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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_158
_database_code_depnum_ccdc_archive 'CCDC 1581634'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;
#complex 1 (H2bpy)(Hbpy)[NbO(C2O4)3]*2H2O
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H23 N4 Nb O15'
_chemical_formula_weight         724.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   31.5658(12)
_cell_length_b                   8.1180(3)
_cell_length_c                   10.7876(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2764.34(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    4611
_cell_measurement_theta_min      3.6680
_cell_measurement_theta_max      29.2960

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_F_000             1472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            9681
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.396
_diffrn_reflns_theta_max         29.449
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.674
_diffrn_reflns_point_group_measured_fraction_full 0.827
_reflns_number_total             5158
_reflns_number_gt                4689
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         0.486
_reflns_Friedel_fraction_max     0.464
_reflns_Friedel_fraction_full    0.638

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0284P)²+0.2467P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1469 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5158
_refine_ls_number_parameters     484
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.46409(14) -0.0132(6) 0.5538(4) 0.0310(11) Uani 1 1 d . . . . .
H8 H 0.4815(13) 0.003(6) 0.493(5) 0.037 Uiso 1 1 d . U . . .
C2 C 0.44893(12) 0.0379(5) 0.7613(4) 0.0206(8) Uani 1 1 d . . . . .
H7 H 0.4557(12) 0.072(5) 0.839(4) 0.025 Uiso 1 1 d . U . . .
C3 C 0.40963(12) -0.0342(5) 0.7494(4) 0.0173(8) Uani 1 1 d . . . . .
H5 H 0.3949(13) -0.047(5) 0.813(4) 0.021 Uiso 1 1 d . U . . .
C4 C 0.42540(13) -0.0864(5) 0.5364(4) 0.0253(9) Uani 1 1 d . . . . .
H6 H 0.4185(14) -0.123(5) 0.471(5) 0.030 Uiso 1 1 d . U . . .
C5 C 0.39690(10) -0.0941(4) 0.6341(4) 0.0160(9) Uani 1 1 d . . . . .
C6 C 0.35364(9) -0.1643(4) 0.6152(5) 0.0151(6) Uani 1 1 d . . . . .
C7 C 0.32118(12) -0.1325(5) 0.7004(4) 0.0186(8) Uani 1 1 d . . . . .
H4 H 0.3267(12) -0.066(5) 0.771(4) 0.022 Uiso 1 1 d . U . . .
C8 C 0.34427(12) -0.2619(5) 0.5120(4) 0.0183(8) Uani 1 1 d . . . . .
H3 H 0.3646(13) -0.287(5) 0.455(4) 0.022 Uiso 1 1 d . U . . .
C9 C 0.30413(12) -0.3238(5) 0.4977(3) 0.0188(8) Uani 1 1 d . . . . .
H2 H 0.2981(13) -0.399(5) 0.433(4) 0.023 Uiso 1 1 d . U . . .
C10 C 0.28135(11) -0.1967(5) 0.6809(4) 0.0189(8) Uani 1 1 d . . . . .
H1 H 0.2580(13) -0.174(5) 0.734(4) 0.023 Uiso 1 1 d . U . . .
C11 C 0.82976(14) 0.2645(5) 0.4989(5) 0.0284(10) Uani 1 1 d . . . . .
H14 H 0.8041(15) 0.289(5) 0.525(5) 0.034 Uiso 1 1 d . U . . .
C12 C 0.87693(16) 0.3030(6) 0.3344(4) 0.0341(11) Uani 1 1 d . . . . .
H15 H 0.8815(14) 0.355(6) 0.258(5) 0.041 Uiso 1 1 d . U . . .
C13 C 0.90785(15) 0.2141(5) 0.3937(4) 0.0302(10) Uani 1 1 d . . . . .
H16 H 0.9359(14) 0.197(6) 0.346(4) 0.036 Uiso 1 1 d . U . . .
C14 C 0.85956(14) 0.1762(6) 0.5629(5) 0.0267(9) Uani 1 1 d . . . . .
H13 H 0.8533(14) 0.157(6) 0.638(5) 0.032 Uiso 1 1 d . U . . .
C15 C 0.89969(12) 0.1487(5) 0.5114(4) 0.0209(8) Uani 1 1 d . . . . .
C16 C 0.93233(12) 0.0541(5) 0.5807(3) 0.0184(8) Uani 1 1 d . . . . .
C17 C 0.96832(13) -0.0070(6) 0.5238(4) 0.0307(10) Uani 1 1 d . . . . .
H11 H 0.9740(14) 0.001(6) 0.442(4) 0.037 Uiso 1 1 d . U . . .
C18 C 0.99817(13) -0.0906(6) 0.5922(5) 0.0371(12) Uani 1 1 d . . . . .
H10 H 1.0262(15) -0.133(6) 0.553(4) 0.045 Uiso 1 1 d . U . . .
C19 C 0.95910(14) -0.0671(6) 0.7669(4) 0.0319(10) Uani 1 1 d . . . . .
H9 H 0.9587(14) -0.101(5) 0.846(5) 0.038 Uiso 1 1 d . U . . .
C20 C 0.92840(13) 0.0216(6) 0.7068(4) 0.0279(10) Uani 1 1 d . . . . .
H12 H 0.9053(14) 0.053(6) 0.760(4) 0.033 Uiso 1 1 d . U . . .
C21 C 0.65265(11) 0.6954(5) 0.4428(3) 0.0161(8) Uani 1 1 d . . . . .
C22 C 0.61440(11) 0.7176(4) 0.5284(3) 0.0168(7) Uani 1 1 d . . . . .
C23 C 0.71058(11) 0.1355(4) 0.5090(3) 0.0163(8) Uani 1 1 d . . . . .
C24 C 0.68712(9) 0.0500(4) 0.6163(4) 0.0149(6) Uani 1 1 d . . . . .
C25 C 0.57281(12) 0.2628(5) 0.6980(3) 0.0163(8) Uani 1 1 d . . . . .
C26 C 0.57189(12) 0.2345(5) 0.5556(4) 0.0151(8) Uani 1 1 d . . . . .
N1 N 0.47467(10) 0.0482(4) 0.6641(3) 0.0231(8) Uani 1 1 d . . . . .
H21 H 0.5014(13) 0.105(5) 0.673(4) 0.028 Uiso 1 1 d . U . . .
N2 N 0.27406(9) -0.2909(4) 0.5821(3) 0.0176(7) Uani 1 1 d . . . . .
H22 H 0.2477(12) -0.346(5) 0.571(3) 0.021 Uiso 1 1 d . U . . .
N3 N 0.83904(13) 0.3252(5) 0.3870(4) 0.0297(10) Uani 1 1 d . . . . .
H23 H 0.8154(15) 0.369(6) 0.347(5) 0.036 Uiso 1 1 d . U . . .
N4 N 0.99468(11) -0.1226(4) 0.7137(4) 0.0301(8) Uani 1 1 d . . . . .
O1 O 0.68767(8) 0.4739(3) 0.7275(2) 0.0183(6) Uani 1 1 d . . . . .
O2 O 0.67319(8) 0.5609(3) 0.4673(2) 0.0191(6) Uani 1 1 d . . . . .
O3 O 0.66136(9) 0.7923(4) 0.3605(3) 0.0228(7) Uani 1 1 d . . . . .
