# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_(1)
_database_code_depnum_ccdc_archive 'CCDC 1403876'
_audit_update_record             
;
2015-05-29 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;
_chemical_name_common            'Complex 3a'
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H64 F N4 Nb'
_chemical_formula_sum            'C44 H64 F N4 Nb'
_chemical_formula_weight         760.90

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   13.0787(4)
_cell_length_b                   16.7557(5)
_cell_length_c                   18.7826(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4116.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    80(2)
_cell_measurement_reflns_used    9663
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      25.38

_exptl_crystal_description       rode
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9520
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      80(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            53723
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.39
_reflns_number_total             7563
_reflns_number_gt                7253
_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)+(0.0279P)²+1.4829P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_number_reflns         7563
_refine_ls_number_parameters     499
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0565
_refine_ls_wR_factor_gt          0.0552
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.58130(15) 0.15293(11) 0.98980(11) 0.0182(4) Uani 1 1 d . A .
C2 C 0.5973(2) 0.23420(13) 0.96134(11) 0.0274(5) Uani 1 1 d . . .
C3 C 0.5123(2) 0.27361(13) 0.93261(11) 0.0313(6) Uani 1 1 d . . .
H3 H 0.4480 0.2472 0.9309 0.038 Uiso 1 1 calc R . .
C4 C 0.5209(3) 0.35068(14) 0.90667(13) 0.0482(8) Uani 1 1 d . . .
H4 H 0.4626 0.3774 0.8882 0.058 Uiso 1 1 calc R . .
C5 C 0.6140(3) 0.38836(17) 0.90777(14) 0.0646(11) Uani 1 1 d . . .
H5 H 0.6200 0.4411 0.8896 0.078 Uiso 1 1 calc R . .
C6 C 0.6989(3) 0.3506(2) 0.93495(15) 0.0667(12) Uani 1 1 d . . .
H6 H 0.7630 0.3774 0.9356 0.080 Uiso 1 1 calc R . .
C7 C 0.6911(2) 0.27255(16) 0.96167(13) 0.0451(7) Uani 1 1 d . . .
H7 H 0.7499 0.2462 0.9799 0.054 Uiso 1 1 calc R . .
C8 C 0.58609(17) 0.16856(12) 1.12435(11) 0.0199(5) Uani 1 1 d . . .
C9 C 0.5381(3) 0.25122(13) 1.12321(12) 0.0422(7) Uani 1 1 d . . .
H9A H 0.5759 0.2854 1.0900 0.063 Uiso 1 1 calc R . .
H9B H 0.5409 0.2744 1.1711 0.063 Uiso 1 1 calc R . .
H9C H 0.4667 0.2471 1.1078 0.063 Uiso 1 1 calc R . .
C10 C 0.7000(2) 0.17152(19) 1.14181(13) 0.0437(7) Uani 1 1 d . . .
H10A H 0.7281 0.1173 1.1412 0.066 Uiso 1 1 calc R . .
H10B H 0.7096 0.1950 1.1891 0.066 Uiso 1 1 calc R . .
H10C H 0.7354 0.2042 1.1063 0.066 Uiso 1 1 calc R . .
C11 C 0.5298(2) 0.11682(13) 1.17806(11) 0.0277(5) Uani 1 1 d . . .
H11A H 0.4569 0.1155 1.1662 0.042 Uiso 1 1 calc R . .
H11B H 0.5388 0.1391 1.2259 0.042 Uiso 1 1 calc R . .
H11C H 0.5576 0.0625 1.1767 0.042 Uiso 1 1 calc R . .
C12 C 0.65659(18) -0.06277(15) 0.78196(12) 0.0303(5) Uani 1 1 d . . .
H12A H 0.6548 -0.0126 0.7552 0.045 Uiso 1 1 calc R . .
H12B H 0.6274 -0.1057 0.7529 0.045 Uiso 1 1 calc R . .
H12C H 0.7275 -0.0759 0.7940 0.045 Uiso 1 1 calc R . .
C13 C 0.59461(16) -0.05376(13) 0.84991(11) 0.0191(5) Uani 1 1 d . . .
C14 C 0.54823(17) -0.12384(12) 0.87379(10) 0.0205(4) Uani 1 1 d . . .
H14 H 0.5770 -0.1722 0.8566 0.025 Uiso 1 1 calc R . .
C15 C 0.46473(17) -0.13200(11) 0.91984(10) 0.0178(4) Uani 1 1 d . . .
C16 C 0.41033(19) -0.21108(13) 0.91678(12) 0.0276(5) Uani 1 1 d . . .
H16A H 0.3895 -0.2268 0.9649 0.041 Uiso 1 1 calc R . .
H16B H 0.4564 -0.2516 0.8971 0.041 Uiso 1 1 calc R . .
H16C H 0.3497 -0.2063 0.8864 0.041 Uiso 1 1 calc R . .
C17 C 0.62987(17) 0.08552(14) 0.84544(11) 0.0218(5) Uani 1 1 d . . .
C18 C 0.56711(17) 0.13588(13) 0.80539(11) 0.0237(5) Uani 1 1 d . . .
C19 C 0.6102(2) 0.20299(15) 0.77285(12) 0.0347(6) Uani 1 1 d . . .
H19 H 0.5680 0.2385 0.7465 0.042 Uiso 1 1 calc R . .
C20 C 0.7140(2) 0.2180(2) 0.77876(14) 0.0543(9) Uani 1 1 d . . .
H20 H 0.7428 0.2639 0.7569 0.065 Uiso 1 1 calc R . .
C21 C 0.7748(2) 0.1664(2) 0.81625(13) 0.0543(9) Uani 1 1 d . . .
H21 H 0.8462 0.1767 0.8189 0.065 Uiso 1 1 calc R . .
C22 C 0.73548(18) 0.09945(17) 0.85058(12) 0.0338(6) Uani 1 1 d . . .
C23 C 0.45384(18) 0.11922(12) 0.79602(11) 0.0212(4) Uani 1 1 d . . .
H23 H 0.4265 0.1007 0.8429 0.025 Uiso 1 1 calc R . .
C24 C 0.3919(2) 0.19220(13) 0.77341(13) 0.0311(6) Uani 1 1 d . . .
H24A H 0.4069 0.2368 0.8055 0.047 Uiso 1 1 calc R . .
H24B H 0.3188 0.1796 0.7757 0.047 Uiso 1 1 calc R . .
H24C H 0.4102 0.2070 0.7246 0.047 Uiso 1 1 calc R . .
C25 C 0.43568(17) 0.05239(13) 0.74166(12) 0.0261(5) Uani 1 1 d . . .
H25A H 0.4702 0.0657 0.6969 0.039 Uiso 1 1 calc R . .
