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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_da770
_database_code_depnum_ccdc_archive 'CCDC 2179578'
loop_
_audit_author_name
_audit_author_address
'Sylvain Duval'
;University of Lille
France
;
_audit_update_record             
;
2022-06-16 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_audit_creation_date             2020-10-22
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C58 H122 Nb6 O34'
_chemical_formula_sum            'C58 H122 Nb6 O34'
_chemical_formula_weight         1921.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'

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

_cell_length_a                   24.0297(14)
_cell_length_b                   18.1938(11)
_cell_length_c                   19.0238(11)
_cell_angle_alpha                90
_cell_angle_beta                 97.312(3)
_cell_angle_gamma                90
_cell_volume                     8249.4(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    106.73
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.692
_shelx_estimated_absorpt_T_min   0.520
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1606 before and 0.0496 after correction.
The Ratio of minimum to maximum transmission is 0.8237.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.45
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62529
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_min         1.707
_diffrn_ambient_temperature      106.73
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6659
_reflns_number_total             8239
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         2.278
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         8239
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0580
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0598P)²+92.2868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1521
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22A-C23A
 1.45 with sigma of 0.02
 C20B-C21B
 1.45 with sigma of 0.02
 C20A-C21A
 1.45 with sigma of 0.02
 C29B-C28B
 1.45 with sigma of 0.02
 C2-C1
 1.45 with sigma of 0.02
3. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20B, C21B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20B \\sim C21B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C28B \\sim C29B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C23B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02
Uanis(C22B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C20A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
5. Others
 Sof(O11B)=Sof(C19B)=Sof(O12B)=Sof(Nb3B)=Sof(O13B)=Sof(O17B)=Sof(O15B)=
 Sof(O14B)=Sof(O16B)=Sof(C28B)=Sof(H28A)=Sof(H28B)=Sof(C23B)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H24C)=Sof(H24D)=
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(C27B)=Sof(H27A)=Sof(H27B)=Sof(H27C)=
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(O12A)=Sof(Nb3A)=Sof(C19A)=Sof(O11A)=Sof(O17A)=
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=
 Sof(O16A)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(O15A)=Sof(O14A)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(O13A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C5(H5A,H5B), C13(H13A,H13B), C3(H3A,H3B), C11(H11A,
 H11B), C1(H1A,H1B), C28B(H28A,H28B), C22B(H22A,H22B), C24(H24C,H24D), C24(H24A,
 H24B), C20B(H20A,H20B), C26B(H26A,H26B), C26A(H26C,H26D), C28A(H28C,H28D),
 C22A(H22C,H22D), C20A(H20C,H20D)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C6(H6A,H6B,
 H6C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C23B(H23A,H23B,H23C),
 C25(H25A,H25B,H25C), C27B(H27A,H27B,H27C), C27A(H27D,H27E,H27F), C29A(H29A,
 H29B,H29C), C23A(H23D,H23E,H23F), C21A(H21A,H21B,H21C), C29B(H29D,H29E,H29F),
 C21B(H21D,H21E,H21F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb2 Nb 0.30722(2) 0.55896(2) 0.47618(3) 0.03300(14) Uani 1 1 d . . . . .
O7 O 0.29574(14) 0.43966(17) 0.48907(17) 0.0281(7) Uani 1 1 d . . . . .
O1 O 0.27568(15) 0.39792(18) 0.37833(18) 0.0305(8) Uani 1 1 d . . . . .
O3 O 0.28289(16) 0.58221(19) 0.25755(19) 0.0359(8) Uani 1 1 d . . . . .
O6 O 0.25177(14) 0.54539(17) 0.39482(17) 0.0290(7) Uani 1 1 d . . . . .
O8 O 0.37501(17) 0.5372(2) 0.5359(2) 0.0463(10) Uani 1 1 d . . . . .
O9 O 0.25849(18) 0.5670(2) 0.54469(19) 0.0404(9) Uani 1 1 d . . . . .
O10 O 0.3203(2) 0.6588(2) 0.4614(2) 0.0528(11) Uani 1 1 d . . . . .
O4 O 0.32750(18) 0.4379(2) 0.2678(2) 0.0432(10) Uani 1 1 d . . . . .
O5 O 0.34971(15) 0.5216(2) 0.3902(2) 0.0390(9) Uani 1 1 d . . . . .
O2 O 0.20892(16) 0.4653(2) 0.27344(19) 0.0378(8) Uani 1 1 d . . . . .
C15 C 0.28202(19) 0.3902(2) 0.4447(3) 0.0250(10) Uani 1 1 d . . . . .
C16 C 0.26750(18) 0.3164(2) 0.4729(2) 0.0204(9) Uani 1 1 d . . . . .
C7 C 0.2300(3) 0.5309(6) 0.5972(4) 0.084(3) Uani 1 1 d . . . . .
H7A H 0.227057 0.565047 0.637096 0.101 Uiso 1 1 calc R U . . .
H7B H 0.252194 0.487707 0.616048 0.101 Uiso 1 1 calc R U . . .
C9 C 0.4067(3) 0.4775(4) 0.5682(3) 0.0472(15) Uani 1 1 d . . . . .
H9A H 0.447172 0.489381 0.572050 0.057 Uiso 1 1 calc R U . . .
H9B H 0.399871 0.433195 0.538100 0.057 Uiso 1 1 calc R U . . .
C5 C 0.2984(3) 0.7207(4) 0.4196(5) 0.069(2) Uani 1 1 d . . . . .
H5A H 0.288235 0.760677 0.450828 0.083 Uiso 1 1 calc R U . . .
H5B H 0.264348 0.706061 0.387779 0.083 Uiso 1 1 calc R U . . .
C13 C 0.4081(3) 0.5045(4) 0.3888(4) 0.0535(16) Uani 1 1 d . . . . .
H13A H 0.411750 0.453485 0.372000 0.064 Uiso 1 1 calc R U . . .
H13B H 0.428400 0.508202 0.437355 0.064 Uiso 1 1 calc R U . . .
C3 C 0.2473(4) 0.6408(4) 0.2313(4) 0.070(2) Uani 1 1 d . . . . .
H3A H 0.238435 0.671098 0.271646 0.084 Uiso 1 1 calc R U . . .
H3B H 0.211651 0.620277 0.207510 0.084 Uiso 1 1 calc R U . . .
C10 C 0.3911(3) 0.4619(4) 0.6401(4) 0.0613(19) Uani 1 1 d . . . . .
H10A H 0.395958 0.506496 0.669131 0.092 Uiso 1 1 calc R U . . .
H10B H 0.415202 0.422837 0.662531 0.092 Uiso 1 1 calc R U . . .
H10C H 0.351794 0.446128 0.635918 0.092 Uiso 1 1 calc R U . . .
C12 C 0.3231(4) 0.3222(4) 0.2071(5) 0.078(3) Uani 1 1 d . . . . .
H12A H 0.283738 0.316233 0.214530 0.117 Uiso 1 1 calc R U . . .
H12B H 0.340980 0.273836 0.206721 0.117 Uiso 1 1 calc R U . . .
H12C H 0.325050 0.346817 0.161655 0.117 Uiso 1 1 calc R U . . .
C11 C 0.3532(3) 0.3682(3) 0.2664(4) 0.0563(18) Uani 1 1 d . . . . .
H11A H 0.352002 0.343010 0.312310 0.068 Uiso 1 1 calc R U . . .
H11B H 0.393067 0.374177 0.259159 0.068 Uiso 1 1 calc R U . . .
C14 C 0.4328(3) 0.5555(5) 0.3418(4) 0.069(2) Uani 1 1 d . . . . .
H14A H 0.410014 0.555912 0.295296 0.104 Uiso 1 1 calc R U . . .
H14B H 0.471009 0.539534 0.336590 0.104 Uiso 1 1 calc R U . . .
H14C H 0.433912 0.605000 0.362194 0.104 Uiso 1 1 calc R U . . .
C1 C 0.1661(3) 0.4179(5) 0.2870(4) 0.070(2) Uani 1 1 d D U . . .
H1A H 0.182065 0.370447 0.305142 0.084 Uiso 1 1 calc R U . . .
H1B H 0.140648 0.408460 0.242748 0.084 Uiso 1 1 calc R U . . .
C6 C 0.3426(4) 0.7462(7) 0.3772(7) 0.124(5) Uani 1 1 d . . . . .
H6A H 0.375359 0.762923 0.409137 0.185 Uiso 1 1 calc R U . . .
H6B H 0.328011 0.786831 0.346435 0.185 Uiso 1 1 calc R U . . .
H6C H 0.353556 0.705528 0.348035 0.185 Uiso 1 1 calc R U . . .
C8 C 0.1710(5) 0.5058(6) 0.5656(7) 0.119(4) Uani 1 1 d . . . . .
H8A H 0.145543 0.548096 0.561604 0.179 Uiso 1 1 calc R U . . .
H8B H 0.157300 0.468705 0.596579 0.179 Uiso 1 1 calc R U . . .
H8C H 0.172570 0.484640 0.518546 0.179 Uiso 1 1 calc R U . . .
C4 C 0.2717(4) 0.6872(4) 0.1821(4) 0.077(3) Uani 1 1 d . . . . .
H4A H 0.308753 0.703882 0.203563 0.115 Uiso 1 1 calc R U . . .
H4B H 0.247394 0.729880 0.170277 0.115 Uiso 1 1 calc R U . . .
H4C H 0.275489 0.659416 0.138791 0.115 Uiso 1 1 calc R U . . .
C2 C 0.1361(4) 0.4506(6) 0.3375(8) 0.124(4) Uani 1 1 d D U . . .
H2A H 0.162283 0.465421 0.378826 0.187 Uiso 1 1 calc R U . . .
H2B H 0.109043 0.415292 0.352129 0.187 Uiso 1 1 calc R U . . .
H2C H 0.116132 0.493988 0.316754 0.187 Uiso 1 1 calc R U . . .
C17 C 0.21213(19) 0.3060(2) 0.4833(2) 0.0231(9) Uani 1 1 d . . . . .
H17 H 0.185924 0.344676 0.471940 0.028 Uiso 1 1 calc R U . . .
C18 C 0.30599(19) 0.2595(3) 0.4901(3) 0.0260(10) Uani 1 1 d . . . . .
O11B O 0.3796(11) 0.3205(16) 0.4412(10) 0.037(5) Uani 0.529(8) 1 d . . P A 2
C19B C 0.3645(12) 0.2624(14) 0.4673(11) 0.028(4) Uani 0.529(8) 1 d . . P A 2
O12B O 0.3949(5) 0.2064(6) 0.4806(7) 0.040(3) Uani 0.529(8) 1 d . . P A 2
Nb3B Nb 0.47882(5) 0.16838(8) 0.4747(3) 0.0477(10) Uani 0.529(8) 1 d . . P A 2
Nb1 Nb 0.28006(2) 0.49869(2) 0.31483(2) 0.03004(14) Uani 1 1 d . . . . .
O13B O 0.4683(4) 0.0765(6) 0.5127(7) 0.051(3) Uani 0.529(8) 1 d . . P A 2
O17B O 0.4479(5) 0.1455(6) 0.3821(7) 0.054(3) Uani 0.529(8) 1 d . . P A 2
O15B O 0.4812(4) 0.2809(5) 0.4317(9) 0.067(4) Uani 0.529(8) 1 d . . P A 2
O14B O 0.5538(4) 0.1591(6) 0.4608(10) 0.073(4) Uani 0.529(8) 1 d . . P A 2
O16B O 0.4940(5) 0.2170(7) 0.5634(10) 0.072(4) Uani 0.529(8) 1 d . . P A 2
C28B C 0.4795(11) 0.2743(14) 0.6043(13) 0.093(7) Uani 0.529(8) 1 d D U P A 2
H28A H 0.454763 0.308274 0.573941 0.112 Uiso 0.529(8) 1 calc R U P A 2
H28B H 0.513898 0.301774 0.622556 0.112 Uiso 0.529(8) 1 calc R U P A 2
C23B C 0.6393(5) 0.1632(10) 0.4136(10) 0.068(5) Uani 0.529(8) 1 d . U P A 2
H23A H 0.638220 0.215033 0.399619 0.101 Uiso 0.529(8) 1 calc R U P A 2
H23B H 0.660945 0.135197 0.382385 0.101 Uiso 0.529(8) 1 calc R U P A 2
H23C H 0.657024 0.158583 0.462701 0.101 Uiso 0.529(8) 1 calc R U P A 2
C22B C 0.5824(7) 0.1344(11) 0.4077(14) 0.096(6) Uani 0.529(8) 1 d . U P A 2
H22A H 0.561934 0.149213 0.361407 0.115 Uiso 0.529(8) 1 calc R U P A 2
H22B H 0.583887 0.080080 0.409077 0.115 Uiso 0.529(8) 1 calc R U P A 2
C24 C 0.5296(3) 0.3385(5) 0.4429(5) 0.074(2) Uani 1 1 d . . . . .
H24C H 0.518086 0.385229 0.463488 0.089 Uiso 0.529(8) 1 calc R U P A 2
H24D H 0.563923 0.319090 0.471041 0.089 Uiso 0.529(8) 1 calc R U P A 2
H24A H 0.565579 0.317091 0.464642 0.089 Uiso 0.471(8) 1 calc R U P A 1
H24B H 0.529363 0.389844 0.460118 0.089 Uiso 0.471(8) 1 calc R U P A 1
C25 C 0.5347(4) 0.3444(5) 0.3673(5) 0.083(3) Uani 1 1 d . . . . .
H25A H 0.539618 0.295272 0.347906 0.124 Uiso 1 1 calc R U . . .
H25B H 0.567308 0.374905 0.360890 0.124 Uiso 1 1 calc R U . . .
H25C H 0.500714 0.366957 0.342591 0.124 Uiso 1 1 calc R U . . .