O4 O 0.59047(8) 0.8349(3) 0.5189(3) 0.0284(7) Uani 1 1 d . . . . .
O5 O 0.61123(6) 0.6000(3) 0.6092(3) 0.0176(4) Uani 1 1 d . . . . .
O6 O 0.60499(8) 0.3419(3) 0.7396(2) 0.0141(6) Uani 1 1 d . . . . .
O7 O 0.60574(8) 0.2813(3) 0.4997(2) 0.0160(6) Uani 1 1 d . . . . .
O8 O 0.54001(8) 0.1768(3) 0.5090(3) 0.0216(6) Uani 1 1 d . . . . .
O9 O 0.54366(9) 0.2063(4) 0.7622(2) 0.0263(7) Uani 1 1 d . . . . .
O10 O 0.66273(7) 0.1475(3) 0.6767(2) 0.0177(5) Uani 1 1 d . . . . .
O11 O 0.69983(7) 0.2886(3) 0.4967(2) 0.0164(5) Uani 1 1 d . . . . .
O12 O 0.73605(8) 0.0615(3) 0.4457(2) 0.0202(6) Uani 1 1 d . . . . .
O13 O 0.69301(7) -0.0971(3) 0.6380(2) 0.0182(6) Uani 1 1 d . . . . .
O1W O 0.76360(9) 0.4874(4) 0.3796(3) 0.0323(8) Uani 1 1 d . . . . .
H19 H 0.7415(16) 0.460(6) 0.399(5) 0.039 Uiso 1 1 d . U . . .
H20 H 0.7510(15) 0.567(6) 0.325(5) 0.039 Uiso 1 1 d . U . . .
O2W O 0.73754(10) 0.7536(4) 0.2320(3) 0.0286(7) Uani 1 1 d . . . . .
H17 H 0.7566(15) 0.827(6) 0.247(4) 0.034 Uiso 1 1 d . U . . .
H18 H 0.7227(16) 0.779(6) 0.269(5) 0.034 Uiso 1 1 d . U . . .
Nb01 Nb 0.65441(2) 0.40158(3) 0.61228(3) 0.01259(8) Uani 1 1 d . . . . .


_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
C1 N1 1.332(5) . ?
C1 C4 1.371(6) . ?
C1 H8 0.87(5) . ?
C2 N1 1.329(5) . ?
C2 C3 1.378(5) . ?
C2 H7 0.91(4) . ?
C3 C5 1.395(5) . ?
C3 H5 0.83(4) . ?
C4 C5 1.387(5) . ?
C4 H6 0.79(5) . ?
C5 C6 1.494(4) . ?
C6 C8 1.399(6) . ?
C6 C7 1.400(6) . ?
C7 C10 1.377(5) . ?
C7 H4 0.95(4) . ?
C8 C9 1.372(5) . ?
C8 H3 0.91(4) . ?
C9 N2 1.343(5) . ?
C9 H2 0.95(4) . ?
C10 N2 1.332(4) . ?
C10 H1 0.95(4) . ?
C11 N3 1.336(6) . ?
C11 C14 1.369(7) . ?
C11 H14 0.88(5) . ?
C12 N3 1.336(6) . ?
C12 C13 1.372(6) . ?
C12 H15 0.94(5) . ?
C13 C15 1.401(6) . ?
C13 H16 1.03(5) . ?
C14 C15 1.401(6) . ?
C14 H13 0.85(6) . ?
C15 C16 1.486(5) . ?
C16 C17 1.383(6) . ?
C16 C20 1.392(6) . ?
C17 C18 1.375(6) . ?
C17 H11 0.90(5) . ?
C18 N4 1.340(7) . ?
C18 H10 1.04(5) . ?
C19 N4 1.339(6) . ?
C19 C20 1.371(6) . ?
C19 H9 0.90(5) . ?
C20 H12 0.96(5) . ?
C21 O3 1.217(4) . ?
C21 O2 1.298(4) . ?
C21 C22 1.531(5) . ?
C22 O4 1.220(4) . ?
C22 O5 1.297(5) . ?
C23 O12 1.214(4) . ?
C23 O11 1.295(4) . ?
C23 C24 1.539(5) . ?
C24 O13 1.231(4) . ?
C24 O10 1.282(4) . ?
C25 O9 1.240(4) . ?
C25 O6 1.283(4) . ?
C25 C26 1.553(5) . ?
C26 O8 1.219(4) . ?
C26 O7 1.284(4) . ?
N1 H21 0.97(4) . ?
N2 H22 0.95(4) . ?
N3 H23 0.93(5) . ?
O1 Nb01 1.730(2) . ?
O2 Nb01 2.114(2) . ?
O5 Nb01 2.110(2) . ?
O6 Nb01 2.134(2) . ?
O7 Nb01 2.188(3) . ?
O10 Nb01 2.193(2) . ?
O11 Nb01 2.110(2) . ?
O1W H19 0.76(5) . ?
O1W H20 0.96(5) . ?
O2W H17 0.87(5) . ?
O2W H18 0.65(5) . ?

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
N1 C1 C4 120.5(4) . . ?
N1 C1 H8 118(3) . . ?
C4 C1 H8 122(3) . . ?
N1 C2 C3 120.3(4) . . ?
N1 C2 H7 124(3) . . ?
C3 C2 H7 115(3) . . ?
C2 C3 C5 119.4(4) . . ?
C2 C3 H5 119(3) . . ?
C5 C3 H5 122(3) . . ?
C1 C4 C5 119.5(4) . . ?
C1 C4 H6 122(3) . . ?
C5 C4 H6 119(3) . . ?
C4 C5 C3 118.4(3) . . ?
C4 C5 C6 120.4(4) . . ?
C3 C5 C6 121.2(4) . . ?
C8 C6 C7 118.2(3) . . ?
C8 C6 C5 121.2(3) . . ?
C7 C6 C5 120.6(4) . . ?
C10 C7 C6 119.9(4) . . ?
C10 C7 H4 120(2) . . ?
C6 C7 H4 120(2) . . ?
C9 C8 C6 119.5(3) . . ?
C9 C8 H3 119(3) . . ?
C6 C8 H3 121(3) . . ?
N2 C9 C8 120.3(3) . . ?
N2 C9 H2 119(2) . . ?
C8 C9 H2 120(2) . . ?
N2 C10 C7 119.8(3) . . ?
N2 C10 H1 117(2) . . ?
C7 C10 H1 123(2) . . ?
N3 C11 C14 119.8(4) . . ?
N3 C11 H14 114(3) . . ?
C14 C11 H14 126(3) . . ?
N3 C12 C13 120.6(4) . . ?
N3 C12 H15 117(3) . . ?
C13 C12 H15 123(3) . . ?
C12 C13 C15 119.4(4) . . ?
C12 C13 H16 117(3) . . ?
C15 C13 H16 124(3) . . ?
C11 C14 C15 120.3(4) . . ?
C11 C14 H13 115(3) . . ?
C15 C14 H13 124(3) . . ?
C13 C15 C14 117.7(4) . . ?
C13 C15 C16 121.6(4) . . ?
C14 C15 C16 120.7(4) . . ?
C17 C16 C20 116.0(4) . . ?
C17 C16 C15 122.1(4) . . ?
C20 C16 C15 121.8(4) . . ?
C18 C17 C16 120.1(4) . . ?
