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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1485267'
_audit_update_record             
;
2016-06-14 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            (BDI)Nb(NtBu)Cp
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H55 N3 Nb'
_chemical_formula_weight         646.76

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.2300(2)
_cell_length_b                   20.0348(6)
_cell_length_c                   33.3052(10)
_cell_angle_alpha                90
_cell_angle_beta                 89.9630(10)
_cell_angle_gamma                90
_cell_volume                     6826.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9206
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      25.36

_exptl_crystal_description       block
_exptl_crystal_colour            green-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_F_000             2760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.382
_shelx_estimated_absorpt_T_min   0.941
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8544
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            43032
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.834
_diffrn_reflns_theta_max         25.353
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12479
_reflns_number_gt                11496
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-2011
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          'Refined as a 2-component twin., Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0312P)²+4.1099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iteratibe
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12479
_refine_ls_number_parameters     784
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0107(3) 0.20515(15) 0.49845(8) 0.0271(7) Uani 1 1 d . . . . .
H1 H 0.0259 0.1623 0.4939 0.033 Uiso 1 1 calc R U . . .
C2 C 0.0484(3) 0.26630(17) 0.48997(8) 0.0253(7) Uani 1 1 d . . . . .
H2 H 0.1319 0.2722 0.4780 0.030 Uiso 1 1 calc R U . . .
C3 C -0.0361(3) 0.31750(15) 0.50211(8) 0.0248(7) Uani 1 1 d . . . . .
H3 H -0.0190 0.3640 0.5005 0.030 Uiso 1 1 calc R U . . .
C4 C -0.1505(3) 0.28787(17) 0.51708(9) 0.0247(7) Uani 1 1 d . . . . .
H4 H -0.2254 0.3107 0.5268 0.030 Uiso 1 1 calc R U . . .
C5 C -0.1344(3) 0.21843(17) 0.51503(9) 0.0283(8) Uani 1 1 d . . . . .
H5 H -0.1964 0.1860 0.5234 0.034 Uiso 1 1 calc R U . . .
C6 C -0.1966(3) 0.26790(15) 0.63587(8) 0.0173(6) Uani 1 1 d . . . . .
C7 C -0.3223(3) 0.28484(19) 0.61368(9) 0.0319(8) Uani 1 1 d . . . . .
H7A H -0.3128 0.3283 0.6005 0.048 Uiso 1 1 calc R U . . .
H7B H -0.3950 0.2867 0.6328 0.048 Uiso 1 1 calc R U . . .
H7C H -0.3400 0.2505 0.5935 0.048 Uiso 1 1 calc R U . . .
C8 C -0.1693(3) 0.32142(16) 0.66754(9) 0.0285(7) Uani 1 1 d . . . . .
H8A H -0.0854 0.3122 0.6806 0.043 Uiso 1 1 calc R U . . .
H8B H -0.2392 0.3210 0.6877 0.043 Uiso 1 1 calc R U . . .
H8C H -0.1660 0.3653 0.6546 0.043 Uiso 1 1 calc R U . . .
C9 C -0.2122(3) 0.20065(16) 0.65673(10) 0.0354(8) Uani 1 1 d . . . . .
H9A H -0.2357 0.1666 0.6369 0.053 Uiso 1 1 calc R U . . .
H9B H -0.2813 0.2038 0.6770 0.053 Uiso 1 1 calc R U . . .
H9C H -0.1297 0.1883 0.6697 0.053 Uiso 1 1 calc R U . . .
C10 C 0.3229(3) 0.13979(13) 0.63198(8) 0.0173(6) Uani 1 1 d . . . . .
H10A H 0.2871 0.0970 0.6229 0.026 Uiso 1 1 calc R U . . .
H10B H 0.3141 0.1433 0.6612 0.026 Uiso 1 1 calc R U . . .
H10C H 0.4155 0.1425 0.6246 0.026 Uiso 1 1 calc R U . . .
C11 C 0.2486(2) 0.19646(13) 0.61213(8) 0.0120(6) Uani 1 1 d . . . . .
C12 C 0.2767(3) 0.25988(14) 0.62744(9) 0.0138(6) Uani 1 1 d . . . . .
H12 H 0.3151 0.2608 0.6534 0.017 Uiso 1 1 calc R U . . .
C13 C 0.2557(2) 0.32205(13) 0.60948(8) 0.0122(6) Uani 1 1 d . . . . .
C14 C 0.3337(3) 0.37997(13) 0.62654(8) 0.0174(6) Uani 1 1 d . . . . .
H14A H 0.3938 0.3969 0.6060 0.026 Uiso 1 1 calc R U . . .
H14B H 0.3836 0.3647 0.6499 0.026 Uiso 1 1 calc R U . . .
H14C H 0.2738 0.4157 0.6347 0.026 Uiso 1 1 calc R U . . .
C15 C 0.1732(2) 0.12010(13) 0.56288(8) 0.0135(5) Uani 1 1 d . . . . .
C16 C 0.0799(3) 0.07079(13) 0.57205(8) 0.0161(6) Uani 1 1 d . . . . .
C17 C 0.0899(3) 0.00894(14) 0.55270(9) 0.0233(7) Uani 1 1 d . . . . .
H17 H 0.0282 -0.0250 0.5589 0.028 Uiso 1 1 calc R U . . .
C18 C 0.1860(3) -0.00391(14) 0.52513(9) 0.0243(7) Uani 1 1 d . . . . .
H18 H 0.1906 -0.0464 0.5125 0.029 Uiso 1 1 calc R U . . .
C19 C 0.2765(3) 0.04510(14) 0.51564(8) 0.0206(6) Uani 1 1 d . . . . .
H19 H 0.3418 0.0363 0.4961 0.025 Uiso 1 1 calc R U . . .
C20 C 0.2729(3) 0.10730(13) 0.53451(8) 0.0162(6) Uani 1 1 d . . . . .
C21 C -0.0265(3) 0.08142(13) 0.60325(8) 0.0196(6) Uani 1 1 d . . . . .
H21 H -0.0295 0.1301 0.6099 0.024 Uiso 1 1 calc R U . . .
C22 C -0.1617(3) 0.06080(16) 0.58761(9) 0.0264(7) Uani 1 1 d . . . . .
H22A H -0.1871 0.0903 0.5655 0.040 Uiso 1 1 calc R U . . .
H22B H -0.2259 0.0644 0.6093 0.040 Uiso 1 1 calc R U . . .
H22C H -0.1583 0.0146 0.5780 0.040 Uiso 1 1 calc R U . . .
C23 C 0.0043(3) 0.04286(15) 0.64193(8) 0.0281(7) Uani 1 1 d . . . . .
H23A H 0.0087 -0.0050 0.6360 0.042 Uiso 1 1 calc R U . . .
H23B H -0.0646 0.0511 0.6618 0.042 Uiso 1 1 calc R U . . .
H23C H 0.0885 0.0578 0.6527 0.042 Uiso 1 1 calc R U . . .
C24 C 0.3748(3) 0.15851(15) 0.52304(8) 0.0214(6) Uani 1 1 d . . . . .
H24 H 0.3547 0.2006 0.5380 0.026 Uiso 1 1 calc R U . . .
C25 C 0.5135(3) 0.13730(16) 0.53415(11) 0.0373(8) Uani 1 1 d . . . . .
H25A H 0.5188 0.1300 0.5632 0.056 Uiso 1 1 calc R U . . .
H25B H 0.5751 0.1724 0.5263 0.056 Uiso 1 1 calc R U . . .
H25C H 0.5355 0.0958 0.5201 0.056 Uiso 1 1 calc R U . . .
C26 C 0.3691(3) 0.17413(16) 0.47814(9) 0.0341(8) Uani 1 1 d . . . . .
H26A H 0.3996 0.1353 0.4629 0.051 Uiso 1 1 calc R U . . .
H26B H 0.4253 0.2126 0.4723 0.051 Uiso 1 1 calc R U . . .
H26C H 0.2789 0.1845 0.4705 0.051 Uiso 1 1 calc R U . . .
C27 C 0.1860(2) 0.39769(13) 0.55952(8) 0.0135(6) Uani 1 1 d . . . . .
C28 C 0.2779(3) 0.40787(13) 0.52845(8) 0.0159(6) Uani 1 1 d . . . . .
C29 C 0.2961(3) 0.47267(14) 0.51415(8) 0.0227(6) Uani 1 1 d . . . . .
H29 H 0.3597 0.4806 0.4939 0.027 Uiso 1 1 calc R U . . .
C30 C 0.2242(3) 0.52534(14) 0.52866(9) 0.0259(7) Uani 1 1 d . . . . .
H30 H 0.2400 0.5693 0.5191 0.031 Uiso 1 1 calc R U . . .
C31 C 0.1287(3) 0.51402(14) 0.55724(9) 0.0238(6) Uani 1 1 d . . . . .
H31 H 0.0764 0.5502 0.5662 0.029 Uiso 1 1 calc R U . . .
C32 C 0.1075(3) 0.45040(14) 0.57315(8) 0.0172(6) Uani 1 1 d . . . . .
C33 C 0.3557(3) 0.35130(14) 0.50993(8) 0.0180(6) Uani 1 1 d . . . . .
H33 H 0.3080 0.3088 0.5158 0.022 Uiso 1 1 calc R U . . .
C34 C 0.4922(3) 0.34501(17) 0.52769(10) 0.0343(8) Uani 1 1 d . . . . .
H34A H 0.5393 0.3872 0.5242 0.052 Uiso 1 1 calc R U . . .
H34B H 0.5397 0.3092 0.5139 0.052 Uiso 1 1 calc R U . . .
H34C H 0.4856 0.3346 0.5564 0.052 Uiso 1 1 calc R U . . .
C35 C 0.3652(4) 0.35827(17) 0.46441(9) 0.0383(8) Uani 1 1 d . . . . .
H35A H 0.2791 0.3695 0.4535 0.057 Uiso 1 1 calc R U . . .
H35B H 0.3953 0.3160 0.4528 0.057 Uiso 1 1 calc R U . . .
H35C H 0.4275 0.3938 0.4577 0.057 Uiso 1 1 calc R U . . .
C36 C -0.0002(3) 0.44140(13) 0.60394(8) 0.0195(6) Uani 1 1 d . . . . .
H36 H 0.0005 0.3938 0.6129 0.023 Uiso 1 1 calc R U . . .
C37 C -0.1343(3) 0.45589(16) 0.58489(9) 0.0253(7) Uani 1 1 d . . . . .
H37A H -0.1364 0.5021 0.5753 0.038 Uiso 1 1 calc R U . . .
H37B H -0.2031 0.4493 0.6050 0.038 Uiso 1 1 calc R U . . .
H37C H -0.1486 0.4255 0.5623 0.038 Uiso 1 1 calc R U . . .
C38 C 0.0188(3) 0.48563(13) 0.64099(8) 0.0242(6) Uani 1 1 d . . . . .
H38A H 0.1000 0.4731 0.6546 0.036 Uiso 1 1 calc R U . . .
H38B H -0.0551 0.4796 0.6594 0.036 Uiso 1 1 calc R U . . .
H38C H 0.0236 0.5325 0.6327 0.036 Uiso 1 1 calc R U . . .
C39 C 0.5010(3) 0.71894(16) 0.75644(8) 0.0258(7) Uani 1 1 d . . . . .
H39 H 0.5494 0.6810 0.7649 0.031 Uiso 1 1 calc R U . . .
C40 C 0.3752(3) 0.71806(16) 0.73981(8) 0.0226(7) Uani 1 1 d . . . . .
H40 H 0.3232 0.6796 0.7350 0.027 Uiso 1 1 calc R U . . .
C41 C 0.3402(3) 0.78482(16) 0.73153(8) 0.0211(7) Uani 1 1 d . . . . .
H41 H 0.2595 0.7993 0.7204 0.025 Uiso 1 1 calc R U . . .
C42 C 0.4449(3) 0.82595(16) 0.74250(8) 0.0241(7) Uani 1 1 d . . . . .
H42 H 0.4488 0.8731 0.7396 0.029 Uiso 1 1 calc R U . . .
C43 C 0.5429(3) 0.78506(17) 0.75850(8) 0.0273(7) Uani 1 1 d . . . . .
H43 H 0.6242 0.7999 0.7690 0.033 Uiso 1 1 calc R U . . .
C44 C 0.2980(3) 0.74492(14) 0.61566(9) 0.0183(7) Uani 1 1 d . . . . .
C45 C 0.2896(4) 0.6746(2) 0.59988(14) 0.0673(15) Uani 1 1 d . . . . .
H45A H 0.3685 0.6644 0.5843 0.101 Uiso 1 1 calc R U . . .
H45B H 0.2126 0.6703 0.5826 0.101 Uiso 1 1 calc R U . . .
H45C H 0.2823 0.6434 0.6224 0.101 Uiso 1 1 calc R U . . .
C46 C 0.1714(3) 0.7625(3) 0.63732(11) 0.0569(14) Uani 1 1 d . . . . .
H46A H 0.1519 0.7281 0.6574 0.085 Uiso 1 1 calc R U . . .
H46B H 0.0998 0.7648 0.6178 0.085 Uiso 1 1 calc R U . . .
H46C H 0.1810 0.8058 0.6507 0.085 Uiso 1 1 calc R U . . .
C47 C 0.3162(4) 0.7918(2) 0.58098(11) 0.0492(11) Uani 1 1 d . . . . .
H47A H 0.3097 0.8380 0.5905 0.074 Uiso 1 1 calc R U . . .
H47B H 0.2482 0.7836 0.5609 0.074 Uiso 1 1 calc R U . . .
H47C H 0.4024 0.7845 0.5689 0.074 Uiso 1 1 calc R U . . .
C48 C 0.8444(3) 0.63832(13) 0.62885(8) 0.0161(6) Uani 1 1 d . . . . .
H48A H 0.9215 0.6354 0.6462 0.024 Uiso 1 1 calc R U . . .
H48B H 0.8723 0.6462 0.6011 0.024 Uiso 1 1 calc R U . . .
H48C H 0.7952 0.5964 0.6303 0.024 Uiso 1 1 calc R U . . .
C49 C 0.7583(2) 0.69538(13) 0.64267(8) 0.0121(6) Uani 1 1 d . . . . .
C50 C 0.7757(3) 0.75580(13) 0.62248(9) 0.0123(6) Uani 1 1 d . . . . .
H50 H 0.8143 0.7527 0.5966 0.015 Uiso 1 1 calc R U . . .
C51 C 0.7440(2) 0.81991(13) 0.63527(8) 0.0118(6) Uani 1 1 d . . . . .
C52 C 0.8099(3) 0.87665(13) 0.61318(8) 0.0186(6) Uani 1 1 d . . . . .
H52A H 0.7451 0.9005 0.5969 0.028 Uiso 1 1 calc R U . . .
H52B H 0.8785 0.8588 0.5957 0.028 Uiso 1 1 calc R U . . .
H52C H 0.8489 0.9075 0.6326 0.028 Uiso 1 1 calc R U . . .
C53 C 0.6912(3) 0.62456(13) 0.69627(8) 0.0145(6) Uani 1 1 d . . . . .
C54 C 0.6048(3) 0.57134(14) 0.69014(9) 0.0205(6) Uani 1 1 d . . . . .
C55 C 0.6233(3) 0.51269(16) 0.71175(10) 0.0340(8) Uani 1 1 d . . . . .
H55 H 0.5655 0.4762 0.7075 0.041 Uiso 1 1 calc R U . . .
C56 C 0.7233(3) 0.50626(16) 0.73907(10) 0.0361(8) Uani 1 1 d . . . . .
H56 H 0.7343 0.4658 0.7536 0.043 Uiso 1 1 calc R U . . .
C57 C 0.8072(3) 0.55877(15) 0.74519(9) 0.0266(7) Uani 1 1 d . . . . .
H57 H 0.8759 0.5543 0.7642 0.032 Uiso 1 1 calc R U . . .
C58 C 0.7936(3) 0.61856(14) 0.72415(8) 0.0175(6) Uani 1 1 d . . . . .
C59 C 0.4955(3) 0.57376(13) 0.65935(8) 0.0223(6) Uani 1 1 d . . . . .
H59 H 0.4849 0.6211 0.6504 0.027 Uiso 1 1 calc R U . . .
C60 C 0.3652(3) 0.55030(17) 0.67739(10) 0.0304(8) Uani 1 1 d . . . . .
H60A H 0.3728 0.5035 0.6857 0.046 Uiso 1 1 calc R U . . .
H60B H 0.2959 0.5546 0.6572 0.046 Uiso 1 1 calc R U . . .
H60C H 0.3437 0.5779 0.7008 0.046 Uiso 1 1 calc R U . . .
C61 C 0.5299(3) 0.53108(14) 0.62249(8) 0.0253(7) Uani 1 1 d . . . . .
H61A H 0.6075 0.5496 0.6093 0.038 Uiso 1 1 calc R U . . .
H61B H 0.4563 0.5313 0.6037 0.038 Uiso 1 1 calc R U . . .
H61C H 0.5478 0.4852 0.6310 0.038 Uiso 1 1 calc R U . . .
C62 C 0.8908(3) 0.67372(14) 0.73270(8) 0.0195(6) Uani 1 1 d . . . . .
H62 H 0.8737 0.7112 0.7136 0.023 Uiso 1 1 calc R U . . .
C63 C 1.0331(3) 0.65053(16) 0.72693(10) 0.0322(8) Uani 1 1 d . . . . .
H63A H 1.0554 0.6179 0.7478 0.048 Uiso 1 1 calc R U . . .
H63B H 1.0918 0.6890 0.7290 0.048 Uiso 1 1 calc R U . . .
H63C H 1.0427 0.6299 0.7004 0.048 Uiso 1 1 calc R U . . .
C64 C 0.8747(3) 0.70020(16) 0.77549(9) 0.0323(8) Uani 1 1 d . . . . .
H64A H 0.7863 0.7182 0.7789 0.048 Uiso 1 1 calc R U . . .
H64B H 0.9390 0.7356 0.7804 0.048 Uiso 1 1 calc R U . . .
H64C H 0.8885 0.6638 0.7947 0.048 Uiso 1 1 calc R U . . .
C65 C 0.6600(2) 0.90126(13) 0.68024(7) 0.0124(5) Uani 1 1 d . . . . .
C66 C 0.7493(2) 0.92004(13) 0.71030(8) 0.0144(6) Uani 1 1 d . . . . .
C67 C 0.7518(3) 0.98666(14) 0.72258(8) 0.0200(6) Uani 1 1 d . . . . .
H67 H 0.8125 1.0001 0.7426 0.024 Uiso 1 1 calc R U . . .
C68 C 0.6682(3) 1.03345(14) 0.70634(8) 0.0246(6) Uani 1 1 d . . . . .
H68 H 0.6728 1.0788 0.7146 0.029 Uiso 1 1 calc R U . . .
C69 C 0.5781(3) 1.01381(14) 0.67805(9) 0.0232(6) Uani 1 1 d . . . . .
H69 H 0.5186 1.0458 0.6676 0.028 Uiso 1 1 calc R U . . .
C70 C 0.5722(3) 0.94816(14) 0.66448(8) 0.0165(6) Uani 1 1 d . . . . .
C71 C 0.8413(3) 0.87053(14) 0.73008(8) 0.0197(6) Uani 1 1 d . . . . .
H71 H 0.8031 0.8249 0.7268 0.024 Uiso 1 1 calc R U . . .
C72 C 0.9778(3) 0.87050(17) 0.71027(11) 0.0377(8) Uani 1 1 d . . . . .
H72A H 1.0121 0.9162 0.7096 0.057 Uiso 1 1 calc R U . . .
H72B H 0.9708 0.8533 0.6828 0.057 Uiso 1 1 calc R U . . .
H72C H 1.0369 0.8420 0.7258 0.057 Uiso 1 1 calc R U . . .
C73 C 0.8547(3) 0.88424(17) 0.77483(9) 0.0357(8) Uani 1 1 d . . . . .
H73A H 0.9069 0.9247 0.7789 0.054 Uiso 1 1 calc R U . . .
H73B H 0.8981 0.8464 0.7878 0.054 Uiso 1 1 calc R U . . .
H73C H 0.7678 0.8905 0.7866 0.054 Uiso 1 1 calc R U . . .
C74 C 0.4705(3) 0.93012(13) 0.63310(8) 0.0198(6) Uani 1 1 d . . . . .
H74 H 0.4811 0.8818 0.6262 0.024 Uiso 1 1 calc R U . . .
C75 C 0.4881(3) 0.97107(13) 0.59471(8) 0.0247(6) Uani 1 1 d . . . . .
H75A H 0.4722 1.0183 0.6005 0.037 Uiso 1 1 calc R U . . .
H75B H 0.4259 0.9557 0.5743 0.037 Uiso 1 1 calc R U . . .
H75C H 0.5775 0.9655 0.5847 0.037 Uiso 1 1 calc R U . . .
C76 C 0.3323(3) 0.94039(16) 0.65018(9) 0.0277(7) Uani 1 1 d . . . . .
H76A H 0.3182 0.9097 0.6727 0.042 Uiso 1 1 calc R U . . .
H76B H 0.2675 0.9315 0.6292 0.042 Uiso 1 1 calc R U . . .
H76C H 0.3229 0.9865 0.6596 0.042 Uiso 1 1 calc R U . . .
N1 N -0.0875(2) 0.26512(11) 0.60727(7) 0.0140(5) Uani 1 1 d . . . . .
N2 N 0.1671(2) 0.18541(10) 0.58183(6) 0.0119(5) Uani 1 1 d . . . . .
N3 N 0.1772(2) 0.33224(10) 0.57813(6) 0.0117(5) Uani 1 1 d . . . . .
N4 N 0.4074(2) 0.75092(11) 0.64365(7) 0.0144(5) Uani 1 1 d . . . . .
N5 N 0.6763(2) 0.68626(11) 0.67375(6) 0.0113(5) Uani 1 1 d . . . . .
N6 N 0.6627(2) 0.83279(10) 0.66585(6) 0.0105(5) Uani 1 1 d . . . . .
Nb1 Nb 0.01935(2) 0.26064(2) 0.56464(2) 0.01006(6) Uani 1 1 d . . . . .
Nb2 Nb 0.51578(2) 0.75882(2) 0.68541(2) 0.01063(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 1.395(4) . ?
C1 C5 1.405(5) . ?
C1 Nb1 2.488(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.401(4) . ?
C2 Nb1 2.507(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(4) . ?
C3 Nb1 2.441(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.403(5) . ?
C4 Nb1 2.415(3) . ?
C4 H4 0.9500 . ?
C5 Nb1 2.434(3) . ?
C5 H5 0.9500 . ?
C6 N1 1.467(4) . ?
C6 C7 1.522(4) . ?
C6 C9 1.524(4) . ?
C6 C8 1.530(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.518(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N2 1.328(3) . ?
C11 C12 1.399(4) . ?
C12 C13 1.398(4) . ?
C12 H12 0.9500 . ?
C13 N3 1.333(3) . ?
C13 C14 1.519(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.407(4) . ?
C15 C20 1.413(4) . ?
C15 N2 1.454(3) . ?
C16 C17 1.400(4) . ?
C16 C21 1.520(4) . ?
C17 C18 1.369(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.396(4) . ?
C19 H19 0.9500 . ?
C20 C24 1.512(4) . ?
C21 C22 1.535(4) . ?
C21 C23 1.535(4) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.527(4) . ?
C24 C26 1.529(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 C32 1.402(4) . ?
C27 C28 1.413(4) . ?
C27 N3 1.453(3) . ?
C28 C29 1.395(4) . ?
C28 C33 1.516(4) . ?
C29 C30 1.374(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.382(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.397(4) . ?
C31 H31 0.9500 . ?
C32 C36 1.516(4) . ?
C33 C34 1.522(4) . ?
C33 C35 1.525(4) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C38 1.532(4) . ?
C36 C37 1.539(4) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C43 1.394(5) . ?
C39 C40 1.401(4) . ?
C39 Nb2 2.502(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.412(4) . ?
C40 Nb2 2.452(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.400(4) . ?
C41 Nb2 2.420(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.400(4) . ?
C42 Nb2 2.439(3) . ?
C42 H42 0.9500 . ?
C43 Nb2 2.506(3) . ?
C43 H43 0.9500 . ?
C44 N4 1.462(4) . ?
C44 C47 1.500(4) . ?
C44 C45 1.506(4) . ?
C44 C46 1.524(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
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 C49 1.515(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 N5 1.344(3) . ?
C49 C50 1.396(4) . ?
C50 C51 1.392(4) . ?
C50 H50 0.9500 . ?
C51 N6 1.339(3) . ?
C51 C52 1.513(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.400(4) . ?
C53 C58 1.405(4) . ?
C53 N5 1.454(3) . ?
C54 C55 1.391(4) . ?
C54 C59 1.518(4) . ?
C55 C56 1.376(4) . ?
C55 H55 0.9500 . ?
C56 C57 1.373(4) . ?
C56 H56 0.9500 . ?
C57 C58 1.395(4) . ?
C57 H57 0.9500 . ?
C58 C62 1.514(4) . ?
C59 C60 1.536(4) . ?
C59 C61 1.537(4) . ?
C59 H59 1.0000 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C64 1.529(4) . ?
C62 C63 1.540(4) . ?
C62 H62 1.0000 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C70 1.402(4) . ?
C65 C66 1.407(3) . ?
C65 N6 1.453(3) . ?
C66 C67 1.396(4) . ?
C66 C71 1.518(4) . ?
C67 C68 1.380(4) . ?
C67 H67 0.9500 . ?
C68 C69 1.376(4) . ?
C68 H68 0.9500 . ?
C69 C70 1.392(4) . ?
C69 H69 0.9500 . ?
C70 C74 1.519(4) . ?
C71 C73 1.522(4) . ?
C71 C72 1.544(4) . ?
C71 H71 1.0000 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.530(4) . ?
C74 C76 1.538(4) . ?
C74 H74 1.0000 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N1 Nb1 1.794(2) . ?
N2 Nb1 2.210(2) . ?
N3 Nb1 2.207(2) . ?
N4 Nb2 1.786(2) . ?
N5 Nb2 2.227(2) . ?
N6 Nb2 2.209(2) . ?

