# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_C10H8N11NbO
_database_code_depnum_ccdc_archive 'CCDC 1419751'
_audit_update_record             
;
2015-08-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C10 H8 N11 Nb O'
_chemical_formula_sum            'C10 H8 N11 Nb O'
_chemical_formula_iupac          ?
_chemical_formula_weight         391.18
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 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'

_cell_length_a                   10.2393(8)
_cell_length_b                   9.8720(7)
_cell_length_c                   14.4784(11)
_cell_angle_alpha                90
_cell_angle_beta                 98.4600(10)
_cell_angle_gamma                90
_cell_volume                     1447.59(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    125
_cell_measurement_theta_min      3.8488
_cell_measurement_theta_max      25.2142
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.148
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776

_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.88

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            13714
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_full        30.55
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20

_refine_special_details          
;
;

_reflns_number_total             4321
_reflns_number_gt                4097
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0518
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.093
_refine_ls_number_reflns         4321
_refine_ls_number_parameters     208
_refine_ls_number_restraints     2
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0157P)²+1.4433P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.929
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Flack x determined using 1920 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(14)

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'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.6076(3) 0.0428(3) 0.4148(3) 0.0319(7) Uani d . . . 1 . .
H H1 0.6493 -0.0005 0.47 0.038 Uiso calc U . R 1 . .
C C2 0.5823(3) -0.0316(3) 0.3334(3) 0.0413(9) Uani d . . . 1 . .
H H2 0.6053 -0.1248 0.3329 0.05 Uiso calc U . R 1 . .
C C3 0.5231(3) 0.0312(4) 0.2526(3) 0.0391(9) Uani d . . . 1 . .
H H3 0.5076 -0.0176 0.1955 0.047 Uiso calc U . R 1 . .
C C4 0.4866(3) 0.1659(3) 0.2559(2) 0.0283(6) Uani d . . . 1 . .
H H4 0.4445 0.2104 0.2014 0.034 Uiso calc U . R 1 . .
C C5 0.5124(3) 0.2357(3) 0.34061(18) 0.0178(5) Uani d . . . 1 . .
C C6 0.4721(2) 0.3776(3) 0.35181(18) 0.0174(5) Uani d . . . 1 . .
C C7 0.4131(3) 0.4572(3) 0.2781(2) 0.0273(6) Uani d . . . 1 . .
H H7 0.3944 0.4208 0.2168 0.033 Uiso calc U . R 1 . .
C C8 0.3819(3) 0.5906(4) 0.2955(3) 0.0384(8) Uani d . . . 1 . .
H H8 0.3418 0.6466 0.246 0.046 Uiso calc U . R 1 . .
C C9 0.4090(4) 0.6413(3) 0.3842(3) 0.0390(8) Uani d . . . 1 . .
H H9 0.3894 0.7329 0.3969 0.047 Uiso calc U . R 1 . .
C C10 0.4657(3) 0.5562(3) 0.4553(2) 0.0291(6) Uani d . . . 1 . .
H H10 0.4828 0.5906 0.5172 0.035 Uiso calc U . R 1 . .
N N1 0.4469(3) 0.2276(3) 0.58490(18) 0.0283(5) Uani d . . . 1 . .
N N2 0.3331(3) 0.2661(3) 0.57043(19) 0.0273(5) Uani d . . . 1 . .
N N3 0.2248(3) 0.2976(3) 0.5599(3) 0.0421(7) Uani d . . . 1 . .
N N4 0.6364(4) 0.4405(5) 0.6544(2) 0.0581(11) Uani d . . . 1 . .
N N5 0.6925(2) 0.5296(3) 0.69924(17) 0.0255(5) Uani d . . . 1 . .
N N6 0.7410(3) 0.6151(3) 0.7438(2) 0.0327(6) Uani d . . . 1 . .
N N7 0.7732(3) 0.3923(3) 0.4935(2) 0.0361(7) Uani d . . . 1 . .
N N8 0.7679(3) 0.4966(4) 0.4467(2) 0.0354(7) Uani d . . . 1 . .
N N9 0.7673(3) 0.5922(4) 0.4024(2) 0.0462(9) Uani d . . . 1 . .
N N10 0.5752(2) 0.1751(2) 0.41873(18) 0.0213(5) Uani d . . . 1 . .
N N11 0.4974(2) 0.4268(2) 0.43987(16) 0.0199(4) Uani d . . . 1 . .
Nb Nb1 0.62665(2) 0.29359(3) 0.55434(2) 0.02723(7) Uani d . . . 1 . .
O O1 0.7244(3) 0.1615(4) 0.5998(2) 0.0513(7) Uani d . . . 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N10 . 1.350(4) ?
C1 C2 . 1.381(5) ?
C1 H1 . 0.95 ?
C2 C3 . 1.383(6) ?
C2 H2 . 0.95 ?
C3 C4 . 1.384(5) ?
C3 H3 . 0.95 ?
C4 C5 . 1.397(4) ?
C4 H4 . 0.95 ?
C5 N10 . 1.355(4) ?
C5 C6 . 1.476(4) ?
C6 N11 . 1.353(3) ?
C6 C7 . 1.390(4) ?
C7 C8 . 1.387(5) ?
C7 H7 . 0.95 ?
C8 C9 . 1.368(6) ?
C8 H8 . 0.95 ?
C9 C10 . 1.389(5) ?
C9 H9 . 0.95 ?
C10 N11 . 1.345(4) ?
C10 H10 . 0.95 ?
N1 N2 . 1.214(4) ?
N1 Nb1 . 2.061(3) ?
N2 N3 . 1.139(4) ?
N4 N5 . 1.189(4) ?
N4 Nb1 . 2.042(3) ?
N5 N6 . 1.132(4) ?
N7 N8 . 1.229(5) ?
N7 Nb1 . 2.090(3) ?
N8 N9 . 1.141(5) ?
N10 Nb1 . 2.280(2) ?
N11 Nb1 . 2.362(2) ?
Nb1 O1 . 1.715(3) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N10 C1 C2 . . 122.3(3) ?
N10 C1 H1 . . 118.9 ?
C2 C1 H1 . . 118.9 ?
C1 C2 C3 . . 119.2(3) ?
C1 C2 H2 . . 120.4 ?
C3 C2 H2 . . 120.4 ?
C2 C3 C4 . . 119.2(3) ?
C2 C3 H3 . . 120.4 ?
C4 C3 H3 . . 120.4 ?
C3 C4 C5 . . 119.2(3) ?
C3 C4 H4 . . 120.4 ?
C5 C4 H4 . . 120.4 ?
N10 C5 C4 . . 121.3(3) ?
N10 C5 C6 . . 115.7(2) ?
C4 C5 C6 . . 123.0(3) ?
N11 C6 C7 . . 121.5(3) ?
N11 C6 C5 . . 115.2(2) ?
C7 C6 C5 . . 123.3(3) ?
C8 C7 C6 . . 118.9(3) ?
C8 C7 H7 . . 120.6 ?
C6 C7 H7 . . 120.6 ?
C9 C8 C7 . . 119.9(3) ?
C9 C8 H8 . . 120.1 ?
C7 C8 H8 . . 120.1 ?
C8 C9 C10 . . 118.6(3) ?
C8 C9 H9 . . 120.7 ?
C10 C9 H9 . . 120.7 ?
N11 C10 C9 . . 122.5(3) ?
N11 C10 H10 . . 118.8 ?
C9 C10 H10 . . 118.8 ?
N2 N1 Nb1 . . 136.7(2) ?
N3 N2 N1 . . 176.6(3) ?
N5 N4 Nb1 . . 151.9(3) ?
N6 N5 N4 . . 176.9(3) ?
N8 N7 Nb1 . . 130.3(2) ?
N9 N8 N7 . . 177.5(4) ?
C1 N10 C5 . . 118.8(3) ?
C1 N10 Nb1 . . 120.3(2) ?
C5 N10 Nb1 . . 120.90(18) ?
C10 N11 C6 . . 118.7(3) ?
C10 N11 Nb1 . . 122.4(2) ?
C6 N11 Nb1 . . 118.12(18) ?
O1 Nb1 N4 . . 107.66(17) ?
O1 Nb1 N1 . . 99.60(13) ?
N4 Nb1 N1 . . 91.41(12) ?
O1 Nb1 N7 . . 95.81(14) ?
N4 Nb1 N7 . . 90.26(13) ?
N1 Nb1 N7 . . 163.20(11) ?
O1 Nb1 N10 . . 89.31(12) ?
N4 Nb1 N10 . . 163.03(14) ?
N1 Nb1 N10 . . 85.53(10) ?
N7 Nb1 N10 . . 88.02(10) ?
O1 Nb1 N11 . . 158.00(12) ?
N4 Nb1 N11 . . 93.79(15) ?
N1 Nb1 N11 . . 84.30(9) ?
N7 Nb1 N11 . . 78.91(10) ?
N10 Nb1 N11 . . 69.31(8) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N10 C1 C2 C3 . . . . 0.8(5) ?
C1 C2 C3 C4 . . . . -2.2(5) ?
C2 C3 C4 C5 . . . . 1.0(5) ?
C3 C4 C5 N10 . . . . 1.6(4) ?
C3 C4 C5 C6 . . . . -177.3(3) ?
N10 C5 C6 N11 . . . . -3.1(3) ?
C4 C5 C6 N11 . . . . 175.9(2) ?
N10 C5 C6 C7 . . . . 176.5(3) ?
C4 C5 C6 C7 . . . . -4.5(4) ?
N11 C6 C7 C8 . . . . 1.2(4) ?
C5 C6 C7 C8 . . . . -178.4(3) ?
C6 C7 C8 C9 . . . . -0.3(5) ?
C7 C8 C9 C10 . . . . -1.0(5) ?
C8 C9 C10 N11 . . . . 1.4(5) ?
C2 C1 N10 C5 . . . . 1.8(4) ?
C2 C1 N10 Nb1 . . . . -177.8(2) ?
C4 C5 N10 C1 . . . . -3.0(4) ?
C6 C5 N10 C1 . . . . 176.0(3) ?
C4 C5 N10 Nb1 . . . . 176.6(2) ?
C6 C5 N10 Nb1 . . . . -4.3(3) ?
C9 C10 N11 C6 . . . . -0.5(4) ?
C9 C10 N11 Nb1 . . . . 169.1(2) ?
C7 C6 N11 C10 . . . . -0.9(4) ?
C5 C6 N11 C10 . . . . 178.8(2) ?
C7 C6 N11 Nb1 . . . . -170.9(2) ?
C5 C6 N11 Nb1 . . . . 8.8(3) ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Heat-sensitive, explosive'
####################################################################### 
# 
# 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_C48H40N15NbOP2
_database_code_depnum_ccdc_archive 'CCDC 1419752'
_audit_update_record             
;
2015-08-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(C24 H20 P), N15 Nb O'
_chemical_formula_sum            'C48 H40 N15 Nb O P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         997.80

