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

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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_(1)
_chemical_name_common            'Complex 2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H106 B F20 N6 Nb2, C2 H4 Cl2'
_chemical_formula_sum            'C98 H110 B Cl2 F20 N6 Nb2'
_chemical_formula_weight         2019.45

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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                   14.224(3)
_cell_length_b                   21.737(3)
_cell_length_c                   31.247(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.83(1)
_cell_angle_gamma                90.00
_cell_volume                     9660.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    9568
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      25.38

_exptl_crystal_description       rode
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4164
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8508
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      80(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  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            79928
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.14
_diffrn_reflns_theta_max         25.40
_reflns_number_total             17729
_reflns_number_gt                14369
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0660P)²+29.5334P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17729
_refine_ls_number_parameters     1188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1422
_refine_ls_wR_factor_gt          0.1321
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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
C1 C -0.1464(3) 0.2181(2) 0.33567(12) 0.0289(9) Uani 1 1 d . . .
H1A H -0.1702 0.2382 0.3096 0.043 Uiso 1 1 calc R . .
H1B H -0.1738 0.2378 0.3608 0.043 Uiso 1 1 calc R . .
H1C H -0.1637 0.1745 0.3351 0.043 Uiso 1 1 calc R . .
C2 C -0.0403(2) 0.22407(17) 0.33792(12) 0.0210(8) Uani 1 1 d . . .
C3 C 0.0004(3) 0.21776(18) 0.37887(11) 0.0214(8) Uani 1 1 d . . .
H3 H -0.0420 0.2222 0.4019 0.026 Uiso 1 1 calc R . .
C4 C 0.0941(3) 0.20592(17) 0.39097(11) 0.0193(7) Uani 1 1 d . . .
C5 C 0.1092(3) 0.1859(2) 0.43678(12) 0.0289(9) Uani 1 1 d . . .
H5A H 0.0818 0.1449 0.4408 0.043 Uiso 1 1 calc R . .
H5B H 0.0788 0.2152 0.4559 0.043 Uiso 1 1 calc R . .
H5C H 0.1767 0.1844 0.4433 0.043 Uiso 1 1 calc R . .
C6 C 0.2560(2) 0.18351(17) 0.37708(11) 0.0180(7) Uani 1 1 d . . .
C7 C 0.2716(3) 0.12093(18) 0.36828(11) 0.0222(8) Uani 1 1 d . . .
C8 C 0.3589(3) 0.0954(2) 0.37889(12) 0.0280(9) Uani 1 1 d . . .
H8 H 0.3706 0.0534 0.3725 0.034 Uiso 1 1 calc R . .
C9 C 0.4289(3) 0.1303(2) 0.39852(13) 0.0302(9) Uani 1 1 d . . .
H9 H 0.4880 0.1122 0.4055 0.036 Uiso 1 1 calc R . .
C10 C 0.4121(3) 0.1911(2) 0.40788(12) 0.0268(9) Uani 1 1 d . . .
H10 H 0.4600 0.2148 0.4215 0.032 Uiso 1 1 calc R . .
C11 C 0.3262(2) 0.21861(18) 0.39776(11) 0.0213(8) Uani 1 1 d . . .
C12 C 0.3108(3) 0.28513(19) 0.41139(13) 0.0280(9) Uani 1 1 d . . .
H12 H 0.2483 0.2989 0.3999 0.034 Uiso 1 1 calc R . .
C13 C 0.3099(3) 0.2906(2) 0.46030(14) 0.0442(12) Uani 1 1 d . . .
H13A H 0.2606 0.2641 0.4717 0.066 Uiso 1 1 calc R . .
H13B H 0.2975 0.3334 0.4683 0.066 Uiso 1 1 calc R . .
H13C H 0.3711 0.2780 0.4721 0.066 Uiso 1 1 calc R . .
C14 C 0.3869(3) 0.3285(2) 0.39407(13) 0.0353(10) Uani 1 1 d . . .
H14A H 0.4484 0.3168 0.4061 0.053 Uiso 1 1 calc R . .
H14B H 0.3725 0.3710 0.4023 0.053 Uiso 1 1 calc R . .
H14C H 0.3884 0.3255 0.3628 0.053 Uiso 1 1 calc R . .
C15 C 0.1961(3) 0.07911(18) 0.34891(14) 0.0296(9) Uani 1 1 d . . .
H15 H 0.1435 0.1056 0.3380 0.035 Uiso 1 1 calc R . .
C16 C 0.2328(3) 0.0411(2) 0.31131(14) 0.0369(10) Uani 1 1 d . . .
H16A H 0.2519 0.0688 0.2883 0.055 Uiso 1 1 calc R . .
H16B H 0.1829 0.0137 0.3008 0.055 Uiso 1 1 calc R . .
H16C H 0.2869 0.0166 0.3209 0.055 Uiso 1 1 calc R . .
C17 C 0.1568(4) 0.0357(2) 0.38306(16) 0.0470(12) Uani 1 1 d . . .
H17A H 0.2069 0.0084 0.3935 0.070 Uiso 1 1 calc R . .
H17B H 0.1057 0.0111 0.3705 0.070 Uiso 1 1 calc R . .
H17C H 0.1327 0.0600 0.4069 0.070 Uiso 1 1 calc R . .
C18 C -0.0409(2) 0.22603(17) 0.26180(11) 0.0180(7) Uani 1 1 d . . .
C19 C -0.0857(2) 0.27627(18) 0.24177(11) 0.0210(8) Uani 1 1 d . . .
C20 C -0.1362(3) 0.26547(19) 0.20387(12) 0.0258(9) Uani 1 1 d . . .
H20 H -0.1656 0.2991 0.1896 0.031 Uiso 1 1 calc R . .
C21 C -0.1444(3) 0.2077(2) 0.18668(12) 0.0264(9) Uani 1 1 d . . .
H21 H -0.1817 0.2014 0.1616 0.032 Uiso 1 1 calc R . .
C22 C -0.0985(3) 0.15888(19) 0.20581(12) 0.0241(8) Uani 1 1 d . . .
H22 H -0.1037 0.1190 0.1935 0.029 Uiso 1 1 calc R . .
C23 C -0.0443(2) 0.16736(17) 0.24323(11) 0.0200(8) Uani 1 1 d . . .
C24 C 0.0095(3) 0.11268(18) 0.26224(12) 0.0257(8) Uani 1 1 d . . .
H24 H 0.0622 0.1295 0.2803 0.031 Uiso 1 1 calc R . .
C25 C -0.0517(4) 0.0735(2) 0.29111(17) 0.0503(13) Uani 1 1 d . . .
H25A H -0.0730 0.0984 0.3153 0.075 Uiso 1 1 calc R . .
H25B H -0.0151 0.0385 0.3019 0.075 Uiso 1 1 calc R . .
H25C H -0.1064 0.0585 0.2748 0.075 Uiso 1 1 calc R . .
C26 C 0.0530(3) 0.07193(19) 0.22778(13) 0.0320(9) Uani 1 1 d . . .
H26A H 0.0029 0.0513 0.2114 0.048 Uiso 1 1 calc R . .
H26B H 0.0937 0.0410 0.2414 0.048 Uiso 1 1 calc R . .
H26C H 0.0903 0.0974 0.2085 0.048 Uiso 1 1 calc R . .
C27 C -0.0839(3) 0.34120(19) 0.25963(12) 0.0271(9) Uani 1 1 d . . .
H27 H -0.0413 0.3414 0.2854 0.032 Uiso 1 1 calc R . .
C28 C -0.0460(3) 0.3882(2) 0.22768(14) 0.0331(9) Uani 1 1 d . . .
H28A H 0.0177 0.3764 0.2194 0.050 Uiso 1 1 calc R . .
H28B H -0.0444 0.4290 0.2410 0.050 Uiso 1 1 calc R . .
H28C H -0.0870 0.3892 0.2022 0.050 Uiso 1 1 calc R . .
C29 C -0.1816(3) 0.3629(2) 0.27380(17) 0.0464(12) Uani 1 1 d . . .
H29A H -0.2256 0.3612 0.2494 0.070 Uiso 1 1 calc R . .
H29B H -0.1774 0.4053 0.2843 0.070 Uiso 1 1 calc R . .
H29C H -0.2041 0.3361 0.2967 0.070 Uiso 1 1 calc R . .
C30 C 0.0850(3) 0.39734(19) 0.36247(13) 0.0321(9) Uani 1 1 d . . .
C31 C 0.1463(4) 0.4072(2) 0.40264(14) 0.0419(11) Uani 1 1 d . . .
H31A H 0.1376 0.3727 0.4224 0.063 Uiso 1 1 calc R . .
H31B H 0.1280 0.4456 0.4167 0.063 Uiso 1 1 calc R . .
H31C H 0.2125 0.4095 0.3945 0.063 Uiso 1 1 calc R . .
C32 C -0.0180(4) 0.3903(3) 0.37682(19) 0.0622(17) Uani 1 1 d . . .
H32A H -0.0594 0.3878 0.3515 0.093 Uiso 1 1 calc R . .
H32B H -0.0356 0.4259 0.3942 0.093 Uiso 1 1 calc R . .
H32C H -0.0242 0.3526 0.3938 0.093 Uiso 1 1 calc R . .
C33 C 0.0987(5) 0.4503(2) 0.33221(17) 0.070(2) Uani 1 1 d . . .
H33A H 0.1649 0.4526 0.3241 0.104 Uiso 1 1 calc R . .
H33B H 0.0805 0.4888 0.3463 0.104 Uiso 1 1 calc R . .
H33C H 0.0595 0.4442 0.3065 0.104 Uiso 1 1 calc R . .
C34 C 0.6121(2) 0.24669(19) 0.17537(12) 0.0246(8) Uani 1 1 d . . .
H34A H 0.6439 0.2645 0.2005 0.037 Uiso 1 1 calc R . .
H34B H 0.6350 0.2667 0.1494 0.037 Uiso 1 1 calc R . .
H34C H 0.6254 0.2025 0.1741 0.037 Uiso 1 1 calc R . .
C35 C 0.5075(2) 0.25655(16) 0.17866(11) 0.0176(7) Uani 1 1 d . . .
C36 C 0.4559(2) 0.25576(17) 0.13920(11) 0.0192(7) Uani 1 1 d . . .
H36 H 0.4877 0.2342 0.1173 0.023 Uiso 1 1 calc R . .
C37 C 0.3676(2) 0.27986(16) 0.12519(11) 0.0167(7) Uani 1 1 d . . .
C38 C 0.3557(3) 0.28802(18) 0.07749(11) 0.0214(8) Uani 1 1 d . . .
H38A H 0.3422 0.2481 0.0642 0.032 Uiso 1 1 calc R . .
H38B H 0.4138 0.3049 0.0657 0.032 Uiso 1 1 calc R . .
H38C H 0.3036 0.3164 0.0716 0.032 Uiso 1 1 calc R . .
C39 C 0.2142(2) 0.32364(17) 0.13853(11) 0.0183(7) Uani 1 1 d . . .
C40 C 0.1395(2) 0.29250(18) 0.11835(11) 0.0213(8) Uani 1 1 d . . .
C41 C 0.0579(3) 0.3260(2) 0.10847(12) 0.0286(9) Uani 1 1 d . . .
H41 H 0.0066 0.3059 0.0946 0.034 Uiso 1 1 calc R . .
C42 C 0.0508(3) 0.3874(2) 0.11839(13) 0.0318(10) Uani 1 1 d . . .
H42 H -0.0056 0.4090 0.1118 0.038 Uiso 1 1 calc R . .
C43 C 0.1251(3) 0.4178(2) 0.13796(12) 0.0285(9) Uani 1 1 d . . .
H43 H 0.1193 0.4603 0.1445 0.034 Uiso 1 1 calc R . .
C44 C 0.2085(2) 0.38692(17) 0.14824(11) 0.0201(8) Uani 1 1 d . . .
C45 C 0.2927(3) 0.42124(17) 0.16664(12) 0.0235(8) Uani 1 1 d . . .
H45 H 0.3284 0.3923 0.1857 0.028 Uiso 1 1 calc R . .
C46 C 0.3576(3) 0.4410(2) 0.13071(14) 0.0325(9) Uani 1 1 d . . .
H46A H 0.3809 0.4044 0.1159 0.049 Uiso 1 1 calc R . .
H46B H 0.4109 0.4641 0.1428 0.049 Uiso 1 1 calc R . .
H46C H 0.3228 0.4671 0.1104 0.049 Uiso 1 1 calc R . .
C47 C 0.2665(3) 0.47762(19) 0.19306(13) 0.0329(9) Uani 1 1 d . . .
H47A H 0.2379 0.5088 0.1743 0.049 Uiso 1 1 calc R . .
H47B H 0.3232 0.4946 0.2068 0.049 Uiso 1 1 calc R . .
H47C H 0.2216 0.4657 0.2150 0.049 Uiso 1 1 calc R . .
C48 C 0.1436(3) 0.22515(19) 0.10603(12) 0.0262(8) Uani 1 1 d . . .
H48 H 0.2062 0.2085 0.1152 0.031 Uiso 1 1 calc R . .
C49 C 0.1335(3) 0.2172(2) 0.05736(13) 0.0396(11) Uani 1 1 d . . .
H49A H 0.0697 0.2286 0.0482 0.059 Uiso 1 1 calc R . .
H49B H 0.1454 0.1742 0.0498 0.059 Uiso 1 1 calc R . .
H49C H 0.1791 0.2437 0.0430 0.059 Uiso 1 1 calc R . .
C50 C 0.0670(3) 0.1885(2) 0.12879(13) 0.0308(9) Uani 1 1 d . . .
H50A H 0.0728 0.1949 0.1598 0.046 Uiso 1 1 calc R . .
H50B H 0.0743 0.1446 0.1224 0.046 Uiso 1 1 calc R . .
H50C H 0.0050 0.2024 0.1188 0.046 Uiso 1 1 calc R . .
C51 C 0.5191(2) 0.26866(17) 0.25558(11) 0.0166(7) Uani 1 1 d . . .
C52 C 0.5277(2) 0.32770(17) 0.27329(11) 0.0201(8) Uani 1 1 d . . .
C53 C 0.5746(2) 0.33425(19) 0.31247(12) 0.0236(8) Uani 1 1 d . . .
H53 H 0.5821 0.3740 0.3247 0.028 Uiso 1 1 calc R . .
C54 C 0.6106(3) 0.2834(2) 0.33378(12) 0.0281(9) Uani 1 1 d . . .
H54 H 0.6415 0.2884 0.3607 0.034 Uiso 1 1 calc R . .
C55 C 0.6017(3) 0.22573(19) 0.31603(12) 0.0243(8) Uani 1 1 d . . .
H55 H 0.6263 0.1912 0.3311 0.029 Uiso 1 1 calc R . .
C56 C 0.5570(2) 0.21685(17) 0.27630(11) 0.0198(8) Uani 1 1 d . . .
C57 C 0.5533(3) 0.15232(18) 0.25792(12) 0.0231(8) Uani 1 1 d . . .
H57 H 0.5219 0.1547 0.2291 0.028 Uiso 1 1 calc R . .
C58 C 0.6524(3) 0.1258(2) 0.25192(14) 0.0312(9) Uani 1 1 d . . .
H58A H 0.6905 0.1552 0.2358 0.047 Uiso 1 1 calc R . .
H58B H 0.6481 0.0870 0.2361 0.047 Uiso 1 1 calc R . .
H58C H 0.6819 0.1184 0.2800 0.047 Uiso 1 1 calc R . .
C59 C 0.4956(3) 0.10852(19) 0.28574(13) 0.0292(9) Uani 1 1 d . . .
H59A H 0.5272 0.1032 0.3136 0.044 Uiso 1 1 calc R . .
H59B H 0.4899 0.0685 0.2714 0.044 Uiso 1 1 calc R . .
H59C H 0.4328 0.1259 0.2900 0.044 Uiso 1 1 calc R . .
C60 C 0.4888(3) 0.38401(18) 0.25012(12) 0.0237(8) Uani 1 1 d . . .
H60 H 0.4294 0.3715 0.2349 0.028 Uiso 1 1 calc R . .
C61 C 0.5578(3) 0.4068(2) 0.21631(14) 0.0344(10) Uani 1 1 d . . .
H61A H 0.6180 0.4171 0.2301 0.052 Uiso 1 1 calc R . .
H61B H 0.5319 0.4434 0.2022 0.052 Uiso 1 1 calc R . .
H61C H 0.5674 0.3744 0.1950 0.052 Uiso 1 1 calc R . .
C62 C 0.4652(3) 0.43736(19) 0.27999(14) 0.0312(9) Uani 1 1 d . . .
H62A H 0.4254 0.4224 0.3031 0.047 Uiso 1 1 calc R . .
H62B H 0.4317 0.4694 0.2638 0.047 Uiso 1 1 calc R . .
H62C H 0.5234 0.4545 0.2922 0.047 Uiso 1 1 calc R . .
C63 C 0.3481(3) 0.08376(18) 0.15797(12) 0.0249(8) Uani 1 1 d . . .
C64 C 0.4528(3) 0.0732(2) 0.15060(15) 0.0363(10) Uani 1 1 d . . .
H64A H 0.4781 0.1072 0.1338 0.054 Uiso 1 1 calc R . .
H64B H 0.4614 0.0345 0.1350 0.054 Uiso 1 1 calc R . .
H64C H 0.4860 0.0710 0.1782 0.054 Uiso 1 1 calc R . .
C65 C 0.3094(3) 0.03299(19) 0.18633(16) 0.0367(10) Uani 1 1 d . . .
H65A H 0.3422 0.0337 0.2141 0.055 Uiso 1 1 calc R . .
H65B H 0.3191 -0.0070 0.1726 0.055 Uiso 1 1 calc R . .
H65C H 0.2420 0.0396 0.1905 0.055 Uiso 1 1 calc R . .
C66 C 0.2959(4) 0.0842(2) 0.11452(16) 0.0521(14) Uani 1 1 d . . .
H66A H 0.2290 0.0926 0.1190 0.078 Uiso 1 1 calc R . .
H66B H 0.3029 0.0441 0.1007 0.078 Uiso 1 1 calc R . .
H66C H 0.3225 0.1163 0.0963 0.078 Uiso 1 1 calc R . .
C67 C 0.1997(2) 0.22472(17) 0.23240(11) 0.0181(7) Uani 1 1 d . . .
H67 H 0.1766 0.1937 0.2135 0.022 Uiso 1 1 calc R . .
C68 C 0.2807(2) 0.21232(17) 0.26340(11) 0.0188(7) Uani 1 1 d . . .
H68 H 0.3098 0.1731 0.2651 0.023 Uiso 1 1 calc R . .
C69 C 0.3118(2) 0.26329(18) 0.29035(11) 0.0209(8) Uani 1 1 d . . .
H69 H 0.3529 0.2555 0.3140 0.025 Uiso 1 1 calc R . .
C70 C 0.2823(3) 0.32278(18) 0.28212(11) 0.0225(8) Uani 1 1 d . . .
H70 H 0.3132 0.3563 0.2958 0.027 Uiso 1 1 calc R . .
C71 C 0.2045(2) 0.33428(17) 0.25261(11) 0.0203(8) Uani 1 1 d . . .
H71 H 0.1849 0.3753 0.2469 0.024 Uiso 1 1 calc R . .
C72 C 0.1589(3) 0.28590(17) 0.23282(11) 0.0204(8) Uani 1 1 d . . .
H72 H 0.0997 0.2927 0.2192 0.025 Uiso 1 1 calc R . .
C73 C 0.6567(3) 0.30202(18) 0.49035(11) 0.0215(8) Uani 1 1 d . . .
C74 C 0.6752(3) 0.33623(19) 0.45357(12) 0.0253(8) Uani 1 1 d . . .
C75 C 0.6225(3) 0.38499(19) 0.43939(13) 0.0306(9) Uani 1 1 d . . .
C76 C 0.5461(3) 0.40433(19) 0.46223(14) 0.0324(10) Uani 1 1 d . . .
C77 C 0.5236(3) 0.3727(2) 0.49887(13) 0.0289(9) Uani 1 1 d . . .
C78 C 0.5777(3) 0.32276(18) 0.51171(12) 0.0242(8) Uani 1 1 d . . .
C79 C 0.8160(3) 0.30126(18) 0.52714(11) 0.0212(8) Uani 1 1 d . . .
C80 C 0.8954(3) 0.31914(18) 0.50527(11) 0.0229(8) Uani 1 1 d . . .
C81 C 0.9527(3) 0.36824(19) 0.51705(12) 0.0267(9) Uani 1 1 d . . .
C82 C 0.9321(3) 0.40143(18) 0.55331(13) 0.0286(9) Uani 1 1 d . . .
C83 C 0.8551(3) 0.38547(19) 0.57675(12) 0.0279(9) Uani 1 1 d . . .
C84 C 0.7995(3) 0.33711(18) 0.56327(11) 0.0231(8) Uani 1 1 d . . .
C85 C 0.6943(2) 0.20500(17) 0.54608(11) 0.0188(7) Uani 1 1 d . . .
C86 C 0.7428(2) 0.18545(17) 0.58266(11) 0.0205(8) Uani 1 1 d . . .
C87 C 0.7148(3) 0.13648(18) 0.60758(11) 0.0223(8) Uani 1 1 d . . .
C88 C 0.6345(3) 0.10477(17) 0.59730(11) 0.0217(8) Uani 1 1 d . . .
C89 C 0.5824(2) 0.12261(17) 0.56178(11) 0.0207(8) Uani 1 1 d . . .
C90 C 0.6135(2) 0.17089(17) 0.53737(11) 0.0197(7) Uani 1 1 d . . .
C91 C 0.7737(3) 0.20132(17) 0.47492(11) 0.0206(8) Uani 1 1 d . . .
C92 C 0.7259(3) 0.18110(18) 0.43847(11) 0.0222(8) Uani 1 1 d . . .
C93 C 0.7525(3) 0.13044(18) 0.41477(11) 0.0245(8) Uani 1 1 d . . .
C94 C 0.8307(3) 0.09738(18) 0.42641(12) 0.0268(9) Uani 1 1 d . . .
C95 C 0.8813(3) 0.11443(18) 0.46267(12) 0.0247(8) Uani 1 1 d . . .
C96 C 0.8518(3) 0.16520(18) 0.48542(11) 0.0220(8) Uani 1 1 d . . .
C97 C 0.3080(3) 0.0795(2) 0.49399(15) 0.0395(11) Uani 1 1 d . . .
H97A H 0.2997 0.1046 0.4678 0.047 Uiso 1 1 calc R . .
H97B H 0.3549 0.1004 0.5126 0.047 Uiso 1 1 calc R . .
C98 C 0.3460(4) 0.0184(2) 0.48168(14) 0.0428(11) Uani 1 1 d . . .
H98A H 0.4037 0.0247 0.4649 0.051 Uiso 1 1 calc R . .
H98B H 0.2994 -0.0025 0.4629 0.051 Uiso 1 1 calc R . .
B1 B 0.7353(3) 0.2528(2) 0.50953(12) 0.0199(8) Uani 1 1 d . . .
N1 N 0.1669(2) 0.21080(13) 0.36440(9) 0.0168(6) Uani 1 1 d . . .
N2 N 0.0090(2) 0.23363(13) 0.30235(9) 0.0165(6) Uani 1 1 d . . .
N3 N 0.1130(2) 0.34064(15) 0.34095(10) 0.0234(7) Uani 1 1 d . . .
N4 N 0.46510(19) 0.26166(13) 0.21621(9) 0.0155(6) Uani 1 1 d . . .
N5 N 0.29817(19) 0.29090(13) 0.15225(9) 0.0155(6) Uani 1 1 d . . .
N6 N 0.3354(2) 0.14261(14) 0.17930(9) 0.0202(6) Uani 1 1 d . . .
F1 F 0.90359(15) 0.17910(11) 0.52095(7) 0.0275(5) Uani 1 1 d . . .
F2 F 0.95675(16) 0.08205(11) 0.47543(8) 0.0346(6) Uani 1 1 d . . .
F3 F 0.85808(18) 0.04861(11) 0.40339(8) 0.0379(6) Uani 1 1 d . . .
F4 F 0.70175(18) 0.11268(11) 0.38012(7) 0.0329(5) Uani 1 1 d . . .
F5 F 0.64712(15) 0.21000(10) 0.42417(6) 0.0260(5) Uani 1 1 d . . .
F6 F 0.75144(16) 0.32136(11) 0.43004(7) 0.0293(5) Uani 1 1 d . . .
F7 F 0.6453(2) 0.41525(12) 0.40320(8) 0.0424(6) Uani 1 1 d . . .
F8 F 0.4940(2) 0.45243(12) 0.44926(9) 0.0464(7) Uani 1 1 d . . .
F9 F 0.44875(17) 0.39001(12) 0.52193(8) 0.0396(6) Uani 1 1 d . . .
F10 F 0.54972(15) 0.29520(11) 0.54820(7) 0.0297(5) Uani 1 1 d . . .