C20B C 0.4746(18) 0.0415(18) 0.5750(14) 0.192(15) Uani 0.529(8) 1 d D U P A 2
H20A H 0.482296 -0.009707 0.561666 0.231 Uiso 0.529(8) 1 calc R U P A 2
H20B H 0.435966 0.040651 0.587928 0.231 Uiso 0.529(8) 1 calc R U P A 2
C27B C 0.4059(10) 0.1242(13) 0.2645(12) 0.095(6) Uani 0.529(8) 1 d . . P A 2
H27A H 0.384338 0.149136 0.224201 0.142 Uiso 0.529(8) 1 calc R U P A 2
H27B H 0.385027 0.081123 0.277649 0.142 Uiso 0.529(8) 1 calc R U P A 2
H27C H 0.442180 0.108537 0.251313 0.142 Uiso 0.529(8) 1 calc R U P A 2
C26B C 0.4146(9) 0.1723(14) 0.3218(14) 0.086(7) Uani 0.529(8) 1 d . . P A 2
H26A H 0.377566 0.186181 0.335317 0.103 Uiso 0.529(8) 1 calc R U P A 2
H26B H 0.432232 0.217552 0.306076 0.103 Uiso 0.529(8) 1 calc R U P A 2
O12A O 0.4004(5) 0.2188(6) 0.5150(6) 0.028(2) Uani 0.471(8) 1 d . . P A 1
Nb3A Nb 0.48612(7) 0.18532(16) 0.5148(2) 0.0359(10) Uani 0.471(8) 1 d . . P A 1
C19A C 0.3683(12) 0.2729(14) 0.4908(10) 0.019(4) Uani 0.471(8) 1 d . . P A 1
O11A O 0.3840(10) 0.3287(15) 0.4637(10) 0.022(3) Uani 0.471(8) 1 d . . P A 1
O17A O 0.4583(4) 0.1618(7) 0.4201(7) 0.045(3) Uani 0.471(8) 1 d . U P A 1
C26A C 0.4164(8) 0.1768(11) 0.3618(11) 0.052(4) Uani 0.471(8) 1 d . . P A 1
H26C H 0.412752 0.230697 0.356005 0.063 Uiso 0.471(8) 1 calc R U P A 1
H26D H 0.379976 0.157807 0.373241 0.063 Uiso 0.471(8) 1 calc R U P A 1
C27A C 0.4274(10) 0.1452(15) 0.2954(14) 0.096(9) Uani 0.471(8) 1 d . . P A 1
H27D H 0.392097 0.140358 0.263719 0.144 Uiso 0.471(8) 1 calc R U P A 1
H27E H 0.444563 0.096662 0.303924 0.144 Uiso 0.471(8) 1 calc R U P A 1
H27F H 0.453039 0.177279 0.273356 0.144 Uiso 0.471(8) 1 calc R U P A 1
O16A O 0.4955(4) 0.2303(7) 0.6050(8) 0.042(3) Uani 0.471(8) 1 d . . P A 1
C28A C 0.4728(6) 0.2833(7) 0.6449(11) 0.042(4) Uani 0.471(8) 1 d . . P A 1
H28C H 0.454969 0.321987 0.613100 0.051 Uiso 0.471(8) 1 calc R U P A 1
H28D H 0.503188 0.306406 0.677550 0.051 Uiso 0.471(8) 1 calc R U P A 1
C29A C 0.4292(5) 0.2506(9) 0.6879(8) 0.043(3) Uani 0.471(8) 1 d . . P A 1
H29A H 0.397242 0.232192 0.655544 0.064 Uiso 0.471(8) 1 calc R U P A 1
H29B H 0.416378 0.288578 0.718569 0.064 Uiso 0.471(8) 1 calc R U P A 1
H29C H 0.446115 0.209992 0.717034 0.064 Uiso 0.471(8) 1 calc R U P A 1
O15A O 0.4879(4) 0.3022(7) 0.4757(7) 0.050(3) Uani 0.471(8) 1 d . . P A 1
O14A O 0.5615(5) 0.1850(8) 0.4994(6) 0.052(3) Uani 0.471(8) 1 d . . P A 1
C22A C 0.5901(10) 0.168(2) 0.4440(10) 0.151(16) Uani 0.471(8) 1 d D . P A 1
H22C H 0.594237 0.214028 0.417767 0.181 Uiso 0.471(8) 1 calc R U P A 1
H22D H 0.565155 0.135567 0.412003 0.181 Uiso 0.471(8) 1 calc R U P A 1
C23A C 0.6422(10) 0.135(2) 0.4528(15) 0.157(18) Uani 0.471(8) 1 d D . P A 1
H23D H 0.670989 0.171304 0.468514 0.235 Uiso 0.471(8) 1 calc R U P A 1
H23E H 0.649808 0.113284 0.407721 0.235 Uiso 0.471(8) 1 calc R U P A 1
H23F H 0.642820 0.095705 0.488556 0.235 Uiso 0.471(8) 1 calc R U P A 1
O13A O 0.4802(4) 0.0888(6) 0.5514(7) 0.042(3) Uani 0.471(8) 1 d . . P A 1
C20A C 0.5086(6) 0.0461(15) 0.6078(13) 0.075(6) Uani 0.471(8) 1 d D U P A 1
H20C H 0.493897 0.061181 0.651920 0.090 Uiso 0.471(8) 1 calc R U P A 1
H20D H 0.497443 -0.005833 0.598948 0.090 Uiso 0.471(8) 1 calc R U P A 1
C21A C 0.5683(7) 0.0481(15) 0.6213(13) 0.112(9) Uani 0.471(8) 1 d D . P A 1
H21A H 0.584242 0.020659 0.584277 0.168 Uiso 0.471(8) 1 calc R U P A 1
H21B H 0.580625 0.025682 0.667559 0.168 Uiso 0.471(8) 1 calc R U P A 1
H21C H 0.581137 0.099198 0.621458 0.168 Uiso 0.471(8) 1 calc R U P A 1
C29B C 0.4518(19) 0.2526(18) 0.6623(16) 0.203(18) Uani 0.529(8) 1 d D U P A 2
H29D H 0.414462 0.233543 0.644714 0.305 Uiso 0.529(8) 1 calc R U P A 2
H29E H 0.448024 0.295100 0.693037 0.305 Uiso 0.529(8) 1 calc R U P A 2
H29F H 0.473677 0.214227 0.689325 0.305 Uiso 0.529(8) 1 calc R U P A 2
C21B C 0.5086(15) 0.0499(19) 0.6425(15) 0.191(17) Uani 0.529(8) 1 d D U P A 2
H21D H 0.485195 0.043742 0.680680 0.287 Uiso 0.529(8) 1 calc R U P A 2
H21E H 0.525565 0.098981 0.645607 0.287 Uiso 0.529(8) 1 calc R U P A 2
H21F H 0.538333 0.012627 0.647283 0.287 Uiso 0.529(8) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb2 O7 2.206(3) . ?
Nb2 O6 1.925(4) . ?
Nb2 O8 1.906(4) . ?
Nb2 O9 1.865(4) . ?
Nb2 O10 1.871(4) . ?
Nb2 O5 2.147(4) . ?
Nb2 Nb1 3.2467(7) . ?
O7 C15 1.248(6) . ?
O1 C15 1.261(6) . ?
O1 Nb1 2.205(3) . ?
O3 C3 1.418(7) . ?
O3 Nb1 1.876(3) . ?
O6 Nb1 1.940(3) . ?
O8 C9 1.420(7) . ?
O9 C7 1.440(8) . ?
O10 C5 1.439(8) . ?
O4 C11 1.414(7) . ?
O4 Nb1 1.893(4) . ?
O5 C13 1.439(7) . ?
O5 Nb1 2.102(4) . ?
O2 C1 1.392(8) . ?
O2 Nb1 1.889(4) . ?
C15 C16 1.504(6) . ?
C16 C17 1.383(6) . ?
C16 C18 1.398(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.538(14) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.492(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.487(11) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.465(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.439(10) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 C11 1.513(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.403(11) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C17 H17 0.9500 . ?
C17 C18 1.387(6) 7_556 ?
C18 C19B 1.52(3) . ?
C18 C19A 1.52(3) . ?
O11B C19B 1.24(4) . ?
C19B O12B 1.26(3) . ?
O12B Nb3B 2.148(11) . ?
Nb3B O13B 1.852(12) . ?
Nb3B O17B 1.870(14) . ?
Nb3B O15B 2.209(10) . ?
Nb3B O14B 1.861(10) . ?
Nb3B O16B 1.898(19) . ?
O13B C20B 1.34(3) . ?
O17B C26B 1.40(3) . ?
O15B C24 1.559(12) . ?
O14B C22B 1.37(2) . ?
O16B C28B 1.37(2) . ?
C28B H28A 0.9900 . ?
C28B H28B 0.9900 . ?
C28B C29B 1.416(18) . ?
C23B H23A 0.9800 . ?
C23B H23B 0.9800 . ?
C23B H23C 0.9800 . ?
C23B C22B 1.45(2) . ?
C22B H22A 0.9900 . ?
C22B H22B 0.9900 . ?
C24 H24C 0.9900 . ?
C24 H24D 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.462(12) . ?
C24 O15A 1.410(11) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C20B H20A 0.9900 . ?
C20B H20B 0.9900 . ?
C20B C21B 1.44(2) . ?
C27B H27A 0.9800 . ?
C27B H27B 0.9800 . ?
C27B H27C 0.9800 . ?
C27B C26B 1.39(3) . ?
C26B H26A 0.9900 . ?
C26B H26B 0.9900 . ?
O12A Nb3A 2.149(11) . ?
O12A C19A 1.30(3) . ?
Nb3A O17A 1.889(16) . ?
Nb3A O16A 1.888(16) . ?
Nb3A O15A 2.254(11) . ?
Nb3A O14A 1.873(10) . ?
Nb3A O13A 1.901(11) . ?
C19A O11A 1.22(4) . ?
O17A C26A 1.43(2) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C26A C27A 1.44(3) . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 0.9800 . ?
O16A C28A 1.381(19) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C28A C29A 1.529(16) . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
O14A C22A 1.36(2) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C22A C23A 1.380(17) . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
O13A C20A 1.43(2) . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
C20A C21A 1.426(17) . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 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
O7 Nb2 Nb1 76.10(9) . . ?
O6 Nb2 O7 83.09(13) . . ?
O6 Nb2 O5 72.20(14) . . ?
O6 Nb2 Nb1 33.01(10) . . ?
O8 Nb2 O7 80.72(14) . . ?
O8 Nb2 O6 154.75(17) . . ?
O8 Nb2 O5 86.29(17) . . ?
O8 Nb2 Nb1 123.19(14) . . ?
O9 Nb2 O7 84.33(14) . . ?
O9 Nb2 O6 98.05(16) . . ?
O9 Nb2 O8 99.47(18) . . ?
O9 Nb2 O10 99.27(19) . . ?
O9 Nb2 O5 163.60(16) . . ?
O9 Nb2 Nb1 128.22(12) . . ?
O10 Nb2 O7 176.39(18) . . ?
O10 Nb2 O6 96.67(17) . . ?
O10 Nb2 O8 98.28(18) . . ?
O10 Nb2 O5 95.03(18) . . ?
O10 Nb2 Nb1 101.74(14) . . ?
O5 Nb2 O7 81.45(13) . . ?
O5 Nb2 Nb1 39.66(10) . . ?
C15 O7 Nb2 131.3(3) . . ?
C15 O1 Nb1 129.3(3) . . ?
C3 O3 Nb1 138.5(4) . . ?
Nb2 O6 Nb1 114.27(17) . . ?
C9 O8 Nb2 141.9(4) . . ?
C7 O9 Nb2 147.7(4) . . ?
C5 O10 Nb2 141.8(5) . . ?
C11 O4 Nb1 145.5(3) . . ?
C13 O5 Nb2 129.8(4) . . ?
C13 O5 Nb1 129.7(4) . . ?
Nb1 O5 Nb2 99.66(15) . . ?
C1 O2 Nb1 140.7(4) . . ?
O7 C15 O1 125.8(4) . . ?
O7 C15 C16 117.2(4) . . ?
O1 C15 C16 116.9(4) . . ?
C17 C16 C15 116.3(4) . . ?
C17 C16 C18 119.1(4) . . ?
C18 C16 C15 124.6(4) . . ?
O9 C7 H7A 109.4 . . ?
O9 C7 H7B 109.4 . . ?
O9 C7 C8 111.1(6) . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
O8 C9 H9A 109.4 . . ?
O8 C9 H9B 109.4 . . ?
O8 C9 C10 111.0(5) . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
O10 C5 H5A 110.1 . . ?
O10 C5 H5B 110.1 . . ?
O10 C5 C6 107.9(7) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
O5 C13 H13A 109.6 . . ?
O5 C13 H13B 109.6 . . ?
O5 C13 C14 110.2(5) . . ?
H13A C13 H13B 108.1 . . ?
C14 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
O3 C3 H3A 108.9 . . ?
O3 C3 H3B 108.9 . . ?
O3 C3 C4 113.2(6) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
O4 C11 C12 109.9(6) . . ?
O4 C11 H11A 109.7 . . ?
O4 C11 H11B 109.7 . . ?
C12 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C1 H1A 110.0 . . ?
O2 C1 H1B 110.0 . . ?
O2 C1 C2 108.7(8) . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C16 C17 H17 119.3 . . ?
C16 C17 C18 121.4(4) . 7_556 ?
C18 C17 H17 119.3 7_556 . ?
C16 C18 C19B 120.9(12) . . ?
C16 C18 C19A 120.4(11) . . ?
C17 C18 C16 119.5(4) 7_556 . ?
C17 C18 C19B 118.5(11) 7_556 . ?
C17 C18 C19A 119.4(11) 7_556 . ?
O11B C19B C18 118(2) . . ?
O11B C19B O12B 125(3) . . ?
O12B C19B C18 117(2) . . ?
C19B O12B Nb3B 140.8(15) . . ?
O12B Nb3B O15B 77.8(4) . . ?
O13B Nb3B O12B 95.5(4) . . ?
O13B Nb3B O17B 96.2(5) . . ?
O13B Nb3B O15B 173.3(4) . . ?
O13B Nb3B O14B 99.0(5) . . ?
O13B Nb3B O16B 95.5(6) . . ?
O17B Nb3B O12B 81.8(4) . . ?
O17B Nb3B O15B 83.3(5) . . ?
O17B Nb3B O16B 161.7(5) . . ?
O14B Nb3B O12B 165.5(5) . . ?
O14B Nb3B O17B 96.9(6) . . ?
O14B Nb3B O15B 87.7(4) . . ?
O14B Nb3B O16B 95.1(6) . . ?
O16B Nb3B O12B 83.1(5) . . ?
O16B Nb3B O15B 83.5(6) . . ?
O1 Nb1 Nb2 77.33(9) . . ?
O3 Nb1 Nb2 104.94(12) . . ?
O3 Nb1 O1 177.72(15) . . ?
O3 Nb1 O6 98.22(14) . . ?
O3 Nb1 O4 97.45(15) . . ?
O3 Nb1 O5 98.68(16) . . ?
O3 Nb1 O2 96.66(16) . . ?
O6 Nb1 Nb2 32.72(10) . . ?
O6 Nb1 O1 83.60(12) . . ?
O6 Nb1 O5 72.93(15) . . ?
O4 Nb1 Nb2 125.72(13) . . ?
O4 Nb1 O1 81.21(13) . . ?
O4 Nb1 O6 156.80(16) . . ?
O4 Nb1 O5 87.88(17) . . ?
O5 Nb1 Nb2 40.68(10) . . ?
O5 Nb1 O1 83.14(14) . . ?
O2 Nb1 Nb2 124.40(11) . . ?
O2 Nb1 O1 81.81(15) . . ?
O2 Nb1 O6 94.52(15) . . ?
O2 Nb1 O4 100.54(18) . . ?
O2 Nb1 O5 161.39(14) . . ?
C20B O13B Nb3B 140.3(17) . . ?
C26B O17B Nb3B 144.3(13) . . ?
C24 O15B Nb3B 128.8(8) . . ?
C22B O14B Nb3B 136.2(12) . . ?
C28B O16B Nb3B 145.4(15) . . ?
O16B C28B H28A 108.7 . . ?
O16B C28B H28B 108.7 . . ?
O16B C28B C29B 114(2) . . ?
H28A C28B H28B 107.6 . . ?
C29B C28B H28A 108.7 . . ?
C29B C28B H28B 108.7 . . ?
H23A C23B H23B 109.5 . . ?
H23A C23B H23C 109.5 . . ?
H23B C23B H23C 109.5 . . ?
C22B C23B H23A 109.5 . . ?
C22B C23B H23B 109.5 . . ?
C22B C23B H23C 109.5 . . ?
O14B C22B C23B 112.5(17) . . ?
O14B C22B H22A 109.1 . . ?
O14B C22B H22B 109.1 . . ?
C23B C22B H22A 109.1 . . ?
C23B C22B H22B 109.1 . . ?
H22A C22B H22B 107.8 . . ?
O15B C24 H24C 112.9 . . ?
O15B C24 H24D 112.9 . . ?
H24C C24 H24D 110.3 . . ?
H24A C24 H24B 105.9 . . ?
C25 C24 O15B 94.0(9) . . ?
C25 C24 H24C 112.9 . . ?
C25 C24 H24D 112.9 . . ?
C25 C24 H24A 105.2 . . ?
C25 C24 H24B 105.2 . . ?
O15A C24 H24A 105.2 . . ?
O15A C24 H24B 105.2 . . ?
O15A C24 C25 128.6(9) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O13B C20B H20A 103.0 . . ?
O13B C20B H20B 103.0 . . ?
O13B C20B C21B 137(3) . . ?
H20A C20B H20B 105.1 . . ?
C21B C20B H20A 103.0 . . ?
C21B C20B H20B 103.0 . . ?
H27A C27B H27B 109.5 . . ?
H27A C27B H27C 109.5 . . ?
H27B C27B H27C 109.5 . . ?
C26B C27B H27A 109.5 . . ?
C26B C27B H27B 109.5 . . ?
C26B C27B H27C 109.5 . . ?
O17B C26B H26A 108.3 . . ?
O17B C26B H26B 108.3 . . ?
C27B C26B O17B 115.9(19) . . ?
C27B C26B H26A 108.3 . . ?
C27B C26B H26B 108.3 . . ?
H26A C26B H26B 107.4 . . ?
C19A O12A Nb3A 137.8(13) . . ?
O12A Nb3A O15A 78.0(4) . . ?
O17A Nb3A O12A 80.9(4) . . ?
O17A Nb3A O15A 85.3(5) . . ?
O17A Nb3A O13A 96.1(5) . . ?
O16A Nb3A O12A 83.1(4) . . ?
O16A Nb3A O17A 162.0(5) . . ?
O16A Nb3A O15A 83.4(5) . . ?
O16A Nb3A O13A 94.2(5) . . ?
O14A Nb3A O12A 161.5(5) . . ?
O14A Nb3A O17A 94.7(5) . . ?
O14A Nb3A O16A 97.9(5) . . ?
O14A Nb3A O15A 83.8(5) . . ?
O14A Nb3A O13A 100.0(5) . . ?
O13A Nb3A O12A 98.3(4) . . ?
O13A Nb3A O15A 175.8(4) . . ?
O12A C19A C18 115.0(19) . . ?
O11A C19A C18 119(2) . . ?
O11A C19A O12A 125(3) . . ?
C26A O17A Nb3A 145.9(11) . . ?
O17A C26A H26C 108.6 . . ?
O17A C26A H26D 108.6 . . ?
