# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1551417'
_audit_update_record             
;
2017-05-22 deposited with the CCDC.
2018-01-24 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            'C23 H29 Cl6 N2 Nb'
_chemical_formula_weight         639.09

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

_space_group_crystal_system      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                   10.004(2)
_cell_length_b                   10.785(3)
_cell_length_c                   12.934(3)
_cell_angle_alpha                85.466(3)
_cell_angle_beta                 88.650(3)
_cell_angle_gamma                83.733(3)
_cell_volume                     1382.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4339
_cell_measurement_theta_min      2.3795
_cell_measurement_theta_max      25.502

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    1.030
_shelx_estimated_absorpt_T_min   0.805
_shelx_estimated_absorpt_T_max   0.853
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1051 (selected reflections only, before parameter refinement)
 R(int) =  0.0471 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13141
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.580
_diffrn_reflns_theta_max         25.646
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5167
_reflns_number_gt                3866
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0440P)²+0.6164P] 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         5167
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Nb1 Nb 0.69641(3) 0.80825(3) 0.76287(2) 0.01870(11) Uani 1 1 d . . . . .
Cl1 Cl 0.59357(10) 0.62083(10) 0.76142(8) 0.0378(3) Uani 1 1 d . . . . .
Cl2 Cl 0.52327(10) 0.89230(10) 0.87497(8) 0.0382(3) Uani 1 1 d . . . . .
Cl3 Cl 0.81222(9) 0.71892(9) 0.91219(7) 0.0262(2) Uani 1 1 d . . . . .
Cl4 Cl 0.81235(10) 0.98086(9) 0.77155(8) 0.0347(3) Uani 1 1 d . . . . .
Cl5 Cl 0.85964(9) 0.72394(9) 0.64939(7) 0.0280(2) Uani 1 1 d . . . . .
Cl6 Cl 0.56729(10) 0.90500(10) 0.62595(8) 0.0362(3) Uani 1 1 d . . . . .
N1 N 0.3762(3) 0.2893(3) 0.8019(2) 0.0160(6) Uani 1 1 d . . . . .
N2 N 0.6531(3) 0.2480(3) 0.7863(2) 0.0193(7) Uani 1 1 d . . . . .
C1 C 0.5892(3) 0.2332(3) 0.8758(3) 0.0225(8) Uani 1 1 d . . . . .
H1 H 0.6402 0.2070 0.9361 0.027 Uiso 1 1 calc R U . . .
C2 C 0.4485(3) 0.2545(3) 0.8857(3) 0.0203(8) Uani 1 1 d . . . . .
H2 H 0.4058 0.2440 0.9517 0.024 Uiso 1 1 calc R U . . .
C3 C 0.4362(3) 0.3023(3) 0.7048(3) 0.0170(8) Uani 1 1 d . . . . .
C4 C 0.5793(3) 0.2794(3) 0.6998(3) 0.0184(8) Uani 1 1 d . . . . .
C5 C 0.6462(3) 0.2909(3) 0.6016(3) 0.0206(8) Uani 1 1 d . . . . .
C6 C 0.5680(4) 0.3242(4) 0.5166(3) 0.0251(9) Uani 1 1 d . . . . .
H6 H 0.6104 0.3318 0.4503 0.030 Uiso 1 1 calc R U . . .
C7 C 0.4265(4) 0.3478(4) 0.5234(3) 0.0251(9) Uani 1 1 d . . . . .
H7 H 0.3768 0.3722 0.4621 0.030 Uiso 1 1 calc R U . . .
C8 C 0.3597(4) 0.3362(3) 0.6168(3) 0.0218(8) Uani 1 1 d . . . . .
H8 H 0.2644 0.3507 0.6211 0.026 Uiso 1 1 calc R U . . .
C9 C 0.7983(3) 0.2644(3) 0.5927(3) 0.0232(8) Uani 1 1 d . . . . .
H9 H 0.8329 0.2333 0.6630 0.028 Uiso 1 1 calc R U . . .
C10 C 0.8613(4) 0.3843(4) 0.5593(3) 0.0316(10) Uani 1 1 d . . . . .
H10A H 0.9595 0.3665 0.5577 0.047 Uiso 1 1 calc R U . . .
H10B H 0.8349 0.4472 0.6087 0.047 Uiso 1 1 calc R U . . .
H10C H 0.8300 0.4161 0.4900 0.047 Uiso 1 1 calc R U . . .
C11 C 0.8382(4) 0.1631(4) 0.5195(3) 0.0305(9) Uani 1 1 d . . . . .
H11A H 0.7971 0.0873 0.5434 0.046 Uiso 1 1 calc R U . . .
H11B H 0.9363 0.1445 0.5181 0.046 Uiso 1 1 calc R U . . .
H11C H 0.8070 0.1920 0.4495 0.046 Uiso 1 1 calc R U . . .
C12 C 0.2292(3) 0.3162(3) 0.8141(3) 0.0173(8) Uani 1 1 d . . . . .
C13 C 0.1526(3) 0.2153(3) 0.8169(3) 0.0190(8) Uani 1 1 d . . . . .
C14 C 0.0138(3) 0.2449(3) 0.8277(3) 0.0212(8) Uani 1 1 d . . . . .
H14 H -0.0435 0.1800 0.8298 0.025 Uiso 1 1 calc R U . . .
C15 C -0.0415(4) 0.3668(3) 0.8355(3) 0.0235(8) Uani 1 1 d . . . . .
H15 H -0.1363 0.3845 0.8425 0.028 Uiso 1 1 calc R U . . .
C16 C 0.0383(4) 0.4631(4) 0.8333(3) 0.0256(9) Uani 1 1 d . . . . .
H16 H -0.0018 0.5463 0.8391 0.031 Uiso 1 1 calc R U . . .
C17 C 0.1775(3) 0.4395(3) 0.8228(3) 0.0179(8) Uani 1 1 d . . . . .
C18 C 0.2129(4) 0.0811(3) 0.8066(3) 0.0242(9) Uani 1 1 d . . . . .
H18 H 0.3129 0.0794 0.8100 0.029 Uiso 1 1 calc R U . . .
C19 C 0.1680(4) -0.0066(4) 0.8965(3) 0.0314(10) Uani 1 1 d . . . . .
H19A H 0.1919 0.0235 0.9624 0.047 Uiso 1 1 calc R U . . .
H19B H 0.2130 -0.0911 0.8902 0.047 Uiso 1 1 calc R U . . .
H19C H 0.0704 -0.0083 0.8943 0.047 Uiso 1 1 calc R U . . .
C20 C 0.1804(4) 0.0376(4) 0.7021(3) 0.0329(10) Uani 1 1 d . . . . .
H20A H 0.0834 0.0330 0.6982 0.049 Uiso 1 1 calc R U . . .
H20B H 0.2286 -0.0453 0.6940 0.049 Uiso 1 1 calc R U . . .
H20C H 0.2084 0.0969 0.6466 0.049 Uiso 1 1 calc R U . . .
C21 C 0.2674(4) 0.5442(3) 0.8232(3) 0.0205(8) Uani 1 1 d . . . . .
H21 H 0.3552 0.5147 0.7901 0.025 Uiso 1 1 calc R U . . .
C22 C 0.2105(4) 0.6629(4) 0.7616(3) 0.0354(10) Uani 1 1 d . . . . .
H22A H 0.1883 0.6432 0.6918 0.053 Uiso 1 1 calc R U . . .
H22B H 0.2774 0.7231 0.7568 0.053 Uiso 1 1 calc R U . . .
H22C H 0.1290 0.6990 0.7965 0.053 Uiso 1 1 calc R U . . .
C23 C 0.2959(5) 0.5729(4) 0.9344(3) 0.0413(12) Uani 1 1 d . . . . .
H23A H 0.2115 0.6036 0.9685 0.062 Uiso 1 1 calc R U . . .
H23B H 0.3584 0.6370 0.9327 0.062 Uiso 1 1 calc R U . . .
H23C H 0.3358 0.4966 0.9730 0.062 Uiso 1 1 calc R U . . .


_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
Nb1 Cl4 2.3096(11) . ?
Nb1 Cl6 2.3270(11) . ?
Nb1 Cl5 2.3284(10) . ?
Nb1 Cl3 2.3598(10) . ?
Nb1 Cl1 2.3676(11) . ?
Nb1 Cl2 2.3814(11) . ?
N1 C2 1.323(4) . ?
N1 C3 1.383(4) . ?
N1 C12 1.475(4) . ?
N2 C1 1.316(4) . ?
N2 C4 1.354(4) . ?
C1 C2 1.406(5) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 C8 1.390(5) . ?
C3 C4 1.427(5) . ?
C4 C5 1.425(5) . ?
C5 C6 1.366(5) . ?
C5 C9 1.521(5) . ?
C6 C7 1.412(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.371(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C11 1.517(5) . ?
C9 C10 1.528(5) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C17 1.386(5) . ?
C12 C13 1.396(5) . ?
C13 C14 1.396(5) . ?
C13 C18 1.520(5) . ?
C14 C15 1.380(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.375(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(5) . ?
C16 H16 0.9500 . ?
C17 C21 1.519(5) . ?
C18 C20 1.520(5) . ?
C18 C19 1.530(5) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.516(5) . ?
C21 C23 1.534(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
Cl4 Nb1 Cl6 92.01(4) . . ?
Cl4 Nb1 Cl5 90.07(4) . . ?
Cl6 Nb1 Cl5 91.71(4) . . ?
Cl4 Nb1 Cl3 87.77(4) . . ?
Cl6 Nb1 Cl3 174.67(4) . . ?
Cl5 Nb1 Cl3 93.61(4) . . ?
Cl4 Nb1 Cl1 174.99(4) . . ?
Cl6 Nb1 Cl1 92.64(4) . . ?
Cl5 Nb1 Cl1 87.94(4) . . ?
Cl3 Nb1 Cl1 87.77(4) . . ?
Cl4 Nb1 Cl2 91.45(4) . . ?
Cl6 Nb1 Cl2 86.78(4) . . ?
Cl5 Nb1 Cl2 177.89(4) . . ?
Cl3 Nb1 Cl2 87.90(4) . . ?
Cl1 Nb1 Cl2 90.65(4) . . ?
C2 N1 C3 121.2(3) . . ?
C2 N1 C12 118.6(3) . . ?
C3 N1 C12 120.2(3) . . ?
C1 N2 C4 118.3(3) . . ?
N2 C1 C2 122.7(3) . . ?
N2 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
N1 C2 C1 119.2(3) . . ?
N1 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
N1 C3 C8 121.1(3) . . ?
N1 C3 C4 116.9(3) . . ?
C8 C3 C4 122.0(3) . . ?
N2 C4 C5 119.3(3) . . ?
N2 C4 C3 121.6(3) . . ?
C5 C4 C3 119.1(3) . . ?
C6 C5 C4 117.3(3) . . ?
C6 C5 C9 121.9(3) . . ?
C4 C5 C9 120.7(3) . . ?
C5 C6 C7 122.7(3) . . ?
C5 C6 H6 118.7 . . ?
C7 C6 H6 118.7 . . ?
C8 C7 C6 121.2(3) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 C3 117.7(3) . . ?
C7 C8 H8 121.2 . . ?
C3 C8 H8 121.2 . . ?
C11 C9 C5 111.1(3) . . ?
C11 C9 C10 111.5(3) . . ?
C5 C9 C10 110.5(3) . . ?
C11 C9 H9 107.8 . . ?
C5 C9 H9 107.8 . . ?
C10 C9 H9 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C17 C12 C13 124.9(3) . . ?
C17 C12 N1 117.6(3) . . ?
C13 C12 N1 117.5(3) . . ?
C12 C13 C14 115.7(3) . . ?
C12 C13 C18 123.4(3) . . ?
C14 C13 C18 121.0(3) . . ?
C15 C14 C13 121.1(3) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C14 121.1(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.5(4) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C12 C17 C16 116.7(3) . . ?
C12 C17 C21 122.1(3) . . ?
C16 C17 C21 121.2(3) . . ?
C20 C18 C13 110.9(3) . . ?
C20 C18 C19 111.7(3) . . ?
C13 C18 C19 111.4(3) . . ?
C20 C18 H18 107.5 . . ?
C13 C18 H18 107.5 . . ?
C19 C18 H18 107.5 . . ?
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 . . ?
C22 C21 C17 112.9(3) . . ?
C22 C21 C23 109.9(3) . . ?
C17 C21 C23 111.1(3) . . ?
C22 C21 H21 107.6 . . ?
C17 C21 H21 107.6 . . ?
C23 C21 H21 107.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_refine_diff_density_max         0.530
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1814760'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-24 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            'C27 H39 Cl8 N2 Nb'
_chemical_formula_weight         768.11

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   16.0202(4)
_cell_length_b                   13.0226(3)
_cell_length_c                   17.8448(4)
_cell_angle_alpha                90
_cell_angle_beta                 113.1630(10)
_cell_angle_gamma                90
_cell_volume                     3422.76(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5364
_cell_measurement_theta_min      2.1915
_cell_measurement_theta_max      28.223