C18 C17 H11 115(3) . . ?
C16 C17 H11 125(3) . . ?
N4 C18 C17 124.3(4) . . ?
N4 C18 H10 114(3) . . ?
C17 C18 H10 122(3) . . ?
N4 C19 C20 124.5(4) . . ?
N4 C19 H9 109(3) . . ?
C20 C19 H9 127(3) . . ?
C19 C20 C16 119.9(4) . . ?
C19 C20 H12 113(3) . . ?
C16 C20 H12 127(3) . . ?
O3 C21 O2 125.4(3) . . ?
O3 C21 C22 122.8(3) . . ?
O2 C21 C22 111.7(3) . . ?
O4 C22 O5 125.7(3) . . ?
O4 C22 C21 122.0(3) . . ?
O5 C22 C21 112.3(3) . . ?
O12 C23 O11 126.2(3) . . ?
O12 C23 C24 121.3(3) . . ?
O11 C23 C24 112.6(3) . . ?
O13 C24 O10 126.4(4) . . ?
O13 C24 C23 120.5(3) . . ?
O10 C24 C23 113.1(3) . . ?
O9 C25 O6 125.3(3) . . ?
O9 C25 C26 118.9(4) . . ?
O6 C25 C26 115.8(3) . . ?
O8 C26 O7 127.3(4) . . ?
O8 C26 C25 118.7(3) . . ?
O7 C26 C25 113.9(4) . . ?
C2 N1 C1 121.8(3) . . ?
C2 N1 H21 119(3) . . ?
C1 N1 H21 119(3) . . ?
C10 N2 C9 122.3(3) . . ?
C10 N2 H22 121(2) . . ?
C9 N2 H22 116(2) . . ?
C11 N3 C12 122.0(4) . . ?
C11 N3 H23 113(3) . . ?
C12 N3 H23 125(3) . . ?
C19 N4 C18 115.0(4) . . ?
C21 O2 Nb01 121.7(2) . . ?
C22 O5 Nb01 121.5(2) . . ?
C25 O6 Nb01 117.8(2) . . ?
C26 O7 Nb01 117.1(2) . . ?
C24 O10 Nb01 119.5(2) . . ?
C23 O11 Nb01 122.3(2) . . ?
H19 O1W H20 89(4) . . ?
H17 O2W H18 100(6) . . ?
O1 Nb01 O11 99.19(11) . . ?
O1 Nb01 O5 98.29(12) . . ?
O11 Nb01 O5 139.60(11) . . ?
O1 Nb01 O2 98.85(11) . . ?
O11 Nb01 O2 68.79(9) . . ?
O5 Nb01 O2 72.70(11) . . ?
O1 Nb01 O6 93.33(10) . . ?
O11 Nb01 O6 141.11(10) . . ?
O5 Nb01 O6 73.22(10) . . ?
O2 Nb01 O6 145.08(10) . . ?
O1 Nb01 O7 167.52(11) . . ?
O11 Nb01 O7 87.42(10) . . ?
O5 Nb01 O7 83.03(10) . . ?
O2 Nb01 O7 93.40(10) . . ?
O6 Nb01 O7 75.10(9) . . ?
O1 Nb01 O10 91.07(11) . . ?
O11 Nb01 O10 72.35(9) . . ?
O5 Nb01 O10 143.18(9) . . ?
O2 Nb01 O10 140.93(9) . . ?
O6 Nb01 O10 70.73(9) . . ?
O7 Nb01 O10 80.80(10) . . ?

_refine_diff_density_max         0.503
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.066

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# 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_21_a
_database_code_depnum_ccdc_archive 'CCDC 1581635'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;
#complex 2 (phenH)3[NbO(C2O4)3]*3H2O
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H33 N6 Nb O16'
_chemical_formula_weight         970.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.5308(3)
_cell_length_b                   18.3361(4)
_cell_length_c                   18.4899(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.233(2)
_cell_angle_gamma                90
_cell_volume                     3898.65(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    6712
_cell_measurement_theta_min      3.7620
_cell_measurement_theta_max      28.5770

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_F_000             1984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.397
_shelx_estimated_absorpt_T_min   0.961
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.99247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            22656
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.496
_diffrn_reflns_theta_max         29.638
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9194
_reflns_number_gt                6880
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²+0.3648P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9194
_refine_ls_number_parameters     613
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.0838
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3751(2) 0.30197(12) 0.63691(12) 0.0172(5) Uani 1 1 d . . . . .
C2 C 0.4126(2) 0.29792(12) 0.71823(12) 0.0158(5) Uani 1 1 d . . . . .
C3 C 0.8394(2) 0.25891(13) 0.75635(13) 0.0192(5) Uani 1 1 d . . . . .
C4 C 0.8921(2) 0.25255(12) 0.68270(13) 0.0177(5) Uani 1 1 d . . . . .
C5 C 0.5933(2) 0.14992(13) 0.56595(12) 0.0161(5) Uani 1 1 d . . . . .
C6 C 0.6170(2) 0.20855(12) 0.50856(12) 0.0140(5) Uani 1 1 d . . . . .
C7 C 0.8386(3) 0.05485(16) 0.63990(13) 0.0303(7) Uani 1 1 d . . . . .
H7A H 0.774611 0.084957 0.649762 0.036 Uiso 1 1 calc R U . . .
C8 C 0.8386(3) -0.01746(16) 0.66414(14) 0.0351(7) Uani 1 1 d . . . . .
H8A H 0.775996 -0.035383 0.689726 0.042 Uiso 1 1 calc R U . . .
C9 C 0.9299(3) -0.06220(16) 0.65053(13) 0.0316(7) Uani 1 1 d . . . . .
H9A H 0.931144 -0.111457 0.666494 0.038 Uiso 1 1 calc R U . . .
C10 C 1.0212(3) -0.03435(14) 0.61282(13) 0.0259(7) Uani 1 1 d . . . . .
C11 C 1.0132(2) 0.03986(14) 0.59099(13) 0.0237(6) Uani 1 1 d . . . . .
C12 C 1.1068(2) 0.07005(13) 0.55470(13) 0.0240(6) Uani 1 1 d . . . . .
C13 C 1.1916(3) 0.17378(15) 0.50338(16) 0.0336(7) Uani 1 1 d . . . . .
H13A H 1.185906 0.223910 0.490616 0.040 Uiso 1 1 calc R U . . .
C14 C 1.2902(3) 0.13508(16) 0.48990(15) 0.0354(7) Uani 1 1 d . . . . .
H14A H 1.353131 0.158420 0.468868 0.042 Uiso 1 1 calc R U . . .
C15 C 1.2962(3) 0.06194(15) 0.50737(14) 0.0310(7) Uani 1 1 d . . . . .
H15A H 1.362596 0.034284 0.496939 0.037 Uiso 1 1 calc R U . . .
C16 C 1.2046(2) 0.02835(14) 0.54047(13) 0.0249(6) Uani 1 1 d . . . . .
C17 C 1.2080(3) -0.04725(14) 0.56153(13) 0.0275(7) Uani 1 1 d . . . . .
H17A H 1.272517 -0.076649 0.551064 0.033 Uiso 1 1 calc R U . . .
C18 C 1.1203(3) -0.07648(14) 0.59596(13) 0.0287(7) Uani 1 1 d . . . . .
H18A H 1.124196 -0.126451 0.609473 0.034 Uiso 1 1 calc R U . . .
