# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_matlv08
_database_code_depnum_ccdc_archive 'CCDC 1587539'
_audit_update_record             
;
2017-11-24 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_vrf_PLAT971_matlv08             
; 
PROBLEM: _B Check Calcd Resid. Dens.  0.90A   From Hf1 .. 3.06 eA-3 
         _B Check Calcd Resid. Dens.  1.10A   From Hf1 .. 2.73 eA-3 
RESPONSE: These peaks may be due to contributions from a small domain 
set off by a crack or they may be a result of an imperfect absorption 
correction. 
;

_vrf_STRVA01_matlv08             
; 
PROBLEM: _C           Flack test results are ambiguous. 
           From the CIF: _refine_ls_abs_structure_Flack    0.485 
           From the CIF: _refine_ls_abs_structure_Flack_su    0.016 
RESPONSE: The intensity data were ultimately modeled as twinned by 
inversion twin in non-centrosymmetric space group Pna2(1). A solution 
and refinement in centrosymmetric space group Pnma was also considered, 
which resulted in a larger R1 (strong data) of 0.077 versus the current 
structure's 0.055. 
;

_vrf_PLAT301_matlv08             
; 
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 5% 
RESPONSE: Two bridging methoxy ligands were modeled as disordered 
over two positions each with a common component mass ratio of 
0.64(2):0.36(2) due to their adjacency. 
;

_vrf_PLAT860_matlv08             
; 
PROBLEM: _G Number of Least-Squares Restraints ............. 3 
RESPONSE: For each disordered methoxy ligand, O--C bond lengths 
were restrained to be similar and anisotropic displacement 
parameters were constrained to be equivalent. 
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            matlv08
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H39 Hf O19 V5, C16 H36 N'
_chemical_formula_sum            'C29 H75 Hf N O19 V5'
_chemical_formula_weight         1175.09


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   21.282(6)
_cell_length_b                   18.958(6)
_cell_length_c                   11.572(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4669(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    4030
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.34

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_F_000             2380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    3.240
_shelx_estimated_absorpt_T_min   0.464
_shelx_estimated_absorpt_T_max   0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3584
_exptl_absorpt_correction_T_max  0.4923
_exptl_absorpt_process_details   'SADABS-2016/2 (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            88214
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_av_R_equivalents  0.1275
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.914
_diffrn_reflns_theta_max         28.831
_diffrn_reflns_theta_full        28.700
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12086
_reflns_number_gt                8723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX3 (Bruker, 2017)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
; 
The intensity data were ultimately modeled as twinned by 
inversion twin in non-centrosymmetric space group Pna2(1). A solution 
and refinement in centrosymmetric space group Pnma was also considered, 
which resulted in a larger R1 (strong data) of 0.077 versus the current 
structure's 0.055. 
  
