# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_dibrnb
_database_code_depnum_ccdc_archive 'CCDC 1551476'
_audit_update_record             
;
2017-11-01 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H16 Br2 Cl2 N Nb O4 '
_chemical_formula_sum            'C17 H16 Br2 Cl2 N Nb O4'
_chemical_formula_weight         621.94

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

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

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

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

_cell_length_a                   8.7687(15)
_cell_length_b                   15.917(3)
_cell_length_c                   15.407(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.613(8)
_cell_angle_gamma                90
_cell_volume                     2140.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6261
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      26.25

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.568
_shelx_estimated_absorpt_T_min   0.395
_shelx_estimated_absorpt_T_max   0.658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_process_details   'SADABS (Bruker,2014)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16702
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.844
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             3774
_reflns_number_gt                3076
_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    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'


_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)+(0.0355P)²+2.3494P] 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         3774
_refine_ls_number_parameters     267
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.033
_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
Br1 Br 1.04701(6) -0.19521(3) 1.06100(3) 0.07288(17) Uani 1 1 d . . . . .
Br2 Br 1.00076(6) -0.12231(3) 0.70197(3) 0.06649(16) Uani 1 1 d . . . . .
C1 C 0.4342(5) 0.2152(2) 0.8819(3) 0.0494(10) Uani 1 1 d . . . . .
H1 H 0.4116 0.2286 0.8233 0.059 Uiso 1 1 calc R U . . .
C2 C 0.3807(5) 0.2632(3) 0.9465(3) 0.0605(12) Uani 1 1 d . . . . .
H2 H 0.3191 0.3095 0.9314 0.073 Uiso 1 1 calc R U . . .
C3 C 0.4164(5) 0.2441(3) 1.0334(3) 0.0638(13) Uani 1 1 d . . . . .
H3 H 0.3777 0.2779 1.0754 0.077 Uiso 1 1 calc R U . . .
C4 C 0.5073(5) 0.1766(3) 1.0602(3) 0.0535(11) Uani 1 1 d . . . . .
H4 H 0.5320 0.1639 1.1188 0.064 Uiso 1 1 calc R U . . .
C5 C 0.5590(4) 0.1296(2) 0.9947(2) 0.0411(9) Uani 1 1 d . . . . .
C6 C 0.6774(4) 0.0398(2) 0.9197(2) 0.0356(8) Uani 1 1 d . . . . .
C7 C 0.5229(4) 0.1465(2) 0.9076(2) 0.0368(8) Uani 1 1 d . . . . .
C8 C 0.7864(4) -0.0261(2) 0.9065(2) 0.0375(8) Uani 1 1 d . . . . .
C9 C 0.8511(4) -0.0737(2) 0.9770(3) 0.0456(9) Uani 1 1 d . . . . .
H9 H 0.8210 -0.0648 1.0325 0.055 Uiso 1 1 calc R U . . .
C10 C 0.9576(4) -0.1328(2) 0.9642(3) 0.0480(10) Uani 1 1 d . . . . .
C11 C 1.0052(4) -0.1475(2) 0.8839(3) 0.0501(10) Uani 1 1 d . . . . .
H11 H 1.0785 -0.1885 0.8765 0.060 Uiso 1 1 calc R U . . .
C12 C 0.9431(4) -0.1008(2) 0.8139(3) 0.0442(9) Uani 1 1 d . . . . .
C13 C 0.8345(4) -0.0383(2) 0.8236(2) 0.0360(8) Uani 1 1 d . . . . .
C14 C 0.673(2) 0.0818(10) 0.5182(10) 0.070(4) Uani 0.55(2) 1 d . . P A 1
H14A H 0.7193 0.1371 0.5211 0.084 Uiso 0.55(2) 1 calc R U P A 1
H14B H 0.5880 0.0823 0.4727 0.084 Uiso 0.55(2) 1 calc R U P A 1
C15 C 0.787(2) 0.0182(15) 0.4979(9) 0.113(6) Uani 0.55(2) 1 d . . P A 1
H15A H 0.8625 0.0118 0.5470 0.169 Uiso 0.55(2) 1 calc R U P A 1
H15B H 0.8365 0.0360 0.4481 0.169 Uiso 0.55(2) 1 calc R U P A 1
H15C H 0.7369 -0.0346 0.4854 0.169 Uiso 0.55(2) 1 calc R U P A 1
C14A C 0.713(4) 0.049(4) 0.533(2) 0.19(2) Uani 0.45(2) 1 d . . P A 2
H14C H 0.7875 0.0077 0.5548 0.227 Uiso 0.45(2) 1 calc R U P A 2
H14D H 0.6485 0.0224 0.4863 0.227 Uiso 0.45(2) 1 calc R U P A 2
C15A C 0.780(5) 0.100(3) 0.5006(16) 0.191(15) Uani 0.45(2) 1 d . . P A 2
H15D H 0.7117 0.1443 0.4801 0.286 Uiso 0.45(2) 1 calc R U P A 2
H15E H 0.8255 0.0756 0.4522 0.286 Uiso 0.45(2) 1 calc R U P A 2
H15F H 0.8585 0.1217 0.5420 0.286 Uiso 0.45(2) 1 calc R U P A 2
Cl1 Cl 0.48216(15) -0.07035(7) 0.72974(8) 0.0643(3) Uani 1 1 d . . . . .
Cl2 Cl 0.70954(11) 0.20221(6) 0.72573(7) 0.0502(2) Uani 1 1 d . . . . .
N1 N 0.5982(3) 0.08551(18) 0.86065(18) 0.0348(7) Uani 1 1 d . . . . .
Nb1 Nb 0.59057(4) 0.06716(2) 0.71460(2) 0.03533(10) Uani 1 1 d . . . . .
O1 O 0.6560(3) 0.06138(15) 1.00214(15) 0.0421(6) Uani 1 1 d . . . . .
O2 O 0.7819(3) 0.00912(15) 0.75687(15) 0.0410(6) Uani 1 1 d . . . . .
O3 O 0.6185(3) 0.06143(18) 0.59991(16) 0.0530(7) Uani 1 1 d . . . . .
O4 O 0.3898(3) 0.10457(17) 0.71040(16) 0.0455(6) Uani 1 1 d . . . . .
C16 C 0.2380(5) 0.0885(4) 0.7336(3) 0.0736(14) Uani 1 1 d . . . . .
H16A H 0.2109 0.0306 0.7198 0.088 Uiso 1 1 calc R U . . .
H16B H 0.2364 0.0960 0.7960 0.088 Uiso 1 1 calc R U . . .
C17 C 0.1273(6) 0.1427(5) 0.6889(6) 0.135(3) Uani 1 1 d . . . . .
H17A H 0.1518 0.2000 0.7039 0.203 Uiso 1 1 calc R U . . .
H17B H 0.0274 0.1294 0.7055 0.203 Uiso 1 1 calc R U . . .
H17C H 0.1283 0.1353 0.6271 0.203 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0623(3) 0.0700(3) 0.0810(4) 0.0413(3) -0.0197(2) -0.0027(2)
Br2 0.0759(3) 0.0623(3) 0.0628(3) -0.0063(2) 0.0146(2) 0.0224(2)
C1 0.049(2) 0.052(2) 0.046(2) -0.0078(19) -0.0015(18) 0.004(2)
C2 0.060(3) 0.056(3) 0.065(3) -0.017(2) 0.005(2) 0.005(2)
C3 0.064(3) 0.061(3) 0.069(3) -0.034(2) 0.024(2) -0.010(2)
C4 0.062(3) 0.061(3) 0.038(2) -0.0134(19) 0.0115(19) -0.018(2)
C5 0.041(2) 0.044(2) 0.038(2) -0.0066(16) 0.0028(16) -0.0090(18)
C6 0.0397(19) 0.040(2) 0.0265(18) 0.0037(15) 0.0008(15) -0.0091(16)
C7 0.0364(19) 0.040(2) 0.034(2) -0.0054(15) 0.0027(15) -0.0049(17)
C8 0.0379(19) 0.0359(19) 0.037(2) 0.0048(16) -0.0036(15) -0.0060(17)
C9 0.047(2) 0.045(2) 0.042(2) 0.0119(17) -0.0077(17) -0.0100(19)
C10 0.045(2) 0.037(2) 0.059(3) 0.0174(18) -0.0132(19) -0.0055(19)
C11 0.043(2) 0.037(2) 0.068(3) 0.0092(19) -0.009(2) 0.0016(18)
C12 0.045(2) 0.039(2) 0.048(2) -0.0008(17) 0.0017(17) 0.0023(18)
C13 0.0374(19) 0.0322(18) 0.037(2) 0.0039(15) -0.0024(15) -0.0029(16)
C14 0.074(8) 0.105(9) 0.033(6) 0.027(6) 0.021(5) 0.033(7)
C15 0.117(11) 0.147(15) 0.086(9) 0.006(9) 0.072(8) 0.037(10)
C14A 0.13(3) 0.36(6) 0.085(18) 0.08(3) 0.048(16) 0.04(3)
C15A 0.23(3) 0.23(4) 0.12(2) -0.03(2) 0.09(2) -0.06(3)
Cl1 0.0827(8) 0.0478(6) 0.0599(7) 0.0049(5) -0.0046(6) -0.0173(6)
Cl2 0.0486(5) 0.0454(5) 0.0556(6) 0.0135(4) -0.0004(4) -0.0072(4)
N1 0.0377(16) 0.0382(16) 0.0285(15) -0.0007(12) 0.0031(12) -0.0006(13)
Nb1 0.03858(19) 0.04091(19) 0.02602(17) 0.00396(13) 0.00077(13) 0.00060(15)
O1 0.0507(15) 0.0486(15) 0.0263(13) 0.0019(11) 0.0005(11) -0.0064(13)
O2 0.0451(14) 0.0454(15) 0.0326(14) 0.0056(11) 0.0041(11) 0.0102(12)
O3 0.0632(18) 0.0699(19) 0.0263(14) 0.0037(12) 0.0071(12) 0.0022(14)
O4 0.0352(14) 0.0585(16) 0.0420(15) 0.0053(12) -0.0014(11) -0.0024(12)
C16 0.048(3) 0.096(4) 0.078(4) -0.012(3) 0.011(2) -0.016(3)
C17 0.048(3) 0.162(7) 0.197(8) 0.047(6) 0.018(4) 0.026(4)

_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
Br1 C10 1.896(4) . ?
Br2 C12 1.875(4) . ?
C1 C2 1.374(6) . ?
C1 C7 1.378(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.379(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4 0.9300 . ?
C5 C7 1.375(5) . ?
C5 O1 1.377(4) . ?
C6 N1 1.310(4) . ?
C6 O1 1.346(4) . ?
C6 C8 1.447(5) . ?
C7 N1 1.412(4) . ?
C8 C13 1.397(5) . ?
C8 C9 1.399(5) . ?
C9 C10 1.354(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.365(6) . ?
C11 C12 1.377(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.396(5) . ?
C13 O2 1.322(4) . ?
C14 O3 1.427(17) . ?
C14 C15 1.48(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C14A C15A 1.14(5) . ?
C14A O3 1.39(4) . ?
C14A H14C 0.9700 . ?
C14A H14D 0.9700 . ?
C15A H15D 0.9600 . ?
C15A H15E 0.9600 . ?
C15A H15F 0.9600 . ?
Cl1 Nb1 2.4067(11) . ?
Cl2 Nb1 2.3882(10) . ?
N1 Nb1 2.264(3) . ?
Nb1 O3 1.810(2) . ?
Nb1 O4 1.853(2) . ?
Nb1 O2 1.970(2) . ?
O4 C16 1.435(5) . ?
C16 C17 1.425(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

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 C7 117.1(4) . . ?
C2 C1 H1 121.4 . . ?
C7 C1 H1 121.4 . . ?
C1 C2 C3 121.4(4) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C4 C3 C2 122.2(4) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C5 C4 C3 115.4(4) . . ?
C5 C4 H4 122.3 . . ?
C3 C4 H4 122.3 . . ?
C4 C5 C7 123.5(4) . . ?
C4 C5 O1 128.0(4) . . ?
C7 C5 O1 108.5(3) . . ?
N1 C6 O1 113.6(3) . . ?
N1 C6 C8 128.1(3) . . ?
O1 C6 C8 118.2(3) . . ?
C5 C7 C1 120.4(3) . . ?
C5 C7 N1 106.9(3) . . ?
C1 C7 N1 132.7(3) . . ?
C13 C8 C9 120.0(3) . . ?
C13 C8 C6 119.5(3) . . ?
C9 C8 C6 120.4(3) . . ?
C10 C9 C8 119.8(4) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.9(4) . . ?
C9 C10 Br1 119.2(3) . . ?
C11 C10 Br1 118.9(3) . . ?
C10 C11 C12 119.0(4) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C11 C12 C13 121.5(4) . . ?
C11 C12 Br2 120.0(3) . . ?
C13 C12 Br2 118.5(3) . . ?
O2 C13 C12 120.9(3) . . ?
O2 C13 C8 121.2(3) . . ?
C12 C13 C8 117.9(3) . . ?
O3 C14 C15 108.8(12) . . ?
O3 C14 H14A 109.9 . . ?
C15 C14 H14A 109.9 . . ?
O3 C14 H14B 109.9 . . ?
C15 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C15A C14A O3 127(6) . . ?
C15A C14A H14C 105.7 . . ?
O3 C14A H14C 105.7 . . ?
C15A C14A H14D 105.7 . . ?
O3 C14A H14D 105.7 . . ?
H14C C14A H14D 106.1 . . ?
C14A C15A H15D 109.5 . . ?
C14A C15A H15E 109.5 . . ?
H15D C15A H15E 109.5 . . ?
C14A C15A H15F 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C6 N1 C7 105.6(3) . . ?
C6 N1 Nb1 125.5(2) . . ?
C7 N1 Nb1 128.9(2) . . ?
O3 Nb1 O4 101.59(12) . . ?
O3 Nb1 O2 96.13(11) . . ?
O4 Nb1 O2 159.67(10) . . ?
O3 Nb1 N1 169.56(12) . . ?
O4 Nb1 N1 85.92(11) . . ?
O2 Nb1 N1 77.90(10) . . ?
O3 Nb1 Cl2 90.90(10) . . ?
O4 Nb1 Cl2 96.90(9) . . ?
O2 Nb1 Cl2 92.66(8) . . ?
N1 Nb1 Cl2 80.92(8) . . ?
O3 Nb1 Cl1 98.12(10) . . ?
O4 Nb1 Cl1 85.00(9) . . ?
O2 Nb1 Cl1 82.72(8) . . ?
N1 Nb1 Cl1 89.68(8) . . ?
Cl2 Nb1 Cl1 170.24(4) . . ?
C6 O1 C5 105.3(3) . . ?
C13 O2 Nb1 138.2(2) . . ?
C14A O3 Nb1 151.0(14) . . ?
C14 O3 Nb1 159.9(8) . . ?
C16 O4 Nb1 146.6(3) . . ?
C17 C16 O4 112.1(5) . . ?
C17 C16 H16A 109.2 . . ?
O4 C16 H16A 109.2 . . ?
C17 C16 H16B 109.2 . . ?
O4 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
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 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C1 C2 C3 1.1(6) . . . . ?
C1 C2 C3 C4 0.2(7) . . . . ?
C2 C3 C4 C5 -0.4(6) . . . . ?
C3 C4 C5 C7 -0.8(6) . . . . ?
C3 C4 C5 O1 177.1(4) . . . . ?
C4 C5 C7 C1 2.1(6) . . . . ?
O1 C5 C7 C1 -176.1(3) . . . . ?
C4 C5 C7 N1 179.3(3) . . . . ?
O1 C5 C7 N1 1.1(4) . . . . ?
C2 C1 C7 C5 -2.2(6) . . . . ?
C2 C1 C7 N1 -178.5(4) . . . . ?
N1 C6 C8 C13 9.8(5) . . . . ?
O1 C6 C8 C13 -167.0(3) . . . . ?
N1 C6 C8 C9 -174.4(3) . . . . ?
O1 C6 C8 C9 8.8(5) . . . . ?
C13 C8 C9 C10 -1.5(5) . . . . ?
C6 C8 C9 C10 -177.3(3) . . . . ?
C8 C9 C10 C11 0.3(6) . . . . ?
C8 C9 C10 Br1 178.7(3) . . . . ?
C9 C10 C11 C12 0.1(6) . . . . ?
Br1 C10 C11 C12 -178.4(3) . . . . ?
C10 C11 C12 C13 0.8(6) . . . . ?
C10 C11 C12 Br2 -177.7(3) . . . . ?
C11 C12 C13 O2 176.3(3) . . . . ?
Br2 C12 C13 O2 -5.1(5) . . . . ?
C11 C12 C13 C8 -2.0(5) . . . . ?
Br2 C12 C13 C8 176.6(3) . . . . ?
C9 C8 C13 O2 -176.0(3) . . . . ?
C6 C8 C13 O2 -0.2(5) . . . . ?
C9 C8 C13 C12 2.3(5) . . . . ?
C6 C8 C13 C12 178.1(3) . . . . ?
O1 C6 N1 C7 3.4(4) . . . . ?
C8 C6 N1 C7 -173.5(3) . . . . ?
O1 C6 N1 Nb1 -176.9(2) . . . . ?
C8 C6 N1 Nb1 6.1(5) . . . . ?
C5 C7 N1 C6 -2.7(4) . . . . ?
C1 C7 N1 C6 174.0(4) . . . . ?
C5 C7 N1 Nb1 177.7(2) . . . . ?
C1 C7 N1 Nb1 -5.6(6) . . . . ?
N1 C6 O1 C5 -2.7(4) . . . . ?
C8 C6 O1 C5 174.5(3) . . . . ?
C4 C5 O1 C6 -177.3(4) . . . . ?
C7 C5 O1 C6 0.9(4) . . . . ?
C12 C13 O2 Nb1 147.9(3) . . . . ?
C8 C13 O2 Nb1 -33.8(5) . . . . ?
C15A C14A O3 C14 47(6) . . . . ?
C15A C14A O3 Nb1 -90(7) . . . . ?
C15 C14 O3 C14A 4(5) . . . . ?
C15 C14 O3 Nb1 107(2) . . . . ?
O4 Nb1 O3 C14A 173(5) . . . . ?
O2 Nb1 O3 C14A -17(5) . . . . ?
N1 Nb1 O3 C14A 37(5) . . . . ?
Cl2 Nb1 O3 C14A 75(5) . . . . ?
Cl1 Nb1 O3 C14A -101(5) . . . . ?
O4 Nb1 O3 C14 108.2(18) . . . . ?
O2 Nb1 O3 C14 -81.8(18) . . . . ?
N1 Nb1 O3 C14 -27(2) . . . . ?
Cl2 Nb1 O3 C14 11.0(18) . . . . ?
Cl1 Nb1 O3 C14 -165.2(18) . . . . ?
O3 Nb1 O4 C16 121.8(5) . . . . ?
O2 Nb1 O4 C16 -28.4(7) . . . . ?
N1 Nb1 O4 C16 -65.5(5) . . . . ?
Cl2 Nb1 O4 C16 -145.8(5) . . . . ?
Cl1 Nb1 O4 C16 24.5(5) . . . . ?
Nb1 O4 C16 C17 -167.2(5) . . . . ?