C19 C 1.0808(2) 0.35293(14) 0.33142(13) 0.0241(6) Uani 1 1 d . . . . .
H19A H 1.088387 0.303163 0.318274 0.029 Uiso 1 1 calc R U . . .
C20 C 1.1686(2) 0.40159(14) 0.31391(13) 0.0253(6) Uani 1 1 d . . . . .
H20A H 1.233096 0.384769 0.289480 0.030 Uiso 1 1 calc R U . . .
C21 C 1.1599(2) 0.47383(14) 0.33253(12) 0.0221(6) Uani 1 1 d . . . . .
H21A H 1.218438 0.507545 0.321195 0.027 Uiso 1 1 calc R U . . .
C22 C 1.0635(2) 0.49719(13) 0.36853(11) 0.0161(5) Uani 1 1 d . . . . .
C23 C 0.9801(2) 0.44402(13) 0.38304(11) 0.0166(5) Uani 1 1 d . . . . .
C24 C 0.8820(2) 0.46576(12) 0.42084(11) 0.0144(5) Uani 1 1 d . . . . .
C25 C 0.7090(2) 0.43098(13) 0.47262(12) 0.0191(5) Uani 1 1 d . . . . .
H25A H 0.654800 0.393882 0.482303 0.023 Uiso 1 1 calc R U . . .
C26 C 0.6934(2) 0.50152(14) 0.49758(12) 0.0225(6) Uani 1 1 d . . . . .
H26A H 0.628852 0.512792 0.524650 0.027 Uiso 1 1 calc R U . . .
C27 C 0.7721(2) 0.55494(13) 0.48283(12) 0.0192(6) Uani 1 1 d . . . . .
H27A H 0.760922 0.603399 0.499117 0.023 Uiso 1 1 calc R U . . .
C28 C 0.8687(2) 0.53830(12) 0.44385(11) 0.0163(5) Uani 1 1 d . . . . .
C29 C 0.9553(2) 0.59070(13) 0.42775(13) 0.0210(6) Uani 1 1 d . . . . .
H29A H 0.947138 0.639979 0.442422 0.025 Uiso 1 1 calc R U . . .
C30 C 1.0482(2) 0.57095(13) 0.39201(12) 0.0206(6) Uani 1 1 d . . . . .
H30A H 1.104707 0.606622 0.382183 0.025 Uiso 1 1 calc R U . . .
C31 C 0.4582(2) 0.49141(14) 0.66802(13) 0.0240(6) Uani 1 1 d . . . . .
H31A H 0.506072 0.459959 0.642258 0.029 Uiso 1 1 calc R U . . .
C32 C 0.4911(2) 0.56500(14) 0.67537(13) 0.0251(6) Uani 1 1 d . . . . .
H32A H 0.558892 0.582478 0.654841 0.030 Uiso 1 1 calc R U . . .
C33 C 0.4234(2) 0.61116(14) 0.71274(13) 0.0228(6) Uani 1 1 d . . . . .
H33A H 0.444215 0.661038 0.718735 0.027 Uiso 1 1 calc R U . . .
C34 C 0.3235(2) 0.58420(13) 0.74191(12) 0.0184(6) Uani 1 1 d . . . . .
C35 C 0.2977(2) 0.50942(13) 0.73095(12) 0.0174(5) Uani 1 1 d . . . . .
C36 C 0.1959(2) 0.48047(12) 0.75979(12) 0.0165(5) Uani 1 1 d . . . . .
C37 C 0.0831(2) 0.37614(14) 0.78141(13) 0.0242(6) Uani 1 1 d . . . . .
H37A H 0.071532 0.325076 0.776003 0.029 Uiso 1 1 calc R U . . .
C38 C 0.0071(2) 0.41747(14) 0.81914(13) 0.0242(6) Uani 1 1 d . . . . .
H38A H -0.056945 0.395058 0.839861 0.029 Uiso 1 1 calc R U . . .
C39 C 0.0254(2) 0.49120(14) 0.82621(12) 0.0235(6) Uani 1 1 d . . . . .
H39A H -0.027542 0.520000 0.850999 0.028 Uiso 1 1 calc R U . . .
C40 C 0.1209(2) 0.52444(13) 0.79739(12) 0.0190(6) Uani 1 1 d . . . . .
C41 C 0.1495(2) 0.60029(13) 0.80671(13) 0.0232(6) Uani 1 1 d . . . . .
H41A H 0.099323 0.631188 0.831331 0.028 Uiso 1 1 calc R U . . .
C42 C 0.2466(3) 0.62837(13) 0.78106(12) 0.0230(6) Uani 1 1 d . . . . .
H42A H 0.264387 0.678435 0.789083 0.028 Uiso 1 1 calc R U . . .
N1 N 0.9224(2) 0.08374(12) 0.60408(11) 0.0267(5) Uani 1 1 d . . . . .
N2 N 1.1047(2) 0.14160(12) 0.53402(13) 0.0289(6) Uani 1 1 d . . . . .
H1 H 1.043(3) 0.1654(15) 0.5396(15) 0.035 Uiso 1 1 d . U . . .
N3 N 0.98848(19) 0.37220(11) 0.36505(10) 0.0210(5) Uani 1 1 d . . . . .
N4 N 0.80012(18) 0.41546(11) 0.43513(10) 0.0159(4) Uani 1 1 d . . . . .
H2 H 0.808(2) 0.3701(13) 0.4180(12) 0.019 Uiso 1 1 d . U . . .
N5 N 0.36516(19) 0.46332(11) 0.69465(10) 0.0203(5) Uani 1 1 d . . . . .
N6 N 0.1722(2) 0.40828(11) 0.75285(11) 0.0197(5) Uani 1 1 d . . . . .
H3 H 0.217(2) 0.3835(14) 0.7318(14) 0.024 Uiso 1 1 d . U . . .
O1 O 0.66765(15) 0.38251(8) 0.63817(8) 0.0185(4) Uani 1 1 d . . . . .
O2 O 0.46361(15) 0.30171(9) 0.59782(8) 0.0179(4) Uani 1 1 d . . . . .
O3 O 0.27293(16) 0.30413(10) 0.61514(9) 0.0285(4) Uani 1 1 d . . . . .
O4 O 0.34069(15) 0.29757(8) 0.76375(8) 0.0202(4) Uani 1 1 d . . . . .
O5 O 0.52308(15) 0.29408(8) 0.73147(8) 0.0172(4) Uani 1 1 d . . . . .
O6 O 0.72920(15) 0.27354(9) 0.74963(8) 0.0205(4) Uani 1 1 d . . . . .
O7 O 0.89897(16) 0.25184(10) 0.81305(9) 0.0275(4) Uani 1 1 d . . . . .
O8 O 0.99554(16) 0.24325(9) 0.67703(9) 0.0253(4) Uani 1 1 d . . . . .
O9 O 0.81268(15) 0.25975(9) 0.62929(8) 0.0177(4) Uani 1 1 d . . . . .
O10 O 0.60066(15) 0.17420(8) 0.63167(8) 0.0168(4) Uani 1 1 d . . . . .
O11 O 0.57163(16) 0.08723(8) 0.54684(8) 0.0228(4) Uani 1 1 d . . . . .
O12 O 0.61045(16) 0.19314(9) 0.44398(8) 0.0218(4) Uani 1 1 d . . . . .