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_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                   12.9621(12)
_cell_length_b                   13.2840(12)
_cell_length_c                   14.0506(13)
_cell_angle_alpha                86.124(2)
_cell_angle_beta                 85.660(2)
_cell_angle_gamma                73.9850(10)
_cell_volume                     2316.0(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6446
_cell_measurement_theta_min      2.5374
_cell_measurement_theta_max      27.2954
_cell_measurement_temperature    133.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024

_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2012/1'
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.98

_exptl_special_details           
;
;

_diffrn_ambient_temperature      133.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            13718
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       12

_refine_special_details          
;
;

_reflns_number_total             9499
_reflns_number_gt                7512
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0929
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_number_reflns         9499
_refine_ls_number_parameters     604
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.363
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
P P 0.1023 0.0942 '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'

_computing_data_collection       'SMART V5.632'
_computing_cell_refinement       'APEX2 v2014.1-1 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/1 (Bruker AXS)'
_computing_structure_refinement  'SHELXTL XLMP 2014/1 (Bruker AXS)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb Nb1 0.32283(2) 0.21944(2) 0.25635(2) 0.02543(7) Uani d . . . 1 . .
P P1 0.29071(4) 0.40133(4) 0.67499(4) 0.02065(13) Uani d . . . 1 . .
P P2 0.93202(4) 0.02303(4) 0.22139(4) 0.02083(13) Uani d . . . 1 . .
O O1 0.27334(14) 0.11767(13) 0.30136(12) 0.0398(4) Uani d . . . 1 . .
N N1 0.20893(16) 0.26532(15) 0.15173(15) 0.0341(5) Uani d . . . 1 . .
N N2 0.18388(15) 0.34008(15) 0.09626(14) 0.0292(4) Uani d . . . 1 . .
N N3 0.15487(17) 0.40773(17) 0.04171(16) 0.0419(5) Uani d . . . 1 . .
N N4 0.21692(18) 0.33454(17) 0.34351(16) 0.0410(5) Uani d . . . 1 . .
N N5 0.13146(17) 0.32705(14) 0.37867(14) 0.0314(5) Uani d . . . 1 . .
N N6 0.04936(18) 0.32511(17) 0.41297(17) 0.0441(6) Uani d . . . 1 . .
N N7 0.44103(17) 0.19571(16) 0.35456(15) 0.0388(5) Uani d . . . 1 . .
N N8 0.51084(16) 0.23658(15) 0.36654(14) 0.0306(5) Uani d . . . 1 . .
N N9 0.57759(18) 0.27228(18) 0.38258(18) 0.0488(6) Uani d . . . 1 . .
N N10 0.43376(16) 0.13311(15) 0.15523(15) 0.0365(5) Uani d . . . 1 . .
N N11 0.48786(19) 0.16352(17) 0.09260(17) 0.0460(6) Uani d . . . 1 . .
N N12 0.5397(3) 0.1886(2) 0.0319(2) 0.0917(11) Uani d . . . 1 . .
N N13 0.38382(15) 0.35567(14) 0.19671(14) 0.0314(5) Uani d . . . 1 . .
N N14 0.36147(14) 0.44852(14) 0.18697(12) 0.0249(4) Uani d . . . 1 . .
N N15 0.34266(17) 0.53829(15) 0.17576(15) 0.0411(5) Uani d . . . 1 . .
C C1 0.15210(16) 0.40382(15) 0.70220(16) 0.0223(5) Uani d . . . 1 . .
C C2 0.11247(18) 0.39771(16) 0.79712(17) 0.0282(5) Uani d . . . 1 . .
H H2 0.1593 0.3877 0.8479 0.034 Uiso calc U . R 1 . .
C C3 0.0040(2) 0.40642(18) 0.8161(2) 0.0398(6) Uani d . . . 1 . .
H H3 -0.024 0.4034 0.8804 0.048 Uiso calc U . R 1 . .
C C4 -0.06343(19) 0.41949(18) 0.7423(2) 0.0446(7) Uani d . . . 1 . .
H H4 -0.138 0.4269 0.7561 0.054 Uiso calc U . R 1 . .
C C5 -0.0240(2) 0.4218(2) 0.6492(2) 0.0443(7) Uani d . . . 1 . .
H H5 -0.071 0.4291 0.599 0.053 Uiso calc U . R 1 . .
C C6 0.08434(19) 0.41360(18) 0.62788(18) 0.0323(6) Uani d . . . 1 . .
H H6 0.1118 0.4146 0.5633 0.039 Uiso calc U . R 1 . .
C C7 0.34000(16) 0.45273(17) 0.77115(15) 0.0223(5) Uani d . . . 1 . .
C C8 0.35917(18) 0.39545(19) 0.85813(16) 0.0300(5) Uani d . . . 1 . .
H H8 0.3542 0.3253 0.8643 0.036 Uiso calc U . R 1 . .
C C9 0.38541(18) 0.4409(2) 0.93534(17) 0.0364(6) Uani d . . . 1 . .
H H9 0.398 0.4022 0.9946 0.044 Uiso calc U . R 1 . .
C C10 0.39321(18) 0.5427(2) 0.92604(18) 0.0353(6) Uani d . . . 1 . .
H H10 0.4095 0.5742 0.9796 0.042 Uiso calc U . R 1 . .
C C11 0.37754(17) 0.59885(19) 0.83985(17) 0.0303(5) Uani d . . . 1 . .
H H11 0.3855 0.668 0.8335 0.036 Uiso calc U . R 1 . .
C C12 0.35023(16) 0.55446(17) 0.76246(16) 0.0248(5) Uani d . . . 1 . .
H H12 0.3385 0.5936 0.7033 0.03 Uiso calc U . R 1 . .
C C13 0.29659(17) 0.48183(16) 0.56812(15) 0.0226(5) Uani d . . . 1 . .
C C14 0.37776(18) 0.44908(18) 0.49795(16) 0.0280(5) Uani d . . . 1 . .
H H14 0.43 0.3835 0.5059 0.034 Uiso calc U . R 1 . .
C C15 0.38243(19) 0.5123(2) 0.41611(17) 0.0348(6) Uani d . . . 1 . .
H H15 0.4376 0.4897 0.3675 0.042 Uiso calc U . R 1 . .
C C16 0.3074(2) 0.6076(2) 0.40498(17) 0.0349(6) Uani d . . . 1 . .
H H16 0.3111 0.6508 0.3488 0.042 Uiso calc U . R 1 . .
C C17 0.22676(19) 0.64074(18) 0.47495(17) 0.0320(5) Uani d . . . 1 . .
H H17 0.1755 0.7069 0.4668 0.038 Uiso calc U . R 1 . .
C C18 0.21985(18) 0.57849(17) 0.55707(16) 0.0271(5) Uani d . . . 1 . .
H H18 0.1639 0.6011 0.605 0.033 Uiso calc U . R 1 . .
