# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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#######################################################################

data_(1)
_database_code_depnum_ccdc_archive 'CCDC 1026785'
_audit_update_record             
;
2014-09-28 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_chemical_name_common            'Complex 2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H61 Br0 Cl N3 Nb O'
_chemical_formula_sum            'C48 H61 Br0 Cl N3 Nb O'
_chemical_formula_weight         824.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3526(7)
_cell_length_b                   19.7589(12)
_cell_length_c                   20.1301(13)
_cell_angle_alpha                96.454(4)
_cell_angle_beta                 102.126(3)
_cell_angle_gamma                91.320(4)
_cell_volume                     4381.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9576
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.42

_exptl_crystal_description       needdle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9224
_exptl_absorpt_correction_T_max  0.9816
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            84384
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         25.47
_reflns_number_total             16211
_reflns_number_gt                11965
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0284P)²+3.2528P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16211
_refine_ls_number_parameters     999
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0779
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.3908(3) 0.66146(14) 0.64819(15) 0.0245(7) Uani 1 1 d . . .
H1A H 1.3200 0.6471 0.6117 0.037 Uiso 1 1 calc R . .
H1B H 1.3740 0.6526 0.6923 0.037 Uiso 1 1 calc R . .
H1C H 1.4600 0.6358 0.6396 0.037 Uiso 1 1 calc R . .
C2 C 1.4192(2) 0.73685(14) 0.64969(14) 0.0179(6) Uani 1 1 d . . .
C3 C 1.3588(3) 0.77038(14) 0.59982(14) 0.0204(7) Uani 1 1 d . . .
H3 H 1.2961 0.7475 0.5652 0.024 Uiso 1 1 calc R . .
C4 C 1.3900(3) 0.84191(14) 0.59917(14) 0.0203(7) Uani 1 1 d . . .
C5 C 1.3273(3) 0.87588(16) 0.53919(16) 0.0338(8) Uani 1 1 d . . .
H5A H 1.3588 0.9232 0.5440 0.051 Uiso 1 1 calc R . .
H5B H 1.2404 0.8752 0.5377 0.051 Uiso 1 1 calc R . .
H5C H 1.3419 0.8514 0.4968 0.051 Uiso 1 1 calc R . .
C6 C 1.4996(2) 0.94412(14) 0.65266(14) 0.0179(6) Uani 1 1 d . . .
C7 C 1.4296(3) 0.99122(14) 0.68237(14) 0.0199(7) Uani 1 1 d . . .
C8 C 1.4581(3) 1.06016(15) 0.68349(15) 0.0233(7) Uani 1 1 d . . .
H8 H 1.4114 1.0929 0.7031 0.028 Uiso 1 1 calc R . .
C9 C 1.5529(3) 1.08211(15) 0.65664(15) 0.0254(7) Uani 1 1 d . . .
H9 H 1.5709 1.1295 0.6578 0.031 Uiso 1 1 calc R . .
C10 C 1.6207(3) 1.03500(15) 0.62830(15) 0.0266(7) Uani 1 1 d . . .
H10 H 1.6857 1.0503 0.6100 0.032 Uiso 1 1 calc R . .
C11 C 1.5963(3) 0.96509(15) 0.62581(15) 0.0237(7) Uani 1 1 d . . .
C12 C 1.6732(3) 0.91447(16) 0.59387(18) 0.0351(9) Uani 1 1 d . . .
H12 H 1.6526 0.8684 0.6057 0.042 Uiso 1 1 calc R . .
C13 C 1.8063(3) 0.92994(19) 0.62322(18) 0.0444(10) Uani 1 1 d . . .
H13A H 1.8517 0.8906 0.6109 0.067 Uiso 1 1 calc R . .
H13B H 1.8200 0.9393 0.6732 0.067 Uiso 1 1 calc R . .
H13C H 1.8332 0.9699 0.6046 0.067 Uiso 1 1 calc R . .
C14 C 1.6477(4) 0.9103(2) 0.5175(2) 0.0746(15) Uani 1 1 d . . .
H14A H 1.5627 0.8962 0.4989 0.112 Uiso 1 1 calc R . .
H14B H 1.6990 0.8769 0.4995 0.112 Uiso 1 1 calc R . .
H14C H 1.6645 0.9552 0.5041 0.112 Uiso 1 1 calc R . .
C15 C 1.3213(3) 0.96948(15) 0.71019(15) 0.0250(7) Uani 1 1 d . . .
H15 H 1.3181 0.9186 0.7079 0.030 Uiso 1 1 calc R . .
C16 C 1.3312(3) 0.99930(17) 0.78455(15) 0.0310(8) Uani 1 1 d . . .
H16A H 1.4052 0.9846 0.8128 0.047 Uiso 1 1 calc R . .
H16B H 1.2612 0.9832 0.8008 0.047 Uiso 1 1 calc R . .
H16C H 1.3337 1.0492 0.7878 0.047 Uiso 1 1 calc R . .
C17 C 1.2036(3) 0.9906(2) 0.66595(17) 0.0419(9) Uani 1 1 d . . .
H17A H 1.2030 1.0405 0.6694 0.063 Uiso 1 1 calc R . .
H17B H 1.1346 0.9730 0.6821 0.063 Uiso 1 1 calc R . .
H17C H 1.1980 0.9719 0.6181 0.063 Uiso 1 1 calc R . .
C18 C 1.8079(3) 0.76304(15) 0.68518(14) 0.0205(7) Uani 1 1 d . . .
C19 C 1.8153(3) 0.71137(16) 0.63102(15) 0.0261(7) Uani 1 1 d . . .
C20 C 1.9261(3) 0.70198(18) 0.61337(16) 0.0324(8) Uani 1 1 d . . .
H20 H 1.9327 0.6670 0.5780 0.039 Uiso 1 1 calc R . .
C21 C 2.0268(3) 0.74235(19) 0.64612(16) 0.0388(9) Uani 1 1 d . . .
H21 H 2.1015 0.7356 0.6327 0.047 Uiso 1 1 calc R . .
C22 C 2.0193(3) 0.79237(18) 0.69824(16) 0.0330(8) Uani 1 1 d . . .
H22 H 2.0890 0.8204 0.7198 0.040 Uiso 1 1 calc R . .
C23 C 1.9114(3) 0.80299(16) 0.72021(15) 0.0238(7) Uani 1 1 d . . .
C24 C 1.9060(3) 0.85626(16) 0.78020(15) 0.0256(7) Uani 1 1 d . . .
H24 H 1.8260 0.8773 0.7696 0.031 Uiso 1 1 calc R . .
C25 C 1.9125(3) 0.82324(17) 0.84573(16) 0.0352(8) Uani 1 1 d . . .
H25A H 1.8502 0.7863 0.8378 0.053 Uiso 1 1 calc R . .
H25B H 1.8992 0.8575 0.8823 0.053 Uiso 1 1 calc R . .
H25C H 1.9921 0.8047 0.8593 0.053 Uiso 1 1 calc R . .
C26 C 2.0031(3) 0.91375(18) 0.79305(18) 0.0402(9) Uani 1 1 d . . .
H26A H 2.0823 0.8956 0.8091 0.060 Uiso 1 1 calc R . .
H26B H 1.9871 0.9491 0.8278 0.060 Uiso 1 1 calc R . .
H26C H 2.0023 0.9335 0.7504 0.060 Uiso 1 1 calc R . .
C27 C 1.7029(3) 0.67067(16) 0.59151(15) 0.0301(8) Uani 1 1 d . . .
H27 H 1.6517 0.6624 0.6249 0.036 Uiso 1 1 calc R . .
C28 C 1.6311(3) 0.71153(17) 0.53911(17) 0.0423(9) Uani 1 1 d . . .
H28A H 1.6150 0.7558 0.5618 0.064 Uiso 1 1 calc R . .
H28B H 1.5545 0.6867 0.5174 0.064 Uiso 1 1 calc R . .
H28C H 1.6772 0.7185 0.5042 0.064 Uiso 1 1 calc R . .
C29 C 1.7255(4) 0.60072(17) 0.55573(17) 0.0451(10) Uani 1 1 d . . .
H29A H 1.7613 0.6071 0.5165 0.068 Uiso 1 1 calc R . .
H29B H 1.6489 0.5741 0.5399 0.068 Uiso 1 1 calc R . .
H29C H 1.7808 0.5764 0.5880 0.068 Uiso 1 1 calc R . .
C30 C 1.5890(3) 0.69467(14) 0.84270(14) 0.0201(7) Uani 1 1 d . . .
C31 C 1.4968(3) 0.63845(14) 0.84696(15) 0.0256(7) Uani 1 1 d . . .
H31A H 1.4435 0.6562 0.8766 0.038 Uiso 1 1 calc R . .
H31B H 1.5391 0.5999 0.8659 0.038 Uiso 1 1 calc R . .
H31C H 1.4487 0.6232 0.8011 0.038 Uiso 1 1 calc R . .
C32 C 1.6545(3) 0.72459(15) 0.91486(14) 0.0263(7) Uani 1 1 d . . .
H32A H 1.7113 0.7616 0.9118 0.039 Uiso 1 1 calc R . .
H32B H 1.6986 0.6889 0.9382 0.039 Uiso 1 1 calc R . .
H32C H 1.5954 0.7424 0.9407 0.039 Uiso 1 1 calc R . .
C33 C 1.6795(3) 0.66169(15) 0.80447(15) 0.0240(7) Uani 1 1 d . . .
H33A H 1.6379 0.6433 0.7580 0.036 Uiso 1 1 calc R . .
H33B H 1.7169 0.6247 0.8287 0.036 Uiso 1 1 calc R . .
H33C H 1.7419 0.6959 0.8022 0.036 Uiso 1 1 calc R . .
C34 C 1.4446(2) 0.79628(13) 0.82876(14) 0.0165(6) Uani 1 1 d . . .
H34 H 1.4073 0.8190 0.7880 0.020 Uiso 1 1 calc R . .
C35 C 1.5096(2) 0.85358(14) 0.87895(14) 0.0178(6) Uani 1 1 d . . .
H35 H 1.4980 0.8594 0.9246 0.021 Uiso 1 1 calc R . .
C36 C 1.5840(3) 0.89641(14) 0.85881(14) 0.0188(6) Uani 1 1 d . . .
C37 C 1.6604(3) 0.95149(14) 0.90586(14) 0.0199(7) Uani 1 1 d . . .
C38 C 1.7625(3) 0.97874(15) 0.88928(15) 0.0253(7) Uani 1 1 d . . .
H38 H 1.7803 0.9648 0.8459 0.030 Uiso 1 1 calc R . .
C39 C 1.8392(3) 1.02629(15) 0.93545(16) 0.0298(8) Uani 1 1 d . . .
H39 H 1.9100 1.0436 0.9238 0.036 Uiso 1 1 calc R . .
C40 C 1.8134(3) 1.04852(17) 0.99802(16) 0.0375(9) Uani 1 1 d . . .
H40 H 1.8657 1.0812 1.0295 0.045 Uiso 1 1 calc R . .
C41 C 1.7109(4) 1.02274(18) 1.01428(17) 0.0444(10) Uani 1 1 d . . .
H41 H 1.6919 1.0382 1.0570 0.053 Uiso 1 1 calc R . .
C42 C 1.6350(3) 0.97451(16) 0.96905(16) 0.0345(8) Uani 1 1 d . . .
H42 H 1.5649 0.9570 0.9812 0.041 Uiso 1 1 calc R . .
C43 C 1.3383(2) 0.76089(13) 0.84739(14) 0.0153(6) Uani 1 1 d . . .
C44 C 1.3249(3) 0.76074(14) 0.91472(14) 0.0206(7) Uani 1 1 d . . .
H44 H 1.3829 0.7850 0.9510 0.025 Uiso 1 1 calc R . .
C45 C 1.2284(3) 0.72573(14) 0.92935(15) 0.0212(7) Uani 1 1 d . . .
H45 H 1.2209 0.7253 0.9754 0.025 Uiso 1 1 calc R . .
C46 C 1.1432(2) 0.69137(14) 0.87659(14) 0.0187(6) Uani 1 1 d . . .
C47 C 1.1515(3) 0.69252(14) 0.80920(14) 0.0208(7) Uani 1 1 d . . .
H47 H 1.0912 0.6699 0.7729 0.025 Uiso 1 1 calc R . .
C48 C 1.2489(2) 0.72713(14) 0.79569(14) 0.0183(6) Uani 1 1 d . . .
H48 H 1.2550 0.7279 0.7494 0.022 Uiso 1 1 calc R . .
C49 C 1.0569(3) 0.58925(15) 0.06020(14) 0.0229(7) Uani 1 1 d . . .
H49A H 1.0867 0.5473 0.0401 0.034 Uiso 1 1 calc R . .
H49B H 1.1061 0.6285 0.0540 0.034 Uiso 1 1 calc R . .
H49C H 0.9727 0.5939 0.0375 0.034 Uiso 1 1 calc R . .
C50 C 1.0651(2) 0.58631(14) 0.13552(14) 0.0183(6) Uani 1 1 d . . .
C51 C 1.1126(3) 0.53268(14) 0.16467(14) 0.0205(7) Uani 1 1 d . . .
H51 H 1.1426 0.4968 0.1383 0.025 Uiso 1 1 calc R . .
C52 C 1.1180(2) 0.52988(14) 0.23723(14) 0.0184(6) Uani 1 1 d . . .
C53 C 1.1741(3) 0.46991(15) 0.26860(15) 0.0303(8) Uani 1 1 d . . .
H53A H 1.2611 0.4723 0.2705 0.045 Uiso 1 1 calc R . .
H53B H 1.1381 0.4277 0.2408 0.045 Uiso 1 1 calc R . .
H53C H 1.1599 0.4705 0.3150 0.045 Uiso 1 1 calc R . .
C54 C 1.0845(3) 0.58140(14) 0.34325(13) 0.0173(6) Uani 1 1 d . . .
C55 C 0.9828(3) 0.56232(14) 0.36825(14) 0.0191(6) Uani 1 1 d . . .
C56 C 0.9963(3) 0.56552(14) 0.43910(14) 0.0222(7) Uani 1 1 d . . .
H56 H 0.9296 0.5529 0.4575 0.027 Uiso 1 1 calc R . .
C57 C 1.1050(3) 0.58679(15) 0.48308(15) 0.0269(7) Uani 1 1 d . . .
H57 H 1.1122 0.5886 0.5311 0.032 Uiso 1 1 calc R . .
C58 C 1.2025(3) 0.60530(15) 0.45756(15) 0.0242(7) Uani 1 1 d . . .
H58 H 1.2765 0.6197 0.4884 0.029 Uiso 1 1 calc R . .
C59 C 1.1952(3) 0.60336(14) 0.38719(14) 0.0205(7) Uani 1 1 d . . .