Two bridging methoxy ligands were modeled as disordered over two 
positions each with a common component mass ratio of 0.64(2):0.36(2) 
due to their adjacency. For each disordered methoxy ligand, O--C 
bond lengths were restrained to be similar and anisotropic 
displacement parameters were constrained to be equivalent. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0527P)²+6.6637P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.485(16)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         12086
_refine_ls_number_parameters     519
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1243
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.47507(2) 0.88456(2) 0.49385(9) 0.02446(11) Uani 1 1 d . . . . .
V1 V 0.58896(7) 0.67551(8) 0.5113(2) 0.0201(4) Uani 1 1 d . . . . .
V2 V 0.60184(12) 0.82538(16) 0.3619(2) 0.0211(5) Uani 1 1 d . . . . .
V3 V 0.59610(12) 0.82923(15) 0.6501(2) 0.0214(5) Uani 1 1 d . . . . .
V4 V 0.46245(13) 0.73697(18) 0.6409(2) 0.0236(6) Uani 1 1 d . . . . .
V5 V 0.46849(11) 0.73336(18) 0.3541(2) 0.0226(6) Uani 1 1 d . . . . .
O1 O 0.6282(3) 0.6030(4) 0.5161(9) 0.030(2) Uani 1 1 d . . . . .
O2 O 0.6505(5) 0.8552(6) 0.2676(9) 0.029(2) Uani 1 1 d . . . . .
O3 O 0.6404(5) 0.8596(6) 0.7492(8) 0.025(2) Uani 1 1 d . . . . .
O4 O 0.4159(5) 0.7075(6) 0.7400(10) 0.032(3) Uani 1 1 d . . . . .
O5 O 0.4252(5) 0.6991(6) 0.2565(10) 0.034(3) Uani 1 1 d . . . . .
O6 O 0.4258(3) 0.9697(3) 0.4887(13) 0.0300(17) Uani 1 1 d . . . . .
O7 O 0.6365(5) 0.7301(6) 0.3912(8) 0.022(2) Uani 1 1 d . . . . .
O8 O 0.6329(5) 0.7331(6) 0.6299(8) 0.025(2) Uani 1 1 d . . . . .
O9 O 0.5219(5) 0.6572(7) 0.6259(10) 0.028(3) Uani 1 1 d . . . . .
O10 O 0.5265(5) 0.6530(6) 0.3858(9) 0.021(2) Uani 1 1 d . . . . .
O11 O 0.6416(3) 0.8603(3) 0.5065(11) 0.0222(16) Uani 1 1 d . . . . .
O12 O 0.5263(4) 0.7847(6) 0.7415(9) 0.024(2) Uani 1 1 d . . . . .
O13 O 0.4205(3) 0.7054(3) 0.4969(13) 0.0270(14) Uani 1 1 d D . . . .
O14 O 0.5379(5) 0.7796(7) 0.2624(9) 0.025(2) Uani 1 1 d . . . . .
O15 O 0.5380(5) 0.9148(7) 0.6244(10) 0.025(3) Uani 1 1 d . . . . .
O16 O 0.4212(5) 0.8337(6) 0.6186(9) 0.026(2) Uani 1 1 d D . . . .
O17 O 0.4272(5) 0.8284(7) 0.3654(10) 0.031(3) Uani 1 1 d . . . . .
O18 O 0.5434(5) 0.9100(6) 0.3717(10) 0.024(2) Uani 1 1 d . . . . .
O19 O 0.5269(3) 0.7875(3) 0.5016(12) 0.0179(13) Uani 1 1 d . . . . .
C1 C 0.3851(5) 1.0277(5) 0.492(2) 0.040(3) Uani 1 1 d . . . . .
H1A H 0.402858 1.066340 0.446299 0.060 Uiso 1 1 calc R U . . .
H1B H 0.379829 1.043153 0.572345 0.060 Uiso 1 1 calc R U . . .
H1C H 0.344229 1.014163 0.460175 0.060 Uiso 1 1 calc R U . . .
C2 C 0.7011(6) 0.7125(8) 0.3832(15) 0.051(4) Uani 1 1 d . . . . .
H2A H 0.724053 0.751656 0.347409 0.076 Uiso 1 1 calc R U . . .
H2B H 0.706020 0.670008 0.335851 0.076 Uiso 1 1 calc R U . . .
H2C H 0.717880 0.703759 0.460715 0.076 Uiso 1 1 calc R U . . .
C3 C 0.6524(6) 0.6991(7) 0.7315(11) 0.035(3) Uani 1 1 d . . . . .
H3A H 0.681890 0.729504 0.773324 0.052 Uiso 1 1 calc R U . . .
H3B H 0.673135 0.654578 0.711692 0.052 Uiso 1 1 calc R U . . .
H3C H 0.615753 0.689558 0.780282 0.052 Uiso 1 1 calc R U . . .
C4 C 0.4958(7) 0.5877(6) 0.6229(13) 0.036(3) Uani 1 1 d . . . . .
H4A H 0.458534 0.585864 0.672573 0.053 Uiso 1 1 calc R U . . .
H4B H 0.527065 0.553766 0.650772 0.053 Uiso 1 1 calc R U . . .
H4C H 0.483940 0.575898 0.543443 0.053 Uiso 1 1 calc R U . . .
C5 C 0.5488(6) 0.6158(7) 0.2871(12) 0.037(3) Uani 1 1 d . . . . .
H5A H 0.513248 0.603070 0.237517 0.056 Uiso 1 1 calc R U . . .
H5B H 0.570626 0.572875 0.311968 0.056 Uiso 1 1 calc R U . . .
H5C H 0.577976 0.645864 0.243818 0.056 Uiso 1 1 calc R U . . .
C6 C 0.7087(5) 0.8637(8) 0.5169(14) 0.043(4) Uani 1 1 d . . . . .
H6A H 0.727498 0.867971 0.439877 0.065 Uiso 1 1 calc R U . . .
H6B H 0.724179 0.820619 0.554197 0.065 Uiso 1 1 calc R U . . .
H6C H 0.720368 0.904727 0.563676 0.065 Uiso 1 1 calc R U . . .
C7 C 0.5083(11) 0.8206(11) 0.8378(13) 0.041(5) Uani 1 1 d . . . . .
H7A H 0.544993 0.828891 0.887103 0.061 Uiso 1 1 calc R U . . .
H7B H 0.477119 0.792785 0.880381 0.061 Uiso 1 1 calc R U . . .
H7C H 0.489818 0.865896 0.815316 0.061 Uiso 1 1 calc R U . . .
C8 C 0.3554(6) 0.7008(9) 0.495(3) 0.035(4) Uani 0.639(18) 1 d D . P A 1
H8A H 0.341522 0.684612 0.418746 0.052 Uiso 0.639(18) 1 calc R U P A 1
H8B H 0.341377 0.667207 0.554063 0.052 Uiso 0.639(18) 1 calc R U P A 1
H8C H 0.337241 0.747297 0.511032 0.052 Uiso 0.639(18) 1 calc R U P A 1
C8' C 0.3727(12) 0.6557(15) 0.482(4) 0.035(4) Uani 0.361(18) 1 d D . P A 5
H8D H 0.362204 0.652052 0.399811 0.052 Uiso 0.361(18) 1 calc R U P A 5
H8E H 0.386991 0.609720 0.510430 0.052 Uiso 0.361(18) 1 calc R U P A 5
H8F H 0.335445 0.670492 0.525468 0.052 Uiso 0.361(18) 1 calc R U P A 5
C9 C 0.5169(10) 0.8149(13) 0.1530(17) 0.046(5) Uani 1 1 d . . . . .
H9A H 0.552364 0.817928 0.099130 0.069 Uiso 1 1 calc R U . . .
H9B H 0.501735 0.862540 0.170639 0.069 Uiso 1 1 calc R U . . .
H9C H 0.482970 0.787452 0.117707 0.069 Uiso 1 1 calc R U . . .
C10 C 0.5630(8) 0.9832(9) 0.6414(16) 0.032(4) Uani 1 1 d . . . . .
H10A H 0.563289 0.994256 0.724147 0.049 Uiso 1 1 calc R U . . .
H10B H 0.536994 1.017777 0.600451 0.049 Uiso 1 1 calc R U . . .
H10C H 0.606041 0.985014 0.611395 0.049 Uiso 1 1 calc R U . . .
C11 C 0.3702(12) 0.8559(19) 0.686(3) 0.043(7) Uani 0.639(18) 1 d D . P A 1
H11A H 0.357480 0.903410 0.661725 0.064 Uiso 0.639(18) 1 calc R U P A 1
H11B H 0.334979 0.823276 0.675072 0.064 Uiso 0.639(18) 1 calc R U P A 1
H11C H 0.382416 0.856680 0.767369 0.064 Uiso 0.639(18) 1 calc R U P A 1
C11' C 0.3560(11) 0.842(3) 0.628(4) 0.043(7) Uani 0.361(18) 1 d D . P A 5
H11D H 0.345276 0.892067 0.614281 0.064 Uiso 0.361(18) 1 calc R U P A 5
H11E H 0.335032 0.812980 0.569746 0.064 Uiso 0.361(18) 1 calc R U P A 5
H11F H 0.342202 0.828472 0.705045 0.064 Uiso 0.361(18) 1 calc R U P A 5
C12 C 0.3705(9) 0.8484(10) 0.306(2) 0.050(5) Uani 1 1 d . . . . .
H12A H 0.370400 0.827880 0.228530 0.075 Uiso 1 1 calc R U . . .
H12B H 0.368414 0.899945 0.300454 0.075 Uiso 1 1 calc R U . . .
H12C H 0.334030 0.831087 0.349454 0.075 Uiso 1 1 calc R U . . .
C13 C 0.5658(11) 0.9777(10) 0.3388(18) 0.047(5) Uani 1 1 d . . . . .
H13A H 0.589223 0.973835 0.266111 0.070 Uiso 1 1 calc R U . . .
H13B H 0.593516 0.996163 0.399241 0.070 Uiso 1 1 calc R U . . .
H13C H 0.530127 1.009708 0.328233 0.070 Uiso 1 1 calc R U . . .
N1 N 0.6683(3) 0.3983(4) 0.5070(13) 0.022(2) Uani 1 1 d . . . . .
C14 C 0.7180(4) 0.3407(5) 0.5047(17) 0.030(3) Uani 1 1 d . . . . .
H14A H 0.715192 0.316159 0.429411 0.036 Uiso 1 1 calc R U . . .
H14B H 0.759775 0.363499 0.508509 0.036 Uiso 1 1 calc R U . . .
C15 C 0.7147(6) 0.2879(8) 0.5957(13) 0.043(3) Uani 1 1 d . . . . .
H15A H 0.670318 0.274794 0.609297 0.052 Uiso 1 1 calc R U . . .
H15B H 0.731725 0.307916 0.668283 0.052 Uiso 1 1 calc R U . . .
C16 C 0.7532(7) 0.2205(7) 0.5617(15) 0.051(4) Uani 1 1 d . . . . .
H16A H 0.746155 0.183828 0.621126 0.061 Uiso 1 1 calc R U . . .
H16B H 0.736774 0.202191 0.487522 0.061 Uiso 1 1 calc R U . . .
C17 C 0.8236(7) 0.2324(9) 0.5493(14) 0.065(5) Uani 1 1 d . . . . .
H17A H 0.844977 0.186728 0.542641 0.098 Uiso 1 1 calc R U . . .
H17B H 0.839427 0.257457 0.617436 0.098 Uiso 1 1 calc R U . . .
H17C H 0.831885 0.260517 0.479936 0.098 Uiso 1 1 calc R U . . .
C18 C 0.6650(6) 0.4325(7) 0.6251(12) 0.031(3) Uani 1 1 d . . . . .
H18A H 0.631349 0.468528 0.622112 0.038 Uiso 1 1 calc R U . . .
H18B H 0.651178 0.395904 0.680519 0.038 Uiso 1 1 calc R U . . .
C19 C 0.7220(6) 0.4671(7) 0.6749(12) 0.035(3) Uani 1 1 d . . . . .
H19A H 0.756368 0.432126 0.681753 0.042 Uiso 1 1 calc R U . . .
H19B H 0.736295 0.505393 0.623093 0.042 Uiso 1 1 calc R U . . .
C20 C 0.7070(8) 0.4963(10) 0.7902(15) 0.037(4) Uani 1 1 d . . . . .
H20A H 0.693981 0.456901 0.841007 0.044 Uiso 1 1 calc R U . . .
H20B H 0.670525 0.528305 0.782128 0.044 Uiso 1 1 calc R U . . .
C21 C 0.7585(7) 0.5356(9) 0.8488(14) 0.048(4) Uani 1 1 d . . . . .
H21A H 0.744687 0.549767 0.926203 0.073 Uiso 1 1 calc R U . . .
H21B H 0.769043 0.577677 0.803618 0.073 Uiso 1 1 calc R U . . .
H21C H 0.795584 0.505240 0.855194 0.073 Uiso 1 1 calc R U . . .
C22 C 0.6042(4) 0.3641(5) 0.4890(19) 0.030(2) Uani 1 1 d . . . . .
H22A H 0.606931 0.331305 0.422556 0.037 Uiso 1 1 calc R U . . .
H22B H 0.593760 0.335781 0.558297 0.037 Uiso 1 1 calc R U . . .
C23 C 0.5517(5) 0.4156(6) 0.4672(16) 0.045(5) Uani 1 1 d . . . . .
H23A H 0.560996 0.443434 0.396898 0.054 Uiso 1 1 calc R U . . .
H23B H 0.548300 0.448603 0.533171 0.054 Uiso 1 1 calc R U . . .
C24 C 0.4892(5) 0.3764(7) 0.4515(12) 0.038(3) Uani 1 1 d . . . . .
H24A H 0.482653 0.344088 0.517658 0.045 Uiso 1 1 calc R U . . .
H24B H 0.491133 0.347548 0.380263 0.045 Uiso 1 1 calc R U . . .
C25 C 0.4336(6) 0.4279(7) 0.4434(14) 0.047(4) Uani 1 1 d . . . . .
H25A H 0.395028 0.401557 0.426687 0.070 Uiso 1 1 calc R U . . .
H25B H 0.441389 0.461986 0.381354 0.070 Uiso 1 1 calc R U . . .
H25C H 0.428914 0.452982 0.516927 0.070 Uiso 1 1 calc R U . . .
C26 C 0.6856(6) 0.4526(6) 0.4167(12) 0.030(3) Uani 1 1 d . . . . .
H26A H 0.655176 0.491973 0.421980 0.036 Uiso 1 1 calc R U . . .
H26B H 0.727526 0.471717 0.436076 0.036 Uiso 1 1 calc R U . . .
C27 C 0.6870(6) 0.4274(7) 0.2941(12) 0.032(3) Uani 1 1 d . . . . .
H27A H 0.648443 0.399961 0.278080 0.039 Uiso 1 1 calc R U . . .
H27B H 0.723478 0.395618 0.283535 0.039 Uiso 1 1 calc R U . . .
C28 C 0.6917(8) 0.4889(10) 0.2064(14) 0.033(4) Uani 1 1 d . . . . .
H28A H 0.687950 0.470381 0.126746 0.040 Uiso 1 1 calc R U . . .
H28B H 0.656984 0.522690 0.219598 0.040 Uiso 1 1 calc R U . . .
C29 C 0.7535(7) 0.5258(7) 0.2202(13) 0.042(3) Uani 1 1 d . . . . .
H29A H 0.762532 0.553331 0.150505 0.063 Uiso 1 1 calc R U . . .
H29B H 0.786754 0.490856 0.232143 0.063 Uiso 1 1 calc R U . . .
H29C H 0.751522 0.557450 0.287137 0.063 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O6 1.925(6) . ?
Hf1 O16 2.080(11) . ?
Hf1 O18 2.085(12) . ?
Hf1 O17 2.093(12) . ?
Hf1 O15 2.100(11) . ?
Hf1 O19 2.147(5) . ?
V1 O1 1.610(7) . ?
V1 O9 1.979(11) . ?
V1 O8 1.988(11) . ?
V1 O7 2.006(10) . ?
V1 O10 2.014(11) . ?
V1 O19 2.503(6) . ?
V2 O2 1.606(12) . ?
V2 O7 1.981(11) . ?
V2 O14 1.982(11) . ?
V2 O11 1.989(11) . ?
V2 O18 2.033(12) . ?
V2 O19 2.383(11) . ?
V3 O3 1.592(11) . ?
V3 O8 1.997(11) . ?
V3 O12 2.010(10) . ?
V3 O11 2.011(11) . ?
V3 O15 2.061(12) . ?
V3 O19 2.398(11) . ?
V4 O4 1.615(11) . ?
V4 O9 1.980(12) . ?
V4 O13 1.984(13) . ?
V4 O12 2.004(11) . ?
V4 O16 2.049(12) . ?
V4 O19 2.323(11) . ?
V5 O5 1.596(11) . ?
V5 O10 1.995(11) . ?
V5 O17 2.009(13) . ?
V5 O13 2.014(13) . ?
V5 O14 2.019(11) . ?
V5 O19 2.348(11) . ?
O6 C1 1.400(10) . ?
O7 C2 1.417(15) . ?
O8 C3 1.403(15) . ?
O9 C4 1.430(17) . ?
O10 C5 1.425(16) . ?
O11 C6 1.436(12) . ?
O12 C7 1.36(2) . ?
O13 C8 1.389(13) . ?
O13 C8' 1.396(16) . ?
O14 C9 1.50(2) . ?
O15 C10 1.415(19) . ?
O16 C11 1.40(2) . ?
O16 C11' 1.40(2) . ?
O17 C12 1.44(2) . ?
O18 C13 1.42(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8' H8D 0.9800 . ?
C8' H8E 0.9800 . ?
C8' H8F 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11' H11D 0.9800 . ?
C11' H11E 0.9800 . ?
C11' H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N1 C26 1.512(16) . ?
N1 C18 1.514(19) . ?
N1 C14 1.520(11) . ?
N1 C22 1.525(12) . ?
C14 C15 1.45(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.568(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.52(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.494(16) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.48(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.49(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.506(15) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.533(15) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.538(16) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.497(18) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.55(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.50(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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
O6 Hf1 O16 96.3(5) . . ?
O6 Hf1 O18 99.5(5) . . ?
O16 Hf1 O18 164.2(4) . . ?
O6 Hf1 O17 98.0(5) . . ?
O16 Hf1 O17 89.4(3) . . ?
O18 Hf1 O17 88.6(5) . . ?
O6 Hf1 O15 98.1(5) . . ?
O16 Hf1 O15 88.8(5) . . ?
O18 Hf1 O15 88.8(3) . . ?
O17 Hf1 O15 163.9(5) . . ?
O6 Hf1 O19 177.8(3) . . ?
O16 Hf1 O19 81.7(4) . . ?
O18 Hf1 O19 82.4(4) . . ?
O17 Hf1 O19 81.0(4) . . ?
O15 Hf1 O19 82.9(4) . . ?
O1 V1 O9 101.6(5) . . ?
O1 V1 O8 101.6(5) . . ?
O9 V1 O8 88.5(5) . . ?
O1 V1 O7 101.7(4) . . ?
O9 V1 O7 156.7(5) . . ?
O8 V1 O7 87.6(3) . . ?
O1 V1 O10 100.8(5) . . ?
O9 V1 O10 88.3(3) . . ?
O8 V1 O10 157.6(5) . . ?
O7 V1 O10 86.7(4) . . ?
O1 V1 O19 179.2(4) . . ?
O9 V1 O19 78.4(4) . . ?
O8 V1 O19 79.2(4) . . ?
O7 V1 O19 78.4(4) . . ?
O10 V1 O19 78.4(4) . . ?
O2 V2 O7 101.4(5) . . ?
O2 V2 O14 101.7(5) . . ?
O7 V2 O14 87.5(5) . . ?
O2 V2 O11 100.4(5) . . ?
O7 V2 O11 90.0(4) . . ?
O14 V2 O11 157.8(4) . . ?
O2 V2 O18 98.9(6) . . ?
O7 V2 O18 159.7(5) . . ?
O14 V2 O18 87.6(5) . . ?
O11 V2 O18 87.2(4) . . ?
O2 V2 O19 176.7(5) . . ?
O7 V2 O19 81.8(3) . . ?
O14 V2 O19 78.6(4) . . ?
O11 V2 O19 79.2(3) . . ?
O18 V2 O19 77.9(4) . . ?
O3 V3 O8 100.5(5) . . ?
O3 V3 O12 102.2(5) . . ?
O8 V3 O12 88.2(5) . . ?
O3 V3 O11 101.8(5) . . ?
O8 V3 O11 88.9(4) . . ?
O12 V3 O11 156.0(4) . . ?
O3 V3 O15 100.0(5) . . ?
O8 V3 O15 159.5(5) . . ?
O12 V3 O15 87.9(5) . . ?
O11 V3 O15 86.5(4) . . ?
O3 V3 O19 177.7(4) . . ?
O8 V3 O19 81.7(3) . . ?
O12 V3 O19 77.5(4) . . ?
O11 V3 O19 78.5(3) . . ?
O15 V3 O19 77.8(4) . . ?
O4 V4 O9 101.0(6) . . ?
O4 V4 O13 102.4(5) . . ?
O9 V4 O13 89.1(4) . . ?
O4 V4 O12 99.2(5) . . ?
O9 V4 O12 87.9(5) . . ?
O13 V4 O12 158.3(4) . . ?
O4 V4 O16 97.8(5) . . ?
O9 V4 O16 161.1(5) . . ?
O13 V4 O16 88.4(4) . . ?
O12 V4 O16 87.7(5) . . ?
O4 V4 O19 175.9(5) . . ?
O9 V4 O19 82.9(4) . . ?
O13 V4 O19 78.9(4) . . ?
O12 V4 O19 79.4(4) . . ?
O16 V4 O19 78.2(4) . . ?
O5 V5 O10 100.2(6) . . ?
O5 V5 O17 99.1(5) . . ?
O10 V5 O17 160.7(5) . . ?
O5 V5 O13 100.4(5) . . ?
O10 V5 O13 87.8(4) . . ?
O17 V5 O13 87.8(4) . . ?
O5 V5 O14 103.1(5) . . ?
O10 V5 O14 88.6(5) . . ?
O17 V5 O14 88.0(5) . . ?
O13 V5 O14 156.4(4) . . ?
O5 V5 O19 176.5(5) . . ?
O10 V5 O19 82.7(3) . . ?
O17 V5 O19 78.0(4) . . ?
O13 V5 O19 77.7(4) . . ?
O14 V5 O19 78.8(4) . . ?
C1 O6 Hf1 173.7(10) . . ?
C2 O7 V2 124.3(9) . . ?
C2 O7 V1 114.4(8) . . ?
V2 O7 V1 113.7(5) . . ?
C3 O8 V1 117.7(9) . . ?
C3 O8 V3 115.9(8) . . ?
V1 O8 V3 113.4(5) . . ?
C4 O9 V1 115.2(9) . . ?
C4 O9 V4 117.2(8) . . ?
V1 O9 V4 112.7(6) . . ?
C5 O10 V5 115.9(9) . . ?
C5 O10 V1 117.5(8) . . ?
V5 O10 V1 112.3(5) . . ?
C6 O11 V2 120.6(9) . . ?
C6 O11 V3 115.0(10) . . ?
V2 O11 V3 113.2(3) . . ?
C7 O12 V4 120.7(11) . . ?
C7 O12 V3 115.4(11) . . ?
V4 O12 V3 112.7(5) . . ?
C8 O13 V4 118.8(18) . . ?
C8' O13 V4 129(2) . . ?
C8 O13 V5 120.7(18) . . ?
C8' O13 V5 116(2) . . ?
V4 O13 V5 112.4(3) . . ?
C9 O14 V2 119.9(12) . . ?
C9 O14 V5 114.8(10) . . ?
V2 O14 V5 112.8(5) . . ?
C10 O15 V3 118.4(10) . . ?
C10 O15 Hf1 126.1(10) . . ?
V3 O15 Hf1 105.8(5) . . ?
C11 O16 V4 122.1(17) . . ?
C11' O16 V4 121(2) . . ?
C11 O16 Hf1 132.3(17) . . ?
C11' O16 Hf1 123(2) . . ?
V4 O16 Hf1 105.5(5) . . ?
C12 O17 V5 124.9(11) . . ?
C12 O17 Hf1 127.7(12) . . ?
V5 O17 Hf1 106.8(5) . . ?
C13 O18 V2 119.5(11) . . ?
C13 O18 Hf1 128.6(12) . . ?
V2 O18 Hf1 106.4(5) . . ?
Hf1 O19 V4 94.6(3) . . ?
Hf1 O19 V5 94.2(3) . . ?
V4 O19 V5 90.7(2) . . ?
Hf1 O19 V2 93.3(3) . . ?
V4 O19 V2 172.1(3) . . ?
V5 O19 V2 89.6(5) . . ?
Hf1 O19 V3 93.6(3) . . ?
V4 O19 V3 90.1(5) . . ?
V5 O19 V3 172.1(3) . . ?
V2 O19 V3 88.60(19) . . ?
Hf1 O19 V1 179.0(3) . . ?
V4 O19 V1 86.0(3) . . ?
V5 O19 V1 86.6(3) . . ?
V2 O19 V1 86.1(3) . . ?
V3 O19 V1 85.6(3) . . ?
O6 C1 H1A 109.5 . . ?
O6 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O6 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O7 C2 H2A 109.5 . . ?
O7 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O7 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O8 C3 H3A 109.5 . . ?
O8 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O8 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O9 C4 H4A 109.5 . . ?
O9 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O9 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O10 C5 H5A 109.5 . . ?
O10 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O10 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O11 C6 H6A 109.5 . . ?
O11 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O11 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O12 C7 H7A 109.5 . . ?
O12 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O12 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O13 C8 H8A 109.5 . . ?
O13 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O13 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O13 C8' H8D 109.5 . . ?
O13 C8' H8E 109.5 . . ?
H8D C8' H8E 109.5 . . ?
O13 C8' H8F 109.5 . . ?
H8D C8' H8F 109.5 . . ?
H8E C8' H8F 109.5 . . ?
O14 C9 H9A 109.5 . . ?
O14 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O14 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O15 C10 H10A 109.5 . . ?
O15 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O15 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O16 C11 H11A 109.5 . . ?
O16 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O16 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O16 C11' H11D 109.5 . . ?
O16 C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
O16 C11' H11F 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
O17 C12 H12A 109.5 . . ?
O17 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O17 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O18 C13 H13A 109.5 . . ?
O18 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O18 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C26 N1 C18 110.1(10) . . ?
C26 N1 C14 107.9(10) . . ?
C18 N1 C14 110.8(12) . . ?
C26 N1 C22 114.4(12) . . ?
C18 N1 C22 105.3(11) . . ?
C14 N1 C22 108.3(7) . . ?
C15 C14 N1 116.7(13) . . ?
C15 C14 H14A 108.1 . . ?
N1 C14 H14A 108.1 . . ?
C15 C14 H14B 108.1 . . ?
N1 C14 H14B 108.1 . . ?
H14A C14 H14B 107.3 . . ?
C14 C15 C16 110.7(13) . . ?
C14 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C15 114.7(12) . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C15 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N1 119.9(11) . . ?
C19 C18 H18A 107.3 . . ?
N1 C18 H18A 107.3 . . ?
C19 C18 H18B 107.3 . . ?
N1 C18 H18B 107.3 . . ?
H18A C18 H18B 106.9 . . ?
C20 C19 C18 109.7(12) . . ?
C20 C19 H19A 109.7 . . ?
C18 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
C18 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C19 C20 C21 116.1(14) . . ?
C19 C20 H20A 108.3 . . ?
C21 C20 H20A 108.3 . . ?
C19 C20 H20B 108.3 . . ?
C21 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N1 114.3(8) . . ?
C23 C22 H22A 108.7 . . ?
N1 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
N1 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C22 C23 C24 110.4(9) . . ?
C22 C23 H23A 109.6 . . ?
C24 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
C24 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 C25 111.5(10) . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N1 116.3(10) . . ?
C27 C26 H26A 108.2 . . ?
N1 C26 H26A 108.2 . . ?
C27 C26 H26B 108.2 . . ?
N1 C26 H26B 108.2 . . ?
H26A C26 H26B 107.4 . . ?
C26 C27 C28 112.5(11) . . ?
C26 C27 H27A 109.1 . . ?
C28 C27 H27A 109.1 . . ?
C26 C27 H27B 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C29 C28 C27 109.8(13) . . ?
C29 C28 H28A 109.7 . . ?
C27 C28 H28A 109.7 . . ?
C29 C28 H28B 109.7 . . ?
C27 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
C26 N1 C14 C15 172.1(12) . . . . ?
C18 N1 C14 C15 51.5(13) . . . . ?
C22 N1 C14 C15 -63.6(17) . . . . ?
N1 C14 C15 C16 161.8(11) . . . . ?
C14 C15 C16 C17 64.6(17) . . . . ?
C26 N1 C18 C19 -60.6(13) . . . . ?
C14 N1 C18 C19 58.7(15) . . . . ?
C22 N1 C18 C19 175.7(12) . . . . ?
N1 C18 C19 C20 -179.9(13) . . . . ?
C18 C19 C20 C21 -177.1(14) . . . . ?
C26 N1 C22 C23 -48.8(19) . . . . ?
C18 N1 C22 C23 72.1(18) . . . . ?
C14 N1 C22 C23 -169.3(16) . . . . ?
N1 C22 C23 C24 -179.4(15) . . . . ?
C22 C23 C24 C25 173.3(14) . . . . ?
C18 N1 C26 C27 -176.6(10) . . . . ?
C14 N1 C26 C27 62.3(14) . . . . ?
C22 N1 C26 C27 -58.3(14) . . . . ?
N1 C26 C27 C28 168.4(10) . . . . ?
C26 C27 C28 C29 65.5(16) . . . . ?

