# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_2a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H86 N10 Nb2 O'
_chemical_formula_weight         981.07

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.279(13)
_cell_length_b                   17.841(17)
_cell_length_c                   22.19(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.390(18)
_cell_angle_gamma                90.00
_cell_volume                     5257(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    583
_cell_measurement_theta_min      2.283
_cell_measurement_theta_max      13.676

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2088
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5715
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43828
_diffrn_reflns_av_R_equivalents  0.2755
_diffrn_reflns_av_sigmaI/netI    0.3828
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         29.31
_reflns_number_total             13348
_reflns_number_gt                3932
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0531P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13348
_refine_ls_number_parameters     576
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.2973
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.2760
_refine_ls_wR_factor_gt          0.1742
_refine_ls_goodness_of_fit_ref   0.849
_refine_ls_restrained_S_all      0.849
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.002

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.12450(7) 0.60625(5) 0.30624(4) 0.0421(3) Uani 1 1 d . . .
Nb2 Nb 0.33688(7) 0.55485(5) 0.20003(4) 0.0441(3) Uani 1 1 d . . .
O1 O 0.2151(4) 0.5931(3) 0.2382(3) 0.0441(16) Uani 1 1 d . . .
N1 N 0.1764(5) 0.5522(4) 0.3661(3) 0.043(2) Uani 1 1 d . . .
N2 N -0.0338(6) 0.6112(5) 0.3411(4) 0.051(2) Uani 1 1 d . . .
N3 N 0.0019(6) 0.5495(4) 0.2579(4) 0.052(2) Uani 1 1 d . . .
N4 N -0.1642(6) 0.5385(4) 0.2930(4) 0.061(2) Uani 1 1 d . . .
N5 N 0.1424(6) 0.7133(4) 0.3265(4) 0.049(2) Uani 1 1 d . . .
N1A N 0.3019(6) 0.4954(4) 0.1392(4) 0.050(2) Uani 1 1 d . . .
N2A N 0.3764(6) 0.6680(4) 0.1675(4) 0.054(2) Uani 1 1 d . . .
N3A N 0.4951(6) 0.5823(4) 0.1724(4) 0.048(2) Uani 1 1 d . . .
N4A N 0.5431(7) 0.7029(5) 0.1362(4) 0.062(3) Uani 1 1 d . . .
N5A N 0.3885(6) 0.4920(4) 0.2666(4) 0.052(2) Uani 1 1 d . . .
C1 C 0.2129(7) 0.4971(5) 0.4048(4) 0.043(2) Uani 1 1 d . . .
C2 C 0.2856(7) 0.5162(5) 0.4500(5) 0.048(3) Uani 1 1 d . . .
C3 C 0.3240(8) 0.4612(6) 0.4859(5) 0.060(3) Uani 1 1 d . . .
H3 H 0.3709 0.4742 0.5154 0.072 Uiso 1 1 calc R . .
C4 C 0.2966(9) 0.3879(6) 0.4804(5) 0.067(3) Uani 1 1 d . . .
H4 H 0.3262 0.3513 0.5046 0.081 Uiso 1 1 calc R . .
C5 C 0.2242(9) 0.3692(6) 0.4383(5) 0.058(3) Uani 1 1 d . . .
H5 H 0.2036 0.3196 0.4351 0.070 Uiso 1 1 calc R . .
C6 C 0.1816(8) 0.4220(5) 0.4008(5) 0.048(3) Uani 1 1 d . . .
C7 C 0.3113(8) 0.5991(6) 0.4592(5) 0.059(3) Uani 1 1 d . . .
H7 H 0.2924 0.6264 0.4225 0.071 Uiso 1 1 calc R . .
C8 C 0.4237(9) 0.6115(7) 0.4710(6) 0.095(4) Uani 1 1 d . . .
H8A H 0.4377 0.6643 0.4715 0.114 Uiso 1 1 calc R . .
H8B H 0.4621 0.5880 0.4398 0.114 Uiso 1 1 calc R . .
H8C H 0.4419 0.5901 0.5093 0.114 Uiso 1 1 calc R . .
C9 C 0.2494(11) 0.6301(6) 0.5114(6) 0.102(5) Uani 1 1 d . . .
H9A H 0.2747 0.6102 0.5487 0.123 Uiso 1 1 calc R . .
H9B H 0.1801 0.6158 0.5063 0.123 Uiso 1 1 calc R . .
H9C H 0.2544 0.6838 0.5119 0.123 Uiso 1 1 calc R . .
C10 C 0.0993(7) 0.4000(5) 0.3570(5) 0.053(3) Uani 1 1 d . . .
H10 H 0.0603 0.4453 0.3479 0.063 Uiso 1 1 calc R . .
C11 C 0.0263(9) 0.3424(6) 0.3826(6) 0.089(4) Uani 1 1 d . . .
H11A H 0.0604 0.2954 0.3880 0.106 Uiso 1 1 calc R . .
H11B H -0.0293 0.3359 0.3553 0.106 Uiso 1 1 calc R . .
H11C H 0.0018 0.3596 0.4208 0.106 Uiso 1 1 calc R . .
C12 C 0.1445(9) 0.3729(7) 0.2981(5) 0.085(4) Uani 1 1 d . . .
H12A H 0.1833 0.4125 0.2804 0.102 Uiso 1 1 calc R . .
H12B H 0.0914 0.3585 0.2709 0.102 Uiso 1 1 calc R . .
H12C H 0.1873 0.3306 0.3058 0.102 Uiso 1 1 calc R . .
C13 C -0.0691(7) 0.5674(5) 0.2987(5) 0.048(3) Uani 1 1 d . . .
C14 C -0.0772(9) 0.6161(6) 0.4009(5) 0.065(3) Uani 1 1 d . . .
H14 H -0.1494 0.6260 0.3960 0.078 Uiso 1 1 calc R . .
C15 C -0.0659(9) 0.5427(6) 0.4350(5) 0.088(4) Uani 1 1 d . . .
H15A H -0.1053 0.5045 0.4155 0.106 Uiso 1 1 calc R . .
H15B H -0.0888 0.5491 0.4756 0.106 Uiso 1 1 calc R . .
H15 H 0.0037 0.5280 0.4356 0.106 Uiso 1 1 calc R . .
C16 C -0.0328(9) 0.6803(7) 0.4336(5) 0.087(4) Uani 1 1 d . . .
H16A H 0.0361 0.6693 0.4437 0.104 Uiso 1 1 calc R . .
H16B H -0.0700 0.6892 0.4698 0.104 Uiso 1 1 calc R . .
H16C H -0.0355 0.7241 0.4085 0.104 Uiso 1 1 calc R . .
C17 C -0.0261(9) 0.5400(6) 0.1941(5) 0.064(3) Uani 1 1 d . . .
H17 H -0.0963 0.5231 0.1934 0.077 Uiso 1 1 calc R . .