C C19 0.36950(17) 0.26970(16) 0.65497(15) 0.0249(5) Uani d . . . 1 . .
C C20 0.3255(2) 0.20394(18) 0.60902(17) 0.0326(5) Uani d . . . 1 . .
H H20 0.2533 0.2275 0.5909 0.039 Uiso calc U . R 1 . .
C C21 0.3871(2) 0.10364(19) 0.58955(18) 0.0408(6) Uani d . . . 1 . .
H H21 0.3573 0.0584 0.5576 0.049 Uiso calc U . R 1 . .
C C22 0.4918(2) 0.0692(2) 0.61647(18) 0.0432(7) Uani d . . . 1 . .
H H22 0.5337 0.0001 0.6035 0.052 Uiso calc U . R 1 . .
C C23 0.5354(2) 0.1347(2) 0.66205(18) 0.0401(6) Uani d . . . 1 . .
H H23 0.6075 0.1106 0.6805 0.048 Uiso calc U . R 1 . .
C C24 0.47531(18) 0.23559(19) 0.68130(17) 0.0335(6) Uani d . . . 1 . .
H H24 0.506 0.281 0.7121 0.04 Uiso calc U . R 1 . .
C C25 0.89359(17) 0.02195(16) 0.34659(15) 0.0237(5) Uani d . . . 1 . .
C C26 0.81393(18) 0.10527(17) 0.38416(16) 0.0270(5) Uani d . . . 1 . .
H H26 0.7849 0.1661 0.3449 0.032 Uiso calc U . R 1 . .
C C27 0.77680(19) 0.09918(19) 0.47963(16) 0.0326(5) Uani d . . . 1 . .
H H27 0.7221 0.1556 0.5056 0.039 Uiso calc U . R 1 . .
C C28 0.8200(2) 0.0109(2) 0.53591(17) 0.0360(6) Uani d . . . 1 . .
H H28 0.7949 0.0071 0.601 0.043 Uiso calc U . R 1 . .
C C29 0.8988(2) -0.07199(19) 0.49954(17) 0.0373(6) Uani d . . . 1 . .
H H29 0.9276 -0.1324 0.5394 0.045 Uiso calc U . R 1 . .
C C30 0.93600(19) -0.06744(18) 0.40493(17) 0.0312(5) Uani d . . . 1 . .
H H30 0.9901 -0.1247 0.3796 0.037 Uiso calc U . R 1 . .
C C31 0.91456(16) 0.15540(16) 0.17574(15) 0.0214(5) Uani d . . . 1 . .
C C32 0.95393(17) 0.22407(16) 0.22460(16) 0.0245(5) Uani d . . . 1 . .
H H32 0.9848 0.2023 0.2843 0.029 Uiso calc U . R 1 . .
C C33 0.94766(17) 0.32373(16) 0.18545(16) 0.0268(5) Uani d . . . 1 . .
H H33 0.9744 0.3705 0.2185 0.032 Uiso calc U . R 1 . .
C C34 0.90303(18) 0.35563(17) 0.09910(16) 0.0284(5) Uani d . . . 1 . .
H H34 0.8998 0.424 0.0724 0.034 Uiso calc U . R 1 . .
C C35 0.86261(18) 0.28843(17) 0.05062(16) 0.0294(5) Uani d . . . 1 . .
H H35 0.8312 0.3114 -0.0087 0.035 Uiso calc U . R 1 . .
C C36 0.86777(17) 0.18839(17) 0.08823(15) 0.0247(5) Uani d . . . 1 . .
H H36 0.8399 0.1425 0.0552 0.03 Uiso calc U . R 1 . .
C C37 0.84803(17) -0.03674(16) 0.16161(15) 0.0237(5) Uani d . . . 1 . .
C C38 0.8880(2) -0.09351(18) 0.08096(17) 0.0330(5) Uani d . . . 1 . .
H H38 0.9605 -0.1019 0.0579 0.04 Uiso calc U . R 1 . .
C C39 0.8227(2) -0.1377(2) 0.03447(18) 0.0393(6) Uani d . . . 1 . .
H H39 0.8507 -0.1777 -0.0198 0.047 Uiso calc U . R 1 . .
C C40 0.7171(2) -0.1240(2) 0.06644(19) 0.0420(7) Uani d . . . 1 . .
H H40 0.6723 -0.1545 0.0341 0.05 Uiso calc U . R 1 . .
C C41 0.6757(2) -0.0657(2) 0.14579(19) 0.0407(6) Uani d . . . 1 . .
H H41 0.6024 -0.0553 0.167 0.049 Uiso calc U . R 1 . .
C C42 0.74109(19) -0.02287(18) 0.19391(18) 0.0330(6) Uani d . . . 1 . .
H H42 0.7132 0.016 0.2489 0.04 Uiso calc U . R 1 . .
C C43 1.06948(17) -0.05000(16) 0.19910(15) 0.0239(5) Uani d . . . 1 . .
C C44 1.09661(18) -0.15997(17) 0.20317(16) 0.0296(5) Uani d . . . 1 . .
H H44 1.0429 -0.1954 0.2199 0.035 Uiso calc U . R 1 . .
C C45 1.20235(19) -0.21666(18) 0.18266(17) 0.0332(6) Uani d . . . 1 . .
H H45 1.2214 -0.2911 0.1857 0.04 Uiso calc U . R 1 . .
C C46 1.27996(19) -0.16431(19) 0.15781(17) 0.0348(6) Uani d . . . 1 . .
H H46 1.3518 -0.2034 0.1421 0.042 Uiso calc U . R 1 . .
C C47 1.25474(19) -0.05669(19) 0.15559(17) 0.0343(6) Uani d . . . 1 . .
H H47 1.3091 -0.0218 0.1399 0.041 Uiso calc U . R 1 . .
C C48 1.14911(17) 0.00096(18) 0.17640(16) 0.0280(5) Uani d . . . 1 . .
H H48 1.1314 0.0753 0.1751 0.034 Uiso calc U . R 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Nb1 O1 . 1.7147(15) ?
Nb1 N7 . 2.085(2) ?
Nb1 N10 . 2.098(2) ?
Nb1 N1 . 2.1030(19) ?
Nb1 N4 . 2.136(2) ?
Nb1 N13 . 2.2553(18) ?
P1 C7 . 1.788(2) ?
P1 C13 . 1.793(2) ?
P1 C19 . 1.794(2) ?
P1 C1 . 1.800(2) ?
P2 C31 . 1.790(2) ?
P2 C25 . 1.792(2) ?
P2 C43 . 1.794(2) ?
P2 C37 . 1.796(2) ?
N1 N2 . 1.206(3) ?
N2 N3 . 1.140(3) ?
N4 N5 . 1.205(3) ?
N5 N6 . 1.141(3) ?
N7 N8 . 1.204(3) ?
N8 N9 . 1.138(3) ?
N10 N11 . 1.202(3) ?
N11 N12 . 1.135(3) ?
N13 N14 . 1.187(2) ?
N14 N15 . 1.152(2) ?
C1 C6 . 1.392(3) ?
C1 C2 . 1.398(3) ?
C2 C3 . 1.385(3) ?
C2 H2 . 0.95 ?
C3 C4 . 1.379(4) ?
C3 H3 . 0.95 ?
C4 C5 . 1.368(4) ?
C4 H4 . 0.95 ?
C5 C6 . 1.390(3) ?
C5 H5 . 0.95 ?
C6 H6 . 0.95 ?
C7 C12 . 1.390(3) ?
C7 C8 . 1.396(3) ?
C8 C9 . 1.384(3) ?
C8 H8 . 0.95 ?
C9 C10 . 1.380(4) ?
C9 H9 . 0.95 ?
C10 C11 . 1.377(3) ?
C10 H10 . 0.95 ?
C11 C12 . 1.384(3) ?
C11 H11 . 0.95 ?
C12 H12 . 0.95 ?
C13 C14 . 1.384(3) ?
C13 C18 . 1.398(3) ?
C14 C15 . 1.385(3) ?
C14 H14 . 0.95 ?
C15 C16 . 1.375(3) ?
C15 H15 . 0.95 ?
C16 C17 . 1.379(3) ?
C16 H16 . 0.95 ?
C17 C18 . 1.386(3) ?
C17 H17 . 0.95 ?
C18 H18 . 0.95 ?
C19 C20 . 1.383(3) ?
C19 C24 . 1.391(3) ?
C20 C21 . 1.385(3) ?
C20 H20 . 0.95 ?
C21 C22 . 1.380(4) ?
C21 H21 . 0.95 ?
C22 C23 . 1.375(4) ?
C22 H22 . 0.95 ?
C23 C24 . 1.384(3) ?
C23 H23 . 0.95 ?
C24 H24 . 0.95 ?
C25 C26 . 1.391(3) ?
C25 C30 . 1.400(3) ?
C26 C27 . 1.395(3) ?
C26 H26 . 0.95 ?
C27 C28 . 1.376(3) ?
C27 H27 . 0.95 ?
C28 C29 . 1.376(4) ?
C28 H28 . 0.95 ?
C29 C30 . 1.383(3) ?
C29 H29 . 0.95 ?
C30 H30 . 0.95 ?
C31 C32 . 1.400(3) ?
C31 C36 . 1.402(3) ?
C32 C33 . 1.382(3) ?
C32 H32 . 0.95 ?
C33 C34 . 1.374(3) ?
C33 H33 . 0.95 ?
C34 C35 . 1.389(3) ?
