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

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

data_matrm23
_database_code_depnum_ccdc_archive 'CCDC 2145266'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2022-01-28 deposited with the CCDC.	2022-04-29 downloaded from the CCDC.
;

_vrf_PLAT301_matrm23             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 13% 
RESPONSE: In the asymmetric unit, one tBu group (C17-C20) and one
methoxy ligand (O10-C28) are modeled as disordered over two positions
each (0.560(5):0.440(5) and 0.59(4):0.41(4), respectively).
;

_vrf_PLAT606_matrm23             
;
PROBLEM: _G Solvent Accessible VOID(S) in Structure! 
RESPONSE: Reflection contributions from highly disordered
solvent (likely acetonitrile) were fixed and added to the
calculated structure factors using the SQUEEZE routine of
program Platon (Spek, 2015), which determined there to be
395 electrons in 1736 \%A^3^ treated this way. Because the
exact identity and amount of solvent were unknown, no
solvent was included in the atom list or molecular formula.
Thus all calculated quantities that derive from the molecular
formula (e.g., F(000), density, molecular weight, etc.) are
known to be incorrect.
;

_vrf_PLAT860_matrm23             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 92 
RESPONSE: Analogous bond lengths and angles between the two
positions of the disordered species were restrained to be
similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and restrained toward
the expected motion relative to bond direction.
;

_vrf_PLAT869_matrm23             
;
PROBLEM: _G ALERTS Related to the Use of SQUEEZE Suppressed! 
RESPONSE: Reflection contributions from highly disordered
solvent (likely acetonitrile) were fixed and added to the
calculated structure factors using the SQUEEZE routine of
program Platon (Spek, 2015), which determined there to be
395 electrons in 1736 \%A^3^ treated this way. Because the
exact identity and amount of solvent were unknown, no
solvent was included in the atom list or molecular formula.
Thus all calculated quantities that derive from the molecular
formula (e.g., F(000), density, molecular weight, etc.) are
known to be incorrect.
;

_audit_creation_date             2020-12-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H79 N O18 V6'
_chemical_formula_sum            'C54 H79 N O18 V6'
_chemical_formula_weight         1335.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   20.0174(2)
_cell_length_b                   17.51540(10)
_cell_length_c                   21.2630(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.9550(10)
_cell_angle_gamma                90
_cell_volume                     7202.57(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27639
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8340
_cell_measurement_theta_min      3.3190
_shelx_estimated_absorpt_T_max   0.725
_shelx_estimated_absorpt_T_min   0.337
_exptl_absorpt_coefficient_mu    6.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.051
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46776
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.905
_diffrn_reflns_theta_min         3.316
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  22.00   0.50    1.88    --  -49.87  58.00 158.00  170
  2  ω    -67.00 -12.00   0.50    7.50    --  -84.25  58.00 158.00  110
  3  ω    -42.00 -12.00   0.50    7.50    --  -84.25  45.00 -30.00   60
  4  ω    -42.00 -12.00   0.50    7.50    --  -84.25  45.00 -60.00   60
  5  ω   -121.00 -37.00   0.50    1.88    --  -49.87 -58.00  17.00  168
  6  ω   -121.00 -37.00   0.50    1.88    --  -49.87 -57.00 -60.00  168
  7  ω    -21.00  63.00   0.50    1.88    --   49.87 -58.00  17.00  168
  8  ω     34.00  79.00   0.50    7.50    --  105.75 -58.00  17.00   90
  9  ω     34.00 127.00   0.50    7.50    --  105.75 -77.00 120.00  186
 10  ω     34.00 109.00   0.50    7.50    --  105.75 -94.00  30.00  150
 11  ω     34.00 109.00   0.50    7.50    --  105.75 -94.00 -60.00  150
 12  ω     31.00  95.00   0.50    1.88    --   49.87-125.00-180.00  128
 13  ω     34.00  87.00   0.50    7.50    --  105.75 -61.00-120.00  106
 14  ω     34.00  87.00   0.50    7.50    --  105.75 -61.00-150.00  106
 15  ω     98.00 164.00   0.50    7.50    --  105.75  15.00 -90.00  132
 16  ω     98.00 178.00   0.50    7.50    --  105.75  30.00-150.00  160
 17  ω     98.00 164.00   0.50    7.50    --  105.75  15.00-180.00  132
 18  ω     98.00 164.00   0.50    7.50    --  105.75  15.00 -60.00  132
 19  ω     92.00 178.00   0.50    7.50    --  105.75  61.00  90.00  172
 20  ω     93.00 178.00   0.50    7.50    --  105.75  58.00 158.00  170
 21  ω     37.00 121.00   0.50    1.88    --   49.87  58.00 158.00  168
 22  ω     29.00 121.00   0.50    1.88    --   49.87  77.00  60.00  184
 23  ω     29.00  64.00   0.50    1.88    --   49.87  77.00-150.00   70
 24  ω    -22.00   5.00   0.50    1.88    --   49.87 -19.00-150.00   54
 25  ω     34.00  87.00   0.50    7.50    --  105.75 -61.00-180.00  106
 26  ω     34.00 127.00   0.50    7.50    --  105.75 -77.00   0.00  186
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0039723000
_diffrn_orient_matrix_UB_12      -0.0024820000
_diffrn_orient_matrix_UB_13      0.0732836000
_diffrn_orient_matrix_UB_21      0.0571956000
_diffrn_orient_matrix_UB_22      -0.0610327000
_diffrn_orient_matrix_UB_23      0.0098668000
_diffrn_orient_matrix_UB_31      0.0553097000
_diffrn_orient_matrix_UB_32      0.0633029000
_diffrn_orient_matrix_UB_33      0.0124170000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7010
_reflns_number_total             7578
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7578
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²+11.0091P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.0991
_refine_special_details          
;
Reflection contributions from highly disordered solvent
(likely acetonitrile) were fixed and added to the
calculated structure factors using the SQUEEZE routine of
program Platon (Spek, 2015), which determined there to be
395 electrons in 1736 Å³ treated this way. Because the
exact identity and amount of solvent were unknown, no
solvent was included in the atom list or molecular formula.
Thus all calculated quantities that derive from the molecular
formula (e.g., F(000), density, molecular weight, etc.) are
known to be incorrect.