_refine_diff_density_max         0.878
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.074

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL dibrnb in P2(1)/c
CELL 0.71073   8.76870  15.91700  15.40750  90.0000  95.6133  90.0000
ZERR   4.00   0.00150   0.00270   0.00290   0.0000   0.0082   0.0000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C  H  N  O  Br Nb Cl
UNIT 68  64  4  16  8  4  8
OMIT -3 50
L.S. 8
ACTA
BOND $H
FMAP 2
PLAN 5
CONF
SIZE 0.10 0.15 0.25
SUMP 1.0 0.001 1. 2. 1. 3.
TEMP 23.000
WGHT    0.035500    2.349400
FVAR       0.11071   0.55272   0.44762
MOLE 1
BR1   5    1.047010   -0.195212    1.060997    11.00000    0.06234    0.07002 =
         0.08100    0.04125   -0.01973   -0.00268
BR2   5    1.000764   -0.122307    0.701968    11.00000    0.07590    0.06226 =
         0.06285   -0.00627    0.01457    0.02243
C1    1    0.434227    0.215238    0.881874    11.00000    0.04903    0.05181 =
         0.04612   -0.00780   -0.00147    0.00413
AFIX  43
H1    2    0.411619    0.228614    0.823271    11.00000   -1.20000
AFIX   0
C2    1    0.380700    0.263188    0.946546    11.00000    0.06009    0.05612 =
         0.06526   -0.01704    0.00530    0.00492
AFIX  43
H2    2    0.319109    0.309502    0.931403    11.00000   -1.20000
AFIX   0
C3    1    0.416401    0.244071    1.033447    11.00000    0.06394    0.06138 =
         0.06943   -0.03372    0.02414   -0.01014
AFIX  43
H3    2    0.377722    0.277892    1.075369    11.00000   -1.20000
AFIX   0
C4    1    0.507339    0.176633    1.060245    11.00000    0.06238    0.06142 =
         0.03790   -0.01341    0.01151   -0.01752
AFIX  43
H4    2    0.531993    0.163884    1.118844    11.00000   -1.20000
AFIX   0
C5    1    0.559040    0.129583    0.994700    11.00000    0.04104    0.04411 =
         0.03792   -0.00663    0.00282   -0.00896
C6    1    0.677373    0.039822    0.919726    11.00000    0.03970    0.04005 =
         0.02650    0.00367    0.00084   -0.00912
C7    1    0.522861    0.146468    0.907575    11.00000    0.03641    0.04034 =
         0.03361   -0.00544    0.00266   -0.00487
C8    1    0.786427   -0.026092    0.906490    11.00000    0.03790    0.03587 =
         0.03743    0.00481   -0.00357   -0.00597
C9    1    0.851084   -0.073703    0.977012    11.00000    0.04707    0.04490 =
         0.04240    0.01194   -0.00771   -0.00998
AFIX  43
H9    2    0.821011   -0.064781    1.032507    11.00000   -1.20000
AFIX   0
C10   1    0.957601   -0.132824    0.964218    11.00000    0.04471    0.03710 =
         0.05865    0.01744   -0.01324   -0.00554
C11   1    1.005221   -0.147544    0.883853    11.00000    0.04257    0.03724 =
         0.06757    0.00915   -0.00908    0.00161
AFIX  43
H11   2    1.078478   -0.188501    0.876461    11.00000   -1.20000
AFIX   0
C12   1    0.943132   -0.100826    0.813900    11.00000    0.04546    0.03897 =
         0.04760   -0.00082    0.00171    0.00233
C13   1    0.834461   -0.038296    0.823620    11.00000    0.03742    0.03224 =
         0.03714    0.00389   -0.00244   -0.00294
PART 1
C14   1    0.672811    0.081794    0.518163    21.00000    0.07389    0.10463 =
         0.03328    0.02743    0.02057    0.03286
AFIX  23
H14A  2    0.719296    0.137150    0.521057    21.00000   -1.20000
H14B  2    0.588049    0.082308    0.472721    21.00000   -1.20000
AFIX   0
C15   1    0.787225    0.018157    0.497902    21.00000    0.11745    0.14691 =
         0.08616    0.00601    0.07217    0.03735
AFIX 137
H15A  2    0.862520    0.011841    0.547048    21.00000   -1.50000
H15B  2    0.836477    0.036007    0.448071    21.00000   -1.50000
H15C  2    0.736877   -0.034649    0.485448    21.00000   -1.50000
PART 2
AFIX   0
C14A  1    0.712501    0.049334    0.533131    31.00000    0.12701    0.36318 =
         0.08525    0.08347    0.04825    0.04304
AFIX  23
H14C  2    0.787536    0.007698    0.554838    31.00000   -1.20000
H14D  2    0.648525    0.022380    0.486266    31.00000   -1.20000
AFIX   0
C15A  1    0.779704    0.099744    0.500593    31.00000    0.23096    0.23437 =
         0.12193   -0.02896    0.09279   -0.06153
AFIX 137
H15D  2    0.711688    0.144302    0.480098    31.00000   -1.50000
H15E  2    0.825476    0.075649    0.452244    31.00000   -1.50000
H15F  2    0.858527    0.121720    0.542043    31.00000   -1.50000
PART 0
AFIX   0
CL1   7    0.482158   -0.070347    0.729736    11.00000    0.08269    0.04784 =
         0.05994    0.00486   -0.00464   -0.01732
CL2   7    0.709544    0.202210    0.725733    11.00000    0.04859    0.04544 =
         0.05562    0.01348   -0.00042   -0.00724
N1    3    0.598190    0.085511    0.860654    11.00000    0.03769    0.03821 =
         0.02852   -0.00075    0.00308   -0.00063
NB1   6    0.590566    0.067165    0.714596    11.00000    0.03858    0.04091 =
         0.02602    0.00396    0.00077    0.00060
O1    4    0.656008    0.061380    1.002138    11.00000    0.05073    0.04863 =
         0.02632    0.00190    0.00053   -0.00642
O2    4    0.781946    0.009121    0.756872    11.00000    0.04506    0.04538 =
         0.03261    0.00560    0.00411    0.01020
O3    4    0.618511    0.061428    0.599914    11.00000    0.06323    0.06991 =
         0.02625    0.00372    0.00709    0.00224
O4    4    0.389844    0.104569    0.710395    11.00000    0.03515    0.05846 =
         0.04201    0.00532   -0.00135   -0.00241
C16   1    0.238045    0.088480    0.733600    11.00000    0.04769    0.09557 =
         0.07842   -0.01164    0.01102   -0.01598
AFIX  23
H16A  2    0.210916    0.030585    0.719833    11.00000   -1.20000
H16B  2    0.236412    0.096029    0.795974    11.00000   -1.20000
AFIX   0
C17   1    0.127340    0.142717    0.688859    11.00000    0.04823    0.16184 =
         0.19736    0.04719    0.01848    0.02636
AFIX 137
H17A  2    0.151768    0.200015    0.703894    11.00000   -1.50000
H17B  2    0.027443    0.129399    0.705468    11.00000   -1.50000
H17C  2    0.128252    0.135265    0.627082    11.00000   -1.50000
AFIX   0
HKLF 4

REM  dibrnb in P2(1)/c
REM R1 =  0.0304 for    3076 Fo > 4sig(Fo)  and  0.0430 for all    3774 data
REM    267 parameters refined using      1 restraints

END

WGHT      0.0357      2.3451

REM Highest difference peak  0.878,  deepest hole -0.844,  1-sigma level  0.074
Q1    1   0.9278 -0.1576  0.7123  11.00000  0.05    0.88
Q2    1   0.9833 -0.2361  1.0389  11.00000  0.05    0.68
Q3    1   1.0479 -0.1055  0.7483  11.00000  0.05    0.59
Q4    1   0.4157 -0.0350  0.7596  11.00000  0.05    0.36
Q5    1   0.9885 -0.1725  1.0962  11.00000  0.05    0.34
;
_shelx_res_checksum              73492
####################################################################### 
# 
# 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_tri_ta_1
_database_code_depnum_ccdc_archive 'CCDC 1551478'
_audit_update_record             
;
2017-11-01 deposited with the CCDC.
2017-11-07 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         'C13 H10 Cl4 N3 O Ta'
_chemical_formula_sum            'C13 H10 Cl4 N3 O Ta'
_chemical_formula_weight         546.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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                   10.0945(7)
_cell_length_b                   10.1728(8)
_cell_length_c                   10.1749(8)
_cell_angle_alpha                90.006(3)
_cell_angle_beta                 119.103(3)
_cell_angle_gamma                111.100(3)
_cell_volume                     831.82(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8401
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.19

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_F_000             516
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    7.251
_shelx_estimated_absorpt_T_min   0.264
_shelx_estimated_absorpt_T_max   0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.264
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_process_details   'SADBAS (Bruker,2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11824
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.197
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             2896
_reflns_number_gt                2723
_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)+(0.0276P)²+0.4761P] 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         2896
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0189
_refine_ls_wR_factor_ref         0.0515
_refine_ls_wR_factor_gt          0.0505
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.8025(5) 1.1174(5) 0.5716(5) 0.0429(9) Uani 1 1 d . . . . .
H1 H 0.6940 1.0798 0.5510 0.051 Uiso 1 1 calc R U . . .
C2 C 0.8665(5) 1.2428(5) 0.5333(5) 0.0481(10) Uani 1 1 d . . . . .
H2 H 0.7992 1.2914 0.4849 0.058 Uiso 1 1 calc R U . . .
C3 C 1.0320(5) 1.3026(5) 0.5640(5) 0.0448(10) Uani 1 1 d . . . . .
H3 H 1.0702 1.3898 0.5372 0.054 Uiso 1 1 calc R U . . .
C4 C 1.1352(5) 1.2361(4) 0.6311(5) 0.0433(10) Uani 1 1 d . . . . .
H4 H 1.2433 1.2749 0.6508 0.052 Uiso 1 1 calc R U . . .
C5 C 1.0703(4) 1.1045(4) 0.6699(4) 0.0353(8) Uani 1 1 d . . . . .
C6 C 0.9084(4) 1.0477(4) 0.6437(4) 0.0334(8) Uani 1 1 d . . . . .
C7 C 1.0608(5) 0.7884(4) 0.7997(4) 0.0363(9) Uani 1 1 d . . . . .
C8 C 1.2253(5) 0.8020(5) 0.8828(4) 0.0446(10) Uani 1 1 d . . . . .
H8 H 1.3122 0.8905 0.9062 0.054 Uiso 1 1 calc R U . . .
C9 C 1.2587(6) 0.6847(5) 0.9300(5) 0.0494(11) Uani 1 1 d . . . . .
C10 C 1.1280(6) 0.5546(6) 0.8887(5) 0.0569(12) Uani 1 1 d . . . . .
H10 H 1.1500 0.4744 0.9168 0.068 Uiso 1 1 calc R U . . .
C11 C 0.9632(6) 0.5382(5) 0.8060(5) 0.0500(11) Uani 1 1 d . . . . .
H11 H 0.8763 0.4489 0.7800 0.060 Uiso 1 1 calc R U . . .
C12 C 0.9320(5) 0.6575(4) 0.7636(4) 0.0392(9) Uani 1 1 d . . . . .
C13 C 1.4364(7) 0.7016(7) 1.0271(6) 0.0726(16) Uani 1 1 d . . . . .
H13A H 1.4805 0.7427 1.1323 0.109 Uiso 1 1 calc R U . . .
H13B H 1.5019 0.7640 0.9901 0.109 Uiso 1 1 calc R U . . .
H13C H 1.4398 0.6088 1.0206 0.109 Uiso 1 1 calc R U . . .
Cl1 Cl 0.84741(15) 0.80096(13) 0.96899(12) 0.0536(3) Uani 1 1 d . . . . .
Cl2 Cl 0.44449(15) 0.57855(13) 0.69124(16) 0.0613(3) Uani 1 1 d . . . . .
Cl3 Cl 0.51702(13) 0.75256(13) 0.43908(12) 0.0498(3) Uani 1 1 d . . . . .
Cl4 Cl 0.62008(15) 0.95492(13) 0.76037(14) 0.0542(3) Uani 1 1 d . . . . .
N1 N 0.8844(4) 0.9230(3) 0.6944(3) 0.0337(7) Uani 1 1 d . . . . .
N2 N 1.0304(4) 0.9095(3) 0.7457(3) 0.0347(7) Uani 1 1 d . . . . .
N3 N 1.1429(4) 1.0150(4) 0.7334(4) 0.0394(8) Uani 1 1 d . . . . .
O1 O 0.7713(3) 0.6451(3) 0.6875(3) 0.0405(6) Uani 1 1 d . . . . .
Ta1 Ta 0.66673(2) 0.76059(2) 0.70203(2) 0.03538(7) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.036(2) 0.043(2) 0.051(2) 0.0108(19) 0.0243(19) 0.0156(19)
C2 0.048(2) 0.043(3) 0.055(3) 0.016(2) 0.028(2) 0.020(2)
C3 0.051(2) 0.033(2) 0.050(2) 0.0125(19) 0.030(2) 0.011(2)
C4 0.036(2) 0.037(2) 0.048(2) 0.0006(18) 0.0245(18) 0.0016(18)
C5 0.0312(19) 0.035(2) 0.0333(19) 0.0018(16) 0.0168(16) 0.0077(17)
C6 0.0323(19) 0.030(2) 0.0319(18) 0.0017(15) 0.0173(16) 0.0061(16)
C7 0.040(2) 0.039(2) 0.0314(19) 0.0067(16) 0.0194(17) 0.0163(18)
C8 0.038(2) 0.053(3) 0.037(2) 0.0058(19) 0.0160(18) 0.018(2)
C9 0.052(3) 0.065(3) 0.042(2) 0.016(2) 0.026(2) 0.032(3)
C10 0.076(3) 0.064(3) 0.058(3) 0.026(2) 0.041(3) 0.047(3)
C11 0.063(3) 0.039(2) 0.054(3) 0.012(2) 0.035(2) 0.021(2)
C12 0.043(2) 0.041(2) 0.0326(19) 0.0034(17) 0.0189(18) 0.0169(19)
C13 0.068(3) 0.106(5) 0.059(3) 0.032(3) 0.029(3) 0.058(4)
Cl1 0.0627(7) 0.0548(7) 0.0380(5) 0.0070(5) 0.0257(5) 0.0197(6)
Cl2 0.0501(6) 0.0430(6) 0.0853(8) 0.0122(6) 0.0427(6) 0.0028(5)
Cl3 0.0391(5) 0.0571(7) 0.0408(5) 0.0031(5) 0.0156(4) 0.0149(5)
Cl4 0.0625(7) 0.0471(6) 0.0648(7) 0.0061(5) 0.0407(6) 0.0236(6)
N1 0.0283(15) 0.0352(18) 0.0351(16) 0.0046(14) 0.0170(13) 0.0096(14)
N2 0.0276(15) 0.0327(17) 0.0362(16) 0.0022(13) 0.0151(13) 0.0072(14)
N3 0.0312(16) 0.0383(19) 0.0418(18) 0.0019(15) 0.0198(15) 0.0062(15)
O1 0.0387(14) 0.0311(15) 0.0454(15) 0.0024(12) 0.0204(13) 0.0102(12)
Ta1 0.03266(10) 0.03031(11) 0.03911(11) 0.00233(7) 0.02089(8) 0.00575(7)

_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 1.359(6) . ?
C1 C6 1.403(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.421(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.352(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.413(6) . ?
C4 H4 0.9300 . ?
C5 N3 1.342(5) . ?
C5 C6 1.404(5) . ?
C6 N1 1.354(5) . ?
C7 C12 1.373(6) . ?
C7 C8 1.400(5) . ?
C7 N2 1.422(5) . ?
C8 C9 1.379(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.369(7) . ?
C9 C13 1.509(6) . ?
C10 C11 1.394(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(6) . ?
C11 H11 0.9300 . ?
C12 O1 1.370(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
Cl1 Ta1 2.3484(11) . ?
Cl2 Ta1 2.2899(11) . ?
Cl3 Ta1 2.3295(10) . ?
Cl4 Ta1 2.3291(11) . ?
N1 N2 1.364(4) . ?
N1 Ta1 2.262(3) . ?
N2 N3 1.311(4) . ?
O1 Ta1 1.887(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 116.6(4) . . ?
C2 C1 H1 121.7 . . ?
C6 C1 H1 121.7 . . ?
C1 C2 C3 122.7(4) . . ?
C1 C2 H2 118.6 . . ?
C3 C2 H2 118.6 . . ?
C4 C3 C2 121.7(4) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 116.5(4) . . ?
C3 C4 H4 121.7 . . ?
C5 C4 H4 121.7 . . ?
N3 C5 C6 109.1(3) . . ?
N3 C5 C4 129.1(4) . . ?
C6 C5 C4 121.8(4) . . ?
N1 C6 C1 131.7(3) . . ?
N1 C6 C5 107.6(3) . . ?
C1 C6 C5 120.7(4) . . ?
C12 C7 C8 120.0(4) . . ?
C12 C7 N2 121.2(3) . . ?
C8 C7 N2 118.6(4) . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 118.6(4) . . ?
C10 C9 C13 121.2(5) . . ?
C8 C9 C13 120.1(5) . . ?
C9 C10 C11 122.2(4) . . ?
C9 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C12 C11 C10 118.4(4) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C7 C12 O1 120.2(3) . . ?
C7 C12 C11 120.4(4) . . ?
O1 C12 C11 119.4(4) . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 N1 N2 103.8(3) . . ?
C6 N1 Ta1 132.8(2) . . ?
N2 N1 Ta1 123.4(2) . . ?
N3 N2 N1 114.7(3) . . ?
N3 N2 C7 120.4(3) . . ?
N1 N2 C7 124.7(3) . . ?
N2 N3 C5 104.8(3) . . ?
C12 O1 Ta1 134.3(2) . . ?
O1 Ta1 N1 77.99(11) . . ?
O1 Ta1 Cl2 96.99(9) . . ?
N1 Ta1 Cl2 173.77(8) . . ?
O1 Ta1 Cl4 162.72(9) . . ?
N1 Ta1 Cl4 87.28(8) . . ?
Cl2 Ta1 Cl4 98.24(5) . . ?
O1 Ta1 Cl3 95.84(9) . . ?
N1 Ta1 Cl3 84.36(8) . . ?
Cl2 Ta1 Cl3 92.56(5) . . ?
Cl4 Ta1 Cl3 91.61(4) . . ?
O1 Ta1 Cl1 84.91(9) . . ?
N1 Ta1 Cl1 87.50(8) . . ?
Cl2 Ta1 Cl1 95.77(5) . . ?
Cl4 Ta1 Cl1 85.47(4) . . ?
Cl3 Ta1 Cl1 171.48(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.2(6) . . . . ?
C1 C2 C3 C4 1.3(7) . . . . ?
C2 C3 C4 C5 -0.4(6) . . . . ?
C3 C4 C5 N3 178.3(4) . . . . ?
C3 C4 C5 C6 -1.6(6) . . . . ?
C2 C1 C6 N1 -179.2(4) . . . . ?
C2 C1 C6 C5 -1.7(6) . . . . ?
N3 C5 C6 N1 0.9(4) . . . . ?
C4 C5 C6 N1 -179.3(3) . . . . ?
N3 C5 C6 C1 -177.2(3) . . . . ?
C4 C5 C6 C1 2.7(6) . . . . ?
C12 C7 C8 C9 -0.7(6) . . . . ?
N2 C7 C8 C9 -176.6(4) . . . . ?
C7 C8 C9 C10 2.5(6) . . . . ?
C7 C8 C9 C13 -176.6(4) . . . . ?
C8 C9 C10 C11 -2.5(7) . . . . ?
C13 C9 C10 C11 176.5(4) . . . . ?
C9 C10 C11 C12 0.6(7) . . . . ?
C8 C7 C12 O1 177.5(3) . . . . ?
N2 C7 C12 O1 -6.7(5) . . . . ?
C8 C7 C12 C11 -1.3(6) . . . . ?
N2 C7 C12 C11 174.5(3) . . . . ?
C10 C11 C12 C7 1.3(6) . . . . ?
C10 C11 C12 O1 -177.5(4) . . . . ?
C1 C6 N1 N2 176.7(4) . . . . ?
C5 C6 N1 N2 -1.0(4) . . . . ?
C1 C6 N1 Ta1 -3.0(6) . . . . ?
C5 C6 N1 Ta1 179.3(2) . . . . ?
C6 N1 N2 N3 0.9(4) . . . . ?
Ta1 N1 N2 N3 -179.3(2) . . . . ?
C6 N1 N2 C7 -175.0(3) . . . . ?
Ta1 N1 N2 C7 4.7(4) . . . . ?
C12 C7 N2 N3 -156.4(3) . . . . ?
C8 C7 N2 N3 19.5(5) . . . . ?
C12 C7 N2 N1 19.4(5) . . . . ?
C8 C7 N2 N1 -164.7(3) . . . . ?
N1 N2 N3 C5 -0.4(4) . . . . ?
C7 N2 N3 C5 175.8(3) . . . . ?
C6 C5 N3 N2 -0.3(4) . . . . ?
C4 C5 N3 N2 179.9(4) . . . . ?
C7 C12 O1 Ta1 -41.1(5) . . . . ?
C11 C12 O1 Ta1 137.6(3) . . . . ?
C12 O1 Ta1 N1 48.7(3) . . . . ?
C12 O1 Ta1 Cl2 -135.0(3) . . . . ?
C12 O1 Ta1 Cl4 16.6(6) . . . . ?
C12 O1 Ta1 Cl3 131.6(3) . . . . ?
C12 O1 Ta1 Cl1 -39.8(3) . . . . ?