C34 H34 . 0.95 ?
C35 C36 . 1.383(3) ?
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
C37 C38 . 1.390(3) ?
C37 C42 . 1.392(3) ?
C38 C39 . 1.377(3) ?
C38 H38 . 0.95 ?
C39 C40 . 1.374(4) ?
C39 H39 . 0.95 ?
C40 C41 . 1.388(4) ?
C40 H40 . 0.95 ?
C41 C42 . 1.380(3) ?
C41 H41 . 0.95 ?
C42 H42 . 0.95 ?
C43 C48 . 1.390(3) ?
C43 C44 . 1.403(3) ?
C44 C45 . 1.389(3) ?
C44 H44 . 0.95 ?
C45 C46 . 1.385(3) ?
C45 H45 . 0.95 ?
C46 C47 . 1.374(3) ?
C46 H46 . 0.95 ?
C47 C48 . 1.392(3) ?
C47 H47 . 0.95 ?
C48 H48 . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Nb1 N7 . . 95.34(8) ?
O1 Nb1 N10 . . 96.15(8) ?
N7 Nb1 N10 . . 91.27(9) ?
O1 Nb1 N1 . . 93.22(8) ?
N7 Nb1 N1 . . 171.24(7) ?
N10 Nb1 N1 . . 89.61(8) ?
O1 Nb1 N4 . . 95.36(8) ?
N7 Nb1 N4 . . 90.19(9) ?
N10 Nb1 N4 . . 168.21(8) ?
N1 Nb1 N4 . . 87.20(8) ?
O1 Nb1 N13 . . 178.62(8) ?
N7 Nb1 N13 . . 85.70(7) ?
N10 Nb1 N13 . . 84.73(7) ?
N1 Nb1 N13 . . 85.71(7) ?
N4 Nb1 N13 . . 83.72(8) ?
C7 P1 C13 . . 109.76(10) ?
C7 P1 C19 . . 110.43(10) ?
C13 P1 C19 . . 109.35(10) ?
C7 P1 C1 . . 109.72(10) ?
C13 P1 C1 . . 107.57(10) ?
C19 P1 C1 . . 109.96(10) ?
C31 P2 C25 . . 109.64(10) ?
C31 P2 C43 . . 109.27(10) ?
C25 P2 C43 . . 111.24(10) ?
C31 P2 C37 . . 109.78(10) ?
C25 P2 C37 . . 108.42(10) ?
C43 P2 C37 . . 108.47(10) ?
N2 N1 Nb1 . . 134.05(16) ?
N3 N2 N1 . . 175.2(2) ?
N5 N4 Nb1 . . 123.82(16) ?
N6 N5 N4 . . 176.6(2) ?
N8 N7 Nb1 . . 134.53(16) ?
N9 N8 N7 . . 176.2(2) ?
N11 N10 Nb1 . . 129.15(17) ?
N12 N11 N10 . . 177.4(3) ?
N14 N13 Nb1 . . 143.97(16) ?
N15 N14 N13 . . 177.9(2) ?
C6 C1 C2 . . 120.3(2) ?
C6 C1 P1 . . 119.37(17) ?
C2 C1 P1 . . 120.32(17) ?
C3 C2 C1 . . 119.1(2) ?
C3 C2 H2 . . 120.5 ?
C1 C2 H2 . . 120.5 ?
C4 C3 C2 . . 120.3(2) ?
C4 C3 H3 . . 119.8 ?
C2 C3 H3 . . 119.8 ?
C5 C4 C3 . . 120.6(2) ?
C5 C4 H4 . . 119.7 ?
C3 C4 H4 . . 119.7 ?
C4 C5 C6 . . 120.4(2) ?
C4 C5 H5 . . 119.8 ?
C6 C5 H5 . . 119.8 ?
C5 C6 C1 . . 119.2(2) ?
C5 C6 H6 . . 120.4 ?
C1 C6 H6 . . 120.4 ?
C12 C7 C8 . . 119.4(2) ?
C12 C7 P1 . . 119.69(16) ?
C8 C7 P1 . . 120.70(17) ?
C9 C8 C7 . . 120.0(2) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
C10 C9 C8 . . 119.9(2) ?
C10 C9 H9 . . 120.1 ?
C8 C9 H9 . . 120.1 ?
C11 C10 C9 . . 120.6(2) ?
C11 C10 H10 . . 119.7 ?
C9 C10 H10 . . 119.7 ?
C10 C11 C12 . . 119.9(2) ?
C10 C11 H11 . . 120.0 ?
C12 C11 H11 . . 120.0 ?
C11 C12 C7 . . 120.2(2) ?
C11 C12 H12 . . 119.9 ?
C7 C12 H12 . . 119.9 ?
C14 C13 C18 . . 120.4(2) ?
C14 C13 P1 . . 120.09(16) ?
C18 C13 P1 . . 119.50(17) ?
C13 C14 C15 . . 119.7(2) ?
C13 C14 H14 . . 120.1 ?
C15 C14 H14 . . 120.1 ?
C16 C15 C14 . . 120.2(2) ?
C16 C15 H15 . . 119.9 ?
C14 C15 H15 . . 119.9 ?
C15 C16 C17 . . 120.3(2) ?
C15 C16 H16 . . 119.9 ?
C17 C16 H16 . . 119.9 ?
C16 C17 C18 . . 120.6(2) ?
C16 C17 H17 . . 119.7 ?
C18 C17 H17 . . 119.7 ?
C17 C18 C13 . . 118.8(2) ?
C17 C18 H18 . . 120.6 ?
C13 C18 H18 . . 120.6 ?
C20 C19 C24 . . 120.3(2) ?
C20 C19 P1 . . 119.22(17) ?
C24 C19 P1 . . 120.44(18) ?
C19 C20 C21 . . 119.7(2) ?
C19 C20 H20 . . 120.1 ?
C21 C20 H20 . . 120.1 ?
C22 C21 C20 . . 120.2(2) ?
C22 C21 H21 . . 119.9 ?
C20 C21 H21 . . 119.9 ?
C23 C22 C21 . . 120.0(2) ?
C23 C22 H22 . . 120.0 ?
C21 C22 H22 . . 120.0 ?
C22 C23 C24 . . 120.6(2) ?
C22 C23 H23 . . 119.7 ?
C24 C23 H23 . . 119.7 ?
C23 C24 C19 . . 119.2(2) ?
C23 C24 H24 . . 120.4 ?
C19 C24 H24 . . 120.4 ?
C26 C25 C30 . . 119.7(2) ?
C26 C25 P2 . . 120.17(16) ?
C30 C25 P2 . . 119.79(17) ?
C25 C26 C27 . . 119.8(2) ?
C25 C26 H26 . . 120.1 ?
C27 C26 H26 . . 120.1 ?
C28 C27 C26 . . 119.5(2) ?
C28 C27 H27 . . 120.2 ?
C26 C27 H27 . . 120.2 ?
C29 C28 C27 . . 121.2(2) ?
C29 C28 H28 . . 119.4 ?
C27 C28 H28 . . 119.4 ?
C28 C29 C30 . . 120.0(2) ?
C28 C29 H29 . . 120.0 ?
C30 C29 H29 . . 120.0 ?
C29 C30 C25 . . 119.7(2) ?
C29 C30 H30 . . 120.1 ?
C25 C30 H30 . . 120.1 ?
C32 C31 C36 . . 119.94(19) ?
C32 C31 P2 . . 119.79(16) ?
C36 C31 P2 . . 120.14(16) ?
C33 C32 C31 . . 119.6(2) ?
C33 C32 H32 . . 120.2 ?
C31 C32 H32 . . 120.2 ?
C34 C33 C32 . . 120.4(2) ?
C34 C33 H33 . . 119.8 ?
C32 C33 H33 . . 119.8 ?
C33 C34 C35 . . 120.3(2) ?
C33 C34 H34 . . 119.8 ?
C35 C34 H34 . . 119.8 ?
C36 C35 C34 . . 120.4(2) ?
C36 C35 H35 . . 119.8 ?
C34 C35 H35 . . 119.8 ?
C35 C36 C31 . . 119.2(2) ?
C35 C36 H36 . . 120.4 ?
C31 C36 H36 . . 120.4 ?
C38 C37 C42 . . 119.6(2) ?
C38 C37 P2 . . 120.42(18) ?
C42 C37 P2 . . 119.89(17) ?
C39 C38 C37 . . 120.2(2) ?
C39 C38 H38 . . 119.9 ?
C37 C38 H38 . . 119.9 ?
C40 C39 C38 . . 120.1(2) ?
C40 C39 H39 . . 119.9 ?
C38 C39 H39 . . 119.9 ?
C39 C40 C41 . . 120.2(2) ?
C39 C40 H40 . . 119.9 ?
C41 C40 H40 . . 119.9 ?
C42 C41 C40 . . 120.0(3) ?
C42 C41 H41 . . 120.0 ?
C40 C41 H41 . . 120.0 ?
C41 C42 C37 . . 119.8(2) ?
C41 C42 H42 . . 120.1 ?
C37 C42 H42 . . 120.1 ?
C48 C43 C44 . . 119.6(2) ?
C48 C43 P2 . . 120.84(16) ?
C44 C43 P2 . . 119.53(17) ?
C45 C44 C43 . . 119.7(2) ?
C45 C44 H44 . . 120.2 ?
C43 C44 H44 . . 120.2 ?
C46 C45 C44 . . 119.8(2) ?
C46 C45 H45 . . 120.1 ?
C44 C45 H45 . . 120.1 ?
C47 C46 C45 . . 121.0(2) ?
C47 C46 H46 . . 119.5 ?
C45 C46 H46 . . 119.5 ?
C46 C47 C48 . . 119.7(2) ?
C46 C47 H47 . . 120.2 ?
C48 C47 H47 . . 120.2 ?
C43 C48 C47 . . 120.2(2) ?
C43 C48 H48 . . 119.9 ?
C47 C48 H48 . . 119.9 ?