O13 O 0.64437(14) 0.27209(8) 0.53479(8) 0.0148(4) Uani 1 1 d . . . . .
O1W O 0.77850(19) 0.27496(10) 0.38889(10) 0.0254(5) Uani 1 1 d . . . . .
H4 H 0.722(3) 0.2504(15) 0.4000(15) 0.030 Uiso 1 1 d . U . . .
H5 H 0.793(3) 0.2640(16) 0.3549(15) 0.030 Uiso 1 1 d . U . . .
O2W O 0.94415(18) 0.24721(10) 0.50861(10) 0.0259(4) Uani 1 1 d . . . . .
H6 H 0.904(3) 0.2506(15) 0.4721(15) 0.031 Uiso 1 1 d . U . . .
H7 H 0.902(3) 0.2517(15) 0.5424(15) 0.031 Uiso 1 1 d . U . . .
O3W O 0.8768(3) 0.17546(15) 0.94693(12) 0.0748(11) Uani 1 1 d . . . . .
H8 H 0.915(4) 0.188(2) 0.983(2) 0.090 Uiso 1 1 d . U . . .
H9 H 0.888(4) 0.199(2) 0.917(2) 0.090 Uiso 1 1 d . U . . .
Nb1 Nb 0.63862(2) 0.29121(2) 0.64786(2) 0.01248(6) Uani 1 1 d . . . . .


_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
C1 O3 1.217(3) . ?
C1 O2 1.293(3) . ?
C1 C2 1.535(3) . ?
C2 O4 1.225(3) . ?
C2 O5 1.281(3) . ?
C3 O7 1.217(3) . ?
C3 O6 1.296(3) . ?
C3 C4 1.536(4) . ?
C4 O8 1.217(3) . ?
C4 O9 1.303(3) . ?
C5 O11 1.223(3) . ?
C5 O10 1.291(3) . ?
C5 C6 1.549(3) . ?
C6 O12 1.224(3) . ?
C6 O13 1.292(3) . ?
C7 N1 1.322(4) . ?
C7 C8 1.400(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.372(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.401(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.420(4) . ?
C10 C18 1.433(4) . ?
C11 N1 1.356(3) . ?
C11 C12 1.425(4) . ?
C12 N2 1.366(3) . ?
C12 C16 1.403(4) . ?
C13 N2 1.325(4) . ?
C13 C14 1.378(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.380(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.402(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.439(4) . ?
C17 C18 1.346(4) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 N3 1.320(3) . ?
C19 C20 1.405(4) . ?
C19 H19A 0.9500 . ?
C20 C21 1.374(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.404(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.409(3) . ?
C22 C30 1.435(3) . ?
C23 N3 1.363(3) . ?
C23 C24 1.430(3) . ?
C24 N4 1.359(3) . ?
C24 C28 1.408(3) . ?
C25 N4 1.331(3) . ?
C25 C26 1.390(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.376(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.405(4) . ?
C27 H27A 0.9500 . ?
C28 C29 1.433(4) . ?
C29 C30 1.350(4) . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9500 . ?
C31 N5 1.318(3) . ?
C31 C32 1.405(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.372(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.397(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.414(3) . ?
C34 C42 1.436(4) . ?
C35 N5 1.359(3) . ?
C35 C36 1.427(4) . ?
C36 N6 1.356(3) . ?
C36 C40 1.404(3) . ?
C37 N6 1.327(4) . ?
C37 C38 1.386(4) . ?
C37 H37A 0.9500 . ?
C38 C39 1.373(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.398(4) . ?
C39 H39A 0.9500 . ?
C40 C41 1.437(3) . ?
C41 C42 1.349(4) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
N2 H1 0.85(3) . ?
N4 H2 0.90(2) . ?
N6 H3 0.81(3) . ?
O1 Nb1 1.7192(16) . ?
O2 Nb1 2.1657(16) . ?
O5 Nb1 2.1147(16) . ?
O6 Nb1 2.1086(14) . ?
O9 Nb1 2.1402(17) . ?
O10 Nb1 2.2058(15) . ?
O13 Nb1 2.1258(14) . ?
O1W H4 0.83(3) . ?
O1W H5 0.69(3) . ?
O2W H6 0.79(3) . ?
O2W H7 0.83(3) . ?
O3W H8 0.80(4) . ?
O3W H9 0.71(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
O3 C1 O2 126.9(2) . . ?
O3 C1 C2 121.4(2) . . ?
O2 C1 C2 111.7(2) . . ?
O4 C2 O5 125.6(2) . . ?
O4 C2 C1 121.1(2) . . ?
O5 C2 C1 113.2(2) . . ?
O7 C3 O6 126.3(2) . . ?
O7 C3 C4 121.4(2) . . ?
O6 C3 C4 112.34(19) . . ?
O8 C4 O9 126.0(2) . . ?
O8 C4 C3 122.8(2) . . ?
O9 C4 C3 111.2(2) . . ?
O11 C5 O10 126.4(2) . . ?
O11 C5 C6 119.8(2) . . ?
O10 C5 C6 113.74(19) . . ?
O12 C6 O13 124.7(2) . . ?
O12 C6 C5 120.4(2) . . ?
O13 C6 C5 114.80(18) . . ?
N1 C7 C8 123.9(3) . . ?
N1 C7 H7A 118.1 . . ?
C8 C7 H7A 118.1 . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8A 120.4 . . ?
C7 C8 H8A 120.4 . . ?
C8 C9 C10 119.2(3) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
C9 C10 C11 117.1(3) . . ?
C9 C10 C18 123.5(3) . . ?
C11 C10 C18 119.4(3) . . ?
N1 C11 C10 123.5(3) . . ?
N1 C11 C12 118.4(2) . . ?
C10 C11 C12 118.1(3) . . ?
N2 C12 C16 117.9(3) . . ?
N2 C12 C11 120.4(3) . . ?
C16 C12 C11 121.6(2) . . ?
N2 C13 C14 120.5(3) . . ?
N2 C13 H13A 119.8 . . ?
C14 C13 H13A 119.8 . . ?
C13 C14 C15 119.1(3) . . ?
C13 C14 H14A 120.5 . . ?
C15 C14 H14A 120.5 . . ?
C14 C15 C16 120.2(3) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
C15 C16 C12 118.9(3) . . ?
C15 C16 C17 122.3(3) . . ?
C12 C16 C17 118.7(3) . . ?
C18 C17 C16 120.3(3) . . ?
C18 C17 H17A 119.8 . . ?
C16 C17 H17A 119.8 . . ?
C17 C18 C10 121.9(3) . . ?
C17 C18 H18A 119.1 . . ?
C10 C18 H18A 119.1 . . ?
N3 C19 C20 123.9(2) . . ?
N3 C19 H19A 118.0 . . ?
C20 C19 H19A 118.0 . . ?
C21 C20 C19 119.2(3) . . ?
C21 C20 H20A 120.4 . . ?
C19 C20 H20A 120.4 . . ?
C20 C21 C22 119.2(3) . . ?
C20 C21 H21A 120.4 . . ?
C22 C21 H21A 120.4 . . ?
C21 C22 C23 117.0(2) . . ?
C21 C22 C30 123.4(2) . . ?
C23 C22 C30 119.6(2) . . ?
N3 C23 C22 124.1(2) . . ?