H25B H 0.3621 0.0466 0.7331 0.039 Uiso 1 1 calc R . .
H25C H 0.4631 0.0021 0.7603 0.039 Uiso 1 1 calc R . .
C26 C 0.80769(18) 0.04552(19) 0.89168(12) 0.0397(7) Uani 1 1 d . . .
H26 H 0.7686 -0.0024 0.9079 0.048 Uiso 1 1 calc R . .
C27 C 0.8506(2) 0.08803(18) 0.95743(14) 0.0463(8) Uani 1 1 d . . .
H27A H 0.8829 0.1383 0.9430 0.069 Uiso 1 1 calc R . .
H27B H 0.9016 0.0538 0.9805 0.069 Uiso 1 1 calc R . .
H27C H 0.7950 0.0992 0.9909 0.069 Uiso 1 1 calc R . .
C28 C 0.8971(2) 0.0173(3) 0.84508(14) 0.0735(12) Uani 1 1 d . . .
H28A H 0.8709 -0.0009 0.7990 0.110 Uiso 1 1 calc R . .
H28B H 0.9325 -0.0268 0.8688 0.110 Uiso 1 1 calc R . .
H28C H 0.9449 0.0615 0.8377 0.110 Uiso 1 1 calc R . .
C29 C 0.32857(14) -0.08514(11) 0.99001(11) 0.0177(4) Uani 1 1 d . . .
C30 C 0.24431(16) -0.06427(12) 0.94796(12) 0.0214(5) Uani 1 1 d . . .
C31 C 0.14574(17) -0.07903(14) 0.97373(13) 0.0283(5) Uani 1 1 d . . .
H31 H 0.0883 -0.0648 0.9455 0.034 Uiso 1 1 calc R . .
C32 C 0.13042(19) -0.11377(14) 1.03909(15) 0.0331(6) Uani 1 1 d . . .
H32 H 0.0631 -0.1244 1.0554 0.040 Uiso 1 1 calc R . .
C33 C 0.21342(19) -0.13303(14) 1.08072(13) 0.0298(6) Uani 1 1 d . . .
H33 H 0.2026 -0.1567 1.1261 0.036 Uiso 1 1 calc R . .
C34 C 0.31297(17) -0.11859(13) 1.05782(12) 0.0235(5) Uani 1 1 d . . .
C35 C 0.4007(2) -0.13939(15) 1.10771(12) 0.0329(6) Uani 1 1 d . . .
H35 H 0.4660 -0.1244 1.0835 0.039 Uiso 1 1 calc R . .
C36 C 0.4057(2) -0.22874(17) 1.12502(15) 0.0452(7) Uani 1 1 d . . .
H36A H 0.3444 -0.2443 1.1516 0.068 Uiso 1 1 calc R . .
H36B H 0.4666 -0.2396 1.1539 0.068 Uiso 1 1 calc R . .
H36C H 0.4093 -0.2594 1.0806 0.068 Uiso 1 1 calc R . .
C37 C 0.3933(2) -0.09095(19) 1.17652(13) 0.0527(9) Uani 1 1 d . . .
H37A H 0.3862 -0.0342 1.1649 0.079 Uiso 1 1 calc R . .
H37B H 0.4554 -0.0990 1.2048 0.079 Uiso 1 1 calc R . .
H37C H 0.3337 -0.1086 1.2039 0.079 Uiso 1 1 calc R . .
C38 C 0.25521(16) -0.02451(14) 0.87567(11) 0.0233(4) Uani 1 1 d . . .
H38 H 0.3297 -0.0217 0.8638 0.028 Uiso 1 1 calc R . .
C39 C 0.21353(19) 0.06055(14) 0.87853(14) 0.0321(6) Uani 1 1 d . . .
H39A H 0.1411 0.0592 0.8917 0.048 Uiso 1 1 calc R . .
H39B H 0.2210 0.0857 0.8317 0.048 Uiso 1 1 calc R . .
H39C H 0.2518 0.0913 0.9140 0.048 Uiso 1 1 calc R . .
C40 C 0.2015(2) -0.07167(16) 0.81706(13) 0.0404(6) Uani 1 1 d . . .
H40A H 0.2218 -0.1279 0.8199 0.061 Uiso 1 1 calc R . .
H40B H 0.2208 -0.0501 0.7705 0.061 Uiso 1 1 calc R . .
H40C H 0.1272 -0.0674 0.8232 0.061 Uiso 1 1 calc R . .
C41 C 0.7022(2) -0.09397(15) 1.06333(13) 0.0342(6) Uani 1 1 d . . .
N1 N 0.57649(12) 0.12929(10) 1.05313(9) 0.0149(4) Uani 1 1 d . A .
N2 N 0.58552(12) 0.01702(10) 0.88184(8) 0.0163(3) Uani 1 1 d . A .
N3 N 0.43086(12) -0.07362(10) 0.96189(9) 0.0154(4) Uani 1 1 d . A .
N4 N 0.63298(12) -0.03838(10) 1.02774(8) 0.0184(4) Uani 1 1 d . A .
F1 F 0.40957(9) 0.04448(7) 1.04914(7) 0.0278(3) Uani 1 1 d . A .
Nb1 Nb 0.535703(12) 0.024792(9) 0.994686(8) 0.01216(5) Uani 1 1 d . . .