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_compound_source        acetonitrile
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_Cs2NbON15
_database_code_depnum_ccdc_archive 'CCDC 1419753'
_audit_update_record             
;
2015-08-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            Cs2NbON15
_chemical_formula_moiety         'N15 Nb O, 2(Cs)'
_chemical_formula_sum            'Cs2 N15 Nb O'
_chemical_formula_iupac          ?
_chemical_formula_weight         584.88

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_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                   12.5793(15)
_cell_length_b                   16.4373(19)
_cell_length_c                   12.8012(15)
_cell_angle_alpha                90
_cell_angle_beta                 92.433(2)
_cell_angle_gamma                90
_cell_volume                     2644.5(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6025
_cell_measurement_theta_min      2.4807
_cell_measurement_theta_max      28.6922
_cell_measurement_temperature    133.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.090
_exptl_crystal_density_diffrn    2.938
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112

_exptl_absorpt_coefficient_mu    6.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2012/1'
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_T_max  0.60

_exptl_special_details           
;
;

_diffrn_ambient_temperature      133.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            8376
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
;

_reflns_number_total             3157
_reflns_number_gt                2931
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0450
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.062
_refine_ls_number_reflns         3157
_refine_ls_number_parameters     182
_refine_ls_number_restraints     39
_refine_ls_hydrogen_treatment    undef
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²+4.2919P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   ?
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.772
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Cs Cs -0.3680 2.1192 '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'

