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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1459078'
_audit_update_record             
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;

_audit_creation_method           shelxl-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            (BDI)Nb(NtBu)Ph
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H54 N3 Nb'
_chemical_formula_weight         657.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
c c 0.0033 0.0016 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
h h 0.0000 0.0000 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
n n 0.0061 0.0033 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
nb nb -2.0727 0.6215 'international tables vol c tables 4.2.6.8 and 6.1.1.4'
b b 0.0013 0.0007 'international tables vol c tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_it_number           1
_space_group_name_h-m_alt        'p 1'
_space_group_name_hall           'p 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.6363(4)
_cell_length_b                   10.3540(4)
_cell_length_c                   10.4978(4)
_cell_angle_alpha                107.0190(10)
_cell_angle_beta                 113.6050(10)
_cell_angle_gamma                91.5850(10)
_cell_volume                     905.11(6)
_cell_formula_units_z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_f_000             350
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.361
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_t_min  0.6989
_exptl_absorpt_correction_t_max  0.7452
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           mok\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            12336
_diffrn_reflns_av_uneti/neti     0.0629
_diffrn_reflns_av_r_equivalents  0.0364
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.086
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_point_group_measured_fraction_full 0.882
_reflns_number_total             5814
_reflns_number_gt                5687
_reflns_threshold_expression     'i > 2σ(i)'
_reflns_friedel_coverage         0.748
_reflns_friedel_fraction_max     0.746
_reflns_friedel_fraction_full    0.765

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    SIR-92
_computing_structure_refinement  'shelxl-2014 (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)+(0.0318p)²+0.3065p] 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_abs_structure_details 
;
 flack x determined using 2318 quotients [(i+)-(i-)]/[(i+)+(i-)]
 (parsons, flack and wagner, acta cryst. b69 (2013) 249-259).
;
_refine_ls_abs_structure_flack   0.089(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5814
_refine_ls_number_parameters     388
_refine_ls_number_restraints     3
_refine_ls_r_factor_all          0.0412
_refine_ls_r_factor_gt           0.0393
_refine_ls_wr_factor_ref         0.0786
_refine_ls_wr_factor_gt          0.0773
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_s_all      1.056
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
c1 c 0.1214(6) 0.1335(5) 0.3060(6) 0.0192(12) uani 1 1 d . . . . .
c2 c 0.2586(7) 0.0810(6) 0.3492(7) 0.0310(14) uani 1 1 d . . . . .
h2 h 0.2976 0.0650 0.4409 0.037 uiso 1 1 calc r u . . .
c3 c 0.3401(8) 0.0513(6) 0.2650(8) 0.0379(16) uani 1 1 d . . . . .
h3 h 0.4330 0.0157 0.2986 0.046 uiso 1 1 calc r u . . .
c4 c 0.2848(7) 0.0740(6) 0.1305(7) 0.0359(16) uani 1 1 d . . . . .
h4 h 0.3400 0.0546 0.0715 0.043 uiso 1 1 calc r u . . .
c5 c 0.1509(7) 0.1245(6) 0.0838(6) 0.0334(15) uani 1 1 d . . . . .
h5 h 0.1131 0.1404 -0.0080 0.040 uiso 1 1 calc r u . . .
c6 c 0.0693(7) 0.1527(6) 0.1687(6) 0.0305(14) uani 1 1 d . . . . .
h6 h -0.0248 0.1860 0.1328 0.037 uiso 1 1 calc r u . . .
c7 c -0.2253(6) 0.3849(5) 0.3407(6) 0.0223(12) uani 1 1 d . . . . .
c8 c -0.3878(6) 0.3295(6) 0.3052(7) 0.0324(15) uani 1 1 d . . . . .
h8a h -0.3911 0.3152 0.3922 0.049 uiso 1 1 calc r u . . .
h8b h -0.4228 0.2422 0.2239 0.049 uiso 1 1 calc r u . . .
h8c h -0.4550 0.3951 0.2764 0.049 uiso 1 1 calc r u . . .
c9 c -0.2178(7) 0.4059(7) 0.2065(7) 0.0425(17) uani 1 1 d . . . . .
h9a h -0.1119 0.4418 0.2308 0.064 uiso 1 1 calc r u . . .
h9b h -0.2848 0.4712 0.1762 0.064 uiso 1 1 calc r u . . .
h9c h -0.2519 0.3182 0.1258 0.064 uiso 1 1 calc r u . . .
c10 c -0.1705(7) 0.5191(6) 0.4717(7) 0.0413(17) uani 1 1 d . . . . .
h10a h -0.1765 0.5018 0.5564 0.062 uiso 1 1 calc r u . . .
h10b h -0.2360 0.5864 0.4447 0.062 uiso 1 1 calc r u . . .
h10c h -0.0640 0.5548 0.4975 0.062 uiso 1 1 calc r u . . .
c11 c 0.1888(6) 0.4414(5) 0.7356(6) 0.0153(13) uani 1 1 d . . . . .
c12 c 0.2735(6) 0.5221(6) 0.6947(7) 0.0164(13) uani 1 1 d . . . . .
c13 c 0.2956(6) 0.6646(5) 0.7590(6) 0.0224(13) uani 1 1 d . . . . .
h13 h 0.3541 0.7214 0.7354 0.027 uiso 1 1 calc r u . . .
c14 c 0.2345(6) 0.7237(6) 0.8549(6) 0.0260(14) uani 1 1 d . . . . .
h14 h 0.2459 0.8206 0.8926 0.031 uiso 1 1 calc r u . . .
c15 c 0.1561(6) 0.6434(6) 0.8975(6) 0.0268(14) uani 1 1 d . . . . .
h15 h 0.1173 0.6861 0.9667 0.032 uiso 1 1 calc r u . . .
c16 c 0.1332(6) 0.5011(5) 0.8406(6) 0.0206(12) uani 1 1 d . . . . .
c17 c 0.3428(7) 0.4608(6) 0.5908(7) 0.0229(14) uani 1 1 d . . . . .
h17 h 0.3175 0.3589 0.5604 0.028 uiso 1 1 calc r u . . .
c18 c 0.5174(7) 0.4997(9) 0.6654(7) 0.057(2) uani 1 1 d . . . . .
h18a h 0.5592 0.4583 0.5946 0.086 uiso 1 1 calc r u . . .
h18b h 0.5595 0.4663 0.7493 0.086 uiso 1 1 calc r u . . .
h18c h 0.5457 0.5996 0.7001 0.086 uiso 1 1 calc r u . . .
c19 c 0.2808(9) 0.4998(9) 0.4514(8) 0.044(2) uani 1 1 d . . . . .
h19a h 0.3307 0.4567 0.3885 0.066 uiso 1 1 calc r u . . .
h19b h 0.3022 0.5996 0.4780 0.066 uiso 1 1 calc r u . . .
h19c h 0.1697 0.4683 0.3981 0.066 uiso 1 1 calc r u . . .
c20 c 0.0492(6) 0.4152(6) 0.8915(6) 0.0251(13) uani 1 1 d . . . . .
h20 h 0.0636 0.3181 0.8553 0.030 uiso 1 1 calc r u . . .
c21 c -0.1219(7) 0.4191(6) 0.8246(7) 0.0373(16) uani 1 1 d . . . . .
h21a h -0.1737 0.3636 0.8591 0.056 uiso 1 1 calc r u . . .
h21b h -0.1633 0.3823 0.7169 0.056 uiso 1 1 calc r u . . .
h21c h -0.1391 0.5139 0.8547 0.056 uiso 1 1 calc r u . . .
c22 c 0.1152(8) 0.4600(7) 1.0581(7) 0.0410(17) uani 1 1 d . . . . .
h22a h 0.2257 0.4575 1.0985 0.062 uiso 1 1 calc r u . . .
h22b h 0.0646 0.3981 1.0873 0.062 uiso 1 1 calc r u . . .
h22c h 0.0981 0.5535 1.0964 0.062 uiso 1 1 calc r u . . .
c23 c 0.3665(7) 0.2560(6) 0.8628(6) 0.0360(16) uani 1 1 d . . . . .
h23a h 0.4011 0.3517 0.9113 0.043 uiso 1 1 calc r u . . .
h23b h 0.4206 0.1930 0.9056 0.043 uiso 1 1 calc r u . . .
c24 c 0.2402(6) 0.2094(5) 0.7328(6) 0.0198(12) uani 1 1 d . . . . .
c25 c 0.1943(6) 0.0619(6) 0.6545(6) 0.0236(13) uani 1 1 d . . . . .
h25 h 0.2778 0.0135 0.6815 0.028 uiso 1 1 calc r u . . .
c26 c 0.0599(6) -0.0236(5) 0.5515(6) 0.0234(13) uani 1 1 d . . . . .
c27 c 0.0603(7) -0.1743(6) 0.4940(7) 0.0342(15) uani 1 1 d . . . . .
h27a h -0.0437 -0.2208 0.4222 0.051 uiso 1 1 calc r u . . .
h27b h 0.0946 -0.2107 0.5759 0.051 uiso 1 1 calc r u . . .
h27c h 0.1303 -0.1897 0.4463 0.051 uiso 1 1 calc r u . . .
c29 c -0.2216(6) -0.0694(5) 0.4185(6) 0.0183(12) uani 1 1 d . . . . .
c30 c -0.2941(7) -0.1406(6) 0.2658(7) 0.0202(14) uani 1 1 d . . . . .
c31 c -0.4284(6) -0.2316(6) 0.2108(6) 0.0267(13) uani 1 1 d . . . . .
h31 h -0.4780 -0.2809 0.1082 0.032 uiso 1 1 calc r u . . .
c32 c -0.4922(7) -0.2529(6) 0.3007(6) 0.0280(14) uani 1 1 d . . . . .
h32 h -0.5850 -0.3155 0.2601 0.034 uiso 1 1 calc r u . . .
c33 c -0.4211(6) -0.1832(6) 0.4487(6) 0.0274(13) uani 1 1 d . . . . .
h33 h -0.4656 -0.1990 0.5100 0.033 uiso 1 1 calc r u . . .
c34 c -0.2862(7) -0.0902(6) 0.5122(7) 0.0227(14) uani 1 1 d . . . . .
c35 c -0.2094(6) -0.0170(6) 0.6772(6) 0.0275(14) uani 1 1 d . . . . .
h35 h -0.1185 0.0497 0.7005 0.033 uiso 1 1 calc r u . . .
c36 c -0.3194(8) 0.0622(7) 0.7284(7) 0.0428(17) uani 1 1 d . . . . .
h36a h -0.2673 0.1102 0.8349 0.064 uiso 1 1 calc r u . . .
h36b h -0.4095 -0.0017 0.7060 0.064 uiso 1 1 calc r u . . .
h36c h -0.3521 0.1290 0.6772 0.064 uiso 1 1 calc r u . . .
c37 c -0.1530(8) -0.1198(7) 0.7588(7) 0.0408(17) uani 1 1 d . . . . .
h37a h -0.1020 -0.0709 0.8651 0.061 uiso 1 1 calc r u . . .
h37b h -0.0802 -0.1676 0.7268 0.061 uiso 1 1 calc r u . . .
h37c h -0.2407 -0.1864 0.7365 0.061 uiso 1 1 calc r u . . .
c38 c -0.2316(7) -0.1206(6) 0.1604(7) 0.0225(15) uani 1 1 d . . . . .
h38 h -0.1279 -0.0623 0.2208 0.027 uiso 1 1 calc r u . . .
c39 c -0.2111(9) -0.2561(7) 0.0661(7) 0.0443(18) uani 1 1 d . . . . .
h39a h -0.1695 -0.2383 0.0005 0.066 uiso 1 1 calc r u . . .
h39b h -0.3106 -0.3166 0.0072 0.066 uiso 1 1 calc r u . . .
h39c h -0.1399 -0.3001 0.1304 0.066 uiso 1 1 calc r u . . .
c40 c -0.3317(7) -0.0451(6) 0.0634(6) 0.0330(15) uani 1 1 d . . . . .
h40a h -0.2879 -0.0327 -0.0027 0.050 uiso 1 1 calc r u . . .
h40b h -0.3366 0.0446 0.1253 0.050 uiso 1 1 calc r u . . .
h40c h -0.4354 -0.0985 0.0049 0.050 uiso 1 1 calc r u . . .
n1 n -0.1236(5) 0.2869(4) 0.3856(4) 0.0169(10) uani 1 1 d . . . . .
n2 n 0.1537(5) 0.2960(4) 0.6622(4) 0.0175(10) uani 1 1 d . . . . .
n3 n -0.0789(5) 0.0229(4) 0.4825(4) 0.0178(10) uani 1 1 d . . . . .
nb1 nb 0.00969(2) 0.18529(2) 0.45585(2) 0.01475(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 1.398(7) . ?
c1 c6 1.400(8) . ?
c1 nb1 2.194(5) . ?
c2 c3 1.379(8) . ?
c2 h2 0.9500 . ?
c3 c4 1.390(9) . ?
c3 h3 0.9500 . ?
c4 c5 1.363(8) . ?
c4 h4 0.9500 . ?
c5 c6 1.386(8) . ?
c5 h5 0.9500 . ?
c6 h6 0.9500 . ?
c7 n1 1.476(7) . ?
c7 c8 1.509(7) . ?
c7 c9 1.515(8) . ?
c7 c10 1.536(8) . ?
c8 h8a 0.9800 . ?
c8 h8b 0.9800 . ?
c8 h8c 0.9800 . ?
c9 h9a 0.9800 . ?
c9 h9b 0.9800 . ?
c9 h9c 0.9800 . ?
c10 h10a 0.9800 . ?
c10 h10b 0.9800 . ?
c10 h10c 0.9800 . ?
c11 c16 1.406(8) . ?
c11 c12 1.415(8) . ?
c11 n2 1.435(7) . ?
c12 c13 1.401(7) . ?
c12 c17 1.496(8) . ?
c13 c14 1.367(8) . ?
c13 h13 0.9500 . ?
c14 c15 1.383(8) . ?
c14 h14 0.9500 . ?
c15 c16 1.392(8) . ?
c15 h15 0.9500 . ?
c16 c20 1.522(7) . ?
c17 c19 1.524(9) . ?
c17 c18 1.527(8) . ?
c17 h17 1.0000 . ?
c18 h18a 0.9800 . ?
c18 h18b 0.9800 . ?
c18 h18c 0.9800 . ?
c19 h19a 0.9800 . ?
c19 h19b 0.9800 . ?
c19 h19c 0.9800 . ?
c20 c22 1.516(8) . ?
c20 c21 1.519(8) . ?
c20 h20 1.0000 . ?
c21 h21a 0.9800 . ?
c21 h21b 0.9800 . ?
c21 h21c 0.9800 . ?
c22 h22a 0.9800 . ?
c22 h22b 0.9800 . ?
c22 h22c 0.9800 . ?
c23 c24 1.352(7) . ?
c23 h23a 0.9500 . ?
c23 h23b 0.9500 . ?
c24 n2 1.408(6) . ?
c24 c25 1.463(8) . ?
c25 c26 1.373(7) . ?
c25 h25 0.9500 . ?
c26 n3 1.418(7) . ?
c26 c27 1.499(8) . ?
c26 nb1 2.619(5) . ?
c27 h27a 0.9800 . ?
c27 h27b 0.9800 . ?
c27 h27c 0.9800 . ?
c29 c30 1.409(8) . ?
c29 c34 1.417(8) . ?
c29 n3 1.437(7) . ?
c30 c31 1.383(8) . ?
c30 c38 1.514(9) . ?
c31 c32 1.376(8) . ?
c31 h31 0.9500 . ?
c32 c33 1.367(8) . ?
c32 h32 0.9500 . ?
c33 c34 1.387(8) . ?
c33 h33 0.9500 . ?
c34 c35 1.515(8) . ?
c35 c36 1.527(8) . ?
c35 c37 1.534(8) . ?
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 c40 1.516(8) . ?
c38 c39 1.532(8) . ?
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 . ?
n1 nb1 1.752(4) . ?
n2 nb1 1.996(4) . ?
n3 nb1 2.005(4) . ?

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 c6 115.4(5) . . ?
c2 c1 nb1 119.2(4) . . ?
c6 c1 nb1 125.3(4) . . ?
c3 c2 c1 123.1(6) . . ?
c3 c2 h2 118.4 . . ?
c1 c2 h2 118.4 . . ?
c2 c3 c4 119.2(6) . . ?
c2 c3 h3 120.4 . . ?
c4 c3 h3 120.4 . . ?
c5 c4 c3 119.6(6) . . ?
c5 c4 h4 120.2 . . ?
c3 c4 h4 120.2 . . ?
c4 c5 c6 120.6(6) . . ?
c4 c5 h5 119.7 . . ?
c6 c5 h5 119.7 . . ?
c5 c6 c1 122.0(6) . . ?
c5 c6 h6 119.0 . . ?
c1 c6 h6 119.0 . . ?
n1 c7 c8 109.6(4) . . ?
n1 c7 c9 109.0(5) . . ?
c8 c7 c9 110.1(5) . . ?
n1 c7 c10 107.7(4) . . ?
c8 c7 c10 108.7(5) . . ?
c9 c7 c10 111.6(5) . . ?
c7 c8 h8a 109.5 . . ?
c7 c8 h8b 109.5 . . ?
h8a c8 h8b 109.5 . . ?
c7 c8 h8c 109.5 . . ?
h8a c8 h8c 109.5 . . ?
h8b c8 h8c 109.5 . . ?
c7 c9 h9a 109.5 . . ?
c7 c9 h9b 109.5 . . ?
h9a c9 h9b 109.5 . . ?
c7 c9 h9c 109.5 . . ?
h9a c9 h9c 109.5 . . ?
h9b c9 h9c 109.5 . . ?
c7 c10 h10a 109.5 . . ?
c7 c10 h10b 109.5 . . ?
h10a c10 h10b 109.5 . . ?
c7 c10 h10c 109.5 . . ?
h10a c10 h10c 109.5 . . ?
h10b c10 h10c 109.5 . . ?
c16 c11 c12 121.6(5) . . ?
c16 c11 n2 119.9(5) . . ?
c12 c11 n2 118.5(5) . . ?
c13 c12 c11 117.5(5) . . ?
c13 c12 c17 119.9(6) . . ?
c11 c12 c17 122.6(5) . . ?
c14 c13 c12 121.3(5) . . ?
c14 c13 h13 119.4 . . ?
c12 c13 h13 119.4 . . ?
c13 c14 c15 120.5(6) . . ?
c13 c14 h14 119.7 . . ?
c15 c14 h14 119.7 . . ?
c14 c15 c16 121.1(6) . . ?
c14 c15 h15 119.4 . . ?
c16 c15 h15 119.4 . . ?
c15 c16 c11 117.9(5) . . ?
c15 c16 c20 120.1(5) . . ?
c11 c16 c20 122.1(5) . . ?
c12 c17 c19 113.5(5) . . ?
c12 c17 c18 111.4(5) . . ?
c19 c17 c18 108.7(6) . . ?
c12 c17 h17 107.6 . . ?
c19 c17 h17 107.6 . . ?
c18 c17 h17 107.6 . . ?
c17 c18 h18a 109.5 . . ?
c17 c18 h18b 109.5 . . ?
h18a c18 h18b 109.5 . . ?
c17 c18 h18c 109.5 . . ?
h18a c18 h18c 109.5 . . ?
h18b c18 h18c 109.5 . . ?
c17 c19 h19a 109.5 . . ?
c17 c19 h19b 109.5 . . ?
h19a c19 h19b 109.5 . . ?
c17 c19 h19c 109.5 . . ?
h19a c19 h19c 109.5 . . ?
h19b c19 h19c 109.5 . . ?
c22 c20 c21 111.1(5) . . ?
c22 c20 c16 111.5(5) . . ?
c21 c20 c16 110.8(5) . . ?
c22 c20 h20 107.7 . . ?
c21 c20 h20 107.7 . . ?
c16 c20 h20 107.7 . . ?
c20 c21 h21a 109.5 . . ?
c20 c21 h21b 109.5 . . ?
h21a c21 h21b 109.5 . . ?
c20 c21 h21c 109.5 . . ?
h21a c21 h21c 109.5 . . ?
h21b c21 h21c 109.5 . . ?
c20 c22 h22a 109.5 . . ?
c20 c22 h22b 109.5 . . ?
h22a c22 h22b 109.5 . . ?
c20 c22 h22c 109.5 . . ?
h22a c22 h22c 109.5 . . ?
h22b c22 h22c 109.5 . . ?
c24 c23 h23a 120.0 . . ?
c24 c23 h23b 120.0 . . ?
h23a c23 h23b 120.0 . . ?
c23 c24 n2 123.4(5) . . ?
c23 c24 c25 119.4(5) . . ?
n2 c24 c25 117.1(4) . . ?
c26 c25 c24 135.6(5) . . ?
c26 c25 h25 112.2 . . ?
c24 c25 h25 112.2 . . ?
c25 c26 n3 123.8(5) . . ?
c25 c26 c27 119.4(5) . . ?
n3 c26 c27 116.4(5) . . ?
c25 c26 nb1 82.9(3) . . ?
n3 c26 nb1 49.2(2) . . ?
c27 c26 nb1 139.4(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 . . ?
c30 c29 c34 120.5(5) . . ?
c30 c29 n3 120.6(5) . . ?
c34 c29 n3 118.9(5) . . ?
c31 c30 c29 118.2(6) . . ?
c31 c30 c38 119.1(6) . . ?
c29 c30 c38 122.7(6) . . ?
c32 c31 c30 121.8(6) . . ?
c32 c31 h31 119.1 . . ?
c30 c31 h31 119.1 . . ?
c33 c32 c31 119.5(5) . . ?
c33 c32 h32 120.2 . . ?
c31 c32 h32 120.2 . . ?
c32 c33 c34 122.1(6) . . ?
c32 c33 h33 119.0 . . ?
c34 c33 h33 119.0 . . ?
c33 c34 c29 117.9(6) . . ?
c33 c34 c35 120.4(5) . . ?
c29 c34 c35 121.7(5) . . ?
c34 c35 c36 110.6(5) . . ?
c34 c35 c37 110.4(5) . . ?
c36 c35 c37 110.6(5) . . ?
c34 c35 h35 108.4 . . ?
c36 c35 h35 108.4 . . ?
c37 c35 h35 108.4 . . ?
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 c40 111.3(5) . . ?
c30 c38 c39 112.3(5) . . ?
c40 c38 c39 110.6(5) . . ?
c30 c38 h38 107.5 . . ?
c40 c38 h38 107.5 . . ?
c39 c38 h38 107.5 . . ?
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 . . ?
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 . . ?
c7 n1 nb1 173.9(4) . . ?
c24 n2 c11 119.8(4) . . ?
c24 n2 nb1 109.2(3) . . ?
c11 n2 nb1 130.5(3) . . ?
c26 n3 c29 118.8(4) . . ?
c26 n3 nb1 98.4(3) . . ?
c29 n3 nb1 139.1(3) . . ?
n1 nb1 n2 107.79(18) . . ?
n1 nb1 n3 114.74(18) . . ?
n2 nb1 n3 102.36(17) . . ?
n1 nb1 c1 104.45(19) . . ?
n2 nb1 c1 113.33(18) . . ?
n3 nb1 c1 114.29(18) . . ?
n1 nb1 c26 146.90(18) . . ?
n2 nb1 c26 84.61(17) . . ?
n3 nb1 c26 32.37(16) . . ?
c1 nb1 c26 97.94(18) . . ?