O17A C26A C27A 114.6(17) . . ?
H26C C26A H26D 107.6 . . ?
C27A C26A H26C 108.6 . . ?
C27A C26A H26D 108.6 . . ?
C26A C27A H27D 109.5 . . ?
C26A C27A H27E 109.5 . . ?
C26A C27A H27F 109.5 . . ?
H27D C27A H27E 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C28A O16A Nb3A 142.4(12) . . ?
O16A C28A H28C 109.3 . . ?
O16A C28A H28D 109.3 . . ?
O16A C28A C29A 111.6(10) . . ?
H28C C28A H28D 108.0 . . ?
C29A C28A H28C 109.3 . . ?
C29A C28A H28D 109.3 . . ?
C28A C29A H29A 109.5 . . ?
C28A C29A H29B 109.5 . . ?
C28A C29A H29C 109.5 . . ?
H29A C29A H29B 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C24 O15A Nb3A 129.3(8) . . ?
C22A O14A Nb3A 135.5(15) . . ?
O14A C22A H22C 106.6 . . ?
O14A C22A H22D 106.6 . . ?
O14A C22A C23A 122.9(19) . . ?
H22C C22A H22D 106.6 . . ?
C23A C22A H22C 106.6 . . ?
C23A C22A H22D 106.6 . . ?
C22A C23A H23D 109.5 . . ?
C22A C23A H23E 109.5 . . ?
C22A C23A H23F 109.5 . . ?
H23D C23A H23E 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C20A O13A Nb3A 136.7(13) . . ?
O13A C20A H20C 107.4 . . ?
O13A C20A H20D 107.4 . . ?
H20C C20A H20D 106.9 . . ?
C21A C20A O13A 119.7(16) . . ?
C21A C20A H20C 107.4 . . ?
C21A C20A H20D 107.4 . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
H21A C21A H21B 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C28B C29B H29D 109.5 . . ?
C28B C29B H29E 109.5 . . ?
C28B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C20B C21B H21D 109.5 . . ?
C20B C21B H21E 109.5 . . ?
C20B C21B H21F 109.5 . . ?
H21D C21B H21E 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 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
Nb2 O7 C15 O1 6.3(7) . . . . ?
Nb2 O7 C15 C16 -168.7(3) . . . . ?
Nb2 O8 C9 C10 -90.9(8) . . . . ?
Nb2 O9 C7 C8 -93.4(9) . . . . ?
Nb2 O10 C5 C6 -119.3(9) . . . . ?
Nb2 O5 C13 C14 -115.7(6) . . . . ?
O7 Nb2 O9 C7 12.2(9) . . . . ?
O7 C15 C16 C17 88.2(5) . . . . ?
O7 C15 C16 C18 -90.4(5) . . . . ?
O1 C15 C16 C17 -87.3(5) . . . . ?
O1 C15 C16 C18 94.1(6) . . . . ?
O6 Nb2 O9 C7 94.4(9) . . . . ?
O6 Nb2 O10 C5 11.2(8) . . . . ?
O8 Nb2 O9 C7 -67.4(9) . . . . ?
O8 Nb2 O10 C5 170.8(7) . . . . ?
O9 Nb2 O10 C5 -88.2(8) . . . . ?
O10 Nb2 O9 C7 -167.5(9) . . . . ?
O5 Nb2 O9 C7 42.1(12) . . . . ?
O5 Nb2 O10 C5 83.8(8) . . . . ?
C15 C16 C17 C18 -179.2(4) . . . 7_556 ?
C15 C16 C18 C17 179.0(4) . . . 7_556 ?
C15 C16 C18 C19B -12.8(10) . . . . ?
C15 C16 C18 C19A 8.5(10) . . . . ?
C16 C18 C19B O11B 9.2(19) . . . . ?
C16 C18 C19B O12B -175.0(11) . . . . ?
C16 C18 C19A O12A 172.7(10) . . . . ?
C16 C18 C19A O11A -13.7(19) . . . . ?
C3 O3 Nb1 Nb2 -83.3(7) . . . . ?
C3 O3 Nb1 O6 -50.6(7) . . . . ?
C3 O3 Nb1 O4 146.6(7) . . . . ?
C3 O3 Nb1 O5 -124.4(7) . . . . ?
C3 O3 Nb1 O2 45.0(7) . . . . ?
C11 O4 Nb1 Nb2 64.7(8) . . . . ?
C11 O4 Nb1 O1 -2.7(8) . . . . ?
C11 O4 Nb1 O3 179.2(8) . . . . ?
C11 O4 Nb1 O6 47.0(10) . . . . ?
C11 O4 Nb1 O5 80.7(8) . . . . ?
C11 O4 Nb1 O2 -82.6(8) . . . . ?
C1 O2 Nb1 Nb2 -49.7(7) . . . . ?
C1 O2 Nb1 O1 18.8(7) . . . . ?
C1 O2 Nb1 O3 -162.9(7) . . . . ?
C1 O2 Nb1 O6 -64.1(7) . . . . ?
C1 O2 Nb1 O4 98.2(7) . . . . ?
C1 O2 Nb1 O5 -17.6(10) . . . . ?
C17 C16 C18 C17 0.4(7) . . . 7_556 ?
C17 C16 C18 C19B 168.6(8) . . . . ?
C17 C16 C18 C19A -170.1(8) . . . . ?
C17 C18 C19B O11B 177.5(13) 7_556 . . . ?
C17 C18 C19B O12B -6.7(17) 7_556 . . . ?
C17 C18 C19A O12A 2.2(16) 7_556 . . . ?
C17 C18 C19A O11A 175.8(13) 7_556 . . . ?
C18 C16 C17 C18 -0.4(8) . . . 7_556 ?
C18 C19B O12B Nb3B -174.3(9) . . . . ?
O11B C19B O12B Nb3B 1(3) . . . . ?
O12B Nb3B O13B C20B -93(3) . . . . ?
O12B Nb3B O17B C26B 47(2) . . . . ?
O12B Nb3B O14B C22B -93(3) . . . . ?
O12B Nb3B O16B C28B -31(3) . . . . ?
Nb3B O13B C20B C21B -25(7) . . . . ?
Nb3B O17B C26B C27B -179.7(15) . . . . ?
Nb3B O15B C24 C25 120.7(10) . . . . ?
Nb3B O14B C22B C23B 159.2(12) . . . . ?
Nb3B O16B C28B C29B 109(4) . . . . ?
Nb1 Nb2 O9 C7 79.5(9) . . . . ?
Nb1 Nb2 O10 C5 44.2(8) . . . . ?
Nb1 O1 C15 O7 -4.6(7) . . . . ?
Nb1 O1 C15 C16 170.5(3) . . . . ?
Nb1 O3 C3 C4 -174.3(5) . . . . ?
Nb1 O4 C11 C12 104.6(8) . . . . ?
Nb1 O5 C13 C14 77.0(7) . . . . ?
Nb1 O2 C1 C2 75.2(11) . . . . ?
O13B Nb3B O17B C26B 141(2) . . . . ?
O13B Nb3B O14B C22B 88.8(19) . . . . ?
O13B Nb3B O16B C28B -126(3) . . . . ?
O17B Nb3B O13B C20B -176(3) . . . . ?
O17B Nb3B O14B C22B -8.7(19) . . . . ?
O17B Nb3B O16B C28B 4(4) . . . . ?
O15B Nb3B O17B C26B -32(2) . . . . ?
O15B Nb3B O14B C22B -91.7(19) . . . . ?
O15B Nb3B O16B C28B 48(3) . . . . ?
O14B Nb3B O13B C20B 86(3) . . . . ?
O14B Nb3B O17B C26B -119(2) . . . . ?
O14B Nb3B O16B C28B 135(3) . . . . ?
O16B Nb3B O13B C20B -10(3) . . . . ?
O16B Nb3B O17B C26B 12(3) . . . . ?
O16B Nb3B O14B C22B -174.9(19) . . . . ?
C25 C24 O15A Nb3A 90.6(13) . . . . ?
O12A Nb3A O17A C26A 24.4(19) . . . . ?
O12A Nb3A O16A C28A -25.1(13) . . . . ?
O12A Nb3A O14A C22A -81(3) . . . . ?
Nb3A O12A C19A C18 164.9(9) . . . . ?
Nb3A O12A C19A O11A -8(3) . . . . ?
Nb3A O17A C26A C27A 168.1(18) . . . . ?
Nb3A O16A C28A C29A 91.5(18) . . . . ?
Nb3A O14A C22A C23A -144(3) . . . . ?
Nb3A O13A C20A C21A -43(3) . . . . ?
O17A Nb3A O16A C28A 2(2) . . . . ?
O17A Nb3A O14A C22A -6(3) . . . . ?
O16A Nb3A O17A C26A -3(3) . . . . ?
O16A Nb3A O14A C22A -173(3) . . . . ?
O15A Nb3A O17A C26A -54.2(19) . . . . ?
O15A Nb3A O16A C28A 53.5(13) . . . . ?
O15A Nb3A O14A C22A -91(3) . . . . ?
O14A Nb3A O17A C26A -138(2) . . . . ?
O14A Nb3A O16A C28A 136.3(13) . . . . ?
O13A Nb3A O17A C26A 121.9(19) . . . . ?
O13A Nb3A O16A C28A -123.0(13) . . . . ?
O13A Nb3A O14A C22A 91(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_gar218
_database_code_depnum_ccdc_archive 'CCDC 2179580'
loop_
_audit_author_name
_audit_author_address
'Sylvain Duval'
;University of Lille
France
;
_audit_update_record             
;
2022-06-16 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_audit_creation_date             2022-01-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H146 N2 Nb8 O40'
_chemical_formula_sum            'C72 H146 N2 Nb8 O40'
_chemical_formula_weight         2423.18
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'

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

_cell_length_a                   8.0483(9)
_cell_length_b                   18.5558(19)
_cell_length_c                   18.624(2)
_cell_angle_alpha                68.271(4)
_cell_angle_beta                 81.253(5)
_cell_angle_gamma                84.084(5)
_cell_volume                     2550.4(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2832
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      23.67
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   0.926
_shelx_estimated_absorpt_T_min   0.885
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0751 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8913.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.083
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.1692
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31082
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         1.339
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5345
_reflns_number_total             10333
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.746
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10333
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.0675
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0530P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1442
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21B-C22B
 1.5 with sigma of 0.02
 O10-C21B
 1.4 with sigma of 0.02
 C21A-O10
 1.4 with sigma of 0.02
 C22A-C21A
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C35A, C36A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13B, C14B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33A, C34A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33B, C34B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C13B) \\sim Ueq, Uanis(C14B) \\sim Ueq, Uanis(C13A) \\sim Ueq,
Uanis(C21B) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C35B) \\sim Ueq,
Uanis(C35A) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.02
Uanis(C24B) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Others
 Sof(C13B)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=1-FVAR(1)
 Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=1-FVAR(2)
 Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=FVAR(2)
 Sof(C36B)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35B)=Sof(H35A)=Sof(H35B)=1-FVAR(3)
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=FVAR(3)
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(4)
 Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=FVAR(4)
 Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H22C)=1-FVAR(5)
 Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C11(H11A,H11B), C9(H9A,H9B),
 C23(H23A,H23B), C23(H23C,H23D), C33B(H33A,H33B), C29(H29A,H29B), C31(H31A,
 H31B), C35B(H35A,H35B), C13B(H13A,H13B), C27(H27A,H27B), C25(H25A,H25B),
 C13A(H13C,H13D), C21B(H21A,H21B), C35A(H35C,H35D), C33A(H33C,H33D), C21A(H21C,
 H21D)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C12(H12A,H12B,
 H12C), C10(H10A,H10B,H10C), C36B(H36A,H36B,H36C), C26(H26A,H26B,H26C),
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C34A(H34A,H34B,H34C), C14A(H14A,H14B,
 H14C), C24A(H24A,H24B,H24C), C14B(H14D,H14E,H14F), C22B(H22A,H22B,H22C),
 C24B(H24D,H24E,H24F), C36A(H36D,H36E,H36F), C34B(H34D,H34E,H34F), C28(H28A,
 H28B,H28C), C22A(H22D,H22E,H22F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.53512(9) 0.28620(4) 0.54508(3) 0.02121(19) Uani 1 1 d . . . . .
Nb2 Nb 0.58652(10) 0.40065(4) 0.36466(4) 0.0238(2) Uani 1 1 d . . . . .
Nb3 Nb 0.19858(11) 0.26474(5) 0.04083(4) 0.0419(3) Uani 1 1 d . . . . .
Nb4 Nb 0.00177(12) 0.10622(5) 0.10846(4) 0.0465(3) Uani 1 1 d . . . . .
O3 O 0.4189(6) 0.2243(2) 0.4864(2) 0.0215(12) Uani 1 1 d . . . . .
O6 O 0.6367(7) 0.3356(3) 0.5960(3) 0.0298(13) Uani 1 1 d . . . . .
O12 O 0.2295(7) 0.2214(3) 0.1673(2) 0.0330(14) Uani 1 1 d . . . . .
C8 C 0.1626(10) 0.1648(5) 0.2214(4) 0.027(2) Uani 1 1 d . . . . .
O13 O 0.0794(7) 0.1151(3) 0.2124(2) 0.0307(14) Uani 1 1 d . . . . .
O2 O 0.4634(6) 0.3002(3) 0.3599(2) 0.0241(12) Uani 1 1 d . . . . .
O5 O 0.6550(6) 0.1878(3) 0.5797(2) 0.0245(12) Uani 1 1 d . . . . .
O14 O -0.2119(8) 0.0882(4) 0.1636(3) 0.060(2) Uani 1 1 d . . . . .
O8 O 0.6943(7) 0.4804(3) 0.3733(3) 0.0319(14) Uani 1 1 d . . . . .
O1 O 0.4472(6) 0.3738(3) 0.4649(2) 0.0208(12) Uani 1 1 d . . . . .
O9 O 0.7427(7) 0.3794(3) 0.2872(3) 0.0307(13) Uani 1 1 d . . . . .
C4 C 0.1186(9) 0.0825(4) 0.4412(3) 0.0152(16) Uani 1 1 d . . . . .
C15 C 0.8949(10) 0.2879(4) 0.4411(4) 0.029(2) Uani 1 1 d . . . . .
H15A H 0.945801 0.310984 0.386200 0.035 Uiso 1 1 calc R U . . .
H15B H 0.906558 0.230706 0.456772 0.035 Uiso 1 1 calc R U . . .
O20 O 0.1368(8) 0.3580(3) 0.0566(3) 0.0502(17) Uani 1 1 d . . . . .
C7 C 0.2758(9) 0.2034(4) 0.3209(4) 0.0206(17) Uani 1 1 d . . . . .
H7 H 0.329521 0.245019 0.279690 0.025 Uiso 1 1 calc R U . . .
O15 O 0.1046(9) 0.0052(3) 0.1530(4) 0.065(2) Uani 1 1 d . . . . .
O7 O 0.7208(6) 0.3119(3) 0.4473(2) 0.0199(12) Uani 1 1 d . . . . .
O16 O -0.0415(9) 0.0990(4) 0.0169(3) 0.067(2) Uani 1 1 d . . . . .
N1 N 0.0446(7) 0.0214(3) 0.5083(3) 0.0174(14) Uani 1 1 d . . . . .
O18 O 0.1707(8) 0.2978(4) -0.0653(3) 0.065(2) Uani 1 1 d . . . . .
C5 C 0.0982(9) 0.0944(4) 0.3651(3) 0.0180(17) Uani 1 1 d . . . . .
H5 H 0.029692 0.061767 0.354331 0.022 Uiso 1 1 calc R U . . .
C6 C 0.1802(9) 0.1553(4) 0.3038(4) 0.0199(17) Uani 1 1 d . . . . .
O17 O 0.2463(8) 0.1450(3) 0.0583(3) 0.0425(16) Uani 1 1 d . . . . .
C3 C 0.2142(9) 0.1307(4) 0.4568(4) 0.0196(17) Uani 1 1 d . . . . .
H3 H 0.225864 0.122345 0.509314 0.024 Uiso 1 1 calc R U . . .
C17 C 0.7118(12) 0.5170(5) 0.4268(5) 0.048(3) Uani 1 1 d . . . . .
H17A H 0.717707 0.476679 0.479188 0.058 Uiso 1 1 calc R U . . .
H17B H 0.610812 0.551518 0.430001 0.058 Uiso 1 1 calc R U . . .
C2 C 0.2945(9) 0.1918(4) 0.3967(4) 0.0184(17) Uani 1 1 d . . . . .
C19 C 0.8094(11) 0.3215(5) 0.2570(4) 0.040(2) Uani 1 1 d . . . . .
H19A H 0.780256 0.269812 0.295866 0.048 Uiso 1 1 calc R U . . .
