# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_NbCl3
_database_code_depnum_ccdc_archive 'CCDC 2062321'
loop_
_audit_author_name
_audit_author_address
'Stefano Zacchini'
;Universita di Bologna
Italy
;
_audit_update_record             
;
2021-02-09 deposited with the CCDC.	2021-03-16 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            'C10 H20 Cl3 N2 Nb O4'
_chemical_formula_weight         431.54

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   15.3038(15)
_cell_length_b                   16.5965(16)
_cell_length_c                   13.8932(14)
_cell_angle_alpha                90
_cell_angle_beta                 90.886(2)
_cell_angle_gamma                90
_cell_volume                     3528.3(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9144
_cell_measurement_theta_min      2.4545
_cell_measurement_theta_max      34.632

_exptl_crystal_description       plate
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.147
_shelx_estimated_absorpt_T_min   0.762
_shelx_estimated_absorpt_T_max   0.856
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5572
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1465 (selected reflections only, before parameter refinement)
 R(int) =  0.0588 (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  'PHOTON100 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56714
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.331
_diffrn_reflns_theta_max         28.999
_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             9373
_reflns_number_gt                8323
_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)+(0.0210P)²+2.1840P] 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         9373
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0553
_refine_ls_wR_factor_gt          0.0536
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.39093(2) 0.73091(2) 0.60903(2) 0.01030(4) Uani 1 1 d . . . . .
Nb2 Nb 0.89208(2) 0.60451(2) 0.82802(2) 0.01307(4) Uani 1 1 d . . . . .
Cl1 Cl 0.39087(3) 0.58913(2) 0.63248(3) 0.01490(8) Uani 1 1 d . . . . .
Cl2 Cl 0.39512(3) 0.75362(3) 0.77521(3) 0.01625(8) Uani 1 1 d . . . . .
Cl3 Cl 0.39021(3) 0.86856(3) 0.57188(3) 0.01928(9) Uani 1 1 d . . . . .
Cl4 Cl 0.89269(3) 0.54962(3) 0.98230(3) 0.02075(9) Uani 1 1 d . . . . .
Cl5 Cl 0.89381(3) 0.73840(3) 0.88745(4) 0.02412(10) Uani 1 1 d . . . . .
Cl6 Cl 0.89226(3) 0.65125(3) 0.66660(3) 0.02517(10) Uani 1 1 d . . . . .
N1 N 0.61961(9) 0.71660(9) 0.50489(10) 0.0150(3) Uani 1 1 d . . . . .
N2 N 0.15737(9) 0.72118(9) 0.51158(10) 0.0146(3) Uani 1 1 d . . . . .
N3 N 0.65930(9) 0.53796(8) 0.77068(10) 0.0125(3) Uani 1 1 d . . . . .
N4 N 1.12180(9) 0.53265(9) 0.77140(11) 0.0164(3) Uani 1 1 d . . . . .
O1 O 0.52770(8) 0.73270(7) 0.63320(8) 0.0156(2) Uani 1 1 d . . . . .
O2 O 0.47045(7) 0.71272(7) 0.49091(8) 0.0145(2) Uani 1 1 d . . . . .
O3 O 0.25648(7) 0.73525(7) 0.63651(8) 0.0147(2) Uani 1 1 d . . . . .
O4 O 0.30588(7) 0.71197(7) 0.49335(8) 0.0141(2) Uani 1 1 d . . . . .
O5 O 0.80728(7) 0.51469(7) 0.78045(9) 0.0164(2) Uani 1 1 d . . . . .
O6 O 0.75784(7) 0.62832(7) 0.83494(9) 0.0158(2) Uani 1 1 d . . . . .
O7 O 1.02759(8) 0.62507(7) 0.83631(9) 0.0173(3) Uani 1 1 d . . . . .
O8 O 0.97406(7) 0.51206(7) 0.78300(9) 0.0167(2) Uani 1 1 d . . . . .
C1 C 0.54178(11) 0.72064(10) 0.54230(12) 0.0135(3) Uani 1 1 d . . . . .
C2 C 0.69822(11) 0.72249(12) 0.56722(14) 0.0199(4) Uani 1 1 d . . . . .
H2A H 0.7473 0.6944 0.5360 0.024 Uiso 1 1 calc R U . . .
H2B H 0.6870 0.6951 0.6291 0.024 Uiso 1 1 calc R U . . .