_refine_diff_density_max         1.414
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.094

_shelx_res_file                  
; 
  
    tri_ta_1.res created by SHELXL-2014/7 
  
TITL tri_ta_1 in P-1 
CELL 0.71073  10.09450  10.17280  10.17490  90.0063 119.1031 111.0998 
ZERR    2.00   0.00070   0.00080   0.00080   0.0030   0.0028   0.0030 
LATT 1 
SFAC C  H  N  O  Cl Ta 
UNIT 26  20  6  2  8  2 
OMIT -3 50 
L.S. 8 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
CONF 
SIZE 0.100 0.150 0.250 
TEMP 23.000 
WGHT    0.027600    0.476100 
FVAR       0.16167 
MOLE 1 
C1    1    0.802497    1.117446    0.571559    11.00000    0.03632    0.04268 = 
         0.05114    0.01077    0.02427    0.01557 
AFIX  43 
H1    2    0.694000    1.079819    0.550976    11.00000   -1.20000 
AFIX   0 
C2    1    0.866485    1.242779    0.533264    11.00000    0.04809    0.04311 = 
         0.05534    0.01592    0.02758    0.02005 
AFIX  43 
H2    2    0.799175    1.291388    0.484946    11.00000   -1.20000 
AFIX   0 
C3    1    1.031950    1.302617    0.563990    11.00000    0.05058    0.03304 = 
         0.04996    0.01249    0.02969    0.01135 
AFIX  43 
H3    2    1.070187    1.389769    0.537246    11.00000   -1.20000 
AFIX   0 
C4    1    1.135199    1.236071    0.631114    11.00000    0.03604    0.03690 = 
         0.04760    0.00057    0.02448    0.00160 
AFIX  43 
H4    2    1.243337    1.274859    0.650751    11.00000   -1.20000 
AFIX   0 
C5    1    1.070315    1.104517    0.669900    11.00000    0.03118    0.03539 = 
         0.03330    0.00183    0.01682    0.00774 
C6    1    0.908437    1.047662    0.643746    11.00000    0.03234    0.03010 = 
         0.03190    0.00171    0.01731    0.00606 
C7    1    1.060768    0.788360    0.799723    11.00000    0.03953    0.03933 = 
         0.03142    0.00672    0.01941    0.01627 
C8    1    1.225251    0.802021    0.882792    11.00000    0.03806    0.05285 = 
         0.03724    0.00577    0.01596    0.01837 
AFIX  43 
H8    2    1.312225    0.890482    0.906240    11.00000   -1.20000 
AFIX   0 
C9    1    1.258713    0.684713    0.929961    11.00000    0.05151    0.06501 = 
         0.04236    0.01635    0.02626    0.03226 
C10   1    1.128033    0.554571    0.888696    11.00000    0.07571    0.06391 = 
         0.05821    0.02558    0.04148    0.04666 
AFIX  43 
H10   2    1.149956    0.474368    0.916796    11.00000   -1.20000 
AFIX   0 
C11   1    0.963185    0.538161    0.805976    11.00000    0.06343    0.03916 = 
         0.05391    0.01180    0.03517    0.02109 
AFIX  43 
H11   2    0.876307    0.448870    0.779980    11.00000   -1.20000 
AFIX   0 
C12   1    0.931970    0.657544    0.763582    11.00000    0.04257    0.04111 = 
         0.03262    0.00343    0.01891    0.01686 
C13   1    1.436376    0.701582    1.027084    11.00000    0.06830    0.10647 = 
         0.05930    0.03196    0.02941    0.05801 
AFIX 137 
H13A  2    1.480483    0.742688    1.132313    11.00000   -1.50000 
H13B  2    1.501893    0.763974    0.990112    11.00000   -1.50000 
H13C  2    1.439785    0.608818    1.020619    11.00000   -1.50000 
AFIX   0 
CL1   5    0.847412    0.800963    0.968991    11.00000    0.06275    0.05483 = 
         0.03799    0.00698    0.02570    0.01967 
CL2   5    0.444492    0.578548    0.691240    11.00000    0.05009    0.04300 = 
         0.08531    0.01215    0.04271    0.00282 
CL3   5    0.517019    0.752560    0.439084    11.00000    0.03914    0.05713 = 
         0.04084    0.00307    0.01561    0.01492 
CL4   5    0.620079    0.954924    0.760371    11.00000    0.06250    0.04712 = 
         0.06480    0.00612    0.04069    0.02356 
N1    3    0.884447    0.923049    0.694418    11.00000    0.02827    0.03516 = 
         0.03509    0.00460    0.01704    0.00963 
N2    3    1.030426    0.909475    0.745699    11.00000    0.02765    0.03275 = 
         0.03619    0.00219    0.01510    0.00716 
N3    3    1.142880    1.015045    0.733405    11.00000    0.03123    0.03832 = 
         0.04178    0.00192    0.01982    0.00621 
O1    4    0.771288    0.645053    0.687483    11.00000    0.03866    0.03114 = 
         0.04539    0.00244    0.02043    0.01020 
TA1   6    0.666734    0.760587    0.702025    11.00000    0.03266    0.03031 = 
         0.03911    0.00233    0.02089    0.00575 
HKLF 4 
  
REM  tri_ta_1 in P-1 
REM R1 =  0.0189 for    2723 Fo > 4sig(Fo)  and  0.0209 for all    2896 data 
REM    200 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0266      0.4646 
  
REM Highest difference peak  1.414,  deepest hole -0.427,  1-sigma level  0.094 
Q1    1   1.2864  1.3764  0.5822  11.00000  0.05    1.41 
Q2    1   0.5809  0.6646  0.6329  11.00000  0.05    0.71 
Q3    1   0.6016  0.7493  0.5746  11.00000  0.05    0.64 
Q4    1   0.7524  0.8658  0.7588  11.00000  0.05    0.53 
Q5    1   0.7550  0.7255  0.9148  11.00000  0.05    0.51 
;
_shelx_res_checksum              24874
####################################################################### 
# 
# 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_ta
_database_code_depnum_ccdc_archive 'CCDC 1551477'
_audit_update_record             
;
2017-11-01 deposited with the CCDC.
2017-11-07 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         'C21 H24 Cl4 N O2 Ta'
_chemical_formula_sum            'C21 H24 Cl4 N O2 Ta'
_chemical_formula_weight         645.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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                   6.3077(15)
_cell_length_b                   10.738(3)
_cell_length_c                   18.004(5)
_cell_angle_alpha                96.826(10)
_cell_angle_beta                 90.660(11)
_cell_angle_gamma                97.503(11)
_cell_volume                     1200.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9676
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      30.69

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_F_000             628
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.042
_shelx_estimated_absorpt_T_min   0.518
_shelx_estimated_absorpt_T_max   0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17135
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4215
_reflns_number_gt                3998
_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)+(0.0006P)²+5.1248P] 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         4215
_refine_ls_number_parameters     268
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0630
_refine_ls_wR_factor_gt          0.0623
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.192
_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 0.1568(7) 0.7194(4) 0.7695(3) 0.0273(10) Uani 1 1 d . . . . .
C2 C 0.2024(8) 0.7130(5) 0.8456(3) 0.0317(11) Uani 1 1 d . . . . .
C3 C 0.2631(9) 0.5998(5) 0.8617(3) 0.0375(12) Uani 1 1 d . . . . .
H3 H 0.2920 0.5922 0.9116 0.045 Uiso 1 1 calc R U . . .
C4 C 0.2845(8) 0.4963(5) 0.8093(3) 0.0325(11) Uani 1 1 d . . . . .
C5 C 0.2366(8) 0.5061(5) 0.7358(3) 0.0307(11) Uani 1 1 d . . . . .
H5 H 0.2457 0.4378 0.6995 0.037 Uiso 1 1 calc R U . . .
C6 C 0.1746(7) 0.6172(4) 0.7149(2) 0.0265(10) Uani 1 1 d . . . . .
C7 C 0.1582(7) 0.6339(4) 0.6369(3) 0.0264(10) Uani 1 1 d . . . . .
C8 C 0.2218(7) 0.5934(5) 0.5189(3) 0.0296(11) Uani 1 1 d . . . . .
C9 C 0.2827(8) 0.5375(5) 0.4513(3) 0.0349(12) Uani 1 1 d . . . . .
H9 H 0.3353 0.4600 0.4459 0.042 Uiso 1 1 calc R U . . .
C10 C 0.2597(9) 0.6052(6) 0.3924(3) 0.0447(14) Uani 1 1 d . . . . .
H10 H 0.2986 0.5731 0.3450 0.054 Uiso 1 1 calc R U . . .
C11 C 0.1799(10) 0.7205(6) 0.4016(3) 0.0513(16) Uani 1 1 d . . . . .
H11 H 0.1682 0.7633 0.3601 0.062 Uiso 1 1 calc R U . . .
C12 C 0.1173(10) 0.7737(5) 0.4700(3) 0.0443(14) Uani 1 1 d . . . . .
H12 H 0.0646 0.8512 0.4757 0.053 Uiso 1 1 calc R U . . .
C13 C 0.1374(8) 0.7054(5) 0.5295(3) 0.0319(11) Uani 1 1 d . . . . .
C14 C 0.1796(10) 0.8245(5) 0.9056(3) 0.0422(13) Uani 1 1 d . . . . .
C15 C -0.0594(11) 0.8420(7) 0.9094(4) 0.066(2) Uani 1 1 d . . . . .
H15A H -0.0805 0.9018 0.9519 0.098 Uiso 1 1 calc R U . . .
H15B H -0.1433 0.7623 0.9142 0.098 Uiso 1 1 calc R U . . .
H15C H -0.1029 0.8730 0.8645 0.098 Uiso 1 1 calc R U . . .
C16 C 0.3153(12) 0.9446(6) 0.8887(4) 0.0630(19) Uani 1 1 d . . . . .
H16A H 0.4571 0.9267 0.8768 0.094 Uiso 1 1 calc R U . . .
H16B H 0.3222 1.0073 0.9316 0.094 Uiso 1 1 calc R U . . .
H16C H 0.2527 0.9757 0.8469 0.094 Uiso 1 1 calc R U . . .
C17 C 0.2520(13) 0.7963(6) 0.9833(3) 0.0631(19) Uani 1 1 d . . . . .
H17A H 0.3995 0.7828 0.9821 0.095 Uiso 1 1 calc R U . . .
H17B H 0.1660 0.7218 0.9962 0.095 Uiso 1 1 calc R U . . .
H17C H 0.2357 0.8668 1.0199 0.095 Uiso 1 1 calc R U . . .
C18 C 0.3655(10) 0.3800(5) 0.8347(3) 0.0443(14) Uani 1 1 d . . . . .
C19 C 0.2366(16) 0.3356(8) 0.8993(4) 0.093(3) Uani 1 1 d . . . . .
H19A H 0.2348 0.4051 0.9379 0.139 Uiso 1 1 calc R U . . .
H19B H 0.3005 0.2694 0.9187 0.139 Uiso 1 1 calc R U . . .
H19C H 0.0928 0.3041 0.8820 0.139 Uiso 1 1 calc R U . . .
C20 C 0.6000(13) 0.4172(8) 0.8603(5) 0.092(3) Uani 1 1 d . . . . .
H20A H 0.6098 0.4825 0.9020 0.139 Uiso 1 1 calc R U . . .
H20B H 0.6813 0.4476 0.8198 0.139 Uiso 1 1 calc R U . . .
H20C H 0.6560 0.3446 0.8751 0.139 Uiso 1 1 calc R U . . .
C21 C 0.3557(13) 0.2708(6) 0.7719(4) 0.068(2) Uani 1 1 d . . . . .
H21A H 0.4190 0.2025 0.7892 0.102 Uiso 1 1 calc R U . . .
H21B H 0.4327 0.2990 0.7300 0.102 Uiso 1 1 calc R U . . .
H21C H 0.2092 0.2422 0.7569 0.102 Uiso 1 1 calc R U . . .
Cl2 Cl 0.2002(3) 1.01625(13) 0.62863(8) 0.0498(4) Uani 1 1 d . . . . .
Cl3 Cl -0.3250(2) 0.71256(15) 0.70266(9) 0.0528(4) Uani 1 1 d . . . . .
Cl4 Cl -0.2045(3) 1.03427(15) 0.74684(9) 0.0610(4) Uani 1 1 d . . . . .
Cl5 Cl -0.2839(3) 0.87356(19) 0.56528(9) 0.0642(5) Uani 1 1 d . . . . .
N1 N 0.0944(6) 0.7283(4) 0.6067(2) 0.0281(9) Uani 1 1 d . . . . .
O1 O 0.0986(5) 0.8256(3) 0.74674(18) 0.0301(7) Uani 1 1 d . . . . .
O2 O 0.2352(5) 0.5480(3) 0.58771(17) 0.0298(7) Uani 1 1 d . . . . .
Ta1 Ta -0.06780(4) 0.87698(2) 0.67119(2) 0.03165(7) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.027(2) 0.026(3) 0.028(2) 0.006(2) 0.002(2) 0.002(2)
C2 0.034(3) 0.033(3) 0.028(2) 0.003(2) 0.002(2) 0.005(2)
C3 0.042(3) 0.039(3) 0.031(3) 0.008(2) -0.001(2) 0.001(2)
C4 0.036(3) 0.029(3) 0.034(3) 0.010(2) 0.004(2) 0.008(2)
C5 0.034(3) 0.028(3) 0.031(3) 0.004(2) 0.003(2) 0.006(2)
C6 0.028(2) 0.027(3) 0.024(2) 0.0034(19) 0.0024(19) 0.004(2)
C7 0.023(2) 0.028(3) 0.028(2) 0.002(2) 0.0023(19) 0.0050(19)
C8 0.025(2) 0.038(3) 0.027(2) 0.006(2) -0.001(2) 0.005(2)
C9 0.031(3) 0.041(3) 0.031(3) -0.002(2) 0.003(2) 0.006(2)
C10 0.048(3) 0.058(4) 0.027(3) 0.000(3) 0.003(2) 0.005(3)
C11 0.069(4) 0.057(4) 0.032(3) 0.017(3) 0.007(3) 0.012(3)
C12 0.062(4) 0.037(3) 0.037(3) 0.009(2) 0.007(3) 0.013(3)
C13 0.033(3) 0.036(3) 0.027(2) 0.004(2) 0.002(2) 0.005(2)
C14 0.057(4) 0.039(3) 0.031(3) 0.001(2) 0.001(3) 0.010(3)
C15 0.075(5) 0.077(5) 0.047(4) -0.007(3) 0.010(3) 0.033(4)
C16 0.091(5) 0.040(4) 0.052(4) -0.004(3) -0.009(4) -0.003(3)
C17 0.103(6) 0.057(4) 0.031(3) -0.002(3) -0.009(3) 0.022(4)
C18 0.066(4) 0.035(3) 0.037(3) 0.014(2) 0.003(3) 0.016(3)
C19 0.154(9) 0.071(5) 0.073(5) 0.046(4) 0.048(6) 0.051(6)
C20 0.088(6) 0.090(6) 0.111(7) 0.029(5) -0.028(5) 0.043(5)
C21 0.112(6) 0.040(4) 0.060(4) 0.014(3) 0.013(4) 0.032(4)
Cl2 0.0628(10) 0.0360(8) 0.0515(8) 0.0123(6) 0.0107(7) 0.0027(7)
Cl3 0.0346(7) 0.0547(9) 0.0672(10) 0.0058(7) 0.0108(7) -0.0008(7)
Cl4 0.0804(12) 0.0490(9) 0.0615(10) 0.0061(7) 0.0212(9) 0.0368(9)
Cl5 0.0569(10) 0.0894(13) 0.0522(9) 0.0121(9) -0.0140(8) 0.0297(9)
N1 0.031(2) 0.029(2) 0.025(2) 0.0030(17) 0.0020(17) 0.0077(18)
O1 0.0376(19) 0.0251(18) 0.0288(17) 0.0025(14) 0.0015(15) 0.0094(15)
O2 0.0337(19) 0.0316(19) 0.0253(17) 0.0008(14) 0.0016(14) 0.0118(15)
Ta1 0.03395(12) 0.03052(12) 0.03299(12) 0.00522(8) 0.00156(8) 0.01238(8)

_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 O1 1.348(5) . ?
C1 C6 1.400(7) . ?
C1 C2 1.410(6) . ?
C2 C3 1.382(7) . ?
C2 C14 1.536(7) . ?
C3 C4 1.391(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(7) . ?
C4 C18 1.526(7) . ?
C5 C6 1.394(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.440(6) . ?
C7 N1 1.312(6) . ?
C7 O2 1.343(5) . ?
C8 C13 1.371(7) . ?
C8 C9 1.375(7) . ?
C8 O2 1.389(5) . ?
C9 C10 1.372(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.388(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(7) . ?
C12 H12 0.9300 . ?
C13 N1 1.418(6) . ?
C14 C16 1.516(8) . ?
C14 C17 1.542(8) . ?
C14 C15 1.545(9) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.513(9) . ?
C18 C21 1.524(8) . ?
C18 C20 1.531(10) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
Cl2 Ta1 2.3073(15) . ?
Cl3 Ta1 2.3624(16) . ?
Cl4 Ta1 2.3048(15) . ?
Cl5 Ta1 2.3251(16) . ?
N1 Ta1 2.226(4) . ?
O1 Ta1 1.885(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
O1 C1 C6 117.9(4) . . ?
O1 C1 C2 120.8(4) . . ?
C6 C1 C2 121.3(4) . . ?
C3 C2 C1 115.3(5) . . ?
C3 C2 C14 123.4(5) . . ?
C1 C2 C14 121.3(4) . . ?
C2 C3 C4 125.4(5) . . ?
C2 C3 H3 117.3 . . ?
C4 C3 H3 117.3 . . ?
C5 C4 C3 117.5(5) . . ?
C5 C4 C18 122.9(5) . . ?
C3 C4 C18 119.5(5) . . ?
C4 C5 C6 120.7(5) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.9(4) . . ?
C5 C6 C7 120.1(4) . . ?
C1 C6 C7 119.5(4) . . ?
N1 C7 O2 113.9(4) . . ?
N1 C7 C6 128.8(4) . . ?
O2 C7 C6 117.0(4) . . ?
C13 C8 C9 125.0(5) . . ?
C13 C8 O2 108.4(4) . . ?
C9 C8 O2 126.6(4) . . ?
C10 C9 C8 114.5(5) . . ?
C10 C9 H9 122.7 . . ?
C8 C9 H9 122.7 . . ?
C9 C10 C11 121.8(5) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C12 C11 C10 122.5(5) . . ?
C12 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
C11 C12 C13 116.2(5) . . ?
C11 C12 H12 121.9 . . ?
C13 C12 H12 121.9 . . ?
C8 C13 C12 119.9(5) . . ?
C8 C13 N1 107.0(4) . . ?
C12 C13 N1 133.0(5) . . ?
C16 C14 C2 111.3(5) . . ?
C16 C14 C17 107.6(5) . . ?
C2 C14 C17 110.8(5) . . ?
C16 C14 C15 111.2(5) . . ?
C2 C14 C15 108.2(5) . . ?
C17 C14 C15 107.7(5) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C21 108.9(6) . . ?
C19 C18 C4 110.4(5) . . ?
C21 C18 C4 112.4(5) . . ?
C19 C18 C20 109.4(6) . . ?
C21 C18 C20 107.8(6) . . ?
C4 C18 C20 107.9(5) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C13 105.4(4) . . ?
C7 N1 Ta1 122.8(3) . . ?
C13 N1 Ta1 131.6(3) . . ?
C1 O1 Ta1 140.2(3) . . ?
C7 O2 C8 105.2(4) . . ?
O1 Ta1 N1 78.34(14) . . ?
O1 Ta1 Cl4 96.14(11) . . ?
N1 Ta1 Cl4 173.82(11) . . ?
O1 Ta1 Cl2 96.40(11) . . ?
N1 Ta1 Cl2 84.67(11) . . ?
Cl4 Ta1 Cl2 93.26(6) . . ?
O1 Ta1 Cl5 162.17(11) . . ?
N1 Ta1 Cl5 87.39(11) . . ?
Cl4 Ta1 Cl5 98.54(7) . . ?
Cl2 Ta1 Cl5 92.82(7) . . ?
O1 Ta1 Cl3 83.45(11) . . ?
N1 Ta1 Cl3 87.45(11) . . ?
Cl4 Ta1 Cl3 94.73(6) . . ?
Cl2 Ta1 Cl3 171.97(5) . . ?
Cl5 Ta1 Cl3 85.30(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -179.1(4) . . . . ?
C6 C1 C2 C3 -0.5(7) . . . . ?
O1 C1 C2 C14 2.3(7) . . . . ?
C6 C1 C2 C14 -179.1(5) . . . . ?
C1 C2 C3 C4 1.0(8) . . . . ?
C14 C2 C3 C4 179.6(5) . . . . ?
C2 C3 C4 C5 -1.6(8) . . . . ?
C2 C3 C4 C18 176.5(5) . . . . ?
C3 C4 C5 C6 1.6(8) . . . . ?
C18 C4 C5 C6 -176.4(5) . . . . ?
C4 C5 C6 C1 -1.2(7) . . . . ?
C4 C5 C6 C7 170.0(5) . . . . ?
O1 C1 C6 C5 179.3(4) . . . . ?
C2 C1 C6 C5 0.6(7) . . . . ?
O1 C1 C6 C7 8.0(7) . . . . ?
C2 C1 C6 C7 -170.7(4) . . . . ?
C5 C6 C7 N1 176.8(5) . . . . ?
C1 C6 C7 N1 -12.0(8) . . . . ?
C5 C6 C7 O2 -9.7(7) . . . . ?
C1 C6 C7 O2 161.5(4) . . . . ?
C13 C8 C9 C10 2.1(8) . . . . ?
O2 C8 C9 C10 -177.6(5) . . . . ?
C8 C9 C10 C11 -0.3(8) . . . . ?
C9 C10 C11 C12 -0.5(10) . . . . ?
C10 C11 C12 C13 -0.3(9) . . . . ?
C9 C8 C13 C12 -3.0(8) . . . . ?
O2 C8 C13 C12 176.7(5) . . . . ?
C9 C8 C13 N1 179.3(5) . . . . ?
O2 C8 C13 N1 -1.0(5) . . . . ?
C11 C12 C13 C8 1.9(8) . . . . ?
C11 C12 C13 N1 179.0(6) . . . . ?
C3 C2 C14 C16 124.6(6) . . . . ?
C1 C2 C14 C16 -56.9(7) . . . . ?
C3 C2 C14 C17 4.9(8) . . . . ?
C1 C2 C14 C17 -176.6(5) . . . . ?
C3 C2 C14 C15 -113.0(6) . . . . ?
C1 C2 C14 C15 65.6(7) . . . . ?
C5 C4 C18 C19 -130.1(7) . . . . ?
C3 C4 C18 C19 51.9(8) . . . . ?
C5 C4 C18 C21 -8.3(8) . . . . ?
C3 C4 C18 C21 173.7(6) . . . . ?
C5 C4 C18 C20 110.4(7) . . . . ?
C3 C4 C18 C20 -67.6(7) . . . . ?
O2 C7 N1 C13 -1.5(5) . . . . ?
C6 C7 N1 C13 172.1(5) . . . . ?
O2 C7 N1 Ta1 174.4(3) . . . . ?
C6 C7 N1 Ta1 -12.0(7) . . . . ?
C8 C13 N1 C7 1.5(5) . . . . ?
C12 C13 N1 C7 -175.8(6) . . . . ?
C8 C13 N1 Ta1 -173.8(3) . . . . ?
C12 C13 N1 Ta1 8.8(9) . . . . ?
C6 C1 O1 Ta1 30.9(7) . . . . ?
C2 C1 O1 Ta1 -150.4(4) . . . . ?
N1 C7 O2 C8 0.9(5) . . . . ?
C6 C7 O2 C8 -173.5(4) . . . . ?
C13 C8 O2 C7 0.1(5) . . . . ?
C9 C8 O2 C7 179.8(5) . . . . ?
C1 O1 Ta1 N1 -41.8(5) . . . . ?
C1 O1 Ta1 Cl4 141.1(5) . . . . ?
C1 O1 Ta1 Cl2 -124.9(5) . . . . ?
C1 O1 Ta1 Cl5 -4.2(7) . . . . ?
C1 O1 Ta1 Cl3 47.0(5) . . . . ?