C18 C 0.0352(9) 0.4786(6) 0.1650(5) 0.078(4) Uani 1 1 d . . .
H18A H 0.1055 0.4902 0.1688 0.094 Uiso 1 1 calc R . .
H18B H 0.0173 0.4749 0.1231 0.094 Uiso 1 1 calc R . .
H18C H 0.0216 0.4318 0.1846 0.094 Uiso 1 1 calc R . .
C19 C -0.0237(11) 0.6128(7) 0.1615(5) 0.106(5) Uani 1 1 d . . .
H19A H -0.0609 0.6496 0.1837 0.127 Uiso 1 1 calc R . .
H19B H -0.0533 0.6068 0.1222 0.127 Uiso 1 1 calc R . .
H19C H 0.0449 0.6291 0.1575 0.127 Uiso 1 1 calc R . .
C20 C -0.1808(10) 0.4596(6) 0.2797(6) 0.101(5) Uani 1 1 d . . .
H20A H -0.1172 0.4341 0.2783 0.122 Uiso 1 1 calc R . .
H20B H -0.2144 0.4549 0.2415 0.122 Uiso 1 1 calc R . .
H20C H -0.2217 0.4378 0.3106 0.122 Uiso 1 1 calc R . .
C21 C -0.2530(8) 0.5798(7) 0.3123(6) 0.096(5) Uani 1 1 d . . .
H21A H -0.2756 0.5604 0.3502 0.115 Uiso 1 1 calc R . .
H21B H -0.3056 0.5742 0.2827 0.115 Uiso 1 1 calc R . .
H21C H -0.2364 0.6319 0.3166 0.115 Uiso 1 1 calc R . .
C22 C 0.0763(9) 0.7590(6) 0.2905(5) 0.070(3) Uani 1 1 d . . .
H22A H 0.0250 0.7801 0.3156 0.084 Uiso 1 1 calc R . .
H22B H 0.0454 0.7287 0.2597 0.084 Uiso 1 1 calc R . .
H22C H 0.1142 0.7986 0.2721 0.084 Uiso 1 1 calc R . .
C23 C 0.1921(9) 0.7576(6) 0.3719(5) 0.079(4) Uani 1 1 d . . .
H23A H 0.2296 0.7971 0.3529 0.095 Uiso 1 1 calc R . .
H23B H 0.2372 0.7264 0.3947 0.095 Uiso 1 1 calc R . .
H23C H 0.1428 0.7790 0.3982 0.095 Uiso 1 1 calc R . .
C1A C 0.2684(7) 0.4592(6) 0.0871(5) 0.051(3) Uani 1 1 d . . .
C2A C 0.2853(9) 0.3810(6) 0.0810(5) 0.059(3) Uani 1 1 d . B .
C3A C 0.2469(8) 0.3466(6) 0.0297(6) 0.069(3) Uani 1 1 d . . .
H3A H 0.2558 0.2951 0.0258 0.082 Uiso 1 1 calc R . .
C4A C 0.1973(10) 0.3829(7) -0.0151(6) 0.088(4) Uani 1 1 d . . .
H4A H 0.1732 0.3572 -0.0487 0.105 Uiso 1 1 calc R . .
C5A C 0.1837(8) 0.4588(7) -0.0094(5) 0.069(3) Uani 1 1 d . . .
H5A H 0.1505 0.4848 -0.0399 0.082 Uiso 1 1 calc R . .
C6A C 0.2183(8) 0.4976(6) 0.0408(5) 0.057(3) Uani 1 1 d . . .
C7A C 0.3374(11) 0.3374(7) 0.1289(6) 0.082(4) Uani 1 1 d D . .
H7A H 0.3619 0.3760 0.1567 0.098 Uiso 1 1 calc R A 1
C8A C 0.264(4) 0.292(5) 0.167(3) 0.13(3) Uani 0.50 1 d PD B 1
H8A1 H 0.2345 0.2530 0.1428 0.158 Uiso 0.50 1 calc PR B 1
H8A2 H 0.2126 0.3240 0.1822 0.158 Uiso 0.50 1 calc PR B 1
H8A3 H 0.3002 0.2694 0.2003 0.158 Uiso 0.50 1 calc PR B 1
C9A C 0.433(3) 0.300(4) 0.107(3) 0.13(2) Uani 0.50 1 d PD B 1
H9A1 H 0.4650 0.2739 0.1395 0.157 Uiso 0.50 1 calc PR B 1
H9A2 H 0.4785 0.3381 0.0919 0.157 Uiso 0.50 1 calc PR B 1
H9A3 H 0.4173 0.2658 0.0750 0.157 Uiso 0.50 1 calc PR B 1
C8B C 0.260(5) 0.286(4) 0.158(3) 0.18(4) Uani 0.50 1 d PD B 2
H8B1 H 0.2564 0.2395 0.1358 0.212 Uiso 0.50 1 calc PR B 2
H8B2 H 0.1957 0.3095 0.1582 0.212 Uiso 0.50 1 calc PR B 2
H8B3 H 0.2808 0.2751 0.1989 0.212 Uiso 0.50 1 calc PR B 2
C9B C 0.409(3) 0.282(4) 0.100(3) 0.16(4) Uani 0.50 1 d PD B 3
H9B1 H 0.3891 0.2320 0.1099 0.198 Uiso 0.50 1 calc PR B 3
H9B2 H 0.4763 0.2909 0.1151 0.198 Uiso 0.50 1 calc PR B 3
H9B3 H 0.4082 0.2886 0.0572 0.198 Uiso 0.50 1 calc PR B 3
C10A C 0.2018(9) 0.5833(6) 0.0441(5) 0.066(3) Uani 1 1 d . . .
H10A H 0.1990 0.5971 0.0868 0.080 Uiso 1 1 calc R . .
C11A C 0.1052(9) 0.6109(7) 0.0144(6) 0.093(4) Uani 1 1 d . . .
H11D H 0.1104 0.6059 -0.0286 0.112 Uiso 1 1 calc R . .
H11E H 0.0947 0.6627 0.0245 0.112 Uiso 1 1 calc R . .
H11F H 0.0494 0.5817 0.0284 0.112 Uiso 1 1 calc R . .
C12A C 0.2941(9) 0.6237(6) 0.0165(6) 0.085(4) Uani 1 1 d . . .
H12D H 0.2908 0.6204 -0.0266 0.103 Uiso 1 1 calc R . .
H12E H 0.3549 0.6004 0.0307 0.103 Uiso 1 1 calc R . .
H12F H 0.2938 0.6755 0.0284 0.103 Uiso 1 1 calc R . .
C13A C 0.4733(8) 0.6520(6) 0.1583(5) 0.052(3) Uani 1 1 d . . .
C14A C 0.3433(9) 0.7448(6) 0.1808(6) 0.067(3) Uani 1 1 d . . .
H14A H 0.3847 0.7792 0.1570 0.080 Uiso 1 1 calc R . .