_refine_diff_density_max         0.455
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.073

_shelxl_version_number           2014-1



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1459079'
_audit_update_record             
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H55 N6 Nb'
_chemical_formula_sum            'C39 H55 N6 Nb'
_chemical_formula_weight         700.80

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                   11.6490(6)
_cell_length_b                   18.9555(10)
_cell_length_c                   17.0768(9)
_cell_angle_alpha                90
_cell_angle_beta                 97.526(2)
_cell_angle_gamma                90
_cell_volume                     3738.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9865
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      25.36

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.356
_shelx_estimated_absorpt_T_min   0.871
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            41292
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.613
_diffrn_reflns_theta_max         25.382
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6818
_reflns_number_gt                5347
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0029P)²+6.8231P] 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         6818
_refine_ls_number_parameters     428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0824
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4497(2) 0.15753(17) 0.39507(16) 0.0212(7) Uani 1 1 d . . . . .
C2 C 0.4020(3) 0.22429(17) 0.40489(17) 0.0245(7) Uani 1 1 d . . . . .
H2 H 0.3421 0.2410 0.3662 0.029 Uiso 1 1 calc R U . . .
C3 C 0.4394(3) 0.26669(18) 0.46903(18) 0.0277(7) Uani 1 1 d . . . . .
H3 H 0.4057 0.3118 0.4741 0.033 Uiso 1 1 calc R U . . .
C4 C 0.5266(3) 0.24253(19) 0.52597(19) 0.0314(8) Uani 1 1 d . . . . .
H4 H 0.5531 0.2712 0.5703 0.038 Uiso 1 1 calc R U . . .
C5 C 0.5746(3) 0.17710(19) 0.51796(18) 0.0313(8) Uani 1 1 d . . . . .
H5 H 0.6342 0.1606 0.5570 0.038 Uiso 1 1 calc R U . . .
C6 C 0.5371(3) 0.13512(19) 0.45369(18) 0.0282(8) Uani 1 1 d . . . . .
H6 H 0.5714 0.0901 0.4492 0.034 Uiso 1 1 calc R U . . .
C7 C 0.5355(3) -0.02691(16) 0.25978(19) 0.0260(7) Uani 1 1 d . . . . .
C8 C 0.6233(3) -0.01193(19) 0.2032(2) 0.0371(8) Uani 1 1 d . . . . .
H8A H 0.5830 0.0055 0.1530 0.056 Uiso 1 1 calc R U . . .
H8B H 0.6650 -0.0554 0.1940 0.056 Uiso 1 1 calc R U . . .
H8C H 0.6785 0.0238 0.2263 0.056 Uiso 1 1 calc R U . . .
C9 C 0.5965(3) -0.0523(2) 0.3403(2) 0.0404(9) Uani 1 1 d . . . . .
H9A H 0.6514 -0.0163 0.3628 0.061 Uiso 1 1 calc R U . . .
H9B H 0.6383 -0.0963 0.3331 0.061 Uiso 1 1 calc R U . . .
H9C H 0.5388 -0.0607 0.3761 0.061 Uiso 1 1 calc R U . . .
C10 C 0.4465(3) -0.08145(19) 0.2248(3) 0.0501(11) Uani 1 1 d . . . . .
H10A H 0.3907 -0.0901 0.2620 0.075 Uiso 1 1 calc R U . . .
H10B H 0.4861 -0.1256 0.2152 0.075 Uiso 1 1 calc R U . . .
H10C H 0.4057 -0.0636 0.1749 0.075 Uiso 1 1 calc R U . . .
C11 C 0.4758(2) 0.16167(15) 0.15522(16) 0.0167(6) Uani 1 1 d . . . . .
C12 C 0.5911(2) 0.18134(16) 0.17929(17) 0.0188(6) Uani 1 1 d . . . . .
C13 C 0.6731(3) 0.16781(16) 0.12824(18) 0.0243(7) Uani 1 1 d . . . . .
H13 H 0.7516 0.1807 0.1438 0.029 Uiso 1 1 calc R U . . .
C14 C 0.6427(3) 0.13619(17) 0.05599(18) 0.0259(7) Uani 1 1 d . . . . .
H14 H 0.7001 0.1263 0.0228 0.031 Uiso 1 1 calc R U . . .
C15 C 0.5283(3) 0.11886(16) 0.03191(18) 0.0243(7) Uani 1 1 d . . . . .
H15 H 0.5074 0.0980 -0.0185 0.029 Uiso 1 1 calc R U . . .
C16 C 0.4431(2) 0.13152(16) 0.08027(17) 0.0187(6) Uani 1 1 d . . . . .
C17 C 0.3175(2) 0.11367(16) 0.04919(17) 0.0219(7) Uani 1 1 d . . . . .
H17 H 0.2689 0.1237 0.0920 0.026 Uiso 1 1 calc R U . . .
C18 C 0.2731(3) 0.15937(19) -0.02233(19) 0.0331(8) Uani 1 1 d . . . . .
H18A H 0.2776 0.2092 -0.0071 0.050 Uiso 1 1 calc R U . . .
H18B H 0.1925 0.1470 -0.0410 0.050 Uiso 1 1 calc R U . . .
H18C H 0.3208 0.1512 -0.0646 0.050 Uiso 1 1 calc R U . . .
C19 C 0.3039(3) 0.03565(18) 0.0273(2) 0.0316(8) Uani 1 1 d . . . . .
H19A H 0.3514 0.0246 -0.0144 0.047 Uiso 1 1 calc R U . . .
H19B H 0.2224 0.0256 0.0084 0.047 Uiso 1 1 calc R U . . .
H19C H 0.3291 0.0067 0.0739 0.047 Uiso 1 1 calc R U . . .
C20 C 0.6316(2) 0.21702(16) 0.25807(17) 0.0224(7) Uani 1 1 d . . . . .
H20 H 0.5617 0.2275 0.2843 0.027 Uiso 1 1 calc R U . . .
C21 C 0.6939(3) 0.28712(17) 0.24742(19) 0.0288(8) Uani 1 1 d . . . . .
H21A H 0.7670 0.2778 0.2268 0.043 Uiso 1 1 calc R U . . .
H21B H 0.7097 0.3112 0.2985 0.043 Uiso 1 1 calc R U . . .
H21C H 0.6447 0.3171 0.2102 0.043 Uiso 1 1 calc R U . . .
C22 C 0.7102(3) 0.16794(18) 0.31223(18) 0.0281(8) Uani 1 1 d . . . . .
H22A H 0.6700 0.1232 0.3182 0.042 Uiso 1 1 calc R U . . .
H22B H 0.7293 0.1901 0.3641 0.042 Uiso 1 1 calc R U . . .
H22C H 0.7815 0.1590 0.2891 0.042 Uiso 1 1 calc R U . . .
C23 C 0.3775(3) 0.29450(16) 0.15365(18) 0.0229(7) Uani 1 1 d . . . . .
H23A H 0.4550 0.3049 0.1810 0.034 Uiso 1 1 calc R U . . .
H23B H 0.3281 0.3362 0.1549 0.034 Uiso 1 1 calc R U . . .
H23C H 0.3831 0.2818 0.0987 0.034 Uiso 1 1 calc R U . . .
C24 C 0.3257(2) 0.23373(15) 0.19433(15) 0.0158(6) Uani 1 1 d . . . . .
C25 C 0.2172(2) 0.24439(15) 0.21643(16) 0.0158(6) Uani 1 1 d . . . . .
H25 H 0.1894 0.2915 0.2127 0.019 Uiso 1 1 calc R U . . .
C26 C 0.1422(2) 0.19416(16) 0.24387(16) 0.0182(6) Uani 1 1 d . . . . .
C27 C 0.0168(2) 0.21692(17) 0.23967(17) 0.0224(7) Uani 1 1 d . . . . .
H27A H -0.0338 0.1768 0.2235 0.034 Uiso 1 1 calc R U . . .
H27B H 0.0013 0.2552 0.2011 0.034 Uiso 1 1 calc R U . . .
H27C H 0.0018 0.2335 0.2917 0.034 Uiso 1 1 calc R U . . .
C28 C 0.0874(2) 0.08555(16) 0.29634(16) 0.0186(7) Uani 1 1 d . . . . .
C29 C 0.0488(2) 0.09675(17) 0.36970(16) 0.0193(6) Uani 1 1 d . . . . .
C30 C -0.0344(3) 0.04981(18) 0.39118(18) 0.0262(7) Uani 1 1 d . . . . .
H30 H -0.0615 0.0555 0.4409 0.031 Uiso 1 1 calc R U . . .
C31 C -0.0783(3) -0.00434(18) 0.34235(19) 0.0284(8) Uani 1 1 d . . . . .
H31 H -0.1364 -0.0345 0.3579 0.034 Uiso 1 1 calc R U . . .
C32 C -0.0378(3) -0.01468(17) 0.27096(18) 0.0266(7) Uani 1 1 d . . . . .
H32 H -0.0678 -0.0524 0.2378 0.032 Uiso 1 1 calc R U . . .
C33 C 0.0469(2) 0.02948(16) 0.24668(17) 0.0216(7) Uani 1 1 d . . . . .
C34 C 0.0937(3) 0.15536(17) 0.42611(17) 0.0241(7) Uani 1 1 d . . . . .
H34 H 0.1392 0.1887 0.3968 0.029 Uiso 1 1 calc R U . . .
C35 C 0.1743(3) 0.12780(19) 0.49764(18) 0.0352(8) Uani 1 1 d . . . . .
H35A H 0.1339 0.0917 0.5248 0.053 Uiso 1 1 calc R U . . .
H35B H 0.1969 0.1669 0.5340 0.053 Uiso 1 1 calc R U . . .
H35C H 0.2436 0.1072 0.4799 0.053 Uiso 1 1 calc R U . . .
C36 C -0.0062(3) 0.1972(2) 0.4549(2) 0.0381(9) Uani 1 1 d . . . . .
H36A H -0.0565 0.2162 0.4093 0.057 Uiso 1 1 calc R U . . .
H36B H 0.0255 0.2361 0.4889 0.057 Uiso 1 1 calc R U . . .
H36C H -0.0513 0.1658 0.4849 0.057 Uiso 1 1 calc R U . . .
C37 C 0.0880(3) 0.01759(17) 0.16710(17) 0.0249(7) Uani 1 1 d . . . . .
H37 H 0.1669 0.0388 0.1696 0.030 Uiso 1 1 calc R U . . .
C38 C 0.0089(3) 0.0566(2) 0.10247(18) 0.0387(9) Uani 1 1 d . . . . .
H38A H -0.0699 0.0378 0.0994 0.058 Uiso 1 1 calc R U . . .
H38B H 0.0378 0.0500 0.0516 0.058 Uiso 1 1 calc R U . . .
H38C H 0.0083 0.1070 0.1151 0.058 Uiso 1 1 calc R U . . .
C39 C 0.0982(3) -0.06018(18) 0.1458(2) 0.0383(9) Uani 1 1 d . . . . .
H39A H 0.1445 -0.0849 0.1894 0.057 Uiso 1 1 calc R U . . .
H39B H 0.1359 -0.0643 0.0980 0.057 Uiso 1 1 calc R U . . .
H39C H 0.0208 -0.0812 0.1363 0.057 Uiso 1 1 calc R U . . .
N1 N 0.4745(2) 0.03855(13) 0.27437(14) 0.0213(6) Uani 1 1 d . . . . .
N2 N 0.38629(18) 0.17242(12) 0.20634(13) 0.0149(5) Uani 1 1 d . . . . .
N3 N 0.17648(19) 0.13139(13) 0.27150(13) 0.0158(5) Uani 1 1 d . . . . .
N4 N 0.2983(2) 0.02389(15) 0.36580(15) 0.0292(6) Uani 1 1 d . . . . .
N5 N 0.2517(2) -0.01574(14) 0.40619(15) 0.0230(6) Uani 1 1 d . . . . .
N6 N 0.2074(2) -0.05361(15) 0.44521(16) 0.0342(7) Uani 1 1 d . . . . .
Nb1 Nb 0.36594(2) 0.09755(2) 0.29675(2) 0.01718(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
C1 C6 1.397(4) . ?
C1 C2 1.401(4) . ?
C1 Nb1 2.153(3) . ?
C2 C3 1.382(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 N1 1.468(4) . ?
C7 C8 1.522(4) . ?
C7 C10 1.529(5) . ?
C7 C9 1.540(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.402(4) . ?
C11 C16 1.408(4) . ?
C11 N2 1.459(3) . ?
C12 C13 1.400(4) . ?
C12 C20 1.524(4) . ?
C13 C14 1.376(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.392(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.528(4) . ?
C17 C19 1.529(4) . ?
C17 C18 1.531(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.529(4) . ?
C20 C21 1.536(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.511(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N2 1.361(4) . ?
C24 C25 1.381(4) . ?
C25 C26 1.413(4) . ?
C25 H25 0.9500 . ?
C26 N3 1.322(4) . ?
C26 C27 1.516(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.402(4) . ?
C28 C33 1.402(4) . ?
C28 N3 1.458(3) . ?
C29 C30 1.400(4) . ?
C29 C34 1.518(4) . ?
C30 C31 1.378(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.378(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.397(4) . ?
C32 H32 0.9500 . ?
C33 C37 1.515(4) . ?
C34 C35 1.531(4) . ?
C34 C36 1.542(4) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C39 1.527(5) . ?
C37 C38 1.532(4) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
N1 Nb1 1.767(2) . ?
N2 Nb1 2.133(2) . ?
N3 Nb1 2.285(2) . ?
N4 N5 1.197(3) . ?
N4 Nb1 2.050(3) . ?
N5 N6 1.147(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 116.9(3) . . ?
C6 C1 Nb1 127.7(2) . . ?
C2 C1 Nb1 115.1(2) . . ?
C3 C2 C1 122.1(3) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 121.3(3) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
N1 C7 C8 109.3(3) . . ?
N1 C7 C10 108.6(3) . . ?
C8 C7 C10 110.8(3) . . ?
N1 C7 C9 106.9(3) . . ?
C8 C7 C9 110.8(3) . . ?
C10 C7 C9 110.3(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 120.6(3) . . ?
C12 C11 N2 121.3(2) . . ?
C16 C11 N2 118.1(2) . . ?
C13 C12 C11 118.3(3) . . ?
C13 C12 C20 118.2(3) . . ?
C11 C12 C20 123.4(2) . . ?
C14 C13 C12 121.5(3) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C15 119.7(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C14 C15 C16 121.1(3) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C15 C16 C11 118.7(3) . . ?
C15 C16 C17 118.7(3) . . ?
C11 C16 C17 122.6(2) . . ?
C16 C17 C19 111.3(2) . . ?
C16 C17 C18 111.1(2) . . ?
C19 C17 C18 109.8(3) . . ?
C16 C17 H17 108.2 . . ?
C19 C17 H17 108.2 . . ?
C18 C17 H17 108.2 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C20 C22 110.8(3) . . ?
C12 C20 C21 112.1(2) . . ?
C22 C20 C21 110.1(2) . . ?
C12 C20 H20 107.9 . . ?
C22 C20 H20 107.9 . . ?
C21 C20 H20 107.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 C25 124.0(3) . . ?
N2 C24 C23 119.3(2) . . ?
C25 C24 C23 116.7(3) . . ?
C24 C25 C26 128.3(3) . . ?
C24 C25 H25 115.8 . . ?
C26 C25 H25 115.8 . . ?
N3 C26 C25 123.6(3) . . ?
N3 C26 C27 121.1(3) . . ?
C25 C26 C27 115.2(3) . . ?
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 . . ?
C29 C28 C33 122.2(3) . . ?
C29 C28 N3 119.6(3) . . ?
C33 C28 N3 118.1(2) . . ?
C30 C29 C28 116.9(3) . . ?
C30 C29 C34 119.5(3) . . ?
C28 C29 C34 123.6(3) . . ?
C31 C30 C29 122.0(3) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C30 C31 C32 119.9(3) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C33 121.0(3) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C32 C33 C28 118.0(3) . . ?
C32 C33 C37 119.7(3) . . ?
C28 C33 C37 122.3(3) . . ?
C29 C34 C35 112.4(3) . . ?
C29 C34 C36 111.5(2) . . ?
C35 C34 C36 109.3(3) . . ?
C29 C34 H34 107.8 . . ?
C35 C34 H34 107.8 . . ?
C36 C34 H34 107.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 C39 113.6(3) . . ?
C33 C37 C38 110.1(3) . . ?
C39 C37 C38 110.7(3) . . ?
C33 C37 H37 107.4 . . ?
C39 C37 H37 107.4 . . ?
C38 C37 H37 107.4 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C7 N1 Nb1 161.5(2) . . ?
C24 N2 C11 115.2(2) . . ?
C24 N2 Nb1 124.94(17) . . ?
C11 N2 Nb1 119.74(17) . . ?
C26 N3 C28 116.5(2) . . ?
C26 N3 Nb1 124.01(18) . . ?
C28 N3 Nb1 118.97(17) . . ?
N5 N4 Nb1 175.0(2) . . ?
N6 N5 N4 179.6(4) . . ?
N1 Nb1 N4 91.90(11) . . ?
N1 Nb1 N2 96.55(10) . . ?
N4 Nb1 N2 163.11(9) . . ?
N1 Nb1 C1 103.82(11) . . ?
N4 Nb1 C1 94.60(11) . . ?
N2 Nb1 C1 97.53(10) . . ?
N1 Nb1 N3 146.91(10) . . ?
N4 Nb1 N3 82.26(9) . . ?
N2 Nb1 N3 82.69(8) . . ?
C1 Nb1 N3 109.08(10) . . ?

_refine_diff_density_max         0.570
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.073



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1459080'
_audit_update_record             
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H49 N3 Nb'
_chemical_formula_weight         640.71

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      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

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

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

_cell_length_a                   12.4801(5)
_cell_length_b                   13.7720(5)
_cell_length_c                   19.2824(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3314.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9894
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      25.38

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_F_000             1356
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    0.393
_shelx_estimated_absorpt_T_min   0.798
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            56485
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.1267
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.817
_diffrn_reflns_theta_max         25.400
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3160
_reflns_number_gt                2980
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0335P)²+6.8797P] 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         3160
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2852(3) 0.5801(3) 0.0000 0.0226(8) Uani 1 2 d S T P . .
C2 C 0.3056(4) 0.6769(4) 0.0000 0.084(3) Uani 1 2 d S T P . .
H2 H 0.3780 0.6980 0.0000 0.101 Uiso 1 2 calc R U P . .
C3 C 0.2246(4) 0.7467(4) 0.0000 0.111(4) Uani 1 2 d S T P . .
H3 H 0.2432 0.8136 0.0000 0.133 Uiso 1 2 calc R U P . .
C4 C 0.1204(3) 0.7210(3) 0.0000 0.0412(11) Uani 1 2 d S T P . .
H4 H 0.0653 0.7686 0.0000 0.049 Uiso 1 2 calc R U P . .
C5 C 0.0969(3) 0.6245(4) 0.0000 0.0515(14) Uani 1 2 d S T P . .
H5 H 0.0242 0.6038 0.0000 0.062 Uiso 1 2 calc R U P . .
C6 C 0.1781(4) 0.5563(3) 0.0000 0.0543(15) Uani 1 2 d S T P . .
H6 H 0.1591 0.4895 0.0000 0.065 Uiso 1 2 calc R U P . .
C7 C 0.3610(2) 0.35066(19) 0.14605(13) 0.0238(5) Uani 1 1 d . . . . .
C8 C 0.4264(3) 0.2711(2) 0.16247(15) 0.0345(7) Uani 1 1 d . . . . .
C9 C 0.4515(3) 0.2550(2) 0.23196(16) 0.0427(8) Uani 1 1 d . . . . .
H9 H 0.4945 0.2007 0.2441 0.051 Uiso 1 1 calc R U . . .
C10 C 0.4153(3) 0.3158(3) 0.28305(16) 0.0442(8) Uani 1 1 d . . . . .
H10 H 0.4305 0.3019 0.3303 0.053 Uiso 1 1 calc R U . . .
C11 C 0.3572(2) 0.3968(3) 0.26570(15) 0.0379(7) Uani 1 1 d . . . . .
H11 H 0.3354 0.4403 0.3013 0.045 Uiso 1 1 calc R U . . .
C12 C 0.3295(2) 0.4169(2) 0.19713(14) 0.0272(6) Uani 1 1 d . . . . .
C13 C 0.4660(4) 0.2023(2) 0.10706(17) 0.0593(12) Uani 1 1 d . . . . .
H13 H 0.4706 0.2398 0.0628 0.071 Uiso 1 1 calc R U . . .
C14 C 0.3902(5) 0.1171(3) 0.0945(3) 0.105(2) Uani 1 1 d . . . . .
H14A H 0.4198 0.0751 0.0582 0.158 Uiso 1 1 calc R U . . .
H14B H 0.3820 0.0798 0.1375 0.158 Uiso 1 1 calc R U . . .
H14C H 0.3201 0.1417 0.0798 0.158 Uiso 1 1 calc R U . . .
C15 C 0.5770(5) 0.1625(4) 0.1223(2) 0.0914(19) Uani 1 1 d . . . . .
H15A H 0.5987 0.1185 0.0849 0.137 Uiso 1 1 calc R U . . .
H15B H 0.6281 0.2164 0.1254 0.137 Uiso 1 1 calc R U . . .
H15C H 0.5758 0.1271 0.1663 0.137 Uiso 1 1 calc R U . . .
C16 C 0.2655(2) 0.5072(2) 0.18069(15) 0.0344(7) Uani 1 1 d . . . . .
H16 H 0.2670 0.5150 0.1291 0.041 Uiso 1 1 calc R U . . .
C17 C 0.1495(3) 0.5004(4) 0.2013(3) 0.0832(16) Uani 1 1 d . . . . .
H17A H 0.1181 0.4413 0.1815 0.125 Uiso 1 1 calc R U . . .
H17B H 0.1439 0.4981 0.2520 0.125 Uiso 1 1 calc R U . . .
H17C H 0.1108 0.5573 0.1838 0.125 Uiso 1 1 calc R U . . .
C18 C 0.3145(3) 0.5973(3) 0.2107(3) 0.0849(17) Uani 1 1 d . . . . .
H18A H 0.3900 0.6012 0.1970 0.127 Uiso 1 1 calc R U . . .
H18B H 0.2762 0.6545 0.1932 0.127 Uiso 1 1 calc R U . . .
H18C H 0.3093 0.5953 0.2614 0.127 Uiso 1 1 calc R U . . .
C30 C 0.4052(3) 0.5018(3) 0.46400(19) 0.0494(9) Uani 1 1 d . . . . .
H19 H 0.3394 0.5030 0.4392 0.059 Uiso 1 1 calc R U . . .
C19 C 0.1850(3) 0.2945(3) 0.0000 0.0266(8) Uani 1 2 d S T P . .
H20 H 0.1139 0.2700 0.0000 0.032 Uiso 1 2 calc R U P . .
C20 C 0.2297(2) 0.30999(18) 0.06478(14) 0.0260(6) Uani 1 1 d . . . . .
C21 C 0.1672(3) 0.2653(3) 0.12397(18) 0.0597(12) Uani 1 1 d . . . . .
H22A H 0.1035 0.2325 0.1056 0.090 Uiso 1 1 calc R U . . .
H22B H 0.2124 0.2181 0.1483 0.090 Uiso 1 1 calc R U . . .
H22C H 0.1452 0.3164 0.1563 0.090 Uiso 1 1 calc R U . . .
C31 C 0.5000 0.5000 0.4290(3) 0.0544(14) Uani 1 2 d S T P . .
H25 H 0.5000 0.5000 0.3798 0.065 Uiso 1 2 calc R U P . .
N1 N 0.5000 0.5000 0.07195(16) 0.0244(7) Uani 1 2 d S T P . .
N2 N 0.32093(16) 0.35944(14) 0.07590(11) 0.0195(4) Uani 1 1 d . . . . .
Nb1 Nb 0.39763(2) 0.46044(2) 0.0000 0.01496(12) Uani 1 2 d S T P . .


_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 1.356(6) . ?
C1 C6 1.376(6) . ?
C1 Nb1 2.165(4) . ?
C2 C3 1.395(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.347(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.362(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.403(4) . ?
C7 C12 1.399(4) . ?
C7 N2 1.447(3) . ?
C8 C9 1.394(4) . ?
C8 C13 1.511(4) . ?
C9 C10 1.369(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(4) . ?
C11 H11 0.9500 . ?
C12 C16 1.512(4) . ?
C13 C14 1.526(7) . ?
C13 C15 1.518(6) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C18 1.500(5) . ?
C16 C17 1.505(5) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C30 C31 1.362(4) . ?
C30 C30 1.388(7) 6_556 ?
C30 H19 0.9500 . ?
C19 C20 1.385(3) . ?
C19 C20 1.385(3) 6 ?
C19 H20 0.9500 . ?
C20 N2 1.344(3) . ?
C20 C21 1.513(4) . ?
C21 H22A 0.9800 . ?
C21 H22B 0.9800 . ?
C21 H22C 0.9800 . ?
C31 C30 1.362(4) 2_665 ?
C31 H25 0.9500 . ?
N1 Nb1 1.963(2) 5_665 ?
N1 Nb1 1.963(2) . ?
N2 Nb1 2.235(2) . ?
Nb1 N1 1.963(2) 5_665 ?
Nb1 N2 2.235(2) 6 ?
Nb1 Nb1 2.7778(6) 5_665 ?

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 C6 114.6(4) . . ?
C2 C1 Nb1 128.8(3) . . ?
C6 C1 Nb1 116.6(3) . . ?
C1 C2 C3 122.8(4) . . ?
C1 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C4 C3 C2 121.2(5) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 117.7(4) . . ?
C3 C4 H4 121.1 . . ?
C5 C4 H4 121.1 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 123.4(4) . . ?
C1 C6 H6 118.3 . . ?
C5 C6 H6 118.3 . . ?
C8 C7 C12 120.9(3) . . ?
C8 C7 N2 118.5(2) . . ?
C12 C7 N2 120.4(2) . . ?
C9 C8 C7 118.1(3) . . ?
C9 C8 C13 120.5(3) . . ?
C7 C8 C13 121.4(3) . . ?
C10 C9 C8 121.4(3) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C9 C10 C11 119.7(3) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 121.6(3) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C7 118.0(3) . . ?
C11 C12 C16 119.5(3) . . ?
C7 C12 C16 122.5(2) . . ?
C8 C13 C14 113.1(4) . . ?
C8 C13 C15 112.8(3) . . ?
C14 C13 C15 108.6(3) . . ?
C8 C13 H13 107.3 . . ?
C14 C13 H13 107.3 . . ?
C15 C13 H13 107.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C16 C17 110.0(3) . . ?
C18 C16 C12 112.6(3) . . ?
C17 C16 C12 113.7(3) . . ?
C18 C16 H16 106.7 . . ?
C17 C16 H16 106.7 . . ?
C12 C16 H16 106.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C31 C30 C30 119.7(2) . 6_556 ?
C31 C30 H19 120.2 . . ?
C30 C30 H19 120.2 6_556 . ?
C20 C19 C20 128.9(3) . 6 ?
C20 C19 H20 115.5 . . ?
C20 C19 H20 115.5 6 . ?
N2 C20 C19 124.3(2) . . ?
N2 C20 C21 121.5(3) . . ?
C19 C20 C21 114.2(3) . . ?
C20 C21 H22A 109.5 . . ?
C20 C21 H22B 109.5 . . ?
H22A C21 H22B 109.5 . . ?
C20 C21 H22C 109.5 . . ?
H22A C21 H22C 109.5 . . ?
H22B C21 H22C 109.5 . . ?
C30 C31 C30 120.6(5) . 2_665 ?
C30 C31 H25 119.7 . . ?
C30 C31 H25 119.7 2_665 . ?
Nb1 N1 Nb1 90.07(13) 5_665 . ?
C20 N2 C7 113.5(2) . . ?
C20 N2 Nb1 125.03(17) . . ?
C7 N2 Nb1 121.08(15) . . ?
N1 Nb1 N1 89.93(13) 5_665 . ?
N1 Nb1 C1 102.15(7) 5_665 . ?
N1 Nb1 C1 102.15(7) . . ?
N1 Nb1 N2 156.12(5) 5_665 . ?
N1 Nb1 N2 89.35(8) . . ?
C1 Nb1 N2 101.33(9) . . ?
N1 Nb1 N2 89.35(8) 5_665 6 ?
N1 Nb1 N2 156.12(5) . 6 ?
C1 Nb1 N2 101.33(9) . 6 ?
N2 Nb1 N2 81.83(10) . 6 ?
N1 Nb1 Nb1 44.97(6) 5_665 5_665 ?
N1 Nb1 Nb1 44.97(6) . 5_665 ?
C1 Nb1 Nb1 107.31(10) . 5_665 ?
N2 Nb1 Nb1 129.66(5) . 5_665 ?
N2 Nb1 Nb1 129.66(5) 6 5_665 ?