F11 F 0.72220(15) 0.32565(11) 0.58695(7) 0.0284(5) Uani 1 1 d . . .
F12 F 0.83445(19) 0.41695(12) 0.61255(7) 0.0395(6) Uani 1 1 d . . .
F13 F 0.98814(18) 0.44833(12) 0.56587(8) 0.0419(6) Uani 1 1 d . . .
F14 F 1.02810(16) 0.38325(12) 0.49383(8) 0.0353(6) Uani 1 1 d . . .
F15 F 0.92265(15) 0.28892(11) 0.46960(7) 0.0295(5) Uani 1 1 d . . .
F16 F 0.82227(15) 0.21398(10) 0.59610(6) 0.0250(5) Uani 1 1 d . . .
F17 F 0.76557(17) 0.11944(10) 0.64255(7) 0.0300(5) Uani 1 1 d . . .
F18 F 0.60584(16) 0.05687(10) 0.62109(7) 0.0292(5) Uani 1 1 d . . .
F19 F 0.50375(15) 0.09144(10) 0.55103(7) 0.0277(5) Uani 1 1 d . . .
F20 F 0.56087(14) 0.18387(10) 0.50203(6) 0.0248(5) Uani 1 1 d . . .
Nb1 Nb 0.33422(2) 0.219735(14) 0.196967(9) 0.01454(9) Uani 1 1 d . . .
Nb2 Nb 0.14659(2) 0.275653(14) 0.311485(9) 0.01479(9) Uani 1 1 d . . .
Cl1 Cl 0.37292(8) -0.03036(5) 0.52599(3) 0.0374(3) Uani 1 1 d . . .
Cl2 Cl 0.20057(10) 0.07675(9) 0.52081(5) 0.0689(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.515(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N2 1.339(5) . ?
C2 C3 1.403(5) . ?
C3 C4 1.404(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.341(5) . ?
C4 C5 1.509(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.406(5) . ?
C6 C11 1.407(5) . ?
C6 N1 1.450(4) . ?
C7 C8 1.395(5) . ?
C7 C15 1.525(5) . ?
C8 C9 1.387(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.376(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.524(6) . ?
C12 C13 1.533(6) . ?
C12 C14 1.540(6) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.533(6) . ?
C15 C17 1.535(6) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.402(5) . ?
C18 C19 1.407(5) . ?
C18 N2 1.453(4) . ?
C19 C20 1.396(5) . ?
C19 C27 1.518(6) . ?
C20 C21 1.370(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.378(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.404(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.529(5) . ?
C24 C25 1.523(6) . ?
C24 C26 1.532(6) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.532(6) . ?
C27 C29 1.539(6) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.462(5) . ?
C30 C33 1.505(7) . ?
C30 C31 1.532(6) . ?
C30 C32 1.546(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.509(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N4 1.332(4) . ?
C35 C36 1.426(5) . ?
C35 Nb1 2.661(3) . ?
C36 C37 1.424(5) . ?
C36 Nb1 2.638(3) . ?
C36 H36 0.9500 . ?
C37 N5 1.331(4) . ?
C37 C38 1.508(5) . ?
C37 Nb1 2.645(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.402(5) . ?
C39 C44 1.411(5) . ?
C39 N5 1.450(4) . ?
C40 C41 1.401(5) . ?
C40 C48 1.515(6) . ?
C41 C42 1.373(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.382(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.397(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.518(5) . ?
C45 C46 1.525(5) . ?
C45 C47 1.527(5) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C50 1.533(5) . ?
C48 C49 1.535(5) . ?
C48 H48 1.0000 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.402(5) . ?
C51 C56 1.403(5) . ?
C51 N4 1.448(4) . ?
C52 C53 1.394(5) . ?
C52 C60 1.522(5) . ?
C53 C54 1.384(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.376(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.400(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.516(5) . ?
C57 C59 1.535(5) . ?
C57 C58 1.537(5) . ?
C57 H57 1.0000 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C62 1.529(5) . ?
C60 C61 1.534(5) . ?
C60 H60 1.0000 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 N6 1.455(5) . ?
C63 C65 1.523(6) . ?
C63 C64 1.528(6) . ?
C63 C66 1.538(6) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C72 1.451(5) . ?
C67 C68 1.519(5) . ?
C67 Nb1 2.228(3) . ?
C67 H67 0.9500 . ?
C68 C69 1.456(5) . ?
C68 Nb1 2.227(3) . ?
C68 H68 0.9500 . ?
C69 C70 1.382(5) . ?
C69 Nb2 2.465(3) . ?
C69 H69 0.9500 . ?
C70 C71 1.453(5) . ?
C70 Nb2 2.381(3) . ?
C70 H70 0.9500 . ?
C71 C72 1.377(5) . ?
C71 Nb2 2.394(3) . ?
C71 H71 0.9500 . ?
C72 Nb2 2.477(3) . ?
C72 H72 0.9500 . ?
C73 C78 1.391(5) . ?
C73 C74 1.397(5) . ?
C73 B1 1.653(6) . ?
C74 F6 1.357(4) . ?
C74 C75 1.368(6) . ?
C75 F7 1.352(5) . ?
C75 C76 1.374(6) . ?
C76 F8 1.341(5) . ?
C76 C77 1.378(6) . ?
C77 F9 1.348(5) . ?
C77 C78 1.385(6) . ?
C78 F10 1.353(4) . ?
C79 C80 1.384(5) . ?
C79 C84 1.394(5) . ?
C79 B1 1.647(5) . ?
C80 F15 1.355(4) . ?
C80 C81 1.389(5) . ?
C81 F14 1.344(4) . ?
C81 C82 1.378(6) . ?
C82 F13 1.349(4) . ?
C82 C83 1.371(6) . ?
C83 F12 1.347(4) . ?
C83 C84 1.378(5) . ?
C84 F11 1.357(4) . ?
C85 C90 1.392(5) . ?
C85 C86 1.393(5) . ?
C85 B1 1.656(5) . ?
C86 F16 1.351(4) . ?
C86 C87 1.381(5) . ?
C87 F17 1.353(4) . ?
C87 C88 1.368(5) . ?
C88 F18 1.346(4) . ?
C88 C89 1.382(5) . ?
C89 F19 1.346(4) . ?
C89 C90 1.374(5) . ?
C90 F20 1.355(4) . ?
C91 C92 1.389(5) . ?
C91 C96 1.395(5) . ?
C91 B1 1.655(6) . ?
C92 F5 1.355(4) . ?
C92 C93 1.383(5) . ?
C93 F4 1.349(4) . ?
C93 C94 1.369(6) . ?
C94 F3 1.342(4) . ?
C94 C95 1.384(5) . ?
C95 F2 1.339(5) . ?
C95 C96 1.381(5) . ?
C96 F1 1.357(4) . ?
C97 C98 1.485(6) . ?
C97 Cl2 1.754(5) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C98 Cl1 1.782(5) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
N1 Nb2 2.189(3) . ?
N2 Nb2 2.175(3) . ?
N3 Nb2 1.756(3) . ?
N4 Nb1 2.151(3) . ?
N5 Nb1 2.142(3) . ?
N6 Nb1 1.765(3) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C2 C3 123.9(3) . . ?
N2 C2 C1 120.5(3) . . ?
C3 C2 C1 115.5(3) . . ?
C2 C3 C4 129.9(3) . . ?
C2 C3 H3 115.1 . . ?
C4 C3 H3 115.1 . . ?
N1 C4 C3 123.9(3) . . ?
N1 C4 C5 120.6(3) . . ?
C3 C4 C5 115.5(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 120.1(3) . . ?
C7 C6 N1 118.8(3) . . ?
C11 C6 N1 121.1(3) . . ?
C8 C7 C6 118.7(4) . . ?
C8 C7 C15 118.4(4) . . ?
C6 C7 C15 122.8(3) . . ?
C9 C8 C7 121.3(4) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C10 C9 C8 119.6(4) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 121.2(4) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 119.1(4) . . ?
C10 C11 C12 118.3(3) . . ?
C6 C11 C12 122.6(3) . . ?
C11 C12 C13 110.9(4) . . ?
C11 C12 C14 112.2(3) . . ?
C13 C12 C14 108.6(3) . . ?
C11 C12 H12 108.4 . . ?
C13 C12 H12 108.4 . . ?
C14 C12 H12 108.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 C16 112.3(3) . . ?
C7 C15 C17 110.6(3) . . ?
C16 C15 C17 109.5(4) . . ?
C7 C15 H15 108.1 . . ?
C16 C15 H15 108.1 . . ?
C17 C15 H15 108.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.6(3) . . ?
C23 C18 N2 118.6(3) . . ?
C19 C18 N2 120.8(3) . . ?
C20 C19 C18 118.1(4) . . ?
C20 C19 C27 118.3(3) . . ?
C18 C19 C27 123.6(3) . . ?
C21 C20 C19 121.8(4) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C20 C21 C22 119.9(4) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C23 120.7(4) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C22 118.7(3) . . ?
C18 C23 C24 122.2(3) . . ?
C22 C23 C24 119.2(3) . . ?
C25 C24 C23 112.2(3) . . ?
C25 C24 C26 109.5(4) . . ?
C23 C24 C26 112.4(3) . . ?
C25 C24 H24 107.5 . . ?
C23 C24 H24 107.5 . . ?
C26 C24 H24 107.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 C28 112.6(3) . . ?
C19 C27 C29 112.3(4) . . ?
C28 C27 C29 108.1(3) . . ?
C19 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
C29 C27 H27 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C33 108.5(4) . . ?
N3 C30 C31 109.8(3) . . ?
C33 C30 C31 109.3(4) . . ?
N3 C30 C32 108.4(4) . . ?
C33 C30 C32 112.9(5) . . ?
C31 C30 C32 107.8(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N4 C35 C36 122.0(3) . . ?
N4 C35 C34 122.1(3) . . ?
C36 C35 C34 115.8(3) . . ?
N4 C35 Nb1 53.36(17) . . ?
C36 C35 Nb1 73.5(2) . . ?
C34 C35 Nb1 152.8(3) . . ?
C37 C36 C35 134.6(3) . . ?
C37 C36 Nb1 74.6(2) . . ?
C35 C36 Nb1 75.3(2) . . ?
C37 C36 H36 112.7 . . ?
C35 C36 H36 112.7 . . ?
Nb1 C36 H36 132.2 . . ?
N5 C37 C36 122.0(3) . . ?
N5 C37 C38 122.2(3) . . ?
C36 C37 C38 115.6(3) . . ?
N5 C37 Nb1 53.59(17) . . ?
C36 C37 Nb1 74.08(19) . . ?
C38 C37 Nb1 151.3(2) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C44 121.4(3) . . ?
C40 C39 N5 120.8(3) . . ?
C44 C39 N5 117.7(3) . . ?
C41 C40 C39 117.9(4) . . ?
C41 C40 C48 118.8(3) . . ?
C39 C40 C48 123.3(3) . . ?
C42 C41 C40 121.3(4) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C43 120.4(4) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C42 C43 C44 120.8(4) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C43 C44 C39 118.1(4) . . ?
C43 C44 C45 120.9(4) . . ?
C39 C44 C45 120.9(3) . . ?
C44 C45 C46 110.0(3) . . ?
C44 C45 C47 113.7(3) . . ?
C46 C45 C47 109.1(3) . . ?
C44 C45 H45 107.9 . . ?
C46 C45 H45 107.9 . . ?
C47 C45 H45 107.9 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C40 C48 C50 110.8(3) . . ?
C40 C48 C49 110.9(3) . . ?
C50 C48 C49 110.2(3) . . ?
C40 C48 H48 108.3 . . ?
C50 C48 H48 108.3 . . ?
C49 C48 H48 108.3 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 C56 121.4(3) . . ?
C52 C51 N4 118.3(3) . . ?
C56 C51 N4 120.2(3) . . ?
C53 C52 C51 118.6(3) . . ?
C53 C52 C60 120.1(3) . . ?
C51 C52 C60 121.3(3) . . ?
C54 C53 C52 120.7(4) . . ?
C54 C53 H53 119.7 . . ?
C52 C53 H53 119.7 . . ?
C55 C54 C53 120.1(4) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C54 C55 C56 121.4(3) . . ?
C54 C55 H55 119.3 . . ?
C56 C55 H55 119.3 . . ?
C55 C56 C51 117.7(3) . . ?
C55 C56 C57 118.5(3) . . ?
C51 C56 C57 123.8(3) . . ?
C56 C57 C59 112.1(3) . . ?
C56 C57 C58 111.4(3) . . ?
C59 C57 C58 109.6(3) . . ?
C56 C57 H57 107.9 . . ?
C59 C57 H57 107.9 . . ?
C58 C57 H57 107.9 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C52 C60 C62 113.6(3) . . ?
C52 C60 C61 110.8(3) . . ?
C62 C60 C61 108.9(3) . . ?
C52 C60 H60 107.8 . . ?
C62 C60 H60 107.8 . . ?
C61 C60 H60 107.8 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N6 C63 C65 108.8(3) . . ?
N6 C63 C64 109.3(3) . . ?
C65 C63 C64 109.8(3) . . ?
N6 C63 C66 109.7(3) . . ?
C65 C63 C66 110.2(4) . . ?
C64 C63 C66 109.1(4) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C72 C67 C68 117.2(3) . . ?
C72 C67 Nb1 113.3(2) . . ?
C68 C67 Nb1 70.05(18) . . ?
C72 C67 H67 121.4 . . ?
C68 C67 H67 121.4 . . ?
Nb1 C67 H67 87.0 . . ?
C69 C68 C67 117.1(3) . . ?
C69 C68 Nb1 112.3(2) . . ?
C67 C68 Nb1 70.07(18) . . ?
C69 C68 H68 121.5 . . ?
C67 C68 H68 121.5 . . ?
Nb1 C68 H68 87.9 . . ?
C70 C69 C68 121.0(3) . . ?
C70 C69 Nb2 70.1(2) . . ?
C68 C69 Nb2 87.4(2) . . ?
C70 C69 H69 119.5 . . ?
C68 C69 H69 119.5 . . ?
Nb2 C69 H69 113.0 . . ?
C69 C70 C71 120.4(3) . . ?
C69 C70 Nb2 76.8(2) . . ?
C71 C70 Nb2 72.76(19) . . ?
C69 C70 H70 119.8 . . ?
C71 C70 H70 119.8 . . ?
Nb2 C70 H70 121.9 . . ?
C72 C71 C70 120.2(3) . . ?
C72 C71 Nb2 76.9(2) . . ?
C70 C71 Nb2 71.83(19) . . ?
C72 C71 H71 119.9 . . ?
C70 C71 H71 119.9 . . ?
Nb2 C71 H71 122.7 . . ?
C71 C72 C67 121.2(3) . . ?
C71 C72 Nb2 70.3(2) . . ?
C67 C72 Nb2 87.7(2) . . ?
C71 C72 H72 119.4 . . ?
C67 C72 H72 119.4 . . ?
Nb2 C72 H72 112.6 . . ?
C78 C73 C74 112.7(4) . . ?
C78 C73 B1 125.6(3) . . ?
C74 C73 B1 120.6(3) . . ?
F6 C74 C75 116.6(3) . . ?
F6 C74 C73 118.7(3) . . ?
C75 C74 C73 124.7(4) . . ?
F7 C75 C74 120.7(4) . . ?
F7 C75 C76 119.1(4) . . ?
C74 C75 C76 120.2(4) . . ?
F8 C76 C75 121.3(4) . . ?
F8 C76 C77 120.4(4) . . ?
C75 C76 C77 118.3(4) . . ?
F9 C77 C76 119.9(4) . . ?
F9 C77 C78 120.2(4) . . ?
C76 C77 C78 119.8(4) . . ?
F10 C78 C77 115.0(3) . . ?
F10 C78 C73 120.7(3) . . ?
C77 C78 C73 124.3(4) . . ?
C80 C79 C84 113.0(3) . . ?
C80 C79 B1 125.8(3) . . ?
C84 C79 B1 120.2(3) . . ?
F15 C80 C79 121.0(3) . . ?
F15 C80 C81 114.6(3) . . ?
C79 C80 C81 124.4(4) . . ?
F14 C81 C82 119.8(4) . . ?
F14 C81 C80 120.9(4) . . ?
C82 C81 C80 119.3(4) . . ?
F13 C82 C83 120.6(4) . . ?
F13 C82 C81 120.2(4) . . ?
C83 C82 C81 119.2(4) . . ?
F12 C83 C82 120.0(4) . . ?
F12 C83 C84 120.7(4) . . ?
C82 C83 C84 119.3(4) . . ?
F11 C84 C83 116.1(3) . . ?
F11 C84 C79 119.1(3) . . ?
C83 C84 C79 124.9(4) . . ?
C90 C85 C86 113.3(3) . . ?
C90 C85 B1 119.8(3) . . ?
C86 C85 B1 125.6(3) . . ?
F16 C86 C87 115.2(3) . . ?
F16 C86 C85 121.1(3) . . ?
C87 C86 C85 123.7(3) . . ?
F17 C87 C88 119.0(3) . . ?
F17 C87 C86 120.8(3) . . ?
C88 C87 C86 120.2(3) . . ?
F18 C88 C87 121.3(3) . . ?
F18 C88 C89 119.8(3) . . ?
C87 C88 C89 118.9(3) . . ?
F19 C89 C90 121.3(3) . . ?
F19 C89 C88 119.6(3) . . ?
C90 C89 C88 119.1(3) . . ?
F20 C90 C89 115.7(3) . . ?
F20 C90 C85 119.6(3) . . ?
C89 C90 C85 124.8(3) . . ?
C92 C91 C96 113.2(3) . . ?
C92 C91 B1 126.0(3) . . ?
C96 C91 B1 119.7(3) . . ?
F5 C92 C93 115.1(3) . . ?
F5 C92 C91 121.1(3) . . ?
C93 C92 C91 123.8(4) . . ?
F4 C93 C94 119.1(3) . . ?
F4 C93 C92 120.7(4) . . ?
C94 C93 C92 120.2(3) . . ?
F3 C94 C93 120.9(3) . . ?
F3 C94 C95 119.9(4) . . ?
C93 C94 C95 119.2(4) . . ?
F2 C95 C96 121.0(3) . . ?
F2 C95 C94 120.5(4) . . ?
C96 C95 C94 118.5(4) . . ?
F1 C96 C95 115.7(3) . . ?
F1 C96 C91 119.2(3) . . ?
C95 C96 C91 125.1(3) . . ?
C98 C97 Cl2 114.6(4) . . ?
C98 C97 H97A 108.6 . . ?
Cl2 C97 H97A 108.6 . . ?
C98 C97 H97B 108.6 . . ?
Cl2 C97 H97B 108.6 . . ?
H97A C97 H97B 107.6 . . ?
C97 C98 Cl1 113.9(3) . . ?
C97 C98 H98A 108.8 . . ?
Cl1 C98 H98A 108.8 . . ?
C97 C98 H98B 108.8 . . ?
Cl1 C98 H98B 108.8 . . ?
H98A C98 H98B 107.7 . . ?
C79 B1 C73 99.9(3) . . ?
C79 B1 C91 114.6(3) . . ?
C73 B1 C91 115.4(3) . . ?
C79 B1 C85 114.9(3) . . ?
C73 B1 C85 114.4(3) . . ?
C91 B1 C85 98.6(3) . . ?
C4 N1 C6 118.6(3) . . ?
C4 N1 Nb2 115.1(2) . . ?
C6 N1 Nb2 125.1(2) . . ?
C2 N2 C18 116.8(3) . . ?
C2 N2 Nb2 115.9(2) . . ?
C18 N2 Nb2 126.1(2) . . ?
C30 N3 Nb2 175.7(3) . . ?
C35 N4 C51 121.1(3) . . ?
C35 N4 Nb1 96.9(2) . . ?
C51 N4 Nb1 136.7(2) . . ?
C37 N5 C39 121.1(3) . . ?
C37 N5 Nb1 96.4(2) . . ?
C39 N5 Nb1 137.4(2) . . ?
C63 N6 Nb1 168.5(3) . . ?
N6 Nb1 N5 119.02(12) . . ?
N6 Nb1 N4 118.56(12) . . ?
N5 Nb1 N4 94.27(11) . . ?
N6 Nb1 C68 103.16(13) . . ?
N5 Nb1 C68 125.34(12) . . ?
N4 Nb1 C68 94.37(12) . . ?
N6 Nb1 C67 102.33(13) . . ?
N5 Nb1 C67 95.15(12) . . ?
N4 Nb1 C67 125.93(12) . . ?
C68 Nb1 C67 39.87(12) . . ?
N6 Nb1 C36 93.37(12) . . ?
N5 Nb1 C36 59.50(11) . . ?
N4 Nb1 C36 59.45(11) . . ?
C68 Nb1 C36 153.61(12) . . ?
C67 Nb1 C36 154.52(12) . . ?
N6 Nb1 C37 101.63(12) . . ?
N5 Nb1 C37 30.02(11) . . ?
N4 Nb1 C37 82.09(10) . . ?
C68 Nb1 C37 153.40(12) . . ?
C67 Nb1 C37 124.30(12) . . ?
C36 Nb1 C37 31.28(11) . . ?
N6 Nb1 C35 101.87(12) . . ?
N5 Nb1 C35 81.74(11) . . ?
N4 Nb1 C35 29.79(11) . . ?
C68 Nb1 C35 123.52(12) . . ?
C67 Nb1 C35 153.80(12) . . ?
C36 Nb1 C35 31.21(11) . . ?
C37 Nb1 C35 59.40(11) . . ?
N3 Nb2 N2 98.95(13) . . ?
N3 Nb2 N1 98.97(13) . . ?
N2 Nb2 N1 86.41(10) . . ?
N3 Nb2 C70 94.84(14) . . ?
N2 Nb2 C70 149.68(11) . . ?
N1 Nb2 C70 117.98(12) . . ?
N3 Nb2 C71 94.24(14) . . ?
N2 Nb2 C71 116.20(11) . . ?
N1 Nb2 C71 151.68(11) . . ?
C70 Nb2 C71 35.42(12) . . ?
N3 Nb2 C69 119.73(13) . . ?
N2 Nb2 C69 141.14(11) . . ?
N1 Nb2 C69 90.92(11) . . ?
C70 Nb2 C69 33.09(13) . . ?
C71 Nb2 C69 60.81(12) . . ?
N3 Nb2 C72 118.14(13) . . ?
N2 Nb2 C72 89.08(11) . . ?
N1 Nb2 C72 142.86(12) . . ?
C70 Nb2 C72 60.63(12) . . ?
C71 Nb2 C72 32.79(12) . . ?
C69 Nb2 C72 70.28(12) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         4.099
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.093
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_database_code_depnum_ccdc_archive 'CCDC 1022634'
#######################################################################
#
#                 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_(2)
_chemical_name_common            'Complex 3'
_chemical_melting_point          ?
_chemical_formula_moiety         'C65 H66 B F20 N3 Nb O2'
_chemical_formula_sum            'C65 H66 B F20 N3 Nb O2'
_chemical_formula_weight         1404.93