C60 C 1.3061(3) 0.62535(15) 0.36233(15) 0.0239(7) Uani 1 1 d . . .
H60 H 1.2854 0.6199 0.3112 0.029 Uiso 1 1 calc R . .
C61 C 1.3425(3) 0.70066(15) 0.38742(16) 0.0295(8) Uani 1 1 d . . .
H61A H 1.2745 0.7288 0.3718 0.044 Uiso 1 1 calc R . .
H61B H 1.4116 0.7142 0.3689 0.044 Uiso 1 1 calc R . .
H61C H 1.3646 0.7071 0.4375 0.044 Uiso 1 1 calc R . .
C62 C 1.4131(3) 0.58055(16) 0.38513(16) 0.0320(8) Uani 1 1 d . . .
H62A H 1.4357 0.5855 0.4352 0.048 Uiso 1 1 calc R . .
H62B H 1.4819 0.5949 0.3668 0.048 Uiso 1 1 calc R . .
H62C H 1.3897 0.5327 0.3678 0.048 Uiso 1 1 calc R . .
C63 C 0.8641(3) 0.53859(15) 0.32009(14) 0.0214(7) Uani 1 1 d . . .
H63 H 0.8526 0.5675 0.2817 0.026 Uiso 1 1 calc R . .
C64 C 0.8659(3) 0.46467(16) 0.28872(17) 0.0363(8) Uani 1 1 d . . .
H64A H 0.9285 0.4606 0.2618 0.054 Uiso 1 1 calc R . .
H64B H 0.7872 0.4507 0.2590 0.054 Uiso 1 1 calc R . .
H64C H 0.8833 0.4352 0.3253 0.054 Uiso 1 1 calc R . .
C65 C 0.7550(3) 0.54655(17) 0.35281(16) 0.0318(8) Uani 1 1 d . . .
H65A H 0.7568 0.5136 0.3859 0.048 Uiso 1 1 calc R . .
H65B H 0.6809 0.5383 0.3172 0.048 Uiso 1 1 calc R . .
H65C H 0.7570 0.5929 0.3764 0.048 Uiso 1 1 calc R . .
C66 C 0.7169(2) 0.62683(13) 0.18228(14) 0.0159(6) Uani 1 1 d . . .
C67 C 0.6576(3) 0.57269(14) 0.13389(14) 0.0190(6) Uani 1 1 d . . .
C68 C 0.5382(3) 0.55542(15) 0.13353(16) 0.0253(7) Uani 1 1 d . . .
H68 H 0.4968 0.5195 0.1010 0.030 Uiso 1 1 calc R . .
C69 C 0.4782(3) 0.58924(15) 0.17935(16) 0.0265(7) Uani 1 1 d . . .
H69 H 0.3966 0.5764 0.1784 0.032 Uiso 1 1 calc R . .
C70 C 0.5370(3) 0.64174(15) 0.22654(15) 0.0236(7) Uani 1 1 d . . .
H70 H 0.4946 0.6650 0.2575 0.028 Uiso 1 1 calc R . .
C71 C 0.6570(3) 0.66161(14) 0.22998(14) 0.0191(7) Uani 1 1 d . . .
C72 C 0.7229(3) 0.71843(14) 0.28318(14) 0.0217(7) Uani 1 1 d . . .
H72 H 0.8055 0.7029 0.3012 0.026 Uiso 1 1 calc R . .
C73 C 0.7386(3) 0.78382(15) 0.25182(16) 0.0307(8) Uani 1 1 d . . .
H73A H 0.7840 0.7749 0.2156 0.046 Uiso 1 1 calc R . .
H73B H 0.7828 0.8187 0.2873 0.046 Uiso 1 1 calc R . .
H73C H 0.6592 0.7999 0.2324 0.046 Uiso 1 1 calc R . .
C74 C 0.6643(3) 0.73494(16) 0.34461(16) 0.0326(8) Uani 1 1 d . . .
H74A H 0.5882 0.7568 0.3300 0.049 Uiso 1 1 calc R . .
H74B H 0.7187 0.7658 0.3799 0.049 Uiso 1 1 calc R . .
H74C H 0.6485 0.6927 0.3632 0.049 Uiso 1 1 calc R . .
C75 C 0.7239(3) 0.53641(14) 0.08317(14) 0.0203(7) Uani 1 1 d . . .
H75 H 0.8123 0.5432 0.1034 0.024 Uiso 1 1 calc R . .
C76 C 0.6938(3) 0.45908(15) 0.06910(18) 0.0363(8) Uani 1 1 d . . .
H76A H 0.7080 0.4394 0.1125 0.054 Uiso 1 1 calc R . .
H76B H 0.7452 0.4379 0.0400 0.054 Uiso 1 1 calc R . .
H76C H 0.6089 0.4507 0.0458 0.054 Uiso 1 1 calc R . .
C77 C 0.6991(3) 0.56867(17) 0.01718(16) 0.0370(9) Uani 1 1 d . . .
H77A H 0.6125 0.5640 -0.0032 0.056 Uiso 1 1 calc R . .
H77B H 0.7440 0.5458 -0.0147 0.056 Uiso 1 1 calc R . .
H77C H 0.7246 0.6171 0.0268 0.056 Uiso 1 1 calc R . .
C78 C 0.9742(2) 0.79018(14) 0.11179(13) 0.0172(6) Uani 1 1 d . . .
C79 C 0.8497(2) 0.75712(14) 0.07873(14) 0.0215(7) Uani 1 1 d . . .
H79A H 0.8587 0.7116 0.0559 0.032 Uiso 1 1 calc R . .
H79B H 0.8076 0.7853 0.0450 0.032 Uiso 1 1 calc R . .
H79C H 0.8031 0.7532 0.1140 0.032 Uiso 1 1 calc R . .
C80 C 1.0414(3) 0.79509(15) 0.05349(14) 0.0214(7) Uani 1 1 d . . .
H80A H 1.1198 0.8192 0.0718 0.032 Uiso 1 1 calc R . .
H80B H 0.9936 0.8200 0.0186 0.032 Uiso 1 1 calc R . .
H80C H 1.0534 0.7491 0.0329 0.032 Uiso 1 1 calc R . .
C81 C 0.9601(3) 0.86171(14) 0.14709(15) 0.0221(7) Uani 1 1 d . . .
H81A H 0.9165 0.8580 0.1838 0.033 Uiso 1 1 calc R . .
H81B H 0.9150 0.8890 0.1135 0.033 Uiso 1 1 calc R . .
H81C H 1.0401 0.8838 0.1665 0.033 Uiso 1 1 calc R . .
C82 C 1.1556(2) 0.76554(13) 0.20825(13) 0.0155(6) Uani 1 1 d . . .
H82 H 1.1831 0.7221 0.2263 0.019 Uiso 1 1 calc R . .
C83 C 1.1409(2) 0.81028(14) 0.27125(13) 0.0167(6) Uani 1 1 d . . .
H83 H 1.1736 0.8559 0.2811 0.020 Uiso 1 1 calc R . .
C84 C 1.0797(2) 0.78332(13) 0.31305(13) 0.0149(6) Uani 1 1 d . . .
C85 C 1.0530(2) 0.81931(14) 0.37620(14) 0.0167(6) Uani 1 1 d . . .
C86 C 1.0206(3) 0.78202(15) 0.42481(14) 0.0225(7) Uani 1 1 d . . .
H86 H 1.0174 0.7336 0.4176 0.027 Uiso 1 1 calc R . .
C87 C 0.9931(3) 0.81498(16) 0.48369(15) 0.0279(7) Uani 1 1 d . . .
H87 H 0.9725 0.7892 0.5170 0.033 Uiso 1 1 calc R . .
C88 C 0.9957(3) 0.88497(16) 0.49398(15) 0.0293(8) Uani 1 1 d . . .
H88 H 0.9759 0.9075 0.5341 0.035 Uiso 1 1 calc R . .
C89 C 1.0271(3) 0.92237(16) 0.44611(16) 0.0300(8) Uani 1 1 d . . .
H89 H 1.0297 0.9708 0.4537 0.036 Uiso 1 1 calc R . .
C90 C 1.0548(3) 0.89020(14) 0.38706(14) 0.0223(7) Uani 1 1 d . . .
H90 H 1.0751 0.9164 0.3540 0.027 Uiso 1 1 calc R . .
C91 C 1.2567(2) 0.78646(14) 0.17457(13) 0.0163(6) Uani 1 1 d . . .
C92 C 1.2974(3) 0.85374(14) 0.17753(14) 0.0195(7) Uani 1 1 d . . .
H92 H 1.2611 0.8888 0.2014 0.023 Uiso 1 1 calc R . .
C93 C 1.3902(3) 0.87072(15) 0.14622(14) 0.0216(7) Uani 1 1 d . . .
H93 H 1.4166 0.9170 0.1480 0.026 Uiso 1 1 calc R . .
C94 C 1.4432(2) 0.81936(15) 0.11261(14) 0.0205(7) Uani 1 1 d . . .
C95 C 1.4063(3) 0.75167(15) 0.10920(14) 0.0222(7) Uani 1 1 d . . .
H95 H 1.4440 0.7166 0.0862 0.027 Uiso 1 1 calc R . .
C96 C 1.3126(2) 0.73634(14) 0.14033(14) 0.0187(6) Uani 1 1 d . . .
H96 H 1.2860 0.6900 0.1381 0.022 Uiso 1 1 calc R . .
N1 N 1.4712(2) 0.87195(11) 0.64991(11) 0.0174(5) Uani 1 1 d . . .
N2 N 1.6955(2) 0.77426(12) 0.70211(11) 0.0185(5) Uani 1 1 d . . .
N3 N 1.5340(2) 0.74997(11) 0.80298(11) 0.0154(5) Uani 1 1 d . . .
N4 N 1.0734(2) 0.57977(11) 0.27028(11) 0.0156(5) Uani 1 1 d . . .
N5 N 0.8384(2) 0.64321(11) 0.18477(11) 0.0160(5) Uani 1 1 d . . .
N6 N 1.03447(19) 0.74466(11) 0.16182(11) 0.0140(5) Uani 1 1 d . . .
O1 O 1.59981(17) 0.88879(9) 0.79340(9) 0.0185(4) Uani 1 1 d . . .
O2 O 1.03696(16) 0.71803(9) 0.29941(9) 0.0170(4) Uani 1 1 d . . .
Nb1 Nb 1.56170(2) 0.800469(13) 0.728596(12) 0.01525(7) Uani 1 1 d . . .
Nb2 Nb 0.99587(2) 0.664937(12) 0.205274(12) 0.01378(7) Uani 1 1 d . . .
Cl1 Cl 1.02091(7) 0.64708(4) 0.89440(4) 0.02882(18) Uani 1 1 d . . .
Cl2 Cl 1.56239(7) 0.84073(4) 0.07484(4) 0.02864(18) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.512(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.341(4) . ?
C2 Nb1 2.258(3) . ?
C3 C4 1.451(4) . ?
C3 H3 0.9500 . ?
C4 N1 1.299(3) . ?
C4 C5 1.503(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.396(4) . ?
C6 C7 1.401(4) . ?
C6 N1 1.447(3) . ?
C7 C8 1.389(4) . ?
C7 C15 1.525(4) . ?
C8 C9 1.384(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.396(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.519(4) . ?
C12 C14 1.496(5) . ?
C12 C13 1.513(5) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.526(4) . ?
C15 C17 1.538(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N2 1.405(3) . ?
C18 C23 1.409(4) . ?
C18 C19 1.425(4) . ?
C19 C20 1.388(4) . ?
C19 C27 1.513(4) . ?
C20 C21 1.379(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.376(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.399(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.523(4) . ?
C24 C25 1.525(4) . ?
C24 C26 1.526(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.513(4) . ?
C27 C29 1.538(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.497(3) . ?
C30 C33 1.524(4) . ?
C30 C31 1.531(4) . ?
C30 C32 1.531(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.496(4) . ?
C34 N3 1.515(3) . ?
C34 C43 1.515(4) . ?
C34 Nb1 2.646(3) . ?
C34 H34 1.0000 . ?
C35 C36 1.335(4) . ?
C35 H35 0.9500 . ?
C36 O1 1.358(3) . ?
C36 C37 1.488(4) . ?
C37 C38 1.385(4) . ?
C37 C42 1.392(4) . ?
C38 C39 1.390(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.379(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.375(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.388(4) . ?
C43 C44 1.395(4) . ?
C44 C45 1.382(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.379(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.382(4) . ?
C46 Cl1 1.745(3) . ?
C47 C48 1.377(4) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.507(4) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.338(4) . ?
C50 Nb2 2.243(3) . ?
C51 C52 1.457(4) . ?
C51 H51 0.9500 . ?
C52 N4 1.299(3) . ?
C52 C53 1.498(4) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C59 1.405(4) . ?
C54 C55 1.412(4) . ?
C54 N4 1.444(3) . ?
C55 C56 1.396(4) . ?
C55 C63 1.515(4) . ?
C56 C57 1.385(4) . ?
C56 H56 0.9500 . ?
C57 C58 1.373(4) . ?
C57 H57 0.9500 . ?
C58 C59 1.398(4) . ?
C58 H58 0.9500 . ?
C59 C60 1.520(4) . ?
C60 C61 1.535(4) . ?
C60 C62 1.541(4) . ?
C60 H60 1.0000 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C65 1.524(4) . ?
C63 C64 1.527(4) . ?
C63 H63 1.0000 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 N5 1.398(3) . ?
C66 C67 1.415(4) . ?
C66 C71 1.416(4) . ?
C67 C68 1.389(4) . ?
C67 C75 1.518(4) . ?
C68 C69 1.381(4) . ?
C68 H68 0.9500 . ?
C69 C70 1.380(4) . ?
C69 H69 0.9500 . ?
C70 C71 1.394(4) . ?
C70 H70 0.9500 . ?
C71 C72 1.524(4) . ?
C72 C73 1.523(4) . ?
C72 C74 1.531(4) . ?
C72 H72 1.0000 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C77 1.514(4) . ?
C75 C76 1.539(4) . ?
C75 H75 1.0000 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 N6 1.495(3) . ?
C78 C79 1.526(4) . ?
C78 C81 1.536(4) . ?
C78 C80 1.538(4) . ?
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 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 C83 1.504(4) . ?
C82 N6 1.510(3) . ?
C82 C91 1.522(4) . ?
C82 Nb2 2.647(3) . ?
C82 H82 1.0000 . ?
C83 C84 1.343(4) . ?
C83 H83 0.9500 . ?
C84 O2 1.346(3) . ?
C84 C85 1.477(4) . ?
C85 C86 1.391(4) . ?
C85 C90 1.392(4) . ?
C86 C87 1.385(4) . ?