C43A C 0.6651(3) -0.1825(2) 1.0390(3) 0.0311(11) Uani 0.576(4) 1 d P A 1
H43A H 0.7020 -0.2229 1.0666 0.047 Uiso 0.576(4) 1 calc PR A 1
H43B H 0.6795 -0.1900 0.9882 0.047 Uiso 0.576(4) 1 calc PR A 1
H43C H 0.5915 -0.1880 1.0474 0.047 Uiso 0.576(4) 1 calc PR A 1
C44A C 0.6720(3) -0.0927(3) 1.1459(2) 0.0321(11) Uani 0.576(4) 1 d P A 1
H44A H 0.5987 -0.1035 1.1510 0.048 Uiso 0.576(4) 1 calc PR A 1
H44B H 0.6877 -0.0401 1.1660 0.048 Uiso 0.576(4) 1 calc PR A 1
H44C H 0.7111 -0.1337 1.1713 0.048 Uiso 0.576(4) 1 calc PR A 1
C42A C 0.8069(3) -0.0834(3) 1.0523(3) 0.0310(11) Uani 0.576(4) 1 d P A 1
H42A H 0.8451 -0.1224 1.0807 0.046 Uiso 0.576(4) 1 calc PR A 1
H42B H 0.8266 -0.0293 1.0666 0.046 Uiso 0.576(4) 1 calc PR A 1
H42C H 0.8227 -0.0911 1.0017 0.046 Uiso 0.576(4) 1 calc PR A 1
C42B C 0.7947(4) -0.1103(3) 1.0031(3) 0.0292(13) Uani 0.424(4) 1 d P A 2
H42D H 0.8459 -0.1466 1.0232 0.044 Uiso 0.424(4) 1 calc PR A 2
H42E H 0.8274 -0.0595 0.9906 0.044 Uiso 0.424(4) 1 calc PR A 2
H42F H 0.7649 -0.1343 0.9602 0.044 Uiso 0.424(4) 1 calc PR A 2
C44B C 0.7694(4) -0.0404(3) 1.1198(3) 0.0258(14) Uani 0.424(4) 1 d P A 2
H44D H 0.7247 -0.0211 1.1579 0.039 Uiso 0.424(4) 1 calc PR A 2
H44E H 0.7998 0.0051 1.0948 0.039 Uiso 0.424(4) 1 calc PR A 2
H44F H 0.8238 -0.0735 1.1403 0.039 Uiso 0.424(4) 1 calc PR A 2
C43B C 0.6675(4) -0.1612(3) 1.0907(3) 0.0275(14) Uani 0.424(4) 1 d P A 2
H43D H 0.7250 -0.1932 1.1082 0.041 Uiso 0.424(4) 1 calc PR A 2
H43E H 0.6307 -0.1912 1.0539 0.041 Uiso 0.424(4) 1 calc PR A 2
H43F H 0.6210 -0.1492 1.1301 0.041 Uiso 0.424(4) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.255(3) . ?
C1 C2 1.478(3) . ?
C1 Nb1 2.2302(19) . ?
C2 C7 1.386(4) . ?
C2 C3 1.401(4) . ?
C3 C4 1.385(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.376(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.405(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 N1 1.496(2) . ?
C8 C11 1.520(3) . ?
C8 C9 1.521(3) . ?
C8 C10 1.526(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.520(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N2 1.334(3) . ?
C13 C14 1.396(3) . ?
C14 C15 1.400(3) . ?
C14 H14 0.9500 . ?
C15 N3 1.333(2) . ?
C15 C16 1.505(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.397(3) . ?
C17 C22 1.404(3) . ?
C17 N2 1.456(3) . ?
C18 C19 1.398(3) . ?
C18 C23 1.518(3) . ?
C19 C20 1.385(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.370(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(4) . ?
C21 H21 0.9500 . ?
C22 C26 1.518(4) . ?
C23 C24 1.527(3) . ?
C23 C25 1.534(3) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.532(3) . ?
C26 C28 1.535(4) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.400(3) . ?
C29 C34 1.406(3) . ?
C29 N3 1.451(2) . ?
C30 C31 1.399(3) . ?
C30 C38 1.519(3) . ?
C31 C32 1.373(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.376(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.392(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.522(3) . ?
C35 C36 1.533(4) . ?
C35 C37 1.529(3) . ?
C35 H35 1.0000 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.527(3) . ?
C38 C40 1.527(3) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C43B 1.319(6) . ?
C41 C42A 1.396(5) . ?
C41 N4 1.461(3) . ?
C41 C44A 1.601(5) . ?
C41 C43A 1.627(5) . ?
C41 C44B 1.644(5) . ?
C41 C42B 1.679(6) . ?
N1 Nb1 2.1344(16) . ?
N2 Nb1 2.2213(15) . ?
N3 Nb1 2.2313(16) . ?
N4 Nb1 1.7677(16) . ?
F1 Nb1 1.9688(11) . ?
C43A H43A 0.9800 . ?
C43A H43B 0.9800 . ?
C43A H43C 0.9800 . ?
C44A H44A 0.9800 . ?
C44A H44B 0.9800 . ?
C44A H44C 0.9800 . ?
C42A H42A 0.9800 . ?
C42A H42B 0.9800 . ?
C42A H42C 0.9800 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?
C44B H44D 0.9800 . ?
C44B H44E 0.9800 . ?
C44B H44F 0.9800 . ?
C43B H43D 0.9800 . ?
C43B H43E 0.9800 . ?
C43B H43F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 129.84(19) . . ?
N1 C1 Nb1 69.14(11) . . ?
C2 C1 Nb1 160.01(16) . . ?
C7 C2 C3 119.1(2) . . ?
C7 C2 C1 123.4(2) . . ?
C3 C2 C1 117.5(2) . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.7(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 120.1(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 119.6(3) . . ?
C2 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N1 C8 C11 107.58(16) . . ?
N1 C8 C9 110.69(16) . . ?
C11 C8 C9 109.2(2) . . ?
N1 C8 C10 106.76(18) . . ?
C11 C8 C10 110.39(19) . . ?
C9 C8 C10 112.1(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 124.38(18) . . ?
N2 C13 C12 120.89(19) . . ?
C14 C13 C12 114.71(19) . . ?
C13 C14 C15 128.30(19) . . ?
C13 C14 H14 115.8 . . ?
C15 C14 H14 115.8 . . ?
N3 C15 C14 123.62(18) . . ?
N3 C15 C16 120.77(19) . . ?
C14 C15 C16 115.55(18) . . ?
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 . . ?
C18 C17 C22 121.0(2) . . ?
C18 C17 N2 119.65(19) . . ?
C22 C17 N2 119.4(2) . . ?
C17 C18 C19 119.0(2) . . ?
C17 C18 C23 121.65(19) . . ?
C19 C18 C23 119.4(2) . . ?
C20 C19 C18 120.4(3) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C19 119.8(2) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 122.1(2) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C21 C22 C17 117.7(2) . . ?
C21 C22 C26 119.0(2) . . ?
C17 C22 C26 123.2(2) . . ?
C18 C23 C24 113.74(18) . . ?
C18 C23 C25 111.26(19) . . ?
C24 C23 C25 108.50(17) . . ?
C18 C23 H23 107.7 . . ?
C24 C23 H23 107.7 . . ?
C25 C23 H23 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 C27 111.2(2) . . ?
C22 C26 C28 111.6(2) . . ?
C27 C26 C28 108.9(2) . . ?
C22 C26 H26 108.4 . . ?
C27 C26 H26 108.4 . . ?
C28 C26 H26 108.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 119.75(19) . . ?
C30 C29 N3 119.15(18) . . ?
C34 C29 N3 121.09(18) . . ?
C31 C30 C29 119.1(2) . . ?
C31 C30 C38 118.2(2) . . ?
C29 C30 C38 122.67(19) . . ?
C32 C31 C30 121.2(2) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C33 119.5(2) . . ?
C31 C32 H32 120.3 . . ?
C33 C32 H32 120.3 . . ?
C32 C33 C34 121.4(2) . . ?
C32 C33 H33 119.3 . . ?
C34 C33 H33 119.3 . . ?