_refine_diff_density_max         0.831
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.097



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1459081'
_audit_update_record             
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H54 B F15 N4 Nb, C4 H12 N, C6 H6'
_chemical_formula_sum            'C67 H72 B F15 N5 Nb'
_chemical_formula_weight         1336.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.5396(9)
_cell_length_b                   17.4757(11)
_cell_length_c                   29.990(2)
_cell_angle_alpha                84.127(3)
_cell_angle_beta                 82.987(3)
_cell_angle_gamma                73.602(3)
_cell_volume                     6241.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9980
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.43

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_F_000             2760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.283
_shelx_estimated_absorpt_T_min   0.871
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6271
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            58734
_diffrn_reflns_av_unetI/netI     0.1330
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.354
_diffrn_reflns_theta_max         25.475
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             22438
_reflns_number_gt                13166
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-2014
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0857P)²+14.4699P] 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         22438
_refine_ls_number_parameters     1666
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.0799
_refine_ls_wR_factor_ref         0.2127
_refine_ls_wR_factor_gt          0.1818
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0001(5) 0.8387(4) 0.5313(2) 0.0240(15) Uani 1 1 d . . . . .
C2 C -0.0184(6) 0.8604(4) 0.4815(2) 0.0374(19) Uani 1 1 d . . . . .
H2A H 0.0534 0.8589 0.4640 0.056 Uiso 1 1 calc R U . . .
H2B H -0.0691 0.9143 0.4781 0.056 Uiso 1 1 calc R U . . .
H2C H -0.0511 0.8220 0.4706 0.056 Uiso 1 1 calc R U . . .
C3 C 0.0343(5) 0.9068(4) 0.5484(2) 0.0253(15) Uani 1 1 d . . . . .
H3A H 0.0522 0.8930 0.5797 0.038 Uiso 1 1 calc R U . . .
H3B H -0.0273 0.9559 0.5470 0.038 Uiso 1 1 calc R U . . .
H3C H 0.1002 0.9153 0.5296 0.038 Uiso 1 1 calc R U . . .
C4 C -0.1082(6) 0.8314(4) 0.5582(3) 0.041(2) Uani 1 1 d . . . . .
H4A H -0.1362 0.7926 0.5451 0.062 Uiso 1 1 calc R U . . .
H4B H -0.1638 0.8837 0.5573 0.062 Uiso 1 1 calc R U . . .
H4C H -0.0942 0.8134 0.5895 0.062 Uiso 1 1 calc R U . . .
C5 C 0.0879(5) 0.7022(4) 0.5091(2) 0.0221(15) Uani 1 1 d . . . . .
C6 C 0.1563(5) 0.6893(4) 0.4693(2) 0.0292(16) Uani 1 1 d . . . . .
H6 H 0.2077 0.7202 0.4608 0.035 Uiso 1 1 calc R U . . .
C7 C 0.1512(6) 0.6310(5) 0.4413(2) 0.040(2) Uani 1 1 d . . . . .
H7 H 0.2007 0.6212 0.4146 0.048 Uiso 1 1 calc R U . . .
C8 C 0.0745(7) 0.5886(4) 0.4527(3) 0.044(2) Uani 1 1 d . . . . .
H8 H 0.0686 0.5507 0.4332 0.053 Uiso 1 1 calc R U . . .
C9 C 0.0054(6) 0.6004(4) 0.4924(3) 0.039(2) Uani 1 1 d . . . . .
H9 H -0.0464 0.5695 0.5003 0.047 Uiso 1 1 calc R U . . .
C10 C 0.0106(5) 0.6567(4) 0.5208(2) 0.0297(16) Uani 1 1 d . . . . .
H10 H -0.0374 0.6645 0.5480 0.036 Uiso 1 1 calc R U . . .
C11 C 0.4443(5) 0.7697(4) 0.5413(2) 0.0246(15) Uani 1 1 d . . . . .
C12 C 0.5398(5) 0.7524(4) 0.5661(2) 0.0301(16) Uani 1 1 d . . . . .
C13 C 0.6081(6) 0.8048(5) 0.5571(3) 0.0398(19) Uani 1 1 d . . . . .
H13 H 0.6717 0.7953 0.5732 0.048 Uiso 1 1 calc R U . . .
C14 C 0.5868(6) 0.8687(5) 0.5260(3) 0.0396(19) Uani 1 1 d . . . . .
H14 H 0.6345 0.9030 0.5212 0.048 Uiso 1 1 calc R U . . .
C15 C 0.4958(6) 0.8834(4) 0.5015(2) 0.0349(18) Uani 1 1 d . . . . .
H15 H 0.4824 0.9273 0.4795 0.042 Uiso 1 1 calc R U . . .
C16 C 0.4223(5) 0.8343(4) 0.5087(2) 0.0263(16) Uani 1 1 d . . . . .
C17 C 0.5751(6) 0.6810(5) 0.5984(2) 0.0359(18) Uani 1 1 d . . . . .
H17 H 0.5153 0.6525 0.6023 0.043 Uiso 1 1 calc R U . . .
C18 C 0.5908(6) 0.7021(5) 0.6447(2) 0.045(2) Uani 1 1 d . . . . .
H18A H 0.6488 0.7304 0.6419 0.068 Uiso 1 1 calc R U . . .
H18B H 0.6134 0.6530 0.6643 0.068 Uiso 1 1 calc R U . . .
H18C H 0.5204 0.7364 0.6579 0.068 Uiso 1 1 calc R U . . .
C19 C 0.6842(6) 0.6227(5) 0.5792(3) 0.048(2) Uani 1 1 d . . . . .
H19A H 0.6717 0.6039 0.5511 0.071 Uiso 1 1 calc R U . . .
H19B H 0.7070 0.5769 0.6010 0.071 Uiso 1 1 calc R U . . .
H19C H 0.7430 0.6503 0.5732 0.071 Uiso 1 1 calc R U . . .
C20 C 0.3288(5) 0.8502(4) 0.4795(2) 0.0285(16) Uani 1 1 d . . . . .
H20 H 0.2698 0.8269 0.4960 0.034 Uiso 1 1 calc R U . . .
C21 C 0.2751(6) 0.9392(4) 0.4685(3) 0.0384(18) Uani 1 1 d . . . . .
H21A H 0.2542 0.9667 0.4964 0.058 Uiso 1 1 calc R U . . .
H21B H 0.2082 0.9457 0.4530 0.058 Uiso 1 1 calc R U . . .
H21C H 0.3283 0.9622 0.4489 0.058 Uiso 1 1 calc R U . . .
C22 C 0.3684(6) 0.8088(5) 0.4350(2) 0.0377(18) Uani 1 1 d . . . . .
H22A H 0.4229 0.8330 0.4171 0.057 Uiso 1 1 calc R U . . .
H22B H 0.3042 0.8153 0.4179 0.057 Uiso 1 1 calc R U . . .
H22C H 0.4032 0.7517 0.4417 0.057 Uiso 1 1 calc R U . . .
C23 C 0.5104(6) 0.6280(4) 0.4981(2) 0.0314(17) Uani 1 1 d . . . . .
H23A H 0.5565 0.6634 0.4934 0.038 Uiso 1 1 calc R U . . .
H23B H 0.5320 0.5792 0.4837 0.038 Uiso 1 1 calc R U . . .
C24 C 0.4159(5) 0.6466(4) 0.5247(2) 0.0238(15) Uani 1 1 d . . . . .
C25 C 0.3453(5) 0.5896(4) 0.5297(2) 0.0211(14) Uani 1 1 d . . . . .
H25 H 0.3474 0.5643 0.5029 0.025 Uiso 1 1 calc R U . . .
C26 C 0.2792(5) 0.5667(4) 0.5642(2) 0.0224(15) Uani 1 1 d . . . . .
C27 C 0.2320(5) 0.4987(4) 0.5589(2) 0.0286(16) Uani 1 1 d . . . . .
H27A H 0.2479 0.4843 0.5276 0.043 Uiso 1 1 calc R U . . .
H27B H 0.1510 0.5149 0.5668 0.043 Uiso 1 1 calc R U . . .
H27C H 0.2661 0.4525 0.5788 0.043 Uiso 1 1 calc R U . . .
C28 C 0.2423(5) 0.5543(4) 0.6443(2) 0.0239(15) Uani 1 1 d . . . . .
C29 C 0.3422(6) 0.4970(4) 0.6572(2) 0.0319(17) Uani 1 1 d . . . . .
C30 C 0.3349(7) 0.4410(5) 0.6922(3) 0.044(2) Uani 1 1 d . . . . .
H30 H 0.4015 0.4037 0.7010 0.053 Uiso 1 1 calc R U . . .
C31 C 0.2350(8) 0.4371(5) 0.7147(3) 0.058(2) Uani 1 1 d . . . . .
H31 H 0.2310 0.3958 0.7375 0.069 Uiso 1 1 calc R U . . .
C32 C 0.1403(7) 0.4945(5) 0.7034(3) 0.049(2) Uani 1 1 d . . . . .
H32 H 0.0711 0.4938 0.7201 0.059 Uiso 1 1 calc R U . . .
C33 C 0.1413(6) 0.5539(4) 0.6687(2) 0.0345(18) Uani 1 1 d . . . . .
C34 C 0.0304(6) 0.6135(4) 0.6588(2) 0.0334(18) Uani 1 1 d . . . . .
H34 H 0.0465 0.6562 0.6363 0.040 Uiso 1 1 calc R U . . .
C35 C -0.0434(6) 0.5721(5) 0.6382(3) 0.044(2) Uani 1 1 d . . . . .
H35A H -0.0061 0.5518 0.6094 0.066 Uiso 1 1 calc R U . . .
H35B H -0.1154 0.6107 0.6332 0.066 Uiso 1 1 calc R U . . .
H35C H -0.0557 0.5275 0.6588 0.066 Uiso 1 1 calc R U . . .
C36 C -0.0314(6) 0.6527(5) 0.7004(3) 0.043(2) Uani 1 1 d . . . . .
H36A H -0.0486 0.6118 0.7228 0.065 Uiso 1 1 calc R U . . .
H36B H -0.1011 0.6915 0.6926 0.065 Uiso 1 1 calc R U . . .
H36C H 0.0151 0.6802 0.7129 0.065 Uiso 1 1 calc R U . . .
C37 C 0.4563(6) 0.4950(5) 0.6332(2) 0.0396(19) Uani 1 1 d . . . . .
H37 H 0.4481 0.5402 0.6094 0.047 Uiso 1 1 calc R U . . .
C38 C 0.5347(6) 0.5047(5) 0.6662(2) 0.0404(19) Uani 1 1 d . . . . .
H38A H 0.5032 0.5557 0.6800 0.061 Uiso 1 1 calc R U . . .
H38B H 0.6078 0.5038 0.6500 0.061 Uiso 1 1 calc R U . . .
H38C H 0.5434 0.4607 0.6897 0.061 Uiso 1 1 calc R U . . .
C39 C 0.5068(7) 0.4157(5) 0.6107(3) 0.060(3) Uani 1 1 d . . . . .
H39A H 0.5176 0.3711 0.6339 0.090 Uiso 1 1 calc R U . . .
H39B H 0.5790 0.4162 0.5941 0.090 Uiso 1 1 calc R U . . .
H39C H 0.4560 0.4094 0.5898 0.090 Uiso 1 1 calc R U . . .
C40 C 0.1854(5) 0.7816(4) 0.7097(2) 0.0227(15) Uani 1 1 d . . . . .
C41 C 0.2639(5) 0.7059(4) 0.7117(2) 0.0252(15) Uani 1 1 d . . . . .
C42 C 0.2705(6) 0.6531(4) 0.7491(2) 0.0317(17) Uani 1 1 d . . . . .
C43 C 0.2035(6) 0.6722(4) 0.7872(2) 0.0318(17) Uani 1 1 d . . . . .
C44 C 0.1280(5) 0.7476(4) 0.7880(2) 0.0292(17) Uani 1 1 d . . . . .
C45 C 0.1205(5) 0.7984(4) 0.7496(2) 0.0277(16) Uani 1 1 d . . . . .
C46 C 0.0622(5) 0.9125(4) 0.6643(2) 0.0237(15) Uani 1 1 d . . . . .
C47 C -0.0375(6) 0.8918(4) 0.6652(2) 0.0323(17) Uani 1 1 d . . . . .
C48 C -0.1404(6) 0.9468(5) 0.6661(3) 0.041(2) Uani 1 1 d . . . . .
C49 C -0.1503(7) 1.0261(5) 0.6642(3) 0.047(2) Uani 1 1 d . . . . .
C50 C -0.0551(8) 1.0503(4) 0.6635(2) 0.044(2) Uani 1 1 d . . . . .
C51 C 0.0472(6) 0.9941(4) 0.6642(2) 0.0301(16) Uani 1 1 d . . . . .
C52 C 0.2899(5) 0.8787(4) 0.6544(2) 0.0241(15) Uani 1 1 d . . . . .
C53 C 0.3030(6) 0.9257(4) 0.6154(2) 0.0321(17) Uani 1 1 d . . . . .
C54 C 0.3877(7) 0.9622(5) 0.6051(2) 0.040(2) Uani 1 1 d . . . . .
C55 C 0.4707(6) 0.9478(5) 0.6333(3) 0.043(2) Uani 1 1 d . . . . .
C56 C 0.4626(6) 0.9034(5) 0.6721(3) 0.043(2) Uani 1 1 d . . . . .
C57 C 0.3727(6) 0.8697(4) 0.6827(2) 0.0311(17) Uani 1 1 d . . . . .
C100 C 1.0282(5) 0.1685(4) 0.9397(2) 0.0255(16) Uani 1 1 d . . . . .
C101 C 1.1215(6) 0.1861(4) 0.9619(3) 0.0379(18) Uani 1 1 d . . . . .
H10A H 1.1339 0.2369 0.9487 0.057 Uiso 1 1 calc R U . . .
H10B H 1.1904 0.1429 0.9570 0.057 Uiso 1 1 calc R U . . .
H10C H 1.1001 0.1896 0.9943 0.057 Uiso 1 1 calc R U . . .
C102 C 1.0072(6) 0.0905(4) 0.9607(2) 0.0313(17) Uani 1 1 d . . . . .
H10D H 0.9881 0.0941 0.9932 0.047 Uiso 1 1 calc R U . . .
H10E H 1.0747 0.0465 0.9551 0.047 Uiso 1 1 calc R U . . .
H10F H 0.9453 0.0806 0.9473 0.047 Uiso 1 1 calc R U . . .
C104 C 1.0665(5) 0.1618(4) 0.8905(2) 0.0301(16) Uani 1 1 d . . . . .
H10G H 1.0074 0.1526 0.8750 0.045 Uiso 1 1 calc R U . . .
H10H H 1.1338 0.1169 0.8868 0.045 Uiso 1 1 calc R U . . .
H10I H 1.0834 0.2114 0.8777 0.045 Uiso 1 1 calc R U . . .
C105 C 0.9099(5) 0.2781(4) 0.9847(2) 0.0210(14) Uani 1 1 d . . . . .
C106 C 0.8832(5) 0.2462(4) 1.0272(2) 0.0290(16) Uani 1 1 d . . . . .
H106 H 0.8704 0.1948 1.0305 0.035 Uiso 1 1 calc R U . . .
C107 C 0.8747(6) 0.2879(5) 1.0653(2) 0.0355(18) Uani 1 1 d . . . . .
H107 H 0.8572 0.2644 1.0943 0.043 Uiso 1 1 calc R U . . .
C108 C 0.8916(6) 0.3634(4) 1.0610(3) 0.0368(18) Uani 1 1 d . . . . .
H108 H 0.8844 0.3924 1.0868 0.044 Uiso 1 1 calc R U . . .
C109 C 0.9187(6) 0.3955(5) 1.0191(3) 0.0392(19) Uani 1 1 d . . . . .
H109 H 0.9311 0.4471 1.0159 0.047 Uiso 1 1 calc R U . . .
C110 C 0.9285(6) 0.3532(4) 0.9807(2) 0.0307(16) Uani 1 1 d . . . . .
H110 H 0.9481 0.3762 0.9519 0.037 Uiso 1 1 calc R U . . .
C111 C 0.7658(5) 0.4195(3) 0.8426(2) 0.0234(15) Uani 1 1 d . . . . .
C112 C 0.8685(6) 0.4376(4) 0.8276(2) 0.0261(15) Uani 1 1 d . . . . .
C113 C 0.8777(6) 0.4799(4) 0.7864(2) 0.0327(17) Uani 1 1 d . . . . .
H113 H 0.9461 0.4923 0.7762 0.039 Uiso 1 1 calc R U . . .
C114 C 0.7913(6) 0.5043(4) 0.7598(2) 0.0351(18) Uani 1 1 d . . . . .
H114 H 0.7988 0.5353 0.7322 0.042 Uiso 1 1 calc R U . . .
C115 C 0.6920(6) 0.4835(4) 0.7733(2) 0.0335(17) Uani 1 1 d . . . . .
H115 H 0.6341 0.4973 0.7538 0.040 Uiso 1 1 calc R U . . .
C116 C 0.6770(6) 0.4428(4) 0.8150(2) 0.0266(16) Uani 1 1 d . . . . .
C117 C 0.9673(6) 0.4132(4) 0.8562(2) 0.0310(17) Uani 1 1 d . . . . .
H117 H 0.9547 0.3701 0.8792 0.037 Uiso 1 1 calc R U . . .
C118 C 1.0797(6) 0.3801(5) 0.8291(3) 0.0415(19) Uani 1 1 d . . . . .
H11A H 1.0739 0.3390 0.8103 0.062 Uiso 1 1 calc R U . . .
H11B H 1.1371 0.3566 0.8497 0.062 Uiso 1 1 calc R U . . .
H11C H 1.1001 0.4235 0.8098 0.062 Uiso 1 1 calc R U . . .
C119 C 0.9771(6) 0.4827(4) 0.8815(3) 0.0397(19) Uani 1 1 d . . . . .
H11D H 0.9940 0.5245 0.8597 0.060 Uiso 1 1 calc R U . . .
H11E H 1.0372 0.4632 0.9013 0.060 Uiso 1 1 calc R U . . .
H11F H 0.9064 0.5047 0.8995 0.060 Uiso 1 1 calc R U . . .
C120 C 0.5649(5) 0.4285(4) 0.8307(2) 0.0280(16) Uani 1 1 d . . . . .
H120 H 0.5738 0.3913 0.8585 0.034 Uiso 1 1 calc R U . . .
C121 C 0.4782(6) 0.5079(4) 0.8436(2) 0.0385(19) Uani 1 1 d . . . . .
H12A H 0.5077 0.5328 0.8654 0.058 Uiso 1 1 calc R U . . .
H12B H 0.4085 0.4967 0.8571 0.058 Uiso 1 1 calc R U . . .
H12C H 0.4638 0.5442 0.8166 0.058 Uiso 1 1 calc R U . . .
C122 C 0.5205(6) 0.3902(5) 0.7967(3) 0.042(2) Uani 1 1 d . . . . .
H12D H 0.5187 0.4224 0.7679 0.064 Uiso 1 1 calc R U . . .
H12E H 0.4447 0.3872 0.8076 0.064 Uiso 1 1 calc R U . . .
H12F H 0.5692 0.3362 0.7924 0.064 Uiso 1 1 calc R U . . .
C123 C 0.6884(6) 0.5182(4) 0.9128(2) 0.0288(16) Uani 1 1 d . . . . .
H23C H 0.7114 0.5402 0.8842 0.035 Uiso 1 1 calc R U . . .
H23D H 0.6566 0.5521 0.9366 0.035 Uiso 1 1 calc R U . . .
C124 C 0.7008(5) 0.4388(4) 0.9196(2) 0.0208(14) Uani 1 1 d . . . . .
C125 C 0.6672(5) 0.4062(4) 0.9647(2) 0.0206(14) Uani 1 1 d . . . . .
H125 H 0.6706 0.4383 0.9879 0.025 Uiso 1 1 calc R U . . .
C126 C 0.6327(5) 0.3414(4) 0.9807(2) 0.0237(15) Uani 1 1 d . . . . .
C127 C 0.5954(5) 0.3345(4) 1.0303(2) 0.0264(16) Uani 1 1 d . . . . .
H12G H 0.5974 0.3826 1.0440 0.040 Uiso 1 1 calc R U . . .
H12H H 0.6454 0.2874 1.0447 0.040 Uiso 1 1 calc R U . . .
H12I H 0.5190 0.3292 1.0344 0.040 Uiso 1 1 calc R U . . .
C128 C 0.5492(5) 0.2375(4) 0.9710(2) 0.0239(15) Uani 1 1 d . . . . .
C129 C 0.5737(5) 0.1622(4) 0.9947(2) 0.0298(16) Uani 1 1 d . . . . .
C130 C 0.4859(6) 0.1307(4) 1.0139(2) 0.0339(17) Uani 1 1 d . . . . .
H130 H 0.5021 0.0795 1.0297 0.041 Uiso 1 1 calc R U . . .
C131 C 0.3762(6) 0.1736(4) 1.0102(3) 0.0379(18) Uani 1 1 d . . . . .
H131 H 0.3168 0.1534 1.0244 0.045 Uiso 1 1 calc R U . . .
C132 C 0.3543(6) 0.2462(4) 0.9855(2) 0.0347(18) Uani 1 1 d . . . . .
H132 H 0.2787 0.2750 0.9826 0.042 Uiso 1 1 calc R U . . .
C133 C 0.4372(5) 0.2789(4) 0.9646(2) 0.0273(16) Uani 1 1 d . . . . .
C134 C 0.6915(5) 0.1095(4) 1.0015(2) 0.0253(15) Uani 1 1 d . . . . .
H134 H 0.7463 0.1347 0.9831 0.030 Uiso 1 1 calc R U . . .
C135 C 0.7138(6) 0.1033(4) 1.0505(2) 0.0374(18) Uani 1 1 d . . . . .
H13A H 0.7021 0.1570 1.0605 0.056 Uiso 1 1 calc R U . . .
H13B H 0.7911 0.0720 1.0538 0.056 Uiso 1 1 calc R U . . .
H13C H 0.6626 0.0769 1.0690 0.056 Uiso 1 1 calc R U . . .
C136 C 0.7090(6) 0.0260(4) 0.9857(2) 0.0335(17) Uani 1 1 d . . . . .
H13D H 0.6677 -0.0038 1.0073 0.050 Uiso 1 1 calc R U . . .
H13E H 0.7888 -0.0023 0.9838 0.050 Uiso 1 1 calc R U . . .
H13F H 0.6818 0.0306 0.9560 0.050 Uiso 1 1 calc R U . . .
C137 C 0.4057(6) 0.3566(4) 0.9359(2) 0.0274(16) Uani 1 1 d . . . . .
H137 H 0.4753 0.3632 0.9177 0.033 Uiso 1 1 calc R U . . .
C138 C 0.3595(6) 0.4286(4) 0.9633(2) 0.0374(18) Uani 1 1 d . . . . .
H13G H 0.2922 0.4232 0.9822 0.056 Uiso 1 1 calc R U . . .
H13H H 0.3406 0.4770 0.9430 0.056 Uiso 1 1 calc R U . . .
H13I H 0.4156 0.4323 0.9824 0.056 Uiso 1 1 calc R U . . .
C139 C 0.3229(6) 0.3545(4) 0.9028(2) 0.0383(18) Uani 1 1 d . . . . .
H13J H 0.3529 0.3073 0.8854 0.057 Uiso 1 1 calc R U . . .
H13K H 0.3111 0.4029 0.8823 0.057 Uiso 1 1 calc R U . . .
H13L H 0.2516 0.3521 0.9196 0.057 Uiso 1 1 calc R U . . .
C140 C 0.9087(5) 0.0830(4) 0.8262(2) 0.0262(16) Uani 1 1 d . . . . .
C141 C 0.9118(6) 0.0310(4) 0.8643(2) 0.0255(15) Uani 1 1 d . . . . .
C142 C 1.0018(6) -0.0360(4) 0.8725(2) 0.0310(17) Uani 1 1 d . . . . .
C143 C 1.0908(6) -0.0529(4) 0.8411(3) 0.0352(18) Uani 1 1 d . . . . .
C144 C 1.0921(6) -0.0061(4) 0.8021(3) 0.0352(18) Uani 1 1 d . . . . .
C145 C 1.0011(5) 0.0616(4) 0.7950(2) 0.0256(15) Uani 1 1 d . . . . .
C146 C 0.6892(5) 0.1313(4) 0.8250(2) 0.0248(15) Uani 1 1 d . . . . .