_refine_diff_density_max         3.557
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.160

####################################################################### 
# 
# 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_matlv07
_database_code_depnum_ccdc_archive 'CCDC 1587541'
_audit_update_record             
;
2017-11-24 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_vrf_RINTA01_matlv07             
; 
PROBLEM: _B  The value of Rint is greater than 0.18 
            Rint given   0.194 
RESPONSE: The high angle intensity data were extremely weak due 
to the small crystal size. 
;

_vrf_PLAT026_matlv07             
; 
PROBLEM: _C Ratio Observed / Unique Reflections (too) Low .. 48 % 
RESPONSE: See above. 
;

_vrf_PLAT341_matlv07             
; 
PROBLEM: _C Low Bond Precision on C-C Bonds ............... 0.01267 Ang. 
RESPONSE: See above. 
;

_vrf_PLAT020_matlv07             
; 
PROBLEM: _G The value of Rint is greater than 0.12 ......... 0.194 
RESPONSE: See above. 
;

_vrf_PLAT083_matlv07             
; 
PROBLEM: _G SHELXL Second Parameter in WGHT Unusually Large .. 10.18 
RESPONSE: See above. 
;

_vrf_PLAT301_matlv07             
; 
PROBLEM: _G Main Residue Disorder .............. (Resd  1) .. 13 % 
RESPONSE: Methyl groups of five bridging methoxy ligands were 
modeled as disordered over two positions (0.61:0.39, all related 
due to adjacency). 
;

_vrf_PLAT302_matlv07             
; 
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2) .. 47 % 
RESPONSE: Two n-butyl groups are modeled as disordered over two positions 
each (0.70:0.30 and 0.52:0.48, for C22-C25 and C26-C29, respectively). 
;

_vrf_PLAT860_matlv07             
; 
PROBLEM: _G Number of Least-Squares Restraints ............. 23 
RESPONSE: O--C distances within each of the disordered methoxy groups 
were restrained to be similar. Anisotropic displacement parameters for 
each disordered methyl group pair were constrained to be equivalent. 
Analogous bond lengths and angles between the two positions of each 
n-butyl group disorder were restrained to be similar. Anisotropic 
displacement parameters for pairs of proximal atoms were constrained 
to be equivalent. 
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            matlv07
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H39 O19 Ti V5, C16 H36 N'
_chemical_formula_sum            'C29 H75 N O19 Ti V5'
_chemical_formula_weight         1044.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   11.5947(17)
_cell_length_b                   18.157(3)
_cell_length_c                   23.178(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.2149(18)
_cell_angle_gamma                90
_cell_volume                     4750.3(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    3888
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      22.30

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             2180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.169
_shelx_estimated_absorpt_T_min   0.736
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4156
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_process_details   'SADABS-2016/2 (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51687
_diffrn_reflns_av_unetI/netI     0.1198
_diffrn_reflns_av_R_equivalents  0.1942
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.804
_diffrn_reflns_theta_max         25.295
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8626
_reflns_number_gt                4161
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
; 
Methyl groups of five bridging methoxy ligands were modeled as 
disordered over two positions (0.61:0.39, all related due to 
adjacency). Two n-butyl groups are modeled as disordered over two 
positions each (0.70:0.30 and 0.52:0.48, for C22-C25 and C26-C29, 
respectively). 
  