C15A C 0.3592(9) 0.7629(6) 0.2458(5) 0.084(4) Uani 1 1 d . . .
H15D H 0.3226 0.7279 0.2701 0.100 Uiso 1 1 calc R . .
H15E H 0.3355 0.8128 0.2537 0.100 Uiso 1 1 calc R . .
H15F H 0.4296 0.7598 0.2555 0.100 Uiso 1 1 calc R . .
C16A C 0.2347(9) 0.7543(6) 0.1605(5) 0.081(4) Uani 1 1 d . . .
H16D H 0.2298 0.7461 0.1179 0.097 Uiso 1 1 calc R . .
H16E H 0.2125 0.8041 0.1698 0.097 Uiso 1 1 calc R . .
H16F H 0.1932 0.7186 0.1811 0.097 Uiso 1 1 calc R . .
C17A C 0.5724(8) 0.5385(6) 0.1410(6) 0.067(3) Uani 1 1 d . . .
H17A H 0.6363 0.5657 0.1449 0.080 Uiso 1 1 calc R . .
C18A C 0.5857(9) 0.4631(5) 0.1712(6) 0.078(4) Uani 1 1 d . . .
H18D H 0.6029 0.4704 0.2129 0.093 Uiso 1 1 calc R . .
H18E H 0.6386 0.4359 0.1516 0.093 Uiso 1 1 calc R . .
H18F H 0.5241 0.4353 0.1682 0.093 Uiso 1 1 calc R . .
C19A C 0.5483(10) 0.5319(8) 0.0750(6) 0.097(5) Uani 1 1 d . . .
H19D H 0.4888 0.5020 0.0697 0.117 Uiso 1 1 calc R . .
H19E H 0.6036 0.5084 0.0547 0.117 Uiso 1 1 calc R . .
H19F H 0.5372 0.5809 0.0584 0.117 Uiso 1 1 calc R . .
C20A C 0.6460(8) 0.7030(6) 0.1569(6) 0.090(4) Uani 1 1 d . . .
H20D H 0.6516 0.6734 0.1929 0.108 Uiso 1 1 calc R . .
H20E H 0.6667 0.7535 0.1654 0.108 Uiso 1 1 calc R . .
H20F H 0.6884 0.6822 0.1263 0.108 Uiso 1 1 calc R . .
C21A C 0.5215(9) 0.7497(6) 0.0854(5) 0.085(4) Uani 1 1 d . . .
H21D H 0.4521 0.7439 0.0740 0.102 Uiso 1 1 calc R . .
H21E H 0.5637 0.7355 0.0524 0.102 Uiso 1 1 calc R . .
H21F H 0.5343 0.8010 0.0959 0.102 Uiso 1 1 calc R . .
C22A C 0.4053(8) 0.4141(5) 0.2835(5) 0.068(3) Uani 1 1 d . . .
H22D H 0.4759 0.4058 0.2900 0.082 Uiso 1 1 calc R . .
H22E H 0.3815 0.3820 0.2518 0.082 Uiso 1 1 calc R . .
H22F H 0.3694 0.4033 0.3199 0.082 Uiso 1 1 calc R . .
C23A C 0.4315(8) 0.5429(6) 0.3107(5) 0.070(3) Uani 1 1 d . . .
H23D H 0.4031 0.5328 0.3496 0.084 Uiso 1 1 calc R . .
H23E H 0.4166 0.5937 0.2993 0.084 Uiso 1 1 calc R . .
H23F H 0.5031 0.5361 0.3125 0.084 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 N1 1.776(8) . ?
Nb1 O1 1.952(6) . ?
Nb1 N5 1.977(8) . ?
Nb1 N3 2.191(8) . ?
Nb1 N2 2.246(8) . ?
Nb1 C13 2.667(10) . ?
Nb2 N1A 1.776(8) . ?
Nb2 O1 1.953(6) . ?
Nb2 N5A 1.974(8) . ?
Nb2 N2A 2.209(8) . ?
Nb2 N3A 2.247(8) . ?
N1 C1 1.391(11) . ?
N2 C13 1.308(12) . ?
N2 C14 1.453(12) . ?
N3 C13 1.349(12) . ?
N3 C17 1.472(13) . ?
N4 C13 1.369(12) . ?
N4 C20 1.454(13) . ?
N4 C21 1.457(12) . ?
N5 C23 1.437(12) . ?
N5 C22 1.436(12) . ?
N1A C1A 1.394(12) . ?
N2A C13A 1.335(11) . ?
N2A C14A 1.469(12) . ?
N3A C13A 1.313(12) . ?
N3A C17A 1.469(12) . ?
N4A C13A 1.390(12) . ?
N4A C21A 1.429(13) . ?
N4A C20A 1.439(13) . ?
N5A C23A 1.449(12) . ?
N5A C22A 1.456(11) . ?
C1 C6 1.405(13) . ?
C1 C2 1.428(13) . ?
C2 C3 1.361(13) . ?
C2 C7 1.530(13) . ?
C3 C4 1.363(14) . ?
C4 C5 1.377(15) . ?
C5 C6 1.376(13) . ?
C6 C10 1.509(13) . ?
C7 C9 1.529(14) . ?
C7 C8 1.531(14) . ?
C10 C11 1.525(13) . ?
C10 C12 1.522(14) . ?
C14 C16 1.476(14) . ?
C14 C15 1.521(14) . ?
C17 C19 1.487(14) . ?
C17 C18 1.512(14) . ?
C1A C2A 1.421(13) . ?
C1A C6A 1.399(14) . ?
C2A C3A 1.387(14) . ?
C2A C7A 1.484(15) . ?
C3A C4A 1.353(15) . ?
C4A C5A 1.372(15) . ?
C5A C6A 1.387(14) . ?
C6A C10A 1.546(14) . ?
C7A C9B 1.52(2) . ?
C7A C9A 1.52(2) . ?
C7A C8B 1.53(2) . ?
C7A C8A 1.53(2) . ?
C10A C12A 1.552(15) . ?
C10A C11A 1.521(15) . ?
C14A C15A 1.494(14) . ?
C14A C16A 1.516(14) . ?
C17A C19A 1.502(15) . ?
C17A C18A 1.512(14) . ?

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 Nb1 O1 106.0(3) . . ?
N1 Nb1 N5 108.0(3) . . ?
O1 Nb1 N5 102.6(3) . . ?
N1 Nb1 N3 113.4(3) . . ?
O1 Nb1 N3 91.5(3) . . ?
N5 Nb1 N3 130.2(3) . . ?
N1 Nb1 N2 97.0(3) . . ?
O1 Nb1 N2 148.7(3) . . ?
N5 Nb1 N2 89.7(3) . . ?
N3 Nb1 N2 59.5(3) . . ?
N1 Nb1 C13 105.9(3) . . ?
O1 Nb1 C13 121.3(3) . . ?
N5 Nb1 C13 112.3(3) . . ?
N3 Nb1 C13 30.3(3) . . ?