_refine_diff_density_max         1.341
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.098

_shelx_res_file                  
; 
  
    ta.res created by SHELXL-2014/7 
  
TITL ta in P-1 
CELL 0.71073   6.30770  10.73770  18.00430  96.8255  90.6602  97.5027 
ZERR    2.00   0.00150   0.00260   0.00460   0.0099   0.0105   0.0107 
LATT 1 
SFAC C  H  N  O  Cl Ta 
UNIT 42  48  2  4  8  2 
OMIT -3 50 
L.S. 8 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.100 0.100 0.150 
CONF 
TEMP 23.000 
WGHT    0.000600    5.124800 
FVAR       0.15540 
C1    1    0.156762    0.719410    0.769451    11.00000    0.02749    0.02637 = 
         0.02829    0.00614    0.00230    0.00172 
C2    1    0.202353    0.713046    0.845643    11.00000    0.03400    0.03273 = 
         0.02833    0.00258    0.00153    0.00485 
C3    1    0.263106    0.599819    0.861697    11.00000    0.04220    0.03901 = 
         0.03081    0.00827   -0.00150    0.00064 
AFIX  43 
H3    2    0.292046    0.592208    0.911603    11.00000   -1.20000 
AFIX   0 
C4    1    0.284499    0.496343    0.809326    11.00000    0.03649    0.02949 = 
         0.03381    0.00966    0.00415    0.00750 
C5    1    0.236635    0.506085    0.735773    11.00000    0.03418    0.02780 = 
         0.03097    0.00429    0.00347    0.00599 
AFIX  43 
H5    2    0.245729    0.437813    0.699517    11.00000   -1.20000 
AFIX   0 
C6    1    0.174570    0.617246    0.714910    11.00000    0.02799    0.02716 = 
         0.02448    0.00339    0.00239    0.00382 
C7    1    0.158239    0.633856    0.636938    11.00000    0.02310    0.02770 = 
         0.02845    0.00173    0.00235    0.00501 
C8    1    0.221760    0.593414    0.518949    11.00000    0.02463    0.03805 = 
         0.02697    0.00571   -0.00106    0.00543 
C9    1    0.282716    0.537483    0.451268    11.00000    0.03085    0.04140 = 
         0.03105   -0.00239    0.00251    0.00552 
AFIX  43 
H9    2    0.335294    0.460017    0.445852    11.00000   -1.20000 
AFIX   0 
C10   1    0.259670    0.605249    0.392366    11.00000    0.04812    0.05770 = 
         0.02656    0.00048    0.00334    0.00453 
AFIX  43 
H10   2    0.298582    0.573092    0.344958    11.00000   -1.20000 
AFIX   0 
C11   1    0.179890    0.720470    0.401563    11.00000    0.06871    0.05662 = 
         0.03242    0.01700    0.00651    0.01171 
AFIX  43 
H11   2    0.168209    0.763328    0.360059    11.00000   -1.20000 
AFIX   0 
C12   1    0.117311    0.773749    0.469951    11.00000    0.06177    0.03674 = 
         0.03732    0.00907    0.00667    0.01280 
AFIX  43 
H12   2    0.064637    0.851183    0.475685    11.00000   -1.20000 
AFIX   0 
C13   1    0.137388    0.705406    0.529527    11.00000    0.03254    0.03645 = 
         0.02697    0.00382    0.00239    0.00523 
C14   1    0.179581    0.824490    0.905606    11.00000    0.05674    0.03938 = 
         0.03099    0.00146    0.00135    0.01042 
C15   1   -0.059396    0.842033    0.909424    11.00000    0.07485    0.07720 = 
         0.04739   -0.00723    0.00972    0.03320 
AFIX 137 
H15A  2   -0.080467    0.901771    0.951885    11.00000   -1.50000 
H15B  2   -0.143345    0.762277    0.914238    11.00000   -1.50000 
H15C  2   -0.102901    0.872955    0.864522    11.00000   -1.50000 
AFIX   0 
C16   1    0.315332    0.944564    0.888666    11.00000    0.09131    0.03989 = 
         0.05211   -0.00377   -0.00891   -0.00303 
AFIX 137 
H16A  2    0.457064    0.926670    0.876760    11.00000   -1.50000 
H16B  2    0.322176    1.007289    0.931628    11.00000   -1.50000 
H16C  2    0.252691    0.975745    0.846886    11.00000   -1.50000 
AFIX   0 
C17   1    0.252002    0.796320    0.983296    11.00000    0.10301    0.05694 = 
         0.03057   -0.00221   -0.00944    0.02247 
AFIX 137 
H17A  2    0.399451    0.782784    0.982135    11.00000   -1.50000 
H17B  2    0.165955    0.721842    0.996181    11.00000   -1.50000 
H17C  2    0.235680    0.866797    1.019930    11.00000   -1.50000 
AFIX   0 
C18   1    0.365538    0.380020    0.834747    11.00000    0.06567    0.03512 = 
         0.03696    0.01406    0.00319    0.01603 
C19   1    0.236615    0.335613    0.899257    11.00000    0.15400    0.07075 = 
         0.07285    0.04617    0.04815    0.05068 
AFIX 137 
H19A  2    0.234765    0.405141    0.937948    11.00000   -1.50000 
H19B  2    0.300462    0.269383    0.918727    11.00000   -1.50000 
H19C  2    0.092829    0.304142    0.882023    11.00000   -1.50000 
AFIX   0 
C20   1    0.600044    0.417160    0.860292    11.00000    0.08766    0.09043 = 
         0.11070    0.02869   -0.02803    0.04344 
AFIX 137 
H20A  2    0.609791    0.482524    0.901956    11.00000   -1.50000 
H20B  2    0.681297    0.447621    0.819838    11.00000   -1.50000 
H20C  2    0.656048    0.344618    0.875095    11.00000   -1.50000 
AFIX   0 
C21   1    0.355691    0.270834    0.771871    11.00000    0.11186    0.04002 = 
         0.06032    0.01366    0.01344    0.03153 
AFIX 137 
H21A  2    0.418957    0.202546    0.789160    11.00000   -1.50000 
H21B  2    0.432738    0.298999    0.729951    11.00000   -1.50000 
H21C  2    0.209176    0.242196    0.756906    11.00000   -1.50000 
AFIX   0 
CL2   5    0.200227    1.016248    0.628631    11.00000    0.06276    0.03604 = 
         0.05146    0.01228    0.01075    0.00273 
CL3   5   -0.324998    0.712558    0.702658    11.00000    0.03455    0.05474 = 
         0.06718    0.00578    0.01077   -0.00084 
CL4   5   -0.204513    1.034274    0.746844    11.00000    0.08044    0.04903 = 
         0.06146    0.00610    0.02120    0.03676 
CL5   5   -0.283941    0.873563    0.565283    11.00000    0.05688    0.08939 = 
         0.05216    0.01207   -0.01405    0.02974 
N1    3    0.094382    0.728339    0.606713    11.00000    0.03095    0.02936 = 
         0.02493    0.00297    0.00202    0.00769 
O1    4    0.098624    0.825591    0.746739    11.00000    0.03757    0.02513 = 
         0.02880    0.00247    0.00153    0.00945 
O2    4    0.235178    0.548039    0.587712    11.00000    0.03373    0.03163 = 
         0.02533    0.00084    0.00162    0.01182 
TA1   6   -0.067798    0.876983    0.671188    11.00000    0.03395    0.03052 = 
         0.03299    0.00522    0.00156    0.01238 
HKLF 4 
  
REM  ta in P-1 
REM R1 =  0.0252 for    3998 Fo > 4sig(Fo)  and  0.0271 for all    4215 data 
REM    268 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0006      5.1246 
  
REM Highest difference peak  1.341,  deepest hole -1.170,  1-sigma level  0.098 
Q1    1  -0.5237  0.8797  0.5243  11.00000  0.05    1.34 
Q2    1   0.3898  0.8765  0.8159  11.00000  0.05    1.22 
Q3    1  -0.1539  0.8693  0.9610  11.00000  0.05    0.81 
Q4    1   0.0246  0.8846  0.3793  11.00000  0.05    0.79 
Q5    1   0.4088  0.6263  0.4371  11.00000  0.05    0.65 
;
_shelx_res_checksum              57262
####################################################################### 
# 
# 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_tri-nb-sq
_database_code_depnum_ccdc_archive 'CCDC 1551480'
_audit_update_record             
;
2017-11-01 deposited with the CCDC.
2017-11-07 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            'C52 H40 Cl8 N12 Nb4 O8'
_chemical_formula_weight         1616.20

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

_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'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   20.028(4)
_cell_length_b                   20.028(4)
_cell_length_c                   20.966(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8410(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    880
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      16.18

_exptl_crystal_description       rectangular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_F_000             3200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.831
_shelx_estimated_absorpt_T_min   0.886
_shelx_estimated_absorpt_T_max   0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29020
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_av_R_equivalents  0.1824
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.406
_diffrn_reflns_theta_max         20.036
_diffrn_reflns_theta_full        20.036
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1985
_reflns_number_gt                1353
_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)+(0.0859P)²] 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         1985
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1395
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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 0.5428(7) 0.0690(6) 0.3742(5) 0.087(4) Uani 1 1 d . . . . .
H1 H 0.5850 0.0730 0.3561 0.104 Uiso 1 1 calc R U . . .
C2 C 0.4906(8) 0.0497(7) 0.3398(6) 0.095(5) Uani 1 1 d . . . . .
H2 H 0.4968 0.0401 0.2968 0.114 Uiso 1 1 calc R U . . .
C3 C 0.4270(9) 0.0433(7) 0.3659(7) 0.097(5) Uani 1 1 d . . . . .
H3 H 0.3920 0.0312 0.3391 0.117 Uiso 1 1 calc R U . . .
C4 C 0.4140(6) 0.0536(6) 0.4272(6) 0.072(4) Uani 1 1 d . . . . .
H4 H 0.3717 0.0477 0.4447 0.087 Uiso 1 1 calc R U . . .
C5 C 0.4698(6) 0.0743(5) 0.4641(5) 0.054(3) Uani 1 1 d . . . . .
C6 C 0.5319(7) 0.0833(6) 0.4393(5) 0.056(3) Uani 1 1 d . . . . .
C7 C 0.5566(6) 0.1245(5) 0.6003(5) 0.049(3) Uani 1 1 d . . . . .
C8 C 0.5101(6) 0.1348(5) 0.6466(5) 0.062(3) Uani 1 1 d . . . . .
H8 H 0.4650 0.1321 0.6365 0.075 Uiso 1 1 calc R U . . .
C9 C 0.5293(8) 0.1495(6) 0.7093(5) 0.071(4) Uani 1 1 d . . . . .
C10 C 0.5942(9) 0.1555(7) 0.7210(5) 0.084(4) Uani 1 1 d . . . . .
H10 H 0.6072 0.1689 0.7616 0.101 Uiso 1 1 calc R U . . .
C11 C 0.6426(6) 0.1433(6) 0.6775(5) 0.069(3) Uani 1 1 d . . . . .
H11 H 0.6874 0.1457 0.6889 0.083 Uiso 1 1 calc R U . . .
C12 C 0.6238(7) 0.1267(5) 0.6143(5) 0.057(3) Uani 1 1 d . . . . .
C13 C 0.4755(6) 0.1620(7) 0.7604(5) 0.104(5) Uani 1 1 d . . . . .
H13A H 0.4653 0.1208 0.7817 0.156 Uiso 1 1 calc R U . . .
H13B H 0.4359 0.1791 0.7405 0.156 Uiso 1 1 calc R U . . .
H13C H 0.4918 0.1939 0.7909 0.156 Uiso 1 1 calc R U . . .
Cl1 Cl 0.70336(17) 0.02235(16) 0.44866(15) 0.0845(11) Uani 1 1 d . . . . .
Cl2 Cl 0.67442(16) 0.17406(16) 0.38009(12) 0.0734(10) Uani 1 1 d . . . . .
N1 N 0.4720(5) 0.0893(5) 0.5272(4) 0.064(3) Uani 1 1 d . . . . .
N2 N 0.5342(5) 0.1066(4) 0.5367(4) 0.053(2) Uani 1 1 d . . . . .
N3 N 0.5748(4) 0.1052(4) 0.4852(4) 0.056(2) Uani 1 1 d . . . . .
Nb1 Nb 0.69021(5) 0.13172(5) 0.48390(4) 0.0496(5) Uani 1 1 d . . . . .
O1 O 0.6720(4) 0.1134(3) 0.5708(3) 0.057(2) Uani 1 1 d . . . . .
O2 O 0.7751(3) 0.1521(3) 0.4916(2) 0.0515(19) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.108(12) 0.123(12) 0.030(7) -0.022(7) -0.016(7) -0.021(9)
C2 0.103(13) 0.126(13) 0.055(8) -0.016(8) -0.029(9) -0.037(10)
C3 0.116(15) 0.104(12) 0.072(11) -0.001(8) -0.038(9) -0.051(10)
C4 0.052(9) 0.092(10) 0.072(9) 0.010(7) -0.025(7) -0.017(7)
C5 0.065(10) 0.061(8) 0.036(7) 0.007(5) -0.008(7) -0.018(7)
C6 0.060(9) 0.066(9) 0.043(8) -0.013(6) -0.013(7) 0.001(7)
C7 0.052(9) 0.058(8) 0.036(7) 0.007(5) -0.010(7) -0.008(6)
C8 0.076(10) 0.053(8) 0.058(8) 0.009(6) 0.012(7) -0.016(7)
C9 0.085(12) 0.087(10) 0.039(8) 0.009(6) 0.006(7) 0.008(9)
C10 0.101(13) 0.128(13) 0.023(7) 0.011(6) 0.009(8) 0.000(10)
C11 0.061(9) 0.103(11) 0.044(8) 0.006(6) -0.008(7) -0.011(7)
C12 0.078(11) 0.076(9) 0.018(7) 0.011(5) 0.000(7) -0.004(7)
C13 0.106(12) 0.162(15) 0.043(7) -0.018(8) 0.020(7) -0.026(10)
Cl1 0.103(3) 0.068(2) 0.083(2) -0.0116(17) 0.0178(18) -0.003(2)
Cl2 0.097(3) 0.089(3) 0.0334(14) -0.0014(14) -0.0062(15) -0.0035(19)
N1 0.057(8) 0.086(8) 0.048(7) 0.004(5) -0.007(5) -0.007(6)
N2 0.063(8) 0.060(7) 0.036(6) 0.005(4) -0.004(6) -0.010(5)
N3 0.061(7) 0.069(6) 0.039(5) 0.003(5) 0.001(6) -0.002(5)
Nb1 0.0604(8) 0.0588(8) 0.0296(6) -0.0008(5) -0.0038(5) -0.0024(5)
O1 0.068(6) 0.080(6) 0.024(4) 0.016(3) -0.007(4) -0.006(4)
O2 0.064(5) 0.063(5) 0.027(3) 0.006(3) 0.001(3) 0.013(4)

_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 1.327(16) . ?
C1 C6 1.411(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.393(17) . ?
C2 H2 0.9300 . ?
C3 C4 1.329(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.420(14) . ?
C4 H4 0.9300 . ?
C5 N1 1.357(12) . ?
C5 C6 1.361(13) . ?
C6 N3 1.364(11) . ?
C7 C8 1.361(13) . ?
C7 C12 1.378(14) . ?
C7 N2 1.452(12) . ?
C8 C9 1.400(14) . ?
C8 H8 0.9300 . ?
C9 C10 1.329(16) . ?
C9 C13 1.539(15) . ?
C10 C11 1.354(15) . ?
C10 H10 0.9300 . ?
C11 C12 1.416(14) . ?
C11 H11 0.9300 . ?
C12 O1 1.355(12) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
Cl1 Nb1 2.327(3) . ?
Cl2 Nb1 2.357(3) . ?
N1 N2 1.308(11) . ?
N2 N3 1.352(10) . ?
N3 Nb1 2.371(9) . ?
Nb1 O2 1.756(6) . ?
Nb1 O1 1.894(6) . ?
Nb1 O2 2.081(6) 11_666 ?
O2 Nb1 2.081(6) 12_656 ?

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 117.6(13) . . ?
C2 C1 H1 121.2 . . ?
C6 C1 H1 121.2 . . ?
C1 C2 C3 122.3(13) . . ?
C1 C2 H2 118.8 . . ?
C3 C2 H2 118.8 . . ?
C4 C3 C2 122.9(12) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 114.8(12) . . ?
C3 C4 H4 122.6 . . ?
C5 C4 H4 122.6 . . ?
N1 C5 C6 108.2(9) . . ?
N1 C5 C4 128.5(13) . . ?
C6 C5 C4 123.4(11) . . ?
C5 C6 N3 110.4(9) . . ?
C5 C6 C1 118.9(11) . . ?
N3 C6 C1 130.6(13) . . ?
C8 C7 C12 120.7(10) . . ?
C8 C7 N2 118.8(11) . . ?
C12 C7 N2 120.3(10) . . ?
C7 C8 C9 121.0(11) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C10 C9 C8 117.4(11) . . ?
C10 C9 C13 122.8(11) . . ?
C8 C9 C13 119.7(13) . . ?
C9 C10 C11 124.1(11) . . ?
C9 C10 H10 118.0 . . ?
C11 C10 H10 118.0 . . ?
C10 C11 C12 118.8(12) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
O1 C12 C7 123.1(9) . . ?
O1 C12 C11 119.1(11) . . ?
C7 C12 C11 117.8(10) . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 N1 C5 103.9(8) . . ?
N1 N2 N3 116.4(8) . . ?
N1 N2 C7 120.0(10) . . ?
N3 N2 C7 123.6(10) . . ?
N2 N3 C6 101.0(8) . . ?
N2 N3 Nb1 126.2(7) . . ?
C6 N3 Nb1 132.7(8) . . ?
O2 Nb1 O1 98.2(3) . . ?
O2 Nb1 O2 97.1(4) . 11_666 ?
O1 Nb1 O2 82.3(3) . 11_666 ?
O2 Nb1 Cl1 98.0(2) . . ?
O1 Nb1 Cl1 98.3(2) . . ?
O2 Nb1 Cl1 164.7(2) 11_666 . ?
O2 Nb1 Cl2 97.54(19) . . ?
O1 Nb1 Cl2 158.7(2) . . ?
O2 Nb1 Cl2 81.71(17) 11_666 . ?
Cl1 Nb1 Cl2 93.48(11) . . ?
O2 Nb1 N3 174.0(3) . . ?
O1 Nb1 N3 76.0(3) . . ?
O2 Nb1 N3 80.8(3) 11_666 . ?
Cl1 Nb1 N3 84.5(2) . . ?
Cl2 Nb1 N3 87.7(2) . . ?
C12 O1 Nb1 138.4(6) . . ?
Nb1 O2 Nb1 167.6(4) . 12_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0(2) . . . . ?
C1 C2 C3 C4 -2(2) . . . . ?
C2 C3 C4 C5 2(2) . . . . ?
C3 C4 C5 N1 179.2(11) . . . . ?
C3 C4 C5 C6 0.1(17) . . . . ?
N1 C5 C6 N3 -1.1(13) . . . . ?
C4 C5 C6 N3 178.1(10) . . . . ?
N1 C5 C6 C1 178.3(10) . . . . ?
C4 C5 C6 C1 -2.5(18) . . . . ?
C2 C1 C6 C5 2.4(18) . . . . ?
C2 C1 C6 N3 -178.3(12) . . . . ?
C12 C7 C8 C9 1.5(16) . . . . ?
N2 C7 C8 C9 177.4(9) . . . . ?
C7 C8 C9 C10 2.6(18) . . . . ?
C7 C8 C9 C13 179.1(11) . . . . ?
C8 C9 C10 C11 -5(2) . . . . ?
C13 C9 C10 C11 178.3(12) . . . . ?
C9 C10 C11 C12 4(2) . . . . ?
C8 C7 C12 O1 176.5(9) . . . . ?
N2 C7 C12 O1 0.6(16) . . . . ?
C8 C7 C12 C11 -3.0(16) . . . . ?
N2 C7 C12 C11 -178.8(9) . . . . ?
C10 C11 C12 O1 -179.0(11) . . . . ?
C10 C11 C12 C7 0.5(17) . . . . ?
C6 C5 N1 N2 0.3(12) . . . . ?
C4 C5 N1 N2 -178.8(11) . . . . ?
C5 N1 N2 N3 0.6(12) . . . . ?
C5 N1 N2 C7 -178.2(8) . . . . ?
C8 C7 N2 N1 -11.9(14) . . . . ?
C12 C7 N2 N1 164.1(10) . . . . ?
C8 C7 N2 N3 169.4(9) . . . . ?
C12 C7 N2 N3 -14.6(14) . . . . ?
N1 N2 N3 C6 -1.2(11) . . . . ?
C7 N2 N3 C6 177.5(9) . . . . ?
N1 N2 N3 Nb1 -179.2(6) . . . . ?
C7 N2 N3 Nb1 -0.5(12) . . . . ?
C5 C6 N3 N2 1.3(11) . . . . ?
C1 C6 N3 N2 -178.0(12) . . . . ?
C5 C6 N3 Nb1 179.2(7) . . . . ?
C1 C6 N3 Nb1 -0.1(18) . . . . ?
C7 C12 O1 Nb1 41.4(16) . . . . ?
C11 C12 O1 Nb1 -139.2(9) . . . . ?
O2 Nb1 O1 C12 136.2(10) . . . . ?
O2 Nb1 O1 C12 40.1(10) 11_666 . . . ?
Cl1 Nb1 O1 C12 -124.4(10) . . . . ?
Cl2 Nb1 O1 C12 -1.4(14) . . . . ?
N3 Nb1 O1 C12 -42.3(10) . . . . ?
O1 Nb1 O2 Nb1 -51.3(16) . . . 12_656 ?
O2 Nb1 O2 Nb1 31.9(15) 11_666 . . 12_656 ?
Cl1 Nb1 O2 Nb1 -151.0(15) . . . 12_656 ?
Cl2 Nb1 O2 Nb1 114.4(16) . . . 12_656 ?