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 C5 107.7(3) . . ?
C2 C1 Nb1 74.53(16) . . ?
C5 C1 Nb1 71.29(16) . . ?
C2 C1 H1 126.2 . . ?
C5 C1 H1 126.2 . . ?
Nb1 C1 H1 119.9 . . ?
C1 C2 C3 108.5(3) . . ?
C1 C2 Nb1 73.03(16) . . ?
C3 C2 Nb1 70.97(16) . . ?
C1 C2 H2 125.8 . . ?
C3 C2 H2 125.8 . . ?
Nb1 C2 H2 121.9 . . ?
C2 C3 C4 107.9(3) . . ?
C2 C3 Nb1 76.16(17) . . ?
C4 C3 Nb1 72.18(16) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
Nb1 C3 H3 117.6 . . ?
C5 C4 C3 107.7(3) . . ?
C5 C4 Nb1 73.92(16) . . ?
C3 C4 Nb1 74.22(16) . . ?
C5 C4 H4 126.1 . . ?
C3 C4 H4 126.1 . . ?
Nb1 C4 H4 117.7 . . ?
C4 C5 C1 108.2(3) . . ?
C4 C5 Nb1 72.45(16) . . ?
C1 C5 Nb1 75.55(16) . . ?
C4 C5 H5 125.9 . . ?
C1 C5 H5 125.9 . . ?
Nb1 C5 H5 118.0 . . ?
N1 C6 C7 109.6(2) . . ?
N1 C6 C9 110.0(2) . . ?
C7 C6 C9 109.3(3) . . ?
N1 C6 C8 109.6(2) . . ?
C7 C6 C8 109.5(3) . . ?
C9 C6 C8 108.9(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 123.9(2) . . ?
N2 C11 C10 121.4(2) . . ?
C12 C11 C10 114.7(2) . . ?
C13 C12 C11 128.4(3) . . ?
C13 C12 H12 115.8 . . ?
C11 C12 H12 115.8 . . ?
N3 C13 C12 124.3(3) . . ?
N3 C13 C14 119.5(2) . . ?
C12 C13 C14 116.1(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 120.4(2) . . ?
C16 C15 N2 120.6(2) . . ?
C20 C15 N2 119.0(2) . . ?
C17 C16 C15 118.2(2) . . ?
C17 C16 C21 119.4(2) . . ?
C15 C16 C21 122.4(2) . . ?
C18 C17 C16 121.8(3) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 120.8(3) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C15 118.8(3) . . ?
C19 C20 C24 118.3(3) . . ?
C15 C20 C24 122.9(2) . . ?
C16 C21 C22 112.1(2) . . ?
C16 C21 C23 110.9(2) . . ?
C22 C21 C23 109.6(2) . . ?
C16 C21 H21 108.1 . . ?
C22 C21 H21 108.1 . . ?
C23 C21 H21 108.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 C25 113.0(2) . . ?
C20 C24 C26 111.1(2) . . ?
C25 C24 C26 109.2(3) . . ?
C20 C24 H24 107.8 . . ?
C25 C24 H24 107.8 . . ?
C26 C24 H24 107.8 . . ?
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 . . ?
C32 C27 C28 120.6(2) . . ?
C32 C27 N3 120.4(2) . . ?
C28 C27 N3 118.9(2) . . ?
C29 C28 C27 118.2(3) . . ?
C29 C28 C33 119.2(2) . . ?
C27 C28 C33 122.6(2) . . ?
C30 C29 C28 121.6(3) . . ?
C30 C29 H29 119.2 . . ?
C28 C29 H29 119.2 . . ?
C29 C30 C31 119.6(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 121.3(3) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
C31 C32 C27 118.4(3) . . ?
C31 C32 C36 118.5(2) . . ?
C27 C32 C36 123.1(2) . . ?
C28 C33 C34 112.7(2) . . ?
C28 C33 C35 111.7(2) . . ?
C34 C33 C35 109.6(3) . . ?
C28 C33 H33 107.6 . . ?
C34 C33 H33 107.6 . . ?
C35 C33 H33 107.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C38 112.6(2) . . ?
C32 C36 C37 110.3(2) . . ?
C38 C36 C37 109.7(2) . . ?
C32 C36 H36 108.1 . . ?
C38 C36 H36 108.1 . . ?
C37 C36 H36 108.1 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C43 C39 C40 108.3(3) . . ?
C43 C39 Nb2 74.01(15) . . ?
C40 C39 Nb2 71.65(15) . . ?
C43 C39 H39 125.9 . . ?
C40 C39 H39 125.9 . . ?
Nb2 C39 H39 120.3 . . ?
C39 C40 C41 107.4(3) . . ?
C39 C40 Nb2 75.51(16) . . ?
C41 C40 Nb2 71.89(15) . . ?
C39 C40 H40 126.3 . . ?
C41 C40 H40 126.3 . . ?
Nb2 C40 H40 118.3 . . ?
C42 C41 C40 108.2(3) . . ?
C42 C41 Nb2 73.99(16) . . ?
C40 C41 Nb2 74.42(15) . . ?
C42 C41 H41 125.9 . . ?
C40 C41 H41 125.9 . . ?
Nb2 C41 H41 117.6 . . ?
C43 C42 C41 107.6(3) . . ?
C43 C42 Nb2 76.21(17) . . ?
C41 C42 Nb2 72.50(16) . . ?
C43 C42 H42 126.2 . . ?
C41 C42 H42 126.2 . . ?
Nb2 C42 H42 117.2 . . ?
C39 C43 C42 108.5(3) . . ?
C39 C43 Nb2 73.66(15) . . ?
C42 C43 Nb2 70.93(16) . . ?
C39 C43 H43 125.8 . . ?
C42 C43 H43 125.8 . . ?
Nb2 C43 H43 121.4 . . ?
N4 C44 C47 110.2(3) . . ?
N4 C44 C45 110.1(2) . . ?
C47 C44 C45 108.9(3) . . ?
N4 C44 C46 109.3(2) . . ?
C47 C44 C46 109.0(3) . . ?
C45 C44 C46 109.4(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N5 C49 C50 124.6(2) . . ?
N5 C49 C48 119.6(2) . . ?
C50 C49 C48 115.7(2) . . ?
C51 C50 C49 128.6(3) . . ?
C51 C50 H50 115.7 . . ?
C49 C50 H50 115.7 . . ?
N6 C51 C50 123.7(2) . . ?
N6 C51 C52 120.1(2) . . ?
C50 C51 C52 116.2(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 C58 120.1(2) . . ?
C54 C53 N5 120.4(2) . . ?
C58 C53 N5 119.5(2) . . ?
C55 C54 C53 118.8(3) . . ?
C55 C54 C59 118.5(3) . . ?
C53 C54 C59 122.7(2) . . ?
C56 C55 C54 121.5(3) . . ?
C56 C55 H55 119.2 . . ?
C54 C55 H55 119.2 . . ?
C57 C56 C55 119.4(3) . . ?
C57 C56 H56 120.3 . . ?
C55 C56 H56 120.3 . . ?
C56 C57 C58 121.4(3) . . ?
C56 C57 H57 119.3 . . ?
C58 C57 H57 119.3 . . ?
C57 C58 C53 118.7(3) . . ?
C57 C58 C62 117.8(2) . . ?
C53 C58 C62 123.5(2) . . ?
C54 C59 C60 111.4(2) . . ?
C54 C59 C61 110.7(2) . . ?
C60 C59 C61 109.9(2) . . ?
C54 C59 H59 108.2 . . ?
C60 C59 H59 108.2 . . ?
C61 C59 H59 108.2 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C58 C62 C64 111.0(2) . . ?
C58 C62 C63 112.2(2) . . ?
C64 C62 C63 108.8(2) . . ?
C58 C62 H62 108.3 . . ?
C64 C62 H62 108.3 . . ?
C63 C62 H62 108.3 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C70 C65 C66 120.2(2) . . ?
C70 C65 N6 121.4(2) . . ?
C66 C65 N6 118.4(2) . . ?
C67 C66 C65 118.4(2) . . ?
C67 C66 C71 119.1(2) . . ?
C65 C66 C71 122.5(2) . . ?
C68 C67 C66 121.5(3) . . ?
C68 C67 H67 119.2 . . ?
C66 C67 H67 119.2 . . ?
C69 C68 C67 119.3(3) . . ?
C69 C68 H68 120.3 . . ?
C67 C68 H68 120.3 . . ?
C68 C69 C70 121.5(3) . . ?
C68 C69 H69 119.3 . . ?
C70 C69 H69 119.3 . . ?
C69 C70 C65 118.9(3) . . ?
C69 C70 C74 118.6(2) . . ?
C65 C70 C74 122.5(2) . . ?
C66 C71 C73 111.3(2) . . ?
C66 C71 C72 112.1(2) . . ?
C73 C71 C72 109.7(2) . . ?
C66 C71 H71 107.9 . . ?
C73 C71 H71 107.9 . . ?
C72 C71 H71 107.9 . . ?
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 . . ?
C70 C74 C75 111.5(2) . . ?
C70 C74 C76 110.1(2) . . ?
C75 C74 C76 110.2(2) . . ?
C70 C74 H74 108.3 . . ?
C75 C74 H74 108.3 . . ?
C76 C74 H74 108.3 . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C74 C76 H76A 109.5 . . ?
C74 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C74 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C6 N1 Nb1 168.07(19) . . ?
C11 N2 C15 116.9(2) . . ?
C11 N2 Nb1 120.86(17) . . ?
C15 N2 Nb1 122.05(16) . . ?
C13 N3 C27 115.8(2) . . ?
C13 N3 Nb1 120.07(17) . . ?
C27 N3 Nb1 123.03(16) . . ?
C44 N4 Nb2 168.4(2) . . ?
C49 N5 C53 116.6(2) . . ?
C49 N5 Nb2 120.34(17) . . ?
C53 N5 Nb2 122.87(16) . . ?
C51 N6 C65 116.4(2) . . ?
C51 N6 Nb2 121.13(17) . . ?
C65 N6 Nb2 121.53(16) . . ?
N1 Nb1 N3 104.61(9) . . ?
N1 Nb1 N2 104.23(9) . . ?
N3 Nb1 N2 83.68(8) . . ?
N1 Nb1 C4 93.98(10) . . ?
N3 Nb1 C4 120.92(10) . . ?
N2 Nb1 C4 144.74(10) . . ?
N1 Nb1 C5 99.26(11) . . ?
N3 Nb1 C5 146.88(9) . . ?
N2 Nb1 C5 112.41(10) . . ?
C4 Nb1 C5 33.63(12) . . ?
N1 Nb1 C3 120.67(10) . . ?
N3 Nb1 C3 92.34(9) . . ?
N2 Nb1 C3 134.32(9) . . ?
C4 Nb1 C3 33.60(10) . . ?
C5 Nb1 C3 55.40(10) . . ?
N1 Nb1 C1 130.38(11) . . ?
N3 Nb1 C1 124.18(10) . . ?
N2 Nb1 C1 90.56(9) . . ?
C4 Nb1 C1 55.26(10) . . ?
C5 Nb1 C1 33.15(11) . . ?
C3 Nb1 C1 54.81(10) . . ?
N1 Nb1 C2 148.74(10) . . ?
N3 Nb1 C2 94.94(9) . . ?
N2 Nb1 C2 101.95(9) . . ?
C4 Nb1 C2 54.83(10) . . ?
C5 Nb1 C2 54.45(10) . . ?
C3 Nb1 C2 32.87(10) . . ?
C1 Nb1 C2 32.44(10) . . ?
N4 Nb2 N6 104.62(9) . . ?
N4 Nb2 N5 105.33(9) . . ?
N6 Nb2 N5 83.39(8) . . ?
N4 Nb2 C41 93.00(10) . . ?
N6 Nb2 C41 123.21(9) . . ?
N5 Nb2 C41 142.97(9) . . ?
N4 Nb2 C42 118.14(10) . . ?
N6 Nb2 C42 93.55(9) . . ?
N5 Nb2 C42 135.62(9) . . ?
C41 Nb2 C42 33.50(10) . . ?
N4 Nb2 C40 100.48(11) . . ?
N6 Nb2 C40 147.13(9) . . ?
N5 Nb2 C40 110.08(9) . . ?
C41 Nb2 C40 33.69(10) . . ?
C42 Nb2 C40 55.51(10) . . ?
N4 Nb2 C39 132.14(11) . . ?
N6 Nb2 C39 122.27(9) . . ?
N5 Nb2 C39 90.03(9) . . ?
C41 Nb2 C39 54.83(10) . . ?
C42 Nb2 C39 54.62(10) . . ?
C40 Nb2 C39 32.84(10) . . ?
N4 Nb2 C43 147.57(11) . . ?
N6 Nb2 C43 94.02(9) . . ?
N5 Nb2 C43 102.96(9) . . ?
C41 Nb2 C43 54.60(10) . . ?
C42 Nb2 C43 32.86(10) . . ?
C40 Nb2 C43 54.36(10) . . ?
C39 Nb2 C43 32.32(11) . . ?