N2 Nb1 C13 29.3(3) . . ?
N1A Nb2 O1 109.0(3) . . ?
N1A Nb2 N5A 108.6(3) . . ?
O1 Nb2 N5A 99.1(3) . . ?
N1A Nb2 N2A 111.0(3) . . ?
O1 Nb2 N2A 91.2(3) . . ?
N5A Nb2 N2A 132.9(3) . . ?
N1A Nb2 N3A 99.4(3) . . ?
O1 Nb2 N3A 145.2(3) . . ?
N5A Nb2 N3A 90.4(3) . . ?
N2A Nb2 N3A 59.1(3) . . ?
Nb2 O1 Nb1 153.4(3) . . ?
C1 N1 Nb1 167.8(7) . . ?
C13 N2 C14 123.4(9) . . ?
C13 N2 Nb1 93.5(6) . . ?
C14 N2 Nb1 134.0(7) . . ?
C13 N3 C17 120.0(9) . . ?
C13 N3 Nb1 94.8(6) . . ?
C17 N3 Nb1 134.9(7) . . ?
C13 N4 C20 121.4(9) . . ?
C13 N4 C21 122.1(9) . . ?
C20 N4 C21 115.3(9) . . ?
C23 N5 C22 110.8(8) . . ?
C23 N5 Nb1 138.1(7) . . ?
C22 N5 Nb1 110.4(7) . . ?
C1A N1A Nb2 170.8(7) . . ?
C13A N2A C14A 121.4(9) . . ?
C13A N2A Nb2 94.9(6) . . ?
C14A N2A Nb2 135.6(6) . . ?
C13A N3A C17A 122.9(9) . . ?
C13A N3A Nb2 93.8(6) . . ?
C17A N3A Nb2 132.2(6) . . ?
C13A N4A C21A 122.0(10) . . ?
C13A N4A C20A 121.5(9) . . ?
C21A N4A C20A 115.8(9) . . ?
C23A N5A C22A 111.5(8) . . ?
C23A N5A Nb2 106.4(6) . . ?
C22A N5A Nb2 141.8(7) . . ?
C6 C1 N1 122.2(9) . . ?
C6 C1 C2 118.1(9) . . ?
N1 C1 C2 119.8(9) . . ?
C3 C2 C1 119.2(9) . . ?
C3 C2 C7 122.4(9) . . ?
C1 C2 C7 118.2(9) . . ?
C4 C3 C2 122.7(11) . . ?
C3 C4 C5 118.5(10) . . ?
C4 C5 C6 121.8(10) . . ?
C5 C6 C1 119.6(10) . . ?
C5 C6 C10 120.3(9) . . ?
C1 C6 C10 120.1(9) . . ?
C9 C7 C2 109.3(9) . . ?
C9 C7 C8 110.2(9) . . ?
C2 C7 C8 112.3(9) . . ?
C6 C10 C11 113.2(9) . . ?
C6 C10 C12 110.4(8) . . ?
C11 C10 C12 111.2(9) . . ?
N2 C13 N4 128.1(10) . . ?
N2 C13 N3 112.0(9) . . ?
N4 C13 N3 119.9(10) . . ?
N2 C13 Nb1 57.2(5) . . ?
N4 C13 Nb1 172.7(7) . . ?
N3 C13 Nb1 55.0(5) . . ?
C16 C14 N2 109.6(9) . . ?
C16 C14 C15 112.7(11) . . ?
N2 C14 C15 111.3(9) . . ?
C19 C17 N3 111.2(9) . . ?
C19 C17 C18 114.3(10) . . ?
N3 C17 C18 111.2(9) . . ?
C2A C1A N1A 119.0(9) . . ?
C2A C1A C6A 119.1(10) . . ?
N1A C1A C6A 121.9(9) . . ?
C3A C2A C1A 117.1(11) . . ?
C3A C2A C7A 121.5(10) . . ?
C1A C2A C7A 121.3(10) . . ?
C4A C3A C2A 124.4(11) . . ?
C3A C4A C5A 117.9(12) . . ?
C4A C5A C6A 121.6(12) . . ?
C5A C6A C1A 119.9(10) . . ?
C5A C6A C10A 119.1(10) . . ?
C1A C6A C10A 121.0(10) . . ?
C9B C7A C2A 109(3) . . ?
C9B C7A C9A 18(4) . . ?
C2A C7A C9A 113(4) . . ?
C9B C7A C8B 102(5) . . ?
C2A C7A C8B 108(3) . . ?
C9A C7A C8B 116(5) . . ?
C9B C7A C8A 107(5) . . ?
C2A C7A C8A 112(2) . . ?
C9A C7A C8A 119(5) . . ?
C8B C7A C8A 9(6) . . ?
C12A C10A C6A 109.2(9) . . ?
C12A C10A C11A 110.1(9) . . ?
C6A C10A C11A 114.8(10) . . ?
N3A C13A N2A 112.2(9) . . ?
N3A C13A N4A 123.8(9) . . ?
N2A C13A N4A 124.0(9) . . ?
N2A C14A C15A 110.8(10) . . ?
N2A C14A C16A 109.3(9) . . ?
C15A C14A C16A 112.9(10) . . ?
N3A C17A C19A 111.0(10) . . ?
N3A C17A C18A 110.1(9) . . ?
C19A C17A C18A 112.6(10) . . ?

_diffrn_measured_fraction_theta_max 0.927
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 1009639'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H49 N6 Nb'
_chemical_formula_weight         526.61

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   22.658(5)
_cell_length_b                   9.5025(17)
_cell_length_c                   17.340(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.288(11)
_cell_angle_gamma                90.00
_cell_volume                     2930.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    1818
_cell_measurement_theta_min      2.2904
_cell_measurement_theta_max      23.1121

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6546
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26779
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_av_sigmaI/netI    0.1310
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         30.62
_reflns_number_total             8896
_reflns_number_gt                4572
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0378P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0061(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8896
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1206
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.943
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.049533(16) 0.36025(3) 0.36092(2) 0.03303(10) Uani 1 1 d . . .
N1 N 0.13144(14) 0.4581(3) 0.40577(18) 0.0371(6) Uani 1 1 d . . .
N2 N 0.04505(15) 0.1859(3) 0.27055(19) 0.0393(7) Uani 1 1 d . . .
N3 N -0.02970(15) 0.3670(3) 0.2019(2) 0.0485(7) Uani 1 1 d . . .
N4 N -0.05571(19) 0.1745(3) 0.0970(2) 0.0644(10) Uani 1 1 d . . .
N5 N 0.06956(17) 0.2249(3) 0.4611(2) 0.0492(8) Uani 1 1 d . . .
N6 N -0.01027(17) 0.5088(3) 0.3668(2) 0.0503(8) Uani 1 1 d . . .
C1 C 0.18500(17) 0.5552(3) 0.4238(2) 0.0362(8) Uani 1 1 d . . .