_refine_diff_density_max         0.671
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.099

_shelx_res_file                  
;

    tri.res created by SHELXL-2014/7

TITL tri in P4/nnc
CELL 0.71073  20.02825  20.02825  20.96620  90.0000  90.0000  90.0000
ZERR   4.00   0.00428   0.00428   0.00450   0.0000   0.0000   0.0000
LATT 1
SYMM 0.5-X, 0.5-Y, Z
SYMM 0.5-Y, X, Z
SYMM Y, 0.5-X, Z
SYMM 0.5-X, Y, 0.5-Z
SYMM X, 0.5-Y, 0.5-Z
SYMM Y, X, 0.5-Z
SYMM 0.5-Y, 0.5-X, 0.5-Z
SFAC C  H  N  O  Cl Nb
UNIT 208  160  48  32  32  16
OMIT -3 50
L.S. 8
ACTA
BOND $H
FMAP 2
PLAN 5
SIZE 0.10 0.12 0.15
CONF
TEMP 23.000
WGHT    0.085900
FVAR       0.37078
MOLE 1
C1    1    0.542801    0.069020    0.374200    11.00000    0.10816    0.12301 =
         0.02973   -0.02204   -0.01567   -0.02111
AFIX  43
H1    2    0.584985    0.073007    0.356056    11.00000   -1.20000
AFIX   0
C2    1    0.490626    0.049691    0.339824    11.00000    0.10267    0.12583 =
         0.05528   -0.01647   -0.02930   -0.03737
AFIX  43
H2    2    0.496789    0.040100    0.296824    11.00000   -1.20000
AFIX   0
C3    1    0.426966    0.043257    0.365853    11.00000    0.11613    0.10381 =
         0.07227   -0.00134   -0.03768   -0.05079
AFIX  43
H3    2    0.391962    0.031175    0.339090    11.00000   -1.20000
AFIX   0
C4    1    0.414014    0.053613    0.427229    11.00000    0.05212    0.09196 =
         0.07234    0.00959   -0.02518   -0.01685
AFIX  43
H4    2    0.371728    0.047741    0.444675    11.00000   -1.20000
AFIX   0
C5    1    0.469756    0.074339    0.464099    11.00000    0.06523    0.06081 =
         0.03571    0.00668   -0.00801   -0.01768
C6    1    0.531936    0.083303    0.439298    11.00000    0.05963    0.06643 =
         0.04327   -0.01340   -0.01324    0.00130
C7    1    0.556600    0.124467    0.600338    11.00000    0.05225    0.05838 =
         0.03595    0.00712   -0.00966   -0.00753
C8    1    0.510139    0.134830    0.646638    11.00000    0.07580    0.05267 =
         0.05845    0.00928    0.01203   -0.01632
AFIX  43
H8    2    0.465014    0.132110    0.636507    11.00000   -1.20000
AFIX   0
C9    1    0.529279    0.149532    0.709317    11.00000    0.08528    0.08716 =
         0.03917    0.00856    0.00646    0.00774
C10   1    0.594213    0.155514    0.721025    11.00000    0.10078    0.12782 =
         0.02325    0.01134    0.00914   -0.00047
AFIX  43
H10   2    0.607209    0.168941    0.761633    11.00000   -1.20000
AFIX   0
C11   1    0.642612    0.143274    0.677504    11.00000    0.06123    0.10262 =
         0.04424    0.00601   -0.00816   -0.01105
AFIX  43
H11   2    0.687431    0.145684    0.688872    11.00000   -1.20000
AFIX   0
C12   1    0.623762    0.126729    0.614336    11.00000    0.07798    0.07558 =
         0.01827    0.01125   -0.00042   -0.00419
C13   1    0.475497    0.162013    0.760390    11.00000    0.10583    0.16224 =
         0.04306   -0.01754    0.01981   -0.02630
AFIX 137
H13A  2    0.465279    0.120834    0.781693    11.00000   -1.50000
H13B  2    0.435891    0.179136    0.740452    11.00000   -1.50000
H13C  2    0.491781    0.193854    0.790876    11.00000   -1.50000
AFIX   0
CL1   5    0.703358    0.022351    0.448657    11.00000    0.10264    0.06778 =
         0.08306   -0.01157    0.01780   -0.00278
CL2   5    0.674415    0.174065    0.380090    11.00000    0.09721    0.08944 =
         0.03341   -0.00135   -0.00616   -0.00352
N1    3    0.472049    0.089320    0.527163    11.00000    0.05662    0.08634 =
         0.04759    0.00383   -0.00700   -0.00694
N2    3    0.534240    0.106560    0.536735    11.00000    0.06278    0.05979 =
         0.03635    0.00523   -0.00430   -0.01022
N3    3    0.574848    0.105237    0.485234    11.00000    0.06097    0.06898 =
         0.03934    0.00256    0.00096   -0.00161
NB1   6    0.690213    0.131718    0.483904    11.00000    0.06041    0.05876 =
         0.02957   -0.00076   -0.00375   -0.00244
O1    4    0.671961    0.113400    0.570798    11.00000    0.06784    0.07954 =
         0.02384    0.01609   -0.00736   -0.00554
O2    4    0.775091    0.152126    0.491610    11.00000    0.06441    0.06278 =
         0.02718    0.00553    0.00097    0.01312
HKLF 4

REM  tri in P4/nnc
REM R1 =  0.0619 for    1353 Fo > 4sig(Fo)  and  0.1040 for all    1985 data
REM    191 parameters refined using      0 restraints

END

WGHT      0.0860      0.0000

REM Highest difference peak  0.671,  deepest hole -0.932,  1-sigma level  0.099
Q1    1   0.6295  0.1254  0.4843  11.00000  0.05    0.67
Q2    1   0.7349  0.1927  0.4928  11.00000  0.05    0.53
Q3    1   0.7955  0.1619  0.5103  11.00000  0.05    0.51
Q4    1   0.8018  0.1983  0.5095  11.00000  0.05    0.50
Q5    1   0.7667  0.1377  0.4986  11.00000  0.05    0.46
;
_shelx_res_checksum              16260

_shelx_fab_file                  
;
    0    2    0   -210.63      0.00
    2    2    0    -74.18      0.00
    1    3    0     53.73      0.00
    3    3    0     57.91      0.00
    0    4    0    146.76      0.00
    2    4    0     32.74      0.00
    4    4    0      2.20      0.00
    1    5    0    -18.57      0.00
    3    5    0    -43.08      0.00
    5    5    0     10.15      0.00
    0    6    0    -49.14      0.00
    2    6    0    -54.60      0.00
    4    6    0     12.53      0.00
    6    6    0    -10.49      0.00
    1    7    0     10.49      0.00
    3    7    0     27.85      0.00
    5    7    0      8.27      0.00
    7    7    0     -6.28      0.00
    0    8    0     56.80      0.00
    2    8    0     16.93      0.00
    4    8    0     20.33      0.00
    6    8    0    -13.06      0.00
    8    8    0     20.56      0.00
    1    9    0    -13.72      0.00
    3    9    0    -12.04      0.00
    5    9    0    -16.84      0.00
    7    9    0      5.51      0.00
    9    9    0     -6.51      0.00
    0   10    0    -26.99      0.00
    2   10    0    -27.22      0.00
    4   10    0     -7.65      0.00
    6   10    0      0.27      0.00
    8   10    0      0.60      0.00
   10   10    0    -18.04      0.00
    1   11    0     11.15      0.00
    3   11    0      2.82      0.00
    5   11    0     13.21      0.00
    7   11    0      3.16      0.00
    9   11    0     -4.00      0.00
   11   11    0     15.46      0.00
    0   12    0     23.26      0.00
    2   12    0      9.16      0.00
    4   12    0     10.51      0.00
    6   12    0     -5.13      0.00
    8   12    0      2.01      0.00
   10   12    0      7.38      0.00
   12   12    0     -3.54      0.00
    1   13    0     11.50      0.00
    3   13    0    -11.40      0.00
    5   13    0      1.00      0.00
    7   13    0     -6.65      0.00
    9   13    0     -0.83      0.00
   11   13    0    -10.77      0.00
   13   13    0      7.44      0.00
    0   14    0     -1.00      0.00
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    7   11   15      0.25      0.00
    5   12   15      4.43      0.00
    0   13   15      3.83      0.00
    1   13   15      0.93      0.00
    2   13   15     -0.47      0.00
    8    9   16      1.09      0.00
    5   11   16     -1.32      0.00
    0   12   16      7.52      0.00
    1   12   16     -2.10      0.00
    7    8   17      1.76      0.00
    3   10   17     -1.98      0.00
    4   10   17      2.36      0.00
    4    8   18     -6.81      0.00
    1    9   18     -1.55      0.00
    3    6   19     -3.78      0.00
    0    7   19     -3.09      0.00
    1    7   19     -0.95      0.00
    2    2   20    -12.00      0.00
    1    3   20     -3.64      0.00
    2    3   20      0.58      0.00
    0    0    0      0.00      0.00
# SQUEEZE RESULTS (Version = 110917)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.250  0.250  0.243      1464       247 ' '
   2 -0.250  0.750  0.743      1464       247 ' '
   3  0.250  0.750  0.250        23        -1 ' '
   4  0.250  0.750  0.750        23        -1 ' '
   5  0.750  0.250  0.750        23        -1 ' '
   6  0.750  0.250  0.250        23        -1 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
    1    1    0     1.438
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details
 
# Solvent Accessible Volume =      3026
# Electrons Found in S.A.V. =       490
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others

;


# start Validation Reply Form
_vrf_THETM01_tri-nb-sq           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Even though crystal data was collected up to 0.78 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle.
;
_vrf_RINTA01_tri-nb-sq           
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The crystal size, the largest available still 
diffracted quite weakly at high angle.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_tbu_nb_sq
_database_code_depnum_ccdc_archive 'CCDC 1551479'
_audit_update_record             
;
2017-11-01 deposited with the CCDC.
2017-11-07 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            'C84 H96 Cl4 N4 Nb4 O14'
_chemical_formula_weight         1899.08

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.8788(9)
_cell_length_b                   27.1666(10)
_cell_length_c                   19.8149(11)
_cell_angle_alpha                90
_cell_angle_beta                 133.7840(10)
_cell_angle_gamma                90
_cell_volume                     10834.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7532
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      21.71

