8(4) . . ?
C01J O00I V008 118.4(4) . 3_575 ?
V006 O00I V008 109.0(2) . 3_575 ?
V008 O00M V006 111.9(2) . . ?
C018 O00N V007 119.4(4) . . ?
C018 O00N V006 117.2(4) . . ?
V007 O00N V006 109.8(2) . . ?
V006 O00O V007 111.3(2) . 3_575 ?
V007 O00P V008 112.0(3) . . ?
C019 O00Q C01P 113.8(5) . . ?
C01H O00U C020 110.4(5) . . ?
C013 N00V C00X 111.4(5) . . ?
C013 N00V C015 107.0(5) . . ?
C00X N00V C015 110.0(6) . . ?
C013 N00V C014 110.0(5) . . ?
C00X N00V C014 108.0(5) . . ?
C015 N00V C014 110.5(5) . . ?
C01U N00W C01I 111.1(5) . . ?
C01U N00W C01M 110.1(6) . . ?
C01I N00W C01M 107.3(5) . . ?
C01U N00W C01V 106.9(6) . . ?
C01I N00W C01V 110.2(6) . . ?
C01M N00W C01V 111.2(5) . . ?
N00V C00X C022 115.4(6) . . ?
N00V C00X H00A 108.4 . . ?
C022 C00X H00A 108.4 . . ?
N00V C00X H00B 108.4 . . ?
C022 C00X H00B 108.4 . . ?
H00A C00X H00B 107.5 . . ?
C00Z C00Y C01W 119.3(7) . . ?
C00Z C00Y C019 118.6(6) . . ?
C01W C00Y C019 122.0(7) . . ?
C010 C00Z C00Y 120.9(7) . . ?
C010 C00Z H00Z 119.5 . . ?
C00Y C00Z H00Z 119.5 . . ?
C01L C010 C00Z 119.3(7) . . ?
C01L C010 H010 120.3 . . ?
C00Z C010 H010 120.3 . . ?
O00B C011 C012 112.1(5) . . ?
O00B C011 H4AA 109.2 . . ?
C012 C011 H4AA 109.2 . . ?
O00B C011 H 109.2 . . ?
C012 C011 H 109.2 . . ?
H4AA C011 H 107.9 . . ?
C01H C012 C011 109.7(5) . . ?
C01H C012 C01G 105.2(5) . . ?
C011 C012 C01G 111.4(6) . . ?
C01H C012 C017 110.7(6) . . ?
C011 C012 C017 109.8(5) . . ?
C01G C012 C017 109.9(5) . . ?
N00V C013 C01E 115.2(5) . . ?
N00V C013 H01Q 108.5 . . ?
C01E C013 H01Q 108.5 . . ?
N00V C013 H01R 108.5 . . ?
C01E C013 H01R 108.5 . . ?
H01Q C013 H01R 107.5 . . ?
C016 C014 N00V 115.4(5) . . ?
C016 C014 H01S 108.4 . . ?
N00V C014 H01S 108.4 . . ?
C016 C014 H01T 108.4 . . ?
N00V C014 H01T 108.4 . . ?
H01S C014 H01T 107.5 . . ?
N00V C015 C01D 115.9(5) . . ?
N00V C015 H01U 108.3 . . ?
C01D C015 H01U 108.3 . . ?
N00V C015 H01V 108.3 . . ?
C01D C015 H01V 108.3 . . ?
H01U C015 H01V 107.4 . . ?
C014 C016 C01K 110.3(6) . . ?
C014 C016 H01W 109.6 . . ?
C01K C016 H01W 109.6 . . ?
C014 C016 H01X 109.6 . . ?
C01K C016 H01X 109.6 . . ?
H01W C016 H01X 108.1 . . ?
O009 C017 C012 111.6(5) . . ?
O009 C017 H5AA 109.3 . . ?
C012 C017 H5AA 109.3 . . ?
O009 C017 HA 109.3 . . ?
C012 C017 HA 109.3 . . ?
H5AA C017 HA 108.0 . . ?
O00N C018 C01C 113.6(5) . . ?
O00N C018 H1BA 108.8 . . ?
C01C C018 H1BA 108.8 . . ?
O00N C018 HB 108.8 . . ?
C01C C018 HB 108.8 . . ?
H1BA C018 HB 107.7 . . ?
O00Q C019 C00Y 109.8(6) . . ?
O00Q C019 H2BA 109.7 . . ?
C00Y C019 H2BA 109.7 . . ?
O00Q C019 HC 109.7 . . ?
C00Y C019 HC 109.7 . . ?
H2BA C019 HC 108.2 . . ?
C02D C01A C01D 112.0(6) . . ?
C02D C01A H01Y 109.2 . . ?
C01D C01A H01Y 109.2 . . ?
C02D C01A HD 109.2 . . ?
C01D C01A HD 109.2 . . ?
H01Y C01A HD 107.9 . . ?
C029 C01B C01Z 118.2(7) . . ?
C029 C01B C020 120.5(8) . . ?
C01Z C01B C020 121.3(7) . . ?
C01J C01C C01F 110.5(6) . . ?
C01J C01C C01P 110.6(6) . . ?
C01F C01C C01P 107.3(6) . . ?
C01J C01C C018 110.0(6) . . ?
C01F C01C C018 109.5(6) . . ?
C01P C01C C018 108.9(6) . . ?
C015 C01D C01A 109.1(5) . . ?
C015 C01D H01Z 109.9 . . ?
C01A C01D H01Z 109.9 . . ?
C015 C01D HE 109.9 . . ?
C01A C01D HE 109.9 . . ?
H01Z C01D HE 108.3 . . ?
C013 C01E C01Q 111.4(6) . . ?
C013 C01E H01 109.4 . . ?
C01Q C01E H01 109.4 . . ?
C013 C01E HF 109.4 . . ?
C01Q C01E HF 109.4 . . ?
H01 C01E HF 108.0 . . ?
O00F C01F C01C 112.2(5) . . ?
O00F C01F H3BA 109.2 . . ?
C01C C01F H3BA 109.2 . . ?
O00F C01F HG 109.2 . . ?
C01C C01F HG 109.2 . . ?
H3BA C01F HG 107.9 . . ?
O00C C01G C012 112.0(5) . . ?
O00C C01G H6AA 109.2 . . ?
C012 C01G H6AA 109.2 . . ?
O00C C01G HH 109.2 . . ?
C012 C01G HH 109.2 . . ?
H6AA C01G HH 107.9 . . ?
O00U C01H C012 110.0(5) . . ?
O00U C01H H7AA 109.7 . . ?
C012 C01H H7AA 109.7 . . ?
O00U C01H HI 109.7 . . ?
C012 C01H HI 109.7 . . ?
H7AA C01H HI 108.2 . . ?
N00W C01I C01S 114.5(6) . . ?
N00W C01I H01A 108.6 . . ?
C01S C01I H01A 108.6 . . ?
N00W C01I H01B 108.6 . . ?
C01S C01I H01B 108.6 . . ?
H01A C01I H01B 107.6 . . ?
O00I C01J C01C 112.0(6) . . ?
O00I C01J H4BA 109.2 . . ?
C01C C01J H4BA 109.2 . . ?
O00I C01J HJ 109.2 . . ?
C01C C01J HJ 109.2 . . ?
H4BA C01J HJ 107.9 . . ?
C027 C01K C016 110.5(6) . . ?
C027 C01K H1AA 109.5 . . ?
C016 C01K H1AA 109.5 . . ?
C027 C01K HK 109.5 . . ?
C016 C01K HK 109.5 . . ?
H1AA C01K HK 108.1 . . ?
C01O C01L C010 121.3(7) . . ?
C01O C01L I002 119.4(6) . . ?
C010 C01L I002 119.2(6) . . ?
C023 C01M N00W 114.7(6) . . ?
C023 C01M H01C 108.6 . . ?
N00W C01M H01C 108.6 . . ?
C023 C01M H01D 108.6 . . ?
N00W C01M H01D 108.6 . . ?
H01C C01M H01D 107.6 . . ?
C023 C01N C02A 113.3(7) . . ?
C023 C01N H01E 108.9 . . ?
C02A C01N H01E 108.9 . . ?
C023 C01N H01F 108.9 . . ?
C02A C01N H01F 108.9 . . ?
H01E C01N H01F 107.7 . . ?
C01L C01O C01W 119.1(7) . . ?
C01L C01O H5BA 120.4 . . ?
C01W C01O H5BA 120.4 . . ?
O00Q C01P C01C 109.6(5) . . ?
O00Q C01P H6BA 109.7 . . ?
C01C C01P H6BA 109.7 . . ?
O00Q C01P HL 109.7 . . ?
C01C C01P HL 109.7 . . ?
H6BA C01P HL 108.2 . . ?
C028 C01Q C01E 114.2(7) . . ?
C028 C01Q H3AA 108.7 . . ?
C01E C01Q H3AA 108.7 . . ?
C028 C01Q HM 108.7 . . ?
C01E C01Q HM 108.7 . . ?
H3AA C01Q HM 107.6 . . ?
C025 C01R C01Y 111.6(6) . . ?
C025 C01R H01G 109.3 . . ?
C01Y C01R H01G 109.3 . . ?
C025 C01R H01H 109.3 . . ?
C01Y C01R H01H 109.3 . . ?
H01G C01R H01H 108.0 . . ?
C026 C01S C01I 111.3(6) . . ?
C026 C01S H01I 109.4 . . ?
C01I C01S H01I 109.4 . . ?
C026 C01S H01J 109.4 . . ?
C01I C01S H01J 109.4 . . ?
H01I C01S H01J 108.0 . . ?
C01X C01T C024 122.7(7) . . ?
C01X C01T I001 118.9(6) . . ?
C024 C01T I001 118.4(6) . . ?
N00W C01U C01Y 114.6(6) . . ?
N00W C01U H01K 108.6 . . ?
C01Y C01U H01K 108.6 . . ?
N00W C01U H01L 108.6 . . ?