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'
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 '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                   18.1669(5)
_cell_length_b                   17.1279(5)
_cell_length_c                   19.7092(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5590(10)
_cell_angle_gamma                90.00
_cell_volume                     6132.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    9754
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.40

_exptl_crystal_description       rode
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2876
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9140
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      80(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  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            57885
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.42
_reflns_number_total             11263
_reflns_number_gt                9552
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-2004
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0501P)²+6.8467P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11263
_refine_ls_number_parameters     842
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.1014
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.41779(15) -0.30000(16) 0.85526(14) 0.0307(6) Uani 1 1 d . . .
H1A H 0.4112 -0.3384 0.8188 0.046 Uiso 1 1 calc R . .
H1B H 0.4148 -0.3263 0.8993 0.046 Uiso 1 1 calc R . .
H1C H 0.4661 -0.2751 0.8510 0.046 Uiso 1 1 calc R . .
C2 C 0.35807(13) -0.23856(15) 0.85001(12) 0.0217(5) Uani 1 1 d . . .
C3 C 0.29912(14) -0.24850(15) 0.89356(12) 0.0243(6) Uani 1 1 d . . .
H3 H 0.3078 -0.2824 0.9310 0.029 Uiso 1 1 calc R . .
C4 C 0.22846(13) -0.21544(15) 0.88997(11) 0.0223(5) Uani 1 1 d . . .
C5 C 0.16963(15) -0.26359(17) 0.92438(13) 0.0313(6) Uani 1 1 d . . .
H5A H 0.1240 -0.2333 0.9267 0.047 Uiso 1 1 calc R . .
H5B H 0.1861 -0.2772 0.9704 0.047 Uiso 1 1 calc R . .
H5C H 0.1608 -0.3114 0.8983 0.047 Uiso 1 1 calc R . .
C6 C 0.13507(12) -0.12859(15) 0.84922(12) 0.0214(5) Uani 1 1 d . . .
C7 C 0.10614(13) -0.06876(16) 0.89003(13) 0.0264(6) Uani 1 1 d . . .
C8 C 0.03562(14) -0.04128(19) 0.87492(14) 0.0338(7) Uani 1 1 d . . .
H8 H 0.0159 0.0005 0.9008 0.041 Uiso 1 1 calc R . .
C9 C -0.00616(15) -0.0735(2) 0.82318(15) 0.0396(8) Uani 1 1 d . . .
H9 H -0.0532 -0.0525 0.8124 0.048 Uiso 1 1 calc R . .
C10 C 0.02050(14) -0.1360(2) 0.78731(14) 0.0385(8) Uani 1 1 d . . .
H10 H -0.0097 -0.1598 0.7535 0.046 Uiso 1 1 calc R . .
C11 C 0.09152(13) -0.16550(17) 0.79964(12) 0.0274(6) Uani 1 1 d . . .
C12 C 0.11623(15) -0.23699(19) 0.76038(13) 0.0349(7) Uani 1 1 d . . .
H12 H 0.1663 -0.2522 0.7773 0.042 Uiso 1 1 calc R . .
C13 C 0.12129(18) -0.2201(2) 0.68412(14) 0.0442(8) Uani 1 1 d . . .
H13A H 0.0736 -0.2012 0.6673 0.066 Uiso 1 1 calc R . .
H13B H 0.1346 -0.2680 0.6600 0.066 Uiso 1 1 calc R . .
H13C H 0.1589 -0.1802 0.6764 0.066 Uiso 1 1 calc R . .
C14 C 0.06395(18) -0.3059(2) 0.77190(18) 0.0514(9) Uani 1 1 d . . .
H14A H 0.0585 -0.3148 0.8207 0.077 Uiso 1 1 calc R . .
H14B H 0.0842 -0.3529 0.7507 0.077 Uiso 1 1 calc R . .
H14C H 0.0158 -0.2942 0.7516 0.077 Uiso 1 1 calc R . .
C15 C 0.14876(14) -0.03661(17) 0.95133(14) 0.0307(6) Uani 1 1 d . . .
H15 H 0.2009 -0.0284 0.9371 0.037 Uiso 1 1 calc R . .
C16 C 0.14956(17) -0.0943(2) 1.01059(14) 0.0386(7) Uani 1 1 d . . .
H16A H 0.0989 -0.1071 1.0230 0.058 Uiso 1 1 calc R . .
H16B H 0.1750 -0.0707 1.0496 0.058 Uiso 1 1 calc R . .
H16C H 0.1753 -0.1420 0.9971 0.058 Uiso 1 1 calc R . .
C17 C 0.12001(18) 0.0410(2) 0.97807(17) 0.0465(8) Uani 1 1 d . . .
H17A H 0.1144 0.0779 0.9404 0.070 Uiso 1 1 calc R . .
H17B H 0.1550 0.0622 1.0115 0.070 Uiso 1 1 calc R . .
H17C H 0.0722 0.0329 0.9996 0.070 Uiso 1 1 calc R . .
C18 C 0.41709(13) -0.19566(14) 0.75110(11) 0.0191(5) Uani 1 1 d . . .
C19 C 0.39815(14) -0.24448(15) 0.69636(12) 0.0242(5) Uani 1 1 d . . .
C20 C 0.45425(15) -0.27154(16) 0.65454(13) 0.0304(6) Uani 1 1 d . . .
H20 H 0.4425 -0.3063 0.6184 0.037 Uiso 1 1 calc R . .
C21 C 0.52594(15) -0.24897(16) 0.66455(13) 0.0302(6) Uani 1 1 d . . .
H21 H 0.5637 -0.2708 0.6375 0.036 Uiso 1 1 calc R . .
C22 C 0.54341(14) -0.19452(16) 0.71390(12) 0.0260(6) Uani 1 1 d . . .
H22 H 0.5926 -0.1762 0.7182 0.031 Uiso 1 1 calc R . .
C23 C 0.48922(13) -0.16598(15) 0.75773(12) 0.0216(5) Uani 1 1 d . . .
C24 C 0.51068(13) -0.10595(16) 0.81073(12) 0.0228(5) Uani 1 1 d . . .
H24 H 0.4643 -0.0830 0.8290 0.027 Uiso 1 1 calc R . .
C25 C 0.55567(16) -0.03912(18) 0.77996(15) 0.0357(7) Uani 1 1 d . . .
H25A H 0.6047 -0.0583 0.7680 0.054 Uiso 1 1 calc R . .
H25B H 0.5605 0.0032 0.8131 0.054 Uiso 1 1 calc R . .
H25C H 0.5305 -0.0196 0.7391 0.054 Uiso 1 1 calc R . .
C26 C 0.55324(17) -0.14205(19) 0.87024(14) 0.0390(7) Uani 1 1 d . . .
H26A H 0.5204 -0.1759 0.8962 0.058 Uiso 1 1 calc R . .
H26B H 0.5722 -0.1005 0.8998 0.058 Uiso 1 1 calc R . .
H26C H 0.5944 -0.1729 0.8529 0.058 Uiso 1 1 calc R . .
C27 C 0.31890(15) -0.26848(17) 0.68103(14) 0.0307(6) Uani 1 1 d . . .
H27 H 0.2862 -0.2315 0.7059 0.037 Uiso 1 1 calc R . .
C28 C 0.30086(18) -0.2603(2) 0.60556(15) 0.0430(8) Uani 1 1 d . . .
H28A H 0.3156 -0.2083 0.5899 0.065 Uiso 1 1 calc R . .
H28B H 0.2478 -0.2671 0.5983 0.065 Uiso 1 1 calc R . .
H28C H 0.3276 -0.3001 0.5800 0.065 Uiso 1 1 calc R . .
C29 C 0.30082(19) -0.3508(2) 0.70568(19) 0.0513(9) Uani 1 1 d . . .
H29A H 0.3339 -0.3883 0.6841 0.077 Uiso 1 1 calc R . .
H29B H 0.2497 -0.3634 0.6937 0.077 Uiso 1 1 calc R . .
H29C H 0.3073 -0.3533 0.7551 0.077 Uiso 1 1 calc R . .
C30 C 0.36415(13) 0.01493(15) 0.94278(12) 0.0227(5) Uani 1 1 d . . .
C31 C 0.36073(16) -0.04378(19) 1.00077(13) 0.0354(7) Uani 1 1 d . . .
H31A H 0.3094 -0.0582 1.0088 0.053 Uiso 1 1 calc R . .
H31B H 0.3817 -0.0203 1.0420 0.053 Uiso 1 1 calc R . .
H31C H 0.3889 -0.0905 0.9888 0.053 Uiso 1 1 calc R . .
C32 C 0.44370(14) 0.03944(17) 0.93011(13) 0.0280(6) Uani 1 1 d . . .
H32A H 0.4740 -0.0071 0.9230 0.042 Uiso 1 1 calc R . .
H32B H 0.4625 0.0685 0.9695 0.042 Uiso 1 1 calc R . .
H32C H 0.4456 0.0727 0.8897 0.042 Uiso 1 1 calc R . .
C33 C 0.31979(16) 0.08822(18) 0.95790(15) 0.0379(7) Uani 1 1 d . . .
H33A H 0.3214 0.1234 0.9187 0.057 Uiso 1 1 calc R . .
H33B H 0.3409 0.1146 0.9977 0.057 Uiso 1 1 calc R . .
H33C H 0.2686 0.0738 0.9670 0.057 Uiso 1 1 calc R . .
C34 C 0.36730(15) -0.03823(17) 0.65908(12) 0.0283(6) Uani 1 1 d . . .
H34A H 0.3263 -0.0730 0.6452 0.034 Uiso 1 1 calc R . .
H34B H 0.4145 -0.0649 0.6498 0.034 Uiso 1 1 calc R . .
C35 C 0.36293(17) 0.03868(19) 0.62204(14) 0.0393(7) Uani 1 1 d . . .
H35A H 0.3112 0.0551 0.6149 0.047 Uiso 1 1 calc R . .
H35B H 0.3877 0.0357 0.5776 0.047 Uiso 1 1 calc R . .
C36 C 0.40312(16) 0.09395(17) 0.66992(14) 0.0330(6) Uani 1 1 d . . .
H36A H 0.4571 0.0902 0.6644 0.040 Uiso 1 1 calc R . .
H36B H 0.3875 0.1487 0.6624 0.040 Uiso 1 1 calc R . .
C37 C 0.38025(18) 0.06546(16) 0.73865(15) 0.0375(7) Uani 1 1 d . . .
H37A H 0.4209 0.0720 0.7720 0.045 Uiso 1 1 calc R . .
H37B H 0.3369 0.0949 0.7547 0.045 Uiso 1 1 calc R . .
C38 C 0.19009(17) 0.07876(17) 0.80274(15) 0.0367(7) Uani 1 1 d . . .
H38A H 0.2327 0.1147 0.8054 0.044 Uiso 1 1 calc R . .
H38B H 0.1712 0.0704 0.8491 0.044 Uiso 1 1 calc R . .
C39 C 0.13219(19) 0.1115(2) 0.7585(2) 0.0549(9) Uani 1 1 d . . .
H39A H 0.0828 0.1008 0.7772 0.066 Uiso 1 1 calc R . .
H39B H 0.1383 0.1686 0.7536 0.066 Uiso 1 1 calc R . .
C40 C 0.1413(3) 0.0727(3) 0.6940(2) 0.0932(18) Uani 1 1 d . . .
H40A H 0.1758 0.1023 0.6651 0.112 Uiso 1 1 calc R . .
H40B H 0.0934 0.0686 0.6698 0.112 Uiso 1 1 calc R . .
C41 C 0.17094(17) -0.00582(19) 0.70892(14) 0.0380(7) Uani 1 1 d . . .
H41A H 0.1306 -0.0442 0.7143 0.046 Uiso 1 1 calc R . .
H41B H 0.2037 -0.0237 0.6722 0.046 Uiso 1 1 calc R . .
C42 C 0.22035(13) 0.38580(15) 0.82072(12) 0.0224(5) Uani 1 1 d . . .
C43 C 0.20640(14) 0.44440(16) 0.77328(13) 0.0251(6) Uani 1 1 d . . .
C44 C 0.21373(14) 0.43405(17) 0.70385(13) 0.0276(6) Uani 1 1 d . . .
C45 C 0.23698(14) 0.36413(18) 0.67867(12) 0.0286(6) Uani 1 1 d . . .
C46 C 0.25344(14) 0.30461(17) 0.72321(13) 0.0279(6) Uani 1 1 d . . .
C47 C 0.24532(13) 0.31723(16) 0.79179(12) 0.0248(6) Uani 1 1 d . . .
C48 C 0.30338(13) 0.39046(15) 0.92777(11) 0.0211(5) Uani 1 1 d . . .
C49 C 0.34960(14) 0.45145(15) 0.90959(12) 0.0231(5) Uani 1 1 d . . .
C50 C 0.42411(14) 0.45414(16) 0.92389(12) 0.0247(5) Uani 1 1 d . . .
C51 C 0.45711(13) 0.39317(17) 0.95735(12) 0.0259(6) Uani 1 1 d . . .
C52 C 0.41437(14) 0.33051(16) 0.97615(12) 0.0263(6) Uani 1 1 d . . .
C53 C 0.33976(14) 0.33000(15) 0.96098(12) 0.0235(5) Uani 1 1 d . . .
C54 C 0.17231(14) 0.47141(15) 0.93180(12) 0.0237(5) Uani 1 1 d . . .
C55 C 0.19530(14) 0.51890(16) 0.98445(13) 0.0261(6) Uani 1 1 d . . .
C56 C 0.15119(16) 0.57377(17) 1.01539(14) 0.0323(6) Uani 1 1 d . . .
C57 C 0.08071(17) 0.58513(18) 0.99314(16) 0.0385(7) Uani 1 1 d . . .
C58 C 0.05509(15) 0.54120(19) 0.93977(15) 0.0373(7) Uani 1 1 d . . .
C59 C 0.09976(14) 0.48590(17) 0.91127(13) 0.0294(6) Uani 1 1 d . . .
C60 C 0.16488(13) 0.32442(15) 0.93913(12) 0.0223(5) Uani 1 1 d . . .
C61 C 0.16289(13) 0.31731(15) 1.00969(12) 0.0235(5) Uani 1 1 d . . .
C62 C 0.11575(14) 0.26961(16) 1.04462(12) 0.0260(6) Uani 1 1 d . . .
C63 C 0.06477(14) 0.22614(16) 1.00907(13) 0.0269(6) Uani 1 1 d . . .
C64 C 0.06323(14) 0.23056(16) 0.93953(13) 0.0266(6) Uani 1 1 d . . .
C65 C 0.11222(14) 0.27918(16) 0.90636(12) 0.0244(5) Uani 1 1 d . . .
N1 N 0.36233(10) -0.18117(12) 0.80296(9) 0.0177(4) Uani 1 1 d . . .
N2 N 0.21227(10) -0.15045(12) 0.85659(9) 0.0173(4) Uani 1 1 d . . .
N3 N 0.33386(10) -0.02241(12) 0.88159(9) 0.0186(4) Uani 1 1 d . . .
O1 O 0.36197(9) -0.01792(10) 0.73024(8) 0.0243(4) Uani 1 1 d . . .
O2 O 0.21177(9) 0.00415(10) 0.77218(8) 0.0227(4) Uani 1 1 d . . .
F1 F 0.32110(8) 0.51398(9) 0.87624(8) 0.0320(4) Uani 1 1 d . . .
F2 F 0.46473(8) 0.51591(10) 0.90477(8) 0.0367(4) Uani 1 1 d . . .
F3 F 0.52979(8) 0.39342(11) 0.96994(8) 0.0390(4) Uani 1 1 d . . .
F4 F 0.44601(9) 0.26911(10) 1.00704(8) 0.0381(4) Uani 1 1 d . . .
F5 F 0.30365(8) 0.26512(9) 0.97965(8) 0.0332(4) Uani 1 1 d . . .
F6 F 0.18409(9) 0.51582(9) 0.79297(7) 0.0320(4) Uani 1 1 d . . .
F7 F 0.19772(9) 0.49331(10) 0.66126(8) 0.0380(4) Uani 1 1 d . . .
F8 F 0.24455(9) 0.35355(11) 0.61155(7) 0.0405(4) Uani 1 1 d . . .
F9 F 0.27756(9) 0.23546(10) 0.69991(8) 0.0398(4) Uani 1 1 d . . .
F10 F 0.26284(8) 0.25598(9) 0.83287(7) 0.0300(3) Uani 1 1 d . . .
F11 F 0.26398(9) 0.51370(10) 1.00997(8) 0.0410(4) Uani 1 1 d . . .
F12 F 0.17809(11) 0.61664(11) 1.06555(9) 0.0536(5) Uani 1 1 d . . .
F13 F 0.03756(12) 0.63816(13) 1.02103(11) 0.0678(6) Uani 1 1 d . . .
F14 F -0.01420(11) 0.55056(14) 0.91578(11) 0.0653(6) Uani 1 1 d . . .
F15 F 0.07026(9) 0.44070(11) 0.86030(9) 0.0467(5) Uani 1 1 d . . .
F16 F 0.21014(8) 0.36072(9) 1.04798(7) 0.0298(3) Uani 1 1 d . . .
F17 F 0.11812(9) 0.26594(10) 1.11290(7) 0.0349(4) Uani 1 1 d . . .
F18 F 0.01696(9) 0.18053(10) 1.04195(8) 0.0375(4) Uani 1 1 d . . .
F19 F 0.01382(8) 0.18832(10) 0.90409(8) 0.0357(4) Uani 1 1 d . . .
F20 F 0.10440(8) 0.28046(10) 0.83799(7) 0.0334(4) Uani 1 1 d . . .
Nb01 Nb 0.297969(10) -0.075447(12) 0.812769(9) 0.01431(7) Uani 1 1 d . . .
B1 B 0.21583(15) 0.39320(18) 0.90425(13) 0.0217(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.514(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.354(3) . ?
C2 C3 1.389(4) . ?
C3 C4 1.404(4) . ?
C3 H3 0.9500 . ?
C4 N2 1.325(3) . ?
C4 C5 1.515(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.402(3) . ?
C6 C7 1.408(4) . ?
C6 N2 1.458(3) . ?
C7 C8 1.394(4) . ?
C7 C15 1.531(4) . ?
C8 C9 1.380(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.404(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.519(4) . ?
C12 C14 1.534(4) . ?
C12 C13 1.534(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.524(4) . ?
C15 C16 1.530(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.405(3) . ?
C18 C23 1.410(3) . ?
C18 N1 1.455(3) . ?
C19 C20 1.396(4) . ?
C19 C27 1.525(4) . ?
C20 C21 1.371(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.404(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.514(3) . ?
C24 C26 1.529(3) . ?
C24 C25 1.535(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.527(4) . ?
C27 C29 1.527(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.467(3) . ?
C30 C33 1.523(4) . ?
C30 C31 1.524(4) . ?
C30 C32 1.528(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 O1 1.449(3) . ?
C34 C35 1.508(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.519(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.502(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 O1 1.475(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 O2 1.468(3) . ?
C38 C39 1.470(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.447(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.477(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 O2 1.455(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C47 1.384(4) . ?
C42 C43 1.393(4) . ?
C42 B1 1.654(3) . ?
C43 F6 1.347(3) . ?
C43 C44 1.388(4) . ?
C44 F7 1.347(3) . ?
C44 C45 1.365(4) . ?
C45 F8 1.343(3) . ?
C45 C46 1.376(4) . ?
C46 F9 1.345(3) . ?
C46 C47 1.378(4) . ?
C47 F10 1.361(3) . ?
C48 C53 1.389(4) . ?
C48 C49 1.389(4) . ?
C48 B1 1.653(4) . ?
C49 F1 1.357(3) . ?
C49 C50 1.381(4) . ?
C50 F2 1.346(3) . ?
C50 C51 1.370(4) . ?
C51 F3 1.341(3) . ?
C51 C52 1.378(4) . ?
C52 F4 1.342(3) . ?
C52 C53 1.385(4) . ?
C53 F5 1.344(3) . ?
C54 C55 1.380(4) . ?
C54 C59 1.397(4) . ?
C54 B1 1.650(4) . ?
C55 F11 1.344(3) . ?
C55 C56 1.381(4) . ?
C56 F12 1.321(3) . ?
C56 C57 1.363(4) . ?
C57 F13 1.323(3) . ?
C57 C58 1.371(5) . ?
C58 F14 1.350(3) . ?
C58 C59 1.371(4) . ?
C59 F15 1.373(3) . ?
C60 C65 1.386(4) . ?
C60 C61 1.397(3) . ?
C60 B1 1.652(4) . ?
C61 F16 1.359(3) . ?
C61 C62 1.373(4) . ?
C62 F17 1.347(3) . ?
C62 C63 1.375(4) . ?
C63 F18 1.340(3) . ?
C63 C64 1.373(4) . ?
C64 F19 1.344(3) . ?
C64 C65 1.387(4) . ?
C65 F20 1.354(3) . ?
N1 Nb01 2.165(2) . ?
N2 Nb01 2.2014(19) . ?
N3 Nb01 1.7531(19) . ?
O1 Nb01 2.2374(16) . ?
O2 Nb01 2.2195(16) . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 124.2(2) . . ?
N1 C2 C1 120.4(2) . . ?
C3 C2 C1 115.4(2) . . ?
C2 C3 C4 129.0(2) . . ?
C2 C3 H3 115.5 . . ?
C4 C3 H3 115.5 . . ?
N2 C4 C3 124.2(2) . . ?
N2 C4 C5 121.7(2) . . ?
C3 C4 C5 114.0(2) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 121.0(2) . . ?
C11 C6 N2 119.3(2) . . ?
C7 C6 N2 119.6(2) . . ?
C8 C7 C6 118.1(2) . . ?
C8 C7 C15 120.2(3) . . ?
C6 C7 C15 121.6(2) . . ?
C9 C8 C7 121.3(3) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.3(3) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C6 C11 C10 118.0(3) . . ?
C6 C11 C12 123.4(2) . . ?
C10 C11 C12 118.5(2) . . ?
C11 C12 C14 111.0(2) . . ?
C11 C12 C13 111.6(3) . . ?
C14 C12 C13 109.5(2) . . ?
C11 C12 H12 108.2 . . ?
C14 C12 H12 108.2 . . ?
C13 C12 H12 108.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C15 C16 107.5(2) . . ?
C17 C15 C7 114.5(2) . . ?
C16 C15 C7 111.8(2) . . ?
C17 C15 H15 107.6 . . ?
C16 C15 H15 107.6 . . ?
C7 C15 H15 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 120.4(2) . . ?
C19 C18 N1 118.5(2) . . ?
C23 C18 N1 121.0(2) . . ?
C20 C19 C18 118.4(2) . . ?
C20 C19 C27 119.1(2) . . ?
C18 C19 C27 122.4(2) . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C20 C21 C22 120.2(2) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C23 120.7(2) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C18 118.3(2) . . ?
C22 C23 C24 118.9(2) . . ?
C18 C23 C24 122.8(2) . . ?
C23 C24 C26 112.3(2) . . ?
C23 C24 C25 111.6(2) . . ?
C26 C24 C25 109.7(2) . . ?
C23 C24 H24 107.7 . . ?
C26 C24 H24 107.7 . . ?
C25 C24 H24 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C19 111.2(2) . . ?
C28 C27 C29 110.5(2) . . ?
C19 C27 C29 113.0(2) . . ?
C28 C27 H27 107.3 . . ?
C19 C27 H27 107.3 . . ?
C29 C27 H27 107.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C33 109.0(2) . . ?
N3 C30 C31 108.1(2) . . ?
C33 C30 C31 111.8(2) . . ?
N3 C30 C32 109.5(2) . . ?
C33 C30 C32 108.0(2) . . ?
C31 C30 C32 110.5(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O1 C34 C35 104.8(2) . . ?
O1 C34 H34A 110.8 . . ?
C35 C34 H34A 110.8 . . ?
O1 C34 H34B 110.8 . . ?
C35 C34 H34B 110.8 . . ?
H34A C34 H34B 108.9 . . ?
C34 C35 C36 102.8(2) . . ?
C34 C35 H35A 111.2 . . ?
C36 C35 H35A 111.2 . . ?
C34 C35 H35B 111.2 . . ?
C36 C35 H35B 111.2 . . ?
H35A C35 H35B 109.1 . . ?
C37 C36 C35 102.8(2) . . ?
C37 C36 H36A 111.2 . . ?
C35 C36 H36A 111.2 . . ?
C37 C36 H36B 111.2 . . ?
C35 C36 H36B 111.2 . . ?
H36A C36 H36B 109.1 . . ?
O1 C37 C36 106.1(2) . . ?
O1 C37 H37A 110.5 . . ?
C36 C37 H37A 110.5 . . ?
O1 C37 H37B 110.5 . . ?
C36 C37 H37B 110.5 . . ?
H37A C37 H37B 108.7 . . ?
O2 C38 C39 106.4(2) . . ?
O2 C38 H38A 110.5 . . ?
C39 C38 H38A 110.5 . . ?
O2 C38 H38B 110.5 . . ?
C39 C38 H38B 110.5 . . ?
H38A C38 H38B 108.6 . . ?
C40 C39 C38 105.0(3) . . ?
C40 C39 H39A 110.7 . . ?
C38 C39 H39A 110.7 . . ?
C40 C39 H39B 110.7 . . ?
C38 C39 H39B 110.7 . . ?
H39A C39 H39B 108.8 . . ?
C39 C40 C41 106.7(3) . . ?
C39 C40 H40A 110.4 . . ?
C41 C40 H40A 110.4 . . ?
C39 C40 H40B 110.4 . . ?
C41 C40 H40B 110.4 . . ?
H40A C40 H40B 108.6 . . ?
O2 C41 C40 104.3(3) . . ?
O2 C41 H41A 110.9 . . ?
C40 C41 H41A 110.9 . . ?
O2 C41 H41B 110.9 . . ?
C40 C41 H41B 110.9 . . ?
H41A C41 H41B 108.9 . . ?
C47 C42 C43 113.1(2) . . ?
C47 C42 B1 119.7(2) . . ?
C43 C42 B1 127.0(2) . . ?
F6 C43 C44 115.6(2) . . ?
F6 C43 C42 120.9(2) . . ?
C44 C43 C42 123.4(3) . . ?
F7 C44 C45 120.0(2) . . ?
F7 C44 C43 119.7(3) . . ?
C45 C44 C43 120.2(2) . . ?
F8 C45 C44 120.8(2) . . ?
F8 C45 C46 120.3(3) . . ?
C44 C45 C46 119.0(2) . . ?
F9 C46 C47 120.8(2) . . ?
F9 C46 C45 120.3(2) . . ?
C47 C46 C45 119.0(3) . . ?
F10 C47 C46 115.8(2) . . ?
F10 C47 C42 119.0(2) . . ?
C46 C47 C42 125.2(2) . . ?
C53 C48 C49 113.3(2) . . ?
C53 C48 B1 127.3(2) . . ?
C49 C48 B1 119.2(2) . . ?
F1 C49 C50 116.2(2) . . ?
F1 C49 C48 119.3(2) . . ?
C50 C49 C48 124.5(2) . . ?
F2 C50 C51 119.7(2) . . ?
F2 C50 C49 120.5(2) . . ?
C51 C50 C49 119.8(2) . . ?
F3 C51 C50 120.8(2) . . ?
F3 C51 C52 120.6(2) . . ?
C50 C51 C52 118.6(2) . . ?
F4 C52 C51 119.5(2) . . ?
F4 C52 C53 120.5(2) . . ?
C51 C52 C53 120.0(2) . . ?
F5 C53 C52 115.2(2) . . ?
F5 C53 C48 121.0(2) . . ?
C52 C53 C48 123.9(2) . . ?
C55 C54 C59 113.0(2) . . ?
C55 C54 B1 125.7(2) . . ?
C59 C54 B1 120.2(2) . . ?
F11 C55 C54 121.0(2) . . ?
F11 C55 C56 114.9(2) . . ?
C54 C55 C56 124.1(2) . . ?
F12 C56 C57 120.1(3) . . ?
F12 C56 C55 119.8(3) . . ?
C57 C56 C55 120.2(3) . . ?
F13 C57 C56 121.5(3) . . ?
F13 C57 C58 119.8(3) . . ?
C56 C57 C58 118.6(3) . . ?
F14 C58 C57 120.8(3) . . ?
F14 C58 C59 119.5(3) . . ?
C57 C58 C59 119.7(3) . . ?
F15 C59 C58 117.5(2) . . ?
F15 C59 C54 118.2(2) . . ?
C58 C59 C54 124.4(3) . . ?
C65 C60 C61 113.0(2) . . ?
C65 C60 B1 126.3(2) . . ?
C61 C60 B1 119.8(2) . . ?
F16 C61 C62 116.1(2) . . ?
F16 C61 C60 118.9(2) . . ?
C62 C61 C60 125.0(2) . . ?
F17 C62 C61 121.0(2) . . ?
F17 C62 C63 119.9(2) . . ?
C61 C62 C63 119.1(2) . . ?
F18 C63 C64 120.5(2) . . ?
F18 C63 C62 120.4(2) . . ?
C64 C63 C62 119.1(2) . . ?
F19 C64 C63 119.8(2) . . ?
F19 C64 C65 120.4(2) . . ?
C63 C64 C65 119.8(2) . . ?
F20 C65 C60 121.3(2) . . ?
F20 C65 C64 114.7(2) . . ?
C60 C65 C64 124.0(2) . . ?
C2 N1 C18 113.7(2) . . ?
C2 N1 Nb01 120.76(16) . . ?
C18 N1 Nb01 125.39(15) . . ?
C4 N2 C6 118.30(19) . . ?
C4 N2 Nb01 122.06(15) . . ?
C6 N2 Nb01 119.63(15) . . ?
C30 N3 Nb01 174.53(17) . . ?
C34 O1 C37 108.91(19) . . ?
C34 O1 Nb01 129.64(15) . . ?
C37 O1 Nb01 117.56(14) . . ?
C41 O2 C38 108.5(2) . . ?
C41 O2 Nb01 126.08(16) . . ?
C38 O2 Nb01 125.31(15) . . ?
N3 Nb01 N1 107.78(8) . . ?
N3 Nb01 N2 104.95(8) . . ?
N1 Nb01 N2 86.07(7) . . ?
N3 Nb01 O2 102.49(8) . . ?
N1 Nb01 O2 149.46(7) . . ?
N2 Nb01 O2 90.04(7) . . ?
N3 Nb01 O1 98.18(8) . . ?
N1 Nb01 O1 91.06(7) . . ?
N2 Nb01 O1 156.46(7) . . ?
O2 Nb01 O1 80.63(6) . . ?
C54 B1 C60 99.77(19) . . ?
C54 B1 C42 114.7(2) . . ?
C60 B1 C42 113.1(2) . . ?
C54 B1 C48 113.2(2) . . ?
C60 B1 C48 113.9(2) . . ?
C42 B1 C48 102.71(19) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 1022635'
#######################################################################
#
#                 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)
_chemical_name_common            'Complex 4'
_chemical_melting_point          ?
_chemical_formula_moiety         'C89 H98 B Cl8 F20 N6 Nb2, C6 H12 Cl6'
_chemical_formula_sum            'C95 H110 B Cl9 F20 N6 Nb2'
_chemical_formula_weight         2196.12