O--C distances within each of the disordered methoxy groups were 
restrained to be similar. Anisotropic displacement parameters for 
each disordered methyl group pair were constrained to be equivalent. 
Analogous bond lengths and angles between the two positions of each 
n-butyl group disorder were restrained to be similar. Anisotropic 
displacement parameters for pairs of proximal atoms were constrained 
to be equivalent. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0429P)²+10.1763P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8626
_refine_ls_number_parameters     546
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.1626
_refine_ls_wR_factor_gt          0.1260
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.75566(11) 0.34857(7) 0.62212(6) 0.0393(3) Uani 1 1 d . . . . .
V2 V 0.63578(10) 0.20131(7) 0.66846(5) 0.0322(3) Uani 1 1 d . . . . .
V3 V 0.92516(10) 0.20848(7) 0.68130(5) 0.0344(3) Uani 1 1 d . . . . .
V4 V 0.88225(12) 0.24238(9) 0.53770(6) 0.0501(4) Uani 1 1 d . . . . .
V5 V 0.59235(11) 0.23463(8) 0.52467(5) 0.0426(4) Uani 1 1 d . . . . .
Ti1 Ti 0.76117(12) 0.10332(8) 0.58582(6) 0.0427(4) Uani 1 1 d . . . . .
O1 O 0.7531(5) 0.4347(3) 0.6358(3) 0.0580(16) Uani 1 1 d . . . . .
O2 O 0.5514(4) 0.1860(3) 0.7131(2) 0.0418(13) Uani 1 1 d . . . . .
O3 O 1.0404(4) 0.1978(3) 0.7342(2) 0.0450(13) Uani 1 1 d . . . . .
O4 O 0.9659(5) 0.2544(4) 0.4921(2) 0.0723(19) Uani 1 1 d . . . . .
O5 O 0.4775(4) 0.2422(3) 0.4713(2) 0.0569(16) Uani 1 1 d . . . . .
O6 O 0.7631(5) 0.0069(3) 0.5714(2) 0.0606(16) Uani 1 1 d . . . . .
O7 O 0.6515(4) 0.3103(3) 0.67210(19) 0.0349(12) Uani 1 1 d D . . . .
O8 O 0.8938(4) 0.3159(3) 0.6852(2) 0.0426(13) Uani 1 1 d D . . . .
O9 O 0.8610(4) 0.3448(3) 0.5648(2) 0.0561(16) Uani 1 1 d D . . . .
O10 O 0.6179(4) 0.3383(3) 0.5531(2) 0.0437(13) Uani 1 1 d D . . . .
O11 O 0.7954(4) 0.1928(2) 0.72350(18) 0.0331(11) Uani 1 1 d . . . . .
O12 O 1.0016(4) 0.2261(3) 0.6140(2) 0.0427(13) Uani 1 1 d . . . . .
O13 O 0.7229(5) 0.2486(3) 0.4826(2) 0.0599(17) Uani 1 1 d . . . . .
O14 O 0.5157(4) 0.2134(3) 0.59208(19) 0.0361(12) Uani 1 1 d D . . . .
O15 O 0.6573(4) 0.0971(3) 0.6423(2) 0.0378(12) Uani 1 1 d . . . . .
O16 O 0.9008(4) 0.1029(3) 0.65351(19) 0.0388(12) Uani 1 1 d . . . . .
O17 O 0.8649(5) 0.1312(3) 0.5336(2) 0.0534(15) Uani 1 1 d . . . . .
O18 O 0.6214(4) 0.1248(3) 0.5220(2) 0.0514(15) Uani 1 1 d . . . . .
O19 O 0.7587(4) 0.2138(2) 0.60216(18) 0.0302(11) Uani 1 1 d . . . . .
C1 C 0.7711(10) -0.0679(5) 0.5549(6) 0.116(5) Uani 1 1 d . . . . .
H1A H 0.782910 -0.070362 0.514365 0.173 Uiso 1 1 calc R U . . .
H1B H 0.697706 -0.093652 0.556705 0.173 Uiso 1 1 calc R U . . .
H1C H 0.838137 -0.091424 0.582095 0.173 Uiso 1 1 calc R U . . .
C2 C 0.6600(14) 0.3498(8) 0.7252(6) 0.072(4) Uani 0.607(7) 1 d D . P A 1
H2A H 0.606430 0.328087 0.747645 0.108 Uiso 0.607(7) 1 calc R U P A 1
H2B H 0.741570 0.347531 0.748822 0.108 Uiso 0.607(7) 1 calc R U P A 1
H2C H 0.637827 0.401285 0.715945 0.108 Uiso 0.607(7) 1 calc R U P A 1
C3 C 0.9934(19) 0.3664(15) 0.6947(11) 0.076(8) Uani 0.607(7) 1 d D . P A 1
H3A H 0.964600 0.416996 0.695596 0.113 Uiso 0.607(7) 1 calc R U P A 1
H3B H 1.048089 0.354970 0.732587 0.113 Uiso 0.607(7) 1 calc R U P A 1
H3C H 1.034693 0.361190 0.662492 0.113 Uiso 0.607(7) 1 calc R U P A 1
C4 C 0.8339(17) 0.3952(8) 0.5142(6) 0.064(5) Uani 0.607(7) 1 d D . P A 1
H4A H 0.823720 0.445176 0.528151 0.096 Uiso 0.607(7) 1 calc R U P A 1
H4B H 0.899151 0.394673 0.493736 0.096 Uiso 0.607(7) 1 calc R U P A 1
H4C H 0.760685 0.379431 0.486703 0.096 Uiso 0.607(7) 1 calc R U P A 1
C5 C 0.5178(11) 0.3845(8) 0.5471(7) 0.065(4) Uani 0.607(7) 1 d D . P A 1
H5A H 0.459380 0.371522 0.510812 0.097 Uiso 0.607(7) 1 calc R U P A 1
H5B H 0.482568 0.377985 0.581392 0.097 Uiso 0.607(7) 1 calc R U P A 1
H5C H 0.541870 0.435930 0.544898 0.097 Uiso 0.607(7) 1 calc R U P A 1
C9 C 0.4000(9) 0.2344(11) 0.5942(8) 0.062(5) Uani 0.607(7) 1 d D . P A 1
H9A H 0.351119 0.238181 0.553847 0.093 Uiso 0.607(7) 1 calc R U P A 1
H9B H 0.366088 0.197407 0.616337 0.093 Uiso 0.607(7) 1 calc R U P A 1
H9C H 0.402309 0.282226 0.614064 0.093 Uiso 0.607(7) 1 calc R U P A 1
C2' C 0.5469(15) 0.3496(12) 0.6735(10) 0.072(4) Uani 0.393(7) 1 d D . P A 5
H2D H 0.504558 0.324419 0.699878 0.108 Uiso 0.393(7) 1 calc R U P A 5
H2E H 0.567550 0.399619 0.688218 0.108 Uiso 0.393(7) 1 calc R U P A 5
H2F H 0.496126 0.352053 0.633479 0.108 Uiso 0.393(7) 1 calc R U P A 5
C3' C 0.970(3) 0.369(2) 0.7224(19) 0.076(8) Uani 0.393(7) 1 d D . P A 5
H3D H 0.934273 0.418026 0.715899 0.113 Uiso 0.393(7) 1 calc R U P A 5
H3E H 0.979616 0.355133 0.764123 0.113 Uiso 0.393(7) 1 calc R U P A 5
H3F H 1.047711 0.369514 0.712407 0.113 Uiso 0.393(7) 1 calc R U P A 5
C4' C 0.886(3) 0.4171(9) 0.5423(11) 0.064(5) Uani 0.393(7) 1 d D . P A 5
H4D H 0.863539 0.455782 0.567283 0.096 Uiso 0.393(7) 1 calc R U P A 5
H4E H 0.970233 0.421007 0.543079 0.096 Uiso 0.393(7) 1 calc R U P A 5
H4F H 0.839449 0.423021 0.501512 0.096 Uiso 0.393(7) 1 calc R U P A 5
C5' C 0.592(2) 0.4047(9) 0.5202(9) 0.065(4) Uani 0.393(7) 1 d D . P A 5
H5D H 0.523505 0.396773 0.486955 0.097 Uiso 0.393(7) 1 calc R U P A 5
H5E H 0.572781 0.443498 0.545991 0.097 Uiso 0.393(7) 1 calc R U P A 5
H5F H 0.660384 0.419523 0.505074 0.097 Uiso 0.393(7) 1 calc R U P A 5
C9' C 0.3955(12) 0.1927(17) 0.5775(13) 0.062(5) Uani 0.393(7) 1 d D . P A 5
H9D H 0.360486 0.206271 0.536337 0.093 Uiso 0.393(7) 1 calc R U P A 5
H9E H 0.389093 0.139369 0.582345 0.093 Uiso 0.393(7) 1 calc R U P A 5
H9F H 0.353321 0.218152 0.603844 0.093 Uiso 0.393(7) 1 calc R U P A 5
C6 C 0.8127(8) 0.2151(5) 0.7840(3) 0.070(3) Uani 1 1 d . . . . .
H6A H 0.885254 0.192622 0.807331 0.105 Uiso 1 1 calc R U . . .
H6B H 0.744894 0.199207 0.799538 0.105 Uiso 1 1 calc R U . . .
H6C H 0.819621 0.268894 0.786571 0.105 Uiso 1 1 calc R U . . .
C7 C 1.1185(7) 0.2507(7) 0.6199(4) 0.100(4) Uani 1 1 d . . . . .
H7A H 1.166967 0.234046 0.658037 0.149 Uiso 1 1 calc R U . . .
H7B H 1.119503 0.304576 0.618255 0.149 Uiso 1 1 calc R U . . .
H7C H 1.150594 0.230468 0.587638 0.149 Uiso 1 1 calc R U . . .
C8 C 0.7119(9) 0.2444(7) 0.4233(4) 0.102(4) Uani 1 1 d . . . . .
H8A H 0.779379 0.269003 0.412694 0.152 Uiso 1 1 calc R U . . .
H8B H 0.638211 0.268583 0.402935 0.152 Uiso 1 1 calc R U . . .
H8C H 0.710021 0.192586 0.411300 0.152 Uiso 1 1 calc R U . . .
C10 C 0.5630(9) 0.0466(5) 0.6377(4) 0.083(3) Uani 1 1 d . . . . .
H10A H 0.501646 0.057422 0.602030 0.125 Uiso 1 1 calc R U . . .
H10B H 0.529332 0.050888 0.672719 0.125 Uiso 1 1 calc R U . . .
H10C H 0.592514 -0.003629 0.635261 0.125 Uiso 1 1 calc R U . . .
C11 C 0.9166(7) 0.0460(4) 0.6973(3) 0.049(2) Uani 1 1 d . . . . .
H11A H 0.849089 0.045838 0.716145 0.074 Uiso 1 1 calc R U . . .
H11B H 0.989742 0.054956 0.727303 0.074 Uiso 1 1 calc R U . . .
H11C H 0.921724 -0.001785 0.678362 0.074 Uiso 1 1 calc R U . . .
C12 C 0.9660(7) 0.0885(5) 0.5282(4) 0.070(3) Uani 1 1 d . . . . .
H12A H 1.028978 0.094290 0.564150 0.105 Uiso 1 1 calc R U . . .
H12B H 0.994396 0.105604 0.493824 0.105 Uiso 1 1 calc R U . . .
H12C H 0.943535 0.036496 0.522978 0.105 Uiso 1 1 calc R U . . .
C13 C 0.5873(9) 0.0830(5) 0.4706(4) 0.087(4) Uani 1 1 d . . . . .
H13A H 0.648073 0.086540 0.447440 0.131 Uiso 1 1 calc R U . . .
H13B H 0.511843 0.101608 0.446909 0.131 Uiso 1 1 calc R U . . .
H13C H 0.577936 0.031432 0.481096 0.131 Uiso 1 1 calc R U . . .
N1 N 0.6528(5) 0.6247(3) 0.6815(2) 0.0375(15) Uani 1 1 d D . . . .
C14 C 0.6868(7) 0.6107(5) 0.7482(3) 0.055(2) Uani 1 1 d . . . . .
H14A H 0.757461 0.640992 0.765006 0.066 Uiso 1 1 calc R U . . .
H14B H 0.621480 0.629065 0.765308 0.066 Uiso 1 1 calc R U . . .
C15 C 0.7130(7) 0.5338(5) 0.7689(3) 0.052(2) Uani 1 1 d . . . . .
H15A H 0.765190 0.510665 0.745713 0.062 Uiso 1 1 calc R U . . .
H15B H 0.638146 0.505374 0.761583 0.062 Uiso 1 1 calc R U . . .
C16 C 0.7716(8) 0.5301(5) 0.8333(3) 0.068(3) Uani 1 1 d . . . . .
H16A H 0.848213 0.556497 0.839821 0.081 Uiso 1 1 calc R U . . .
H16B H 0.721376 0.556456 0.855868 0.081 Uiso 1 1 calc R U . . .
C17 C 0.7938(10) 0.4543(6) 0.8576(4) 0.109(4) Uani 1 1 d . . . . .
H17A H 0.718583 0.427450 0.851364 0.163 Uiso 1 1 calc R U . . .
H17B H 0.829837 0.456888 0.900141 0.163 Uiso 1 1 calc R U . . .
H17C H 0.847461 0.428560 0.837340 0.163 Uiso 1 1 calc R U . . .
C18 C 0.5566(7) 0.5707(5) 0.6508(3) 0.049(2) Uani 1 1 d . . . . .
H18A H 0.537795 0.581607 0.607840 0.058 Uiso 1 1 calc R U . . .
H18B H 0.590247 0.520410 0.656039 0.058 Uiso 1 1 calc R U . . .
C19 C 0.4452(7) 0.5705(5) 0.6707(4) 0.063(3) Uani 1 1 d . . . . .
H19A H 0.411324 0.620815 0.666543 0.076 Uiso 1 1 calc R U . . .
H19B H 0.462222 0.557343 0.713299 0.076 Uiso 1 1 calc R U . . .
C20 C 0.3548(7) 0.5174(5) 0.6365(4) 0.063(3) Uani 1 1 d . . . . .
H20A H 0.345759 0.527594 0.593734 0.076 Uiso 1 1 calc R U . . .
H20B H 0.387319 0.466962 0.643922 0.076 Uiso 1 1 calc R U . . .
C21 C 0.2357(9) 0.5180(6) 0.6493(5) 0.095(4) Uani 1 1 d . . . . .
H21A H 0.243088 0.514732 0.692152 0.143 Uiso 1 1 calc R U . . .
H21B H 0.189930 0.475947 0.629735 0.143 Uiso 1 1 calc R U . . .
H21C H 0.194953 0.563880 0.634346 0.143 Uiso 1 1 calc R U . . .
C22 C 0.7626(7) 0.6132(5) 0.6564(4) 0.057(2) Uani 0.699(9) 1 d D . P B 1
H22A H 0.822314 0.650476 0.674440 0.068 Uiso 0.699(9) 1 calc R U P B 1
H22B H 0.796151 0.564229 0.669541 0.068 Uiso 0.699(9) 1 calc R U P B 1
C23 C 0.7459(11) 0.6175(8) 0.5901(5) 0.049(4) Uani 0.699(9) 1 d D . P B 1
H23A H 0.704146 0.663978 0.576191 0.058 Uiso 0.699(9) 1 calc R U P B 1
H23B H 0.693893 0.576363 0.572077 0.058 Uiso 0.699(9) 1 calc R U P B 1
C24 C 0.8604(10) 0.6143(8) 0.5673(5) 0.055(4) Uani 0.699(9) 1 d D . P B 1
H24A H 0.909744 0.657913 0.581754 0.066 Uiso 0.699(9) 1 calc R U P B 1
H24B H 0.906000 0.569764 0.583340 0.066 Uiso 0.699(9) 1 calc R U P B 1
C25 C 0.8336(12) 0.6123(8) 0.5000(5) 0.077(4) Uani 0.699(9) 1 d D . P B 1
H25A H 0.793735 0.565948 0.485820 0.115 Uiso 0.699(9) 1 calc R U P B 1
H25B H 0.907837 0.615896 0.486681 0.115 Uiso 0.699(9) 1 calc R U P B 1
H25C H 0.782103 0.653788 0.483998 0.115 Uiso 0.699(9) 1 calc R U P B 1
C26 C 0.6050(8) 0.7023(5) 0.6714(4) 0.067(3) Uani 0.482(11) 1 d D . P B 1
H26A H 0.556116 0.713206 0.700282 0.080 Uiso 0.482(11) 1 calc R U P B 1
H26B H 0.553117 0.705819 0.631156 0.080 Uiso 0.482(11) 1 calc R U P B 1
C27 C 0.7024(12) 0.7593(8) 0.6778(9) 0.063(4) Uani 0.482(11) 1 d D . P B 1
H27A H 0.740351 0.755545 0.643749 0.075 Uiso 0.482(11) 1 calc R U P B 1
H27B H 0.763580 0.749461 0.714424 0.075 Uiso 0.482(11) 1 calc R U P B 1
C28 C 0.653(3) 0.8374(6) 0.6805(10) 0.089(11) Uani 0.482(11) 1 d D . P B 1
H28A H 0.710261 0.873657 0.671002 0.107 Uiso 0.482(11) 1 calc R U P B 1
H28B H 0.577847 0.842501 0.650557 0.107 Uiso 0.482(11) 1 calc R U P B 1
C29 C 0.634(2) 0.8526(12) 0.7391(11) 0.103(6) Uani 0.482(11) 1 d D . P B 1
H29A H 0.568938 0.821851 0.745923 0.154 Uiso 0.482(11) 1 calc R U P B 1
H29B H 0.613540 0.904671 0.741741 0.154 Uiso 0.482(11) 1 calc R U P B 1
H29C H 0.706294 0.841521 0.769067 0.154 Uiso 0.482(11) 1 calc R U P B 1
C22' C 0.7626(7) 0.6132(5) 0.6564(4) 0.057(2) Uani 0.301(9) 1 d D . P B 5
H22C H 0.830696 0.639866 0.681170 0.068 Uiso 0.301(9) 1 calc R U P B 5
H22D H 0.782587 0.560134 0.657352 0.068 Uiso 0.301(9) 1 calc R U P B 5
C23' C 0.740(2) 0.641(2) 0.5937(9) 0.049(4) Uani 0.301(9) 1 d D . P B 5
H23C H 0.686911 0.684548 0.588535 0.058 Uiso 0.301(9) 1 calc R U P B 5
H23D H 0.702142 0.602285 0.565538 0.058 Uiso 0.301(9) 1 calc R U P B 5
C24' C 0.862(3) 0.6619(14) 0.5830(12) 0.055(4) Uani 0.301(9) 1 d D . P B 5
H24C H 0.923652 0.629274 0.606453 0.066 Uiso 0.301(9) 1 calc R U P B 5
H24D H 0.861930 0.655755 0.540548 0.066 Uiso 0.301(9) 1 calc R U P B 5
C25' C 0.888(3) 0.7424(15) 0.6017(13) 0.077(4) Uani 0.301(9) 1 d D . P B 5
H25D H 0.844359 0.775126 0.570735 0.115 Uiso 0.301(9) 1 calc R U P B 5
H25E H 0.973509 0.751794 0.607351 0.115 Uiso 0.301(9) 1 calc R U P B 5
H25F H 0.864272 0.751738 0.638872 0.115 Uiso 0.301(9) 1 calc R U P B 5
C26' C 0.6050(8) 0.7023(5) 0.6714(4) 0.067(3) Uani 0.518(11) 1 d D U P B 5
H26C H 0.600546 0.715267 0.629483 0.080 Uiso 0.518(11) 1 calc R U P B 5
H26D H 0.522904 0.702274 0.677123 0.080 Uiso 0.518(11) 1 calc R U P B 5
C27' C 0.6725(16) 0.7628(7) 0.7097(8) 0.063(4) Uani 0.518(11) 1 d D U P B 5
H27C H 0.754222 0.765063 0.703611 0.075 Uiso 0.518(11) 1 calc R U P B 5
H27D H 0.677432 0.751226 0.751926 0.075 Uiso 0.518(11) 1 calc R U P B 5
C28' C 0.612(3) 0.8377(7) 0.6947(12) 0.089(11) Uani 0.518(11) 1 d D . P B 5
H28C H 0.601258 0.847508 0.651787 0.107 Uiso 0.518(11) 1 calc R U P B 5
H28D H 0.533111 0.836879 0.704071 0.107 Uiso 0.518(11) 1 calc R U P B 5
C29' C 0.683(2) 0.8962(9) 0.7282(11) 0.103(6) Uani 0.518(11) 1 d D . P B 5
H29D H 0.702851 0.883330 0.770403 0.154 Uiso 0.518(11) 1 calc R U P B 5
H29E H 0.637964 0.942323 0.722571 0.154 Uiso 0.518(11) 1 calc R U P B 5
H29F H 0.756180 0.902405 0.714296 0.154 Uiso 0.518(11) 1 calc R U P B 5