H19B H 0.933655 0.323020 0.247562 0.048 Uiso 1 1 calc R U . . .
C20 C 0.7434(13) 0.3326(5) 0.1831(5) 0.056(3) Uani 1 1 d . . . . .
H20A H 0.620294 0.332016 0.192059 0.084 Uiso 1 1 calc R U . . .
H20B H 0.789113 0.290486 0.164831 0.084 Uiso 1 1 calc R U . . .
H20C H 0.777327 0.382536 0.143634 0.084 Uiso 1 1 calc R U . . .
C18 C 0.8606(13) 0.5623(7) 0.4048(7) 0.092(4) Uani 1 1 d . . . . .
H18A H 0.863997 0.587757 0.442120 0.138 Uiso 1 1 calc R U . . .
H18B H 0.856606 0.601713 0.352539 0.138 Uiso 1 1 calc R U . . .
H18C H 0.961504 0.527868 0.404775 0.138 Uiso 1 1 calc R U . . .
C16 C 0.9861(12) 0.3126(6) 0.4915(6) 0.072(3) Uani 1 1 d . . . . .
H16A H 1.105617 0.296553 0.485433 0.108 Uiso 1 1 calc R U . . .
H16B H 0.938451 0.288238 0.546074 0.108 Uiso 1 1 calc R U . . .
H16C H 0.973934 0.369240 0.476211 0.108 Uiso 1 1 calc R U . . .
O4 O 0.3420(6) 0.2612(3) 0.6170(2) 0.0257(13) Uani 1 1 d . . . . .
O10 O 0.4226(8) 0.4601(3) 0.3033(3) 0.0348(14) Uani 1 1 d D . . . .
O11 O -0.0164(7) 0.2180(3) 0.0778(3) 0.0409(15) Uani 1 1 d . . . . .
O19 O 0.4310(8) 0.2740(3) 0.0259(3) 0.0479(17) Uani 1 1 d . . . . .
C1 C 0.3985(9) 0.2434(4) 0.4153(4) 0.0161(16) Uani 1 1 d . . . . .
C11 C 0.6995(10) 0.1229(4) 0.5562(4) 0.028(2) Uani 1 1 d . . . . .
H11A H 0.815177 0.102957 0.567578 0.034 Uiso 1 1 calc R U . . .
H11B H 0.697582 0.139330 0.499280 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5792(11) 0.0593(4) 0.5981(4) 0.036(2) Uani 1 1 d . . . . .
H12A H 0.581097 0.042946 0.654400 0.054 Uiso 1 1 calc R U . . .
H12B H 0.612903 0.014908 0.581648 0.054 Uiso 1 1 calc R U . . .
H12C H 0.465125 0.078520 0.585557 0.054 Uiso 1 1 calc R U . . .
C9 C 0.2313(12) 0.2051(5) 0.6672(5) 0.052(3) Uani 1 1 d . . . . .
H9A H 0.204607 0.171574 0.640135 0.063 Uiso 1 1 calc R U . . .
H9B H 0.124897 0.231174 0.681643 0.063 Uiso 1 1 calc R U . . .
C10 C 0.3099(13) 0.1548(5) 0.7414(5) 0.064(3) Uani 1 1 d . . . . .
H10A H 0.425114 0.137545 0.726937 0.096 Uiso 1 1 calc R U . . .
H10B H 0.242784 0.109351 0.770077 0.096 Uiso 1 1 calc R U . . .
H10C H 0.311973 0.185343 0.774266 0.096 Uiso 1 1 calc R U . . .
C36B C -0.340(3) 0.1174(14) 0.2677(17) 0.051(9) Uani 0.58(3) 1 d . . P A 6
H36A H -0.237527 0.132522 0.279748 0.076 Uiso 0.58(3) 1 calc R U P A 6
H36B H -0.416221 0.095467 0.315907 0.076 Uiso 0.58(3) 1 calc R U P A 6
H36C H -0.395791 0.163096 0.231878 0.076 Uiso 0.58(3) 1 calc R U P A 6
C23 C 0.1833(17) 0.4084(7) 0.0878(6) 0.080(4) Uani 1 1 d . . . . .
H23A H 0.113479 0.399847 0.138512 0.096 Uiso 0.49(5) 1 calc R U P B 3
H23B H 0.301797 0.395063 0.098071 0.096 Uiso 0.49(5) 1 calc R U P B 3
H23C H 0.098579 0.452498 0.076548 0.096 Uiso 0.51(5) 1 calc R U P B 4
H23D H 0.169519 0.381207 0.144983 0.096 Uiso 0.51(5) 1 calc R U P B 4
C33B C 0.229(5) -0.039(2) 0.1941(13) 0.034(8) Uani 0.44(2) 1 d . U P C 8
H33A H 0.305350 -0.006390 0.204998 0.041 Uiso 0.44(2) 1 calc R U P C 8
H33B H 0.295243 -0.071547 0.167455 0.041 Uiso 0.44(2) 1 calc R U P C 8
C26 C 0.6865(14) 0.3358(7) -0.0307(7) 0.115(5) Uani 1 1 d . . . . .
H26A H 0.806098 0.332819 -0.024471 0.173 Uiso 1 1 calc R U . . .
H26B H 0.632722 0.383600 -0.025058 0.173 Uiso 1 1 calc R U . . .
H26C H 0.675362 0.336113 -0.082468 0.173 Uiso 1 1 calc R U . . .
C29 C 0.4048(14) 0.1022(6) 0.0577(5) 0.067(3) Uani 1 1 d . . . . .
H29A H 0.389117 0.046428 0.088410 0.080 Uiso 1 1 calc R U . . .
H29B H 0.484002 0.120862 0.081922 0.080 Uiso 1 1 calc R U . . .
C31 C 0.0127(15) 0.1151(8) -0.0652(6) 0.102(5) Uani 1 1 d . . . . .
H31A H -0.018808 0.072633 -0.079840 0.122 Uiso 1 1 calc R U . . .
H31B H 0.136685 0.117821 -0.075569 0.122 Uiso 1 1 calc R U . . .
C35B C -0.295(3) 0.0571(15) 0.2301(9) 0.042(6) Uani 0.58(3) 1 d . U P A 6
H35A H -0.225980 0.013584 0.263232 0.050 Uiso 0.58(3) 1 calc R U P A 6
H35B H -0.398191 0.036168 0.224610 0.050 Uiso 0.58(3) 1 calc R U P A 6
C32 C -0.0658(15) 0.1883(8) -0.1117(6) 0.107(5) Uani 1 1 d . . . . .
H32A H -0.009613 0.204867 -0.165310 0.160 Uiso 1 1 calc R U . . .
H32B H -0.055544 0.227872 -0.089611 0.160 Uiso 1 1 calc R U . . .
H32C H -0.185067 0.181600 -0.111441 0.160 Uiso 1 1 calc R U . . .
C30 C 0.4802(16) 0.1127(8) -0.0287(7) 0.122(5) Uani 1 1 d . . . . .
H30A H 0.492749 0.168040 -0.059346 0.184 Uiso 1 1 calc R U . . .
H30B H 0.404210 0.091726 -0.051694 0.184 Uiso 1 1 calc R U . . .
H30C H 0.590485 0.084848 -0.028768 0.184 Uiso 1 1 calc R U . . .
C34A C 0.224(5) -0.1161(14) 0.2351(19) 0.085(14) Uani 0.44(2) 1 d . U P C 7
H34A H 0.253778 -0.144929 0.287701 0.127 Uiso 0.44(2) 1 calc R U P C 7
H34B H 0.322857 -0.115480 0.196878 0.127 Uiso 0.44(2) 1 calc R U P C 7
H34C H 0.133158 -0.141431 0.225519 0.127 Uiso 0.44(2) 1 calc R U P C 7
C13B C 0.621(5) 0.3617(16) 0.662(2) 0.041(7) Uani 0.49(3) 1 d . U P D 2
H13A H 0.501998 0.360618 0.686141 0.049 Uiso 0.49(3) 1 calc R U P D 2
H13B H 0.656231 0.415773 0.644264 0.049 Uiso 0.49(3) 1 calc R U P D 2
C27 C 0.2634(16) 0.3385(8) -0.1375(5) 0.102(5) Uani 1 1 d . . . . .
H27A H 0.384181 0.322378 -0.134851 0.122 Uiso 1 1 calc R U . . .
H27B H 0.226479 0.324234 -0.178591 0.122 Uiso 1 1 calc R U . . .
C14A C 0.601(5) 0.3335(17) 0.7233(13) 0.065(10) Uani 0.49(3) 1 d . U P D 1
H14A H 0.483777 0.349488 0.713476 0.097 Uiso 0.49(3) 1 calc R U P D 1
H14B H 0.633845 0.359060 0.756110 0.097 Uiso 0.49(3) 1 calc R U P D 1
H14C H 0.610519 0.277028 0.749915 0.097 Uiso 0.49(3) 1 calc R U P D 1
C25 C 0.6047(13) 0.2682(6) 0.0292(5) 0.056(3) Uani 1 1 d . . . . .
H25A H 0.653750 0.220202 0.021220 0.068 Uiso 1 1 calc R U . . .
H25B H 0.625850 0.264980 0.081323 0.068 Uiso 1 1 calc R U . . .
C24A C 0.169(11) 0.483(2) 0.044(2) 0.20(4) Uani 0.49(5) 1 d . U P B 3
H24A H 0.118742 0.512661 0.077169 0.299 Uiso 0.49(5) 1 calc R U P B 3
H24B H 0.097960 0.490704 0.003726 0.299 Uiso 0.49(5) 1 calc R U P B 3
H24C H 0.281272 0.502105 0.020000 0.299 Uiso 0.49(5) 1 calc R U P B 3
C13A C 0.714(5) 0.3564(19) 0.6473(13) 0.047(7) Uani 0.51(3) 1 d . U P D 1
H13C H 0.728396 0.413047 0.626453 0.056 Uiso 0.51(3) 1 calc R U P D 1
H13D H 0.825591 0.329059 0.654549 0.056 Uiso 0.51(3) 1 calc R U P D 1
C14B C 0.730(4) 0.3093(12) 0.7220(11) 0.049(7) Uani 0.51(3) 1 d . U P D 2
H14D H 0.668500 0.263261 0.755628 0.074 Uiso 0.51(3) 1 calc R U P D 2
H14E H 0.757841 0.337217 0.753721 0.074 Uiso 0.51(3) 1 calc R U P D 2
H14F H 0.833260 0.293271 0.695511 0.074 Uiso 0.51(3) 1 calc R U P D 2
C21B C 0.331(2) 0.4664(10) 0.2414(8) 0.047(6) Uani 0.57(2) 1 d D U P E 9
H21A H 0.374339 0.427060 0.218020 0.057 Uiso 0.57(2) 1 calc R U P E 9
H21B H 0.339481 0.518690 0.200289 0.057 Uiso 0.57(2) 1 calc R U P E 9
C22B C 0.154(3) 0.453(2) 0.2780(18) 0.120(13) Uani 0.57(2) 1 d D . P E 9
H22A H 0.084610 0.452047 0.239272 0.180 Uiso 0.57(2) 1 calc R U P E 9
H22B H 0.110796 0.494147 0.297493 0.180 Uiso 0.57(2) 1 calc R U P E 9
H22C H 0.149586 0.402479 0.321392 0.180 Uiso 0.57(2) 1 calc R U P E 9
C24B C 0.334(7) 0.439(3) 0.069(4) 0.20(4) Uani 0.51(5) 1 d . U P B 4
H24D H 0.421657 0.398674 0.067651 0.301 Uiso 0.51(5) 1 calc R U P B 4
H24E H 0.352167 0.460871 0.107266 0.301 Uiso 0.51(5) 1 calc R U P B 4
H24F H 0.338218 0.480380 0.017123 0.301 Uiso 0.51(5) 1 calc R U P B 4
C35A C -0.372(4) 0.106(3) 0.2246(13) 0.043(10) Uani 0.42(3) 1 d . U P A 5
H35C H -0.416139 0.159708 0.200555 0.052 Uiso 0.42(3) 1 calc R U P A 5
H35D H -0.462903 0.070890 0.230870 0.052 Uiso 0.42(3) 1 calc R U P A 5
C36A C -0.328(4) 0.094(2) 0.3047(16) 0.037(8) Uani 0.42(3) 1 d . U P A 5
H36D H -0.282041 0.040728 0.328943 0.056 Uiso 0.42(3) 1 calc R U P A 5
H36E H -0.429240 0.103079 0.337300 0.056 Uiso 0.42(3) 1 calc R U P A 5
H36F H -0.243512 0.130681 0.299694 0.056 Uiso 0.42(3) 1 calc R U P A 5
C33A C 0.173(5) -0.0430(15) 0.228(2) 0.072(10) Uani 0.56(2) 1 d . U P C 7
H33C H 0.269362 -0.016738 0.233344 0.086 Uiso 0.56(2) 1 calc R U P C 7
H33D H 0.084863 -0.044692 0.272114 0.086 Uiso 0.56(2) 1 calc R U P C 7
C34B C 0.115(3) -0.0888(13) 0.2710(9) 0.036(6) Uani 0.56(2) 1 d . U P C 8
H34D H 0.182855 -0.132684 0.302538 0.054 Uiso 0.56(2) 1 calc R U P C 8
H34E H 0.021311 -0.108296 0.256491 0.054 Uiso 0.56(2) 1 calc R U P C 8
H34F H 0.069895 -0.056118 0.301274 0.054 Uiso 0.56(2) 1 calc R U P C 8
C28 C 0.244(3) 0.4181(10) -0.1574(9) 0.240(14) Uani 1 1 d . . . . .
H28A H 0.126458 0.434988 -0.165301 0.359 Uiso 1 1 calc R U . . .
H28B H 0.317395 0.443451 -0.205594 0.359 Uiso 1 1 calc R U . . .
H28C H 0.273967 0.432226 -0.115461 0.359 Uiso 1 1 calc R U . . .
C21A C 0.251(3) 0.4462(17) 0.304(2) 0.113(16) Uani 0.43(2) 1 d D U P E 10
H21C H 0.192881 0.435121 0.357337 0.135 Uiso 0.43(2) 1 calc R U P E 10
H21D H 0.248389 0.398998 0.291252 0.135 Uiso 0.43(2) 1 calc R U P E 10
C22A C 0.152(4) 0.5109(17) 0.2487(17) 0.072(11) Uani 0.43(2) 1 d D . P E 10
H22D H 0.227302 0.539441 0.202452 0.108 Uiso 0.43(2) 1 calc R U P E 10
H22E H 0.099853 0.546414 0.274697 0.108 Uiso 0.43(2) 1 calc R U P E 10
H22F H 0.063809 0.489065 0.233058 0.108 Uiso 0.43(2) 1 calc R U P E 10


_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
Nb1 Nb2 3.2322(9) . ?
Nb1 O3 2.202(4) . ?
Nb1 O6 1.855(5) . ?
Nb1 O5 1.907(4) . ?
Nb1 O1 1.913(4) . ?
Nb1 O7 2.111(4) . ?
Nb1 O4 1.865(5) . ?
Nb2 O2 2.234(4) . ?
Nb2 O8 1.858(5) . ?
Nb2 O1 1.944(4) . ?
Nb2 O9 1.894(5) . ?
Nb2 O7 2.124(4) . ?
Nb2 O10 1.868(5) . ?
Nb3 Nb4 3.2184(12) . ?
Nb3 O12 2.234(4) . ?
Nb3 O20 1.865(6) . ?
Nb3 O18 1.883(5) . ?
Nb3 O17 2.124(6) . ?
Nb3 O11 1.930(6) . ?
Nb3 O19 1.865(6) . ?
Nb4 O13 2.188(4) . ?
Nb4 O14 1.858(7) . ?
Nb4 O15 1.904(6) . ?
Nb4 O16 1.846(5) . ?
Nb4 O17 2.121(6) . ?
Nb4 O11 1.933(5) . ?
O3 C1 1.270(7) . ?
O6 C13B 1.47(3) . ?
O6 C13A 1.39(3) . ?
O12 C8 1.256(8) . ?
C8 O13 1.266(8) . ?
C8 C6 1.506(9) . ?
O2 C1 1.263(7) . ?
O5 C11 1.423(8) . ?
O14 C35B 1.267(16) . ?
O14 C35A 1.67(3) . ?
O8 C17 1.428(8) . ?
O9 C19 1.411(8) . ?
C4 N1 1.437(8) . ?
C4 C5 1.384(8) . ?
C4 C3 1.370(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 O7 1.426(8) . ?
C15 C16 1.493(10) . ?
O20 C23 1.376(12) . ?
C7 H7 0.9500 . ?
C7 C6 1.384(9) . ?
C7 C2 1.376(8) . ?