C33 C34 C29 119.0(2) . . ?
C33 C34 C35 118.4(2) . . ?
C29 C34 C35 122.66(19) . . ?
C34 C35 C36 112.7(2) . . ?
C34 C35 C37 110.6(2) . . ?
C36 C35 C37 110.0(2) . . ?
C34 C35 H35 107.8 . . ?
C36 C35 H35 107.8 . . ?
C37 C35 H35 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C30 C38 C39 110.14(18) . . ?
C30 C38 C40 111.98(19) . . ?
C39 C38 C40 110.13(19) . . ?
C30 C38 H38 108.2 . . ?
C39 C38 H38 108.2 . . ?
C40 C38 H38 108.2 . . ?
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 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C43B C41 C42A 120.3(3) . . ?
C43B C41 N4 120.6(3) . . ?
C42A C41 N4 117.3(3) . . ?
C43B C41 C44A 63.2(3) . . ?
C42A C41 C44A 112.6(3) . . ?
N4 C41 C44A 106.4(2) . . ?
C43B C41 C43A 39.4(3) . . ?
C42A C41 C43A 111.5(3) . . ?
N4 C41 C43A 105.5(2) . . ?
C44A C41 C43A 102.2(3) . . ?
C43B C41 C44B 113.5(4) . . ?
C42A C41 C44B 60.2(3) . . ?
N4 C41 C44B 106.2(2) . . ?
C44A C41 C44B 60.0(3) . . ?
C43A C41 C44B 147.0(3) . . ?
C43B C41 C42B 111.8(3) . . ?
C42A C41 C42B 38.2(3) . . ?
N4 C41 C42B 104.0(2) . . ?
C44A C41 C42B 146.4(3) . . ?
C43A C41 C42B 82.9(3) . . ?
C44B C41 C42B 98.0(3) . . ?
C1 N1 C8 134.78(17) . . ?
C1 N1 Nb1 77.53(12) . . ?
C8 N1 Nb1 147.32(13) . . ?
C13 N2 C17 117.00(16) . . ?
C13 N2 Nb1 120.47(13) . . ?
C17 N2 Nb1 121.23(12) . . ?
C15 N3 C29 115.11(17) . . ?
C15 N3 Nb1 120.11(14) . . ?
C29 N3 Nb1 124.36(12) . . ?
C41 N4 Nb1 171.35(16) . . ?
N4 Nb1 F1 121.40(7) . . ?
N4 Nb1 N1 97.51(7) . . ?
F1 Nb1 N1 78.74(5) . . ?
N4 Nb1 N2 95.10(7) . . ?
F1 Nb1 N2 138.70(6) . . ?
N1 Nb1 N2 117.75(6) . . ?
N4 Nb1 C1 113.48(8) . . ?
F1 Nb1 C1 94.82(6) . . ?
N1 Nb1 C1 33.34(7) . . ?
N2 Nb1 C1 86.49(7) . . ?
N4 Nb1 N3 95.55(7) . . ?
F1 Nb1 N3 75.66(5) . . ?
N1 Nb1 N3 154.40(6) . . ?
N2 Nb1 N3 82.73(6) . . ?
C1 Nb1 N3 149.82(7) . . ?
C41 C43A H43A 109.5 . . ?
C41 C43A H43B 109.5 . . ?
C41 C43A H43C 109.5 . . ?
C41 C44A H44A 109.5 . . ?
C41 C44A H44B 109.5 . . ?
C41 C44A H44C 109.5 . . ?
C41 C42A H42A 109.5 . . ?
C41 C42A H42B 109.5 . . ?
C41 C42A H42C 109.5 . . ?
C41 C42B H42D 109.5 . . ?
C41 C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41 C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
C41 C44B H44D 109.5 . . ?
C41 C44B H44E 109.5 . . ?
H44D C44B H44E 109.5 . . ?
C41 C44B H44F 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
C41 C43B H43D 109.5 . . ?
C41 C43B H43E 109.5 . . ?
H43D C43B H43E 109.5 . . ?
C41 C43B H43F 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.040
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: diethyl ether'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Hygroscopic'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_(2)
_database_code_depnum_ccdc_archive 'CCDC 1403877'
_audit_update_record             
;
2015-05-29 deposited with the CCDC.
2015-07-17 downloaded from the CCDC.
;
_audit_creation_method           shelxl-2014/7
_shelx_shelxl_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            'Complex 5'
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H65 N4 Nb'
_chemical_formula_sum            'C48 H65 N4 Nb'
_chemical_formula_weight         790.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
c c 0.0033 0.0016 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
h h 0.0000 0.0000 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
n n 0.0061 0.0033 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
nb nb -2.0727 0.6215 'international tables vol c tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_it_number           14
_space_group_name_h-m_alt        'p 21/n'
_space_group_name_hall           '-p 2yn'

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

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

_cell_length_a                   11.0558(4)
_cell_length_b                   21.2612(7)
_cell_length_c                   18.2635(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.612(2)
_cell_angle_gamma                90
_cell_volume                     4279.1(3)
_cell_formula_units_z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9874
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25.39

_exptl_crystal_description       rode
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_f_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.318
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9202
_exptl_absorpt_correction_T_max  0.9533
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           mok\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            51073
_diffrn_reflns_av_uneti/neti     0.0459
_diffrn_reflns_av_r_equivalents  0.0592
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.473
_diffrn_reflns_theta_max         25.433
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7862
_reflns_number_gt                6076
_reflns_threshold_expression     'i > 2σ(i)'
_reflns_friedel_coverage         0.000
_reflns_friedel_fraction_max     .
_reflns_friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 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-2014/7 (sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(fo²)+(0.0395p)²+4.7075p] where p=(fo²+2fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7862
_refine_ls_number_parameters     492
_refine_ls_number_restraints     0
_refine_ls_r_factor_all          0.0578
_refine_ls_r_factor_gt           0.0379
_refine_ls_wr_factor_ref         0.0944
_refine_ls_wr_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_s_all      1.019
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_u_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
c16 c 0.6630(3) 0.13001(14) -0.06791(16) 0.0311(8) uani 1 1 d . . . . .
h16a h 0.7167 0.1114 -0.1005 0.047 uiso 1 1 calc r u . . .
h16b h 0.6229 0.1656 -0.0914 0.047 uiso 1 1 calc r u . . .
h16c h 0.6036 0.0996 -0.0559 0.047 uiso 1 1 calc r u . . .
c17 c 0.7354(3) 0.15135(13) 0.00183(15) 0.0193(6) uani 1 1 d . . . . .
c18 c 0.7617(3) 0.21612(13) 0.00612(14) 0.0181(6) uani 1 1 d . . . . .