C01Y C01U H01L 108.6 . . ?
H01K C01U H01L 107.6 . . ?
C02B C01V N00W 114.6(6) . . ?
C02B C01V H01M 108.6 . . ?
N00W C01V H01M 108.6 . . ?
C02B C01V H01N 108.6 . . ?
N00W C01V H01N 108.6 . . ?
H01M C01V H01N 107.6 . . ?
C00Y C01W C01O 119.9(7) . . ?
C00Y C01W H7BA 120.0 . . ?
C01O C01W H7BA 120.0 . . ?
C029 C01X C01T 118.9(8) . . ?
C029 C01X H8AA 120.6 . . ?
C01T C01X H8AA 120.6 . . ?
C01R C01Y C01U 110.6(6) . . ?
C01R C01Y H01O 109.5 . . ?
C01U C01Y H01O 109.5 . . ?
C01R C01Y H01P 109.5 . . ?
C01U C01Y H01P 109.5 . . ?
H01O C01Y H01P 108.1 . . ?
C024 C01Z C01B 120.9(7) . . ?
C024 C01Z H9AA 119.6 . . ?
C01B C01Z H9AA 119.6 . . ?
O00U C020 C01B 107.3(6) . . ?
O00U C020 H0BA 110.2 . . ?
C01B C020 H0BA 110.2 . . ?
O00U C020 HN 110.2 . . ?
C01B C020 HN 110.2 . . ?
H0BA C020 HN 108.5 . . ?
C022 C021 C02C 112.7(6) . . ?
C022 C021 H02Q 109.1 . . ?
C02C C021 H02Q 109.1 . . ?
C022 C021 H02R 109.1 . . ?
C02C C021 H02R 109.1 . . ?
H02Q C021 H02R 107.8 . . ?
C021 C022 C00X 112.1(6) . . ?
C021 C022 H02S 109.2 . . ?
C00X C022 H02S 109.2 . . ?
C021 C022 H02T 109.2 . . ?
C00X C022 H02T 109.2 . . ?
H02S C022 H02T 107.9 . . ?
C01N C023 C01M 110.4(7) . . ?
C01N C023 H02A 109.6 . . ?
C01M C023 H02A 109.6 . . ?
C01N C023 H02B 109.6 . . ?
C01M C023 H02B 109.6 . . ?
H02A C023 H02B 108.1 . . ?
C01T C024 C01Z 117.8(8) . . ?
C01T C024 H024 121.1 . . ?
C01Z C024 H024 121.1 . . ?
C01R C025 H02C 109.5 . . ?
C01R C025 H02D 109.5 . . ?
H02C C025 H02D 109.5 . . ?
C01R C025 H02E 109.5 . . ?
H02C C025 H02E 109.5 . . ?
H02D C025 H02E 109.5 . . ?
C02F C026 C01S 112.8(7) . . ?
C02F C026 H02F 109.0 . . ?
C01S C026 H02F 109.0 . . ?
C02F C026 H02G 109.0 . . ?
C01S C026 H02G 109.0 . . ?
H02F C026 H02G 107.8 . . ?
C01K C027 H02U 109.5 . . ?
C01K C027 H02V 109.5 . . ?
H02U C027 H02V 109.5 . . ?
C01K C027 H02W 109.5 . . ?
H02U C027 H02W 109.5 . . ?
H02V C027 H02W 109.5 . . ?
C01Q C028 H02X 109.5 . . ?
C01Q C028 H02Y 109.5 . . ?
H02X C028 H02Y 109.5 . . ?
C01Q C028 HO 109.5 . . ?
H02X C028 HO 109.5 . . ?
H02Y C028 HO 109.5 . . ?
C01X C029 C01B 121.5(8) . . ?
C01X C029 H029 119.3 . . ?
C01B C029 H029 119.3 . . ?
C01N C02A H02H 109.5 . . ?
C01N C02A H02I 109.5 . . ?
H02H C02A H02I 109.5 . . ?
C01N C02A H02J 109.5 . . ?
H02H C02A H02J 109.5 . . ?
H02I C02A H02J 109.5 . . ?
C01V C02B C0 118.6(11) . . ?
C01V C02B C2AA 99.6(9) . . ?
C021 C02C H02Z 109.5 . . ?
C021 C02C HP 109.5 . . ?
H02Z C02C HP 109.5 . . ?
C021 C02C HQ 109.5 . . ?
H02Z C02C HQ 109.5 . . ?
HP C02C HQ 109.5 . . ?
C01A C02D H02 109.5 . . ?
C01A C02D HR 109.5 . . ?
H02 C02D HR 109.5 . . ?
C01A C02D HS 109.5 . . ?
H02 C02D HS 109.5 . . ?
HR C02D HS 109.5 . . ?
N02H C02E C02G 178.3(12) . . ?
C026 C02F H02K 109.5 . . ?
C026 C02F H02L 109.5 . . ?
H02K C02F H02L 109.5 . . ?
C026 C02F H02M 109.5 . . ?
H02K C02F H02M 109.5 . . ?
H02L C02F H02M 109.5 . . ?
C02E C02G H8BA 109.5 . . ?
C02E C02G HT 109.5 . . ?
H8BA C02G HT 109.5 . . ?
C02E C02G HU 109.5 . . ?
H8BA C02G HU 109.5 . . ?
HT C02G HU 109.5 . . ?
C0AA C0 C02B 111.6(17) . . ?
C0AA C0 H0A 109.3 . . ?
C02B C0 H0A 109.3 . . ?
C0AA C0 H0B 109.3 . . ?
C02B C0 H0B 109.3 . . ?
H0A C0 H0B 108.0 . . ?
C2AA C02L H02N 109.5 . . ?
C2AA C02L H02O 109.5 . . ?
H02N C02L H02O 109.5 . . ?
C2AA C02L H02P 109.5 . . ?
H02N C02L H02P 109.5 . . ?
H02O C02L H02P 109.5 . . ?
C0 C0AA H0AA 109.5 . . ?
C0 C0AA H0AB 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
C0 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
C02L C2AA C02B 108.3(14) . . ?
C02L C2AA H2AA 110.0 . . ?
C02B C2AA H2AA 110.0 . . ?
C02L C2AA H2AB 110.0 . . ?
C02B C2AA H2AB 110.0 . . ?
H2AA C2AA H2AB 108.4 . . ?
N2 C1 C1AA 169.6(19) . . ?
C1 C1AA H1AB 109.5 . . ?
C1 C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
C1 C1AA H1AD 109.5 . . ?
H1AB C1AA H1AD 109.5 . . ?
H1AC C1AA H1AD 109.5 . . ?

_refine_diff_density_max         2.444
_refine_diff_density_min         -2.475
_refine_diff_density_rms         0.169

####################################################################### 
# 
# 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_pd2i6
_database_code_depnum_ccdc_archive 'CCDC 1581483'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2018-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        (TBA)2[Pd2I6]
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C16 H36 N), 2(Pd2 I6)'
_chemical_formula_sum            'C64 H144 I12 N4 Pd4'
_chemical_formula_weight         2918.22

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'
I I -0.4742 1.8119 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   14.5016(6)
_cell_length_b                   13.7745(5)
_cell_length_c                   23.8492(9)
_cell_angle_alpha                90
_cell_angle_beta                 101.7210(10)
_cell_angle_gamma                90
_cell_volume                     4664.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9837
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      30.64

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_F_000             2752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    4.764
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4934
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1052 before and 0.0420 after correction. The Ratio of minimum to maximum transmission is 0.6613. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69700
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.744
_diffrn_reflns_theta_max         31.006
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13810
_reflns_number_gt                12091
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0310P)²+12.5850P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13810
_refine_ls_number_parameters     387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0657
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
IRR I 0.30156(2) 0.24582(2) 0.94564(2) 0.01942(4) Uani 1 1 d . . . . .
I1 I 0.53789(2) 0.26122(2) 0.91085(2) 0.01998(4) Uani 1 1 d . . . . .
I2 I 0.07233(2) 0.21780(2) 0.98949(2) 0.02159(5) Uani 1 1 d . . . . .
I3 I 0.41917(2) 0.36637(2) 0.76625(2) 0.02162(5) Uani 1 1 d . . . . .
I4 I -0.03912(2) 0.33564(2) 0.84604(2) 0.02401(5) Uani 1 1 d . . . . .
I5 I 0.19485(2) 0.35069(2) 0.81384(2) 0.02567(5) Uani 1 1 d . . . . .
Pd00 Pd 0.12782(2) 0.28664(2) 0.89993(2) 0.01588(5) Uani 1 1 d . . . . .
Pd1 Pd 0.36802(2) 0.30667(2) 0.85844(2) 0.01495(5) Uani 1 1 d . . . . .
N009 N 0.70166(17) 0.56440(17) 0.86383(10) 0.0146(4) Uani 1 1 d . . . . .
N00A N 1.22488(17) 0.55178(17) 0.61596(10) 0.0147(4) Uani 1 1 d . . . . .
C00B C 1.4186(2) 0.3714(2) 0.58926(12) 0.0156(5) Uani 1 1 d . . . . .
H00Z H 1.4519 0.3703 0.6289 0.019 Uiso 1 1 calc R U . . .
H H 1.4159 0.3053 0.5750 0.019 Uiso 1 1 calc R U . . .
C00C C 0.6266(2) 0.6138(2) 0.89030(12) 0.0167(5) Uani 1 1 d . . . . .
H00A H 0.6570 0.6407 0.9270 0.020 Uiso 1 1 calc R U . . .
H00B H 0.6009 0.6677 0.8659 0.020 Uiso 1 1 calc R U . . .
C00D C 1.17646(19) 0.5703(2) 0.55416(12) 0.0165(5) Uani 1 1 d . . . . .
H00 H 1.1559 0.5085 0.5365 0.020 Uiso 1 1 calc R U . . .
HA H 1.1206 0.6091 0.5541 0.020 Uiso 1 1 calc R U . . .