_refine_diff_density_max         0.426
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.055



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method hexane
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1485268'
_audit_update_record             
;
2016-06-14 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            (BDI)Nb(NtBu)CpH
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H56 N3 Nb'
_chemical_formula_weight         647.76

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.8167(5)
_cell_length_b                   19.9697(6)
_cell_length_c                   20.4459(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.0010(10)
_cell_angle_gamma                90
_cell_volume                     6866.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9227
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      25.33

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             2768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.380
_shelx_estimated_absorpt_T_min   0.963
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 0.8366
_diffrn_reflns_number            96219
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         0.996
_diffrn_reflns_theta_max         25.400
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12357
_reflns_number_gt                11114
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-2011
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          'Refined as a 2-component twin., Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²+4.6471P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12357
_refine_ls_number_parameters     792
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0766
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5043(2) 0.2882(2) 0.18632(19) 0.0444(11) Uani 1 1 d . . . . .
H1A H 0.5132 0.3240 0.1565 0.053 Uiso 1 1 calc R U . . .
C2 C 0.4723(2) 0.29370(16) 0.2508(2) 0.0368(9) Uani 1 1 d . . . . .
H2 H 0.4549 0.3338 0.2714 0.044 Uiso 1 1 calc R U . . .
C3 C 0.4711(2) 0.23136(19) 0.27751(18) 0.0346(9) Uani 1 1 d . . . . .
H3 H 0.4527 0.2206 0.3202 0.042 Uiso 1 1 calc R U . . .
C4 C 0.5011(2) 0.18581(17) 0.23245(17) 0.0383(9) Uani 1 1 d . . . . .
H4 H 0.5078 0.1390 0.2389 0.046 Uiso 1 1 calc R U . . .
C5 C 0.5198(2) 0.2221(2) 0.17545(18) 0.0394(10) Uani 1 1 d . . . . .
H5 H 0.5398 0.2036 0.1359 0.047 Uiso 1 1 calc R U . . .
C6 C 0.7546(2) 0.23841(16) 0.14989(16) 0.0224(7) Uani 1 1 d . . . . .
C7 C 0.7133(2) 0.21136(19) 0.08911(14) 0.0373(9) Uani 1 1 d . . . . .
H7A H 0.6895 0.1677 0.0990 0.056 Uiso 1 1 calc R U . . .
H7B H 0.7523 0.2063 0.0538 0.056 Uiso 1 1 calc R U . . .
H7C H 0.6716 0.2426 0.0754 0.056 Uiso 1 1 calc R U . . .
C8 C 0.8211(2) 0.19045(17) 0.16965(17) 0.0381(9) Uani 1 1 d . . . . .
H8A H 0.8436 0.2046 0.2116 0.057 Uiso 1 1 calc R U . . .
H8B H 0.8628 0.1908 0.1361 0.057 Uiso 1 1 calc R U . . .
H8C H 0.7996 0.1451 0.1739 0.057 Uiso 1 1 calc R U . . .
C9 C 0.7875(2) 0.30677(17) 0.13624(17) 0.0366(8) Uani 1 1 d . . . . .
H9A H 0.7440 0.3370 0.1242 0.055 Uiso 1 1 calc R U . . .
H9B H 0.8258 0.3041 0.1002 0.055 Uiso 1 1 calc R U . . .
H9C H 0.8142 0.3238 0.1755 0.055 Uiso 1 1 calc R U . . .
C10 C 0.7431(2) 0.13109(13) 0.41328(18) 0.0242(8) Uani 1 1 d . . . . .
H10A H 0.7003 0.0995 0.4236 0.036 Uiso 1 1 calc R U . . .
H10B H 0.7673 0.1472 0.4540 0.036 Uiso 1 1 calc R U . . .
H10C H 0.7835 0.1085 0.3867 0.036 Uiso 1 1 calc R U . . .
C11 C 0.70945(19) 0.18989(14) 0.37559(14) 0.0149(7) Uani 1 1 d . . . . .
C12 C 0.7482(2) 0.25074(12) 0.38602(19) 0.0156(8) Uani 1 1 d . . . . .
H12 H 0.8007 0.2481 0.4031 0.019 Uiso 1 1 calc R U . . .
C13 C 0.71893(18) 0.31479(14) 0.37428(14) 0.0143(7) Uani 1 1 d . . . . .
C14 C 0.7587(2) 0.37068(13) 0.41260(17) 0.0246(8) Uani 1 1 d . . . . .
H14A H 0.7833 0.4024 0.3821 0.037 Uiso 1 1 calc R U . . .
H14B H 0.7997 0.3517 0.4412 0.037 Uiso 1 1 calc R U . . .
H14C H 0.7189 0.3940 0.4392 0.037 Uiso 1 1 calc R U . . .
C15 C 0.6052(2) 0.11827(13) 0.34433(15) 0.0185(7) Uani 1 1 d . . . . .
C16 C 0.6238(2) 0.06563(14) 0.30178(15) 0.0278(8) Uani 1 1 d . . . . .
C17 C 0.5826(2) 0.00537(16) 0.30844(19) 0.0454(10) Uani 1 1 d . . . . .
H17 H 0.5942 -0.0306 0.2795 0.054 Uiso 1 1 calc R U . . .
C18 C 0.5257(3) -0.00316(17) 0.3557(2) 0.0513(11) Uani 1 1 d . . . . .
H18 H 0.4980 -0.0445 0.3591 0.062 Uiso 1 1 calc R U . . .
C19 C 0.5089(2) 0.04820(16) 0.39802(19) 0.0381(9) Uani 1 1 d . . . . .
H19 H 0.4701 0.0416 0.4312 0.046 Uiso 1 1 calc R U . . .
C20 C 0.5473(2) 0.10979(14) 0.39348(17) 0.0247(7) Uani 1 1 d . . . . .
C21 C 0.6869(2) 0.07095(13) 0.24857(17) 0.0316(8) Uani 1 1 d . . . . .
H21 H 0.7066 0.1182 0.2476 0.038 Uiso 1 1 calc R U . . .
C22 C 0.7579(2) 0.02482(15) 0.26259(19) 0.0417(9) Uani 1 1 d . . . . .
H22A H 0.7815 0.0368 0.3048 0.062 Uiso 1 1 calc R U . . .
H22B H 0.7977 0.0300 0.2280 0.062 Uiso 1 1 calc R U . . .
H22C H 0.7397 -0.0218 0.2639 0.062 Uiso 1 1 calc R U . . .
C23 C 0.6535(3) 0.05412(18) 0.18133(17) 0.0463(11) Uani 1 1 d . . . . .
H23A H 0.6306 0.0090 0.1821 0.069 Uiso 1 1 calc R U . . .
H23B H 0.6963 0.0559 0.1489 0.069 Uiso 1 1 calc R U . . .
H23C H 0.6122 0.0866 0.1697 0.069 Uiso 1 1 calc R U . . .
C24 C 0.5286(2) 0.16305(15) 0.44331(18) 0.0323(9) Uani 1 1 d . . . . .
H24 H 0.5503 0.2065 0.4269 0.039 Uiso 1 1 calc R U . . .
C25 C 0.4396(2) 0.1725(2) 0.4567(2) 0.0584(12) Uani 1 1 d . . . . .
H25A H 0.4124 0.1845 0.4160 0.088 Uiso 1 1 calc R U . . .
H25B H 0.4322 0.2083 0.4889 0.088 Uiso 1 1 calc R U . . .
H25C H 0.4173 0.1306 0.4738 0.088 Uiso 1 1 calc R U . . .
C26 C 0.5678(3) 0.1478(2) 0.5094(2) 0.0662(14) Uani 1 1 d . . . . .
H26A H 0.5464 0.1059 0.5269 0.099 Uiso 1 1 calc R U . . .
H26B H 0.5566 0.1844 0.5400 0.099 Uiso 1 1 calc R U . . .
H26C H 0.6254 0.1436 0.5035 0.099 Uiso 1 1 calc R U . . .
C27 C 0.62676(18) 0.39619(12) 0.34007(14) 0.0151(6) Uani 1 1 d . . . . .
C28 C 0.56464(19) 0.40844(14) 0.38392(15) 0.0205(7) Uani 1 1 d . . . . .
C29 C 0.5377(2) 0.47444(14) 0.39173(17) 0.0290(8) Uani 1 1 d . . . . .
H29 H 0.4956 0.4836 0.4215 0.035 Uiso 1 1 calc R U . . .
C30 C 0.5715(2) 0.52645(15) 0.35661(18) 0.0358(9) Uani 1 1 d . . . . .
H30 H 0.5535 0.5711 0.3630 0.043 Uiso 1 1 calc R U . . .
C31 C 0.6309(2) 0.51325(14) 0.31257(17) 0.0337(9) Uani 1 1 d . . . . .
H31 H 0.6532 0.5492 0.2883 0.040 Uiso 1 1 calc R U . . .
C32 C 0.65960(19) 0.44857(14) 0.30236(15) 0.0218(7) Uani 1 1 d . . . . .
C33 C 0.5251(2) 0.35376(15) 0.42196(16) 0.0254(8) Uani 1 1 d . . . . .
H33 H 0.5388 0.3104 0.4002 0.030 Uiso 1 1 calc R U . . .
C34 C 0.4350(2) 0.3600(2) 0.42166(19) 0.0496(10) Uani 1 1 d . . . . .
H34A H 0.4187 0.3939 0.4536 0.074 Uiso 1 1 calc R U . . .
H34B H 0.4113 0.3168 0.4333 0.074 Uiso 1 1 calc R U . . .
H34C H 0.4170 0.3732 0.3779 0.074 Uiso 1 1 calc R U . . .
C35 C 0.5552(3) 0.3500(2) 0.4914(2) 0.0561(13) Uani 1 1 d . . . . .
H35A H 0.6121 0.3394 0.4912 0.084 Uiso 1 1 calc R U . . .
H35B H 0.5262 0.3150 0.5151 0.084 Uiso 1 1 calc R U . . .
H35C H 0.5467 0.3932 0.5131 0.084 Uiso 1 1 calc R U . . .
C36 C 0.72434(19) 0.43861(13) 0.25144(16) 0.0241(7) Uani 1 1 d . . . . .
H36 H 0.7400 0.3903 0.2516 0.029 Uiso 1 1 calc R U . . .
C37 C 0.7987(2) 0.48070(14) 0.26524(17) 0.0305(8) Uani 1 1 d . . . . .
H37A H 0.7841 0.5282 0.2672 0.046 Uiso 1 1 calc R U . . .
H37B H 0.8377 0.4738 0.2302 0.046 Uiso 1 1 calc R U . . .
H37C H 0.8220 0.4670 0.3071 0.046 Uiso 1 1 calc R U . . .
C38 C 0.6924(2) 0.45583(15) 0.18341(16) 0.0294(8) Uani 1 1 d . . . . .
H38A H 0.6506 0.4240 0.1714 0.044 Uiso 1 1 calc R U . . .
H38B H 0.7357 0.4533 0.1515 0.044 Uiso 1 1 calc R U . . .
H38C H 0.6705 0.5013 0.1838 0.044 Uiso 1 1 calc R U . . .
C39 C 0.00594(19) 0.33019(17) 0.51380(15) 0.0298(8) Uani 1 1 d . . . . .
H39 H 0.0162 0.3759 0.5043 0.036 Uiso 1 1 calc R U . . .
C40 C 0.0213(2) 0.29683(18) 0.57341(17) 0.0318(8) Uani 1 1 d . . . . .
H40 H 0.0413 0.3173 0.6120 0.038 Uiso 1 1 calc R U . . .
C41 C 0.0028(2) 0.2304(2) 0.56705(18) 0.0349(9) Uani 1 1 d . . . . .
H41 H 0.0102 0.1964 0.5990 0.042 Uiso 1 1 calc R U . . .
C42 C -0.0298(2) 0.22199(19) 0.50301(17) 0.0340(9) Uani 1 1 d . . . . .
H42 H -0.0497 0.1813 0.4853 0.041 Uiso 1 1 calc R U . . .
C43 C -0.0273(2) 0.28265(18) 0.47138(17) 0.0334(9) Uani 1 1 d . . . . .
H43 H -0.0452 0.2910 0.4281 0.040 Uiso 1 1 calc R U . . .
C44 C 0.25350(19) 0.27277(15) 0.60013(15) 0.0192(7) Uani 1 1 d . . . . .
C45 C 0.3238(2) 0.31642(16) 0.57843(17) 0.0341(8) Uani 1 1 d . . . . .
H45A H 0.3452 0.2993 0.5371 0.051 Uiso 1 1 calc R U . . .
H45B H 0.3654 0.3152 0.6120 0.051 Uiso 1 1 calc R U . . .
H45C H 0.3057 0.3627 0.5723 0.051 Uiso 1 1 calc R U . . .
C46 C 0.2136(2) 0.30353(17) 0.66006(14) 0.0317(8) Uani 1 1 d . . . . .
H46A H 0.1896 0.3465 0.6481 0.047 Uiso 1 1 calc R U . . .
H46B H 0.2533 0.3106 0.6944 0.047 Uiso 1 1 calc R U . . .
H46C H 0.1721 0.2732 0.6761 0.047 Uiso 1 1 calc R U . . .
C47 C 0.2832(2) 0.20341(15) 0.61778(16) 0.0318(8) Uani 1 1 d . . . . .
H47A H 0.2380 0.1751 0.6303 0.048 Uiso 1 1 calc R U . . .
H47B H 0.3205 0.2066 0.6545 0.048 Uiso 1 1 calc R U . . .
H47C H 0.3102 0.1836 0.5800 0.048 Uiso 1 1 calc R U . . .
C48 C 0.2502(2) 0.36673(14) 0.33308(17) 0.0216(7) Uani 1 1 d . . . . .
H48A H 0.2107 0.3854 0.3029 0.032 Uiso 1 1 calc R U . . .
H48B H 0.2955 0.3494 0.3081 0.032 Uiso 1 1 calc R U . . .
H48C H 0.2685 0.4019 0.3629 0.032 Uiso 1 1 calc R U . . .
C49 C 0.21326(18) 0.31093(13) 0.37178(14) 0.0138(7) Uani 1 1 d . . . . .
C50 C 0.2490(2) 0.24826(11) 0.36382(19) 0.0149(8) Uani 1 1 d . . . . .
H50 H 0.3015 0.2482 0.3466 0.018 Uiso 1 1 calc R U . . .
C51 C 0.21618(19) 0.18571(14) 0.37832(14) 0.0157(8) Uani 1 1 d . . . . .
C52 C 0.2537(2) 0.12778(14) 0.34332(18) 0.0237(8) Uani 1 1 d . . . . .
H52A H 0.2611 0.0906 0.3740 0.036 Uiso 1 1 calc R U . . .
H52B H 0.3054 0.1415 0.3257 0.036 Uiso 1 1 calc R U . . .
H52C H 0.2190 0.1134 0.3074 0.036 Uiso 1 1 calc R U . . .
C53 C 0.1122(2) 0.38732(13) 0.39968(15) 0.0189(7) Uani 1 1 d . . . . .
C54 C 0.05574(19) 0.39573(15) 0.34908(17) 0.0233(7) Uani 1 1 d . . . . .
C55 C 0.0242(2) 0.45895(15) 0.33861(17) 0.0341(9) Uani 1 1 d . . . . .
H55 H -0.0139 0.4651 0.3049 0.041 Uiso 1 1 calc R U . . .
C56 C 0.0469(2) 0.51308(16) 0.37597(17) 0.0401(10) Uani 1 1 d . . . . .
H56 H 0.0247 0.5560 0.3679 0.048 Uiso 1 1 calc R U . . .
C57 C 0.1021(2) 0.50445(15) 0.42511(16) 0.0353(9) Uani 1 1 d . . . . .
H57 H 0.1176 0.5419 0.4508 0.042 Uiso 1 1 calc R U . . .
C58 C 0.1357(2) 0.44242(14) 0.43787(15) 0.0237(8) Uani 1 1 d . . . . .
C59 C 0.0319(2) 0.33850(16) 0.30416(18) 0.0345(9) Uani 1 1 d . . . . .
H59 H 0.0471 0.2957 0.3262 0.041 Uiso 1 1 calc R U . . .
C60 C -0.0570(2) 0.3361(2) 0.2911(2) 0.0599(12) Uani 1 1 d . . . . .
H60A H -0.0859 0.3395 0.3326 0.090 Uiso 1 1 calc R U . . .
H60B H -0.0704 0.2937 0.2696 0.090 Uiso 1 1 calc R U . . .
H60C H -0.0720 0.3735 0.2626 0.090 Uiso 1 1 calc R U . . .
C61 C 0.0755(3) 0.3414(2) 0.2389(2) 0.0616(13) Uani 1 1 d . . . . .
H61A H 0.0689 0.3860 0.2196 0.092 Uiso 1 1 calc R U . . .
H61B H 0.0534 0.3077 0.2092 0.092 Uiso 1 1 calc R U . . .
H61C H 0.1321 0.3325 0.2459 0.092 Uiso 1 1 calc R U . . .
C62 C 0.1978(2) 0.43782(14) 0.49199(16) 0.0260(8) Uani 1 1 d . . . . .
H62 H 0.2166 0.3904 0.4946 0.031 Uiso 1 1 calc R U . . .
C63 C 0.1611(2) 0.45691(17) 0.55855(16) 0.0357(9) Uani 1 1 d . . . . .
H63A H 0.1381 0.5019 0.5558 0.054 Uiso 1 1 calc R U . . .
H63B H 0.2025 0.4563 0.5923 0.054 Uiso 1 1 calc R U . . .
H63C H 0.1194 0.4247 0.5699 0.054 Uiso 1 1 calc R U . . .
C64 C 0.2695(2) 0.48231(15) 0.47846(17) 0.0330(9) Uani 1 1 d . . . . .
H64A H 0.2520 0.5288 0.4737 0.050 Uiso 1 1 calc R U . . .
H64B H 0.2956 0.4677 0.4381 0.050 Uiso 1 1 calc R U . . .
H64C H 0.3071 0.4790 0.5150 0.050 Uiso 1 1 calc R U . . .
C65 C 0.1200(2) 0.10945(13) 0.41868(14) 0.0180(7) Uani 1 1 d . . . . .
C66 C 0.1497(2) 0.05869(14) 0.45906(16) 0.0265(8) Uani 1 1 d . . . . .
C67 C 0.1161(3) -0.00511(14) 0.45384(16) 0.0399(9) Uani 1 1 d . . . . .
H67 H 0.1363 -0.0402 0.4805 0.048 Uiso 1 1 calc R U . . .
C68 C 0.0549(3) -0.01877(17) 0.41164(18) 0.0488(11) Uani 1 1 d . . . . .
H68 H 0.0332 -0.0626 0.4092 0.059 Uiso 1 1 calc R U . . .
C69 C 0.0255(2) 0.03153(17) 0.37306(16) 0.0366(9) Uani 1 1 d . . . . .
H69 H -0.0172 0.0221 0.3441 0.044 Uiso 1 1 calc R U . . .
C70 C 0.05667(19) 0.09623(15) 0.37532(14) 0.0223(8) Uani 1 1 d . . . . .
C71 C 0.2166(2) 0.06875(15) 0.50791(16) 0.0273(8) Uani 1 1 d . . . . .
H71 H 0.2327 0.1169 0.5065 0.033 Uiso 1 1 calc R U . . .
C72 C 0.1875(2) 0.05311(15) 0.57758(16) 0.0344(9) Uani 1 1 d . . . . .
H72A H 0.1424 0.0822 0.5883 0.052 Uiso 1 1 calc R U . . .
H72B H 0.2307 0.0610 0.6088 0.052 Uiso 1 1 calc R U . . .
H72C H 0.1707 0.0062 0.5800 0.052 Uiso 1 1 calc R U . . .
C73 C 0.2902(2) 0.02627(15) 0.49180(18) 0.0363(9) Uani 1 1 d . . . . .
H73A H 0.2749 -0.0210 0.4892 0.054 Uiso 1 1 calc R U . . .
H73B H 0.3302 0.0321 0.5262 0.054 Uiso 1 1 calc R U . . .
H73C H 0.3123 0.0406 0.4497 0.054 Uiso 1 1 calc R U . . .
C74 C 0.0223(2) 0.14916(16) 0.33090(17) 0.0283(8) Uani 1 1 d . . . . .
H74 H 0.0413 0.1934 0.3476 0.034 Uiso 1 1 calc R U . . .