In the asymmetric unit, one tBu group (C17-C20) and one methoxy
ligand (O10-C28) are modeled as disordered over two positions
each (0.560(5):0.440(5) and 0.59(4):0.41(4), respectively).
Analogous bond lengths and angles between the two
positions of the disordered species were restrained to be
similar. Anisotropic displacement parameters for proximal
atoms were restrained to be similar and restrained toward
the expected motion relative to bond direction.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C17 \\sim C6-C17'
 with sigma of 0.01
 C17-C18 \\sim C17-C20 \\sim C17-C19 \\sim C17'-C18' \\sim C17'-C20' \\sim
C17'-C19'
 with sigma of 0.01
 C18-C20 \\sim C20-C19 \\sim C19-C18 \\sim C18'-C20' \\sim C20'-C19' \\sim
C19'-C18'
 with sigma of 0.02
 O10-C28 \\sim O10-C28'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.2A
4. Rigid body (RIGU) restrains
 C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17', C18', C19', C20'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C28'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C17')=Sof(C18')=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19')=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(2)
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C11(H11), C13(H13)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C),
 C18'(H18D,H18E,H18F), C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F), C28'(H28D,
 H28E,H28F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.250000 0.40472(2) 0.500000 0.01599(9) Uani 1 2 d S T P C .
V2 V 0.16329(2) 0.52334(2) 0.40072(2) 0.02215(9) Uani 1 1 d . . . . .
V3 V 0.16415(2) 0.52396(2) 0.55771(2) 0.02324(9) Uani 1 1 d . . . . .
V4 V 0.250000 0.65106(3) 0.500000 0.02701(11) Uani 1 2 d S T P C .
O2 O 0.10466(8) 0.52207(8) 0.33372(7) 0.0330(3) Uani 1 1 d . . . . .
O3 O 0.10746(8) 0.52652(8) 0.59822(8) 0.0344(3) Uani 1 1 d . . . . .
O4 O 0.250000 0.74162(12) 0.500000 0.0394(5) Uani 1 2 d S T P . .
O5 O 0.17910(6) 0.41029(7) 0.41787(6) 0.0189(2) Uani 1 1 d . . . . .
O6 O 0.17825(6) 0.41061(7) 0.54705(6) 0.0196(2) Uani 1 1 d . . . . .
O7 O 0.10662(6) 0.52539(7) 0.46562(7) 0.0249(3) Uani 1 1 d . . . . .
O8 O 0.25079(7) 0.52379(7) 0.63059(6) 0.0256(3) Uani 1 1 d . . . . .
O9 O 0.17873(7) 0.63627(7) 0.42042(7) 0.0290(3) Uani 1 1 d . . . . .
O10 O 0.18210(7) 0.63670(8) 0.54822(7) 0.0306(3) Uani 1 1 d D . . . .
O11 O 0.250000 0.52276(9) 0.500000 0.0204(4) Uani 1 2 d S T P . .
N1 N 0.250000 0.28454(12) 0.500000 0.0211(4) Uani 1 2 d S TU P . .
C1 C 0.250000 0.21931(16) 0.500000 0.0269(5) Uani 1 2 d S TU P C .
C2 C 0.250000 0.1365(2) 0.500000 0.0619(11) Uani 1 2 d S T P . .
H2A H 0.291831 0.118213 0.529251 0.093 Uiso 0.5 1 calc R U P A -1
H2B H 0.247260 0.118213 0.456841 0.093 Uiso 0.5 1 calc R U P A -1
H2C H 0.210909 0.118213 0.513909 0.093 Uiso 0.5 1 calc R U P A -1
C3 C 0.15262(9) 0.34360(10) 0.38716(8) 0.0203(3) Uani 1 1 d . . . . .
C4 C 0.18660(10) 0.30797(10) 0.34514(8) 0.0232(4) Uani 1 1 d . . . . .
C5 C 0.16130(11) 0.23806(11) 0.31825(9) 0.0280(4) Uani 1 1 d . . . . .
H5 H 0.183200 0.214223 0.289950 0.034 Uiso 1 1 calc R U . . .
C6 C 0.10438(11) 0.20214(11) 0.33196(9) 0.0298(4) Uani 1 1 d D . . . .
C7 C 0.07325(10) 0.23885(11) 0.37503(9) 0.0270(4) Uani 1 1 d . . . . .
H7 H 0.035561 0.215732 0.385242 0.032 Uiso 1 1 calc R U . . .
C8 C 0.09640(9) 0.30908(10) 0.40354(8) 0.0228(4) Uani 1 1 d . . . . .
C9 C 0.15005(9) 0.34499(10) 0.56479(9) 0.0211(3) Uani 1 1 d . . . . .
C10 C 0.09312(9) 0.31130(10) 0.52091(9) 0.0236(4) Uani 1 1 d . . . . .
C11 C 0.06768(10) 0.24291(11) 0.53901(10) 0.0275(4) Uani 1 1 d . . . . .
H11 H 0.029187 0.220853 0.510765 0.033 Uiso 1 1 calc R U . . .
C12 C 0.09752(11) 0.20630(11) 0.59762(10) 0.0287(4) Uani 1 1 d . . . . .
C13 C 0.15534(11) 0.24039(11) 0.63865(9) 0.0275(4) Uani 1 1 d . . . . .
H13 H 0.176660 0.216410 0.677692 0.033 Uiso 1 1 calc R U . . .
C14 C 0.18254(10) 0.30933(10) 0.62333(9) 0.0235(4) Uani 1 1 d . . . . .
C15 C 0.06335(9) 0.34446(11) 0.45358(9) 0.0241(4) Uani 1 1 d . . . . .
H15A H 0.070890 0.399206 0.454917 0.029 Uiso 1 1 calc R U . . .
H15B H 0.013871 0.335479 0.440570 0.029 Uiso 1 1 calc R U . . .
C16 C 0.24848(10) 0.34191(10) 0.66795(8) 0.0233(4) Uani 1 1 d . . . . .
H16A H 0.248973 0.396807 0.662063 0.028 Uiso 1 1 calc R U . . .
H16B H 0.248541 0.332040 0.712851 0.028 Uiso 1 1 calc R U . . .
C21 C 0.06586(13) 0.13131(13) 0.61460(11) 0.0382(5) Uani 1 1 d . . . . .
C22 C 0.06326(17) 0.07281(14) 0.56075(13) 0.0537(7) Uani 1 1 d . . . . .
H22A H 0.042705 0.026422 0.570871 0.081 Uiso 1 1 calc R U . . .
H22B H 0.109334 0.062540 0.557425 0.081 Uiso 1 1 calc R U . . .
H22C H 0.036103 0.092711 0.520094 0.081 Uiso 1 1 calc R U . . .
C23 C -0.00807(15) 0.14770(17) 0.61946(15) 0.0573(7) Uani 1 1 d . . . . .
H23A H -0.028400 0.101483 0.630241 0.086 Uiso 1 1 calc R U . . .
H23B H -0.035241 0.166690 0.578460 0.086 Uiso 1 1 calc R U . . .
H23C H -0.006760 0.185170 0.652707 0.086 Uiso 1 1 calc R U . . .
C24 C 0.10729(16) 0.09778(15) 0.67914(13) 0.0524(7) Uani 1 1 d . . . . .
H24A H 0.153951 0.088530 0.677077 0.079 Uiso 1 1 calc R U . . .
H24B H 0.086580 0.050594 0.687252 0.079 Uiso 1 1 calc R U . . .
H24C H 0.107408 0.133111 0.713678 0.079 Uiso 1 1 calc R U . . .
C25 C 0.04383(10) 0.56803(12) 0.44870(12) 0.0360(5) Uani 1 1 d . . . . .
H25A H 0.013832 0.547237 0.409773 0.054 Uiso 1 1 calc R U . . .
H25B H 0.053864 0.620384 0.441394 0.054 Uiso 1 1 calc R U . . .
H25C H 0.021507 0.565158 0.483534 0.054 Uiso 1 1 calc R U . . .
C26 C 0.24937(13) 0.55596(14) 0.69162(11) 0.0394(5) Uani 1 1 d . . . . .
H26A H 0.216088 0.529244 0.708794 0.059 Uiso 1 1 calc R U . . .
H26B H 0.236759 0.608874 0.685896 0.059 Uiso 1 1 calc R U . . .
H26C H 0.294290 0.551484 0.721386 0.059 Uiso 1 1 calc R U . . .
C27 C 0.15963(14) 0.69392(13) 0.37210(13) 0.0480(6) Uani 1 1 d . . . . .
H27A H 0.120185 0.677219 0.338812 0.072 Uiso 1 1 calc R U . . .
H27B H 0.197505 0.703569 0.353223 0.072 Uiso 1 1 calc R U . . .
H27C H 0.148294 0.739920 0.391624 0.072 Uiso 1 1 calc R U . . .
C17 C 0.0747(3) 0.1265(3) 0.2998(3) 0.0396(19) Uani 0.560(5) 1 d D U P B 1
C18 C 0.1330(3) 0.0670(3) 0.3179(4) 0.078(2) Uani 0.560(5) 1 d D . P B 1
H18A H 0.171371 0.083398 0.302089 0.117 Uiso 0.560(5) 1 calc R U P B 1
H18B H 0.116377 0.018747 0.298612 0.117 Uiso 0.560(5) 1 calc R U P B 1
H18C H 0.147491 0.061555 0.364407 0.117 Uiso 0.560(5) 1 calc R U P B 1
C19 C 0.0534(3) 0.1349(3) 0.22575(19) 0.0551(15) Uani 0.560(5) 1 d D . P B 1
H19A H 0.018082 0.173238 0.213699 0.083 Uiso 0.560(5) 1 calc R U P B 1
H19B H 0.035896 0.087097 0.206276 0.083 Uiso 0.560(5) 1 calc R U P B 1
H19C H 0.092807 0.149818 0.210772 0.083 Uiso 0.560(5) 1 calc R U P B 1
C20 C 0.0125(3) 0.0959(3) 0.3210(3) 0.066(2) Uani 0.560(5) 1 d D . P B 1
H20A H -0.000793 0.047196 0.300849 0.099 Uiso 0.560(5) 1 calc R U P B 1
H20B H -0.025387 0.130988 0.307957 0.099 Uiso 0.560(5) 1 calc R U P B 1
H20C H 0.024481 0.090127 0.367460 0.099 Uiso 0.560(5) 1 calc R U P B 1
C28 C 0.1501(11) 0.6956(10) 0.5759(11) 0.046(3) Uani 0.41(4) 1 d D U P C 1
H28A H 0.118164 0.673546 0.597528 0.069 Uiso 0.41(4) 1 calc R U P C 1
H28B H 0.125670 0.729282 0.542069 0.069 Uiso 0.41(4) 1 calc R U P C 1
H28C H 0.184755 0.723870 0.606703 0.069 Uiso 0.41(4) 1 calc R U P C 1
C17' C 0.0809(4) 0.1253(3) 0.3000(3) 0.037(2) Uani 0.440(5) 1 d D U P B 2
C18' C 0.0101(4) 0.1425(4) 0.2552(4) 0.074(3) Uani 0.440(5) 1 d D . P B 2
H18D H -0.019683 0.161703 0.280444 0.112 Uiso 0.440(5) 1 calc R U P B 2
H18E H -0.009267 0.096645 0.233236 0.112 Uiso 0.440(5) 1 calc R U P B 2
H18F H 0.014631 0.180125 0.223730 0.112 Uiso 0.440(5) 1 calc R U P B 2
C19' C 0.0751(4) 0.0682(3) 0.3525(3) 0.0454(16) Uani 0.440(5) 1 d D . P B 2
H19D H 0.056476 0.021071 0.332414 0.068 Uiso 0.440(5) 1 calc R U P B 2
H19E H 0.045117 0.088466 0.377057 0.068 Uiso 0.440(5) 1 calc R U P B 2
H19F H 0.120115 0.059282 0.380963 0.068 Uiso 0.440(5) 1 calc R U P B 2
C20' C 0.1279(4) 0.0918(3) 0.2608(4) 0.061(2) Uani 0.440(5) 1 d D . P B 2
H20D H 0.126621 0.123731 0.223815 0.092 Uiso 0.440(5) 1 calc R U P B 2
H20E H 0.112180 0.041451 0.246180 0.092 Uiso 0.440(5) 1 calc R U P B 2
H20F H 0.174393 0.089050 0.287687 0.092 Uiso 0.440(5) 1 calc R U P B 2
C28' C 0.1359(7) 0.6958(6) 0.5546(12) 0.058(4) Uani 0.59(4) 1 d D U P C 2
H28D H 0.098693 0.698363 0.515717 0.086 Uiso 0.59(4) 1 calc R U P C 2
H28E H 0.160137 0.743612 0.561031 0.086 Uiso 0.59(4) 1 calc R U P C 2
H28F H 0.117637 0.685373 0.591203 0.086 Uiso 0.59(4) 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O5 1.9479(12) . ?
V1 O5 1.9479(12) 2_556 ?
V1 O6 1.9534(11) . ?
V1 O6 1.9534(11) 2_556 ?
V1 O11 2.0676(17) . ?
V1 N1 2.105(2) . ?
V2 O2 1.5950(14) . ?
V2 O5 2.0235(12) . ?
V2 O7 1.9999(14) . ?
V2 O8 1.9981(14) 2_556 ?
V2 O9 2.0291(14) . ?
V2 O11 2.3618(3) . ?
V3 O3 1.5926(14) . ?
V3 O6 2.0263(12) . ?
V3 O7 1.9993(14) . ?
V3 O8 2.0055(14) . ?
V3 O10 2.0265(14) . ?
V3 O11 2.3553(3) . ?
V4 O4 1.586(2) . ?
V4 O9 1.9287(14) 2_556 ?
V4 O9 1.9286(14) . ?
V4 O10 1.9186(14) 2_556 ?
V4 O10 1.9186(14) . ?
V4 O11 2.2472(17) . ?
O5 C3 1.376(2) . ?
O6 C9 1.375(2) . ?
O7 C25 1.426(2) . ?
O8 C26 1.422(2) . ?
O9 C27 1.421(3) . ?