C2 C 0.22772(19) 0.6311(3) 0.5127(2) 0.0449(8) Uani 1 1 d . . .
C3 C 0.2805(2) 0.7267(4) 0.5280(3) 0.0579(11) Uani 1 1 d . . .
H3 H 0.3092 0.7777 0.5863 0.070 Uiso 1 1 calc R . .
C4 C 0.2913(2) 0.7477(4) 0.4598(3) 0.0605(11) Uani 1 1 d . . .
H4 H 0.3271 0.8121 0.4720 0.073 Uiso 1 1 calc R . .
C5 C 0.2494(2) 0.6739(4) 0.3730(3) 0.0561(10) Uani 1 1 d . . .
H5 H 0.2574 0.6886 0.3270 0.067 Uiso 1 1 calc R . .
C6 C 0.19527(18) 0.5777(3) 0.3528(3) 0.0405(8) Uani 1 1 d . . .
C7 C 0.2166(2) 0.6123(4) 0.5887(3) 0.0567(11) Uani 1 1 d . . .
H7 H 0.1710 0.5560 0.5591 0.068 Uiso 1 1 calc R . .
C8 C 0.2056(3) 0.7506(5) 0.6219(4) 0.0949(17) Uani 1 1 d . . .
H8A H 0.2492 0.8087 0.6503 0.142 Uiso 1 1 calc R . .
H8B H 0.1982 0.7327 0.6699 0.142 Uiso 1 1 calc R . .
H8C H 0.1622 0.7980 0.5664 0.142 Uiso 1 1 calc R . .
C9 C 0.2822(3) 0.5304(5) 0.6773(3) 0.1020(18) Uani 1 1 d . . .
H9A H 0.2857 0.4394 0.6562 0.153 Uiso 1 1 calc R . .
H9B H 0.2740 0.5193 0.7250 0.153 Uiso 1 1 calc R . .
H9C H 0.3282 0.5812 0.7061 0.153 Uiso 1 1 calc R . .
C10 C 0.1443(2) 0.5055(4) 0.2539(3) 0.0518(10) Uani 1 1 d . . .
H10 H 0.1253 0.4194 0.2627 0.062 Uiso 1 1 calc R . .
C11 C 0.0767(3) 0.5994(4) 0.1812(3) 0.0735(13) Uani 1 1 d . . .
H11A H 0.0491 0.6172 0.2055 0.110 Uiso 1 1 calc R . .
H11B H 0.0446 0.5529 0.1187 0.110 Uiso 1 1 calc R . .
H11C H 0.0938 0.6869 0.1738 0.110 Uiso 1 1 calc R . .
C12 C 0.1844(3) 0.4632(5) 0.2128(4) 0.0964(18) Uani 1 1 d . . .
H12A H 0.2024 0.5459 0.2015 0.145 Uiso 1 1 calc R . .
H12B H 0.1500 0.4138 0.1519 0.145 Uiso 1 1 calc R . .
H12C H 0.2260 0.4030 0.2589 0.145 Uiso 1 1 calc R . .
C13 C -0.01457(19) 0.2389(4) 0.1868(2) 0.0427(8) Uani 1 1 d . . .
C14 C 0.0987(2) 0.0788(4) 0.2860(3) 0.0505(9) Uani 1 1 d . . .
C15 C 0.1756(2) 0.1263(4) 0.3748(3) 0.0815(15) Uani 1 1 d . . .
H15A H 0.1885 0.2128 0.3600 0.122 Uiso 1 1 calc R . .
H15B H 0.2121 0.0556 0.3918 0.122 Uiso 1 1 calc R . .
H15C H 0.1749 0.1407 0.4291 0.122 Uiso 1 1 calc R . .
C16 C 0.1000(3) 0.0636(5) 0.2000(3) 0.0781(13) Uani 1 1 d . . .
H16A H 0.0527 0.0262 0.1444 0.117 Uiso 1 1 calc R . .
H16B H 0.1398 0.0009 0.2176 0.117 Uiso 1 1 calc R . .
H16C H 0.1081 0.1541 0.1834 0.117 Uiso 1 1 calc R . .
C17 C 0.0828(3) -0.0629(4) 0.3120(4) 0.0847(15) Uani 1 1 d . . .
H17A H 0.0880 -0.0531 0.3711 0.127 Uiso 1 1 calc R . .
H17B H 0.1180 -0.1318 0.3220 0.127 Uiso 1 1 calc R . .
H17C H 0.0326 -0.0925 0.2593 0.127 Uiso 1 1 calc R . .
C18 C -0.1046(2) 0.4306(5) 0.1386(3) 0.0781(14) Uani 1 1 d . . .
H18A H -0.1181 0.4464 0.0741 0.094 Uiso 1 1 calc R . .
H18B H -0.1025 0.5217 0.1655 0.094 Uiso 1 1 calc R . .
C19 C -0.1656(3) 0.3441(6) 0.1268(4) 0.1068(19) Uani 1 1 d . . .
H19A H -0.1726 0.2585 0.0926 0.160 Uiso 1 1 calc R . .
H19B H -0.2116 0.3967 0.0900 0.160 Uiso 1 1 calc R . .
H19C H -0.1512 0.3220 0.1904 0.160 Uiso 1 1 calc R . .
C20 C -0.0842(3) 0.2502(6) 0.0085(3) 0.114(2) Uani 1 1 d . . .
H20A H -0.0567 0.3365 0.0248 0.171 Uiso 1 1 calc R . .
H20B H -0.1365 0.2710 -0.0260 0.171 Uiso 1 1 calc R . .
H20C H -0.0785 0.1939 -0.0324 0.171 Uiso 1 1 calc R . .
C21 C -0.0858(3) 0.0345(5) 0.0823(3) 0.0888(16) Uani 1 1 d . . .
H21A H -0.0637 -0.0273 0.0627 0.133 Uiso 1 1 calc R . .
H21B H -0.1394 0.0367 0.0319 0.133 Uiso 1 1 calc R . .
H21C H -0.0744 0.0010 0.1424 0.133 Uiso 1 1 calc R . .
C22 C 0.1339(3) 0.1962(5) 0.5620(3) 0.0776(14) Uani 1 1 d . . .
H22A H 0.1183 0.1941 0.6023 0.116 Uiso 1 1 calc R . .
H22B H 0.1709 0.2687 0.5850 0.116 Uiso 1 1 calc R . .
H22C H 0.1552 0.1069 0.5655 0.116 Uiso 1 1 calc R . .
C23 C 0.0084(3) 0.1258(4) 0.4242(3) 0.0757(13) Uani 1 1 d . . .
H23A H 0.0272 0.0314 0.4357 0.113 Uiso 1 1 calc R . .
H23B H -0.0298 0.1402 0.3549 0.113 Uiso 1 1 calc R . .
H23C H -0.0127 0.1405 0.4575 0.113 Uiso 1 1 calc R . .