_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 1.598(5) . ?
V1 O7 1.981(5) . ?
V1 O10 1.994(5) . ?
V1 O8 1.996(5) . ?
V1 O9 2.001(5) . ?
V2 O2 1.603(5) . ?
V2 O7 1.987(5) . ?
V2 O14 1.998(4) . ?
V2 O11 1.999(4) . ?
V2 O15 2.020(5) . ?
V2 O19 2.334(4) . ?
V2 Ti1 3.1970(18) . ?
V3 O3 1.605(4) . ?
V3 O8 1.989(5) . ?
V3 O12 1.989(5) . ?
V3 O11 1.993(4) . ?
V3 O16 2.021(5) . ?
V3 O19 2.341(4) . ?
V3 Ti1 3.1992(18) . ?
V4 O4 1.604(5) . ?
V4 O13 1.994(5) . ?
V4 O9 1.996(6) . ?
V4 O12 2.002(5) . ?
V4 O17 2.028(6) . ?
V4 O19 2.352(4) . ?
V4 Ti1 3.210(2) . ?
V5 O5 1.603(5) . ?
V5 O10 1.994(5) . ?
V5 O13 1.995(5) . ?
V5 O14 2.003(5) . ?
V5 O18 2.026(5) . ?
V5 O19 2.346(4) . ?
V5 Ti1 3.2025(19) . ?
Ti1 O6 1.783(5) . ?
Ti1 O17 1.958(5) . ?
Ti1 O18 1.968(5) . ?
Ti1 O15 1.975(5) . ?
Ti1 O16 1.980(5) . ?
Ti1 O19 2.042(5) . ?
O6 C1 1.421(10) . ?
O7 C2 1.408(11) . ?
O7 C2' 1.414(13) . ?
O8 C3 1.450(11) . ?
O8 C3' 1.451(13) . ?
O9 C4 1.465(10) . ?
O9 C4' 1.465(12) . ?
O10 C5 1.413(11) . ?
O10 C5' 1.422(13) . ?
O11 C6 1.429(8) . ?
O12 C7 1.402(9) . ?
O13 C8 1.354(9) . ?
O14 C9 1.406(10) . ?
O14 C9' 1.408(12) . ?
O15 C10 1.412(9) . ?
O16 C11 1.430(8) . ?
O17 C12 1.434(8) . ?
O18 C13 1.391(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C2' H2D 0.9800 . ?
C2' H2E 0.9800 . ?
C2' H2F 0.9800 . ?
C3' H3D 0.9800 . ?
C3' H3E 0.9800 . ?
C3' H3F 0.9800 . ?
C4' H4D 0.9800 . ?
C4' H4E 0.9800 . ?
C4' H4F 0.9800 . ?
C5' H5D 0.9800 . ?
C5' H5E 0.9800 . ?
C5' H5F 0.9800 . ?
C9' H9D 0.9800 . ?
C9' H9E 0.9800 . ?
C9' H9F 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N1 C26' 1.513(10) . ?
N1 C26 1.513(10) . ?
N1 C14 1.526(8) . ?
N1 C22 1.530(10) . ?
N1 C22' 1.530(10) . ?
N1 C18 1.532(9) . ?
C14 C15 1.485(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.494(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.488(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.468(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.510(11) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.478(11) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.506(12) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.538(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.521(14) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.514(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.534(14) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.454(19) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C22' C23' 1.505(18) . ?
C22' H22C 0.9900 . ?
C22' H22D 0.9900 . ?
C23' C24' 1.540(19) . ?
C23' H23C 0.9900 . ?
C23' H23D 0.9900 . ?
C24' C25' 1.54(2) . ?
C24' H24C 0.9900 . ?
C24' H24D 0.9900 . ?
C25' H25D 0.9800 . ?
C25' H25E 0.9800 . ?
C25' H25F 0.9800 . ?
C26' C27' 1.512(12) . ?
C26' H26C 0.9900 . ?
C26' H26D 0.9900 . ?
C27' C28' 1.534(14) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28' C29' 1.453(19) . ?
C28' H28C 0.9900 . ?
C28' H28D 0.9900 . ?
C29' H29D 0.9800 . ?
C29' H29E 0.9800 . ?
C29' H29F 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 O7 100.7(2) . . ?
O1 V1 O10 101.7(2) . . ?
O7 V1 O10 87.26(19) . . ?
O1 V1 O8 101.2(2) . . ?
O7 V1 O8 87.85(19) . . ?
O10 V1 O8 157.1(2) . . ?
O1 V1 O9 101.9(3) . . ?
O7 V1 O9 157.3(2) . . ?
O10 V1 O9 87.9(2) . . ?
O8 V1 O9 88.1(2) . . ?
O2 V2 O7 102.0(2) . . ?
O2 V2 O14 100.7(2) . . ?
O7 V2 O14 88.09(19) . . ?
O2 V2 O11 100.8(2) . . ?
O7 V2 O11 89.26(19) . . ?
O14 V2 O11 158.36(19) . . ?
O2 V2 O15 99.6(2) . . ?
O7 V2 O15 158.36(19) . . ?
O14 V2 O15 86.92(19) . . ?
O11 V2 O15 87.68(18) . . ?
O2 V2 O19 175.6(2) . . ?
O7 V2 O19 82.39(17) . . ?
O14 V2 O19 79.20(17) . . ?
O11 V2 O19 79.16(16) . . ?
O15 V2 O19 75.99(17) . . ?
O2 V2 Ti1 135.97(19) . . ?
O7 V2 Ti1 121.99(14) . . ?
O14 V2 Ti1 81.40(13) . . ?
O11 V2 Ti1 81.84(13) . . ?
O15 V2 Ti1 36.38(14) . . ?
O19 V2 Ti1 39.61(11) . . ?
O3 V3 O8 102.3(2) . . ?
O3 V3 O12 100.1(2) . . ?
O8 V3 O12 89.8(2) . . ?
O3 V3 O11 101.4(2) . . ?
O8 V3 O11 87.2(2) . . ?
O12 V3 O11 158.39(19) . . ?
O3 V3 O16 99.2(2) . . ?
O8 V3 O16 158.48(19) . . ?
O12 V3 O16 87.6(2) . . ?
O11 V3 O16 87.44(19) . . ?
O3 V3 O19 175.3(2) . . ?
O8 V3 O19 82.46(17) . . ?
O12 V3 O19 79.28(17) . . ?
O11 V3 O19 79.10(16) . . ?
O16 V3 O19 76.07(17) . . ?
O3 V3 Ti1 135.70(19) . . ?
O8 V3 Ti1 122.03(14) . . ?
O12 V3 Ti1 81.64(15) . . ?
O11 V3 Ti1 81.87(13) . . ?
O16 V3 Ti1 36.49(13) . . ?
O19 V3 Ti1 39.58(11) . . ?
O4 V4 O13 100.5(3) . . ?
O4 V4 O9 102.5(3) . . ?
O13 V4 O9 89.2(2) . . ?
O4 V4 O12 101.6(2) . . ?
O13 V4 O12 157.8(2) . . ?
O9 V4 O12 88.3(2) . . ?
O4 V4 O17 100.0(3) . . ?
O13 V4 O17 87.7(2) . . ?
O9 V4 O17 157.5(2) . . ?
O12 V4 O17 86.3(2) . . ?
O4 V4 O19 175.0(3) . . ?
O13 V4 O19 79.03(18) . . ?
O9 V4 O19 82.47(18) . . ?
O12 V4 O19 78.77(17) . . ?
O17 V4 O19 75.04(18) . . ?
O4 V4 Ti1 135.6(3) . . ?
O13 V4 Ti1 81.52(18) . . ?
O9 V4 Ti1 121.88(15) . . ?
O12 V4 Ti1 81.17(15) . . ?
O17 V4 Ti1 35.62(14) . . ?
O19 V4 Ti1 39.41(11) . . ?
O5 V5 O10 102.1(3) . . ?
O5 V5 O13 101.6(2) . . ?
O10 V5 O13 88.3(2) . . ?
O5 V5 O14 100.4(2) . . ?
O10 V5 O14 88.98(19) . . ?
O13 V5 O14 157.94(19) . . ?
O5 V5 O18 100.1(3) . . ?
O10 V5 O18 157.87(19) . . ?
O13 V5 O18 87.7(2) . . ?
O14 V5 O18 86.6(2) . . ?
O5 V5 O19 175.6(3) . . ?
O10 V5 O19 82.25(18) . . ?
O13 V5 O19 79.14(18) . . ?
O14 V5 O19 78.79(16) . . ?
O18 V5 O19 75.62(17) . . ?
O5 V5 Ti1 136.2(2) . . ?
O10 V5 Ti1 121.79(14) . . ?
O13 V5 Ti1 81.71(16) . . ?
O14 V5 Ti1 81.19(14) . . ?
O18 V5 Ti1 36.08(13) . . ?
O19 V5 Ti1 39.53(11) . . ?
O6 Ti1 O17 95.9(2) . . ?
O6 Ti1 O18 95.6(2) . . ?
O17 Ti1 O18 90.0(2) . . ?
O6 Ti1 O15 95.9(2) . . ?
O17 Ti1 O15 168.2(2) . . ?
O18 Ti1 O15 89.3(2) . . ?
O6 Ti1 O16 95.8(2) . . ?
O17 Ti1 O16 89.1(2) . . ?
O18 Ti1 O16 168.6(2) . . ?
O15 Ti1 O16 89.24(19) . . ?
O6 Ti1 O19 179.9(3) . . ?
O17 Ti1 O19 84.1(2) . . ?
O18 Ti1 O19 84.3(2) . . ?
O15 Ti1 O19 84.10(18) . . ?
O16 Ti1 O19 84.29(18) . . ?
O6 Ti1 V2 133.3(2) . . ?
O17 Ti1 V2 130.84(17) . . ?
O18 Ti1 V2 86.06(14) . . ?
O15 Ti1 V2 37.34(14) . . ?
O16 Ti1 V2 85.93(14) . . ?
O19 Ti1 V2 46.76(12) . . ?
O6 Ti1 V3 133.20(19) . . ?
O17 Ti1 V3 85.47(16) . . ?
O18 Ti1 V3 131.24(16) . . ?
O15 Ti1 V3 86.09(14) . . ?
O16 Ti1 V3 37.37(14) . . ?
O19 Ti1 V3 46.92(12) . . ?
V2 Ti1 V3 62.17(4) . . ?
O6 Ti1 V5 132.88(19) . . ?
O17 Ti1 V5 86.19(16) . . ?
O18 Ti1 V5 37.32(15) . . ?
O15 Ti1 V5 86.14(14) . . ?
O16 Ti1 V5 131.29(15) . . ?
O19 Ti1 V5 47.00(12) . . ?
V2 Ti1 V5 62.30(4) . . ?
V3 Ti1 V5 93.92(5) . . ?
O6 Ti1 V4 133.0(2) . . ?
O17 Ti1 V4 37.10(16) . . ?
O18 Ti1 V4 86.18(17) . . ?
O15 Ti1 V4 131.09(15) . . ?
O16 Ti1 V4 86.27(15) . . ?
O19 Ti1 V4 46.99(13) . . ?
V2 Ti1 V4 93.75(5) . . ?
V3 Ti1 V4 62.16(4) . . ?
V5 Ti1 V4 62.11(4) . . ?
C1 O6 Ti1 173.7(7) . . ?
C2 O7 V1 113.7(7) . . ?
C2' O7 V1 118.5(10) . . ?
C2 O7 V2 122.1(7) . . ?
C2' O7 V2 115.7(10) . . ?
V1 O7 V2 112.8(2) . . ?
C3 O8 V3 118.6(13) . . ?
C3' O8 V3 126(2) . . ?
C3 O8 V1 113.7(14) . . ?
C3' O8 V1 121(2) . . ?
V3 O8 V1 112.5(2) . . ?
C4 O9 V4 110.4(7) . . ?
C4' O9 V4 132.5(12) . . ?
C4 O9 V1 117.3(8) . . ?
C4' O9 V1 113.8(12) . . ?
V4 O9 V1 112.3(2) . . ?
C5 O10 V1 120.9(6) . . ?
C5' O10 V1 112.6(9) . . ?
C5 O10 V5 118.1(7) . . ?
C5' O10 V5 128.7(9) . . ?
V1 O10 V5 112.6(2) . . ?
C6 O11 V3 119.3(5) . . ?
C6 O11 V2 120.4(5) . . ?
V3 O11 V2 111.6(2) . . ?
C7 O12 V3 124.6(5) . . ?
C7 O12 V4 119.8(5) . . ?
V3 O12 V4 112.0(2) . . ?
C8 O13 V4 120.4(6) . . ?
C8 O13 V5 125.7(6) . . ?
V4 O13 V5 112.0(2) . . ?
C9 O14 V2 118.4(8) . . ?
C9' O14 V2 129.3(14) . . ?
C9 O14 V5 124.9(9) . . ?
C9' O14 V5 117.1(13) . . ?
V2 O14 V5 111.6(2) . . ?
C10 O15 Ti1 124.5(5) . . ?
C10 O15 V2 119.0(5) . . ?
Ti1 O15 V2 106.3(2) . . ?
C11 O16 Ti1 120.9(4) . . ?
C11 O16 V3 118.2(4) . . ?
Ti1 O16 V3 106.1(2) . . ?
C12 O17 Ti1 122.9(5) . . ?
C12 O17 V4 117.9(5) . . ?
Ti1 O17 V4 107.3(2) . . ?
C13 O18 Ti1 124.1(5) . . ?
C13 O18 V5 123.1(5) . . ?
Ti1 O18 V5 106.6(2) . . ?
Ti1 O19 V2 93.63(18) . . ?
Ti1 O19 V3 93.50(17) . . ?
V2 O19 V3 89.90(15) . . ?
Ti1 O19 V5 93.47(17) . . ?
V2 O19 V5 90.04(16) . . ?
V3 O19 V5 173.0(2) . . ?
Ti1 O19 V4 93.60(17) . . ?
V2 O19 V4 172.8(2) . . ?
V3 O19 V4 89.67(16) . . ?
V5 O19 V4 89.52(15) . . ?
O6 C1 H1A 109.5 . . ?
O6 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O6 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O7 C2 H2A 109.5 . . ?
O7 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O7 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O8 C3 H3A 109.5 . . ?
O8 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O8 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O9 C4 H4A 109.5 . . ?
O9 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O9 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O10 C5 H5A 109.5 . . ?
O10 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O10 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O14 C9 H9A 109.5 . . ?
O14 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O14 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O7 C2' H2D 109.5 . . ?
O7 C2' H2E 109.5 . . ?
H2D C2' H2E 109.5 . . ?
O7 C2' H2F 109.5 . . ?
H2D C2' H2F 109.5 . . ?
H2E C2' H2F 109.5 . . ?
O8 C3' H3D 109.5 . . ?
O8 C3' H3E 109.5 . . ?
H3D C3' H3E 109.5 . . ?
O8 C3' H3F 109.5 . . ?
H3D C3' H3F 109.5 . . ?
H3E C3' H3F 109.5 . . ?
O9 C4' H4D 109.5 . . ?
O9 C4' H4E 109.5 . . ?
H4D C4' H4E 109.5 . . ?
O9 C4' H4F 109.5 . . ?
H4D C4' H4F 109.5 . . ?
H4E C4' H4F 109.5 . . ?
O10 C5' H5D 109.5 . . ?
O10 C5' H5E 109.5 . . ?
H5D C5' H5E 109.5 . . ?
O10 C5' H5F 109.5 . . ?
H5D C5' H5F 109.5 . . ?
H5E C5' H5F 109.5 . . ?
O14 C9' H9D 109.5 . . ?
O14 C9' H9E 109.5 . . ?
H9D C9' H9E 109.5 . . ?
O14 C9' H9F 109.5 . . ?
H9D C9' H9F 109.5 . . ?
H9E C9' H9F 109.5 . . ?
O11 C6 H6A 109.5 . . ?
O11 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O11 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O12 C7 H7A 109.5 . . ?
O12 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O12 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O13 C8 H8A 109.5 . . ?
O13 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O13 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O15 C10 H10A 109.5 . . ?
O15 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O15 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O16 C11 H11A 109.5 . . ?
O16 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O16 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O17 C12 H12A 109.5 . . ?
O17 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O17 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O18 C13 H13A 109.5 . . ?
O18 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O18 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C26' N1 C14 108.2(6) . . ?
C26 N1 C14 108.2(6) . . ?
C26 N1 C22 112.1(6) . . ?
C14 N1 C22 108.5(6) . . ?
C26' N1 C22' 112.1(6) . . ?
C14 N1 C22' 108.5(6) . . ?
C26' N1 C18 108.8(6) . . ?
C26 N1 C18 108.8(6) . . ?
C14 N1 C18 110.8(6) . . ?
C22 N1 C18 108.5(6) . . ?
C22' N1 C18 108.5(6) . . ?
C15 C14 N1 118.1(6) . . ?
C15 C14 H14A 107.8 . . ?
N1 C14 H14A 107.8 . . ?
C15 C14 H14B 107.8 . . ?
N1 C14 H14B 107.8 . . ?
H14A C14 H14B 107.1 . . ?
C14 C15 C16 112.2(7) . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C15 114.8(8) . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C15 C16 H16B 108.6 . . ?
H16A C16 H16B 107.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N1 117.1(7) . . ?
C19 C18 H18A 108.0 . . ?
N1 C18 H18A 108.0 . . ?
C19 C18 H18B 108.0 . . ?
N1 C18 H18B 108.0 . . ?
H18A C18 H18B 107.3 . . ?
C18 C19 C20 113.0(7) . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C21 C20 C19 117.3(8) . . ?
C21 C20 H20A 108.0 . . ?
C19 C20 H20A 108.0 . . ?
C21 C20 H20B 108.0 . . ?
C19 C20 H20B 108.0 . . ?
H20A C20 H20B 107.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N1 117.2(7) . . ?
C23 C22 H22A 108.0 . . ?
N1 C22 H22A 108.0 . . ?
C23 C22 H22B 108.0 . . ?
N1 C22 H22B 108.0 . . ?
H22A C22 H22B 107.3 . . ?
C22 C23 C24 115.4(9) . . ?
C22 C23 H23A 108.4 . . ?
C24 C23 H23A 108.4 . . ?
C22 C23 H23B 108.4 . . ?
C24 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
C25 C24 C23 111.3(9) . . ?
C25 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N1 C26 C27 112.5(9) . . ?
N1 C26 H26A 109.1 . . ?
C27 C26 H26A 109.1 . . ?
N1 C26 H26B 109.1 . . ?
C27 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
C26 C27 C28 111.2(10) . . ?
C26 C27 H27A 109.4 . . ?
C28 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C29 C28 C27 110.5(12) . . ?
C29 C28 H28A 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C23' C22' N1 110.1(14) . . ?
C23' C22' H22C 109.6 . . ?
N1 C22' H22C 109.6 . . ?
C23' C22' H22D 109.6 . . ?
N1 C22' H22D 109.6 . . ?
H22C C22' H22D 108.2 . . ?
C22' C23' C24' 105.8(17) . . ?
C22' C23' H23C 110.6 . . ?
C24' C23' H23C 110.6 . . ?
C22' C23' H23D 110.6 . . ?
C24' C23' H23D 110.6 . . ?
H23C C23' H23D 108.7 . . ?
C25' C24' C23' 109(2) . . ?
C25' C24' H24C 110.0 . . ?
C23' C24' H24C 110.0 . . ?
C25' C24' H24D 110.0 . . ?
C23' C24' H24D 110.0 . . ?
H24C C24' H24D 108.3 . . ?
C24' C25' H25D 109.5 . . ?
C24' C25' H25E 109.5 . . ?
H25D C25' H25E 109.5 . . ?
C24' C25' H25F 109.5 . . ?
H25D C25' H25F 109.5 . . ?
H25E C25' H25F 109.5 . . ?
C27' C26' N1 117.6(9) . . ?
C27' C26' H26C 107.9 . . ?
N1 C26' H26C 107.9 . . ?
C27' C26' H26D 107.9 . . ?
N1 C26' H26D 107.9 . . ?
H26C C26' H26D 107.2 . . ?
C26' C27' C28' 111.3(9) . . ?
C26' C27' H27C 109.4 . . ?
C28' C27' H27C 109.4 . . ?
C26' C27' H27D 109.4 . . ?
C28' C27' H27D 109.4 . . ?
H27C C27' H27D 108.0 . . ?
C29' C28' C27' 110.8(12) . . ?
C29' C28' H28C 109.5 . . ?
C27' C28' H28C 109.5 . . ?
C29' C28' H28D 109.5 . . ?
C27' C28' H28D 109.5 . . ?
H28C C28' H28D 108.1 . . ?
C28' C29' H29D 109.5 . . ?
C28' C29' H29E 109.5 . . ?
H29D C29' H29E 109.5 . . ?
C28' C29' H29F 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 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
C26' N1 C14 C15 167.8(7) . . . . ?
C26 N1 C14 C15 167.8(7) . . . . ?
C22 N1 C14 C15 -70.4(9) . . . . ?
C22' N1 C14 C15 -70.4(9) . . . . ?
C18 N1 C14 C15 48.6(9) . . . . ?
N1 C14 C15 C16 166.6(7) . . . . ?
C14 C15 C16 C17 176.6(8) . . . . ?
C26' N1 C18 C19 -60.6(9) . . . . ?
C26 N1 C18 C19 -60.6(9) . . . . ?
C14 N1 C18 C19 58.2(9) . . . . ?
C22 N1 C18 C19 177.2(7) . . . . ?
C22' N1 C18 C19 177.2(7) . . . . ?
N1 C18 C19 C20 178.1(7) . . . . ?
C18 C19 C20 C21 -174.4(9) . . . . ?
C26 N1 C22 C23 -66.1(10) . . . . ?
C14 N1 C22 C23 174.5(8) . . . . ?
C18 N1 C22 C23 54.1(10) . . . . ?
N1 C22 C23 C24 173.4(9) . . . . ?
C22 C23 C24 C25 175.1(11) . . . . ?
C14 N1 C26 C27 82.2(11) . . . . ?
C22 N1 C26 C27 -37.4(11) . . . . ?
C18 N1 C26 C27 -157.3(10) . . . . ?
N1 C26 C27 C28 -168.0(13) . . . . ?
C26 C27 C28 C29 78(2) . . . . ?
C26' N1 C22' C23' -49.2(17) . . . . ?
C14 N1 C22' C23' -168.6(16) . . . . ?
C18 N1 C22' C23' 70.9(17) . . . . ?
N1 C22' C23' C24' 153.7(18) . . . . ?
C22' C23' C24' C25' -89(3) . . . . ?
C14 N1 C26' C27' 44.8(13) . . . . ?
C22' N1 C26' C27' -74.7(12) . . . . ?
C18 N1 C26' C27' 165.4(11) . . . . ?
N1 C26' C27' C28' -179.2(19) . . . . ?
C26' C27' C28' C29' -175(2) . . . . ?

