#------------------------------------------------------------------------------
#$Date: 2022-08-03 01:36:50 +0300 (Wed, 03 Aug 2022) $
#$Revision: 277046 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/52/7245241.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7245241
loop_
_publ_author_name
'Andriotou, Despoina'
'Duval, Sylvain'
'Trivelli, Xavier'
'Volkringer, Christophe'
'Loiseau, Thierry'
_publ_section_title
;
 Molecular niobium(V) complexes with mononuclear {Nb1} and dinuclear oxo
 species {Nb2O} connected through aryl di- or tetra-carboxylate linker
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00828A
_journal_year                    2022
_chemical_formula_moiety         'C58 H122 Nb6 O34'
_chemical_formula_sum            'C58 H122 Nb6 O34'
_chemical_formula_weight         1921.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-22
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2022-06-16 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.312(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0297(14)
_cell_length_b                   18.1938(11)
_cell_length_c                   19.0238(11)
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    106.73
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.67
_cell_volume                     8249.4(8)
_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)'
_diffrn_ambient_temperature      106.73
_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_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_standards_number         0
_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_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.547
_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
_refine_diff_density_max         2.278
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.124
_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_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0580
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6659
_reflns_number_total             8239
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00828a2.cif
_cod_data_source_block           da770
_cod_database_code               7245241
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.520
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
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
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'
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_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_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) . . . . ?