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_F_000             3888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.561
_shelx_estimated_absorpt_T_min   0.873
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_process_details   'SADABS (Bruker,2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24020
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.024
_diffrn_reflns_theta_max         21.865
_diffrn_reflns_theta_full        21.865
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             6455
_reflns_number_gt                5153
_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)+(0.0373P)²+21.7839P] 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         6455
_refine_ls_number_parameters     528
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0827
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.01943(18) 0.50756(14) 0.1190(3) 0.0299(10) Uani 1 1 d . . . . .
C2 C 1.07615(19) 0.53544(16) 0.1691(3) 0.0423(11) Uani 1 1 d . . . . .
H2 H 1.0796 0.5662 0.1926 0.051 Uiso 1 1 calc R U . . .
C3 C 1.1279(2) 0.51537(17) 0.1826(3) 0.0473(12) Uani 1 1 d . . . . .
H3 H 1.1673 0.5330 0.2170 0.057 Uiso 1 1 calc R U . . .
C4 C 1.1228(2) 0.46972(16) 0.1464(3) 0.0412(11) Uani 1 1 d . . . . .
H4 H 1.1585 0.4578 0.1565 0.049 Uiso 1 1 calc R U . . .
C5 C 1.0659(2) 0.44176(16) 0.0961(3) 0.0425(11) Uani 1 1 d . . . . .
H5 H 1.0620 0.4111 0.0717 0.051 Uiso 1 1 calc R U . . .
C6 C 1.01532(19) 0.46217(15) 0.0842(3) 0.0339(10) Uani 1 1 d . . . . .
C7 C 0.9218(2) 0.47788(15) 0.0434(3) 0.0350(10) Uani 1 1 d . . . . .
C8 C 0.85427(19) 0.46701(16) -0.0016(3) 0.0395(11) Uani 1 1 d . . . . .
C9 C 0.8216(2) 0.42658(19) -0.0613(4) 0.0658(16) Uani 1 1 d . . . . .
H9 H 0.8434 0.4071 -0.0717 0.079 Uiso 1 1 calc R U . . .
C10 C 0.7580(3) 0.4151(2) -0.1049(4) 0.082 Uani 1 1 d D . . . .
C11 C 0.7274(2) 0.4455(2) -0.0885(4) 0.066 Uani 1 1 d . . . . .
H11 H 0.6840 0.4378 -0.1185 0.079 Uiso 1 1 calc R U . . .
C12 C 0.7560(2) 0.48646(16) -0.0309(3) 0.0419(11) Uani 1 1 d . . . . .
C13 C 0.8228(2) 0.49646(15) 0.0158(3) 0.0349(10) Uani 1 1 d . . . . .
C14 C 0.7217(4) 0.3700(3) -0.1697(7) 0.161(3) Uani 1 1 d D U . . .
C17 C 0.7690(7) 0.3313(6) -0.1453(15) 0.169(5) Uani 0.619(11) 1 d D U P A 1
H17A H 0.8030 0.3456 -0.1400 0.254 Uiso 0.619(11) 1 calc R U P A 1
H17B H 0.7457 0.3066 -0.1933 0.254 Uiso 0.619(11) 1 calc R U P A 1
H17C H 0.7890 0.3165 -0.0868 0.254 Uiso 0.619(11) 1 calc R U P A 1
C16 C 0.7040(6) 0.3872(5) -0.2649(10) 0.170(4) Uani 0.619(11) 1 d D U P A 1
H16A H 0.6797 0.3615 -0.3108 0.254 Uiso 0.619(11) 1 calc R U P A 1
H16B H 0.7445 0.3935 -0.2496 0.254 Uiso 0.619(11) 1 calc R U P A 1
H16C H 0.6776 0.4166 -0.2895 0.254 Uiso 0.619(11) 1 calc R U P A 1
C15 C 0.6568(7) 0.3592(7) -0.2012(15) 0.169(4) Uani 0.619(11) 1 d D U P A 1
H15A H 0.6395 0.3289 -0.2359 0.253 Uiso 0.619(11) 1 calc R U P A 1
H15B H 0.6263 0.3855 -0.2404 0.253 Uiso 0.619(11) 1 calc R U P A 1
H15C H 0.6624 0.3562 -0.1478 0.253 Uiso 0.619(11) 1 calc R U P A 1
C17A C 0.6532(11) 0.3869(9) -0.2646(13) 0.148(10) Uani 0.381(11) 1 d D U P A 2
H17D H 0.6600 0.4093 -0.2949 0.222 Uiso 0.381(11) 1 calc R U P A 2
H17E H 0.6286 0.4031 -0.2535 0.222 Uiso 0.381(11) 1 calc R U P A 2
H17F H 0.6288 0.3588 -0.3039 0.222 Uiso 0.381(11) 1 calc R U P A 2
C16A C 0.6957(12) 0.3378(7) -0.1354(16) 0.117(8) Uani 0.381(11) 1 d D U P A 2
H16D H 0.6645 0.3140 -0.1826 0.176 Uiso 0.381(11) 1 calc R U P A 2
H16E H 0.6742 0.3585 -0.1237 0.176 Uiso 0.381(11) 1 calc R U P A 2
H16F H 0.7323 0.3211 -0.0789 0.176 Uiso 0.381(11) 1 calc R U P A 2
C15A C 0.7574(12) 0.3312(9) -0.1734(18) 0.113(9) Uani 0.381(11) 1 d D U P A 2
H15D H 0.7351 0.3254 -0.2373 0.169 Uiso 0.381(11) 1 calc R U P A 2
H15E H 0.7581 0.3013 -0.1468 0.169 Uiso 0.381(11) 1 calc R U P A 2
H15F H 0.8022 0.3417 -0.1385 0.169 Uiso 0.381(11) 1 calc R U P A 2
C18 C 0.7169(2) 0.52043(17) -0.0218(3) 0.0499(13) Uani 1 1 d . . . . .
C19 C 0.6475(2) 0.4992(2) -0.0734(4) 0.0726(16) Uani 1 1 d . . . . .
H19A H 0.6221 0.4968 -0.1390 0.109 Uiso 1 1 calc R U . . .
H19B H 0.6250 0.5205 -0.0641 0.109 Uiso 1 1 calc R U . . .
H19C H 0.6522 0.4671 -0.0493 0.109 Uiso 1 1 calc R U . . .
C20 C 0.7524(2) 0.5274(2) 0.0799(3) 0.0716(16) Uani 1 1 d . . . . .
H20A H 0.7627 0.4958 0.1089 0.107 Uiso 1 1 calc R U . . .
H20B H 0.7241 0.5452 0.0828 0.107 Uiso 1 1 calc R U . . .
H20C H 0.7927 0.5455 0.1121 0.107 Uiso 1 1 calc R U . . .
C21 C 0.7072(2) 0.57029(19) -0.0661(4) 0.0698(16) Uani 1 1 d . . . . .
H21A H 0.7496 0.5859 -0.0308 0.105 Uiso 1 1 calc R U . . .
H21B H 0.6793 0.5908 -0.0658 0.105 Uiso 1 1 calc R U . . .
H21C H 0.6867 0.5654 -0.1293 0.105 Uiso 1 1 calc R U . . .
C22 C 1.14752(19) 0.74836(15) 0.4153(3) 0.0323(10) Uani 1 1 d . . . . .
C23 C 1.1444(2) 0.72418(15) 0.4735(3) 0.0377(11) Uani 1 1 d . . . . .
H23 H 1.1190 0.6959 0.4542 0.045 Uiso 1 1 calc R U . . .
C24 C 1.1806(2) 0.74368(16) 0.5608(3) 0.0427(11) Uani 1 1 d . . . . .
H24 H 1.1798 0.7280 0.6017 0.051 Uiso 1 1 calc R U . . .
C25 C 1.2185(2) 0.78620(16) 0.5902(3) 0.0428(11) Uani 1 1 d . . . . .
H25 H 1.2418 0.7984 0.6498 0.051 Uiso 1 1 calc R U . . .
C26 C 1.2221(2) 0.81050(16) 0.5333(3) 0.0449(12) Uani 1 1 d . . . . .
H26 H 1.2478 0.8386 0.5525 0.054 Uiso 1 1 calc R U . . .
C27 C 1.1853(2) 0.79051(15) 0.4460(3) 0.0356(10) Uani 1 1 d . . . . .
C28 C 1.1396(2) 0.77325(15) 0.3043(3) 0.0362(10) Uani 1 1 d . . . . .
C29 C 1.1252(2) 0.78128(15) 0.2199(3) 0.0361(11) Uani 1 1 d . . . . .
C30 C 1.1637(2) 0.81437(17) 0.2207(3) 0.0500(13) Uani 1 1 d . . . . .
H30 H 1.1975 0.8315 0.2752 0.060 Uiso 1 1 calc R U . . .
C31 C 1.1525(3) 0.82214(18) 0.1420(3) 0.0568(14) Uani 1 1 d . . . . .
C32 C 1.1001(2) 0.79575(18) 0.0616(3) 0.0549(13) Uani 1 1 d . . . . .
H32 H 1.0921 0.8008 0.0081 0.066 Uiso 1 1 calc R U . . .
C33 C 1.0591(2) 0.76262(15) 0.0555(3) 0.0389(11) Uani 1 1 d . . . . .
C34 C 1.0732(2) 0.75513(15) 0.1379(3) 0.0364(11) Uani 1 1 d . . . . .
C35 C 1.1967(3) 0.8577(2) 0.1445(4) 0.0780(18) Uani 1 1 d . . . . .
C36 C 1.1919(3) 0.9087(2) 0.1727(5) 0.106(2) Uani 1 1 d . . . . .
H36A H 1.2189 0.9316 0.1743 0.159 Uiso 1 1 calc R U . . .
H36B H 1.2073 0.9068 0.2335 0.159 Uiso 1 1 calc R U . . .
H36C H 1.1465 0.9195 0.1280 0.159 Uiso 1 1 calc R U . . .
C37 C 1.2696(3) 0.8408(3) 0.2203(4) 0.097(2) Uani 1 1 d . . . . .
H37A H 1.2737 0.8081 0.2063 0.146 Uiso 1 1 calc R U . . .
H37B H 1.2834 0.8409 0.2801 0.146 Uiso 1 1 calc R U . . .
H37C H 1.2973 0.8629 0.2218 0.146 Uiso 1 1 calc R U . . .
C38 C 1.1778(3) 0.8601(3) 0.0526(4) 0.116(3) Uani 1 1 d . . . . .
H38A H 1.1338 0.8734 0.0055 0.174 Uiso 1 1 calc R U . . .
H38B H 1.1789 0.8276 0.0346 0.174 Uiso 1 1 calc R U . . .
H38C H 1.2086 0.8809 0.0590 0.174 Uiso 1 1 calc R U . . .
C39 C 1.0044(2) 0.73480(18) -0.0350(3) 0.0484(12) Uani 1 1 d . . . . .
C40 C 0.9949(3) 0.7536(2) -0.1165(3) 0.0696(16) Uani 1 1 d . . . . .
H40A H 0.9881 0.7885 -0.1225 0.104 Uiso 1 1 calc R U . . .
H40B H 0.9570 0.7378 -0.1733 0.104 Uiso 1 1 calc R U . . .
H40C H 1.0338 0.7462 -0.1048 0.104 Uiso 1 1 calc R U . . .
C41 C 0.9378(2) 0.7419(3) -0.0643(4) 0.101(2) Uani 1 1 d . . . . .
H41A H 0.9387 0.7254 -0.0206 0.151 Uiso 1 1 calc R U . . .
H41B H 0.9029 0.7282 -0.1256 0.151 Uiso 1 1 calc R U . . .
H41C H 0.9298 0.7763 -0.0653 0.151 Uiso 1 1 calc R U . . .
C42 C 1.0220(3) 0.68025(19) -0.0217(4) 0.087(2) Uani 1 1 d . . . . .
H42A H 1.0658 0.6766 0.0023 0.130 Uiso 1 1 calc R U . . .
H42B H 0.9905 0.6636 -0.0807 0.130 Uiso 1 1 calc R U . . .
H42C H 1.0208 0.6663 0.0217 0.130 Uiso 1 1 calc R U . . .
Cl1 Cl 0.85349(5) 0.60738(4) -0.03670(7) 0.0369(3) Uani 1 1 d . . . . .
Cl2 Cl 1.14229(5) 0.64874(4) 0.24049(7) 0.0378(3) Uani 1 1 d . . . . .
N3 N 0.95800(15) 0.51702(12) 0.0902(2) 0.0298(8) Uani 1 1 d . . . . .
N4 N 1.11966(15) 0.73778(12) 0.3248(2) 0.0306(8) Uani 1 1 d . . . . .
Nb1 Nb 0.92485(2) 0.58196(2) 0.12495(2) 0.02635(12) Uani 1 1 d . . . . .
Nb2 Nb 1.05146(2) 0.67490(2) 0.22432(2) 0.02761(12) Uani 1 1 d . . . . .
O1 O 0.95310(13) 0.44292(10) 0.0364(2) 0.0428(7) Uani 1 1 d . . . . .
O2 O 0.85740(12) 0.53386(9) 0.07736(18) 0.0326(7) Uani 1 1 d . . . . .
O3 O 1.0000 0.55987(12) 0.2500 0.0264(8) Uani 1 2 d S T P . .
O4 O 0.90241(11) 0.62988(9) 0.16392(17) 0.0288(6) Uani 1 1 d . . . . .
O5 O 0.99099(11) 0.62741(9) 0.14230(16) 0.0285(6) Uani 1 1 d . . . . .
O6 O 1.0000 0.69755(13) 0.2500 0.0300(9) Uani 1 2 d S T P . .
O7 O 1.03678(12) 0.72322(9) 0.14093(17) 0.0334(7) Uani 1 1 d . . . . .
O8 O 1.17980(13) 0.80675(10) 0.37445(19) 0.0400(7) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.024(2) 0.029(3) 0.033(2) -0.001(2) 0.018(2) 0.005(2)
C2 0.031(3) 0.036(3) 0.057(3) -0.013(2) 0.029(2) 0.001(2)
C3 0.030(3) 0.048(3) 0.052(3) -0.017(2) 0.023(2) -0.006(2)
C4 0.033(3) 0.047(3) 0.044(3) -0.010(2) 0.027(2) 0.002(2)
C5 0.051(3) 0.033(3) 0.048(3) -0.004(2) 0.036(3) 0.005(2)
C6 0.032(3) 0.032(3) 0.037(2) -0.002(2) 0.024(2) 0.003(2)
C7 0.040(3) 0.028(3) 0.038(2) 0.000(2) 0.027(2) 0.002(2)
C8 0.031(3) 0.036(3) 0.045(3) -0.013(2) 0.024(2) -0.008(2)
C9 0.052(3) 0.060(4) 0.089(4) -0.043(3) 0.050(3) -0.025(3)
C10 0.065 0.077 0.111 -0.065 0.064 -0.044
C11 0.041 0.078 0.078 -0.042 0.041 -0.034
C12 0.032(3) 0.045(3) 0.046(3) -0.008(2) 0.026(2) -0.009(2)
C13 0.035(3) 0.028(3) 0.038(2) -0.006(2) 0.023(2) -0.006(2)
C14 0.116(5) 0.164(6) 0.246(7) -0.172(6) 0.142(5) -0.106(4)
C17 0.121(5) 0.149(7) 0.249(8) -0.179(6) 0.133(6) -0.105(5)
C16 0.127(5) 0.173(7) 0.240(8) -0.172(6) 0.138(6) -0.103(5)
C15 0.114(5) 0.163(7) 0.252(8) -0.171(7) 0.136(6) -0.116(5)
C17A 0.149(11) 0.146(11) 0.144(11) -0.003(4) 0.099(8) -0.004(4)
C16A 0.116(9) 0.117(9) 0.122(9) -0.004(4) 0.084(6) -0.005(4)
C15A 0.116(9) 0.111(10) 0.112(9) -0.002(4) 0.079(7) -0.004(4)
C18 0.039(3) 0.048(3) 0.064(3) -0.017(3) 0.036(3) -0.013(2)
C19 0.041(3) 0.080(4) 0.095(4) -0.024(3) 0.047(3) -0.018(3)
C20 0.054(3) 0.103(5) 0.071(4) -0.027(3) 0.048(3) -0.019(3)
C21 0.053(3) 0.059(4) 0.092(4) -0.006(3) 0.048(3) 0.001(3)
C22 0.034(2) 0.029(3) 0.034(2) -0.004(2) 0.024(2) -0.004(2)
C23 0.040(3) 0.033(3) 0.041(3) -0.010(2) 0.028(2) -0.014(2)
C24 0.044(3) 0.046(3) 0.041(3) -0.003(2) 0.030(2) -0.010(2)
C25 0.042(3) 0.048(3) 0.038(3) -0.011(2) 0.028(2) -0.011(2)
C26 0.044(3) 0.035(3) 0.055(3) -0.012(2) 0.035(3) -0.014(2)
C27 0.039(3) 0.033(3) 0.037(3) -0.002(2) 0.027(2) -0.005(2)
C28 0.043(3) 0.025(3) 0.041(3) -0.006(2) 0.029(2) -0.009(2)
C29 0.038(3) 0.030(3) 0.038(3) -0.003(2) 0.026(2) -0.010(2)
C30 0.056(3) 0.047(3) 0.045(3) -0.005(2) 0.035(3) -0.019(2)
C31 0.073(4) 0.049(3) 0.054(3) -0.001(3) 0.046(3) -0.020(3)
C32 0.065(3) 0.053(3) 0.053(3) 0.004(3) 0.043(3) -0.012(3)
C33 0.042(3) 0.035(3) 0.037(3) 0.004(2) 0.027(2) -0.002(2)
C34 0.035(3) 0.029(3) 0.043(3) 0.008(2) 0.027(2) 0.002(2)
C35 0.090(5) 0.084(5) 0.066(4) -0.005(3) 0.056(4) -0.042(4)
C36 0.126(6) 0.067(5) 0.127(6) -0.002(4) 0.088(5) -0.042(4)
C37 0.071(4) 0.136(6) 0.084(4) -0.008(4) 0.054(4) -0.042(4)
C38 0.125(6) 0.150(7) 0.082(4) -0.008(4) 0.075(4) -0.077(5)
C39 0.047(3) 0.056(3) 0.038(3) 0.002(2) 0.028(2) -0.010(2)
C40 0.075(4) 0.080(4) 0.051(3) -0.002(3) 0.042(3) -0.020(3)
C41 0.047(4) 0.184(7) 0.053(3) -0.008(4) 0.028(3) -0.022(4)
C42 0.123(5) 0.051(4) 0.061(4) -0.014(3) 0.054(4) -0.022(4)
Cl1 0.0354(6) 0.0357(6) 0.0338(6) -0.0018(5) 0.0218(5) 0.0027(5)
Cl2 0.0342(6) 0.0376(7) 0.0481(6) -0.0061(5) 0.0309(6) -0.0068(5)
N3 0.0256(19) 0.023(2) 0.0350(19) -0.0037(16) 0.0189(17) -0.0010(16)
N4 0.034(2) 0.027(2) 0.032(2) -0.0001(16) 0.0231(17) -0.0029(16)
Nb1 0.0225(2) 0.0228(2) 0.0312(2) -0.00268(16) 0.01758(19) -0.00141(16)
Nb2 0.0272(2) 0.0233(2) 0.0326(2) -0.00128(17) 0.02082(19) -0.00366(17)
O1 0.0374(18) 0.0288(18) 0.0587(19) -0.0140(14) 0.0319(16) -0.0060(14)
O2 0.0297(15) 0.0281(17) 0.0404(16) -0.0067(14) 0.0244(14) -0.0068(13)
O3 0.027(2) 0.021(2) 0.033(2) 0.000 0.0211(18) 0.000
O4 0.0218(14) 0.0266(16) 0.0337(15) 0.0009(12) 0.0176(13) 0.0015(12)
O5 0.0282(15) 0.0269(16) 0.0326(15) -0.0012(12) 0.0219(13) 0.0001(12)
O6 0.031(2) 0.022(2) 0.034(2) 0.000 0.0209(19) 0.000
O7 0.0359(16) 0.0279(16) 0.0363(16) 0.0003(13) 0.0249(14) -0.0048(13)
O8 0.0486(18) 0.0312(17) 0.0431(17) -0.0075(15) 0.0329(16) -0.0144(15)

_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 1.374(5) . ?
C1 C6 1.378(5) . ?
C1 N3 1.405(5) . ?
C2 C3 1.384(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(5) . ?
C5 H5 0.9300 . ?
C6 O1 1.380(4) . ?
C7 N3 1.309(5) . ?
C7 O1 1.361(5) . ?
C7 C8 1.450(5) . ?
C8 C9 1.395(6) . ?
C8 C13 1.395(5) . ?
C9 C10 1.367(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.377(7) . ?
C10 C14 1.541(7) . ?
C11 C12 1.385(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.418(5) . ?
C12 C18 1.532(6) . ?
C13 O2 1.350(4) . ?
C14 C17 1.483(14) . ?
C14 C15 1.479(11) . ?
C14 C15A 1.487(17) . ?
C14 C16A 1.562(14) . ?
C14 C17A 1.557(16) . ?
C14 C16 1.652(14) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C17A H17D 0.9600 . ?
C17A H17E 0.9600 . ?
C17A H17F 0.9600 . ?
C16A H16D 0.9600 . ?
C16A H16E 0.9600 . ?
C16A H16F 0.9600 . ?
C15A H15D 0.9600 . ?
C15A H15E 0.9600 . ?
C15A H15F 0.9600 . ?
C18 C20 1.523(6) . ?
C18 C21 1.533(7) . ?
C18 C19 1.544(6) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C27 1.379(5) . ?
C22 C23 1.380(5) . ?
C22 N4 1.404(5) . ?
C23 C24 1.370(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.370(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.372(6) . ?
C26 H26 0.9300 . ?
C27 O8 1.389(5) . ?
C28 N4 1.309(5) . ?
C28 O8 1.364(5) . ?
C28 C29 1.443(6) . ?
C29 C30 1.391(6) . ?
C29 C34 1.409(6) . ?
C30 C31 1.377(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.402(6) . ?
C31 C35 1.540(7) . ?
C32 C33 1.391(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.407(6) . ?
C33 C39 1.525(6) . ?
C34 O7 1.368(4) . ?
C35 C37 1.540(8) . ?
C35 C38 1.508(7) . ?
C35 C36 1.534(8) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C42 1.525(7) . ?
C39 C41 1.526(7) . ?
C39 C40 1.533(6) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
Cl1 Nb1 2.4239(11) . ?
Cl2 Nb2 2.4285(10) . ?
N3 Nb1 2.306(3) . ?
N4 Nb2 2.293(3) . ?
Nb1 O4 1.831(2) . ?
Nb1 O2 1.918(2) . ?
Nb1 O3 1.9249(11) . ?
Nb1 O5 2.041(2) . ?
Nb2 O5 1.832(2) . ?
Nb2 O7 1.920(2) . ?
Nb2 O6 1.9250(11) . ?
Nb2 O4 2.028(2) 2_755 ?
O3 Nb1 1.9249(11) 2_755 ?
O4 Nb2 2.028(2) 2_755 ?
O6 Nb2 1.9251(11) 2_755 ?

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 120.7(3) . . ?
C2 C1 N3 131.5(4) . . ?
C6 C1 N3 107.7(3) . . ?
C3 C2 C1 116.6(4) . . ?
C3 C2 H2 121.7 . . ?
C1 C2 H2 121.7 . . ?
C2 C3 C4 122.0(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C5 C4 C3 121.5(4) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C6 C5 C4 115.5(4) . . ?
C6 C5 H5 122.2 . . ?
C4 C5 H5 122.2 . . ?
C5 C6 O1 128.1(4) . . ?
C5 C6 C1 123.7(4) . . ?
O1 C6 C1 108.2(3) . . ?
N3 C7 O1 113.9(3) . . ?
N3 C7 C8 129.6(4) . . ?
O1 C7 C8 116.5(4) . . ?
C9 C8 C13 120.5(4) . . ?
C9 C8 C7 119.4(4) . . ?
C13 C8 C7 120.1(4) . . ?
C8 C9 C10 121.1(4) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 117.3(4) . . ?
C11 C10 C14 121.2(5) . . ?
C9 C10 C14 121.6(5) . . ?
C12 C11 C10 125.4(4) . . ?
C12 C11 H11 117.3 . . ?
C10 C11 H11 117.3 . . ?
C11 C12 C13 116.1(4) . . ?
C11 C12 C18 122.0(4) . . ?
C13 C12 C18 121.9(4) . . ?
O2 C13 C8 118.5(3) . . ?
O2 C13 C12 121.9(4) . . ?
C8 C13 C12 119.6(4) . . ?
C17 C14 C15 123.3(12) . . ?
C17 C14 C10 111.7(7) . . ?
C15 C14 C10 114.5(6) . . ?
C15A C14 C10 122.0(12) . . ?
C15A C14 C16A 98.8(16) . . ?
C10 C14 C16A 108.4(10) . . ?
C15A C14 C17A 117.0(15) . . ?
C10 C14 C17A 108.7(12) . . ?
C16A C14 C17A 98.0(12) . . ?
C17 C14 C16 94.0(12) . . ?
C15 C14 C16 105.2(12) . . ?
C10 C14 C16 103.5(7) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C17A H17D 109.5 . . ?
C14 C17A H17E 109.5 . . ?
H17D C17A H17E 109.5 . . ?
C14 C17A H17F 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
C14 C16A H16D 109.5 . . ?
C14 C16A H16E 109.5 . . ?
H16D C16A H16E 109.5 . . ?
C14 C16A H16F 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
C14 C15A H15D 109.5 . . ?
C14 C15A H15E 109.5 . . ?
H15D C15A H15E 109.5 . . ?
C14 C15A H15F 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
C12 C18 C20 111.5(4) . . ?
C12 C18 C21 108.8(4) . . ?
C20 C18 C21 110.1(4) . . ?
C12 C18 C19 111.4(4) . . ?
C20 C18 C19 107.0(4) . . ?
C21 C18 C19 107.9(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C23 119.7(4) . . ?
C27 C22 N4 108.2(3) . . ?
C23 C22 N4 132.0(4) . . ?
C24 C23 C22 117.0(4) . . ?
C24 C23 H23 121.5 . . ?
C22 C23 H23 121.5 . . ?
C23 C24 C25 122.1(4) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C26 C25 C24 121.5(4) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C27 C26 C25 115.4(4) . . ?
C27 C26 H26 122.3 . . ?
C25 C26 H26 122.3 . . ?
C22 C27 C26 124.2(4) . . ?
C22 C27 O8 107.6(3) . . ?
C26 C27 O8 128.2(4) . . ?
N4 C28 O8 113.7(3) . . ?
N4 C28 C29 129.4(4) . . ?
O8 C28 C29 116.9(3) . . ?
C30 C29 C34 120.6(4) . . ?
C30 C29 C28 119.4(4) . . ?
C34 C29 C28 120.0(4) . . ?
C31 C30 C29 121.1(4) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C30 C31 C32 116.7(4) . . ?
C30 C31 C35 120.7(4) . . ?
C32 C31 C35 122.6(4) . . ?
C33 C32 C31 125.3(4) . . ?
C33 C32 H32 117.4 . . ?
C31 C32 H32 117.4 . . ?
C32 C33 C34 116.0(4) . . ?
C32 C33 C39 121.1(4) . . ?
C34 C33 C39 122.8(4) . . ?
O7 C34 C33 121.6(4) . . ?
O7 C34 C29 118.2(4) . . ?
C33 C34 C29 120.3(4) . . ?
C37 C35 C38 108.3(5) . . ?
C37 C35 C36 107.6(5) . . ?
C38 C35 C36 110.8(5) . . ?
C37 C35 C31 109.4(5) . . ?
C38 C35 C31 112.7(4) . . ?
C36 C35 C31 107.9(5) . . ?
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 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C33 C39 C42 109.7(4) . . ?
C33 C39 C41 110.5(4) . . ?
C42 C39 C41 110.4(5) . . ?
C33 C39 C40 112.1(4) . . ?
C42 C39 C40 107.8(4) . . ?
C41 C39 C40 106.2(4) . . ?
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 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C7 N3 C1 105.4(3) . . ?
C7 N3 Nb1 124.1(3) . . ?
C1 N3 Nb1 130.3(2) . . ?
C28 N4 C22 105.5(3) . . ?
C28 N4 Nb2 123.6(3) . . ?
C22 N4 Nb2 130.9(2) . . ?
O4 Nb1 O2 100.77(10) . . ?
O4 Nb1 O3 93.67(10) . . ?
O2 Nb1 O3 104.12(11) . . ?
O4 Nb1 O5 91.80(10) . . ?
O2 Nb1 O5 163.56(10) . . ?
O3 Nb1 O5 85.42(9) . . ?
O4 Nb1 N3 173.84(11) . . ?
O2 Nb1 N3 77.94(11) . . ?
O3 Nb1 N3 80.89(10) . . ?
O5 Nb1 N3 90.64(10) . . ?
O4 Nb1 Cl1 98.47(8) . . ?
O2 Nb1 Cl1 85.15(8) . . ?
O3 Nb1 Cl1 163.12(3) . . ?
O5 Nb1 Cl1 82.53(7) . . ?
N3 Nb1 Cl1 87.45(8) . . ?
O5 Nb2 O7 101.57(11) . . ?
O5 Nb2 O6 93.62(10) . . ?
O7 Nb2 O6 104.77(11) . . ?
O5 Nb2 O4 92.46(10) . 2_755 ?
O7 Nb2 O4 161.58(10) . 2_755 ?
O6 Nb2 O4 85.97(9) . 2_755 ?
O5 Nb2 N4 174.89(11) . . ?
O7 Nb2 N4 78.06(11) . . ?
O6 Nb2 N4 81.60(10) . . ?
O4 Nb2 N4 89.00(10) 2_755 . ?
O5 Nb2 Cl2 98.41(8) . . ?
O7 Nb2 Cl2 84.00(8) . . ?
O6 Nb2 Cl2 163.43(3) . . ?
O4 Nb2 Cl2 82.18(7) 2_755 . ?
N4 Nb2 Cl2 86.63(8) . . ?
C7 O1 C6 104.8(3) . . ?
C13 O2 Nb1 143.3(2) . . ?
Nb1 O3 Nb1 143.66(19) 2_755 . ?
Nb1 O4 Nb2 138.24(13) . 2_755 ?
Nb2 O5 Nb1 138.15(13) . . ?
Nb2 O6 Nb2 142.72(19) . 2_755 ?
C34 O7 Nb2 138.5(2) . . ?
C28 O8 C27 105.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.4(6) . . . . ?
N3 C1 C2 C3 -177.7(4) . . . . ?
C1 C2 C3 C4 1.0(7) . . . . ?
C2 C3 C4 C5 -0.9(7) . . . . ?
C3 C4 C5 C6 0.2(6) . . . . ?
C4 C5 C6 O1 179.2(4) . . . . ?
C4 C5 C6 C1 0.3(6) . . . . ?
C2 C1 C6 C5 -0.2(6) . . . . ?
N3 C1 C6 C5 177.7(4) . . . . ?
C2 C1 C6 O1 -179.3(4) . . . . ?
N3 C1 C6 O1 -1.4(4) . . . . ?
N3 C7 C8 C9 168.9(5) . . . . ?
O1 C7 C8 C9 -10.5(6) . . . . ?
N3 C7 C8 C13 -11.9(7) . . . . ?
O1 C7 C8 C13 168.7(4) . . . . ?
C13 C8 C9 C10 0.7(8) . . . . ?
C7 C8 C9 C10 179.9(5) . . . . ?
C8 C9 C10 C11 1.0(9) . . . . ?
C8 C9 C10 C14 -179.0(7) . . . . ?
C9 C10 C11 C12 -0.5(10) . . . . ?
C14 C10 C11 C12 179.5(7) . . . . ?
C10 C11 C12 C13 -1.6(8) . . . . ?
C10 C11 C12 C18 175.6(6) . . . . ?
C9 C8 C13 O2 177.0(4) . . . . ?
C7 C8 C13 O2 -2.1(6) . . . . ?
C9 C8 C13 C12 -2.9(7) . . . . ?
C7 C8 C13 C12 178.0(4) . . . . ?
C11 C12 C13 O2 -176.7(4) . . . . ?
C18 C12 C13 O2 6.1(6) . . . . ?
C11 C12 C13 C8 3.2(6) . . . . ?
C18 C12 C13 C8 -174.0(4) . . . . ?
C11 C10 C14 C17 -153.7(13) . . . . ?
C9 C10 C14 C17 26.3(15) . . . . ?
C11 C10 C14 C15 -7.6(18) . . . . ?
C9 C10 C14 C15 172.4(14) . . . . ?
C11 C10 C14 C15A -167.2(15) . . . . ?
C9 C10 C14 C15A 12.8(19) . . . . ?
C11 C10 C14 C16A -53.7(14) . . . . ?
C9 C10 C14 C16A 126.3(12) . . . . ?
C11 C10 C14 C17A 51.8(16) . . . . ?
C9 C10 C14 C17A -128.2(13) . . . . ?
C11 C10 C14 C16 106.4(8) . . . . ?
C9 C10 C14 C16 -73.6(9) . . . . ?
C11 C12 C18 C20 126.7(5) . . . . ?
C13 C12 C18 C20 -56.2(6) . . . . ?
C11 C12 C18 C21 -111.6(5) . . . . ?
C13 C12 C18 C21 65.4(5) . . . . ?
C11 C12 C18 C19 7.3(7) . . . . ?
C13 C12 C18 C19 -175.7(4) . . . . ?
C27 C22 C23 C24 -0.8(6) . . . . ?
N4 C22 C23 C24 177.1(4) . . . . ?
C22 C23 C24 C25 0.6(6) . . . . ?
C23 C24 C25 C26 -0.8(7) . . . . ?
C24 C25 C26 C27 1.1(6) . . . . ?
C23 C22 C27 C26 1.2(6) . . . . ?
N4 C22 C27 C26 -177.1(4) . . . . ?
C23 C22 C27 O8 179.6(3) . . . . ?
N4 C22 C27 O8 1.3(4) . . . . ?
C25 C26 C27 C22 -1.3(6) . . . . ?
C25 C26 C27 O8 -179.4(4) . . . . ?
N4 C28 C29 C30 -164.7(4) . . . . ?
O8 C28 C29 C30 15.0(6) . . . . ?
N4 C28 C29 C34 14.3(7) . . . . ?
O8 C28 C29 C34 -166.0(4) . . . . ?
C34 C29 C30 C31 -0.5(7) . . . . ?
C28 C29 C30 C31 178.4(4) . . . . ?
C29 C30 C31 C32 0.9(7) . . . . ?
C29 C30 C31 C35 -178.1(5) . . . . ?
C30 C31 C32 C33 -0.1(8) . . . . ?
C35 C31 C32 C33 178.9(5) . . . . ?
C31 C32 C33 C34 -1.0(7) . . . . ?
C31 C32 C33 C39 -178.5(5) . . . . ?
C32 C33 C34 O7 -179.6(4) . . . . ?
C39 C33 C34 O7 -2.2(6) . . . . ?
C32 C33 C34 C29 1.4(6) . . . . ?
C39 C33 C34 C29 178.9(4) . . . . ?
C30 C29 C34 O7 -179.7(4) . . . . ?
C28 C29 C34 O7 1.3(6) . . . . ?
C30 C29 C34 C33 -0.7(6) . . . . ?
C28 C29 C34 C33 -179.7(4) . . . . ?
C30 C31 C35 C37 57.9(7) . . . . ?
C32 C31 C35 C37 -121.2(6) . . . . ?
C30 C31 C35 C38 178.4(6) . . . . ?
C32 C31 C35 C38 -0.6(9) . . . . ?
C30 C31 C35 C36 -59.0(7) . . . . ?
C32 C31 C35 C36 122.0(6) . . . . ?
C32 C33 C39 C42 111.3(5) . . . . ?
C34 C33 C39 C42 -66.0(6) . . . . ?
C32 C33 C39 C41 -126.7(5) . . . . ?
C34 C33 C39 C41 56.0(6) . . . . ?
C32 C33 C39 C40 -8.4(6) . . . . ?
C34 C33 C39 C40 174.3(4) . . . . ?
O1 C7 N3 C1 -1.2(4) . . . . ?
C8 C7 N3 C1 179.3(4) . . . . ?
O1 C7 N3 Nb1 -176.0(2) . . . . ?
C8 C7 N3 Nb1 4.5(6) . . . . ?
C2 C1 N3 C7 179.1(4) . . . . ?
C6 C1 N3 C7 1.6(4) . . . . ?
C2 C1 N3 Nb1 -6.5(6) . . . . ?
C6 C1 N3 Nb1 175.9(3) . . . . ?
O8 C28 N4 C22 1.1(4) . . . . ?
C29 C28 N4 C22 -179.2(4) . . . . ?
O8 C28 N4 Nb2 179.9(2) . . . . ?
C29 C28 N4 Nb2 -0.3(6) . . . . ?
C27 C22 N4 C28 -1.5(4) . . . . ?
C23 C22 N4 C28 -179.5(4) . . . . ?
C27 C22 N4 Nb2 179.8(3) . . . . ?
C23 C22 N4 Nb2 1.8(6) . . . . ?
N3 C7 O1 C6 0.4(4) . . . . ?
C8 C7 O1 C6 179.9(3) . . . . ?
C5 C6 O1 C7 -178.3(4) . . . . ?
C1 C6 O1 C7 0.7(4) . . . . ?
C8 C13 O2 Nb1 33.2(6) . . . . ?
C12 C13 O2 Nb1 -146.9(3) . . . . ?
O2 Nb1 O4 Nb2 136.37(19) . . . 2_755 ?
O3 Nb1 O4 Nb2 31.2(2) . . . 2_755 ?
O5 Nb1 O4 Nb2 -54.3(2) . . . 2_755 ?
Cl1 Nb1 O4 Nb2 -136.99(18) . . . 2_755 ?
O7 Nb2 O5 Nb1 -138.51(19) . . . . ?
O6 Nb2 O5 Nb1 -32.6(2) . . . . ?
O4 Nb2 O5 Nb1 53.5(2) 2_755 . . . ?
Cl2 Nb2 O5 Nb1 135.94(18) . . . . ?
C33 C34 O7 Nb2 139.4(3) . . . . ?
C29 C34 O7 Nb2 -41.6(6) . . . . ?
N4 C28 O8 C27 -0.3(4) . . . . ?
C29 C28 O8 C27 179.9(3) . . . . ?
C22 C27 O8 C28 -0.7(4) . . . . ?
C26 C27 O8 C28 177.7(4) . . . . ?