_exptl_crystal_description       prism
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.997
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8568
_exptl_absorpt_correction_T_max  0.9069
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0976 (selected reflections only, before parameter refinement)
 R(int) =  0.0623 (selected reflections only, after parameter refinement)
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36558
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.450
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6047
_reflns_number_gt                4805
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0321P)²+5.2183P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6047
_refine_ls_number_parameters     346
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0903
_refine_ls_wR_factor_gt          0.0836
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Nb1 Nb 0.47550(2) 0.20871(2) 0.20343(2) 0.01679(10) Uani 1 1 d . . . . .
Cl1 Cl 0.48685(6) 0.28733(7) 0.09041(5) 0.0244(2) Uani 1 1 d . . . . .
Cl2 Cl 0.62228(6) 0.14184(7) 0.24495(5) 0.0226(2) Uani 1 1 d . . . . .
Cl3 Cl 0.53728(6) 0.36003(7) 0.27968(5) 0.0233(2) Uani 1 1 d . . . . .
Cl4 Cl 0.32765(6) 0.27685(7) 0.16702(5) 0.0232(2) Uani 1 1 d . . . . .
Cl5 Cl 0.46440(6) 0.13808(7) 0.32199(5) 0.0236(2) Uani 1 1 d . . . . .
Cl6 Cl 0.41556(6) 0.06104(7) 0.12999(6) 0.0293(2) Uani 1 1 d . . . . .
C1 C 0.1760(2) 0.2484(3) 0.9469(2) 0.0181(8) Uani 1 1 d . . . . .
H1 H 0.1356 0.3034 0.9221 0.022 Uiso 1 1 calc R U . . .
C2 C 0.1462(2) 0.1590(3) 0.98055(19) 0.0168(7) Uani 1 1 d . . . . .
H2 H 0.0880 0.1551 0.9826 0.020 Uiso 1 1 calc R U . . .
N1 N 0.2576(2) 0.2496(2) 0.95203(17) 0.0159(6) Uani 1 1 d D . . . .
H1A H 0.286(2) 0.1941(19) 0.9774(19) 0.019 Uiso 1 1 d D U . . .
N2 N 0.20466(19) 0.0872(2) 1.00664(16) 0.0161(6) Uani 1 1 d . . . . .
C3 C 0.3031(2) 0.3222(2) 0.92012(19) 0.0151(7) Uani 1 1 d . . . . .
C4 C 0.3081(2) 0.4260(3) 0.9424(2) 0.0180(8) Uani 1 1 d . . . . .
C5 C 0.3586(2) 0.4880(3) 0.9118(2) 0.0211(8) Uani 1 1 d . . . . .
H5 H 0.3641 0.5592 0.9246 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4007(2) 0.4496(3) 0.8636(2) 0.0242(8) Uani 1 1 d . . . . .
H6 H 0.4349 0.4942 0.8444 0.029 Uiso 1 1 calc R U . . .
C7 C 0.3935(2) 0.3468(3) 0.8430(2) 0.0223(8) Uani 1 1 d . . . . .
H7 H 0.4230 0.3213 0.8099 0.027 Uiso 1 1 calc R U . . .
C8 C 0.3434(2) 0.2798(3) 0.8701(2) 0.0182(7) Uani 1 1 d . . . . .
C9 C 0.2637(2) 0.4713(3) 0.9955(2) 0.0203(8) Uani 1 1 d . . . . .
H9 H 0.2424 0.4130 1.0198 0.024 Uiso 1 1 calc R U . . .
C10 C 0.3304(3) 0.5349(3) 1.0660(2) 0.0258(9) Uani 1 1 d . . . . .
H10A H 0.2989 0.5627 1.0987 0.039 Uiso 1 1 calc R U . . .
H10B H 0.3806 0.4911 1.1002 0.039 Uiso 1 1 calc R U . . .
H10C H 0.3542 0.5915 1.0440 0.039 Uiso 1 1 calc R U . . .
C11 C 0.1799(3) 0.5350(3) 0.9441(2) 0.0252(8) Uani 1 1 d . . . . .
H11A H 0.1521 0.5637 0.9796 0.038 Uiso 1 1 calc R U . . .
H11B H 0.1983 0.5909 0.9172 0.038 Uiso 1 1 calc R U . . .
H11C H 0.1359 0.4908 0.9029 0.038 Uiso 1 1 calc R U . . .
C12 C 0.3322(2) 0.1667(3) 0.8457(2) 0.0207(8) Uani 1 1 d . . . . .
H12 H 0.2809 0.1391 0.8583 0.025 Uiso 1 1 calc R U . . .
C13 C 0.4164(3) 0.1061(3) 0.8958(2) 0.0310(9) Uani 1 1 d . . . . .
H13A H 0.4308 0.1170 0.9539 0.046 Uiso 1 1 calc R U . . .
H13B H 0.4054 0.0329 0.8830 0.046 Uiso 1 1 calc R U . . .
H13C H 0.4674 0.1292 0.8829 0.046 Uiso 1 1 calc R U . . .
C14 C 0.3071(3) 0.1522(3) 0.7548(2) 0.0313(9) Uani 1 1 d . . . . .
H14A H 0.2525 0.1923 0.7241 0.047 Uiso 1 1 calc R U . . .
H14B H 0.3573 0.1756 0.7409 0.047 Uiso 1 1 calc R U . . .
H14C H 0.2953 0.0793 0.7410 0.047 Uiso 1 1 calc R U . . .
C15 C 0.1907(2) -0.0052(3) 1.0416(2) 0.0162(7) Uani 1 1 d . . . . .
C16 C 0.2241(2) -0.0943(3) 1.0171(2) 0.0172(8) Uani 1 1 d . . . . .
C17 C 0.2110(3) -0.1882(3) 1.0478(2) 0.0240(8) Uani 1 1 d . . . . .
H17 H 0.2305 -0.2494 1.0305 0.029 Uiso 1 1 calc R U . . .
C18 C 0.1703(3) -0.1942(3) 1.1028(2) 0.0275(9) Uani 1 1 d . . . . .
H18 H 0.1609 -0.2592 1.1224 0.033 Uiso 1 1 calc R U . . .
C19 C 0.1431(3) -0.1053(3) 1.1295(2) 0.0239(8) Uani 1 1 d . . . . .
H19 H 0.1171 -0.1107 1.1689 0.029 Uiso 1 1 calc R U . . .
C20 C 0.1524(2) -0.0085(3) 1.1007(2) 0.0185(8) Uani 1 1 d . . . . .
C21 C 0.2685(2) -0.0874(3) 0.9560(2) 0.0188(8) Uani 1 1 d . . . . .
H21 H 0.3034 -0.0215 0.9669 0.023 Uiso 1 1 calc R U . . .
C22 C 0.1991(3) -0.0828(3) 0.8688(2) 0.0272(9) Uani 1 1 d . . . . .
H22A H 0.2305 -0.0785 0.8315 0.041 Uiso 1 1 calc R U . . .
H22B H 0.1614 -0.1448 0.8566 0.041 Uiso 1 1 calc R U . . .
H22C H 0.1605 -0.0222 0.8618 0.041 Uiso 1 1 calc R U . . .
C23 C 0.3367(3) -0.1746(3) 0.9652(2) 0.0281(9) Uani 1 1 d . . . . .
H23A H 0.3813 -0.1771 1.0216 0.042 Uiso 1 1 calc R U . . .
H23B H 0.3042 -0.2402 0.9511 0.042 Uiso 1 1 calc R U . . .
H23C H 0.3679 -0.1620 0.9286 0.042 Uiso 1 1 calc R U . . .
C24 C 0.1257(2) 0.0858(3) 1.1361(2) 0.0202(8) Uani 1 1 d . . . . .
H24 H 0.1473 0.1478 1.1159 0.024 Uiso 1 1 calc R U . . .
C25 C 0.0231(3) 0.0933(3) 1.1075(2) 0.0269(9) Uani 1 1 d . . . . .
H25A H 0.0075 0.1547 1.1310 0.040 Uiso 1 1 calc R U . . .
H25B H -0.0044 0.0980 1.0479 0.040 Uiso 1 1 calc R U . . .
H25C H 0.0001 0.0322 1.1251 0.040 Uiso 1 1 calc R U . . .
C26 C 0.1713(3) 0.0855(3) 1.2295(2) 0.0317(9) Uani 1 1 d . . . . .
H26A H 0.1530 0.1470 1.2509 0.048 Uiso 1 1 calc R U . . .
H26B H 0.1526 0.0241 1.2507 0.048 Uiso 1 1 calc R U . . .
H26C H 0.2374 0.0852 1.2467 0.048 Uiso 1 1 calc R U . . .
C101 C 0.3781(3) 0.8818(4) 0.3080(4) 0.0582(15) Uani 1 1 d . . . . .
H10D H 0.3271 0.8325 0.2869 0.070 Uiso 1 1 calc R U . . .
H10E H 0.3548 0.9505 0.2859 0.070 Uiso 1 1 calc R U . . .
Cl7 Cl 0.46221(9) 0.84562(10) 0.27436(9) 0.0592(4) Uani 1 1 d . . . . .
Cl8 Cl 0.41902(11) 0.88542(11) 0.41519(10) 0.0728(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Cl6 2.3125(9) . ?
Nb1 Cl1 2.3319(9) . ?
Nb1 Cl2 2.3380(9) . ?
Nb1 Cl4 2.3684(9) . ?
Nb1 Cl5 2.3769(9) . ?
Nb1 Cl3 2.3779(9) . ?
C1 N1 1.275(4) . ?
C1 C2 1.473(5) . ?
C1 H1 0.9500 . ?
C2 N2 1.274(4) . ?
C2 H2 0.9500 . ?
N1 C3 1.441(4) . ?
N1 H1A 0.881(18) . ?
N2 C15 1.414(4) . ?
C3 C4 1.402(5) . ?
C3 C8 1.404(5) . ?
C4 C5 1.399(5) . ?
C4 C9 1.510(5) . ?
C5 C6 1.379(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.382(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.394(5) . ?
C7 H7 0.9500 . ?
C8 C12 1.525(5) . ?
C9 C10 1.533(5) . ?
C9 C11 1.537(5) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.515(5) . ?
C12 C14 1.522(5) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.414(5) . ?
C15 C16 1.416(5) . ?
C16 C17 1.390(5) . ?
C16 C21 1.520(5) . ?
C17 C18 1.378(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.392(5) . ?
C19 H19 0.9500 . ?
C20 C24 1.518(5) . ?
C21 C22 1.518(5) . ?
C21 C23 1.539(5) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.520(5) . ?
C24 C26 1.536(5) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C101 Cl7 1.742(5) . ?
C101 Cl8 1.762(6) . ?
C101 H10D 0.9900 . ?
C101 H10E 0.9900 . ?

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
Cl6 Nb1 Cl1 91.79(4) . . ?
Cl6 Nb1 Cl2 90.66(3) . . ?
Cl1 Nb1 Cl2 91.53(3) . . ?
Cl6 Nb1 Cl4 90.49(3) . . ?
Cl1 Nb1 Cl4 90.46(3) . . ?
Cl2 Nb1 Cl4 177.67(3) . . ?
Cl6 Nb1 Cl5 91.31(4) . . ?
Cl1 Nb1 Cl5 176.71(3) . . ?
Cl2 Nb1 Cl5 89.53(3) . . ?
Cl4 Nb1 Cl5 88.41(3) . . ?
Cl6 Nb1 Cl3 179.66(4) . . ?
Cl1 Nb1 Cl3 88.54(3) . . ?
Cl2 Nb1 Cl3 89.25(3) . . ?
Cl4 Nb1 Cl3 89.58(3) . . ?
Cl5 Nb1 Cl3 88.36(3) . . ?
N1 C1 C2 117.9(3) . . ?
N1 C1 H1 121.0 . . ?
C2 C1 H1 121.0 . . ?
N2 C2 C1 114.8(3) . . ?
N2 C2 H2 122.6 . . ?
C1 C2 H2 122.6 . . ?
C1 N1 C3 130.1(3) . . ?
C1 N1 H1A 110(2) . . ?
C3 N1 H1A 120(2) . . ?
C2 N2 C15 124.4(3) . . ?
C4 C3 C8 124.8(3) . . ?
C4 C3 N1 120.1(3) . . ?
C8 C3 N1 115.1(3) . . ?
C5 C4 C3 115.0(3) . . ?
C5 C4 C9 120.5(3) . . ?
C3 C4 C9 124.5(3) . . ?
C6 C5 C4 122.3(3) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 120.9(3) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C3 116.5(3) . . ?
C7 C8 C12 121.6(3) . . ?
C3 C8 C12 121.9(3) . . ?
C4 C9 C10 112.2(3) . . ?
C4 C9 C11 110.7(3) . . ?
C10 C9 C11 111.2(3) . . ?
C4 C9 H9 107.5 . . ?
C10 C9 H9 107.5 . . ?
C11 C9 H9 107.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 111.4(3) . . ?
C13 C12 C8 111.0(3) . . ?
C14 C12 C8 112.1(3) . . ?
C13 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C8 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 N2 123.0(3) . . ?
C20 C15 C16 122.2(3) . . ?
N2 C15 C16 114.6(3) . . ?
C17 C16 C15 117.7(3) . . ?
C17 C16 C21 121.3(3) . . ?
C15 C16 C21 120.9(3) . . ?
C18 C17 C16 121.2(3) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C20 122.4(3) . . ?
C18 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
C19 C20 C15 116.4(3) . . ?
C19 C20 C24 119.4(3) . . ?
C15 C20 C24 124.2(3) . . ?
C22 C21 C16 112.2(3) . . ?
C22 C21 C23 109.9(3) . . ?
C16 C21 C23 113.2(3) . . ?
C22 C21 H21 107.1 . . ?
C16 C21 H21 107.1 . . ?
C23 C21 H21 107.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 C25 110.9(3) . . ?
C20 C24 C26 111.0(3) . . ?
C25 C24 C26 110.7(3) . . ?
C20 C24 H24 108.0 . . ?
C25 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Cl7 C101 Cl8 111.9(3) . . ?
Cl7 C101 H10D 109.2 . . ?
Cl8 C101 H10D 109.2 . . ?
Cl7 C101 H10E 109.2 . . ?
Cl8 C101 H10E 109.2 . . ?
H10D C101 H10E 107.9 . . ?

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
N1 C1 C2 N2 -4.9(4) . . . . ?
C2 C1 N1 C3 175.3(3) . . . . ?
C1 C2 N2 C15 179.8(3) . . . . ?
C1 N1 C3 C4 58.2(5) . . . . ?
C1 N1 C3 C8 -124.4(4) . . . . ?
C8 C3 C4 C5 -0.9(5) . . . . ?
N1 C3 C4 C5 176.2(3) . . . . ?
C8 C3 C4 C9 179.3(3) . . . . ?
N1 C3 C4 C9 -3.6(5) . . . . ?
C3 C4 C5 C6 -0.3(5) . . . . ?
C9 C4 C5 C6 179.5(3) . . . . ?
C4 C5 C6 C7 0.6(6) . . . . ?
C5 C6 C7 C8 0.3(6) . . . . ?
C6 C7 C8 C3 -1.3(5) . . . . ?
C6 C7 C8 C12 178.0(3) . . . . ?
C4 C3 C8 C7 1.7(5) . . . . ?
N1 C3 C8 C7 -175.6(3) . . . . ?
C4 C3 C8 C12 -177.7(3) . . . . ?
N1 C3 C8 C12 5.1(5) . . . . ?
C5 C4 C9 C10 -50.6(4) . . . . ?
C3 C4 C9 C10 129.2(4) . . . . ?
C5 C4 C9 C11 74.2(4) . . . . ?
C3 C4 C9 C11 -106.0(4) . . . . ?
C7 C8 C12 C13 78.6(4) . . . . ?
C3 C8 C12 C13 -102.1(4) . . . . ?
C7 C8 C12 C14 -46.6(5) . . . . ?
C3 C8 C12 C14 132.7(3) . . . . ?
C2 N2 C15 C20 -45.5(5) . . . . ?
C2 N2 C15 C16 138.9(3) . . . . ?
C20 C15 C16 C17 5.7(5) . . . . ?
N2 C15 C16 C17 -178.7(3) . . . . ?
C20 C15 C16 C21 -177.4(3) . . . . ?
N2 C15 C16 C21 -1.7(4) . . . . ?
C15 C16 C17 C18 -2.7(5) . . . . ?
C21 C16 C17 C18 -179.6(3) . . . . ?
C16 C17 C18 C19 -1.1(6) . . . . ?
C17 C18 C19 C20 2.2(6) . . . . ?
C18 C19 C20 C15 0.6(5) . . . . ?
C18 C19 C20 C24 -176.8(3) . . . . ?
N2 C15 C20 C19 -179.9(3) . . . . ?
C16 C15 C20 C19 -4.6(5) . . . . ?
N2 C15 C20 C24 -2.6(5) . . . . ?
C16 C15 C20 C24 172.7(3) . . . . ?
C17 C16 C21 C22 95.8(4) . . . . ?
C15 C16 C21 C22 -81.1(4) . . . . ?
C17 C16 C21 C23 -29.3(5) . . . . ?
C15 C16 C21 C23 153.8(3) . . . . ?
C19 C20 C24 C25 -71.9(4) . . . . ?
C15 C20 C24 C25 110.9(4) . . . . ?
C19 C20 C24 C26 51.6(4) . . . . ?
C15 C20 C24 C26 -125.5(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A N2 0.881(18) 2.11(3) 2.606(4) 115(3) .

_refine_diff_density_max         0.717
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_7a
_database_code_depnum_ccdc_archive 'CCDC 1814758'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-24 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            'C26 H36 Br10 N2 Nb2'
_chemical_formula_weight         1361.49

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   10.805(4)
_cell_length_b                   13.497(4)
_cell_length_c                   13.691(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.104(4)
_cell_angle_gamma                90
_cell_volume                     1886.7(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7462
_cell_measurement_theta_min      2.501
_cell_measurement_theta_max      25.6135