C86 H86 0.9500 . ?
C87 C88 1.374(4) . ?
C87 H87 0.9500 . ?
C88 C89 1.376(4) . ?
C88 H88 0.9500 . ?
C89 C90 1.383(4) . ?
C89 H89 0.9500 . ?
C90 H90 0.9500 . ?
C91 C96 1.385(4) . ?
C91 C92 1.388(4) . ?
C92 C93 1.389(4) . ?
C92 H92 0.9500 . ?
C93 C94 1.377(4) . ?
C93 H93 0.9500 . ?
C94 C95 1.382(4) . ?
C94 Cl2 1.751(3) . ?
C95 C96 1.387(4) . ?
C95 H95 0.9500 . ?
C96 H96 0.9500 . ?
N1 Nb1 2.334(2) . ?
N2 Nb1 1.781(2) . ?
N3 Nb1 1.963(2) . ?
N4 Nb2 2.323(2) . ?
N5 Nb2 1.779(2) . ?
N6 Nb2 1.969(2) . ?
O1 Nb1 2.0373(18) . ?
O2 Nb2 2.0170(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 Nb1 115.1(2) . . ?
C1 C2 Nb1 125.61(19) . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
N1 C4 C3 117.9(2) . . ?
N1 C4 C5 124.5(3) . . ?
C3 C4 C5 117.6(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 121.6(3) . . ?
C11 C6 N1 119.1(2) . . ?
C7 C6 N1 119.2(2) . . ?
C8 C7 C6 117.9(3) . . ?
C8 C7 C15 119.5(3) . . ?
C6 C7 C15 122.5(3) . . ?
C9 C8 C7 121.4(3) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 119.6(3) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 121.5(3) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C6 C11 C10 117.9(3) . . ?
C6 C11 C12 122.1(3) . . ?
C10 C11 C12 120.0(3) . . ?
C14 C12 C13 110.3(3) . . ?
C14 C12 C11 112.7(3) . . ?
C13 C12 C11 111.6(3) . . ?
C14 C12 H12 107.3 . . ?
C13 C12 H12 107.3 . . ?
C11 C12 H12 107.3 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C7 112.0(3) . . ?
C16 C15 C17 109.7(2) . . ?
C7 C15 C17 110.5(2) . . ?
C16 C15 H15 108.2 . . ?
C7 C15 H15 108.2 . . ?
C17 C15 H15 108.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C23 120.7(3) . . ?
N2 C18 C19 118.9(3) . . ?
C23 C18 C19 120.4(3) . . ?
C20 C19 C18 118.5(3) . . ?
C20 C19 C27 121.2(3) . . ?
C18 C19 C27 120.2(3) . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 121.6(3) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C22 C23 C18 118.1(3) . . ?
C22 C23 C24 120.9(3) . . ?
C18 C23 C24 121.0(3) . . ?
C23 C24 C25 110.9(3) . . ?
C23 C24 C26 114.3(3) . . ?
C25 C24 C26 109.2(3) . . ?
C23 C24 H24 107.4 . . ?
C25 C24 H24 107.4 . . ?
C26 C24 H24 107.4 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C19 110.4(3) . . ?
C28 C27 C29 109.1(3) . . ?
C19 C27 C29 115.0(3) . . ?
C28 C27 H27 107.4 . . ?
C19 C27 H27 107.4 . . ?
C29 C27 H27 107.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C33 107.0(2) . . ?
N3 C30 C31 113.0(2) . . ?
C33 C30 C31 107.1(2) . . ?
N3 C30 C32 110.4(2) . . ?
C33 C30 C32 109.5(2) . . ?
C31 C30 C32 109.8(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 N3 110.3(2) . . ?
C35 C34 C43 117.0(2) . . ?
N3 C34 C43 115.9(2) . . ?
C35 C34 Nb1 100.49(17) . . ?
N3 C34 Nb1 47.27(11) . . ?
C43 C34 Nb1 142.32(18) . . ?
C35 C34 H34 103.9 . . ?
N3 C34 H34 103.9 . . ?
C43 C34 H34 103.9 . . ?
Nb1 C34 H34 61.2 . . ?
C36 C35 C34 119.2(3) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C35 C36 O1 120.7(3) . . ?
C35 C36 C37 123.5(3) . . ?
O1 C36 C37 115.7(2) . . ?
C38 C37 C42 118.3(3) . . ?
C38 C37 C36 120.6(3) . . ?
C42 C37 C36 121.1(3) . . ?
C37 C38 C39 120.7(3) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C40 C39 C38 120.5(3) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C41 C40 C39 119.1(3) . . ?
C41 C40 H40 120.5 . . ?
C39 C40 H40 120.5 . . ?
C40 C41 C42 120.8(3) . . ?
C40 C41 H41 119.6 . . ?
C42 C41 H41 119.6 . . ?
C41 C42 C37 120.6(3) . . ?
C41 C42 H42 119.7 . . ?
C37 C42 H42 119.7 . . ?
C48 C43 C44 117.7(3) . . ?
C48 C43 C34 119.3(2) . . ?
C44 C43 C34 123.0(2) . . ?
C45 C44 C43 120.9(3) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C46 C45 C44 119.5(3) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
C45 C46 C47 121.0(3) . . ?
C45 C46 Cl1 120.0(2) . . ?
C47 C46 Cl1 119.0(2) . . ?
C48 C47 C46 118.6(3) . . ?
C48 C47 H47 120.7 . . ?
C46 C47 H47 120.7 . . ?
C47 C48 C43 122.2(3) . . ?
C47 C48 H48 118.9 . . ?
C43 C48 H48 118.9 . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C50 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C49 119.9(3) . . ?
C51 C50 Nb2 115.3(2) . . ?
C49 C50 Nb2 124.78(19) . . ?
C50 C51 C52 119.3(3) . . ?
C50 C51 H51 120.3 . . ?
C52 C51 H51 120.3 . . ?
N4 C52 C51 117.5(2) . . ?
N4 C52 C53 124.5(3) . . ?
C51 C52 C53 118.0(2) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C59 C54 C55 122.1(3) . . ?
C59 C54 N4 119.0(3) . . ?
C55 C54 N4 119.0(2) . . ?
C56 C55 C54 117.4(3) . . ?
C56 C55 C63 121.3(3) . . ?
C54 C55 C63 121.3(2) . . ?
C57 C56 C55 121.2(3) . . ?
C57 C56 H56 119.4 . . ?
C55 C56 H56 119.4 . . ?
C58 C57 C56 120.3(3) . . ?
C58 C57 H57 119.8 . . ?
C56 C57 H57 119.8 . . ?
C57 C58 C59 121.4(3) . . ?
C57 C58 H58 119.3 . . ?
C59 C58 H58 119.3 . . ?
C58 C59 C54 117.6(3) . . ?
C58 C59 C60 118.8(3) . . ?
C54 C59 C60 123.6(3) . . ?
C59 C60 C61 111.0(2) . . ?
C59 C60 C62 111.6(2) . . ?
C61 C60 C62 110.1(2) . . ?
C59 C60 H60 108.0 . . ?
C61 C60 H60 108.0 . . ?
C62 C60 H60 108.0 . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 H62A 109.5 . . ?
C60 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C60 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C55 C63 C65 113.9(2) . . ?
C55 C63 C64 111.8(2) . . ?
C65 C63 C64 109.1(3) . . ?
C55 C63 H63 107.3 . . ?
C65 C63 H63 107.3 . . ?
C64 C63 H63 107.3 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N5 C66 C67 118.8(2) . . ?
N5 C66 C71 120.2(2) . . ?
C67 C66 C71 121.0(3) . . ?
C68 C67 C66 118.2(3) . . ?
C68 C67 C75 121.9(3) . . ?
C66 C67 C75 119.9(3) . . ?
C69 C68 C67 121.5(3) . . ?
C69 C68 H68 119.3 . . ?
C67 C68 H68 119.3 . . ?
C70 C69 C68 119.9(3) . . ?
C70 C69 H69 120.1 . . ?
C68 C69 H69 120.1 . . ?
C69 C70 C71 121.7(3) . . ?
C69 C70 H70 119.1 . . ?
C71 C70 H70 119.1 . . ?
C70 C71 C66 117.7(3) . . ?
C70 C71 C72 121.8(3) . . ?
C66 C71 C72 120.5(2) . . ?
C73 C72 C71 111.9(2) . . ?
C73 C72 C74 108.8(2) . . ?
C71 C72 C74 114.4(2) . . ?
C73 C72 H72 107.1 . . ?
C71 C72 H72 107.1 . . ?
C74 C72 H72 107.1 . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C72 C74 H74A 109.5 . . ?
C72 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C72 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C77 C75 C67 110.0(2) . . ?
C77 C75 C76 110.8(3) . . ?
C67 C75 C76 113.2(2) . . ?
C77 C75 H75 107.5 . . ?
C67 C75 H75 107.5 . . ?
C76 C75 H75 107.5 . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
N6 C78 C79 107.0(2) . . ?
N6 C78 C81 111.6(2) . . ?
C79 C78 C81 109.5(2) . . ?
N6 C78 C80 111.8(2) . . ?
C79 C78 C80 106.5(2) . . ?
C81 C78 C80 110.2(2) . . ?
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 . . ?
C78 C81 H81A 109.5 . . ?
C78 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C78 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C83 C82 N6 110.9(2) . . ?
C83 C82 C91 116.7(2) . . ?
N6 C82 C91 117.2(2) . . ?
C83 C82 Nb2 100.59(17) . . ?
N6 C82 Nb2 47.43(11) . . ?
C91 C82 Nb2 142.26(18) . . ?
C83 C82 H82 103.2 . . ?
N6 C82 H82 103.2 . . ?
C91 C82 H82 103.2 . . ?
Nb2 C82 H82 60.2 . . ?
C84 C83 C82 117.4(2) . . ?
C84 C83 H83 121.3 . . ?
C82 C83 H83 121.3 . . ?
C83 C84 O2 120.5(2) . . ?
C83 C84 C85 125.7(2) . . ?
O2 C84 C85 113.8(2) . . ?
C86 C85 C90 118.9(3) . . ?
C86 C85 C84 119.8(2) . . ?
C90 C85 C84 121.3(2) . . ?
C87 C86 C85 120.5(3) . . ?
C87 C86 H86 119.8 . . ?
C85 C86 H86 119.8 . . ?
C88 C87 C86 120.1(3) . . ?
C88 C87 H87 120.0 . . ?
C86 C87 H87 120.0 . . ?
C87 C88 C89 120.0(3) . . ?
C87 C88 H88 120.0 . . ?
C89 C88 H88 120.0 . . ?
C88 C89 C90 120.6(3) . . ?
C88 C89 H89 119.7 . . ?
C90 C89 H89 119.7 . . ?
C89 C90 C85 119.9(3) . . ?
C89 C90 H90 120.0 . . ?
C85 C90 H90 120.0 . . ?
C96 C91 C92 118.1(3) . . ?
C96 C91 C82 118.9(2) . . ?
C92 C91 C82 123.0(2) . . ?
C91 C92 C93 121.2(3) . . ?
C91 C92 H92 119.4 . . ?
C93 C92 H92 119.4 . . ?
C94 C93 C92 118.9(3) . . ?
C94 C93 H93 120.6 . . ?
C92 C93 H93 120.6 . . ?
C93 C94 C95 121.7(3) . . ?
C93 C94 Cl2 118.8(2) . . ?
C95 C94 Cl2 119.5(2) . . ?
C94 C95 C96 118.1(3) . . ?
C94 C95 H95 120.9 . . ?
C96 C95 H95 120.9 . . ?
C91 C96 C95 122.0(3) . . ?
C91 C96 H96 119.0 . . ?
C95 C96 H96 119.0 . . ?
C4 N1 C6 119.2(2) . . ?
C4 N1 Nb1 114.81(18) . . ?
C6 N1 Nb1 125.94(17) . . ?
C18 N2 Nb1 171.8(2) . . ?
C30 N3 C34 121.1(2) . . ?
C30 N3 Nb1 139.30(17) . . ?
C34 N3 Nb1 98.20(15) . . ?
C52 N4 C54 119.2(2) . . ?
C52 N4 Nb2 115.02(18) . . ?
C54 N4 Nb2 125.52(16) . . ?
C66 N5 Nb2 168.97(19) . . ?
C78 N6 C82 120.8(2) . . ?
C78 N6 Nb2 139.77(17) . . ?
C82 N6 Nb2 98.17(15) . . ?
C36 O1 Nb1 124.27(17) . . ?
C84 O2 Nb2 124.75(16) . . ?
N2 Nb1 N3 110.29(9) . . ?
N2 Nb1 O1 109.07(9) . . ?
N3 Nb1 O1 91.41(8) . . ?
N2 Nb1 C2 101.15(10) . . ?
N3 Nb1 C2 92.90(10) . . ?
O1 Nb1 C2 145.79(9) . . ?
N2 Nb1 N1 105.73(9) . . ?
N3 Nb1 N1 143.18(8) . . ?
O1 Nb1 N1 83.84(7) . . ?
C2 Nb1 N1 72.62(9) . . ?
N2 Nb1 C34 142.60(9) . . ?
N3 Nb1 C34 34.53(8) . . ?
O1 Nb1 C34 70.91(8) . . ?
C2 Nb1 C34 94.58(9) . . ?
N1 Nb1 C34 111.32(8) . . ?
N5 Nb2 N6 111.59(9) . . ?
N5 Nb2 O2 108.29(9) . . ?
N6 Nb2 O2 92.15(8) . . ?
N5 Nb2 C50 101.76(10) . . ?
N6 Nb2 C50 96.74(9) . . ?
O2 Nb2 C50 142.83(9) . . ?
N5 Nb2 N4 102.56(9) . . ?
N6 Nb2 N4 145.72(8) . . ?
O2 Nb2 N4 79.59(7) . . ?
C50 Nb2 N4 72.84(9) . . ?
N5 Nb2 C82 142.69(9) . . ?
N6 Nb2 C82 34.40(8) . . ?
O2 Nb2 C82 70.05(8) . . ?
C50 Nb2 C82 98.43(9) . . ?
N4 Nb2 C82 113.29(8) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.075
_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/. 
# 
# Audit and citation data items have may 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_(2)
_database_code_depnum_ccdc_archive 'CCDC 1026786'
_audit_update_record             
;
2014-09-28 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_chemical_name_common            'Compex 3'
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H82 N4 N2 O2'
_chemical_formula_sum            'C29 H41 N2 Nb O'
_chemical_formula_weight         526.55

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.1260(7)
_cell_length_b                   16.7319(11)
_cell_length_c                   15.5707(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.0600(10)
_cell_angle_gamma                90.00
_cell_volume                     2755.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9858
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.16

_exptl_crystal_description       rode
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9542
_exptl_absorpt_correction_T_max  0.9813
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            41926
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         25.21
_reflns_number_total             4934
_reflns_number_gt                4366
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0269P)²+1.9871P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4934
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7335(2) 0.14708(16) 0.32100(16) 0.0417(6) Uani 1 1 d . . .