_computing_data_collection       'SMART V5.632'
_computing_cell_refinement       'APEX2 v2014.1-1 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/1 (Bruker AXS)'
_computing_structure_refinement  'SHELXTL XLMP 2014/1 (Bruker AXS)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs Cs1 0.07691(2) 0.38598(2) -0.09819(2) 0.02238(6) Uani d . . . 1.0 . .
Cs Cs2 0.34604(2) 0.62577(2) 0.06078(2) 0.02510(6) Uani d . . . 1.0 . .
N N1 0.3140(2) 0.34738(15) 0.2886(2) 0.0246(5) Uani d . . . 1.0 . .
N N2 0.3395(2) 0.27840(15) 0.29288(18) 0.0210(5) Uani d . . . 1.0 . .
N N3 0.3653(3) 0.21076(17) 0.3000(2) 0.0404(8) Uani d . . . 1.0 . .
N N4 0.3077(2) 0.41863(15) 0.0712(2) 0.0259(5) Uani d . . . 1.0 . .
N N5 0.3759(2) 0.36650(15) 0.0662(2) 0.0262(6) Uani d . . . 1.0 . .
N N6 0.4409(2) 0.31847(17) 0.0581(2) 0.0377(7) Uani d . . . 1.0 . .
N N7 0.3001(2) 0.52140(15) 0.26627(19) 0.0244(5) Uani d . . . 1.0 . .
N N8 0.3786(2) 0.51415(14) 0.32361(19) 0.0216(5) Uani d . . . 1.0 . .
N N9 0.4533(2) 0.51024(16) 0.3769(2) 0.0313(6) Uani d . . . 1.0 . .
N N10 0.1125(2) 0.42707(15) 0.3282(2) 0.0268(6) Uani d . . . 1.0 . .
N N11 0.11502(19) 0.37121(15) 0.3884(2) 0.0219(5) Uani d . . . 1.0 . .
N N12 0.1159(2) 0.31907(17) 0.4482(2) 0.0311(6) Uani d . . . 1.0 . .
N N13_a 0.1186(10) 0.3279(6) 0.1467(11) 0.0205(17) Uani d U P D 0.547(5) A 1
N N14_a 0.1029(5) 0.2628(4) 0.1773(5) 0.0261(11) Uani d U P D 0.547(5) A 1
N N15_a 0.0707(6) 0.2024(4) 0.2093(5) 0.0530(13) Uani d U P D 0.547(5) A 1
N N13'_b 0.1371(12) 0.3276(7) 0.1319(14) 0.0205(17) Uani d U P D 0.453(5) A 2
N N14'_b 0.1418(6) 0.2597(5) 0.1533(6) 0.0261(11) Uani d U P D 0.453(5) A 2
N N15'_b 0.1534(7) 0.1911(4) 0.1659(6) 0.0530(13) Uani d U P D 0.453(5) A 2
Nb Nb1 0.20361(2) 0.43388(2) 0.19315(2) 0.01592(6) Uani d . . . 1.0 . .
O O1 0.12599(17) 0.50311(12) 0.12205(17) 0.0257(5) Uani d . . . 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cs1 O1 5_565 3.141(2) ?
Cs1 N3 7 3.145(3) ?
Cs1 N13'_b . 3.159(16) ?
Cs1 N10 6_565 3.251(3) ?
Cs1 N13_a . 3.297(13) ?
Cs1 N3 8_455 3.319(3) ?
Cs1 N12 2 3.343(3) ?
Cs1 N6 7 3.408(3) ?
Cs1 O1 . 3.448(2) ?
Cs1 N4 . 3.589(3) ?
Cs1 N7 6_565 3.691(3) ?
Cs1 N11 2 3.695(2) ?
Cs2 N7 . 3.213(3) ?
Cs2 N12 4 3.216(3) ?
Cs2 N9 2_655 3.232(3) ?
Cs2 N6 5_665 3.268(3) ?
Cs2 N12 6_565 3.305(3) ?
Cs2 N15_a 4 3.329(6) ?
Cs2 N4 . 3.442(3) ?
Cs2 N1 6_565 3.519(3) ?
Cs2 O1 . 3.539(2) ?
Cs2 N3 4 3.549(3) ?
Cs2 N9 6_565 3.554(3) ?
Cs2 N15_a 3 3.568(6) ?
N1 N2 . 1.179(3) ?
N1 Nb1 . 2.302(2) ?
N1 Cs2 6_566 3.519(3) ?
N2 N3 . 1.161(3) ?
N2 Cs2 6_566 3.772(2) ?
N3 Cs1 7 3.145(3) ?
N3 Cs1 8_556 3.319(3) ?
N3 Cs2 4_545 3.549(3) ?
N4 N5 . 1.216(4) ?
N4 Nb1 . 2.095(2) ?
N5 N6 . 1.145(4) ?
N6 Cs2 5_665 3.268(3) ?
N6 Cs1 7 3.408(3) ?
N7 N8 . 1.211(3) ?
N7 Nb1 . 2.079(2) ?
N7 Cs1 6_566 3.691(3) ?
N8 N9 . 1.139(4) ?
N8 Cs2 6_566 3.845(2) ?
N9 Cs2 2_655 3.232(3) ?
N9 Cs2 6_566 3.554(3) ?
N10 N11 . 1.198(3) ?
N10 Nb1 . 2.118(3) ?
N10 Cs1 6_566 3.251(3) ?
N11 N12 . 1.149(3) ?
N11 Cs2 6_566 3.574(2) ?
N11 Cs1 2 3.695(2) ?
N12 Cs2 4_545 3.216(3) ?
N12 Cs2 6_566 3.305(3) ?
N12 Cs1 2 3.343(3) ?
N13_a N14_a . 1.159(9) ?
N13_a Nb1 . 2.116(12) ?
N14_a N15_a . 1.155(7) ?
N15_a Cs2 4_545 3.329(6) ?
N15_a Cs2 3_445 3.568(6) ?
N13'_b N14'_b . 1.150(11) ?
N13'_b Nb1 . 2.076(15) ?
N14'_b N15'_b . 1.149(9) ?
N15'_b Cs2 4_545 3.660(8) ?
N15'_b Cs1 7 3.757(9) ?
Nb1 O1 . 1.732(2) ?
Nb1 Cs1 6_566 4.3364(4) ?
O1 Cs1 5_565 3.141(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cs1 N3 5_565 7 115.38(7) ?