C00E C 1.1620(2) 0.4861(2) 0.64323(13) 0.0168(5) Uani 1 1 d . . . . .
H0AA H 1.1968 0.4660 0.6805 0.020 Uiso 1 1 calc R U . . .
HB H 1.1480 0.4282 0.6199 0.020 Uiso 1 1 calc R U . . .
C00F C 1.3184(2) 0.4077(2) 0.58687(12) 0.0163(5) Uani 1 1 d . . . . .
H1AA H 1.2871 0.4173 0.5473 0.020 Uiso 1 1 calc R U . . .
HC H 1.2833 0.3594 0.6035 0.020 Uiso 1 1 calc R U . . .
C00G C 1.31989(19) 0.5023(2) 0.61929(12) 0.0151(5) Uani 1 1 d . . . . .
H2AA H 1.3612 0.5471 0.6049 0.018 Uiso 1 1 calc R U . . .
HD H 1.3472 0.4900 0.6593 0.018 Uiso 1 1 calc R U . . .
C00H C 0.4805(2) 0.6096(2) 0.92971(13) 0.0187(6) Uani 1 1 d . . . . .
H00C H 0.5151 0.6295 0.9671 0.022 Uiso 1 1 calc R U . . .
H00D H 0.4605 0.6677 0.9076 0.022 Uiso 1 1 calc R U . . .
C00I C 0.7985(2) 0.5068(2) 0.96149(13) 0.0209(6) Uani 1 1 d . . . . .
H00E H 0.7548 0.5371 0.9820 0.025 Uiso 1 1 calc R U . . .
H00F H 0.8490 0.5524 0.9601 0.025 Uiso 1 1 calc R U . . .
C00J C 0.5453(2) 0.5502(2) 0.89958(13) 0.0189(6) Uani 1 1 d . . . . .
H00G H 0.5693 0.4944 0.9228 0.023 Uiso 1 1 calc R U . . .
H00H H 0.5103 0.5269 0.8630 0.023 Uiso 1 1 calc R U . . .
C00K C 0.7732(2) 0.6437(2) 0.85839(13) 0.0166(5) Uani 1 1 d . . . . .
H00I H 0.7397 0.6971 0.8368 0.020 Uiso 1 1 calc R U . . .
H00J H 0.7996 0.6678 0.8965 0.020 Uiso 1 1 calc R U . . .
C00L C 0.7482(2) 0.4810(2) 0.90119(12) 0.0158(5) Uani 1 1 d . . . . .
H00K H 0.7002 0.4332 0.9038 0.019 Uiso 1 1 calc R U . . .
H00L H 0.7933 0.4503 0.8819 0.019 Uiso 1 1 calc R U . . .
C00M C 1.2845(3) 0.6432(2) 0.71100(13) 0.0239(6) Uani 1 1 d . . . . .
H3AA H 1.2417 0.6093 0.7307 0.029 Uiso 1 1 calc R U . . .
HE H 1.3431 0.6070 0.7168 0.029 Uiso 1 1 calc R U . . .
C00N C 0.6596(2) 0.5197(2) 0.80607(11) 0.0147(5) Uani 1 1 d . . . . .
H00M H 0.6180 0.4673 0.8120 0.018 Uiso 1 1 calc R U . . .
H00N H 0.7102 0.4916 0.7904 0.018 Uiso 1 1 calc R U . . .
C00O C 1.2357(2) 0.6215(2) 0.51727(13) 0.0198(6) Uani 1 1 d . . . . .
H4AA H 1.2893 0.5814 0.5140 0.024 Uiso 1 1 calc R U . . .
HF H 1.2591 0.6824 0.5350 0.024 Uiso 1 1 calc R U . . .
C00P C 1.0695(2) 0.5312(2) 0.65064(16) 0.0255(7) Uani 1 1 d . . . . .
H5AA H 1.0373 0.5591 0.6146 0.031 Uiso 1 1 calc R U . . .
HG H 1.0819 0.5828 0.6788 0.031 Uiso 1 1 calc R U . . .
C00Q C 0.9217(2) 0.7006(2) 0.83417(13) 0.0212(6) Uani 1 1 d . . . . .
H00O H 0.8870 0.7575 0.8178 0.025 Uiso 1 1 calc R U . . .
H00P H 0.9475 0.7142 0.8742 0.025 Uiso 1 1 calc R U . . .
C00R C 1.2417(2) 0.6488(2) 0.64728(12) 0.0171(5) Uani 1 1 d . . . . .
H6AA H 1.2829 0.6877 0.6289 0.021 Uiso 1 1 calc R U . . .
HH H 1.1819 0.6827 0.6425 0.021 Uiso 1 1 calc R U . . .
C00S C 0.8538(2) 0.6153(2) 0.83035(14) 0.0212(6) Uani 1 1 d . . . . .
H00Q H 0.8299 0.5985 0.7905 0.025 Uiso 1 1 calc R U . . .
H00R H 0.8862 0.5592 0.8496 0.025 Uiso 1 1 calc R U . . .
C00T C 0.5847(2) 0.5445(2) 0.70207(12) 0.0208(6) Uani 1 1 d . . . . .
H00S H 0.5560 0.4812 0.7038 0.025 Uiso 1 1 calc R U . . .
H00T H 0.5397 0.5851 0.6768 0.025 Uiso 1 1 calc R U . . .
C00U C 1.1761(2) 0.6407(3) 0.45791(13) 0.0252(7) Uani 1 1 d . . . . .
H7AA H 1.1498 0.5799 0.4415 0.030 Uiso 1 1 calc R U . . .
HI H 1.1243 0.6832 0.4614 0.030 Uiso 1 1 calc R U . . .
C00V C 0.6050(2) 0.5894(2) 0.76221(13) 0.0209(6) Uani 1 1 d . . . . .
H00U H 0.6410 0.6487 0.7618 0.025 Uiso 1 1 calc R U . . .
H00V H 0.5460 0.6061 0.7730 0.025 Uiso 1 1 calc R U . . .
C00W C 1.2326(3) 0.6870(3) 0.41790(14) 0.0274(7) Uani 1 1 d . . . . .
H8AA H 1.1927 0.6970 0.3810 0.041 Uiso 1 1 calc R U . . .
HJ H 1.2838 0.6450 0.4141 0.041 Uiso 1 1 calc R U . . .
HK H 1.2572 0.7483 0.4333 0.041 Uiso 1 1 calc R U . . .
C00X C 1.3517(3) 0.7423(3) 0.79851(15) 0.0307(7) Uani 1 1 d . . . . .
H9AA H 1.4138 0.7156 0.8021 0.046 Uiso 1 1 calc R U . . .
HL H 1.3159 0.7028 0.8195 0.046 Uiso 1 1 calc R U . . .
HM H 1.3561 0.8071 0.8135 0.046 Uiso 1 1 calc R U . . .
C00Y C 1.3031(2) 0.7442(2) 0.73573(14) 0.0250(7) Uani 1 1 d . . . . .
H0BA H 1.2438 0.7787 0.7318 0.030 Uiso 1 1 calc R U . . .
HN H 1.3422 0.7794 0.7141 0.030 Uiso 1 1 calc R U . . .
C00Z C 1.0023(2) 0.6828(3) 0.80354(14) 0.0268(7) Uani 1 1 d . . . . .
H00W H 0.9781 0.6792 0.7630 0.040 Uiso 1 1 calc R U . . .
H00X H 1.0329 0.6228 0.8166 0.040 Uiso 1 1 calc R U . . .
H00Y H 1.0467 0.7351 0.8116 0.040 Uiso 1 1 calc R U . . .
C010 C 0.6723(2) 0.5331(3) 0.67694(14) 0.0270(7) Uani 1 1 d . . . . .
H01A H 0.6546 0.5115 0.6380 0.041 Uiso 1 1 calc R U . . .
H01B H 0.7136 0.4863 0.6989 0.041 Uiso 1 1 calc R U . . .
H01C H 0.7040 0.5945 0.6781 0.041 Uiso 1 1 calc R U . . .
C011 C 0.9142(2) 0.4952(3) 0.67940(17) 0.0332(8) Uani 1 1 d . . . . .
H01L H 0.8806 0.5235 0.6444 0.050 Uiso 1 1 calc R U . . .
H01M H 0.9260 0.5439 0.7087 0.050 Uiso 1 1 calc R U . . .
H01N H 0.8772 0.4439 0.6909 0.050 Uiso 1 1 calc R U . . .
C012 C 1.4744(2) 0.4332(2) 0.55468(14) 0.0238(6) Uani 1 1 d . . . . .
H01O H 1.4414 0.4358 0.5155 0.036 Uiso 1 1 calc R U . . .
H01P H 1.5355 0.4049 0.5566 0.036 Uiso 1 1 calc R U . . .
H01Q H 1.4813 0.4977 0.5702 0.036 Uiso 1 1 calc R U . . .
C013 C 1.0074(2) 0.4542(2) 0.67010(14) 0.0231(6) Uani 1 1 d . . . . .
H01R H 0.9949 0.4032 0.6415 0.028 Uiso 1 1 calc R U . . .
H01S H 1.0409 0.4254 0.7056 0.028 Uiso 1 1 calc R U . . .
C014 C 0.3936(2) 0.5515(3) 0.93681(15) 0.0268(7) Uani 1 1 d . . . . .
H01D H 0.3553 0.5384 0.8998 0.040 Uiso 1 1 calc R U . . .
H01E H 0.3580 0.5884 0.9592 0.040 Uiso 1 1 calc R U . . .
H01F H 0.4132 0.4914 0.9559 0.040 Uiso 1 1 calc R U . . .
C015 C 0.8386(2) 0.4143(2) 0.99231(13) 0.0231(6) Uani 1 1 d . . . . .
H01G H 0.7876 0.3691 0.9933 0.028 Uiso 1 1 calc R U . . .
H01H H 0.8813 0.3840 0.9711 0.028 Uiso 1 1 calc R U . . .