N3 C23 C24 117.5(2) . . ?
C22 C23 C24 118.4(2) . . ?
N4 C24 C28 119.3(2) . . ?
N4 C24 C23 119.5(2) . . ?
C28 C24 C23 121.2(2) . . ?
N4 C25 C26 119.9(2) . . ?
N4 C25 H25A 120.0 . . ?
C26 C25 H25A 120.0 . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 120.4(2) . . ?
C26 C27 H27A 119.8 . . ?
C28 C27 H27A 119.8 . . ?
C27 C28 C24 117.9(2) . . ?
C27 C28 C29 123.5(2) . . ?
C24 C28 C29 118.5(2) . . ?
C30 C29 C28 120.8(2) . . ?
C30 C29 H29A 119.6 . . ?
C28 C29 H29A 119.6 . . ?
C29 C30 C22 121.4(2) . . ?
C29 C30 H30A 119.3 . . ?
C22 C30 H30A 119.3 . . ?
N5 C31 C32 124.0(3) . . ?
N5 C31 H31A 118.0 . . ?
C32 C31 H31A 118.0 . . ?
C33 C32 C31 118.8(3) . . ?
C33 C32 H32A 120.6 . . ?
C31 C32 H32A 120.6 . . ?
C32 C33 C34 119.4(2) . . ?
C32 C33 H33A 120.3 . . ?
C34 C33 H33A 120.3 . . ?
C33 C34 C35 117.3(2) . . ?
C33 C34 C42 123.5(2) . . ?
C35 C34 C42 119.2(3) . . ?
N5 C35 C34 123.5(2) . . ?
N5 C35 C36 118.0(2) . . ?
C34 C35 C36 118.5(2) . . ?
N6 C36 C40 118.7(2) . . ?
N6 C36 C35 119.6(2) . . ?
C40 C36 C35 121.7(2) . . ?
N6 C37 C38 119.6(3) . . ?
N6 C37 H37A 120.2 . . ?
C38 C37 H37A 120.2 . . ?
C39 C38 C37 119.2(3) . . ?
C39 C38 H38A 120.4 . . ?
C37 C38 H38A 120.4 . . ?
C38 C39 C40 120.8(3) . . ?
C38 C39 H39A 119.6 . . ?
C40 C39 H39A 119.6 . . ?
C39 C40 C36 118.0(2) . . ?
C39 C40 C41 123.8(2) . . ?
C36 C40 C41 118.1(3) . . ?
C42 C41 C40 121.1(3) . . ?
C42 C41 H41A 119.5 . . ?
C40 C41 H41A 119.5 . . ?
C41 C42 C34 121.4(2) . . ?
C41 C42 H42A 119.3 . . ?
C34 C42 H42A 119.3 . . ?
C7 N1 C11 117.0(2) . . ?
C13 N2 C12 123.3(3) . . ?
C13 N2 H1 119(2) . . ?
C12 N2 H1 117(2) . . ?
C19 N3 C23 116.6(2) . . ?
C25 N4 C24 122.8(2) . . ?
C25 N4 H2 119.1(18) . . ?
C24 N4 H2 118.1(18) . . ?
C31 N5 C35 116.9(2) . . ?
C37 N6 C36 123.5(2) . . ?
C37 N6 H3 119(2) . . ?
C36 N6 H3 118(2) . . ?
C1 O2 Nb1 120.69(14) . . ?
C2 O5 Nb1 122.19(14) . . ?
C3 O6 Nb1 122.35(15) . . ?
C4 O9 Nb1 121.38(15) . . ?
C5 O10 Nb1 117.51(14) . . ?
C6 O13 Nb1 119.56(14) . . ?
H4 O1W H5 108(3) . . ?
H6 O2W H7 107(3) . . ?
H8 O3W H9 110(4) . . ?
O1 Nb1 O6 98.93(7) . . ?
O1 Nb1 O5 100.95(7) . . ?
O6 Nb1 O5 69.44(6) . . ?
O1 Nb1 O13 92.16(6) . . ?
O6 Nb1 O13 143.41(7) . . ?
O5 Nb1 O13 142.20(6) . . ?
O1 Nb1 O9 93.08(7) . . ?
O6 Nb1 O9 72.13(6) . . ?
O5 Nb1 O9 140.61(6) . . ?
O13 Nb1 O9 72.55(6) . . ?
O1 Nb1 O2 92.94(7) . . ?
O6 Nb1 O2 141.21(7) . . ?
O5 Nb1 O2 72.10(6) . . ?
O13 Nb1 O2 71.95(6) . . ?
O9 Nb1 O2 144.17(6) . . ?
O1 Nb1 O10 166.24(6) . . ?
O6 Nb1 O10 92.98(6) . . ?
O5 Nb1 O10 89.65(6) . . ?
O13 Nb1 O10 74.12(6) . . ?
O9 Nb1 O10 83.98(6) . . ?
O2 Nb1 O10 81.90(6) . . ?

_refine_diff_density_max         0.353
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.085

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_a
_database_code_depnum_ccdc_archive 'CCDC 1581636'
_audit_update_record             
;
2017-10-24 deposited with the CCDC.
2018-01-09 downloaded from the CCDC.
;
#complex 3 (HNC5H4-NH2)3[NbO(C2O4)3]*2H2O 
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H25 N6 Nb O15'
_chemical_formula_weight         694.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8603(5)
_cell_length_b                   9.5609(4)
_cell_length_c                   17.5015(8)
_cell_angle_alpha                78.475(4)
_cell_angle_beta                 81.023(4)
_cell_angle_gamma                71.048(4)
_cell_volume                     1367.29(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    5947
_cell_measurement_theta_min      3.9280
_cell_measurement_theta_max      29.2270

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.525
_shelx_estimated_absorpt_T_min   0.925
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            11640
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.265
_diffrn_reflns_theta_max         29.631
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6403
_reflns_number_gt                5574
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²+0.7983P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6403
_refine_ls_number_parameters     427
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0835
_refine_ls_wR_factor_gt          0.0800
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7452(3) 1.2596(3) 0.39525(14) 0.0198(5) Uani 1 1 d . . . . .
C2 C 0.7232(3) 1.1401(3) 0.35499(13) 0.0172(5) Uani 1 1 d . . . . .
C3 C 1.0517(3) 1.0319(3) 0.16280(14) 0.0194(5) Uani 1 1 d . . . . .
C4 C 0.9638(3) 1.2033(3) 0.14579(14) 0.0215(5) Uani 1 1 d . . . . .
C5 C 1.3552(3) 1.2426(3) 0.23454(14) 0.0191(5) Uani 1 1 d . . . . .
C6 C 1.2587(3) 1.3555(3) 0.28878(14) 0.0181(5) Uani 1 1 d . . . . .
C7 C 0.2676(3) 1.3938(3) 0.52485(13) 0.0194(5) Uani 1 1 d . . . . .
H7A H 0.317429 1.468697 0.523421 0.023 Uiso 1 1 calc R U . . .
C8 C 0.1223(3) 1.4056(3) 0.56535(13) 0.0178(5) Uani 1 1 d . . . . .
H8A H 0.070418 1.488865 0.591827 0.021 Uiso 1 1 calc R U . . .
C9 C 0.0469(3) 1.2944(3) 0.56849(13) 0.0168(5) Uani 1 1 d . . . . .