O10 C28 1.420(7) . ?
O10 C28' 1.417(5) . ?
N1 C1 1.143(4) . ?
C1 C2 1.451(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.401(3) . ?
C3 C8 1.399(2) . ?
C4 C5 1.390(3) . ?
C4 C16 1.519(3) 2_556 ?
C5 H5 0.9300 . ?
C5 C6 1.397(3) . ?
C6 C7 1.391(3) . ?
C6 C17 1.538(5) . ?
C6 C17' 1.527(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.396(3) . ?
C8 C15 1.522(3) . ?
C9 C10 1.403(3) . ?
C9 C14 1.395(3) . ?
C10 C11 1.394(3) . ?
C10 C15 1.517(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.392(3) . ?
C12 C13 1.391(3) . ?
C12 C21 1.541(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.397(3) . ?
C14 C16 1.524(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C21 C22 1.527(3) . ?
C21 C23 1.537(4) . ?
C21 C24 1.526(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C17 C18 1.537(6) . ?
C17 C19 1.529(5) . ?
C17 C20 1.527(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C17' C18' 1.519(6) . ?
C17' C19' 1.524(6) . ?
C17' C20' 1.526(6) . ?
C18' H18D 0.9600 . ?
C18' H18E 0.9600 . ?
C18' H18F 0.9600 . ?
C19' H19D 0.9600 . ?
C19' H19E 0.9600 . ?
C19' H19F 0.9600 . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?
C28' H28D 0.9600 . ?
C28' H28E 0.9600 . ?
C28' H28F 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
O5 V1 O5 174.26(7) . 2_556 ?
O5 V1 O6 89.69(5) 2_556 2_556 ?
O5 V1 O6 89.69(5) . . ?
O5 V1 O6 90.00(5) . 2_556 ?
O5 V1 O6 90.01(5) 2_556 . ?
O5 V1 O11 87.13(4) 2_556 . ?
O5 V1 O11 87.13(4) . . ?
O5 V1 N1 92.87(4) 2_556 . ?
O5 V1 N1 92.87(4) . . ?
O6 V1 O6 173.94(7) 2_556 . ?
O6 V1 O11 86.97(4) . . ?
O6 V1 O11 86.97(4) 2_556 . ?
O6 V1 N1 93.03(4) 2_556 . ?
O6 V1 N1 93.03(4) . . ?
O11 V1 N1 180.0 . . ?
O2 V2 O5 101.08(6) . . ?
O2 V2 O7 101.48(7) . . ?
O2 V2 O8 101.57(7) . 2_556 ?
O2 V2 O9 103.63(7) . . ?
O2 V2 O11 178.96(7) . . ?
O5 V2 O9 155.28(6) . . ?
O5 V2 O11 77.88(5) . . ?
O7 V2 O5 89.06(5) . . ?
O7 V2 O9 85.60(6) . . ?
O7 V2 O11 78.48(4) . . ?
O8 V2 O5 87.47(5) 2_556 . ?
O8 V2 O7 156.93(6) 2_556 . ?
O8 V2 O9 88.08(6) 2_556 . ?
O8 V2 O11 78.50(4) 2_556 . ?
O9 V2 O11 77.41(6) . . ?
O3 V3 O6 103.14(6) . . ?
O3 V3 O7 102.63(7) . . ?
O3 V3 O8 100.19(7) . . ?
O3 V3 O10 101.29(7) . . ?
O3 V3 O11 178.30(6) . . ?
O6 V3 O10 155.54(5) . . ?
O6 V3 O11 77.97(5) . . ?
O7 V3 O6 87.96(5) . . ?
O7 V3 O8 157.14(6) . . ?
O7 V3 O10 87.84(6) . . ?
O7 V3 O11 78.65(4) . . ?
O8 V3 O6 88.13(5) . . ?
O8 V3 O10 86.46(6) . . ?
O8 V3 O11 78.51(4) . . ?
O10 V3 O11 77.58(6) . . ?
O4 V4 O9 97.72(4) . 2_556 ?
O4 V4 O9 97.72(4) . . ?
O4 V4 O10 97.53(4) . 2_556 ?
O4 V4 O10 97.53(4) . . ?
O4 V4 O11 180.0 . . ?
O9 V4 O9 164.56(8) . 2_556 ?
O9 V4 O11 82.28(4) . . ?
O9 V4 O11 82.28(4) 2_556 . ?
O10 V4 O9 89.17(6) 2_556 2_556 ?
O10 V4 O9 89.17(6) . . ?
O10 V4 O9 88.81(6) 2_556 . ?
O10 V4 O9 88.81(6) . 2_556 ?
O10 V4 O10 164.93(8) 2_556 . ?
O10 V4 O11 82.47(4) . . ?
O10 V4 O11 82.47(4) 2_556 . ?
V1 O5 V2 104.74(5) . . ?
C3 O5 V1 119.03(10) . . ?
C3 O5 V2 136.23(10) . . ?
V1 O6 V3 104.54(5) . . ?
C9 O6 V1 120.29(10) . . ?
C9 O6 V3 135.17(10) . . ?
V3 O7 V2 112.93(6) . . ?
C25 O7 V2 117.08(13) . . ?
C25 O7 V3 120.07(13) . . ?
V2 O8 V3 112.93(6) 2_556 . ?
C26 O8 V2 121.83(13) . 2_556 ?
C26 O8 V3 119.19(13) . . ?
V4 O9 V2 110.54(6) . . ?
C27 O9 V2 123.05(14) . . ?
C27 O9 V4 122.62(14) . . ?
V4 O10 V3 110.44(6) . . ?
C28 O10 V3 123.8(10) . . ?
C28 O10 V4 125.7(10) . . ?
C28' O10 V3 124.4(6) . . ?
C28' O10 V4 121.6(8) . . ?
V1 O11 V2 90.24(4) . . ?
V1 O11 V2 90.24(4) . 2_556 ?
V1 O11 V3 90.51(4) . 2_556 ?
V1 O11 V3 90.51(4) . . ?
V1 O11 V4 180.0 . . ?
V2 O11 V2 179.51(8) . 2_556 ?
V3 O11 V2 90.061(11) . 2_556 ?
V3 O11 V2 89.933(11) . . ?
V3 O11 V2 90.064(11) 2_556 . ?
V3 O11 V2 89.933(11) 2_556 2_556 ?
V3 O11 V3 178.98(8) . 2_556 ?
V4 O11 V2 89.76(4) . . ?
V4 O11 V2 89.76(4) . 2_556 ?
V4 O11 V3 89.49(4) . . ?
V4 O11 V3 89.49(4) . 2_556 ?
C1 N1 V1 180.0 . . ?
N1 C1 C2 180.0 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O5 C3 C4 119.32(16) . . ?
O5 C3 C8 119.02(16) . . ?
C8 C3 C4 121.36(16) . . ?
C3 C4 C16 121.44(16) . 2_556 ?
C5 C4 C3 117.98(17) . . ?
C5 C4 C16 120.50(17) . 2_556 ?
C4 C5 H5 118.6 . . ?
C4 C5 C6 122.76(18) . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C17 122.5(3) . . ?
C5 C6 C17' 118.6(3) . . ?
C7 C6 C5 117.21(17) . . ?
C7 C6 C17 120.2(3) . . ?
C7 C6 C17' 124.2(3) . . ?
C6 C7 H7 118.7 . . ?
C6 C7 C8 122.55(18) . . ?
C8 C7 H7 118.7 . . ?
C3 C8 C15 121.39(16) . . ?
C7 C8 C3 118.10(17) . . ?
C7 C8 C15 120.44(16) . . ?
O6 C9 C10 119.31(16) . . ?
O6 C9 C14 119.29(16) . . ?
C14 C9 C10 121.12(16) . . ?
C9 C10 C15 121.35(16) . . ?
C11 C10 C9 118.01(17) . . ?
C11 C10 C15 120.46(17) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.70(18) . . ?
C12 C11 H11 118.7 . . ?
C11 C12 C21 119.67(18) . . ?
C13 C12 C11 117.32(17) . . ?
C13 C12 C21 123.01(19) . . ?
C12 C13 H13 118.8 . . ?
C12 C13 C14 122.41(18) . . ?
C14 C13 H13 118.8 . . ?
C9 C14 C13 118.37(17) . . ?
C9 C14 C16 121.17(16) . . ?
C13 C14 C16 120.37(17) . . ?
C8 C15 H15A 109.3 . . ?
C8 C15 H15B 109.3 . . ?
C10 C15 C8 111.59(15) . . ?
C10 C15 H15A 109.3 . . ?
C10 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C4 C16 C14 112.59(14) 2_556 . ?
C4 C16 H16A 109.1 2_556 . ?
C4 C16 H16B 109.1 2_556 . ?
C14 C16 H16A 109.1 . . ?
C14 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C22 C21 C12 109.43(17) . . ?
C22 C21 C23 109.2(2) . . ?
C23 C21 C12 108.5(2) . . ?
C24 C21 C12 112.20(19) . . ?
C24 C21 C22 108.8(2) . . ?
C24 C21 C23 108.7(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O7 C25 H25A 109.5 . . ?
O7 C25 H25B 109.5 . . ?
O7 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O8 C26 H26A 109.5 . . ?
O8 C26 H26B 109.5 . . ?
O8 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O9 C27 H27A 109.5 . . ?
O9 C27 H27B 109.5 . . ?
O9 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C18 C17 C6 107.0(4) . . ?
C19 C17 C6 110.3(4) . . ?
C19 C17 C18 108.4(5) . . ?
C20 C17 C6 115.0(4) . . ?
C20 C17 C18 108.2(5) . . ?
C20 C17 C19 107.8(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O10 C28 H28A 109.5 . . ?
O10 C28 H28B 109.5 . . ?
O10 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C18' C17' C6 103.5(4) . . ?
C18' C17' C19' 110.8(6) . . ?
C18' C17' C20' 109.9(6) . . ?
C19' C17' C6 108.9(4) . . ?
C19' C17' C20' 108.8(5) . . ?
C20' C17' C6 114.8(5) . . ?
C17' C18' H18D 109.5 . . ?
C17' C18' H18E 109.5 . . ?
C17' C18' H18F 109.5 . . ?
H18D C18' H18E 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
C17' C19' H19D 109.5 . . ?
C17' C19' H19E 109.5 . . ?
C17' C19' H19F 109.5 . . ?
H19D C19' H19E 109.5 . . ?
H19D C19' H19F 109.5 . . ?
H19E C19' H19F 109.5 . . ?
C17' C20' H20D 109.5 . . ?
C17' C20' H20E 109.5 . . ?
C17' C20' H20F 109.5 . . ?
H20D C20' H20E 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
O10 C28' H28D 109.5 . . ?
O10 C28' H28E 109.5 . . ?
O10 C28' H28F 109.5 . . ?
H28D C28' H28E 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O5 C3 C4 -86.28(17) . . . . ?
V1 O5 C3 C8 87.50(17) . . . . ?
V1 O6 C9 C10 -87.61(17) . . . . ?
V1 O6 C9 C14 86.31(17) . . . . ?
V2 O5 C3 C4 94.41(19) . . . . ?
V2 O5 C3 C8 -91.81(19) . . . . ?
V3 O6 C9 C10 92.50(19) . . . . ?
V3 O6 C9 C14 -93.58(19) . . . . ?
O5 C3 C4 C5 175.75(15) . . . . ?
O5 C3 C4 C16 -0.8(2) . . . 2_556 ?
O5 C3 C8 C7 -175.80(15) . . . . ?
O5 C3 C8 C15 1.1(2) . . . . ?
O6 C9 C10 C11 177.05(16) . . . . ?
O6 C9 C10 C15 1.8(2) . . . . ?
O6 C9 C14 C13 -176.34(15) . . . . ?
O6 C9 C14 C16 0.2(2) . . . . ?
C3 C4 C5 C6 -0.7(3) . . . . ?
C3 C8 C15 C10 -94.6(2) . . . . ?
C4 C3 C8 C7 -2.2(3) . . . . ?
C4 C3 C8 C15 174.71(16) . . . . ?
C4 C5 C6 C7 -0.7(3) . . . . ?
C4 C5 C6 C17 177.3(3) . . . . ?
C4 C5 C6 C17' -179.8(3) . . . . ?
C5 C6 C7 C8 0.7(3) . . . . ?
C5 C6 C17 C18 59.7(5) . . . . ?
C5 C6 C17 C19 -58.0(5) . . . . ?
C5 C6 C17 C20 179.9(4) . . . . ?
C5 C6 C17' C18' -114.0(5) . . . . ?
C5 C6 C17' C19' 128.1(4) . . . . ?
C5 C6 C17' C20' 5.9(6) . . . . ?
C6 C7 C8 C3 0.7(3) . . . . ?
C6 C7 C8 C15 -176.18(17) . . . . ?
C7 C6 C17 C18 -122.3(4) . . . . ?
C7 C6 C17 C19 120.0(4) . . . . ?
C7 C6 C17 C20 -2.1(6) . . . . ?
C7 C6 C17' C18' 67.0(6) . . . . ?
C7 C6 C17' C19' -50.9(6) . . . . ?
C7 C6 C17' C20' -173.2(4) . . . . ?
C7 C8 C15 C10 82.2(2) . . . . ?
C8 C3 C4 C5 2.1(3) . . . . ?
C8 C3 C4 C16 -174.44(16) . . . 2_556 ?
C9 C10 C11 C12 -1.7(3) . . . . ?
C9 C10 C15 C8 91.4(2) . . . . ?
C9 C14 C16 C4 -92.7(2) . . . 2_556 ?
C10 C9 C14 C13 -2.5(3) . . . . ?
C10 C9 C14 C16 173.99(16) . . . . ?
C10 C11 C12 C13 -0.5(3) . . . . ?
C10 C11 C12 C21 179.24(18) . . . . ?
C11 C10 C15 C8 -83.7(2) . . . . ?
C11 C12 C13 C14 1.2(3) . . . . ?
C11 C12 C21 C22 56.6(3) . . . . ?
C11 C12 C21 C23 -62.4(3) . . . . ?
C11 C12 C21 C24 177.4(2) . . . . ?
C12 C13 C14 C9 0.2(3) . . . . ?
C12 C13 C14 C16 -176.32(17) . . . . ?
C13 C12 C21 C22 -123.7(2) . . . . ?
C13 C12 C21 C23 117.3(2) . . . . ?
C13 C12 C21 C24 -2.9(3) . . . . ?
C13 C14 C16 C4 83.8(2) . . . 2_556 ?
C14 C9 C10 C11 3.2(3) . . . . ?
C14 C9 C10 C15 -172.02(16) . . . . ?
C15 C10 C11 C12 173.58(17) . . . . ?
C16 C4 C5 C6 175.94(17) 2_556 . . . ?
C21 C12 C13 C14 -178.46(19) . . . . ?
C17 C6 C7 C8 -177.4(3) . . . . ?
C17' C6 C7 C8 179.7(3) . . . . ?