_refine_diff_density_max         0.526
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.092

####################################################################### 
# 
# 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_matlv05
_database_code_depnum_ccdc_archive 'CCDC 1587540'
_audit_update_record             
;
2017-11-24 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_vrf_STRVA01_matlv05             
; 
PROBLEM: _C           Flack test results are ambiguous. 
           From the CIF: _refine_ls_abs_structure_Flack    0.480 
           From the CIF: _refine_ls_abs_structure_Flack_su    0.030 
RESPONSE: The crystal was an inversion twin whose component mass 
ratio refined to 0.52(3):0.48(3). A model in centrosymmetric space 
group Pnma resulted in a significantly worse structure and an 
increase in R1 (strong data) from 4.4 to 13.2 %. 
;

_vrf_PLAT301_matlv05             
; 
PROBLEM: _G Main Residue Disorder ..............(Resd  1) .. 5 % 
RESPONSE: Two adjacent methoxy groups are modeled as disordered over 
two positions each (both 0.66:0.34 due to proximity, as well as refining 
to the common value when refined independently). 
;

_vrf_PLAT860_matlv05             
; 
PROBLEM: _G Number of Least-Squares Restraints ............. 9 
RESPONSE: For both methoxy group disorders the O--C bond lengths 
were restrained to be similar. Anisotropic displacement parameters 
for atom pair C12/C12' were restrained to be similar. 
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            matlv05
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, C13 H39 O19 V5 Zr'
_chemical_formula_sum            'C29 H75 N O19 V5 Zr'
_chemical_formula_weight         1087.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   21.402(2)
_cell_length_b                   18.960(2)
_cell_length_c                   11.5527(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4687.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    3841
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      31.49

_exptl_crystal_description       block
_exptl_crystal_colour            blue-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_F_000             2252
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.236
_shelx_estimated_absorpt_T_min   0.665
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6100
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            134612
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.903
_diffrn_reflns_theta_max         31.590
_diffrn_reflns_theta_full        31.506
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             15660
_reflns_number_gt                12165
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
; 
The crystal was an inversion twin whose component mass ratio 
refined to 0.52(3):0.48(3). A model in centrosymmetric space 
group Pnma resulted in a significantly worse structure and an 
increase in R1 (strong data) from 4.4 to 13.2 %. 
  