H1A H 0.7096 0.2006 0.3005 0.063 Uiso 1 1 calc R . .
H1B H 0.7055 0.1357 0.3722 0.063 Uiso 1 1 calc R . .
H1C H 0.6951 0.1100 0.2733 0.063 Uiso 1 1 calc R . .
C2 C 0.87441(18) 0.13911(12) 0.34766(12) 0.0259(4) Uani 1 1 d . . .
C3 C 0.94518(19) 0.20086(12) 0.33723(13) 0.0277(4) Uani 1 1 d . . .
H3 H 0.9079 0.2499 0.3168 0.033 Uiso 1 1 calc R . .
C4 C 1.08101(19) 0.19040(12) 0.35815(12) 0.0248(4) Uani 1 1 d . . .
C5 C 1.1577(2) 0.26033(13) 0.34519(15) 0.0359(5) Uani 1 1 d . . .
H5A H 1.2431 0.2435 0.3535 0.054 Uiso 1 1 calc R . .
H5B H 1.1573 0.3011 0.3885 0.054 Uiso 1 1 calc R . .
H5C H 1.1219 0.2812 0.2853 0.054 Uiso 1 1 calc R . .
C6 C 1.26061(17) 0.10574(11) 0.40732(12) 0.0211(4) Uani 1 1 d . . .
C7 C 1.30292(18) 0.06482(11) 0.34323(13) 0.0243(4) Uani 1 1 d . . .
C8 C 1.43271(19) 0.05238(12) 0.36352(14) 0.0284(4) Uani 1 1 d . . .
H8 H 1.4633 0.0268 0.3215 0.034 Uiso 1 1 calc R . .
C9 C 1.51659(19) 0.07714(12) 0.44436(14) 0.0306(5) Uani 1 1 d . . .
H9 H 1.6027 0.0677 0.4568 0.037 Uiso 1 1 calc R . .
C10 C 1.47242(19) 0.11598(12) 0.50679(14) 0.0293(5) Uani 1 1 d . . .
H10 H 1.5297 0.1321 0.5613 0.035 Uiso 1 1 calc R . .
C11 C 1.34434(18) 0.13155(11) 0.49014(13) 0.0246(4) Uani 1 1 d . . .
C12 C 1.3016(2) 0.17431(13) 0.56120(13) 0.0309(5) Uani 1 1 d . . .
H12 H 1.2098 0.1817 0.5373 0.037 Uiso 1 1 calc R . .
C13 C 1.3301(2) 0.12535(14) 0.64810(14) 0.0357(5) Uani 1 1 d . . .
H13A H 1.2928 0.0733 0.6344 0.054 Uiso 1 1 calc R . .
H13B H 1.2954 0.1519 0.6898 0.054 Uiso 1 1 calc R . .
H13C H 1.4199 0.1201 0.6747 0.054 Uiso 1 1 calc R . .
C14 C 1.3630(3) 0.25716(14) 0.58228(16) 0.0458(6) Uani 1 1 d . . .
H14A H 1.4529 0.2512 0.6082 0.069 Uiso 1 1 calc R . .
H14B H 1.3298 0.2844 0.6243 0.069 Uiso 1 1 calc R . .
H14C H 1.3449 0.2877 0.5275 0.069 Uiso 1 1 calc R . .
C15 C 1.21116(19) 0.03644(12) 0.25462(13) 0.0281(4) Uani 1 1 d . . .
H15 H 1.1308 0.0248 0.2656 0.034 Uiso 1 1 calc R . .
C16 C 1.1855(3) 0.10180(15) 0.18259(15) 0.0467(6) Uani 1 1 d . . .
H16A H 1.1577 0.1494 0.2052 0.070 Uiso 1 1 calc R . .
H16B H 1.1211 0.0841 0.1293 0.070 Uiso 1 1 calc R . .
H16C H 1.2616 0.1129 0.1681 0.070 Uiso 1 1 calc R . .
C17 C 1.2532(2) -0.03986(14) 0.21858(15) 0.0386(5) Uani 1 1 d . . .
H17A H 1.3257 -0.0287 0.1995 0.058 Uiso 1 1 calc R . .
H17B H 1.1856 -0.0593 0.1682 0.058 Uiso 1 1 calc R . .
H17C H 1.2747 -0.0796 0.2654 0.058 Uiso 1 1 calc R . .
C18 C 0.95028(18) -0.09554(12) 0.25096(12) 0.0245(4) Uani 1 1 d . . .
C19 C 1.00850(18) -0.16979(12) 0.28053(14) 0.0284(4) Uani 1 1 d . . .
C20 C 1.0192(2) -0.22401(13) 0.21546(15) 0.0341(5) Uani 1 1 d . . .
H20 H 1.0602 -0.2725 0.2337 0.041 Uiso 1 1 calc R . .
C21 C 0.9704(2) -0.20737(14) 0.12463(16) 0.0397(6) Uani 1 1 d . . .
H21 H 0.9809 -0.2437 0.0823 0.048 Uiso 1 1 calc R . .
C22 C 0.9063(2) -0.13717(14) 0.09663(15) 0.0412(6) Uani 1 1 d . . .
H22 H 0.8708 -0.1277 0.0351 0.049 Uiso 1 1 calc R . .
C23 C 0.8931(2) -0.07967(13) 0.15814(13) 0.0334(5) Uani 1 1 d . . .
C24 C 0.8170(3) -0.00439(15) 0.12826(14) 0.0472(6) Uani 1 1 d . . .
H24 H 0.8585 0.0384 0.1698 0.057 Uiso 1 1 calc R . .
C25 C 0.8082(4) 0.02261(16) 0.03240(17) 0.0663(9) Uani 1 1 d . . .
H25A H 0.8918 0.0296 0.0281 0.099 Uiso 1 1 calc R . .
H25B H 0.7631 0.0723 0.0193 0.099 Uiso 1 1 calc R . .
H25C H 0.7643 -0.0172 -0.0102 0.099 Uiso 1 1 calc R . .
C26 C 0.6854(3) -0.0152(2) 0.1363(2) 0.0681(9) Uani 1 1 d . . .
H26A H 0.6431 -0.0579 0.0974 0.102 Uiso 1 1 calc R . .
H26B H 0.6381 0.0334 0.1188 0.102 Uiso 1 1 calc R . .
H26C H 0.6917 -0.0279 0.1976 0.102 Uiso 1 1 calc R . .
C27 C 1.0600(2) -0.19025(13) 0.38065(14) 0.0348(5) Uani 1 1 d . . .
H27 H 1.0248 -0.1512 0.4132 0.042 Uiso 1 1 calc R . .
C28 C 1.2026(2) -0.18095(18) 0.41445(18) 0.0559(7) Uani 1 1 d . . .
H28A H 1.2403 -0.2174 0.3826 0.084 Uiso 1 1 calc R . .
H28B H 1.2331 -0.1924 0.4779 0.084 Uiso 1 1 calc R . .
H28C H 1.2248 -0.1271 0.4041 0.084 Uiso 1 1 calc R . .
C29 C 1.0201(3) -0.27308(15) 0.40329(17) 0.0472(6) Uani 1 1 d . . .
H29A H 0.9298 -0.2778 0.3802 0.071 Uiso 1 1 calc R . .
H29B H 1.0472 -0.2802 0.4676 0.071 Uiso 1 1 calc R . .
H29C H 1.0584 -0.3132 0.3762 0.071 Uiso 1 1 calc R . .
N1 N 1.12668(14) 0.12037(9) 0.38635(9) 0.0198(3) Uani 1 1 d . . .
N2 N 0.95193(15) -0.03550(9) 0.31317(10) 0.0230(3) Uani 1 1 d . . .
Nb1 Nb 0.982029(15) 0.030289(10) 0.407753(10) 0.01857(6) Uani 1 1 d . . .
O1 O 0.87971(12) -0.00074(8) 0.48098(8) 0.0214(3) 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 1.498(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.339(3) . ?
C2 Nb1 2.220(2) . ?
C3 C4 1.454(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.298(2) . ?
C4 C5 1.498(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C11 1.404(3) . ?
C6 C7 1.406(3) . ?
C6 N1 1.444(2) . ?
C7 C8 1.395(3) . ?
C7 C15 1.516(3) . ?
C8 C9 1.378(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.392(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.513(3) . ?
C12 C13 1.529(3) . ?
C12 C14 1.536(3) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C17 1.525(3) . ?
C15 C16 1.529(3) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N2 1.392(2) . ?
C18 C19 1.411(3) . ?
C18 C23 1.412(3) . ?
C19 C20 1.392(3) . ?
C19 C27 1.524(3) . ?
C20 C21 1.377(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.373(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.397(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.509(3) . ?
C24 C26 1.518(4) . ?
C24 C25 1.534(3) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.518(3) . ?
C27 C29 1.529(3) . ?
C27 H27 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
N1 Nb1 2.3033(15) . ?
N2 Nb1 1.7853(15) . ?
Nb1 O1 1.9158(12) . ?
Nb1 O1 1.9899(12) 3_756 ?
Nb1 Nb1 2.9542(4) 3_756 ?
O1 Nb1 1.9899(12) 3_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 120.13(19) . . ?
C3 C2 Nb1 115.04(14) . . ?
C1 C2 Nb1 124.82(15) . . ?
C2 C3 C4 119.29(18) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
N1 C4 C3 117.06(17) . . ?
N1 C4 C5 124.80(18) . . ?
C3 C4 C5 118.14(18) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 121.91(18) . . ?
C11 C6 N1 119.98(16) . . ?
C7 C6 N1 118.10(16) . . ?
C8 C7 C6 117.56(18) . . ?
C8 C7 C15 121.15(18) . . ?
C6 C7 C15 121.28(17) . . ?
C9 C8 C7 121.50(19) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 119.78(19) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 121.65(19) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C6 117.57(18) . . ?
C10 C11 C12 119.24(18) . . ?
C6 C11 C12 123.19(18) . . ?
C11 C12 C13 111.58(17) . . ?
C11 C12 C14 111.27(18) . . ?
C13 C12 C14 109.77(17) . . ?
C11 C12 H12 108.0 . . ?
C13 C12 H12 108.0 . . ?
C14 C12 H12 108.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 C17 113.59(18) . . ?
C7 C15 C16 111.32(17) . . ?
C17 C15 C16 109.74(18) . . ?
C7 C15 H15 107.3 . . ?
C17 C15 H15 107.3 . . ?
C16 C15 H15 107.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C19 120.19(17) . . ?
N2 C18 C23 118.77(18) . . ?
C19 C18 C23 121.00(18) . . ?
C20 C19 C18 118.07(19) . . ?
C20 C19 C27 120.5(2) . . ?
C18 C19 C27 121.37(18) . . ?
C21 C20 C19 121.3(2) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C22 C21 C20 120.0(2) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 121.7(2) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 117.6(2) . . ?
C22 C23 C24 122.14(19) . . ?
C18 C23 C24 120.27(18) . . ?
C23 C24 C26 109.8(2) . . ?
C23 C24 C25 113.9(2) . . ?
C26 C24 C25 110.1(2) . . ?
C23 C24 H24 107.6 . . ?
C26 C24 H24 107.6 . . ?
C25 C24 H24 107.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C19 110.6(2) . . ?
C28 C27 C29 111.1(2) . . ?
C19 C27 C29 113.31(18) . . ?
C28 C27 H27 107.2 . . ?
C19 C27 H27 107.2 . . ?
C29 C27 H27 107.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C4 N1 C6 119.85(16) . . ?
C4 N1 Nb1 114.95(13) . . ?
C6 N1 Nb1 125.07(11) . . ?
C18 N2 Nb1 167.94(14) . . ?
N2 Nb1 O1 109.25(6) . . ?
N2 Nb1 O1 117.50(6) . 3_756 ?
O1 Nb1 O1 81.73(5) . 3_756 ?
N2 Nb1 C2 102.67(7) . . ?
O1 Nb1 C2 97.51(6) . . ?
O1 Nb1 C2 137.81(6) 3_756 . ?
N2 Nb1 N1 104.18(6) . . ?
O1 Nb1 N1 146.53(5) . . ?
O1 Nb1 N1 84.40(5) 3_756 . ?
C2 Nb1 N1 73.27(6) . . ?
N2 Nb1 Nb1 121.66(5) . 3_756 ?
O1 Nb1 Nb1 41.80(4) . 3_756 ?
O1 Nb1 Nb1 39.92(4) 3_756 3_756 ?
C2 Nb1 Nb1 125.72(5) . 3_756 ?
N1 Nb1 Nb1 118.37(4) . 3_756 ?
Nb1 O1 Nb1 98.27(5) . 3_756 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.052
_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/. 
# 
# Audit and citation data items have may 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_(3)
_database_code_depnum_ccdc_archive 'CCDC 1026787'
_audit_update_record             
;
2014-09-28 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_chemical_name_common            'Complex 4'
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H60 N3 Nb'
_chemical_formula_sum            'C47 H60 N3 Nb'
_chemical_formula_weight         759.89

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7140(19)
_cell_length_b                   11.714(2)
_cell_length_c                   18.976(3)
_cell_angle_alpha                86.853(10)
_cell_angle_beta                 76.422(9)
_cell_angle_gamma                65.449(8)
_cell_volume                     2103.3(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9810
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.56

_exptl_crystal_description       rode
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9387
_exptl_absorpt_correction_T_max  0.9810
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            45285
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.11
_diffrn_reflns_theta_max         25.56
_reflns_number_total             7757
_reflns_number_gt                6831
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0429P)²+1.5412P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7757
_refine_ls_number_parameters     473
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0809
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7259(2) 0.2648(2) 0.35281(12) 0.0210(5) Uani 1 1 d . . .
H1A H 0.6531 0.3210 0.3908 0.031 Uiso 1 1 calc R . .
H1B H 0.8072 0.2154 0.3714 0.031 Uiso 1 1 calc R . .
H1C H 0.6920 0.2103 0.3353 0.031 Uiso 1 1 calc R . .
C2 C 0.7658(2) 0.3403(2) 0.29103(12) 0.0152(4) Uani 1 1 d . . .
C3 C 0.6510(2) 0.4588(2) 0.27926(12) 0.0157(4) Uani 1 1 d . . .
H3 H 0.5611 0.4691 0.3046 0.019 Uiso 1 1 calc R . .
C4 C 0.6551(2) 0.5585(2) 0.23614(12) 0.0165(5) Uani 1 1 d . . .
C5 C 0.5217(2) 0.6782(2) 0.24455(13) 0.0238(5) Uani 1 1 d . . .