O1 Cs1 N13'_b 5_565 . 115.4(3) ?
N3 Cs1 N13'_b 7 . 123.9(3) ?
O1 Cs1 N10 5_565 6_565 62.89(6) ?
N3 Cs1 N10 7 6_565 101.56(7) ?
N13'_b Cs1 N10 . 6_565 121.8(3) ?
O1 Cs1 N13_a 5_565 . 110.9(2) ?
N3 Cs1 N13_a 7 . 127.0(2) ?
N10 Cs1 N13_a 6_565 . 122.1(2) ?
O1 Cs1 N3 5_565 8_455 66.74(7) ?
N3 Cs1 N3 7 8_455 69.18(11) ?
N13'_b Cs1 N3 . 8_455 112.2(3) ?
N10 Cs1 N3 6_565 8_455 117.20(7) ?
N13_a Cs1 N3 . 8_455 109.1(2) ?
O1 Cs1 N12 5_565 2 68.92(6) ?
N3 Cs1 N12 7 2 120.26(8) ?
N13'_b Cs1 N12 . 2 61.0(3) ?
N10 Cs1 N12 6_565 2 126.12(7) ?
N13_a Cs1 N12 . 2 56.6(2) ?
N3 Cs1 N12 8_455 2 58.56(7) ?
O1 Cs1 N6 5_565 7 121.90(6) ?
N3 Cs1 N6 7 7 69.17(7) ?
N13'_b Cs1 N6 . 7 64.8(3) ?
N10 Cs1 N6 6_565 7 170.58(7) ?
N13_a Cs1 N6 . 7 65.2(2) ?
N3 Cs1 N6 8_455 7 61.96(7) ?
N12 Cs1 N6 2 7 62.29(7) ?
O1 Cs1 O1 5_565 . 82.64(5) ?
N3 Cs1 O1 7 . 156.13(7) ?
N13'_b Cs1 O1 . . 51.7(3) ?
N10 Cs1 O1 6_565 . 71.76(6) ?
N13_a Cs1 O1 . . 50.9(2) ?
N3 Cs1 O1 8_455 . 134.53(7) ?
N12 Cs1 O1 2 . 79.82(6) ?
N6 Cs1 O1 7 . 115.97(6) ?
O1 Cs1 N4 5_565 . 127.23(6) ?
N3 Cs1 N4 7 . 111.27(7) ?
N13'_b Cs1 N4 . . 47.7(3) ?
N10 Cs1 N4 6_565 . 85.18(6) ?
N13_a Cs1 N4 . . 51.5(2) ?
N3 Cs1 N4 8_455 . 157.42(7) ?
N12 Cs1 N4 2 . 106.88(6) ?
N6 Cs1 N4 7 . 96.50(7) ?
O1 Cs1 N4 . . 46.40(5) ?
O1 Cs1 N7 5_565 6_565 110.24(5) ?
N3 Cs1 N7 7 6_565 67.39(7) ?
N13'_b Cs1 N7 . 6_565 114.0(3) ?
N10 Cs1 N7 6_565 6_565 49.99(6) ?
N13_a Cs1 N7 . 6_565 118.2(2) ?
N3 Cs1 N7 8_455 6_565 128.78(7) ?
N12 Cs1 N7 2 6_565 172.15(6) ?
N6 Cs1 N7 7 6_565 122.27(6) ?
O1 Cs1 N7 . 6_565 92.33(5) ?
N4 Cs1 N7 . 6_565 67.07(5) ?
O1 Cs1 N11 5_565 2 63.60(5) ?
N3 Cs1 N11 7 2 138.14(7) ?
N13'_b Cs1 N11 . 2 56.0(3) ?
N10 Cs1 N11 6_565 2 112.02(6) ?
N13_a Cs1 N11 . 2 51.1(2) ?
N3 Cs1 N11 8_455 2 73.50(7) ?
N12 Cs1 N11 2 2 17.91(6) ?
N6 Cs1 N11 7 2 77.08(6) ?
O1 Cs1 N11 . 2 62.75(5) ?
N4 Cs1 N11 . 2 96.17(6) ?
N7 Cs1 N11 6_565 2 154.47(6) ?
N7 Cs2 N12 . 4 126.09(6) ?
N7 Cs2 N9 . 2_655 69.50(7) ?
N12 Cs2 N9 4 2_655 118.27(7) ?
N7 Cs2 N6 . 5_665 135.26(7) ?
N12 Cs2 N6 4 5_665 65.17(7) ?
N9 Cs2 N6 2_655 5_665 68.44(7) ?
N7 Cs2 N12 . 6_565 108.59(7) ?
N12 Cs2 N12 4 6_565 80.92(8) ?
N9 Cs2 N12 2_655 6_565 158.33(7) ?
N6 Cs2 N12 5_665 6_565 116.13(7) ?
N7 Cs2 N15_a . 4 62.55(13) ?
N12 Cs2 N15_a 4 4 67.44(12) ?
N9 Cs2 N15_a 2_655 4 77.92(12) ?
N6 Cs2 N15_a 5_665 4 94.12(15) ?
N12 Cs2 N15_a 6_565 4 121.24(12) ?
N7 Cs2 N4 . . 53.84(6) ?
N12 Cs2 N4 4 . 179.49(7) ?
N9 Cs2 N4 2_655 . 61.22(7) ?
N6 Cs2 N4 5_665 . 114.48(6) ?
N12 Cs2 N4 6_565 . 99.58(7) ?
N15_a Cs2 N4 4 . 112.30(11) ?
N7 Cs2 N1 . 6_565 149.39(6) ?
N12 Cs2 N1 4 6_565 81.46(6) ?
N9 Cs2 N1 2_655 6_565 111.94(7) ?
N6 Cs2 N1 5_665 6_565 64.24(7) ?
N12 Cs2 N1 6_565 6_565 58.17(6) ?
N15_a Cs2 N1 4 6_565 147.84(12) ?
N4 Cs2 N1 . 6_565 98.74(6) ?
N7 Cs2 O1 . . 49.08(5) ?
N12 Cs2 O1 4 . 133.61(6) ?
N9 Cs2 O1 2_655 . 102.74(6) ?
N6 Cs2 O1 5_665 . 158.02(6) ?
N12 Cs2 O1 6_565 . 64.79(6) ?
N15_a Cs2 O1 4 . 103.85(14) ?
N4 Cs2 O1 . . 46.82(5) ?
N1 Cs2 O1 6_565 . 103.49(5) ?
N7 Cs2 N3 . 4 68.57(7) ?
N12 Cs2 N3 4 4 75.22(7) ?
N9 Cs2 N3 2_655 4 134.52(7) ?
N6 Cs2 N3 5_665 4 140.33(7) ?
N12 Cs2 N3 6_565 4 56.63(7) ?
N15_a Cs2 N3 4 4 67.78(14) ?
N4 Cs2 N3 . 4 105.11(6) ?
N1 Cs2 N3 6_565 4 113.03(7) ?
O1 Cs2 N3 . 4 60.23(6) ?
N7 Cs2 N9 . 6_565 107.03(6) ?
N12 Cs2 N9 4 6_565 122.44(7) ?
N9 Cs2 N9 2_655 6_565 58.63(8) ?
N6 Cs2 N9 5_665 6_565 61.72(7) ?
N12 Cs2 N9 6_565 6_565 103.53(6) ?
N15_a Cs2 N9 4 6_565 135.19(12) ?
N4 Cs2 N9 . 6_565 57.39(6) ?