C24 C -0.0030(3) 0.6589(4) 0.3608(3) 0.0766(14) Uani 1 1 d . . .
H24A H -0.0491 0.6955 0.3028 0.115 Uiso 1 1 calc R . .
H24B H 0.0373 0.6769 0.3580 0.115 Uiso 1 1 calc R . .
H24C H 0.0076 0.7040 0.4178 0.115 Uiso 1 1 calc R . .
C25 C -0.0721(2) 0.4795(4) 0.3689(3) 0.0762(13) Uani 1 1 d . . .
H25A H -0.0644 0.5293 0.4227 0.114 Uiso 1 1 calc R . .
H25B H -0.0743 0.3802 0.3772 0.114 Uiso 1 1 calc R . .
H25C H -0.1185 0.5096 0.3083 0.114 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 N1 1.768(3) . ?
Nb1 N5 1.975(3) . ?
Nb1 N6 2.002(3) . ?
Nb1 N3 2.167(3) . ?
Nb1 N2 2.239(3) . ?
Nb1 C13 2.669(3) . ?
N1 C1 1.397(4) . ?
N2 C13 1.325(4) . ?
N2 C14 1.477(4) . ?
N3 C13 1.334(4) . ?
N3 C18 1.464(4) . ?
N4 C13 1.367(4) . ?
N4 C20 1.436(5) . ?
N4 C21 1.444(5) . ?
N5 C22 1.449(4) . ?
N5 C23 1.456(5) . ?
N6 C24 1.447(4) . ?
N6 C25 1.452(5) . ?
C1 C6 1.404(5) . ?
C1 C2 1.408(4) . ?
C2 C3 1.391(5) . ?
C2 C7 1.498(5) . ?
C3 C4 1.362(5) . ?
C4 C5 1.374(5) . ?
C5 C6 1.390(5) . ?
C6 C10 1.513(5) . ?
C7 C8 1.517(5) . ?
C7 C9 1.531(6) . ?
C10 C12 1.515(5) . ?
C10 C11 1.530(5) . ?
C14 C15 1.512(5) . ?
C14 C16 1.517(5) . ?
C14 C17 1.531(5) . ?
C18 C19 1.509(7) . ?

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 Nb1 N5 110.43(12) . . ?
N1 Nb1 N6 99.55(12) . . ?
N5 Nb1 N6 102.03(13) . . ?
N1 Nb1 N3 111.13(12) . . ?
N5 Nb1 N3 134.12(12) . . ?
N6 Nb1 N3 89.46(12) . . ?
N1 Nb1 N2 106.08(11) . . ?
N5 Nb1 N2 91.15(11) . . ?
N6 Nb1 N2 144.92(11) . . ?
N3 Nb1 N2 59.24(10) . . ?
N1 Nb1 C13 114.33(11) . . ?
N5 Nb1 C13 112.41(11) . . ?
N6 Nb1 C13 116.81(12) . . ?
N3 Nb1 C13 29.78(10) . . ?
N2 Nb1 C13 29.71(10) . . ?
C1 N1 Nb1 167.3(2) . . ?
C13 N2 C14 128.7(3) . . ?
C13 N2 Nb1 93.4(2) . . ?
C14 N2 Nb1 135.0(2) . . ?
C13 N3 C18 123.3(3) . . ?
C13 N3 Nb1 96.4(2) . . ?
C18 N3 Nb1 128.9(3) . . ?
C13 N4 C20 122.0(3) . . ?
C13 N4 C21 121.9(3) . . ?
C20 N4 C21 115.0(3) . . ?
C22 N5 C23 112.4(3) . . ?
C22 N5 Nb1 134.0(3) . . ?
C23 N5 Nb1 113.4(2) . . ?
C24 N6 C25 110.2(3) . . ?
C24 N6 Nb1 125.5(3) . . ?
C25 N6 Nb1 124.1(2) . . ?
N1 C1 C6 119.8(3) . . ?
N1 C1 C2 119.8(3) . . ?
C6 C1 C2 120.4(3) . . ?
C3 C2 C1 118.0(3) . . ?
C3 C2 C7 120.3(3) . . ?
C1 C2 C7 121.7(3) . . ?
C4 C3 C2 121.7(4) . . ?
C3 C4 C5 120.2(4) . . ?
C4 C5 C6 120.9(4) . . ?
C5 C6 C1 118.7(3) . . ?
C5 C6 C10 121.1(3) . . ?
C1 C6 C10 120.0(3) . . ?
C2 C7 C8 112.8(3) . . ?
C2 C7 C9 110.8(4) . . ?
C8 C7 C9 110.2(4) . . ?
C6 C10 C12 113.3(4) . . ?
C6 C10 C11 109.9(3) . . ?
C12 C10 C11 110.7(4) . . ?
N2 C13 N3 110.0(3) . . ?
N2 C13 N4 126.2(3) . . ?
N3 C13 N4 123.7(3) . . ?
N2 C13 Nb1 56.86(17) . . ?
N3 C13 Nb1 53.80(16) . . ?
N4 C13 Nb1 172.3(3) . . ?
N2 C14 C15 106.1(3) . . ?
N2 C14 C16 113.7(3) . . ?
C15 C14 C16 108.6(4) . . ?
N2 C14 C17 110.0(3) . . ?
C15 C14 C17 107.2(3) . . ?
C16 C14 C17 110.9(3) . . ?
N3 C18 C19 114.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        30.62
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.086
_database_code_depnum_ccdc_archive 'CCDC 1009640'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_10

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H51 N6 Nb S2'
_chemical_formula_weight         616.77

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.1088(4)
_cell_length_b                   16.4664(6)
_cell_length_c                   18.0246(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.968(2)
_cell_angle_gamma                90.00
_cell_volume                     3295.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    1617
_cell_measurement_theta_min      2.4738
_cell_measurement_theta_max      18.9690

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27687
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_sigmaI/netI    0.1346
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         30.57
_reflns_number_total             10101
_reflns_number_gt                4106
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0960P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10101
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1862
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.2198
_refine_ls_wR_factor_gt          0.1580
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.69543(4) 0.91200(3) 0.80979(2) 0.05259(18) Uani 1 1 d . . .
S1 S 0.56111(13) 0.96451(12) 0.70389(8) 0.0822(5) Uani 1 1 d . . .
S2 S 0.47213(14) 0.96059(11) 0.85376(8) 0.0777(5) Uani 1 1 d . . .
N1 N 0.8171(3) 0.8803(3) 0.7548(2) 0.0510(10) Uani 1 1 d . . .
N2 N 0.7035(4) 0.8371(3) 0.9087(2) 0.0536(10) Uani 1 1 d . . .
N3 N 0.6005(3) 0.7920(3) 0.8122(2) 0.0548(10) Uani 1 1 d . . .
N4 N 0.5961(4) 0.7134(3) 0.9236(3) 0.0712(13) Uani 1 1 d . . .
H4A H 0.6515 0.6835 0.9440 0.085 Uiso 1 1 calc R . .