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'
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 '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                   20.744(2)
_cell_length_b                   20.888(2)
_cell_length_c                   22.683(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.709(2)
_cell_angle_gamma                90.00
_cell_volume                     9827.6(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9676
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.34

_exptl_crystal_description       rode
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.34
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4500
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9564
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            157286
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         25.35
_reflns_number_total             17992
_reflns_number_gt                16548
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0244P)²+10.7478P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17992
_refine_ls_number_parameters     1234
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0646
_refine_ls_wR_factor_gt          0.0620
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.02023(8) 0.09711(9) 0.37120(9) 0.0205(4) Uani 1 1 d . . .
H1A H 0.0295 0.0790 0.4093 0.031 Uiso 1 1 calc R . .
H1B H 0.0575 0.1196 0.3574 0.031 Uiso 1 1 calc R . .
H1C H 0.0092 0.0635 0.3440 0.031 Uiso 1 1 calc R . .
C2 C -0.03567(8) 0.14319(8) 0.37586(7) 0.0136(3) Uani 1 1 d . . .
C3 C -0.02062(8) 0.20021(8) 0.40771(7) 0.0148(3) Uani 1 1 d . . .
H3 H 0.0152 0.1972 0.4327 0.018 Uiso 1 1 calc R . .
C4 C -0.05075(8) 0.25929(8) 0.40741(7) 0.0126(3) Uani 1 1 d . . .
C5 C -0.01477(8) 0.31517(8) 0.43379(8) 0.0168(4) Uani 1 1 d . . .
H5A H -0.0067 0.3464 0.4037 0.025 Uiso 1 1 calc R . .
H5B H 0.0255 0.3006 0.4503 0.025 Uiso 1 1 calc R . .
H5C H -0.0402 0.3342 0.4642 0.025 Uiso 1 1 calc R . .
C6 C -0.10113(8) 0.07182(8) 0.31799(7) 0.0133(3) Uani 1 1 d . . .
C7 C -0.11426(8) 0.01453(8) 0.34816(8) 0.0163(4) Uani 1 1 d . . .
C8 C -0.12519(9) -0.04068(9) 0.31490(8) 0.0206(4) Uani 1 1 d . . .
H8 H -0.1339 -0.0790 0.3341 0.025 Uiso 1 1 calc R . .
C9 C -0.12332(9) -0.03966(9) 0.25413(9) 0.0233(4) Uani 1 1 d . . .
H9 H -0.1319 -0.0767 0.2327 0.028 Uiso 1 1 calc R . .
C10 C -0.10870(9) 0.01664(9) 0.22530(8) 0.0208(4) Uani 1 1 d . . .
H10 H -0.1065 0.0167 0.1844 0.025 Uiso 1 1 calc R . .
C11 C -0.09720(8) 0.07340(8) 0.25614(8) 0.0160(4) Uani 1 1 d . . .
C12 C -0.07787(9) 0.13334(9) 0.22280(8) 0.0181(4) Uani 1 1 d . . .
H12 H -0.0923 0.1704 0.2455 0.022 Uiso 1 1 calc R . .
C13 C -0.10861(13) 0.13758(11) 0.16183(10) 0.0380(6) Uani 1 1 d . . .
H13A H -0.0918 0.1041 0.1374 0.057 Uiso 1 1 calc R . .
H13B H -0.0989 0.1784 0.1447 0.057 Uiso 1 1 calc R . .
H13C H -0.1545 0.1328 0.1649 0.057 Uiso 1 1 calc R . .
C14 C -0.00469(11) 0.13733(14) 0.21803(13) 0.0478(7) Uani 1 1 d . . .
H14A H 0.0142 0.1393 0.2568 0.072 Uiso 1 1 calc R . .
H14B H 0.0067 0.1750 0.1963 0.072 Uiso 1 1 calc R . .
H14C H 0.0110 0.1001 0.1979 0.072 Uiso 1 1 calc R . .
C15 C -0.11606(9) 0.00907(8) 0.41498(8) 0.0200(4) Uani 1 1 d . . .
H15 H -0.1075 0.0516 0.4316 0.024 Uiso 1 1 calc R . .
C16 C -0.06339(10) -0.03676(10) 0.43778(9) 0.0286(5) Uani 1 1 d . . .
H16A H -0.0730 -0.0795 0.4249 0.043 Uiso 1 1 calc R . .
H16B H -0.0619 -0.0355 0.4801 0.043 Uiso 1 1 calc R . .
H16C H -0.0224 -0.0239 0.4225 0.043 Uiso 1 1 calc R . .
C17 C -0.18186(10) -0.01326(10) 0.43688(9) 0.0287(4) Uani 1 1 d . . .
H17A H -0.2139 0.0183 0.4271 0.043 Uiso 1 1 calc R . .
H17B H -0.1799 -0.0189 0.4789 0.043 Uiso 1 1 calc R . .
H17C H -0.1930 -0.0532 0.4184 0.043 Uiso 1 1 calc R . .
C18 C -0.12089(8) 0.33388(8) 0.36034(7) 0.0124(3) Uani 1 1 d . . .
C19 C -0.15644(8) 0.37856(8) 0.39311(8) 0.0149(3) Uani 1 1 d . . .
C20 C -0.15837(9) 0.44188(8) 0.37301(8) 0.0194(4) Uani 1 1 d . . .
H20 H -0.1822 0.4720 0.3937 0.023 Uiso 1 1 calc R . .
C21 C -0.12574(9) 0.46073(9) 0.32312(9) 0.0225(4) Uani 1 1 d . . .
H21 H -0.1264 0.5034 0.3113 0.027 Uiso 1 1 calc R . .
C22 C -0.09216(9) 0.41591(9) 0.29085(8) 0.0192(4) Uani 1 1 d . . .
H22 H -0.0708 0.4288 0.2571 0.023 Uiso 1 1 calc R . .
C23 C -0.08971(8) 0.35184(8) 0.30793(7) 0.0147(3) Uani 1 1 d . . .
C24 C -0.05276(8) 0.30464(9) 0.27021(8) 0.0162(4) Uani 1 1 d . . .
H24 H -0.0612 0.2615 0.2852 0.019 Uiso 1 1 calc R . .
C25 C 0.02002(9) 0.31642(11) 0.27377(9) 0.0279(5) Uani 1 1 d . . .
H25A H 0.0296 0.3578 0.2578 0.042 Uiso 1 1 calc R . .
H25B H 0.0420 0.2841 0.2516 0.042 Uiso 1 1 calc R . .
H25C H 0.0341 0.3147 0.3142 0.042 Uiso 1 1 calc R . .
C26 C -0.07524(9) 0.30713(9) 0.20571(8) 0.0213(4) Uani 1 1 d . . .
H26A H -0.1202 0.2965 0.2032 0.032 Uiso 1 1 calc R . .
H26B H -0.0509 0.2770 0.1831 0.032 Uiso 1 1 calc R . .
H26C H -0.0687 0.3495 0.1904 0.032 Uiso 1 1 calc R . .
C27 C -0.19204(8) 0.36326(8) 0.44969(8) 0.0155(3) Uani 1 1 d . . .
H27 H -0.1900 0.3169 0.4563 0.019 Uiso 1 1 calc R . .
C28 C -0.16174(9) 0.39702(9) 0.50341(8) 0.0217(4) Uani 1 1 d . . .
H28A H -0.1633 0.4425 0.4976 0.033 Uiso 1 1 calc R . .
H28B H -0.1177 0.3837 0.5080 0.033 Uiso 1 1 calc R . .
H28C H -0.1852 0.3859 0.5381 0.033 Uiso 1 1 calc R . .
C29 C -0.26314(9) 0.38303(9) 0.44464(9) 0.0213(4) Uani 1 1 d . . .
H29A H -0.2662 0.4289 0.4431 0.032 Uiso 1 1 calc R . .
H29B H -0.2860 0.3675 0.4783 0.032 Uiso 1 1 calc R . .
H29C H -0.2818 0.3651 0.4094 0.032 Uiso 1 1 calc R . .
C30 C -0.14744(9) 0.16633(9) 0.52166(7) 0.0175(4) Uani 1 1 d . . .
C31 C -0.21408(11) 0.15473(12) 0.54749(9) 0.0363(5) Uani 1 1 d . . .
H31A H -0.2416 0.1905 0.5385 0.055 Uiso 1 1 calc R . .
H31B H -0.2103 0.1500 0.5895 0.055 Uiso 1 1 calc R . .
H31C H -0.2323 0.1165 0.5308 0.055 Uiso 1 1 calc R . .
C32 C -0.10262(12) 0.11095(11) 0.53732(9) 0.0342(5) Uani 1 1 d . . .
H32A H -0.1223 0.0713 0.5255 0.051 Uiso 1 1 calc R . .
H32B H -0.0948 0.1105 0.5791 0.051 Uiso 1 1 calc R . .
H32C H -0.0625 0.1161 0.5172 0.051 Uiso 1 1 calc R . .
C33 C -0.11947(13) 0.22877(10) 0.54499(9) 0.0362(5) Uani 1 1 d . . .
H33A H -0.0776 0.2355 0.5284 0.054 Uiso 1 1 calc R . .
H33B H -0.1157 0.2266 0.5872 0.054 Uiso 1 1 calc R . .
H33C H -0.1474 0.2636 0.5341 0.054 Uiso 1 1 calc R . .
C34 C -0.48899(9) 0.29767(9) 0.24285(8) 0.0206(4) Uani 1 1 d . . .
H34A H -0.4885 0.3354 0.2670 0.031 Uiso 1 1 calc R . .
H34B H -0.5325 0.2827 0.2382 0.031 Uiso 1 1 calc R . .
H34C H -0.4717 0.3076 0.2049 0.031 Uiso 1 1 calc R . .
C35 C -0.44847(8) 0.24632(8) 0.27193(7) 0.0140(3) Uani 1 1 d . . .
C36 C -0.47346(8) 0.18478(8) 0.27218(8) 0.0151(3) Uani 1 1 d . . .
H36 H -0.5080 0.1783 0.2463 0.018 Uiso 1 1 calc R . .
C37 C -0.45509(8) 0.12988(8) 0.30535(7) 0.0142(3) Uani 1 1 d . . .
C38 C -0.50749(9) 0.07989(9) 0.30946(9) 0.0217(4) Uani 1 1 d . . .
H38A H -0.5152 0.0614 0.2713 0.032 Uiso 1 1 calc R . .
H38B H -0.5464 0.0995 0.3232 0.032 Uiso 1 1 calc R . .
H38C H -0.4942 0.0470 0.3366 0.032 Uiso 1 1 calc R . .
C39 C -0.38768(8) 0.06645(8) 0.36851(8) 0.0140(3) Uani 1 1 d . . .
C40 C -0.39674(8) 0.07083(9) 0.42968(8) 0.0172(4) Uani 1 1 d . . .
C41 C -0.38566(10) 0.01583(10) 0.46344(9) 0.0247(4) Uani 1 1 d . . .
H41 H -0.3911 0.0177 0.5040 0.030 Uiso 1 1 calc R . .
C42 C -0.36688(10) -0.04110(10) 0.43824(9) 0.0281(4) Uani 1 1 d . . .
H42 H -0.3596 -0.0770 0.4617 0.034 Uiso 1 1 calc R . .
C042 C 0.63952(8) 0.85041(8) 0.80610(7) 0.0133(3) Uani 1 1 d . . .
C43 C -0.35901(9) -0.04453(9) 0.37804(9) 0.0234(4) Uani 1 1 d . . .
H43 H -0.3464 -0.0831 0.3612 0.028 Uiso 1 1 calc R . .
C44 C -0.36947(8) 0.00843(8) 0.34180(8) 0.0166(4) Uani 1 1 d . . .
C45 C -0.36316(9) -0.00099(9) 0.27550(8) 0.0198(4) Uani 1 1 d . . .
H45 H -0.3685 0.0407 0.2562 0.024 Uiso 1 1 calc R . .
C46 C -0.41597(10) -0.04655(11) 0.25180(10) 0.0323(5) Uani 1 1 d . . .
H46A H -0.4086 -0.0888 0.2671 0.049 Uiso 1 1 calc R . .
H46B H -0.4147 -0.0476 0.2095 0.049 Uiso 1 1 calc R . .
H46C H -0.4575 -0.0316 0.2641 0.049 Uiso 1 1 calc R . .
C47 C -0.29715(9) -0.02833(9) 0.25895(9) 0.0242(4) Uani 1 1 d . . .
H47A H -0.2637 -0.0004 0.2733 0.036 Uiso 1 1 calc R . .
H47B H -0.2945 -0.0318 0.2168 0.036 Uiso 1 1 calc R . .
H47C H -0.2919 -0.0699 0.2764 0.036 Uiso 1 1 calc R . .
C48 C -0.42187(9) 0.13087(9) 0.45951(8) 0.0185(4) Uani 1 1 d . . .
H48 H -0.4081 0.1678 0.4361 0.022 Uiso 1 1 calc R . .
C49 C -0.49562(10) 0.13094(12) 0.46044(11) 0.0376(5) Uani 1 1 d . . .
H49A H -0.5122 0.1328 0.4208 0.056 Uiso 1 1 calc R . .
H49B H -0.5104 0.1675 0.4820 0.056 Uiso 1 1 calc R . .
H49C H -0.5106 0.0925 0.4791 0.056 Uiso 1 1 calc R . .
C50 C -0.39500(12) 0.13947(11) 0.52181(9) 0.0335(5) Uani 1 1 d . . .
H50A H -0.4135 0.1079 0.5473 0.050 Uiso 1 1 calc R . .
H50B H -0.4056 0.1815 0.5359 0.050 Uiso 1 1 calc R . .
H50C H -0.3490 0.1344 0.5215 0.050 Uiso 1 1 calc R . .
C51 C -0.38483(8) 0.32724(8) 0.31856(7) 0.0138(3) Uani 1 1 d . . .
C52 C -0.41853(8) 0.34430(9) 0.36981(8) 0.0165(4) Uani 1 1 d . . .
C53 C -0.41928(9) 0.40871(9) 0.38624(8) 0.0217(4) Uani 1 1 d . . .
H53 H -0.4420 0.4210 0.4195 0.026 Uiso 1 1 calc R . .
C54 C -0.38714(10) 0.45456(9) 0.35428(9) 0.0254(4) Uani 1 1 d . . .
H54 H -0.3883 0.4972 0.3659 0.030 Uiso 1 1 calc R . .
C55 C -0.35321(10) 0.43689(9) 0.30502(8) 0.0225(4) Uani 1 1 d . . .
H55 H -0.3308 0.4680 0.2842 0.027 Uiso 1 1 calc R . .
C56 C -0.35159(8) 0.37341(8) 0.28554(8) 0.0162(4) Uani 1 1 d . . .
C57 C -0.31630(9) 0.35970(8) 0.22862(8) 0.0172(4) Uani 1 1 d . . .
H57 H -0.3140 0.3132 0.2235 0.021 Uiso 1 1 calc R . .
C58 C -0.35201(10) 0.38815(10) 0.17502(8) 0.0266(4) Uani 1 1 d . . .
H58A H -0.3937 0.3685 0.1711 0.040 Uiso 1 1 calc R . .
H58B H -0.3276 0.3803 0.1401 0.040 Uiso 1 1 calc R . .
H58C H -0.3571 0.4334 0.1804 0.040 Uiso 1 1 calc R . .
C59 C -0.24738(9) 0.38608(9) 0.23067(9) 0.0223(4) Uani 1 1 d . . .
H59A H -0.2487 0.4320 0.2299 0.033 Uiso 1 1 calc R . .
H59B H -0.2242 0.3708 0.1971 0.033 Uiso 1 1 calc R . .
H59C H -0.2261 0.3720 0.2662 0.033 Uiso 1 1 calc R . .
C60 C -0.45490(8) 0.29639(9) 0.40707(8) 0.0181(4) Uani 1 1 d . . .
H60 H -0.4435 0.2533 0.3936 0.022 Uiso 1 1 calc R . .
C61 C -0.43520(10) 0.30204(10) 0.47214(8) 0.0236(4) Uani 1 1 d . . .
H61A H -0.3894 0.2963 0.4761 0.035 Uiso 1 1 calc R . .
H61B H -0.4570 0.2697 0.4945 0.035 Uiso 1 1 calc R . .
H61C H -0.4468 0.3436 0.4866 0.035 Uiso 1 1 calc R . .
C62 C -0.52812(9) 0.30440(11) 0.40000(10) 0.0313(5) Uani 1 1 d . . .