_exptl_crystal_description       prism
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_F_000             1276
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    11.217
_shelx_estimated_absorpt_T_min   0.192
_shelx_estimated_absorpt_T_max   0.346
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1916
_exptl_absorpt_correction_T_max  0.3463
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1793 (selected reflections only, before parameter refinement)
 R(int) =  0.0857 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15974
_diffrn_reflns_av_unetI/netI     0.1618
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.574
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6558
_reflns_number_gt                4541
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1162P)²+42.5467P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6558
_refine_ls_number_parameters     338
_refine_ls_number_restraints     465
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2441
_refine_ls_wR_factor_gt          0.2153
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.015
_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
Nb1 Nb 0.1816(3) 0.7843(2) 0.1772(2) 0.0130(6) Uani 1 1 d . . . . .
Br1 Br 0.0499(6) 0.7394(4) 0.2842(4) 0.0573(15) Uani 1 1 d . . . . .
Br2 Br 0.3173(4) 0.8902(3) 0.3277(3) 0.0280(9) Uani 1 1 d . . . . .
Br3 Br 0.3260(5) 0.6439(4) 0.2384(5) 0.0562(15) Uani 1 1 d . . . . .
Br4 Br 0.0434(4) 0.6870(3) 0.0302(4) 0.0322(10) Uani 1 1 d . . . . .
Br5 Br 0.0307(3) 0.9312(2) 0.1058(3) 0.0241(9) Uani 1 1 d . . . . .
Br6 Br 0.3283(4) 0.8425(3) 0.0854(4) 0.0487(13) Uani 1 1 d . . . . .
Nb2 Nb 0.5513(2) 0.7796(2) 0.6793(2) 0.0098(6) Uani 1 1 d . U . . .
Br7 Br 0.4597(5) 0.6773(4) 0.5312(4) 0.0509(13) Uani 1 1 d . U . . .
Br8 Br 0.6684(6) 0.8569(4) 0.8395(5) 0.0605(15) Uani 1 1 d . U . . .
Br9 Br 0.5881(4) 0.9136(3) 0.5783(3) 0.0276(9) Uani 1 1 d . U . . .
Br10 Br 0.3473(4) 0.8127(3) 0.7019(4) 0.0454(13) Uani 1 1 d . U . . .
C1 C 0.684(3) 0.592(2) 0.795(3) 0.009(4) Uani 1 1 d . U . . .
H1 H 0.7065 0.5375 0.8409 0.011 Uiso 1 1 calc R U . . .
C2 C 0.770(3) 0.624(2) 0.741(3) 0.008(4) Uani 1 1 d . U . . .
H2 H 0.8447 0.5861 0.7441 0.009 Uiso 1 1 calc R U . . .
C3 C 0.4926(17) 0.6076(16) 0.8374(14) 0.014(4) Uani 1 1 d G U . . .
C4 C 0.3745(18) 0.5594(16) 0.7900(11) 0.017(4) Uani 1 1 d DG U . . .
C5 C 0.2911(15) 0.5382(16) 0.8460(15) 0.020(5) Uani 1 1 d G U . . .
H5 H 0.2104 0.5052 0.8136 0.024 Uiso 1 1 calc R U . . .
C6 C 0.3259(18) 0.5653(17) 0.9494(15) 0.020(5) Uani 1 1 d G U . . .
H6 H 0.2689 0.5509 0.9877 0.024 Uiso 1 1 calc R U . . .
C7 C 0.4440(18) 0.6136(16) 0.9969(11) 0.019(5) Uani 1 1 d G U . . .
H7 H 0.4678 0.6321 1.0676 0.022 Uiso 1 1 calc R U . . .
C8 C 0.5273(14) 0.6347(15) 0.9409(14) 0.014(4) Uani 1 1 d DG U . . .
C9 C 0.341(3) 0.5172(19) 0.680(2) 0.023(5) Uani 1 1 d D U . . .
H9 H 0.4117 0.5363 0.6516 0.028 Uiso 1 1 calc R U . . .
C10 C 0.335(3) 0.402(2) 0.685(3) 0.023(7) Uani 1 1 d D U . . .
H10A H 0.4190 0.3771 0.7312 0.035 Uiso 1 1 calc R U . . .
H10B H 0.2645 0.3821 0.7101 0.035 Uiso 1 1 calc R U . . .
H10C H 0.3197 0.3748 0.6152 0.035 Uiso 1 1 calc R U . . .
C11 C 0.210(3) 0.557(3) 0.607(3) 0.040(9) Uani 1 1 d D U . . .
H11A H 0.1927 0.5282 0.5378 0.059 Uiso 1 1 calc R U . . .
H11B H 0.1392 0.5389 0.6333 0.059 Uiso 1 1 calc R U . . .
H11C H 0.2146 0.6293 0.6023 0.059 Uiso 1 1 calc R U . . .
C12 C 0.666(2) 0.6712(17) 1.007(2) 0.013(5) Uani 1 1 d D U . . .
H12 H 0.7125 0.6917 0.9586 0.016 Uiso 1 1 calc R U . . .
C13 C 0.661(3) 0.762(2) 1.074(2) 0.017(6) Uani 1 1 d D U . . .
H13A H 0.6074 0.8144 1.0301 0.025 Uiso 1 1 calc R U . . .
H13B H 0.6214 0.7434 1.1267 0.025 Uiso 1 1 calc R U . . .
H13C H 0.7495 0.7872 1.1081 0.025 Uiso 1 1 calc R U . . .
C14 C 0.749(3) 0.592(2) 1.079(3) 0.026(7) Uani 1 1 d D U . . .
H14A H 0.7543 0.5328 1.0386 0.039 Uiso 1 1 calc R U . . .
H14B H 0.8379 0.6175 1.1130 0.039 Uiso 1 1 calc R U . . .
H14C H 0.7098 0.5738 1.1316 0.039 Uiso 1 1 calc R U . . .
C15 C 0.8337(18) 0.7300(13) 0.6314(14) 0.011(4) Uani 1 1 d G U . . .
C16 C 0.9187(19) 0.8093(13) 0.6667(12) 0.014(4) Uani 1 1 d DG U . . .
C17 C 0.9933(17) 0.8439(12) 0.6082(15) 0.015(5) Uani 1 1 d G U . . .
H17 H 1.0514 0.8981 0.6323 0.019 Uiso 1 1 calc R U . . .
C18 C 0.9830(18) 0.7992(14) 0.5144(15) 0.017(5) Uani 1 1 d G U . . .
H18 H 1.0340 0.8228 0.4744 0.020 Uiso 1 1 calc R U . . .
C19 C 0.8980(19) 0.7199(13) 0.4791(12) 0.015(4) Uani 1 1 d G U . . .
H19 H 0.8910 0.6893 0.4150 0.018 Uiso 1 1 calc R U . . .
C20 C 0.8234(17) 0.6853(12) 0.5376(15) 0.012(4) Uani 1 1 d DG U . . .
C21 C 0.740(2) 0.5928(17) 0.497(2) 0.017(5) Uani 1 1 d D U . . .
H21 H 0.6818 0.5813 0.5401 0.020 Uiso 1 1 calc R U . . .
C22 C 0.836(3) 0.505(2) 0.513(3) 0.017(6) Uani 1 1 d D U . . .
H22A H 0.7873 0.4440 0.4881 0.025 Uiso 1 1 calc R U . . .
H22B H 0.8964 0.5174 0.4738 0.025 Uiso 1 1 calc R U . . .
H22C H 0.8866 0.4986 0.5865 0.025 Uiso 1 1 calc R U . . .
C23 C 0.654(3) 0.604(3) 0.383(2) 0.025(7) Uani 1 1 d D U . . .
H23A H 0.6019 0.5434 0.3601 0.038 Uiso 1 1 calc R U . . .
H23B H 0.5946 0.6605 0.3756 0.038 Uiso 1 1 calc R U . . .
H23C H 0.7097 0.6145 0.3402 0.038 Uiso 1 1 calc R U . . .
C24 C 0.952(2) 0.8532(19) 0.777(2) 0.018(5) Uani 1 1 d D U . . .
H24 H 0.8976 0.8184 0.8133 0.021 Uiso 1 1 calc R U . . .
C25 C 1.098(2) 0.833(3) 0.838(3) 0.022(7) Uani 1 1 d D U . . .
H25A H 1.1192 0.8608 0.9082 0.033 Uiso 1 1 calc R U . . .
H25B H 1.1139 0.7617 0.8428 0.033 Uiso 1 1 calc R U . . .
H25C H 1.1530 0.8647 0.8028 0.033 Uiso 1 1 calc R U . . .
C26 C 0.925(4) 0.967(2) 0.779(3) 0.031(8) Uani 1 1 d D U . . .
H26A H 0.8330 0.9798 0.7401 0.047 Uiso 1 1 calc R U . . .
H26B H 0.9451 0.9891 0.8502 0.047 Uiso 1 1 calc R U . . .
H26C H 0.9808 1.0023 0.7463 0.047 Uiso 1 1 calc R U . . .
N1 N 0.576(2) 0.6379(19) 0.779(2) 0.012(3) Uani 1 1 d . U . . .
N2 N 0.746(2) 0.7027(18) 0.690(2) 0.013(3) Uani 1 1 d . U . . .


_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
Nb1 Br3 2.423(6) . ?
Nb1 Br1 2.428(6) . ?
Nb1 Br6 2.452(6) . ?
Nb1 Br4 2.457(5) . ?
Nb1 Br2 2.542(5) . ?
Nb1 Br5 2.551(4) . ?
Nb2 N2 2.31(2) . ?
Nb2 N1 2.31(3) . ?
Nb2 Br10 2.367(5) . ?
Nb2 Br7 2.384(6) . ?
Nb2 Br8 2.384(7) . ?
Nb2 Br9 2.388(4) . ?
C1 N1 1.28(4) . ?
C1 C2 1.43(4) . ?
C1 H1 0.9500 . ?
C2 N2 1.25(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 N1 1.44(3) . ?
C4 C5 1.3900 . ?
C4 C9 1.54(2) . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 C8 1.3900 . ?
C7 H7 0.9500 . ?
C8 C12 1.55(2) . ?
C9 C11 1.54(2) . ?
C9 C10 1.56(2) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.54(2) . ?
C12 C13 1.55(2) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C15 N2 1.48(3) . ?
C16 C17 1.3900 . ?
C16 C24 1.56(2) . ?
C17 C18 1.3900 . ?
C17 H17 0.9500 . ?
C18 C19 1.3900 . ?
C18 H18 0.9500 . ?
C19 C20 1.3900 . ?
C19 H19 0.9500 . ?
C20 C21 1.53(2) . ?
C21 C22 1.55(2) . ?
C21 C23 1.55(2) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.54(2) . ?
C24 C26 1.56(2) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

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
Br3 Nb1 Br1 92.0(2) . . ?
Br3 Nb1 Br6 88.66(19) . . ?
Br1 Nb1 Br6 173.4(2) . . ?
Br3 Nb1 Br4 90.88(19) . . ?
Br1 Nb1 Br4 92.40(19) . . ?
Br6 Nb1 Br4 94.16(19) . . ?
Br3 Nb1 Br2 91.38(19) . . ?
Br1 Nb1 Br2 87.02(18) . . ?
Br6 Nb1 Br2 86.40(17) . . ?
Br4 Nb1 Br2 177.68(18) . . ?
Br3 Nb1 Br5 177.8(2) . . ?
Br1 Nb1 Br5 89.87(19) . . ?
Br6 Nb1 Br5 89.65(17) . . ?
Br4 Nb1 Br5 87.76(16) . . ?
Br2 Nb1 Br5 89.99(15) . . ?
N2 Nb2 N1 70.5(8) . . ?
N2 Nb2 Br10 161.0(6) . . ?
N1 Nb2 Br10 90.6(6) . . ?
N2 Nb2 Br7 84.8(7) . . ?
N1 Nb2 Br7 87.6(7) . . ?
Br10 Nb2 Br7 94.3(2) . . ?
N2 Nb2 Br8 86.6(7) . . ?
N1 Nb2 Br8 84.0(7) . . ?
Br10 Nb2 Br8 91.9(2) . . ?
Br7 Nb2 Br8 169.6(2) . . ?
N2 Nb2 Br9 93.2(6) . . ?
N1 Nb2 Br9 163.6(6) . . ?
Br10 Nb2 Br9 105.74(17) . . ?
Br7 Nb2 Br9 92.73(19) . . ?
Br8 Nb2 Br9 93.56(19) . . ?
N1 C1 C2 119(3) . . ?
N1 C1 H1 120.7 . . ?
C2 C1 H1 120.7 . . ?
N2 C2 C1 120(3) . . ?
N2 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C8 120.0 . . ?
C4 C3 N1 121.0(16) . . ?
C8 C3 N1 118.8(16) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C9 118.4(16) . . ?
C3 C4 C9 121.2(16) . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 C12 114.5(16) . . ?
C3 C8 C12 124.6(16) . . ?
C11 C9 C4 112(3) . . ?
C11 C9 C10 110(3) . . ?
C4 C9 C10 109(2) . . ?
C11 C9 H9 108.5 . . ?
C4 C9 H9 108.5 . . ?
C10 C9 H9 108.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 108(3) . . ?
C14 C12 C8 114(2) . . ?
C13 C12 C8 113(2) . . ?
C14 C12 H12 107.4 . . ?
C13 C12 H12 107.4 . . ?
C8 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 120.0 . . ?
C16 C15 N2 118.2(16) . . ?
C20 C15 N2 121.4(16) . . ?
C15 C16 C17 120.0 . . ?
C15 C16 C24 123.3(16) . . ?
C17 C16 C24 116.1(16) . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C15 120.0 . . ?
C19 C20 C21 116.8(16) . . ?
C15 C20 C21 123.1(16) . . ?
C20 C21 C22 106(2) . . ?
C20 C21 C23 112(2) . . ?
C22 C21 C23 112(3) . . ?
C20 C21 H21 108.9 . . ?
C22 C21 H21 108.9 . . ?
C23 C21 H21 108.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C16 109(2) . . ?
C25 C24 C26 109(3) . . ?
C16 C24 C26 113(2) . . ?
C25 C24 H24 108.3 . . ?
C16 C24 H24 108.3 . . ?
C26 C24 H24 108.3 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C1 N1 C3 118(3) . . ?
C1 N1 Nb2 114.9(19) . . ?
C3 N1 Nb2 126.2(17) . . ?
C2 N2 C15 118(2) . . ?
C2 N2 Nb2 116(2) . . ?
C15 N2 Nb2 126.0(17) . . ?

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
N1 C1 C2 N2 8(5) . . . . ?
C8 C3 C4 C5 0.0 . . . . ?
N1 C3 C4 C5 -175(2) . . . . ?
C8 C3 C4 C9 -173(2) . . . . ?
N1 C3 C4 C9 13(2) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C9 C4 C5 C6 173(2) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 C3 0.0 . . . . ?
C6 C7 C8 C12 -169.5(19) . . . . ?
C4 C3 C8 C7 0.0 . . . . ?
N1 C3 C8 C7 175(2) . . . . ?
C4 C3 C8 C12 168(2) . . . . ?
N1 C3 C8 C12 -17(2) . . . . ?
C5 C4 C9 C11 63(3) . . . . ?
C3 C4 C9 C11 -125(3) . . . . ?
C5 C4 C9 C10 -59(3) . . . . ?
C3 C4 C9 C10 113(2) . . . . ?
C7 C8 C12 C14 68(3) . . . . ?
C3 C8 C12 C14 -101(3) . . . . ?
C7 C8 C12 C13 -55(3) . . . . ?
C3 C8 C12 C13 136(2) . . . . ?
C20 C15 C16 C17 0.0 . . . . ?
N2 C15 C16 C17 -173(2) . . . . ?
C20 C15 C16 C24 -170(2) . . . . ?
N2 C15 C16 C24 16(2) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C24 C16 C17 C18 171.0(19) . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 C15 0.0 . . . . ?
C18 C19 C20 C21 -175.6(19) . . . . ?
C16 C15 C20 C19 0.0 . . . . ?
N2 C15 C20 C19 173(2) . . . . ?
C16 C15 C20 C21 175(2) . . . . ?
N2 C15 C20 C21 -11(2) . . . . ?
C19 C20 C21 C22 71(3) . . . . ?
C15 C20 C21 C22 -105(2) . . . . ?
C19 C20 C21 C23 -52(3) . . . . ?
C15 C20 C21 C23 133(2) . . . . ?
C15 C16 C24 C25 113(2) . . . . ?
C17 C16 C24 C25 -57(3) . . . . ?
C15 C16 C24 C26 -125(2) . . . . ?
C17 C16 C24 C26 65(3) . . . . ?
C2 C1 N1 C3 -177(2) . . . . ?
C2 C1 N1 Nb2 -7(4) . . . . ?
C4 C3 N1 C1 -110(3) . . . . ?
C8 C3 N1 C1 75(3) . . . . ?
C4 C3 N1 Nb2 82(2) . . . . ?
C8 C3 N1 Nb2 -93(2) . . . . ?
C1 C2 N2 C15 -177(3) . . . . ?
C1 C2 N2 Nb2 -5(4) . . . . ?
C16 C15 N2 C2 -108(3) . . . . ?
C20 C15 N2 C2 78(3) . . . . ?
C16 C15 N2 Nb2 80(2) . . . . ?
C20 C15 N2 Nb2 -93(2) . . . . ?

_refine_diff_density_max         2.690
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.375

####################################################################### 
# 
# 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_4b
_database_code_depnum_ccdc_archive 'CCDC 1814759'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-24 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            'C27 H39 Cl8 N2 Ta'
_chemical_formula_weight         856.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   16.105(7)
_cell_length_b                   13.078(5)
_cell_length_c                   17.933(8)
_cell_angle_alpha                90
_cell_angle_beta                 113.164(5)
_cell_angle_gamma                90
_cell_volume                     3473(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9188
_cell_measurement_theta_min      2.4705
_cell_measurement_theta_max      26.265