_refine_diff_density_max         0.475
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.062

_shelx_res_file                  
;

    tbu_nb.res created by SHELXL-2014/7

TITL tbu_nb in C2/c
CELL  0.71073  27.8788  27.1666  19.8149   90.000  133.784   90.000
ZERR     4.00   0.0009   0.0010   0.0011    0.000    0.001    0.000
LATT 7
SYMM  - X,   Y, 1/2 - Z
SFAC C  H  N  O  Cl Nb
UNIT 336  384  16  56  16  16
MERG 2
OMIT -3 50
L.S. 20
ACTA
BOND   $H
FMAP 2
PLAN 3
CONF
SIZE     0.160   0.200   0.250
DFIX 1.54 0.02 C10 C14  C14 C16  C14 C15  C14 C17
DFIX 1.54 0.02 C14 C15A C14 C16A C14 C17A
DELU 0.002 C14 C15 C16 C17
DELU 0.002 C15A C16A C17A
SIMU 0.002 C14 C15 C16 C17
SIMU 0.002  C15A C16A C17A
ISOR 0.002 C15A C16A
ISOR 0.002 C17A
TEMP    23.00
WGHT    0.037300   21.783901
FVAR       0.46006   0.61863
MOLE 1
C1    1    1.019425    0.507560    0.118980    11.00000    0.02371    0.02909 =
         0.03302   -0.00079    0.01818    0.00503
C2    1    1.076155    0.535442    0.169056    11.00000    0.03118    0.03592 =
         0.05683   -0.01322    0.02938    0.00059
AFIX  43
H2    2    1.079600    0.566227    0.192637    11.00000   -1.20000
AFIX   0
C3    1    1.127892    0.515365    0.182596    11.00000    0.02979    0.04781 =
         0.05176   -0.01748    0.02346   -0.00589
AFIX  43
H3    2    1.167321    0.532973    0.216978    11.00000   -1.20000
AFIX   0
C4    1    1.122771    0.469720    0.146426    11.00000    0.03264    0.04737 =
         0.04405   -0.00969    0.02671    0.00196
AFIX  43
H4    2    1.158545    0.457785    0.156463    11.00000   -1.20000
AFIX   0
C5    1    1.065937    0.441756    0.096063    11.00000    0.05108    0.03296 =
         0.04827   -0.00353    0.03617    0.00546
AFIX  43
H5    2    1.062005    0.411115    0.071690    11.00000   -1.20000
AFIX   0
C6    1    1.015317    0.462174    0.084187    11.00000    0.03203    0.03166 =
         0.03748   -0.00240    0.02390    0.00317
C7    1    0.921796    0.477883    0.043433    11.00000    0.04043    0.02753 =
         0.03792   -0.00044    0.02741    0.00198
C8    1    0.854275    0.467006   -0.001599    11.00000    0.03059    0.03633 =
         0.04538   -0.01254    0.02399   -0.00813
C9    1    0.821581    0.426576   -0.061313    11.00000    0.05242    0.05995 =
         0.08891   -0.04331    0.05031   -0.02455
AFIX  43
H9    2    0.843408    0.407112   -0.071674    11.00000   -1.20000
AFIX   2
C10   1    0.757966    0.415082   -0.104878    11.00000    0.06495    0.07719 =
         0.11073   -0.06535    0.06352   -0.04442
C11   1    0.727427    0.445461   -0.088466    11.00000    0.04077    0.07838 =
         0.07822   -0.04173    0.04107   -0.03401
AFIX  43
H11   2    0.684023    0.437834   -0.118486    11.00000   -1.20000
AFIX   0
C12   1    0.756043    0.486457   -0.030909    11.00000    0.03193    0.04511 =
         0.04593   -0.00770    0.02586   -0.00940
C13   1    0.822830    0.496460    0.015826    11.00000    0.03467    0.02757 =
         0.03794   -0.00628    0.02347   -0.00649
C14   1    0.721719    0.370022   -0.169729    11.00000    0.11619    0.16364 =
         0.24640   -0.17233    0.14226   -0.10581
PART 1
C17   1    0.769000    0.331252   -0.145310    21.00000    0.12137    0.14854 =
         0.24904   -0.17863    0.13251   -0.10533
AFIX 137
H17A  2    0.802959    0.345625   -0.139983    21.00000   -1.50000
H17B  2    0.745679    0.306563   -0.193319    21.00000   -1.50000
H17C  2    0.788976    0.316464   -0.086818    21.00000   -1.50000
AFIX   0
C16   1    0.704026    0.387204   -0.264858    21.00000    0.12674    0.17272 =
         0.23988   -0.17190    0.13832   -0.10254
AFIX 137
H16A  2    0.679734    0.361484   -0.310756    21.00000   -1.50000
H16B  2    0.744491    0.393520   -0.249606    21.00000   -1.50000
H16C  2    0.677568    0.416595   -0.289509    21.00000   -1.50000
AFIX   0
C15   1    0.656808    0.359201   -0.201222    21.00000    0.11442    0.16284 =
         0.25189   -0.17147    0.13560   -0.11616
AFIX 137
H15A  2    0.639547    0.328942   -0.235880    21.00000   -1.50000
H15B  2    0.626328    0.385483   -0.240398    21.00000   -1.50000
H15C  2    0.662420    0.356155   -0.147829    21.00000   -1.50000
PART 2
AFIX   0
C17A  1    0.653182    0.386928   -0.264601   -21.00000    0.14901    0.14633 =
         0.14364   -0.00312    0.09911   -0.00431
AFIX 137
H17D  2    0.659961    0.409293   -0.294873   -21.00000   -1.50000
H17E  2    0.628574    0.403147   -0.253515   -21.00000   -1.50000
H17F  2    0.628757    0.358766   -0.303902   -21.00000   -1.50000
AFIX   0
C16A  1    0.695680    0.337803   -0.135415   -21.00000    0.11641    0.11672 =
         0.12233   -0.00406    0.08412   -0.00524
AFIX 137
H16D  2    0.664506    0.314040   -0.182591   -21.00000   -1.50000
H16E  2    0.674193    0.358491   -0.123678   -21.00000   -1.50000
H16F  2    0.732334    0.321070   -0.078880   -21.00000   -1.50000
AFIX   0
C15A  1    0.757441    0.331168   -0.173416   -21.00000    0.11588    0.11096 =
         0.11156   -0.00246    0.07891   -0.00391
AFIX 137
H15D  2    0.735064    0.325427   -0.237256   -21.00000   -1.50000
H15E  2    0.758149    0.301299   -0.146847   -21.00000   -1.50000
H15F  2    0.802167    0.341698   -0.138525   -21.00000   -1.50000
PART 0
AFIX   0
C18   1    0.716876    0.520428   -0.021839    11.00000    0.03862    0.04791 =
         0.06433   -0.01737    0.03605   -0.01346
C19   1    0.647466    0.499195   -0.073442    11.00000    0.04141    0.08008 =
         0.09532   -0.02398    0.04688   -0.01752
AFIX 137
H19A  2    0.622084    0.496843   -0.139044    11.00000   -1.50000
H19B  2    0.624994    0.520477   -0.064095    11.00000   -1.50000
H19C  2    0.652167    0.467066   -0.049268    11.00000   -1.50000
AFIX   0
C20   1    0.752368    0.527379    0.079896    11.00000    0.05375    0.10270 =
         0.07103   -0.02742    0.04790   -0.01885
AFIX 137
H20A  2    0.762705    0.495781    0.108941    11.00000   -1.50000
H20B  2    0.724087    0.545195    0.082784    11.00000   -1.50000
H20C  2    0.792689    0.545543    0.112109    11.00000   -1.50000
AFIX   0
C21   1    0.707219    0.570287   -0.066067    11.00000    0.05319    0.05931 =
         0.09171   -0.00649    0.04818    0.00147
AFIX 137
H21A  2    0.749606    0.585883   -0.030822    11.00000   -1.50000
H21B  2    0.679328    0.590833   -0.065813    11.00000   -1.50000
H21C  2    0.686672    0.565376   -0.129271    11.00000   -1.50000
AFIX   0
C22   1    1.147521    0.748365    0.415298    11.00000    0.03440    0.02858 =
         0.03400   -0.00393    0.02364   -0.00437
C23   1    1.144435    0.724184    0.473459    11.00000    0.03952    0.03331 =
         0.04112   -0.01012    0.02824   -0.01400
AFIX  43
H23   2    1.118953    0.695920    0.454237    11.00000   -1.20000
AFIX   0
C24   1    1.180596    0.743682    0.560792    11.00000    0.04358    0.04593 =
         0.04058   -0.00292    0.02982   -0.00997
AFIX  43
H24   2    1.179809    0.727997    0.601736    11.00000   -1.20000
AFIX   0
C25   1    1.218465    0.786196    0.590211    11.00000    0.04242    0.04815 =
         0.03833   -0.01081    0.02818   -0.01089
AFIX  43
H25   2    1.241809    0.798381    0.649836    11.00000   -1.20000
AFIX   0
C26   1    1.222130    0.810503    0.533312    11.00000    0.04444    0.03509 =
         0.05525   -0.01186    0.03452   -0.01428
AFIX  43
H26   2    1.247840    0.838630    0.552533    11.00000   -1.20000
AFIX   0
C27   1    1.185265    0.790506    0.446015    11.00000    0.03914    0.03313 =
         0.03718   -0.00247    0.02744   -0.00524
C28   1    1.139560    0.773245    0.304347    11.00000    0.04271    0.02542 =
         0.04091   -0.00624    0.02905   -0.00894
C29   1    1.125183    0.781281    0.219867    11.00000    0.03842    0.03048 =
         0.03849   -0.00287    0.02622   -0.00963
C30   1    1.163672    0.814367    0.220662    11.00000    0.05628    0.04664 =
         0.04538   -0.00488    0.03458   -0.01925
AFIX  43
H30   2    1.197536    0.831524    0.275224    11.00000   -1.20000
AFIX   0
C31   1    1.152471    0.822139    0.142029    11.00000    0.07344    0.04909 =
         0.05368   -0.00101    0.04617   -0.02003
C32   1    1.100087    0.795751    0.061637    11.00000    0.06481    0.05271 =
         0.05264    0.00392    0.04272   -0.01185
AFIX  43
H32   2    1.092063    0.800803    0.008126    11.00000   -1.20000
AFIX   0
C33   1    1.059144    0.762619    0.055454    11.00000    0.04214    0.03490 =
         0.03727    0.00390    0.02659   -0.00176
C34   1    1.073216    0.755130    0.137919    11.00000    0.03539    0.02870 =
         0.04345    0.00806    0.02660    0.00193
C35   1    1.196737    0.857671    0.144547    11.00000    0.09002    0.08397 =
         0.06590   -0.00459    0.05621   -0.04186
C36   1    1.191905    0.908662    0.172713    11.00000    0.12593    0.06689 =
         0.12749   -0.00158    0.08826   -0.04167
AFIX 137
H36A  2    1.218886    0.931574    0.174293    11.00000   -1.50000
H36B  2    1.207284    0.906801    0.233474    11.00000   -1.50000
H36C  2    1.146521    0.919526    0.127999    11.00000   -1.50000
AFIX   0
C37   1    1.269639    0.840789    0.220337    11.00000    0.07145    0.13577 =
         0.08436   -0.00808    0.05378   -0.04182
AFIX 137
H37A  2    1.273698    0.808119    0.206291    11.00000   -1.50000
H37B  2    1.283392    0.840872    0.280117    11.00000   -1.50000
H37C  2    1.297264    0.862855    0.221841    11.00000   -1.50000
AFIX   0
C38   1    1.177795    0.860112    0.052563    11.00000    0.12472    0.15027 =
         0.08152   -0.00848    0.07461   -0.07704
AFIX 137
H38A  2    1.133783    0.873385    0.005531    11.00000   -1.50000
H38B  2    1.178932    0.827628    0.034632    11.00000   -1.50000
H38C  2    1.208609    0.880877    0.058959    11.00000   -1.50000
AFIX   0
C39   1    1.004416    0.734796   -0.034965    11.00000    0.04686    0.05606 =
         0.03774    0.00242    0.02755   -0.01005
C40   1    0.994944    0.753576   -0.116511    11.00000    0.07502    0.08001 =
         0.05059   -0.00237    0.04221   -0.01979
AFIX 137
H40A  2    0.988071    0.788541   -0.122484    11.00000   -1.50000
H40B  2    0.957007    0.737794   -0.173297    11.00000   -1.50000
H40C  2    1.033824    0.746152   -0.104813    11.00000   -1.50000
AFIX   0
C41   1    0.937783    0.741850   -0.064340    11.00000    0.04651    0.18436 =
         0.05278   -0.00787    0.02758   -0.02215
AFIX 137
H41A  2    0.938652    0.725408   -0.020618    11.00000   -1.50000
H41B  2    0.902950    0.728237   -0.125583    11.00000   -1.50000
H41C  2    0.929840    0.776342   -0.065293    11.00000   -1.50000
AFIX   0
C42   1    1.022009    0.680250   -0.021667    11.00000    0.12278    0.05052 =
         0.06090   -0.01389    0.05353   -0.02181
AFIX 137
H42A  2    1.065772    0.676566    0.002347    11.00000   -1.50000
H42B  2    0.990479    0.663598   -0.080653    11.00000   -1.50000
H42C  2    1.020847    0.666257    0.021675    11.00000   -1.50000
AFIX   0
CL1   5    0.853494    0.607375   -0.036696    11.00000    0.03541    0.03569 =
         0.03382   -0.00179    0.02178    0.00270
CL2   5    1.142289    0.648739    0.240489    11.00000    0.03425    0.03757 =
         0.04812   -0.00610    0.03093   -0.00682
N3    3    0.957997    0.517024    0.090215    11.00000    0.02562    0.02332 =
         0.03499   -0.00369    0.01890   -0.00099
N4    3    1.119657    0.737777    0.324848    11.00000    0.03407    0.02684 =
         0.03175   -0.00014    0.02313   -0.00295
NB1   6    0.924851    0.581960    0.124948    11.00000    0.02250    0.02277 =
         0.03116   -0.00268    0.01758   -0.00141
NB2   6    1.051458    0.674904    0.224322    11.00000    0.02724    0.02329 =
         0.03260   -0.00128    0.02082   -0.00366
O1    4    0.953103    0.442923    0.036413    11.00000    0.03740    0.02876 =
         0.05869   -0.01396    0.03193   -0.00604
O2    4    0.857400    0.533855    0.077355    11.00000    0.02967    0.02815 =
         0.04044   -0.00674    0.02441   -0.00679
O3    4    1.000000    0.559868    0.250000    10.50000    0.02691    0.02055 =
         0.03289    0.00000    0.02108    0.00000
O4    4    0.902408    0.629877    0.163922    11.00000    0.02178    0.02660 =
         0.03366    0.00093    0.01756    0.00153
O5    4    0.990993    0.627413    0.142297    11.00000    0.02815    0.02688 =
         0.03259   -0.00123    0.02186    0.00005
O6    4    1.000000    0.697552    0.250000    10.50000    0.03053    0.02169 =
         0.03400    0.00000    0.02093    0.00000
O7    4    1.036775    0.723224    0.140927    11.00000    0.03588    0.02787 =
         0.03626    0.00029    0.02486   -0.00476
O8    4    1.179802    0.806748    0.374451    11.00000    0.04859    0.03123 =
         0.04314   -0.00749    0.03287   -0.01437
HKLF    4