N5 N 0.3305(4) 0.9863(3) 0.7345(3) 0.0695(13) Uani 1 1 d . . .
N6 N 0.7774(5) 1.0123(3) 0.8511(3) 0.0735(13) Uani 1 1 d . . .
C1 C 0.9127(4) 0.8549(3) 0.7124(3) 0.0495(12) Uani 1 1 d . . .
C2 C 0.9226(4) 0.8806(3) 0.6385(3) 0.0536(12) Uani 1 1 d . . .
C3 C 1.0187(5) 0.8538(4) 0.5992(3) 0.0729(16) Uani 1 1 d . . .
H3 H 1.0257 0.8699 0.5501 0.087 Uiso 1 1 calc R . .
C4 C 1.1047(6) 0.8038(4) 0.6312(4) 0.090(2) Uani 1 1 d . . .
H4 H 1.1701 0.7874 0.6040 0.108 Uiso 1 1 calc R . .
C5 C 1.0945(5) 0.7775(4) 0.7037(4) 0.0766(18) Uani 1 1 d . . .
H5 H 1.1521 0.7424 0.7242 0.092 Uiso 1 1 calc R . .
C6 C 1.0002(4) 0.8028(3) 0.7460(3) 0.0623(14) Uani 1 1 d . . .
C7 C 0.8299(5) 0.9371(3) 0.6037(3) 0.0562(13) Uani 1 1 d . . .
H7 H 0.7519 0.9230 0.6240 0.067 Uiso 1 1 calc R . .
C8 C 0.8571(7) 1.0231(4) 0.6260(4) 0.105(2) Uani 1 1 d . . .
H8A H 0.8650 1.0265 0.6791 0.157 Uiso 1 1 calc R . .
H8B H 0.7927 1.0578 0.6086 0.157 Uiso 1 1 calc R . .
H8C H 0.9310 1.0400 0.6046 0.157 Uiso 1 1 calc R . .
C9 C 0.8158(6) 0.9322(5) 0.5206(4) 0.101(2) Uani 1 1 d . . .
H9A H 0.8848 0.9560 0.4985 0.151 Uiso 1 1 calc R . .
H9B H 0.7446 0.9610 0.5043 0.151 Uiso 1 1 calc R . .
H9C H 0.8090 0.8763 0.5058 0.151 Uiso 1 1 calc R . .
C10 C 0.9878(5) 0.7737(4) 0.8243(3) 0.0685(15) Uani 1 1 d . . .
H10 H 0.9420 0.8150 0.8504 0.082 Uiso 1 1 calc R . .
C11 C 1.1059(5) 0.7619(5) 0.8675(4) 0.099(2) Uani 1 1 d . . .
H11A H 1.1564 0.7256 0.8408 0.148 Uiso 1 1 calc R . .
H11B H 1.0905 0.7392 0.9153 0.148 Uiso 1 1 calc R . .
H11C H 1.1457 0.8133 0.8737 0.148 Uiso 1 1 calc R . .
C12 C 0.9169(6) 0.6953(4) 0.8272(4) 0.099(2) Uani 1 1 d . . .
H12A H 0.8373 0.7040 0.8063 0.148 Uiso 1 1 calc R . .
H12B H 0.9118 0.6781 0.8779 0.148 Uiso 1 1 calc R . .
H12C H 0.9566 0.6542 0.7993 0.148 Uiso 1 1 calc R . .
C13 C 0.6298(4) 0.7791(3) 0.8819(3) 0.0524(12) Uani 1 1 d . . .
C14 C 0.7360(5) 0.8466(4) 0.9886(3) 0.0705(16) Uani 1 1 d . . .
H14 H 0.7078 0.7970 1.0124 0.085 Uiso 1 1 calc R . .
C15 C 0.8654(8) 0.8478(9) 1.0024(5) 0.203(6) Uani 1 1 d . . .
H15A H 0.8974 0.8983 0.9852 0.304 Uiso 1 1 calc R . .
H15B H 0.9014 0.8037 0.9763 0.304 Uiso 1 1 calc R . .
H15C H 0.8829 0.8423 1.0546 0.304 Uiso 1 1 calc R . .
C16 C 0.6708(12) 0.9102(6) 1.0203(4) 0.194(6) Uani 1 1 d . . .
H16A H 0.6644 0.9007 1.0725 0.291 Uiso 1 1 calc R . .
H16B H 0.5917 0.9127 0.9972 0.291 Uiso 1 1 calc R . .
H16C H 0.7119 0.9607 1.0127 0.291 Uiso 1 1 calc R . .
C17 C 0.5459(5) 0.7313(4) 0.7632(3) 0.0735(16) Uani 1 1 d . . .
H17 H 0.5469 0.6787 0.7887 0.088 Uiso 1 1 calc R . .
C18 C 0.6179(6) 0.7243(5) 0.6930(4) 0.097(2) Uani 1 1 d . . .
H18A H 0.6164 0.7754 0.6674 0.146 Uiso 1 1 calc R . .
H18B H 0.5829 0.6831 0.6614 0.146 Uiso 1 1 calc R . .
H18C H 0.6997 0.7100 0.7061 0.146 Uiso 1 1 calc R . .
C19 C 0.4162(5) 0.7533(6) 0.7416(4) 0.114(3) Uani 1 1 d . . .
H19A H 0.3716 0.7618 0.7856 0.170 Uiso 1 1 calc R . .
H19B H 0.3801 0.7099 0.7131 0.170 Uiso 1 1 calc R . .
H19C H 0.4151 0.8021 0.7124 0.170 Uiso 1 1 calc R . .
C20 C 0.4685(5) 0.6922(5) 0.9348(4) 0.087(2) Uani 1 1 d . . .
H20 H 0.4297 0.6803 0.8864 0.105 Uiso 1 1 calc R . .
C21 C 0.4662(7) 0.6160(5) 0.9823(5) 0.110(3) Uani 1 1 d . . .
H21A H 0.5089 0.5733 0.9582 0.165 Uiso 1 1 calc R . .
H21B H 0.3843 0.5996 0.9886 0.165 Uiso 1 1 calc R . .
H21C H 0.5040 0.6269 1.0299 0.165 Uiso 1 1 calc R . .
C22 C 0.4023(6) 0.7586(5) 0.9700(5) 0.110(3) Uani 1 1 d . . .
H22A H 0.4439 0.7743 1.0153 0.165 Uiso 1 1 calc R . .
H22B H 0.3226 0.7404 0.9808 0.165 Uiso 1 1 calc R . .
H22C H 0.3972 0.8042 0.9369 0.165 Uiso 1 1 calc R . .
C23 C 0.4410(5) 0.9728(4) 0.7616(3) 0.0662(15) Uani 1 1 d . . .
C24 C 0.2263(5) 0.9911(4) 0.7806(3) 0.0798(18) Uani 1 1 d . . .
H24A H 0.2490 0.9757 0.8305 0.120 Uiso 1 1 calc R . .