C3 C 0.72398(13) 0.80919(13) 0.58664(16) 0.0291(4) Uani 1 1 d . . . . .
H3A H 0.7352 0.8365 0.5255 0.044 Uiso 1 1 calc R U . . .
H3B H 0.7769 0.8105 0.6272 0.044 Uiso 1 1 calc R U . . .
H3C H 0.6764 0.8367 0.6198 0.044 Uiso 1 1 calc R U . . .
C4 C 0.62861(11) 0.70552(11) 0.40004(12) 0.0163(3) Uani 1 1 d . . . . .
H4A H 0.6829 0.7321 0.3788 0.020 Uiso 1 1 calc R U . . .
H4B H 0.5787 0.7316 0.3662 0.020 Uiso 1 1 calc R U . . .
C5 C 0.63149(14) 0.61680(12) 0.37300(15) 0.0284(4) Uani 1 1 d . . . . .
H5A H 0.6811 0.5910 0.4060 0.043 Uiso 1 1 calc R U . . .
H5B H 0.6381 0.6116 0.3032 0.043 Uiso 1 1 calc R U . . .
H5C H 0.5771 0.5906 0.3923 0.043 Uiso 1 1 calc R U . . .
C6 C 0.23745(10) 0.72258(10) 0.54605(12) 0.0127(3) Uani 1 1 d . . . . .
C7 C 0.08366(11) 0.73641(12) 0.57576(14) 0.0217(4) Uani 1 1 d . . . . .
H7A H 0.0947 0.7089 0.6380 0.026 Uiso 1 1 calc R U . . .
H7B H 0.0297 0.7133 0.5467 0.026 Uiso 1 1 calc R U . . .
C8 C 0.07007(14) 0.82540(14) 0.59365(16) 0.0329(5) Uani 1 1 d . . . . .
H8A H 0.1223 0.8480 0.6251 0.049 Uiso 1 1 calc R U . . .
H8B H 0.0196 0.8329 0.6353 0.049 Uiso 1 1 calc R U . . .
H8C H 0.0595 0.8529 0.5322 0.049 Uiso 1 1 calc R U . . .
C9 C 0.14021(11) 0.70643(11) 0.40801(12) 0.0178(3) Uani 1 1 d . . . . .
H9A H 0.1942 0.7169 0.3717 0.021 Uiso 1 1 calc R U . . .
H9B H 0.0947 0.7443 0.3844 0.021 Uiso 1 1 calc R U . . .
C10 C 0.11018(15) 0.62071(13) 0.38935(16) 0.0316(5) Uani 1 1 d . . . . .
H10A H 0.1566 0.5831 0.4089 0.047 Uiso 1 1 calc R U . . .
H10B H 0.0970 0.6138 0.3206 0.047 Uiso 1 1 calc R U . . .
H10C H 0.0576 0.6097 0.4265 0.047 Uiso 1 1 calc R U . . .
C11 C 0.73891(11) 0.55905(10) 0.79534(12) 0.0137(3) Uani 1 1 d . . . . .
C12 C 0.58557(11) 0.59272(11) 0.78872(12) 0.0154(3) Uani 1 1 d . . . . .
H12A H 0.5400 0.5843 0.7384 0.019 Uiso 1 1 calc R U . . .
H12B H 0.6061 0.6491 0.7837 0.019 Uiso 1 1 calc R U . . .
C13 C 0.54586(14) 0.58011(13) 0.88661(16) 0.0313(5) Uani 1 1 d . . . . .
H13A H 0.5244 0.5247 0.8916 0.047 Uiso 1 1 calc R U . . .
H13B H 0.4972 0.6177 0.8948 0.047 Uiso 1 1 calc R U . . .
H13C H 0.5903 0.5898 0.9368 0.047 Uiso 1 1 calc R U . . .
C14 C 0.64321(11) 0.46264(10) 0.71672(12) 0.0156(3) Uani 1 1 d . . . . .
H14A H 0.5877 0.4383 0.7380 0.019 Uiso 1 1 calc R U . . .
H14B H 0.6909 0.4239 0.7310 0.019 Uiso 1 1 calc R U . . .
C15 C 0.63818(15) 0.47785(13) 0.60913(14) 0.0288(4) Uani 1 1 d . . . . .