_olex2_submission_original_sample_id matrm23
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.905
_oxdiff_exptl_absorpt_empirical_full_min 0.538
####################################################################### 
# 
# 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_matrm24
_database_code_depnum_ccdc_archive 'CCDC 2145268'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2022-01-28 deposited with the CCDC.	2022-04-29 downloaded from the CCDC.
;

_vrf_PLAT301_matrm24             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 10% 
RESPONSE: One tBu group in the asymmetric unit is modeled as
disordered over two positions (0.875(3):0.125(3)).
;

_vrf_PLAT860_matrm24             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 31 
RESPONSE: Analogous bond lengths and angles in the tBu group
disorder were restrained to be similar. Anisotropic displacement
parameters for proximal and opposing atoms were constrained to
be equivalent.
;

_audit_creation_date             2020-12-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H76 O19 V6, 5(C2 H3 N)'
_chemical_formula_sum            'C62 H91 N5 O19 V6'
_chemical_formula_weight         1516.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   21.2605(2)
_cell_length_b                   17.61780(10)
_cell_length_c                   20.1094(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.8300(10)
_cell_angle_gamma                90
_cell_volume                     7281.34(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31409
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.4470
_cell_measurement_theta_min      3.3250
_shelx_estimated_absorpt_T_max   0.569
_shelx_estimated_absorpt_T_min   0.255
_exptl_absorpt_coefficient_mu    6.772
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.094
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46057
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.870
_diffrn_reflns_theta_min         3.304
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00  22.00   0.50    0.48    --  -49.75  96.00-167.00  202
  2  ω    -30.00  22.00   0.50    0.48    --  -49.75  38.00 -60.00  104
  3  ω    -42.00 -12.00   0.50    1.94    --  -84.25  45.00  60.00   60
  4  ω    -83.00 -12.00   0.50    1.94    --  -84.25  96.00-167.00  142
  5  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00 -90.00   56
  6  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00-150.00   56
  7  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00-180.00   56
  8  ω     34.00 109.00   0.50    1.94    --  105.75 -94.00 -90.00  150
  9  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00-120.00  106
 10  ω     34.00 127.00   0.50    1.94    --  105.75 -77.00-120.00  186
 11  ω     98.00 164.00   0.50    1.94    --  105.75  15.00   0.00  132
 12  ω     97.00 178.00   0.50    1.94    --  105.75  45.00  60.00  162
 13  ω     98.00 164.00   0.50    1.94    --  105.75  15.00 -30.00  132
 14  ω    103.00 178.00   0.50    1.94    --  105.75  96.00-167.00  150
 15  ω     92.00 178.00   0.50    1.94    --  105.75 125.00 -30.00  172
 16  ω     98.00 139.00   0.50    1.94    --  105.75  15.00 120.00   82
 17  ω     34.00 109.00   0.50    1.94    --  105.75 -96.00  83.00  150
 18  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00  90.00  106
 19  ω     34.00 109.00   0.50    1.94    --  105.75 -94.00 120.00  150
 20  ω     34.00 127.00   0.50    1.94    --  105.75 -77.00 120.00  186
 21  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00 120.00  106
 22  ω     34.00 109.00   0.50    1.94    --  105.75 -94.00   0.00  150
 23  ω     34.00  87.00   0.50    1.94    --  105.75 -61.00 -30.00  106
 24  ω    -10.00  80.00   0.50    0.48    --   49.75 -96.00  83.00  180
 25  ω    -23.00   5.00   0.50    0.48    --   49.75 -19.00 120.00   56
 26  ω   -121.00 -70.00   0.50    0.48    --  -49.75-125.00-120.00  102
 27  ω   -156.00 -81.00   0.50    1.94    --  -84.25 -96.00  83.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0121332000
_diffrn_orient_matrix_UB_12      0.0608240000
_diffrn_orient_matrix_UB_13      -0.0503689000
_diffrn_orient_matrix_UB_21      -0.0256262000
_diffrn_orient_matrix_UB_22      -0.0547193000
_diffrn_orient_matrix_UB_23      -0.0606273000
_diffrn_orient_matrix_UB_31      -0.0693942000
_diffrn_orient_matrix_UB_32      0.0308415000
_diffrn_orient_matrix_UB_33      -0.0083901000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7171
_reflns_number_total             7666
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7666
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.078
_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)+(0.0855P)²+8.4034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1302
_refine_special_details          
;
One tBu group in the asymmetric unit is modeled as disordered
over two positions (0.875(3):0.125(3)). Analogous bond lengths
and angles in the tBu group disorder were restrained to be
similar. Anisotropic displacement parameters for proximal and
opposing atoms were constrained to be equivalent.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C15 \\sim C4-C15'
 with sigma of 0.02
 C15-C16 \\sim C15-C17 \\sim C15-C18 \\sim C15'-C16' \\sim C15'-C17' \\sim
C15'-C18'
 with sigma of 0.02
 C16-C17 \\sim C17-C18 \\sim C18-C16 \\sim C16'-C17' \\sim C17'-C18' \\sim
C18'-C16'
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(C15')
Uanis(C16) = Uanis(C16')
Uanis(C17) = Uanis(C17')
Uanis(C18) = Uanis(C18')
4. Others
 Sof(C15')=Sof(C16')=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17')=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C18')=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
 Fixed Sof: H32A(0.5) H32B(0.5) H32C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C16'(H16D,H16E,H16F),
 C17'(H17D,H17E,H17F), C18'(H18D,H18E,H18F), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.750000 0.64727(2) 0.500000 0.01273(11) Uani 1 2 d S T P . .
V2 V 0.65120(2) 0.77055(2) 0.41457(2) 0.01695(11) Uani 1 1 d . . . . .
V3 V 0.69276(2) 0.77126(2) 0.58561(2) 0.01711(11) Uani 1 1 d . . . . .
V4 V 0.750000 0.89776(3) 0.500000 0.01972(12) Uani 1 2 d S T P . .
O1 O 0.750000 0.55602(11) 0.500000 0.0177(4) Uani 1 2 d S T P . .
O2 O 0.58434(8) 0.76665(8) 0.35674(8) 0.0265(3) Uani 1 1 d . . . . .
O3 O 0.65279(8) 0.77214(8) 0.64239(8) 0.0259(3) Uani 1 1 d . . . . .
O4 O 0.750000 0.98772(12) 0.500000 0.0285(5) Uani 1 2 d S T P . .
O5 O 0.66910(6) 0.65761(7) 0.43091(7) 0.0146(3) Uani 1 1 d . . . . .
O6 O 0.70421(6) 0.65819(7) 0.57095(7) 0.0149(3) Uani 1 1 d . . . . .
O7 O 0.61993(7) 0.77045(7) 0.49997(8) 0.0199(3) Uani 1 1 d . . . . .
O8 O 0.78448(7) 0.77267(7) 0.64265(7) 0.0195(3) Uani 1 1 d . . . . .
O9 O 0.67048(7) 0.88248(8) 0.42953(7) 0.0218(3) Uani 1 1 d . . . . .
O10 O 0.70201(7) 0.88251(8) 0.56771(7) 0.0221(3) Uani 1 1 d . . . . .
O11 O 0.750000 0.76807(9) 0.500000 0.0164(4) Uani 1 2 d S T P . .
C1 C 0.63724(8) 0.59128(10) 0.40415(9) 0.0157(3) Uani 1 1 d . . . . .
C2 C 0.65282(8) 0.55751(10) 0.34731(9) 0.0173(3) Uani 1 1 d . . . . .
C3 C 0.62398(9) 0.48827(11) 0.32419(10) 0.0195(4) Uani 1 1 d . . . . .
H3 H 0.633504 0.465476 0.286202 0.023 Uiso 1 1 calc R U . . .
C4 C 0.58112(9) 0.45177(11) 0.35617(11) 0.0215(4) Uani 1 1 d D . . . .
C5 C 0.56822(9) 0.48691(11) 0.41323(11) 0.0211(4) Uani 1 1 d . . . . .
H5 H 0.540185 0.463196 0.435419 0.025 Uiso 1 1 calc R U . . .
C6 C 0.59581(8) 0.55649(10) 0.43843(10) 0.0173(4) Uani 1 1 d . . . . .
C7 C 0.68620(9) 0.59298(10) 0.60038(10) 0.0164(3) Uani 1 1 d . . . . .
C8 C 0.62706(9) 0.55823(10) 0.56856(10) 0.0179(4) Uani 1 1 d . . . . .
C9 C 0.61143(9) 0.49073(11) 0.59728(10) 0.0204(4) Uani 1 1 d . . . . .
H9 H 0.572054 0.467181 0.576948 0.024 Uiso 1 1 calc R U . . .
C10 C 0.65255(10) 0.45731(11) 0.65519(11) 0.0219(4) Uani 1 1 d . . . . .
C11 C 0.71189(9) 0.49353(11) 0.68389(10) 0.0209(4) Uani 1 1 d . . . . .
H11 H 0.740237 0.471974 0.722261 0.025 Uiso 1 1 calc R U . . .
C12 C 0.73014(9) 0.56047(10) 0.65730(9) 0.0175(4) Uani 1 1 d . . . . .
C13 C 0.58257(8) 0.59049(11) 0.50302(10) 0.0182(4) Uani 1 1 d . . . . .
H13A H 0.537670 0.580693 0.503018 0.022 Uiso 1 1 calc R U . . .
H13B H 0.588455 0.645058 0.502429 0.022 Uiso 1 1 calc R U . . .
C14 C 0.79781(9) 0.59306(11) 0.68622(9) 0.0177(4) Uani 1 1 d . . . . .
H14A H 0.811171 0.584127 0.735432 0.021 Uiso 1 1 calc R U . . .
H14B H 0.796677 0.647484 0.678712 0.021 Uiso 1 1 calc R U . . .
C19 C 0.63584(11) 0.38356(12) 0.68758(12) 0.0283(4) Uani 1 1 d . . . . .
C20 C 0.57024(12) 0.35076(14) 0.64801(15) 0.0392(6) Uani 1 1 d . . . . .
H20A H 0.571189 0.340729 0.601350 0.059 Uiso 1 1 calc R U . . .
H20B H 0.536335 0.386604 0.648426 0.059 Uiso 1 1 calc R U . . .
H20C H 0.562075 0.304389 0.669431 0.059 Uiso 1 1 calc R U . . .
C21 C 0.63317(14) 0.40065(15) 0.76178(14) 0.0412(6) Uani 1 1 d . . . . .
H21A H 0.600165 0.437970 0.761328 0.062 Uiso 1 1 calc R U . . .
H21B H 0.674588 0.419693 0.787431 0.062 Uiso 1 1 calc R U . . .
H21C H 0.623091 0.354937 0.782912 0.062 Uiso 1 1 calc R U . . .
C22 C 0.68864(12) 0.32431(13) 0.68850(15) 0.0377(5) Uani 1 1 d . . . . .
H22A H 0.729728 0.342867 0.715474 0.056 Uiso 1 1 calc R U . . .
H22B H 0.691414 0.314847 0.642326 0.056 Uiso 1 1 calc R U . . .
H22C H 0.677918 0.278028 0.708291 0.056 Uiso 1 1 calc R U . . .
C23 C 0.55869(10) 0.80227(14) 0.50121(13) 0.0309(5) Uani 1 1 d . . . . .
H23A H 0.528679 0.796198 0.456896 0.046 Uiso 1 1 calc R U . . .
H23B H 0.563988 0.855301 0.512212 0.046 Uiso 1 1 calc R U . . .
H23C H 0.542103 0.776783 0.535360 0.046 Uiso 1 1 calc R U . . .
C24 C 0.80164(11) 0.81714(12) 0.70441(11) 0.0277(4) Uani 1 1 d . . . . .
H24A H 0.767438 0.814132 0.727563 0.042 Uiso 1 1 calc R U . . .
H24B H 0.807692 0.869076 0.692984 0.042 Uiso 1 1 calc R U . . .
H24C H 0.841273 0.797989 0.734021 0.042 Uiso 1 1 calc R U . . .
C25 C 0.62164(12) 0.94006(13) 0.41216(15) 0.0374(6) Uani 1 1 d . . . . .
H25A H 0.640061 0.985120 0.398017 0.056 Uiso 1 1 calc R U . . .
H25B H 0.605580 0.951229 0.451566 0.056 Uiso 1 1 calc R U . . .
H25C H 0.586482 0.922495 0.375246 0.056 Uiso 1 1 calc R U . . .
C26 C 0.68541(15) 0.94246(13) 0.60759(13) 0.0398(6) Uani 1 1 d . . . . .
H26A H 0.723384 0.957795 0.642199 0.060 Uiso 1 1 calc R U . . .
H26B H 0.652668 0.925194 0.629233 0.060 Uiso 1 1 calc R U . . .
H26C H 0.668983 0.984799 0.578219 0.060 Uiso 1 1 calc R U . . .
C15 C 0.54919(17) 0.37654(19) 0.3275(2) 0.0299(5) Uani 0.875(3) 1 d D . P A 1
C16 C 0.50403(17) 0.3926(2) 0.25656(19) 0.0543(9) Uani 0.875(3) 1 d D . P A 1
H16A H 0.485073 0.345959 0.236232 0.081 Uiso 0.875(3) 1 calc R U P A 1
H16B H 0.528487 0.415369 0.227713 0.081 Uiso 0.875(3) 1 calc R U P A 1
H16C H 0.470162 0.426713 0.261177 0.081 Uiso 0.875(3) 1 calc R U P A 1
C17 C 0.60149(14) 0.31979(15) 0.32099(19) 0.0405(7) Uani 0.875(3) 1 d D . P A 1
H17A H 0.581457 0.272233 0.304445 0.061 Uiso 0.875(3) 1 calc R U P A 1
H17B H 0.631390 0.312456 0.365192 0.061 Uiso 0.875(3) 1 calc R U P A 1
H17C H 0.624524 0.338976 0.289251 0.061 Uiso 0.875(3) 1 calc R U P A 1
C18 C 0.50941(17) 0.34184(18) 0.3733(2) 0.0508(9) Uani 0.875(3) 1 d D . P A 1
H18A H 0.492062 0.293821 0.354704 0.076 Uiso 0.875(3) 1 calc R U P A 1
H18B H 0.474335 0.375384 0.375263 0.076 Uiso 0.875(3) 1 calc R U P A 1
H18C H 0.536870 0.334536 0.418865 0.076 Uiso 0.875(3) 1 calc R U P A 1
C15' C 0.5496(10) 0.3752(10) 0.3287(11) 0.0299(5) Uani 0.125(3) 1 d D . P A 2
C16' C 0.5667(11) 0.3155(12) 0.3862(11) 0.0543(9) Uani 0.125(3) 1 d D . P A 2
H16D H 0.612300 0.304129 0.396349 0.081 Uiso 0.125(3) 1 calc R U P A 2
H16E H 0.542054 0.270099 0.371489 0.081 Uiso 0.125(3) 1 calc R U P A 2