H5A H 0.5272 0.7395 0.2738 0.036 Uiso 1 1 calc R . .
H5B H 0.4419 0.6609 0.2676 0.036 Uiso 1 1 calc R . .
H5C H 0.5113 0.7101 0.1976 0.036 Uiso 1 1 calc R . .
C6 C 0.7813(2) 0.6481(2) 0.14346(12) 0.0158(5) Uani 1 1 d . . .
C7 C 0.8000(2) 0.7563(2) 0.15759(12) 0.0199(5) Uani 1 1 d . . .
C8 C 0.7912(2) 0.8441(2) 0.10432(13) 0.0218(5) Uani 1 1 d . . .
H8 H 0.8036 0.9155 0.1133 0.026 Uiso 1 1 calc R . .
C9 C 0.7648(2) 0.8285(2) 0.03875(12) 0.0214(5) Uani 1 1 d . . .
H9 H 0.7566 0.8897 0.0046 0.026 Uiso 1 1 calc R . .
C10 C 0.7508(2) 0.7205(2) 0.02435(13) 0.0216(5) Uani 1 1 d . . .
H10 H 0.7349 0.7088 -0.0203 0.026 Uiso 1 1 calc R . .
C11 C 0.7598(2) 0.6286(2) 0.07536(12) 0.0177(5) Uani 1 1 d . . .
C12 C 0.7461(3) 0.5112(2) 0.05545(12) 0.0233(5) Uani 1 1 d . . .
H12 H 0.7787 0.4488 0.0912 0.028 Uiso 1 1 calc R . .
C13 C 0.8373(3) 0.4541(2) -0.01922(13) 0.0328(6) Uani 1 1 d . . .
H13A H 0.8082 0.5136 -0.0554 0.049 Uiso 1 1 calc R . .
H13B H 0.8269 0.3795 -0.0292 0.049 Uiso 1 1 calc R . .
H13C H 0.9344 0.4332 -0.0202 0.049 Uiso 1 1 calc R . .
C14 C 0.5920(3) 0.5381(3) 0.05954(18) 0.0419(7) Uani 1 1 d . . .
H14A H 0.5363 0.5707 0.1074 0.063 Uiso 1 1 calc R . .
H14B H 0.5856 0.4618 0.0490 0.063 Uiso 1 1 calc R . .
H14C H 0.5573 0.5987 0.0248 0.063 Uiso 1 1 calc R . .
C15 C 0.8292(3) 0.7838(2) 0.22777(14) 0.0298(6) Uani 1 1 d . . .
H15 H 0.8357 0.7132 0.2592 0.036 Uiso 1 1 calc R . .
C16 C 0.9697(3) 0.7955(3) 0.21233(18) 0.0482(8) Uani 1 1 d . . .
H16A H 1.0444 0.7178 0.1903 0.072 Uiso 1 1 calc R . .
H16B H 0.9866 0.8138 0.2570 0.072 Uiso 1 1 calc R . .
H16C H 0.9665 0.8620 0.1800 0.072 Uiso 1 1 calc R . .
C17 C 0.7097(4) 0.9032(3) 0.26747(16) 0.0497(8) Uani 1 1 d . . .
H17A H 0.7023 0.9735 0.2376 0.074 Uiso 1 1 calc R . .
H17B H 0.7294 0.9172 0.3122 0.074 Uiso 1 1 calc R . .
H17C H 0.6225 0.8938 0.2775 0.074 Uiso 1 1 calc R . .
C18 C 1.1666(2) 0.2626(2) 0.30609(11) 0.0164(5) Uani 1 1 d . . .
C19 C 1.2495(2) 0.3319(2) 0.29666(12) 0.0174(5) Uani 1 1 d . . .
C20 C 1.3748(2) 0.2814(2) 0.32041(12) 0.0208(5) Uani 1 1 d . . .
H20 H 1.4307 0.3260 0.3142 0.025 Uiso 1 1 calc R . .
C21 C 1.4183(2) 0.1678(2) 0.35268(13) 0.0233(5) Uani 1 1 d . . .
H21 H 1.5039 0.1348 0.3664 0.028 Uiso 1 1 calc R . .
C22 C 1.3331(2) 0.1035(2) 0.36451(12) 0.0228(5) Uani 1 1 d . . .
H22 H 1.3614 0.0276 0.3873 0.027 Uiso 1 1 calc R . .
C23 C 1.2061(2) 0.1491(2) 0.34320(12) 0.0181(5) Uani 1 1 d . . .
C24 C 1.1064(2) 0.0857(2) 0.36734(12) 0.0201(5) Uani 1 1 d . . .
H24 H 1.0419 0.1090 0.3347 0.024 Uiso 1 1 calc R . .
C25 C 1.0184(3) 0.1380(2) 0.44406(13) 0.0268(5) Uani 1 1 d . . .
H25A H 1.0795 0.1164 0.4771 0.040 Uiso 1 1 calc R . .
H25B H 0.9506 0.1027 0.4592 0.040 Uiso 1 1 calc R . .
H25C H 0.9702 0.2278 0.4439 0.040 Uiso 1 1 calc R . .
C26 C 1.1808(3) -0.0585(2) 0.36515(15) 0.0299(6) Uani 1 1 d . . .
H26A H 1.2410 -0.0889 0.3178 0.045 Uiso 1 1 calc R . .
H26B H 1.1114 -0.0927 0.3754 0.045 Uiso 1 1 calc R . .
H26C H 1.2363 -0.0839 0.4008 0.045 Uiso 1 1 calc R . .
C27 C 1.2092(2) 0.4603(2) 0.26356(12) 0.0202(5) Uani 1 1 d . . .
H27 H 1.1218 0.4807 0.2479 0.024 Uiso 1 1 calc R . .
C28 C 1.3216(3) 0.4618(2) 0.19722(14) 0.0277(6) Uani 1 1 d . . .
H28A H 1.4075 0.4450 0.2116 0.041 Uiso 1 1 calc R . .
H28B H 1.2893 0.5428 0.1767 0.041 Uiso 1 1 calc R . .
H28C H 1.3385 0.3985 0.1617 0.041 Uiso 1 1 calc R . .
C29 C 1.1802(3) 0.5604(2) 0.32061(15) 0.0328(6) Uani 1 1 d . . .
H29A H 1.1050 0.5622 0.3604 0.049 Uiso 1 1 calc R . .
H29B H 1.1536 0.6410 0.2995 0.049 Uiso 1 1 calc R . .
H29C H 1.2638 0.5410 0.3379 0.049 Uiso 1 1 calc R . .
C30 C 0.7324(3) 0.6194(2) 0.44385(13) 0.0300(6) Uani 1 1 d . . .
C31 C 0.8214(5) 0.6734(6) 0.4647(2) 0.123(3) Uani 1 1 d . . .
H31A H 0.9061 0.6069 0.4730 0.184 Uiso 1 1 calc R . .
H31B H 0.7707 0.7256 0.5083 0.184 Uiso 1 1 calc R . .
H31C H 0.8454 0.7231 0.4264 0.184 Uiso 1 1 calc R . .
C32 C 0.7002(4) 0.5315(3) 0.50012(17) 0.0593(10) Uani 1 1 d . . .
H32A H 0.6428 0.4978 0.4846 0.089 Uiso 1 1 calc R . .
H32B H 0.6506 0.5773 0.5459 0.089 Uiso 1 1 calc R . .
H32C H 0.7869 0.4641 0.5054 0.089 Uiso 1 1 calc R . .
C33 C 0.5884(4) 0.7221(4) 0.43773(19) 0.0779(14) Uani 1 1 d . . .
H33A H 0.6025 0.7810 0.4031 0.117 Uiso 1 1 calc R . .
H33B H 0.5381 0.7650 0.4842 0.117 Uiso 1 1 calc R . .
H33C H 0.5347 0.6842 0.4221 0.117 Uiso 1 1 calc R . .
C34 C 0.8834(2) 0.26427(19) 0.22747(11) 0.0139(4) Uani 1 1 d . . .
C35 C 1.0212(2) 0.2348(2) 0.23103(11) 0.0147(4) Uani 1 1 d . . .
C36 C 1.1468(2) 0.1305(2) 0.18703(11) 0.0149(4) Uani 1 1 d . . .
C37 C 1.2692(2) 0.1450(2) 0.15266(11) 0.0175(5) Uani 1 1 d . . .
H37 H 1.2723 0.2228 0.1552 0.021 Uiso 1 1 calc R . .
C38 C 1.3858(2) 0.0445(2) 0.11490(12) 0.0214(5) Uani 1 1 d . . .
H38 H 1.4669 0.0551 0.0921 0.026 Uiso 1 1 calc R . .
C39 C 1.3826(2) -0.0717(2) 0.11071(13) 0.0225(5) Uani 1 1 d . . .
H39 H 1.4612 -0.1389 0.0850 0.027 Uiso 1 1 calc R . .
C40 C 1.2622(2) -0.0874(2) 0.14483(13) 0.0225(5) Uani 1 1 d . . .
H40 H 1.2596 -0.1654 0.1420 0.027 Uiso 1 1 calc R . .
C41 C 1.1453(2) 0.0127(2) 0.18326(12) 0.0186(5) Uani 1 1 d . . .
H41 H 1.0651 0.0012 0.2067 0.022 Uiso 1 1 calc R . .
C42 C 0.8429(2) 0.22422(19) 0.16662(12) 0.0159(4) Uani 1 1 d . . .
C43 C 0.9269(2) 0.1966(2) 0.09595(12) 0.0198(5) Uani 1 1 d . . .
H43 H 1.0129 0.2031 0.0859 0.024 Uiso 1 1 calc R . .
C44 C 0.8854(3) 0.1597(2) 0.04041(13) 0.0231(5) Uani 1 1 d . . .
H44 H 0.9452 0.1386 -0.0057 0.028 Uiso 1 1 calc R . .
C45 C 0.7551(3) 0.1541(2) 0.05321(14) 0.0264(6) Uani 1 1 d . . .
H45 H 0.7266 0.1301 0.0160 0.032 Uiso 1 1 calc R . .
C46 C 0.6689(3) 0.1845(2) 0.12192(14) 0.0270(6) Uani 1 1 d . . .
H46 H 0.5808 0.1822 0.1309 0.032 Uiso 1 1 calc R . .
C47 C 0.7115(2) 0.2188(2) 0.17819(13) 0.0205(5) Uani 1 1 d . . .
H47 H 0.6517 0.2384 0.2243 0.025 Uiso 1 1 calc R . .
N1 N 0.78261(18) 0.55697(16) 0.19736(9) 0.0146(4) Uani 1 1 d . . .
N2 N 1.04202(18) 0.30937(16) 0.27830(9) 0.0149(4) Uani 1 1 d . . .
N3 N 0.8029(2) 0.54941(17) 0.37431(10) 0.0206(4) Uani 1 1 d . . .
Nb1 Nb 0.857240(19) 0.470679(17) 0.288059(10) 0.01363(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.518(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.472(3) . ?
C2 C34 1.519(3) . ?
C2 Nb1 2.123(2) . ?
C3 C4 1.399(3) . ?
C3 Nb1 2.316(2) . ?
C3 H3 0.9300 . ?
C4 N1 1.385(3) . ?
C4 C5 1.512(3) . ?
C4 Nb1 2.400(2) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C11 1.411(3) . ?
C6 C7 1.412(3) . ?
C6 N1 1.435(3) . ?
C7 C8 1.393(3) . ?
C7 C15 1.517(3) . ?
C8 C9 1.376(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.384(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.519(3) . ?
C12 C13 1.524(3) . ?
C12 C14 1.530(4) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.527(4) . ?
C15 C17 1.529(4) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.410(3) . ?
C18 C23 1.419(3) . ?
C18 N2 1.432(3) . ?
C19 C20 1.397(3) . ?
C19 C27 1.525(3) . ?
C20 C21 1.375(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.389(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.515(3) . ?
C24 C25 1.536(3) . ?
C24 C26 1.537(3) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C29 1.524(3) . ?
C27 C28 1.529(3) . ?
C27 H27 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 N3 1.456(3) . ?
C30 C31 1.474(4) . ?
C30 C32 1.523(4) . ?
C30 C33 1.539(4) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.387(3) . ?
C34 C42 1.485(3) . ?
C34 Nb1 2.615(2) . ?
C35 N2 1.400(3) . ?
C35 C36 1.490(3) . ?
C36 C41 1.392(3) . ?
C36 C37 1.395(3) . ?
C37 C38 1.382(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.382(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.382(3) . ?
C39 H39 0.9300 . ?
C40 C41 1.386(3) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 C43 1.397(3) . ?
C42 C47 1.401(3) . ?
C43 C44 1.388(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.388(3) . ?
C44 H44 0.9300 . ?
C45 C46 1.375(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.392(3) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
N1 Nb1 2.0993(18) . ?
N2 Nb1 2.0693(18) . ?
N3 Nb1 1.7721(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 115.85(18) . . ?
C3 C2 C34 120.47(18) . . ?
C1 C2 C34 115.74(18) . . ?
C3 C2 Nb1 77.91(12) . . ?
C1 C2 Nb1 130.46(16) . . ?
C34 C2 Nb1 90.22(13) . . ?
C4 C3 C2 130.45(19) . . ?
C4 C3 Nb1 76.06(13) . . ?
C2 C3 Nb1 63.66(11) . . ?
C4 C3 H3 114.8 . . ?
C2 C3 H3 114.8 . . ?
Nb1 C3 H3 144.8 . . ?
N1 C4 C3 120.65(19) . . ?
N1 C4 C5 120.04(19) . . ?
C3 C4 C5 118.19(19) . . ?
N1 C4 Nb1 60.53(10) . . ?
C3 C4 Nb1 69.48(12) . . ?
C5 C4 Nb1 137.87(16) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 119.8(2) . . ?
C11 C6 N1 118.86(19) . . ?
C7 C6 N1 121.30(19) . . ?
C8 C7 C6 118.6(2) . . ?
C8 C7 C15 117.3(2) . . ?
C6 C7 C15 124.0(2) . . ?
C9 C8 C7 122.0(2) . . ?
C9 C8 H8 119.0 . . ?
C7 C8 H8 119.0 . . ?
C8 C9 C10 119.1(2) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C11 121.5(2) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C6 118.9(2) . . ?
C10 C11 C12 118.7(2) . . ?
C6 C11 C12 122.4(2) . . ?
C11 C12 C13 112.3(2) . . ?
C11 C12 C14 111.1(2) . . ?
C13 C12 C14 110.3(2) . . ?
C11 C12 H12 107.7 . . ?
C13 C12 H12 107.7 . . ?
C14 C12 H12 107.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 C16 110.1(2) . . ?
C7 C15 C17 111.1(2) . . ?