H62A H -0.5399 0.3475 0.4097 0.047 Uiso 1 1 calc R . .
H62B H -0.5496 0.2752 0.4259 0.047 Uiso 1 1 calc R . .
H62C H -0.5406 0.2955 0.3600 0.047 Uiso 1 1 calc R . .
C63 C -0.33074(9) 0.15796(9) 0.16104(8) 0.0186(4) Uani 1 1 d . . .
C64 C -0.39971(11) 0.16352(13) 0.13758(9) 0.0375(6) Uani 1 1 d . . .
H64A H -0.4262 0.1320 0.1563 0.056 Uiso 1 1 calc R . .
H64B H -0.4003 0.1565 0.0957 0.056 Uiso 1 1 calc R . .
H64C H -0.4161 0.2055 0.1459 0.056 Uiso 1 1 calc R . .
C65 C -0.30302(10) 0.09190(9) 0.14718(8) 0.0246(4) Uani 1 1 d . . .
H65A H -0.2625 0.0867 0.1675 0.037 Uiso 1 1 calc R . .
H65B H -0.2967 0.0881 0.1055 0.037 Uiso 1 1 calc R . .
H65C H -0.3325 0.0594 0.1599 0.037 Uiso 1 1 calc R . .
C66 C -0.28827(12) 0.21006(10) 0.13387(9) 0.0306(5) Uani 1 1 d . . .
H66A H -0.3069 0.2513 0.1411 0.046 Uiso 1 1 calc R . .
H66B H -0.2854 0.2032 0.0921 0.046 Uiso 1 1 calc R . .
H66C H -0.2459 0.2082 0.1513 0.046 Uiso 1 1 calc R . .
C67 C 0.75131(8) 0.74070(8) 0.70752(7) 0.0130(3) Uani 1 1 d . . .
C68 C 0.70268(8) 0.69797(8) 0.69165(7) 0.0145(3) Uani 1 1 d . . .
C69 C 0.70928(8) 0.65090(8) 0.64942(8) 0.0161(4) Uani 1 1 d . . .
C70 C 0.76668(9) 0.64415(9) 0.62029(8) 0.0183(4) Uani 1 1 d . . .
C71 C 0.81619(8) 0.68616(9) 0.63303(8) 0.0177(4) Uani 1 1 d . . .
C72 C 0.80732(8) 0.73294(8) 0.67491(8) 0.0148(3) Uani 1 1 d . . .
C73 C 0.68189(8) 0.80029(8) 0.79595(7) 0.0128(3) Uani 1 1 d . . .
C74 C 0.67049(8) 0.74721(8) 0.83164(7) 0.0143(3) Uani 1 1 d . . .
C75 C 0.62187(9) 0.74296(8) 0.87250(8) 0.0164(4) Uani 1 1 d . . .
C76 C 0.58115(8) 0.79432(9) 0.88017(8) 0.0168(4) Uani 1 1 d . . .
C77 C 0.59001(8) 0.84814(8) 0.84654(8) 0.0154(3) Uani 1 1 d . . .
C78 C 0.74817(8) 0.86337(8) 0.70826(7) 0.0137(3) Uani 1 1 d . . .
C79 C 0.69663(8) 0.87209(8) 0.66906(8) 0.0158(3) Uani 1 1 d . . .
C80 C 0.69333(9) 0.91947(9) 0.62681(8) 0.0202(4) Uani 1 1 d . . .
C81 C 0.74432(9) 0.96106(9) 0.62088(8) 0.0219(4) Uani 1 1 d . . .
C82 C 0.79736(9) 0.95407(9) 0.65713(8) 0.0196(4) Uani 1 1 d . . .
C83 C 0.79855(8) 0.90579(8) 0.69917(8) 0.0154(3) Uani 1 1 d . . .
C84 C 0.80506(8) 0.80156(8) 0.80391(7) 0.0130(3) Uani 1 1 d . . .
C85 C 0.84407(8) 0.75003(8) 0.81940(8) 0.0153(3) Uani 1 1 d . . .
C86 C 0.88962(8) 0.75185(9) 0.86456(8) 0.0184(4) Uani 1 1 d . . .
C87 C 0.89708(9) 0.80643(9) 0.89768(8) 0.0208(4) Uani 1 1 d . . .
C88 C 0.85844(9) 0.85853(9) 0.88564(8) 0.0193(4) Uani 1 1 d . . .
C89 C 0.81385(8) 0.85487(8) 0.84003(8) 0.0157(3) Uani 1 1 d . . .
C90 C 0.37401(11) 0.42525(11) 0.50815(9) 0.0339(5) Uani 1 1 d . . .
H90A H 0.4127 0.4257 0.5325 0.041 Uiso 1 1 calc R . .
H90B H 0.3773 0.3903 0.4802 0.041 Uiso 1 1 calc R . .
C91 C 0.36673(11) 0.48745(10) 0.47630(10) 0.0313(5) Uani 1 1 d . . .
H91A H 0.3611 0.5219 0.5044 0.038 Uiso 1 1 calc R . .
H91B H 0.3290 0.4861 0.4506 0.038 Uiso 1 1 calc R . .
C94 C 0.00081(11) 0.00568(11) 0.03256(9) 0.0317(5) Uani 1 1 d . . .
H94A H -0.0007 0.0513 0.0406 0.038 Uiso 1 1 calc R . .
H94B H 0.0404 -0.0114 0.0495 0.038 Uiso 1 1 calc R . .
N1 N -0.09296(7) 0.13126(7) 0.35175(6) 0.0117(3) Uani 1 1 d . . .
N2 N -0.11029(6) 0.26878(6) 0.38248(6) 0.0112(3) Uani 1 1 d . . .
N3 N -0.15598(6) 0.17147(7) 0.45773(6) 0.0116(3) Uani 1 1 d . . .
N4 N -0.39057(7) 0.26122(7) 0.29770(6) 0.0121(3) Uani 1 1 d . . .
N5 N -0.39779(7) 0.12320(7) 0.33144(6) 0.0119(3) Uani 1 1 d . . .
N6 N -0.33121(6) 0.16676(7) 0.22499(6) 0.0125(3) Uani 1 1 d . . .
F1 F 0.64416(5) 0.70085(5) 0.71740(4) 0.0182(2) Uani 1 1 d . . .
F2 F 0.65966(5) 0.61182(5) 0.63533(5) 0.0209(2) Uani 1 1 d . . .
F3 F 0.77368(5) 0.59863(6) 0.57914(5) 0.0279(3) Uani 1 1 d . . .
F4 F 0.87182(5) 0.68160(6) 0.60336(5) 0.0263(3) Uani 1 1 d . . .
F5 F 0.85755(5) 0.77322(5) 0.68467(4) 0.0184(2) Uani 1 1 d . . .
F6 F 0.74243(6) 1.00715(6) 0.57961(5) 0.0325(3) Uani 1 1 d . . .
F7 F 0.84834(5) 0.99353(5) 0.65109(5) 0.0274(3) Uani 1 1 d . . .
F8 F 0.85373(5) 0.90211(5) 0.73159(4) 0.0188(2) Uani 1 1 d . . .
F9 F 0.64516(5) 0.83216(5) 0.67186(4) 0.0187(2) Uani 1 1 d . . .
F10 F 0.64124(5) 0.92501(6) 0.59116(5) 0.0290(3) Uani 1 1 d . . .
F11 F 0.64487(5) 0.90672(5) 0.77701(4) 0.0170(2) Uani 1 1 d . . .
F12 F 0.55091(5) 0.89911(5) 0.85397(5) 0.0204(2) Uani 1 1 d . . .
F13 F 0.53423(5) 0.79177(5) 0.92039(5) 0.0252(2) Uani 1 1 d . . .
F14 F 0.61406(5) 0.68972(5) 0.90491(5) 0.0238(2) Uani 1 1 d . . .
F15 F 0.70952(5) 0.69539(5) 0.82760(5) 0.0179(2) Uani 1 1 d . . .
F16 F 0.83939(5) 0.69344(5) 0.79075(4) 0.0176(2) Uani 1 1 d . . .
F17 F 0.92641(5) 0.70002(5) 0.87665(5) 0.0256(2) Uani 1 1 d . . .
F18 F 0.94192(6) 0.80915(6) 0.94089(5) 0.0322(3) Uani 1 1 d . . .
F19 F 0.86482(6) 0.91205(5) 0.91810(5) 0.0283(3) Uani 1 1 d . . .
F20 F 0.77705(5) 0.90744(5) 0.83091(4) 0.0187(2) Uani 1 1 d . . .
Cl1 Cl -0.244111(18) 0.102533(18) 0.339635(18) 0.01347(8) Uani 1 1 d . . .
Cl2 Cl -0.214972(18) 0.238578(19) 0.280990(17) 0.01420(8) Uani 1 1 d . . .
Cl3 Cl -0.284735(18) 0.229710(19) 0.406783(17) 0.01391(8) Uani 1 1 d . . .
Cl4 Cl 0.30418(3) 0.41490(3) 0.55316(2) 0.03547(12) Uani 1 1 d . . .
Cl5 Cl 0.43805(3) 0.50137(3) 0.43343(2) 0.03436(12) Uani 1 1 d . . .
Nb1 Nb -0.172698(7) 0.190379(7) 0.383899(6) 0.00862(4) Uani 1 1 d . . .
Nb2 Nb -0.322251(7) 0.187078(7) 0.299535(6) 0.00905(4) Uani 1 1 d . . .
B1 B 0.74649(9) 0.80150(9) 0.75359(8) 0.0124(4) Uani 1 1 d . . .
C92 C 0.24673(12) 0.24747(13) 0.51520(12) 0.0450(6) Uani 1 1 d . . .
H92A H 0.2588 0.2627 0.5542 0.054 Uiso 1 1 calc R A 1
H92B H 0.2163 0.2779 0.4985 0.054 Uiso 1 1 calc R A 1
Cl7A Cl 0.31615(3) 0.24649(4) 0.47101(3) 0.05586(18) Uani 1 1 d . B .
Cl6A Cl 0.17171(4) 0.16456(4) 0.45452(3) 0.0385(3) Uani 0.765(2) 1 d P B 1
C93A C 0.21354(15) 0.18418(14) 0.52137(13) 0.0337(7) Uani 0.765(2) 1 d P B 1
H93A H 0.1832 0.1861 0.5536 0.040 Uiso 0.765(2) 1 calc PR B 1
H93B H 0.2451 0.1512 0.5304 0.040 Uiso 0.765(2) 1 calc PR B 1
C93B C 0.2192(5) 0.1837(6) 0.4727(5) 0.047(3) Uani 0.235(2) 1 d P B 2
H93C H 0.2424 0.1446 0.4818 0.057 Uiso 0.235(2) 1 calc PR B 2
H93D H 0.2222 0.1927 0.4309 0.057 Uiso 0.235(2) 1 calc PR B 2
Cl6B Cl 0.13901(14) 0.17991(13) 0.49551(13) 0.0455(10) Uani 0.235(2) 1 d P B 2
Cl8 Cl -0.06738(3) -0.03328(3) 0.06454(3) 0.03812(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.512(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.326(2) . ?
C2 C3 1.426(2) . ?
C3 C4 1.383(2) . ?
C3 H3 0.9300 . ?
C4 N2 1.366(2) . ?
C4 C5 1.505(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C11 1.407(2) . ?
C6 C7 1.407(2) . ?
C6 N1 1.467(2) . ?
C7 C8 1.395(3) . ?
C7 C15 1.521(2) . ?
C8 C9 1.379(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.381(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.519(2) . ?
C12 C13 1.518(3) . ?
C12 C14 1.525(3) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C17 1.531(3) . ?
C15 C16 1.537(3) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.407(2) . ?
C18 C23 1.411(2) . ?
C18 N2 1.465(2) . ?
C19 C20 1.399(2) . ?
C19 C27 1.523(2) . ?
C20 C21 1.383(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.394(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.519(2) . ?
C24 C25 1.531(2) . ?
C24 C26 1.531(2) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C29 1.534(2) . ?
C27 C28 1.536(2) . ?
C27 H27 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 N3 1.463(2) . ?
C30 C33 1.520(3) . ?
C30 C32 1.523(3) . ?
C30 C31 1.527(3) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.509(2) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N4 1.365(2) . ?
C35 C36 1.386(2) . ?
C36 C37 1.421(2) . ?
C36 H36 0.9300 . ?
C37 N5 1.329(2) . ?
C37 C38 1.511(2) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.405(2) . ?
C39 C44 1.409(2) . ?
C39 N5 1.467(2) . ?
C40 C41 1.398(3) . ?
C40 C48 1.520(3) . ?
C41 C42 1.378(3) . ?
C41 H41 0.9300 . ?
C42 C43 1.379(3) . ?
C42 H42 0.9300 . ?
C042 F11 1.3538(19) . ?
C042 C77 1.386(2) . ?
C042 C73 1.388(2) . ?
C43 C44 1.394(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.524(3) . ?
C45 C47 1.535(3) . ?
C45 C46 1.543(3) . ?
C45 H45 0.9800 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 C50 1.523(3) . ?
C48 C49 1.530(3) . ?
C48 H48 0.9800 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 C56 1.407(3) . ?
C51 C52 1.410(2) . ?
C51 N4 1.462(2) . ?
C52 C53 1.396(3) . ?
C52 C60 1.517(3) . ?
C53 C54 1.378(3) . ?
C53 H53 0.9300 . ?
C54 C55 1.378(3) . ?
C54 H54 0.9300 . ?
C55 C56 1.398(3) . ?
C55 H55 0.9300 . ?
C56 C57 1.519(2) . ?
C57 C59 1.532(2) . ?
C57 C58 1.535(2) . ?
C57 H57 0.9800 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 C61 1.531(3) . ?
C60 C62 1.534(3) . ?
C60 H60 0.9800 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 N6 1.462(2) . ?
C63 C64 1.525(3) . ?
C63 C65 1.529(3) . ?
C63 C66 1.534(3) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 C68 1.391(2) . ?
C67 C72 1.394(2) . ?
C67 B1 1.649(2) . ?
C68 F1 1.355(2) . ?
C68 C69 1.381(2) . ?
C69 F2 1.349(2) . ?
C69 C70 1.376(3) . ?
C70 F3 1.342(2) . ?
C70 C71 1.379(3) . ?
C71 F4 1.346(2) . ?
C71 C72 1.377(3) . ?
C72 F5 1.355(2) . ?
C73 C74 1.395(2) . ?
C73 B1 1.659(2) . ?
C74 F15 1.356(2) . ?
C74 C75 1.381(2) . ?
C75 F14 1.344(2) . ?
C75 C76 1.378(3) . ?
C76 F13 1.343(2) . ?
C76 C77 1.372(3) . ?
C77 F12 1.350(2) . ?
C78 C83 1.388(2) . ?
C78 C79 1.394(2) . ?
C78 B1 1.652(2) . ?
C79 F9 1.357(2) . ?
C79 C80 1.379(3) . ?
C80 F10 1.347(2) . ?
C80 C81 1.377(3) . ?
C81 F6 1.343(2) . ?
C81 C82 1.373(3) . ?
C82 F7 1.349(2) . ?
C82 C83 1.388(3) . ?
C83 F8 1.355(2) . ?
C84 C85 1.389(2) . ?
C84 C89 1.393(2) . ?
C84 B1 1.657(2) . ?
C85 F16 1.352(2) . ?
C85 C86 1.386(2) . ?
C86 F17 1.351(2) . ?
C86 C87 1.373(3) . ?
C87 F18 1.344(2) . ?
C87 C88 1.377(3) . ?
C88 F19 1.344(2) . ?
C88 C89 1.381(2) . ?
C89 F20 1.352(2) . ?
C90 C91 1.493(3) . ?
C90 Cl4 1.796(2) . ?
C90 H90A 0.9700 . ?
C90 H90B 0.9700 . ?
C91 Cl5 1.804(2) . ?
C91 H91A 0.9700 . ?
C91 H91B 0.9700 . ?
C94 C94 1.496(4) 3 ?
C94 Cl8 1.793(2) . ?
C94 H94A 0.9700 . ?
C94 H94B 0.9700 . ?
N1 Nb1 2.1959(14) . ?
N2 Nb1 2.0880(14) . ?
N3 Nb1 1.7512(14) . ?
N4 Nb2 2.0993(14) . ?
N5 Nb2 2.1880(14) . ?
N6 Nb2 1.7509(14) . ?
Cl1 Nb1 2.5559(4) . ?
Cl1 Nb2 2.5567(4) . ?
Cl2 Nb2 2.5119(5) . ?
Cl2 Nb1 2.6797(5) . ?
Cl3 Nb1 2.5249(5) . ?
Cl3 Nb2 2.6963(5) . ?
C92 C93A 1.498(4) . ?
C92 C93B 1.736(14) . ?
C92 Cl7A 1.765(3) . ?
C92 H92A 0.9700 . ?
C92 H92B 0.9700 . ?
Cl6A C93A 1.785(3) . ?
C93A H93A 0.9700 . ?
C93A H93B 0.9700 . ?
C93B Cl6B 1.749(11) . ?
C93B H93C 0.9700 . ?
C93B H93D 0.9700 . ?