O15 C33B 1.36(4) . ?
O15 C33A 1.51(3) . ?
O16 C31 1.451(11) . ?
N1 N1 1.269(10) 2_556 ?
O18 C27 1.411(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.410(9) . ?
O17 C29 1.433(11) . ?
C3 H3 0.9500 . ?
C3 C2 1.396(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.453(12) . ?
C2 C1 1.495(9) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.487(11) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O4 C9 1.404(9) . ?
O10 C21B 1.424(11) . ?
O10 C21A 1.430(19) . ?
O19 C25 1.400(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.504(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.539(11) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C36B H36A 0.9800 . ?
C36B H36B 0.9800 . ?
C36B H36C 0.9800 . ?
C36B C35B 1.51(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 H23C 0.9900 . ?
C23 H23D 0.9900 . ?
C23 C24A 1.33(4) . ?
C23 C24B 1.33(4) . ?
C33B H33A 0.9900 . ?
C33B H33B 0.9900 . ?
C33B C34B 1.60(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 C25 1.470(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.578(13) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.453(15) . ?
C35B H35A 0.9900 . ?
C35B H35B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C34A C33A 1.34(4) . ?
C13B H13A 0.9900 . ?
C13B H13B 0.9900 . ?
C13B C14B 1.50(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.381(18) . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C14A C13A 1.50(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C13A H13C 0.9900 . ?
C13A H13D 0.9900 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C21B H21A 0.9900 . ?
C21B H21B 0.9900 . ?
C21B C22B 1.488(17) . ?
C22B H22A 0.9800 . ?
C22B H22B 0.9800 . ?
C22B H22C 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C35A C36A 1.52(4) . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?
C33A H33C 0.9900 . ?
C33A H33D 0.9900 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C21A C22A 1.506(19) . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 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
O3 Nb1 Nb2 77.24(11) . . ?
O6 Nb1 Nb2 103.88(15) . . ?
O6 Nb1 O3 178.3(2) . . ?
O6 Nb1 O5 98.8(2) . . ?
O6 Nb1 O1 100.7(2) . . ?
O6 Nb1 O7 95.1(2) . . ?
O6 Nb1 O4 96.3(2) . . ?
O5 Nb1 Nb2 121.13(13) . . ?
O5 Nb1 O3 79.52(18) . . ?
O5 Nb1 O1 151.60(17) . . ?
O5 Nb1 O7 84.48(19) . . ?
O1 Nb1 Nb2 33.36(13) . . ?
O1 Nb1 O3 80.93(17) . . ?
O1 Nb1 O7 73.43(18) . . ?
O7 Nb1 Nb2 40.40(12) . . ?
O7 Nb1 O3 84.89(17) . . ?
O4 Nb1 Nb2 131.30(14) . . ?
O4 Nb1 O3 83.88(18) . . ?
O4 Nb1 O5 98.3(2) . . ?
O4 Nb1 O1 99.9(2) . . ?
O4 Nb1 O7 167.72(19) . . ?
O2 Nb2 Nb1 77.08(11) . . ?
O8 Nb2 Nb1 100.24(14) . . ?
O8 Nb2 O2 176.89(19) . . ?
O8 Nb2 O1 96.60(19) . . ?
O8 Nb2 O9 98.9(2) . . ?
O8 Nb2 O7 93.8(2) . . ?
O8 Nb2 O10 99.0(2) . . ?
O1 Nb2 Nb1 32.77(13) . . ?
O1 Nb2 O2 82.01(17) . . ?
O1 Nb2 O7 72.54(18) . . ?
O9 Nb2 Nb1 123.87(15) . . ?
O9 Nb2 O2 81.47(19) . . ?
O9 Nb2 O1 154.7(2) . . ?
O9 Nb2 O7 86.53(19) . . ?
O7 Nb2 Nb1 40.09(12) . . ?
O7 Nb2 O2 83.13(17) . . ?
O10 Nb2 Nb1 128.14(18) . . ?
O10 Nb2 O2 84.0(2) . . ?
O10 Nb2 O1 97.5(2) . . ?
O10 Nb2 O9 99.7(2) . . ?
O10 Nb2 O7 164.7(2) . . ?
O12 Nb3 Nb4 77.68(13) . . ?
O20 Nb3 Nb4 128.55(18) . . ?
O20 Nb3 O12 82.9(2) . . ?
O20 Nb3 O18 98.8(3) . . ?
O20 Nb3 O17 163.3(2) . . ?
O20 Nb3 O11 97.7(2) . . ?
O18 Nb3 Nb4 100.5(2) . . ?
O18 Nb3 O12 178.1(2) . . ?
O18 Nb3 O17 96.4(2) . . ?
O18 Nb3 O11 94.9(2) . . ?
O17 Nb3 Nb4 40.68(17) . . ?
O17 Nb3 O12 81.81(18) . . ?
O11 Nb3 Nb4 33.60(16) . . ?
O11 Nb3 O12 83.94(19) . . ?
O11 Nb3 O17 74.0(2) . . ?
O19 Nb3 Nb4 126.90(19) . . ?
O19 Nb3 O12 84.3(2) . . ?
O19 Nb3 O20 97.4(3) . . ?
O19 Nb3 O18 96.4(2) . . ?
O19 Nb3 O17 87.8(3) . . ?
O19 Nb3 O11 159.5(2) . . ?
O13 Nb4 Nb3 76.62(13) . . ?
O14 Nb4 Nb3 128.6(2) . . ?
O14 Nb4 O13 86.9(2) . . ?
O14 Nb4 O15 98.8(3) . . ?
O14 Nb4 O17 167.0(2) . . ?
O14 Nb4 O11 96.5(3) . . ?
O15 Nb4 Nb3 124.7(2) . . ?
O15 Nb4 O13 79.8(2) . . ?
O15 Nb4 O17 87.4(3) . . ?
O15 Nb4 O11 155.0(2) . . ?
O16 Nb4 Nb3 100.3(2) . . ?
O16 Nb4 O13 174.3(3) . . ?
O16 Nb4 O14 98.7(3) . . ?
O16 Nb4 O15 98.4(3) . . ?
O16 Nb4 O17 91.6(3) . . ?
O16 Nb4 O11 98.7(2) . . ?
O17 Nb4 Nb3 40.75(16) . . ?
O17 Nb4 O13 82.94(19) . . ?
O11 Nb4 Nb3 33.56(17) . . ?
O11 Nb4 O13 81.42(19) . . ?
O11 Nb4 O17 74.0(2) . . ?
C1 O3 Nb1 130.5(4) . . ?
C13B O6 Nb1 146.2(17) . . ?
C13A O6 Nb1 167.3(13) . . ?
C8 O12 Nb3 128.1(5) . . ?
O12 C8 O13 125.2(6) . . ?
O12 C8 C6 117.8(7) . . ?
O13 C8 C6 117.0(6) . . ?
C8 O13 Nb4 131.9(4) . . ?
C1 O2 Nb2 129.0(4) . . ?
C11 O5 Nb1 139.2(4) . . ?
C35B O14 Nb4 145.1(13) . . ?
C35A O14 Nb4 152.1(11) . . ?
C17 O8 Nb2 142.0(5) . . ?
Nb1 O1 Nb2 113.9(2) . . ?
C19 O9 Nb2 144.6(5) . . ?
C5 C4 N1 124.4(6) . . ?
C3 C4 N1 115.3(5) . . ?
C3 C4 C5 120.3(6) . . ?
H15A C15 H15B 108.0 . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.4 . . ?
O7 C15 C16 110.9(6) . . ?
C16 C15 H15A 109.4 . . ?
C16 C15 H15B 109.5 . . ?
C23 O20 Nb3 143.7(7) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C2 C7 C6 121.1(7) . . ?
C33B O15 Nb4 146.7(15) . . ?
C33A O15 Nb4 137.3(12) . . ?
Nb1 O7 Nb2 99.5(2) . . ?
C15 O7 Nb1 130.6(4) . . ?
C15 O7 Nb2 129.0(4) . . ?
C31 O16 Nb4 147.3(7) . . ?
N1 N1 C4 113.5(6) 2_556 . ?
C27 O18 Nb3 137.1(7) . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.3(6) . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C8 122.3(6) . . ?
C7 C6 C5 119.4(6) . . ?
C5 C6 C8 118.3(6) . . ?
Nb4 O17 Nb3 98.6(2) . . ?
C29 O17 Nb3 128.8(6) . . ?
C29 O17 Nb4 130.4(6) . . ?
C4 C3 H3 119.5 . . ?
C4 C3 C2 121.0(6) . . ?
C2 C3 H3 119.5 . . ?
O8 C17 H17A 109.0 . . ?
O8 C17 H17B 109.0 . . ?
O8 C17 C18 112.8(7) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
C7 C2 C3 118.9(6) . . ?
C7 C2 C1 121.2(6) . . ?
C3 C2 C1 119.9(6) . . ?
O9 C19 H19A 109.3 . . ?
O9 C19 H19B 109.3 . . ?
O9 C19 C20 111.7(7) . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 O4 Nb1 149.3(5) . . ?
C21B O10 Nb2 144.3(7) . . ?
C21A O10 Nb2 131.2(10) . . ?
Nb3 O11 Nb4 112.8(3) . . ?
C25 O19 Nb3 168.3(5) . . ?
O3 C1 C2 116.4(6) . . ?
O2 C1 O3 125.1(6) . . ?
O2 C1 C2 118.4(6) . . ?
O5 C11 H11A 109.5 . . ?
O5 C11 H11B 109.5 . . ?
O5 C11 C12 110.8(6) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O4 C9 H9A 109.5 . . ?
O4 C9 H9B 109.5 . . ?
O4 C9 C10 110.7(8) . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H36A C36B H36B 109.5 . . ?
H36A C36B H36C 109.5 . . ?
H36B C36B H36C 109.5 . . ?
C35B C36B H36A 109.5 . . ?
C35B C36B H36B 109.5 . . ?
C35B C36B H36C 109.5 . . ?
O20 C23 H23A 108.3 . . ?
O20 C23 H23B 108.3 . . ?
O20 C23 H23C 106.5 . . ?
O20 C23 H23D 106.5 . . ?
H23A C23 H23B 107.4 . . ?
H23C C23 H23D 106.5 . . ?
C24A C23 O20 115.8(18) . . ?
C24A C23 H23A 108.3 . . ?
C24A C23 H23B 108.3 . . ?
C24B C23 O20 123(2) . . ?
C24B C23 H23C 106.5 . . ?
C24B C23 H23D 106.5 . . ?
O15 C33B H33A 112.0 . . ?
O15 C33B H33B 112.0 . . ?
O15 C33B C34B 99(2) . . ?
H33A C33B H33B 109.7 . . ?
C34B C33B H33A 112.0 . . ?
C34B C33B H33B 112.0 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
O17 C29 H29A 109.7 . . ?
O17 C29 H29B 109.7 . . ?
O17 C29 C30 110.0(8) . . ?
H29A C29 H29B 108.2 . . ?
C30 C29 H29A 109.7 . . ?
C30 C29 H29B 109.7 . . ?
O16 C31 H31A 109.7 . . ?
O16 C31 H31B 109.7 . . ?
O16 C31 C32 110.0(8) . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
O14 C35B C36B 109(2) . . ?
O14 C35B H35A 109.8 . . ?
O14 C35B H35B 109.8 . . ?
C36B C35B H35A 109.8 . . ?
C36B C35B H35B 109.8 . . ?
H35A C35B H35B 108.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
O6 C13B H13A 109.7 . . ?
O6 C13B H13B 109.7 . . ?
O6 C13B C14B 109.6(18) . . ?
H13A C13B H13B 108.2 . . ?
C14B C13B H13A 109.7 . . ?
C14B C13B H13B 109.7 . . ?
O18 C27 H27A 109.1 . . ?
O18 C27 H27B 109.1 . . ?
H27A C27 H27B 107.8 . . ?
C28 C27 O18 112.6(12) . . ?
C28 C27 H27A 109.1 . . ?
C28 C27 H27B 109.1 . . ?
H14A C14A H14B 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C13A C14A H14A 109.5 . . ?
C13A C14A H14B 109.5 . . ?
C13A C14A H14C 109.5 . . ?
O19 C25 C26 110.9(8) . . ?
O19 C25 H25A 109.5 . . ?
O19 C25 H25B 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C23 C24A H24A 109.5 . . ?
C23 C24A H24B 109.5 . . ?
C23 C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
O6 C13A C14A 107(2) . . ?
O6 C13A H13C 110.3 . . ?
O6 C13A H13D 110.3 . . ?
C14A C13A H13C 110.3 . . ?
C14A C13A H13D 110.3 . . ?
H13C C13A H13D 108.6 . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
O10 C21B H21A 110.7 . . ?
O10 C21B H21B 110.7 . . ?
O10 C21B C22B 105.0(17) . . ?
H21A C21B H21B 108.8 . . ?
C22B C21B H21A 110.7 . . ?
C22B C21B H21B 110.7 . . ?
C21B C22B H22A 109.5 . . ?
C21B C22B H22B 109.5 . . ?
C21B C22B H22C 109.5 . . ?
H22A C22B H22B 109.5 . . ?
H22A C22B H22C 109.5 . . ?
H22B C22B H22C 109.5 . . ?
C23 C24B H24D 109.5 . . ?
C23 C24B H24E 109.5 . . ?
C23 C24B H24F 109.5 . . ?
H24D C24B H24E 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
O14 C35A H35C 108.5 . . ?
O14 C35A H35D 108.5 . . ?
H35C C35A H35D 107.5 . . ?
C36A C35A O14 115(3) . . ?
C36A C35A H35C 108.5 . . ?
C36A C35A H35D 108.5 . . ?
C35A C36A H36D 109.5 . . ?
C35A C36A H36E 109.5 . . ?
C35A C36A H36F 109.5 . . ?
H36D C36A H36E 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 109.5 . . ?
O15 C33A H33C 108.5 . . ?
O15 C33A H33D 108.5 . . ?
C34A C33A O15 115(2) . . ?
C34A C33A H33C 108.5 . . ?
C34A C33A H33D 108.5 . . ?
H33C C33A H33D 107.5 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O10 C21A H21C 108.2 . . ?
O10 C21A H21D 108.2 . . ?
O10 C21A C22A 116(2) . . ?
H21C C21A H21D 107.4 . . ?
C22A C21A H21C 108.2 . . ?
C22A C21A H21D 108.2 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 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
Nb1 Nb2 O8 C17 -26.2(9) . . . . ?
Nb1 Nb2 O9 C19 43.6(9) . . . . ?
Nb1 Nb2 O10 C21B -106.6(14) . . . . ?
Nb1 Nb2 O10 C21A -32(3) . . . . ?
Nb1 O3 C1 O2 9.9(10) . . . . ?
Nb1 O3 C1 C2 -172.6(4) . . . . ?
Nb1 O6 C13B C14B 106(2) . . . . ?
Nb1 O6 C13A C14A -56(8) . . . . ?
Nb1 O5 C11 C12 -97.5(7) . . . . ?
Nb1 O4 C9 C10 75.0(12) . . . . ?
Nb2 Nb1 O6 C13B 132.2(18) . . . . ?
Nb2 Nb1 O6 C13A -161(7) . . . . ?
Nb2 Nb1 O4 C9 119.0(9) . . . . ?
Nb2 O2 C1 O3 -14.3(10) . . . . ?
Nb2 O2 C1 C2 168.3(4) . . . . ?
Nb2 O8 C17 C18 161.0(7) . . . . ?
Nb2 O9 C19 C20 104.6(9) . . . . ?
Nb2 O10 C21B C22B 112.6(18) . . . . ?
Nb2 O10 C21A C22A 176(2) . . . . ?
Nb3 Nb4 O14 C35B -105(2) . . . . ?
Nb3 Nb4 O14 C35A -30(3) . . . . ?
Nb3 Nb4 O16 C31 30.9(12) . . . . ?
Nb3 O12 C8 O13 9.3(12) . . . . ?
Nb3 O12 C8 C6 -169.8(5) . . . . ?
Nb3 O20 C23 C24A 136(4) . . . . ?
Nb3 O20 C23 C24B 55(5) . . . . ?
Nb3 O18 C27 C28 -82.8(18) . . . . ?
Nb3 O17 C29 C30 -83.2(9) . . . . ?
Nb3 O19 C25 C26 -169(3) . . . . ?
Nb4 Nb3 O20 C23 116.6(10) . . . . ?
Nb4 Nb3 O18 C27 -147.2(11) . . . . ?
Nb4 Nb3 O19 C25 -41(3) . . . . ?
Nb4 O14 C35B C36B 95(4) . . . . ?
Nb4 O14 C35A C36A -58(5) . . . . ?
Nb4 O15 C33B C34B 114(2) . . . . ?