_exptl_crystal_description       prism
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    3.801
_shelx_estimated_absorpt_T_min   0.599
_shelx_estimated_absorpt_T_max   0.680
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5994
_exptl_absorpt_correction_T_max  0.6799
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1412 (selected reflections only, before parameter refinement)
 R(int) =  0.0785 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28556
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.442
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6772
_reflns_number_gt                4885
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0462P)²+12.8044P] 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         6772
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6768(6) 0.7495(6) 0.4476(4) 0.0246(17) Uani 1 1 d . . . . .
H1 H 0.6370 0.8047 0.4232 0.029 Uiso 1 1 calc R U . . .
C2 C 0.6462(5) 0.6591(5) 0.4811(4) 0.0211(16) Uani 1 1 d . . . . .
H2 H 0.5881 0.6547 0.4830 0.025 Uiso 1 1 calc R U . . .
C3 C 0.8031(5) 0.8227(5) 0.4202(4) 0.0223(16) Uani 1 1 d . . . . .
C4 C 0.8439(5) 0.7805(5) 0.3708(4) 0.0210(15) Uani 1 1 d . . . . .
C5 C 0.8940(5) 0.8470(6) 0.3429(5) 0.0271(17) Uani 1 1 d . . . . .
H5 H 0.9236 0.8215 0.3103 0.033 Uiso 1 1 calc R U . . .
C6 C 0.9001(6) 0.9509(6) 0.3634(5) 0.0292(18) Uani 1 1 d . . . . .
H6 H 0.9333 0.9958 0.3436 0.035 Uiso 1 1 calc R U . . .
C7 C 0.8583(5) 0.9893(5) 0.4123(4) 0.0249(16) Uani 1 1 d . . . . .
H7 H 0.8638 1.0600 0.4255 0.030 Uiso 1 1 calc R U . . .
C8 C 0.8086(5) 0.9266(5) 0.4423(4) 0.0224(16) Uani 1 1 d . . . . .
C9 C 0.8309(5) 0.6688(6) 0.3454(4) 0.0245(16) Uani 1 1 d . . . . .
H9 H 0.7796 0.6419 0.3578 0.029 Uiso 1 1 calc R U . . .
C10 C 0.8065(6) 0.6530(6) 0.2543(5) 0.035(2) Uani 1 1 d . . . . .
H10A H 0.7990 0.5798 0.2417 0.053 Uiso 1 1 calc R U . . .
H10B H 0.7499 0.6888 0.2232 0.053 Uiso 1 1 calc R U . . .
H10C H 0.8549 0.6802 0.2400 0.053 Uiso 1 1 calc R U . . .
C11 C 0.9155(6) 0.6063(6) 0.3958(5) 0.036(2) Uani 1 1 d . . . . .
H11A H 0.9061 0.5345 0.3788 0.054 Uiso 1 1 calc R U . . .
H11B H 0.9678 0.6333 0.3873 0.054 Uiso 1 1 calc R U . . .
H11C H 0.9264 0.6112 0.4535 0.054 Uiso 1 1 calc R U . . .
C12 C 0.7642(5) 0.9717(5) 0.4955(4) 0.0243(16) Uani 1 1 d . . . . .
H12 H 0.7430 0.9136 0.5198 0.029 Uiso 1 1 calc R U . . .
C13 C 0.8313(6) 1.0360(6) 0.5660(5) 0.0309(19) Uani 1 1 d . . . . .
H13A H 0.8002 1.0637 0.5988 0.046 Uiso 1 1 calc R U . . .
H13B H 0.8816 0.9926 0.6000 0.046 Uiso 1 1 calc R U . . .
H13C H 0.8546 1.0924 0.5439 0.046 Uiso 1 1 calc R U . . .
C14 C 0.6812(5) 1.0354(6) 0.4450(5) 0.0301(18) Uani 1 1 d . . . . .
H14A H 0.6537 1.0637 0.4805 0.045 Uiso 1 1 calc R U . . .
H14B H 0.6996 1.0914 0.4185 0.045 Uiso 1 1 calc R U . . .
H14C H 0.6373 0.9919 0.4037 0.045 Uiso 1 1 calc R U . . .
C15 C 0.6912(5) 0.4954(5) 0.5415(4) 0.0199(15) Uani 1 1 d . . . . .
C16 C 0.7241(5) 0.4060(5) 0.5165(4) 0.0218(16) Uani 1 1 d . . . . .
C17 C 0.7112(6) 0.3125(6) 0.5480(5) 0.0284(18) Uani 1 1 d . . . . .
H17 H 0.7305 0.2514 0.5309 0.034 Uiso 1 1 calc R U . . .
C18 C 0.6712(6) 0.3062(6) 0.6031(5) 0.0306(18) Uani 1 1 d . . . . .
H18 H 0.6628 0.2414 0.6231 0.037 Uiso 1 1 calc R U . . .
C19 C 0.6435(5) 0.3937(6) 0.6294(5) 0.0276(17) Uani 1 1 d . . . . .
H19 H 0.6170 0.3882 0.6682 0.033 Uiso 1 1 calc R U . . .
C20 C 0.6533(5) 0.4917(5) 0.6003(4) 0.0215(15) Uani 1 1 d . . . . .
C21 C 0.7682(5) 0.4132(5) 0.4555(5) 0.0247(16) Uani 1 1 d . . . . .
H21 H 0.8025 0.4790 0.4662 0.030 Uiso 1 1 calc R U . . .
C22 C 0.8361(6) 0.3269(6) 0.4655(5) 0.0313(18) Uani 1 1 d . . . . .
H22A H 0.8804 0.3253 0.5217 0.047 Uiso 1 1 calc R U . . .
H22B H 0.8041 0.2614 0.4520 0.047 Uiso 1 1 calc R U . . .
H22C H 0.8672 0.3390 0.4291 0.047 Uiso 1 1 calc R U . . .
C23 C 0.6990(6) 0.4171(6) 0.3688(5) 0.0314(18) Uani 1 1 d . . . . .
H23A H 0.7301 0.4217 0.3317 0.047 Uiso 1 1 calc R U . . .
H23B H 0.6620 0.3550 0.3570 0.047 Uiso 1 1 calc R U . . .
H23C H 0.6602 0.4771 0.3617 0.047 Uiso 1 1 calc R U . . .
C24 C 0.6257(5) 0.5852(5) 0.6350(4) 0.0248(17) Uani 1 1 d . . . . .
H24 H 0.6473 0.6470 0.6151 0.030 Uiso 1 1 calc R U . . .
C25 C 0.6714(7) 0.5849(6) 0.7295(5) 0.038(2) Uani 1 1 d . . . . .
H25A H 0.6527 0.6458 0.7507 0.056 Uiso 1 1 calc R U . . .
H25B H 0.6531 0.5235 0.7504 0.056 Uiso 1 1 calc R U . . .
H25C H 0.7372 0.5852 0.7468 0.056 Uiso 1 1 calc R U . . .
C26 C 0.5230(5) 0.5935(6) 0.6067(5) 0.0307(18) Uani 1 1 d . . . . .
H26A H 0.5080 0.6547 0.6303 0.046 Uiso 1 1 calc R U . . .
H26B H 0.4955 0.5984 0.5474 0.046 Uiso 1 1 calc R U . . .
H26C H 0.4999 0.5328 0.6242 0.046 Uiso 1 1 calc R U . . .
C101 C 0.3784(7) 0.1180(8) 0.3068(7) 0.061(3) Uani 1 1 d . . . . .
H10D H 0.3558 0.0496 0.2843 0.074 Uiso 1 1 calc R U . . .
H10E H 0.3275 0.1668 0.2853 0.074 Uiso 1 1 calc R U . . .
Cl1 Cl 0.37808(12) 0.14222(14) 0.75492(11) 0.0260(4) Uani 1 1 d . . . . .
Cl2 Cl 0.51343(13) 0.28648(14) 0.90933(10) 0.0278(4) Uani 1 1 d . . . . .
Cl3 Cl 0.58457(14) 0.06089(14) 0.86901(12) 0.0328(4) Uani 1 1 d . . . . .
Cl4 Cl 0.53542(13) 0.13815(14) 0.67745(11) 0.0282(4) Uani 1 1 d . . . . .
Cl5 Cl 0.46304(13) 0.35997(13) 0.72045(11) 0.0264(4) Uani 1 1 d . . . . .
Cl6 Cl 0.67173(13) 0.27678(14) 0.83210(11) 0.0265(4) Uani 1 1 d . . . . .
Cl7 Cl 0.4175(2) 0.1136(2) 0.4138(2) 0.0806(10) Uani 1 1 d . . . . .
Cl8 Cl 0.4634(2) 0.1552(2) 0.2750(2) 0.0672(8) Uani 1 1 d . . . . .
N1 N 0.7581(4) 0.7501(4) 0.4527(3) 0.0189(13) Uani 1 1 d . . . . .
H1A H 0.7917 0.6988 0.4799 0.023 Uiso 1 1 calc R U . . .
N2 N 0.7048(4) 0.5889(4) 0.5068(3) 0.0189(13) Uani 1 1 d . . . . .
Ta1 Ta 0.52453(2) 0.20875(2) 0.79579(2) 0.02041(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.275(10) . ?
C1 C2 1.496(10) . ?
C1 H1 0.9500 . ?
C2 N2 1.267(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.407(10) . ?
C3 C8 1.408(10) . ?
C3 N1 1.448(9) . ?
C4 C5 1.405(10) . ?
C4 C9 1.520(10) . ?
C5 C6 1.401(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.393(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.394(10) . ?
C7 H7 0.9500 . ?
C8 C12 1.518(10) . ?
C9 C10 1.537(10) . ?
C9 C11 1.540(11) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.533(11) . ?
C12 C13 1.549(11) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.411(9) . ?
C15 C16 1.426(10) . ?
C15 N2 1.428(8) . ?
C16 C17 1.397(10) . ?
C16 C21 1.524(9) . ?
C17 C18 1.378(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.378(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.416(10) . ?
C19 H19 0.9500 . ?
C20 C24 1.515(10) . ?
C21 C23 1.516(11) . ?
C21 C22 1.532(10) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.531(11) . ?
C24 C25 1.560(11) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C101 Cl8 1.745(11) . ?
C101 Cl7 1.771(12) . ?
C101 H10D 0.9900 . ?
C101 H10E 0.9900 . ?
Cl1 Ta1 2.345(2) . ?
Cl2 Ta1 2.3446(19) . ?
Cl3 Ta1 2.324(2) . ?
Cl4 Ta1 2.3832(19) . ?
Cl5 Ta1 2.3801(19) . ?
Cl6 Ta1 2.371(2) . ?
N1 H1A 0.8800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 117.9(7) . . ?
N1 C1 H1 121.1 . . ?
C2 C1 H1 121.1 . . ?
N2 C2 C1 113.7(7) . . ?
N2 C2 H2 123.2 . . ?
C1 C2 H2 123.2 . . ?
C4 C3 C8 124.2(6) . . ?
C4 C3 N1 115.3(6) . . ?
C8 C3 N1 120.4(6) . . ?
C5 C4 C3 117.2(6) . . ?
C5 C4 C9 121.3(6) . . ?
C3 C4 C9 121.5(6) . . ?
C6 C5 C4 119.9(7) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C5 120.8(7) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 121.7(7) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C3 116.2(6) . . ?
C7 C8 C12 119.9(6) . . ?
C3 C8 C12 124.0(6) . . ?
C4 C9 C10 113.3(6) . . ?
C4 C9 C11 110.4(6) . . ?
C10 C9 C11 110.5(6) . . ?
C4 C9 H9 107.5 . . ?
C10 C9 H9 107.5 . . ?
C11 C9 H9 107.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 C14 110.9(6) . . ?
C8 C12 C13 111.9(6) . . ?
C14 C12 C13 110.7(6) . . ?
C8 C12 H12 107.7 . . ?
C14 C12 H12 107.7 . . ?
C13 C12 H12 107.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 122.0(6) . . ?
C20 C15 N2 122.7(6) . . ?
C16 C15 N2 115.1(6) . . ?
C17 C16 C15 117.3(6) . . ?
C17 C16 C21 122.0(6) . . ?
C15 C16 C21 120.7(6) . . ?
C18 C17 C16 121.8(7) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C19 C18 C17 120.2(7) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 121.8(7) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 . . ?
C15 C20 C19 116.8(6) . . ?
C15 C20 C24 124.2(6) . . ?
C19 C20 C24 119.0(6) . . ?
C23 C21 C16 112.1(6) . . ?
C23 C21 C22 110.3(6) . . ?
C16 C21 C22 112.6(6) . . ?
C23 C21 H21 107.2 . . ?
C16 C21 H21 107.2 . . ?
C22 C21 H21 107.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 C26 112.0(6) . . ?
C20 C24 C25 110.7(6) . . ?
C26 C24 C25 110.3(6) . . ?
C20 C24 H24 107.9 . . ?
C26 C24 H24 107.9 . . ?
C25 C24 H24 107.9 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Cl8 C101 Cl7 111.9(6) . . ?
Cl8 C101 H10D 109.2 . . ?
Cl7 C101 H10D 109.2 . . ?
Cl8 C101 H10E 109.2 . . ?
Cl7 C101 H10E 109.2 . . ?
H10D C101 H10E 107.9 . . ?
C1 N1 C3 129.6(6) . . ?
C1 N1 H1A 115.2 . . ?
C3 N1 H1A 115.2 . . ?
C2 N2 C15 123.9(6) . . ?
Cl3 Ta1 Cl2 91.55(8) . . ?
Cl3 Ta1 Cl1 90.66(7) . . ?
Cl2 Ta1 Cl1 91.23(7) . . ?
Cl3 Ta1 Cl6 90.47(7) . . ?
Cl2 Ta1 Cl6 90.48(6) . . ?
Cl1 Ta1 Cl6 177.92(6) . . ?
Cl3 Ta1 Cl5 179.83(7) . . ?
Cl2 Ta1 Cl5 88.62(7) . . ?
Cl1 Ta1 Cl5 89.32(7) . . ?
Cl6 Ta1 Cl5 89.54(7) . . ?
Cl3 Ta1 Cl4 91.19(7) . . ?
Cl2 Ta1 Cl4 177.09(7) . . ?
Cl1 Ta1 Cl4 89.72(7) . . ?
Cl6 Ta1 Cl4 88.51(6) . . ?
Cl5 Ta1 Cl4 88.64(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
N1 C1 C2 N2 -4.3(9) . . . . ?
C8 C3 C4 C5 0.8(12) . . . . ?
N1 C3 C4 C5 -175.5(7) . . . . ?
C8 C3 C4 C9 -176.5(7) . . . . ?
N1 C3 C4 C9 7.3(10) . . . . ?
C3 C4 C5 C6 -1.2(11) . . . . ?
C9 C4 C5 C6 176.1(7) . . . . ?
C4 C5 C6 C7 1.0(12) . . . . ?
C5 C6 C7 C8 -0.4(12) . . . . ?
C6 C7 C8 C3 -0.1(11) . . . . ?
C6 C7 C8 C12 180.0(7) . . . . ?
C4 C3 C8 C7 -0.1(11) . . . . ?
N1 C3 C8 C7 175.9(7) . . . . ?
C4 C3 C8 C12 179.8(7) . . . . ?
N1 C3 C8 C12 -4.1(12) . . . . ?
C5 C4 C9 C10 -44.7(10) . . . . ?
C3 C4 C9 C10 132.4(8) . . . . ?
C5 C4 C9 C11 79.7(9) . . . . ?
C3 C4 C9 C11 -103.1(8) . . . . ?
C7 C8 C12 C14 73.8(9) . . . . ?
C3 C8 C12 C14 -106.2(8) . . . . ?
C7 C8 C12 C13 -50.4(9) . . . . ?
C3 C8 C12 C13 129.6(8) . . . . ?
C20 C15 C16 C17 4.8(11) . . . . ?
N2 C15 C16 C17 -179.1(7) . . . . ?
C20 C15 C16 C21 -177.4(7) . . . . ?
N2 C15 C16 C21 -1.3(10) . . . . ?
C15 C16 C17 C18 -2.2(12) . . . . ?
C21 C16 C17 C18 -180.0(7) . . . . ?
C16 C17 C18 C19 -0.6(13) . . . . ?
C17 C18 C19 C20 1.1(13) . . . . ?
C16 C15 C20 C19 -4.4(11) . . . . ?
N2 C15 C20 C19 179.8(7) . . . . ?
C16 C15 C20 C24 173.9(7) . . . . ?
N2 C15 C20 C24 -1.9(12) . . . . ?
C18 C19 C20 C15 1.4(12) . . . . ?
C18 C19 C20 C24 -177.0(8) . . . . ?
C17 C16 C21 C23 95.7(9) . . . . ?
C15 C16 C21 C23 -82.0(9) . . . . ?
C17 C16 C21 C22 -29.4(10) . . . . ?
C15 C16 C21 C22 153.0(7) . . . . ?
C15 C20 C24 C26 110.4(8) . . . . ?
C19 C20 C24 C26 -71.4(9) . . . . ?
C15 C20 C24 C25 -126.0(8) . . . . ?
C19 C20 C24 C25 52.2(9) . . . . ?
C2 C1 N1 C3 174.7(6) . . . . ?
C4 C3 N1 C1 -125.1(8) . . . . ?
C8 C3 N1 C1 58.5(11) . . . . ?
C1 C2 N2 C15 179.9(6) . . . . ?
C20 C15 N2 C2 -45.9(10) . . . . ?
C16 C15 N2 C2 138.0(7) . . . . ?

_refine_diff_density_max         2.402
_refine_diff_density_min         -1.942
_refine_diff_density_rms         0.182

####################################################################### 
# 
# 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_4b_bis
_database_code_depnum_ccdc_archive 'CCDC 1814764'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-24 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            'C27 H37 Cl10 N2 Ta'
_chemical_formula_weight         925.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.9501(4)
_cell_length_b                   19.2803(7)
_cell_length_c                   18.9646(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.508(3)
_cell_angle_gamma                90
_cell_volume                     3607.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3395
_cell_measurement_theta_min      2.319
_cell_measurement_theta_max      21.3005