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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 123.75(15) . . ?
N1 C2 C1 122.41(15) . . ?
C3 C2 C1 113.83(15) . . ?
C4 C3 C2 130.30(15) . . ?
C4 C3 H3 114.8 . . ?
C2 C3 H3 114.9 . . ?
N2 C4 C3 122.51(15) . . ?
N2 C4 C5 119.55(15) . . ?
C3 C4 C5 117.90(15) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 121.27(16) . . ?
C11 C6 N1 119.53(15) . . ?
C7 C6 N1 119.19(15) . . ?
C8 C7 C6 118.11(16) . . ?
C8 C7 C15 118.11(16) . . ?
C6 C7 C15 123.77(16) . . ?
C9 C8 C7 121.41(17) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 119.69(17) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C9 C10 C11 121.55(17) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C6 117.93(16) . . ?
C10 C11 C12 119.67(16) . . ?
C6 C11 C12 122.33(16) . . ?
C13 C12 C11 113.02(16) . . ?
C13 C12 C14 109.84(19) . . ?
C11 C12 C14 110.45(16) . . ?
C13 C12 H12 107.8 . . ?
C11 C12 H12 107.8 . . ?
C14 C12 H12 107.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 C17 112.29(16) . . ?
C7 C15 C16 110.85(16) . . ?
C17 C15 C16 109.51(16) . . ?
C7 C15 H15 108.0 . . ?
C17 C15 H15 108.0 . . ?
C16 C15 H15 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 121.15(15) . . ?
C19 C18 N2 120.78(15) . . ?
C23 C18 N2 117.84(15) . . ?
C20 C19 C18 117.88(16) . . ?
C20 C19 C27 117.44(16) . . ?
C18 C19 C27 124.66(15) . . ?
C21 C20 C19 121.56(17) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C22 C21 C20 119.70(17) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.33(17) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C18 118.28(16) . . ?
C22 C23 C24 118.91(16) . . ?
C18 C23 C24 122.80(15) . . ?
C23 C24 C25 111.72(15) . . ?
C23 C24 C26 111.50(15) . . ?
C25 C24 C26 109.49(15) . . ?
C23 C24 H24 108.0 . . ?
C25 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 C29 110.87(15) . . ?
C19 C27 C28 111.98(14) . . ?
C29 C27 C28 108.62(15) . . ?
C19 C27 H27 108.4 . . ?
C29 C27 H27 108.4 . . ?
C28 C27 H27 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C33 108.85(14) . . ?
N3 C30 C32 110.67(15) . . ?
C33 C30 C32 109.95(17) . . ?
N3 C30 C31 107.04(15) . . ?
C33 C30 C31 110.25(18) . . ?
C32 C30 C31 110.05(17) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N4 C35 C36 122.46(15) . . ?
N4 C35 C34 120.49(15) . . ?
C36 C35 C34 117.04(15) . . ?
C35 C36 C37 130.75(16) . . ?
C35 C36 H36 114.6 . . ?
C37 C36 H36 114.6 . . ?
N5 C37 C36 123.58(15) . . ?
N5 C37 C38 122.70(16) . . ?
C36 C37 C38 113.71(15) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C44 121.36(16) . . ?
C40 C39 N5 119.56(15) . . ?
C44 C39 N5 119.07(15) . . ?
C41 C40 C39 117.66(17) . . ?
C41 C40 C48 119.27(16) . . ?
C39 C40 C48 122.95(16) . . ?
C42 C41 C40 121.83(18) . . ?
C42 C41 H41 119.1 . . ?
C40 C41 H41 119.1 . . ?
C41 C42 C43 119.55(18) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
F11 C042 C77 114.71(15) . . ?
F11 C042 C73 121.24(15) . . ?
C77 C042 C73 124.04(16) . . ?
C42 C43 C44 121.55(18) . . ?
C42 C43 H43 119.2 . . ?
C44 C43 H43 119.2 . . ?
C43 C44 C39 118.03(17) . . ?
C43 C44 C45 117.71(16) . . ?
C39 C44 C45 124.21(16) . . ?
C44 C45 C47 112.16(15) . . ?
C44 C45 C46 110.75(16) . . ?
C47 C45 C46 108.48(15) . . ?
C44 C45 H45 108.5 . . ?
C47 C45 H45 108.5 . . ?
C46 C45 H45 108.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C40 C48 C50 112.74(16) . . ?
C40 C48 C49 110.81(15) . . ?
C50 C48 C49 109.97(17) . . ?
C40 C48 H48 107.7 . . ?
C50 C48 H48 107.7 . . ?
C49 C48 H48 107.7 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C56 C51 C52 121.13(16) . . ?
C56 C51 N4 120.85(15) . . ?
C52 C51 N4 117.78(15) . . ?
C53 C52 C51 118.10(17) . . ?
C53 C52 C60 118.67(16) . . ?
C51 C52 C60 123.22(16) . . ?
C54 C53 C52 121.48(18) . . ?
C54 C53 H53 119.3 . . ?
C52 C53 H53 119.3 . . ?
C53 C54 C55 119.70(17) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
C54 C55 C56 121.65(18) . . ?
C54 C55 H55 119.2 . . ?
C56 C55 H55 119.2 . . ?
C55 C56 C51 117.91(17) . . ?
C55 C56 C57 117.45(16) . . ?
C51 C56 C57 124.59(16) . . ?
C56 C57 C59 111.45(15) . . ?
C56 C57 C58 111.54(15) . . ?
C59 C57 C58 109.01(15) . . ?
C56 C57 H57 108.2 . . ?
C59 C57 H57 108.2 . . ?
C58 C57 H57 108.2 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C52 C60 C61 110.96(15) . . ?
C52 C60 C62 111.62(16) . . ?
C61 C60 C62 110.14(16) . . ?
C52 C60 H60 108.0 . . ?
C61 C60 H60 108.0 . . ?
C62 C60 H60 108.0 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N6 C63 C64 108.59(15) . . ?
N6 C63 C65 108.93(15) . . ?
C64 C63 C65 110.53(17) . . ?
N6 C63 C66 108.68(15) . . ?
C64 C63 C66 110.29(18) . . ?
C65 C63 C66 109.77(16) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C68 C67 C72 113.22(15) . . ?
C68 C67 B1 127.51(15) . . ?
C72 C67 B1 118.91(15) . . ?
F1 C68 C69 115.32(15) . . ?
F1 C68 C67 120.71(15) . . ?
C69 C68 C67 123.97(16) . . ?
F2 C69 C70 119.11(15) . . ?
F2 C69 C68 120.89(16) . . ?
C70 C69 C68 119.99(16) . . ?
F3 C70 C69 120.56(16) . . ?
F3 C70 C71 120.66(16) . . ?
C69 C70 C71 118.75(16) . . ?
F4 C71 C72 121.19(16) . . ?
F4 C71 C70 119.41(16) . . ?
C72 C71 C70 119.38(16) . . ?
F5 C72 C71 116.37(15) . . ?
F5 C72 C67 119.01(15) . . ?
C71 C72 C67 124.61(16) . . ?
C042 C73 C74 113.02(15) . . ?
C042 C73 B1 127.03(15) . . ?
C74 C73 B1 119.49(15) . . ?
F15 C74 C75 115.83(15) . . ?
F15 C74 C73 119.34(15) . . ?
C75 C74 C73 124.83(16) . . ?
F14 C75 C76 119.81(16) . . ?
F14 C75 C74 120.95(16) . . ?
C76 C75 C74 119.24(16) . . ?
F13 C76 C77 120.87(16) . . ?
F13 C76 C75 120.35(16) . . ?
C77 C76 C75 118.77(16) . . ?
F12 C77 C76 119.47(15) . . ?
F12 C77 C042 120.44(16) . . ?
C76 C77 C042 120.08(16) . . ?
C83 C78 C79 113.25(15) . . ?
C83 C78 B1 127.86(15) . . ?
C79 C78 B1 118.52(15) . . ?
F9 C79 C80 116.19(15) . . ?
F9 C79 C78 119.17(15) . . ?
C80 C79 C78 124.64(17) . . ?
F10 C80 C81 119.93(16) . . ?
F10 C80 C79 120.78(17) . . ?
C81 C80 C79 119.29(17) . . ?
F6 C81 C82 120.65(17) . . ?
F6 C81 C80 120.31(17) . . ?
C82 C81 C80 119.03(17) . . ?
F7 C82 C81 119.84(16) . . ?
F7 C82 C83 120.42(16) . . ?
C81 C82 C83 119.74(17) . . ?
F8 C83 C78 121.05(15) . . ?
F8 C83 C82 114.95(15) . . ?
C78 C83 C82 123.99(16) . . ?
C85 C84 C89 113.52(15) . . ?
C85 C84 B1 126.41(15) . . ?
C89 C84 B1 119.69(15) . . ?
F16 C85 C86 115.07(15) . . ?
F16 C85 C84 121.19(15) . . ?
C86 C85 C84 123.74(16) . . ?
F17 C86 C87 119.66(16) . . ?
F17 C86 C85 120.42(17) . . ?
C87 C86 C85 119.92(17) . . ?
F18 C87 C86 120.43(17) . . ?
F18 C87 C88 120.48(17) . . ?
C86 C87 C88 119.09(16) . . ?
F19 C88 C87 119.69(16) . . ?
F19 C88 C89 121.11(16) . . ?
C87 C88 C89 119.20(17) . . ?
F20 C89 C88 116.19(15) . . ?
F20 C89 C84 119.32(15) . . ?
C88 C89 C84 124.48(16) . . ?
C91 C90 Cl4 107.60(15) . . ?
C91 C90 H90A 110.2 . . ?
Cl4 C90 H90A 110.2 . . ?
C91 C90 H90B 110.2 . . ?
Cl4 C90 H90B 110.2 . . ?
H90A C90 H90B 108.5 . . ?
C90 C91 Cl5 108.80(15) . . ?
C90 C91 H91A 109.9 . . ?
Cl5 C91 H91A 109.9 . . ?
C90 C91 H91B 109.9 . . ?
Cl5 C91 H91B 109.9 . . ?
H91A C91 H91B 108.3 . . ?
C94 C94 Cl8 108.6(2) 3 . ?
C94 C94 H94A 110.0 3 . ?
Cl8 C94 H94A 110.0 . . ?
C94 C94 H94B 110.0 3 . ?
Cl8 C94 H94B 110.0 . . ?
H94A C94 H94B 108.3 . . ?
C2 N1 C6 118.12(14) . . ?
C2 N1 Nb1 115.62(11) . . ?
C6 N1 Nb1 124.51(10) . . ?
C4 N2 C18 114.05(13) . . ?
C4 N2 Nb1 115.93(11) . . ?
C18 N2 Nb1 129.99(10) . . ?
C30 N3 Nb1 170.01(12) . . ?
C35 N4 C51 114.90(13) . . ?
C35 N4 Nb2 115.50(11) . . ?
C51 N4 Nb2 129.58(10) . . ?
C37 N5 C39 117.44(14) . . ?
C37 N5 Nb2 115.42(11) . . ?
C39 N5 Nb2 125.76(10) . . ?
C63 N6 Nb2 170.55(12) . . ?
Nb1 Cl1 Nb2 90.325(15) . . ?
Nb2 Cl2 Nb1 88.525(14) . . ?
Nb1 Cl3 Nb2 87.889(13) . . ?
N3 Nb1 N2 94.36(6) . . ?
N3 Nb1 N1 92.85(6) . . ?
N2 Nb1 N1 88.06(5) . . ?
N3 Nb1 Cl3 92.79(5) . . ?
N2 Nb1 Cl3 108.69(4) . . ?
N1 Nb1 Cl3 161.84(4) . . ?
N3 Nb1 Cl1 108.71(5) . . ?
N2 Nb1 Cl1 155.99(4) . . ?
N1 Nb1 Cl1 84.33(4) . . ?
Cl3 Nb1 Cl1 77.519(15) . . ?
N3 Nb1 Cl2 167.58(5) . . ?
N2 Nb1 Cl2 83.58(4) . . ?
N1 Nb1 Cl2 99.31(4) . . ?
Cl3 Nb1 Cl2 76.392(14) . . ?
Cl1 Nb1 Cl2 75.268(14) . . ?
N6 Nb2 N4 95.52(6) . . ?
N6 Nb2 N5 95.95(6) . . ?
N4 Nb2 N5 88.30(5) . . ?
N6 Nb2 Cl2 91.48(5) . . ?
N4 Nb2 Cl2 106.26(4) . . ?
N5 Nb2 Cl2 162.97(4) . . ?
N6 Nb2 Cl1 103.61(5) . . ?
N4 Nb2 Cl1 160.29(4) . . ?
N5 Nb2 Cl1 85.10(4) . . ?
Cl2 Nb2 Cl1 78.248(15) . . ?
N6 Nb2 Cl3 167.78(5) . . ?
N4 Nb2 Cl3 87.79(4) . . ?
N5 Nb2 Cl3 95.91(4) . . ?
Cl2 Nb2 Cl3 76.305(14) . . ?
Cl1 Nb2 Cl3 74.485(14) . . ?
C67 B1 C78 101.89(13) . . ?
C67 B1 C84 112.80(14) . . ?
C78 B1 C84 114.04(14) . . ?
C67 B1 C73 114.28(14) . . ?
C78 B1 C73 113.32(13) . . ?
C84 B1 C73 101.06(13) . . ?
C93A C92 C93B 39.3(4) . . ?
C93A C92 Cl7A 115.0(2) . . ?
C93B C92 Cl7A 86.6(4) . . ?
C93A C92 H92A 108.5 . . ?
C93B C92 H92A 146.8 . . ?
Cl7A C92 H92A 108.5 . . ?
C93A C92 H92B 108.5 . . ?
C93B C92 H92B 94.5 . . ?
Cl7A C92 H92B 108.5 . . ?
H92A C92 H92B 107.5 . . ?
C92 C93A Cl6A 110.0(2) . . ?
C92 C93A H93A 109.7 . . ?
Cl6A C93A H93A 109.7 . . ?
C92 C93A H93B 109.7 . . ?
Cl6A C93A H93B 109.7 . . ?
H93A C93A H93B 108.2 . . ?
C92 C93B Cl6B 100.3(6) . . ?
C92 C93B H93C 111.7 . . ?
Cl6B C93B H93C 111.7 . . ?
C92 C93B H93D 111.7 . . ?
Cl6B C93B H93D 111.7 . . ?
H93C C93B H93D 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.768
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.054
_database_code_depnum_ccdc_archive 'CCDC 1022636'
#######################################################################
#
#                 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_(4)

_chemical_name_common            'Complex 6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C61 H60 B Cl0 F20 N4 Nb'
_chemical_formula_sum            'C61 H60 B Cl0 F20 N4 Nb'
_chemical_formula_weight         1332.85

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'
C C 0.0033 0.0016 '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'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Pn

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

_cell_length_a                   15.2666(6)
_cell_length_b                   16.9177(6)
_cell_length_c                   25.5770(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.658(2)
_cell_angle_gamma                90.00
_cell_volume                     6547.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9755
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.41

_exptl_crystal_description       rode
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2716
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9592
_exptl_absorpt_correction_T_max  0.9834
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            66108
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         25.44
_reflns_number_total             23491
_reflns_number_gt                19242
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX

_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)+(0.0534P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(18)
_refine_ls_number_reflns         23491
_refine_ls_number_parameters     1602
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1007
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001