C75 C 0.0509(3) 0.1429(2) 0.26272(19) 0.0626(13) Uani 1 1 d . . . . .
H75A H 0.1089 0.1470 0.2619 0.094 Uiso 1 1 calc R U . . .
H75B H 0.0272 0.1785 0.2360 0.094 Uiso 1 1 calc R U . . .
H75C H 0.0353 0.0992 0.2452 0.094 Uiso 1 1 calc R U . . .
C76 C -0.0677(2) 0.1504(2) 0.33366(19) 0.0563(12) Uani 1 1 d . . . . .
H76A H -0.0889 0.1122 0.3092 0.084 Uiso 1 1 calc R U . . .
H76B H -0.0872 0.1921 0.3142 0.084 Uiso 1 1 calc R U . . .
H76C H -0.0851 0.1477 0.3793 0.084 Uiso 1 1 calc R U . . .
N1 N 0.69672(18) 0.24349(11) 0.20384(14) 0.0196(6) Uani 1 1 d . . . . .
N2 N 0.64579(15) 0.18252(10) 0.33837(12) 0.0141(6) Uani 1 1 d . . . . .
N3 N 0.65793(15) 0.32853(10) 0.33531(12) 0.0121(5) Uani 1 1 d . . . . .
N4 N 0.19644(16) 0.26701(12) 0.54630(12) 0.0155(6) Uani 1 1 d . . . . .
N5 N 0.14887(15) 0.32218(11) 0.40893(12) 0.0131(5) Uani 1 1 d . . . . .
N6 N 0.15406(16) 0.17630(10) 0.41850(12) 0.0139(6) Uani 1 1 d . . . . .
Nb1 Nb 0.61475(2) 0.25764(2) 0.25669(2) 0.01260(7) Uani 1 1 d . . . . .
Nb2 Nb 0.11462(2) 0.25238(2) 0.49359(2) 0.01302(7) Uani 1 1 d . . . . .
H1 H 0.609(2) 0.3419(18) 0.2257(19) 0.075(13) Uiso 1 1 d . . . . .
H100 H 0.107(2) 0.1748(16) 0.5280(16) 0.048(10) 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 C5 1.363(6) . ?
C1 C2 1.429(6) . ?
C1 Nb1 2.427(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.359(5) . ?
C2 Nb1 2.504(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(5) . ?
C3 Nb1 2.508(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(5) . ?
C4 Nb1 2.440(3) . ?
C4 H4 0.9500 . ?
C5 Nb1 2.411(3) . ?
C5 H5 0.9500 . ?
C6 N1 1.475(4) . ?
C6 C9 1.499(4) . ?
C6 C7 1.523(4) . ?
C6 C8 1.526(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.514(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N2 1.322(4) . ?
C11 C12 1.396(4) . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 N3 1.328(4) . ?
C13 C14 1.519(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.400(4) . ?
C15 C20 1.410(5) . ?
C15 N2 1.458(3) . ?
C16 C17 1.395(4) . ?
C16 C21 1.523(5) . ?
C17 C18 1.371(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.371(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.392(4) . ?
C19 H19 0.9500 . ?
C20 C24 1.506(5) . ?
C21 C23 1.522(5) . ?
C21 C22 1.535(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.533(5) . ?
C24 C26 1.534(5) . ?
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 1.398(4) . ?
C27 C32 1.412(4) . ?
C27 N3 1.453(3) . ?
C28 C29 1.403(4) . ?
C28 C33 1.496(4) . ?
C29 C30 1.385(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.371(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.395(4) . ?
C31 H31 0.9500 . ?
C32 C36 1.520(5) . ?
C33 C35 1.509(5) . ?
C33 C34 1.520(5) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C38 1.530(4) . ?
C36 C37 1.533(4) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C43 1.402(5) . ?
C39 C40 1.413(5) . ?
C39 Nb2 2.434(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.369(5) . ?
C40 Nb2 2.432(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.429(5) . ?
C41 Nb2 2.446(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.374(5) . ?
C42 Nb2 2.510(3) . ?
C42 H42 0.9500 . ?
C43 Nb2 2.504(4) . ?
C43 H43 0.9500 . ?
C44 N4 1.465(4) . ?
C44 C47 1.516(4) . ?
C44 C46 1.526(4) . ?
C44 C45 1.534(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
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 C49 1.501(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 N5 1.342(4) . ?
C49 C50 1.398(4) . ?
C50 C51 1.398(4) . ?
C50 H50 0.9500 . ?
C51 N6 1.342(4) . ?
C51 C52 1.499(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C58 1.406(4) . ?
C53 C54 1.414(5) . ?
C53 N5 1.452(3) . ?
C54 C55 1.386(4) . ?
C54 C59 1.520(4) . ?
C55 C56 1.378(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.379(5) . ?
C56 H56 0.9500 . ?
C57 C58 1.386(4) . ?
C57 H57 0.9500 . ?
C58 C62 1.525(5) . ?
C59 C60 1.519(5) . ?
C59 C61 1.523(6) . ?
C59 H59 1.0000 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C64 1.523(5) . ?
C62 C63 1.542(5) . ?
C62 H62 1.0000 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C66 1.399(4) . ?
C65 C70 1.411(4) . ?
C65 N6 1.453(3) . ?
C66 C67 1.398(4) . ?
C66 C71 1.519(5) . ?
C67 C68 1.370(5) . ?
C67 H67 0.9500 . ?
C68 C69 1.370(5) . ?
C68 H68 0.9500 . ?
C69 C70 1.395(4) . ?
C69 H69 0.9500 . ?
C70 C74 1.509(4) . ?
C71 C73 1.535(5) . ?
C71 C72 1.539(5) . ?
C71 H71 1.0000 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.479(5) . ?
C74 C76 1.514(5) . ?
C74 H74 1.0000 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N1 Nb1 1.774(3) . ?
N2 Nb1 2.305(2) . ?
N3 Nb1 2.262(2) . ?
N4 Nb2 1.772(3) . ?
N5 Nb2 2.296(2) . ?
N6 Nb2 2.259(2) . ?
Nb1 H1 1.80(4) . ?
Nb2 H100 1.71(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
C5 C1 C2 107.3(3) . . ?
C5 C1 Nb1 72.99(19) . . ?
C2 C1 Nb1 76.14(19) . . ?
C5 C1 H1A 126.4 . . ?
C2 C1 H1A 126.4 . . ?
Nb1 C1 H1A 116.6 . . ?
C3 C2 C1 107.8(3) . . ?
C3 C2 Nb1 74.40(19) . . ?
C1 C2 Nb1 70.21(19) . . ?
C3 C2 H2 126.1 . . ?
C1 C2 H2 126.1 . . ?
Nb1 C2 H2 121.0 . . ?
C2 C3 C4 109.2(3) . . ?
C2 C3 Nb1 74.1(2) . . ?
C4 C3 Nb1 71.0(2) . . ?
C2 C3 H3 125.4 . . ?
C4 C3 H3 125.4 . . ?
Nb1 C3 H3 121.1 . . ?
C3 C4 C5 107.0(3) . . ?
C3 C4 Nb1 76.4(2) . . ?
C5 C4 Nb1 72.01(19) . . ?
C3 C4 H4 126.5 . . ?
C5 C4 H4 126.5 . . ?
Nb1 C4 H4 117.2 . . ?
C1 C5 C4 108.7(3) . . ?
C1 C5 Nb1 74.28(19) . . ?
C4 C5 Nb1 74.25(19) . . ?
C1 C5 H5 125.6 . . ?
C4 C5 H5 125.6 . . ?
Nb1 C5 H5 117.7 . . ?
N1 C6 C9 108.7(3) . . ?
N1 C6 C7 109.5(3) . . ?
C9 C6 C7 109.8(3) . . ?
N1 C6 C8 109.2(3) . . ?
C9 C6 C8 110.5(3) . . ?
C7 C6 C8 109.1(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 124.3(3) . . ?
N2 C11 C10 120.6(3) . . ?
C12 C11 C10 115.0(3) . . ?
C13 C12 C11 127.5(4) . . ?
C13 C12 H12 116.3 . . ?
C11 C12 H12 116.3 . . ?
N3 C13 C12 124.6(3) . . ?
N3 C13 C14 119.9(2) . . ?
C12 C13 C14 115.5(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 120.5(3) . . ?
C16 C15 N2 120.3(3) . . ?
C20 C15 N2 119.3(2) . . ?
C17 C16 C15 118.4(3) . . ?
C17 C16 C21 118.4(3) . . ?
C15 C16 C21 123.2(3) . . ?
C18 C17 C16 121.5(3) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 119.7(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C20 121.5(3) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C19 C20 C15 118.3(3) . . ?
C19 C20 C24 118.8(3) . . ?
C15 C20 C24 122.8(3) . . ?
C23 C21 C16 111.9(3) . . ?
C23 C21 C22 108.8(3) . . ?
C16 C21 C22 111.5(3) . . ?
C23 C21 H21 108.2 . . ?
C16 C21 H21 108.2 . . ?
C22 C21 H21 108.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 C25 114.3(3) . . ?
C20 C24 C26 111.5(3) . . ?
C25 C24 C26 106.6(3) . . ?
C20 C24 H24 108.1 . . ?
C25 C24 H24 108.1 . . ?
C26 C24 H24 108.1 . . ?
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 . . ?
C28 C27 C32 120.9(3) . . ?
C28 C27 N3 118.4(2) . . ?
C32 C27 N3 120.8(3) . . ?
C27 C28 C29 118.6(3) . . ?
C27 C28 C33 122.5(3) . . ?
C29 C28 C33 118.9(3) . . ?
C30 C29 C28 120.9(3) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C31 C30 C29 119.7(3) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 121.9(3) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C31 C32 C27 118.0(3) . . ?
C31 C32 C36 118.2(3) . . ?
C27 C32 C36 123.9(2) . . ?
C28 C33 C35 112.1(3) . . ?
C28 C33 C34 112.4(3) . . ?
C35 C33 C34 110.0(3) . . ?
C28 C33 H33 107.4 . . ?
C35 C33 H33 107.4 . . ?
C34 C33 H33 107.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C38 110.0(3) . . ?
C32 C36 C37 112.8(3) . . ?
C38 C36 C37 109.3(3) . . ?
C32 C36 H36 108.2 . . ?
C38 C36 H36 108.2 . . ?
C37 C36 H36 108.2 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C43 C39 C40 106.7(3) . . ?
C43 C39 Nb2 76.27(19) . . ?
C40 C39 Nb2 73.04(18) . . ?
C43 C39 H39 126.7 . . ?
C40 C39 H39 126.7 . . ?
Nb2 C39 H39 116.3 . . ?
C41 C40 C39 109.5(3) . . ?
C41 C40 Nb2 74.3(2) . . ?
C39 C40 Nb2 73.20(18) . . ?
C41 C40 H40 125.3 . . ?
C39 C40 H40 125.3 . . ?
Nb2 C40 H40 119.0 . . ?
C40 C41 C42 106.7(3) . . ?
C40 C41 Nb2 73.1(2) . . ?
C42 C41 Nb2 75.7(2) . . ?
C40 C41 H41 126.6 . . ?
C42 C41 H41 126.6 . . ?
Nb2 C41 H41 116.7 . . ?
C43 C42 C41 108.4(3) . . ?
C43 C42 Nb2 73.9(2) . . ?
C41 C42 Nb2 70.8(2) . . ?
C43 C42 H42 125.8 . . ?
C41 C42 H42 125.8 . . ?
Nb2 C42 H42 121.3 . . ?
C42 C43 C39 108.5(3) . . ?
C42 C43 Nb2 74.3(2) . . ?
C39 C43 Nb2 70.78(19) . . ?
C42 C43 H43 125.7 . . ?
C39 C43 H43 125.7 . . ?
Nb2 C43 H43 120.9 . . ?
N4 C44 C47 108.8(3) . . ?
N4 C44 C46 110.3(3) . . ?
C47 C44 C46 108.8(2) . . ?
N4 C44 C45 109.4(2) . . ?
C47 C44 C45 109.5(3) . . ?
C46 C44 C45 110.0(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N5 C49 C50 124.3(3) . . ?
N5 C49 C48 120.5(2) . . ?
C50 C49 C48 115.2(3) . . ?
C51 C50 C49 127.3(4) . . ?
C51 C50 H50 116.4 . . ?
C49 C50 H50 116.4 . . ?
N6 C51 C50 124.2(3) . . ?
N6 C51 C52 120.8(3) . . ?
C50 C51 C52 115.0(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C58 C53 C54 120.1(3) . . ?
C58 C53 N5 120.6(3) . . ?
C54 C53 N5 119.1(2) . . ?
C55 C54 C53 118.5(3) . . ?
C55 C54 C59 119.4(3) . . ?
C53 C54 C59 122.0(3) . . ?
C56 C55 C54 121.6(3) . . ?
C56 C55 H55 119.2 . . ?
C54 C55 H55 119.2 . . ?
C55 C56 C57 119.5(3) . . ?
C55 C56 H56 120.2 . . ?
C57 C56 H56 120.2 . . ?
C56 C57 C58 121.5(3) . . ?
C56 C57 H57 119.2 . . ?
C58 C57 H57 119.2 . . ?
C57 C58 C53 118.7(3) . . ?
C57 C58 C62 118.0(3) . . ?
C53 C58 C62 123.3(3) . . ?
C60 C59 C54 113.0(3) . . ?
C60 C59 C61 108.7(3) . . ?
C54 C59 C61 111.9(3) . . ?
C60 C59 H59 107.7 . . ?
C54 C59 H59 107.7 . . ?
C61 C59 H59 107.7 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C64 C62 C58 112.1(3) . . ?
C64 C62 C63 109.5(3) . . ?
C58 C62 C63 110.6(3) . . ?
C64 C62 H62 108.2 . . ?
C58 C62 H62 108.2 . . ?
C63 C62 H62 108.2 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C66 C65 C70 120.3(3) . . ?
C66 C65 N6 121.8(3) . . ?
C70 C65 N6 117.9(3) . . ?
C67 C66 C65 118.1(3) . . ?
C67 C66 C71 118.1(3) . . ?
C65 C66 C71 123.8(3) . . ?
C68 C67 C66 122.2(3) . . ?
C68 C67 H67 118.9 . . ?
C66 C67 H67 118.9 . . ?
C67 C68 C69 119.2(3) . . ?
C67 C68 H68 120.4 . . ?
C69 C68 H68 120.4 . . ?
C68 C69 C70 121.6(3) . . ?
C68 C69 H69 119.2 . . ?
C70 C69 H69 119.2 . . ?
C69 C70 C65 118.5(3) . . ?
C69 C70 C74 119.0(3) . . ?
C65 C70 C74 122.4(3) . . ?
C66 C71 C73 112.5(3) . . ?
C66 C71 C72 110.2(3) . . ?
C73 C71 C72 110.1(3) . . ?
C66 C71 H71 108.0 . . ?
C73 C71 H71 108.0 . . ?
C72 C71 H71 108.0 . . ?
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 . . ?
C75 C74 C70 112.6(3) . . ?
C75 C74 C76 111.1(3) . . ?
C70 C74 C76 111.8(3) . . ?
C75 C74 H74 107.0 . . ?
C70 C74 H74 107.0 . . ?
C76 C74 H74 107.0 . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C74 C76 H76A 109.5 . . ?
C74 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C74 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C6 N1 Nb1 168.4(2) . . ?
C11 N2 C15 115.4(2) . . ?
C11 N2 Nb1 121.88(18) . . ?
C15 N2 Nb1 121.83(19) . . ?
C13 N3 C27 115.5(2) . . ?
C13 N3 Nb1 123.05(17) . . ?
C27 N3 Nb1 120.94(18) . . ?
C44 N4 Nb2 168.1(2) . . ?
C49 N5 C53 114.8(2) . . ?
C49 N5 Nb2 121.85(17) . . ?
C53 N5 Nb2 122.38(19) . . ?
C51 N6 C65 115.9(2) . . ?
C51 N6 Nb2 123.39(17) . . ?
C65 N6 Nb2 120.04(19) . . ?
N1 Nb1 N3 106.45(11) . . ?
N1 Nb1 N2 99.31(11) . . ?
N3 Nb1 N2 79.62(9) . . ?
N1 Nb1 C5 92.77(14) . . ?
N3 Nb1 C5 152.43(12) . . ?
N2 Nb1 C5 117.24(12) . . ?
N1 Nb1 C1 105.86(14) . . ?
N3 Nb1 C1 120.63(12) . . ?
N2 Nb1 C1 140.04(12) . . ?
C5 Nb1 C1 32.73(14) . . ?
N1 Nb1 C4 113.02(12) . . ?
N3 Nb1 C4 139.80(11) . . ?
N2 Nb1 C4 86.67(10) . . ?
C5 Nb1 C4 33.73(12) . . ?
C1 Nb1 C4 55.14(13) . . ?
N1 Nb1 C2 139.46(13) . . ?
N3 Nb1 C2 99.27(10) . . ?
N2 Nb1 C2 116.00(11) . . ?
C5 Nb1 C2 54.41(13) . . ?
C1 Nb1 C2 33.65(13) . . ?
C4 Nb1 C2 53.87(12) . . ?
N1 Nb1 C3 144.91(12) . . ?
N3 Nb1 C3 108.64(11) . . ?
N2 Nb1 C3 87.65(10) . . ?
C5 Nb1 C3 54.37(12) . . ?
C1 Nb1 C3 54.30(13) . . ?
C4 Nb1 C3 32.59(12) . . ?
C2 Nb1 C3 31.47(11) . . ?
N1 Nb1 H1 88.8(13) . . ?
N3 Nb1 H1 71.6(12) . . ?
N2 Nb1 H1 151.2(12) . . ?
C5 Nb1 H1 89.7(12) . . ?
C1 Nb1 H1 60.9(13) . . ?
C4 Nb1 H1 115.7(13) . . ?
C2 Nb1 H1 70.1(13) . . ?
C3 Nb1 H1 101.6(13) . . ?
N4 Nb2 N6 107.23(10) . . ?
N4 Nb2 N5 99.41(10) . . ?
N6 Nb2 N5 79.77(9) . . ?
N4 Nb2 C40 91.88(12) . . ?
N6 Nb2 C40 152.98(11) . . ?
N5 Nb2 C40 116.50(10) . . ?
N4 Nb2 C39 111.99(11) . . ?
N6 Nb2 C39 139.90(10) . . ?
N5 Nb2 C39 85.92(10) . . ?
C40 Nb2 C39 33.75(11) . . ?
N4 Nb2 C41 104.65(13) . . ?
N6 Nb2 C41 121.48(11) . . ?
N5 Nb2 C41 139.88(11) . . ?
C40 Nb2 C41 32.59(12) . . ?
C39 Nb2 C41 55.48(12) . . ?
N4 Nb2 C43 144.17(11) . . ?
N6 Nb2 C43 108.60(11) . . ?
N5 Nb2 C43 87.47(10) . . ?
C40 Nb2 C43 54.43(12) . . ?
C39 Nb2 C43 32.95(11) . . ?
C41 Nb2 C43 54.69(12) . . ?
N4 Nb2 C42 138.10(12) . . ?
N6 Nb2 C42 100.00(11) . . ?
N5 Nb2 C42 116.57(11) . . ?
C40 Nb2 C42 54.02(12) . . ?
C39 Nb2 C42 54.20(12) . . ?
C41 Nb2 C42 33.49(12) . . ?
C43 Nb2 C42 31.80(11) . . ?
N4 Nb2 H100 87.4(11) . . ?
N6 Nb2 H100 72.0(11) . . ?
N5 Nb2 H100 151.7(11) . . ?
C40 Nb2 H100 90.4(12) . . ?
C39 Nb2 H100 117.1(12) . . ?
C41 Nb2 H100 61.8(12) . . ?
C43 Nb2 H100 103.0(12) . . ?
C42 Nb2 H100 71.2(12) . . ?