C16 C15 C17 110.5(2) . . ?
C7 C15 H15 108.3 . . ?
C16 C15 H15 108.3 . . ?
C17 C15 H15 108.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 120.1(2) . . ?
C19 C18 N2 118.97(19) . . ?
C23 C18 N2 120.91(19) . . ?
C20 C19 C18 118.2(2) . . ?
C20 C19 C27 117.8(2) . . ?
C18 C19 C27 124.01(19) . . ?
C21 C20 C19 122.1(2) . . ?
C21 C20 H20 118.9 . . ?
C19 C20 H20 118.9 . . ?
C20 C21 C22 119.1(2) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C21 C22 C23 121.7(2) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 118.5(2) . . ?
C22 C23 C24 119.5(2) . . ?
C18 C23 C24 121.57(19) . . ?
C23 C24 C25 108.19(19) . . ?
C23 C24 C26 113.93(19) . . ?
C25 C24 C26 110.8(2) . . ?
C23 C24 H24 107.9 . . ?
C25 C24 H24 107.9 . . ?
C26 C24 H24 107.9 . . ?
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 . . ?
C29 C27 C19 110.08(19) . . ?
C29 C27 C28 110.4(2) . . ?
C19 C27 C28 112.50(19) . . ?
C29 C27 H27 107.9 . . ?
C19 C27 H27 107.9 . . ?
C28 C27 H27 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C31 110.1(2) . . ?
N3 C30 C32 108.6(2) . . ?
C31 C30 C32 111.9(3) . . ?
N3 C30 C33 108.7(2) . . ?
C31 C30 C33 111.5(4) . . ?
C32 C30 C33 105.9(3) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C42 124.58(19) . . ?
C35 C34 C2 117.75(19) . . ?
C42 C34 C2 117.65(18) . . ?
C35 C34 Nb1 78.33(12) . . ?
C42 C34 Nb1 139.33(14) . . ?
C2 C34 Nb1 54.27(10) . . ?
C34 C35 N2 117.38(19) . . ?
C34 C35 C36 123.91(19) . . ?
N2 C35 C36 118.70(18) . . ?
C41 C36 C37 118.7(2) . . ?
C41 C36 C35 119.11(19) . . ?
C37 C36 C35 122.1(2) . . ?
C38 C37 C36 120.4(2) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 120.5(2) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C40 C39 C38 119.7(2) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C39 C40 C41 120.1(2) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 H40 119.9 . . ?
C40 C41 C36 120.6(2) . . ?
C40 C41 H41 119.7 . . ?
C36 C41 H41 119.7 . . ?
C43 C42 C47 116.9(2) . . ?
C43 C42 C34 123.3(2) . . ?
C47 C42 C34 119.7(2) . . ?
C44 C43 C42 121.7(2) . . ?
C44 C43 H43 119.1 . . ?
C42 C43 H43 119.1 . . ?
C43 C44 C45 120.4(2) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C46 C45 C44 118.8(2) . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C45 C46 C47 121.0(2) . . ?
C45 C46 H46 119.5 . . ?
C47 C46 H46 119.5 . . ?
C46 C47 C42 121.2(2) . . ?
C46 C47 H47 119.4 . . ?
C42 C47 H47 119.4 . . ?
C4 N1 C6 118.62(17) . . ?
C4 N1 Nb1 84.42(12) . . ?
C6 N1 Nb1 147.12(14) . . ?
C35 N2 C18 121.03(17) . . ?
C35 N2 Nb1 100.47(13) . . ?
C18 N2 Nb1 138.48(14) . . ?
C30 N3 Nb1 169.60(17) . . ?
N3 Nb1 N2 112.04(8) . . ?
N3 Nb1 N1 123.22(8) . . ?
N2 Nb1 N1 122.16(7) . . ?
N3 Nb1 C2 109.74(9) . . ?
N2 Nb1 C2 83.11(8) . . ?
N1 Nb1 C2 92.94(8) . . ?
N3 Nb1 C3 100.89(8) . . ?
N2 Nb1 C3 120.38(7) . . ?
N1 Nb1 C3 66.22(7) . . ?
C2 Nb1 C3 38.43(8) . . ?
N3 Nb1 C4 105.49(8) . . ?
N2 Nb1 C4 139.48(7) . . ?
N1 Nb1 C4 35.05(7) . . ?
C2 Nb1 C4 70.09(8) . . ?
C3 Nb1 C4 34.45(7) . . ?
N3 Nb1 C34 140.84(8) . . ?
N2 Nb1 C34 59.76(7) . . ?
N1 Nb1 C34 84.79(7) . . ?
C2 Nb1 C34 35.51(7) . . ?
C3 Nb1 C34 63.21(7) . . ?
C4 Nb1 C34 81.58(7) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.072
_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/. 
# 
# Audit and citation data items have may 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_(4)
_database_code_depnum_ccdc_archive 'CCDC 1026788'
_audit_update_record             
;
2014-09-28 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_chemical_name_common            'Complex 5'
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H60 N3 Nb'
_chemical_formula_sum            'C39 H60 N3 Nb'
_chemical_formula_weight         663.81

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc

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

_cell_length_a                   12.5601(4)
_cell_length_b                   35.9930(11)
_cell_length_c                   9.2081(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.264(2)
_cell_angle_gamma                90.00
_cell_volume                     3733.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3039
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      25.36

_exptl_crystal_description       rode
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9691
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            7266
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         25.41
_reflns_number_total             4182
_reflns_number_gt                3393
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0312P)²+1.5918P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_number_reflns         4182
_refine_ls_number_parameters     404
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.0886
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7709(5) 0.19975(19) 0.0843(8) 0.0293(16) Uani 1 1 d . . .
H1A H 0.7983 0.2175 0.0307 0.044 Uiso 1 1 calc R . .
H1B H 0.7371 0.2126 0.1454 0.044 Uiso 1 1 calc R . .
H1C H 0.7118 0.1841 0.0050 0.044 Uiso 1 1 calc R . .
C2 C 0.8753(7) 0.1759(2) 0.1983(10) 0.021(2) Uani 1 1 d . . .
C3 C 0.9084(5) 0.14488(17) 0.1239(7) 0.0212(15) Uani 1 1 d . . .
H3 H 0.8669 0.1433 0.0117 0.025 Uiso 1 1 calc R . .
C4 C 0.9935(5) 0.11739(18) 0.1976(7) 0.0210(14) Uani 1 1 d . . .
C5 C 0.9984(5) 0.08400(19) 0.0995(7) 0.0276(17) Uani 1 1 d . . .
H5A H 1.0796 0.0785 0.1252 0.041 Uiso 1 1 calc R . .
H5B H 0.9556 0.0895 -0.0139 0.041 Uiso 1 1 calc R . .
H5C H 0.9631 0.0629 0.1253 0.041 Uiso 1 1 calc R . .
C6 C 1.1688(5) 0.09613(18) 0.4343(7) 0.0189(14) Uani 1 1 d . . .
C7 C 1.1813(6) 0.06617(19) 0.5362(8) 0.0242(16) Uani 1 1 d . . .
C8 C 1.2876(5) 0.04545(19) 0.5962(9) 0.0274(17) Uani 1 1 d . . .
H8 H 1.2977 0.0255 0.6652 0.033 Uiso 1 1 calc R . .
C9 C 1.3778(6) 0.0547(2) 0.5525(9) 0.033(2) Uani 1 1 d . . .
H9 H 1.4461 0.0403 0.5881 0.040 Uiso 1 1 calc R . .
C10 C 1.3645(5) 0.08570(19) 0.4555(7) 0.0293(17) Uani 1 1 d . . .
H10 H 1.4257 0.0922 0.4294 0.035 Uiso 1 1 calc R . .
C11 C 1.2610(5) 0.10741(18) 0.3959(7) 0.0215(15) Uani 1 1 d . . .
C12 C 1.2584(5) 0.14232(19) 0.3039(8) 0.0308(17) Uani 1 1 d . . .
H12 H 1.1814 0.1543 0.2741 0.037 Uiso 1 1 calc R . .
C13 C 1.3540(6) 0.1695(2) 0.4093(9) 0.045(2) Uani 1 1 d . . .
H13A H 1.3470 0.1739 0.5075 0.067 Uiso 1 1 calc R . .
H13B H 1.3446 0.1925 0.3520 0.067 Uiso 1 1 calc R . .
H13C H 1.4308 0.1592 0.4349 0.067 Uiso 1 1 calc R . .
C14 C 1.2698(8) 0.1355(3) 0.1477(9) 0.063(2) Uani 1 1 d . . .
H14A H 1.3458 0.1247 0.1732 0.095 Uiso 1 1 calc R . .
H14B H 1.2624 0.1587 0.0924 0.095 Uiso 1 1 calc R . .
H14C H 1.2082 0.1189 0.0794 0.095 Uiso 1 1 calc R . .
C15 C 1.0854(5) 0.05417(18) 0.5831(8) 0.0277(16) Uani 1 1 d . . .
H15 H 1.0089 0.0599 0.4914 0.033 Uiso 1 1 calc R . .
C16 C 1.0854(7) 0.0125(2) 0.6191(11) 0.052(2) Uani 1 1 d . . .
H16A H 1.0889 -0.0016 0.5328 0.078 Uiso 1 1 calc R . .
H16B H 1.0142 0.0063 0.6279 0.078 Uiso 1 1 calc R . .
H16C H 1.1532 0.0067 0.7190 0.078 Uiso 1 1 calc R . .
C17 C 1.0933(7) 0.0773(2) 0.7278(9) 0.049(2) Uani 1 1 d . . .
H17A H 1.1627 0.0702 0.8234 0.073 Uiso 1 1 calc R . .
H17B H 1.0239 0.0730 0.7441 0.073 Uiso 1 1 calc R . .
H17C H 1.0981 0.1032 0.7064 0.073 Uiso 1 1 calc R . .
C18 C 0.6675(6) 0.0814(2) 0.2594(8) 0.0204(15) Uani 1 1 d . . .
C19 C 0.6566(5) 0.05159(17) 0.3513(7) 0.0231(15) Uani 1 1 d . . .
C20 C 0.5490(5) 0.03187(19) 0.2909(8) 0.0311(17) Uani 1 1 d . . .
H20 H 0.5397 0.0121 0.3490 0.037 Uiso 1 1 calc R . .
C21 C 0.4578(6) 0.0421(2) 0.1454(10) 0.037(2) Uani 1 1 d . . .
H21 H 0.3862 0.0294 0.1087 0.045 Uiso 1 1 calc R . .
C22 C 0.4677(6) 0.0699(2) 0.0529(9) 0.0401(19) Uani 1 1 d . . .
H22 H 0.4053 0.0749 -0.0479 0.048 Uiso 1 1 calc R . .
C23 C 0.5705(5) 0.09068(19) 0.1084(8) 0.0267(16) Uani 1 1 d . . .
C24 C 0.5811(5) 0.12073(19) 0.0044(8) 0.0340(18) Uani 1 1 d . . .
H24 H 0.6408 0.1385 0.0751 0.041 Uiso 1 1 calc R . .
C25 C 0.4694(7) 0.1418(2) -0.0918(12) 0.076(3) Uani 1 1 d . . .
H25A H 0.4096 0.1251 -0.1632 0.114 Uiso 1 1 calc R . .
H25B H 0.4843 0.1606 -0.1543 0.114 Uiso 1 1 calc R . .
H25C H 0.4425 0.1532 -0.0198 0.114 Uiso 1 1 calc R . .
C26 C 0.6283(7) 0.1034(2) -0.1135(9) 0.056(2) Uani 1 1 d . . .
H26A H 0.5720 0.0855 -0.1829 0.084 Uiso 1 1 calc R . .
H26B H 0.7031 0.0914 -0.0513 0.084 Uiso 1 1 calc R . .
H26C H 0.6384 0.1227 -0.1782 0.084 Uiso 1 1 calc R . .
C27 C 0.7544(5) 0.0409(2) 0.5114(8) 0.0302(17) Uani 1 1 d . . .
H27 H 0.8289 0.0497 0.5135 0.036 Uiso 1 1 calc R . .
C28 C 0.7423(8) 0.0591(2) 0.6499(9) 0.068(3) Uani 1 1 d . . .
H28A H 0.7424 0.0856 0.6382 0.102 Uiso 1 1 calc R . .
H28B H 0.8077 0.0519 0.7501 0.102 Uiso 1 1 calc R . .
H28C H 0.6692 0.0515 0.6501 0.102 Uiso 1 1 calc R . .
C29 C 0.7670(7) -0.0011(2) 0.5430(9) 0.049(2) Uani 1 1 d . . .
H29A H 0.6981 -0.0103 0.5510 0.073 Uiso 1 1 calc R . .
H29B H 0.8364 -0.0059 0.6424 0.073 Uiso 1 1 calc R . .
H29C H 0.7745 -0.0133 0.4553 0.073 Uiso 1 1 calc R . .
C30 C 0.8393(9) 0.1895(2) 0.6034(11) 0.057(3) Uani 1 1 d . . .
C31 C 0.9118(12) 0.1861(3) 0.7847(11) 0.107(5) Uani 1 1 d . . .
H31A H 0.9383 0.1609 0.8119 0.161 Uiso 1 1 calc R . .
H31B H 0.8639 0.1929 0.8377 0.161 Uiso 1 1 calc R . .
H31C H 0.9794 0.2023 0.8197 0.161 Uiso 1 1 calc R . .
C32 C 0.8016(7) 0.2300(2) 0.5529(10) 0.045(2) Uani 1 1 d . . .
H32A H 0.8710 0.2452 0.5847 0.067 Uiso 1 1 calc R . .
H32B H 0.7548 0.2387 0.6049 0.067 Uiso 1 1 calc R . .
H32C H 0.7554 0.2312 0.4375 0.067 Uiso 1 1 calc R . .
C33 C 0.7263(11) 0.1657(3) 0.5445(17) 0.129(6) Uani 1 1 d . . .
H33A H 0.6815 0.1684 0.4294 0.194 Uiso 1 1 calc R . .
H33B H 0.6791 0.1739 0.5968 0.194 Uiso 1 1 calc R . .
H33C H 0.7476 0.1401 0.5704 0.194 Uiso 1 1 calc R . .
C39 C 1.0277(6) 0.2576(2) 0.2342(9) 0.0349(18) Uani 1 1 d . . .
H39A H 0.9546 0.2584 0.1366 0.052 Uiso 1 1 calc R . .
H39B H 1.0890 0.2697 0.2165 0.052 Uiso 1 1 calc R . .
H39C H 1.0175 0.2701 0.3194 0.052 Uiso 1 1 calc R . .
C38 C 1.0622(6) 0.21746(19) 0.2820(8) 0.0269(17) Uani 1 1 d . . .