_exptl_crystal_description       plate
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.810
_shelx_estimated_absorpt_T_min   0.618
_shelx_estimated_absorpt_T_max   0.702
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_T_max  0.7019
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1118 (selected reflections only, before parameter refinement)
 R(int) =  0.0765 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33961
_diffrn_reflns_av_unetI/netI     0.1396
_diffrn_reflns_av_R_equivalents  0.2112
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.513
_diffrn_reflns_theta_max         23.533
_diffrn_reflns_theta_full        23.533
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5356
_reflns_number_gt                2842
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0993P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5356
_refine_ls_number_parameters     364
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.0696
_refine_ls_wR_factor_ref         0.2077
_refine_ls_wR_factor_gt          0.1654
_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
Ta1 Ta 0.98480(8) 0.21724(4) 0.23064(4) 0.0384(3) Uani 1 1 d . . . . .
Cl1 Cl 1.1273(5) 0.2085(3) 0.1424(2) 0.0658(15) Uani 1 1 d . . . . .
Cl2 Cl 0.8415(5) 0.1307(2) 0.1777(3) 0.0605(15) Uani 1 1 d . . . . .
Cl3 Cl 0.8595(5) 0.3020(2) 0.1654(3) 0.0721(18) Uani 1 1 d . . . . .
Cl4 Cl 1.1261(5) 0.3040(2) 0.2880(2) 0.0512(13) Uani 1 1 d . . . . .
Cl5 Cl 0.8477(5) 0.2226(3) 0.3215(3) 0.0694(15) Uani 1 1 d . . . . .
Cl6 Cl 1.1231(5) 0.1340(2) 0.2959(2) 0.0448(12) Uani 1 1 d . . . . .
N1 N 0.5189(15) 0.1642(7) 0.2627(7) 0.036(3) Uani 1 1 d D . . . .
H1A H 0.603(6) 0.179(8) 0.265(8) 0.044 Uiso 1 1 d D U . . .
N2 N 0.5215(14) 0.2611(6) 0.1626(7) 0.037(4) Uani 1 1 d . . . . .
C1 C 0.4336(18) 0.2126(9) 0.2587(8) 0.041(4) Uani 1 1 d . . . . .
H1 H 0.3675 0.2137 0.2906 0.049 Uiso 1 1 calc R U . . .
C2 C 0.4351(16) 0.2666(8) 0.2061(9) 0.034(4) Uani 1 1 d . . . . .
H2 H 0.3742 0.3047 0.2041 0.041 Uiso 1 1 calc R U . . .
C3 C 0.5298(17) 0.1016(8) 0.3036(8) 0.032(4) Uani 1 1 d . . . . .
C4 C 0.5118(18) 0.0394(8) 0.2653(9) 0.038(4) Uani 1 1 d . . . . .
C5 C 0.5114(19) -0.0209(10) 0.3025(10) 0.054(5) Uani 1 1 d . . . . .
H5 H 0.4954 -0.0633 0.2774 0.065 Uiso 1 1 calc R U . . .
C6 C 0.5343(19) -0.0220(9) 0.3782(9) 0.050(5) Uani 1 1 d . . . . .
H6 H 0.5361 -0.0645 0.4037 0.059 Uiso 1 1 calc R U . . .
C7 C 0.5537(19) 0.0403(9) 0.4134(9) 0.049(5) Uani 1 1 d . . . . .
H7 H 0.5698 0.0402 0.4638 0.059 Uiso 1 1 calc R U . . .
C8 C 0.5507(17) 0.1043(9) 0.3777(8) 0.039(4) Uani 1 1 d . . . . .
C9 C 0.4788(19) 0.0392(9) 0.1835(9) 0.045(5) Uani 1 1 d . . . . .
H9 H 0.5026 0.0856 0.1651 0.054 Uiso 1 1 calc R U . . .
C10 C 0.3265(19) 0.0260(10) 0.1612(10) 0.062(6) Uani 1 1 d . . . . .
H10A H 0.2737 0.0616 0.1822 0.092 Uiso 1 1 calc R U . . .
H10B H 0.3066 0.0279 0.1092 0.092 Uiso 1 1 calc R U . . .
H10C H 0.3025 -0.0199 0.1780 0.092 Uiso 1 1 calc R U . . .
C11 C 0.561(2) -0.0158(10) 0.1511(9) 0.061(6) Uani 1 1 d . . . . .
H11A H 0.6575 -0.0074 0.1653 0.091 Uiso 1 1 calc R U . . .
H11B H 0.5365 -0.0617 0.1679 0.091 Uiso 1 1 calc R U . . .
H11C H 0.5406 -0.0140 0.0992 0.091 Uiso 1 1 calc R U . . .
C12 C 0.5676(18) 0.1706(9) 0.4206(8) 0.039(4) Uani 1 1 d . . . . .
H12 H 0.5839 0.2092 0.3876 0.046 Uiso 1 1 calc R U . . .
C13 C 0.6842(18) 0.1676(10) 0.4774(10) 0.055(5) Uani 1 1 d . . . . .
H13A H 0.7668 0.1570 0.4565 0.083 Uiso 1 1 calc R U . . .
H13B H 0.6944 0.2125 0.5017 0.083 Uiso 1 1 calc R U . . .
H13C H 0.6686 0.1314 0.5117 0.083 Uiso 1 1 calc R U . . .
C14 C 0.4403(18) 0.1868(9) 0.4521(9) 0.051(5) Uani 1 1 d . . . . .
H14A H 0.3634 0.1886 0.4142 0.076 Uiso 1 1 calc R U . . .
H14B H 0.4243 0.1506 0.4863 0.076 Uiso 1 1 calc R U . . .
H14C H 0.4502 0.2317 0.4764 0.076 Uiso 1 1 calc R U . . .
C15 C 0.5356(16) 0.3052(7) 0.1037(7) 0.027(4) Uani 1 1 d . . . . .
C16 C 0.5317(17) 0.3771(8) 0.1092(7) 0.033(4) Uani 1 1 d . U . . .
C17 C 0.5548(17) 0.4134(8) 0.0477(8) 0.039(4) Uani 1 1 d . . . . .
H17 H 0.5541 0.4627 0.0488 0.046 Uiso 1 1 calc R U . . .
C18 C 0.5783(19) 0.3811(10) -0.0138(9) 0.052(5) Uani 1 1 d . . . . .
H18 H 0.5878 0.4075 -0.0551 0.063 Uiso 1 1 calc R U . . .
C19 C 0.5879(17) 0.3099(9) -0.0151(9) 0.040(4) Uani 1 1 d . . . . .
H19 H 0.6081 0.2871 -0.0569 0.048 Uiso 1 1 calc R U . . .
C20 C 0.5686(15) 0.2718(8) 0.0435(8) 0.033(4) Uani 1 1 d . . . . .
C21 C 0.5015(16) 0.4178(8) 0.1746(8) 0.031(4) Uani 1 1 d . . . . .
H21 H 0.5134 0.3854 0.2161 0.037 Uiso 1 1 calc R U . . .
C22 C 0.3589(18) 0.4452(9) 0.1675(8) 0.047(5) Uani 1 1 d . . . . .
H22A H 0.2949 0.4068 0.1567 0.070 Uiso 1 1 calc R U . . .
H22B H 0.3428 0.4672 0.2122 0.070 Uiso 1 1 calc R U . . .
H22C H 0.3459 0.4793 0.1289 0.070 Uiso 1 1 calc R U . . .
C23 C 0.5989(18) 0.4772(9) 0.1911(9) 0.049(5) Uani 1 1 d . . . . .
H23A H 0.6922 0.4597 0.1958 0.073 Uiso 1 1 calc R U . . .
H23B H 0.5856 0.5113 0.1525 0.073 Uiso 1 1 calc R U . . .
H23C H 0.5825 0.4992 0.2358 0.073 Uiso 1 1 calc R U . . .
C24 C 0.5759(17) 0.1909(8) 0.0419(9) 0.035(4) Uani 1 1 d . . . . .
H24 H 0.6049 0.1745 0.0916 0.042 Uiso 1 1 calc R U . . .
C25 C 0.677(2) 0.1650(10) -0.0037(9) 0.057(6) Uani 1 1 d . . . . .
H25A H 0.7664 0.1842 0.0133 0.086 Uiso 1 1 calc R U . . .
H25B H 0.6808 0.1142 -0.0014 0.086 Uiso 1 1 calc R U . . .
H25C H 0.6496 0.1795 -0.0530 0.086 Uiso 1 1 calc R U . . .
C26 C 0.4321(19) 0.1626(9) 0.0180(9) 0.055(5) Uani 1 1 d . . . . .
H26A H 0.3696 0.1809 0.0493 0.082 Uiso 1 1 calc R U . . .
H26B H 0.4021 0.1771 -0.0310 0.082 Uiso 1 1 calc R U . . .
H26C H 0.4334 0.1118 0.0206 0.082 Uiso 1 1 calc R U . . .
C101 C 0.9464(18) 0.9000(10) 0.0944(10) 0.054(5) Uani 1 1 d . . . . .
Cl7 Cl 0.8252(5) 0.8588(3) 0.1393(3) 0.0617(14) Uani 1 1 d . . . . .
Cl8 Cl 1.1085(6) 0.8683(3) 0.1350(3) 0.0685(16) Uani 1 1 d . . . . .
Cl9 Cl 0.9268(6) 0.8760(3) 0.0052(3) 0.0717(16) Uani 1 1 d . . . . .
Cl10 Cl 0.9432(7) 0.9883(3) 0.1048(3) 0.0862(19) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta1 Cl3 2.314(5) . ?
Ta1 Cl2 2.335(5) . ?
Ta1 Cl5 2.335(5) . ?
Ta1 Cl1 2.337(5) . ?
Ta1 Cl4 2.357(5) . ?
Ta1 Cl6 2.357(4) . ?
N1 C1 1.26(2) . ?
N1 C3 1.43(2) . ?
N1 H1A 0.88(2) . ?
N2 C2 1.271(19) . ?
N2 C15 1.426(18) . ?
C1 C2 1.44(2) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 C8 1.39(2) . ?
C3 C4 1.40(2) . ?
C4 C5 1.36(2) . ?
C4 C9 1.54(2) . ?
C5 C6 1.42(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.38(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.40(2) . ?
C7 H7 0.9500 . ?
C8 C12 1.51(2) . ?
C9 C11 1.52(2) . ?
C9 C10 1.54(2) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.48(2) . ?
C12 C14 1.50(2) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.39(2) . ?
C15 C16 1.39(2) . ?
C16 C17 1.40(2) . ?
C16 C21 1.53(2) . ?
C17 C18 1.37(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.38(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.37(2) . ?
C19 H19 0.9500 . ?
C20 C24 1.56(2) . ?
C21 C22 1.50(2) . ?
C21 C23 1.51(2) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.49(2) . ?
C24 C26 1.54(2) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C101 Cl10 1.71(2) . ?
C101 Cl9 1.739(18) . ?
C101 Cl7 1.755(19) . ?
C101 Cl8 1.80(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3 Ta1 Cl2 91.05(17) . . ?
Cl3 Ta1 Cl5 92.2(2) . . ?
Cl2 Ta1 Cl5 88.0(2) . . ?
Cl3 Ta1 Cl1 90.2(2) . . ?
Cl2 Ta1 Cl1 91.95(19) . . ?
Cl5 Ta1 Cl1 177.7(2) . . ?
Cl3 Ta1 Cl4 89.60(17) . . ?
Cl2 Ta1 Cl4 177.91(18) . . ?
Cl5 Ta1 Cl4 89.96(18) . . ?
Cl1 Ta1 Cl4 90.03(18) . . ?
Cl3 Ta1 Cl6 176.94(18) . . ?
Cl2 Ta1 Cl6 91.21(15) . . ?
Cl5 Ta1 Cl6 89.97(18) . . ?
Cl1 Ta1 Cl6 87.71(17) . . ?
Cl4 Ta1 Cl6 88.21(15) . . ?
C1 N1 C3 131.5(15) . . ?
C1 N1 H1A 113(10) . . ?
C3 N1 H1A 104(10) . . ?
C2 N2 C15 127.0(14) . . ?
N1 C1 C2 120.7(16) . . ?
N1 C1 H1 119.7 . . ?
C2 C1 H1 119.7 . . ?
N2 C2 C1 117.2(15) . . ?
N2 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C8 C3 C4 123.1(14) . . ?
C8 C3 N1 120.3(14) . . ?
C4 C3 N1 116.6(14) . . ?
C5 C4 C3 118.2(16) . . ?
C5 C4 C9 120.4(16) . . ?
C3 C4 C9 121.2(14) . . ?
C4 C5 C6 121.7(17) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 117.9(16) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
C6 C7 C8 122.7(17) . . ?
C6 C7 H7 118.6 . . ?
C8 C7 H7 118.6 . . ?
C3 C8 C7 116.4(15) . . ?
C3 C8 C12 124.4(14) . . ?
C7 C8 C12 119.2(15) . . ?
C11 C9 C10 109.5(15) . . ?
C11 C9 C4 110.7(15) . . ?
C10 C9 C4 110.5(15) . . ?
C11 C9 H9 108.7 . . ?
C10 C9 H9 108.7 . . ?
C4 C9 H9 108.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 109.9(14) . . ?
C13 C12 C8 112.4(15) . . ?
C14 C12 C8 110.5(15) . . ?
C13 C12 H12 108.0 . . ?
C14 C12 H12 108.0 . . ?
C8 C12 H12 108.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 122.4(14) . . ?
C20 C15 N2 115.1(13) . . ?
C16 C15 N2 122.0(13) . . ?
C15 C16 C17 115.2(14) . . ?
C15 C16 C21 125.6(13) . . ?
C17 C16 C21 119.3(14) . . ?
C18 C17 C16 123.1(16) . . ?
C18 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
C17 C18 C19 119.2(16) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C20 C19 C18 120.3(16) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C15 119.6(15) . . ?
C19 C20 C24 120.5(14) . . ?
C15 C20 C24 119.8(13) . . ?
C22 C21 C23 109.0(14) . . ?
C22 C21 C16 113.0(13) . . ?
C23 C21 C16 111.7(13) . . ?
C22 C21 H21 107.6 . . ?
C23 C21 H21 107.6 . . ?
C16 C21 H21 107.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C26 112.3(15) . . ?
C25 C24 C20 112.5(14) . . ?
C26 C24 C20 108.4(13) . . ?
C25 C24 H24 107.8 . . ?
C26 C24 H24 107.8 . . ?
C20 C24 H24 107.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Cl10 C101 Cl9 111.9(12) . . ?
Cl10 C101 Cl7 111.6(10) . . ?
Cl9 C101 Cl7 110.8(10) . . ?
Cl10 C101 Cl8 108.4(10) . . ?
Cl9 C101 Cl8 107.9(10) . . ?
Cl7 C101 Cl8 105.9(11) . . ?

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
C3 N1 C1 C2 -171.9(16) . . . . ?
C15 N2 C2 C1 175.5(15) . . . . ?
N1 C1 C2 N2 3(3) . . . . ?
C1 N1 C3 C8 -63(3) . . . . ?
C1 N1 C3 C4 114(2) . . . . ?
C8 C3 C4 C5 2(3) . . . . ?
N1 C3 C4 C5 -175.2(16) . . . . ?
C8 C3 C4 C9 175.6(16) . . . . ?
N1 C3 C4 C9 -1(3) . . . . ?
C3 C4 C5 C6 -3(3) . . . . ?
C9 C4 C5 C6 -176.6(17) . . . . ?
C4 C5 C6 C7 2(3) . . . . ?
C5 C6 C7 C8 1(3) . . . . ?
C4 C3 C8 C7 0(3) . . . . ?
N1 C3 C8 C7 177.1(16) . . . . ?
C4 C3 C8 C12 -178.7(17) . . . . ?
N1 C3 C8 C12 -2(3) . . . . ?
C6 C7 C8 C3 -1(3) . . . . ?
C6 C7 C8 C12 177.6(17) . . . . ?
C5 C4 C9 C11 -49(2) . . . . ?
C3 C4 C9 C11 137.2(18) . . . . ?
C5 C4 C9 C10 72(2) . . . . ?
C3 C4 C9 C10 -101(2) . . . . ?
C3 C8 C12 C13 -132.7(17) . . . . ?
C7 C8 C12 C13 48(2) . . . . ?
C3 C8 C12 C14 104.1(19) . . . . ?
C7 C8 C12 C14 -75(2) . . . . ?
C2 N2 C15 C20 -142.1(16) . . . . ?
C2 N2 C15 C16 45(2) . . . . ?
C20 C15 C16 C17 4(2) . . . . ?
N2 C15 C16 C17 176.5(15) . . . . ?
C20 C15 C16 C21 -177.6(15) . . . . ?
N2 C15 C16 C21 -5(3) . . . . ?
C15 C16 C17 C18 1(3) . . . . ?
C21 C16 C17 C18 -177.9(16) . . . . ?
C16 C17 C18 C19 -4(3) . . . . ?
C17 C18 C19 C20 3(3) . . . . ?
C18 C19 C20 C15 2(3) . . . . ?
C18 C19 C20 C24 178.5(16) . . . . ?
C16 C15 C20 C19 -5(3) . . . . ?
N2 C15 C20 C19 -178.2(15) . . . . ?
C16 C15 C20 C24 177.9(15) . . . . ?
N2 C15 C20 C24 5(2) . . . . ?
C15 C16 C21 C22 -101.7(19) . . . . ?
C17 C16 C21 C22 76.7(19) . . . . ?
C15 C16 C21 C23 135.0(17) . . . . ?
C17 C16 C21 C23 -47(2) . . . . ?
C19 C20 C24 C25 34(2) . . . . ?
C15 C20 C24 C25 -149.5(16) . . . . ?
C19 C20 C24 C26 -91.1(18) . . . . ?
C15 C20 C24 C26 85.8(18) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl5 0.88(2) 2.66(6) 3.501(15) 160(14) .