h18 h 0.7484 0.2390 -0.0372 0.022 uiso 1 1 calc r u . . .
c19 c 0.8052(2) 0.24931(12) 0.06756(14) 0.0153(6) uani 1 1 d . . . . .
c20 c 0.8237(3) 0.31909(12) 0.05748(15) 0.0197(6) uani 1 1 d . . . . .
h20a h 0.7768 0.3419 0.0906 0.030 uiso 1 1 calc r u . . .
h20b h 0.7981 0.3306 0.0078 0.030 uiso 1 1 calc r u . . .
h20c h 0.9081 0.3291 0.0676 0.030 uiso 1 1 calc r u . . .
c21 c 0.8400(2) 0.26779(12) 0.19464(14) 0.0142(6) uani 1 1 d . . . . .
c22 c 0.7317(2) 0.28417(12) 0.22589(14) 0.0147(6) uani 1 1 d . . . . .
c23 c 0.7370(3) 0.33053(13) 0.28000(15) 0.0207(6) uani 1 1 d . . . . .
h23 h 0.6663 0.3421 0.3009 0.025 uiso 1 1 calc r u . . .
c24 c 0.8449(3) 0.35961(13) 0.30324(15) 0.0215(7) uani 1 1 d . . . . .
h24 h 0.8465 0.3904 0.3395 0.026 uiso 1 1 calc r u . . .
c25 c 0.9499(3) 0.34303(12) 0.27270(15) 0.0187(6) uani 1 1 d . . . . .
h25 h 1.0221 0.3630 0.2888 0.022 uiso 1 1 calc r u . . .
c26 c 0.9513(2) 0.29708(12) 0.21807(14) 0.0145(6) uani 1 1 d . . . . .
c27 c 1.0715(2) 0.27982(13) 0.18831(15) 0.0189(6) uani 1 1 d . . . . .
h27 h 1.0544 0.2516 0.1463 0.023 uiso 1 1 calc r u . . .
c28 c 1.1403(3) 0.33719(14) 0.16178(18) 0.0279(7) uani 1 1 d . . . . .
h28a h 1.0892 0.3597 0.1257 0.042 uiso 1 1 calc r u . . .
h28b h 1.2122 0.3234 0.1403 0.042 uiso 1 1 calc r u . . .
h28c h 1.1625 0.3643 0.2027 0.042 uiso 1 1 calc r u . . .
c29 c 1.1525(3) 0.24455(14) 0.24662(17) 0.0254(7) uani 1 1 d . . . . .
h29a h 1.1714 0.2716 0.2881 0.038 uiso 1 1 calc r u . . .
h29b h 1.2262 0.2320 0.2263 0.038 uiso 1 1 calc r u . . .
h29c h 1.1106 0.2079 0.2621 0.038 uiso 1 1 calc r u . . .
c45 c 0.7522(3) 0.04319(13) 0.05698(15) 0.0212(7) uani 1 1 d . . . . .
c48 c 0.7857(4) 0.00710(16) -0.00897(19) 0.0540(12) uani 1 1 d . . . . .
h48a h 0.7299 0.0171 -0.0503 0.081 uiso 1 1 calc r u . . .
h48b h 0.7821 -0.0372 0.0010 0.081 uiso 1 1 calc r u . . .
h48c h 0.8665 0.0182 -0.0198 0.081 uiso 1 1 calc r u . . .
c46 c 0.8322(3) 0.02746(13) 0.12624(16) 0.0242(7) uani 1 1 d . . . . .
h46a h 0.9012 0.0017 0.1158 0.029 uiso 1 1 calc r u . . .
h46b h 0.7870 0.0069 0.1628 0.029 uiso 1 1 calc r u . . .
c47 c 0.6200(3) 0.02906(16) 0.0727(2) 0.0480(10) uani 1 1 d . . . . .
h47a h 0.6012 0.0508 0.1165 0.072 uiso 1 1 calc r u . . .
h47b h 0.6102 -0.0154 0.0795 0.072 uiso 1 1 calc r u . . .
h47c h 0.5662 0.0430 0.0321 0.072 uiso 1 1 calc r u . . .
c1 c 0.7455(2) 0.12241(13) 0.28363(14) 0.0171(6) uani 1 1 d . . . . .
h1a h 0.6954 0.1222 0.2375 0.021 uiso 1 1 calc r u . . .
h1b h 0.7377 0.1636 0.3055 0.021 uiso 1 1 calc r u . . .
c2 c 0.6957(2) 0.07417(13) 0.33393(15) 0.0166(6) uani 1 1 d . . . . .
c30 c 0.6089(2) 0.25617(13) 0.19923(14) 0.0173(6) uani 1 1 d . . . . .
h30 h 0.6238 0.2152 0.1771 0.021 uiso 1 1 calc r u . . .
c3 c 0.6954(3) 0.08693(14) 0.40872(16) 0.0230(7) uani 1 1 d . . . . .
h3 h 0.7240 0.1255 0.4269 0.028 uiso 1 1 calc r u . . .
c4 c 0.6530(3) 0.04311(14) 0.45627(17) 0.0266(7) uani 1 1 d . . . . .
h4 h 0.6540 0.0520 0.5062 0.032 uiso 1 1 calc r u . . .
c5 c 0.6093(3) -0.01384(14) 0.42969(17) 0.0267(7) uani 1 1 d . . . . .
h5 h 0.5802 -0.0433 0.4616 0.032 uiso 1 1 calc r u . . .
c6 c 0.6085(3) -0.02726(14) 0.35582(17) 0.0253(7) uani 1 1 d . . . . .
h6 h 0.5793 -0.0658 0.3380 0.030 uiso 1 1 calc r u . . .
c7 c 0.6513(3) 0.01680(13) 0.30812(16) 0.0226(7) uani 1 1 d . . . . .
h7 h 0.6501 0.0077 0.2583 0.027 uiso 1 1 calc r u . . .
c8 c 0.9531(2) 0.09781(13) 0.33185(14) 0.0152(6) uani 1 1 d . . . . .
c13 c 0.9808(2) 0.14345(13) 0.38621(14) 0.0181(6) uani 1 1 d . . . . .
c12 c 1.0528(3) 0.12587(15) 0.44947(15) 0.0248(7) uani 1 1 d . . . . .
h12 h 1.0720 0.1558 0.4857 0.030 uiso 1 1 calc r u . . .
c11 c 1.0956(3) 0.06566(15) 0.45944(16) 0.0283(7) uani 1 1 d . . . . .
h11 h 1.1427 0.0549 0.5021 0.034 uiso 1 1 calc r u . . .
c10 c 1.0683(3) 0.02142(14) 0.40581(16) 0.0250(7) uani 1 1 d . . . . .
h10 h 1.0980 -0.0193 0.4125 0.030 uiso 1 1 calc r u . . .