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
C1 C 0.6552(3) 0.5017(3) 0.69598(15) 0.0443(12) Uani 1 1 d . . .
H1A H 0.7150 0.4986 0.6884 0.067 Uiso 1 1 calc R . .
H1B H 0.6442 0.4594 0.7193 0.067 Uiso 1 1 calc R . .
H1C H 0.6461 0.5515 0.7125 0.067 Uiso 1 1 calc R . .
C2 C 0.5934(2) 0.4950(2) 0.64592(14) 0.0261(9) Uani 1 1 d . . .
C3 C 0.5088(2) 0.4620(2) 0.64937(14) 0.0253(8) Uani 1 1 d . . .
H3 H 0.4913 0.4665 0.6827 0.030 Uiso 1 1 calc R . .
C4 C 0.4455(3) 0.4236(2) 0.61210(14) 0.0242(8) Uani 1 1 d . . .
C5 C 0.3752(3) 0.3766(2) 0.63337(15) 0.0304(9) Uani 1 1 d . . .
H5A H 0.3184 0.3912 0.6152 0.046 Uiso 1 1 calc R . .
H5B H 0.3770 0.3872 0.6704 0.046 Uiso 1 1 calc R . .
H5C H 0.3852 0.3213 0.6282 0.046 Uiso 1 1 calc R . .
C6 C 0.3921(3) 0.3768(2) 0.52437(14) 0.0282(9) Uani 1 1 d . . .
C7 C 0.3117(3) 0.4025(2) 0.49785(15) 0.0361(10) Uani 1 1 d . . .
C8 C 0.2609(3) 0.3472(3) 0.46541(16) 0.0471(12) Uani 1 1 d . . .
H8 H 0.2067 0.3625 0.4472 0.057 Uiso 1 1 calc R . .
C9 C 0.2900(3) 0.2718(3) 0.46038(18) 0.0474(12) Uani 1 1 d . . .
H9 H 0.2558 0.2364 0.4386 0.057 Uiso 1 1 calc R . .
C10 C 0.3672(3) 0.2483(3) 0.48643(16) 0.0411(11) Uani 1 1 d . . .
H10 H 0.3850 0.1962 0.4825 0.049 Uiso 1 1 calc R . .
C11 C 0.4229(3) 0.2991(2) 0.51964(16) 0.0345(10) Uani 1 1 d . . .
C12 C 0.5095(3) 0.2683(3) 0.54666(18) 0.0387(11) Uani 1 1 d . . .
H12 H 0.5390 0.3119 0.5673 0.046 Uiso 1 1 calc R . .
C13 C 0.4994(3) 0.2003(3) 0.58464(19) 0.0492(12) Uani 1 1 d . . .
H13A H 0.4627 0.2168 0.6103 0.074 Uiso 1 1 calc R . .
H13B H 0.5566 0.1854 0.6022 0.074 Uiso 1 1 calc R . .
H13C H 0.4727 0.1559 0.5653 0.074 Uiso 1 1 calc R . .
C14 C 0.5684(4) 0.2441(3) 0.5055(2) 0.0578(14) Uani 1 1 d . . .
H14A H 0.5395 0.2035 0.4833 0.087 Uiso 1 1 calc R . .
H14B H 0.6236 0.2243 0.5230 0.087 Uiso 1 1 calc R . .
H14C H 0.5791 0.2891 0.4844 0.087 Uiso 1 1 calc R . .
C15 C 0.2748(3) 0.4854(3) 0.50173(18) 0.0437(11) Uani 1 1 d . . .
H15 H 0.3166 0.5154 0.5266 0.052 Uiso 1 1 calc R . .
C16 C 0.2676(4) 0.5271(3) 0.4485(2) 0.0583(15) Uani 1 1 d . . .
H16A H 0.3231 0.5236 0.4349 0.087 Uiso 1 1 calc R . .
H16B H 0.2529 0.5817 0.4528 0.087 Uiso 1 1 calc R . .
H16C H 0.2224 0.5024 0.4243 0.087 Uiso 1 1 calc R . .
C17 C 0.1866(3) 0.4866(3) 0.52222(19) 0.0556(14) Uani 1 1 d . . .
H17A H 0.1426 0.4631 0.4966 0.083 Uiso 1 1 calc R . .
H17B H 0.1704 0.5403 0.5285 0.083 Uiso 1 1 calc R . .
H17C H 0.1907 0.4573 0.5546 0.083 Uiso 1 1 calc R . .
C18 C 0.7046(3) 0.5419(2) 0.59277(14) 0.0242(9) Uani 1 1 d . . .
C19 C 0.7327(3) 0.6197(3) 0.60103(15) 0.0341(10) Uani 1 1 d . . .
C20 C 0.8176(3) 0.6387(3) 0.59007(16) 0.0419(12) Uani 1 1 d . . .
H20 H 0.8380 0.6902 0.5956 0.050 Uiso 1 1 calc R . .
C21 C 0.8722(3) 0.5829(3) 0.57125(17) 0.0491(13) Uani 1 1 d . . .
H21 H 0.9285 0.5966 0.5645 0.059 Uiso 1 1 calc R . .
C22 C 0.8413(3) 0.5065(3) 0.56276(18) 0.0505(13) Uani 1 1 d . . .
H22 H 0.8774 0.4691 0.5498 0.061 Uiso 1 1 calc R . .
C23 C 0.7572(3) 0.4841(3) 0.57318(16) 0.0363(10) Uani 1 1 d . . .
C24 C 0.7259(3) 0.3998(3) 0.56346(18) 0.0439(12) Uani 1 1 d . . .
H24 H 0.6628 0.4021 0.5497 0.053 Uiso 1 1 calc R . .
C25 C 0.7342(4) 0.3524(3) 0.6138(2) 0.0573(14) Uani 1 1 d . . .
H25A H 0.7954 0.3474 0.6278 0.086 Uiso 1 1 calc R . .
H25B H 0.7093 0.3008 0.6065 0.086 Uiso 1 1 calc R . .
H25C H 0.7031 0.3787 0.6390 0.086 Uiso 1 1 calc R . .
C26 C 0.7724(3) 0.3581(3) 0.52185(19) 0.0523(13) Uani 1 1 d . . .
H26A H 0.8319 0.3453 0.5366 0.078 Uiso 1 1 calc R . .
H26B H 0.7735 0.3923 0.4920 0.078 Uiso 1 1 calc R . .
H26C H 0.7412 0.3104 0.5108 0.078 Uiso 1 1 calc R . .
C27 C 0.6772(3) 0.6851(3) 0.62031(18) 0.0416(11) Uani 1 1 d . . .
H27 H 0.6172 0.6650 0.6209 0.050 Uiso 1 1 calc R . .
C28 C 0.7151(4) 0.7118(3) 0.6776(2) 0.0610(15) Uani 1 1 d . . .
H28A H 0.7224 0.6663 0.7003 0.092 Uiso 1 1 calc R . .
H28B H 0.6748 0.7482 0.6906 0.092 Uiso 1 1 calc R . .
H28C H 0.7713 0.7371 0.6771 0.092 Uiso 1 1 calc R . .
C29 C 0.6722(4) 0.7567(3) 0.5836(2) 0.0655(15) Uani 1 1 d . . .
H29A H 0.7307 0.7767 0.5820 0.098 Uiso 1 1 calc R . .
H29B H 0.6369 0.7972 0.5968 0.098 Uiso 1 1 calc R . .
H29C H 0.6459 0.7413 0.5489 0.098 Uiso 1 1 calc R . .
C30 C 0.3944(3) 0.7113(2) 0.56462(17) 0.0357(10) Uani 1 1 d . . .
C31 C 0.4259(3) 0.7663(3) 0.61076(18) 0.0437(11) Uani 1 1 d . . .
H31A H 0.4893 0.7666 0.6168 0.066 Uiso 1 1 calc R . .
H31B H 0.4034 0.7479 0.6419 0.066 Uiso 1 1 calc R . .
H31C H 0.4047 0.8188 0.6026 0.066 Uiso 1 1 calc R . .
C32 C 0.2942(3) 0.7065(3) 0.55723(19) 0.0477(12) Uani 1 1 d . . .
H32A H 0.2698 0.7577 0.5478 0.072 Uiso 1 1 calc R . .
H32B H 0.2746 0.6894 0.5895 0.072 Uiso 1 1 calc R . .
H32C H 0.2748 0.6695 0.5297 0.072 Uiso 1 1 calc R . .
C33 C 0.4264(3) 0.7404(3) 0.51414(18) 0.0463(12) Uani 1 1 d . . .
H33A H 0.4897 0.7444 0.5194 0.069 Uiso 1 1 calc R . .
H33B H 0.4013 0.7914 0.5051 0.069 Uiso 1 1 calc R . .
H33C H 0.4083 0.7038 0.4861 0.069 Uiso 1 1 calc R . .
C34 C 0.5647(3) 0.5636(3) 0.44061(16) 0.0438(12) Uani 1 1 d . . .
C35 C 0.5013(4) 0.6015(3) 0.39971(18) 0.0598(15) Uani 1 1 d . . .
H35A H 0.4481 0.5706 0.3940 0.090 Uiso 1 1 calc R . .
H35B H 0.5268 0.6050 0.3674 0.090 Uiso 1 1 calc R . .
H35C H 0.4876 0.6536 0.4111 0.090 Uiso 1 1 calc R . .
C36 C 0.6525(5) 0.6092(7) 0.4516(2) 0.156(5) Uani 1 1 d . . .
H36A H 0.6823 0.6077 0.4208 0.234 Uiso 1 1 calc R . .
H36B H 0.6891 0.5853 0.4807 0.234 Uiso 1 1 calc R . .
H36C H 0.6407 0.6631 0.4600 0.234 Uiso 1 1 calc R . .
C37 C 0.5794(6) 0.4770(4) 0.4235(2) 0.111(3) Uani 1 1 d . . .
H37A H 0.5278 0.4462 0.4272 0.167 Uiso 1 1 calc R . .
H37B H 0.6295 0.4551 0.4454 0.167 Uiso 1 1 calc R . .
H37C H 0.5899 0.4763 0.3873 0.167 Uiso 1 1 calc R . .
C38 C 0.2627(3) -0.1202(2) 0.66964(16) 0.0323(9) Uani 1 1 d . . .
H38A H 0.2494 -0.1754 0.6722 0.048 Uiso 1 1 calc R . .
H38B H 0.3180 -0.1089 0.6909 0.048 Uiso 1 1 calc R . .
H38C H 0.2668 -0.1069 0.6335 0.048 Uiso 1 1 calc R . .
C39 C 0.1910(3) -0.0723(2) 0.68882(15) 0.0267(8) Uani 1 1 d . . .
C40 C 0.2103(2) -0.0350(2) 0.73875(16) 0.0314(9) Uani 1 1 d . . .
H40 H 0.2704 -0.0326 0.7510 0.038 Uiso 1 1 calc R . .
C41 C 0.1562(2) -0.0009(3) 0.77358(16) 0.0332(10) Uani 1 1 d . . .
C42 C 0.1942(3) 0.0037(4) 0.83045(19) 0.0577(15) Uani 1 1 d . . .
H42A H 0.2398 0.0433 0.8349 0.087 Uiso 1 1 calc R . .
H42B H 0.2189 -0.0466 0.8418 0.087 Uiso 1 1 calc R . .
H42C H 0.1485 0.0175 0.8512 0.087 Uiso 1 1 calc R . .
C43 C 0.0160(3) 0.0522(3) 0.79295(19) 0.0352(11) Uani 1 1 d . . .
C44 C 0.0172(3) 0.1328(3) 0.80768(18) 0.0399(11) Uani 1 1 d . . .
C45 C -0.0382(3) 0.1558(3) 0.8449(2) 0.0484(12) Uani 1 1 d . . .
H45 H -0.0381 0.2080 0.8564 0.058 Uiso 1 1 calc R . .
C46 C -0.0921(3) 0.1015(3) 0.8644(2) 0.0558(14) Uani 1 1 d . . .
H46 H -0.1269 0.1168 0.8898 0.067 Uiso 1 1 calc R . .
C47 C -0.0951(3) 0.0242(3) 0.8467(3) 0.0611(16) Uani 1 1 d . . .
H47 H -0.1343 -0.0113 0.8589 0.073 Uiso 1 1 calc R . .
C48 C -0.0406(3) -0.0006(3) 0.8111(2) 0.0495(13) Uani 1 1 d . . .
C49 C -0.0456(3) -0.0873(3) 0.7921(2) 0.0553(14) Uani 1 1 d . . .
H49 H -0.0238 -0.0867 0.7577 0.066 Uiso 1 1 calc R . .
C50 C -0.1387(3) -0.1157(3) 0.78115(19) 0.0464(12) Uani 1 1 d . . .
H50A H -0.1701 -0.1008 0.8097 0.070 Uiso 1 1 calc R . .
H50B H -0.1391 -0.1722 0.7777 0.070 Uiso 1 1 calc R . .
H50C H -0.1667 -0.0924 0.7490 0.070 Uiso 1 1 calc R . .
C51 C 0.0141(6) -0.1387(5) 0.8249(3) 0.114(3) Uiso 1 1 d . . .
H51A H -0.0075 -0.1465 0.8581 0.170 Uiso 1 1 calc R . .
H51B H 0.0717 -0.1150 0.8308 0.170 Uiso 1 1 calc R . .
H51C H 0.0176 -0.1888 0.8076 0.170 Uiso 1 1 calc R . .
C52 C 0.0722(3) 0.1954(3) 0.7851(2) 0.0475(12) Uani 1 1 d . . .
H52 H 0.0985 0.1719 0.7559 0.057 Uiso 1 1 calc R . .
C53 C 0.1469(4) 0.2250(4) 0.8261(3) 0.103(3) Uani 1 1 d . . .
H53A H 0.1227 0.2438 0.8566 0.155 Uiso 1 1 calc R . .
H53B H 0.1776 0.2673 0.8114 0.155 Uiso 1 1 calc R . .
H53C H 0.1873 0.1825 0.8362 0.155 Uiso 1 1 calc R . .
C54 C 0.0163(3) 0.2664(3) 0.7638(2) 0.0635(16) Uani 1 1 d . . .
H54A H -0.0280 0.2494 0.7359 0.095 Uiso 1 1 calc R . .
H54B H 0.0536 0.3052 0.7505 0.095 Uiso 1 1 calc R . .
H54C H -0.0118 0.2892 0.7917 0.095 Uiso 1 1 calc R . .
C55 C 0.0877(3) -0.1221(2) 0.61702(15) 0.0291(9) Uani 1 1 d . . .
C56 C 0.0863(3) -0.0977(2) 0.56445(16) 0.0370(10) Uani 1 1 d . . .
C57 C 0.0619(3) -0.1534(3) 0.52466(18) 0.0496(12) Uani 1 1 d . . .
H57 H 0.0589 -0.1381 0.4895 0.060 Uiso 1 1 calc R . .
C58 C 0.0420(3) -0.2305(3) 0.53641(18) 0.0504(13) Uani 1 1 d . . .
H58 H 0.0257 -0.2668 0.5096 0.060 Uiso 1 1 calc R . .
C59 C 0.0466(3) -0.2529(3) 0.58872(17) 0.0391(11) Uani 1 1 d . . .
H59 H 0.0349 -0.3052 0.5965 0.047 Uiso 1 1 calc R . .
C60 C 0.0679(3) -0.2005(2) 0.62970(15) 0.0304(9) Uani 1 1 d . . .
C61 C 0.0669(3) -0.2291(2) 0.68595(17) 0.0346(10) Uani 1 1 d . . .
H61 H 0.0901 -0.1865 0.7098 0.041 Uiso 1 1 calc R . .
C62 C -0.0280(3) -0.2452(3) 0.6953(2) 0.0528(13) Uani 1 1 d . . .
H62A H -0.0611 -0.1968 0.6920 0.079 Uiso 1 1 calc R . .
H62B H -0.0283 -0.2663 0.7301 0.079 Uiso 1 1 calc R . .
H62C H -0.0545 -0.2827 0.6697 0.079 Uiso 1 1 calc R . .
C63 C 0.1250(3) -0.3025(3) 0.69922(19) 0.0531(13) Uani 1 1 d . . .
H63A H 0.0999 -0.3467 0.6790 0.080 Uiso 1 1 calc R . .
H63B H 0.1279 -0.3141 0.7361 0.080 Uiso 1 1 calc R . .
H63C H 0.1834 -0.2924 0.6908 0.080 Uiso 1 1 calc R . .
C64 C 0.1117(3) -0.0151(3) 0.54815(17) 0.0440(12) Uani 1 1 d . . .
H64 H 0.1257 0.0166 0.5803 0.053 Uiso 1 1 calc R . .
C65 C 0.0348(4) 0.0253(3) 0.5132(2) 0.0665(16) Uani 1 1 d . . .
H65A H 0.0151 -0.0080 0.4835 0.100 Uiso 1 1 calc R . .
H65B H 0.0543 0.0751 0.5009 0.100 Uiso 1 1 calc R . .
H65C H -0.0131 0.0339 0.5333 0.100 Uiso 1 1 calc R . .
C66 C 0.1932(4) -0.0173(3) 0.52031(19) 0.0548(14) Uani 1 1 d . . .
H66A H 0.2420 -0.0382 0.5438 0.082 Uiso 1 1 calc R . .
H66B H 0.2070 0.0353 0.5099 0.082 Uiso 1 1 calc R . .
H66C H 0.1822 -0.0503 0.4896 0.082 Uiso 1 1 calc R . .
C67 C 0.1500(3) 0.2121(3) 0.6332(2) 0.0424(11) Uani 1 1 d . . .
C68 C 0.2012(3) 0.2698(3) 0.6723(2) 0.0478(12) Uani 1 1 d . . .
H68A H 0.1749 0.2709 0.7043 0.072 Uiso 1 1 calc R . .
H68B H 0.1994 0.3217 0.6571 0.072 Uiso 1 1 calc R . .
H68C H 0.2616 0.2527 0.6799 0.072 Uiso 1 1 calc R . .
C69 C 0.0568(3) 0.2390(3) 0.6175(2) 0.0465(12) Uani 1 1 d . . .
H69A H 0.0283 0.2048 0.5904 0.070 Uiso 1 1 calc R . .
H69B H 0.0569 0.2922 0.6044 0.070 Uiso 1 1 calc R . .
H69C H 0.0254 0.2373 0.6476 0.070 Uiso 1 1 calc R . .
C70 C 0.1988(4) 0.2063(3) 0.5853(2) 0.0574(14) Uani 1 1 d . . .
H70A H 0.2582 0.1887 0.5961 0.086 Uiso 1 1 calc R . .
H70B H 0.1999 0.2572 0.5689 0.086 Uiso 1 1 calc R . .
H70C H 0.1691 0.1692 0.5606 0.086 Uiso 1 1 calc R . .
C71 C -0.1326(3) 0.0688(3) 0.63929(19) 0.0387(11) Uani 1 1 d . . .
C72 C -0.1716(3) 0.0989(3) 0.6867(2) 0.0492(12) Uani 1 1 d . . .
H72A H -0.1540 0.0650 0.7163 0.074 Uiso 1 1 calc R . .
H72B H -0.2349 0.0993 0.6790 0.074 Uiso 1 1 calc R . .
H72C H -0.1508 0.1516 0.6948 0.074 Uiso 1 1 calc R . .
C73 C -0.1661(3) -0.0140(3) 0.6240(2) 0.0601(15) Uani 1 1 d . . .
H73A H -0.1363 -0.0336 0.5959 0.090 Uiso 1 1 calc R . .
H73B H -0.2285 -0.0120 0.6125 0.090 Uiso 1 1 calc R . .
H73C H -0.1546 -0.0484 0.6540 0.090 Uiso 1 1 calc R . .
C74 C -0.1556(3) 0.1261(4) 0.5925(2) 0.0672(17) Uani 1 1 d . . .
H74A H -0.1442 0.1794 0.6044 0.101 Uiso 1 1 calc R . .
H74B H -0.2169 0.1206 0.5788 0.101 Uiso 1 1 calc R . .
H74C H -0.1199 0.1140 0.5654 0.101 Uiso 1 1 calc R . .
C75 C 0.3691(3) 0.6751(2) 0.87254(13) 0.0245(8) Uani 1 1 d . . .
C76 C 0.4222(2) 0.7019(2) 0.91755(14) 0.0224(8) Uani 1 1 d . . .
C77 C 0.3956(3) 0.7564(2) 0.95278(15) 0.0279(9) Uani 1 1 d . . .
C78 C 0.3119(3) 0.7873(2) 0.94276(16) 0.0320(10) Uani 1 1 d . . .
C79 C 0.2575(3) 0.7643(2) 0.89890(16) 0.0292(9) Uani 1 1 d . . .
C80 C 0.2865(3) 0.7101(2) 0.86534(14) 0.0251(8) Uani 1 1 d . . .
C81 C 0.4829(2) 0.6804(2) 0.80799(13) 0.0218(8) Uani 1 1 d . . .
C82 C 0.5741(2) 0.6810(2) 0.82013(13) 0.0233(8) Uani 1 1 d . . .
C83 C 0.6289(3) 0.7395(2) 0.80470(14) 0.0271(9) Uani 1 1 d . . .
C84 C 0.5912(3) 0.8017(2) 0.77520(14) 0.0270(9) Uani 1 1 d . . .
C85 C 0.5023(3) 0.8041(2) 0.76219(14) 0.0265(9) Uani 1 1 d . . .
C86 C 0.4506(2) 0.7454(2) 0.77831(14) 0.0243(8) Uani 1 1 d . . .
C87 C 0.3386(2) 0.5800(2) 0.78418(14) 0.0220(8) Uani 1 1 d . . .
C88 C 0.3406(3) 0.5789(2) 0.73045(15) 0.0265(8) Uani 1 1 d . . .
C89 C 0.2789(3) 0.5422(2) 0.69440(14) 0.0275(9) Uani 1 1 d . . .
C90 C 0.2112(3) 0.5016(2) 0.71150(16) 0.0332(10) Uani 1 1 d . . .
C91 C 0.2062(3) 0.4985(2) 0.76442(16) 0.0286(9) Uani 1 1 d . . .
C92 C 0.2691(3) 0.5369(2) 0.79875(14) 0.0262(8) Uani 1 1 d . . .
C93 C 0.4606(2) 0.5378(2) 0.85805(13) 0.0196(8) Uani 1 1 d . . .
C94 C 0.5112(2) 0.4922(2) 0.82887(13) 0.0222(8) Uani 1 1 d . . .
C95 C 0.5553(2) 0.4237(2) 0.84605(14) 0.0232(8) Uani 1 1 d . . .
C96 C 0.5464(2) 0.3968(2) 0.89621(14) 0.0238(8) Uani 1 1 d . . .
C97 C 0.4960(2) 0.4382(2) 0.92709(13) 0.0221(8) Uani 1 1 d . . .
C98 C 0.4535(2) 0.5071(2) 0.90770(14) 0.0230(8) Uani 1 1 d . . .
C99 C 0.5534(2) 0.0413(2) 0.83170(14) 0.0222(8) Uani 1 1 d . . .
C100 C 0.4803(2) -0.0053(2) 0.83746(15) 0.0244(8) Uani 1 1 d . . .
C101 C 0.4813(3) -0.0754(2) 0.86332(14) 0.0250(8) Uani 1 1 d . . .
C102 C 0.5612(3) -0.1056(2) 0.88590(14) 0.0255(8) Uani 1 1 d . . .
C103 C 0.6373(3) -0.0638(2) 0.88151(15) 0.0256(9) Uani 1 1 d . . .
C104 C 0.6321(2) 0.0074(2) 0.85461(15) 0.0254(8) Uani 1 1 d . . .
C105 C 0.6297(2) 0.1774(2) 0.80101(15) 0.0233(8) Uani 1 1 d . . .
C106 C 0.6698(2) 0.2002(2) 0.85098(15) 0.0252(8) Uani 1 1 d . . .
C107 C 0.7410(3) 0.2511(2) 0.86031(16) 0.0313(9) Uani 1 1 d . . .
C108 C 0.7738(3) 0.2839(2) 0.81775(19) 0.0347(10) Uani 1 1 d . . .
C109 C 0.7379(3) 0.2646(2) 0.76741(17) 0.0308(9) Uani 1 1 d . . .
C110 C 0.6679(2) 0.2132(2) 0.76013(15) 0.0243(8) Uani 1 1 d . . .
C111 C 0.4682(2) 0.1837(2) 0.81464(14) 0.0209(8) Uani 1 1 d . . .
C112 C 0.4416(2) 0.2499(2) 0.78306(14) 0.0237(8) Uani 1 1 d . . .
C113 C 0.3880(2) 0.3097(2) 0.79698(14) 0.0247(8) Uani 1 1 d . . .
C114 C 0.3582(2) 0.3071(2) 0.84530(15) 0.0248(8) Uani 1 1 d . . .
C115 C 0.3825(2) 0.2445(2) 0.87821(14) 0.0261(9) Uani 1 1 d . . .
C116 C 0.4358(2) 0.1861(2) 0.86258(14) 0.0240(8) Uani 1 1 d . . .
C117 C 0.5127(3) 0.0840(2) 0.73583(15) 0.0258(8) Uani 1 1 d . . .
C118 C 0.4292(3) 0.0844(2) 0.70653(14) 0.0258(8) Uani 1 1 d . . .
C119 C 0.4100(3) 0.0448(2) 0.65937(16) 0.0317(9) Uani 1 1 d . . .
C120 C 0.4721(3) 0.0025(2) 0.63922(16) 0.0355(10) Uani 1 1 d . . .
C121 C 0.5558(3) -0.0017(2) 0.66701(17) 0.0348(10) Uani 1 1 d . . .
C122 C 0.5739(3) 0.0395(2) 0.71368(16) 0.0277(9) Uani 1 1 d . . .
N1 N 0.6153(2) 0.51951(19) 0.59915(12) 0.0248(7) Uani 1 1 d . . .
N2 N 0.4469(2) 0.43015(18) 0.55939(12) 0.0212(7) Uani 1 1 d . . .
N3 N 0.4321(2) 0.6312(2) 0.57711(14) 0.0279(8) Uani 1 1 d . . .
N4 N 0.5274(2) 0.55945(19) 0.49097(12) 0.0301(8) Uani 1 1 d . . .
N5 N 0.1110(2) -0.06698(19) 0.65894(12) 0.0243(7) Uani 1 1 d . . .
N6 N 0.0752(2) 0.02671(19) 0.75621(14) 0.0317(8) Uani 1 1 d . . .
N7 N 0.1486(3) 0.1343(2) 0.65912(15) 0.0343(9) Uani 1 1 d . . .
N8 N -0.0364(2) 0.0642(2) 0.65255(14) 0.0317(8) Uani 1 1 d . . .
F1 F 0.50528(14) 0.67338(12) 0.92885(8) 0.0272(5) Uani 1 1 d . . .
F2 F 0.45049(16) 0.77778(14) 0.99549(9) 0.0392(6) Uani 1 1 d . . .
F3 F 0.28407(17) 0.83988(14) 0.97632(10) 0.0452(6) Uani 1 1 d . . .
F4 F 0.17443(16) 0.79391(14) 0.88949(10) 0.0425(6) Uani 1 1 d . . .
F5 F 0.22667(14) 0.69217(13) 0.82271(8) 0.0329(5) Uani 1 1 d . . .
F6 F 0.61706(14) 0.62250(13) 0.85013(8) 0.0286(5) Uani 1 1 d . . .
F7 F 0.71647(14) 0.73573(14) 0.81846(9) 0.0358(6) Uani 1 1 d . . .
F8 F 0.64248(15) 0.86015(13) 0.76010(9) 0.0344(5) Uani 1 1 d . . .
F9 F 0.46487(15) 0.86634(13) 0.73382(8) 0.0350(5) Uani 1 1 d . . .
F10 F 0.36167(13) 0.75272(12) 0.76456(8) 0.0297(5) Uani 1 1 d . . .
F11 F 0.40674(14) 0.61642(13) 0.70880(8) 0.0298(5) Uani 1 1 d . . .
F12 F 0.28469(17) 0.54603(14) 0.64242(8) 0.0390(6) Uani 1 1 d . . .
F13 F 0.14906(17) 0.46592(14) 0.67680(9) 0.0429(6) Uani 1 1 d . . .
F14 F 0.13909(16) 0.45799(14) 0.78305(10) 0.0422(6) Uani 1 1 d . . .
F15 F 0.26032(14) 0.53133(12) 0.85121(8) 0.0283(5) Uani 1 1 d . . .
F16 F 0.52103(14) 0.51455(12) 0.77900(7) 0.0276(5) Uani 1 1 d . . .
F17 F 0.60280(15) 0.38343(13) 0.81499(8) 0.0330(5) Uani 1 1 d . . .
F18 F 0.58777(15) 0.33014(13) 0.91481(9) 0.0330(5) Uani 1 1 d . . .
F19 F 0.48606(15) 0.41185(13) 0.97518(8) 0.0328(5) Uani 1 1 d . . .
F20 F 0.40349(15) 0.54234(12) 0.94038(8) 0.0279(5) Uani 1 1 d . . .
F21 F 0.39942(13) 0.02015(12) 0.81469(8) 0.0284(5) Uani 1 1 d . . .
F22 F 0.40660(15) -0.11610(14) 0.86581(9) 0.0383(6) Uani 1 1 d . . .
F23 F 0.56636(16) -0.17461(13) 0.91217(9) 0.0371(6) Uani 1 1 d . . .
F24 F 0.71633(15) -0.09326(13) 0.90250(9) 0.0351(5) Uani 1 1 d . . .
F25 F 0.71051(13) 0.04212(12) 0.85178(10) 0.0338(5) Uani 1 1 d . . .
F26 F 0.63804(14) 0.17210(12) 0.89377(8) 0.0307(5) Uani 1 1 d . . .
F27 F 0.77573(16) 0.26990(14) 0.90950(10) 0.0434(6) Uani 1 1 d . . .
F28 F 0.84172(16) 0.33590(14) 0.82579(11) 0.0462(6) Uani 1 1 d . . .