C016 C 0.8911(3) 0.4344(3) 1.05340(15) 0.0362(9) Uani 1 1 d . . . . .
H01I H 0.9429 0.4773 1.0526 0.054 Uiso 1 1 calc R U . . .
H01J H 0.9143 0.3744 1.0714 0.054 Uiso 1 1 calc R U . . .
H01K H 0.8490 0.4641 1.0746 0.054 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
IRR Pd00 2.5956(3) . ?
IRR Pd1 2.6020(3) . ?
I1 Pd1 2.6022(3) . ?
I2 Pd00 2.6090(3) . ?
I3 Pd1 2.5928(3) . ?
I4 Pd00 2.5892(3) . ?
I5 Pd1 2.5923(3) . ?
I5 Pd00 2.5980(3) . ?
N009 C00N 1.519(3) . ?
N009 C00C 1.525(4) . ?
N009 C00L 1.525(4) . ?
N009 C00K 1.530(4) . ?
N00A C00D 1.520(4) . ?
N00A C00E 1.521(4) . ?
N00A C00G 1.525(3) . ?
N00A C00R 1.527(4) . ?
C00B C012 1.526(4) . ?
C00B C00F 1.527(4) . ?
C00B H00Z 0.9700 . ?
C00B H 0.9700 . ?
C00C C00J 1.521(4) . ?
C00C H00A 0.9700 . ?
C00C H00B 0.9700 . ?
C00D C00O 1.521(4) . ?
C00D H00 0.9700 . ?
C00D HA 0.9700 . ?
C00E C00P 1.520(4) . ?
C00E H0AA 0.9700 . ?
C00E HB 0.9700 . ?
C00F C00G 1.513(4) . ?
C00F H1AA 0.9700 . ?
C00F HC 0.9700 . ?
C00G H2AA 0.9700 . ?
C00G HD 0.9700 . ?
C00H C014 1.530(4) . ?
C00H C00J 1.531(4) . ?
C00H H00C 0.9700 . ?
C00H H00D 0.9700 . ?
C00I C00L 1.517(4) . ?
C00I C015 1.527(4) . ?
C00I H00E 0.9700 . ?
C00I H00F 0.9700 . ?
C00J H00G 0.9700 . ?
C00J H00H 0.9700 . ?
C00K C00S 1.510(4) . ?
C00K H00I 0.9700 . ?
C00K H00J 0.9700 . ?
C00L H00K 0.9700 . ?
C00L H00L 0.9700 . ?
C00M C00Y 1.514(4) . ?
C00M C00R 1.523(4) . ?
C00M H3AA 0.9700 . ?
C00M HE 0.9700 . ?
C00N C00V 1.519(4) . ?
C00N H00M 0.9700 . ?
C00N H00N 0.9700 . ?
C00O C00U 1.524(4) . ?
C00O H4AA 0.9700 . ?
C00O HF 0.9700 . ?
C00P C013 1.525(4) . ?
C00P H5AA 0.9700 . ?
C00P HG 0.9700 . ?
C00Q C00Z 1.519(4) . ?
C00Q C00S 1.523(4) . ?
C00Q H00O 0.9700 . ?
C00Q H00P 0.9700 . ?
C00R H6AA 0.9700 . ?
C00R HH 0.9700 . ?
C00S H00Q 0.9700 . ?
C00S H00R 0.9700 . ?
C00T C010 1.519(4) . ?
C00T C00V 1.535(4) . ?
C00T H00S 0.9700 . ?
C00T H00T 0.9700 . ?
C00U C00W 1.519(5) . ?
C00U H7AA 0.9700 . ?
C00U HI 0.9700 . ?
C00V H00U 0.9700 . ?
C00V H00V 0.9700 . ?
C00W H8AA 0.9600 . ?
C00W HJ 0.9600 . ?
C00W HK 0.9600 . ?
C00X C00Y 1.520(5) . ?
C00X H9AA 0.9600 . ?
C00X HL 0.9600 . ?
C00X HM 0.9600 . ?
C00Y H0BA 0.9700 . ?
C00Y HN 0.9700 . ?
C00Z H00W 0.9600 . ?
C00Z H00X 0.9600 . ?
C00Z H00Y 0.9600 . ?
C010 H01A 0.9600 . ?
C010 H01B 0.9600 . ?
C010 H01C 0.9600 . ?
C011 C013 1.522(4) . ?
C011 H01L 0.9600 . ?
C011 H01M 0.9600 . ?
C011 H01N 0.9600 . ?
C012 H01O 0.9600 . ?
C012 H01P 0.9600 . ?
C012 H01Q 0.9600 . ?
C013 H01R 0.9700 . ?
C013 H01S 0.9700 . ?
C014 H01D 0.9600 . ?
C014 H01E 0.9600 . ?
C014 H01F 0.9600 . ?
C015 C016 1.526(5) . ?
C015 H01G 0.9700 . ?
C015 H01H 0.9700 . ?
C016 H01I 0.9600 . ?
C016 H01J 0.9600 . ?
C016 H01K 0.9600 . ?

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
Pd00 IRR Pd1 94.592(9) . . ?
Pd1 I5 Pd00 94.766(9) . . ?
I4 Pd00 IRR 174.222(12) . . ?
I4 Pd00 I5 88.934(10) . . ?
IRR Pd00 I5 85.318(9) . . ?
I4 Pd00 I2 95.068(10) . . ?
IRR Pd00 I2 90.686(9) . . ?
I5 Pd00 I2 175.974(11) . . ?
I5 Pd1 I3 89.889(9) . . ?
I5 Pd1 IRR 85.302(9) . . ?
I3 Pd1 IRR 174.930(11) . . ?
I5 Pd1 I1 175.536(11) . . ?
I3 Pd1 I1 94.453(10) . . ?
IRR Pd1 I1 90.386(9) . . ?
C00N N009 C00C 111.6(2) . . ?
C00N N009 C00L 105.9(2) . . ?
C00C N009 C00L 111.3(2) . . ?
C00N N009 C00K 111.5(2) . . ?
C00C N009 C00K 105.7(2) . . ?
C00L N009 C00K 111.1(2) . . ?
C00D N00A C00E 108.4(2) . . ?
C00D N00A C00G 111.1(2) . . ?
C00E N00A C00G 109.0(2) . . ?
C00D N00A C00R 108.9(2) . . ?
C00E N00A C00R 111.2(2) . . ?
C00G N00A C00R 108.3(2) . . ?
C012 C00B C00F 113.7(2) . . ?
C012 C00B H00Z 108.8 . . ?
C00F C00B H00Z 108.8 . . ?
C012 C00B H 108.8 . . ?
C00F C00B H 108.8 . . ?
H00Z C00B H 107.7 . . ?
C00J C00C N009 116.3(2) . . ?
C00J C00C H00A 108.2 . . ?
N009 C00C H00A 108.2 . . ?
C00J C00C H00B 108.2 . . ?
N009 C00C H00B 108.2 . . ?
H00A C00C H00B 107.4 . . ?
C00O C00D N00A 115.8(2) . . ?
C00O C00D H00 108.3 . . ?
N00A C00D H00 108.3 . . ?
C00O C00D HA 108.3 . . ?
N00A C00D HA 108.3 . . ?
H00 C00D HA 107.4 . . ?
N00A C00E C00P 115.2(2) . . ?
N00A C00E H0AA 108.5 . . ?
C00P C00E H0AA 108.5 . . ?
N00A C00E HB 108.5 . . ?
C00P C00E HB 108.5 . . ?
H0AA C00E HB 107.5 . . ?
C00G C00F C00B 110.4(2) . . ?
C00G C00F H1AA 109.6 . . ?
C00B C00F H1AA 109.6 . . ?
C00G C00F HC 109.6 . . ?
C00B C00F HC 109.6 . . ?
H1AA C00F HC 108.1 . . ?
C00F C00G N00A 116.1(2) . . ?
C00F C00G H2AA 108.3 . . ?
N00A C00G H2AA 108.3 . . ?
C00F C00G HD 108.3 . . ?
N00A C00G HD 108.3 . . ?
H2AA C00G HD 107.4 . . ?
C014 C00H C00J 111.7(3) . . ?
C014 C00H H00C 109.3 . . ?
C00J C00H H00C 109.3 . . ?
C014 C00H H00D 109.3 . . ?
C00J C00H H00D 109.3 . . ?
H00C C00H H00D 107.9 . . ?
C00L C00I C015 108.9(2) . . ?
C00L C00I H00E 109.9 . . ?
C015 C00I H00E 109.9 . . ?
C00L C00I H00F 109.9 . . ?
C015 C00I H00F 109.9 . . ?
H00E C00I H00F 108.3 . . ?
C00C C00J C00H 109.2(2) . . ?
C00C C00J H00G 109.8 . . ?
C00H C00J H00G 109.8 . . ?
C00C C00J H00H 109.8 . . ?
C00H C00J H00H 109.8 . . ?
H00G C00J H00H 108.3 . . ?
C00S C00K N009 116.9(2) . . ?
C00S C00K H00I 108.1 . . ?
N009 C00K H00I 108.1 . . ?
C00S C00K H00J 108.1 . . ?
N009 C00K H00J 108.1 . . ?
H00I C00K H00J 107.3 . . ?
C00I C00L N009 116.6(2) . . ?
C00I C00L H00K 108.1 . . ?
N009 C00L H00K 108.1 . . ?
C00I C00L H00L 108.1 . . ?
N009 C00L H00L 108.1 . . ?
H00K C00L H00L 107.3 . . ?
C00Y C00M C00R 110.3(3) . . ?
C00Y C00M H3AA 109.6 . . ?
C00R C00M H3AA 109.6 . . ?
C00Y C00M HE 109.6 . . ?
C00R C00M HE 109.6 . . ?
H3AA C00M HE 108.1 . . ?
N009 C00N C00V 115.2(2) . . ?
N009 C00N H00M 108.5 . . ?
C00V C00N H00M 108.5 . . ?
N009 C00N H00N 108.5 . . ?