H16F H 0.556297 0.334911 0.426737 0.081 Uiso 0.125(3) 1 calc R U P A 2
C17' C 0.4750(8) 0.3815(10) 0.3076(12) 0.0405(7) Uani 0.125(3) 1 d D . P A 2
H17D H 0.456976 0.338049 0.280615 0.061 Uiso 0.125(3) 1 calc R U P A 2
H17E H 0.462504 0.426786 0.280857 0.061 Uiso 0.125(3) 1 calc R U P A 2
H17F H 0.458996 0.383724 0.348034 0.061 Uiso 0.125(3) 1 calc R U P A 2
C18' C 0.5694(11) 0.3419(12) 0.2664(12) 0.0508(9) Uani 0.125(3) 1 d D . P A 2
H18D H 0.553140 0.291022 0.258262 0.076 Uiso 0.125(3) 1 calc R U P A 2
H18E H 0.616011 0.341406 0.275463 0.076 Uiso 0.125(3) 1 calc R U P A 2
H18F H 0.551519 0.372502 0.226536 0.076 Uiso 0.125(3) 1 calc R U P A 2
N1 N 0.3387(2) 0.89635(16) 0.32609(16) 0.0717(9) Uani 1 1 d . . . . .
N2 N 0.4804(3) 0.5805(4) 0.1037(2) 0.156(3) Uani 1 1 d . . . . .
N3 N 0.750000 0.2455(3) 0.500000 0.119(3) Uani 1 2 d S T P . .
C27 C 0.35682(19) 0.87370(19) 0.3802(2) 0.0622(9) Uani 1 1 d . . . . .
C28 C 0.3754(3) 0.8454(3) 0.4524(2) 0.0927(15) Uani 1 1 d . . . . .
H28A H 0.403329 0.881656 0.481232 0.139 Uiso 1 1 calc R U . . .
H28B H 0.397784 0.797826 0.454210 0.139 Uiso 1 1 calc R U . . .
H28C H 0.336871 0.838377 0.468378 0.139 Uiso 1 1 calc R U . . .
C29 C 0.5054(2) 0.6098(2) 0.1537(2) 0.0676(10) Uani 1 1 d . . . . .
C30 C 0.53822(12) 0.64442(17) 0.21542(16) 0.0463(7) Uani 1 1 d . . . . .
H30A H 0.575403 0.671326 0.208769 0.069 Uiso 1 1 calc R U . . .
H30B H 0.552248 0.606360 0.250229 0.069 Uiso 1 1 calc R U . . .
H30C H 0.509530 0.679351 0.229614 0.069 Uiso 1 1 calc R U . . .
C31 C 0.750000 0.3118(3) 0.500000 0.0840(18) Uani 1 2 d S T P . .
C32 C 0.750000 0.3928(3) 0.500000 0.0815(18) Uani 1 2 d S T P . .
H32A H 0.757491 0.411007 0.457674 0.122 Uiso 0.5 1 calc R U P B -1
H32B H 0.783838 0.411007 0.537963 0.122 Uiso 0.5 1 calc R U P B -1
H32C H 0.708672 0.411007 0.504363 0.122 Uiso 0.5 1 calc R U P B -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.608(2) . ?
V1 O5 1.9232(12) 2_656 ?
V1 O5 1.9231(12) . ?
V1 O6 1.9318(13) 2_656 ?
V1 O6 1.9317(13) . ?
V1 O11 2.1282(17) . ?
V2 O2 1.5911(16) . ?
V2 O5 2.0367(13) . ?
V2 O7 1.9939(15) . ?
V2 O8 2.0002(15) 2_656 ?
V2 O9 2.0210(14) . ?
V2 O11 2.3490(3) . ?
V3 O3 1.5883(16) . ?
V3 O6 2.0375(13) . ?
V3 O7 1.9996(15) . ?
V3 O8 1.9935(15) . ?
V3 O10 2.0115(14) . ?
V3 O11 2.3496(3) . ?
V4 O4 1.585(2) . ?
V4 O9 1.9268(15) . ?
V4 O9 1.9268(15) 2_656 ?
V4 O10 1.9179(14) . ?
V4 O10 1.9179(14) 2_656 ?
V4 O11 2.2848(17) . ?
O5 C1 1.388(2) . ?
O6 C7 1.390(2) . ?
O7 C23 1.424(2) . ?
O8 C24 1.434(2) . ?
O9 C25 1.429(2) . ?
O10 C26 1.424(2) . ?
C1 C2 1.401(3) . ?
C1 C6 1.392(3) . ?
C2 C3 1.391(3) . ?
C2 C14 1.520(2) 2_656 ?
C3 H3 0.9300 . ?
C3 C4 1.399(3) . ?
C4 C5 1.392(3) . ?
C4 C15 1.533(4) . ?
C4 C15' 1.543(16) . ?
C5 H5 0.9300 . ?
C5 C6 1.397(3) . ?
C6 C13 1.521(3) . ?
C7 C8 1.398(3) . ?
C7 C12 1.401(3) . ?
C8 C9 1.399(3) . ?
C8 C13 1.522(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.395(3) . ?
C10 C11 1.400(3) . ?
C10 C19 1.535(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.390(3) . ?
C12 C14 1.520(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C19 C20 1.531(3) . ?
C19 C21 1.537(3) . ?
C19 C22 1.530(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C15 C16 1.528(5) . ?
C15 C17 1.525(4) . ?
C15 C18 1.529(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C15' C16' 1.537(15) . ?
C15' C17' 1.537(15) . ?
C15' C18' 1.537(14) . ?
C16' H16D 0.9600 . ?
C16' H16E 0.9600 . ?
C16' H16F 0.9600 . ?
C17' H17D 0.9600 . ?
C17' H17E 0.9600 . ?
C17' H17F 0.9600 . ?
C18' H18D 0.9600 . ?
C18' H18E 0.9600 . ?
C18' H18F 0.9600 . ?
N1 C27 1.130(5) . ?
N2 C29 1.134(5) . ?
N3 C31 1.168(9) . ?
C27 C28 1.491(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.398(5) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.428(8) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 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
O1 V1 O5 95.43(4) . . ?
O1 V1 O5 95.43(4) . 2_656 ?
O1 V1 O6 95.71(4) . 2_656 ?
O1 V1 O6 95.71(4) . . ?
O1 V1 O11 180.0 . . ?
O5 V1 O5 169.14(8) . 2_656 ?
O5 V1 O6 89.06(6) . 2_656 ?
O5 V1 O6 89.86(6) 2_656 2_656 ?
O5 V1 O6 89.86(6) . . ?
O5 V1 O6 89.06(6) 2_656 . ?
O5 V1 O11 84.57(4) 2_656 . ?
O5 V1 O11 84.57(4) . . ?
O6 V1 O6 168.57(8) . 2_656 ?
O6 V1 O11 84.29(4) . . ?
O6 V1 O11 84.29(4) 2_656 . ?
O2 V2 O5 99.83(6) . . ?
O2 V2 O7 101.36(8) . . ?
O2 V2 O8 101.23(8) . 2_656 ?
O2 V2 O9 105.08(7) . . ?
O2 V2 O11 176.46(7) . . ?
O5 V2 O11 76.63(6) . . ?
O7 V2 O5 87.13(5) . . ?
O7 V2 O8 157.41(6) . 2_656 ?
O7 V2 O9 88.41(6) . . ?
O7 V2 O11 78.64(4) . . ?
O8 V2 O5 89.09(5) 2_656 . ?
O8 V2 O9 85.70(6) 2_656 . ?
O8 V2 O11 78.82(4) 2_656 . ?
O9 V2 O5 155.09(6) . . ?
O9 V2 O11 78.46(6) . . ?
O3 V3 O6 102.66(6) . . ?
O3 V3 O7 100.39(8) . . ?
O3 V3 O8 102.17(8) . . ?
O3 V3 O10 102.36(7) . . ?
O3 V3 O11 178.64(7) . . ?
O6 V3 O11 76.53(6) . . ?
O7 V3 O6 87.90(5) . . ?
O7 V3 O10 86.70(6) . . ?
O7 V3 O11 78.51(4) . . ?
O8 V3 O6 87.70(5) . . ?
O8 V3 O7 157.43(6) . . ?
O8 V3 O10 87.99(6) . . ?
O8 V3 O11 78.93(4) . . ?
O10 V3 O6 154.96(6) . . ?
O10 V3 O11 78.43(6) . . ?
O4 V4 O9 98.03(4) . . ?
O4 V4 O9 98.03(4) . 2_656 ?
O4 V4 O10 98.05(4) . 2_656 ?
O4 V4 O10 98.05(4) . . ?
O4 V4 O11 180.0 . . ?
O9 V4 O9 163.94(8) 2_656 . ?
O9 V4 O11 81.97(4) 2_656 . ?
O9 V4 O11 81.97(4) . . ?
O10 V4 O9 88.65(6) 2_656 2_656 ?
O10 V4 O9 89.11(6) 2_656 . ?
O10 V4 O9 89.11(6) . 2_656 ?
O10 V4 O9 88.65(6) . . ?
O10 V4 O10 163.89(8) . 2_656 ?
O10 V4 O11 81.95(4) 2_656 . ?
O10 V4 O11 81.95(4) . . ?
V1 O5 V2 107.73(6) . . ?
C1 O5 V1 117.24(11) . . ?
C1 O5 V2 135.02(11) . . ?
V1 O6 V3 107.80(6) . . ?
C7 O6 V1 118.55(11) . . ?
C7 O6 V3 133.65(11) . . ?
V2 O7 V3 112.73(7) . . ?
C23 O7 V2 121.52(13) . . ?
C23 O7 V3 119.48(13) . . ?
V3 O8 V2 112.39(7) . 2_656 ?
C24 O8 V2 116.65(12) . 2_656 ?
C24 O8 V3 119.97(13) . . ?
V4 O9 V2 110.62(7) . . ?
C25 O9 V2 123.31(14) . . ?
C25 O9 V4 121.76(14) . . ?
V4 O10 V3 110.96(7) . . ?
C26 O10 V3 124.90(13) . . ?
C26 O10 V4 123.33(14) . . ?
V1 O11 V2 91.06(4) . . ?
V1 O11 V2 91.06(4) . 2_656 ?
V1 O11 V3 91.37(4) . . ?
V1 O11 V3 91.37(4) . 2_656 ?
V1 O11 V4 180.0 . . ?
V2 O11 V2 177.87(8) . 2_656 ?
V2 O11 V3 89.863(12) . 2_656 ?
V2 O11 V3 89.860(12) 2_656 . ?
V2 O11 V3 90.088(12) 2_656 2_656 ?
V2 O11 V3 90.088(12) . . ?
V3 O11 V3 177.26(8) . 2_656 ?
V4 O11 V2 88.94(4) . . ?
V4 O11 V2 88.94(4) . 2_656 ?
V4 O11 V3 88.63(4) . . ?
V4 O11 V3 88.63(4) . 2_656 ?
O5 C1 C2 118.67(16) . . ?
O5 C1 C6 119.11(16) . . ?
C6 C1 C2 121.91(17) . . ?
C1 C2 C14 121.40(16) . 2_656 ?
C3 C2 C1 117.98(17) . . ?
C3 C2 C14 120.56(16) . 2_656 ?
C2 C3 H3 118.9 . . ?
C2 C3 C4 122.19(18) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C15 120.2(2) . . ?
C3 C4 C15' 120.7(8) . . ?
C5 C4 C3 117.62(18) . . ?
C5 C4 C15 122.2(2) . . ?
C5 C4 C15' 121.6(8) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.43(18) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 C5 117.84(17) . . ?
C1 C6 C13 121.91(16) . . ?
C5 C6 C13 120.20(17) . . ?
O6 C7 C8 118.73(16) . . ?
O6 C7 C12 119.13(16) . . ?
C8 C7 C12 121.90(17) . . ?
C7 C8 C9 117.67(17) . . ?
C7 C8 C13 121.32(16) . . ?
C9 C8 C13 120.95(17) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 C8 122.63(18) . . ?
C10 C9 H9 118.7 . . ?
C9 C10 C11 117.25(18) . . ?
C9 C10 C19 123.20(18) . . ?
C11 C10 C19 119.54(18) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.61(18) . . ?
C12 C11 H11 118.7 . . ?
C7 C12 C14 121.74(16) . . ?
C11 C12 C7 117.87(17) . . ?
C11 C12 C14 120.22(17) . . ?
C6 C13 C8 112.49(15) . . ?
C6 C13 H13A 109.1 . . ?
C6 C13 H13B 109.1 . . ?
C8 C13 H13A 109.1 . . ?
C8 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C2 C14 H14A 109.3 2_656 . ?
C2 C14 H14B 109.3 2_656 . ?
C12 C14 C2 111.60(15) . 2_656 ?
C12 C14 H14A 109.3 . . ?
C12 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C10 C19 C21 108.43(18) . . ?
C20 C19 C10 112.21(18) . . ?
C20 C19 C21 108.9(2) . . ?
C22 C19 C10 109.51(17) . . ?
C22 C19 C20 108.5(2) . . ?
C22 C19 C21 109.3(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O7 C23 H23A 109.5 . . ?
O7 C23 H23B 109.5 . . ?
O7 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O8 C24 H24A 109.5 . . ?
O8 C24 H24B 109.5 . . ?
O8 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O9 C25 H25A 109.5 . . ?
O9 C25 H25B 109.5 . . ?
O9 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O10 C26 H26A 109.5 . . ?
O10 C26 H26B 109.5 . . ?
O10 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C16 C15 C4 107.6(3) . . ?
C16 C15 C18 108.9(3) . . ?
C17 C15 C4 109.7(2) . . ?
C17 C15 C16 109.8(3) . . ?
C17 C15 C18 108.5(3) . . ?
C18 C15 C4 112.3(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16' C15' C4 109.4(15) . . ?
C16' C15' C17' 106.6(14) . . ?
C16' C15' C18' 106.9(15) . . ?
C17' C15' C4 111.0(14) . . ?
C18' C15' C4 116.2(15) . . ?
C18' C15' C17' 106.3(14) . . ?
C15' C16' H16D 109.5 . . ?
C15' C16' H16E 109.5 . . ?
C15' C16' H16F 109.5 . . ?
H16D C16' H16E 109.5 . . ?
H16D C16' H16F 109.5 . . ?
H16E C16' H16F 109.5 . . ?
C15' C17' H17D 109.5 . . ?
C15' C17' H17E 109.5 . . ?
C15' C17' H17F 109.5 . . ?
H17D C17' H17E 109.5 . . ?
H17D C17' H17F 109.5 . . ?
H17E C17' H17F 109.5 . . ?
C15' C18' H18D 109.5 . . ?
C15' C18' H18E 109.5 . . ?
C15' C18' H18F 109.5 . . ?
H18D C18' H18E 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
N1 C27 C28 175.3(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N2 C29 C30 178.0(6) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 C32 180.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O5 C1 C2 -88.16(17) . . . . ?
V1 O5 C1 C6 85.58(17) . . . . ?
V1 O6 C7 C8 -86.49(17) . . . . ?
V1 O6 C7 C12 88.01(18) . . . . ?
V2 O5 C1 C2 91.59(19) . . . . ?
V2 O5 C1 C6 -94.7(2) . . . . ?
V3 O6 C7 C8 93.3(2) . . . . ?
V3 O6 C7 C12 -92.25(19) . . . . ?
O5 C1 C2 C3 175.46(16) . . . . ?
O5 C1 C2 C14 -1.6(3) . . . 2_656 ?
O5 C1 C6 C5 -175.32(16) . . . . ?
O5 C1 C6 C13 2.2(3) . . . . ?
O6 C7 C8 C9 177.04(16) . . . . ?
O6 C7 C8 C13 -0.1(3) . . . . ?
O6 C7 C12 C11 -177.38(16) . . . . ?
O6 C7 C12 C14 -2.1(3) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C1 C6 C13 C8 -94.3(2) . . . . ?
C2 C1 C6 C5 -1.8(3) . . . . ?
C2 C1 C6 C13 175.71(16) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C2 C3 C4 C15 178.4(2) . . . . ?
C2 C3 C4 C15' 179.5(10) . . . . ?
C3 C4 C5 C6 0.6(3) . . . . ?
C3 C4 C15 C16 -65.7(3) . . . . ?
C3 C4 C15 C17 53.7(4) . . . . ?
C3 C4 C15 C18 174.4(3) . . . . ?
C3 C4 C15' C16' 122.5(12) . . . . ?
C3 C4 C15' C17' -120.2(13) . . . . ?
C3 C4 C15' C18' 1.4(19) . . . . ?
C4 C5 C6 C1 0.5(3) . . . . ?
C4 C5 C6 C13 -177.06(17) . . . . ?
C5 C4 C15 C16 113.1(3) . . . . ?
C5 C4 C15 C17 -127.5(3) . . . . ?
C5 C4 C15 C18 -6.8(4) . . . . ?
C5 C4 C15' C16' -57.5(16) . . . . ?
C5 C4 C15' C17' 59.8(17) . . . . ?
C5 C4 C15' C18' -178.6(13) . . . . ?
C5 C6 C13 C8 83.1(2) . . . . ?
C6 C1 C2 C3 1.9(3) . . . . ?
C6 C1 C2 C14 -175.15(16) . . . 2_656 ?
C7 C8 C9 C10 -0.6(3) . . . . ?
C7 C8 C13 C6 91.7(2) . . . . ?
C7 C12 C14 C2 -90.3(2) . . . 2_656 ?
C8 C7 C12 C11 -3.1(3) . . . . ?
C8 C7 C12 C14 172.21(17) . . . . ?
C8 C9 C10 C11 -1.0(3) . . . . ?
C8 C9 C10 C19 179.56(18) . . . . ?
C9 C8 C13 C6 -85.4(2) . . . . ?
C9 C10 C11 C12 0.6(3) . . . . ?
C9 C10 C19 C20 1.4(3) . . . . ?
C9 C10 C19 C21 -118.9(2) . . . . ?
C9 C10 C19 C22 121.9(2) . . . . ?
C10 C11 C12 C7 1.4(3) . . . . ?
C10 C11 C12 C14 -174.00(17) . . . . ?
C11 C10 C19 C20 -178.1(2) . . . . ?
C11 C10 C19 C21 61.7(3) . . . . ?
C11 C10 C19 C22 -57.6(3) . . . . ?
C11 C12 C14 C2 84.9(2) . . . 2_656 ?
C12 C7 C8 C9 2.7(3) . . . . ?
C12 C7 C8 C13 -174.48(16) . . . . ?
C13 C8 C9 C10 176.58(17) . . . . ?
C14 C2 C3 C4 176.37(17) 2_656 . . . ?
C19 C10 C11 C12 -179.92(18) . . . . ?
C15 C4 C5 C6 -178.2(2) . . . . ?
C15' C4 C5 C6 -179.4(10) . . . . ?