C147 C 0.5888(6) 0.1581(4) 0.8509(2) 0.0351(18) Uani 1 1 d . . . . .
C148 C 0.5011(6) 0.1237(4) 0.8540(3) 0.0397(19) Uani 1 1 d . . . . .
C149 C 0.5113(6) 0.0596(4) 0.8289(3) 0.0395(19) Uani 1 1 d . . . . .
C150 C 0.6051(7) 0.0338(4) 0.8001(3) 0.0391(19) Uani 1 1 d . . . . .
C151 C 0.6923(6) 0.0684(4) 0.7988(2) 0.0307(17) Uani 1 1 d . . . . .
C152 C 0.8157(5) 0.2245(4) 0.7792(2) 0.0253(15) Uani 1 1 d . . . . .
C153 C 0.9041(6) 0.2596(4) 0.7730(2) 0.0268(16) Uani 1 1 d . . . . .
C154 C 0.9280(6) 0.3067(4) 0.7356(2) 0.0275(16) Uani 1 1 d . . . . .
C155 C 0.8573(6) 0.3260(4) 0.7022(2) 0.0325(17) Uani 1 1 d . . . . .
C156 C 0.7702(6) 0.2932(4) 0.7058(2) 0.0312(17) Uani 1 1 d . . . . .
C157 C 0.7512(6) 0.2450(4) 0.7435(2) 0.0298(16) Uani 1 1 d . . . . .
C200 C 0.4050(7) 0.2202(5) 0.7453(3) 0.053(2) Uani 1 1 d . . . . .
H200 H 0.4317 0.2634 0.7515 0.064 Uiso 1 1 calc R U . . .
C201 C 0.3025(8) 0.2141(6) 0.7640(4) 0.076(3) Uani 1 1 d . . . . .
H201 H 0.2567 0.2534 0.7830 0.091 Uiso 1 1 calc R U . . .
C202 C 0.2655(9) 0.1491(7) 0.7548(4) 0.082(3) Uani 1 1 d . . . . .
H202 H 0.1945 0.1438 0.7675 0.099 Uiso 1 1 calc R U . . .
C203 C 0.3326(10) 0.0940(7) 0.7275(4) 0.080(3) Uani 1 1 d . . . . .
H203 H 0.3076 0.0504 0.7208 0.096 Uiso 1 1 calc R U . . .
C204 C 0.4339(8) 0.1002(5) 0.7100(3) 0.060(2) Uani 1 1 d . . . . .
H204 H 0.4813 0.0598 0.6921 0.071 Uiso 1 1 calc R U . . .
C205 C 0.4684(7) 0.1637(6) 0.7177(3) 0.054(2) Uani 1 1 d . . . . .
H205 H 0.5383 0.1691 0.7037 0.065 Uiso 1 1 calc R U . . .
C206 C 0.8554(7) 0.7004(6) 0.8273(3) 0.057(2) Uani 1 1 d . . . . .
H206 H 0.8696 0.6500 0.8151 0.069 Uiso 1 1 calc R U . . .
C207 C 0.8342(7) 0.7687(7) 0.7991(3) 0.070(3) Uani 1 1 d . . . . .
H207 H 0.8350 0.7661 0.7676 0.084 Uiso 1 1 calc R U . . .
C208 C 0.8111(7) 0.8432(6) 0.8182(5) 0.086(4) Uani 1 1 d . . . . .
H208 H 0.7956 0.8915 0.7995 0.103 Uiso 1 1 calc R U . . .
C209 C 0.8110(7) 0.8453(7) 0.8642(5) 0.079(4) Uani 1 1 d . . . . .
H209 H 0.7942 0.8951 0.8773 0.094 Uiso 1 1 calc R U . . .
C210 C 0.8351(7) 0.7756(7) 0.8909(4) 0.062(3) Uani 1 1 d . . . . .
H210 H 0.8371 0.7771 0.9223 0.074 Uiso 1 1 calc R U . . .
C211 C 0.8565(7) 0.7032(6) 0.8725(3) 0.058(2) Uani 1 1 d . . . . .
H211 H 0.8721 0.6550 0.8914 0.069 Uiso 1 1 calc R U . . .
C300 C 0.5667(7) 0.7134(6) 0.7935(3) 0.061(3) Uani 1 1 d . . . . .
H30A H 0.5874 0.6562 0.8030 0.091 Uiso 1 1 calc R U . . .
H30B H 0.6345 0.7309 0.7848 0.091 Uiso 1 1 calc R U . . .
H30C H 0.5223 0.7229 0.7678 0.091 Uiso 1 1 calc R U . . .
C301 C 0.4779(9) 0.8461(5) 0.8177(3) 0.065(3) Uani 1 1 d . . . . .
H30D H 0.4361 0.8585 0.7911 0.097 Uiso 1 1 calc R U . . .
H30E H 0.5491 0.8595 0.8104 0.097 Uiso 1 1 calc R U . . .
H30F H 0.4342 0.8774 0.8423 0.097 Uiso 1 1 calc R U . . .
C302 C 0.5609(7) 0.7417(6) 0.8731(3) 0.059(2) Uani 1 1 d . . . . .
H30G H 0.5137 0.7710 0.8978 0.089 Uiso 1 1 calc R U . . .
H30H H 0.6300 0.7583 0.8670 0.089 Uiso 1 1 calc R U . . .
H30I H 0.5790 0.6842 0.8816 0.089 Uiso 1 1 calc R U . . .
C303 C 0.3923(6) 0.7391(5) 0.8414(3) 0.057(2) Uani 1 1 d . . . . .
H30J H 0.3490 0.7679 0.8670 0.085 Uiso 1 1 calc R U . . .
H30K H 0.4065 0.6814 0.8488 0.085 Uiso 1 1 calc R U . . .
H30L H 0.3501 0.7545 0.8150 0.085 Uiso 1 1 calc R U . . .
C400 C 0.2085(12) 0.2792(8) 0.5636(4) 0.112(4) Uani 1 1 d . U . . .
H40A H 0.2561 0.2420 0.5422 0.168 Uiso 1 1 calc R U . . .
H40B H 0.2296 0.3295 0.5598 0.168 Uiso 1 1 calc R U . . .
H40C H 0.1302 0.2896 0.5578 0.168 Uiso 1 1 calc R U . . .
C401 C 0.3459(17) 0.2175(13) 0.6048(8) 0.100(8) Uani 0.597(15) 1 d . U P A 1
H40D H 0.3719 0.1904 0.5769 0.150 Uiso 0.597(15) 1 calc R U P A 1
H40E H 0.3723 0.1806 0.6305 0.150 Uiso 0.597(15) 1 calc R U P A 1
H40F H 0.3752 0.2641 0.6037 0.150 Uiso 0.597(15) 1 calc R U P A 1
C402 C 0.1753(18) 0.3095(11) 0.6395(6) 0.091(7) Uani 0.597(15) 1 d . U P A 1
H40G H 0.2110 0.3526 0.6305 0.136 Uiso 0.597(15) 1 calc R U P A 1
H40H H 0.1883 0.2898 0.6707 0.136 Uiso 0.597(15) 1 calc R U P A 1
H40I H 0.0948 0.3299 0.6371 0.136 Uiso 0.597(15) 1 calc R U P A 1
C403 C 0.1754(19) 0.1777(12) 0.6242(7) 0.094(7) Uani 0.597(15) 1 d . U P A 1
H40J H 0.0952 0.1945 0.6209 0.140 Uiso 0.597(15) 1 calc R U P A 1
H40K H 0.1873 0.1609 0.6558 0.140 Uiso 0.597(15) 1 calc R U P A 1
H40L H 0.2118 0.1328 0.6056 0.140 Uiso 0.597(15) 1 calc R U P A 1
C404 C 0.299(2) 0.2693(15) 0.6330(8) 0.063(8) Uani 0.403(15) 1 d . U P A 2
H40M H 0.2619 0.3219 0.6444 0.095 Uiso 0.403(15) 1 calc R U P A 2
H40N H 0.3645 0.2729 0.6122 0.095 Uiso 0.403(15) 1 calc R U P A 2
H40O H 0.3231 0.2306 0.6583 0.095 Uiso 0.403(15) 1 calc R U P A 2
C405 C 0.110(2) 0.266(2) 0.6246(10) 0.095(11) Uani 0.403(15) 1 d . U P A 2
H40P H 0.0995 0.2523 0.6571 0.143 Uiso 0.403(15) 1 calc R U P A 2
H40Q H 0.0701 0.2383 0.6087 0.143 Uiso 0.403(15) 1 calc R U P A 2
H40R H 0.0797 0.3242 0.6187 0.143 Uiso 0.403(15) 1 calc R U P A 2
C406 C 0.265(2) 0.1556(14) 0.6022(8) 0.067(8) Uani 0.403(15) 1 d . U P A 2
H40S H 0.2694 0.1244 0.6313 0.100 Uiso 0.403(15) 1 calc R U P A 2
H40T H 0.3400 0.1446 0.5857 0.100 Uiso 0.403(15) 1 calc R U P A 2
H40U H 0.2144 0.1406 0.5847 0.100 Uiso 0.403(15) 1 calc R U P A 2
B1 B 0.1824(6) 0.8409(4) 0.6628(2) 0.0204(16) Uani 1 1 d . . . . .
B2 B 0.8004(6) 0.1641(5) 0.8250(3) 0.0269(18) Uani 1 1 d . . . . .
N1 N 0.0920(4) 0.7629(3) 0.53763(16) 0.0195(12) Uani 1 1 d . . . . .
N2 N 0.3744(4) 0.7169(3) 0.54809(16) 0.0195(12) Uani 1 1 d . . . . .
N3 N 0.2478(4) 0.6056(3) 0.60445(17) 0.0229(12) Uani 1 1 d . . . . .
N4 N 0.1909(4) 0.7886(3) 0.62237(17) 0.0194(12) Uani 1 1 d . . . . .
N5 N 0.9215(4) 0.2348(3) 0.94523(17) 0.0246(13) Uani 1 1 d . . . . .
N6 N 0.6351(4) 0.2762(3) 0.95554(16) 0.0207(12) Uani 1 1 d . . . . .
N7 N 0.7466(4) 0.3844(3) 0.88677(16) 0.0212(12) Uani 1 1 d . . . . .
N8 N 0.7936(4) 0.2098(3) 0.86750(17) 0.0206(12) Uani 1 1 d . . . . .
N300 N 0.4996(5) 0.7595(4) 0.8316(2) 0.0422(16) Uani 1 1 d . . . . .
N400 N 0.2229(5) 0.2438(4) 0.6098(2) 0.0450(17) Uani 1 1 d . . . . .
F1 F 0.3407(3) 0.6842(2) 0.67676(12) 0.0367(10) Uani 1 1 d . . . . .
F2 F 0.3505(4) 0.5818(3) 0.74911(14) 0.0580(14) Uani 1 1 d . . . . .
F3 F 0.2099(4) 0.6222(3) 0.82493(13) 0.0503(12) Uani 1 1 d . . . . .
F4 F 0.0639(3) 0.7696(3) 0.82662(13) 0.0449(11) Uani 1 1 d . . . . .
F5 F 0.0440(3) 0.8699(2) 0.75406(13) 0.0399(10) Uani 1 1 d . . . . .
F6 F -0.0350(3) 0.8147(2) 0.66741(14) 0.0427(11) Uani 1 1 d . . . . .
F7 F -0.2331(3) 0.9200(3) 0.66765(17) 0.0632(14) Uani 1 1 d . . . . .
F8 F -0.2513(4) 1.0807(3) 0.66453(16) 0.0678(15) Uani 1 1 d . . . . .
F9 F -0.0625(4) 1.1299(3) 0.66193(15) 0.0610(14) Uani 1 1 d . . . . .
F10 F 0.1344(4) 1.0258(2) 0.66495(14) 0.0438(11) Uani 1 1 d . . . . .
F11 F 0.2255(3) 0.9434(2) 0.58545(12) 0.0347(10) Uani 1 1 d . . . . .
F12 F 0.3900(4) 1.0115(3) 0.56753(15) 0.0541(13) Uani 1 1 d . . . . .
F13 F 0.5558(4) 0.9814(3) 0.62269(16) 0.0737(17) Uani 1 1 d . . . . .
F14 F 0.5423(4) 0.8869(3) 0.70123(15) 0.0598(14) Uani 1 1 d . . . . .
F15 F 0.3719(3) 0.8269(3) 0.72260(13) 0.0419(11) Uani 1 1 d . . . . .
F100 F 0.8269(3) 0.0422(2) 0.89664(13) 0.0338(9) Uani 1 1 d . . . . .
F101 F 0.9991(4) -0.0832(2) 0.91057(14) 0.0440(11) Uani 1 1 d . . . . .
F102 F 1.1796(3) -0.1171(2) 0.84786(16) 0.0518(12) Uani 1 1 d . . . . .
F103 F 1.1780(3) -0.0230(2) 0.77009(15) 0.0450(11) Uani 1 1 d . . . . .
F104 F 1.0088(3) 0.1020(2) 0.75500(13) 0.0354(10) Uani 1 1 d . . . . .
F105 F 0.5670(3) 0.2249(3) 0.87358(14) 0.0451(11) Uani 1 1 d . . . . .
F106 F 0.4068(4) 0.1516(3) 0.87998(15) 0.0550(13) Uani 1 1 d . . . . .
F107 F 0.4258(4) 0.0259(3) 0.83061(18) 0.0613(14) Uani 1 1 d . . . . .
F108 F 0.6133(4) -0.0253(2) 0.77312(16) 0.0524(12) Uani 1 1 d . . . . .
F109 F 0.7808(3) 0.0413(2) 0.76878(13) 0.0393(10) Uani 1 1 d . . . . .
F110 F 0.9786(3) 0.2419(2) 0.80382(12) 0.0359(10) Uani 1 1 d . . . . .
F111 F 1.0181(3) 0.3350(3) 0.73137(13) 0.0412(10) Uani 1 1 d . . . . .
F112 F 0.8782(4) 0.3724(3) 0.66584(13) 0.0477(11) Uani 1 1 d . . . . .
F113 F 0.7017(4) 0.3088(3) 0.67255(14) 0.0491(12) Uani 1 1 d . . . . .
F114 F 0.6611(3) 0.2166(2) 0.74360(13) 0.0372(10) Uani 1 1 d . . . . .
Nb1 Nb 0.21631(4) 0.72280(3) 0.57955(2) 0.01752(15) Uani 1 1 d . . . . .
Nb2 Nb 0.78002(5) 0.26832(3) 0.91339(2) 0.01945(16) 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 N1 1.503(8) . ?
C1 C4 1.521(9) . ?
C1 C3 1.529(8) . ?
C1 C2 1.531(9) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.380(9) . ?
C5 C10 1.411(9) . ?
C5 N1 1.445(8) . ?
C6 C7 1.405(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.364(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(9) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C16 1.404(9) . ?
C11 N2 1.427(8) . ?
C11 C12 1.429(9) . ?
C12 C13 1.407(9) . ?
C12 C17 1.497(10) . ?
C13 C14 1.367(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.412(9) . ?
C15 H15 0.9500 . ?
C16 C20 1.497(9) . ?
C17 C18 1.522(10) . ?
C17 C19 1.543(9) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.529(9) . ?
C20 C22 1.544(9) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.323(9) . ?
C23 H23A 0.9500 . ?
C23 H23B 0.9500 . ?
C24 N2 1.414(8) . ?
C24 C25 1.495(9) . ?
C25 C26 1.347(9) . ?
C25 H25 0.9500 . ?
C26 N3 1.405(8) . ?
C26 C27 1.499(9) . ?
C26 Nb1 2.689(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.385(9) . ?
C28 N3 1.427(8) . ?
C28 C29 1.433(9) . ?
C29 C30 1.373(9) . ?
C29 C37 1.514(10) . ?
C30 C31 1.364(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.374(11) . ?
C31 H31 0.9500 . ?
C32 C33 1.395(10) . ?
C32 H32 0.9500 . ?
C33 C34 1.525(10) . ?
C34 C36 1.505(10) . ?
C34 C35 1.541(10) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.529(10) . ?
C37 C39 1.539(10) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C45 1.369(9) . ?
C40 C41 1.409(9) . ?
C40 B1 1.659(10) . ?
C41 F1 1.341(7) . ?
C41 C42 1.373(9) . ?
C42 C43 1.344(9) . ?
C42 F2 1.361(8) . ?
C43 F3 1.353(8) . ?
C43 C44 1.390(10) . ?
C44 F4 1.351(7) . ?
C44 C45 1.377(9) . ?
C45 F5 1.350(7) . ?
C46 C51 1.385(9) . ?
C46 C47 1.393(9) . ?
C46 B1 1.664(10) . ?
C47 F6 1.335(8) . ?
C47 C48 1.374(10) . ?
C48 C49 1.352(11) . ?
C48 F7 1.365(8) . ?
C49 F8 1.353(8) . ?
C49 C50 1.371(12) . ?
C50 F9 1.363(8) . ?
C50 C51 1.379(10) . ?
C51 F10 1.362(8) . ?
C52 C53 1.379(9) . ?
C52 C57 1.386(9) . ?
C52 B1 1.643(9) . ?
C53 F11 1.353(8) . ?
C53 C54 1.376(9) . ?
C54 F12 1.349(8) . ?
C54 C55 1.374(11) . ?
C55 C56 1.339(11) . ?
C55 F13 1.349(8) . ?
C56 F14 1.359(8) . ?
C56 C57 1.402(9) . ?
C57 F15 1.346(8) . ?
C100 C104 1.500(9) . ?
C100 N5 1.506(8) . ?
C100 C102 1.520(9) . ?
C100 C101 1.530(9) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C102 H10F 0.9800 . ?
C104 H10G 0.9800 . ?
C104 H10H 0.9800 . ?
C104 H10I 0.9800 . ?
C105 C106 1.378(9) . ?
C105 C110 1.388(9) . ?
C105 N5 1.439(8) . ?
C106 C107 1.396(9) . ?
C106 H106 0.9500 . ?
C107 C108 1.385(10) . ?
C107 H107 0.9500 . ?
C108 C109 1.367(10) . ?
C108 H108 0.9500 . ?
C109 C110 1.406(9) . ?
C109 H109 0.9500 . ?
C110 H110 0.9500 . ?
C111 C116 1.411(9) . ?
C111 C112 1.420(9) . ?
C111 N7 1.424(8) . ?
C112 C113 1.385(9) . ?
C112 C117 1.529(9) . ?
C113 C114 1.369(9) . ?
C113 H113 0.9500 . ?
C114 C115 1.395(10) . ?
C114 H114 0.9500 . ?
C115 C116 1.395(9) . ?
C115 H115 0.9500 . ?
C116 C120 1.507(9) . ?
C117 C118 1.529(10) . ?
C117 C119 1.536(9) . ?
C117 H117 1.0000 . ?
C118 H11A 0.9800 . ?
C118 H11B 0.9800 . ?
C118 H11C 0.9800 . ?
C119 H11D 0.9800 . ?
C119 H11E 0.9800 . ?
C119 H11F 0.9800 . ?
C120 C122 1.514(9) . ?
C120 C121 1.552(9) . ?
C120 H120 1.0000 . ?
C121 H12A 0.9800 . ?
C121 H12B 0.9800 . ?
C121 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C122 H12E 0.9800 . ?
C122 H12F 0.9800 . ?
C123 C124 1.349(8) . ?
C123 H23C 0.9500 . ?
C123 H23D 0.9500 . ?
C124 N7 1.397(7) . ?
C124 C125 1.472(9) . ?
C125 C126 1.347(9) . ?
C125 H125 0.9500 . ?
C126 N6 1.422(8) . ?
C126 C127 1.505(9) . ?
C127 H12G 0.9800 . ?
C127 H12H 0.9800 . ?
C127 H12I 0.9800 . ?
C128 C129 1.402(9) . ?
C128 C133 1.413(9) . ?
C128 N6 1.434(8) . ?
C129 C130 1.404(9) . ?
C129 C134 1.529(9) . ?
C130 C131 1.380(10) . ?
C130 H130 0.9500 . ?
C131 C132 1.376(10) . ?
C131 H131 0.9500 . ?
C132 C133 1.379(9) . ?
C132 H132 0.9500 . ?
C133 C137 1.509(9) . ?
C134 C135 1.518(9) . ?
C134 C136 1.528(9) . ?
C134 H134 1.0000 . ?
C135 H13A 0.9800 . ?
C135 H13B 0.9800 . ?
C135 H13C 0.9800 . ?
C136 H13D 0.9800 . ?
C136 H13E 0.9800 . ?
C136 H13F 0.9800 . ?
C137 C138 1.509(9) . ?
C137 C139 1.530(9) . ?
C137 H137 1.0000 . ?
C138 H13G 0.9800 . ?
C138 H13H 0.9800 . ?
C138 H13I 0.9800 . ?
C139 H13J 0.9800 . ?
C139 H13K 0.9800 . ?
C139 H13L 0.9800 . ?
C140 C141 1.385(9) . ?
C140 C145 1.385(9) . ?
C140 B2 1.664(10) . ?
C141 F100 1.334(7) . ?
C141 C142 1.402(9) . ?
C142 F101 1.343(8) . ?
C142 C143 1.353(10) . ?
C143 F102 1.357(8) . ?
C143 C144 1.358(10) . ?
C144 F103 1.340(8) . ?
C144 C145 1.412(10) . ?
C145 F104 1.336(7) . ?
C146 C147 1.383(9) . ?
C146 C151 1.405(9) . ?
C146 B2 1.650(10) . ?
C147 F105 1.355(8) . ?
C147 C148 1.384(10) . ?
C148 F106 1.331(8) . ?
C148 C149 1.380(10) . ?
C149 F107 1.356(8) . ?
C149 C150 1.366(10) . ?
C150 F108 1.351(8) . ?
C150 C151 1.386(10) . ?
C151 F109 1.346(8) . ?
C152 C157 1.376(9) . ?
C152 C153 1.396(9) . ?
C152 B2 1.670(10) . ?
C153 F110 1.345(7) . ?
C153 C154 1.377(9) . ?
C154 F111 1.344(7) . ?
C154 C155 1.371(9) . ?
C155 F112 1.336(8) . ?
C155 C156 1.358(10) . ?
C156 F113 1.353(7) . ?
C156 C157 1.378(10) . ?
C157 F114 1.356(7) . ?
C200 C205 1.362(11) . ?
C200 C201 1.367(12) . ?
C200 H200 0.9500 . ?
C201 C202 1.405(14) . ?
C201 H201 0.9500 . ?
C202 C203 1.356(14) . ?
C202 H202 0.9500 . ?
C203 C204 1.344(13) . ?
C203 H203 0.9500 . ?
C204 C205 1.349(11) . ?
C204 H204 0.9500 . ?
C205 H205 0.9500 . ?
C206 C211 1.365(12) . ?
C206 C207 1.371(13) . ?
C206 H206 0.9500 . ?
C207 C208 1.416(15) . ?
C207 H207 0.9500 . ?
C208 C209 1.386(15) . ?
C208 H208 0.9500 . ?
C209 C210 1.366(14) . ?
C209 H209 0.9500 . ?
C210 C211 1.374(12) . ?
C210 H210 0.9500 . ?
C211 H211 0.9500 . ?
C300 N300 1.495(10) . ?
C300 H30A 0.9800 . ?
C300 H30B 0.9800 . ?
C300 H30C 0.9800 . ?
C301 N300 1.484(10) . ?
C301 H30D 0.9800 . ?
C301 H30E 0.9800 . ?
C301 H30F 0.9800 . ?
C302 N300 1.502(9) . ?
C302 H30G 0.9800 . ?
C302 H30H 0.9800 . ?
C302 H30I 0.9800 . ?
C303 N300 1.475(9) . ?
C303 H30J 0.9800 . ?
C303 H30K 0.9800 . ?
C303 H30L 0.9800 . ?
C400 N400 1.470(12) . ?
C400 H40A 0.9800 . ?
C400 H40B 0.9800 . ?
C400 H40C 0.9800 . ?
C401 N400 1.47(2) . ?
C401 H40D 0.9800 . ?
C401 H40E 0.9800 . ?
C401 H40F 0.9800 . ?
C402 N400 1.471(17) . ?
C402 H40G 0.9800 . ?
C402 H40H 0.9800 . ?
C402 H40I 0.9800 . ?
C403 N400 1.449(18) . ?
C403 H40J 0.9800 . ?
C403 H40K 0.9800 . ?
C403 H40L 0.9800 . ?
C404 N400 1.44(2) . ?
C404 H40M 0.9800 . ?
C404 H40N 0.9800 . ?
C404 H40O 0.9800 . ?
C405 N400 1.39(3) . ?
C405 H40P 0.9800 . ?
C405 H40Q 0.9800 . ?
C405 H40R 0.9800 . ?
C406 N400 1.51(2) . ?
C406 H40S 0.9800 . ?
C406 H40T 0.9800 . ?
C406 H40U 0.9800 . ?
B1 N4 1.568(8) . ?
B2 N8 1.554(9) . ?
N1 Nb1 2.045(5) . ?
N2 Nb1 2.068(5) . ?
N3 Nb1 2.051(5) . ?
N4 Nb1 1.752(5) . ?
N5 Nb2 2.029(5) . ?
N6 Nb2 2.062(5) . ?
N7 Nb2 2.049(5) . ?
N8 Nb2 1.762(5) . ?