H38A H 1.1408 0.2167 0.3724 0.032 Uiso 1 1 calc R . .
H38B H 1.0657 0.2044 0.1920 0.032 Uiso 1 1 calc R . .
C34 C 0.9746(5) 0.19737(17) 0.3299(7) 0.0190(14) Uani 1 1 d . . .
C35 C 0.9839(5) 0.19822(18) 0.4801(8) 0.0253(15) Uani 1 1 d . . .
C36 C 1.0868(7) 0.2169(2) 0.6196(8) 0.0391(19) Uani 1 1 d . . .
H36A H 1.0577 0.2287 0.6897 0.047 Uiso 1 1 calc R . .
H36B H 1.1194 0.2361 0.5771 0.047 Uiso 1 1 calc R . .
C37 C 1.1852(6) 0.1894(2) 0.7189(8) 0.045(2) Uani 1 1 d . . .
H37A H 1.1568 0.1726 0.7749 0.068 Uiso 1 1 calc R . .
H37B H 1.2526 0.2028 0.7962 0.068 Uiso 1 1 calc R . .
H37C H 1.2081 0.1756 0.6480 0.068 Uiso 1 1 calc R . .
N1 N 1.0595(4) 0.11668(15) 0.3659(6) 0.0173(12) Uani 1 1 d . . .
N2 N 0.7722(4) 0.10274(15) 0.3154(6) 0.0212(12) Uani 1 1 d . . .
N3 N 0.9059(6) 0.17517(19) 0.5161(8) 0.0290(19) Uani 1 1 d . . .
Nb1 Nb 0.89935(4) 0.132698(14) 0.36724(5) 0.01728(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.528(10) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.465(10) . ?
C2 C34 1.511(10) . ?
C2 Nb1 2.125(8) . ?
C3 C4 1.392(8) . ?
C3 Nb1 2.335(6) . ?
C3 H3 0.9300 . ?
C4 N1 1.397(7) . ?
C4 C5 1.521(9) . ?
C4 Nb1 2.403(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.392(9) . ?
C6 C11 1.411(8) . ?
C6 N1 1.437(7) . ?
C7 C8 1.410(9) . ?
C7 C15 1.511(9) . ?
C8 C9 1.400(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.392(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.404(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.508(9) . ?
C12 C13 1.519(9) . ?
C12 C14 1.527(9) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C17 1.538(9) . ?
C15 C16 1.537(9) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.410(9) . ?
C18 N2 1.409(8) . ?
C18 C23 1.426(8) . ?
C19 C20 1.404(8) . ?
C19 C27 1.493(8) . ?
C20 C21 1.373(9) . ?
C20 H20 0.9300 . ?
C21 C22 1.354(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.380(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.489(9) . ?
C24 C25 1.492(9) . ?
C24 C26 1.578(10) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.500(10) . ?
C27 C29 1.533(9) . ?
C27 H27 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 N3 1.485(10) . ?
C30 C31 1.512(13) . ?
C30 C33 1.535(12) . ?
C30 C32 1.540(10) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C39 C38 1.516(9) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C38 C34 1.535(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C34 C35 1.336(8) . ?
C34 Nb1 2.592(6) . ?
C35 N3 1.430(9) . ?
C35 C36 1.517(9) . ?
C35 Nb1 2.606(6) . ?
C36 C37 1.530(9) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
N1 Nb1 2.097(5) . ?
N2 Nb1 1.807(5) . ?
N3 Nb1 2.030(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C34 117.4(6) . . ?
C3 C2 C1 116.2(6) . . ?
C34 C2 C1 114.7(7) . . ?
C3 C2 Nb1 78.8(4) . . ?
C34 C2 Nb1 89.3(4) . . ?
C1 C2 Nb1 135.6(5) . . ?
C4 C3 C2 129.0(6) . . ?
C4 C3 Nb1 75.6(4) . . ?
C2 C3 Nb1 63.2(4) . . ?
C4 C3 H3 115.5 . . ?
C2 C3 H3 115.5 . . ?
Nb1 C3 H3 144.3 . . ?
C3 C4 N1 120.3(6) . . ?
C3 C4 C5 119.7(5) . . ?
N1 C4 C5 119.0(5) . . ?
C3 C4 Nb1 70.3(4) . . ?
N1 C4 Nb1 60.3(3) . . ?
C5 C4 Nb1 136.7(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 122.1(5) . . ?
C7 C6 N1 119.7(6) . . ?
C11 C6 N1 118.2(6) . . ?
C6 C7 C8 118.6(6) . . ?
C6 C7 C15 123.2(6) . . ?
C8 C7 C15 118.2(6) . . ?
C9 C8 C7 120.4(7) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C8 119.6(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 121.6(6) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C6 117.6(6) . . ?
C10 C11 C12 118.0(5) . . ?
C6 C11 C12 124.3(6) . . ?
C11 C12 C13 111.3(5) . . ?
C11 C12 C14 114.0(6) . . ?
C13 C12 C14 109.1(6) . . ?
C11 C12 H12 107.4 . . ?
C13 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 C17 109.8(6) . . ?
C7 C15 C16 114.6(6) . . ?
C17 C15 C16 110.4(6) . . ?
C7 C15 H15 107.2 . . ?
C17 C15 H15 107.2 . . ?
C16 C15 H15 107.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N2 121.2(6) . . ?
C19 C18 C23 119.7(6) . . ?
N2 C18 C23 119.1(6) . . ?
C20 C19 C18 118.6(6) . . ?
C20 C19 C27 119.2(6) . . ?
C18 C19 C27 122.2(6) . . ?
C21 C20 C19 119.5(7) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C22 C21 C20 122.9(7) . . ?
C22 C21 H21 118.6 . . ?
C20 C21 H21 118.6 . . ?
C21 C22 C23 119.9(7) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C18 119.3(6) . . ?
C22 C23 C24 119.5(6) . . ?
C18 C23 C24 121.1(6) . . ?
C23 C24 C25 115.0(6) . . ?
C23 C24 C26 108.8(6) . . ?
C25 C24 C26 109.4(7) . . ?
C23 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 . . ?
C19 C27 C28 112.2(6) . . ?
C19 C27 C29 114.4(6) . . ?
C28 C27 C29 108.1(6) . . ?
C19 C27 H27 107.3 . . ?
C28 C27 H27 107.3 . . ?
C29 C27 H27 107.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C31 111.2(8) . . ?
N3 C30 C33 105.7(7) . . ?
C31 C30 C33 110.9(9) . . ?
N3 C30 C32 109.6(6) . . ?
C31 C30 C32 111.3(7) . . ?
C33 C30 C32 107.9(8) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C39 C38 C34 112.5(5) . . ?
C39 C38 H38A 109.1 . . ?
C34 C38 H38A 109.1 . . ?
C39 C38 H38B 109.1 . . ?
C34 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
C35 C34 C2 120.3(6) . . ?
C35 C34 C38 122.8(6) . . ?
C2 C34 C38 116.9(5) . . ?
C35 C34 Nb1 75.7(4) . . ?
C2 C34 Nb1 55.1(4) . . ?
C38 C34 Nb1 144.2(4) . . ?
C34 C35 N3 118.2(6) . . ?
C34 C35 C36 122.6(6) . . ?
N3 C35 C36 118.3(6) . . ?
C34 C35 Nb1 74.5(4) . . ?
N3 C35 Nb1 50.8(3) . . ?
C36 C35 Nb1 141.4(4) . . ?
C35 C36 C37 112.4(6) . . ?
C35 C36 H36A 109.1 . . ?
C37 C36 H36A 109.1 . . ?
C35 C36 H36B 109.1 . . ?
C37 C36 H36B 109.1 . . ?
H36A C36 H36B 107.9 . . ?
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 . . ?
C4 N1 C6 118.6(5) . . ?
C4 N1 Nb1 84.4(3) . . ?
C6 N1 Nb1 150.7(4) . . ?
C18 N2 Nb1 174.0(5) . . ?
C35 N3 C30 122.2(7) . . ?
C35 N3 Nb1 96.2(4) . . ?
C30 N3 Nb1 139.6(6) . . ?
N2 Nb1 N3 113.2(3) . . ?
N2 Nb1 N1 124.9(2) . . ?
N3 Nb1 N1 117.3(2) . . ?
N2 Nb1 C2 114.9(3) . . ?
N3 Nb1 C2 83.8(2) . . ?
N1 Nb1 C2 91.3(3) . . ?
N2 Nb1 C3 105.7(2) . . ?
N3 Nb1 C3 120.1(2) . . ?
N1 Nb1 C3 65.91(19) . . ?
C2 Nb1 C3 38.0(3) . . ?
N2 Nb1 C4 108.8(2) . . ?
N3 Nb1 C4 136.6(2) . . ?
N1 Nb1 C4 35.36(18) . . ?
C2 Nb1 C4 69.1(3) . . ?
C3 Nb1 C4 34.14(19) . . ?
N2 Nb1 C34 146.4(2) . . ?
N3 Nb1 C34 60.4(2) . . ?
N1 Nb1 C34 80.74(19) . . ?
C2 Nb1 C34 35.6(2) . . ?
C3 Nb1 C34 61.9(2) . . ?
C4 Nb1 C34 78.8(2) . . ?
N2 Nb1 C35 143.3(2) . . ?
N3 Nb1 C35 33.1(2) . . ?
N1 Nb1 C35 91.6(2) . . ?
C2 Nb1 C35 62.0(3) . . ?
C3 Nb1 C35 91.6(2) . . ?
C4 Nb1 C35 103.6(2) . . ?
C34 Nb1 C35 29.78(18) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.083
_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/. 
# 
# Audit and citation data items have may 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_(5)
_database_code_depnum_ccdc_archive 'CCDC 1026789'
_audit_update_record             
;
2014-09-28 deposited with the CCDC.
2014-11-28 downloaded from the CCDC.
;
_chemical_name_common            'Complex 6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H60 N3 Nb'
_chemical_formula_sum            'C40 H60 N3 Nb'
_chemical_formula_weight         675.82

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   34.020(3)
_cell_length_b                   13.2760(13)
_cell_length_c                   16.2477(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.893(5)
_cell_angle_gamma                90.00
_cell_volume                     7285.2(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9930
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      25.41

_exptl_crystal_description       rode
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2896
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9479
_exptl_absorpt_correction_T_max  0.9822
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            48813
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.21
_diffrn_reflns_theta_max         25.45
_reflns_number_total             6702
_reflns_number_gt                5523
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0239P)²+13.4705P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6702
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0638
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.11939(7) 0.18247(17) -0.05760(13) 0.0173(5) Uani 1 1 d . . .
H1A H 0.1012 0.2092 -0.1038 0.026 Uiso 1 1 calc R . .
H1B H 0.1164 0.1091 -0.0550 0.026 Uiso 1 1 calc R . .
H1C H 0.1467 0.1991 -0.0659 0.026 Uiso 1 1 calc R . .
C2 C 0.10980(6) 0.22895(16) 0.02302(13) 0.0130(5) Uani 1 1 d . . .
C3 C 0.12845(6) 0.32717(16) 0.04098(13) 0.0122(4) Uani 1 1 d . . .
H3 H 0.1394 0.3569 -0.0044 0.015 Uiso 1 1 calc R . .
C4 C 0.13295(6) 0.38471(16) 0.11360(13) 0.0116(4) Uani 1 1 d . . .
C5 C 0.16078(6) 0.47409(16) 0.11847(13) 0.0143(5) Uani 1 1 d . . .
H5A H 0.1620 0.5050 0.1735 0.021 Uiso 1 1 calc R . .
H5B H 0.1511 0.5236 0.0761 0.021 Uiso 1 1 calc R . .
H5C H 0.1873 0.4515 0.1090 0.021 Uiso 1 1 calc R . .
C6 C 0.10719(6) 0.41307(15) 0.24795(13) 0.0103(4) Uani 1 1 d . . .
C7 C 0.11578(6) 0.38188(16) 0.33138(13) 0.0116(4) Uani 1 1 d . . .
C8 C 0.10258(6) 0.44043(17) 0.39401(13) 0.0151(5) Uani 1 1 d . . .
H8 H 0.1081 0.4190 0.4500 0.018 Uiso 1 1 calc R . .
C9 C 0.08174(6) 0.52865(17) 0.37677(14) 0.0165(5) Uani 1 1 d . . .
H9 H 0.0732 0.5678 0.4202 0.020 Uiso 1 1 calc R . .
C10 C 0.07352(6) 0.55897(17) 0.29519(14) 0.0157(5) Uani 1 1 d . . .
H10 H 0.0595 0.6202 0.2834 0.019 Uiso 1 1 calc R . .
C11 C 0.08506(6) 0.50273(16) 0.22943(13) 0.0124(5) Uani 1 1 d . . .
C12 C 0.07057(6) 0.54069(16) 0.14220(13) 0.0144(5) Uani 1 1 d . . .
H12 H 0.0812 0.4947 0.1014 0.017 Uiso 1 1 calc R . .
C13 C 0.08551(7) 0.64783(17) 0.12765(14) 0.0201(5) Uani 1 1 d . . .
H13A H 0.0734 0.6953 0.1634 0.030 Uiso 1 1 calc R . .
H13B H 0.0782 0.6666 0.0695 0.030 Uiso 1 1 calc R . .
H13C H 0.1144 0.6499 0.1408 0.030 Uiso 1 1 calc R . .
C14 C 0.02514(6) 0.53808(18) 0.12649(14) 0.0194(5) Uani 1 1 d . . .
H14A H 0.0157 0.4704 0.1382 0.029 Uiso 1 1 calc R . .
H14B H 0.0165 0.5553 0.0685 0.029 Uiso 1 1 calc R . .
H14C H 0.0142 0.5869 0.1628 0.029 Uiso 1 1 calc R . .
C15 C 0.13826(6) 0.28552(16) 0.35732(13) 0.0133(4) Uani 1 1 d . . .
H15 H 0.1523 0.2632 0.3098 0.016 Uiso 1 1 calc R . .
C16 C 0.16936(6) 0.30057(17) 0.43248(13) 0.0174(5) Uani 1 1 d . . .
H16A H 0.1857 0.3595 0.4234 0.026 Uiso 1 1 calc R . .
H16B H 0.1862 0.2407 0.4401 0.026 Uiso 1 1 calc R . .
H16C H 0.1561 0.3112 0.4821 0.026 Uiso 1 1 calc R . .
C17 C 0.10970(7) 0.20169(17) 0.37530(14) 0.0193(5) Uani 1 1 d . . .
H17A H 0.0943 0.2234 0.4194 0.029 Uiso 1 1 calc R . .
H17B H 0.1248 0.1409 0.3930 0.029 Uiso 1 1 calc R . .
H17C H 0.0917 0.1870 0.3250 0.029 Uiso 1 1 calc R . .