H15A H 0.5907 0.5158 0.5948 0.043 Uiso 1 1 calc R U . . .
H15B H 0.6269 0.4269 0.5754 0.043 Uiso 1 1 calc R U . . .
H15C H 0.6937 0.5006 0.5876 0.043 Uiso 1 1 calc R U . . .
C16 C 1.04360(11) 0.55565(11) 0.79721(12) 0.0154(3) Uani 1 1 d . . . . .
C17 C 1.19760(11) 0.58697(12) 0.78330(14) 0.0206(4) Uani 1 1 d . . . . .
H17A H 1.1763 0.6431 0.7888 0.025 Uiso 1 1 calc R U . . .
H17B H 1.2339 0.5837 0.7250 0.025 Uiso 1 1 calc R U . . .
C18 C 1.25337(16) 0.56754(19) 0.86980(19) 0.0536(8) Uani 1 1 d . . . . .
H18A H 1.2187 0.5734 0.9281 0.080 Uiso 1 1 calc R U . . .
H18B H 1.3032 0.6045 0.8728 0.080 Uiso 1 1 calc R U . . .
H18C H 1.2746 0.5120 0.8650 0.080 Uiso 1 1 calc R U . . .
C19 C 1.13308(12) 0.45622(11) 0.71839(14) 0.0216(4) Uani 1 1 d . . . . .
H19A H 1.0866 0.4180 0.7367 0.026 Uiso 1 1 calc R U . . .
H19B H 1.1901 0.4320 0.7364 0.026 Uiso 1 1 calc R U . . .
C20 C 1.12909(14) 0.47005(14) 0.61043(15) 0.0313(5) Uani 1 1 d . . . . .
H20A H 1.0723 0.4934 0.5925 0.047 Uiso 1 1 calc R U . . .
H20B H 1.1366 0.4186 0.5770 0.047 Uiso 1 1 calc R U . . .
H20C H 1.1758 0.5072 0.5921 0.047 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 O4 2.0764(11) . ?
Nb1 O2 2.0802(12) . ?
Nb1 O3 2.0998(12) . ?
Nb1 O1 2.1149(12) . ?
Nb1 Cl2 2.3392(5) . ?
Nb1 Cl3 2.3420(5) . ?
Nb1 Cl1 2.3754(5) . ?
Nb1 C6 2.4977(16) . ?
Nb1 C1 2.5068(17) . ?
Nb2 O5 2.0777(12) . ?
Nb2 O8 2.0842(12) . ?
Nb2 O6 2.0957(12) . ?
Nb2 O7 2.1031(12) . ?
Nb2 Cl4 2.3290(5) . ?
Nb2 Cl5 2.3704(5) . ?
Nb2 Cl6 2.3730(5) . ?
Nb2 C11 2.4975(17) . ?
Nb2 C16 2.4997(17) . ?
N1 C1 1.309(2) . ?
N1 C2 1.475(2) . ?
N1 C4 1.477(2) . ?
N2 C6 1.309(2) . ?
N2 C7 1.471(2) . ?
N2 C9 1.479(2) . ?
N3 C11 1.308(2) . ?
N3 C12 1.473(2) . ?
N3 C14 1.476(2) . ?
N4 C16 1.311(2) . ?
N4 C17 1.477(2) . ?
N4 C19 1.478(2) . ?
O1 C1 1.300(2) . ?
O2 C1 1.3016(19) . ?
O3 C6 1.303(2) . ?
O4 C6 1.299(2) . ?
O5 C11 1.299(2) . ?
O6 C11 1.305(2) . ?
O7 C16 1.299(2) . ?
O8 C16 1.299(2) . ?
C2 C3 1.515(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.520(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7 C8 1.513(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.516(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 C13 1.513(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.517(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 C18 1.498(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.518(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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
O4 Nb1 O2 74.62(4) . . ?
O4 Nb1 O3 62.72(4) . . ?
O2 Nb1 O3 137.33(4) . . ?
O4 Nb1 O1 137.06(5) . . ?
O2 Nb1 O1 62.46(4) . . ?
O3 Nb1 O1 160.19(5) . . ?
O4 Nb1 Cl2 142.71(3) . . ?
O2 Nb1 Cl2 142.62(3) . . ?
O3 Nb1 Cl2 80.04(3) . . ?
O1 Nb1 Cl2 80.16(3) . . ?