C00V C00N H00N 108.5 . . ?
H00M C00N H00N 107.5 . . ?
C00D C00O C00U 109.7(2) . . ?
C00D C00O H4AA 109.7 . . ?
C00U C00O H4AA 109.7 . . ?
C00D C00O HF 109.7 . . ?
C00U C00O HF 109.7 . . ?
H4AA C00O HF 108.2 . . ?
C00E C00P C013 109.9(3) . . ?
C00E C00P H5AA 109.7 . . ?
C013 C00P H5AA 109.7 . . ?
C00E C00P HG 109.7 . . ?
C013 C00P HG 109.7 . . ?
H5AA C00P HG 108.2 . . ?
C00Z C00Q C00S 113.5(3) . . ?
C00Z C00Q H00O 108.9 . . ?
C00S C00Q H00O 108.9 . . ?
C00Z C00Q H00P 108.9 . . ?
C00S C00Q H00P 108.9 . . ?
H00O C00Q H00P 107.7 . . ?
C00M C00R N00A 115.9(2) . . ?
C00M C00R H6AA 108.3 . . ?
N00A C00R H6AA 108.3 . . ?
C00M C00R HH 108.3 . . ?
N00A C00R HH 108.3 . . ?
H6AA C00R HH 107.4 . . ?
C00K C00S C00Q 108.9(2) . . ?
C00K C00S H00Q 109.9 . . ?
C00Q C00S H00Q 109.9 . . ?
C00K C00S H00R 109.9 . . ?
C00Q C00S H00R 109.9 . . ?
H00Q C00S H00R 108.3 . . ?
C010 C00T C00V 113.2(3) . . ?
C010 C00T H00S 108.9 . . ?
C00V C00T H00S 108.9 . . ?
C010 C00T H00T 108.9 . . ?
C00V C00T H00T 108.9 . . ?
H00S C00T H00T 107.8 . . ?
C00W C00U C00O 112.4(3) . . ?
C00W C00U H7AA 109.1 . . ?
C00O C00U H7AA 109.1 . . ?
C00W C00U HI 109.1 . . ?
C00O C00U HI 109.1 . . ?
H7AA C00U HI 107.9 . . ?
C00N C00V C00T 111.3(2) . . ?
C00N C00V H00U 109.4 . . ?
C00T C00V H00U 109.4 . . ?
C00N C00V H00V 109.4 . . ?
C00T C00V H00V 109.4 . . ?
H00U C00V H00V 108.0 . . ?
C00U C00W H8AA 109.5 . . ?
C00U C00W HJ 109.5 . . ?
H8AA C00W HJ 109.5 . . ?
C00U C00W HK 109.5 . . ?
H8AA C00W HK 109.5 . . ?
HJ C00W HK 109.5 . . ?
C00Y C00X H9AA 109.5 . . ?
C00Y C00X HL 109.5 . . ?
H9AA C00X HL 109.5 . . ?
C00Y C00X HM 109.5 . . ?
H9AA C00X HM 109.5 . . ?
HL C00X HM 109.5 . . ?
C00M C00Y C00X 112.2(3) . . ?
C00M C00Y H0BA 109.2 . . ?
C00X C00Y H0BA 109.2 . . ?
C00M C00Y HN 109.2 . . ?
C00X C00Y HN 109.2 . . ?
H0BA C00Y HN 107.9 . . ?
C00Q C00Z H00W 109.5 . . ?
C00Q C00Z H00X 109.5 . . ?
H00W C00Z H00X 109.5 . . ?
C00Q C00Z H00Y 109.5 . . ?
H00W C00Z H00Y 109.5 . . ?
H00X C00Z H00Y 109.5 . . ?
C00T C010 H01A 109.5 . . ?
C00T C010 H01B 109.5 . . ?
H01A C010 H01B 109.5 . . ?
C00T C010 H01C 109.5 . . ?
H01A C010 H01C 109.5 . . ?
H01B C010 H01C 109.5 . . ?
C013 C011 H01L 109.5 . . ?
C013 C011 H01M 109.5 . . ?
H01L C011 H01M 109.5 . . ?
C013 C011 H01N 109.5 . . ?
H01L C011 H01N 109.5 . . ?
H01M C011 H01N 109.5 . . ?
C00B C012 H01O 109.5 . . ?
C00B C012 H01P 109.5 . . ?
H01O C012 H01P 109.5 . . ?
C00B C012 H01Q 109.5 . . ?
H01O C012 H01Q 109.5 . . ?
H01P C012 H01Q 109.5 . . ?
C011 C013 C00P 112.5(3) . . ?
C011 C013 H01R 109.1 . . ?
C00P C013 H01R 109.1 . . ?
C011 C013 H01S 109.1 . . ?
C00P C013 H01S 109.1 . . ?
H01R C013 H01S 107.8 . . ?
C00H C014 H01D 109.5 . . ?
C00H C014 H01E 109.5 . . ?
H01D C014 H01E 109.5 . . ?
C00H C014 H01F 109.5 . . ?
H01D C014 H01F 109.5 . . ?
H01E C014 H01F 109.5 . . ?
C016 C015 C00I 112.0(3) . . ?
C016 C015 H01G 109.2 . . ?
C00I C015 H01G 109.2 . . ?
C016 C015 H01H 109.2 . . ?
C00I C015 H01H 109.2 . . ?
H01G C015 H01H 107.9 . . ?
C015 C016 H01I 109.5 . . ?
C015 C016 H01J 109.5 . . ?
H01I C016 H01J 109.5 . . ?
C015 C016 H01K 109.5 . . ?
H01I C016 H01K 109.5 . . ?
H01J C016 H01K 109.5 . . ?

_refine_diff_density_max         2.273
_refine_diff_density_min         -2.307
_refine_diff_density_rms         0.139

####################################################################### 
# 
# 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_2e
_database_code_depnum_ccdc_archive 'CCDC 1581482'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2018-08-17 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_CHEMW03_2e                  
;
PROBLEM: The ratio of given/expected molecular weight as calculated from 
the _atom_site* data lies outside the range 0.90 <> 1.10.

RESPONSE: SQUEEZE used to remove disordered dichloromethane solvent 
molecules, but the reported formula includes the solvent.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        (TBA)2_2e
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C34 H44 N2 O23 V6), 2(C16 H36 N), 2(C H2 Cl2)'
_chemical_formula_sum            'C68 H120 Cl4 N4 O23 V6'
_chemical_formula_weight         1809.16

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.5526(11)
_cell_length_b                   15.1317(8)
_cell_length_c                   30.7827(17)
_cell_angle_alpha                90
_cell_angle_beta                 107.3380(10)
_cell_angle_gamma                90
_cell_volume                     8693.7(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4385
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.24
_cell_measurement_theta_min      2.18

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_F_000             3435
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    0.810
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0977 before and 0.0489 after correction. The Ratio of minimum to maximum transmission is 0.9163. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48623
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.733
_diffrn_reflns_theta_max         25.413
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7994
_reflns_number_gt                4605
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    ShelXS
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1100P)²+35.2450P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7994
_refine_ls_number_parameters     441
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0778
_refine_ls_wR_factor_ref         0.2563
_refine_ls_wR_factor_gt          0.2147
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C0AA C 0.3837(3) 0.3030(4) 0.13257(19) 0.0786(18) Uani 1 1 d . . . . .
H0AA H 0.3319 0.3032 0.1251 0.094 Uiso 1 1 calc R U . . .
H0AB H 0.3975 0.2511 0.1187 0.094 Uiso 1 1 calc R U . . .
C1AA C 0.5121(4) 0.3836(6) 0.3777(2) 0.101(2) Uani 1 1 d . . . . .
H1AA H 0.4980 0.3317 0.3914 0.122 Uiso 1 1 calc R U . . .
H1AB H 0.4984 0.4354 0.3918 0.122 Uiso 1 1 calc R U . . .
C2AA C 0.6166(3) 0.4676(4) 0.3689(2) 0.0830(19) Uani 1 1 d . . . . .
H2AA H 0.6014 0.5182 0.3830 0.100 Uiso 1 1 calc R U . . .
H2AB H 0.6685 0.4688 0.3768 0.100 Uiso 1 1 calc R U . . .
C3AA C 0.6263(4) 0.3824(6) 0.4397(2) 0.111(3) Uani 1 1 d . . . . .
H3AA H 0.6102 0.4339 0.4528 0.133 Uiso 1 1 calc R U . . .
H3AB H 0.6110 0.3299 0.4523 0.133 Uiso 1 1 calc R U . . .
C4 C 0.7350(4) 0.3790(5) 0.4973(2) 0.103(2) Uani 1 1 d . . . . .
H4A H 0.7198 0.3261 0.5096 0.123 Uiso 1 1 calc R U . . .
H4B H 0.7213 0.4298 0.5121 0.123 Uiso 1 1 calc R U . . .
C4AA C 1.0456(5) 0.3618(6) 0.5410(3) 0.128(4) Uani 1 1 d . . . . .
H4AA H 1.0688 0.3470 0.5712 0.153 Uiso 1 1 calc R U . . .
C5AA C 0.8471(5) 0.3776(6) 0.4723(3) 0.117(3) Uani 1 1 d . . . . .
H5AA H 0.8196 0.3804 0.4419 0.141 Uiso 1 1 calc R U . . .
C6 C 0.8142(4) 0.3777(5) 0.5067(3) 0.097(2) Uani 1 1 d . . . . .
C6AA C 0.5930(3) 0.3832(5) 0.3869(2) 0.085(2) Uani 1 1 d . . . . .
C7 C 0.9313(5) 0.3742(6) 0.5611(3) 0.124(3) Uani 1 1 d . . . . .
H7 H 0.9592 0.3739 0.5914 0.149 Uiso 1 1 calc R U . . .
C7AA C 1.2821(5) 0.3682(6) 0.5267(3) 0.133(3) Uani 1 1 d . . . . .
H7AA H 1.3009 0.4270 0.5327 0.200 Uiso 1 1 calc R U . . .