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 C4 110.7(5) . . ?
N1 C1 C3 108.2(5) . . ?
C4 C1 C3 108.6(5) . . ?
N1 C1 C2 111.6(5) . . ?
C4 C1 C2 110.2(6) . . ?
C3 C1 C2 107.3(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 118.7(6) . . ?
C6 C5 N1 121.1(6) . . ?
C10 C5 N1 120.2(6) . . ?
C5 C6 C7 121.1(7) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 119.4(7) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 120.5(6) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 120.8(7) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C9 C10 C5 119.5(7) . . ?
C9 C10 H10 120.3 . . ?
C5 C10 H10 120.3 . . ?
C16 C11 N2 119.7(6) . . ?
C16 C11 C12 121.3(6) . . ?
N2 C11 C12 118.9(6) . . ?
C13 C12 C11 116.6(7) . . ?
C13 C12 C17 118.4(6) . . ?
C11 C12 C17 124.9(6) . . ?
C14 C13 C12 122.7(7) . . ?
C14 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
C13 C14 C15 120.0(6) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C16 121.0(7) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 118.3(6) . . ?
C11 C16 C20 122.9(6) . . ?
C15 C16 C20 118.7(6) . . ?
C12 C17 C18 113.5(6) . . ?
C12 C17 C19 110.5(6) . . ?
C18 C17 C19 109.2(6) . . ?
C12 C17 H17 107.8 . . ?
C18 C17 H17 107.8 . . ?
C19 C17 H17 107.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 C21 113.6(6) . . ?
C16 C20 C22 111.1(5) . . ?
C21 C20 C22 108.9(6) . . ?
C16 C20 H20 107.7 . . ?
C21 C20 H20 107.7 . . ?
C22 C20 H20 107.7 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 120.0 . . ?
C24 C23 H23B 120.0 . . ?
H23A C23 H23B 120.0 . . ?
C23 C24 N2 125.6(6) . . ?
C23 C24 C25 117.4(6) . . ?
N2 C24 C25 117.0(5) . . ?
C26 C25 C24 133.3(6) . . ?
C26 C25 H25 113.4 . . ?
C24 C25 H25 113.4 . . ?
C25 C26 N3 123.3(6) . . ?
C25 C26 C27 118.6(6) . . ?
N3 C26 C27 118.0(6) . . ?
C25 C26 Nb1 83.9(4) . . ?
N3 C26 Nb1 48.6(3) . . ?
C27 C26 Nb1 141.5(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 . . ?
C33 C28 N3 121.4(6) . . ?
C33 C28 C29 119.1(6) . . ?
N3 C28 C29 119.2(6) . . ?
C30 C29 C28 119.2(7) . . ?
C30 C29 C37 118.4(6) . . ?
C28 C29 C37 122.4(6) . . ?
C31 C30 C29 122.1(7) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C30 C31 C32 118.2(8) . . ?
C30 C31 H31 120.9 . . ?
C32 C31 H31 120.9 . . ?
C31 C32 C33 123.0(8) . . ?
C31 C32 H32 118.5 . . ?
C33 C32 H32 118.5 . . ?
C28 C33 C32 118.3(7) . . ?
C28 C33 C34 123.5(6) . . ?
C32 C33 C34 118.2(6) . . ?
C36 C34 C33 111.9(6) . . ?
C36 C34 C35 109.8(6) . . ?
C33 C34 C35 110.5(6) . . ?
C36 C34 H34 108.2 . . ?
C33 C34 H34 108.2 . . ?
C35 C34 H34 108.2 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C29 C37 C38 110.7(6) . . ?
C29 C37 C39 110.2(7) . . ?
C38 C37 C39 109.6(6) . . ?
C29 C37 H37 108.8 . . ?
C38 C37 H37 108.8 . . ?
C39 C37 H37 108.8 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C45 C40 C41 113.1(6) . . ?
C45 C40 B1 127.0(6) . . ?
C41 C40 B1 119.8(5) . . ?
F1 C41 C42 116.7(6) . . ?
F1 C41 C40 120.0(6) . . ?
C42 C41 C40 123.2(6) . . ?
C43 C42 F2 118.5(6) . . ?
C43 C42 C41 121.3(7) . . ?
F2 C42 C41 120.1(6) . . ?
C42 C43 F3 122.6(7) . . ?
C42 C43 C44 118.2(6) . . ?
F3 C43 C44 119.1(6) . . ?
F4 C44 C45 121.5(6) . . ?
F4 C44 C43 119.1(6) . . ?
C45 C44 C43 119.4(6) . . ?
F5 C45 C40 120.8(6) . . ?
F5 C45 C44 114.4(6) . . ?
C40 C45 C44 124.8(6) . . ?
C51 C46 C47 113.2(6) . . ?
C51 C46 B1 127.4(6) . . ?
C47 C46 B1 119.4(6) . . ?
F6 C47 C48 117.4(7) . . ?
F6 C47 C46 119.2(6) . . ?
C48 C47 C46 123.4(7) . . ?
C49 C48 F7 120.3(7) . . ?
C49 C48 C47 121.1(7) . . ?
F7 C48 C47 118.6(7) . . ?
C48 C49 F8 121.5(8) . . ?
C48 C49 C50 118.3(7) . . ?
F8 C49 C50 120.2(8) . . ?
F9 C50 C49 119.6(7) . . ?
F9 C50 C51 120.6(8) . . ?
C49 C50 C51 119.8(7) . . ?
F10 C51 C50 114.0(6) . . ?
F10 C51 C46 121.9(6) . . ?
C50 C51 C46 124.1(7) . . ?
C53 C52 C57 113.4(6) . . ?
C53 C52 B1 119.2(6) . . ?
C57 C52 B1 127.5(6) . . ?
F11 C53 C54 115.1(6) . . ?
F11 C53 C52 120.3(6) . . ?
C54 C53 C52 124.5(7) . . ?
F12 C54 C55 120.0(6) . . ?
F12 C54 C53 120.5(7) . . ?
C55 C54 C53 119.4(7) . . ?
C56 C55 F13 121.2(7) . . ?
C56 C55 C54 119.1(6) . . ?
F13 C55 C54 119.6(7) . . ?
C55 C56 F14 121.6(7) . . ?
C55 C56 C57 120.2(7) . . ?
F14 C56 C57 118.1(7) . . ?
F15 C57 C52 121.4(6) . . ?
F15 C57 C56 115.4(6) . . ?
C52 C57 C56 123.2(7) . . ?
C104 C100 N5 109.3(5) . . ?
C104 C100 C102 110.2(5) . . ?
N5 C100 C102 109.2(5) . . ?
C104 C100 C101 107.2(5) . . ?
N5 C100 C101 111.2(5) . . ?
C102 C100 C101 109.7(5) . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C100 C102 H10D 109.5 . . ?
C100 C102 H10E 109.5 . . ?
H10D C102 H10E 109.5 . . ?
C100 C102 H10F 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
C100 C104 H10G 109.5 . . ?
C100 C104 H10H 109.5 . . ?
H10G C104 H10H 109.5 . . ?
C100 C104 H10I 109.5 . . ?
H10G C104 H10I 109.5 . . ?
H10H C104 H10I 109.5 . . ?
C106 C105 C110 118.1(6) . . ?
C106 C105 N5 121.9(6) . . ?
C110 C105 N5 120.0(6) . . ?
C105 C106 C107 121.4(6) . . ?
C105 C106 H106 119.3 . . ?
C107 C106 H106 119.3 . . ?
C108 C107 C106 120.1(7) . . ?
C108 C107 H107 119.9 . . ?
C106 C107 H107 119.9 . . ?
C109 C108 C107 119.1(7) . . ?
C109 C108 H108 120.5 . . ?
C107 C108 H108 120.5 . . ?
C108 C109 C110 120.8(7) . . ?
C108 C109 H109 119.6 . . ?
C110 C109 H109 119.6 . . ?
C105 C110 C109 120.4(7) . . ?
C105 C110 H110 119.8 . . ?
C109 C110 H110 119.8 . . ?
C116 C111 C112 120.0(6) . . ?
C116 C111 N7 118.5(6) . . ?
C112 C111 N7 121.3(5) . . ?
C113 C112 C111 118.6(6) . . ?
C113 C112 C117 119.6(6) . . ?
C111 C112 C117 121.8(6) . . ?
C114 C113 C112 121.9(7) . . ?
C114 C113 H113 119.0 . . ?
C112 C113 H113 119.0 . . ?
C113 C114 C115 119.7(7) . . ?
C113 C114 H114 120.1 . . ?
C115 C114 H114 120.1 . . ?
C114 C115 C116 120.7(6) . . ?
C114 C115 H115 119.6 . . ?
C116 C115 H115 119.6 . . ?
C115 C116 C111 118.9(6) . . ?
C115 C116 C120 119.5(6) . . ?
C111 C116 C120 121.5(6) . . ?
C112 C117 C118 113.5(6) . . ?
C112 C117 C119 112.4(6) . . ?
C118 C117 C119 107.6(6) . . ?
C112 C117 H117 107.7 . . ?
C118 C117 H117 107.7 . . ?
C119 C117 H117 107.7 . . ?
C117 C118 H11A 109.5 . . ?
C117 C118 H11B 109.5 . . ?
H11A C118 H11B 109.5 . . ?
C117 C118 H11C 109.5 . . ?
H11A C118 H11C 109.5 . . ?
H11B C118 H11C 109.5 . . ?
C117 C119 H11D 109.5 . . ?
C117 C119 H11E 109.5 . . ?
H11D C119 H11E 109.5 . . ?
C117 C119 H11F 109.5 . . ?
H11D C119 H11F 109.5 . . ?
H11E C119 H11F 109.5 . . ?
C116 C120 C122 113.5(6) . . ?
C116 C120 C121 110.5(6) . . ?
C122 C120 C121 109.7(6) . . ?
C116 C120 H120 107.6 . . ?
C122 C120 H120 107.6 . . ?
C121 C120 H120 107.6 . . ?
C120 C121 H12A 109.5 . . ?
C120 C121 H12B 109.5 . . ?
H12A C121 H12B 109.5 . . ?
C120 C121 H12C 109.5 . . ?
H12A C121 H12C 109.5 . . ?
H12B C121 H12C 109.5 . . ?
C120 C122 H12D 109.5 . . ?
C120 C122 H12E 109.5 . . ?
H12D C122 H12E 109.5 . . ?
C120 C122 H12F 109.5 . . ?
H12D C122 H12F 109.5 . . ?
H12E C122 H12F 109.5 . . ?
C124 C123 H23C 120.0 . . ?
C124 C123 H23D 120.0 . . ?
H23C C123 H23D 120.0 . . ?
C123 C124 N7 124.0(6) . . ?
C123 C124 C125 118.8(6) . . ?
N7 C124 C125 117.2(5) . . ?
C126 C125 C124 135.0(6) . . ?
C126 C125 H125 112.5 . . ?
C124 C125 H125 112.5 . . ?
C125 C126 N6 125.6(6) . . ?
C125 C126 C127 117.4(5) . . ?
N6 C126 C127 116.9(5) . . ?
C126 C127 H12G 109.5 . . ?
C126 C127 H12H 109.5 . . ?
H12G C127 H12H 109.5 . . ?
C126 C127 H12I 109.5 . . ?
H12G C127 H12I 109.5 . . ?
H12H C127 H12I 109.5 . . ?
C129 C128 C133 119.9(6) . . ?
C129 C128 N6 121.2(5) . . ?
C133 C128 N6 118.8(6) . . ?
C128 C129 C130 119.3(6) . . ?
C128 C129 C134 124.8(6) . . ?
C130 C129 C134 115.9(6) . . ?
C131 C130 C129 120.6(7) . . ?
C131 C130 H130 119.7 . . ?
C129 C130 H130 119.7 . . ?
C132 C131 C130 118.9(7) . . ?
C132 C131 H131 120.5 . . ?
C130 C131 H131 120.5 . . ?
C131 C132 C133 123.0(7) . . ?
C131 C132 H132 118.5 . . ?
C133 C132 H132 118.5 . . ?
C132 C133 C128 118.0(6) . . ?
C132 C133 C137 119.4(6) . . ?
C128 C133 C137 122.6(6) . . ?
C135 C134 C136 109.9(6) . . ?
C135 C134 C129 110.8(6) . . ?
C136 C134 C129 111.1(5) . . ?
C135 C134 H134 108.3 . . ?
C136 C134 H134 108.3 . . ?
C129 C134 H134 108.3 . . ?
C134 C135 H13A 109.5 . . ?
C134 C135 H13B 109.5 . . ?
H13A C135 H13B 109.5 . . ?
C134 C135 H13C 109.5 . . ?
H13A C135 H13C 109.5 . . ?
H13B C135 H13C 109.5 . . ?
C134 C136 H13D 109.5 . . ?
C134 C136 H13E 109.5 . . ?
H13D C136 H13E 109.5 . . ?
C134 C136 H13F 109.5 . . ?
H13D C136 H13F 109.5 . . ?
H13E C136 H13F 109.5 . . ?
C138 C137 C133 113.1(6) . . ?
C138 C137 C139 109.8(6) . . ?
C133 C137 C139 111.4(6) . . ?
C138 C137 H137 107.4 . . ?
C133 C137 H137 107.4 . . ?
C139 C137 H137 107.4 . . ?
C137 C138 H13G 109.5 . . ?
C137 C138 H13H 109.5 . . ?
H13G C138 H13H 109.5 . . ?
C137 C138 H13I 109.5 . . ?
H13G C138 H13I 109.5 . . ?
H13H C138 H13I 109.5 . . ?
C137 C139 H13J 109.5 . . ?
C137 C139 H13K 109.5 . . ?
H13J C139 H13K 109.5 . . ?
C137 C139 H13L 109.5 . . ?
H13J C139 H13L 109.5 . . ?
H13K C139 H13L 109.5 . . ?
C141 C140 C145 114.1(6) . . ?
C141 C140 B2 116.8(6) . . ?
C145 C140 B2 128.9(6) . . ?
F100 C141 C140 121.1(6) . . ?
F100 C141 C142 114.9(6) . . ?
C140 C141 C142 124.0(7) . . ?
F101 C142 C143 120.5(6) . . ?
F101 C142 C141 120.4(6) . . ?
C143 C142 C141 119.1(7) . . ?
C142 C143 F102 120.7(7) . . ?
C142 C143 C144 120.3(6) . . ?
F102 C143 C144 119.0(7) . . ?
F103 C144 C143 121.3(7) . . ?
F103 C144 C145 119.2(7) . . ?
C143 C144 C145 119.5(7) . . ?
F104 C145 C140 122.2(6) . . ?
F104 C145 C144 114.7(6) . . ?
C140 C145 C144 123.0(6) . . ?
C147 C146 C151 113.7(6) . . ?
C147 C146 B2 125.7(6) . . ?
C151 C146 B2 120.6(6) . . ?
F105 C147 C146 120.9(6) . . ?
F105 C147 C148 114.6(6) . . ?
C146 C147 C148 124.4(6) . . ?
F106 C148 C149 119.3(6) . . ?
F106 C148 C147 121.6(6) . . ?
C149 C148 C147 119.1(7) . . ?
F107 C149 C150 120.1(6) . . ?
F107 C149 C148 120.2(7) . . ?
C150 C149 C148 119.5(7) . . ?
F108 C150 C149 120.3(7) . . ?
F108 C150 C151 120.0(7) . . ?
C149 C150 C151 119.6(6) . . ?
F109 C151 C150 116.2(6) . . ?
F109 C151 C146 120.2(6) . . ?
C150 C151 C146 123.4(6) . . ?
C157 C152 C153 111.6(6) . . ?
C157 C152 B2 127.9(6) . . ?
C153 C152 B2 120.4(5) . . ?
F110 C153 C154 115.7(6) . . ?
F110 C153 C152 118.9(6) . . ?
C154 C153 C152 125.2(6) . . ?
F111 C154 C155 119.4(6) . . ?
F111 C154 C153 121.4(6) . . ?
C155 C154 C153 119.2(6) . . ?
F112 C155 C156 121.2(6) . . ?
F112 C155 C154 120.2(7) . . ?
C156 C155 C154 118.5(7) . . ?
F113 C156 C155 119.7(6) . . ?
F113 C156 C157 120.3(6) . . ?
C155 C156 C157 119.9(6) . . ?
F114 C157 C152 120.1(6) . . ?
F114 C157 C156 114.6(6) . . ?
C152 C157 C156 125.4(6) . . ?
C205 C200 C201 119.3(9) . . ?
C205 C200 H200 120.4 . . ?
C201 C200 H200 120.4 . . ?
C200 C201 C202 119.2(10) . . ?
C200 C201 H201 120.4 . . ?
C202 C201 H201 120.4 . . ?
C203 C202 C201 119.1(10) . . ?
C203 C202 H202 120.5 . . ?
C201 C202 H202 120.5 . . ?
C204 C203 C202 121.0(10) . . ?
C204 C203 H203 119.5 . . ?
C202 C203 H203 119.5 . . ?
C203 C204 C205 120.1(10) . . ?
C203 C204 H204 120.0 . . ?
C205 C204 H204 120.0 . . ?
C204 C205 C200 121.3(9) . . ?
C204 C205 H205 119.4 . . ?
C200 C205 H205 119.4 . . ?
C211 C206 C207 121.4(9) . . ?
C211 C206 H206 119.3 . . ?
C207 C206 H206 119.3 . . ?
C206 C207 C208 118.3(10) . . ?
C206 C207 H207 120.8 . . ?
C208 C207 H207 120.8 . . ?
C209 C208 C207 119.7(10) . . ?
C209 C208 H208 120.1 . . ?
C207 C208 H208 120.1 . . ?
C210 C209 C208 119.9(10) . . ?
C210 C209 H209 120.1 . . ?
C208 C209 H209 120.1 . . ?
C209 C210 C211 120.6(10) . . ?
C209 C210 H210 119.7 . . ?
C211 C210 H210 119.7 . . ?
C206 C211 C210 120.1(9) . . ?
C206 C211 H211 120.0 . . ?
C210 C211 H211 120.0 . . ?
N300 C300 H30A 109.5 . . ?
N300 C300 H30B 109.5 . . ?
H30A C300 H30B 109.5 . . ?
N300 C300 H30C 109.5 . . ?
H30A C300 H30C 109.5 . . ?
H30B C300 H30C 109.5 . . ?
N300 C301 H30D 109.5 . . ?
N300 C301 H30E 109.5 . . ?
H30D C301 H30E 109.5 . . ?
N300 C301 H30F 109.5 . . ?
H30D C301 H30F 109.5 . . ?
H30E C301 H30F 109.5 . . ?
N300 C302 H30G 109.5 . . ?
N300 C302 H30H 109.5 . . ?
H30G C302 H30H 109.5 . . ?
N300 C302 H30I 109.5 . . ?
H30G C302 H30I 109.5 . . ?
H30H C302 H30I 109.5 . . ?
N300 C303 H30J 109.5 . . ?
N300 C303 H30K 109.5 . . ?
H30J C303 H30K 109.5 . . ?
N300 C303 H30L 109.5 . . ?
H30J C303 H30L 109.5 . . ?
H30K C303 H30L 109.5 . . ?
N400 C400 H40A 109.5 . . ?
N400 C400 H40B 109.5 . . ?
H40A C400 H40B 109.5 . . ?
N400 C400 H40C 109.5 . . ?
H40A C400 H40C 109.5 . . ?
H40B C400 H40C 109.5 . . ?
N400 C401 H40D 109.5 . . ?
N400 C401 H40E 109.5 . . ?
H40D C401 H40E 109.5 . . ?
N400 C401 H40F 109.5 . . ?
H40D C401 H40F 109.5 . . ?
H40E C401 H40F 109.5 . . ?
N400 C402 H40G 109.5 . . ?
N400 C402 H40H 109.5 . . ?
H40G C402 H40H 109.5 . . ?
N400 C402 H40I 109.5 . . ?
H40G C402 H40I 109.5 . . ?
H40H C402 H40I 109.5 . . ?
N400 C403 H40J 109.5 . . ?
N400 C403 H40K 109.5 . . ?
H40J C403 H40K 109.5 . . ?
N400 C403 H40L 109.5 . . ?
H40J C403 H40L 109.5 . . ?
H40K C403 H40L 109.5 . . ?
N400 C404 H40M 109.5 . . ?
N400 C404 H40N 109.5 . . ?
H40M C404 H40N 109.5 . . ?
N400 C404 H40O 109.5 . . ?
H40M C404 H40O 109.5 . . ?
H40N C404 H40O 109.5 . . ?
N400 C405 H40P 109.5 . . ?
N400 C405 H40Q 109.5 . . ?
H40P C405 H40Q 109.5 . . ?
N400 C405 H40R 109.5 . . ?
H40P C405 H40R 109.5 . . ?
H40Q C405 H40R 109.5 . . ?
N400 C406 H40S 109.5 . . ?
N400 C406 H40T 109.5 . . ?
H40S C406 H40T 109.5 . . ?
N400 C406 H40U 109.5 . . ?
H40S C406 H40U 109.5 . . ?
H40T C406 H40U 109.5 . . ?
N4 B1 C52 106.8(5) . . ?
N4 B1 C40 107.6(5) . . ?
C52 B1 C40 112.1(5) . . ?
N4 B1 C46 109.4(5) . . ?
C52 B1 C46 111.4(5) . . ?
C40 B1 C46 109.5(5) . . ?
N8 B2 C146 111.2(5) . . ?
N8 B2 C140 108.7(5) . . ?
C146 B2 C140 105.9(5) . . ?
N8 B2 C152 108.8(5) . . ?
C146 B2 C152 111.5(5) . . ?
C140 B2 C152 110.7(5) . . ?
C5 N1 C1 112.4(5) . . ?
C5 N1 Nb1 112.2(4) . . ?
C1 N1 Nb1 135.3(4) . . ?
C24 N2 C11 114.3(5) . . ?
C24 N2 Nb1 110.3(4) . . ?
C11 N2 Nb1 135.1(4) . . ?
C26 N3 C28 115.1(5) . . ?
C26 N3 Nb1 100.5(4) . . ?
C28 N3 Nb1 144.2(4) . . ?
B1 N4 Nb1 172.8(4) . . ?
C105 N5 C100 114.3(5) . . ?
C105 N5 Nb2 111.6(4) . . ?
C100 N5 Nb2 133.6(4) . . ?
C126 N6 C128 113.9(5) . . ?
C126 N6 Nb2 101.2(4) . . ?
C128 N6 Nb2 144.4(4) . . ?
C124 N7 C111 115.0(5) . . ?
C124 N7 Nb2 112.0(4) . . ?
C111 N7 Nb2 132.9(4) . . ?
B2 N8 Nb2 175.5(5) . . ?
C303 N300 C301 109.3(7) . . ?
C303 N300 C300 109.2(6) . . ?
C301 N300 C300 108.3(7) . . ?
C303 N300 C302 109.7(6) . . ?
C301 N300 C302 109.0(6) . . ?
C300 N300 C302 111.3(6) . . ?
C405 N400 C404 118.8(18) . . ?
C405 N400 C400 95.1(14) . . ?
C404 N400 C400 115.7(12) . . ?
C403 N400 C400 117.0(10) . . ?
C403 N400 C402 110.2(13) . . ?
C400 N400 C402 106.3(11) . . ?
C403 N400 C401 111.7(13) . . ?
C400 N400 C401 97.0(11) . . ?
C402 N400 C401 114.1(13) . . ?
C405 N400 C406 112.3(17) . . ?
C404 N400 C406 111.2(15) . . ?
C400 N400 C406 101.5(12) . . ?
N4 Nb1 N1 108.4(2) . . ?
N4 Nb1 N3 112.2(2) . . ?
N1 Nb1 N3 116.90(19) . . ?
N4 Nb1 N2 107.5(2) . . ?
N1 Nb1 N2 113.95(19) . . ?
N3 Nb1 N2 97.3(2) . . ?
N4 Nb1 C26 142.7(2) . . ?
N1 Nb1 C26 99.69(18) . . ?
N3 Nb1 C26 30.92(19) . . ?
N2 Nb1 C26 81.8(2) . . ?
N8 Nb2 N5 110.5(2) . . ?
N8 Nb2 N7 105.7(2) . . ?
N5 Nb2 N7 112.4(2) . . ?
N8 Nb2 N6 114.0(2) . . ?
N5 Nb2 N6 114.4(2) . . ?
N7 Nb2 N6 99.0(2) . . ?