C18 C 0.23082(6) 0.15209(15) 0.15265(13) 0.0105(4) Uani 1 1 d . . .
C19 C 0.25820(6) 0.18059(15) 0.22145(13) 0.0121(5) Uani 1 1 d . . .
C20 C 0.29801(6) 0.15752(16) 0.22001(13) 0.0149(5) Uani 1 1 d . . .
H20 H 0.3166 0.1772 0.2655 0.018 Uiso 1 1 calc R . .
C21 C 0.31128(6) 0.10659(17) 0.15402(14) 0.0162(5) Uani 1 1 d . . .
H21 H 0.3386 0.0914 0.1544 0.019 Uiso 1 1 calc R . .
C22 C 0.28416(6) 0.07829(16) 0.08762(13) 0.0149(5) Uani 1 1 d . . .
H22 H 0.2932 0.0429 0.0426 0.018 Uiso 1 1 calc R . .
C23 C 0.24396(6) 0.10025(15) 0.08498(13) 0.0121(5) Uani 1 1 d . . .
C24 C 0.21575(6) 0.07212(16) 0.00847(13) 0.0136(5) Uani 1 1 d . . .
H24 H 0.1882 0.0885 0.0200 0.016 Uiso 1 1 calc R . .
C25 C 0.21714(8) -0.03979(18) -0.01121(16) 0.0285(6) Uani 1 1 d . . .
H25A H 0.2437 -0.0577 -0.0238 0.043 Uiso 1 1 calc R . .
H25B H 0.1978 -0.0550 -0.0592 0.043 Uiso 1 1 calc R . .
H25C H 0.2108 -0.0788 0.0367 0.043 Uiso 1 1 calc R . .
C26 C 0.22450(7) 0.13495(18) -0.06600(14) 0.0209(5) Uani 1 1 d . . .
H26A H 0.2212 0.2066 -0.0539 0.031 Uiso 1 1 calc R . .
H26B H 0.2061 0.1160 -0.1147 0.031 Uiso 1 1 calc R . .
H26C H 0.2518 0.1226 -0.0771 0.031 Uiso 1 1 calc R . .
C27 C 0.24424(6) 0.23675(16) 0.29379(13) 0.0128(5) Uani 1 1 d . . .
H27 H 0.2181 0.2076 0.3037 0.015 Uiso 1 1 calc R . .
C28 C 0.27239(7) 0.22586(17) 0.37421(13) 0.0185(5) Uani 1 1 d . . .
H28A H 0.2789 0.1546 0.3838 0.028 Uiso 1 1 calc R . .
H28B H 0.2596 0.2520 0.4207 0.028 Uiso 1 1 calc R . .
H28C H 0.2967 0.2640 0.3696 0.028 Uiso 1 1 calc R . .
C29 C 0.23767(7) 0.34822(17) 0.27237(14) 0.0200(5) Uani 1 1 d . . .
H29A H 0.2629 0.3792 0.2633 0.030 Uiso 1 1 calc R . .
H29B H 0.2270 0.3825 0.3182 0.030 Uiso 1 1 calc R . .
H29C H 0.2189 0.3544 0.2219 0.030 Uiso 1 1 calc R . .
C30 C 0.11205(6) -0.01621(16) 0.17913(14) 0.0162(5) Uani 1 1 d . . .
C31 C 0.14877(7) -0.01747(18) 0.24341(16) 0.0251(6) Uani 1 1 d . . .
H31A H 0.1714 0.0097 0.2186 0.038 Uiso 1 1 calc R . .
H31B H 0.1545 -0.0868 0.2617 0.038 Uiso 1 1 calc R . .
H31C H 0.1439 0.0239 0.2911 0.038 Uiso 1 1 calc R . .
C32 C 0.12092(7) -0.07756(18) 0.10341(15) 0.0236(6) Uani 1 1 d . . .
H32A H 0.0970 -0.0814 0.0633 0.035 Uiso 1 1 calc R . .
H32B H 0.1292 -0.1457 0.1210 0.035 Uiso 1 1 calc R . .
H32C H 0.1422 -0.0448 0.0776 0.035 Uiso 1 1 calc R . .
C33 C 0.07795(7) -0.06548(18) 0.21815(15) 0.0230(5) Uani 1 1 d . . .
H33A H 0.0716 -0.0246 0.2650 0.035 Uiso 1 1 calc R . .
H33B H 0.0859 -0.1331 0.2378 0.035 Uiso 1 1 calc R . .
H33C H 0.0546 -0.0702 0.1766 0.035 Uiso 1 1 calc R . .
C34 C 0.06705(6) 0.19832(16) 0.03989(13) 0.0140(5) Uani 1 1 d . . .
H34 H 0.0538 0.1748 -0.0150 0.017 Uiso 1 1 calc R . .
C35 C 0.06501(6) 0.10466(16) 0.09968(13) 0.0140(5) Uani 1 1 d . . .
H35 H 0.0592 0.0425 0.0657 0.017 Uiso 1 1 calc R . .
C36 C 0.02847(6) 0.13208(17) 0.14312(14) 0.0178(5) Uani 1 1 d . . .
H36 H 0.0249 0.0897 0.1925 0.021 Uiso 1 1 calc R . .
C37 C -0.00798(7) 0.13499(18) 0.07594(16) 0.0247(6) Uani 1 1 d . . .
H37A H -0.0330 0.1311 0.1014 0.030 Uiso 1 1 calc R . .
H37B H -0.0072 0.0788 0.0361 0.030 Uiso 1 1 calc R . .
C38 C -0.00406(7) 0.23850(18) 0.03261(15) 0.0229(5) Uani 1 1 d . . .
H38A H -0.0054 0.2308 -0.0283 0.027 Uiso 1 1 calc R . .
H38B H -0.0249 0.2860 0.0455 0.027 Uiso 1 1 calc R . .
C39 C 0.03749(6) 0.27373(17) 0.07116(13) 0.0158(5) Uani 1 1 d . . .
H39 H 0.0435 0.3464 0.0621 0.019 Uiso 1 1 calc R . .
C40 C 0.03505(6) 0.24404(17) 0.16194(14) 0.0169(5) Uani 1 1 d . . .
H40A H 0.0600 0.2573 0.1984 0.020 Uiso 1 1 calc R . .
H40B H 0.0124 0.2758 0.1850 0.020 Uiso 1 1 calc R . .
N1 N 0.11817(5) 0.34969(13) 0.18411(10) 0.0101(4) Uani 1 1 d . . .
N2 N 0.19045(5) 0.17447(13) 0.15031(10) 0.0113(4) Uani 1 1 d . . .
N3 N 0.10284(5) 0.09069(13) 0.15480(11) 0.0125(4) Uani 1 1 d . . .
Nb1 Nb 0.139283(5) 0.209229(14) 0.148113(11) 0.00890(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 1.518(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.464(3) . ?
C2 C34 1.566(3) . ?
C2 Nb1 2.172(2) . ?
C3 C4 1.399(3) . ?
C3 Nb1 2.337(2) . ?
C3 H3 0.9500 . ?
C4 N1 1.385(3) . ?
C4 C5 1.514(3) . ?
C4 Nb1 2.400(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.414(3) . ?
C6 N1 1.420(3) . ?
C6 C11 1.421(3) . ?
C7 C8 1.397(3) . ?
C7 C15 1.524(3) . ?
C8 C9 1.380(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.398(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.529(3) . ?
C12 C14 1.536(3) . ?
C12 C13 1.538(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.528(3) . ?
C15 C16 1.530(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N2 1.401(3) . ?
C18 C23 1.414(3) . ?
C18 C19 1.418(3) . ?
C19 C20 1.391(3) . ?
C19 C27 1.516(3) . ?
C20 C21 1.388(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.385(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.394(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.523(3) . ?
C24 C25 1.522(3) . ?
C24 C26 1.528(3) . ?
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 C29 1.531(3) . ?
C27 C28 1.531(3) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.496(3) . ?
C30 C31 1.529(3) . ?
C30 C33 1.534(3) . ?
C30 C32 1.535(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C39 1.547(3) . ?
C34 C35 1.585(3) . ?
C34 H34 1.0000 . ?
C35 N3 1.489(3) . ?
C35 C36 1.545(3) . ?
C35 H35 1.0000 . ?
C36 C40 1.529(3) . ?
C36 C37 1.551(3) . ?
C36 H36 1.0000 . ?
C37 C38 1.557(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.548(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.539(3) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
N1 Nb1 2.1061(17) . ?
N2 Nb1 1.7970(17) . ?
N3 Nb1 2.0143(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 113.64(18) . . ?
C3 C2 C34 125.87(18) . . ?
C1 C2 C34 110.23(17) . . ?
C3 C2 Nb1 77.31(12) . . ?
C1 C2 Nb1 129.45(15) . . ?
C34 C2 Nb1 98.01(13) . . ?
C4 C3 C2 131.0(2) . . ?
C4 C3 Nb1 75.29(12) . . ?
C2 C3 Nb1 65.02(11) . . ?
C4 C3 H3 114.5 . . ?
C2 C3 H3 114.5 . . ?
Nb1 C3 H3 144.6 . . ?
N1 C4 C3 120.03(19) . . ?
N1 C4 C5 120.43(18) . . ?
C3 C4 C5 118.46(19) . . ?
N1 C4 Nb1 60.81(10) . . ?
C3 C4 Nb1 70.40(12) . . ?
C5 C4 Nb1 135.28(14) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 118.97(18) . . ?
C7 C6 C11 119.45(19) . . ?
N1 C6 C11 121.38(18) . . ?
C8 C7 C6 119.19(19) . . ?
C8 C7 C15 117.41(19) . . ?
C6 C7 C15 123.39(18) . . ?
C9 C8 C7 121.8(2) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 118.8(2) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C9 C10 C11 122.3(2) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C10 C11 C6 118.41(19) . . ?
C10 C11 C12 116.33(19) . . ?
C6 C11 C12 125.17(19) . . ?
C11 C12 C14 110.64(18) . . ?
C11 C12 C13 111.81(18) . . ?
C14 C12 C13 109.86(18) . . ?
C11 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C13 C12 H12 108.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C15 C17 110.79(17) . . ?
C7 C15 C16 112.77(17) . . ?
C17 C15 C16 109.71(17) . . ?
C7 C15 H15 107.8 . . ?
C17 C15 H15 107.8 . . ?
C16 C15 H15 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C23 118.84(18) . . ?
N2 C18 C19 120.93(18) . . ?
C23 C18 C19 120.23(19) . . ?
C20 C19 C18 118.47(19) . . ?
C20 C19 C27 121.17(19) . . ?
C18 C19 C27 120.34(18) . . ?
C21 C20 C19 121.8(2) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C22 C21 C20 119.1(2) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C21 C22 C23 121.8(2) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 118.58(19) . . ?
C22 C23 C24 119.58(19) . . ?
C18 C23 C24 121.78(18) . . ?
C25 C24 C23 112.23(18) . . ?
C25 C24 C26 110.65(19) . . ?
C23 C24 C26 110.42(18) . . ?
C25 C24 H24 107.8 . . ?
C23 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 . . ?
C19 C27 C29 110.49(18) . . ?
C19 C27 C28 113.15(18) . . ?
C29 C27 C28 110.15(18) . . ?
C19 C27 H27 107.6 . . ?
C29 C27 H27 107.6 . . ?
C28 C27 H27 107.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C31 108.58(17) . . ?
N3 C30 C33 111.66(18) . . ?
C31 C30 C33 108.03(19) . . ?
N3 C30 C32 110.28(18) . . ?
C31 C30 C32 108.56(19) . . ?
C33 C30 C32 109.64(19) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C39 C34 C2 122.91(18) . . ?
C39 C34 C35 103.21(17) . . ?
C2 C34 C35 114.90(17) . . ?
C39 C34 H34 104.7 . . ?
C2 C34 H34 104.7 . . ?
C35 C34 H34 104.7 . . ?
N3 C35 C36 116.07(17) . . ?
N3 C35 C34 111.61(16) . . ?
C36 C35 C34 101.07(16) . . ?
N3 C35 H35 109.2 . . ?
C36 C35 H35 109.2 . . ?
C34 C35 H35 109.2 . . ?
C40 C36 C35 102.35(17) . . ?
C40 C36 C37 101.66(18) . . ?
C35 C36 C37 107.67(18) . . ?
C40 C36 H36 114.6 . . ?
C35 C36 H36 114.6 . . ?
C37 C36 H36 114.6 . . ?
C36 C37 C38 103.62(18) . . ?
C36 C37 H37A 111.0 . . ?
C38 C37 H37A 111.0 . . ?
C36 C37 H37B 111.0 . . ?
C38 C37 H37B 111.0 . . ?
H37A C37 H37B 109.0 . . ?
C39 C38 C37 101.97(17) . . ?
C39 C38 H38A 111.4 . . ?
C37 C38 H38A 111.4 . . ?
C39 C38 H38B 111.4 . . ?
C37 C38 H38B 111.4 . . ?
H38A C38 H38B 109.2 . . ?
C40 C39 C34 105.13(17) . . ?
C40 C39 C38 99.13(18) . . ?
C34 C39 C38 105.63(18) . . ?
C40 C39 H39 115.1 . . ?
C34 C39 H39 115.1 . . ?
C38 C39 H39 115.1 . . ?
C36 C40 C39 94.63(17) . . ?
C36 C40 H40A 112.8 . . ?
C39 C40 H40A 112.8 . . ?
C36 C40 H40B 112.8 . . ?
C39 C40 H40B 112.8 . . ?
H40A C40 H40B 110.3 . . ?
C4 N1 C6 123.95(17) . . ?
C4 N1 Nb1 84.14(12) . . ?
C6 N1 Nb1 148.85(14) . . ?
C18 N2 Nb1 177.33(15) . . ?
C35 N3 C30 114.55(16) . . ?
C35 N3 Nb1 111.31(13) . . ?
C30 N3 Nb1 130.14(13) . . ?
N2 Nb1 N3 113.53(7) . . ?
N2 Nb1 N1 125.71(7) . . ?
N3 Nb1 N1 116.37(7) . . ?
N2 Nb1 C2 112.77(8) . . ?
N3 Nb1 C2 85.79(8) . . ?
N1 Nb1 C2 91.06(7) . . ?
N2 Nb1 C3 104.63(8) . . ?
N3 Nb1 C3 121.37(7) . . ?
N1 Nb1 C3 65.49(7) . . ?
C2 Nb1 C3 37.67(7) . . ?
N2 Nb1 C4 108.27(7) . . ?
N3 Nb1 C4 137.10(7) . . ?
N1 Nb1 C4 35.05(7) . . ?
C2 Nb1 C4 69.26(7) . . ?
C3 Nb1 C4 34.31(7) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.063
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