H7AB H 1.3024 0.3398 0.5055 0.200 Uiso 1 1 calc R U . . .
H7AC H 1.2943 0.3351 0.5546 0.200 Uiso 1 1 calc R U . . .
C8 C 1.1773(6) 0.3831(7) 0.4588(3) 0.145(4) Uani 1 1 d . . . . .
H8A H 1.1618 0.4430 0.4520 0.217 Uiso 1 1 calc R U . . .
H8B H 1.1376 0.3439 0.4468 0.217 Uiso 1 1 calc R U . . .
H8C H 1.2144 0.3697 0.4453 0.217 Uiso 1 1 calc R U . . .
C9 C 1.1645(6) 0.3643(7) 0.5359(4) 0.131(4) Uani 1 1 d . . . . .
C11 C 1.0838(5) 0.3727(5) 0.5160(3) 0.105(3) Uani 1 1 d . . . . .
H11 H 1.0634 0.3859 0.4854 0.126 Uiso 1 1 calc R U . . .
C12 C 0.9648(5) 0.3700(5) 0.5278(3) 0.107(3) Uani 1 1 d . . . . .
C13 C 0.8581(5) 0.3789(5) 0.5513(3) 0.117(3) Uani 1 1 d . . . . .
H13 H 0.8377 0.3829 0.5749 0.141 Uiso 1 1 calc R U . . .
C16 C 0.9219(5) 0.3732(6) 0.4838(3) 0.126(3) Uani 1 1 d . . . . .
H16 H 0.9432 0.3725 0.4605 0.151 Uiso 1 1 calc R U . . .
N2 N 1.2046(5) 0.3720(4) 0.5075(3) 0.119(2) Uani 1 1 d . . . . .
O0AA O 0.5000 0.3853(3) 0.2500 0.0551(12) Uani 1 2 d S T P . .
O1 O 0.3882(2) 0.4731(3) 0.25970(15) 0.0841(13) Uani 1 1 d . . . . .
O2 O 0.3878(2) 0.2968(3) 0.25973(13) 0.0799(12) Uani 1 1 d . . . . .
O4 O 0.41353(19) 0.2973(2) 0.18036(12) 0.0644(10) Uani 1 1 d . . . . .
O5 O 0.5000 0.5615(3) 0.2500 0.087(2) Uani 1 2 d S T P . .
O6 O 0.58649(19) 0.4733(2) 0.32032(13) 0.0703(11) Uani 1 1 d . . . . .
O7 O 0.29820(19) 0.3843(3) 0.18957(14) 0.0760(11) Uani 1 1 d . . . . .
O8 O 0.5000 0.2090(3) 0.2500 0.0778(17) Uani 1 2 d S T P . .
O9 O 0.4735(2) 0.2052(3) 0.33049(14) 0.0997(16) Uani 1 1 d . . . . .
O11 O 0.4750(2) 0.3843(3) 0.32984(13) 0.0811(12) Uani 1 1 d . . . . .
O12 O 0.7009(3) 0.3833(3) 0.45010(14) 0.0988(16) Uani 1 1 d . . . . .
O19 O 0.4728(2) 0.5633(4) 0.33117(19) 0.117(2) Uani 1 1 d . . . . .
V1 V 0.38125(5) 0.38508(6) 0.21880(3) 0.0629(3) Uani 1 1 d . . . . .
V2 V 0.48019(5) 0.27602(7) 0.29362(3) 0.0658(3) Uani 1 1 d . . . . .
V3 V 0.48040(5) 0.49399(7) 0.29359(4) 0.0790(4) Uani 1 1 d . . . . .
O3B O 1.1924(4) 0.3522(7) 0.5762(3) 0.188(4) Uani 1 1 d . . . A 2
C0BA C 0.6838(7) 0.6712(9) 0.3195(5) 0.091(4) Uiso 0.551(9) 1 d D . P B 2
H0BA H 0.7172 0.6676 0.3498 0.109 Uiso 0.551(9) 1 calc R U P B 2
H0BB H 0.6666 0.6115 0.3112 0.109 Uiso 0.551(9) 1 calc R U P B 2
C0CA C 0.7470(10) 0.6012(12) 0.3104(6) 0.160(7) Uiso 0.651(10) 1 d D . P B 1
H0CA H 0.7691 0.6075 0.3430 0.192 Uiso 0.651(10) 1 calc R U P B 1
H0CB H 0.7038 0.5665 0.3061 0.192 Uiso 0.651(10) 1 calc R U P B 1
C0DA C 0.919(2) 0.462(4) 0.3663(18) 0.20(2) Uiso 0.349(10) 1 d D . P B 2
H0DA H 0.9233 0.4640 0.3361 0.299 Uiso 0.349(10) 1 calc R U P B 2
H0DB H 0.9223 0.4022 0.3768 0.299 Uiso 0.349(10) 1 calc R U P B 2
H0DC H 0.9565 0.4967 0.3863 0.299 Uiso 0.349(10) 1 calc R U P B 2
C1 C 0.6731(8) 0.6925(9) 0.1562(4) 0.089(4) Uiso 0.642(19) 1 d . . P B 2
H1A H 0.6441 0.6397 0.1538 0.107 Uiso 0.642(19) 1 calc R U P B 2
H1B H 0.6399 0.7414 0.1469 0.107 Uiso 0.642(19) 1 calc R U P B 2
C1CA C 0.735(2) 0.685(2) 0.2488(13) 0.155(13) Uiso 0.358(19) 1 d . . P B 1
H1CA H 0.7753 0.6447 0.2536 0.186 Uiso 0.358(19) 1 calc R U P B 1
H1CB H 0.7528 0.7422 0.2424 0.186 Uiso 0.358(19) 1 calc R U P B 1
C2BA C 0.8009(8) 0.6421(10) 0.3015(5) 0.053(4) Uiso 0.349(10) 1 d D . P B 2
H2BA H 0.8034 0.6217 0.2721 0.064 Uiso 0.349(10) 1 calc R U P B 2
H2BB H 0.8369 0.6881 0.3107 0.064 Uiso 0.349(10) 1 calc R U P B 2
C2CA C 0.6765(17) 0.653(2) 0.1995(11) 0.125(10) Uiso 0.358(19) 1 d . . P B 1
C3 C 0.6229(6) 0.7208(8) 0.3237(4) 0.078(4) Uiso 0.551(9) 1 d D . P B 2
H3A H 0.6378 0.7820 0.3235 0.093 Uiso 0.551(9) 1 calc R U P B 2
H3B H 0.5867 0.7119 0.2946 0.093 Uiso 0.551(9) 1 calc R U P B 2
C3BA C 0.6104(16) 0.7668(19) 0.2828(12) 0.205(14) Uiso 0.449(9) 1 d D . P B 1
H3BA H 0.5888 0.7717 0.2501 0.246 Uiso 0.449(9) 1 calc R U P B 1
H3BB H 0.6412 0.8177 0.2930 0.246 Uiso 0.449(9) 1 calc R U P B 1
C3CA C 0.8060(8) 0.9223(10) 0.3402(5) 0.061(4) Uiso 0.427(12) 1 d . . P B 2
H3CA H 0.7845 0.9799 0.3407 0.073 Uiso 0.427(12) 1 calc R U P B 2
H3CB H 0.8473 0.9288 0.3292 0.073 Uiso 0.427(12) 1 calc R U P B 2
C4BA C 0.5298(12) 0.7550(16) 0.3668(8) 0.127(8) Uiso 0.449(9) 1 d D . P B 1
H4BA H 0.5608 0.7955 0.3877 0.190 Uiso 0.449(9) 1 calc R U P B 1
H4BB H 0.5405 0.6957 0.3779 0.190 Uiso 0.449(9) 1 calc R U P B 1
H4BC H 0.4809 0.7685 0.3643 0.190 Uiso 0.449(9) 1 calc R U P B 1
C4CA C 0.8366(8) 0.9492(11) 0.3961(5) 0.110(5) Uiso 0.573(12) 1 d . . P B 1
H4CA H 0.7954 0.9621 0.4059 0.165 Uiso 0.573(12) 1 calc R U P B 1
H4CB H 0.8576 1.0034 0.3901 0.165 Uiso 0.573(12) 1 calc R U P B 1
H4CC H 0.8711 0.9172 0.4197 0.165 Uiso 0.573(12) 1 calc R U P B 1
C5BA C 0.7830(7) 0.8160(9) 0.3475(5) 0.093(4) Uiso 0.573(12) 1 d . . P B 1
H5BA H 0.8072 0.7806 0.3738 0.112 Uiso 0.573(12) 1 calc R U P B 1
H5BB H 0.7358 0.8270 0.3506 0.112 Uiso 0.573(12) 1 calc R U P B 1
C5CA C 0.7702(7) 0.7627(9) 0.3179(5) 0.079(3) Uiso 0.573(12) 1 d . . P B 1
H5CA H 0.8149 0.7300 0.3275 0.094 Uiso 0.573(12) 1 calc R U P B 1
H5CB H 0.7756 0.8002 0.2935 0.094 Uiso 0.573(12) 1 calc R U P B 1
C6BA C 0.5443(11) 0.7654(15) 0.3094(7) 0.119(7) Uiso 0.449(9) 1 d D . P B 1
H6BA H 0.5130 0.7193 0.2925 0.143 Uiso 0.449(9) 1 calc R U P B 1
H6BB H 0.5191 0.8200 0.2984 0.143 Uiso 0.449(9) 1 calc R U P B 1
C6CA C 0.7475(12) 0.8527(16) 0.3080(8) 0.117(7) Uiso 0.427(12) 1 d . . P B 2
C7BA C 0.5891(8) 0.7199(10) 0.3512(5) 0.108(5) Uiso 0.551(9) 1 d D . P B 2
H7BA H 0.6217 0.7355 0.3807 0.130 Uiso 0.551(9) 1 calc R U P B 2