_refine_diff_density_max         1.753
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.112



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1459082'
_audit_update_record             
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H55 B F15 N6 Nb'
_chemical_formula_sum            'C57 H55 B F15 N6 Nb'
_chemical_formula_weight         1212.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.2684(5)
_cell_length_b                   12.7008(5)
_cell_length_c                   19.2268(8)
_cell_angle_alpha                79.4526(19)
_cell_angle_beta                 83.1067(17)
_cell_angle_gamma                68.9230(16)
_cell_volume                     2743.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9633
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      25.41

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_F_000             1240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.315
_shelx_estimated_absorpt_T_min   0.859
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7153
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            61535
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.079
_diffrn_reflns_theta_max         25.435
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10077
_reflns_number_gt                9002
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0250P)²+2.6287P] 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         10077
_refine_ls_number_parameters     734
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0749
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.29288(18) 0.48867(17) 0.35813(10) 0.0217(4) Uani 1 1 d . . . . .
C2 C 0.41195(19) 0.47171(18) 0.35916(11) 0.0272(5) Uani 1 1 d . . . . .
H2 H 0.4675 0.4186 0.3321 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4505(2) 0.5308(2) 0.39880(12) 0.0364(5) Uani 1 1 d . . . . .
H3 H 0.5318 0.5161 0.4003 0.044 Uiso 1 1 calc R U . . .
C4 C 0.3698(2) 0.6114(2) 0.43610(13) 0.0430(6) Uani 1 1 d . . . . .
H4 H 0.3957 0.6527 0.4630 0.052 Uiso 1 1 calc R U . . .
C5 C 0.2517(2) 0.6320(2) 0.43443(13) 0.0395(6) Uani 1 1 d . . . . .
H5 H 0.1964 0.6888 0.4592 0.047 Uiso 1 1 calc R U . . .
C6 C 0.2136(2) 0.57043(18) 0.39681(11) 0.0285(5) Uani 1 1 d . . . . .
H6 H 0.1322 0.5837 0.3972 0.034 Uiso 1 1 calc R U . . .
C7 C 0.00359(17) 0.37215(17) 0.35123(11) 0.0240(4) Uani 1 1 d . . . . .
C8 C -0.0390(2) 0.3520(2) 0.28550(13) 0.0354(5) Uani 1 1 d . . . . .
H8A H -0.0356 0.4119 0.2460 0.053 Uiso 1 1 calc R U . . .
H8B H -0.1199 0.3538 0.2949 0.053 Uiso 1 1 calc R U . . .
H8C H 0.0109 0.2774 0.2731 0.053 Uiso 1 1 calc R U . . .
C9 C -0.07563(19) 0.48553(19) 0.37365(13) 0.0331(5) Uani 1 1 d . . . . .
H9A H -0.0450 0.4983 0.4149 0.050 Uiso 1 1 calc R U . . .
H9B H -0.1548 0.4835 0.3859 0.050 Uiso 1 1 calc R U . . .
H9C H -0.0780 0.5476 0.3345 0.050 Uiso 1 1 calc R U . . .
C10 C 0.00996(19) 0.27452(19) 0.41231(13) 0.0329(5) Uani 1 1 d . . . . .
H10A H 0.0641 0.2026 0.3982 0.049 Uiso 1 1 calc R U . . .
H10B H -0.0680 0.2690 0.4239 0.049 Uiso 1 1 calc R U . . .
H10C H 0.0378 0.2894 0.4539 0.049 Uiso 1 1 calc R U . . .
C11 C 0.32100(16) 0.15026(16) 0.37406(10) 0.0204(4) Uani 1 1 d . . . . .
C12 C 0.29191(17) 0.06799(17) 0.34778(11) 0.0234(4) Uani 1 1 d . . . . .
C13 C 0.25313(18) -0.00893(18) 0.39655(12) 0.0283(5) Uani 1 1 d . . . . .
H13 H 0.2341 -0.0659 0.3800 0.034 Uiso 1 1 calc R U . . .
C14 C 0.24197(19) -0.00376(18) 0.46828(12) 0.0313(5) Uani 1 1 d . . . . .
H14 H 0.2138 -0.0557 0.5005 0.038 Uiso 1 1 calc R U . . .
C15 C 0.27168(18) 0.07669(18) 0.49305(11) 0.0281(5) Uani 1 1 d . . . . .
H15 H 0.2637 0.0794 0.5425 0.034 Uiso 1 1 calc R U . . .
C16 C 0.31345(17) 0.15481(17) 0.44693(11) 0.0231(4) Uani 1 1 d . . . . .
C17 C 0.30175(18) 0.05907(18) 0.26931(11) 0.0255(4) Uani 1 1 d . . . . .
H17 H 0.3046 0.1331 0.2420 0.031 Uiso 1 1 calc R U . . .
C18 C 0.4151(2) -0.0355(2) 0.25020(13) 0.0402(6) Uani 1 1 d . . . . .
H18A H 0.4824 -0.0186 0.2613 0.060 Uiso 1 1 calc R U . . .
H18B H 0.4196 -0.0396 0.1995 0.060 Uiso 1 1 calc R U . . .
H18C H 0.4157 -0.1088 0.2776 0.060 Uiso 1 1 calc R U . . .
C19 C 0.1970(2) 0.0387(2) 0.24668(13) 0.0371(6) Uani 1 1 d . . . . .
H19A H 0.1992 -0.0386 0.2671 0.056 Uiso 1 1 calc R U . . .
H19B H 0.2000 0.0470 0.1949 0.056 Uiso 1 1 calc R U . . .
H19C H 0.1245 0.0945 0.2635 0.056 Uiso 1 1 calc R U . . .
C20 C 0.34911(18) 0.23779(17) 0.47819(10) 0.0251(5) Uani 1 1 d . . . . .
H20 H 0.3830 0.2818 0.4386 0.030 Uiso 1 1 calc R U . . .
C21 C 0.2441(2) 0.32325(19) 0.51325(12) 0.0340(5) Uani 1 1 d . . . . .
H21A H 0.1848 0.3638 0.4786 0.051 Uiso 1 1 calc R U . . .
H21B H 0.2697 0.3782 0.5304 0.051 Uiso 1 1 calc R U . . .
H21C H 0.2106 0.2824 0.5532 0.051 Uiso 1 1 calc R U . . .
C22 C 0.4432(2) 0.17593(19) 0.53208(11) 0.0298(5) Uani 1 1 d . . . . .
H22A H 0.4077 0.1454 0.5758 0.045 Uiso 1 1 calc R U . . .
H22B H 0.4773 0.2298 0.5426 0.045 Uiso 1 1 calc R U . . .
H22C H 0.5047 0.1131 0.5122 0.045 Uiso 1 1 calc R U . . .
C23 C 0.56150(18) 0.10022(18) 0.35138(11) 0.0275(5) Uani 1 1 d . . . . .
H23A H 0.6400 0.0768 0.3278 0.041 Uiso 1 1 calc R U . . .
H23B H 0.5341 0.0351 0.3619 0.041 Uiso 1 1 calc R U . . .
H23C H 0.5641 0.1270 0.3956 0.041 Uiso 1 1 calc R U . . .
C24 C 0.47905(17) 0.19513(16) 0.30351(10) 0.0206(4) Uani 1 1 d . . . . .
C25 C 0.52692(17) 0.24038(17) 0.24241(10) 0.0216(4) Uani 1 1 d . . . . .
H25 H 0.6100 0.2153 0.2387 0.026 Uiso 1 1 calc R U . . .
C26 C 0.47082(17) 0.31898(17) 0.18405(10) 0.0206(4) Uani 1 1 d . . . . .
C27 C 0.54921(18) 0.32204(19) 0.11725(11) 0.0275(5) Uani 1 1 d . . . . .
H27A H 0.5011 0.3533 0.0761 0.041 Uiso 1 1 calc R U . . .
H27B H 0.6023 0.2445 0.1125 0.041 Uiso 1 1 calc R U . . .
H27C H 0.5950 0.3703 0.1199 0.041 Uiso 1 1 calc R U . . .
C28 C 0.31054(16) 0.45821(16) 0.12263(10) 0.0192(4) Uani 1 1 d . . . . .
C29 C 0.33403(16) 0.56021(17) 0.10145(10) 0.0202(4) Uani 1 1 d . . . . .
C30 C 0.27963(17) 0.63223(17) 0.04191(10) 0.0221(4) Uani 1 1 d . . . . .
H30 H 0.2929 0.7023 0.0266 0.027 Uiso 1 1 calc R U . . .
C31 C 0.20703(18) 0.60377(18) 0.00482(10) 0.0249(4) Uani 1 1 d . . . . .
H31 H 0.1722 0.6535 -0.0360 0.030 Uiso 1 1 calc R U . . .
C32 C 0.18510(17) 0.50314(17) 0.02702(10) 0.0235(4) Uani 1 1 d . . . . .
H32 H 0.1351 0.4843 0.0012 0.028 Uiso 1 1 calc R U . . .
C33 C 0.23527(17) 0.42897(17) 0.08666(10) 0.0213(4) Uani 1 1 d . . . . .
C34 C 0.41209(18) 0.59649(18) 0.14090(11) 0.0241(4) Uani 1 1 d . . . . .
H34 H 0.4592 0.5275 0.1727 0.029 Uiso 1 1 calc R U . . .
C35 C 0.3400(2) 0.68583(19) 0.18777(11) 0.0296(5) Uani 1 1 d . . . . .
H35A H 0.2845 0.7502 0.1591 0.044 Uiso 1 1 calc R U . . .
H35B H 0.3923 0.7131 0.2084 0.044 Uiso 1 1 calc R U . . .
H35C H 0.2970 0.6515 0.2258 0.044 Uiso 1 1 calc R U . . .
C36 C 0.49821(19) 0.6401(2) 0.09001(12) 0.0315(5) Uani 1 1 d . . . . .
H36A H 0.4546 0.7090 0.0588 0.047 Uiso 1 1 calc R U . . .
H36B H 0.5450 0.5811 0.0614 0.047 Uiso 1 1 calc R U . . .
H36C H 0.5501 0.6580 0.1173 0.047 Uiso 1 1 calc R U . . .
C37 C 0.21102(17) 0.31806(17) 0.11099(11) 0.0233(4) Uani 1 1 d . . . . .
H37 H 0.2101 0.3035 0.1639 0.028 Uiso 1 1 calc R U . . .
C38 C 0.3107(2) 0.21792(19) 0.08389(13) 0.0344(5) Uani 1 1 d . . . . .
H38A H 0.3152 0.2301 0.0320 0.052 Uiso 1 1 calc R U . . .
H38B H 0.2956 0.1467 0.1016 0.052 Uiso 1 1 calc R U . . .
H38C H 0.3849 0.2129 0.1008 0.052 Uiso 1 1 calc R U . . .
C39 C 0.09294(19) 0.32176(19) 0.09043(12) 0.0304(5) Uani 1 1 d . . . . .
H39A H 0.0312 0.3904 0.1038 0.046 Uiso 1 1 calc R U . . .
H39B H 0.0767 0.2538 0.1151 0.046 Uiso 1 1 calc R U . . .
H39C H 0.0952 0.3234 0.0391 0.046 Uiso 1 1 calc R U . . .
C40 C -0.17640(17) 0.73106(16) 0.20243(10) 0.0208(4) Uani 1 1 d . . . . .
C41 C -0.16586(17) 0.64314(18) 0.16560(10) 0.0233(4) Uani 1 1 d . . . . .
C42 C -0.22978(18) 0.57131(18) 0.18231(11) 0.0258(5) Uani 1 1 d . . . . .
C43 C -0.31114(17) 0.58619(18) 0.23912(11) 0.0247(4) Uani 1 1 d . . . . .
C44 C -0.32731(17) 0.67337(18) 0.27670(10) 0.0237(4) Uani 1 1 d . . . . .
C45 C -0.26111(17) 0.74285(17) 0.25835(10) 0.0214(4) Uani 1 1 d . . . . .
C46 C -0.14433(18) 0.88435(17) 0.09819(11) 0.0231(4) Uani 1 1 d . . . . .
C47 C -0.26390(18) 0.94521(18) 0.09255(11) 0.0277(5) Uani 1 1 d . . . . .
C48 C -0.31470(18) 1.00695(18) 0.03131(12) 0.0291(5) Uani 1 1 d . . . . .
C49 C -0.24490(19) 1.01025(17) -0.03023(11) 0.0274(5) Uani 1 1 d . . . . .
C50 C -0.12646(19) 0.95272(17) -0.02810(11) 0.0262(5) Uani 1 1 d . . . . .
C51 C -0.07876(17) 0.89229(17) 0.03487(11) 0.0233(4) Uani 1 1 d . . . . .
C52 C -0.09840(17) 0.89650(18) 0.23118(11) 0.0247(4) Uani 1 1 d . . . . .
C53 C -0.13370(18) 1.01503(18) 0.21905(12) 0.0286(5) Uani 1 1 d . . . . .
C54 C -0.1296(2) 1.0789(2) 0.26875(14) 0.0363(6) Uani 1 1 d . . . . .
C55 C -0.0880(2) 1.0262(2) 0.33381(14) 0.0383(6) Uani 1 1 d . . . . .
C56 C -0.0510(2) 0.9091(2) 0.34882(12) 0.0343(5) Uani 1 1 d . . . . .
C57 C -0.05746(18) 0.84834(19) 0.29816(11) 0.0281(5) Uani 1 1 d . . . . .
N1 N 0.12048(14) 0.37908(13) 0.33358(8) 0.0203(3) Uani 1 1 d . . . . .
N2 N 0.36125(13) 0.23170(13) 0.32314(8) 0.0183(3) Uani 1 1 d . . . . .
N3 N 0.35924(13) 0.38349(13) 0.18655(8) 0.0174(3) Uani 1 1 d . . . . .
N4 N 0.13629(14) 0.55256(14) 0.22592(9) 0.0225(4) Uani 1 1 d . . . . .
N5 N 0.08229(14) 0.64194(14) 0.19768(8) 0.0203(4) Uani 1 1 d . . . . .
N6 N 0.03506(14) 0.73347(14) 0.16559(9) 0.0236(4) Uani 1 1 d . . . . .
F1 F -0.08789(10) 0.62412(10) 0.10880(6) 0.0297(3) Uani 1 1 d . . . . .
F2 F -0.21281(11) 0.48589(11) 0.14533(7) 0.0332(3) Uani 1 1 d . . . . .
F3 F -0.37207(11) 0.51535(11) 0.25724(7) 0.0337(3) Uani 1 1 d . . . . .
F4 F -0.40685(10) 0.68926(11) 0.33181(6) 0.0321(3) Uani 1 1 d . . . . .
F5 F -0.28376(10) 0.82711(10) 0.29780(6) 0.0271(3) Uani 1 1 d . . . . .
F6 F -0.33628(10) 0.95013(11) 0.15216(7) 0.0373(3) Uani 1 1 d . . . . .
F7 F -0.43037(11) 1.06480(12) 0.03054(7) 0.0415(3) Uani 1 1 d . . . . .
F8 F -0.29314(12) 1.06822(11) -0.09077(7) 0.0392(3) Uani 1 1 d . . . . .
F9 F -0.05774(11) 0.95555(11) -0.08801(6) 0.0355(3) Uani 1 1 d . . . . .
F10 F 0.03837(10) 0.84056(10) 0.03200(6) 0.0312(3) Uani 1 1 d . . . . .
F11 F -0.17706(11) 1.07653(10) 0.15700(7) 0.0358(3) Uani 1 1 d . . . . .
F12 F -0.16832(13) 1.19403(12) 0.25328(9) 0.0521(4) Uani 1 1 d . . . . .
F13 F -0.08385(14) 1.08808(14) 0.38247(9) 0.0562(4) Uani 1 1 d . . . . .
F14 F -0.00951(13) 0.85569(13) 0.41221(7) 0.0459(4) Uani 1 1 d . . . . .
F15 F -0.02333(11) 0.73373(11) 0.31649(6) 0.0331(3) Uani 1 1 d . . . . .
Nb1 Nb 0.24843(2) 0.39596(2) 0.29000(2) 0.01695(6) Uani 1 1 d . . . . .
B1 B -0.0991(2) 0.8144(2) 0.17500(12) 0.0233(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.400(3) . ?
C1 C6 1.400(3) . ?
C1 Nb1 2.144(2) . ?
C2 C3 1.385(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 N1 1.464(2) . ?
C7 C8 1.519(3) . ?
C7 C9 1.524(3) . ?
C7 C10 1.530(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C16 1.403(3) . ?
C11 C12 1.407(3) . ?
C11 N2 1.467(2) . ?
C12 C13 1.397(3) . ?
C12 C17 1.521(3) . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.375(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.403(3) . ?
C15 H15 0.9500 . ?
C16 C20 1.513(3) . ?
C17 C19 1.524(3) . ?
C17 C18 1.533(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.532(3) . ?
C20 C22 1.537(3) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.505(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.373(3) . ?
C24 N2 1.377(2) . ?
C25 C26 1.418(3) . ?
C25 H25 0.9500 . ?
C26 N3 1.319(2) . ?
C26 C27 1.513(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C33 1.401(3) . ?
C28 C29 1.405(3) . ?
C28 N3 1.452(2) . ?
C29 C30 1.398(3) . ?
C29 C34 1.525(3) . ?
C30 C31 1.382(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.381(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(3) . ?
C32 H32 0.9500 . ?
C33 C37 1.523(3) . ?
C34 C35 1.531(3) . ?
C34 C36 1.535(3) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C39 1.529(3) . ?
C37 C38 1.535(3) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.389(3) . ?
C40 C45 1.392(3) . ?
C40 B1 1.642(3) . ?
C41 F1 1.358(2) . ?
C41 C42 1.377(3) . ?
C42 F2 1.345(2) . ?
C42 C43 1.380(3) . ?
C43 F3 1.340(2) . ?
C43 C44 1.374(3) . ?
C44 F4 1.343(2) . ?
C44 C45 1.377(3) . ?
C45 F5 1.353(2) . ?
C46 C51 1.385(3) . ?
C46 C47 1.397(3) . ?
C46 B1 1.625(3) . ?
C47 F6 1.359(2) . ?
C47 C48 1.370(3) . ?
C48 F7 1.343(2) . ?
C48 C49 1.378(3) . ?
C49 F8 1.336(2) . ?
C49 C50 1.373(3) . ?
C50 F9 1.346(2) . ?
C50 C51 1.380(3) . ?
C51 F10 1.347(2) . ?
C52 C57 1.389(3) . ?
C52 C53 1.391(3) . ?
C52 B1 1.636(3) . ?
C53 F11 1.352(3) . ?
C53 C54 1.377(3) . ?
C54 F12 1.352(3) . ?
C54 C55 1.369(4) . ?
C55 F13 1.343(3) . ?
C55 C56 1.375(4) . ?
C56 F14 1.342(3) . ?
C56 C57 1.375(3) . ?
C57 F15 1.352(2) . ?
N1 Nb1 1.7529(16) . ?
N2 Nb1 2.0790(16) . ?
N3 Nb1 2.2673(15) . ?
N4 N5 1.159(2) . ?
N4 Nb1 2.2155(17) . ?
N5 N6 1.186(2) . ?
N6 B1 1.606(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 117.57(19) . . ?
C2 C1 Nb1 116.27(15) . . ?
C6 C1 Nb1 125.95(15) . . ?
C3 C2 C1 121.4(2) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C4 C3 C2 119.6(2) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 121.1(2) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
N1 C7 C8 108.13(16) . . ?
N1 C7 C9 107.48(16) . . ?
C8 C7 C9 110.70(18) . . ?
N1 C7 C10 109.24(17) . . ?
C8 C7 C10 111.06(18) . . ?
C9 C7 C10 110.13(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 121.64(18) . . ?
C16 C11 N2 120.11(17) . . ?
C12 C11 N2 118.25(17) . . ?
C13 C12 C11 117.94(19) . . ?
C13 C12 C17 119.13(19) . . ?
C11 C12 C17 122.93(18) . . ?
C14 C13 C12 121.3(2) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 119.97(19) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 121.5(2) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C11 117.65(19) . . ?
C15 C16 C20 118.59(18) . . ?
C11 C16 C20 123.75(17) . . ?
C12 C17 C19 112.28(17) . . ?
C12 C17 C18 110.90(18) . . ?
C19 C17 C18 109.84(18) . . ?
C12 C17 H17 107.9 . . ?
C19 C17 H17 107.9 . . ?
C18 C17 H17 107.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 C21 111.77(18) . . ?
C16 C20 C22 111.85(17) . . ?
C21 C20 C22 109.49(17) . . ?
C16 C20 H20 107.9 . . ?
C21 C20 H20 107.9 . . ?
C22 C20 H20 107.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 N2 123.93(18) . . ?
C25 C24 C23 117.29(17) . . ?
N2 C24 C23 118.78(17) . . ?
C24 C25 C26 129.62(18) . . ?
C24 C25 H25 115.2 . . ?
C26 C25 H25 115.2 . . ?
N3 C26 C25 123.52(17) . . ?
N3 C26 C27 122.02(17) . . ?
C25 C26 C27 114.45(17) . . ?
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 . . ?
C33 C28 C29 122.21(18) . . ?
C33 C28 N3 118.25(17) . . ?
C29 C28 N3 119.41(17) . . ?
C30 C29 C28 117.14(18) . . ?
C30 C29 C34 119.32(17) . . ?
C28 C29 C34 123.52(17) . . ?
C31 C30 C29 121.51(19) . . ?
C31 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
C32 C31 C30 120.10(19) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C33 120.93(19) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C32 C33 C28 118.07(18) . . ?
C32 C33 C37 120.84(18) . . ?
C28 C33 C37 121.07(18) . . ?
C29 C34 C35 111.62(17) . . ?
C29 C34 C36 111.80(17) . . ?
C35 C34 C36 110.61(17) . . ?
C29 C34 H34 107.5 . . ?
C35 C34 H34 107.5 . . ?
C36 C34 H34 107.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C33 C37 C39 114.00(17) . . ?
C33 C37 C38 110.38(17) . . ?
C39 C37 C38 110.49(17) . . ?
C33 C37 H37 107.2 . . ?
C39 C37 H37 107.2 . . ?
C38 C37 H37 107.2 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C45 113.57(18) . . ?
C41 C40 B1 119.86(17) . . ?
C45 C40 B1 126.42(18) . . ?
F1 C41 C42 115.95(18) . . ?
F1 C41 C40 119.45(18) . . ?
C42 C41 C40 124.60(18) . . ?
F2 C42 C41 121.40(18) . . ?
F2 C42 C43 119.53(18) . . ?
C41 C42 C43 119.06(19) . . ?
F3 C43 C44 121.09(18) . . ?
F3 C43 C42 119.89(18) . . ?
C44 C43 C42 119.01(19) . . ?
F4 C44 C43 119.59(18) . . ?
F4 C44 C45 120.43(18) . . ?
C43 C44 C45 119.98(18) . . ?
F5 C45 C44 115.93(17) . . ?
F5 C45 C40 120.32(18) . . ?
C44 C45 C40 123.75(18) . . ?
C51 C46 C47 113.45(19) . . ?
C51 C46 B1 128.19(18) . . ?
C47 C46 B1 118.36(17) . . ?
F6 C47 C48 116.15(18) . . ?
F6 C47 C46 118.88(18) . . ?
C48 C47 C46 124.87(19) . . ?
F7 C48 C47 121.23(19) . . ?
F7 C48 C49 119.84(19) . . ?
C47 C48 C49 118.9(2) . . ?
F8 C49 C50 121.18(19) . . ?
F8 C49 C48 119.80(19) . . ?
C50 C49 C48 119.02(19) . . ?
F9 C50 C49 119.35(19) . . ?
F9 C50 C51 120.49(19) . . ?
C49 C50 C51 120.16(18) . . ?
F10 C51 C50 115.84(17) . . ?
F10 C51 C46 120.58(18) . . ?
C50 C51 C46 123.57(19) . . ?
C57 C52 C53 113.5(2) . . ?
C57 C52 B1 119.97(18) . . ?
C53 C52 B1 126.49(19) . . ?
F11 C53 C54 114.9(2) . . ?
F11 C53 C52 121.75(19) . . ?
C54 C53 C52 123.4(2) . . ?
F12 C54 C55 120.1(2) . . ?
F12 C54 C53 119.6(2) . . ?
C55 C54 C53 120.3(2) . . ?
F13 C55 C54 120.5(2) . . ?
F13 C55 C56 120.4(2) . . ?
C54 C55 C56 119.1(2) . . ?
F14 C56 C57 120.9(2) . . ?
F14 C56 C55 120.1(2) . . ?
C57 C56 C55 119.0(2) . . ?
F15 C57 C56 116.5(2) . . ?
F15 C57 C52 118.73(19) . . ?
C56 C57 C52 124.7(2) . . ?
C7 N1 Nb1 165.12(14) . . ?
C24 N2 C11 115.73(15) . . ?
C24 N2 Nb1 122.80(12) . . ?
C11 N2 Nb1 121.28(11) . . ?
C26 N3 C28 118.55(15) . . ?
C26 N3 Nb1 121.74(12) . . ?
C28 N3 Nb1 119.31(11) . . ?
N5 N4 Nb1 171.24(15) . . ?
N4 N5 N6 174.70(19) . . ?
N5 N6 B1 127.77(16) . . ?
N1 Nb1 N2 97.04(7) . . ?
N1 Nb1 C1 101.98(7) . . ?
N2 Nb1 C1 100.26(7) . . ?
N1 Nb1 N4 88.06(7) . . ?
N2 Nb1 N4 163.83(6) . . ?
C1 Nb1 N4 93.62(7) . . ?
N1 Nb1 N3 144.04(7) . . ?
N2 Nb1 N3 85.61(6) . . ?
C1 Nb1 N3 112.87(7) . . ?
N4 Nb1 N3 81.36(6) . . ?
N6 B1 C46 109.24(16) . . ?
N6 B1 C52 104.63(17) . . ?
C46 B1 C52 113.47(17) . . ?
N6 B1 C40 107.30(16) . . ?
C46 B1 C40 107.01(17) . . ?
C52 B1 C40 114.93(16) . . ?