c9 c 0.9971(2) 0.03618(13) 0.34146(15) 0.0182(6) uani 1 1 d . . . . .
c15 c 0.9687(3) -0.01487(13) 0.28581(16) 0.0241(7) uani 1 1 d . . . . .
h15a h 0.8829 -0.0228 0.2815 0.036 uiso 1 1 calc r u . . .
h15b h 1.0111 -0.0526 0.3013 0.036 uiso 1 1 calc r u . . .
h15c h 0.9939 -0.0018 0.2391 0.036 uiso 1 1 calc r u . . .
c14 c 0.9338(3) 0.20945(13) 0.38072(15) 0.0220(7) uani 1 1 d . . . . .
h14a h 0.8620 0.2128 0.4067 0.033 uiso 1 1 calc r u . . .
h14b h 0.9147 0.2201 0.3300 0.033 uiso 1 1 calc r u . . .
h14c h 0.9945 0.2378 0.4019 0.033 uiso 1 1 calc r u . . .
c33 c 1.1621(2) 0.12940(13) 0.12257(14) 0.0166(6) uani 1 1 d . . . . .
c34 c 1.2620(3) 0.10669(13) 0.16811(16) 0.0198(6) uani 1 1 d . . . . .
c35 c 1.3781(3) 0.11643(14) 0.14626(16) 0.0259(7) uani 1 1 d . . . . .
h35 h 1.4444 0.1017 0.1759 0.031 uiso 1 1 calc r u . . .
c36 c 1.3974(3) 0.14734(14) 0.08188(17) 0.0273(7) uani 1 1 d . . . . .
h36 h 1.4760 0.1530 0.0682 0.033 uiso 1 1 calc r u . . .
c37 c 1.2998(3) 0.16985(14) 0.03777(16) 0.0245(7) uani 1 1 d . . . . .
h37 h 1.3134 0.1908 -0.0055 0.029 uiso 1 1 calc r u . . .
c38 c 1.1812(3) 0.16190(13) 0.05665(15) 0.0188(6) uani 1 1 d . . . . .
c39 c 1.0752(3) 0.18628(13) 0.00699(15) 0.0199(6) uani 1 1 d . . . . .
h39 h 1.0071 0.1922 0.0375 0.024 uiso 1 1 calc r u . . .
c41 c 1.0356(3) 0.13746(15) -0.05187(17) 0.0310(8) uani 1 1 d . . . . .
h41a h 1.1021 0.1287 -0.0811 0.046 uiso 1 1 calc r u . . .
h41b h 0.9684 0.1536 -0.0828 0.046 uiso 1 1 calc r u . . .
h41c h 1.0117 0.0994 -0.0286 0.046 uiso 1 1 calc r u . . .
c40 c 1.0994(3) 0.24960(14) -0.02826(18) 0.0327(8) uani 1 1 d . . . . .
h40a h 1.1297 0.2787 0.0090 0.049 uiso 1 1 calc r u . . .
h40b h 1.0253 0.2656 -0.0524 0.049 uiso 1 1 calc r u . . .
h40c h 1.1583 0.2444 -0.0636 0.049 uiso 1 1 calc r u . . .
c42 c 1.2437(3) 0.07161(13) 0.23898(15) 0.0210(6) uani 1 1 d . . . . .
h42 h 1.1586 0.0766 0.2492 0.025 uiso 1 1 calc r u . . .
c44 c 1.3226(3) 0.09716(15) 0.30528(17) 0.0289(7) uani 1 1 d . . . . .
h44a h 1.4067 0.0907 0.2979 0.043 uiso 1 1 calc r u . . .
h44b h 1.3031 0.0755 0.3489 0.043 uiso 1 1 calc r u . . .
h44c h 1.3075 0.1413 0.3106 0.043 uiso 1 1 calc r u . . .
c43 c 1.2675(3) 0.00152(14) 0.22943(18) 0.0319(8) uani 1 1 d . . . . .
h43a h 1.2139 -0.0146 0.1899 0.048 uiso 1 1 calc r u . . .
h43b h 1.2534 -0.0203 0.2740 0.048 uiso 1 1 calc r u . . .
h43c h 1.3501 -0.0047 0.2184 0.048 uiso 1 1 calc r u . . .
c32 c 0.5426(3) 0.29753(14) 0.13988(16) 0.0257(7) uani 1 1 d . . . . .
h32a h 0.5324 0.3391 0.1590 0.039 uiso 1 1 calc r u . . .
h32b h 0.4645 0.2797 0.1256 0.039 uiso 1 1 calc r u . . .
h32c h 0.5895 0.2997 0.0979 0.039 uiso 1 1 calc r u . . .
c31 c 0.5249(3) 0.24555(15) 0.26086(16) 0.0274(7) uani 1 1 d . . . . .
h31a h 0.5680 0.2232 0.3005 0.041 uiso 1 1 calc r u . . .
h31b h 0.4557 0.2213 0.2424 0.041 uiso 1 1 calc r u . . .
h31c h 0.4983 0.2854 0.2783 0.041 uiso 1 1 calc r u . . .
n4 n 0.7739(2) 0.11284(10) 0.05508(12) 0.0168(5) uani 1 1 d . . . . .
n2 n 0.83232(19) 0.22268(10) 0.13454(11) 0.0127(5) uani 1 1 d . . . . .
n1 n 0.87431(19) 0.11340(10) 0.26750(11) 0.0130(5) uani 1 1 d . . . . .
n3 n 1.04390(19) 0.12187(10) 0.14381(11) 0.0142(5) uani 1 1 d . . . . .
nb1 nb 0.88767(2) 0.12496(2) 0.15982(2) 0.01143(8) 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
c16 c17 1.518(4) . ?
c16 h16a 0.9600 . ?
c16 h16b 0.9600 . ?
c16 h16c 0.9600 . ?
c17 n4 1.316(3) . ?
c17 c18 1.409(4) . ?
c18 c19 1.379(4) . ?
c18 h18 0.9300 . ?
c19 n2 1.359(3) . ?
c19 c20 1.511(4) . ?
c20 h20a 0.9600 . ?
c20 h20b 0.9600 . ?
c20 h20c 0.9600 . ?
c21 c22 1.411(4) . ?
c21 c26 1.415(4) . ?
c21 n2 1.455(3) . ?
c22 c23 1.394(4) . ?
c22 c30 1.525(4) . ?
c23 c24 1.379(4) . ?
c23 h23 0.9300 . ?
c24 c25 1.374(4) . ?
c24 h24 0.9300 . ?
c25 c26 1.397(4) . ?
c25 h25 0.9300 . ?
c26 c27 1.520(4) . ?
c27 c29 1.531(4) . ?
c27 c28 1.536(4) . ?