H7BB H 0.5735 0.6597 0.3534 0.130 Uiso 0.551(9) 1 calc R U P B 2
C7CA C 0.8175(14) 0.9017(18) 0.3594(10) 0.163(9) Uiso 0.573(12) 1 d . . P B 1
H7CA H 0.8614 0.8960 0.3511 0.196 Uiso 0.573(12) 1 calc R U P B 1
H7CB H 0.7874 0.9414 0.3370 0.196 Uiso 0.573(12) 1 calc R U P B 1
C8AA C 0.6878(10) 0.6861(11) 0.2391(5) 0.119(5) Uiso 0.642(19) 1 d . . P B 2
H8AA H 0.6739 0.6245 0.2340 0.143 Uiso 0.642(19) 1 calc R U P B 2
H8AB H 0.6436 0.7194 0.2335 0.143 Uiso 0.642(19) 1 calc R U P B 2
C8BA C 0.6441(7) 0.7024(8) 0.2912(4) 0.058(3) Uiso 0.449(9) 1 d D . P B 1
H8BA H 0.6172 0.6575 0.2706 0.069 Uiso 0.449(9) 1 calc R U P B 1
H8BB H 0.6442 0.6850 0.3215 0.069 Uiso 0.449(9) 1 calc R U P B 1
C8CA C 0.8282(15) 0.5720(17) 0.3311(9) 0.116(8) Uiso 0.349(10) 1 d D . P B 2
H8CA H 0.8766 0.5952 0.3384 0.139 Uiso 0.349(10) 1 calc R U P B 2
H8CB H 0.8257 0.5322 0.3059 0.139 Uiso 0.349(10) 1 calc R U P B 2
C9AA C 0.7124(9) 0.7060(12) 0.2085(5) 0.117(5) Uiso 0.642(19) 1 d . . P B 2
H9AA H 0.7577 0.6751 0.2147 0.141 Uiso 0.642(19) 1 calc R U P B 2
H9AB H 0.7238 0.7685 0.2123 0.141 Uiso 0.642(19) 1 calc R U P B 2
C9BA C 0.7087(12) 0.6845(15) 0.1219(7) 0.163(8) Uiso 0.642(19) 1 d . . P B 2
H9BA H 0.7196 0.7424 0.1129 0.244 Uiso 0.642(19) 1 calc R U P B 2
H9BB H 0.6781 0.6543 0.0959 0.244 Uiso 0.642(19) 1 calc R U P B 2
H9BC H 0.7523 0.6517 0.1338 0.244 Uiso 0.642(19) 1 calc R U P B 2
C9CA C 0.8521(15) 0.4974(18) 0.3659(10) 0.116(9) Uiso 0.349(10) 1 d D . P B 2
H9CA H 0.8551 0.5198 0.3959 0.139 Uiso 0.349(10) 1 calc R U P B 2
H9CB H 0.8164 0.4507 0.3587 0.139 Uiso 0.349(10) 1 calc R U P B 2
C14 C 0.7500(7) 0.7926(10) 0.2952(5) 0.057(4) Uiso 0.427(12) 1 d . . P B 2
H6CA H 0.8015 0.7838 0.3055 0.069 Uiso 0.427(12) 1 calc R U P B 2
H6CB H 0.7399 0.8080 0.2633 0.069 Uiso 0.427(12) 1 calc R U P B 2
C15 C 0.6746(14) 0.7289(18) 0.1272(8) 0.103(8) Uiso 0.358(19) 1 d . . P B 1
H15A H 0.6453 0.6913 0.1039 0.154 Uiso 0.358(19) 1 calc R U P B 1
H15B H 0.7090 0.7590 0.1158 0.154 Uiso 0.358(19) 1 calc R U P B 1
H15C H 0.6449 0.7716 0.1360 0.154 Uiso 0.358(19) 1 calc R U P B 1
N13 N 0.7252(3) 0.6943(3) 0.29008(17) 0.0725(13) Uiso 1 1 d . . . . .
C2 C 0.8551(8) 0.4910(10) 0.3057(5) 0.125(5) Uiso 0.651(10) 1 d D . P B 1
H2A H 0.8387 0.4348 0.2912 0.150 Uiso 0.651(10) 1 calc R U P B 1
H2B H 0.8919 0.5125 0.2932 0.150 Uiso 0.651(10) 1 calc R U P B 1
C5 C 0.7950(8) 0.5525(11) 0.2921(5) 0.125(5) Uiso 0.651(10) 1 d D . P B 1
H5A H 0.8144 0.5990 0.2775 0.150 Uiso 0.651(10) 1 calc R U P B 1
H5B H 0.7619 0.5209 0.2672 0.150 Uiso 0.651(10) 1 calc R U P B 1
C10 C 0.8878(19) 0.474(3) 0.3523(9) 0.240(15) Uiso 0.651(10) 1 d D . P B 1
H10A H 0.8746 0.5197 0.3700 0.359 Uiso 0.651(10) 1 calc R U P B 1
H10B H 0.9389 0.4738 0.3585 0.359 Uiso 0.651(10) 1 calc R U P B 1
H10C H 0.8721 0.4180 0.3601 0.359 Uiso 0.651(10) 1 calc R U P B 1
C1DA C 0.7137(17) 0.6733(18) 0.1682(9) 0.112(9) Uiso 0.358(19) 1 d . . P B 1
H1DA H 0.7275 0.6181 0.1572 0.134 Uiso 0.358(19) 1 calc R U P B 1
H1DB H 0.7574 0.7040 0.1844 0.134 Uiso 0.358(19) 1 calc R U P B 1
C18 C 0.831(3) 0.874(3) 0.3952(17) 0.27(2) Uiso 0.427(12) 1 d . . P B 2
H18A H 0.8150 0.9107 0.4156 0.409 Uiso 0.427(12) 1 calc R U P B 2
H18B H 0.8821 0.8678 0.4061 0.409 Uiso 0.427(12) 1 calc R U P B 2
H18C H 0.8092 0.8165 0.3936 0.409 Uiso 0.427(12) 1 calc R U P B 2
C1BA C 0.5286(10) 0.7753(13) 0.3429(7) 0.125(6) Uiso 0.551(9) 1 d D . P B 2
H7BC H 0.5181 0.7863 0.3709 0.188 Uiso 0.551(9) 1 calc R U P B 2
H1BA H 0.4883 0.7471 0.3217 0.188 Uiso 0.551(9) 1 calc R U P B 2
H1BB H 0.5383 0.8303 0.3303 0.188 Uiso 0.551(9) 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
C0AA O4 1.414(6) . ?
C0AA C6AA 1.484(9) 2_655 ?
C1AA O11 1.436(7) . ?
C1AA C6AA 1.522(10) . ?
C2AA O6 1.436(7) . ?
C2AA C6AA 1.517(9) . ?
C3AA O12 1.398(9) . ?
C3AA C6AA 1.562(9) . ?
C4 O12 1.408(7) . ?
C4 C6 1.488(11) . ?
C4AA C11 1.233(12) . ?
C4AA C12 1.513(13) . ?
C5AA C6 1.394(12) . ?
C5AA C16 1.399(12) . ?
C6 C13 1.386(9) . ?
C6AA C0AA 1.484(9) 2_655 ?
C7 C12 1.373(13) . ?
C7 C13 1.374(13) . ?
C7AA N2 1.455(11) . ?
C8 N2 1.443(11) . ?
C9 O3B 1.211(10) . ?
C9 N2 1.341(12) . ?
C9 C11 1.519(12) . ?
C12 C16 1.366(10) . ?
O0AA V3 2.227(3) 2_655 ?
O0AA V3 2.227(3) . ?
O0AA V1 2.2325(8) . ?
O0AA V1 2.2326(8) 2_655 ?
O0AA V2 2.235(3) . ?
O0AA V2 2.235(3) 2_655 ?
O1 V1 1.809(4) . ?
O1 V3 1.821(4) . ?
O2 V1 1.814(4) . ?
O2 V2 1.824(4) . ?
O4 V1 2.002(4) . ?
O4 V2 2.018(3) 2_655 ?
O5 V3 1.816(3) 2_655 ?
O5 V3 1.816(3) . ?
O6 V3 2.015(4) . ?
O6 V1 2.020(4) 2_655 ?
O7 V1 1.605(4) . ?
O8 V2 1.814(3) 2_655 ?
O8 V2 1.814(3) . ?
O9 V2 1.594(4) . ?
O11 V2 2.001(4) . ?
O11 V3 2.020(5) . ?
O19 V3 1.601(5) . ?
V1 O6 2.020(4) 2_655 ?
V1 V3 3.0191(13) . ?
V1 V2 3.0192(13) . ?
V2 O4 2.018(3) 2_655 ?
V2 V2 3.009(2) 2_655 ?
V3 V3 3.003(3) 2_655 ?
C0BA N13 1.426(13) . ?
C0BA C3 1.445(15) . ?
C0CA C5 1.435(18) . ?
C0CA N13 1.549(17) . ?
C0DA C9CA 1.41(3) . ?
C1 C9BA 1.43(3) . ?
C1 C9AA 1.58(2) . ?
C1CA N13 1.35(3) . ?
C1CA C2CA 1.68(6) . ?
C2BA C8CA 1.40(3) . ?
C2BA N13 1.621(15) . ?
C2CA C1DA 1.40(4) . ?
C3 C7BA 1.220(17) . ?
C3BA C8BA 1.16(2) . ?
C3BA C6BA 1.72(4) . ?
C3CA C6CA 1.65(3) . ?
C3CA C18 1.77(5) . ?
C4BA C6BA 1.88(3) . ?
C4CA C7CA 1.30(3) . ?
C5BA C5CA 1.187(15) . ?
C5BA C7CA 1.46(3) . ?
C5CA N13 1.459(13) . ?
C6CA C14 1.00(2) . ?
C7BA C1BA 1.41(2) . ?
C8AA C9AA 1.216(19) . ?
C8AA N13 1.526(16) . ?
C8BA N13 1.600(13) . ?
C8CA C9CA 1.53(3) . ?