_olex2_submission_original_sample_id matrm24
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.143
_oxdiff_exptl_absorpt_empirical_full_min 0.643
####################################################################### 
# 
# 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_matrm28
_database_code_depnum_ccdc_archive 'CCDC 2145267'
loop_
_audit_author_name
_audit_author_address
'William Brennessel'
;University of Rochester
United States of America
;
_audit_update_record             
;
2022-01-28 deposited with the CCDC.	2022-04-29 downloaded from the CCDC.
;

_vrf_PLAT301_matrm28             
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 20% 
RESPONSE: Tert-butyl group C20-C23 is modeled as disordered over
two positions (0.640(6):0.360(6)). The V-O=PPhMe2 group is disordered
across a crystallographic inversion center with a V=O group of
the symmetry equivalent molecule (0.50:0.50). Due to resolution
limitations, oxygen atom O2 was unable to be placed in two positions
based on electron density and thus lies in an average position between
the two types of V-O bond lengths. Additionally, the PPhMe2
group is disordered with solvent along zigzagging channels
such that the Ph group is oriented unidirectionally in each channel
(but both packing directions are present in a 1:1 ratio throughout
the crystal due to space group symmetry).
;

_vrf_PLAT302_matrm28             
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2-3  ) .. 100% 
RESPONSE: The solvent of crystallization is disordered with the
PPhMe2 groups in channels (see response to alert PLAT301). The
solvent is a disordered mixture of diethyl ether and acetonitrile
(0.58(1):0.21(1)). The ether molecule is modeled as disordered over
a crystallographic mirror plane on which sits the acetonitrile
molecule. It seems logical that there may be additional solvent
present when acetonitrile is the local solvate, because this would
create a void space. However the electron density of such a proposed
solvent molecule is not identifiable due to the dominance of the
phenyl ring in that crystallographic position.
;

_vrf_PLAT860_matrm28             
;
PROBLEM: _G Number of Least-Squares Restraints ............. 127 
RESPONSE: Analogous bond lengths and angles between the two positions
of each disordered species were restrained to be similar. Anisotropic
displacement parameters for proximal and symmetry-equivalent atoms
were restrained to be similar and, in some cases, restrained toward
the expected motion relative to bond direction.
;

_audit_creation_date             2021-03-09
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C60 H87 O19 P V6, 0.584(C4 H10 O), 0.208(C4 H6 N2)'
_chemical_formula_sum            'C63.17 H94.09 N0.42 O19.59 P V6'
_chemical_formula_weight         1509.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   22.5148(4)
_cell_length_b                   20.0029(3)
_cell_length_c                   15.83572(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7131.78(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22024
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.0600
_cell_measurement_theta_min      3.3990
_shelx_estimated_absorpt_T_max   0.789
_shelx_estimated_absorpt_T_min   0.259
_exptl_absorpt_coefficient_mu    7.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow-brown
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3143
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48193
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.779
_diffrn_reflns_theta_min         3.412
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -120.00 -22.00   0.50    3.10    --  -47.20 -83.00 -93.00  196
  2  ω     93.00 178.00   0.50   12.38    --  107.75  58.00 -88.00  170
  3  ω     82.00 178.00   0.50   12.38    --  107.75  83.00  28.00  192
  4  ω     82.00 178.00   0.50   12.38    --  107.75  83.00 136.00  192
  5  ω   -120.00 -34.00   0.50    3.10    --  -47.20 -38.00-180.00  172
  6  ω    -30.00  26.00   0.50    3.10    --  -47.20  38.00  30.00  112
  7  ω    -27.00   5.00   0.50    3.10    --   47.20 -19.00 120.00   64
  8  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00  60.00  104
  9  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00 -30.00  104
 10  ω     35.00 109.00   0.50   12.38    --  107.75 -94.00-150.00  148
 11  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00 150.00  104
 12  ω     35.00  87.00   0.50   12.38    --  107.75 -61.00   0.00  104
 13  ω     94.00 164.00   0.50   12.38    --  107.75  15.00  90.00  140
 14  ω     94.00 164.00   0.50   12.38    --  107.75  15.00-120.00  140
 15  ω     32.00  57.00   0.50    3.10    --   47.20  57.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0505007000
_diffrn_orient_matrix_UB_12      0.0491935000
_diffrn_orient_matrix_UB_13      -0.0210196000
_diffrn_orient_matrix_UB_21      -0.0320459000
_diffrn_orient_matrix_UB_22      0.0194643000
_diffrn_orient_matrix_UB_23      -0.0823268000
_diffrn_orient_matrix_UB_31      -0.0332470000
_diffrn_orient_matrix_UB_32      0.0559663000
_diffrn_orient_matrix_UB_33      0.0473732000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7056
_reflns_number_total             7723
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7723
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0587
_refine_ls_restrained_S_all      1.088
_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)+(0.0504P)²+21.0480P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1475
_refine_special_details          
;
Tert-butyl group C20-C23 is modeled as disordered over two
positions (0.640(6):0.360(6)). The V-O=PPhMe2 group is disordered
across a crystallographic inversion center with a V=O group of
the symmetry equivalent molecule (0.50:0.50). Due to resolution
limitations, oxygen atom O2 was unable to be placed in two positions
based on electron density and thus lies in an average position between
the two types of V-O bond lengths. Additionally, the PPhMe2
group is disordered with solvent along zigzagging channels
such that the Ph group is oriented unidirectionally in each channel
(but both packing directions are present in a 1:1 ratio throughout
the crystal due to space group symmetry).

The solvent of crystallization is disordered with the PPhMe2
groups in channels (see response to alert PLAT301). The
solvent is a disordered mixture of diethyl ether and acetonitrile
(0.58(1):0.21(1)). The ether molecule is modeled as disordered over
a crystallographic mirror plane on which sits the acetonitrile
molecule. It seems logical that there may be additional solvent
present when acetonitrile is the local solvate, because this would
create a void space. However the electron density of such a proposed
solvent molecule is not identifiable due to the dominance of the
phenyl ring in that crystallographic position.