_refine_diff_density_max         0.441
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.054



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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1459083'
_audit_update_record             
;
2016-03-08 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            '[Nb(BDI)(NPhtBu)(NB(C6F5)3)].(toluene)0.5'
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C57 H55 B F15 N4 Nb), C7 H8'
_chemical_formula_sum            'C121 H118 B2 F30 N8 Nb2'
_chemical_formula_weight         2461.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   19.3473(5)
_cell_length_b                   22.4336(7)
_cell_length_c                   25.5172(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11075.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9199
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.35

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_F_000             5048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.312
_shelx_estimated_absorpt_T_min   0.885
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7020
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            159023
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.596
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10157
_reflns_number_gt                7948
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0324P)²+14.4418P] 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         10157
_refine_ls_number_parameters     780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.76859(12) 0.06073(11) 0.11155(10) 0.0205(5) Uani 1 1 d . . . . .
C2 C 0.82270(13) 0.08566(12) 0.08267(11) 0.0257(6) Uani 1 1 d . . . . .
H2 H 0.8130 0.1060 0.0508 0.031 Uiso 1 1 calc R U . . .
C3 C 0.89035(14) 0.08112(13) 0.09995(12) 0.0332(7) Uani 1 1 d . . . . .
H3 H 0.9267 0.0982 0.0799 0.040 Uiso 1 1 calc R U . . .
C4 C 0.90511(14) 0.05177(13) 0.14624(12) 0.0327(7) Uani 1 1 d . . . . .
H4 H 0.9515 0.0492 0.1583 0.039 Uiso 1 1 calc R U . . .
C5 C 0.85211(14) 0.02616(12) 0.17499(11) 0.0282(6) Uani 1 1 d . . . . .
H5 H 0.8621 0.0059 0.2068 0.034 Uiso 1 1 calc R U . . .
C6 C 0.78422(13) 0.03024(11) 0.15717(10) 0.0212(5) Uani 1 1 d . . . . .
H6 H 0.7482 0.0118 0.1766 0.025 Uiso 1 1 calc R U . . .
C7 C 0.67035(13) 0.02267(11) 0.05793(10) 0.0238(6) Uani 1 1 d . . . . .
C8 C 0.72027(15) 0.01494(13) 0.01206(11) 0.0327(7) Uani 1 1 d . . . . .
H8A H 0.7251 0.0529 -0.0065 0.049 Uiso 1 1 calc R U . . .
H8B H 0.7022 -0.0153 -0.0120 0.049 Uiso 1 1 calc R U . . .
H8C H 0.7655 0.0023 0.0253 0.049 Uiso 1 1 calc R U . . .
C9 C 0.66299(14) -0.03684(12) 0.08658(12) 0.0301(6) Uani 1 1 d . . . . .
H9A H 0.7081 -0.0490 0.1004 0.045 Uiso 1 1 calc R U . . .
H9B H 0.6460 -0.0672 0.0621 0.045 Uiso 1 1 calc R U . . .
H9C H 0.6301 -0.0324 0.1156 0.045 Uiso 1 1 calc R U . . .
C10 C 0.60063(14) 0.04280(12) 0.03645(11) 0.0261(6) Uani 1 1 d . . . . .
H10A H 0.5676 0.0467 0.0653 0.039 Uiso 1 1 calc R U . . .
H10B H 0.5836 0.0133 0.0113 0.039 Uiso 1 1 calc R U . . .
H10C H 0.6059 0.0814 0.0189 0.039 Uiso 1 1 calc R U . . .
C11 C 0.69651(12) 0.26459(11) 0.08047(10) 0.0197(5) Uani 1 1 d . . . . .
C12 C 0.67759(12) 0.32062(11) 0.10062(11) 0.0228(6) Uani 1 1 d . . . . .
C13 C 0.67677(14) 0.36838(12) 0.06665(12) 0.0297(7) Uani 1 1 d . . . . .
H13 H 0.6649 0.4067 0.0797 0.036 Uiso 1 1 calc R U . . .
C14 C 0.69292(14) 0.36189(12) 0.01359(11) 0.0295(6) Uani 1 1 d . . . . .
H14 H 0.6942 0.3957 -0.0088 0.035 Uiso 1 1 calc R U . . .
C15 C 0.70707(13) 0.30576(13) -0.00587(11) 0.0279(6) Uani 1 1 d . . . . .
H15 H 0.7158 0.3010 -0.0423 0.034 Uiso 1 1 calc R U . . .
C16 C 0.70880(12) 0.25580(12) 0.02679(10) 0.0225(6) Uani 1 1 d . . . . .
C17 C 0.65912(13) 0.33003(11) 0.15811(11) 0.0257(6) Uani 1 1 d . . . . .
H17 H 0.6492 0.2901 0.1739 0.031 Uiso 1 1 calc R U . . .
C18 C 0.72018(15) 0.35756(13) 0.18808(11) 0.0326(7) Uani 1 1 d . . . . .
H18A H 0.7590 0.3295 0.1882 0.049 Uiso 1 1 calc R U . . .
H18B H 0.7062 0.3660 0.2242 0.049 Uiso 1 1 calc R U . . .
H18C H 0.7343 0.3947 0.1709 0.049 Uiso 1 1 calc R U . . .
C19 C 0.59449(15) 0.36881(13) 0.16463(13) 0.0349(7) Uani 1 1 d . . . . .
H19A H 0.6029 0.4082 0.1494 0.052 Uiso 1 1 calc R U . . .
H19B H 0.5838 0.3731 0.2020 0.052 Uiso 1 1 calc R U . . .
H19C H 0.5554 0.3499 0.1467 0.052 Uiso 1 1 calc R U . . .
C20 C 0.72320(13) 0.19532(12) 0.00228(11) 0.0258(6) Uani 1 1 d . . . . .
H20 H 0.7258 0.1651 0.0310 0.031 Uiso 1 1 calc R U . . .
C21 C 0.79186(15) 0.19421(15) -0.02783(12) 0.0385(7) Uani 1 1 d . . . . .
H21A H 0.7898 0.2227 -0.0569 0.058 Uiso 1 1 calc R U . . .
H21B H 0.7999 0.1541 -0.0417 0.058 Uiso 1 1 calc R U . . .
H21C H 0.8297 0.2052 -0.0042 0.058 Uiso 1 1 calc R U . . .
C22 C 0.66330(15) 0.17819(13) -0.03416(11) 0.0305(6) Uani 1 1 d . . . . .
H22A H 0.6206 0.1748 -0.0137 0.046 Uiso 1 1 calc R U . . .
H22B H 0.6734 0.1399 -0.0510 0.046 Uiso 1 1 calc R U . . .
H22C H 0.6576 0.2090 -0.0611 0.046 Uiso 1 1 calc R U . . .
C23 C 0.83127(12) 0.24796(13) 0.11234(11) 0.0281(6) Uani 1 1 d . . . . .
H23A H 0.8367 0.2352 0.0758 0.042 Uiso 1 1 calc R U . . .
H23B H 0.8743 0.2406 0.1315 0.042 Uiso 1 1 calc R U . . .
H23C H 0.8204 0.2906 0.1134 0.042 Uiso 1 1 calc R U . . .
C24 C 0.77344(12) 0.21329(11) 0.13741(10) 0.0197(5) Uani 1 1 d . . . . .
C26 C 0.79146(12) 0.17776(11) 0.18093(9) 0.0183(5) Uani 1 1 d . . . . .
H26 H 0.8397 0.1702 0.1835 0.022 Uiso 1 1 calc R U . . .
C27 C 0.75292(12) 0.15132(11) 0.22121(9) 0.0176(5) Uani 1 1 d . . . . .
C28 C 0.79325(12) 0.13052(12) 0.26822(10) 0.0232(6) Uani 1 1 d . . . . .
H28A H 0.7979 0.1634 0.2932 0.035 Uiso 1 1 calc R U . . .
H28B H 0.8392 0.1173 0.2571 0.035 Uiso 1 1 calc R U . . .
H28C H 0.7689 0.0973 0.2849 0.035 Uiso 1 1 calc R U . . .
C30 C 0.64977(12) 0.13592(11) 0.27002(9) 0.0166(5) Uani 1 1 d . . . . .
C31 C 0.62551(12) 0.07970(11) 0.28602(10) 0.0194(5) Uani 1 1 d . . . . .
C32 C 0.60030(12) 0.07428(12) 0.33693(10) 0.0235(6) Uani 1 1 d . . . . .
H32 H 0.5846 0.0365 0.3488 0.028 Uiso 1 1 calc R U . . .
C33 C 0.59758(13) 0.12235(13) 0.37064(10) 0.0262(6) Uani 1 1 d . . . . .
H33 H 0.5805 0.1175 0.4053 0.031 Uiso 1 1 calc R U . . .
C34 C 0.61968(13) 0.17728(12) 0.35380(10) 0.0239(6) Uani 1 1 d . . . . .
H34 H 0.6170 0.2103 0.3770 0.029 Uiso 1 1 calc R U . . .
C35 C 0.64601(12) 0.18565(11) 0.30344(10) 0.0197(5) Uani 1 1 d . . . . .
C36 C 0.62782(13) 0.02350(11) 0.25280(10) 0.0226(6) Uani 1 1 d . . . . .
H36 H 0.6357 0.0354 0.2155 0.027 Uiso 1 1 calc R U . . .
C37 C 0.68797(15) -0.01678(13) 0.26998(12) 0.0331(7) Uani 1 1 d . . . . .
H37A H 0.7316 0.0051 0.2667 0.050 Uiso 1 1 calc R U . . .
H37B H 0.6894 -0.0523 0.2477 0.050 Uiso 1 1 calc R U . . .
H37C H 0.6813 -0.0288 0.3066 0.050 Uiso 1 1 calc R U . . .
C38 C 0.56033(15) -0.01202(12) 0.25565(12) 0.0317(7) Uani 1 1 d . . . . .
H38A H 0.5551 -0.0290 0.2908 0.048 Uiso 1 1 calc R U . . .
H38B H 0.5614 -0.0442 0.2297 0.048 Uiso 1 1 calc R U . . .
H38C H 0.5212 0.0145 0.2483 0.048 Uiso 1 1 calc R U . . .
C39 C 0.66869(13) 0.24848(12) 0.28787(10) 0.0231(6) Uani 1 1 d . . . . .
H39 H 0.6852 0.2472 0.2507 0.028 Uiso 1 1 calc R U . . .
C40 C 0.60828(14) 0.29175(12) 0.29089(13) 0.0356(7) Uani 1 1 d . . . . .
H40A H 0.5739 0.2812 0.2643 0.053 Uiso 1 1 calc R U . . .
H40B H 0.6249 0.3324 0.2846 0.053 Uiso 1 1 calc R U . . .
H40C H 0.5871 0.2895 0.3257 0.053 Uiso 1 1 calc R U . . .
C41 C 0.72825(15) 0.27107(14) 0.32219(12) 0.0363(7) Uani 1 1 d . . . . .
H41A H 0.7444 0.3096 0.3089 0.054 Uiso 1 1 calc R U . . .
H41B H 0.7663 0.2423 0.3213 0.054 Uiso 1 1 calc R U . . .
H41C H 0.7121 0.2757 0.3584 0.054 Uiso 1 1 calc R U . . .
C42 C 0.49031(12) 0.18155(11) 0.05506(10) 0.0194(5) Uani 1 1 d . . . . .
C43 C 0.51542(12) 0.23841(12) 0.04406(11) 0.0244(6) Uani 1 1 d . . . . .
C44 C 0.51507(13) 0.26446(13) -0.00475(13) 0.0340(7) Uani 1 1 d . . . . .
C45 C 0.49203(13) 0.23233(15) -0.04680(11) 0.0349(7) Uani 1 1 d . . . . .
C46 C 0.46907(13) 0.17541(14) -0.03930(11) 0.0311(7) Uani 1 1 d . . . . .
C47 C 0.46843(12) 0.15136(12) 0.01071(10) 0.0242(6) Uani 1 1 d . . . . .
C48 C 0.44372(12) 0.09547(11) 0.12180(9) 0.0185(5) Uani 1 1 d . . . . .
C49 C 0.37303(12) 0.10028(11) 0.11215(10) 0.0211(6) Uani 1 1 d . . . . .
C50 C 0.32682(13) 0.05382(13) 0.11658(10) 0.0255(6) Uani 1 1 d . . . . .
C51 C 0.34973(14) -0.00133(12) 0.13162(11) 0.0302(7) Uani 1 1 d . . . . .
C52 C 0.41899(14) -0.00876(12) 0.14260(11) 0.0281(6) Uani 1 1 d . . . . .
C53 C 0.46372(13) 0.03905(12) 0.13788(10) 0.0228(6) Uani 1 1 d . . . . .
C54 C 0.46386(12) 0.20174(11) 0.16071(10) 0.0195(5) Uani 1 1 d . . . . .
C55 C 0.47381(12) 0.18674(11) 0.21291(10) 0.0212(6) Uani 1 1 d . . . . .
C56 C 0.45429(13) 0.22144(13) 0.25491(10) 0.0259(6) Uani 1 1 d . . . . .
C57 C 0.42243(13) 0.27542(13) 0.24589(12) 0.0312(7) Uani 1 1 d . . . . .
C58 C 0.40971(13) 0.29230(12) 0.19500(12) 0.0290(6) Uani 1 1 d . . . . .
C59 C 0.42850(13) 0.25520(12) 0.15414(11) 0.0245(6) Uani 1 1 d . . . . .
C100 C 0.5065(18) 0.5079(15) -0.0079(11) 0.053(6) Uani 0.5 1 d . . P A -1
C101 C 0.5278(6) 0.4549(6) 0.0134(5) 0.076(4) Uani 0.5 1 d . . P A -1
H101 H 0.5715 0.4394 0.0035 0.091 Uiso 0.5 1 calc R U P A -1
C102 C 0.4888(8) 0.4236(4) 0.0483(5) 0.084(4) Uani 0.5 1 d . . P A -1
H102 H 0.5067 0.3877 0.0627 0.101 Uiso 0.5 1 calc R U P A -1
C103 C 0.4239(7) 0.4428(5) 0.0631(5) 0.062(3) Uani 0.5 1 d . . P A -1
H103 H 0.3964 0.4204 0.0868 0.074 Uiso 0.5 1 calc R U P A -1
C104 C 0.4001(4) 0.4963(3) 0.0420(3) 0.0499(19) Uani 0.5 1 d . . P A -1
H104 H 0.3558 0.5110 0.0518 0.060 Uiso 0.5 1 calc R U P A -1
C105 C 0.4399(4) 0.5280(4) 0.0073(4) 0.042(2) Uani 0.5 1 d . . P A -1
H105 H 0.4225 0.5641 -0.0069 0.050 Uiso 0.5 1 calc R U P A -1
C106 C 0.5480(6) 0.5442(7) -0.0458(6) 0.076(5) Uani 0.5 1 d . . P A -1
H10D H 0.5947 0.5276 -0.0486 0.114 Uiso 0.5 1 calc R U P A -1
H10E H 0.5507 0.5855 -0.0333 0.114 Uiso 0.5 1 calc R U P A -1
H10F H 0.5257 0.5434 -0.0802 0.114 Uiso 0.5 1 calc R U P A -1
B2 B 0.49305(14) 0.15515(12) 0.11528(11) 0.0180(6) Uani 1 1 d . . . . .
N1 N 0.69670(10) 0.06899(9) 0.09600(8) 0.0185(4) Uani 1 1 d . . . . .
N2 N 0.70873(10) 0.21657(9) 0.11799(8) 0.0166(4) Uani 1 1 d . . . . .
N3 N 0.68338(10) 0.14394(9) 0.21906(8) 0.0155(4) Uani 1 1 d . . . . .
N4 N 0.57163(10) 0.14411(8) 0.12682(8) 0.0164(4) Uani 1 1 d . . . . .
F1 F 0.54084(7) 0.27176(6) 0.08373(6) 0.0303(4) Uani 1 1 d . . . . .
F2 F 0.53804(9) 0.32032(8) -0.01196(8) 0.0499(5) Uani 1 1 d . . . . .
F3 F 0.49378(8) 0.25592(10) -0.09523(7) 0.0555(6) Uani 1 1 d . . . . .
F4 F 0.44868(9) 0.14274(9) -0.08083(6) 0.0460(5) Uani 1 1 d . . . . .
F5 F 0.44505(8) 0.09462(7) 0.01398(6) 0.0293(4) Uani 1 1 d . . . . .
F6 F 0.34670(7) 0.15341(7) 0.09652(6) 0.0273(3) Uani 1 1 d . . . . .
F7 F 0.25901(7) 0.06233(7) 0.10623(6) 0.0339(4) Uani 1 1 d . . . . .
F8 F 0.30600(9) -0.04752(7) 0.13544(7) 0.0428(5) Uani 1 1 d . . . . .
F9 F 0.44236(9) -0.06251(7) 0.15768(8) 0.0439(5) Uani 1 1 d . . . . .
F10 F 0.53032(8) 0.02740(7) 0.14960(6) 0.0321(4) Uani 1 1 d . . . . .
F11 F 0.50244(7) 0.13338(7) 0.22498(6) 0.0250(3) Uani 1 1 d . . . . .
F12 F 0.46564(8) 0.20298(8) 0.30435(6) 0.0346(4) Uani 1 1 d . . . . .
F13 F 0.40480(9) 0.31101(8) 0.28596(7) 0.0438(5) Uani 1 1 d . . . . .
F14 F 0.37806(8) 0.34473(7) 0.18541(8) 0.0401(4) Uani 1 1 d . . . . .
F15 F 0.40958(7) 0.27459(7) 0.10623(6) 0.0307(4) Uani 1 1 d . . . . .
Nb1 Nb 0.65968(2) 0.13659(2) 0.13862(2) 0.01323(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 C6 1.384(4) . ?
C1 C2 1.397(4) . ?
C1 N1 1.458(3) . ?
C2 C3 1.385(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 N1 1.511(3) . ?
C7 C10 1.524(4) . ?
C7 C8 1.527(4) . ?
C7 C9 1.529(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C16 1.404(4) . ?
C11 C12 1.407(4) . ?
C11 N2 1.461(3) . ?
C12 C13 1.378(4) . ?
C12 C17 1.525(4) . ?
C13 C14 1.397(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.397(4) . ?
C15 H15 0.9500 . ?
C16 C20 1.520(4) . ?
C17 C19 1.532(4) . ?
C17 C18 1.537(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.535(4) . ?
C20 C21 1.535(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.505(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N2 1.348(3) . ?
C24 C26 1.411(3) . ?
C26 C27 1.402(3) . ?
C26 H26 0.9500 . ?
C27 N3 1.357(3) . ?
C27 C28 1.505(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 C31 1.406(3) . ?
C30 C35 1.406(3) . ?
C30 N3 1.465(3) . ?
C31 C32 1.393(4) . ?
C31 C36 1.520(3) . ?
C32 C33 1.381(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.373(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.395(4) . ?
C34 H34 0.9500 . ?
C35 C39 1.529(4) . ?
C36 C38 1.531(4) . ?
C36 C37 1.537(4) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.521(4) . ?
C39 C41 1.534(4) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C47 1.385(4) . ?
C42 C43 1.394(4) . ?
C42 B2 1.648(4) . ?
C43 F1 1.351(3) . ?
C43 C44 1.376(4) . ?
C44 F2 1.342(3) . ?
C44 C45 1.367(4) . ?
C45 F3 1.345(3) . ?
C45 C46 1.366(4) . ?
C46 F4 1.347(3) . ?
C46 C47 1.385(4) . ?
C47 F5 1.353(3) . ?
C48 C53 1.386(4) . ?
C48 C49 1.394(3) . ?
C48 B2 1.653(4) . ?
C49 F6 1.356(3) . ?
C49 C50 1.378(4) . ?
C50 F7 1.352(3) . ?
C50 C51 1.369(4) . ?
C51 F8 1.341(3) . ?
C51 C52 1.379(4) . ?
C52 F9 1.344(3) . ?
C52 C53 1.383(4) . ?
C53 F10 1.348(3) . ?
C54 C55 1.387(4) . ?
C54 C59 1.391(4) . ?
C54 B2 1.660(4) . ?
C55 F11 1.354(3) . ?
C55 C56 1.377(4) . ?
C56 F12 1.346(3) . ?
C56 C57 1.378(4) . ?
C57 F13 1.341(3) . ?
C57 C58 1.375(4) . ?
C58 F14 1.348(3) . ?
C58 C59 1.383(4) . ?
C59 F15 1.348(3) . ?
C100 C101 1.37(4) . ?
C100 C105 1.42(4) . ?
C100 C106 1.50(2) . ?
C101 C102 1.362(17) . ?
C101 H101 0.9500 . ?
C102 C103 1.381(19) . ?
C102 H102 0.9500 . ?
C103 C104 1.393(13) . ?
C103 H103 0.9500 . ?
C104 C105 1.373(11) . ?
C104 H104 0.9500 . ?
C105 H105 0.9500 . ?
C106 H10D 0.9800 . ?
C106 H10E 0.9800 . ?
C106 H10F 0.9800 . ?
B2 N4 1.568(3) . ?
N1 Nb1 1.999(2) . ?
N2 Nb1 2.097(2) . ?
N3 Nb1 2.110(2) . ?
N4 Nb1 1.7381(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
C6 C1 C2 118.5(2) . . ?
C6 C1 N1 120.0(2) . . ?
C2 C1 N1 121.4(2) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 119.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 120.9(2) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
N1 C7 C10 109.0(2) . . ?
N1 C7 C8 110.9(2) . . ?
C10 C7 C8 108.5(2) . . ?
N1 C7 C9 108.9(2) . . ?
C10 C7 C9 110.4(2) . . ?
C8 C7 C9 109.0(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 121.7(2) . . ?
C16 C11 N2 120.6(2) . . ?
C12 C11 N2 117.5(2) . . ?
C13 C12 C11 117.9(3) . . ?
C13 C12 C17 119.6(2) . . ?
C11 C12 C17 122.4(2) . . ?
C12 C13 C14 121.7(3) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 119.2(2) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 121.4(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C11 117.7(2) . . ?
C15 C16 C20 118.4(2) . . ?
C11 C16 C20 123.9(2) . . ?
C12 C17 C19 112.0(2) . . ?
C12 C17 C18 110.7(2) . . ?
C19 C17 C18 110.2(2) . . ?
C12 C17 H17 107.9 . . ?
C19 C17 H17 107.9 . . ?
C18 C17 H17 107.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 C22 109.5(2) . . ?
C16 C20 C21 112.3(2) . . ?
C22 C20 C21 110.3(2) . . ?
C16 C20 H20 108.2 . . ?
C22 C20 H20 108.2 . . ?
C21 C20 H20 108.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 C26 123.3(2) . . ?
N2 C24 C23 120.4(2) . . ?
C26 C24 C23 116.3(2) . . ?
C27 C26 C24 133.2(2) . . ?
C27 C26 H26 113.4 . . ?
C24 C26 H26 113.4 . . ?
N3 C27 C26 123.3(2) . . ?
N3 C27 C28 120.6(2) . . ?
C26 C27 C28 116.1(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 . . ?
C31 C30 C35 121.2(2) . . ?
C31 C30 N3 121.1(2) . . ?
C35 C30 N3 117.6(2) . . ?
C32 C31 C30 117.8(2) . . ?
C32 C31 C36 117.3(2) . . ?
C30 C31 C36 124.9(2) . . ?
C33 C32 C31 121.7(2) . . ?
C33 C32 H32 119.1 . . ?
C31 C32 H32 119.1 . . ?
C34 C33 C32 119.6(2) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 121.5(2) . . ?
C33 C34 H34 119.2 . . ?
C35 C34 H34 119.2 . . ?
C34 C35 C30 118.1(2) . . ?
C34 C35 C39 117.9(2) . . ?
C30 C35 C39 124.0(2) . . ?
C31 C36 C38 112.3(2) . . ?
C31 C36 C37 110.5(2) . . ?
C38 C36 C37 109.0(2) . . ?
C31 C36 H36 108.3 . . ?
C38 C36 H36 108.3 . . ?
C37 C36 H36 108.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C35 110.8(2) . . ?
C40 C39 C41 109.7(2) . . ?
C35 C39 C41 111.8(2) . . ?
C40 C39 H39 108.1 . . ?
C35 C39 H39 108.1 . . ?
C41 C39 H39 108.1 . . ?
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 . . ?
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 . . ?
C47 C42 C43 112.9(2) . . ?
C47 C42 B2 126.6(2) . . ?
C43 C42 B2 120.4(2) . . ?
F1 C43 C44 116.4(2) . . ?
F1 C43 C42 118.9(2) . . ?
C44 C43 C42 124.7(3) . . ?
F2 C44 C45 119.5(3) . . ?
F2 C44 C43 121.3(3) . . ?
C45 C44 C43 119.2(3) . . ?
F3 C45 C46 120.3(3) . . ?
F3 C45 C44 120.4(3) . . ?
C46 C45 C44 119.3(3) . . ?
F4 C46 C45 119.6(3) . . ?
F4 C46 C47 120.7(3) . . ?
C45 C46 C47 119.7(3) . . ?
F5 C47 C42 120.8(2) . . ?
F5 C47 C46 115.2(2) . . ?
C42 C47 C46 124.0(3) . . ?
C53 C48 C49 113.4(2) . . ?
C53 C48 B2 127.5(2) . . ?
C49 C48 B2 119.1(2) . . ?
F6 C49 C50 116.4(2) . . ?
F6 C49 C48 119.2(2) . . ?
C50 C49 C48 124.3(2) . . ?
F7 C50 C51 119.8(2) . . ?
F7 C50 C49 120.5(2) . . ?
C51 C50 C49 119.8(2) . . ?
F8 C51 C50 120.9(2) . . ?
F8 C51 C52 120.3(3) . . ?
C50 C51 C52 118.7(2) . . ?
F9 C52 C51 119.6(2) . . ?
F9 C52 C53 120.7(2) . . ?
C51 C52 C53 119.8(2) . . ?
F10 C53 C52 115.4(2) . . ?
F10 C53 C48 120.6(2) . . ?
C52 C53 C48 124.0(2) . . ?
C55 C54 C59 113.2(2) . . ?
C55 C54 B2 118.1(2) . . ?
C59 C54 B2 128.8(2) . . ?
F11 C55 C56 115.8(2) . . ?
F11 C55 C54 119.3(2) . . ?
C56 C55 C54 124.9(2) . . ?
F12 C56 C55 120.7(2) . . ?
F12 C56 C57 120.0(2) . . ?
C55 C56 C57 119.3(3) . . ?
F13 C57 C58 120.7(3) . . ?
F13 C57 C56 120.6(3) . . ?
C58 C57 C56 118.7(2) . . ?
F14 C58 C57 119.5(2) . . ?
F14 C58 C59 120.5(3) . . ?
C57 C58 C59 120.0(2) . . ?
F15 C59 C58 114.7(2) . . ?
F15 C59 C54 121.4(2) . . ?
C58 C59 C54 123.9(3) . . ?
C101 C100 C105 116.1(14) . . ?
C101 C100 C106 125(3) . . ?
C105 C100 C106 119(3) . . ?
C102 C101 C100 122.8(14) . . ?
C102 C101 H101 118.6 . . ?
C100 C101 H101 118.6 . . ?
C101 C102 C103 121.3(9) . . ?
C101 C102 H102 119.3 . . ?
C103 C102 H102 119.3 . . ?
C102 C103 C104 117.7(11) . . ?
C102 C103 H103 121.1 . . ?
C104 C103 H103 121.1 . . ?
C105 C104 C103 120.6(9) . . ?
C105 C104 H104 119.7 . . ?
C103 C104 H104 119.7 . . ?
C104 C105 C100 121.4(14) . . ?
C104 C105 H105 119.3 . . ?
C100 C105 H105 119.3 . . ?
C100 C106 H10D 109.5 . . ?
C100 C106 H10E 109.5 . . ?
H10D C106 H10E 109.5 . . ?
C100 C106 H10F 109.5 . . ?
H10D C106 H10F 109.5 . . ?
H10E C106 H10F 109.5 . . ?
N4 B2 C42 105.24(19) . . ?
N4 B2 C48 114.4(2) . . ?
C42 B2 C48 111.5(2) . . ?
N4 B2 C54 107.35(19) . . ?
C42 B2 C54 114.5(2) . . ?
C48 B2 C54 104.09(19) . . ?
C1 N1 C7 114.17(19) . . ?
C1 N1 Nb1 106.86(14) . . ?
C7 N1 Nb1 138.64(15) . . ?
C24 N2 C11 115.56(19) . . ?
C24 N2 Nb1 106.34(15) . . ?
C11 N2 Nb1 136.26(15) . . ?
C27 N3 C30 114.79(19) . . ?
C27 N3 Nb1 105.34(15) . . ?
C30 N3 Nb1 139.25(14) . . ?
B2 N4 Nb1 176.37(17) . . ?
N4 Nb1 N1 109.30(8) . . ?
N4 Nb1 N2 108.48(8) . . ?
N1 Nb1 N2 110.51(8) . . ?
N4 Nb1 N3 111.96(8) . . ?
N1 Nb1 N3 120.72(8) . . ?
N2 Nb1 N3 94.53(8) . . ?