F29 F 0.77060(15) 0.29609(14) 0.72595(10) 0.0419(6) Uani 1 1 d . . .
F30 F 0.63524(14) 0.19777(12) 0.70896(8) 0.0301(5) Uani 1 1 d . . .
F31 F 0.47016(14) 0.25706(12) 0.73528(7) 0.0275(5) Uani 1 1 d . . .
F32 F 0.36565(15) 0.37095(12) 0.76403(8) 0.0333(5) Uani 1 1 d . . .
F33 F 0.30723(14) 0.36586(13) 0.85954(9) 0.0340(5) Uani 1 1 d . . .
F34 F 0.35446(16) 0.24212(14) 0.92619(9) 0.0406(6) Uani 1 1 d . . .
F35 F 0.45669(15) 0.12778(14) 0.89832(8) 0.0333(6) Uani 1 1 d . . .
F36 F 0.36072(14) 0.12336(13) 0.72330(8) 0.0299(5) Uani 1 1 d . . .
F37 F 0.32587(16) 0.04874(14) 0.63287(9) 0.0416(6) Uani 1 1 d . . .
F38 F 0.45382(19) -0.03689(15) 0.59316(11) 0.0540(7) Uani 1 1 d . . .
F39 F 0.61966(18) -0.04451(14) 0.64804(11) 0.0500(7) Uani 1 1 d . . .
F40 F 0.65641(14) 0.03213(13) 0.73922(9) 0.0346(5) Uani 1 1 d . . .
Nb01 Nb 0.496726(19) 0.542388(19) 0.552943(12) 0.02273(8) Uani 1 1 d . . .
Nb02 Nb 0.07370(2) 0.04681(2) 0.675988(14) 0.02741(9) Uani 1 1 d . . .
B1 B 0.4124(3) 0.6175(3) 0.83078(15) 0.0212(9) Uani 1 1 d . . .
B2 B 0.5411(3) 0.1223(2) 0.79548(17) 0.0225(9) Uani 1 1 d . . .
H1 H 0.420(5) 0.623(4) 0.602(3) 0.10(3) Uiso 1 1 d . . .
H2 H 0.202(4) 0.115(4) 0.666(2) 0.09(2) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.490(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.349(5) . ?
C2 C3 1.420(5) . ?
C3 C4 1.421(5) . ?
C3 H3 0.9300 . ?
C4 N2 1.356(5) . ?
C4 C5 1.495(5) . ?
C4 Nb01 2.694(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.391(6) . ?
C6 C11 1.407(6) . ?
C6 N2 1.455(5) . ?
C7 C8 1.413(6) . ?
C7 C15 1.520(6) . ?
C8 C9 1.363(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.335(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.411(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.500(6) . ?
C12 C14 1.529(6) . ?
C12 C13 1.527(6) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C17 1.508(7) . ?
C15 C16 1.524(6) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.393(5) . ?
C18 C23 1.400(6) . ?
C18 N1 1.445(5) . ?
C19 C20 1.399(6) . ?
C19 C27 1.515(6) . ?
C20 C21 1.387(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.383(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.398(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.514(6) . ?
C24 C25 1.507(7) . ?
C24 C26 1.529(6) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C29 1.528(7) . ?
C27 C28 1.568(6) . ?
C27 H27 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 N3 1.491(5) . ?
C30 C33 1.521(6) . ?
C30 C31 1.528(6) . ?
C30 C32 1.519(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N4 1.477(5) . ?
C34 C35 1.474(7) . ?
C34 C37 1.553(8) . ?
C34 C36 1.540(8) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C39 1.496(5) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N5 1.354(5) . ?
C39 C40 1.419(5) . ?
C39 Nb02 2.686(4) . ?
C40 C41 1.417(5) . ?
C40 H40 0.9300 . ?
C41 N6 1.341(5) . ?
C41 C42 1.495(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C48 1.367(6) . ?
C43 C44 1.414(6) . ?
C43 N6 1.454(5) . ?
C44 C45 1.410(6) . ?
C44 C52 1.513(6) . ?
C45 C46 1.370(7) . ?
C45 H45 0.9300 . ?
C46 C47 1.383(7) . ?
C46 H46 0.9300 . ?
C47 C48 1.378(7) . ?
C47 H47 0.9300 . ?
C48 C49 1.544(7) . ?
C49 C51 1.444(9) . ?
C49 C50 1.491(6) . ?
C49 H49 0.9800 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 C54 1.531(7) . ?
C52 C53 1.527(7) . ?
C52 H52 0.9800 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 C56 1.404(6) . ?
C55 C60 1.406(6) . ?
C55 N5 1.430(5) . ?
C56 C57 1.400(6) . ?
C56 C64 1.523(6) . ?
C57 C58 1.382(7) . ?
C57 H57 0.9300 . ?
C58 C59 1.383(6) . ?
C58 H58 0.9300 . ?
C59 C60 1.378(5) . ?
C59 H59 0.9300 . ?
C60 C61 1.520(6) . ?
C61 C62 1.525(6) . ?
C61 C63 1.536(6) . ?
C61 H61 0.9800 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C64 C66 1.514(7) . ?
C64 C65 1.538(7) . ?
C64 H64 0.9800 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 N7 1.476(6) . ?
C67 C69 1.497(6) . ?
C67 C70 1.520(6) . ?
C67 C68 1.535(6) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 N8 1.464(5) . ?
C71 C72 1.509(7) . ?
C71 C73 1.523(7) . ?
C71 C74 1.544(6) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 C80 1.383(5) . ?
C75 C76 1.393(5) . ?
C75 B1 1.648(5) . ?
C76 F1 1.352(4) . ?
C76 C77 1.388(5) . ?
C77 F2 1.335(4) . ?
C77 C78 1.372(6) . ?
C78 F3 1.344(4) . ?
C78 C79 1.360(6) . ?
C79 F4 1.354(4) . ?
C79 C80 1.370(5) . ?
C80 F5 1.360(4) . ?
C81 C86 1.388(5) . ?
C81 C82 1.386(5) . ?
C81 B1 1.672(6) . ?
C82 F6 1.366(4) . ?
C82 C83 1.387(5) . ?
C83 F7 1.338(4) . ?
C83 C84 1.375(5) . ?
C84 F8 1.349(4) . ?
C84 C85 1.354(5) . ?
C85 F9 1.361(4) . ?
C85 C86 1.366(5) . ?
C86 F10 1.363(4) . ?
C87 C88 1.379(5) . ?
C87 C92 1.379(5) . ?
C87 B1 1.654(6) . ?
C88 F11 1.370(4) . ?
C88 C89 1.375(5) . ?
C89 F12 1.346(4) . ?
C89 C90 1.361(6) . ?
C90 F13 1.352(4) . ?
C90 C91 1.367(6) . ?
C91 F14 1.370(4) . ?
C91 C92 1.375(5) . ?
C92 F15 1.369(4) . ?
C93 C94 1.379(5) . ?
C93 C98 1.390(5) . ?
C93 B1 1.646(5) . ?
C94 F16 1.358(4) . ?
C94 C95 1.382(5) . ?
C95 F17 1.332(4) . ?
C95 C96 1.385(5) . ?
C96 F18 1.348(4) . ?
C96 C97 1.366(5) . ?
C97 F19 1.336(4) . ?
C97 C98 1.393(5) . ?
C98 F20 1.344(4) . ?
C99 C100 1.391(5) . ?
C99 C104 1.390(5) . ?
C99 B2 1.650(5) . ?
C100 C101 1.356(5) . ?
C100 F21 1.363(4) . ?
C101 F22 1.341(4) . ?
C101 C102 1.377(5) . ?
C102 F23 1.344(4) . ?
C102 C103 1.378(5) . ?
C103 F24 1.349(4) . ?
C103 C104 1.384(5) . ?
C104 F25 1.344(4) . ?
C105 C106 1.396(5) . ?
C105 C110 1.400(5) . ?
C105 B2 1.634(5) . ?
C106 F26 1.342(4) . ?
C106 C107 1.382(5) . ?
C107 F27 1.337(5) . ?
C107 C108 1.374(6) . ?
C108 F28 1.355(4) . ?
C108 C109 1.369(6) . ?
C109 F29 1.341(4) . ?
C109 C110 1.372(5) . ?
C110 F30 1.362(4) . ?
C111 C116 1.383(5) . ?
C111 C112 1.409(5) . ?
C111 B2 1.644(5) . ?
C112 F31 1.356(4) . ?
C112 C113 1.377(5) . ?
C113 F32 1.351(4) . ?
C113 C114 1.374(5) . ?
C114 F33 1.342(4) . ?
C114 C115 1.373(5) . ?
C115 F34 1.353(4) . ?
C115 C116 1.373(5) . ?
C116 F35 1.354(4) . ?
C117 C122 1.380(5) . ?
C117 C118 1.390(5) . ?
C117 B2 1.661(6) . ?
C118 F36 1.353(4) . ?
C118 C119 1.376(5) . ?
C119 C120 1.345(6) . ?
C119 F37 1.372(5) . ?
C120 F38 1.349(5) . ?
C120 C121 1.378(6) . ?
C121 F39 1.355(4) . ?
C121 C122 1.379(6) . ?
C122 F40 1.345(5) . ?
N1 Nb01 2.062(3) . ?
N2 Nb01 2.060(3) . ?
N3 Nb01 1.943(4) . ?
N3 H1 0.69(6) . ?
N4 Nb01 1.736(3) . ?
N5 Nb02 2.070(3) . ?
N6 Nb02 2.077(4) . ?
N7 Nb02 1.953(3) . ?
N7 H2 0.87(6) . ?
N8 Nb02 1.733(3) . ?
Nb01 H1 2.28(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
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 120.7(3) . . ?
N1 C2 C1 122.4(3) . . ?
C3 C2 C1 117.0(3) . . ?
C2 C3 C4 132.9(3) . . ?
C2 C3 H3 113.6 . . ?
C4 C3 H3 113.6 . . ?
N2 C4 C3 122.0(3) . . ?
N2 C4 C5 120.8(3) . . ?
C3 C4 C5 117.1(3) . . ?
N2 C4 Nb01 48.40(18) . . ?
C3 C4 Nb01 79.2(2) . . ?
C5 C4 Nb01 151.3(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 122.3(4) . . ?
C7 C6 N2 120.2(4) . . ?
C11 C6 N2 117.5(4) . . ?
C6 C7 C8 117.4(4) . . ?
C6 C7 C15 124.6(4) . . ?
C8 C7 C15 118.0(4) . . ?
C9 C8 C7 121.0(4) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 122.7(4) . . ?
C9 C10 H10 118.7 . . ?
C11 C10 H10 118.7 . . ?
C6 C11 C10 116.1(4) . . ?
C6 C11 C12 124.6(4) . . ?
C10 C11 C12 119.3(4) . . ?
C11 C12 C14 109.8(4) . . ?
C11 C12 C13 113.4(4) . . ?
C14 C12 C13 110.7(4) . . ?
C11 C12 H12 107.6 . . ?
C14 C12 H12 107.6 . . ?
C13 C12 H12 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C15 C7 113.0(4) . . ?
C17 C15 C16 110.1(4) . . ?
C7 C15 C16 110.6(4) . . ?
C17 C15 H15 107.6 . . ?
C7 C15 H15 107.6 . . ?
C16 C15 H15 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 122.3(4) . . ?
C19 C18 N1 120.5(4) . . ?
C23 C18 N1 116.9(3) . . ?
C18 C19 C20 117.5(4) . . ?
C18 C19 C27 124.4(4) . . ?
C20 C19 C27 118.1(4) . . ?
C21 C20 C19 121.9(4) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C22 C21 C20 118.8(4) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
C21 C22 C23 121.8(4) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 117.6(4) . . ?
C22 C23 C24 120.1(4) . . ?
C18 C23 C24 122.2(4) . . ?
C25 C24 C23 111.9(4) . . ?
C25 C24 C26 110.8(4) . . ?
C23 C24 C26 112.5(4) . . ?
C25 C24 H24 107.1 . . ?
C23 C24 H24 107.1 . . ?
C26 C24 H24 107.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 C29 111.3(4) . . ?
C19 C27 C28 111.2(4) . . ?
C29 C27 C28 109.2(4) . . ?
C19 C27 H27 108.4 . . ?
C29 C27 H27 108.4 . . ?
C28 C27 H27 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C33 108.6(3) . . ?
N3 C30 C31 108.4(3) . . ?
C33 C30 C31 110.8(4) . . ?
N3 C30 C32 109.4(4) . . ?
C33 C30 C32 110.1(4) . . ?
C31 C30 C32 109.6(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 C35 110.3(4) . . ?
N4 C34 C37 106.7(4) . . ?
C35 C34 C37 108.4(5) . . ?
N4 C34 C36 107.0(4) . . ?
C35 C34 C36 112.6(5) . . ?
C37 C34 C36 111.7(7) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N5 C39 C40 122.8(3) . . ?
N5 C39 C38 119.7(3) . . ?
C40 C39 C38 117.5(3) . . ?
N5 C39 Nb02 49.10(18) . . ?
C40 C39 Nb02 80.3(2) . . ?
C38 C39 Nb02 150.5(3) . . ?
C41 C40 C39 132.7(3) . . ?
C41 C40 H40 113.7 . . ?
C39 C40 H40 113.7 . . ?
N6 C41 C40 121.6(4) . . ?
N6 C41 C42 121.7(4) . . ?
C40 C41 C42 116.7(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C48 C43 C44 121.8(4) . . ?
C48 C43 N6 120.1(4) . . ?
C44 C43 N6 118.1(4) . . ?
C43 C44 C45 117.2(4) . . ?
C43 C44 C52 124.2(4) . . ?
C45 C44 C52 118.6(4) . . ?
C46 C45 C44 120.3(4) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C47 120.6(4) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
C48 C47 C46 120.5(5) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C43 C48 C47 119.3(4) . . ?
C43 C48 C49 121.4(4) . . ?
C47 C48 C49 119.3(4) . . ?
C51 C49 C50 115.2(5) . . ?
C51 C49 C48 112.8(5) . . ?
C50 C49 C48 111.7(4) . . ?
C51 C49 H49 105.3 . . ?
C50 C49 H49 105.3 . . ?
C48 C49 H49 105.3 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C44 C52 C54 111.9(4) . . ?
C44 C52 C53 111.7(5) . . ?
C54 C52 C53 108.5(4) . . ?
C44 C52 H52 108.2 . . ?
C54 C52 H52 108.2 . . ?
C53 C52 H52 108.2 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 C60 121.4(4) . . ?
C56 C55 N5 119.8(4) . . ?
C60 C55 N5 118.8(3) . . ?
C57 C56 C55 117.8(4) . . ?
C57 C56 C64 118.1(4) . . ?
C55 C56 C64 124.1(4) . . ?
C58 C57 C56 121.5(4) . . ?
C58 C57 H57 119.3 . . ?
C56 C57 H57 119.3 . . ?
C57 C58 C59 119.0(4) . . ?
C57 C58 H58 120.5 . . ?
C59 C58 H58 120.5 . . ?
C60 C59 C58 122.4(4) . . ?
C60 C59 H59 118.8 . . ?
C58 C59 H59 118.8 . . ?
C59 C60 C55 117.8(4) . . ?
C59 C60 C61 118.9(4) . . ?
C55 C60 C61 123.3(3) . . ?
C60 C61 C62 109.6(4) . . ?
C60 C61 C63 112.9(4) . . ?
C62 C61 C63 110.7(4) . . ?
C60 C61 H61 107.8 . . ?
C62 C61 H61 107.8 . . ?
C63 C61 H61 107.8 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C66 C64 C56 111.2(4) . . ?
C66 C64 C65 110.4(4) . . ?
C56 C64 C65 111.3(4) . . ?
C66 C64 H64 107.9 . . ?
C56 C64 H64 107.9 . . ?
C65 C64 H64 107.9 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N7 C67 C69 108.8(4) . . ?
N7 C67 C70 110.0(4) . . ?
C69 C67 C70 110.7(4) . . ?
N7 C67 C68 108.1(4) . . ?
C69 C67 C68 111.4(4) . . ?
C70 C67 C68 107.7(4) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
N8 C71 C72 108.9(4) . . ?
N8 C71 C73 107.7(4) . . ?
C72 C71 C73 111.1(4) . . ?
N8 C71 C74 109.3(4) . . ?
C72 C71 C74 109.7(4) . . ?
C73 C71 C74 110.2(5) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C80 C75 C76 113.0(3) . . ?
C80 C75 B1 127.2(3) . . ?
C76 C75 B1 119.3(3) . . ?
F1 C76 C77 116.5(3) . . ?
F1 C76 C75 119.1(3) . . ?
C77 C76 C75 124.4(4) . . ?
F2 C77 C78 121.2(3) . . ?
F2 C77 C76 120.3(4) . . ?
C78 C77 C76 118.5(4) . . ?
F3 C78 C79 120.4(4) . . ?
F3 C78 C77 119.9(4) . . ?
C79 C78 C77 119.7(4) . . ?
F4 C79 C78 119.7(3) . . ?
F4 C79 C80 120.6(4) . . ?
C78 C79 C80 119.7(4) . . ?
F5 C80 C79 114.4(3) . . ?
F5 C80 C75 120.9(3) . . ?
C79 C80 C75 124.7(4) . . ?
C86 C81 C82 112.9(3) . . ?
C86 C81 B1 119.8(3) . . ?
C82 C81 B1 126.9(3) . . ?
F6 C82 C83 114.5(3) . . ?
F6 C82 C81 120.9(3) . . ?
C83 C82 C81 124.6(3) . . ?
F7 C83 C84 120.8(3) . . ?
F7 C83 C82 120.7(3) . . ?
C84 C83 C82 118.5(4) . . ?
F8 C84 C85 120.6(3) . . ?
F8 C84 C83 120.1(3) . . ?
C85 C84 C83 119.3(4) . . ?
F9 C85 C84 119.3(3) . . ?
F9 C85 C86 120.4(3) . . ?
C84 C85 C86 120.3(3) . . ?
F10 C86 C85 116.8(3) . . ?
F10 C86 C81 118.8(3) . . ?
C85 C86 C81 124.4(4) . . ?
C88 C87 C92 112.5(3) . . ?
C88 C87 B1 128.3(3) . . ?
C92 C87 B1 118.9(3) . . ?
F11 C88 C89 114.5(3) . . ?
F11 C88 C87 120.8(3) . . ?
C89 C88 C87 124.8(4) . . ?
F12 C89 C90 119.6(3) . . ?
F12 C89 C88 120.7(4) . . ?
C90 C89 C88 119.6(3) . . ?
F13 C90 C89 120.7(4) . . ?
F13 C90 C91 120.4(4) . . ?
C89 C90 C91 118.9(4) . . ?
C90 C91 F14 120.5(4) . . ?
C90 C91 C92 119.2(4) . . ?
F14 C91 C92 120.4(3) . . ?
F15 C92 C91 116.2(3) . . ?
F15 C92 C87 118.7(3) . . ?
C91 C92 C87 125.1(3) . . ?
C94 C93 C98 113.7(3) . . ?
C94 C93 B1 118.7(3) . . ?
C98 C93 B1 127.5(3) . . ?
F16 C94 C93 119.5(3) . . ?
F16 C94 C95 115.0(3) . . ?
C93 C94 C95 125.5(3) . . ?
F17 C95 C94 121.3(3) . . ?
F17 C95 C96 120.8(3) . . ?
C94 C95 C96 117.8(3) . . ?
F18 C96 C97 119.9(3) . . ?
F18 C96 C95 120.2(3) . . ?
C97 C96 C95 119.9(3) . . ?
F19 C97 C96 120.2(3) . . ?
F19 C97 C98 120.1(3) . . ?
C96 C97 C98 119.6(3) . . ?
F20 C98 C93 121.5(3) . . ?
F20 C98 C97 115.2(3) . . ?
C93 C98 C97 123.3(3) . . ?
C100 C99 C104 112.4(3) . . ?
C100 C99 B2 119.9(3) . . ?
C104 C99 B2 127.4(3) . . ?
C101 C100 F21 115.9(3) . . ?
C101 C100 C99 126.2(3) . . ?
F21 C100 C99 118.0(3) . . ?
F22 C101 C100 121.1(3) . . ?
F22 C101 C102 120.1(3) . . ?
C100 C101 C102 118.8(3) . . ?
F23 C102 C103 119.5(3) . . ?
F23 C102 C101 121.5(3) . . ?
C103 C102 C101 119.0(3) . . ?
F24 C103 C102 119.8(3) . . ?
F24 C103 C104 120.6(3) . . ?
C102 C103 C104 119.6(3) . . ?
F25 C104 C103 114.5(3) . . ?
F25 C104 C99 121.5(3) . . ?
C103 C104 C99 124.0(3) . . ?
C106 C105 C110 112.9(3) . . ?
C106 C105 B2 119.6(3) . . ?
C110 C105 B2 127.2(3) . . ?
F26 C106 C107 116.2(3) . . ?
F26 C106 C105 119.1(3) . . ?
C107 C106 C105 124.7(4) . . ?
F27 C107 C108 120.6(4) . . ?
F27 C107 C106 121.0(4) . . ?
C108 C107 C106 118.4(4) . . ?
F28 C108 C109 120.0(4) . . ?
F28 C108 C107 119.6(4) . . ?
C109 C108 C107 120.4(4) . . ?
F29 C109 C108 120.3(4) . . ?
F29 C109 C110 120.7(4) . . ?
C108 C109 C110 119.0(4) . . ?
F30 C110 C109 115.5(3) . . ?
F30 C110 C105 120.0(3) . . ?
C109 C110 C105 124.5(4) . . ?
C116 C111 C112 112.1(3) . . ?
C116 C111 B2 128.2(3) . . ?
C112 C111 B2 119.1(3) . . ?
F31 C112 C113 116.2(3) . . ?
F31 C112 C111 119.0(3) . . ?
C113 C112 C111 124.8(3) . . ?
F32 C113 C114 120.0(3) . . ?
F32 C113 C112 120.8(3) . . ?
C114 C113 C112 119.3(3) . . ?
F33 C114 C113 119.6(3) . . ?
F33 C114 C115 121.6(3) . . ?
C113 C114 C115 118.7(3) . . ?
F34 C115 C116 120.9(3) . . ?
F34 C115 C114 119.1(3) . . ?
C116 C115 C114 120.0(3) . . ?
F35 C116 C115 115.0(3) . . ?
F35 C116 C111 119.9(3) . . ?
C115 C116 C111 125.1(3) . . ?
C122 C117 C118 113.9(3) . . ?
C122 C117 B2 118.8(3) . . ?
C118 C117 B2 127.0(3) . . ?
F36 C118 C119 115.6(3) . . ?
F36 C118 C117 121.5(3) . . ?
C119 C118 C117 122.9(4) . . ?
C120 C119 F37 119.8(4) . . ?
C120 C119 C118 121.1(4) . . ?
F37 C119 C118 119.0(4) . . ?
C119 C120 F38 121.6(4) . . ?
C119 C120 C121 118.8(4) . . ?
F38 C120 C121 119.6(4) . . ?
F39 C121 C122 120.6(4) . . ?
F39 C121 C120 120.3(4) . . ?
C122 C121 C120 119.1(4) . . ?
F40 C122 C117 119.6(4) . . ?
F40 C122 C121 116.1(3) . . ?
C117 C122 C121 124.2(4) . . ?
C2 N1 C18 122.0(3) . . ?
C2 N1 Nb01 105.3(2) . . ?
C18 N1 Nb01 130.9(2) . . ?
C4 N2 C6 118.5(3) . . ?
C4 N2 Nb01 102.1(2) . . ?
C6 N2 Nb01 135.3(2) . . ?
C30 N3 Nb01 146.4(3) . . ?
C30 N3 H1 103(6) . . ?
Nb01 N3 H1 111(6) . . ?
C34 N4 Nb01 170.4(3) . . ?
C39 N5 C55 119.7(3) . . ?
C39 N5 Nb02 101.3(2) . . ?
C55 N5 Nb02 135.8(2) . . ?
C41 N6 C43 121.0(4) . . ?
C41 N6 Nb02 105.8(3) . . ?
C43 N6 Nb02 131.6(3) . . ?
C67 N7 Nb02 145.0(3) . . ?
C67 N7 H2 110(4) . . ?
Nb02 N7 H2 104(4) . . ?
C71 N8 Nb02 170.2(3) . . ?
N4 Nb01 N3 111.87(15) . . ?
N4 Nb01 N2 111.96(14) . . ?
N3 Nb01 N2 118.57(14) . . ?
N4 Nb01 N1 103.37(14) . . ?
N3 Nb01 N1 114.02(13) . . ?
N2 Nb01 N1 94.96(12) . . ?
N4 Nb01 C4 140.43(13) . . ?
N3 Nb01 C4 101.56(14) . . ?
N2 Nb01 C4 29.47(11) . . ?
N1 Nb01 C4 80.57(12) . . ?
N4 Nb01 H1 128.4(17) . . ?
N3 Nb01 H1 16.5(16) . . ?
N2 Nb01 H1 106.6(17) . . ?
N1 Nb01 H1 106.1(17) . . ?
C4 Nb01 H1 86.1(17) . . ?
N8 Nb02 N7 111.36(16) . . ?
N8 Nb02 N5 111.50(14) . . ?
N7 Nb02 N5 118.19(14) . . ?
N8 Nb02 N6 104.59(14) . . ?
N7 Nb02 N6 114.38(14) . . ?
N5 Nb02 N6 95.09(13) . . ?
N8 Nb02 C39 140.32(14) . . ?
N7 Nb02 C39 101.25(14) . . ?
N5 Nb02 C39 29.63(11) . . ?
N6 Nb02 C39 80.63(12) . . ?
C93 B1 C87 102.4(3) . . ?
C93 B1 C75 113.9(3) . . ?
C87 B1 C75 113.6(3) . . ?
C93 B1 C81 113.4(3) . . ?
C87 B1 C81 113.6(3) . . ?
C75 B1 C81 100.5(3) . . ?
C105 B2 C111 101.5(3) . . ?
C105 B2 C99 113.2(3) . . ?
C111 B2 C99 112.9(3) . . ?
C105 B2 C117 114.4(3) . . ?
C111 B2 C117 114.6(3) . . ?
C99 B2 C117 100.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.054

_database_code_depnum_ccdc_archive 'CCDC 1022637'