_refine_diff_density_max         1.844
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.194

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1551418'
_audit_update_record             
;
2017-05-22 deposited with the CCDC.
2018-01-24 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            'C26 H36 Cl4 N2 Nb'
_chemical_formula_weight         611.28

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   12.8295(9)
_cell_length_b                   21.6973(15)
_cell_length_c                   10.3071(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2869.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8792
_cell_measurement_theta_min      2.1875
_cell_measurement_theta_max      28.191

_exptl_crystal_description       plate
_exptl_crystal_colour            dark-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_F_000             1260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.809
_shelx_estimated_absorpt_T_min   0.848
_shelx_estimated_absorpt_T_max   0.895
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1045 (selected reflections only, before parameter refinement)
 R(int) =  0.0491 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24389
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.877
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3209
_reflns_number_gt                2908
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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+4.0375P] 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         3209
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0842
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.18387(16) 0.71673(10) 0.1648(2) 0.0164(4) Uani 1 1 d . . . . .
H1 H 0.2412 0.6940 0.1982 0.020 Uiso 1 1 calc R U . . .
C2 C 0.11592(16) 0.62320(10) 0.0893(2) 0.0151(4) Uani 1 1 d . . . . .
C3 C 0.17054(17) 0.60758(10) -0.0243(2) 0.0177(4) Uani 1 1 d . . . . .
C4 C 0.18673(18) 0.54503(11) -0.0489(2) 0.0219(5) Uani 1 1 d . . . . .
H4 H 0.2229 0.5331 -0.1252 0.026 Uiso 1 1 calc R U . . .
C5 C 0.15134(18) 0.50022(11) 0.0353(2) 0.0242(5) Uani 1 1 d . . . . .
H5 H 0.1644 0.4580 0.0174 0.029 Uiso 1 1 calc R U . . .
C6 C 0.09692(18) 0.51683(10) 0.1455(2) 0.0219(5) Uani 1 1 d . . . . .
H6 H 0.0720 0.4855 0.2020 0.026 Uiso 1 1 calc R U . . .
C7 C 0.07774(16) 0.57842(10) 0.1758(2) 0.0162(4) Uani 1 1 d . . . . .
C8 C 0.21370(19) 0.65459(11) -0.1204(2) 0.0227(5) Uani 1 1 d . . . . .
H8 H 0.1873 0.6962 -0.0947 0.027 Uiso 1 1 calc R U . . .
C9 C 0.1757(3) 0.64111(13) -0.2585(2) 0.0360(6) Uani 1 1 d . . . . .
H9A H 0.2044 0.6719 -0.3182 0.054 Uiso 1 1 calc R U . . .
H9B H 0.1989 0.5999 -0.2847 0.054 Uiso 1 1 calc R U . . .
H9C H 0.0993 0.6429 -0.2608 0.054 Uiso 1 1 calc R U . . .
C10 C 0.3330(2) 0.65619(13) -0.1154(3) 0.0326(6) Uani 1 1 d . . . . .
H10A H 0.3590 0.6866 -0.1778 0.049 Uiso 1 1 calc R U . . .
H10B H 0.3557 0.6676 -0.0279 0.049 Uiso 1 1 calc R U . . .
H10C H 0.3607 0.6154 -0.1375 0.049 Uiso 1 1 calc R U . . .
C11 C 0.02117(17) 0.59420(10) 0.3007(2) 0.0183(4) Uani 1 1 d . . . . .
H11 H 0.0002 0.6385 0.2960 0.022 Uiso 1 1 calc R U . . .
C12 C 0.0933(2) 0.58664(15) 0.4171(2) 0.0359(6) Uani 1 1 d . . . . .
H12A H 0.0554 0.5970 0.4967 0.054 Uiso 1 1 calc R U . . .
H12B H 0.1175 0.5439 0.4218 0.054 Uiso 1 1 calc R U . . .
H12C H 0.1534 0.6142 0.4076 0.054 Uiso 1 1 calc R U . . .
C13 C -0.0781(2) 0.55591(13) 0.3189(3) 0.0313(6) Uani 1 1 d . . . . .
H13A H -0.1119 0.5676 0.4005 0.047 Uiso 1 1 calc R U . . .
H13B H -0.1258 0.5636 0.2465 0.047 Uiso 1 1 calc R U . . .
H13C H -0.0600 0.5120 0.3214 0.047 Uiso 1 1 calc R U . . .
Cl1 Cl -0.05647(6) 0.7500 0.31082(8) 0.02122(17) Uani 1 2 d S T P . .
Cl2 Cl -0.00452(7) 0.7500 -0.14541(8) 0.0310(2) Uani 1 2 d S T P . .
Cl3 Cl -0.13908(5) 0.66450(3) 0.06152(7) 0.03177(16) Uani 1 1 d . . . . .
N1 N 0.10272(13) 0.68911(8) 0.11751(16) 0.0131(3) Uani 1 1 d . . . . .
Nb1 Nb -0.03276(2) 0.7500 0.07795(3) 0.01877(10) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.296(3) . ?
C1 C1 1.444(4) 7_575 ?
C1 H1 0.9500 . ?
C2 C7 1.406(3) . ?
C2 C3 1.406(3) . ?
C2 N1 1.469(3) . ?
C3 C4 1.396(3) . ?
C3 C8 1.526(3) . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.394(3) . ?
C6 H6 0.9500 . ?
C7 C11 1.517(3) . ?
C8 C10 1.532(4) . ?
C8 C9 1.533(3) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.524(3) . ?
C11 C13 1.532(3) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
Cl1 Nb1 2.4194(8) . ?
Cl2 Nb1 2.3306(9) . ?
Cl3 Nb1 2.3088(6) . ?
N1 Nb1 2.2211(17) . ?
Nb1 N1 2.2211(17) 7_575 ?
Nb1 Cl3 2.3087(6) 7_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C1 117.54(12) . 7_575 ?
N1 C1 H1 121.2 . . ?
C1 C1 H1 121.2 7_575 . ?
C7 C2 C3 122.3(2) . . ?
C7 C2 N1 120.47(18) . . ?
C3 C2 N1 117.19(19) . . ?
C4 C3 C2 117.4(2) . . ?
C4 C3 C8 118.6(2) . . ?
C2 C3 C8 124.1(2) . . ?
C5 C4 C3 121.5(2) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 121.6(2) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C2 117.3(2) . . ?
C6 C7 C11 119.4(2) . . ?
C2 C7 C11 123.26(19) . . ?
C3 C8 C10 110.9(2) . . ?
C3 C8 C9 111.1(2) . . ?
C10 C8 C9 110.7(2) . . ?
C3 C8 H8 108.0 . . ?
C10 C8 H8 108.0 . . ?
C9 C8 H8 108.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 C12 110.69(19) . . ?
C7 C11 C13 112.29(19) . . ?
C12 C11 C13 110.5(2) . . ?
C7 C11 H11 107.7 . . ?
C12 C11 H11 107.7 . . ?
C13 C11 H11 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1 N1 C2 115.59(17) . . ?
C1 N1 Nb1 114.98(14) . . ?
C2 N1 Nb1 129.27(13) . . ?
N1 Nb1 N1 73.01(9) . 7_575 ?
N1 Nb1 Cl3 162.51(5) . 7_575 ?
N1 Nb1 Cl3 89.88(5) 7_575 7_575 ?
N1 Nb1 Cl3 89.88(5) . . ?
N1 Nb1 Cl3 162.51(5) 7_575 . ?
Cl3 Nb1 Cl3 106.93(3) 7_575 . ?
N1 Nb1 Cl2 93.42(5) . . ?
N1 Nb1 Cl2 93.42(5) 7_575 . ?
Cl3 Nb1 Cl2 91.11(2) 7_575 . ?
Cl3 Nb1 Cl2 91.11(2) . . ?
N1 Nb1 Cl1 85.20(5) . . ?
N1 Nb1 Cl1 85.20(5) 7_575 . ?
Cl3 Nb1 Cl1 89.91(2) 7_575 . ?
Cl3 Nb1 Cl1 89.91(2) . . ?
Cl2 Nb1 Cl1 178.28(3) . . ?

_refine_diff_density_max         0.751
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1814761'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-24 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            'C28.50 H31 Cl7 N3 Nb'
_chemical_formula_weight         756.62

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   8.3272(6)
_cell_length_b                   18.4834(12)
_cell_length_c                   22.5408(15)
_cell_angle_alpha                90
_cell_angle_beta                 97.617(4)
_cell_angle_gamma                90
_cell_volume                     3438.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5278
_cell_measurement_theta_min      2.385
_cell_measurement_theta_max      22.0115

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             1532
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.917
_shelx_estimated_absorpt_T_min   0.852
_shelx_estimated_absorpt_T_max   0.898
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8524
_exptl_absorpt_correction_T_max  0.8979
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1327 (selected reflections only, before parameter refinement)
 R(int) =  0.0666 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49289
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.823
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_full        25.023
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6041
_reflns_number_gt                4492
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.1305P)²+15.5157P] 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         6041
_refine_ls_number_parameters     366
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0670
_refine_ls_wR_factor_ref         0.2200
_refine_ls_wR_factor_gt          0.1984
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.90450(7) 0.11203(3) 0.79008(2) 0.0245(2) Uani 1 1 d . . . . .
Cl1 Cl 0.9846(2) 0.02773(10) 0.86663(8) 0.0382(4) Uani 1 1 d . . . . .
Cl2 Cl 0.6303(2) 0.08771(12) 0.79573(8) 0.0447(5) Uani 1 1 d . . . . .
Cl3 Cl 0.9080(3) 0.02255(10) 0.71779(8) 0.0431(5) Uani 1 1 d . . . . .
Cl4 Cl 1.17949(19) 0.13881(9) 0.78426(7) 0.0285(4) Uani 1 1 d . . . . .
Cl5 Cl 0.9025(2) 0.20019(10) 0.86510(8) 0.0379(4) Uani 1 1 d . . . . .
Cl6 Cl 0.8316(2) 0.20007(9) 0.71630(8) 0.0321(4) Uani 1 1 d . . . . .
N1 N 0.2988(6) 0.8866(3) 0.7880(2) 0.0246(12) Uani 1 1 d . . . . .
N2 N 0.4013(6) 0.8981(3) 0.8817(2) 0.0255(12) Uani 1 1 d . . . . .
N3 N 0.3771(7) 0.7390(3) 0.8928(2) 0.0280(12) Uani 1 1 d . . . . .
C1 C 0.3504(7) 0.8492(3) 0.8389(3) 0.0216(13) Uani 1 1 d . . . . .
C2 C 0.3165(8) 0.9596(4) 0.8000(3) 0.0307(15) Uani 1 1 d . . . . .
H2 H 0.2879 0.9980 0.7726 0.037 Uiso 1 1 calc R U . . .
C3 C 0.3820(8) 0.9662(4) 0.8577(3) 0.0301(15) Uani 1 1 d . . . . .
H3 H 0.4098 1.0103 0.8782 0.036 Uiso 1 1 calc R U . . .
C4 C 0.3468(7) 0.7703(3) 0.8424(3) 0.0239(13) Uani 1 1 d . . . . .
H4 H 0.3219 0.7424 0.8070 0.029 Uiso 1 1 calc R U . . .
C5 C 0.2309(8) 0.8564(3) 0.7313(3) 0.0253(14) Uani 1 1 d . . . . .
C6 C 0.0697(9) 0.8354(4) 0.7241(3) 0.0331(16) Uani 1 1 d . . . . .
C7 C 0.0056(10) 0.8075(4) 0.6680(3) 0.0391(18) Uani 1 1 d . . . . .
H7 H -0.1042 0.7923 0.6609 0.047 Uiso 1 1 calc R U . . .
C8 C 0.1034(11) 0.8025(4) 0.6234(3) 0.046(2) Uani 1 1 d . . . . .
H8 H 0.0590 0.7836 0.5856 0.055 Uiso 1 1 calc R U . . .
C9 C 0.2613(10) 0.8237(4) 0.6316(3) 0.0424(19) Uani 1 1 d . . . . .
H9 H 0.3246 0.8196 0.5996 0.051 Uiso 1 1 calc DR U . . .
C10 C 0.3311(9) 0.8515(4) 0.6869(3) 0.0329(16) Uani 1 1 d . . . . .
C11 C -0.0343(9) 0.8432(4) 0.7733(3) 0.0374(17) Uani 1 1 d . . . . .
H11A H -0.1437 0.8254 0.7594 0.056 Uiso 1 1 calc R U . . .
H11B H 0.0126 0.8151 0.8082 0.056 Uiso 1 1 calc R U . . .
H11C H -0.0398 0.8943 0.7845 0.056 Uiso 1 1 calc R U . . .
C12 C 0.5052(9) 0.8742(4) 0.6980(4) 0.0424(19) Uani 1 1 d . . . . .
H12A H 0.5556 0.8667 0.6616 0.064 Uiso 1 1 calc DR U . . .
H12B H 0.5116 0.9255 0.7090 0.064 Uiso 1 1 calc R U . . .
H12C H 0.5622 0.8453 0.7306 0.064 Uiso 1 1 calc R U . . .
C13 C 0.4818(8) 0.8845(3) 0.9414(3) 0.0263(14) Uani 1 1 d . . . . .
C14 C 0.3884(9) 0.8851(3) 0.9885(3) 0.0303(15) Uani 1 1 d . . . . .
C15 C 0.4708(10) 0.8739(4) 1.0459(3) 0.0374(17) Uani 1 1 d . . . . .
H15 H 0.4117 0.8728 1.0791 0.045 Uiso 1 1 calc R U . . .
C16 C 0.6351(10) 0.8646(4) 1.0549(3) 0.0418(19) Uani 1 1 d . . . . .
H16 H 0.6885 0.8579 1.0945 0.050 Uiso 1 1 calc R U . . .
C17 C 0.7241(9) 0.8648(4) 1.0079(3) 0.0404(18) Uani 1 1 d . . . . .
H17 H 0.8381 0.8582 1.0152 0.049 Uiso 1 1 calc R U . . .
C18 C 0.6478(9) 0.8748(4) 0.9484(3) 0.0328(16) Uani 1 1 d . . . . .
C19 C 0.2075(10) 0.8951(5) 0.9776(4) 0.048(2) Uani 1 1 d . . . . .
H19A H 0.1638 0.8939 1.0159 0.072 Uiso 1 1 calc R U . . .
H19B H 0.1821 0.9418 0.9580 0.072 Uiso 1 1 calc R U . . .
H19C H 0.1587 0.8560 0.9518 0.072 Uiso 1 1 calc R U . . .
C20 C 0.7420(9) 0.8722(5) 0.8963(4) 0.0438(19) Uani 1 1 d . . . . .
H20A H 0.8570 0.8650 0.9109 0.066 Uiso 1 1 calc R U . . .
H20B H 0.7026 0.8321 0.8699 0.066 Uiso 1 1 calc R U . . .
H20C H 0.7279 0.9178 0.8741 0.066 Uiso 1 1 calc R U . . .
C21 C 0.3741(8) 0.6618(4) 0.8946(3) 0.0283(14) Uani 1 1 d . . . . .
C22 C 0.2344(9) 0.6220(4) 0.8728(3) 0.0327(16) Uani 1 1 d . . . . .
C23 C 0.2383(12) 0.5478(4) 0.8796(4) 0.048(2) Uani 1 1 d . . . . .
H23 H 0.1457 0.5198 0.8650 0.058 Uiso 1 1 calc R U . . .
C24 C 0.3759(13) 0.5137(4) 0.9076(4) 0.055(2) Uani 1 1 d . . . . .
H24 H 0.3784 0.4625 0.9110 0.066 Uiso 1 1 calc R U . . .
C25 C 0.5104(12) 0.5541(4) 0.9307(4) 0.048(2) Uani 1 1 d . . . . .
H25 H 0.6031 0.5299 0.9505 0.058 Uiso 1 1 calc R U . . .
C26 C 0.5125(10) 0.6282(4) 0.9257(3) 0.0369(17) Uani 1 1 d . . . . .
C27 C 0.0800(9) 0.6564(4) 0.8451(4) 0.0438(19) Uani 1 1 d . . . . .
H27A H 0.0949 0.7089 0.8431 0.066 Uiso 1 1 calc R U . . .
H27B H 0.0502 0.6373 0.8046 0.066 Uiso 1 1 calc R U . . .
H27C H -0.0063 0.6457 0.8694 0.066 Uiso 1 1 calc R U . . .
C28 C 0.6567(9) 0.6718(4) 0.9510(3) 0.0428(19) Uani 1 1 d . . . . .
H28A H 0.6351 0.7232 0.9429 0.064 Uiso 1 1 calc R U . . .
H28B H 0.6782 0.6640 0.9943 0.064 Uiso 1 1 calc DR U . . .
H28C H 0.7512 0.6567 0.9324 0.064 Uiso 1 1 calc DR U . . .
C101 C 0.912(2) 0.3914(9) 1.0157(10) 0.0414(17) Uiso 0.227(4) 1 d D U P A -1
H10A H 1.0134 0.3839 1.0435 0.050 Uiso 0.227(4) 1 calc R U P A -1
H10B H 0.8263 0.4056 1.0397 0.050 Uiso 0.227(4) 1 calc R U P A -1
Cl11 Cl 0.8586(7) 0.3111(3) 0.9793(2) 0.0100(14) Uiso 0.227(4) 1 d D U P A -1
Cl12 Cl 0.9421(8) 0.4615(4) 0.9667(3) 0.0278(18) Uiso 0.227(4) 1 d D U P A -1
C201 C 0.784(2) 0.3057(8) 0.9727(8) 0.0100(14) Uiso 0.273(4) 1 d D U P A -2
H20D H 0.6970 0.2969 0.9979 0.012 Uiso 0.273(4) 1 calc R U P A -2
H20E H 0.7619 0.2747 0.9368 0.012 Uiso 0.273(4) 1 calc R U P A -2
Cl21 Cl 0.9572(8) 0.2818(4) 1.0102(3) 0.0375(17) Uiso 0.273(4) 1 d D U P A -2
Cl22 Cl 0.7762(9) 0.3931(4) 0.9510(3) 0.0414(17) Uiso 0.273(4) 1 d D U P A -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 Cl3 2.3247(19) . ?
Nb1 Cl2 2.3470(18) . ?
Nb1 Cl6 2.3483(17) . ?
Nb1 Cl5 2.3500(18) . ?
Nb1 Cl1 2.3547(17) . ?
Nb1 Cl4 2.3634(17) . ?
N1 C1 1.360(8) . ?
N1 C2 1.379(8) . ?
N1 C5 1.441(8) . ?
N2 C1 1.348(8) . ?
N2 C3 1.370(9) . ?
N2 C13 1.445(8) . ?
N3 C4 1.270(8) . ?
N3 C21 1.429(9) . ?
C1 C4 1.462(9) . ?
C2 C3 1.349(10) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.386(10) . ?
C5 C10 1.387(9) . ?
C6 C7 1.403(10) . ?
C6 C11 1.503(10) . ?
C7 C8 1.379(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.361(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.402(10) . ?
C9 H9 0.9500 . ?
C10 C12 1.498(11) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.383(10) . ?
C13 C14 1.397(10) . ?
C14 C15 1.395(10) . ?
C14 C19 1.506(11) . ?
C15 C16 1.367(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.372(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.417(10) . ?
C17 H17 0.9500 . ?
C18 C20 1.495(10) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.408(10) . ?
C21 C26 1.411(10) . ?
C22 C23 1.381(10) . ?
C22 C27 1.496(11) . ?
C23 C24 1.385(13) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.375(11) . ?
C25 H25 0.9500 . ?
C26 C28 1.495(11) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C101 Cl11 1.725(17) . ?
C101 Cl12 1.741(17) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C201 Cl21 1.634(15) . ?
C201 Cl22 1.686(14) . ?
C201 H20D 0.9900 . ?
C201 H20E 0.9900 . ?