Two adjacent methoxy groups are modeled as disordered over two 
positions each (both 0.66:0.34 due to proximity, as well as refining 
to the common value when refined independently). The O--C bond 
lengths were restrained to be similar. Anisotropic displacement 
parameters for atom pair C12/C12' were restrained to be similar. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0477P)²+2.0027P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.48(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15660
_refine_ls_number_parameters     535
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.47524(2) 0.11481(2) 0.76443(5) 0.01890(9) Uani 1 1 d . . . . .
V1 V 0.58859(3) 0.32464(3) 0.74577(8) 0.01820(15) Uani 1 1 d . . . . .
V2 V 0.60205(4) 0.17527(4) 0.89574(7) 0.01973(17) Uani 1 1 d . . . . .
V3 V 0.59531(4) 0.16976(4) 0.60705(8) 0.02000(17) Uani 1 1 d . . . . .
V4 V 0.46246(4) 0.26213(4) 0.61575(7) 0.01877(16) Uani 1 1 d . . . . .
V5 V 0.46909(4) 0.26738(5) 0.90345(7) 0.01856(17) Uani 1 1 d . . . . .
O1 O 0.62704(15) 0.39700(15) 0.7379(3) 0.0257(8) Uani 1 1 d . . . . .
O2 O 0.64993(18) 0.1466(2) 0.9917(4) 0.0303(9) Uani 1 1 d . . . . .
O3 O 0.63972(19) 0.1386(2) 0.5077(4) 0.0302(9) Uani 1 1 d . . . . .
O4 O 0.41529(18) 0.2920(2) 0.5194(3) 0.0283(8) Uani 1 1 d . . . . .
O5 O 0.42666(17) 0.3024(2) 1.0026(3) 0.0271(8) Uani 1 1 d . . . . .
O6 O 0.42597(13) 0.02982(15) 0.7706(4) 0.0259(7) Uani 1 1 d . . . . .
O7 O 0.63662(16) 0.27100(19) 0.8649(3) 0.0217(7) Uani 1 1 d . . . . .
O8 O 0.63202(16) 0.26617(18) 0.6264(3) 0.0215(7) Uani 1 1 d . . . . .
O9 O 0.52088(16) 0.34323(17) 0.6303(3) 0.0198(7) Uani 1 1 d . . . . .
O10 O 0.52720(16) 0.34698(18) 0.8711(3) 0.0203(7) Uani 1 1 d . . . . .
O11 O 0.64131(12) 0.13936(14) 0.7504(4) 0.0229(6) Uani 1 1 d . . . . .
O12 O 0.52634(16) 0.21413(18) 0.5160(3) 0.0225(8) Uani 1 1 d . . . . .
O13 O 0.42119(12) 0.29450(14) 0.7612(4) 0.0220(5) Uani 1 1 d D . . . .
O14 O 0.53746(16) 0.2224(2) 0.9966(3) 0.0229(8) Uani 1 1 d . . . . .
O15 O 0.54421(16) 0.08967(19) 0.8876(3) 0.0230(7) Uani 1 1 d . . . . .
O16 O 0.53874(16) 0.08531(19) 0.6336(3) 0.0233(8) Uani 1 1 d . . . . .
O17 O 0.42094(16) 0.16675(19) 0.6396(3) 0.0233(8) Uani 1 1 d D . . . .
O18 O 0.42761(16) 0.17063(19) 0.8944(3) 0.0217(7) Uani 1 1 d . . . . .
O19 O 0.52710(11) 0.21200(13) 0.7567(4) 0.0176(5) Uani 1 1 d . . . . .
C1 C 0.3836(2) -0.0273(3) 0.7694(7) 0.0394(12) Uani 1 1 d . . . . .
H1A H 0.379198 -0.046211 0.847912 0.059 Uiso 1 1 calc R U . . .
H1B H 0.399425 -0.064315 0.717904 0.059 Uiso 1 1 calc R U . . .
H1C H 0.342839 -0.011047 0.741509 0.059 Uiso 1 1 calc R U . . .
C2 C 0.7012(2) 0.2877(3) 0.8729(5) 0.0369(13) Uani 1 1 d . . . . .
H2A H 0.721877 0.253921 0.924559 0.055 Uiso 1 1 calc R U . . .
H2B H 0.706107 0.335468 0.903970 0.055 Uiso 1 1 calc R U . . .
H2C H 0.720244 0.285140 0.795893 0.055 Uiso 1 1 calc R U . . .
C3 C 0.6503(3) 0.3005(3) 0.5221(5) 0.0303(11) Uani 1 1 d . . . . .
H3A H 0.672829 0.344081 0.540791 0.045 Uiso 1 1 calc R U . . .
H3B H 0.613131 0.311867 0.476269 0.045 Uiso 1 1 calc R U . . .
H3C H 0.677669 0.269244 0.477362 0.045 Uiso 1 1 calc R U . . .
C4 C 0.4956(2) 0.4120(2) 0.6314(5) 0.0274(11) Uani 1 1 d . . . . .
H4A H 0.460062 0.414271 0.578120 0.041 Uiso 1 1 calc R U . . .
H4B H 0.527669 0.445751 0.606995 0.041 Uiso 1 1 calc R U . . .
H4C H 0.481614 0.423583 0.709883 0.041 Uiso 1 1 calc R U . . .
C5 C 0.5500(2) 0.3847(3) 0.9685(4) 0.0274(10) Uani 1 1 d . . . . .
H5A H 0.514772 0.399410 1.017041 0.041 Uiso 1 1 calc R U . . .
H5B H 0.572939 0.426441 0.942145 0.041 Uiso 1 1 calc R U . . .
H5C H 0.577934 0.354288 1.013423 0.041 Uiso 1 1 calc R U . . .
C6 C 0.7076(2) 0.1341(3) 0.7404(6) 0.0439(15) Uani 1 1 d . . . . .
H6A H 0.725967 0.128060 0.817484 0.066 Uiso 1 1 calc R U . . .
H6B H 0.724072 0.177190 0.704899 0.066 Uiso 1 1 calc R U . . .
H6C H 0.718275 0.093409 0.691978 0.066 Uiso 1 1 calc R U . . .
C7 C 0.5052(3) 0.1777(3) 0.4153(5) 0.0350(13) Uani 1 1 d . . . . .
H7A H 0.541147 0.165272 0.366815 0.052 Uiso 1 1 calc R U . . .
H7B H 0.476752 0.208083 0.371432 0.052 Uiso 1 1 calc R U . . .
H7C H 0.483216 0.134582 0.438470 0.052 Uiso 1 1 calc R U . . .
C8 C 0.3563(3) 0.2985(5) 0.7641(9) 0.030(2) Uani 0.660(14) 1 d D . P A 1
H8A H 0.341857 0.332316 0.705722 0.045 Uiso 0.660(14) 1 calc R U P A 1
H8B H 0.342724 0.314102 0.840973 0.045 Uiso 0.660(14) 1 calc R U P A 1
H8C H 0.338499 0.251947 0.747582 0.045 Uiso 0.660(14) 1 calc R U P A 1
C8' C 0.3741(7) 0.3453(8) 0.7740(17) 0.033(4) Uani 0.340(14) 1 d D . P A 5
H8D H 0.392783 0.390370 0.796652 0.049 Uiso 0.340(14) 1 calc R U P A 5
H8E H 0.344609 0.329924 0.833842 0.049 Uiso 0.340(14) 1 calc R U P A 5
H8F H 0.351874 0.350991 0.700378 0.049 Uiso 0.340(14) 1 calc R U P A 5
C9 C 0.5208(2) 0.1871(3) 1.1007(5) 0.0296(11) Uani 1 1 d . . . . .
H9A H 0.489129 0.214705 1.141987 0.044 Uiso 1 1 calc R U . . .
H9B H 0.557846 0.181758 1.149696 0.044 Uiso 1 1 calc R U . . .
H9C H 0.503809 0.140406 1.082152 0.044 Uiso 1 1 calc R U . . .
C10 C 0.5651(3) 0.0230(3) 0.9207(7) 0.0414(16) Uani 1 1 d . . . . .
H10A H 0.569797 0.021393 1.005005 0.062 Uiso 1 1 calc R U . . .
H10B H 0.605484 0.013322 0.883998 0.062 Uiso 1 1 calc R U . . .
H10C H 0.534650 -0.012664 0.896260 0.062 Uiso 1 1 calc R U . . .
C11 C 0.5643(3) 0.0167(3) 0.6144(6) 0.0357(13) Uani 1 1 d . . . . .
H11A H 0.574090 0.011007 0.532044 0.053 Uiso 1 1 calc R U . . .
H11B H 0.533846 -0.019105 0.637819 0.053 Uiso 1 1 calc R U . . .
H11C H 0.602575 0.011239 0.660123 0.053 Uiso 1 1 calc R U . . .
C12 C 0.3678(5) 0.1440(6) 0.5761(10) 0.032(2) Uani 0.660(14) 1 d D U P A 1
H12A H 0.334803 0.179730 0.581681 0.048 Uiso 0.660(14) 1 calc R U P A 1
H12B H 0.352580 0.099337 0.608058 0.048 Uiso 0.660(14) 1 calc R U P A 1
H12C H 0.379294 0.137366 0.494724 0.048 Uiso 0.660(14) 1 calc R U P A 1
C12' C 0.3545(6) 0.1609(11) 0.631(2) 0.041(5) Uani 0.340(14) 1 d D U P A 5
H12D H 0.334780 0.198327 0.676694 0.061 Uiso 0.340(14) 1 calc R U P A 5
H12E H 0.341139 0.114835 0.660154 0.061 Uiso 0.340(14) 1 calc R U P A 5
H12F H 0.341915 0.165703 0.549622 0.061 Uiso 0.340(14) 1 calc R U P A 5
C13 C 0.3741(3) 0.1526(3) 0.9571(6) 0.0420(16) Uani 1 1 d . . . . .
H13A H 0.376677 0.172877 1.034957 0.063 Uiso 1 1 calc R U . . .
H13B H 0.371049 0.101107 0.962802 0.063 Uiso 1 1 calc R U . . .
H13C H 0.337051 0.171037 0.917521 0.063 Uiso 1 1 calc R U . . .
N1 N 0.33226(15) 0.39808(16) 0.2482(4) 0.0206(7) Uani 1 1 d . . . . .
C14 C 0.3152(2) 0.4530(2) 0.3380(4) 0.0223(9) Uani 1 1 d . . . . .
H14A H 0.273550 0.472405 0.318740 0.027 Uiso 1 1 calc R U . . .
H14B H 0.345675 0.492226 0.333018 0.027 Uiso 1 1 calc R U . . .
C15 C 0.3139(2) 0.4261(3) 0.4623(4) 0.0250(10) Uani 1 1 d . . . . .
H15A H 0.353116 0.400499 0.479157 0.030 Uiso 1 1 calc R U . . .
H15B H 0.278664 0.392759 0.471831 0.030 Uiso 1 1 calc R U . . .
C16 C 0.3064(3) 0.4874(3) 0.5478(5) 0.0292(12) Uani 1 1 d . . . . .
H16A H 0.309220 0.468870 0.627805 0.035 Uiso 1 1 calc R U . . .
H16B H 0.341163 0.521140 0.536570 0.035 Uiso 1 1 calc R U . . .
C17 C 0.2449(3) 0.5258(3) 0.5333(6) 0.0373(13) Uani 1 1 d . . . . .
H17A H 0.241528 0.562926 0.592018 0.056 Uiso 1 1 calc R U . . .
H17B H 0.210335 0.492414 0.542445 0.056 Uiso 1 1 calc R U . . .
H17C H 0.243097 0.547026 0.456005 0.056 Uiso 1 1 calc R U . . .
C18 C 0.28262(19) 0.3407(2) 0.2505(5) 0.0251(9) Uani 1 1 d . . . . .
H18A H 0.285387 0.315832 0.325715 0.030 Uiso 1 1 calc R U . . .
H18B H 0.241069 0.363493 0.246858 0.030 Uiso 1 1 calc R U . . .
C19 C 0.2863(2) 0.2862(3) 0.1548(5) 0.0310(11) Uani 1 1 d . . . . .
H19A H 0.330522 0.273511 0.140620 0.037 Uiso 1 1 calc R U . . .
H19B H 0.268978 0.306204 0.082407 0.037 Uiso 1 1 calc R U . . .
C20 C 0.2494(3) 0.2203(3) 0.1889(6) 0.0392(13) Uani 1 1 d . . . . .
H20A H 0.255889 0.183750 0.128833 0.047 Uiso 1 1 calc R U . . .
H20B H 0.266601 0.201765 0.262431 0.047 Uiso 1 1 calc R U . . .
C21 C 0.1798(3) 0.2318(4) 0.2039(6) 0.0492(17) Uani 1 1 d . . . . .
H21A H 0.159941 0.187342 0.226638 0.074 Uiso 1 1 calc R U . . .
H21B H 0.161828 0.248141 0.130616 0.074 Uiso 1 1 calc R U . . .
H21C H 0.172679 0.267336 0.264005 0.074 Uiso 1 1 calc R U . . .
C22 C 0.3367(2) 0.4333(2) 0.1292(4) 0.0212(9) Uani 1 1 d . . . . .
H22A H 0.369328 0.470155 0.133474 0.025 Uiso 1 1 calc R U . . .
H22B H 0.351226 0.397378 0.073182 0.025 Uiso 1 1 calc R U . . .
C23 C 0.2780(2) 0.4668(3) 0.0806(4) 0.0248(10) Uani 1 1 d . . . . .
H23A H 0.263307 0.504987 0.132381 0.030 Uiso 1 1 calc R U . . .
H23B H 0.244402 0.431200 0.073537 0.030 Uiso 1 1 calc R U . . .
C24 C 0.2946(2) 0.4967(3) -0.0385(5) 0.0266(11) Uani 1 1 d . . . . .
H24A H 0.331178 0.528224 -0.030304 0.032 Uiso 1 1 calc R U . . .
H24B H 0.306909 0.457244 -0.089813 0.032 Uiso 1 1 calc R U . . .
C25 C 0.2423(3) 0.5372(3) -0.0956(5) 0.0386(13) Uani 1 1 d . . . . .
H25A H 0.256073 0.553683 -0.171873 0.058 Uiso 1 1 calc R U . . .
H25B H 0.231151 0.577832 -0.047427 0.058 Uiso 1 1 calc R U . . .
H25C H 0.205877 0.506434 -0.104578 0.058 Uiso 1 1 calc R U . . .
C26 C 0.39590(18) 0.3642(2) 0.2726(5) 0.0208(9) Uani 1 1 d . . . . .
H26A H 0.392255 0.334584 0.342847 0.025 Uiso 1 1 calc R U . . .
H26B H 0.406555 0.332636 0.207196 0.025 Uiso 1 1 calc R U . . .
C27 C 0.4494(2) 0.4162(2) 0.2899(5) 0.0263(11) Uani 1 1 d . . . . .
H27A H 0.451896 0.448277 0.222432 0.032 Uiso 1 1 calc R U . . .
H27B H 0.441332 0.445132 0.359689 0.032 Uiso 1 1 calc R U . . .
C28 C 0.5110(2) 0.3772(2) 0.3038(4) 0.0249(10) Uani 1 1 d . . . . .
H28A H 0.516856 0.344758 0.237576 0.030 Uiso 1 1 calc R U . . .
H28B H 0.509745 0.348643 0.375434 0.030 Uiso 1 1 calc R U . . .
C29 C 0.5660(2) 0.4283(3) 0.3096(5) 0.0317(11) Uani 1 1 d . . . . .
H29A H 0.604563 0.401853 0.324523 0.047 Uiso 1 1 calc R U . . .
H29B H 0.559132 0.462250 0.372278 0.047 Uiso 1 1 calc R U . . .
H29C H 0.569752 0.453479 0.235915 0.047 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O6 1.927(3) . ?
Zr1 O17 2.097(4) . ?
Zr1 O18 2.101(4) . ?
Zr1 O15 2.105(4) . ?
Zr1 O16 2.108(4) . ?
Zr1 O19 2.153(2) . ?
V1 O1 1.603(3) . ?
V1 O7 1.996(4) . ?
V1 O8 1.998(4) . ?
V1 O10 2.000(4) . ?
V1 O9 2.001(3) . ?
V1 O19 2.512(2) . ?
V2 O2 1.604(4) . ?
V2 O7 1.992(4) . ?
V2 O11 1.997(4) . ?
V2 O14 2.017(4) . ?
V2 O15 2.043(4) . ?
V2 O19 2.375(4) . ?
V3 O3 1.604(4) . ?
V3 O12 1.998(4) . ?
V3 O8 2.002(3) . ?
V3 O11 2.011(4) . ?