_refine_diff_density_max         0.843
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.066


_iucr_refine_instructuions_details 
;

    shelx.res created by SHELXL-2014/7

TITL cc_ln_04_0m in Pbca
CELL 0.71073  19.34730  22.43360  25.51720  90.0000  90.0000  90.0000
ZERR    4.00   0.00050   0.00070   0.00090   0.0000   0.0000   0.0000
 
LATT   1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  - X, 1/2 + Y, 1/2 - Z
SYMM  1/2 + X, 1/2 - Y, - Z
SFAC  C    H    B    N    F    NB
UNIT  484 472 8 32 120 8
MERG   2
FMAP   2
PLAN   20
SIZE     0.100   0.400   0.400
ACTA    50.00
BOND   $H
LIST   4
WPDB  -2
L.S.  10
TEMP  -173.00
WGHT    0.032400   14.441800
FVAR       0.04562
C1    1    0.768589    0.060734    0.111550    11.00000    0.01962    0.02185 =
         0.02005   -0.00566    0.00141    0.00478
C2    1    0.822696    0.085663    0.082671    11.00000    0.02420    0.02731 =
         0.02547    0.00134    0.00417    0.00637
AFIX  43
H2    2    0.812977    0.105952    0.050834    11.00000   -1.20000
AFIX   0
C3    1    0.890351    0.081121    0.099948    11.00000    0.01919    0.03636 =
         0.04413    0.00162    0.00805    0.00301
AFIX  43
H3    2    0.926701    0.098216    0.079933    11.00000   -1.20000
AFIX   0
C4    1    0.905107    0.051774    0.146243    11.00000    0.01919    0.03636 =
         0.04260   -0.00656   -0.00379    0.00602
AFIX  43
H4    2    0.951458    0.049174    0.158316    11.00000   -1.20000
AFIX   0
C5    1    0.852113    0.026158    0.174994    11.00000    0.02928    0.02777 =
         0.02758   -0.00237   -0.00619    0.00855
AFIX  43
H5    2    0.862052    0.005860    0.206788    11.00000   -1.20000
AFIX   0
C6    1    0.784223    0.030237    0.157168    11.00000    0.02039    0.02036 =
         0.02275   -0.00170    0.00083    0.00244
AFIX  43
H6    2    0.748176    0.011834    0.176592    11.00000   -1.20000
AFIX   0
C7    1    0.670352    0.022672    0.057933    11.00000    0.02815    0.02289 =
         0.02045   -0.00749   -0.00351    0.00286
C8    1    0.720274    0.014943    0.012064    11.00000    0.03906    0.03538 =
         0.02376   -0.01027   -0.00331    0.01090
AFIX 137
H8A   2    0.725135    0.052924   -0.006547    11.00000   -1.50000
H8B   2    0.702217   -0.015339   -0.011995    11.00000   -1.50000
H8C   2    0.765499    0.002283    0.025303    11.00000   -1.50000
AFIX   0
C9    1    0.662991   -0.036837    0.086577    11.00000    0.03339    0.02105 =
         0.03585   -0.00440   -0.00922    0.00160
AFIX 137
H9A   2    0.708071   -0.049038    0.100420    11.00000   -1.50000
H9B   2    0.646042   -0.067182    0.062120    11.00000   -1.50000
H9C   2    0.630140   -0.032443    0.115554    11.00000   -1.50000
AFIX   0
C10   1    0.600631    0.042805    0.036450    11.00000    0.03095    0.02386 =
         0.02359   -0.00717   -0.00886    0.00261
AFIX 137
H10A  2    0.567564    0.046674    0.065344    11.00000   -1.50000
H10B  2    0.583580    0.013276    0.011273    11.00000   -1.50000
H10C  2    0.605929    0.081406    0.018924    11.00000   -1.50000
AFIX   0
C11   1    0.696512    0.264588    0.080470    11.00000    0.01234    0.02414 =
         0.02248    0.00610   -0.00271   -0.00318
C12   1    0.677590    0.320620    0.100615    11.00000    0.01928    0.01838 =
         0.03074    0.00545   -0.00575   -0.00340
C13   1    0.676770    0.368381    0.066655    11.00000    0.03114    0.01768 =
         0.04022    0.00054   -0.01724   -0.00303
AFIX  43
H13   2    0.664914    0.406719    0.079664    11.00000   -1.20000
AFIX   0
C14   1    0.692919    0.361893    0.013591    11.00000    0.02763    0.02639 =
         0.03443    0.01386   -0.01008   -0.00860
AFIX  43
H14   2    0.694152    0.395684   -0.008828    11.00000   -1.20000
AFIX   0
C15   1    0.707069    0.305758   -0.005872    11.00000    0.02158    0.03892 =
         0.02325    0.00895   -0.00271   -0.00707
AFIX  43
H15   2    0.715817    0.301012   -0.042268    11.00000   -1.20000
AFIX   0
C16   1    0.708801    0.255802    0.026790    11.00000    0.01450    0.02729 =
         0.02573    0.00707   -0.00186   -0.00260
C17   1    0.659121    0.330034    0.158114    11.00000    0.02942    0.01838 =
         0.02931    0.00054   -0.00550   -0.00232
AFIX  13
H17   2    0.649181    0.290125    0.173861    11.00000   -1.20000
AFIX   0
C18   1    0.720179    0.357562    0.188078    11.00000    0.03758    0.03181 =
         0.02849    0.00111   -0.00610   -0.00894
AFIX 137
H18A  2    0.759046    0.329549    0.188168    11.00000   -1.50000
H18B  2    0.706177    0.365970    0.224239    11.00000   -1.50000
H18C  2    0.734252    0.394721    0.170936    11.00000   -1.50000
AFIX   0
C19   1    0.594487    0.368805    0.164626    11.00000    0.03554    0.03163 =
         0.03764   -0.00868   -0.00787    0.00335
AFIX 137
H19A  2    0.602923    0.408232    0.149375    11.00000   -1.50000
H19B  2    0.583782    0.373068    0.201977    11.00000   -1.50000
H19C  2    0.555418    0.349913    0.146692    11.00000   -1.50000
AFIX   0
C20   1    0.723198    0.195319    0.002280    11.00000    0.02464    0.03285 =
         0.02002    0.00602    0.00166    0.00545
AFIX  13
H20   2    0.725798    0.165101    0.031022    11.00000   -1.20000
AFIX   0
C21   1    0.791865    0.194210   -0.027833    11.00000    0.03234    0.05527 =
         0.02778    0.00659    0.00851    0.00920
AFIX 137
H21A  2    0.789816    0.222703   -0.056903    11.00000   -1.50000
H21B  2    0.799948    0.154058   -0.041665    11.00000   -1.50000
H21C  2    0.829672    0.205160   -0.004156    11.00000   -1.50000
AFIX   0
C22   1    0.663300    0.178195   -0.034156    11.00000    0.03845    0.03028 =
         0.02288    0.00134   -0.00237    0.00562
AFIX 137
H22A  2    0.620612    0.174776   -0.013703    11.00000   -1.50000
H22B  2    0.673447    0.139904   -0.050966    11.00000   -1.50000
H22C  2    0.657591    0.208968   -0.061069    11.00000   -1.50000
AFIX   0
C23   1    0.831273    0.247960    0.112336    11.00000    0.01635    0.03968 =
         0.02818    0.00953   -0.00159   -0.00461
AFIX 137
H23A  2    0.836739    0.235207    0.075838    11.00000   -1.50000
H23B  2    0.874345    0.240633    0.131493    11.00000   -1.50000
H23C  2    0.820384    0.290607    0.113352    11.00000   -1.50000
AFIX   0
C24   1    0.773442    0.213292    0.137413    11.00000    0.01752    0.02140 =
         0.02008    0.00001    0.00122   -0.00246
C26   1    0.791462    0.177763    0.180929    11.00000    0.01442    0.02385 =
         0.01668    0.00017   -0.00071   -0.00117
AFIX  43
H26   2    0.839660    0.170201    0.183453    11.00000   -1.20000
AFIX   0
C27   1    0.752924    0.151315    0.221213    11.00000    0.01592    0.01981 =
         0.01715   -0.00326   -0.00190    0.00175
C28   1    0.793253    0.130517    0.268218    11.00000    0.01680    0.03481 =
         0.01810    0.00184   -0.00173    0.00130
AFIX 137
H28A  2    0.797906    0.163416    0.293238    11.00000   -1.50000
H28B  2    0.839244    0.117304    0.257079    11.00000   -1.50000
H28C  2    0.768870    0.097288    0.284945    11.00000   -1.50000
AFIX   0
C30   1    0.649769    0.135917    0.270016    11.00000    0.01461    0.02472 =
         0.01044    0.00221   -0.00163   -0.00019
C31   1    0.625507    0.079700    0.286020    11.00000    0.01425    0.02502 =
         0.01881    0.00004   -0.00130    0.00150
C32   1    0.600296    0.074278    0.336929    11.00000    0.01694    0.02936 =
         0.02415    0.00574   -0.00014   -0.00043
AFIX  43
H32   2    0.584554    0.036494    0.348767    11.00000   -1.20000
AFIX   0
C33   1    0.597579    0.122354    0.370637    11.00000    0.02174    0.04068 =
         0.01609    0.00145    0.00531    0.00201
AFIX  43
H33   2    0.580517    0.117466    0.405281    11.00000   -1.20000
AFIX   0
C34   1    0.619678    0.177282    0.353804    11.00000    0.02100    0.03179 =
         0.01894   -0.00701    0.00021   -0.00002
AFIX  43
H34   2    0.616979    0.210338    0.376984    11.00000   -1.20000
AFIX   0
C35   1    0.646005    0.185651    0.303436    11.00000    0.01669    0.02584 =
         0.01642   -0.00325   -0.00114   -0.00109
C36   1    0.627822    0.023499    0.252803    11.00000    0.02560    0.02271 =
         0.01958    0.00251    0.00196   -0.00006
AFIX  13
H36   2    0.635661    0.035409    0.215509    11.00000   -1.20000
AFIX   0
C37   1    0.687974   -0.016785    0.269979    11.00000    0.03724    0.03112 =
         0.03084    0.00437    0.00433    0.01000
AFIX 137
H37A  2    0.731608    0.005081    0.266672    11.00000   -1.50000
H37B  2    0.689369   -0.052316    0.247662    11.00000   -1.50000
H37C  2    0.681291   -0.028800    0.306554    11.00000   -1.50000
AFIX   0
C38   1    0.560329   -0.012024    0.255655    11.00000    0.03831    0.02764 =
         0.02907   -0.00077    0.00456   -0.00916
AFIX 137
H38A  2    0.555148   -0.029034    0.290810    11.00000   -1.50000
H38B  2    0.561407   -0.044227    0.229717    11.00000   -1.50000
H38C  2    0.521243    0.014459    0.248263    11.00000   -1.50000
AFIX   0
C39   1    0.668688    0.248475    0.287875    11.00000    0.02346    0.02630 =
         0.01957   -0.00372    0.00266   -0.00521
AFIX  13
H39   2    0.685157    0.247192    0.250745    11.00000   -1.20000
AFIX   0
C40   1    0.608279    0.291749    0.290888    11.00000    0.02817    0.02602 =
         0.05274   -0.00016    0.00463   -0.00187
AFIX 137
H40A  2    0.573877    0.281250    0.264253    11.00000   -1.50000
H40B  2    0.624903    0.332394    0.284620    11.00000   -1.50000
H40C  2    0.587142    0.289482    0.325733    11.00000   -1.50000
AFIX   0
C41   1    0.728254    0.271071    0.322192    11.00000    0.03016    0.04313 =
         0.03565   -0.00676   -0.00302   -0.01476
AFIX 137
H41A  2    0.744390    0.309618    0.308895    11.00000   -1.50000
H41B  2    0.766342    0.242291    0.321253    11.00000   -1.50000
H41C  2    0.712096    0.275741    0.358359    11.00000   -1.50000
AFIX   0
C42   1    0.490311    0.181547    0.055063    11.00000    0.01137    0.02432 =
         0.02262    0.00273   -0.00273    0.00093
C43   1    0.515423    0.238412    0.044064    11.00000    0.01574    0.02712 =
         0.03040    0.00318   -0.00374    0.00022
C44   1    0.515071    0.264463   -0.004748    11.00000    0.01760    0.03847 =
         0.04600    0.02107   -0.00252   -0.00601
C45   1    0.492028    0.232330   -0.046798    11.00000    0.01722    0.06033 =
         0.02713    0.02727   -0.00538   -0.00782
C46   1    0.469074    0.175405   -0.039299    11.00000    0.01792    0.05554 =
         0.01969    0.00638   -0.00623   -0.00826
C47   1    0.468432    0.151355    0.010708    11.00000    0.01684    0.03336 =
         0.02240    0.00423   -0.00143   -0.00645
C48   1    0.443718    0.095467    0.121799    11.00000    0.01915    0.02190 =
         0.01435   -0.00334    0.00073   -0.00144
C49   1    0.373034    0.100278    0.112153    11.00000    0.02081    0.02661 =
         0.01583   -0.00515    0.00314   -0.00311
C50   1    0.326822    0.053816    0.116584    11.00000    0.01761    0.03896 =
         0.01998   -0.01152    0.00282   -0.00605
C51   1    0.349731   -0.001331    0.131623    11.00000    0.02964    0.02952 =
         0.03146   -0.00881    0.00966   -0.01524
C52   1    0.418987   -0.008756    0.142603    11.00000    0.03311    0.02151 =
         0.02962    0.00221    0.00493   -0.00392
C53   1    0.463719    0.039046    0.137876    11.00000    0.01883    0.02720 =
         0.02234   -0.00051   -0.00024   -0.00112
C54   1    0.463856    0.201743    0.160712    11.00000    0.01179    0.02282 =
         0.02400   -0.00488   -0.00205   -0.00217
C55   1    0.473809    0.186743    0.212912    11.00000    0.01195    0.02585 =
         0.02577   -0.00338    0.00077   -0.00052
C56   1    0.454286    0.221440    0.254913    11.00000    0.01683    0.04026 =
         0.02070   -0.00773    0.00117   -0.00860
C57   1    0.422432    0.275425    0.245888    11.00000    0.02248    0.03267 =
         0.03835   -0.01785    0.00900   -0.00441
C58   1    0.409707    0.292296    0.194996    11.00000    0.01723    0.02348 =
         0.04624   -0.00537    0.00397    0.00175
C59   1    0.428503    0.255200    0.154136    11.00000    0.01778    0.02504 =
         0.03079    0.00044   -0.00368   -0.00102
PART   -1
C100  1    0.506501    0.507889   -0.007914    10.50000    0.03940    0.06693 =
         0.05181   -0.03588   -0.00919    0.01013
C101  1    0.527771    0.454912    0.013432    10.50000    0.08043    0.08208 =
         0.06594   -0.03345   -0.04210    0.04868
AFIX  43
H101  2    0.571541    0.439412    0.003482    10.50000   -1.20000
AFIX   0
C102  1    0.488823    0.423554    0.048298    10.50000    0.13987    0.05224 =
         0.06006   -0.02082   -0.05071    0.04905
AFIX  43
H102  2    0.506675    0.387692    0.062749    10.50000   -1.20000
AFIX   0
C103  1    0.423898    0.442830    0.063076    10.50000    0.10148    0.03127 =
         0.05347   -0.00933   -0.02938    0.00141
AFIX  43
H103  2    0.396429    0.420389    0.086806    10.50000   -1.20000
AFIX   0
C104  1    0.400054    0.496285    0.042011    10.50000    0.06393    0.03692 =
         0.04877   -0.01719   -0.02650    0.00105
AFIX  43
H104  2    0.355825    0.510957    0.051766    10.50000   -1.20000
AFIX   0
C105  1    0.439913    0.527977    0.007262    10.50000    0.05192    0.02660 =
         0.04663   -0.01515   -0.02061    0.01079
AFIX  43
H105  2    0.422513    0.564141   -0.006922    10.50000   -1.20000
AFIX   0
C106  1    0.547970    0.544220   -0.045755    10.50000    0.05273    0.10497 =
         0.07077   -0.03969    0.00314    0.00279
AFIX 137
H10D  2    0.594651    0.527564   -0.048552    10.50000   -1.50000
H10E  2    0.550734    0.585458   -0.033257    10.50000   -1.50000
H10F  2    0.525675    0.543427   -0.080234    10.50000   -1.50000
AFIX   0
PART    0
B2    3    0.493048    0.155152    0.115284    11.00000    0.01629    0.02049 =
         0.01708   -0.00188   -0.00214   -0.00011
N1    4    0.696698    0.068987    0.095999    11.00000    0.01707    0.02185 =
         0.01656   -0.00228   -0.00123    0.00107
N2    4    0.708733    0.216566    0.117989    11.00000    0.01487    0.01992 =
         0.01510    0.00101   -0.00163   -0.00018
N3    4    0.683379    0.143940    0.219060    11.00000    0.01330    0.01796 =
         0.01517    0.00015   -0.00028   -0.00191
N4    4    0.571630    0.144115    0.126816    11.00000    0.01751    0.01628 =
         0.01543   -0.00092   -0.00130   -0.00198
F1    5    0.540838    0.271759    0.083725    11.00000    0.02361    0.02494 =
         0.04236    0.00080   -0.00390   -0.00587
F2    5    0.538044    0.320320   -0.011956    11.00000    0.03593    0.04268 =
         0.07118    0.03511   -0.01112   -0.01431
F3    5    0.493784    0.255921   -0.095227    11.00000    0.02803    0.09945 =
         0.03902    0.04220   -0.00954   -0.01838
F4    5    0.448679    0.142739   -0.080827    11.00000    0.03681    0.08434 =
         0.01681    0.00294   -0.00652   -0.02075
F5    5    0.445045    0.094622    0.013983    11.00000    0.03270    0.03307 =
         0.02205   -0.00194   -0.00352   -0.01129
F6    5    0.346701    0.153412    0.096516    11.00000    0.01739    0.03306 =
         0.03133   -0.00033   -0.00358    0.00202
F7    5    0.259008    0.062327    0.106226    11.00000    0.01624    0.05088 =
         0.03458   -0.01148    0.00288   -0.00900
F8    5    0.305997   -0.047525    0.135440    11.00000    0.03748    0.03661 =
         0.05443   -0.00995    0.01286   -0.02203
F9    5    0.442358   -0.062505    0.157678    11.00000    0.04574    0.02234 =
         0.06356    0.00826    0.00586   -0.00567
F10   5    0.530319    0.027404    0.149598    11.00000    0.02572    0.02802 =
         0.04265    0.00865   -0.00255    0.00027
F11   5    0.502443    0.133384    0.224977    11.00000    0.02178    0.03273 =
         0.02039    0.00094   -0.00146    0.00336
F12   5    0.465636    0.202982    0.304348    11.00000    0.02700    0.05603 =
         0.02068   -0.00914    0.00255   -0.00426
F13   5    0.404804    0.311011    0.285956    11.00000    0.03960    0.04574 =
         0.04606   -0.02559    0.01593   -0.00311
F14   5    0.378064    0.344727    0.185409    11.00000    0.03163    0.02482 =
         0.06384   -0.00711    0.00613    0.00544
F15   5    0.409575    0.274593    0.106233    11.00000    0.02505    0.02913 =
         0.03786    0.00391   -0.00681    0.00593
NB1   6    0.659678    0.136590    0.138620    11.00000    0.01219    0.01533 =
         0.01217   -0.00048   -0.00029   -0.00041
HKLF    4
 
REM  cc_ln_04_0m in Pbca
REM R1 =  0.0360 for    7948 Fo > 4sig(Fo)  and  0.0530 for all   10157 data
REM    780 parameters refined using      0 restraints
 
END  
     
WGHT      0.0322     14.3771 

REM Highest difference peak  0.843,  deepest hole -0.323,  1-sigma level  0.066
Q1    1   0.5198  0.1375  0.3620  11.00000  0.05    0.84
Q2    1   0.8394  0.0906  0.1389  11.00000  0.05    0.67
Q3    1   0.6601  0.3595  0.0857  11.00000  0.05    0.35
Q4    1   0.7692  0.1375  0.2986  11.00000  0.05    0.34
Q5    1   0.3796  0.0032  0.1505  11.00000  0.05    0.34
Q6    1   0.3600  0.0686  0.1000  11.00000  0.05    0.32
Q7    1   0.6659  0.3640  0.0420  11.00000  0.05    0.32
Q8    1   0.6776  0.0779  0.1201  11.00000  0.05    0.32
Q9    1   0.6003  0.1047  0.3493  11.00000  0.05    0.31
Q10   1   0.6987  0.0187  0.0384  11.00000  0.05    0.30
Q11   1   0.8362  0.1484  0.2724  11.00000  0.05    0.30
Q12   1   0.6160  0.1502  0.1004  11.00000  0.05    0.29
Q13   1   0.3440  0.0207  0.1103  11.00000  0.05    0.28
Q14   1   0.6371  0.0263  0.0507  11.00000  0.05    0.28
Q15   1   0.6219  0.1036  0.2713  11.00000  0.05    0.28
Q16   1   0.6197  0.0801  0.3116  11.00000  0.05    0.28
Q17   1   0.5908  0.1157  0.1294  11.00000  0.05    0.28
Q18   1   0.5024  0.2056  0.0509  11.00000  0.05    0.27
Q19   1   0.5004  0.1943 -0.0494  11.00000  0.05    0.27
Q20   1   0.4760  0.2074  0.2326  11.00000  0.05    0.27
;