Analogous bond lengths and angles between the two positions of
each disordered species were restrained to be similar. Anisotropic
displacement parameters for proximal and symmetry-equivalent atoms
were restrained to be similar and, in some cases, restrained toward
the expected motion relative to bond direction.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C10-C20 \\sim C10-C20'
 with sigma of 0.01
 C20-C21 \\sim C20-C22 \\sim C20-C23 \\sim C20'-C21' \\sim C20'-C22' \\sim
C20'-C23'
 with sigma of 0.01
 C21-C22 \\sim C22-C23 \\sim C23-C21 \\sim C21'-C22' \\sim C22'-C23' \\sim
C23'-C21'
 with sigma of 0.02
 P1-C35 \\sim P1-C36
 with sigma of 0.01
3. Restrained planarity
 C29, C31, C33, C30, C32, C34
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C40 \\sim C42: within 2A with sigma of 0.008 and sigma for terminal atoms of
0.016 within 2A
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) = Uanis(C20')
5. Rigid body (RIGU) restrains
 C37, C38, O13, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C29, C34, C33, C32, C31, C30} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C29, C30, C31, C32, C33, C34}
{C40, C39, O13, C38, C37} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C37, C38, O13, C39, C40}
7. Others
 Sof(C20')=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22')=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Sof(N1)=Sof(C41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=0.5*(1-FVAR(3))
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(O13)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=0.5*FVAR(3)
 Fixed Sof: H25A(0.5) H25B(0.5) H25C(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
 P1(0.5) C29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5)
 C33(0.5) H33(0.5) C34(0.5) H34(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
 C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C38(H38A,H38B), C39(H39A,H39B)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34)
8.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C21'(H21D,H21E,H21F),
 C22'(H22D,H22E,H22F), C23'(H23D,H23E,H23F), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.31175(3) 0.750000 0.42801(4) 0.01885(16) Uani 1 2 d S T P . .
V2 V 0.42573(3) 0.67081(3) 0.37107(3) 0.02664(15) Uani 1 1 d . . . . .
V3 V 0.30771(3) 0.66697(3) 0.25234(3) 0.02693(15) Uani 1 1 d . . . . .
V4 V 0.42878(4) 0.750000 0.19256(5) 0.02466(18) Uani 1 2 d S T P . .
O1 O 0.27070(14) 0.750000 0.5118(2) 0.0244(6) Uani 1 2 d S T P . .
O2 O 0.46845(13) 0.60630(17) 0.42077(17) 0.0480(7) Uani 1 1 d . . . . .
O3 O 0.26561(13) 0.61122(14) 0.21374(16) 0.0419(7) Uani 1 1 d . . . . .
O4 O 0.47106(16) 0.750000 0.1119(2) 0.0317(8) Uani 1 2 d S T P . .
O5 O 0.36679(9) 0.68300(10) 0.46807(12) 0.0194(4) Uani 1 1 d . . . . .
O6 O 0.26814(10) 0.68184(11) 0.36895(13) 0.0233(4) Uani 1 1 d . . . . .
O7 O 0.36741(11) 0.61185(11) 0.31471(14) 0.0278(5) Uani 1 1 d . . . . .
O8 O 0.26674(15) 0.750000 0.2134(2) 0.0314(8) Uani 1 2 d S T P . .
O9 O 0.46961(14) 0.750000 0.41289(19) 0.0262(7) Uani 1 2 d S T P . .
O10 O 0.46875(11) 0.68035(12) 0.26393(14) 0.0305(5) Uani 1 1 d . . . . .
O11 O 0.36832(12) 0.68010(13) 0.16256(15) 0.0357(6) Uani 1 1 d . . . . .
O12 O 0.36661(14) 0.750000 0.31977(18) 0.0210(6) Uani 1 2 d S T P . .
C1 C 0.35928(14) 0.65573(14) 0.54744(18) 0.0194(6) Uani 1 1 d . . . . .
C2 C 0.38630(13) 0.68628(15) 0.61708(18) 0.0196(6) Uani 1 1 d . . . . .
C3 C 0.37723(14) 0.65696(15) 0.69632(18) 0.0216(6) Uani 1 1 d . . . . .
H3 H 0.395698 0.676629 0.744200 0.026 Uiso 1 1 calc R U . . .
C4 C 0.34244(14) 0.60043(15) 0.70800(19) 0.0227(6) Uani 1 1 d . . . . .
C5 C 0.31513(15) 0.57332(15) 0.6366(2) 0.0241(6) Uani 1 1 d . . . . .
H5 H 0.290730 0.534928 0.643247 0.029 Uiso 1 1 calc R U . . .
C6 C 0.32216(15) 0.60020(14) 0.55646(19) 0.0223(6) Uani 1 1 d . . . . .
C7 C 0.21949(14) 0.65538(16) 0.41071(19) 0.0248(6) Uani 1 1 d . . . . .
C8 C 0.22819(15) 0.60345(17) 0.4680(2) 0.0268(7) Uani 1 1 d . . . . .
C9 C 0.17985(17) 0.58374(19) 0.5171(2) 0.0339(8) Uani 1 1 d . . . . .
H9 H 0.184949 0.548228 0.556300 0.041 Uiso 1 1 calc R U . . .
C10 C 0.12443(17) 0.6142(2) 0.5109(2) 0.0372(9) Uani 1 1 d D . . . .
C11 C 0.11800(16) 0.6651(2) 0.4519(2) 0.0364(8) Uani 1 1 d . . . . .
H11 H 0.080106 0.685349 0.445195 0.044 Uiso 1 1 calc R U . . .
C12 C 0.16504(15) 0.68781(19) 0.4020(2) 0.0298(7) Uani 1 1 d . . . . .
C13 C 0.4227(2) 0.750000 0.6080(3) 0.0211(8) Uani 1 2 d S T P . .
H13A H 0.442111 0.750000 0.551862 0.025 Uiso 1 2 calc R U P . .
H13B H 0.454418 0.750000 0.651287 0.025 Uiso 1 2 calc R U P . .
C14 C 0.28861(16) 0.57106(16) 0.4812(2) 0.0268(7) Uani 1 1 d . . . . .
H14A H 0.312794 0.577140 0.429517 0.032 Uiso 1 1 calc R U . . .
H14B H 0.283134 0.522454 0.489994 0.032 Uiso 1 1 calc R U . . .
C15 C 0.1573(2) 0.750000 0.3484(3) 0.0304(10) Uani 1 2 d S T P . .
H15A H 0.186957 0.750000 0.302301 0.036 Uiso 1 2 calc R U P . .
H15B H 0.117212 0.750001 0.322695 0.036 Uiso 1 2 calc R U P . .
C16 C 0.33465(16) 0.56632(17) 0.79448(19) 0.0277(7) Uani 1 1 d . . . . .
C17 C 0.3738(3) 0.5034(3) 0.7962(3) 0.0598(14) Uani 1 1 d . . . . .
H17A H 0.370229 0.481630 0.851391 0.090 Uiso 1 1 calc R U . . .
H17B H 0.415302 0.516072 0.786481 0.090 Uiso 1 1 calc R U . . .
H17C H 0.360869 0.472525 0.751875 0.090 Uiso 1 1 calc R U . . .
C18 C 0.3522(2) 0.6124(2) 0.8670(2) 0.0476(11) Uani 1 1 d . . . . .
H18A H 0.327869 0.653059 0.865048 0.071 Uiso 1 1 calc R U . . .
H18B H 0.394202 0.624435 0.861704 0.071 Uiso 1 1 calc R U . . .
H18C H 0.345681 0.589456 0.920879 0.071 Uiso 1 1 calc R U . . .
C19 C 0.27058(19) 0.5456(2) 0.8081(2) 0.0412(9) Uani 1 1 d . . . . .
H19A H 0.266106 0.526835 0.864953 0.062 Uiso 1 1 calc R U . . .
H19B H 0.259506 0.511854 0.766126 0.062 Uiso 1 1 calc R U . . .
H19C H 0.244708 0.584718 0.802172 0.062 Uiso 1 1 calc R U . . .
C20 C 0.0773(2) 0.5871(3) 0.5733(3) 0.0350(16) Uani 0.640(6) 1 d D U P A 1
C21 C 0.0957(3) 0.6050(3) 0.6635(3) 0.0465(17) Uani 0.640(6) 1 d D . P A 1
H21A H 0.100471 0.653575 0.668200 0.070 Uiso 0.640(6) 1 calc R U P A 1
H21B H 0.133380 0.583002 0.676960 0.070 Uiso 0.640(6) 1 calc R U P A 1
H21C H 0.064979 0.589966 0.702994 0.070 Uiso 0.640(6) 1 calc R U P A 1
C22 C 0.0685(3) 0.5116(3) 0.5651(4) 0.0407(16) Uani 0.640(6) 1 d D U P A 1
H22A H 0.035467 0.497464 0.601300 0.061 Uiso 0.640(6) 1 calc R U P A 1
H22B H 0.104858 0.488509 0.582552 0.061 Uiso 0.640(6) 1 calc R U P A 1
H22C H 0.059463 0.500371 0.506245 0.061 Uiso 0.640(6) 1 calc R U P A 1
C23 C 0.0188(3) 0.6218(4) 0.5519(5) 0.051(2) Uani 0.640(6) 1 d D U P A 1
H23A H -0.013032 0.603479 0.587206 0.077 Uiso 0.640(6) 1 calc R U P A 1
H23B H 0.009261 0.614403 0.492244 0.077 Uiso 0.640(6) 1 calc R U P A 1
H23C H 0.022557 0.669918 0.562517 0.077 Uiso 0.640(6) 1 calc R U P A 1
C20' C 0.0641(4) 0.6075(5) 0.5585(6) 0.0350(16) Uani 0.360(6) 1 d D U P A 2
C21' C 0.0118(5) 0.5899(6) 0.5004(7) 0.047(3) Uani 0.360(6) 1 d D U P A 2
H21D H 0.022315 0.551280 0.465412 0.070 Uiso 0.360(6) 1 calc R U P A 2
H21E H 0.002683 0.628165 0.464008 0.070 Uiso 0.360(6) 1 calc R U P A 2
H21F H -0.023116 0.579002 0.534796 0.070 Uiso 0.360(6) 1 calc R U P A 2
C22' C 0.0456(6) 0.6686(5) 0.6111(8) 0.057(4) Uani 0.360(6) 1 d D . P A 2
H22D H 0.013168 0.656097 0.649152 0.085 Uiso 0.360(6) 1 calc R U P A 2
H22E H 0.032335 0.704372 0.573311 0.085 Uiso 0.360(6) 1 calc R U P A 2
H22F H 0.079643 0.684161 0.644284 0.085 Uiso 0.360(6) 1 calc R U P A 2
C23' C 0.0744(5) 0.5484(5) 0.6178(7) 0.045(3) Uani 0.360(6) 1 d D U P A 2
H23D H 0.107078 0.558887 0.656588 0.067 Uiso 0.360(6) 1 calc R U P A 2
H23E H 0.084686 0.508640 0.584679 0.067 Uiso 0.360(6) 1 calc R U P A 2
H23F H 0.038220 0.539665 0.650349 0.067 Uiso 0.360(6) 1 calc R U P A 2
C24 C 0.38258(19) 0.54780(18) 0.2829(3) 0.0385(9) Uani 1 1 d . . . . .
H24A H 0.408704 0.552826 0.233832 0.058 Uiso 1 1 calc R U . . .
H24B H 0.346374 0.524083 0.266101 0.058 Uiso 1 1 calc R U . . .
H24C H 0.403144 0.522220 0.326868 0.058 Uiso 1 1 calc R U . . .
C25 C 0.2299(3) 0.750000 0.1412(3) 0.0451(14) Uani 1 2 d S T P . .
H25A H 0.195057 0.721775 0.151589 0.068 Uiso 0.5 1 calc R U P B -1
H25B H 0.252079 0.732447 0.092782 0.068 Uiso 0.5 1 calc R U P B -1
H25C H 0.216922 0.795778 0.129040 0.068 Uiso 0.5 1 calc R U P B -1
C26 C 0.5326(2) 0.750000 0.4185(4) 0.0411(13) Uani 1 2 d S T P . .
H26A H 0.545109 0.779974 0.464056 0.062 Uiso 0.5 1 calc R U P C -1
H26B H 0.549452 0.765450 0.364869 0.062 Uiso 0.5 1 calc R U P C -1
H26C H 0.546586 0.704576 0.430319 0.062 Uiso 0.5 1 calc R U P C -1
C27 C 0.5126(2) 0.6380(3) 0.2332(3) 0.0604(15) Uani 1 1 d . . . . .
H27A H 0.523260 0.605348 0.276808 0.091 Uiso 1 1 calc R U . . .
H27B H 0.547796 0.664291 0.218050 0.091 Uiso 1 1 calc R U . . .
H27C H 0.497840 0.614535 0.183149 0.091 Uiso 1 1 calc R U . . .
C28 C 0.3616(3) 0.6582(3) 0.0814(3) 0.0688(17) Uani 1 1 d . . . . .
H28A H 0.333358 0.620883 0.080316 0.103 Uiso 1 1 calc R U . . .
H28B H 0.400010 0.643233 0.059445 0.103 Uiso 1 1 calc R U . . .
H28C H 0.346432 0.694765 0.046287 0.103 Uiso 1 1 calc R U . . .
P1 P 0.49695(9) 0.54365(10) 0.47101(12) 0.0360(4) Uani 0.5 1 d D . P D -1
C29 C 0.5691(4) 0.5776(4) 0.5058(5) 0.055(2) Uani 0.5 1 d D . P D -1
C30 C 0.5730(5) 0.6145(5) 0.5808(6) 0.071(3) Uani 0.5 1 d D . P D -1
H30 H 0.540159 0.616049 0.618454 0.085 Uiso 0.5 1 calc R U P D -1
C31 C 0.6215(6) 0.6468(5) 0.5989(8) 0.081(4) Uani 0.5 1 d D . P D -1
H31 H 0.623393 0.671615 0.649902 0.097 Uiso 0.5 1 calc R U P D -1
C32 C 0.6704(5) 0.6460(5) 0.5459(7) 0.063(3) Uani 0.5 1 d D . P D -1
H32 H 0.705363 0.669930 0.560384 0.075 Uiso 0.5 1 calc R U P D -1
C33 C 0.6676(5) 0.6101(5) 0.4725(8) 0.074(3) Uani 0.5 1 d D . P D -1
H33 H 0.700753 0.608922 0.435448 0.089 Uiso 0.5 1 calc R U P D -1
C34 C 0.6187(5) 0.5772(5) 0.4533(7) 0.068(3) Uani 0.5 1 d D . P D -1
H34 H 0.617319 0.552478 0.402147 0.082 Uiso 0.5 1 calc R U P D -1
C35 C 0.5134(5) 0.4702(5) 0.4082(6) 0.053(2) Uani 0.5 1 d D . P D -1
H35A H 0.476382 0.446618 0.394959 0.080 Uiso 0.5 1 calc R U P D -1
H35B H 0.539766 0.440447 0.440026 0.080 Uiso 0.5 1 calc R U P D -1
H35C H 0.532933 0.483749 0.355606 0.080 Uiso 0.5 1 calc R U P D -1
C36 C 0.4535(5) 0.5158(7) 0.5593(7) 0.072(4) Uani 0.5 1 d D . P D -1
H36A H 0.436593 0.554639 0.588458 0.108 Uiso 0.5 1 calc R U P D -1
H36B H 0.478871 0.490811 0.598426 0.108 Uiso 0.5 1 calc R U P D -1
H36C H 0.421350 0.486892 0.539263 0.108 Uiso 0.5 1 calc R U P D -1
C37 C 0.6419(12) 0.8669(16) 0.5428(17) 0.092(8) Uani 0.292(6) 1 d D U P E -1
H37A H 0.683289 0.873875 0.525651 0.137 Uiso 0.292(6) 1 calc R U P E -1
H37B H 0.620875 0.909780 0.542423 0.137 Uiso 0.292(6) 1 calc R U P E -1
H37C H 0.622666 0.836048 0.503279 0.137 Uiso 0.292(6) 1 calc R U P E -1
C38 C 0.6403(9) 0.8380(12) 0.6296(15) 0.073(6) Uani 0.292(6) 1 d D . P E -1
H38A H 0.633313 0.875714 0.668787 0.088 Uiso 0.292(6) 1 calc R U P E -1
H38B H 0.604562 0.809259 0.632377 0.088 Uiso 0.292(6) 1 calc R U P E -1
O13 O 0.6889(5) 0.7992(6) 0.6650(7) 0.054(3) Uani 0.292(6) 1 d D . P E -1
C39 C 0.6859(12) 0.7839(11) 0.7538(12) 0.089(7) Uani 0.292(6) 1 d D . P E -1
H39A H 0.646054 0.765364 0.765947 0.107 Uiso 0.292(6) 1 calc R U P E -1
H39B H 0.689559 0.826312 0.785630 0.107 Uiso 0.292(6) 1 calc R U P E -1
C40 C 0.7312(11) 0.7361(11) 0.7875(12) 0.058(5) Uani 0.292(6) 1 d D U P E -1
H40A H 0.738483 0.700846 0.745745 0.088 Uiso 0.292(6) 1 calc R U P E -1
H40B H 0.716582 0.716066 0.839945 0.088 Uiso 0.292(6) 1 calc R U P E -1
H40C H 0.768360 0.760100 0.798719 0.088 Uiso 0.292(6) 1 calc R U P E -1
N1 N 0.7410(13) 0.750000 0.6534(12) 0.108(8) Uani 0.416(11) 2 d S TU P E 2
C41 C 0.7367(11) 0.750000 0.7215(13) 0.065(5) Uani 0.416(11) 2 d S TU P E 2
C42 C 0.7315(15) 0.750000 0.8174(14) 0.052(5) Uani 0.416(11) 2 d S TU P E 2
H42A H 0.736309 0.795712 0.838625 0.077 Uiso 0.208(6) 1 calc R U P E 2
H42B H 0.762556 0.721395 0.841502 0.077 Uiso 0.208(6) 1 calc R U P E 2
H42C H 0.692422 0.732893 0.833815 0.077 Uiso 0.208(6) 1 calc R U P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.618(3) . ?
V1 O5 1.932(2) 7_575 ?
V1 O5 1.932(2) . ?
V1 O6 1.923(2) 7_575 ?
V1 O6 1.923(2) . ?
V1 O12 2.113(3) . ?
V2 O2 1.792(3) . ?