C10 C 0.1287(3) 1.1748(3) 0.52667(13) 0.0169(5) Uani 1 1 d . . . . .
H10A H 0.082040 1.098335 0.526551 0.020 Uiso 1 1 calc R U . . .
C11 C 0.2743(3) 1.1696(3) 0.48662(13) 0.0197(5) Uani 1 1 d . . . . .
H11A H 0.328458 1.089210 0.458420 0.024 Uiso 1 1 calc R U . . .
C12 C 0.5167(3) 0.8088(3) 0.31630(16) 0.0262(6) Uani 1 1 d . . . . .
H12A H 0.425851 0.867232 0.344784 0.031 Uiso 1 1 calc R U . . .
C13 C 0.5112(3) 0.6816(3) 0.29526(16) 0.0253(6) Uani 1 1 d . . . . .
H13A H 0.417439 0.650962 0.309552 0.030 Uiso 1 1 calc R U . . .
C14 C 0.6449(3) 0.5947(3) 0.25210(14) 0.0186(5) Uani 1 1 d . . . . .
C15 C 0.7827(3) 0.6423(3) 0.23551(14) 0.0201(5) Uani 1 1 d . . . . .
H15A H 0.876669 0.585035 0.208419 0.024 Uiso 1 1 calc R U . . .
C16 C 0.7806(3) 0.7706(3) 0.25846(14) 0.0219(5) Uani 1 1 d . . . . .
H16A H 0.873514 0.802932 0.246916 0.026 Uiso 1 1 calc R U . . .
C17 C 1.2632(4) 0.2799(3) -0.01347(17) 0.0341(7) Uani 1 1 d . . . . .
H17A H 1.185780 0.349305 0.015699 0.041 Uiso 1 1 calc R U . . .
C18 C 1.2214(3) 0.1690(3) -0.03328(14) 0.0255(6) Uani 1 1 d . . . . .
H18A H 1.116276 0.161230 -0.018416 0.031 Uiso 1 1 calc R U . . .
C19 C 1.3366(3) 0.0638(3) -0.07667(14) 0.0248(6) Uani 1 1 d . . . . .
C20 C 1.4899(3) 0.0860(3) -0.09987(14) 0.0238(5) Uani 1 1 d . . . . .
H20A H 1.569129 0.022137 -0.131235 0.029 Uiso 1 1 calc R U . . .
C21 C 1.5205(4) 0.2008(3) -0.07616(16) 0.0305(6) Uani 1 1 d . . . . .
H21A H 1.623541 0.213984 -0.090400 0.037 Uiso 1 1 calc R U . . .
N1 N 0.3434(3) 1.2763(2) 0.48620(12) 0.0198(4) Uani 1 1 d . . . . .
H11 H 0.434(4) 1.271(3) 0.4610(16) 0.024 Uiso 1 1 d . U . . .
N2 N -0.0953(3) 1.3017(2) 0.60926(13) 0.0231(5) Uani 1 1 d . . . . .
H1 H -0.143(4) 1.372(3) 0.6340(16) 0.028 Uiso 1 1 d . U . . .
H2 H -0.129(4) 1.234(3) 0.6107(17) 0.028 Uiso 1 1 d . U . . .
N3 N 0.6482(3) 0.8530(2) 0.29748(12) 0.0241(5) Uani 1 1 d . . . . .
H12 H 0.643(4) 0.938(3) 0.3094(16) 0.029 Uiso 1 1 d . U . . .
N4 N 0.6388(3) 0.4730(2) 0.22785(15) 0.0259(5) Uani 1 1 d . . . . .
H3 H 0.721(4) 0.422(3) 0.2025(17) 0.031 Uiso 1 1 d . U . . .
H4 H 0.559(4) 0.450(3) 0.2332(17) 0.031 Uiso 1 1 d . U . . .
N5 N 1.4107(3) 0.2958(3) -0.03348(14) 0.0366(6) Uani 1 1 d . . . . .
H13 H 1.444(4) 0.377(4) -0.0178(18) 0.044 Uiso 1 1 d . U . . .
N6 N 1.3036(3) -0.0497(3) -0.09492(14) 0.0307(5) Uani 1 1 d . . . . .
H5 H 1.386(4) -0.121(3) -0.1208(17) 0.037 Uiso 1 1 d . U . . .
H6 H 1.193(4) -0.057(3) -0.0798(17) 0.037 Uiso 1 1 d . U . . .
O1 O 1.1522(2) 0.99902(18) 0.38015(9) 0.0184(3) Uani 1 1 d . . . . .
O2 O 0.8865(2) 1.27458(18) 0.37871(10) 0.0218(4) Uani 1 1 d . . . . .
O3 O 0.6365(2) 1.3292(2) 0.43832(11) 0.0304(4) Uani 1 1 d . . . . .
O4 O 0.5958(2) 1.11134(18) 0.36433(10) 0.0210(4) Uani 1 1 d . . . . .
O5 O 0.8517(2) 1.07575(18) 0.31402(9) 0.0181(3) Uani 1 1 d . . . . .
O6 O 1.1108(2) 0.98627(17) 0.22905(9) 0.0183(3) Uani 1 1 d . . . . .
O7 O 1.0591(2) 0.9523(2) 0.11457(10) 0.0284(4) Uani 1 1 d . . . . .
O8 O 0.8929(3) 1.2563(2) 0.08707(11) 0.0335(5) Uani 1 1 d . . . . .
O9 O 0.9720(2) 1.27542(18) 0.19829(9) 0.0217(4) Uani 1 1 d . . . . .
O10 O 1.2938(2) 1.13507(18) 0.23982(10) 0.0201(4) Uani 1 1 d . . . . .
O11 O 1.4740(2) 1.2585(2) 0.19288(10) 0.0281(4) Uani 1 1 d . . . . .
O12 O 1.2992(2) 1.46442(19) 0.29395(11) 0.0256(4) Uani 1 1 d . . . . .
O13 O 1.1348(2) 1.32316(18) 0.32665(10) 0.0205(4) Uani 1 1 d . . . . .
O1W O 1.1465(3) 0.6506(3) 0.15871(15) 0.0472(6) Uani 1 1 d D . . . .
H7 H 1.194(4) 0.622(4) 0.2086(14) 0.057 Uiso 1 1 d D U . . .
H8 H 1.123(4) 0.758(2) 0.149(2) 0.057 Uiso 1 1 d D U . . .
O2W O 1.3239(3) 0.5733(2) 0.02117(14) 0.0457(6) Uani 1 1 d D . . . .
H9 H 1.238(3) 0.609(4) 0.0678(15) 0.055 Uiso 1 1 d D U . . .
H10 H 1.253(4) 0.625(4) -0.0190(16) 0.055 Uiso 1 1 d D U . . .
Nb1 Nb 1.06769(3) 1.14168(2) 0.30739(2) 0.01454(7) Uani 1 1 d . . . . .


_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
C1 O3 1.223(3) . ?
C1 O2 1.289(3) . ?
C1 C2 1.532(3) . ?
C2 O4 1.226(3) . ?
C2 O5 1.287(3) . ?
C3 O7 1.226(3) . ?
C3 O6 1.284(3) . ?
C3 C4 1.558(3) . ?
C4 O8 1.223(3) . ?
C4 O9 1.277(3) . ?
C5 O11 1.217(3) . ?