_refine_diff_density_max         0.608
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.058



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'diethyl ether'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1485269'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            '[(BDI)CpNb(NtBu)][BPh4]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H55 N3 Nb 1+, C24 H20 B 1-, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C62.50 H76 B Cl N3 Nb'
_chemical_formula_weight         1008.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'

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

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

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

_cell_length_a                   17.283(5)
_cell_length_b                   17.704(5)
_cell_length_c                   19.633(5)
_cell_angle_alpha                66.416(5)
_cell_angle_beta                 83.348(5)
_cell_angle_gamma                88.954(5)
_cell_volume                     5466(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9506
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      25.35

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             2140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.310
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7003
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 0.8366
_diffrn_reflns_number            87658
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.140
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             20049
_reflns_number_gt                16728
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-2011
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0279P)²+5.7779P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20049
_refine_ls_number_parameters     1249
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0857
_refine_ls_wR_factor_gt          0.0800
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.23270(15) 0.98361(14) 0.32663(15) 0.0312(6) Uani 1 1 d . . . . .
H1 H 1.2583 0.9494 0.3680 0.037 Uiso 1 1 calc R U . . .
C2 C 1.15781(15) 1.01485(15) 0.33032(15) 0.0338(6) Uani 1 1 d . . . . .
H2 H 1.1236 1.0049 0.3747 0.041 Uiso 1 1 calc R U . . .
C3 C 1.14220(16) 1.06308(14) 0.25742(17) 0.0385(7) Uani 1 1 d . . . . .
H3 H 1.0962 1.0927 0.2435 0.046 Uiso 1 1 calc R U . . .
C4 C 1.20688(17) 1.05981(15) 0.20875(15) 0.0386(7) Uani 1 1 d . . . . .
H4 H 1.2120 1.0859 0.1557 0.046 Uiso 1 1 calc R U . . .
C5 C 1.26277(15) 1.01149(15) 0.25176(15) 0.0338(6) Uani 1 1 d . . . . .
H5 H 1.3126 0.9998 0.2330 0.041 Uiso 1 1 calc R U . . .
C6 C 1.26437(14) 0.75958(14) 0.28905(15) 0.0299(6) Uani 1 1 d . . . . .
C7 C 1.2463(2) 0.7258(2) 0.2311(2) 0.0723(12) Uani 1 1 d . . . . .
H7A H 1.1905 0.7115 0.2384 0.108 Uiso 1 1 calc R U . . .
H7B H 1.2765 0.6766 0.2375 0.108 Uiso 1 1 calc R U . . .
H7C H 1.2602 0.7680 0.1804 0.108 Uiso 1 1 calc R U . . .
C8 C 1.34783(17) 0.7908(2) 0.2719(2) 0.0673(10) Uani 1 1 d . . . . .
H8A H 1.3558 0.8350 0.2216 0.101 Uiso 1 1 calc R U . . .
H8B H 1.3824 0.7455 0.2742 0.101 Uiso 1 1 calc R U . . .
H8C H 1.3596 0.8122 0.3086 0.101 Uiso 1 1 calc R U . . .
C9 C 1.24872(19) 0.69354(17) 0.36629(18) 0.0547(9) Uani 1 1 d . . . . .
H9A H 1.2606 0.7152 0.4028 0.082 Uiso 1 1 calc R U . . .
H9B H 1.2816 0.6466 0.3704 0.082 Uiso 1 1 calc R U . . .
H9C H 1.1937 0.6756 0.3762 0.082 Uiso 1 1 calc R U . . .
C10 C 1.11878(15) 1.00005(14) 0.10093(12) 0.0271(5) Uani 1 1 d . . . . .
C11 C 1.06753(17) 1.06580(15) 0.08243(13) 0.0356(6) Uani 1 1 d . . . . .
C12 C 1.0879(2) 1.13414(16) 0.01478(14) 0.0476(8) Uani 1 1 d . . . . .
H12 H 1.0552 1.1803 0.0010 0.057 Uiso 1 1 calc R U . . .
C13 C 1.1543(2) 1.13563(17) -0.03204(15) 0.0502(8) Uani 1 1 d . . . . .
H13 H 1.1673 1.1829 -0.0771 0.060 Uiso 1 1 calc R U . . .
C14 C 1.20179(18) 1.06932(16) -0.01395(14) 0.0395(7) Uani 1 1 d . . . . .
H14 H 1.2465 1.0706 -0.0475 0.047 Uiso 1 1 calc R U . . .
C15 C 1.18548(15) 0.99953(14) 0.05318(13) 0.0298(6) Uani 1 1 d . . . . .
C16 C 0.9919(2) 1.06308(17) 0.13140(15) 0.0485(8) Uani 1 1 d . . . . .
H16 H 1.0014 1.0306 0.1845 0.058 Uiso 1 1 calc R U . . .
C17 C 0.9263(2) 1.0172(3) 0.11472(19) 0.0738(11) Uani 1 1 d . . . . .
H17A H 0.9181 1.0451 0.0619 0.111 Uiso 1 1 calc R U . . .
H17B H 0.8780 1.0171 0.1463 0.111 Uiso 1 1 calc R U . . .
H17C H 0.9411 0.9602 0.1253 0.111 Uiso 1 1 calc R U . . .
C18 C 0.9652(3) 1.1471(2) 0.1259(2) 0.0949(16) Uani 1 1 d . . . . .
H18A H 1.0073 1.1760 0.1360 0.142 Uiso 1 1 calc R U . . .
H18B H 0.9196 1.1404 0.1627 0.142 Uiso 1 1 calc R U . . .
H18C H 0.9513 1.1793 0.0755 0.142 Uiso 1 1 calc R U . . .
C19 C 1.24016(15) 0.92798(15) 0.07009(14) 0.0320(6) Uani 1 1 d . . . . .
H19 H 1.2198 0.8839 0.1195 0.038 Uiso 1 1 calc R U . . .
C20 C 1.24367(18) 0.89137(17) 0.01069(16) 0.0445(7) Uani 1 1 d . . . . .
H20A H 1.1910 0.8749 0.0071 0.067 Uiso 1 1 calc R U . . .
H20B H 1.2765 0.8430 0.0251 0.067 Uiso 1 1 calc R U . . .
H20C H 1.2658 0.9328 -0.0379 0.067 Uiso 1 1 calc R U . . .
C21 C 1.32248(16) 0.95351(18) 0.07573(17) 0.0431(7) Uani 1 1 d . . . . .
H21A H 1.3435 0.9972 0.0280 0.065 Uiso 1 1 calc R U . . .
H21B H 1.3560 0.9058 0.0873 0.065 Uiso 1 1 calc R U . . .
H21C H 1.3207 0.9739 0.1155 0.065 Uiso 1 1 calc R U . . .
C22 C 1.04718(16) 0.84778(16) 0.11684(13) 0.0329(6) Uani 1 1 d . . . . .
H22A H 1.0500 0.8999 0.0725 0.049 Uiso 1 1 calc R U . . .
H22B H 0.9949 0.8225 0.1265 0.049 Uiso 1 1 calc R U . . .
H22C H 1.0858 0.8104 0.1081 0.049 Uiso 1 1 calc R U . . .
C23 C 1.06396(13) 0.86397(13) 0.18337(12) 0.0214(5) Uani 1 1 d . . . . .
C24 C 1.03543(13) 0.80384(13) 0.25383(12) 0.0198(5) Uani 1 1 d . . . . .
H24 H 1.0225 0.7522 0.2532 0.024 Uiso 1 1 calc R U . . .
C25 C 1.02244(12) 0.80574(12) 0.32500(12) 0.0174(4) Uani 1 1 d . . . . .
C26 C 0.96873(14) 0.73930(13) 0.38280(12) 0.0235(5) Uani 1 1 d . . . . .
H26A H 0.9985 0.7021 0.4217 0.035 Uiso 1 1 calc R U . . .
H26B H 0.9445 0.7081 0.3590 0.035 Uiso 1 1 calc R U . . .
H26C H 0.9281 0.7645 0.4053 0.035 Uiso 1 1 calc R U . . .
C27 C 1.02290(12) 0.86988(13) 0.41218(11) 0.0171(4) Uani 1 1 d . . . . .
C28 C 0.95682(13) 0.91733(13) 0.41195(12) 0.0212(5) Uani 1 1 d . . . . .
C29 C 0.92285(14) 0.91588(15) 0.48045(13) 0.0288(5) Uani 1 1 d . . . . .
H29 H 0.8777 0.9468 0.4819 0.035 Uiso 1 1 calc R U . . .
C30 C 0.95337(15) 0.87051(16) 0.54610(13) 0.0321(6) Uani 1 1 d . . . . .
H30 H 0.9280 0.8686 0.5924 0.039 Uiso 1 1 calc R U . . .
C31 C 1.02045(14) 0.82809(15) 0.54480(13) 0.0290(6) Uani 1 1 d . . . . .
H31 H 1.0421 0.7989 0.5902 0.035 Uiso 1 1 calc R U . . .
C32 C 1.05740(13) 0.82710(14) 0.47804(12) 0.0218(5) Uani 1 1 d . . . . .
C33 C 0.92402(13) 0.97149(14) 0.33996(13) 0.0248(5) Uani 1 1 d . . . . .
H33 H 0.9643 0.9763 0.2974 0.030 Uiso 1 1 calc R U . . .
C34 C 0.85047(17) 0.93486(19) 0.32860(17) 0.0513(8) Uani 1 1 d . . . . .
H34A H 0.8104 0.9269 0.3707 0.077 Uiso 1 1 calc R U . . .
H34B H 0.8618 0.8816 0.3259 0.077 Uiso 1 1 calc R U . . .
H34C H 0.8317 0.9724 0.2819 0.077 Uiso 1 1 calc R U . . .
C35 C 0.9096(2) 1.05825(18) 0.3357(2) 0.0680(11) Uani 1 1 d . . . . .
H35A H 0.8694 1.0560 0.3760 0.102 Uiso 1 1 calc R U . . .
H35B H 0.8921 1.0923 0.2872 0.102 Uiso 1 1 calc R U . . .
H35C H 0.9580 1.0823 0.3409 0.102 Uiso 1 1 calc R U . . .
C36 C 1.13278(13) 0.78151(14) 0.48048(13) 0.0266(5) Uani 1 1 d . . . . .
H36 H 1.1540 0.7912 0.4280 0.032 Uiso 1 1 calc R U . . .
C37 C 1.19358(15) 0.81486(16) 0.51397(16) 0.0386(7) Uani 1 1 d . . . . .
H37A H 1.1961 0.8752 0.4900 0.058 Uiso 1 1 calc R U . . .
H37B H 1.2448 0.7935 0.5053 0.058 Uiso 1 1 calc R U . . .
H37C H 1.1785 0.7971 0.5679 0.058 Uiso 1 1 calc R U . . .
C38 C 1.12051(14) 0.68842(15) 0.52530(14) 0.0307(6) Uani 1 1 d . . . . .
H38A H 1.1016 0.6774 0.5775 0.046 Uiso 1 1 calc R U . . .
H38B H 1.1700 0.6611 0.5232 0.046 Uiso 1 1 calc R U . . .
H38C H 1.0821 0.6672 0.5039 0.046 Uiso 1 1 calc R U . . .
C39 C 1.08445(12) 0.42633(13) 0.72041(12) 0.0187(5) Uani 1 1 d . . . . .
C40 C 1.13067(13) 0.45896(14) 0.65083(12) 0.0224(5) Uani 1 1 d . . . . .
H40 H 1.1194 0.5120 0.6156 0.027 Uiso 1 1 calc R U . . .
C41 C 1.19211(13) 0.41729(15) 0.63114(13) 0.0247(5) Uani 1 1 d . . . . .
H41 H 1.2227 0.4426 0.5839 0.030 Uiso 1 1 calc R U . . .
C42 C 1.20903(13) 0.33876(15) 0.68027(13) 0.0260(5) Uani 1 1 d . . . . .
H42 H 1.2510 0.3098 0.6672 0.031 Uiso 1 1 calc R U . . .
C43 C 1.16344(13) 0.30357(14) 0.74878(13) 0.0260(5) Uani 1 1 d . . . . .
H43 H 1.1734 0.2494 0.7827 0.031 Uiso 1 1 calc R U . . .
C44 C 1.10321(13) 0.34691(13) 0.76826(13) 0.0213(5) Uani 1 1 d . . . . .
H44 H 1.0736 0.3216 0.8160 0.026 Uiso 1 1 calc R U . . .
C45 C 0.96142(13) 0.42132(13) 0.81894(13) 0.0235(5) Uani 1 1 d . . . . .
C46 C 0.99267(16) 0.39881(15) 0.88737(13) 0.0320(6) Uani 1 1 d . . . . .
H46 H 1.0428 0.4203 0.8868 0.038 Uiso 1 1 calc R U . . .
C47 C 0.95367(17) 0.34689(16) 0.95523(15) 0.0385(6) Uani 1 1 d . . . . .
H47 H 0.9774 0.3327 0.9998 0.046 Uiso 1 1 calc R U . . .
C48 C 0.88041(17) 0.31571(15) 0.95820(15) 0.0392(7) Uani 1 1 d . . . . .
H48 H 0.8533 0.2801 1.0047 0.047 Uiso 1 1 calc R U . . .
C49 C 0.84691(16) 0.33665(16) 0.89316(16) 0.0390(7) Uani 1 1 d . . . . .
H49 H 0.7963 0.3156 0.8948 0.047 Uiso 1 1 calc R U . . .
C50 C 0.88718(14) 0.38913(14) 0.82410(14) 0.0308(6) Uani 1 1 d . . . . .
H50 H 0.8629 0.4029 0.7798 0.037 Uiso 1 1 calc R U . . .
C51 C 0.96243(12) 0.51472(13) 0.66902(12) 0.0197(5) Uani 1 1 d . . . . .
C52 C 0.94204(14) 0.46350(15) 0.63407(14) 0.0291(6) Uani 1 1 d . . . . .
H52 H 0.9540 0.4068 0.6556 0.035 Uiso 1 1 calc R U . . .
C53 C 0.90525(14) 0.49228(17) 0.56943(14) 0.0333(6) Uani 1 1 d . . . . .
H53 H 0.8935 0.4555 0.5474 0.040 Uiso 1 1 calc R U . . .
C54 C 0.88575(13) 0.57400(16) 0.53708(13) 0.0298(6) Uani 1 1 d . . . . .
H54 H 0.8612 0.5940 0.4926 0.036 Uiso 1 1 calc R U . . .
C55 C 0.90262(13) 0.62612(15) 0.57057(12) 0.0251(5) Uani 1 1 d . . . . .
H55 H 0.8884 0.6822 0.5497 0.030 Uiso 1 1 calc R U . . .
C56 C 0.94035(12) 0.59668(14) 0.63477(12) 0.0203(5) Uani 1 1 d . . . . .
H56 H 0.9517 0.6340 0.6564 0.024 Uiso 1 1 calc R U . . .
C57 C 1.04863(13) 0.55904(13) 0.75298(12) 0.0202(5) Uani 1 1 d . . . . .
C58 C 0.99824(14) 0.60601(14) 0.78050(13) 0.0266(5) Uani 1 1 d . . . . .
H58 H 0.9451 0.5884 0.7956 0.032 Uiso 1 1 calc R U . . .
C59 C 1.02253(16) 0.67722(15) 0.78670(14) 0.0333(6) Uani 1 1 d . . . . .
H59 H 0.9861 0.7074 0.8050 0.040 Uiso 1 1 calc R U . . .
C60 C 1.09964(16) 0.70410(15) 0.76625(14) 0.0349(6) Uani 1 1 d . . . . .
H60 H 1.1165 0.7530 0.7698 0.042 Uiso 1 1 calc R U . . .
C61 C 1.15179(15) 0.65851(15) 0.74048(13) 0.0304(6) Uani 1 1 d . . . . .
H61 H 1.2052 0.6756 0.7270 0.036 Uiso 1 1 calc R U . . .
C62 C 1.12620(13) 0.58756(14) 0.73425(12) 0.0226(5) Uani 1 1 d . . . . .
H62 H 1.1632 0.5573 0.7165 0.027 Uiso 1 1 calc R U . . .
C63 C 0.6915(2) 0.54673(17) 0.6068(2) 0.0215(10) Uani 0.662(7) 1 d G . P A 1
H63 H 0.7220 0.5833 0.5628 0.026 Uiso 0.662(7) 1 calc R U P A 1
C64 C 0.6149(2) 0.5163(3) 0.6109(3) 0.0216(10) Uani 0.662(7) 1 d G . P A 1
H64 H 0.5851 0.5290 0.5702 0.026 Uiso 0.662(7) 1 calc R U P A 1
C65 C 0.59058(19) 0.4636(2) 0.6866(3) 0.0252(12) Uani 0.662(7) 1 d G . P A 1
H65 H 0.5417 0.4348 0.7054 0.030 Uiso 0.662(7) 1 calc R U P A 1
C66 C 0.6522(4) 0.4614(2) 0.72931(13) 0.0259(15) Uani 0.662(7) 1 d G . P A 1
H66 H 0.6518 0.4310 0.7817 0.031 Uiso 0.662(7) 1 calc R U P A 1
C67 C 0.7146(2) 0.5128(3) 0.6800(3) 0.0221(13) Uani 0.662(7) 1 d G . P A 1
H67 H 0.7632 0.5227 0.6935 0.026 Uiso 0.662(7) 1 calc R U P A 1
C68 C 0.72630(13) 0.73419(14) 0.70571(13) 0.0240(5) Uani 1 1 d . . . . .
C69 C 0.79791(16) 0.6860(2) 0.7334(2) 0.0508(8) Uani 1 1 d . . . . .
H69A H 0.7831 0.6404 0.7819 0.076 Uiso 1 1 calc R U . . .
H69B H 0.8364 0.7225 0.7389 0.076 Uiso 1 1 calc R U . . .
H69C H 0.8205 0.6640 0.6972 0.076 Uiso 1 1 calc R U . . .
C70 C 0.74885(17) 0.80777(18) 0.63148(16) 0.0457(7) Uani 1 1 d . . . . .
H70A H 0.7744 0.7881 0.5946 0.069 Uiso 1 1 calc R U . . .
H70B H 0.7847 0.8452 0.6391 0.069 Uiso 1 1 calc R U . . .
H70C H 0.7019 0.8372 0.6132 0.069 Uiso 1 1 calc R U . . .
C71 C 0.68602(15) 0.76430(17) 0.76283(16) 0.0379(7) Uani 1 1 d . . . . .
H71A H 0.6387 0.7928 0.7446 0.057 Uiso 1 1 calc R U . . .
H71B H 0.7213 0.8024 0.7702 0.057 Uiso 1 1 calc R U . . .
H71C H 0.6721 0.7171 0.8105 0.057 Uiso 1 1 calc R U . . .
C72 C 0.52058(14) 0.49475(13) 0.84533(12) 0.0216(5) Uani 1 1 d . . . . .
C73 C 0.45695(15) 0.44238(14) 0.85328(13) 0.0274(5) Uani 1 1 d . . . . .
C74 C 0.45340(17) 0.36381(14) 0.91092(14) 0.0346(6) Uani 1 1 d . . . . .
H74 H 0.4108 0.3274 0.9175 0.042 Uiso 1 1 calc R U . . .
C75 C 0.51010(17) 0.33786(15) 0.95842(14) 0.0355(6) Uani 1 1 d . . . . .
H75 H 0.5075 0.2834 0.9961 0.043 Uiso 1 1 calc R U . . .
C76 C 0.57051(15) 0.39098(15) 0.95111(12) 0.0295(6) Uani 1 1 d . . . . .
H76 H 0.6085 0.3729 0.9851 0.035 Uiso 1 1 calc R U . . .
C77 C 0.57763(14) 0.47118(14) 0.89489(12) 0.0236(5) Uani 1 1 d . . . . .
C78 C 0.39061(16) 0.46946(15) 0.80390(14) 0.0361(7) Uani 1 1 d . . . . .
H78 H 0.4107 0.5178 0.7573 0.043 Uiso 1 1 calc R U . . .
C79 C 0.36546(19) 0.40193(18) 0.78036(17) 0.0488(8) Uani 1 1 d . . . . .
H79A H 0.3407 0.3557 0.8243 0.073 Uiso 1 1 calc R U . . .
H79B H 0.4113 0.3828 0.7581 0.073 Uiso 1 1 calc R U . . .
H79C H 0.3283 0.4241 0.7435 0.073 Uiso 1 1 calc R U . . .
C80 C 0.3220(2) 0.4973(3) 0.8413(2) 0.0773(12) Uani 1 1 d . . . . .
H80A H 0.3004 0.4509 0.8869 0.116 Uiso 1 1 calc R U . . .
H80B H 0.2821 0.5173 0.8071 0.116 Uiso 1 1 calc R U . . .
H80C H 0.3388 0.5419 0.8544 0.116 Uiso 1 1 calc R U . . .
C81 C 0.64342(14) 0.52852(15) 0.89188(13) 0.0293(6) Uani 1 1 d . . . . .
H81 H 0.6453 0.5778 0.8433 0.035 Uiso 1 1 calc R U . . .
C82 C 0.6296(2) 0.5585(2) 0.95450(18) 0.0573(9) Uani 1 1 d . . . . .
H82A H 0.5796 0.5858 0.9519 0.086 Uiso 1 1 calc R U . . .
H82B H 0.6716 0.5977 0.9492 0.086 Uiso 1 1 calc R U . . .
H82C H 0.6288 0.5115 1.0029 0.086 Uiso 1 1 calc R U . . .
C83 C 0.72278(19) 0.4894(3) 0.8952(2) 0.0761(12) Uani 1 1 d . . . . .
H83A H 0.7250 0.4456 0.9450 0.114 Uiso 1 1 calc R U . . .
H83B H 0.7636 0.5314 0.8851 0.114 Uiso 1 1 calc R U . . .
H83C H 0.7308 0.4658 0.8575 0.114 Uiso 1 1 calc R U . . .
C84 C 0.4609(2) 0.64286(16) 0.85590(13) 0.0441(8) Uani 1 1 d . . . . .
H84A H 0.4596 0.5872 0.8956 0.066 Uiso 1 1 calc R U . . .
H84B H 0.4080 0.6639 0.8527 0.066 Uiso 1 1 calc R U . . .
H84C H 0.4944 0.6793 0.8673 0.066 Uiso 1 1 calc R U . . .
C85 C 0.49254(13) 0.64007(13) 0.78280(12) 0.0201(5) Uani 1 1 d . . . . .
C86 C 0.48105(12) 0.71031(12) 0.71829(11) 0.0168(4) Uani 1 1 d . . . . .
H86 H 0.4639 0.7566 0.7282 0.020 Uiso 1 1 calc R U . . .
C87 C 0.49012(12) 0.72482(12) 0.64210(11) 0.0163(4) Uani 1 1 d . . . . .
C88 C 0.45002(14) 0.79844(13) 0.59096(12) 0.0233(5) Uani 1 1 d . . . . .
H88A H 0.4892 0.8383 0.5551 0.035 Uiso 1 1 calc R U . . .
H88B H 0.4196 0.8243 0.6207 0.035 Uiso 1 1 calc R U . . .
H88C H 0.4152 0.7806 0.5638 0.035 Uiso 1 1 calc R U . . .
C89 C 0.52471(12) 0.68735(13) 0.53707(11) 0.0169(4) Uani 1 1 d . . . . .
C90 C 0.57674(13) 0.74195(13) 0.47833(12) 0.0219(5) Uani 1 1 d . . . . .
C91 C 0.56969(14) 0.75005(14) 0.40554(12) 0.0257(5) Uani 1 1 d . . . . .
H91 H 0.6050 0.7858 0.3651 0.031 Uiso 1 1 calc R U . . .
C92 C 0.51238(15) 0.70699(14) 0.39153(12) 0.0281(6) Uani 1 1 d . . . . .
H92 H 0.5081 0.7137 0.3416 0.034 Uiso 1 1 calc R U . . .
C93 C 0.46126(14) 0.65418(14) 0.44967(12) 0.0256(5) Uani 1 1 d . . . . .
H93 H 0.4216 0.6254 0.4390 0.031 Uiso 1 1 calc R U . . .
C94 C 0.46634(13) 0.64193(13) 0.52371(12) 0.0194(5) Uani 1 1 d . . . . .
C95 C 0.41108(13) 0.58039(14) 0.58658(12) 0.0227(5) Uani 1 1 d . . . . .
H95 H 0.4363 0.5629 0.6336 0.027 Uiso 1 1 calc R U . . .
C96 C 0.33387(16) 0.61813(17) 0.59919(17) 0.0435(7) Uani 1 1 d . . . . .
H96A H 0.3097 0.6398 0.5526 0.065 Uiso 1 1 calc R U . . .
H96B H 0.3430 0.6631 0.6147 0.065 Uiso 1 1 calc R U . . .
H96C H 0.2992 0.5758 0.6384 0.065 Uiso 1 1 calc R U . . .
C97 C 0.39578(15) 0.50298(15) 0.57289(15) 0.0356(6) Uani 1 1 d . . . . .
H97A H 0.3641 0.5169 0.5314 0.053 Uiso 1 1 calc R U . . .
H97B H 0.3679 0.4610 0.6182 0.053 Uiso 1 1 calc R U . . .
H97C H 0.4455 0.4815 0.5602 0.053 Uiso 1 1 calc R U . . .
C98 C 0.64008(14) 0.79302(14) 0.48964(13) 0.0271(5) Uani 1 1 d . . . . .
H98 H 0.6355 0.7821 0.5440 0.033 Uiso 1 1 calc R U . . .
C99 C 0.72100(15) 0.76758(17) 0.46748(17) 0.0430(7) Uani 1 1 d . . . . .
H99A H 0.7277 0.7092 0.4983 0.064 Uiso 1 1 calc R U . . .
H99B H 0.7609 0.8009 0.4754 0.064 Uiso 1 1 calc R U . . .
H99C H 0.7263 0.7764 0.4146 0.064 Uiso 1 1 calc R U . . .
C100 C 0.63141(15) 0.88581(14) 0.44533(13) 0.0307(6) Uani 1 1 d . . . . .
H10A H 0.6397 0.8985 0.3916 0.046 Uiso 1 1 calc R U . . .
H10B H 0.6701 0.9166 0.4577 0.046 Uiso 1 1 calc R U . . .
H10C H 0.5789 0.9016 0.4584 0.046 Uiso 1 1 calc R U . . .
C101 C 0.50849(12) 0.98672(14) 0.71570(12) 0.0202(5) Uani 1 1 d . . . . .
C102 C 0.53137(14) 0.93140(16) 0.68244(14) 0.0284(5) Uani 1 1 d . . . . .
H102 H 0.5159 0.8749 0.7087 0.034 Uiso 1 1 calc R U . . .
C103 C 0.57534(14) 0.95538(17) 0.61340(14) 0.0334(6) Uani 1 1 d . . . . .
H103 H 0.5887 0.9156 0.5932 0.040 Uiso 1 1 calc R U . . .
C104 C 0.60013(15) 1.03648(17) 0.57337(13) 0.0336(6) Uani 1 1 d . . . . .
H104 H 0.6302 1.0531 0.5258 0.040 Uiso 1 1 calc R U . . .
C105 C 0.58012(15) 1.09303(16) 0.60438(13) 0.0315(6) Uani 1 1 d . . . . .
H105 H 0.5970 1.1491 0.5782 0.038 Uiso 1 1 calc R U . . .
C106 C 0.53544(13) 1.06811(14) 0.67362(12) 0.0234(5) Uani 1 1 d . . . . .
H106 H 0.5225 1.1083 0.6934 0.028 Uiso 1 1 calc R U . . .
C107 C 0.40890(12) 1.03768(13) 0.80173(12) 0.0186(5) Uani 1 1 d . . . . .
C108 C 0.44717(13) 1.09840(13) 0.81592(12) 0.0197(5) Uani 1 1 d . . . . .
H108 H 0.4996 1.0901 0.8267 0.024 Uiso 1 1 calc R U . . .
C109 C 0.41191(13) 1.16979(13) 0.81486(12) 0.0201(5) Uani 1 1 d . . . . .
H109 H 0.4402 1.2090 0.8248 0.024 Uiso 1 1 calc R U . . .
C110 C 0.33548(13) 1.18397(14) 0.79936(12) 0.0228(5) Uani 1 1 d . . . . .
H110 H 0.3110 1.2329 0.7982 0.027 Uiso 1 1 calc R U . . .
C111 C 0.29531(13) 1.12522(14) 0.78560(12) 0.0223(5) Uani 1 1 d . . . . .
H111 H 0.2428 1.1339 0.7750 0.027 Uiso 1 1 calc R U . . .
C112 C 0.33137(12) 1.05379(13) 0.78723(12) 0.0202(5) Uani 1 1 d . . . . .
H112 H 0.3024 1.0144 0.7782 0.024 Uiso 1 1 calc R U . . .
C113 C 0.50989(12) 0.91921(13) 0.86614(12) 0.0187(5) Uani 1 1 d . . . . .
C114 C 0.49034(13) 0.92407(13) 0.93579(12) 0.0208(5) Uani 1 1 d . . . . .
H114 H 0.4453 0.9532 0.9423 0.025 Uiso 1 1 calc R U . . .
C115 C 0.53355(13) 0.88840(13) 0.99556(13) 0.0241(5) Uani 1 1 d . . . . .
H115 H 0.5177 0.8934 1.0415 0.029 Uiso 1 1 calc R U . . .
C116 C 0.59980(14) 0.84549(13) 0.98834(13) 0.0253(5) Uani 1 1 d . . . . .
H116 H 0.6302 0.8218 1.0287 0.030 Uiso 1 1 calc R U . . .
C117 C 0.62063(13) 0.83798(13) 0.92116(13) 0.0241(5) Uani 1 1 d . . . . .
H117 H 0.6653 0.8079 0.9155 0.029 Uiso 1 1 calc R U . . .
C118 C 0.57656(12) 0.87423(13) 0.86174(13) 0.0208(5) Uani 1 1 d . . . . .
H118 H 0.5924 0.8682 0.8162 0.025 Uiso 1 1 calc R U . . .
C119 C 0.38975(12) 0.88441(14) 0.80871(14) 0.0238(5) Uani 1 1 d . . . . .
C120 C 0.36318(13) 0.82411(14) 0.87927(15) 0.0268(5) Uani 1 1 d . . . . .
H120 H 0.3867 0.8226 0.9212 0.032 Uiso 1 1 calc R U . . .
C121 C 0.30397(14) 0.76614(15) 0.89129(17) 0.0358(6) Uani 1 1 d . . . . .
H121 H 0.2875 0.7271 0.9406 0.043 Uiso 1 1 calc R U . . .
C122 C 0.26941(15) 0.76533(17) 0.83202(18) 0.0408(7) Uani 1 1 d . . . . .
H122 H 0.2297 0.7254 0.8398 0.049 Uiso 1 1 calc R U . . .
C123 C 0.29314(15) 0.82337(17) 0.76115(18) 0.0399(7) Uani 1 1 d . . . . .
H123 H 0.2693 0.8236 0.7198 0.048 Uiso 1 1 calc R U . . .
C124 C 0.35244(14) 0.88242(16) 0.74945(16) 0.0309(6) Uani 1 1 d . . . . .
H124 H 0.3676 0.9220 0.7001 0.037 Uiso 1 1 calc R U . . .
N1 N 1.21286(10) 0.82833(11) 0.28077(10) 0.0207(4) Uani 1 1 d . . . . .
N2 N 1.10353(11) 0.93246(11) 0.17466(10) 0.0200(4) Uani 1 1 d . . . . .
N3 N 1.05478(10) 0.86397(10) 0.34238(9) 0.0156(4) Uani 1 1 d . . . . .
N4 N 0.67065(10) 0.68033(11) 0.69390(10) 0.0186(4) Uani 1 1 d . . . . .
N5 N 0.52970(10) 0.57375(10) 0.78054(9) 0.0176(4) Uani 1 1 d . . . . .
N6 N 0.53093(10) 0.67585(10) 0.61427(9) 0.0162(4) Uani 1 1 d . . . . .
Nb1 Nb 1.15727(2) 0.91594(2) 0.27078(2) 0.01654(5) Uani 1 1 d . . . . .
Nb2 Nb 0.61170(2) 0.60511(2) 0.68486(2) 0.01570(5) Uani 1 1 d . . . . .
B1 B 1.01348(15) 0.47994(15) 0.74086(14) 0.0200(5) Uani 1 1 d . . . . .
B2 B 0.45469(14) 0.95698(16) 0.79784(15) 0.0204(5) Uani 1 1 d . . . . .
C66A C 0.6860(6) 0.4808(5) 0.7245(4) 0.024(3) Uani 0.338(7) 1 d G . P A 2
H66A H 0.7114 0.4665 0.7682 0.028 Uiso 0.338(7) 1 calc R U P A 2
C67A C 0.6112(5) 0.4515(3) 0.7211(5) 0.023(2) Uani 0.338(7) 1 d G . P A 2
H67A H 0.5777 0.4141 0.7622 0.028 Uiso 0.338(7) 1 calc R U P A 2
C65A C 0.5953(4) 0.4879(6) 0.6455(7) 0.0252(12) Uani 0.338(7) 1 d G . P A 2
H65A H 0.5492 0.4792 0.6272 0.030 Uiso 0.338(7) 1 calc R U P A 2
C64A C 0.6602(7) 0.5397(4) 0.6022(3) 0.0216(10) Uani 0.338(7) 1 d G . P A 2
H64A H 0.6652 0.5717 0.5498 0.026 Uiso 0.338(7) 1 calc R U P A 2
C63A C 0.7163(4) 0.5353(5) 0.6510(6) 0.028(3) Uani 0.338(7) 1 d G . P A 2
H63A H 0.7654 0.5639 0.6370 0.034 Uiso 0.338(7) 1 calc R U P A 2