H24B H 0.1647 0.9550 0.7615 0.120 Uiso 1 1 calc R . .
H24C H 0.1961 1.0457 0.7803 0.120 Uiso 1 1 calc R . .
C25 C 0.3071(5) 0.9992(4) 0.6554(4) 0.086(2) Uani 1 1 d . . .
H25A H 0.3298 1.0535 0.6425 0.129 Uiso 1 1 calc R . .
H25B H 0.2228 0.9915 0.6438 0.129 Uiso 1 1 calc R . .
H25C H 0.3531 0.9611 0.6277 0.129 Uiso 1 1 calc R . .
C26 C 0.7245(8) 1.0766(4) 0.8980(4) 0.108(3) Uani 1 1 d . . .
H26A H 0.7624 1.0752 0.9467 0.162 Uiso 1 1 calc R . .
H26B H 0.6396 1.0671 0.9018 0.162 Uiso 1 1 calc R . .
H26C H 0.7372 1.1288 0.8760 0.162 Uiso 1 1 calc R . .
C27 C 0.9072(6) 1.0312(5) 0.8431(4) 0.107(2) Uani 1 1 d . . .
H27A H 0.9151 1.0830 0.8193 0.160 Uiso 1 1 calc R . .
H27B H 0.9435 0.9900 0.8135 0.160 Uiso 1 1 calc R . .
H27C H 0.9467 1.0328 0.8913 0.160 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 N1 1.781(4) . ?
Nb1 N6 2.016(5) . ?
Nb1 N2 2.168(4) . ?
Nb1 N3 2.241(4) . ?
Nb1 S1 2.5342(14) . ?
Nb1 C13 2.659(5) . ?
Nb1 S2 2.7490(14) . ?
S1 C23 1.725(5) . ?
S2 C23 1.697(6) . ?
N1 C1 1.394(6) . ?
N2 C13 1.337(6) . ?
N2 C14 1.480(6) . ?
N3 C13 1.303(6) . ?
N3 C17 1.453(6) . ?
N4 C13 1.377(6) . ?
N4 C20 1.481(7) . ?
N5 C23 1.325(7) . ?
N5 C24 1.451(6) . ?
N5 C25 1.456(7) . ?
N6 C27 1.487(8) . ?
N6 C26 1.488(8) . ?
C1 C2 1.404(7) . ?
C1 C6 1.417(7) . ?
C2 C3 1.375(7) . ?
C2 C7 1.509(7) . ?
C3 C4 1.373(8) . ?
C4 C5 1.385(9) . ?
C5 C6 1.380(7) . ?
C6 C10 1.501(8) . ?
C7 C8 1.499(8) . ?
C7 C9 1.504(8) . ?
C10 C12 1.513(8) . ?
C10 C11 1.515(8) . ?
C14 C16 1.406(9) . ?
C14 C15 1.450(9) . ?
C17 C18 1.523(8) . ?
C17 C19 1.524(8) . ?
C20 C22 1.473(10) . ?
C20 C21 1.519(9) . ?

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 Nb1 N6 96.0(2) . . ?
N1 Nb1 N2 106.25(16) . . ?
N6 Nb1 N2 99.05(18) . . ?
N1 Nb1 N3 96.82(17) . . ?
N6 Nb1 N3 157.24(17) . . ?
N2 Nb1 N3 59.23(15) . . ?
N1 Nb1 S1 96.87(13) . . ?
N6 Nb1 S1 104.18(15) . . ?
N2 Nb1 S1 145.14(12) . . ?
N3 Nb1 S1 92.88(11) . . ?
N1 Nb1 C13 104.85(16) . . ?
N6 Nb1 C13 128.45(18) . . ?
N2 Nb1 C13 30.03(14) . . ?
N3 Nb1 C13 29.29(14) . . ?
S1 Nb1 C13 118.98(12) . . ?
N1 Nb1 S2 162.77(13) . . ?
N6 Nb1 S2 93.18(15) . . ?
N2 Nb1 S2 86.60(11) . . ?
N3 Nb1 S2 79.69(11) . . ?
S1 Nb1 S2 66.67(5) . . ?
C13 Nb1 S2 80.41(10) . . ?
C23 S1 Nb1 91.15(19) . . ?
C23 S2 Nb1 84.70(17) . . ?
C1 N1 Nb1 179.5(4) . . ?
C13 N2 C14 123.6(4) . . ?
C13 N2 Nb1 95.8(3) . . ?
C14 N2 Nb1 137.9(4) . . ?
C13 N3 C17 124.0(5) . . ?
C13 N3 Nb1 93.4(3) . . ?
C17 N3 Nb1 141.4(4) . . ?
C13 N4 C20 122.6(5) . . ?
C23 N5 C24 123.0(5) . . ?
C23 N5 C25 121.2(5) . . ?
C24 N5 C25 115.7(5) . . ?
C27 N6 C26 108.1(6) . . ?
C27 N6 Nb1 124.2(4) . . ?
C26 N6 Nb1 127.6(5) . . ?
N1 C1 C2 121.1(4) . . ?
N1 C1 C6 118.1(4) . . ?
C2 C1 C6 120.8(4) . . ?
C3 C2 C1 118.7(5) . . ?
C3 C2 C7 121.0(5) . . ?
C1 C2 C7 120.3(4) . . ?
C4 C3 C2 121.1(6) . . ?
C3 C4 C5 120.4(6) . . ?
C6 C5 C4 121.0(6) . . ?
C5 C6 C1 118.0(5) . . ?
C5 C6 C10 121.2(5) . . ?
C1 C6 C10 120.8(5) . . ?
C8 C7 C9 109.4(5) . . ?
C8 C7 C2 110.1(5) . . ?
C9 C7 C2 115.3(5) . . ?
C6 C10 C12 111.7(5) . . ?
C6 C10 C11 114.7(5) . . ?
C12 C10 C11 108.4(5) . . ?
N3 C13 N2 111.3(5) . . ?
N3 C13 N4 126.2(5) . . ?
N2 C13 N4 122.5(5) . . ?
N3 C13 Nb1 57.3(3) . . ?
N2 C13 Nb1 54.2(2) . . ?
N4 C13 Nb1 176.1(4) . . ?
C16 C14 C15 116.2(8) . . ?
C16 C14 N2 111.3(5) . . ?
C15 C14 N2 112.0(5) . . ?
N3 C17 C18 109.7(5) . . ?
N3 C17 C19 111.3(5) . . ?
C18 C17 C19 108.9(5) . . ?
C22 C20 N4 112.2(6) . . ?
C22 C20 C21 110.6(6) . . ?
N4 C20 C21 107.9(6) . . ?
N5 C23 S2 122.4(4) . . ?
N5 C23 S1 121.1(4) . . ?
S2 C23 S1 116.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.242


# eof===================================================end
_database_code_depnum_ccdc_archive 'CCDC 1009641'