Nb4 O15 C33A C34A 175(2) . . . . ?
Nb4 O16 C31 C32 -94.0(14) . . . . ?
Nb4 O17 C29 C30 117.8(8) . . . . ?
O3 Nb1 O4 C9 51.9(10) . . . . ?
O6 Nb1 O4 C9 -126.3(10) . . . . ?
O12 Nb3 O20 C23 48.6(10) . . . . ?
O12 Nb3 O19 C25 29(3) . . . . ?
O12 C8 O13 Nb4 -4.1(12) . . . . ?
O12 C8 C6 C7 -4.5(11) . . . . ?
O12 C8 C6 C5 176.8(7) . . . . ?
O13 Nb4 O14 C35B -35(2) . . . . ?
O13 Nb4 O14 C35A 41(3) . . . . ?
O13 C8 C6 C7 176.3(7) . . . . ?
O13 C8 C6 C5 -2.5(10) . . . . ?
O2 Nb2 O9 C19 -24.5(8) . . . . ?
O2 Nb2 O10 C21B -38.3(14) . . . . ?
O2 Nb2 O10 C21A 36(3) . . . . ?
O5 Nb1 O6 C13B -102.6(18) . . . . ?
O5 Nb1 O6 C13A -35(7) . . . . ?
O5 Nb1 O4 C9 -26.5(10) . . . . ?
O14 Nb4 O16 C31 162.9(12) . . . . ?
O8 Nb2 O9 C19 152.4(8) . . . . ?
O8 Nb2 O10 C21B 142.7(14) . . . . ?
O8 Nb2 O10 C21A -143(3) . . . . ?
O1 Nb1 O6 C13B 98.2(18) . . . . ?
O1 Nb1 O6 C13A 165(7) . . . . ?
O1 Nb1 O4 C9 131.6(10) . . . . ?
O1 Nb2 O8 C17 6.8(9) . . . . ?
O1 Nb2 O9 C19 25.3(11) . . . . ?
O1 Nb2 O10 C21B -119.4(14) . . . . ?
O1 Nb2 O10 C21A -45(3) . . . . ?
O9 Nb2 O8 C17 -153.2(8) . . . . ?
O9 Nb2 O10 C21B 42.0(14) . . . . ?
O9 Nb2 O10 C21A 116(3) . . . . ?
C4 C5 C6 C8 177.2(6) . . . . ?
C4 C5 C6 C7 -1.6(10) . . . . ?
C4 C3 C2 C7 0.3(11) . . . . ?
C4 C3 C2 C1 -179.8(6) . . . . ?
O20 Nb3 O18 C27 80.8(11) . . . . ?
O20 Nb3 O19 C25 111(3) . . . . ?
C7 C2 C1 O3 -174.7(6) . . . . ?
C7 C2 C1 O2 3.0(10) . . . . ?
O15 Nb4 O14 C35B 44(2) . . . . ?
O15 Nb4 O14 C35A 120(3) . . . . ?
O15 Nb4 O16 C31 -96.8(12) . . . . ?
O7 Nb1 O6 C13B 172.2(18) . . . . ?
O7 Nb1 O6 C13A -121(7) . . . . ?
O7 Nb1 O4 C9 75.9(14) . . . . ?
O7 Nb2 O8 C17 -66.1(8) . . . . ?
O7 Nb2 O9 C19 59.1(8) . . . . ?
O7 Nb2 O10 C21B -71.2(17) . . . . ?
O7 Nb2 O10 C21A 3(3) . . . . ?
O16 Nb4 O14 C35B 144(2) . . . . ?
O16 Nb4 O14 C35A -140(3) . . . . ?
N1 C4 C5 C6 -178.6(6) . . . . ?
N1 C4 C3 C2 179.3(6) . . . . ?
O18 Nb3 O20 C23 -132.3(10) . . . . ?
O18 Nb3 O19 C25 -149(3) . . . . ?
C5 C4 N1 N1 -0.7(11) . . . 2_556 ?
C5 C4 C3 C2 -0.9(11) . . . . ?
C6 C8 O13 Nb4 175.1(5) . . . . ?
C6 C7 C2 C3 -0.4(11) . . . . ?
C6 C7 C2 C1 179.7(6) . . . . ?
O17 Nb3 O20 C23 72.5(15) . . . . ?
O17 Nb3 O18 C27 -106.2(11) . . . . ?
O17 Nb3 O19 C25 -53(3) . . . . ?
O17 Nb4 O14 C35B -74(2) . . . . ?
O17 Nb4 O14 C35A 2(3) . . . . ?
O17 Nb4 O16 C31 -9.2(12) . . . . ?
C3 C4 N1 N1 179.1(7) . . . 2_556 ?
C3 C4 C5 C6 1.6(10) . . . . ?
C3 C2 C1 O3 5.5(10) . . . . ?
C3 C2 C1 O2 -176.9(6) . . . . ?
C2 C7 C6 C8 -177.7(7) . . . . ?
C2 C7 C6 C5 1.1(11) . . . . ?
C16 C15 O7 Nb1 -58.9(9) . . . . ?
C16 C15 O7 Nb2 108.0(7) . . . . ?
O4 Nb1 O6 C13B -3.1(18) . . . . ?
O4 Nb1 O6 C13A 64(7) . . . . ?
O10 Nb2 O8 C17 105.4(8) . . . . ?
O10 Nb2 O9 C19 -106.8(9) . . . . ?
O11 Nb3 O20 C23 131.5(10) . . . . ?
O11 Nb3 O18 C27 179.4(11) . . . . ?
O11 Nb3 O19 C25 -26(3) . . . . ?
O11 Nb4 O14 C35B -116(2) . . . . ?
O11 Nb4 O14 C35A -40(3) . . . . ?
O11 Nb4 O16 C31 64.9(12) . . . . ?
O19 Nb3 O20 C23 -34.7(10) . . . . ?
O19 Nb3 O18 C27 -17.8(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_gar217monop
_database_code_depnum_ccdc_archive 'CCDC 2179579'
loop_
_audit_author_name
_audit_author_address
'Sylvain Duval'
;University of Lille
France
;
_audit_update_record             
;
2022-06-16 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_audit_creation_date             2021-01-15
_audit_creation_method           
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H78 N2 Nb4 O20'
_chemical_formula_sum            'C42 H78 N2 Nb4 O20'
_chemical_formula_weight         1302.70
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'

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

_cell_length_a                   15.3902(12)
_cell_length_b                   20.0542(14)
_cell_length_c                   17.5280(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.114(3)
_cell_angle_gamma                90
_cell_volume                     5409.8(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.899
_shelx_estimated_absorpt_T_min   0.813
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1030 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.9382.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.121
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         1.323
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10247
_reflns_number_total             11078
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11078
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0313
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+6.2184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0764
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.6793(6)
 0.3207(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C27A-C26A
 1.45 with sigma of 0.02
 C26B-C27B
 1.45 with sigma of 0.02
 C32-C33
 1.5 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C14B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
Uanis(C27A) = Uanis(C26A) = Uanis(C26B) = Uanis(C27B)
5. Others
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(1)
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(1)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C14B)=Sof(H14C)=Sof(H14D)=1-FVAR(2)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C38(H38A,H38B), C30(H30A,H30B), C22(H22A,H22B), C40(H40A,
 H40B), C24(H24A,H24B), C32(H32A,H32B), C20(H20A,H20B), C16(H16A,H16B),
 C14A(H14A,H14B), C34(H34A,H34B), C28(H28A,H28B), C36(H36A,H36B), C14B(H14C,
 H14D), C26B(H26A,H26B), C26A(H26C,H26D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C11(H11), C4(H4), C13(H13), C9(H9), C10(H10)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C21(H21A,
 H21B,H21C), C17(H17A,H17B,H17C), C15A(H15A,H15B,H15C), C35(H35A,H35B,H35C),
 C37(H37A,H37B,H37C), C29(H29A,H29B,H29C), C15B(H15D,H15E,H15F), C27A(H27A,H27B,
 H27C), C27B(H27D,H27E,H27F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.07929(2) 0.76867(2) 0.11747(2) 0.01693(8) Uani 1 1 d . . . . .
Nb3 Nb 0.43302(2) 1.24378(2) 0.87977(2) 0.01437(7) Uani 1 1 d . . . . .
Nb2 Nb 0.08795(2) 0.64140(2) 0.22946(2) 0.01750(8) Uani 1 1 d . . . . .
Nb4 Nb 0.38561(2) 1.36722(2) 0.76781(2) 0.02104(8) Uani 1 1 d . . . . .
O5 O 0.00464(16) 0.72215(12) 0.20348(13) 0.0168(5) Uani 1 1 d . . . . .
O1 O 0.15045(16) 0.80680(11) 0.21644(12) 0.0172(5) Uani 1 1 d . . . . .
O11 O 0.37135(16) 1.19536(11) 0.78160(12) 0.0173(5) Uani 1 1 d . . . . .
O7 O 0.15077(16) 0.72111(11) 0.29873(13) 0.0154(5) Uani 1 1 d . . . . .
O17 O 0.34446(16) 1.27928(11) 0.70061(13) 0.0162(5) Uani 1 1 d . . . . .
O16 O 0.49130(16) 1.30315(13) 0.79413(13) 0.0198(5) Uani 1 1 d . . . . .
O4 O 0.01067(18) 0.73413(12) 0.03909(14) 0.0225(6) Uani 1 1 d . . . . .
O6 O 0.13916(16) 0.68751(12) 0.14470(13) 0.0197(5) Uani 1 1 d . . . . .
O14 O 0.49263(17) 1.28389(12) 0.96045(13) 0.0201(5) Uani 1 1 d . . . . .
O15 O 0.35266(17) 1.31414(11) 0.85482(12) 0.0173(5) Uani 1 1 d . . . . .
O12 O 0.35463(18) 1.19247(12) 0.93649(13) 0.0216(5) Uani 1 1 d . . . . .
O9 O 0.0243(2) 0.57969(13) 0.17439(15) 0.0328(7) Uani 1 1 d . . . . .
O13 O 0.51736(17) 1.17724(13) 0.85817(13) 0.0237(6) Uani 1 1 d . . . . .
C1 C 0.1644(2) 0.78091(17) 0.28114(18) 0.0144(7) Uani 1 1 d . . . . .
O2 O 0.16910(18) 0.80562(14) 0.05884(14) 0.0270(6) Uani 1 1 d . . . . .
C2 C 0.1970(2) 0.82782(17) 0.34148(19) 0.0133(7) Uani 1 1 d . . . . .
C3 C 0.2249(2) 0.89137(17) 0.32009(19) 0.0167(7) Uani 1 1 d . . . . .
H3 H 0.228188 0.902609 0.267524 0.020 Uiso 1 1 calc R U . . .
O3 O 0.01440(17) 0.84776(12) 0.13511(13) 0.0226(6) Uani 1 1 d . . . . .
O8 O 0.18485(18) 0.58934(13) 0.25470(16) 0.0303(7) Uani 1 1 d . . . . .
O20 O 0.4274(2) 1.43970(12) 0.82334(14) 0.0349(7) Uani 1 1 d . . . . .
O19 O 0.4401(2) 1.38755(12) 0.67454(14) 0.0294(7) Uani 1 1 d . . . . .
O18 O 0.27445(19) 1.40016(13) 0.74393(15) 0.0308(7) Uani 1 1 d . . . . .
C5 C 0.2421(2) 0.92069(17) 0.45168(18) 0.0154(7) Uani 1 1 d . . . . .
N1 N 0.26026(19) 0.96643(14) 0.51227(15) 0.0153(6) Uani 1 1 d . . . . .
O10 O 0.02679(18) 0.63017(12) 0.32218(14) 0.0229(6) Uani 1 1 d . . . . .
C6 C 0.2184(2) 0.85667(17) 0.47304(19) 0.0173(7) Uani 1 1 d . . . . .
H6 H 0.217880 0.844534 0.525433 0.021 Uiso 1 1 calc R U . . .
C7 C 0.1955(2) 0.81033(18) 0.4177(2) 0.0166(7) Uani 1 1 d . . . . .
H7 H 0.178717 0.766557 0.432277 0.020 Uiso 1 1 calc R U . . .
C43 C 0.3453(2) 1.21848(16) 0.71855(18) 0.0132(7) Uani 1 1 d . . . . .
C11 C 0.3135(2) 1.18532(17) 0.58372(19) 0.0158(7) Uani 1 1 d . . . . .
H11 H 0.325870 1.229682 0.568156 0.019 Uiso 1 1 calc R U . . .
C4 C 0.2478(2) 0.93806(17) 0.37437(19) 0.0166(7) Uani 1 1 d . . . . .
H4 H 0.267092 0.981165 0.359621 0.020 Uiso 1 1 calc R U . . .
N2 N 0.25581(19) 1.02651(14) 0.49249(16) 0.0176(6) Uani 1 1 d . . . . .
C13 C 0.2939(2) 1.10423(17) 0.68318(18) 0.0147(7) Uani 1 1 d . . . . .
H13 H 0.294565 1.093076 0.735849 0.018 Uiso 1 1 calc R U . . .
C9 C 0.2710(2) 1.05622(17) 0.63004(19) 0.0164(7) Uani 1 1 d . . . . .
H9 H 0.254224 1.012814 0.645928 0.020 Uiso 1 1 calc R U . . .
C12 C 0.3158(2) 1.16861(17) 0.66059(19) 0.0150(7) Uani 1 1 d . . . . .
C8 C 0.2731(2) 1.07276(17) 0.55263(19) 0.0153(7) Uani 1 1 d . . . . .
C19 C -0.0600(2) 0.69398(19) -0.07418(19) 0.0227(8) Uani 1 1 d . . . . .
H19A H -0.008186 0.704097 -0.104415 0.034 Uiso 1 1 calc R U . . .
H19B H -0.099421 0.732367 -0.075032 0.034 Uiso 1 1 calc R U . . .
H19C H -0.089598 0.655039 -0.095852 0.034 Uiso 1 1 calc R U . . .
C18 C -0.0336(3) 0.67921(18) 0.0072(2) 0.0242(8) Uani 1 1 d . . . . .
H18A H -0.085998 0.669303 0.037905 0.029 Uiso 1 1 calc R U . . .
H18B H 0.004494 0.639460 0.008332 0.029 Uiso 1 1 calc R U . . .
C23 C 0.0063(3) 0.4764(2) 0.1102(3) 0.0388(11) Uani 1 1 d . . . . .
H23A H 0.037726 0.492735 0.065338 0.058 Uiso 1 1 calc R U . . .
H23B H -0.037106 0.443439 0.094151 0.058 Uiso 1 1 calc R U . . .
H23C H 0.047368 0.455563 0.145702 0.058 Uiso 1 1 calc R U . . .
C38 C 0.4568(4) 1.3671(2) 0.5987(2) 0.0402(12) Uani 1 1 d . . . . .
H38A H 0.403919 1.346062 0.577334 0.048 Uiso 1 1 calc R U . . .
H38B H 0.503567 1.333128 0.599031 0.048 Uiso 1 1 calc R U . . .
C30 C 0.5453(3) 1.1294(2) 0.8042(2) 0.0360(11) Uani 1 1 d . . . . .
H30A H 0.608819 1.133366 0.796665 0.043 Uiso 1 1 calc R U . . .
H30B H 0.516419 1.137764 0.754580 0.043 Uiso 1 1 calc R U . . .
C39 C 0.4826(4) 1.4222(3) 0.5502(2) 0.0529(15) Uani 1 1 d . . . . .
H39A H 0.489850 1.406254 0.497744 0.079 Uiso 1 1 calc R U . . .
H39B H 0.537673 1.440750 0.568645 0.079 Uiso 1 1 calc R U . . .
H39C H 0.437678 1.456802 0.551438 0.079 Uiso 1 1 calc R U . . .
C22 C -0.0383(3) 0.53370(19) 0.1489(2) 0.0262(9) Uani 1 1 d . . . . .
H22A H -0.078664 0.555727 0.112785 0.031 Uiso 1 1 calc R U . . .
H22B H -0.072531 0.517129 0.192788 0.031 Uiso 1 1 calc R U . . .
C40 C 0.2081(3) 1.4011(2) 0.6882(2) 0.0311(10) Uani 1 1 d . . . . .
H40A H 0.150633 1.402733 0.713391 0.037 Uiso 1 1 calc R U . . .
H40B H 0.210856 1.359857 0.657199 0.037 Uiso 1 1 calc R U . . .
C41 C 0.2189(3) 1.4608(2) 0.6375(3) 0.0396(11) Uani 1 1 d . . . . .
H41A H 0.219971 1.501354 0.668759 0.059 Uiso 1 1 calc R U . . .
H41B H 0.170201 1.463120 0.601495 0.059 Uiso 1 1 calc R U . . .