_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 C5 1.388(4) . ?
C1 C2 1.404(4) . ?
C1 Nb1 2.403(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.398(4) . ?
C2 Nb1 2.464(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.400(4) . ?
C3 Nb1 2.523(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.399(4) . ?
C4 Nb1 2.462(2) . ?
C4 H4 0.9500 . ?
C5 Nb1 2.403(2) . ?
C5 H5 0.9500 . ?
C6 N1 1.461(3) . ?
C6 C9 1.496(4) . ?
C6 C8 1.505(4) . ?
C6 C7 1.544(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C15 1.401(3) . ?
C10 C11 1.404(4) . ?
C10 N2 1.461(3) . ?
C11 C12 1.405(4) . ?
C11 C16 1.519(4) . ?
C12 C13 1.379(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.370(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.403(3) . ?
C14 H14 0.9500 . ?
C15 C19 1.517(4) . ?
C16 C18 1.515(4) . ?
C16 C17 1.545(5) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.530(4) . ?
C19 C20 1.540(3) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.504(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 N2 1.343(3) . ?
C23 C24 1.404(3) . ?
C24 C25 1.403(3) . ?
C24 H24 0.9500 . ?
C25 N3 1.356(3) . ?
C25 C26 1.504(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.405(3) . ?
C27 C32 1.407(3) . ?
C27 N3 1.459(3) . ?
C28 C29 1.394(3) . ?
C28 C33 1.523(3) . ?
C29 C30 1.378(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.373(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.396(3) . ?
C31 H31 0.9500 . ?
C32 C36 1.515(3) . ?
C33 C34 1.516(3) . ?
C33 C35 1.522(4) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C38 1.531(3) . ?
C36 C37 1.542(3) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C44 1.401(3) . ?
C39 C40 1.404(3) . ?
C39 B1 1.648(3) . ?
C40 C41 1.388(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.388(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.386(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.390(3) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C50 1.390(3) . ?
C45 C46 1.410(3) . ?
C45 B1 1.636(3) . ?
C46 C47 1.382(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.376(4) . ?
C47 H47 0.9500 . ?
C48 C49 1.374(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.408(4) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 C56 1.401(3) . ?
C51 C52 1.408(3) . ?
C51 B1 1.649(3) . ?
C52 C53 1.390(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.381(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.382(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.392(3) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C62 1.396(3) . ?
C57 C58 1.402(3) . ?
C57 B1 1.649(3) . ?
C58 C59 1.391(3) . ?
C58 H58 0.9500 . ?
C59 C60 1.382(4) . ?
C59 H59 0.9500 . ?
C60 C61 1.384(4) . ?
C60 H60 0.9500 . ?
C61 C62 1.394(3) . ?
C61 H61 0.9500 . ?
C62 H62 0.9500 . ?
C63 C67 1.4200 . ?
C63 C64 1.4200 . ?
C63 Nb2 2.458(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.4200 . ?
C64 Nb2 2.527(3) . ?
C64 H64 0.9500 . ?
C65 C66 1.4200 . ?
C65 Nb2 2.524(3) . ?
C65 H65 0.9500 . ?
C66 C67 1.4200 . ?
C66 Nb2 2.454(4) . ?
C66 H66 0.9500 . ?
C67 Nb2 2.413(4) . ?
C67 H67 0.9500 . ?
C68 N4 1.467(3) . ?
C68 C69 1.517(4) . ?
C68 C71 1.520(3) . ?
C68 C70 1.530(4) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 C73 1.405(3) . ?
C72 C77 1.406(3) . ?
C72 N5 1.462(3) . ?
C73 C74 1.395(3) . ?
C73 C78 1.533(3) . ?
C74 C75 1.376(4) . ?
C74 H74 0.9500 . ?
C75 C76 1.374(4) . ?
C75 H75 0.9500 . ?
C76 C77 1.404(3) . ?
C76 H76 0.9500 . ?
C77 C81 1.518(3) . ?
C78 C80 1.501(4) . ?
C78 C79 1.530(3) . ?
C78 H78 1.0000 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 C82 1.517(4) . ?
C81 C83 1.522(4) . ?
C81 H81 1.0000 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 C85 1.495(3) . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 N5 1.342(3) . ?
C85 C86 1.407(3) . ?
C86 C87 1.403(3) . ?
C86 H86 0.9500 . ?
C87 N6 1.347(3) . ?
C87 C88 1.506(3) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 C90 1.404(3) . ?
C89 C94 1.412(3) . ?
C89 N6 1.463(3) . ?
C90 C91 1.398(3) . ?
C90 C98 1.523(3) . ?
C91 C92 1.377(3) . ?
C91 H91 0.9500 . ?
C92 C93 1.378(3) . ?
C92 H92 0.9500 . ?
C93 C94 1.394(3) . ?
C93 H93 0.9500 . ?
C94 C95 1.520(3) . ?
C95 C96 1.520(3) . ?
C95 C97 1.531(3) . ?
C95 H95 1.0000 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
C98 C99 1.530(4) . ?
C98 C100 1.535(3) . ?
C98 H98 1.0000 . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
C99 H99C 0.9800 . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
C101 C106 1.399(3) . ?
C101 C102 1.407(3) . ?
C101 B2 1.653(3) . ?
C102 C103 1.381(4) . ?
C102 H102 0.9500 . ?
C103 C104 1.380(4) . ?
C103 H103 0.9500 . ?
C104 C105 1.385(3) . ?
C104 H104 0.9500 . ?
C105 C106 1.389(3) . ?
C105 H105 0.9500 . ?
C106 H106 0.9500 . ?
C107 C112 1.403(3) . ?
C107 C108 1.407(3) . ?
C107 B2 1.645(3) . ?
C108 C109 1.387(3) . ?
C108 H108 0.9500 . ?
C109 C110 1.386(3) . ?
C109 H109 0.9500 . ?
C110 C111 1.390(3) . ?
C110 H110 0.9500 . ?
C111 C112 1.390(3) . ?
C111 H111 0.9500 . ?
C112 H112 0.9500 . ?
C113 C118 1.403(3) . ?
C113 C114 1.406(3) . ?
C113 B2 1.646(3) . ?
C114 C115 1.388(3) . ?
C114 H114 0.9500 . ?
C115 C116 1.387(3) . ?
C115 H115 0.9500 . ?
C116 C117 1.384(3) . ?
C116 H116 0.9500 . ?
C117 C118 1.393(3) . ?
C117 H117 0.9500 . ?
C118 H118 0.9500 . ?
C119 C120 1.399(3) . ?
C119 C124 1.406(3) . ?
C119 B2 1.653(3) . ?
C120 C121 1.394(3) . ?
C120 H120 0.9500 . ?
C121 C122 1.373(4) . ?
C121 H121 0.9500 . ?
C122 C123 1.378(4) . ?
C122 H122 0.9500 . ?
C123 C124 1.410(3) . ?
C123 H123 0.9500 . ?
C124 H124 0.9500 . ?
N1 Nb1 1.7644(18) . ?
N2 Nb1 2.1127(19) . ?
N3 Nb1 2.0995(17) . ?
N4 Nb2 1.7672(17) . ?
N5 Nb2 2.1030(18) . ?
N6 Nb2 2.1056(18) . ?
Nb2 C63A 2.352(9) . ?
Nb2 C64A 2.414(7) . ?
Nb2 C66A 2.420(8) . ?
Nb2 C65A 2.517(6) . ?
Nb2 C67A 2.520(6) . ?
C66A C67A 1.4200 . ?
C66A C63A 1.4200 . ?
C66A H66A 0.9500 . ?
C67A C65A 1.4200 . ?
C67A H67A 0.9500 . ?
C65A C64A 1.4200 . ?
C65A H65A 0.9500 . ?
C64A C63A 1.4200 . ?
C64A H64A 0.9500 . ?
C63A H63A 0.9500 . ?