O4 Nb1 Cl3 88.64(4) . . ?
O2 Nb1 Cl3 88.20(4) . . ?
O3 Nb1 Cl3 90.31(4) . . ?
O1 Nb1 Cl3 91.30(4) . . ?
Cl2 Nb1 Cl3 93.461(16) . . ?
O4 Nb1 Cl1 87.40(4) . . ?
O2 Nb1 Cl1 88.04(4) . . ?
O3 Nb1 Cl1 90.38(3) . . ?
O1 Nb1 Cl1 89.69(3) . . ?
Cl2 Nb1 Cl1 91.391(15) . . ?
Cl3 Nb1 Cl1 175.146(16) . . ?
O4 Nb1 C6 31.30(5) . . ?
O2 Nb1 C6 105.91(5) . . ?
O3 Nb1 C6 31.43(5) . . ?
O1 Nb1 C6 168.36(5) . . ?
Cl2 Nb1 C6 111.46(4) . . ?
Cl3 Nb1 C6 88.60(4) . . ?
Cl1 Nb1 C6 89.47(4) . . ?
O4 Nb1 C1 105.86(5) . . ?
O2 Nb1 C1 31.24(5) . . ?
O3 Nb1 C1 168.57(5) . . ?
O1 Nb1 C1 31.23(5) . . ?
Cl2 Nb1 C1 111.39(4) . . ?
Cl3 Nb1 C1 89.20(4) . . ?
Cl1 Nb1 C1 89.18(4) . . ?
C6 Nb1 C1 137.14(5) . . ?
O5 Nb2 O8 75.66(5) . . ?
O5 Nb2 O6 62.74(5) . . ?
O8 Nb2 O6 138.39(5) . . ?
O5 Nb2 O7 138.10(5) . . ?
O8 Nb2 O7 62.50(5) . . ?
O6 Nb2 O7 158.97(5) . . ?
O5 Nb2 Cl4 90.32(4) . . ?
O8 Nb2 Cl4 89.67(4) . . ?
O6 Nb2 Cl4 91.23(4) . . ?
O7 Nb2 Cl4 91.32(4) . . ?
O5 Nb2 Cl5 141.90(3) . . ?
O8 Nb2 Cl5 142.29(3) . . ?
O6 Nb2 Cl5 79.22(3) . . ?
O7 Nb2 Cl5 79.82(4) . . ?
Cl4 Nb2 Cl5 92.649(19) . . ?
O5 Nb2 Cl6 86.78(4) . . ?
O8 Nb2 Cl6 87.00(4) . . ?
O6 Nb2 Cl6 89.84(4) . . ?
O7 Nb2 Cl6 89.04(4) . . ?
Cl4 Nb2 Cl6 176.038(19) . . ?
Cl5 Nb2 Cl6 91.30(2) . . ?
O5 Nb2 C11 31.30(5) . . ?
O8 Nb2 C11 106.90(5) . . ?
O6 Nb2 C11 31.50(5) . . ?
O7 Nb2 C11 168.79(5) . . ?
Cl4 Nb2 C11 92.26(4) . . ?
Cl5 Nb2 C11 110.60(4) . . ?
Cl6 Nb2 C11 86.66(4) . . ?
O5 Nb2 C16 106.81(5) . . ?
O8 Nb2 C16 31.29(5) . . ?
O6 Nb2 C16 169.00(5) . . ?
O7 Nb2 C16 31.29(5) . . ?
Cl4 Nb2 C16 92.30(4) . . ?
Cl5 Nb2 C16 111.00(4) . . ?
Cl6 Nb2 C16 85.96(4) . . ?
C11 Nb2 C16 137.85(6) . . ?
C1 N1 C2 120.18(15) . . ?
C1 N1 C4 119.83(14) . . ?
C2 N1 C4 119.99(14) . . ?
C6 N2 C7 119.84(15) . . ?
C6 N2 C9 120.67(14) . . ?
C7 N2 C9 119.47(14) . . ?
C11 N3 C12 120.21(14) . . ?
C11 N3 C14 120.45(14) . . ?
C12 N3 C14 119.11(13) . . ?
C16 N4 C17 120.69(15) . . ?
C16 N4 C19 120.01(15) . . ?
C17 N4 C19 118.83(14) . . ?
C1 O1 Nb1 91.26(9) . . ?