V3 O16 2.031(4) . ?
V3 O19 2.400(4) . ?
V4 O4 1.606(4) . ?
V4 O9 1.989(3) . ?
V4 O13 1.995(4) . ?
V4 O12 2.006(4) . ?
V4 O17 2.034(4) . ?
V4 O19 2.338(4) . ?
V5 O5 1.606(4) . ?
V5 O10 1.991(4) . ?
V5 O13 2.004(4) . ?
V5 O14 2.007(4) . ?
V5 O18 2.040(4) . ?
V5 O19 2.349(4) . ?
O6 C1 1.413(5) . ?
O7 C2 1.421(6) . ?
O8 C3 1.425(6) . ?
O9 C4 1.411(5) . ?
O10 C5 1.419(6) . ?
O11 C6 1.427(5) . ?
O12 C7 1.427(6) . ?
O13 C8 1.392(6) . ?
O13 C8' 1.402(10) . ?
O14 C9 1.422(6) . ?
O15 C10 1.395(7) . ?
O16 C11 1.428(6) . ?
O17 C12 1.421(8) . ?
O17 C12' 1.431(12) . ?
O18 C13 1.398(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8' H8D 0.9800 . ?
C8' H8E 0.9800 . ?
C8' H8F 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12' H12D 0.9800 . ?
C12' H12E 0.9800 . ?
C12' H12F 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N1 C14 1.514(6) . ?
N1 C18 1.521(5) . ?
N1 C22 1.531(6) . ?
N1 C26 1.532(5) . ?
C14 C15 1.524(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.533(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.514(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.515(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.531(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.515(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.515(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.530(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.508(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.525(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.520(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.526(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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
O6 Zr1 O17 96.59(15) . . ?
O6 Zr1 O18 97.44(15) . . ?
O17 Zr1 O18 89.19(12) . . ?
O6 Zr1 O15 99.76(15) . . ?
O17 Zr1 O15 163.65(14) . . ?
O18 Zr1 O15 88.37(15) . . ?
O6 Zr1 O16 99.05(15) . . ?
O17 Zr1 O16 89.36(15) . . ?
O18 Zr1 O16 163.50(14) . . ?
O15 Zr1 O16 88.42(11) . . ?
O6 Zr1 O19 177.85(11) . . ?
O17 Zr1 O19 81.67(14) . . ?
O18 Zr1 O19 81.29(14) . . ?
O15 Zr1 O19 81.98(14) . . ?
O16 Zr1 O19 82.24(14) . . ?
O1 V1 O7 102.16(16) . . ?
O1 V1 O8 101.36(16) . . ?
O7 V1 O8 87.33(13) . . ?
O1 V1 O10 101.35(16) . . ?
O7 V1 O10 86.97(15) . . ?
O8 V1 O10 157.26(14) . . ?
O1 V1 O9 100.57(16) . . ?
O7 V1 O9 157.27(14) . . ?
O8 V1 O9 88.55(15) . . ?
O10 V1 O9 88.26(12) . . ?
O1 V1 O19 179.23(15) . . ?
O7 V1 O19 78.58(13) . . ?
O8 V1 O19 78.86(13) . . ?
O10 V1 O19 78.45(13) . . ?
O9 V1 O19 78.68(13) . . ?
O2 V2 O7 101.24(18) . . ?
O2 V2 O11 101.34(18) . . ?
O7 V2 O11 90.22(14) . . ?
O2 V2 O14 100.87(19) . . ?
O7 V2 O14 87.39(15) . . ?
O11 V2 O14 157.70(15) . . ?
O2 V2 O15 98.63(18) . . ?
O7 V2 O15 160.10(15) . . ?
O11 V2 O15 86.86(14) . . ?
O14 V2 O15 87.90(15) . . ?
O2 V2 O19 176.56(16) . . ?
O7 V2 O19 82.10(12) . . ?
O11 V2 O19 79.37(13) . . ?
O14 V2 O19 78.34(14) . . ?
O15 V2 O19 78.02(12) . . ?
O3 V3 O12 102.48(19) . . ?
O3 V3 O8 100.60(18) . . ?
O12 V3 O8 87.96(15) . . ?
O3 V3 O11 101.18(18) . . ?
O12 V3 O11 156.32(15) . . ?
O8 V3 O11 88.71(14) . . ?
O3 V3 O16 99.84(18) . . ?
O12 V3 O16 88.34(15) . . ?
O8 V3 O16 159.55(15) . . ?
O11 V3 O16 86.65(14) . . ?
O3 V3 O19 177.80(16) . . ?
O12 V3 O19 77.84(14) . . ?
O8 V3 O19 81.57(12) . . ?
O11 V3 O19 78.48(13) . . ?
O16 V3 O19 77.98(12) . . ?
O4 V4 O9 100.45(18) . . ?
O4 V4 O13 101.36(17) . . ?
O9 V4 O13 88.24(13) . . ?
O4 V4 O12 100.96(18) . . ?
O9 V4 O12 88.34(15) . . ?
O13 V4 O12 157.67(15) . . ?
O4 V4 O17 97.63(17) . . ?
O9 V4 O17 161.92(15) . . ?
O13 V4 O17 88.04(14) . . ?
O12 V4 O17 88.41(15) . . ?
O4 V4 O19 176.24(16) . . ?
O9 V4 O19 83.31(12) . . ?
O13 V4 O19 78.50(13) . . ?
O12 V4 O19 79.19(14) . . ?
O17 V4 O19 78.62(12) . . ?
O5 V5 O10 99.99(18) . . ?
O5 V5 O13 100.94(17) . . ?
O10 V5 O13 88.34(13) . . ?
O5 V5 O14 101.85(18) . . ?
O10 V5 O14 88.13(15) . . ?
O13 V5 O14 157.20(15) . . ?
O5 V5 O18 99.36(17) . . ?
O10 V5 O18 160.65(15) . . ?
O13 V5 O18 88.05(14) . . ?
O14 V5 O18 87.86(15) . . ?
O5 V5 O19 177.12(16) . . ?
O10 V5 O19 82.71(12) . . ?
O13 V5 O19 78.06(13) . . ?
O14 V5 O19 79.15(14) . . ?
O18 V5 O19 77.94(12) . . ?
C1 O6 Zr1 172.8(3) . . ?
C2 O7 V2 123.5(3) . . ?
C2 O7 V1 115.7(3) . . ?
V2 O7 V1 113.35(17) . . ?
C3 O8 V1 117.3(3) . . ?
C3 O8 V3 115.5(3) . . ?
V1 O8 V3 113.64(16) . . ?
C4 O9 V4 118.3(3) . . ?
C4 O9 V1 115.7(3) . . ?
V4 O9 V1 112.05(16) . . ?
C5 O10 V5 116.6(3) . . ?
C5 O10 V1 117.1(3) . . ?
V5 O10 V1 112.67(17) . . ?
C6 O11 V2 120.7(4) . . ?
C6 O11 V3 116.1(4) . . ?
V2 O11 V3 112.87(12) . . ?
C7 O12 V3 117.3(3) . . ?
C7 O12 V4 118.2(3) . . ?
V3 O12 V4 113.07(18) . . ?
C8 O13 V4 118.6(5) . . ?
C8' O13 V4 128.2(8) . . ?
C8 O13 V5 120.3(5) . . ?
C8' O13 V5 117.2(9) . . ?
V4 O13 V5 112.66(12) . . ?
C9 O14 V5 118.1(3) . . ?
C9 O14 V2 116.9(3) . . ?
V5 O14 V2 112.22(18) . . ?
C10 O15 V2 120.9(3) . . ?
C10 O15 Zr1 128.0(4) . . ?
V2 O15 Zr1 106.04(16) . . ?
C11 O16 V3 117.8(3) . . ?
C11 O16 Zr1 126.9(4) . . ?
V3 O16 Zr1 106.46(16) . . ?
C12 O17 V4 123.3(5) . . ?
C12' O17 V4 119.6(9) . . ?
C12 O17 Zr1 131.0(5) . . ?
C12' O17 Zr1 124.3(10) . . ?
V4 O17 Zr1 105.58(15) . . ?
C13 O18 V5 123.4(3) . . ?
C13 O18 Zr1 130.1(4) . . ?
V5 O18 Zr1 106.18(15) . . ?
Zr1 O19 V4 94.12(12) . . ?
Zr1 O19 V5 94.59(12) . . ?
V4 O19 V5 90.47(9) . . ?
Zr1 O19 V2 93.96(12) . . ?
V4 O19 V2 171.84(12) . . ?
V5 O19 V2 89.98(15) . . ?
Zr1 O19 V3 93.32(12) . . ?
V4 O19 V3 89.66(15) . . ?
V5 O19 V3 172.06(12) . . ?
V2 O19 V3 88.77(9) . . ?
Zr1 O19 V1 179.24(18) . . ?
V4 O19 V1 85.95(10) . . ?
V5 O19 V1 86.17(10) . . ?
V2 O19 V1 85.95(10) . . ?
V3 O19 V1 85.93(10) . . ?
O6 C1 H1A 109.5 . . ?
O6 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O6 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O7 C2 H2A 109.5 . . ?
O7 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O7 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O8 C3 H3A 109.5 . . ?
O8 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O8 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O9 C4 H4A 109.5 . . ?
O9 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O9 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O10 C5 H5A 109.5 . . ?
O10 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O10 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O11 C6 H6A 109.5 . . ?
O11 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O11 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O12 C7 H7A 109.5 . . ?
O12 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O12 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O13 C8 H8A 109.5 . . ?
O13 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O13 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O13 C8' H8D 109.5 . . ?
O13 C8' H8E 109.5 . . ?
H8D C8' H8E 109.5 . . ?
O13 C8' H8F 109.5 . . ?
H8D C8' H8F 109.5 . . ?
H8E C8' H8F 109.5 . . ?
O14 C9 H9A 109.5 . . ?
O14 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O14 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O15 C10 H10A 109.5 . . ?
O15 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O15 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O16 C11 H11A 109.5 . . ?
O16 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O16 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O17 C12 H12A 109.5 . . ?
O17 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O17 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O17 C12' H12D 109.5 . . ?
O17 C12' H12E 109.5 . . ?
H12D C12' H12E 109.5 . . ?
O17 C12' H12F 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
O18 C13 H13A 109.5 . . ?
O18 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O18 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 N1 C18 108.2(4) . . ?
C14 N1 C22 109.2(3) . . ?
C18 N1 C22 111.7(4) . . ?
C14 N1 C26 112.1(4) . . ?
C18 N1 C26 108.5(3) . . ?
C22 N1 C26 107.0(3) . . ?
N1 C14 C15 114.8(4) . . ?
N1 C14 H14A 108.6 . . ?
C15 C14 H14A 108.6 . . ?
N1 C14 H14B 108.6 . . ?
C15 C14 H14B 108.6 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 C16 110.9(4) . . ?
C14 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C15 112.6(5) . . ?
C17 C16 H16A 109.1 . . ?
C15 C16 H16A 109.1 . . ?
C17 C16 H16B 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N1 116.0(4) . . ?
C19 C18 H18A 108.3 . . ?
N1 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
N1 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C18 C19 C20 110.0(5) . . ?
C18 C19 H19A 109.7 . . ?
C20 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
C20 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
C21 C20 C19 114.8(5) . . ?
C21 C20 H20A 108.6 . . ?
C19 C20 H20A 108.6 . . ?
C21 C20 H20B 108.6 . . ?
C19 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N1 117.7(4) . . ?
C23 C22 H22A 107.9 . . ?
N1 C22 H22A 107.9 . . ?
C23 C22 H22B 107.9 . . ?
N1 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C22 C23 C24 107.3(4) . . ?
C22 C23 H23A 110.3 . . ?
C24 C23 H23A 110.3 . . ?
C22 C23 H23B 110.3 . . ?
C24 C23 H23B 110.3 . . ?
H23A C23 H23B 108.5 . . ?
C25 C24 C23 114.2(5) . . ?
C25 C24 H24A 108.7 . . ?
C23 C24 H24A 108.7 . . ?
C25 C24 H24B 108.7 . . ?
C23 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N1 114.8(3) . . ?
C27 C26 H26A 108.6 . . ?
N1 C26 H26A 108.6 . . ?
C27 C26 H26B 108.6 . . ?
N1 C26 H26B 108.6 . . ?
H26A C26 H26B 107.5 . . ?
C28 C27 C26 110.5(4) . . ?
C28 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C27 C28 C29 111.5(4) . . ?
C27 C28 H28A 109.3 . . ?
C29 C28 H28A 109.3 . . ?
C27 C28 H28B 109.3 . . ?
C29 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
C18 N1 C14 C15 62.4(5) . . . . ?
C22 N1 C14 C15 -175.8(4) . . . . ?
C26 N1 C14 C15 -57.3(5) . . . . ?
N1 C14 C15 C16 171.1(4) . . . . ?
C14 C15 C16 C17 63.5(6) . . . . ?
C14 N1 C18 C19 171.4(4) . . . . ?
C22 N1 C18 C19 51.1(5) . . . . ?
C26 N1 C18 C19 -66.7(6) . . . . ?
N1 C18 C19 C20 161.2(4) . . . . ?
C18 C19 C20 C21 63.9(6) . . . . ?
C14 N1 C22 C23 -62.4(5) . . . . ?
C18 N1 C22 C23 57.3(5) . . . . ?
C26 N1 C22 C23 176.0(4) . . . . ?
N1 C22 C23 C24 -179.0(4) . . . . ?
C22 C23 C24 C25 -175.5(5) . . . . ?
C14 N1 C26 C27 -52.4(5) . . . . ?
C18 N1 C26 C27 -171.9(5) . . . . ?
C22 N1 C26 C27 67.4(5) . . . . ?
N1 C26 C27 C28 -175.5(4) . . . . ?
C26 C27 C28 C29 174.5(4) . . . . ?

_refine_diff_density_max         1.066
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.093