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
C5 C1 C2 107.9(2) . . ?
C5 C1 Nb1 73.21(14) . . ?
C2 C1 Nb1 75.64(13) . . ?
C5 C1 H1 126.1 . . ?
C2 C1 H1 126.1 . . ?
Nb1 C1 H1 117.1 . . ?
C3 C2 C1 108.3(2) . . ?
C3 C2 Nb1 76.06(14) . . ?
C1 C2 Nb1 70.87(13) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
Nb1 C2 H2 119.0 . . ?
C2 C3 C4 107.4(2) . . ?
C2 C3 Nb1 71.42(13) . . ?
C4 C3 Nb1 71.30(14) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
Nb1 C3 H3 122.7 . . ?
C5 C4 C3 108.3(2) . . ?
C5 C4 Nb1 70.99(13) . . ?
C3 C4 Nb1 76.11(14) . . ?
C5 C4 H4 125.9 . . ?
C3 C4 H4 125.9 . . ?
Nb1 C4 H4 118.9 . . ?
C1 C5 C4 108.1(2) . . ?
C1 C5 Nb1 73.22(13) . . ?
C4 C5 Nb1 75.60(14) . . ?
C1 C5 H5 125.9 . . ?
C4 C5 H5 125.9 . . ?
Nb1 C5 H5 117.2 . . ?
N1 C6 C9 110.1(2) . . ?
N1 C6 C8 109.3(2) . . ?
C9 C6 C8 111.5(3) . . ?
N1 C6 C7 106.8(2) . . ?
C9 C6 C7 109.8(3) . . ?
C8 C6 C7 109.2(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C10 C11 122.4(2) . . ?
C15 C10 N2 119.5(2) . . ?
C11 C10 N2 117.9(2) . . ?
C10 C11 C12 117.0(3) . . ?
C10 C11 C16 122.2(2) . . ?
C12 C11 C16 120.8(2) . . ?
C13 C12 C11 121.4(3) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C12 120.4(2) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 121.2(3) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C10 C15 C14 117.6(2) . . ?
C10 C15 C19 123.7(2) . . ?
C14 C15 C19 118.7(2) . . ?
C18 C16 C11 113.9(3) . . ?
C18 C16 C17 110.0(3) . . ?
C11 C16 C17 111.1(2) . . ?
C18 C16 H16 107.2 . . ?
C11 C16 H16 107.2 . . ?
C17 C16 H16 107.2 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 C21 111.6(2) . . ?
C15 C19 C20 111.6(2) . . ?
C21 C19 C20 109.4(2) . . ?
C15 C19 H19 108.0 . . ?
C21 C19 H19 108.0 . . ?
C20 C19 H19 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 C24 122.93(19) . . ?
N2 C23 C22 121.1(2) . . ?
C24 C23 C22 116.0(2) . . ?
C25 C24 C23 132.0(2) . . ?
C25 C24 H24 114.0 . . ?
C23 C24 H24 114.0 . . ?
N3 C25 C24 123.31(19) . . ?
N3 C25 C26 120.33(19) . . ?
C24 C25 C26 116.36(18) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C32 121.5(2) . . ?
C28 C27 N3 118.55(18) . . ?
C32 C27 N3 119.91(19) . . ?
C29 C28 C27 117.7(2) . . ?
C29 C28 C33 120.1(2) . . ?
C27 C28 C33 122.23(19) . . ?
C30 C29 C28 121.4(2) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C31 C30 C29 120.1(2) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C32 121.2(2) . . ?
C30 C31 H31 119.4 . . ?
C32 C31 H31 119.4 . . ?
C31 C32 C27 117.8(2) . . ?
C31 C32 C36 118.3(2) . . ?
C27 C32 C36 123.9(2) . . ?
C34 C33 C35 110.0(2) . . ?
C34 C33 C28 113.0(2) . . ?
C35 C33 C28 111.7(2) . . ?
C34 C33 H33 107.3 . . ?
C35 C33 H33 107.3 . . ?
C28 C33 H33 107.3 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C38 112.18(19) . . ?
C32 C36 C37 110.7(2) . . ?
C38 C36 C37 109.4(2) . . ?
C32 C36 H36 108.1 . . ?
C38 C36 H36 108.1 . . ?
C37 C36 H36 108.1 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C44 C39 C40 115.0(2) . . ?
C44 C39 B1 124.45(19) . . ?
C40 C39 B1 120.50(19) . . ?
C41 C40 C39 123.0(2) . . ?
C41 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
C40 C41 C42 120.2(2) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 118.5(2) . . ?
C43 C42 H42 120.7 . . ?
C41 C42 H42 120.7 . . ?
C42 C43 C44 120.5(2) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C43 C44 C39 122.7(2) . . ?
C43 C44 H44 118.7 . . ?
C39 C44 H44 118.7 . . ?
C50 C45 C46 115.4(2) . . ?
C50 C45 B1 125.0(2) . . ?
C46 C45 B1 119.5(2) . . ?
C47 C46 C45 123.0(3) . . ?
C47 C46 H46 118.5 . . ?
C45 C46 H46 118.5 . . ?
C48 C47 C46 120.0(3) . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C49 C48 C47 119.3(2) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 H48 120.4 . . ?
C48 C49 C50 120.4(3) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C45 C50 C49 121.8(2) . . ?
C45 C50 H50 119.1 . . ?
C49 C50 H50 119.1 . . ?
C56 C51 C52 114.6(2) . . ?
C56 C51 B1 124.17(19) . . ?
C52 C51 B1 121.2(2) . . ?
C53 C52 C51 122.9(2) . . ?
C53 C52 H52 118.6 . . ?
C51 C52 H52 118.6 . . ?
C54 C53 C52 120.3(2) . . ?
C54 C53 H53 119.8 . . ?
C52 C53 H53 119.8 . . ?
C53 C54 C55 118.8(2) . . ?
C53 C54 H54 120.6 . . ?
C55 C54 H54 120.6 . . ?
C54 C55 C56 120.2(2) . . ?
C54 C55 H55 119.9 . . ?
C56 C55 H55 119.9 . . ?
C55 C56 C51 123.2(2) . . ?
C55 C56 H56 118.4 . . ?
C51 C56 H56 118.4 . . ?
C62 C57 C58 115.0(2) . . ?
C62 C57 B1 125.2(2) . . ?
C58 C57 B1 119.7(2) . . ?
C59 C58 C57 123.0(2) . . ?
C59 C58 H58 118.5 . . ?
C57 C58 H58 118.5 . . ?
C60 C59 C58 120.1(2) . . ?
C60 C59 H59 119.9 . . ?
C58 C59 H59 119.9 . . ?
C59 C60 C61 118.8(2) . . ?
C59 C60 H60 120.6 . . ?
C61 C60 H60 120.6 . . ?
C60 C61 C62 120.2(2) . . ?
C60 C61 H61 119.9 . . ?
C62 C61 H61 119.9 . . ?
C61 C62 C57 122.9(2) . . ?
C61 C62 H62 118.6 . . ?
C57 C62 H62 118.6 . . ?
C67 C63 C64 108.0 . . ?
C67 C63 Nb2 71.28(13) . . ?
C64 C63 Nb2 76.11(12) . . ?
C67 C63 H63 126.0 . . ?
C64 C63 H63 126.0 . . ?
Nb2 C63 H63 118.5 . . ?
C63 C64 C65 108.0 . . ?
C63 C64 Nb2 70.83(12) . . ?
C65 C64 Nb2 73.57(11) . . ?
C63 C64 H64 126.0 . . ?
C65 C64 H64 126.0 . . ?
Nb2 C64 H64 121.3 . . ?
C66 C65 C64 108.0 . . ?
C66 C65 Nb2 70.73(13) . . ?
C64 C65 Nb2 73.78(11) . . ?
C66 C65 H65 126.0 . . ?
C64 C65 H65 126.0 . . ?
Nb2 C65 H65 121.2 . . ?
C67 C66 C65 108.0 . . ?
C67 C66 Nb2 71.44(12) . . ?
C65 C66 Nb2 76.15(12) . . ?
C67 C66 H66 126.0 . . ?
C65 C66 H66 126.0 . . ?
Nb2 C66 H66 118.3 . . ?
C66 C67 C63 108.0 . . ?
C66 C67 Nb2 74.64(11) . . ?
C63 C67 Nb2 74.83(12) . . ?
C66 C67 H67 126.0 . . ?
C63 C67 H67 126.0 . . ?
Nb2 C67 H67 116.6 . . ?
N4 C68 C69 109.20(19) . . ?
N4 C68 C71 107.75(18) . . ?
C69 C68 C71 111.2(2) . . ?
N4 C68 C70 108.76(19) . . ?
C69 C68 C70 110.2(2) . . ?
C71 C68 C70 109.7(2) . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C68 C71 H71A 109.5 . . ?
C68 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C68 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C73 C72 C77 122.0(2) . . ?
C73 C72 N5 118.35(19) . . ?
C77 C72 N5 119.5(2) . . ?
C74 C73 C72 117.7(2) . . ?
C74 C73 C78 119.5(2) . . ?
C72 C73 C78 122.8(2) . . ?
C75 C74 C73 121.6(2) . . ?
C75 C74 H74 119.2 . . ?
C73 C74 H74 119.2 . . ?
C76 C75 C74 119.8(2) . . ?
C76 C75 H75 120.1 . . ?
C74 C75 H75 120.1 . . ?
C75 C76 C77 121.9(2) . . ?
C75 C76 H76 119.1 . . ?
C77 C76 H76 119.1 . . ?
C76 C77 C72 117.0(2) . . ?
C76 C77 C81 119.5(2) . . ?
C72 C77 C81 123.4(2) . . ?
C80 C78 C79 110.6(3) . . ?
C80 C78 C73 111.6(2) . . ?
C79 C78 C73 112.0(2) . . ?
C80 C78 H78 107.4 . . ?
C79 C78 H78 107.4 . . ?
C73 C78 H78 107.4 . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C82 C81 C77 111.7(2) . . ?
C82 C81 C83 108.5(3) . . ?
C77 C81 C83 113.1(2) . . ?
C82 C81 H81 107.8 . . ?
C77 C81 H81 107.8 . . ?
C83 C81 H81 107.8 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C85 C84 H84A 109.5 . . ?
C85 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C85 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
N5 C85 C86 123.18(19) . . ?
N5 C85 C84 120.8(2) . . ?
C86 C85 C84 116.1(2) . . ?
C87 C86 C85 132.08(19) . . ?
C87 C86 H86 114.0 . . ?
C85 C86 H86 114.0 . . ?
N6 C87 C86 123.26(19) . . ?
N6 C87 C88 120.08(18) . . ?
C86 C87 C88 116.64(18) . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C90 C89 C94 121.49(19) . . ?
C90 C89 N6 119.96(18) . . ?
C94 C89 N6 118.54(18) . . ?
C91 C90 C89 118.1(2) . . ?
C91 C90 C98 118.3(2) . . ?
C89 C90 C98 123.6(2) . . ?
C92 C91 C90 121.0(2) . . ?
C92 C91 H91 119.5 . . ?
C90 C91 H91 119.5 . . ?
C91 C92 C93 120.2(2) . . ?
C91 C92 H92 119.9 . . ?
C93 C92 H92 119.9 . . ?
C92 C93 C94 121.6(2) . . ?
C92 C93 H93 119.2 . . ?
C94 C93 H93 119.2 . . ?
C93 C94 C89 117.5(2) . . ?
C93 C94 C95 120.0(2) . . ?
C89 C94 C95 122.46(19) . . ?
C96 C95 C94 112.1(2) . . ?
C96 C95 C97 109.4(2) . . ?
C94 C95 C97 112.08(19) . . ?
C96 C95 H95 107.7 . . ?
C94 C95 H95 107.7 . . ?
C97 C95 H95 107.7 . . ?
C95 C96 H96A 109.5 . . ?
C95 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
C95 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C95 C97 H97A 109.5 . . ?
C95 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
C95 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
C90 C98 C99 110.7(2) . . ?
C90 C98 C100 112.0(2) . . ?
C99 C98 C100 109.7(2) . . ?
C90 C98 H98 108.1 . . ?
C99 C98 H98 108.1 . . ?
C100 C98 H98 108.1 . . ?
C98 C99 H99A 109.5 . . ?
C98 C99 H99B 109.5 . . ?
H99A C99 H99B 109.5 . . ?
C98 C99 H99C 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?
C98 C100 H10A 109.5 . . ?
C98 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C98 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C106 C101 C102 114.3(2) . . ?
C106 C101 B2 123.39(19) . . ?
C102 C101 B2 122.3(2) . . ?
C103 C102 C101 123.1(2) . . ?
C103 C102 H102 118.5 . . ?
C101 C102 H102 118.5 . . ?
C104 C103 C102 120.8(2) . . ?
C104 C103 H103 119.6 . . ?
C102 C103 H103 119.6 . . ?
C103 C104 C105 118.3(2) . . ?
C103 C104 H104 120.8 . . ?
C105 C104 H104 120.8 . . ?
C104 C105 C106 120.3(2) . . ?
C104 C105 H105 119.9 . . ?
C106 C105 H105 119.9 . . ?
C105 C106 C101 123.3(2) . . ?
C105 C106 H106 118.4 . . ?
C101 C106 H106 118.4 . . ?
C112 C107 C108 115.12(19) . . ?
C112 C107 B2 123.33(18) . . ?
C108 C107 B2 121.46(19) . . ?
C109 C108 C107 123.0(2) . . ?
C109 C108 H108 118.5 . . ?
C107 C108 H108 118.5 . . ?
C110 C109 C108 120.1(2) . . ?
C110 C109 H109 119.9 . . ?
C108 C109 H109 119.9 . . ?
C109 C110 C111 118.7(2) . . ?
C109 C110 H110 120.6 . . ?
C111 C110 H110 120.6 . . ?
C110 C111 C112 120.5(2) . . ?
C110 C111 H111 119.8 . . ?
C112 C111 H111 119.8 . . ?
C111 C112 C107 122.5(2) . . ?
C111 C112 H112 118.7 . . ?
C107 C112 H112 118.7 . . ?
C118 C113 C114 114.6(2) . . ?
C118 C113 B2 122.87(19) . . ?
C114 C113 B2 122.34(19) . . ?
C115 C114 C113 123.3(2) . . ?
C115 C114 H114 118.4 . . ?
C113 C114 H114 118.4 . . ?
C116 C115 C114 120.2(2) . . ?
C116 C115 H115 119.9 . . ?
C114 C115 H115 119.9 . . ?
C117 C116 C115 118.6(2) . . ?
C117 C116 H116 120.7 . . ?
C115 C116 H116 120.7 . . ?
C116 C117 C118 120.4(2) . . ?
C116 C117 H117 119.8 . . ?
C118 C117 H117 119.8 . . ?
C117 C118 C113 122.9(2) . . ?
C117 C118 H118 118.5 . . ?
C113 C118 H118 118.5 . . ?
C120 C119 C124 114.9(2) . . ?
C120 C119 B2 121.9(2) . . ?
C124 C119 B2 123.0(2) . . ?
C121 C120 C119 123.4(2) . . ?
C121 C120 H120 118.3 . . ?
C119 C120 H120 118.3 . . ?
C122 C121 C120 120.1(3) . . ?
C122 C121 H121 119.9 . . ?
C120 C121 H121 119.9 . . ?
C121 C122 C123 119.0(2) . . ?
C121 C122 H122 120.5 . . ?
C123 C122 H122 120.5 . . ?
C122 C123 C124 120.6(2) . . ?
C122 C123 H123 119.7 . . ?
C124 C123 H123 119.7 . . ?
C119 C124 C123 121.9(3) . . ?
C119 C124 H124 119.1 . . ?
C123 C124 H124 119.1 . . ?
C6 N1 Nb1 175.41(15) . . ?
C23 N2 C10 120.48(18) . . ?
C23 N2 Nb1 111.53(14) . . ?
C10 N2 Nb1 126.68(14) . . ?
C25 N3 C27 117.20(17) . . ?
C25 N3 Nb1 111.13(13) . . ?
C27 N3 Nb1 130.64(13) . . ?
C68 N4 Nb2 172.68(16) . . ?
C85 N5 C72 120.44(18) . . ?
C85 N5 Nb2 111.70(14) . . ?
C72 N5 Nb2 127.01(14) . . ?
C87 N6 C89 118.63(17) . . ?
C87 N6 Nb2 112.66(13) . . ?
C89 N6 Nb2 127.80(13) . . ?
N1 Nb1 N3 102.37(8) . . ?
N1 Nb1 N2 101.16(8) . . ?
N3 Nb1 N2 92.27(7) . . ?
N1 Nb1 C5 98.17(9) . . ?
N3 Nb1 C5 141.23(8) . . ?
N2 Nb1 C5 115.58(8) . . ?
N1 Nb1 C1 101.44(9) . . ?
N3 Nb1 C1 109.36(8) . . ?
N2 Nb1 C1 144.27(8) . . ?
C5 Nb1 C1 33.57(9) . . ?
N1 Nb1 C4 125.23(9) . . ?
N3 Nb1 C4 131.14(8) . . ?
N2 Nb1 C4 89.05(8) . . ?
C5 Nb1 C4 33.41(9) . . ?
C1 Nb1 C4 55.26(9) . . ?
N1 Nb1 C2 131.92(9) . . ?
N3 Nb1 C2 86.95(7) . . ?
N2 Nb1 C2 125.79(8) . . ?
C5 Nb1 C2 55.23(8) . . ?
C1 Nb1 C2 33.49(9) . . ?
C4 Nb1 C2 54.48(9) . . ?
N1 Nb1 C3 152.72(8) . . ?
N3 Nb1 C3 98.80(8) . . ?
N2 Nb1 C3 94.94(8) . . ?
C5 Nb1 C3 54.77(9) . . ?
C1 Nb1 C3 54.82(9) . . ?
C4 Nb1 C3 32.59(9) . . ?
C2 Nb1 C3 32.52(9) . . ?
N4 Nb2 N5 101.50(7) . . ?
N4 Nb2 N6 103.25(8) . . ?
N5 Nb2 N6 92.14(7) . . ?
N4 Nb2 C63A 95.30(16) . . ?
N5 Nb2 C63A 133.2(2) . . ?
N6 Nb2 C63A 125.9(3) . . ?
N4 Nb2 C67 96.89(10) . . ?
N5 Nb2 C67 120.46(15) . . ?
N6 Nb2 C67 137.16(11) . . ?
N4 Nb2 C64A 119.4(3) . . ?
N5 Nb2 C64A 135.7(2) . . ?
N6 Nb2 C64A 94.1(2) . . ?
C63A Nb2 C64A 34.63(10) . . ?
N4 Nb2 C66A 105.1(2) . . ?
N5 Nb2 C66A 98.7(3) . . ?
N6 Nb2 C66A 146.81(16) . . ?
C63A Nb2 C66A 34.59(11) . . ?
C64A Nb2 C66A 56.76(12) . . ?
N4 Nb2 C66 119.69(17) . . ?
N5 Nb2 C66 89.75(11) . . ?
N6 Nb2 C66 135.68(15) . . ?
C67 Nb2 C66 33.9 . . ?
N4 Nb2 C63 107.01(12) . . ?
N5 Nb2 C63 143.03(7) . . ?
N6 Nb2 C63 103.48(12) . . ?
C67 Nb2 C63 33.9 . . ?
C66 Nb2 C63 55.77(6) . . ?
N4 Nb2 C65A 151.0(2) . . ?
N5 Nb2 C65A 102.7(3) . . ?
N6 Nb2 C65A 91.64(18) . . ?
C63A Nb2 C65A 56.19(10) . . ?
C64A Nb2 C65A 33.39(8) . . ?
C66A Nb2 C65A 55.43(8) . . ?
N4 Nb2 C67A 137.5(3) . . ?
N5 Nb2 C67A 83.41(13) . . ?
N6 Nb2 C67A 118.9(3) . . ?
C63A Nb2 C67A 56.14(10) . . ?
C64A Nb2 C67A 55.45(8) . . ?
C66A Nb2 C67A 33.33(7) . . ?
C65A Nb2 C67A 32.75(7) . . ?
N4 Nb2 C65 151.49(12) . . ?
N5 Nb2 C65 89.28(10) . . ?
N6 Nb2 C65 102.62(15) . . ?
C67 Nb2 C65 55.42(5) . . ?
C66 Nb2 C65 33.1 . . ?
C63 Nb2 C65 54.9 . . ?
C45 B1 C39 109.44(18) . . ?
C45 B1 C57 107.85(18) . . ?
C39 B1 C57 110.88(18) . . ?
C45 B1 C51 112.83(18) . . ?
C39 B1 C51 106.98(17) . . ?
C57 B1 C51 108.89(18) . . ?
C107 B2 C113 110.36(17) . . ?
C107 B2 C101 107.99(18) . . ?
C113 B2 C101 110.42(18) . . ?
C107 B2 C119 109.07(18) . . ?
C113 B2 C119 107.78(18) . . ?
C101 B2 C119 111.23(18) . . ?
C67A C66A C63A 108.0 . . ?
C67A C66A Nb2 77.2(3) . . ?
C63A C66A Nb2 70.1(3) . . ?
C67A C66A H66A 126.0 . . ?
C63A C66A H66A 126.0 . . ?
Nb2 C66A H66A 118.5 . . ?
C66A C67A C65A 108.0 . . ?
C66A C67A Nb2 69.5(3) . . ?
C65A C67A Nb2 73.5(3) . . ?
C66A C67A H67A 126.0 . . ?
C65A C67A H67A 126.0 . . ?
Nb2 C67A H67A 122.7 . . ?
C67A C65A C64A 108.0 . . ?
C67A C65A Nb2 73.8(2) . . ?
C64A C65A Nb2 69.3(3) . . ?
C67A C65A H65A 126.0 . . ?
C64A C65A H65A 126.0 . . ?
Nb2 C65A H65A 122.6 . . ?
C63A C64A C65A 108.0 . . ?
C63A C64A Nb2 70.3(3) . . ?
C65A C64A Nb2 77.3(3) . . ?
C63A C64A H64A 126.0 . . ?
C65A C64A H64A 126.0 . . ?
Nb2 C64A H64A 118.3 . . ?
C64A C63A C66A 108.0 . . ?
C64A C63A Nb2 75.1(3) . . ?
C66A C63A Nb2 75.3(3) . . ?
C64A C63A H63A 126.0 . . ?
C66A C63A H63A 126.0 . . ?
Nb2 C63A H63A 115.8 . . ?