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 . ?
c45 c48 1.499(4) . ?
c45 n4 1.501(3) . ?
c45 c46 1.521(4) . ?
c45 c47 1.543(5) . ?
c48 h48a 0.9600 . ?
c48 h48b 0.9600 . ?
c48 h48c 0.9600 . ?
c46 nb1 2.234(3) . ?
c46 h46a 0.9700 . ?
c46 h46b 0.9700 . ?
c47 h47a 0.9600 . ?
c47 h47b 0.9600 . ?
c47 h47c 0.9600 . ?
c1 n1 1.490(3) . ?
c1 c2 1.510(4) . ?
c1 h1a 0.9700 . ?
c1 h1b 0.9700 . ?
c2 c7 1.383(4) . ?
c2 c3 1.393(4) . ?
c30 c31 1.533(4) . ?
c30 c32 1.535(4) . ?
c30 h30 0.9800 . ?
c3 c4 1.381(4) . ?
c3 h3 0.9300 . ?
c4 c5 1.378(4) . ?
c4 h4 0.9300 . ?
c5 c6 1.378(4) . ?
c5 h5 0.9300 . ?
c6 c7 1.388(4) . ?
c6 h6 0.9300 . ?
c7 h7 0.9300 . ?
c8 c13 1.404(4) . ?
c8 c9 1.404(4) . ?
c8 n1 1.444(3) . ?
c13 c12 1.400(4) . ?
c13 c14 1.497(4) . ?
c12 c11 1.372(4) . ?
c12 h12 0.9300 . ?
c11 c10 1.374(4) . ?
c11 h11 0.9300 . ?
c10 c9 1.397(4) . ?
c10 h10 0.9300 . ?
c9 c15 1.503(4) . ?
c15 h15a 0.9600 . ?
c15 h15b 0.9600 . ?
c15 h15c 0.9600 . ?
c14 h14a 0.9600 . ?
c14 h14b 0.9600 . ?
c14 h14c 0.9600 . ?
c33 n3 1.402(3) . ?
c33 c34 1.413(4) . ?
c33 c38 1.419(4) . ?
c34 c35 1.390(4) . ?
c34 c42 1.521(4) . ?
c35 c36 1.379(4) . ?
c35 h35 0.9300 . ?
c36 c37 1.380(4) . ?
c36 h36 0.9300 . ?
c37 c38 1.392(4) . ?
c37 h37 0.9300 . ?
c38 c39 1.515(4) . ?
c39 c40 1.525(4) . ?
c39 c41 1.533(4) . ?
c39 h39 0.9800 . ?
c41 h41a 0.9600 . ?
c41 h41b 0.9600 . ?
c41 h41c 0.9600 . ?
c40 h40a 0.9600 . ?
c40 h40b 0.9600 . ?
c40 h40c 0.9600 . ?
c42 c43 1.526(4) . ?
c42 c44 1.534(4) . ?
c42 h42 0.9800 . ?
c44 h44a 0.9600 . ?
c44 h44b 0.9600 . ?
c44 h44c 0.9600 . ?
c43 h43a 0.9600 . ?
c43 h43b 0.9600 . ?
c43 h43c 0.9600 . ?
c32 h32a 0.9600 . ?
c32 h32b 0.9600 . ?
c32 h32c 0.9600 . ?
c31 h31a 0.9600 . ?
c31 h31b 0.9600 . ?
c31 h31c 0.9600 . ?
n4 nb1 2.218(2) . ?
n2 nb1 2.204(2) . ?
n1 nb1 1.999(2) . ?
n3 nb1 1.776(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
c17 c16 h16a 109.5 . . ?
c17 c16 h16b 109.5 . . ?
h16a c16 h16b 109.5 . . ?
c17 c16 h16c 109.5 . . ?
h16a c16 h16c 109.5 . . ?
h16b c16 h16c 109.5 . . ?
n4 c17 c18 120.9(2) . . ?
n4 c17 c16 123.5(3) . . ?
c18 c17 c16 115.6(2) . . ?
c19 c18 c17 127.0(2) . . ?
c19 c18 h18 116.5 . . ?
c17 c18 h18 116.5 . . ?
n2 c19 c18 123.8(2) . . ?
n2 c19 c20 119.8(2) . . ?
c18 c19 c20 116.4(2) . . ?
c19 c20 h20a 109.5 . . ?
c19 c20 h20b 109.5 . . ?
h20a c20 h20b 109.5 . . ?
c19 c20 h20c 109.5 . . ?
h20a c20 h20c 109.5 . . ?
h20b c20 h20c 109.5 . . ?
c22 c21 c26 121.0(2) . . ?
c22 c21 n2 117.9(2) . . ?
c26 c21 n2 121.0(2) . . ?
c23 c22 c21 118.2(2) . . ?
c23 c22 c30 119.2(2) . . ?
c21 c22 c30 122.5(2) . . ?
c24 c23 c22 121.4(3) . . ?
c24 c23 h23 119.3 . . ?
c22 c23 h23 119.3 . . ?
c25 c24 c23 119.9(3) . . ?
c25 c24 h24 120.1 . . ?
c23 c24 h24 120.1 . . ?
c24 c25 c26 121.8(3) . . ?
c24 c25 h25 119.1 . . ?
c26 c25 h25 119.1 . . ?
c25 c26 c21 117.7(3) . . ?
c25 c26 c27 119.0(2) . . ?
c21 c26 c27 123.3(2) . . ?
c26 c27 c29 110.4(2) . . ?
c26 c27 c28 113.0(2) . . ?
c29 c27 c28 109.4(2) . . ?
c26 c27 h27 108.0 . . ?
c29 c27 h27 108.0 . . ?
c28 c27 h27 108.0 . . ?