C5 O10 1.293(3) . ?
C5 C6 1.535(3) . ?
C6 O12 1.230(3) . ?
C6 O13 1.285(3) . ?
C7 C8 1.352(3) . ?
C7 N1 1.357(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.416(3) . ?
C8 H8A 0.9500 . ?
C9 N2 1.336(3) . ?
C9 C10 1.414(3) . ?
C10 C11 1.360(3) . ?
C10 H10A 0.9500 . ?
C11 N1 1.348(3) . ?
C11 H11A 0.9500 . ?
C12 N3 1.338(3) . ?
C12 C13 1.356(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.413(3) . ?
C13 H13A 0.9500 . ?
C14 N4 1.335(3) . ?
C14 C15 1.407(3) . ?
C15 C16 1.359(3) . ?
C15 H15A 0.9500 . ?
C16 N3 1.352(3) . ?
C16 H16A 0.9500 . ?
C17 N5 1.348(4) . ?
C17 C18 1.350(4) . ?
C17 H17A 0.9500 . ?
C18 C19 1.423(4) . ?
C18 H18A 0.9500 . ?
C19 N6 1.320(3) . ?
C19 C20 1.427(4) . ?
C20 C21 1.364(4) . ?
C20 H20A 0.9500 . ?
C21 N5 1.342(4) . ?
C21 H21A 0.9500 . ?
N1 H11 0.85(3) . ?
N2 H1 0.83(3) . ?
N2 H2 0.79(3) . ?
N3 H12 0.86(3) . ?
N4 H3 0.85(3) . ?
N4 H4 0.80(3) . ?
N5 H13 1.01(3) . ?
N6 H5 0.95(3) . ?
N6 H6 1.00(3) . ?
O1 Nb1 1.7269(17) . ?
O2 Nb1 2.1053(16) . ?
O5 Nb1 2.1814(16) . ?
O6 Nb1 2.1251(14) . ?
O9 Nb1 2.1968(17) . ?
O10 Nb1 2.1503(17) . ?
O13 Nb1 2.1083(15) . ?
O1W H7 0.979(18) . ?
O1W H8 0.963(18) . ?
O2W H9 1.055(18) . ?
O2W H10 0.964(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C1 O2 126.1(2) . . ?
O3 C1 C2 121.2(2) . . ?
O2 C1 C2 112.6(2) . . ?
O4 C2 O5 126.3(2) . . ?
O4 C2 C1 121.3(2) . . ?
O5 C2 C1 112.4(2) . . ?
O7 C3 O6 125.3(2) . . ?
O7 C3 C4 119.9(2) . . ?
O6 C3 C4 114.80(19) . . ?
O8 C4 O9 126.1(2) . . ?
O8 C4 C3 119.9(2) . . ?
O9 C4 C3 114.0(2) . . ?
O11 C5 O10 126.9(2) . . ?
O11 C5 C6 121.5(2) . . ?
O10 C5 C6 111.6(2) . . ?
O12 C6 O13 125.1(2) . . ?
O12 C6 C5 121.9(2) . . ?
O13 C6 C5 112.91(19) . . ?
C8 C7 N1 120.8(2) . . ?
C8 C7 H7A 119.6 . . ?
N1 C7 H7A 119.6 . . ?
C7 C8 C9 120.3(2) . . ?
C7 C8 H8A 119.9 . . ?
C9 C8 H8A 119.9 . . ?
N2 C9 C10 121.2(2) . . ?
N2 C9 C8 121.6(2) . . ?
C10 C9 C8 117.2(2) . . ?
C11 C10 C9 119.8(2) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
N1 C11 C10 121.2(2) . . ?
N1 C11 H11A 119.4 . . ?
C10 C11 H11A 119.4 . . ?
N3 C12 C13 120.9(2) . . ?
N3 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C14 120.0(2) . . ?
C12 C13 H13A 120.0 . . ?
C14 C13 H13A 120.0 . . ?
N4 C14 C15 121.9(2) . . ?
N4 C14 C13 120.8(2) . . ?
C15 C14 C13 117.4(2) . . ?
C16 C15 C14 119.7(2) . . ?
C16 C15 H15A 120.2 . . ?
C14 C15 H15A 120.2 . . ?
N3 C16 C15 121.0(2) . . ?
N3 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
N5 C17 C18 122.5(3) . . ?
N5 C17 H17A 118.7 . . ?
C18 C17 H17A 118.7 . . ?
C17 C18 C19 119.3(3) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
N6 C19 C18 121.6(3) . . ?
N6 C19 C20 121.1(2) . . ?
C18 C19 C20 117.3(2) . . ?
C21 C20 C19 118.7(2) . . ?
C21 C20 H20A 120.6 . . ?
C19 C20 H20A 120.6 . . ?
N5 C21 C20 122.5(3) . . ?
N5 C21 H21A 118.7 . . ?
C20 C21 H21A 118.7 . . ?
C11 N1 C7 120.7(2) . . ?
C11 N1 H11 119.9(18) . . ?
C7 N1 H11 119.4(18) . . ?
C9 N2 H1 121(2) . . ?
C9 N2 H2 117(2) . . ?
H1 N2 H2 122(3) . . ?
C12 N3 C16 121.0(2) . . ?
C12 N3 H12 117(2) . . ?
C16 N3 H12 122(2) . . ?
C14 N4 H3 119(2) . . ?
C14 N4 H4 123(2) . . ?
H3 N4 H4 118(3) . . ?
C21 N5 C17 119.5(3) . . ?
C21 N5 H13 117.3(19) . . ?
C17 N5 H13 123.1(19) . . ?
C19 N6 H5 119.0(19) . . ?
C19 N6 H6 117.7(17) . . ?
H5 N6 H6 123(3) . . ?
C1 O2 Nb1 122.79(14) . . ?
C2 O5 Nb1 120.24(14) . . ?
C3 O6 Nb1 118.84(14) . . ?
C4 O9 Nb1 116.81(15) . . ?
C5 O10 Nb1 120.75(14) . . ?
C6 O13 Nb1 121.91(14) . . ?
H7 O1W H8 103(3) . . ?
H9 O2W H10 95(3) . . ?
O1 Nb1 O2 98.15(7) . . ?
O1 Nb1 O13 103.12(7) . . ?
O2 Nb1 O13 69.41(6) . . ?
O1 Nb1 O6 90.82(7) . . ?
O2 Nb1 O6 143.16(7) . . ?
O13 Nb1 O6 142.78(7) . . ?
O1 Nb1 O10 93.97(7) . . ?
O2 Nb1 O10 141.47(6) . . ?
O13 Nb1 O10 72.26(6) . . ?
O6 Nb1 O10 72.49(6) . . ?
O1 Nb1 O5 94.41(7) . . ?
O2 Nb1 O5 71.93(6) . . ?
O13 Nb1 O5 139.28(6) . . ?
O6 Nb1 O5 71.81(6) . . ?
O10 Nb1 O5 143.38(6) . . ?
O1 Nb1 O9 165.31(6) . . ?
O2 Nb1 O9 93.31(7) . . ?
O13 Nb1 O9 89.48(6) . . ?
O6 Nb1 O9 74.51(6) . . ?
O10 Nb1 O9 82.58(7) . . ?
O5 Nb1 O9 80.40(6) . . ?

_refine_diff_density_max         0.796
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.081

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