_refine_diff_density_max         0.559
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.056

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 305 94 'position disordered dichloromethane'
2 0.266 -0.042 0.559 24 0 ' '
3 0.424 0.748 0.135 18 0 ' '
4 0.576 0.252 0.865 17 0 ' '
5 0.734 0.042 0.441 24 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?





_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dichloromethane/hexane'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1485270'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT058_Compound2           
;
PROBLEM: Maximum Transmission Factor Missing ............          ?
RESPONSE: Parameter missing because of file loss due to database server crash
;
_vrf_PLAT059_Compound2           
;
PROBLEM: Minimum Transmission Factor Missing ............          ?
RESPONSE: Parameter missing because of file loss due to database server crash
;
_vrf_PLAT183_Compound2           
;
PROBLEM: Missing _cell_measurement_reflns_used value ....     Please Do !
RESPONSE: Parameter missing because of file loss due to database server crash
;
_vrf_PLAT184_Compound2           
;
PROBLEM: Missing _cell_measurement_theta_min value ......     Please Do !
RESPONSE: Parameter missing because of file loss due to database server crash
;
_vrf_PLAT185_Compound2           
;
PROBLEM: Missing _cell_measurement_theta_max value ......     Please Do !
RESPONSE: Parameter missing because of file loss due to database server crash
;
# Added during the CSD deposition process: Thursday 14 July 2016 11:37 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            (BDI)CpClNb(NtBu)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H55 Cl N3 Nb'
_chemical_formula_weight         682.21

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   17.812(5)
_cell_length_b                   17.474(5)
_cell_length_c                   23.717(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7382(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_F_000             2896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.427
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            171791
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.717
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6745
_reflns_number_gt                6152
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-2011
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²+18.9646P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6745
_refine_ls_number_parameters     401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0994
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2924(2) 0.98607(19) 0.50576(16) 0.0413(9) Uani 1 1 d . . . . .
H1 H 0.3175 1.0186 0.4798 0.050 Uiso 1 1 calc R U . . .
C2 C 0.3047(2) 0.98218(17) 0.56460(14) 0.0299(7) Uani 1 1 d . . . . .
H2 H 0.3409 1.0107 0.5852 0.036 Uiso 1 1 calc R U . . .
C3 C 0.25413(18) 0.92878(17) 0.58709(14) 0.0276(7) Uani 1 1 d . . . . .
H3 H 0.2493 0.9156 0.6258 0.033 Uiso 1 1 calc R U . . .
C4 C 0.21225(19) 0.8985(2) 0.54302(18) 0.0381(9) Uani 1 1 d . . . . .
H4 H 0.1741 0.8609 0.5465 0.046 Uiso 1 1 calc R U . . .
C5 C 0.2356(2) 0.9326(2) 0.49292(17) 0.0442(10) Uani 1 1 d . . . . .
H5 H 0.2165 0.9217 0.4564 0.053 Uiso 1 1 calc R U . . .
C6 C 0.43530(18) 0.8717(2) 0.40374(13) 0.0284(7) Uani 1 1 d . . . . .
C7 C 0.5160(2) 0.8892(3) 0.42131(17) 0.0562(13) Uani 1 1 d . . . . .
H7A H 0.5167 0.9347 0.4454 0.084 Uiso 1 1 calc R U . . .
H7B H 0.5466 0.8986 0.3876 0.084 Uiso 1 1 calc R U . . .
H7C H 0.5366 0.8455 0.4421 0.084 Uiso 1 1 calc R U . . .
C8 C 0.4024(2) 0.9396(2) 0.37172(16) 0.0420(9) Uani 1 1 d . . . . .
H8A H 0.3492 0.9302 0.3640 0.063 Uiso 1 1 calc R U . . .
H8B H 0.4295 0.9463 0.3361 0.063 Uiso 1 1 calc R U . . .
H8C H 0.4075 0.9861 0.3946 0.063 Uiso 1 1 calc R U . . .
C9 C 0.4314(2) 0.7994(2) 0.36754(16) 0.0455(10) Uani 1 1 d . . . . .
H9A H 0.4472 0.7552 0.3900 0.068 Uiso 1 1 calc R U . . .
H9B H 0.4647 0.8050 0.3349 0.068 Uiso 1 1 calc R U . . .
H9C H 0.3797 0.7917 0.3545 0.068 Uiso 1 1 calc R U . . .
C10 C 0.32344(16) 0.69304(16) 0.47802(11) 0.0170(6) Uani 1 1 d . . . . .
C11 C 0.27379(16) 0.68901(16) 0.43177(12) 0.0197(6) Uani 1 1 d . . . . .
C12 C 0.28923(18) 0.63661(18) 0.38864(13) 0.0257(7) Uani 1 1 d . . . . .
H12 H 0.2570 0.6340 0.3568 0.031 Uiso 1 1 calc R U . . .
C13 C 0.35102(19) 0.58849(19) 0.39190(13) 0.0297(7) Uani 1 1 d . . . . .
H13 H 0.3610 0.5534 0.3622 0.036 Uiso 1 1 calc R U . . .
C14 C 0.39820(18) 0.59145(17) 0.43829(13) 0.0258(7) Uani 1 1 d . . . . .
H14 H 0.4399 0.5576 0.4403 0.031 Uiso 1 1 calc R U . . .
C15 C 0.38575(17) 0.64309(16) 0.48210(12) 0.0203(6) Uani 1 1 d . . . . .
C16 C 0.20382(16) 0.73894(17) 0.42744(12) 0.0213(6) Uani 1 1 d . . . . .
H16 H 0.1987 0.7678 0.4636 0.026 Uiso 1 1 calc R U . . .
C17 C 0.13289(18) 0.6899(2) 0.41988(14) 0.0299(7) Uani 1 1 d . . . . .
H17A H 0.0887 0.7232 0.4182 0.045 Uiso 1 1 calc R U . . .
H17B H 0.1280 0.6546 0.4518 0.045 Uiso 1 1 calc R U . . .
H17C H 0.1367 0.6605 0.3848 0.045 Uiso 1 1 calc R U . . .
C18 C 0.20947(18) 0.79725(18) 0.37975(12) 0.0254(7) Uani 1 1 d . . . . .
H18A H 0.2550 0.8280 0.3846 0.038 Uiso 1 1 calc R U . . .
H18B H 0.1654 0.8308 0.3805 0.038 Uiso 1 1 calc R U . . .
H18C H 0.2116 0.7704 0.3435 0.038 Uiso 1 1 calc R U . . .
C19 C 0.43694(17) 0.64324(17) 0.53324(13) 0.0229(6) Uani 1 1 d . . . . .
H19 H 0.4276 0.6918 0.5544 0.027 Uiso 1 1 calc R U . . .
C20 C 0.52006(19) 0.6413(2) 0.51729(17) 0.0389(9) Uani 1 1 d . . . . .
H20A H 0.5307 0.5945 0.4960 0.058 Uiso 1 1 calc R U . . .
H20B H 0.5507 0.6421 0.5516 0.058 Uiso 1 1 calc R U . . .
H20C H 0.5321 0.6860 0.4941 0.058 Uiso 1 1 calc R U . . .
C21 C 0.4172(2) 0.57653(19) 0.57226(14) 0.0351(8) Uani 1 1 d . . . . .
H21A H 0.3648 0.5813 0.5845 0.053 Uiso 1 1 calc R U . . .
H21B H 0.4502 0.5775 0.6053 0.053 Uiso 1 1 calc R U . . .
H21C H 0.4239 0.5281 0.5520 0.053 Uiso 1 1 calc R U . . .
C22 C 0.2041(2) 0.6742(2) 0.56005(13) 0.0326(8) Uani 1 1 d . . . . .
H22A H 0.1943 0.6429 0.5935 0.049 Uiso 1 1 calc R U . . .
H22B H 0.2143 0.6409 0.5277 0.049 Uiso 1 1 calc R U . . .
H22C H 0.1601 0.7060 0.5520 0.049 Uiso 1 1 calc R U . . .
C23 C 0.27043(16) 0.72434(15) 0.57061(11) 0.0165(6) Uani 1 1 d . . . . .
C24 C 0.29075(15) 0.75026(15) 0.62204(11) 0.0154(6) Uani 1 1 d . . . . .
H24 H 0.3381 0.7750 0.6244 0.019 Uiso 1 1 calc R U . . .
C25 C 0.24754(16) 0.74441(16) 0.67482(11) 0.0166(6) Uani 1 1 d . . . . .
C26 C 0.28946(18) 0.76782(19) 0.72741(12) 0.0262(7) Uani 1 1 d . . . . .
H26A H 0.2573 0.7601 0.7604 0.039 Uiso 1 1 calc R U . . .
H26B H 0.3034 0.8220 0.7247 0.039 Uiso 1 1 calc R U . . .
H26C H 0.3349 0.7366 0.7312 0.039 Uiso 1 1 calc R U . . .
C27 C 0.13068(15) 0.71626(17) 0.72116(11) 0.0180(6) Uani 1 1 d . . . . .
C28 C 0.09290(16) 0.78186(17) 0.74108(12) 0.0204(6) Uani 1 1 d . . . . .
C29 C 0.03814(17) 0.77203(19) 0.78264(13) 0.0260(7) Uani 1 1 d . . . . .
H29 H 0.0124 0.8156 0.7969 0.031 Uiso 1 1 calc R U . . .
C30 C 0.02065(17) 0.7008(2) 0.80339(13) 0.0284(7) Uani 1 1 d . . . . .
H30 H -0.0169 0.6956 0.8316 0.034 Uiso 1 1 calc R U . . .
C31 C 0.05760(17) 0.63636(19) 0.78329(12) 0.0250(7) Uani 1 1 d . . . . .
H31 H 0.0448 0.5873 0.7977 0.030 Uiso 1 1 calc R U . . .
C32 C 0.11357(16) 0.64297(17) 0.74197(12) 0.0200(6) Uani 1 1 d . . . . .
C33 C 0.10864(17) 0.86023(18) 0.71509(13) 0.0249(7) Uani 1 1 d . . . . .
H33 H 0.1627 0.8610 0.7036 0.030 Uiso 1 1 calc R U . . .
C34 C 0.0619(3) 0.8711(2) 0.66183(17) 0.0475(10) Uani 1 1 d . . . . .
H34A H 0.0085 0.8717 0.6717 0.071 Uiso 1 1 calc R U . . .
H34B H 0.0718 0.8289 0.6356 0.071 Uiso 1 1 calc R U . . .
H34C H 0.0754 0.9197 0.6439 0.071 Uiso 1 1 calc R U . . .
C35 C 0.0965(2) 0.9263(2) 0.75579(16) 0.0377(8) Uani 1 1 d . . . . .
H35A H 0.1079 0.9747 0.7368 0.057 Uiso 1 1 calc R U . . .
H35B H 0.1296 0.9201 0.7885 0.057 Uiso 1 1 calc R U . . .
H35C H 0.0441 0.9266 0.7684 0.057 Uiso 1 1 calc R U . . .
C36 C 0.15574(17) 0.57326(17) 0.72022(13) 0.0241(6) Uani 1 1 d . . . . .
H36 H 0.1717 0.5848 0.6807 0.029 Uiso 1 1 calc R U . . .
C37 C 0.22720(19) 0.5596(2) 0.75480(18) 0.0394(9) Uani 1 1 d . . . . .
H37A H 0.2592 0.6052 0.7530 0.059 Uiso 1 1 calc R U . . .
H37B H 0.2544 0.5156 0.7394 0.059 Uiso 1 1 calc R U . . .
H37C H 0.2137 0.5494 0.7941 0.059 Uiso 1 1 calc R U . . .
C38 C 0.10839(19) 0.50023(19) 0.71836(14) 0.0300(7) Uani 1 1 d . . . . .
H38A H 0.0967 0.4839 0.7569 0.045 Uiso 1 1 calc R U . . .
H38B H 0.1365 0.4597 0.6991 0.045 Uiso 1 1 calc R U . . .
H38C H 0.0616 0.5103 0.6979 0.045 Uiso 1 1 calc R U . . .
N1 N 0.39302(13) 0.85902(14) 0.45568(11) 0.0211(5) Uani 1 1 d . . . . .
N2 N 0.31237(13) 0.74811(13) 0.52307(9) 0.0138(5) Uani 1 1 d . . . . .
N3 N 0.17883(13) 0.72237(13) 0.67337(9) 0.0171(5) Uani 1 1 d . . . . .
Cl1 Cl 0.44828(4) 0.87111(4) 0.58446(3) 0.02667(17) Uani 1 1 d . . . . .
Nb1 Nb 0.34492(2) 0.85938(2) 0.52051(2) 0.01644(9) 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 C5 1.410(6) . ?
C1 C2 1.414(5) . ?
C1 Nb1 2.429(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.403(5) . ?
C2 Nb1 2.492(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(5) . ?
C3 Nb1 2.565(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(6) . ?
C4 Nb1 2.517(3) . ?
C4 H4 0.9500 . ?
C5 Nb1 2.420(3) . ?
C5 H5 0.9500 . ?
C6 N1 1.461(4) . ?
C6 C8 1.526(5) . ?
C6 C9 1.528(5) . ?
C6 C7 1.528(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.411(4) . ?
C10 C15 1.415(4) . ?
C10 N2 1.451(3) . ?
C11 C12 1.400(4) . ?
C11 C16 1.525(4) . ?
C12 C13 1.387(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(4) . ?
C14 H14 0.9500 . ?
C15 C19 1.517(4) . ?
C16 C18 1.526(4) . ?
C16 C17 1.537(4) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.529(5) . ?
C19 C21 1.529(4) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.492(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.351(4) . ?
C23 N2 1.415(3) . ?
C24 C25 1.473(4) . ?
C24 H24 0.9500 . ?
C25 N3 1.284(4) . ?
C25 C26 1.510(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C32 1.406(4) . ?
C27 C28 1.411(4) . ?
C27 N3 1.425(4) . ?
C28 C29 1.397(4) . ?
C28 C33 1.528(4) . ?
C29 C30 1.375(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.388(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.403(4) . ?
C31 H31 0.9500 . ?
C32 C36 1.521(4) . ?
C33 C35 1.520(4) . ?
C33 C34 1.525(5) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C38 1.530(4) . ?
C36 C37 1.533(5) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N1 Nb1 1.760(3) . ?
N2 Nb1 2.030(2) . ?
Cl1 Nb1 2.3941(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 C1 C2 107.0(3) . . ?
C5 C1 Nb1 72.77(19) . . ?
C2 C1 Nb1 75.76(18) . . ?
C5 C1 H1 126.5 . . ?
C2 C1 H1 126.5 . . ?
Nb1 C1 H1 117.1 . . ?
C3 C2 C1 107.9(3) . . ?
C3 C2 Nb1 76.78(18) . . ?
C1 C2 Nb1 70.86(18) . . ?
C3 C2 H2 126.1 . . ?
C1 C2 H2 126.1 . . ?
Nb1 C2 H2 118.2 . . ?
C4 C3 C2 108.2(3) . . ?
C4 C3 Nb1 72.27(19) . . ?
C2 C3 Nb1 71.05(18) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
Nb1 C3 H3 122.4 . . ?
C3 C4 C5 108.6(3) . . ?
C3 C4 Nb1 76.04(19) . . ?
C5 C4 Nb1 69.8(2) . . ?
C3 C4 H4 125.7 . . ?
C5 C4 H4 125.7 . . ?
Nb1 C4 H4 120.2 . . ?
C4 C5 C1 108.2(3) . . ?
C4 C5 Nb1 77.49(19) . . ?
C1 C5 Nb1 73.4(2) . . ?
C4 C5 H5 125.9 . . ?
C1 C5 H5 125.9 . . ?
Nb1 C5 H5 115.3 . . ?
N1 C6 C8 109.8(3) . . ?
N1 C6 C9 109.0(3) . . ?
C8 C6 C9 110.2(3) . . ?
N1 C6 C7 106.6(3) . . ?
C8 C6 C7 109.9(3) . . ?
C9 C6 C7 111.2(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C15 120.9(3) . . ?
C11 C10 N2 121.4(2) . . ?
C15 C10 N2 117.7(2) . . ?
C12 C11 C10 118.5(3) . . ?
C12 C11 C16 119.1(3) . . ?
C10 C11 C16 122.4(2) . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 121.3(3) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C14 C15 C10 118.2(3) . . ?
C14 C15 C19 120.1(3) . . ?
C10 C15 C19 121.7(2) . . ?
C11 C16 C18 112.2(2) . . ?
C11 C16 C17 111.1(3) . . ?
C18 C16 C17 109.9(3) . . ?
C11 C16 H16 107.8 . . ?
C18 C16 H16 107.8 . . ?
C17 C16 H16 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 C20 112.6(3) . . ?
C15 C19 C21 110.1(3) . . ?
C20 C19 C21 110.8(3) . . ?
C15 C19 H19 107.7 . . ?
C20 C19 H19 107.7 . . ?
C21 C19 H19 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N2 118.7(2) . . ?
C24 C23 C22 124.1(3) . . ?
N2 C23 C22 117.2(2) . . ?
C23 C24 C25 127.2(3) . . ?
C23 C24 H24 116.4 . . ?
C25 C24 H24 116.4 . . ?
N3 C25 C24 119.8(2) . . ?
N3 C25 C26 125.1(2) . . ?
C24 C25 C26 115.1(2) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 121.3(3) . . ?
C32 C27 N3 118.5(3) . . ?
C28 C27 N3 119.5(3) . . ?
C29 C28 C27 118.0(3) . . ?
C29 C28 C33 121.5(3) . . ?
C27 C28 C33 120.4(3) . . ?
C30 C29 C28 121.5(3) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C29 C30 C31 120.3(3) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C32 120.7(3) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C27 118.3(3) . . ?
C31 C32 C36 121.5(3) . . ?
C27 C32 C36 120.2(3) . . ?
C35 C33 C34 110.7(3) . . ?
C35 C33 C28 113.5(3) . . ?
C34 C33 C28 110.2(3) . . ?
C35 C33 H33 107.4 . . ?
C34 C33 H33 107.4 . . ?
C28 C33 H33 107.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 C38 113.9(3) . . ?
C32 C36 C37 110.7(3) . . ?
C38 C36 C37 110.1(3) . . ?
C32 C36 H36 107.3 . . ?
C38 C36 H36 107.3 . . ?
C37 C36 H36 107.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C6 N1 Nb1 170.8(2) . . ?
C23 N2 C10 117.6(2) . . ?
C23 N2 Nb1 117.11(17) . . ?
C10 N2 Nb1 125.05(17) . . ?
C25 N3 C27 125.1(2) . . ?
N1 Nb1 N2 99.31(10) . . ?
N1 Nb1 Cl1 100.33(8) . . ?
N2 Nb1 Cl1 106.42(7) . . ?
N1 Nb1 C5 99.05(13) . . ?
N2 Nb1 C5 106.54(12) . . ?
Cl1 Nb1 C5 138.13(9) . . ?
N1 Nb1 C1 93.73(12) . . ?
N2 Nb1 C1 140.11(13) . . ?
Cl1 Nb1 C1 108.04(11) . . ?
C5 Nb1 C1 33.80(14) . . ?
N1 Nb1 C2 120.62(11) . . ?
N2 Nb1 C2 136.90(10) . . ?
Cl1 Nb1 C2 83.18(8) . . ?
C5 Nb1 C2 55.05(12) . . ?
C1 Nb1 C2 33.38(12) . . ?
N1 Nb1 C4 130.02(13) . . ?
N2 Nb1 C4 89.19(10) . . ?
Cl1 Nb1 C4 124.35(9) . . ?
C5 Nb1 C4 32.69(14) . . ?
C1 Nb1 C4 54.62(13) . . ?
C2 Nb1 C4 53.66(11) . . ?
N1 Nb1 C3 147.81(11) . . ?
N2 Nb1 C3 104.74(10) . . ?
Cl1 Nb1 C3 93.12(8) . . ?
C5 Nb1 C3 53.78(12) . . ?
C1 Nb1 C3 54.18(12) . . ?
C2 Nb1 C3 32.17(11) . . ?
C4 Nb1 C3 31.69(11) . . ?

_refine_diff_density_max         2.282
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.070



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Pentane'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