H41C H 0.273525 1.457038 0.609237 0.059 Uiso 1 1 calc R U . . .
C24 C 0.0128(3) 0.6508(2) 0.3980(2) 0.0325(10) Uani 1 1 d . . . . .
H24A H -0.045139 0.672014 0.401747 0.039 Uiso 1 1 calc R U . . .
H24B H 0.056935 0.684506 0.412048 0.039 Uiso 1 1 calc R U . . .
C25 C 0.0174(4) 0.5945(3) 0.4525(2) 0.0528(15) Uani 1 1 d . . . . .
H25A H -0.028267 0.562089 0.440509 0.079 Uiso 1 1 calc R U . . .
H25B H 0.009334 0.611202 0.504516 0.079 Uiso 1 1 calc R U . . .
H25C H 0.074377 0.572887 0.448481 0.079 Uiso 1 1 calc R U . . .
C32 C 0.5605(4) 1.3142(3) 0.9980(2) 0.072(2) Uani 1 1 d D . . . .
H32A H 0.577942 1.353961 0.968285 0.087 Uiso 1 1 calc R U . . .
H32B H 0.610409 1.283049 0.998107 0.087 Uiso 1 1 calc R U . . .
C33 C 0.5443(3) 1.3350(3) 1.0766(2) 0.0474(13) Uani 1 1 d D . . . .
H33A H 0.517986 1.298065 1.104918 0.071 Uiso 1 1 calc R U . . .
H33B H 0.504640 1.373266 1.076682 0.071 Uiso 1 1 calc R U . . .
H33C H 0.599288 1.347675 1.100772 0.071 Uiso 1 1 calc R U . . .
C31 C 0.5239(5) 1.0608(2) 0.8310(3) 0.0606(17) Uani 1 1 d . . . . .
H31A H 0.552827 1.052531 0.879976 0.091 Uiso 1 1 calc R U . . .
H31B H 0.544028 1.028203 0.793349 0.091 Uiso 1 1 calc R U . . .
H31C H 0.460924 1.056679 0.837365 0.091 Uiso 1 1 calc R U . . .
C20 C -0.0752(2) 0.74306(19) 0.2365(2) 0.0246(8) Uani 1 1 d . . . . .
H20A H -0.070947 0.790536 0.251544 0.030 Uiso 1 1 calc R U . . .
H20B H -0.086912 0.716489 0.282975 0.030 Uiso 1 1 calc R U . . .
C10 C 0.2930(2) 1.13704(17) 0.52938(19) 0.0175(7) Uani 1 1 d . . . . .
H10 H 0.292639 1.148132 0.476692 0.021 Uiso 1 1 calc R U . . .
C16 C 0.0035(3) 0.90316(19) 0.1841(2) 0.0299(9) Uani 1 1 d . . . . .
H16A H 0.042172 0.939763 0.167388 0.036 Uiso 1 1 calc R U . . .
H16B H 0.020505 0.890425 0.236620 0.036 Uiso 1 1 calc R U . . .
C21 C -0.1487(3) 0.7343(3) 0.1806(3) 0.0419(12) Uani 1 1 d . . . . .
H21A H -0.136600 0.760069 0.134323 0.063 Uiso 1 1 calc R U . . .
H21B H -0.202910 0.750081 0.203601 0.063 Uiso 1 1 calc R U . . .
H21C H -0.154432 0.686987 0.167449 0.063 Uiso 1 1 calc R U . . .
C17 C -0.0885(3) 0.9273(2) 0.1843(2) 0.0348(10) Uani 1 1 d . . . . .
H17A H -0.106049 0.938759 0.132118 0.052 Uiso 1 1 calc R U . . .
H17B H -0.093166 0.966825 0.216857 0.052 Uiso 1 1 calc R U . . .
H17C H -0.126519 0.892083 0.203922 0.052 Uiso 1 1 calc R U . . .
C14A C 0.2510(9) 0.8390(8) 0.0471(10) 0.040(4) Uani 0.599(13) 1 d . . P A 3
H14A H 0.268524 0.835408 -0.006998 0.049 Uiso 0.599(13) 1 calc R U P A 3
H14B H 0.296610 0.818155 0.079042 0.049 Uiso 0.599(13) 1 calc R U P A 3
C15A C 0.2403(7) 0.9108(5) 0.0687(5) 0.060(3) Uani 0.599(13) 1 d . . P A 3
H15A H 0.196980 0.931617 0.035234 0.090 Uiso 0.599(13) 1 calc R U P A 3
H15B H 0.296036 0.933932 0.063055 0.090 Uiso 0.599(13) 1 calc R U P A 3
H15C H 0.220948 0.913888 0.121773 0.090 Uiso 0.599(13) 1 calc R U P A 3
C34 C 0.5721(3) 1.2941(2) 0.7554(2) 0.0309(9) Uani 1 1 d . . . . .
H34A H 0.577709 1.328159 0.714772 0.037 Uiso 1 1 calc R U . . .
H34B H 0.572945 1.249626 0.730975 0.037 Uiso 1 1 calc R U . . .
C28 C 0.2917(3) 1.1413(2) 0.9321(2) 0.0296(10) Uani 1 1 d . . . . .
H28A H 0.320229 1.097460 0.939289 0.036 Uiso 1 1 calc R U . . .
H28B H 0.264241 1.141678 0.881001 0.036 Uiso 1 1 calc R U . . .
C36 C 0.4508(3) 1.4658(2) 0.8938(2) 0.0392(11) Uani 1 1 d . . . . .
H36A H 0.443495 1.431476 0.933909 0.047 Uiso 1 1 calc R U . . .
H36B H 0.412991 1.504149 0.906443 0.047 Uiso 1 1 calc R U . . .
C35 C 0.6479(3) 1.3000(3) 0.8100(3) 0.0409(11) Uani 1 1 d . . . . .
H35A H 0.643619 1.265233 0.849060 0.061 Uiso 1 1 calc R U . . .
H35B H 0.646906 1.343959 0.834415 0.061 Uiso 1 1 calc R U . . .
H35C H 0.702441 1.294657 0.781820 0.061 Uiso 1 1 calc R U . . .
C37 C 0.5447(3) 1.4881(3) 0.8909(3) 0.0472(13) Uani 1 1 d . . . . .
H37A H 0.562824 1.503619 0.941439 0.071 Uiso 1 1 calc R U . . .
H37B H 0.550606 1.524507 0.853955 0.071 Uiso 1 1 calc R U . . .
H37C H 0.581353 1.450567 0.875236 0.071 Uiso 1 1 calc R U . . .
C29 C 0.2243(4) 1.1506(3) 0.9914(3) 0.0554(15) Uani 1 1 d . . . . .
H29A H 0.251406 1.149513 1.041967 0.083 Uiso 1 1 calc R U . . .
H29B H 0.181158 1.114829 0.987467 0.083 Uiso 1 1 calc R U . . .
H29C H 0.195601 1.193791 0.983828 0.083 Uiso 1 1 calc R U . . .
C15B C 0.3048(11) 0.8367(12) 0.0160(9) 0.094(8) Uani 0.401(13) 1 d . . P A 4
H15D H 0.284427 0.817783 -0.032426 0.141 Uiso 0.401(13) 1 calc R U P A 4
H15E H 0.340663 0.803802 0.042786 0.141 Uiso 0.401(13) 1 calc R U P A 4
H15F H 0.339353 0.876766 0.005828 0.141 Uiso 0.401(13) 1 calc R U P A 4
C14B C 0.2301(13) 0.8542(14) 0.0632(14) 0.044(7) Uani 0.401(13) 1 d . U P A 4
H14C H 0.248966 0.859863 0.116843 0.052 Uiso 0.401(13) 1 calc R U P A 4
H14D H 0.205128 0.897025 0.045483 0.052 Uiso 0.401(13) 1 calc R U P A 4
C26B C 0.2587(8) 0.5848(5) 0.3090(7) 0.0536(15) Uani 0.469(6) 1 d D . P B 1
H26A H 0.313950 0.586332 0.280168 0.064 Uiso 0.469(6) 1 calc R U P B 1
H26B H 0.257385 0.623659 0.343715 0.064 Uiso 0.469(6) 1 calc R U P B 1
C26A C 0.2178(6) 0.5446(5) 0.3065(6) 0.0536(15) Uani 0.531(6) 1 d D . P B 2
H26C H 0.198723 0.498719 0.293790 0.064 Uiso 0.531(6) 1 calc R U P B 2
H26D H 0.197774 0.555495 0.358633 0.064 Uiso 0.531(6) 1 calc R U P B 2
C27A C 0.3169(6) 0.5504(5) 0.3011(6) 0.0536(15) Uani 0.531(6) 1 d D . P B 2
H27A H 0.343747 0.509742 0.321434 0.080 Uiso 0.531(6) 1 calc R U P B 2
H27B H 0.336566 0.588926 0.330831 0.080 Uiso 0.531(6) 1 calc R U P B 2
H27C H 0.333808 0.556119 0.247632 0.080 Uiso 0.531(6) 1 calc R U P B 2
C27B C 0.2558(8) 0.5229(5) 0.3545(7) 0.0536(15) Uani 0.469(6) 1 d D . P B 1
H27D H 0.314429 0.512091 0.372656 0.080 Uiso 0.469(6) 1 calc R U P B 1
H27E H 0.233986 0.486307 0.322746 0.080 Uiso 0.469(6) 1 calc R U P B 1
H27F H 0.217207 0.529236 0.398258 0.080 Uiso 0.469(6) 1 calc R U P B 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Nb2 3.2222(5) . ?
Nb1 O5 2.114(2) . ?
Nb1 O1 2.188(2) . ?
Nb1 O4 1.865(2) . ?
Nb1 O6 1.930(2) . ?
Nb1 O2 1.877(3) . ?
Nb1 O3 1.900(3) . ?
Nb3 Nb4 3.2412(5) . ?
Nb3 O11 2.191(2) . ?
Nb3 O16 2.117(2) . ?
Nb3 O14 1.866(2) . ?
Nb3 O15 1.926(2) . ?
Nb3 O12 1.873(3) . ?
Nb3 O13 1.900(3) . ?
Nb2 O5 2.115(2) . ?
Nb2 O7 2.227(2) . ?
Nb2 O6 1.920(2) . ?
Nb2 O9 1.849(2) . ?
Nb2 O8 1.873(3) . ?
Nb2 O10 1.893(3) . ?
Nb4 O17 2.212(2) . ?
Nb4 O16 2.123(3) . ?
Nb4 O15 1.929(2) . ?
Nb4 O20 1.863(2) . ?
Nb4 O19 1.884(3) . ?
Nb4 O18 1.880(3) . ?
O5 C20 1.423(4) . ?
O1 C1 1.265(4) . ?
O11 C43 1.263(4) . ?
O7 C1 1.256(4) . ?
O17 C43 1.259(4) . ?
O16 C34 1.429(5) . ?
O4 C18 1.410(4) . ?
O14 C32 1.374(5) . ?
O12 C28 1.413(5) . ?
O9 C22 1.406(4) . ?
O13 C30 1.416(4) . ?
C1 C2 1.501(4) . ?
O2 C14A 1.442(17) . ?
O2 C14B 1.36(2) . ?
C2 C3 1.396(5) . ?
C2 C7 1.382(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(5) . ?
O3 C16 1.414(4) . ?
O8 C26B 1.483(10) . ?
O8 C26A 1.373(9) . ?
O20 C36 1.389(4) . ?
O19 C38 1.415(5) . ?
O18 C40 1.412(5) . ?
C5 N1 1.430(4) . ?
C5 C6 1.387(5) . ?
C5 C4 1.402(5) . ?
N1 N2 1.256(4) . ?
O10 C24 1.409(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(5) . ?
C7 H7 0.9500 . ?
C43 C12 1.496(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.389(5) . ?
C11 C10 1.394(5) . ?
C4 H4 0.9500 . ?
N2 C8 1.429(4) . ?
C13 H13 0.9500 . ?
C13 C9 1.384(5) . ?
C13 C12 1.392(5) . ?
C9 H9 0.9500 . ?
C9 C8 1.397(5) . ?
C8 C10 1.386(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C18 1.512(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 C22 1.502(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.450(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.490(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.501(6) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.480(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.462(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.506(6) . ?
C10 H10 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.496(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C14A C15A 1.497(18) . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.513(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.482(7) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.513(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C15B C14B 1.46(3) . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?
C26B H26A 0.9900 . ?
C26B H26B 0.9900 . ?
C26B C27B 1.476(12) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C26A C27A 1.534(12) . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 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
O5 Nb1 Nb2 40.36(6) . . ?
O5 Nb1 O1 81.99(9) . . ?
O1 Nb1 Nb2 76.93(6) . . ?
O4 Nb1 Nb2 100.21(8) . . ?
O4 Nb1 O5 93.08(10) . . ?
O4 Nb1 O1 174.89(11) . . ?
O4 Nb1 O6 97.95(11) . . ?
O4 Nb1 O2 99.20(11) . . ?
O4 Nb1 O3 97.64(11) . . ?
O6 Nb1 Nb2 33.09(7) . . ?
O6 Nb1 O5 73.22(10) . . ?
O6 Nb1 O1 81.99(9) . . ?
O2 Nb1 Nb2 128.08(9) . . ?
O2 Nb1 O5 165.16(10) . . ?
O2 Nb1 O1 85.88(10) . . ?
O2 Nb1 O6 96.70(12) . . ?
O2 Nb1 O3 98.48(12) . . ?
O3 Nb1 Nb2 125.68(8) . . ?
O3 Nb1 O5 88.04(10) . . ?
O3 Nb1 O1 80.89(9) . . ?
O3 Nb1 O6 156.16(10) . . ?
O11 Nb3 Nb4 76.49(6) . . ?
O16 Nb3 Nb4 40.21(7) . . ?
O16 Nb3 O11 82.87(9) . . ?
O14 Nb3 Nb4 103.85(8) . . ?
O14 Nb3 O11 176.23(10) . . ?
O14 Nb3 O16 94.97(10) . . ?
O14 Nb3 O15 99.84(10) . . ?
O14 Nb3 O12 98.67(11) . . ?
O14 Nb3 O13 96.82(11) . . ?
O15 Nb3 Nb4 32.79(7) . . ?
O15 Nb3 O11 82.50(9) . . ?
O15 Nb3 O16 72.53(10) . . ?
O12 Nb3 Nb4 126.62(8) . . ?
O12 Nb3 O11 83.96(10) . . ?
O12 Nb3 O16 163.70(10) . . ?
O12 Nb3 O15 96.25(11) . . ?
O12 Nb3 O13 99.26(12) . . ?
O13 Nb3 Nb4 124.66(8) . . ?
O13 Nb3 O11 80.05(10) . . ?
O13 Nb3 O16 87.88(11) . . ?
O13 Nb3 O15 155.20(10) . . ?
O5 Nb2 Nb1 40.35(7) . . ?
O5 Nb2 O7 80.22(9) . . ?
O7 Nb2 Nb1 77.35(6) . . ?
O6 Nb2 Nb1 33.27(7) . . ?
O6 Nb2 O5 73.40(10) . . ?
O6 Nb2 O7 84.14(9) . . ?
O9 Nb2 Nb1 101.00(9) . . ?
O9 Nb2 O5 94.57(11) . . ?
O9 Nb2 O7 173.70(12) . . ?
O9 Nb2 O6 97.83(11) . . ?
O9 Nb2 O8 99.86(12) . . ?
O9 Nb2 O10 96.00(12) . . ?
O8 Nb2 Nb1 128.13(9) . . ?
O8 Nb2 O5 163.75(11) . . ?
O8 Nb2 O7 85.79(10) . . ?
O8 Nb2 O6 97.09(12) . . ?
O8 Nb2 O10 97.34(12) . . ?
O10 Nb2 Nb1 126.67(8) . . ?
O10 Nb2 O5 88.49(10) . . ?
O10 Nb2 O7 80.41(10) . . ?
O10 Nb2 O6 157.96(10) . . ?
O17 Nb4 Nb3 77.14(6) . . ?
O16 Nb4 Nb3 40.07(7) . . ?
O16 Nb4 O17 81.47(9) . . ?
O15 Nb4 Nb3 32.74(8) . . ?
O15 Nb4 O17 84.59(9) . . ?
O15 Nb4 O16 72.34(10) . . ?
O20 Nb4 Nb3 101.68(8) . . ?
O20 Nb4 O17 176.45(13) . . ?
O20 Nb4 O16 95.46(12) . . ?
O20 Nb4 O15 96.22(11) . . ?
O20 Nb4 O19 97.52(12) . . ?
O20 Nb4 O18 98.91(13) . . ?
O19 Nb4 Nb3 126.21(9) . . ?