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
Cl3 Nb1 Cl2 90.26(8) . . ?
Cl3 Nb1 Cl6 91.30(7) . . ?
Cl2 Nb1 Cl6 90.53(7) . . ?
Cl3 Nb1 Cl5 178.51(7) . . ?
Cl2 Nb1 Cl5 89.66(7) . . ?
Cl6 Nb1 Cl5 90.19(7) . . ?
Cl3 Nb1 Cl1 90.81(7) . . ?
Cl2 Nb1 Cl1 90.96(7) . . ?
Cl6 Nb1 Cl1 177.41(7) . . ?
Cl5 Nb1 Cl1 87.70(7) . . ?
Cl3 Nb1 Cl4 90.44(7) . . ?
Cl2 Nb1 Cl4 178.95(7) . . ?
Cl6 Nb1 Cl4 88.67(6) . . ?
Cl5 Nb1 Cl4 89.66(6) . . ?
Cl1 Nb1 Cl4 89.82(6) . . ?
C1 N1 C2 108.6(5) . . ?
C1 N1 C5 126.5(5) . . ?
C2 N1 C5 124.8(5) . . ?
C1 N2 C3 109.0(5) . . ?
C1 N2 C13 127.8(5) . . ?
C3 N2 C13 122.9(5) . . ?
C4 N3 C21 118.5(6) . . ?
N2 C1 N1 107.2(5) . . ?
N2 C1 C4 129.6(6) . . ?
N1 C1 C4 123.1(5) . . ?
C3 C2 N1 107.2(6) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 108.0(6) . . ?
C2 C3 H3 126.0 . . ?
N2 C3 H3 126.0 . . ?
N3 C4 C1 119.9(6) . . ?
N3 C4 H4 120.0 . . ?
C1 C4 H4 120.0 . . ?
C6 C5 C10 124.3(6) . . ?
C6 C5 N1 118.2(6) . . ?
C10 C5 N1 117.6(6) . . ?
C5 C6 C7 117.0(7) . . ?
C5 C6 C11 122.1(6) . . ?
C7 C6 C11 120.9(7) . . ?
C8 C7 C6 119.4(8) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 122.4(7) . . ?
C9 C8 H8 118.8 . . ?
C7 C8 H8 118.8 . . ?
C8 C9 C10 120.3(7) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C5 C10 C9 116.6(7) . . ?
C5 C10 C12 121.5(7) . . ?
C9 C10 C12 121.9(7) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 124.3(6) . . ?
C18 C13 N2 117.5(6) . . ?
C14 C13 N2 118.1(6) . . ?
C13 C14 C15 116.6(7) . . ?
C13 C14 C19 121.5(7) . . ?
C15 C14 C19 121.9(7) . . ?
C16 C15 C14 121.1(7) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 121.1(7) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C16 C17 C18 120.8(7) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C13 C18 C17 116.1(7) . . ?
C13 C18 C20 122.4(7) . . ?
C17 C18 C20 121.5(7) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 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 . . ?
C22 C21 C26 121.8(6) . . ?
C22 C21 N3 121.9(6) . . ?
C26 C21 N3 115.9(6) . . ?
C23 C22 C21 118.3(7) . . ?
C23 C22 C27 118.4(7) . . ?
C21 C22 C27 123.3(6) . . ?
C22 C23 C24 120.5(8) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C25 120.3(8) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 121.5(8) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C21 117.4(8) . . ?
C25 C26 C28 121.6(8) . . ?
C21 C26 C28 121.0(7) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Cl11 C101 Cl12 112.9(12) . . ?
Cl11 C101 H10A 109.0 . . ?
Cl12 C101 H10A 109.0 . . ?
Cl11 C101 H10B 109.0 . . ?
Cl12 C101 H10B 109.0 . . ?
H10A C101 H10B 107.8 . . ?
Cl21 C201 Cl22 114.0(11) . . ?
Cl21 C201 H20D 108.8 . . ?
Cl22 C201 H20D 108.8 . . ?
Cl21 C201 H20E 108.8 . . ?
Cl22 C201 H20E 108.8 . . ?
H20D C201 H20E 107.6 . . ?

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
C3 N2 C1 N1 -0.1(7) . . . . ?
C13 N2 C1 N1 -173.1(6) . . . . ?
C3 N2 C1 C4 179.9(6) . . . . ?
C13 N2 C1 C4 6.9(11) . . . . ?
C2 N1 C1 N2 -0.7(7) . . . . ?
C5 N1 C1 N2 -178.6(6) . . . . ?
C2 N1 C1 C4 179.3(6) . . . . ?
C5 N1 C1 C4 1.4(10) . . . . ?
C1 N1 C2 C3 1.3(7) . . . . ?
C5 N1 C2 C3 179.2(6) . . . . ?
N1 C2 C3 N2 -1.3(8) . . . . ?
C1 N2 C3 C2 0.9(8) . . . . ?
C13 N2 C3 C2 174.3(6) . . . . ?
C21 N3 C4 C1 -179.4(6) . . . . ?
N2 C1 C4 N3 9.0(10) . . . . ?
N1 C1 C4 N3 -171.0(6) . . . . ?
C1 N1 C5 C6 79.3(8) . . . . ?
C2 N1 C5 C6 -98.2(8) . . . . ?
C1 N1 C5 C10 -101.8(7) . . . . ?
C2 N1 C5 C10 80.7(8) . . . . ?
C10 C5 C6 C7 -0.1(10) . . . . ?
N1 C5 C6 C7 178.7(6) . . . . ?
C10 C5 C6 C11 -178.9(7) . . . . ?
N1 C5 C6 C11 -0.1(9) . . . . ?
C5 C6 C7 C8 -0.2(10) . . . . ?
C11 C6 C7 C8 178.6(7) . . . . ?
C6 C7 C8 C9 0.0(11) . . . . ?
C7 C8 C9 C10 0.4(12) . . . . ?
C6 C5 C10 C9 0.4(10) . . . . ?
N1 C5 C10 C9 -178.4(6) . . . . ?
C6 C5 C10 C12 -179.2(6) . . . . ?
N1 C5 C10 C12 2.0(9) . . . . ?
C8 C9 C10 C5 -0.6(10) . . . . ?
C8 C9 C10 C12 179.0(7) . . . . ?
C1 N2 C13 C18 83.9(8) . . . . ?
C3 N2 C13 C18 -88.2(8) . . . . ?
C1 N2 C13 C14 -98.8(8) . . . . ?
C3 N2 C13 C14 89.1(8) . . . . ?
C18 C13 C14 C15 -1.0(10) . . . . ?
N2 C13 C14 C15 -178.1(6) . . . . ?
C18 C13 C14 C19 -179.3(7) . . . . ?
N2 C13 C14 C19 3.6(10) . . . . ?
C13 C14 C15 C16 1.4(10) . . . . ?
C19 C14 C15 C16 179.7(7) . . . . ?
C14 C15 C16 C17 -1.0(11) . . . . ?
C15 C16 C17 C18 0.1(12) . . . . ?
C14 C13 C18 C17 0.1(10) . . . . ?
N2 C13 C18 C17 177.2(6) . . . . ?
C14 C13 C18 C20 178.0(7) . . . . ?
N2 C13 C18 C20 -4.9(10) . . . . ?
C16 C17 C18 C13 0.3(11) . . . . ?
C16 C17 C18 C20 -177.5(7) . . . . ?
C4 N3 C21 C22 -59.0(9) . . . . ?
C4 N3 C21 C26 128.1(7) . . . . ?
C26 C21 C22 C23 -3.5(10) . . . . ?
N3 C21 C22 C23 -176.0(6) . . . . ?
C26 C21 C22 C27 173.8(7) . . . . ?
N3 C21 C22 C27 1.3(10) . . . . ?
C21 C22 C23 C24 0.5(11) . . . . ?
C27 C22 C23 C24 -176.9(7) . . . . ?
C22 C23 C24 C25 1.8(13) . . . . ?
C23 C24 C25 C26 -1.2(13) . . . . ?
C24 C25 C26 C21 -1.6(11) . . . . ?
C24 C25 C26 C28 179.4(7) . . . . ?
C22 C21 C26 C25 4.0(10) . . . . ?
N3 C21 C26 C25 176.9(6) . . . . ?
C22 C21 C26 C28 -177.0(7) . . . . ?
N3 C21 C26 C28 -4.1(9) . . . . ?

_refine_diff_density_max         2.335
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.168

####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1814762'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-24 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            'C26 H36 Cl3 N2 Nb O'
_chemical_formula_weight         591.83

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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   12.5172(8)
_cell_length_b                   21.3437(14)
_cell_length_c                   10.4112(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2781.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5773
_cell_measurement_theta_min      2.376
_cell_measurement_theta_max      29.007

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.742
_shelx_estimated_absorpt_T_min   0.903
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_T_max  0.9431
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1503 (selected reflections only, before parameter refinement)
 R(int) =  0.0720 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37999
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.908
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2528
_reflns_number_gt                1956
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0427P)²+10.1718P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2528
_refine_ls_number_parameters     164
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1250
_refine_ls_wR_factor_gt          0.1064
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.099
_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
Nb1 Nb 1.05785(4) 0.2500 0.10028(6) 0.0412(3) Uani 1 2 d S TU P . .
O1 O 1.1314(7) 0.3265(4) 0.0985(8) 0.0327(19) Uani 0.5 1 d . . P A 1
Cl1 Cl 1.1850(2) 0.31926(14) 0.0887(3) 0.0304(6) Uani 0.5 1 d . . P A 2
Cl2 Cl 1.01315(12) 0.2500 -0.11810(14) 0.0301(4) Uani 1 2 d S T P A .
Cl3 Cl 1.04074(11) 0.2500 0.32869(13) 0.0222(3) Uani 1 2 d S T P A .
N1 N 0.9004(3) 0.31515(15) 0.1153(3) 0.0201(7) Uani 1 1 d . U . . .
C1 C 0.8144(3) 0.28440(18) 0.1381(3) 0.0177(8) Uani 1 1 d . . . . .
H1 H 0.7500 0.3064 0.1551 0.021 Uiso 1 1 calc R U . . .
C2 C 0.8867(3) 0.38119(18) 0.0876(4) 0.0180(8) Uani 1 1 d . . . . .
C3 C 0.9262(3) 0.42673(18) 0.1726(4) 0.0196(9) Uani 1 1 d . . . . .
C4 C 0.9078(3) 0.48926(19) 0.1425(4) 0.0226(9) Uani 1 1 d . . . . .
H4 H 0.9334 0.5209 0.1988 0.027 Uiso 1 1 calc R U . . .
C5 C 0.8533(3) 0.5066(2) 0.0329(4) 0.0241(9) Uani 1 1 d . . . . .
H5 H 0.8412 0.5497 0.0148 0.029 Uiso 1 1 calc R U . . .
C6 C 0.8163(3) 0.46110(19) -0.0506(4) 0.0217(9) Uani 1 1 d . . . . .
H6 H 0.7796 0.4735 -0.1263 0.026 Uiso 1 1 calc R U . . .
C7 C 0.8316(3) 0.39743(18) -0.0265(4) 0.0188(8) Uani 1 1 d . . . . .
C8 C 0.9814(3) 0.4093(2) 0.2976(4) 0.0230(9) Uani 1 1 d . . . . .
H8 H 0.9962 0.3632 0.2953 0.028 Uiso 1 1 calc R U . . .
C9 C 1.0881(4) 0.4431(2) 0.3140(5) 0.0445(13) Uani 1 1 d . . . . .
H9A H 1.1338 0.4345 0.2397 0.067 Uiso 1 1 calc R U . . .
H9B H 1.0756 0.4883 0.3206 0.067 Uiso 1 1 calc R U . . .
H9C H 1.1233 0.4282 0.3923 0.067 Uiso 1 1 calc R U . . .
C10 C 0.9091(5) 0.4219(4) 0.4116(5) 0.071(2) Uani 1 1 d . . . . .
H10A H 0.9462 0.4103 0.4910 0.107 Uiso 1 1 calc R U . . .
H10B H 0.8908 0.4665 0.4141 0.107 Uiso 1 1 calc R U . . .
H10C H 0.8437 0.3970 0.4033 0.107 Uiso 1 1 calc R U . . .
C11 C 0.7901(3) 0.35055(19) -0.1252(4) 0.0232(9) Uani 1 1 d . . . . .
H11 H 0.8151 0.3079 -0.0991 0.028 Uiso 1 1 calc R U . . .
C12 C 0.6664(3) 0.3497(2) -0.1278(4) 0.0306(10) Uani 1 1 d . . . . .
H12A H 0.6418 0.3192 -0.1918 0.046 Uiso 1 1 calc R U . . .
H12B H 0.6393 0.3378 -0.0429 0.046 Uiso 1 1 calc R U . . .
H12C H 0.6397 0.3914 -0.1502 0.046 Uiso 1 1 calc R U . . .
C13 C 0.8343(4) 0.3640(2) -0.2591(4) 0.0323(11) Uani 1 1 d . . . . .
H13A H 0.8062 0.3332 -0.3200 0.049 Uiso 1 1 calc R U . . .
H13B H 0.8128 0.4062 -0.2860 0.049 Uiso 1 1 calc R U . . .
H13C H 0.9125 0.3614 -0.2573 0.049 Uiso 1 1 calc R U . . .


_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
Nb1 O1 1.874(8) 7_565 ?
Nb1 O1 1.874(8) . ?
Nb1 Cl1 2.176(3) . ?
Nb1 Cl1 2.176(3) 7_565 ?
Nb1 Cl2 2.3415(16) . ?
Nb1 Cl3 2.3876(15) . ?
Nb1 N1 2.417(4) 7_565 ?
Nb1 N1 2.417(4) . ?
N1 C1 1.283(5) . ?
N1 C2 1.449(5) . ?
C1 C1 1.469(8) 7_565 ?
C1 H1 0.9500 . ?
C2 C3 1.404(5) . ?
C2 C7 1.417(5) . ?
C3 C4 1.390(6) . ?
C3 C8 1.520(5) . ?
C4 C5 1.380(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(6) . ?
C6 H6 0.9500 . ?
C7 C11 1.526(5) . ?
C8 C10 1.516(6) . ?
C8 C9 1.528(6) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.528(6) . ?
C11 C12 1.548(6) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O1 121.1(5) 7_565 . ?
Cl1 Nb1 Cl1 85.60(17) . 7_565 ?
O1 Nb1 Cl2 96.2(3) 7_565 . ?
O1 Nb1 Cl2 96.2(3) . . ?
Cl1 Nb1 Cl2 96.94(8) . . ?
Cl1 Nb1 Cl2 96.94(8) 7_565 . ?
O1 Nb1 Cl3 93.1(3) 7_565 . ?
O1 Nb1 Cl3 93.1(3) . . ?
Cl1 Nb1 Cl3 96.95(8) . . ?
Cl1 Nb1 Cl3 96.95(8) 7_565 . ?
Cl2 Nb1 Cl3 161.03(6) . . ?
O1 Nb1 N1 84.3(3) 7_565 7_565 ?
O1 Nb1 N1 154.5(3) . 7_565 ?
Cl1 Nb1 N1 172.32(12) . 7_565 ?
Cl1 Nb1 N1 102.08(11) 7_565 7_565 ?
Cl2 Nb1 N1 82.42(8) . 7_565 ?
Cl3 Nb1 N1 82.08(8) . 7_565 ?
O1 Nb1 N1 154.5(3) 7_565 . ?
O1 Nb1 N1 84.3(3) . . ?
Cl1 Nb1 N1 102.08(11) . . ?
Cl1 Nb1 N1 172.32(12) 7_565 . ?
Cl2 Nb1 N1 82.42(8) . . ?
Cl3 Nb1 N1 82.08(8) . . ?
N1 Nb1 N1 70.25(15) 7_565 . ?
C1 N1 C2 115.8(3) . . ?
C1 N1 Nb1 113.7(3) . . ?
C2 N1 Nb1 130.0(2) . . ?
N1 C1 C1 120.8(2) . 7_565 ?
N1 C1 H1 119.6 . . ?
C1 C1 H1 119.6 7_565 . ?
C3 C2 C7 122.0(3) . . ?
C3 C2 N1 120.4(3) . . ?
C7 C2 N1 117.6(3) . . ?
C4 C3 C2 117.6(4) . . ?
C4 C3 C8 120.3(4) . . ?
C2 C3 C8 122.0(3) . . ?
C5 C4 C3 121.7(4) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C7 121.7(4) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C2 117.1(4) . . ?
C6 C7 C11 118.1(3) . . ?
C2 C7 C11 124.8(3) . . ?
C10 C8 C3 110.8(4) . . ?
C10 C8 C9 110.5(4) . . ?
C3 C8 C9 112.2(4) . . ?
C10 C8 H8 107.7 . . ?
C3 C8 H8 107.7 . . ?
C9 C8 H8 107.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 C13 111.6(3) . . ?
C7 C11 C12 111.1(3) . . ?
C13 C11 C12 110.5(4) . . ?
C7 C11 H11 107.8 . . ?
C13 C11 H11 107.8 . . ?
C12 C11 H11 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
C2 N1 C1 C1 165.9(2) . . . 7_565 ?
Nb1 N1 C1 C1 -7.0(3) . . . 7_565 ?
C1 N1 C2 C3 113.8(4) . . . . ?
Nb1 N1 C2 C3 -74.8(4) . . . . ?
C1 N1 C2 C7 -65.6(4) . . . . ?
Nb1 N1 C2 C7 105.9(4) . . . . ?
C7 C2 C3 C4 1.1(6) . . . . ?
N1 C2 C3 C4 -178.2(4) . . . . ?
C7 C2 C3 C8 177.5(4) . . . . ?
N1 C2 C3 C8 -1.8(6) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C8 C3 C4 C5 -176.8(4) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C4 C5 C6 C7 0.7(6) . . . . ?
C5 C6 C7 C2 0.1(6) . . . . ?
C5 C6 C7 C11 -178.8(4) . . . . ?
C3 C2 C7 C6 -1.0(6) . . . . ?
N1 C2 C7 C6 178.3(3) . . . . ?
C3 C2 C7 C11 177.8(4) . . . . ?
N1 C2 C7 C11 -2.8(6) . . . . ?
C4 C3 C8 C10 70.3(6) . . . . ?
C2 C3 C8 C10 -106.0(5) . . . . ?
C4 C3 C8 C9 -53.7(5) . . . . ?
C2 C3 C8 C9 130.0(4) . . . . ?
C6 C7 C11 C13 55.0(5) . . . . ?
C2 C7 C11 C13 -123.8(4) . . . . ?
C6 C7 C11 C12 -68.8(5) . . . . ?
C2 C7 C11 C12 112.4(4) . . . . ?