N1 Cs2 N9 6_565 6_565 56.87(6) ?
O1 Cs2 N9 . 6_565 96.37(6) ?
N3 Cs2 N9 4 6_565 153.34(7) ?
N7 Cs2 N15_a . 3 85.30(11) ?
N12 Cs2 N15_a 4 3 63.56(11) ?
N9 Cs2 N15_a 2_655 3 58.88(11) ?
N6 Cs2 N15_a 5_665 3 60.17(13) ?
N12 Cs2 N15_a 6_565 3 142.63(11) ?
N15_a Cs2 N15_a 4 3 35.2(3) ?
N4 Cs2 N15_a . 3 115.96(11) ?
N1 Cs2 N15_a 6_565 3 122.56(12) ?
O1 Cs2 N15_a . 3 133.80(11) ?
N3 Cs2 N15_a 4 3 100.77(13) ?
N9 Cs2 N15_a 6_565 3 105.11(13) ?
N2 N1 Nb1 . . 140.8(2) ?
N2 N1 Cs2 . 6_566 93.14(17) ?
Nb1 N1 Cs2 . 6_566 119.28(9) ?
N3 N2 N1 . . 178.1(3) ?
N3 N2 Cs2 . 6_566 109.5(2) ?
N1 N2 Cs2 . 6_566 68.67(16) ?
N2 N3 Cs1 . 7 119.6(2) ?
N2 N3 Cs1 . 8_556 135.0(2) ?
Cs1 N3 Cs1 7 8_556 82.58(7) ?
N2 N3 Cs2 . 4_545 101.7(2) ?
Cs1 N3 Cs2 7 4_545 114.68(9) ?
Cs1 N3 Cs2 8_556 4_545 102.69(7) ?
N5 N4 Nb1 . . 126.0(2) ?
N5 N4 Cs2 . . 126.5(2) ?
Nb1 N4 Cs2 . . 90.20(8) ?
N5 N4 Cs1 . . 114.7(2) ?
Nb1 N4 Cs1 . . 87.32(8) ?
Cs2 N4 Cs1 . . 103.64(7) ?
N6 N5 N4 . . 177.5(3) ?
N5 N6 Cs2 . 5_665 116.9(2) ?
N5 N6 Cs1 . 7 127.9(2) ?
Cs2 N6 Cs1 5_665 7 114.03(8) ?
N8 N7 Nb1 . . 130.6(2) ?
N8 N7 Cs2 . . 112.24(19) ?
Nb1 N7 Cs2 . . 97.05(8) ?
N8 N7 Cs1 . 6_566 111.87(18) ?
Nb1 N7 Cs1 . 6_566 93.20(8) ?
Cs2 N7 Cs1 . 6_566 109.35(7) ?
N9 N8 N7 . . 177.5(3) ?
N9 N8 Cs2 . . 127.3(2) ?
N7 N8 Cs2 . . 50.79(16) ?
N9 N8 Cs2 . 6_566 66.83(19) ?
N7 N8 Cs2 . 6_566 115.22(18) ?
Cs2 N8 Cs2 . 6_566 165.26(7) ?
N8 N9 Cs2 . 2_655 136.9(2) ?
N8 N9 Cs2 . 6_566 96.0(2) ?
Cs2 N9 Cs2 2_655 6_566 121.37(8) ?
N11 N10 Nb1 . . 124.4(2) ?
N11 N10 Cs1 . 6_566 122.58(19) ?
Nb1 N10 Cs1 . 6_566 105.81(9) ?
N12 N11 N10 . . 177.9(3) ?
N12 N11 Cs2 . 6_566 67.28(18) ?
N10 N11 Cs2 . 6_566 112.66(19) ?
N12 N11 Cs1 . 2 63.44(18) ?
N10 N11 Cs1 . 2 114.61(18) ?
Cs2 N11 Cs1 6_566 2 95.14(6) ?
N11 N12 Cs2 . 4_545 135.2(2) ?
N11 N12 Cs2 . 6_566 94.01(19) ?
Cs2 N12 Cs2 4_545 6_566 99.08(8) ?
N11 N12 Cs1 . 2 98.7(2) ?
Cs2 N12 Cs1 4_545 2 117.28(8) ?
Cs2 N12 Cs1 6_566 2 107.64(8) ?
N14_a N13_a Nb1 . . 139.1(11) ?
N14_a N13_a Cs1 . . 124.5(9) ?
Nb1 N13_a Cs1 . . 95.0(3) ?
N15_a N14_a N13_a . . 169.0(9) ?
N14_a N15_a Cs2 . 4_545 122.5(5) ?
N14_a N15_a Cs2 . 3_445 113.4(5) ?
Cs2 N15_a Cs2 4_545 3_445 123.37(18) ?
N14'_b N13'_b Nb1 . . 135.3(13) ?
N14'_b N13'_b Cs1 . . 121.6(12) ?
Nb1 N13'_b Cs1 . . 100.0(4) ?
N15'_b N14'_b N13'_b . . 172.7(12) ?
N14'_b N15'_b Cs2 . 4_545 114.7(6) ?
N14'_b N15'_b Cs1 . 7 114.2(6) ?
Cs2 N15'_b Cs1 4_545 7 99.01(18) ?
O1 Nb1 N13'_b . . 98.3(4) ?
O1 Nb1 N7 . . 95.01(10) ?
N13'_b Nb1 N7 . . 166.0(4) ?
O1 Nb1 N4 . . 92.47(10) ?
N13'_b Nb1 N4 . . 82.7(4) ?
N7 Nb1 N4 . . 92.70(10) ?
O1 Nb1 N13_a . . 97.3(3) ?
N7 Nb1 N13_a . . 167.0(3) ?
N4 Nb1 N13_a . . 90.9(3) ?
O1 Nb1 N10 . . 98.69(10) ?
N13'_b Nb1 N10 . . 92.3(4) ?
N7 Nb1 N10 . . 89.71(10) ?
N4 Nb1 N10 . . 168.34(10) ?
N13_a Nb1 N10 . . 84.3(3) ?
O1 Nb1 N1 . . 176.80(10) ?
N13'_b Nb1 N1 . . 84.6(4) ?
N7 Nb1 N1 . . 82.00(9) ?
N4 Nb1 N1 . . 86.53(10) ?
N13_a Nb1 N1 . . 85.8(3) ?
N10 Nb1 N1 . . 82.50(9) ?
O1 Nb1 Cs1 . 6_566 70.21(7) ?
N13'_b Nb1 Cs1 . 6_566 130.9(4) ?
N7 Nb1 Cs1 . 6_566 58.20(7) ?
N4 Nb1 Cs1 . 6_566 142.99(7) ?
N13_a Nb1 Cs1 . 6_566 122.7(3) ?
N10 Nb1 Cs1 . 6_566 46.16(7) ?
N1 Nb1 Cs1 . 6_566 108.92(6) ?
Nb1 O1 Cs1 . 5_565 150.45(11) ?
Nb1 O1 Cs1 . . 98.06(8) ?
Cs1 O1 Cs1 5_565 . 97.36(5) ?
Nb1 O1 Cs2 . . 93.55(8) ?
Cs1 O1 Cs2 5_565 . 106.72(6) ?
Cs1 O1 Cs2 . . 104.57(6) ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
_chemical_properties_physical    'Moisture-sensitive, Heat-sensitive, explosive'