O19 Nb4 O17 80.68(10) . . ?
O19 Nb4 O16 88.70(11) . . ?
O19 Nb4 O15 157.54(11) . . ?
O18 Nb4 Nb3 127.36(9) . . ?
O18 Nb4 O17 84.39(10) . . ?
O18 Nb4 O16 163.23(11) . . ?
O18 Nb4 O15 97.44(12) . . ?
O18 Nb4 O19 97.89(13) . . ?
Nb1 O5 Nb2 99.28(10) . . ?
C20 O5 Nb1 129.1(2) . . ?
C20 O5 Nb2 131.4(2) . . ?
C1 O1 Nb1 130.6(2) . . ?
C43 O11 Nb3 131.4(2) . . ?
C1 O7 Nb2 128.6(2) . . ?
C43 O17 Nb4 129.5(2) . . ?
Nb3 O16 Nb4 99.72(10) . . ?
C34 O16 Nb3 129.5(2) . . ?
C34 O16 Nb4 129.8(2) . . ?
C18 O4 Nb1 148.7(2) . . ?
Nb2 O6 Nb1 113.64(12) . . ?
C32 O14 Nb3 157.6(3) . . ?
Nb3 O15 Nb4 114.46(13) . . ?
C28 O12 Nb3 144.3(2) . . ?
C22 O9 Nb2 165.2(3) . . ?
C30 O13 Nb3 144.9(2) . . ?
O1 C1 C2 115.5(3) . . ?
O7 C1 O1 125.7(3) . . ?
O7 C1 C2 118.7(3) . . ?
C14A O2 Nb1 155.0(7) . . ?
C14B O2 Nb1 139.8(10) . . ?
C3 C2 C1 119.0(3) . . ?
C7 C2 C1 121.1(3) . . ?
C7 C2 C3 119.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
C16 O3 Nb1 144.8(2) . . ?
C26B O8 Nb2 142.6(5) . . ?
C26A O8 Nb2 144.4(5) . . ?
C36 O20 Nb4 147.9(3) . . ?
C38 O19 Nb4 146.6(3) . . ?
C40 O18 Nb4 144.6(3) . . ?
C6 C5 N1 116.4(3) . . ?
C6 C5 C4 120.5(3) . . ?
C4 C5 N1 123.1(3) . . ?
N2 N1 C5 113.6(3) . . ?
C24 O10 Nb2 148.5(2) . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C7 119.9(3) . . ?
C7 C6 H6 120.1 . . ?
C2 C7 C6 120.0(3) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
O11 C43 C12 116.4(3) . . ?
O17 C43 O11 125.2(3) . . ?
O17 C43 C12 118.4(3) . . ?
C12 C11 H11 120.0 . . ?
C12 C11 C10 120.0(3) . . ?
C10 C11 H11 120.0 . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 N2 C8 114.2(3) . . ?
C9 C13 H13 119.5 . . ?
C9 C13 C12 121.0(3) . . ?
C12 C13 H13 119.5 . . ?
C13 C9 H9 120.6 . . ?
C13 C9 C8 118.8(3) . . ?
C8 C9 H9 120.6 . . ?
C11 C12 C43 120.3(3) . . ?
C11 C12 C13 119.6(3) . . ?
C13 C12 C43 120.0(3) . . ?
C9 C8 N2 123.9(3) . . ?
C10 C8 N2 115.3(3) . . ?
C10 C8 C9 120.8(3) . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
O4 C18 C19 110.5(3) . . ?
O4 C18 H18A 109.6 . . ?
O4 C18 H18B 109.6 . . ?
C19 C18 H18A 109.6 . . ?
C19 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
O19 C38 H38A 109.1 . . ?
O19 C38 H38B 109.1 . . ?
O19 C38 C39 112.3(3) . . ?
H38A C38 H38B 107.9 . . ?
C39 C38 H38A 109.1 . . ?
C39 C38 H38B 109.1 . . ?
O13 C30 H30A 109.6 . . ?
O13 C30 H30B 109.6 . . ?
O13 C30 C31 110.3(4) . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 H30A 109.6 . . ?
C31 C30 H30B 109.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O9 C22 C23 109.4(3) . . ?
O9 C22 H22A 109.8 . . ?
O9 C22 H22B 109.8 . . ?
C23 C22 H22A 109.8 . . ?
C23 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
O18 C40 H40A 109.7 . . ?
O18 C40 H40B 109.7 . . ?
O18 C40 C41 109.8(3) . . ?
H40A C40 H40B 108.2 . . ?
C41 C40 H40A 109.7 . . ?
C41 C40 H40B 109.7 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O10 C24 H24A 109.2 . . ?
O10 C24 H24B 109.2 . . ?
O10 C24 C25 112.2(4) . . ?
H24A C24 H24B 107.9 . . ?
C25 C24 H24A 109.2 . . ?
C25 C24 H24B 109.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O14 C32 H32A 108.2 . . ?
O14 C32 H32B 108.2 . . ?
O14 C32 C33 116.5(4) . . ?
H32A C32 H32B 107.3 . . ?
C33 C32 H32A 108.2 . . ?
C33 C32 H32B 108.2 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O5 C20 H20A 109.6 . . ?
O5 C20 H20B 109.6 . . ?
O5 C20 C21 110.4(3) . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
C11 C10 H10 120.2 . . ?
C8 C10 C11 119.7(3) . . ?
C8 C10 H10 120.2 . . ?
O3 C16 H16A 109.3 . . ?
O3 C16 H16B 109.3 . . ?
O3 C16 C17 111.6(3) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C14A H14A 110.0 . . ?
O2 C14A H14B 110.0 . . ?
O2 C14A C15A 108.4(10) . . ?
H14A C14A H14B 108.4 . . ?
C15A C14A H14A 110.0 . . ?
C15A C14A H14B 110.0 . . ?
C14A C15A H15A 109.5 . . ?
C14A C15A H15B 109.5 . . ?
C14A C15A H15C 109.5 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
O16 C34 H34A 109.4 . . ?
O16 C34 H34B 109.4 . . ?
O16 C34 C35 111.1(3) . . ?
H34A C34 H34B 108.0 . . ?
C35 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
O12 C28 H28A 109.5 . . ?
O12 C28 H28B 109.5 . . ?
O12 C28 C29 110.5(3) . . ?
H28A C28 H28B 108.1 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
O20 C36 H36A 109.9 . . ?
O20 C36 H36B 109.9 . . ?
O20 C36 C37 109.1(4) . . ?
H36A C36 H36B 108.3 . . ?
C37 C36 H36A 109.9 . . ?
C37 C36 H36B 109.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C14B C15B H15D 109.5 . . ?
C14B C15B H15E 109.5 . . ?
C14B C15B H15F 109.5 . . ?
O2 C14B C15B 109.9(19) . . ?
O2 C14B H14C 109.7 . . ?
O2 C14B H14D 109.7 . . ?
C15B C14B H14C 109.7 . . ?
C15B C14B H14D 109.7 . . ?
H14C C14B H14D 108.2 . . ?
O8 C26B H26A 109.2 . . ?
O8 C26B H26B 109.2 . . ?
H26A C26B H26B 107.9 . . ?
C27B C26B O8 112.0(8) . . ?
C27B C26B H26A 109.2 . . ?
C27B C26B H26B 109.2 . . ?
O8 C26A H26C 110.5 . . ?
O8 C26A H26D 110.5 . . ?
O8 C26A C27A 106.0(8) . . ?
H26C C26A H26D 108.7 . . ?
C27A C26A H26C 110.5 . . ?
C27A C26A H26D 110.5 . . ?
C26A C27A H27A 109.5 . . ?
C26A C27A H27B 109.5 . . ?
C26A C27A H27C 109.5 . . ?
H27A C27A H27B 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
C26B C27B H27D 109.5 . . ?
C26B C27B H27E 109.5 . . ?
C26B C27B H27F 109.5 . . ?
H27D C27B H27E 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 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
Nb1 Nb2 O9 C22 -117.1(10) . . . . ?
Nb1 Nb2 O8 C26B 87.5(9) . . . . ?
Nb1 Nb2 O8 C26A 161.3(8) . . . . ?
Nb1 Nb2 O10 C24 -65.7(5) . . . . ?
Nb1 O5 C20 C21 72.0(4) . . . . ?
Nb1 O1 C1 O7 12.1(5) . . . . ?
Nb1 O1 C1 C2 -165.7(2) . . . . ?
Nb1 O4 C18 C19 -167.3(3) . . . . ?
Nb1 O2 C14A C15A -71.9(19) . . . . ?
Nb1 O2 C14B C15B 152.1(10) . . . . ?
Nb1 O3 C16 C17 -150.6(3) . . . . ?
Nb3 Nb4 O20 C36 -22.5(6) . . . . ?
Nb3 Nb4 O19 C38 65.1(6) . . . . ?
Nb3 Nb4 O18 C40 -102.0(5) . . . . ?
Nb3 O11 C43 O17 -5.4(5) . . . . ?
Nb3 O11 C43 C12 172.7(2) . . . . ?
Nb3 O16 C34 C35 -64.8(4) . . . . ?
Nb3 O14 C32 C33 177.4(5) . . . . ?
Nb3 O12 C28 C29 -149.5(4) . . . . ?
Nb3 O13 C30 C31 -106.1(5) . . . . ?
Nb2 Nb1 O4 C18 -4.3(5) . . . . ?
Nb2 Nb1 O2 C14A -65.3(15) . . . . ?
Nb2 Nb1 O2 C14B -94.1(18) . . . . ?
Nb2 Nb1 O3 C16 62.0(5) . . . . ?
Nb2 O5 C20 C21 -113.0(3) . . . . ?
Nb2 O7 C1 O1 -5.9(5) . . . . ?
Nb2 O7 C1 C2 171.8(2) . . . . ?
Nb2 O9 C22 C23 -140.2(9) . . . . ?
Nb2 O8 C26B C27B 119.1(9) . . . . ?
Nb2 O8 C26A C27A -156.1(5) . . . . ?
Nb2 O10 C24 C25 -128.1(5) . . . . ?
Nb4 Nb3 O14 C32 -74.4(9) . . . . ?
Nb4 Nb3 O12 C28 75.7(4) . . . . ?
Nb4 O17 C43 O11 -0.1(5) . . . . ?
Nb4 O17 C43 C12 -178.2(2) . . . . ?
Nb4 O16 C34 C35 128.9(3) . . . . ?
Nb4 O20 C36 C37 121.7(5) . . . . ?
Nb4 O19 C38 C39 160.2(4) . . . . ?
Nb4 O18 C40 C41 -93.6(5) . . . . ?
O5 Nb1 O4 C18 -44.3(5) . . . . ?
O5 Nb1 O2 C14A -30.6(16) . . . . ?
O5 Nb1 O2 C14B -59.4(18) . . . . ?
O5 Nb1 O3 C16 77.6(4) . . . . ?
O5 Nb2 O9 C22 -76.9(10) . . . . ?
O5 Nb2 O8 C26B 47.8(10) . . . . ?
O5 Nb2 O8 C26A 121.5(8) . . . . ?
O5 Nb2 O10 C24 -79.7(5) . . . . ?
O1 Nb1 O2 C14A 4.5(15) . . . . ?
O1 Nb1 O2 C14B -24.3(18) . . . . ?
O1 Nb1 O3 C16 -4.6(4) . . . . ?
O1 C1 C2 C3 -11.8(5) . . . . ?
O1 C1 C2 C7 164.7(3) . . . . ?
O11 Nb3 O12 C28 7.5(4) . . . . ?
O11 C43 C12 C11 -158.7(3) . . . . ?
O11 C43 C12 C13 18.6(5) . . . . ?
O7 Nb2 O8 C26B 17.2(9) . . . . ?
O7 Nb2 O8 C26A 91.0(8) . . . . ?
O7 Nb2 O10 C24 0.6(5) . . . . ?
O7 C1 C2 C3 170.2(3) . . . . ?
O7 C1 C2 C7 -13.2(5) . . . . ?
O17 Nb4 O19 C38 -1.3(5) . . . . ?
O17 Nb4 O18 C40 -32.9(5) . . . . ?
O17 C43 C12 C11 19.6(5) . . . . ?
O17 C43 C12 C13 -163.1(3) . . . . ?
O16 Nb3 O14 C32 -34.6(9) . . . . ?
O16 Nb3 O12 C28 43.7(7) . . . . ?
O16 Nb4 O20 C36 -62.6(6) . . . . ?
O16 Nb4 O19 C38 80.2(5) . . . . ?
O16 Nb4 O18 C40 -65.5(7) . . . . ?
O4 Nb1 O2 C14A -176.1(15) . . . . ?
O4 Nb1 O2 C14B 155.1(18) . . . . ?
O4 Nb1 O3 C16 170.4(4) . . . . ?
O6 Nb1 O4 C18 29.2(5) . . . . ?
O6 Nb1 O2 C14A -76.9(15) . . . . ?
O6 Nb1 O2 C14B -105.7(18) . . . . ?
O6 Nb1 O3 C16 39.9(6) . . . . ?
O6 Nb2 O9 C22 -150.7(10) . . . . ?
O6 Nb2 O8 C26B 100.8(9) . . . . ?
O6 Nb2 O8 C26A 174.5(8) . . . . ?
O6 Nb2 O10 C24 -45.5(6) . . . . ?
O14 Nb3 O12 C28 -169.8(4) . . . . ?
O15 Nb3 O14 C32 -107.7(9) . . . . ?
O15 Nb3 O12 C28 89.2(4) . . . . ?
O15 Nb4 O20 C36 10.2(6) . . . . ?
O15 Nb4 O19 C38 48.3(7) . . . . ?
O15 Nb4 O18 C40 -116.7(5) . . . . ?
O12 Nb3 O14 C32 154.4(9) . . . . ?
O9 Nb2 O8 C26B -160.0(9) . . . . ?
O9 Nb2 O8 C26A -86.2(8) . . . . ?
O9 Nb2 O10 C24 -174.2(5) . . . . ?
O13 Nb3 O14 C32 53.9(9) . . . . ?
O13 Nb3 O12 C28 -71.4(4) . . . . ?
C1 C2 C3 C4 174.0(3) . . . . ?
C1 C2 C7 C6 -174.0(3) . . . . ?
O2 Nb1 O4 C18 127.4(5) . . . . ?
O2 Nb1 O3 C16 -89.0(4) . . . . ?
C2 C3 C4 C5 -0.4(5) . . . . ?
C3 C2 C7 C6 2.5(6) . . . . ?
O3 Nb1 O4 C18 -132.7(5) . . . . ?
O3 Nb1 O2 C14A 84.7(15) . . . . ?
O3 Nb1 O2 C14B 55.9(18) . . . . ?
O8 Nb2 O9 C22 110.6(10) . . . . ?
O8 Nb2 O10 C24 85.0(5) . . . . ?
O20 Nb4 O19 C38 175.6(5) . . . . ?
O20 Nb4 O18 C40 145.8(5) . . . . ?
O19 Nb4 O20 C36 -152.0(6) . . . . ?
O19 Nb4 O18 C40 46.9(5) . . . . ?
O18 Nb4 O20 C36 108.8(6) . . . . ?
O18 Nb4 O19 C38 -84.3(5) . . . . ?
C5 N1 N2 C8 179.6(3) . . . . ?
C5 C6 C7 C2 0.6(6) . . . . ?
N1 C5 C6 C7 176.7(3) . . . . ?
N1 C5 C4 C3 -176.9(3) . . . . ?
N1 N2 C8 C9 -17.4(5) . . . . ?
N1 N2 C8 C10 162.5(3) . . . . ?
O10 Nb2 O9 C22 12.1(10) . . . . ?
O10 Nb2 O8 C26B -62.5(9) . . . . ?
O10 Nb2 O8 C26A 11.2(8) . . . . ?
C6 C5 N1 N2 -159.9(3) . . . . ?
C6 C5 C4 C3 3.4(5) . . . . ?
C7 C2 C3 C4 -2.6(5) . . . . ?
C4 C5 N1 N2 20.3(5) . . . . ?
C4 C5 C6 C7 -3.6(5) . . . . ?
N2 C8 C10 C11 -178.1(3) . . . . ?
C13 C9 C8 N2 176.3(3) . . . . ?
C13 C9 C8 C10 -3.6(5) . . . . ?
C9 C13 C12 C43 -176.4(3) . . . . ?
C9 C13 C12 C11 1.0(5) . . . . ?
C9 C8 C10 C11 1.8(5) . . . . ?
C12 C11 C10 C8 1.4(6) . . . . ?
C12 C13 C9 C8 2.1(5) . . . . ?
C10 C11 C12 C43 174.6(3) . . . . ?
C10 C11 C12 C13 -2.8(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6793(6)
2 0.3207(6)