_refine_diff_density_max         0.896
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.094

####################################################################### 
# 
# 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_7b
_database_code_depnum_ccdc_archive 'CCDC 1814763'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-24 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            'C26 H36 Br10 N2 Ta2'
_chemical_formula_weight         1537.57

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'
Br Br -0.2901 2.4595 '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      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                   11.6797(4)
_cell_length_b                   12.2727(5)
_cell_length_c                   27.3287(10)
_cell_angle_alpha                90
_cell_angle_beta                 98.412(2)
_cell_angle_gamma                90
_cell_volume                     3875.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8202
_cell_measurement_theta_min      2.421
_cell_measurement_theta_max      27.163

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.635
_exptl_crystal_F_000             2808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    15.975
_shelx_estimated_absorpt_T_min   0.198
_shelx_estimated_absorpt_T_max   0.327
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1979
_exptl_absorpt_correction_T_max  0.3274
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1918 (selected reflections only, before parameter refinement)
 R(int) =  0.0867 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54924
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_av_R_equivalents  0.1469
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.506
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6811
_reflns_number_gt                5300
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+15.3469P] 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         6811
_refine_ls_number_parameters     369
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.025
_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
Ta1 Ta 0.56823(3) 0.83164(4) 0.59171(2) 0.00761(12) Uani 1 1 d . . . . .
Ta2 Ta 0.78021(3) 0.28911(4) 0.60952(2) 0.00915(12) Uani 1 1 d . . . . .
Br1 Br 0.36888(8) 0.88143(9) 0.59250(4) 0.0161(3) Uani 1 1 d . . . . .
Br2 Br 0.63738(9) 0.96952(9) 0.54169(4) 0.0176(3) Uani 1 1 d . . . . .
Br3 Br 0.63617(9) 0.92615(9) 0.66941(4) 0.0150(2) Uani 1 1 d . . . . .
Br4 Br 0.52915(8) 0.70240(9) 0.52293(3) 0.0110(2) Uani 1 1 d . . . . .
Br5 Br 0.68342(9) 0.45590(9) 0.56454(4) 0.0147(2) Uani 1 1 d . . . . .
Br6 Br 0.76128(9) 0.37150(9) 0.69328(4) 0.0152(2) Uani 1 1 d . . . . .
Br7 Br 0.96901(9) 0.38812(11) 0.61399(4) 0.0244(3) Uani 1 1 d . . . . .
Br8 Br 0.79879(9) 0.21204(9) 0.52732(4) 0.0152(3) Uani 1 1 d . . . . .
Br9 Br 0.87223(9) 0.12494(10) 0.64918(4) 0.0193(3) Uani 1 1 d . . . . .
Br10 Br 0.58163(8) 0.21278(9) 0.60706(4) 0.0138(2) Uani 1 1 d . . . . .
N1 N 0.7435(6) 0.7436(7) 0.6093(3) 0.0082(17) Uani 1 1 d . U . . .
N2 N 0.5460(7) 0.6823(7) 0.6415(3) 0.0089(17) Uani 1 1 d . U . . .
C1 C 0.7400(8) 0.6508(8) 0.6295(3) 0.0071(19) Uani 1 1 d . U . . .
H1 H 0.8049 0.6034 0.6328 0.008 Uiso 1 1 calc R U . . .
C2 C 0.6342(8) 0.6196(9) 0.6474(3) 0.0085(19) Uani 1 1 d . U . . .
H2 H 0.6302 0.5516 0.6637 0.010 Uiso 1 1 calc R U . . .
C3 C 0.8580(8) 0.7961(8) 0.6081(4) 0.0081(18) Uani 1 1 d . U . . .
C4 C 0.8943(8) 0.8187(9) 0.5623(4) 0.013(2) Uani 1 1 d . U . . .
C5 C 0.9977(9) 0.8777(9) 0.5642(4) 0.019(2) Uani 1 1 d . U . . .
H5 H 1.0247 0.8979 0.5343 0.023 Uiso 1 1 calc R U . . .
C6 C 1.0607(9) 0.9067(10) 0.6090(4) 0.024(2) Uani 1 1 d . U . . .
H6 H 1.1278 0.9507 0.6097 0.029 Uiso 1 1 calc R U . . .
C7 C 1.0277(9) 0.8728(10) 0.6520(4) 0.021(2) Uani 1 1 d . U . . .
H7 H 1.0769 0.8879 0.6821 0.025 Uiso 1 1 calc R U . . .
C8 C 0.9260(9) 0.8176(9) 0.6540(4) 0.014(2) Uani 1 1 d . U . . .
C9 C 0.8348(9) 0.7731(9) 0.5133(4) 0.016(2) Uani 1 1 d . U . . .
H9 H 0.7514 0.7611 0.5163 0.019 Uiso 1 1 calc R U . . .
C10 C 0.8399(10) 0.8462(11) 0.4690(4) 0.028(3) Uani 1 1 d . U . . .
H10A H 0.8229 0.9214 0.4776 0.043 Uiso 1 1 calc R U . . .
H10B H 0.7826 0.8219 0.4413 0.043 Uiso 1 1 calc R U . . .
H10C H 0.9174 0.8426 0.4594 0.043 Uiso 1 1 calc R U . . .
C11 C 0.8894(9) 0.6613(9) 0.5064(4) 0.017(3) Uani 1 1 d . U . . .
H11A H 0.9711 0.6709 0.5030 0.026 Uiso 1 1 calc R U . . .
H11B H 0.8487 0.6264 0.4766 0.026 Uiso 1 1 calc R U . . .
H11C H 0.8832 0.6155 0.5353 0.026 Uiso 1 1 calc R U . . .
C12 C 0.8971(9) 0.7806(9) 0.7043(4) 0.016(2) Uani 1 1 d . U . . .
H12 H 0.8138 0.7585 0.6996 0.019 Uiso 1 1 calc R U . . .
C13 C 0.9690(10) 0.6813(10) 0.7226(4) 0.027(3) Uani 1 1 d . U . . .
H13A H 0.9562 0.6232 0.6978 0.040 Uiso 1 1 calc R U . . .
H13B H 0.9460 0.6557 0.7537 0.040 Uiso 1 1 calc R U . . .
H13C H 1.0512 0.7011 0.7281 0.040 Uiso 1 1 calc R U . . .
C14 C 0.9128(9) 0.8728(10) 0.7421(4) 0.023(3) Uani 1 1 d . U . . .
H14A H 0.9947 0.8935 0.7486 0.034 Uiso 1 1 calc R U . . .
H14B H 0.8875 0.8483 0.7729 0.034 Uiso 1 1 calc R U . . .
H14C H 0.8665 0.9357 0.7291 0.034 Uiso 1 1 calc R U . . .
C15 C 0.4541(8) 0.6575(9) 0.6716(4) 0.0102(19) Uani 1 1 d . U . . .
C16 C 0.3467(8) 0.6208(9) 0.6488(4) 0.0094(19) Uani 1 1 d . U . . .
C17 C 0.2634(9) 0.6012(9) 0.6804(4) 0.015(2) Uani 1 1 d . U . . .
H17 H 0.1890 0.5750 0.6668 0.017 Uiso 1 1 calc R U . . .
C18 C 0.2875(9) 0.6190(9) 0.7299(4) 0.017(2) Uani 1 1 d . U . . .
H18 H 0.2295 0.6057 0.7502 0.021 Uiso 1 1 calc R U . . .
C19 C 0.3934(9) 0.6557(9) 0.7510(4) 0.017(2) Uani 1 1 d . U . . .
H19 H 0.4080 0.6672 0.7857 0.020 Uiso 1 1 calc R U . . .
C20 C 0.4818(9) 0.6769(9) 0.7222(4) 0.013(2) Uani 1 1 d . U . . .
C21 C 0.3236(8) 0.5853(9) 0.5951(3) 0.010(2) Uani 1 1 d . U . . .
H21 H 0.3709 0.6330 0.5762 0.012 Uiso 1 1 calc R U . . .
C22 C 0.3621(9) 0.4679(9) 0.5886(4) 0.020(3) Uani 1 1 d . U . . .
H22A H 0.4458 0.4621 0.5990 0.029 Uiso 1 1 calc R U . . .
H22B H 0.3435 0.4468 0.5538 0.029 Uiso 1 1 calc R U . . .
H22C H 0.3218 0.4194 0.6089 0.029 Uiso 1 1 calc R U . . .
C23 C 0.1964(9) 0.5993(10) 0.5722(4) 0.020(3) Uani 1 1 d . U . . .
H23A H 0.1492 0.5438 0.5855 0.030 Uiso 1 1 calc R U . . .
H23B H 0.1892 0.5913 0.5362 0.030 Uiso 1 1 calc R U . . .
H23C H 0.1695 0.6719 0.5802 0.030 Uiso 1 1 calc R U . . .
C24 C 0.5992(9) 0.7121(9) 0.7500(4) 0.016(2) Uani 1 1 d . U . . .
H24 H 0.6498 0.7331 0.7250 0.019 Uiso 1 1 calc R U . . .
C25 C 0.6582(10) 0.6182(11) 0.7812(4) 0.031(3) Uani 1 1 d . U . . .
H25A H 0.7342 0.6422 0.7977 0.047 Uiso 1 1 calc R U . . .
H25B H 0.6680 0.5560 0.7597 0.047 Uiso 1 1 calc R U . . .
H25C H 0.6102 0.5965 0.8061 0.047 Uiso 1 1 calc R U . . .
C26 C 0.5871(11) 0.8110(11) 0.7828(4) 0.034(3) Uani 1 1 d . U . . .
H26A H 0.5426 0.8679 0.7632 0.051 Uiso 1 1 calc R U . . .
H26B H 0.6641 0.8391 0.7958 0.051 Uiso 1 1 calc R U . . .
H26C H 0.5468 0.7896 0.8103 0.051 Uiso 1 1 calc R U . . .


_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
Ta1 N1 2.302(8) . ?
Ta1 N2 2.320(8) . ?
Ta1 Br2 2.3890(11) . ?
Ta1 Br1 2.4103(10) . ?
Ta1 Br3 2.4476(11) . ?
Ta1 Br4 2.4508(11) . ?
Ta2 Br9 2.4593(12) . ?
Ta2 Br8 2.4759(11) . ?
Ta2 Br10 2.4931(11) . ?
Ta2 Br7 2.5051(11) . ?
Ta2 Br6 2.5414(11) . ?
Ta2 Br5 2.5637(11) . ?
N1 C1 1.270(12) . ?
N1 C3 1.489(12) . ?
N2 C2 1.276(12) . ?
N2 C15 1.475(12) . ?
C1 C2 1.446(13) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 C4 1.406(13) . ?
C3 C8 1.406(14) . ?
C4 C5 1.403(14) . ?
C4 C9 1.523(15) . ?
C5 C6 1.380(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.356(16) . ?
C6 H6 0.9500 . ?
C7 C8 1.375(14) . ?
C7 H7 0.9500 . ?
C8 C12 1.531(15) . ?
C9 C10 1.515(15) . ?
C9 C11 1.535(15) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.523(15) . ?
C12 C14 1.526(15) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.392(14) . ?
C15 C20 1.394(14) . ?
C16 C17 1.412(13) . ?
C16 C21 1.518(13) . ?
C17 C18 1.358(14) . ?
C17 H17 0.9500 . ?
C18 C19 1.362(15) . ?
C18 H18 0.9500 . ?
C19 C20 1.412(14) . ?
C19 H19 0.9500 . ?
C20 C24 1.529(14) . ?
C21 C22 1.527(15) . ?
C21 C23 1.535(14) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C26 1.528(16) . ?
C24 C25 1.536(16) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ta1 N2 71.3(3) . . ?
N1 Ta1 Br2 95.0(2) . . ?
N2 Ta1 Br2 166.27(19) . . ?
N1 Ta1 Br1 161.4(2) . . ?
N2 Ta1 Br1 90.23(19) . . ?
Br2 Ta1 Br1 103.50(4) . . ?
N1 Ta1 Br3 82.9(2) . . ?
N2 Ta1 Br3 85.2(2) . . ?
Br2 Ta1 Br3 93.83(4) . . ?
Br1 Ta1 Br3 93.62(4) . . ?
N1 Ta1 Br4 85.2(2) . . ?
N2 Ta1 Br4 85.1(2) . . ?
Br2 Ta1 Br4 93.45(4) . . ?
Br1 Ta1 Br4 95.69(4) . . ?
Br3 Ta1 Br4 166.52(4) . . ?
Br9 Ta2 Br8 89.79(4) . . ?
Br9 Ta2 Br10 92.81(4) . . ?
Br8 Ta2 Br10 92.10(4) . . ?
Br9 Ta2 Br7 92.93(4) . . ?
Br8 Ta2 Br7 92.07(4) . . ?
Br10 Ta2 Br7 172.92(4) . . ?
Br9 Ta2 Br6 91.09(4) . . ?
Br8 Ta2 Br6 179.01(4) . . ?
Br10 Ta2 Br6 88.32(4) . . ?
Br7 Ta2 Br6 87.42(4) . . ?
Br9 Ta2 Br5 177.50(4) . . ?
Br8 Ta2 Br5 87.77(4) . . ?
Br10 Ta2 Br5 86.78(4) . . ?
Br7 Ta2 Br5 87.67(4) . . ?
Br6 Ta2 Br5 91.36(4) . . ?
C1 N1 C3 118.9(8) . . ?
C1 N1 Ta1 115.3(6) . . ?
C3 N1 Ta1 124.5(6) . . ?
C2 N2 C15 116.4(9) . . ?
C2 N2 Ta1 113.1(6) . . ?
C15 N2 Ta1 129.9(6) . . ?
N1 C1 C2 117.9(9) . . ?
N1 C1 H1 121.0 . . ?
C2 C1 H1 121.0 . . ?
N2 C2 C1 120.7(10) . . ?
N2 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C4 C3 C8 123.5(9) . . ?
C4 C3 N1 119.5(8) . . ?
C8 C3 N1 117.0(8) . . ?
C5 C4 C3 116.1(10) . . ?
C5 C4 C9 120.1(9) . . ?
C3 C4 C9 123.5(9) . . ?
C6 C5 C4 120.6(11) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C7 C6 C5 120.6(11) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 122.8(11) . . ?
C6 C7 H7 118.6 . . ?
C8 C7 H7 118.6 . . ?
C7 C8 C3 115.9(10) . . ?
C7 C8 C12 119.0(10) . . ?
C3 C8 C12 125.1(9) . . ?
C10 C9 C4 114.8(10) . . ?
C10 C9 C11 111.4(9) . . ?
C4 C9 C11 107.0(9) . . ?
C10 C9 H9 107.8 . . ?
C4 C9 H9 107.8 . . ?
C11 C9 H9 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 111.4(9) . . ?
C13 C12 C8 110.5(9) . . ?
C14 C12 C8 111.6(9) . . ?
C13 C12 H12 107.7 . . ?
C14 C12 H12 107.7 . . ?
C8 C12 H12 107.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 124.1(9) . . ?
C16 C15 N2 120.0(9) . . ?
C20 C15 N2 115.8(8) . . ?
C15 C16 C17 116.1(9) . . ?
C15 C16 C21 123.1(8) . . ?
C17 C16 C21 120.1(9) . . ?
C18 C17 C16 121.4(10) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 121.2(10) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C20 121.2(10) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C15 C20 C19 116.1(9) . . ?
C15 C20 C24 127.0(9) . . ?
C19 C20 C24 116.8(9) . . ?
C16 C21 C22 111.7(8) . . ?
C16 C21 C23 112.7(8) . . ?
C22 C21 C23 110.1(9) . . ?
C16 C21 H21 107.4 . . ?
C22 C21 H21 107.4 . . ?
C23 C21 H21 107.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C24 C20 111.3(9) . . ?
C26 C24 C25 110.0(10) . . ?
C20 C24 C25 111.1(9) . . ?
C26 C24 H24 108.1 . . ?
C20 C24 H24 108.1 . . ?
C25 C24 H24 108.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_refine_diff_density_max         2.694
_refine_diff_density_min         -2.486
_refine_diff_density_rms         0.319