V2 O5 2.045(2) . ?
V2 O7 1.978(2) . ?
V2 O9 1.981(2) . ?
V2 O10 1.963(2) . ?
V2 O12 2.223(2) . ?
V3 O3 1.586(3) . ?
V3 O6 2.072(2) . ?
V3 O7 1.999(3) . ?
V3 O8 1.9972(19) . ?
V3 O11 1.988(2) . ?
V3 O12 2.378(2) . ?
V4 O4 1.593(3) . ?
V4 O10 2.007(2) 7_575 ?
V4 O10 2.007(2) . ?
V4 O11 2.008(3) 7_575 ?
V4 O11 2.008(3) . ?
V4 O12 2.453(3) . ?
O2 P1 1.617(3) . ?
O5 C1 1.380(3) . ?
O6 C7 1.384(4) . ?
O7 C24 1.418(4) . ?
O8 C25 1.414(6) . ?
O9 C26 1.420(6) . ?
O10 C27 1.389(5) . ?
O11 C28 1.366(5) . ?
C1 C2 1.400(4) . ?
C1 C6 1.397(4) . ?
C2 C3 1.400(4) . ?
C2 C13 1.522(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(4) . ?
C4 C5 1.396(4) . ?
C4 C16 1.540(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(4) . ?
C6 C14 1.527(4) . ?
C7 C8 1.393(5) . ?
C7 C12 1.394(5) . ?
C8 C9 1.395(5) . ?
C8 C14 1.521(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.392(6) . ?
C10 C11 1.391(6) . ?
C10 C20 1.548(6) . ?
C10 C20' 1.559(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(5) . ?
C12 C15 1.516(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.536(5) . ?
C16 C18 1.525(5) . ?
C16 C19 1.516(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.529(6) . ?
C20 C22 1.530(6) . ?
C20 C23 1.527(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C20' C21' 1.535(7) . ?
C20' C22' 1.536(7) . ?
C20' C23' 1.529(7) . ?
C21' H21D 0.9800 . ?
C21' H21E 0.9800 . ?
C21' H21F 0.9800 . ?
C22' H22D 0.9800 . ?
C22' H22E 0.9800 . ?
C22' H22F 0.9800 . ?
C23' H23D 0.9800 . ?
C23' H23E 0.9800 . ?
C23' H23F 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
P1 C29 1.845(11) . ?
P1 C35 1.813(8) . ?
P1 C36 1.795(9) . ?
C29 C30 1.402(13) . ?
C29 C34 1.392(12) . ?
C30 H30 0.9500 . ?
C30 C31 1.299(15) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(16) . ?
C32 H32 0.9500 . ?
C32 C33 1.368(15) . ?
C33 H33 0.9500 . ?
C33 C34 1.317(14) . ?
C34 H34 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C37 C38 1.49(2) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 O13 1.453(19) . ?
O13 C39 1.441(18) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.50(2) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
N1 C41 1.08(3) . ?
C41 C42 1.52(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O5 95.56(10) . . ?
O1 V1 O5 95.56(10) . 7_575 ?
O1 V1 O6 96.17(10) . 7_575 ?
O1 V1 O6 96.17(10) . . ?
O1 V1 O12 179.06(14) . . ?
O5 V1 O5 87.82(13) . 7_575 ?
O5 V1 O12 83.77(9) 7_575 . ?
O5 V1 O12 83.77(9) . . ?
O6 V1 O5 89.74(9) . . ?
O6 V1 O5 168.20(10) 7_575 . ?
O6 V1 O5 168.20(10) . 7_575 ?
O6 V1 O5 89.73(9) 7_575 7_575 ?
O6 V1 O6 90.31(14) 7_575 . ?
O6 V1 O12 84.49(9) 7_575 . ?
O6 V1 O12 84.49(9) . . ?
O2 V2 O5 95.99(11) . . ?
O2 V2 O7 97.20(13) . . ?
O2 V2 O9 99.28(13) . . ?
O2 V2 O10 100.65(11) . . ?
O2 V2 O12 174.46(12) . . ?
O5 V2 O12 78.52(10) . . ?
O7 V2 O5 88.81(9) . . ?
O7 V2 O9 163.50(10) . . ?
O7 V2 O12 82.09(9) . . ?
O9 V2 O5 88.69(11) . . ?
O9 V2 O12 81.43(9) . . ?
O10 V2 O5 163.35(9) . . ?
O10 V2 O7 89.74(10) . . ?
O10 V2 O9 88.00(12) . . ?
O10 V2 O12 84.85(10) . . ?
O3 V3 O6 100.81(12) . . ?
O3 V3 O7 101.79(14) . . ?
O3 V3 O8 100.94(14) . . ?
O3 V3 O11 103.15(12) . . ?
O3 V3 O12 175.69(12) . . ?
O6 V3 O12 74.89(10) . . ?
O7 V3 O6 85.87(9) . . ?
O7 V3 O12 77.79(8) . . ?
O8 V3 O6 87.53(12) . . ?
O8 V3 O7 157.14(11) . . ?
O8 V3 O12 79.36(10) . . ?
O11 V3 O6 156.01(10) . . ?
O11 V3 O7 87.97(11) . . ?
O11 V3 O8 89.23(13) . . ?
O11 V3 O12 81.15(10) . . ?
O4 V4 O10 100.58(12) . . ?
O4 V4 O10 100.58(12) . 7_575 ?
O4 V4 O11 102.43(12) . 7_575 ?
O4 V4 O11 102.43(12) . . ?
O4 V4 O12 178.10(16) . . ?
O10 V4 O10 87.92(15) 7_575 . ?
O10 V4 O11 87.35(11) 7_575 7_575 ?
O10 V4 O11 156.98(10) . 7_575 ?
O10 V4 O11 87.35(11) . . ?
O10 V4 O11 156.98(10) 7_575 . ?
O10 V4 O12 78.08(8) 7_575 . ?
O10 V4 O12 78.08(8) . . ?
O11 V4 O11 88.24(17) 7_575 . ?
O11 V4 O12 78.90(9) 7_575 . ?
O11 V4 O12 78.90(9) . . ?
P1 O2 V2 170.8(2) . . ?
V1 O5 V2 104.61(9) . . ?
C1 O5 V1 119.63(18) . . ?
C1 O5 V2 135.75(18) . . ?
V1 O6 V3 108.40(10) . . ?
C7 O6 V1 116.27(18) . . ?
C7 O6 V3 135.32(19) . . ?
V2 O7 V3 109.90(11) . . ?
C24 O7 V2 122.6(2) . . ?
C24 O7 V3 119.0(2) . . ?
V3 O8 V3 112.52(16) . 7_575 ?
C25 O8 V3 121.39(11) . . ?
C25 O8 V3 121.39(11) . 7_575 ?
V2 O9 V2 106.20(15) . 7_575 ?
C26 O9 V2 121.24(14) . 7_575 ?
C26 O9 V2 121.24(14) . . ?
V2 O10 V4 109.45(11) . . ?
C27 O10 V2 126.5(2) . . ?
C27 O10 V4 123.0(2) . . ?
V3 O11 V4 112.83(11) . . ?
C28 O11 V3 123.6(3) . . ?
C28 O11 V4 121.4(3) . . ?
V1 O12 V2 93.07(9) . . ?
V1 O12 V2 93.07(9) . 7_575 ?
V1 O12 V3 92.19(10) . 7_575 ?
V1 O12 V3 92.19(10) . . ?
V1 O12 V4 179.02(15) . . ?
V2 O12 V2 90.90(11) . 7_575 ?
V2 O12 V3 174.60(15) . 7_575 ?
V2 O12 V3 90.02(2) 7_575 7_575 ?
V2 O12 V3 174.60(15) 7_575 . ?
V2 O12 V3 90.02(2) . . ?
V2 O12 V4 87.62(9) . . ?
V2 O12 V4 87.62(9) 7_575 . ?
V3 O12 V3 88.58(10) . 7_575 ?
V3 O12 V4 87.11(8) 7_575 . ?
V3 O12 V4 87.11(8) . . ?
O5 C1 C2 119.4(3) . . ?
O5 C1 C6 118.7(3) . . ?
C6 C1 C2 121.8(3) . . ?
C1 C2 C3 117.4(3) . . ?
C1 C2 C13 121.7(3) . . ?
C3 C2 C13 120.9(3) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.9(3) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 117.2(3) . . ?
C3 C4 C16 122.9(3) . . ?
C5 C4 C16 119.8(3) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 C4 122.7(3) . . ?
C6 C5 H5 118.7 . . ?
C1 C6 C14 121.3(3) . . ?
C5 C6 C1 118.0(3) . . ?
C5 C6 C14 120.7(3) . . ?
O6 C7 C8 119.0(3) . . ?
O6 C7 C12 118.1(3) . . ?
C8 C7 C12 122.3(3) . . ?
C7 C8 C9 117.7(3) . . ?
C7 C8 C14 122.2(3) . . ?
C9 C8 C14 120.1(3) . . ?
C8 C9 H9 118.8 . . ?
C10 C9 C8 122.4(3) . . ?
C10 C9 H9 118.8 . . ?
C9 C10 C20 114.7(4) . . ?
C9 C10 C20' 135.2(5) . . ?
C11 C10 C9 117.5(3) . . ?
C11 C10 C20 127.8(4) . . ?
C11 C10 C20' 107.3(5) . . ?
C10 C11 H11 118.7 . . ?
C10 C11 C12 122.6(4) . . ?
C12 C11 H11 118.7 . . ?
C7 C12 C11 117.4(3) . . ?
C7 C12 C15 122.6(3) . . ?
C11 C12 C15 119.7(4) . . ?
C2 C13 C2 113.7(4) . 7_575 ?
C2 C13 H13A 108.8 . . ?
C2 C13 H13A 108.8 7_575 . ?
C2 C13 H13B 108.8 . . ?
C2 C13 H13B 108.8 7_575 . ?
H13A C13 H13B 107.7 . . ?
C6 C14 H14A 109.0 . . ?
C6 C14 H14B 109.0 . . ?
C8 C14 C6 112.8(3) . . ?
C8 C14 H14A 109.0 . . ?
C8 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C12 C15 C12 110.3(4) 7_575 . ?
C12 C15 H15A 109.6 . . ?
C12 C15 H15A 109.6 7_575 . ?
C12 C15 H15B 109.6 . . ?
C12 C15 H15B 109.6 7_575 . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C4 108.2(3) . . ?
C18 C16 C4 111.9(3) . . ?
C18 C16 C17 109.5(4) . . ?
C19 C16 C4 110.9(3) . . ?
C19 C16 C17 108.6(4) . . ?
C19 C16 C18 107.7(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C10 109.1(4) . . ?
C21 C20 C22 110.2(5) . . ?
C22 C20 C10 112.3(5) . . ?
C23 C20 C10 106.9(4) . . ?
C23 C20 C21 109.5(5) . . ?
C23 C20 C22 108.6(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21' C20' C10 113.5(7) . . ?
C21' C20' C22' 107.4(8) . . ?
C22' C20' C10 115.4(8) . . ?
C23' C20' C10 103.3(7) . . ?
C23' C20' C21' 107.9(7) . . ?
C23' C20' C22' 108.8(7) . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21E 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C20' C22' H22D 109.5 . . ?
C20' C22' H22E 109.5 . . ?
C20' C22' H22F 109.5 . . ?
H22D C22' H22E 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
C20' C23' H23D 109.5 . . ?
C20' C23' H23E 109.5 . . ?
C20' C23' H23F 109.5 . . ?
H23D C23' H23E 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
O7 C24 H24A 109.5 . . ?
O7 C24 H24B 109.5 . . ?
O7 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O8 C25 H25A 109.5 . . ?
O8 C25 H25B 109.5 . . ?
O8 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O9 C26 H26A 109.5 . . ?
O9 C26 H26B 109.5 . . ?
O9 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O10 C27 H27A 109.5 . . ?
O10 C27 H27B 109.5 . . ?
O10 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O11 C28 H28A 109.5 . . ?
O11 C28 H28B 109.5 . . ?
O11 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O2 P1 C29 102.2(3) . . ?
O2 P1 C35 116.1(4) . . ?
O2 P1 C36 114.0(4) . . ?
C35 P1 C29 106.4(5) . . ?
C36 P1 C29 111.2(6) . . ?
C36 P1 C35 106.7(6) . . ?
C30 C29 P1 120.1(8) . . ?
C34 C29 P1 121.8(8) . . ?
C34 C29 C30 117.3(11) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 C29 120.0(11) . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 119.0 . . ?
C30 C31 C32 122.0(12) . . ?
C32 C31 H31 119.0 . . ?
C31 C32 H32 120.5 . . ?
C33 C32 C31 119.0(12) . . ?
C33 C32 H32 120.5 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.8(12) . . ?
C34 C33 H33 120.1 . . ?
C29 C34 H34 119.0 . . ?
C33 C34 C29 122.0(11) . . ?
C33 C34 H34 119.0 . . ?
P1 C35 H35A 109.5 . . ?
P1 C35 H35B 109.5 . . ?
P1 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
P1 C36 H36A 109.5 . . ?
P1 C36 H36B 109.5 . . ?
P1 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
C37 C38 H38A 106.6 . . ?
C37 C38 H38B 106.6 . . ?
H38A C38 H38B 106.5 . . ?
O13 C38 C37 123.0(19) . . ?
O13 C38 H38A 106.6 . . ?
O13 C38 H38B 106.6 . . ?
C39 O13 C38 117.1(16) . . ?
O13 C39 H39A 108.1 . . ?
O13 C39 H39B 108.1 . . ?
O13 C39 C40 116.8(17) . . ?
H39A C39 H39B 107.3 . . ?
C40 C39 H39A 108.1 . . ?
C40 C39 H39B 108.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N1 C41 C42 179(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O5 C1 C2 -89.4(3) . . . . ?
V1 O5 C1 C6 87.3(3) . . . . ?
V1 O6 C7 C8 -84.5(3) . . . . ?
V1 O6 C7 C12 87.0(3) . . . . ?
V2 O5 C1 C2 90.9(3) . . . . ?
V2 O5 C1 C6 -92.4(3) . . . . ?
V3 O6 C7 C8 96.4(3) . . . . ?
V3 O6 C7 C12 -92.1(4) . . . . ?
O2 P1 C29 C30 85.0(5) . . . . ?
O2 P1 C29 C34 -84.3(5) . . . . ?
O5 C1 C2 C3 179.8(3) . . . . ?
O5 C1 C2 C13 1.5(4) . . . . ?
O5 C1 C6 C5 179.9(3) . . . . ?
O5 C1 C6 C14 -2.0(4) . . . . ?
O6 C7 C8 C9 171.8(3) . . . . ?
O6 C7 C8 C14 -5.0(4) . . . . ?
O6 C7 C12 C11 -172.9(3) . . . . ?
O6 C7 C12 C15 0.5(5) . . . . ?
C1 C2 C3 C4 -0.9(5) . . . . ?
C1 C2 C13 C2 89.6(4) . . . 7_575 ?
C1 C6 C14 C8 -88.6(4) . . . . ?
C2 C1 C6 C5 -3.5(5) . . . . ?
C2 C1 C6 C14 174.5(3) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C2 C3 C4 C16 177.2(3) . . . . ?
C3 C2 C13 C2 -88.6(4) . . . 7_575 ?
C3 C4 C5 C6 0.7(5) . . . . ?
C3 C4 C16 C17 -102.7(4) . . . . ?
C3 C4 C16 C18 18.0(5) . . . . ?
C3 C4 C16 C19 138.2(3) . . . . ?
C4 C5 C6 C1 1.5(5) . . . . ?
C4 C5 C6 C14 -176.6(3) . . . . ?
C5 C4 C16 C17 75.5(4) . . . . ?
C5 C4 C16 C18 -163.8(3) . . . . ?
C5 C4 C16 C19 -43.6(4) . . . . ?
C5 C6 C14 C8 89.3(4) . . . . ?
C6 C1 C2 C3 3.2(4) . . . . ?
C6 C1 C2 C13 -175.1(3) . . . . ?
C7 C8 C9 C10 -0.4(5) . . . . ?
C7 C8 C14 C6 96.4(4) . . . . ?
C7 C12 C15 C12 -92.8(4) . . . 7_575 ?
C8 C7 C12 C11 -1.7(5) . . . . ?
C8 C7 C12 C15 171.8(3) . . . . ?
C8 C9 C10 C11 1.2(5) . . . . ?
C8 C9 C10 C20 -177.6(4) . . . . ?
C8 C9 C10 C20' -175.7(6) . . . . ?
C9 C8 C14 C6 -80.2(4) . . . . ?
C9 C10 C11 C12 -2.4(5) . . . . ?
C9 C10 C20 C21 66.4(5) . . . . ?
C9 C10 C20 C22 -56.1(5) . . . . ?
C9 C10 C20 C23 -175.2(5) . . . . ?
C9 C10 C20' C21' -122.5(7) . . . . ?
C9 C10 C20' C22' 112.8(8) . . . . ?
C9 C10 C20' C23' -5.8(10) . . . . ?
C10 C11 C12 C7 2.6(5) . . . . ?
C10 C11 C12 C15 -171.1(3) . . . . ?
C11 C10 C20 C21 -112.3(5) . . . . ?
C11 C10 C20 C22 125.2(5) . . . . ?
C11 C10 C20 C23 6.1(7) . . . . ?
C11 C10 C20' C21' 60.4(8) . . . . ?
C11 C10 C20' C22' -64.3(8) . . . . ?
C11 C10 C20' C23' 177.0(6) . . . . ?
C11 C12 C15 C12 80.5(5) . . . 7_575 ?
C12 C7 C8 C9 0.6(5) . . . . ?
C12 C7 C8 C14 -176.1(3) . . . . ?
C13 C2 C3 C4 177.4(3) . . . . ?
C14 C8 C9 C10 176.5(3) . . . . ?
C16 C4 C5 C6 -177.6(3) . . . . ?
C20 C10 C11 C12 176.3(4) . . . . ?
C20' C10 C11 C12 175.3(5) . . . . ?
P1 C29 C30 C31 -169.7(6) . . . . ?
P1 C29 C34 C33 169.5(6) . . . . ?
C29 C30 C31 C32 0.0(5) . . . . ?
C30 C29 C34 C33 -0.1(4) . . . . ?
C30 C31 C32 C33 -0.1(5) . . . . ?
C31 C32 C33 C34 0.1(4) . . . . ?
C32 C33 C34 C29 0.0(5) . . . . ?
C34 C29 C30 C31 0.1(4) . . . . ?
C35 P1 C29 C30 -152.8(5) . . . . ?
C35 P1 C29 C34 37.8(6) . . . . ?
C36 P1 C29 C30 -37.0(7) . . . . ?
C36 P1 C29 C34 153.7(6) . . . . ?
C37 C38 O13 C39 170(2) . . . . ?
C38 O13 C39 C40 171.6(19) . . . . ?

_olex2_submission_original_sample_id matrm28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.191
_oxdiff_exptl_absorpt_empirical_full_min 0.533