REM  tbu_nb in C2/c
REM R1 =  0.0339 for    5153 Fo > 4sig(Fo)  and  0.0453 for all    6455 data
REM    528 parameters refined using     49 restraints

END

WGHT      0.0468      4.8066

REM Highest difference peak  0.475,  deepest hole -0.330,  1-sigma level  0.062
Q1    1   0.7692  0.3171 -0.0714  11.00000  0.05    0.47
Q2    1   0.7136  0.4079 -0.2840  11.00000  0.05    0.38
Q3    1   1.3010  0.8239  0.5273  11.00000  0.05    0.36
;
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    0    0    4     61.20      0.00
  -27    7    4     -4.38      0.00
   18   12    4      0.21      0.00
   17   15    4      1.11      0.00
  -23   19    4      5.29      0.00
   11   25    4     -2.04      0.00
   10   26    4      5.12      0.00
  -12   30    4      0.99      0.00
   -4   32    4     -1.13      0.00
   -2   32    4     -1.26      0.00
  -28    6    5      1.73      0.00
  -27   11    5     -2.45      0.00
  -26   14    5      2.22      0.00
   15   17    5      0.19      0.00
   12   22    5     -1.60      0.00
  -21   23    5     -1.70      0.00
  -17   27    5     -0.76      0.00
  -16   28    5      2.43      0.00
    6   28    5      2.68      0.00
   -6    0    6    -99.81      0.00
   -4    0    6   -109.34      0.00
  -29    1    6      2.67      0.00
  -29    3    6      0.23      0.00
  -27   13    6     -1.97      0.00
   12   20    6      3.35      0.00
  -23   21    6     -5.01      0.00
    3   29    6      0.14      0.00
   -9   31    6     -0.29      0.00
   16    2    7      1.47      0.00
   16    4    7      0.75      0.00
  -28   12    7     -1.88      0.00
  -27   15    7     -3.78      0.00
   12   18    7      2.19      0.00
  -25   19    7     -0.16      0.00
  -15   29    7     -0.22      0.00
    1   29    7     -3.41      0.00
   -7   31    7      0.62      0.00
   -5   31    7      0.21      0.00
  -30    6    8     -4.39      0.00
   14    8    8     -0.71      0.00
  -29   11    8      0.13      0.00
  -28   14    8      0.21      0.00
   11   17    8     -1.75      0.00
  -26   18    8      5.46      0.00
    8   22    8     -4.92      0.00
    7   23    8      3.77      0.00
    4   26    8      1.05      0.00
    3   27    8     -5.41      0.00
  -15   29    8     -3.38      0.00
   -1   29    8      3.48      0.00
  -12   30    8     -1.45      0.00
   -4   30    8      3.68      0.00
  -31    1    9      3.24      0.00
   10   16    9      2.15      0.00
  -27   17    9     -2.39      0.00
    7   21    9      2.46      0.00
  -24   22    9     -0.88      0.00
  -23   23    9      0.01      0.00
  -22   24    9      1.95      0.00
  -21   25    9      0.91      0.00
  -20   26    9      0.26      0.00
    1   27    9     -2.01      0.00
   -3   29    9      6.24      0.00
  -10   30    9     -0.79      0.00
   -8   30    9      1.86      0.00
   12    0   10      1.13      0.00
   12    2   10      3.66      0.00
  -31    7   10      0.66      0.00
   11    9   10     -1.75      0.00
    9   15   10      6.03      0.00
  -28   16   10      2.07      0.00
    7   19   10      3.22      0.00
  -25   21   10      2.62      0.00
  -21   25   10     -1.32      0.00
  -20   26   10     -1.51      0.00
   -1   27   10      0.11      0.00
  -13   29   10     -6.12      0.00
  -32    2   11      0.56      0.00
  -31    3   11     -0.84      0.00
   10    6   11      1.32      0.00
  -31    9   11     -0.86      0.00
    9   11   11     -0.70      0.00
  -30   12   11     -0.04      0.00
    8   14   11      3.31      0.00
    6   18   11      4.01      0.00
  -26   20   11      1.55      0.00
  -21   25   11      5.73      0.00
  -20   26   11     -1.73      0.00
   -6   28   11      1.47      0.00
  -32    0   12      3.63      0.00
  -31    1   12     -2.81      0.00
    9    1   12     -4.50      0.00
  -32    2   12     -1.07      0.00
  -31    3   12     -0.91      0.00
    9    3   12     -2.29      0.00
  -32    4   12     -0.07      0.00
  -32    6   12     -0.91      0.00
  -27   19   12      0.74      0.00
  -26   20   12      4.07      0.00
  -21   25   12      5.01      0.00
   -4   26   12      2.62      0.00
  -17   27   12      5.43      0.00
  -12   28   12     -4.21      0.00
  -10   28   12      0.32      0.00
  -31    1   13      0.84      0.00
  -32    2   13     -0.44      0.00
  -30    2   13      0.25      0.00
  -31    3   13      3.37      0.00
  -32    4   13      0.74      0.00
    7    5   13     -8.20      0.00
    6   10   13     -0.99      0.00
  -31   11   13      0.46      0.00
    5   13   13     -2.01      0.00
    3   17   13     -3.78      0.00
  -27   19   13      1.63      0.00
  -22   24   13      1.34      0.00
   -5   25   13     -0.39      0.00
  -18   26   13      1.58      0.00
  -15   27   13      1.62      0.00
  -13   27   13      1.53      0.00
  -11   27   13      1.72      0.00
  -32    0   14     -2.08      0.00
  -30    0   14      0.09      0.00
  -33    1   14      4.08      0.00
  -31    1   14      2.11      0.00
  -29    1   14     -2.87      0.00
  -32    2   14      1.26      0.00
  -30    2   14      0.28      0.00
  -33    3   14     -0.23      0.00
  -31    3   14     -1.53      0.00
  -32    4   14      0.18      0.00
    5    7   14      3.09      0.00
  -32    8   14      1.11      0.00
  -30   14   14      0.39      0.00
    1   17   14      0.15      0.00
  -27   19   14      1.78      0.00
  -26   20   14     -1.60      0.00
  -25   21   14      2.78      0.00
  -24   22   14     -4.45      0.00
  -23   23   14      0.38      0.00
   -6   24   14      2.61      0.00
  -19   25   14      3.50      0.00
  -16   26   14      3.48      0.00
  -14   26   14      2.84      0.00
  -12   26   14     -3.33      0.00
  -33    1   15     -0.62      0.00
  -31    1   15      2.76      0.00
  -32    2   15     -1.94      0.00
  -30    2   15     -2.10      0.00
    4    2   15      1.99      0.00
  -33    3   15     -1.88      0.00
  -31    3   15      1.10      0.00
  -32    4   15     -2.06      0.00
  -30   14   15      0.92      0.00
   -1   17   15     -3.00      0.00
  -26   20   15      0.06      0.00
  -25   21   15     -2.87      0.00
   -7   23   15     -3.09      0.00
  -20   24   15     -0.70      0.00
  -17   25   15      2.87      0.00
  -15   25   15      2.62      0.00
  -13   25   15     -2.78      0.00
  -32    0   16     -0.18      0.00
    2    0   16      0.62      0.00
  -33    1   16     -1.60      0.00
  -31    1   16     -1.85      0.00
  -32    2   16      2.41      0.00
    2    2   16     -0.06      0.00
  -33    3   16     -4.96      0.00
  -31    3   16     -3.28      0.00
  -32    4   16      3.23      0.00
    2    4   16     -0.44      0.00
  -33    5   16     -0.74      0.00
  -30   14   16     -0.71      0.00
   -3   17   16     -2.66      0.00
   -4   18   16      3.45      0.00
   -5   19   16      4.92      0.00
   -6   20   16     -0.43      0.00
   -7   21   16     -0.18      0.00
  -11   23   16     -2.24      0.00
  -16   24   16      4.75      0.00
  -33    1   17      0.70      0.00
  -31    1   17      5.21      0.00
  -32    2   17     -3.52      0.00
    0    2   17     -1.98      0.00
  -33    3   17      3.23      0.00
  -31    3   17      4.48      0.00
  -32    4   17     -4.04      0.00
    0    4   17     -0.02      0.00
  -33    5   17      0.63      0.00
  -31   11   17     -1.94      0.00
   -3   13   17      6.87      0.00
  -29   15   17      7.84      0.00
  -24   20   17     -3.47      0.00
  -23   21   17      3.97      0.00
  -20   22   17     -5.24      0.00
  -32    0   18    -10.78      0.00
   -2    0   18      0.37      0.00
  -33    1   18      9.74      0.00
  -32    2   18     -4.90      0.00
   -2    2   18     -2.11      0.00
  -33    3   18     -3.70      0.00
  -32    4   18      2.44      0.00
  -32    8   18      1.60      0.00
  -31   11   18      2.73      0.00
   -6   14   18      9.07      0.00
  -11   19   18     -2.47      0.00
  -22   20   18     -1.61      0.00
  -19   21   18     -3.19      0.00
  -17   21   18     -4.88      0.00
  -32    2   19     -9.41      0.00
  -32    4   19      2.84      0.00
  -32    6   19     -0.95      0.00
   -5    7   19      1.00      0.00
  -31    9   19      1.38      0.00
  -29   13   19     -4.07      0.00
  -25   17   19     -1.79      0.00
  -24   18   19     -3.05      0.00
  -21   19   19      4.04      0.00
  -32    0   20      5.83      0.00
  -16    0   20    -20.01      0.00
  -14    0   20    -12.03      0.00
  -12    0   20     -5.72      0.00
  -15    1   20     17.92      0.00
  -13    1   20     12.03      0.00
  -32    2   20      4.60      0.00
  -16    2   20      5.10      0.00
  -14    2   20      1.83      0.00
  -12    2   20      5.23      0.00
  -15    3   20     -8.15      0.00
  -13    3   20     -7.99      0.00
   -7    3   20     -4.70      0.00
  -32    4   20      0.63      0.00
  -16    4   20      7.64      0.00
  -14    4   20      7.28      0.00
  -17    5   20     -2.52      0.00
  -15    5   20     -1.73      0.00
   -7    5   20     -0.66      0.00
  -18    6   20     -5.17      0.00
  -16    6   20     -4.32      0.00
  -14    6   20     -5.95      0.00
  -19    7   20      0.02      0.00
  -17    7   20     -0.43      0.00
  -15    7   20      3.81      0.00
  -20    8   20     -2.58      0.00
  -18    8   20     -2.27      0.00
  -16    8   20     -2.11      0.00
  -14    8   20      1.00      0.00
   -8    8   20     -0.06      0.00
  -19    9   20      1.03      0.00
  -17    9   20     -1.49      0.00
  -30   10   20      4.28      0.00
  -10   12   20     -0.08      0.00
  -11   13   20      3.65      0.00
  -12   14   20     -0.66      0.00
  -13   15   20      0.43      0.00
  -24   16   20     -2.28      0.00
  -21   17   20     -1.36      0.00
  -17   17   20     -1.91      0.00
  -23    1   21     -0.13      0.00
  -21    1   21      6.59      0.00
  -19    1   21     -4.19      0.00
  -17    1   21     -2.78      0.00
  -15    1   21     -4.42      0.00
  -13    1   21      0.27      0.00
  -22    2   21      0.95      0.00
  -20    2   21      8.47      0.00
  -18    2   21      6.23      0.00
  -16    2   21      2.38      0.00
  -14    2   21     -1.77      0.00
  -23    3   21      1.07      0.00
  -21    3   21      5.48      0.00
  -19    3   21      5.33      0.00
  -17    3   21     -6.09      0.00
  -15    3   21     -1.31      0.00
  -13    3   21     -1.74      0.00
  -24    4   21     -0.41      0.00
  -22    4   21     -0.06      0.00
  -20    4   21      3.82      0.00
  -18    4   21     -0.68      0.00
  -16    4   21     -5.48      0.00
  -14    4   21     -4.39      0.00
  -10    4   21     -6.11      0.00
  -31    5   21      1.51      0.00
  -25    5   21      3.45      0.00
  -23    5   21      6.57      0.00
  -21    5   21      5.33      0.00
  -19    5   21     -0.56      0.00
  -17    5   21      5.19      0.00
  -15    5   21      2.47      0.00
  -13    5   21      3.84      0.00
  -26    6   21      5.55      0.00
  -24    6   21      0.68      0.00
  -22    6   21     -0.80      0.00
  -20    6   21     -2.73      0.00
  -18    6   21     -2.70      0.00
  -16    6   21     -0.82      0.00
  -23    7   21     -4.19      0.00
  -21    7   21     -1.74      0.00
  -19    7   21     -3.55      0.00
  -17    7   21     -6.50      0.00
  -15    7   21     -5.46      0.00
  -30    8   21      1.56      0.00
  -22    8   21     -0.52      0.00
  -20    8   21     10.38      0.00
  -18    8   21     10.91      0.00
  -16    8   21      4.47      0.00
  -14    8   21      4.40      0.00
  -23    9   21     -1.20      0.00
  -21    9   21     -1.80      0.00
  -19    9   21     -1.01      0.00
  -17    9   21     -1.35      0.00
  -15    9   21     -3.23      0.00
  -20   10   21      2.89      0.00
  -18   10   21      1.64      0.00
  -16   10   21      1.35      0.00
  -12   10   21     -1.67      0.00
  -13   11   21     -3.86      0.00
  -14   12   21      4.61      0.00
  -15   13   21     -7.93      0.00
  -24   14   21      4.58      0.00
  -16   14   21      3.50      0.00
  -21   15   21     -2.36      0.00
  -19   15   21     -1.42      0.00
  -30    0   22      1.25      0.00
  -28    0   22     -1.01      0.00
  -26    0   22     -3.29      0.00
  -24    0   22      0.24      0.00
  -22    0   22     16.30      0.00
  -20    0   22     11.76      0.00
  -18    0   22      3.39      0.00
  -16    0   22     -3.67      0.00
  -14    0   22     -3.09      0.00
  -29    1   22      1.19      0.00
  -27    1   22     -1.18      0.00
  -25    1   22     -4.49      0.00
  -23    1   22     -0.31      0.00
  -21    1   22     -0.32      0.00
  -19    1   22     -2.74      0.00
  -17    1   22     -1.08      0.00
  -15    1   22      0.27      0.00
  -13    1   22     -0.64      0.00
  -30    2   22      2.38      0.00
  -28    2   22      5.79      0.00
  -26    2   22     -0.48      0.00
  -24    2   22     -1.58      0.00
  -22    2   22      0.48      0.00
  -20    2   22      6.11      0.00
  -18    2   22     -5.50      0.00
  -16    2   22     -2.17      0.00
  -14    2   22     -2.99      0.00
  -29    3   22     -2.54      0.00
  -27    3   22      0.09      0.00
  -25    3   22      7.00      0.00
  -23    3   22      5.34      0.00
  -21    3   22      4.59      0.00
  -19    3   22      6.90      0.00
  -17    3   22      2.36      0.00
  -15    3   22     -0.61      0.00
  -13    3   22      0.63      0.00
  -30    4   22      3.45      0.00
  -28    4   22      6.70      0.00
  -26    4   22      2.58      0.00
  -24    4   22     -2.75      0.00
  -22    4   22     -5.57      0.00
  -20    4   22     -7.73      0.00
  -18    4   22     -1.05      0.00
  -16    4   22      0.20      0.00
  -14    4   22      3.57      0.00
  -29    5   22     -2.36      0.00
  -27    5   22     -2.38      0.00
  -25    5   22      1.55      0.00
  -23    5   22      0.66      0.00
  -21    5   22     -4.73      0.00
  -19    5   22     -2.12      0.00
  -17    5   22      0.60      0.00
  -15    5   22     -3.12      0.00
  -28    6   22     -1.37      0.00
  -26    6   22     -3.01      0.00
  -24    6   22     -3.21      0.00
  -22    6   22      1.51      0.00
  -20    6   22      5.68      0.00
  -18    6   22      0.39      0.00
  -16    6   22      0.93      0.00
  -14    6   22      1.56      0.00
  -27    7   22     -0.05      0.00
  -25    7   22      0.92      0.00
  -23    7   22     -4.15      0.00
  -21    7   22     -2.48      0.00
  -19    7   22      0.51      0.00
  -17    7   22     -0.41      0.00
  -15    7   22     -0.25      0.00
  -28    8   22     -7.05      0.00
  -24    8   22      0.28      0.00
  -22    8   22      0.19      0.00
  -20    8   22      0.68      0.00
  -18    8   22      0.59      0.00
  -16    8   22      0.27      0.00
  -27    9   22      5.15      0.00
  -25    9   22      5.45      0.00
  -23    9   22      3.83      0.00
  -21    9   22     -0.80      0.00
  -19    9   22     -1.62      0.00
  -17    9   22      1.99      0.00
  -26   10   22      0.66      0.00
  -22   10   22     -1.02      0.00
  -20   10   22     -2.73      0.00
  -18   10   22      0.55      0.00
  -25   11   22     -2.05      0.00
  -21   11   22     -4.28      0.00
  -19   11   22     -4.87      0.00
  -22   12   22      1.62      0.00
  -20   12   22     -0.44      0.00
  -27    1   23      3.27      0.00
  -25    1   23      1.83      0.00
  -23    1   23     -5.46      0.00
  -21    1   23     -1.34      0.00
  -19    1   23     -3.70      0.00
  -17    1   23     -1.29      0.00
  -28    2   23     -0.50      0.00
  -26    2   23      2.37      0.00
  -24    2   23     -0.59      0.00
  -22    2   23     -1.79      0.00
  -20    2   23      3.74      0.00
  -18    2   23      4.01      0.00
  -27    3   23      2.96      0.00
  -25    3   23      2.06      0.00
  -23    3   23     -4.30      0.00
  -21    3   23     -9.34      0.00
  -19    3   23     -1.00      0.00
  -17    3   23      0.10      0.00
  -26    4   23     -0.50      0.00
  -24    4   23     -0.51      0.00
  -22    4   23     -1.15      0.00
  -20    4   23     -1.22      0.00
  -18    4   23      1.85      0.00
  -27    5   23     -4.22      0.00
  -25    5   23     -3.13      0.00
  -23    5   23     -3.96      0.00
  -21    5   23     -2.87      0.00
  -19    5   23     -2.83      0.00
  -26    6   23      3.12      0.00
  -24    6   23      1.21      0.00
  -22    6   23      3.02      0.00
  -20    6   23      1.74      0.00
  -25    7   23      0.57      0.00
  -23    7   23     -0.48      0.00
  -21    7   23     -2.60      0.00
  -22    8   23     -1.34      0.00
    0    0    0      0.00      0.00
# SQUEEZE RESULTS (Version = 110917)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.456 -0.066  0.405      3341       603 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
    1    1    0     1.259
    0    2    0     1.499
   -1    1    1     1.272
   -2    0    2     2.056
   -4    0    4     4.115
    0    0    4     5.703
   -6    0    6     6.180
   -4    0    6     6.455
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details
;

# Solvent Accessible Volume =      3355
# Electrons Found in S.A.V. =       601
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others



# start Validation Reply Form
_vrf_THETM01_tbu_nb_sq           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Even though crystal data was collected up to 0.78 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle 
;
_vrf_PLAT213_tbu_nb_sq           
;
PROBLEM: Atom C17             has ADP max/min Ratio .....        5.9 prolat
RESPONSE: This alarm is due to the elongated ADP of C17 carbon atom of the 
tert butyl group which suggest that these are disordered in two positions.
 The partial occupancy factor of C17 is 61:39. 
;
_vrf_PLAT976_tbu_nb_sq           
;
PROBLEM: Check Calcd Residual Density  0.45A From      O5      -1.60 eA-3  
RESPONSE: The large residual density near the atom Nb might be caused 
by the improper absorption correction or the highly polarized electron densities.
;
# end Validation Reply Form