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 . . ?
c48 c45 n4 115.9(3) . . ?
c48 c45 c46 113.0(3) . . ?
n4 c45 c46 98.8(2) . . ?
c48 c45 c47 110.4(3) . . ?
n4 c45 c47 110.6(2) . . ?
c46 c45 c47 107.3(3) . . ?
c45 c48 h48a 109.5 . . ?
c45 c48 h48b 109.5 . . ?
h48a c48 h48b 109.5 . . ?
c45 c48 h48c 109.5 . . ?
h48a c48 h48c 109.5 . . ?
h48b c48 h48c 109.5 . . ?
c45 c46 nb1 98.78(17) . . ?
c45 c46 h46a 112.0 . . ?
nb1 c46 h46a 112.0 . . ?
c45 c46 h46b 112.0 . . ?
nb1 c46 h46b 112.0 . . ?
h46a c46 h46b 109.7 . . ?
c45 c47 h47a 109.5 . . ?
c45 c47 h47b 109.5 . . ?
h47a c47 h47b 109.5 . . ?
c45 c47 h47c 109.5 . . ?
h47a c47 h47c 109.5 . . ?
h47b c47 h47c 109.5 . . ?
n1 c1 c2 115.7(2) . . ?
n1 c1 h1a 108.4 . . ?
c2 c1 h1a 108.4 . . ?
n1 c1 h1b 108.4 . . ?
c2 c1 h1b 108.4 . . ?
h1a c1 h1b 107.4 . . ?
c7 c2 c3 118.5(3) . . ?
c7 c2 c1 121.9(2) . . ?
c3 c2 c1 119.6(2) . . ?
c22 c30 c31 113.5(2) . . ?
c22 c30 c32 111.3(2) . . ?
c31 c30 c32 108.6(2) . . ?
c22 c30 h30 107.7 . . ?
c31 c30 h30 107.7 . . ?
c32 c30 h30 107.7 . . ?
c4 c3 c2 120.9(3) . . ?
c4 c3 h3 119.6 . . ?
c2 c3 h3 119.6 . . ?
c5 c4 c3 119.9(3) . . ?
c5 c4 h4 120.0 . . ?
c3 c4 h4 120.0 . . ?
c4 c5 c6 120.1(3) . . ?
c4 c5 h5 120.0 . . ?
c6 c5 h5 120.0 . . ?
c5 c6 c7 119.9(3) . . ?
c5 c6 h6 120.0 . . ?
c7 c6 h6 120.0 . . ?
c2 c7 c6 120.7(3) . . ?
c2 c7 h7 119.6 . . ?
c6 c7 h7 119.6 . . ?
c13 c8 c9 120.2(2) . . ?
c13 c8 n1 120.0(2) . . ?
c9 c8 n1 119.8(2) . . ?
c12 c13 c8 118.4(3) . . ?
c12 c13 c14 118.5(3) . . ?
c8 c13 c14 123.1(2) . . ?
c11 c12 c13 121.7(3) . . ?
c11 c12 h12 119.1 . . ?
c13 c12 h12 119.1 . . ?
c12 c11 c10 119.4(3) . . ?
c12 c11 h11 120.3 . . ?
c10 c11 h11 120.3 . . ?
c11 c10 c9 121.5(3) . . ?
c11 c10 h10 119.2 . . ?
c9 c10 h10 119.2 . . ?
c10 c9 c8 118.8(3) . . ?
c10 c9 c15 118.7(3) . . ?
c8 c9 c15 122.6(2) . . ?
c9 c15 h15a 109.5 . . ?
c9 c15 h15b 109.5 . . ?
h15a c15 h15b 109.5 . . ?
c9 c15 h15c 109.5 . . ?
h15a c15 h15c 109.5 . . ?
h15b c15 h15c 109.5 . . ?
c13 c14 h14a 109.5 . . ?
c13 c14 h14b 109.5 . . ?
h14a c14 h14b 109.5 . . ?
c13 c14 h14c 109.5 . . ?
h14a c14 h14c 109.5 . . ?
h14b c14 h14c 109.5 . . ?
n3 c33 c34 120.0(2) . . ?
n3 c33 c38 119.7(2) . . ?
c34 c33 c38 120.2(3) . . ?
c35 c34 c33 118.4(3) . . ?
c35 c34 c42 120.4(3) . . ?
c33 c34 c42 121.2(2) . . ?
c36 c35 c34 121.8(3) . . ?
c36 c35 h35 119.1 . . ?
c34 c35 h35 119.1 . . ?
c35 c36 c37 119.7(3) . . ?
c35 c36 h36 120.2 . . ?
c37 c36 h36 120.2 . . ?
c36 c37 c38 121.4(3) . . ?
c36 c37 h37 119.3 . . ?
c38 c37 h37 119.3 . . ?
c37 c38 c33 118.5(3) . . ?
c37 c38 c39 120.6(3) . . ?
c33 c38 c39 120.9(2) . . ?
c38 c39 c40 113.7(2) . . ?
c38 c39 c41 110.6(2) . . ?
c40 c39 c41 110.6(2) . . ?
c38 c39 h39 107.2 . . ?
c40 c39 h39 107.2 . . ?
c41 c39 h39 107.2 . . ?
c39 c41 h41a 109.5 . . ?
c39 c41 h41b 109.5 . . ?
h41a c41 h41b 109.5 . . ?
c39 c41 h41c 109.5 . . ?
h41a c41 h41c 109.5 . . ?
h41b c41 h41c 109.5 . . ?
c39 c40 h40a 109.5 . . ?
c39 c40 h40b 109.5 . . ?
h40a c40 h40b 109.5 . . ?
c39 c40 h40c 109.5 . . ?
h40a c40 h40c 109.5 . . ?
h40b c40 h40c 109.5 . . ?
c34 c42 c43 110.2(2) . . ?
c34 c42 c44 113.1(2) . . ?
c43 c42 c44 110.1(2) . . ?
c34 c42 h42 107.7 . . ?
c43 c42 h42 107.7 . . ?
c44 c42 h42 107.7 . . ?
c42 c44 h44a 109.5 . . ?
c42 c44 h44b 109.5 . . ?
h44a c44 h44b 109.5 . . ?
c42 c44 h44c 109.5 . . ?
h44a c44 h44c 109.5 . . ?
h44b c44 h44c 109.5 . . ?
c42 c43 h43a 109.5 . . ?
c42 c43 h43b 109.5 . . ?
h43a c43 h43b 109.5 . . ?
c42 c43 h43c 109.5 . . ?
h43a c43 h43c 109.5 . . ?
h43b c43 h43c 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 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 . . ?
c17 n4 c45 126.0(2) . . ?
c17 n4 nb1 133.82(18) . . ?
c45 n4 nb1 100.08(15) . . ?
c19 n2 c21 113.5(2) . . ?
c19 n2 nb1 128.22(17) . . ?
c21 n2 nb1 117.70(15) . . ?
c8 n1 c1 113.1(2) . . ?
c8 n1 nb1 137.86(18) . . ?
c1 n1 nb1 109.03(15) . . ?
c33 n3 nb1 169.07(19) . . ?
n3 nb1 n1 107.89(9) . . ?
n3 nb1 n2 104.93(9) . . ?
n1 nb1 n2 106.31(8) . . ?
n3 nb1 n4 110.20(9) . . ?
n1 nb1 n4 138.80(9) . . ?
n2 nb1 n4 78.48(8) . . ?
n3 nb1 c46 99.77(11) . . ?
n1 nb1 c46 96.64(10) . . ?
n2 nb1 c46 138.74(9) . . ?
n4 nb1 c46 62.05(9) . . ?

_refine_diff_density_max         0.910
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.076


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