C14 N13 1.558(15) . ?
C15 C1DA 1.52(4) . ?
C2 C10 1.41(2) . ?
C2 C5 1.459(18) . ?

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
O4 C0AA C6AA 112.8(5) . 2_655 ?
O11 C1AA C6AA 111.7(6) . . ?
O6 C2AA C6AA 110.8(5) . . ?
O12 C3AA C6AA 108.7(6) . . ?
O12 C4 C6 110.2(7) . . ?
C11 C4AA C12 126.7(9) . . ?
C6 C5AA C16 119.5(8) . . ?
C13 C6 C5AA 117.5(8) . . ?
C13 C6 C4 119.6(9) . . ?
C5AA C6 C4 122.9(6) . . ?
C0AA C6AA C2AA 112.2(6) 2_655 . ?
C0AA C6AA C1AA 110.9(5) 2_655 . ?
C2AA C6AA C1AA 110.0(6) . . ?
C0AA C6AA C3AA 109.3(6) 2_655 . ?
C2AA C6AA C3AA 108.0(5) . . ?
C1AA C6AA C3AA 106.2(6) . . ?
C12 C7 C13 122.4(8) . . ?
O3B C9 N2 120.5(10) . . ?
O3B C9 C11 121.5(11) . . ?
N2 C9 C11 118.1(9) . . ?
C4AA C11 C9 119.2(9) . . ?
C16 C12 C7 116.8(9) . . ?
C16 C12 C4AA 123.7(10) . . ?
C7 C12 C4AA 119.6(8) . . ?
C7 C13 C6 121.0(10) . . ?
C12 C16 C5AA 122.6(10) . . ?
C9 N2 C8 125.4(9) . . ?
C9 N2 C7AA 118.2(8) . . ?
C8 N2 C7AA 116.3(10) . . ?
V3 O0AA V3 84.78(17) 2_655 . ?
V3 O0AA V1 94.90(10) 2_655 . ?
V3 O0AA V1 85.22(9) . . ?
V3 O0AA V1 85.21(9) 2_655 2_655 ?
V3 O0AA V1 94.90(10) . 2_655 ?
V1 O0AA V1 179.8(2) . 2_655 ?
V3 O0AA V2 179.88(14) 2_655 . ?
V3 O0AA V2 95.31(4) . . ?
V1 O0AA V2 85.02(9) . . ?
V1 O0AA V2 94.86(10) 2_655 . ?
V3 O0AA V2 95.32(4) 2_655 2_655 ?
V3 O0AA V2 179.87(14) . 2_655 ?
V1 O0AA V2 94.86(10) . 2_655 ?
V1 O0AA V2 85.02(9) 2_655 2_655 ?
V2 O0AA V2 84.60(16) . 2_655 ?
V1 O1 V3 112.5(2) . . ?
V1 O2 V2 112.2(2) . . ?
C0AA O4 V1 118.0(3) . . ?
C0AA O4 V2 118.6(4) . 2_655 ?
V1 O4 V2 109.88(16) . 2_655 ?
V3 O5 V3 111.6(3) 2_655 . ?
C2AA O6 V3 119.1(4) . . ?
C2AA O6 V1 118.5(3) . 2_655 ?
V3 O6 V1 109.01(16) . 2_655 ?
V2 O8 V2 112.0(3) 2_655 . ?
C1AA O11 V2 118.2(4) . . ?
C1AA O11 V3 118.6(4) . . ?
V2 O11 V3 110.2(2) . . ?
C3AA O12 C4 112.1(6) . . ?
O7 V1 O1 104.40(19) . . ?
O7 V1 O2 103.6(2) . . ?
O1 V1 O2 94.8(2) . . ?
O7 V1 O4 96.24(18) . . ?
O1 V1 O4 158.11(16) . . ?
O2 V1 O4 87.28(18) . . ?
O7 V1 O6 96.55(19) . 2_655 ?
O1 V1 O6 87.5(2) . 2_655 ?
O2 V1 O6 158.46(17) . 2_655 ?
O4 V1 O6 82.90(17) . 2_655 ?
O7 V1 O0AA 171.90(17) . . ?
O1 V1 O0AA 81.19(15) . . ?
O2 V1 O0AA 81.54(15) . . ?
O4 V1 O0AA 77.56(13) . . ?
O6 V1 O0AA 77.65(13) 2_655 . ?
O7 V1 V3 138.05(15) . . ?
O1 V1 V3 33.87(12) . . ?
O2 V1 V3 88.60(12) . . ?
O4 V1 V3 124.68(10) . . ?
O6 V1 V3 81.40(11) 2_655 . ?
O0AA V1 V3 47.32(9) . . ?
O7 V1 V2 137.31(16) . . ?
O1 V1 V2 88.46(15) . . ?
O2 V1 V2 34.01(12) . . ?
O4 V1 V2 81.09(10) . . ?
O6 V1 V2 124.95(10) 2_655 . ?
O0AA V1 V2 47.53(9) . . ?
V3 V1 V2 66.22(3) . . ?
O9 V2 O8 103.4(3) . . ?
O9 V2 O2 104.2(2) . . ?
O8 V2 O2 93.81(15) . . ?
O9 V2 O11 97.2(2) . . ?
O8 V2 O11 158.04(19) . . ?
O2 V2 O11 88.37(19) . . ?
O9 V2 O4 96.79(19) . 2_655 ?
O8 V2 O4 87.78(12) . 2_655 ?
O2 V2 O4 157.91(18) . 2_655 ?
O11 V2 O4 82.26(16) . 2_655 ?
O9 V2 O0AA 172.05(16) . . ?
O8 V2 O0AA 81.69(16) . . ?
O2 V2 O0AA 81.25(13) . . ?
O11 V2 O0AA 77.05(15) . . ?
O4 V2 O0AA 77.18(11) 2_655 . ?
O9 V2 V2 137.2(2) . 2_655 ?
O8 V2 V2 33.99(14) . 2_655 ?
O2 V2 V2 87.93(14) . 2_655 ?
O11 V2 V2 124.51(13) . 2_655 ?
O4 V2 V2 81.12(12) 2_655 2_655 ?
O0AA V2 V2 47.70(8) . 2_655 ?
O9 V2 V1 137.77(18) . . ?
O8 V2 V1 88.31(10) . . ?
O2 V2 V1 33.81(13) . . ?
O11 V2 V1 81.39(13) . . ?
O4 V2 V1 124.44(11) 2_655 . ?
O0AA V2 V1 47.45(3) . . ?
V2 V2 V1 66.17(3) 2_655 . ?
O19 V3 O5 104.6(3) . . ?
O19 V3 O1 103.8(2) . . ?
O5 V3 O1 93.75(17) . . ?
O19 V3 O6 96.5(2) . . ?
O5 V3 O6 88.33(13) . . ?
O1 V3 O6 158.35(17) . . ?
O19 V3 O11 96.2(3) . . ?
O5 V3 O11 158.04(19) . . ?
O1 V3 O11 88.15(19) . . ?
O6 V3 O11 82.15(17) . . ?
O19 V3 O0AA 171.5(2) . . ?
O5 V3 O0AA 81.83(16) . . ?
O1 V3 O0AA 81.09(13) . . ?
O6 V3 O0AA 77.88(11) . . ?
O11 V3 O0AA 76.86(15) . . ?
O19 V3 V3 138.6(2) . 2_655 ?
O5 V3 V3 34.22(14) . 2_655 ?
O1 V3 V3 87.75(15) . 2_655 ?
O6 V3 V3 81.89(13) . 2_655 ?
O11 V3 V3 124.25(12) . 2_655 ?
O0AA V3 V3 47.61(9) . 2_655 ?
O19 V3 V1 137.02(17) . . ?
O5 V3 V1 88.41(10) . . ?
O1 V3 V1 33.62(13) . . ?
O6 V3 V1 125.12(11) . . ?
O11 V3 V1 81.10(11) . . ?
O0AA V3 V1 47.47(3) . . ?
V3 V3 V1 66.13(4) 2_655 . ?
N13 C0BA C3 124.6(11) . . ?
C5 C0CA N13 116.2(13) . . ?
C9BA C1 C9AA 124.6(15) . . ?
N13 C1CA C2CA 129(3) . . ?
C8CA C2BA N13 131.2(15) . . ?
C1DA C2CA C1CA 102(3) . . ?
C7BA C3 C0BA 133.4(14) . . ?
C8BA C3BA C6BA 110(3) . . ?
C6CA C3CA C18 104.7(19) . . ?
C5CA C5BA C7CA 140.7(17) . . ?
C5BA C5CA N13 152.2(12) . . ?
C3BA C6BA C4BA 142.4(17) . . ?
C14 C6CA C3CA 135(2) . . ?
C3 C7BA C1BA 117.7(16) . . ?
C4CA C7CA C5BA 135(2) . . ?
C9AA C8AA N13 126.7(17) . . ?
C3BA C8BA N13 124(2) . . ?
C2BA C8CA C9CA 174(2) . . ?
C8AA C9AA C1 125.0(18) . . ?
C0DA C9CA C8CA 112(3) . . ?
C6CA C14 N13 149.2(18) . . ?
C1CA N13 C5CA 113.1(18) . . ?
C0BA N13 C8AA 116.3(10) . . ?
C1CA N13 C0CA 100.8(18) . . ?
C5CA N13 C0CA 111.2(10) . . ?
C0BA N13 C14 112.9(8) . . ?
C8AA N13 C14 102.8(9) . . ?
C1CA N13 C8BA 117(2) . . ?
C5CA N13 C8BA 111.2(7) . . ?
C0CA N13 C8BA 102.5(9) . . ?
C0BA N13 C2BA 113.5(8) . . ?
C8AA N13 C2BA 108.0(9) . . ?
C14 N13 C2BA 101.9(8) . . ?
C10 C2 C5 119(2) . . ?
C0CA C5 C2 141.3(15) . . ?
C2CA C1DA C15 117(3) . . ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.081