C1 O2 Nb1 92.78(10) . . ?
C6 O3 Nb1 91.38(9) . . ?
C6 O4 Nb1 92.55(9) . . ?
C11 O5 Nb2 92.49(10) . . ?
C11 O6 Nb2 91.48(9) . . ?
C16 O7 Nb2 91.46(10) . . ?
C16 O8 Nb2 92.29(10) . . ?
O1 C1 O2 113.47(14) . . ?
O1 C1 N1 124.00(15) . . ?
O2 C1 N1 122.53(15) . . ?
O1 C1 Nb1 57.51(8) . . ?
O2 C1 Nb1 55.98(8) . . ?
N1 C1 Nb1 178.07(13) . . ?
N1 C2 C3 112.04(15) . . ?
N1 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C5 111.59(15) . . ?
N1 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O4 C6 O3 113.29(14) . . ?
O4 C6 N2 123.35(15) . . ?
O3 C6 N2 123.36(15) . . ?
O4 C6 Nb1 56.15(8) . . ?
O3 C6 Nb1 57.19(8) . . ?
N2 C6 Nb1 177.65(13) . . ?
N2 C7 C8 112.10(16) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 111.74(15) . . ?
N2 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
N2 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
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 . . ?
O5 C11 O6 113.10(14) . . ?
O5 C11 N3 123.79(16) . . ?
O6 C11 N3 123.08(15) . . ?
O5 C11 Nb2 56.21(8) . . ?
O6 C11 Nb2 57.02(8) . . ?
N3 C11 Nb2 174.97(13) . . ?
N3 C12 C13 112.77(15) . . ?
N3 C12 H12A 109.0 . . ?
C13 C12 H12A 109.0 . . ?
N3 C12 H12B 109.0 . . ?
C13 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
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 . . ?
N3 C14 C15 111.41(15) . . ?
N3 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
N3 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 O8 113.46(14) . . ?
O7 C16 N4 123.47(16) . . ?
O8 C16 N4 123.03(16) . . ?
O7 C16 Nb2 57.25(8) . . ?
O8 C16 Nb2 56.42(8) . . ?
N4 C16 Nb2 173.79(13) . . ?
N4 C17 C18 113.27(16) . . ?
N4 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
N4 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 C20 111.07(16) . . ?
N4 C19 H19A 109.4 . . ?
C20 C19 H19A 109.4 . . ?
N4 C19 H19B 109.4 . . ?
C20 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_refine_diff_density_max         0.380
_refine_diff_density_min         -0.600
_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_NbBr3
_database_code_depnum_ccdc_archive 'CCDC 2062322'
loop_
_audit_author_name
_audit_author_address
'Stefano Zacchini'
;Universita di Bologna
Italy
;
_audit_update_record             
;
2021-03-11 deposited with the CCDC.	2021-03-16 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            'C10 H20 Br2.06 Cl0.94 N2 Nb O4'
_chemical_formula_weight         522.90

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   7.4915(14)
_cell_length_b                   12.296(2)
_cell_length_c                   9.6832(18)
_cell_angle_alpha                90
_cell_angle_beta                 95.837(8)
_cell_angle_gamma                90
_cell_volume                     887.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4805
_cell_measurement_theta_min      2.686
_cell_measurement_theta_max      26.5215

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_F_000             510
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    5.458
_shelx_estimated_absorpt_T_min   0.380
_shelx_estimated_absorpt_T_max   0.560
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3266
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1619 (selected reflections only, before parameter refinement)
 R(int) =  0.0726 (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  'PHOTON100 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8480
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.114
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.001
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.001
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.001
_reflns_number_total             3474
_reflns_number_gt                3032
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.001

_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)+(0.0417P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3474
_refine_ls_number_parameters     185
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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 0.63100(12) 0.56592(7) 0.69853(10) 0.0146(3) Uani 1 1 d . . . . .
O1 O 0.7662(9) 0.5424(5) 0.5200(7) 0.0188(17) Uani 1 1 d . . . . .
O2 O 0.7303(9) 0.4118(5) 0.6633(8) 0.0199(16) Uani 1 1 d . . . . .
O3 O 0.5066(10) 0.6453(6) 0.8558(7) 0.0197(17) Uani 1 1 d . . . . .
O4 O 0.5599(9) 0.4710(6) 0.8628(7) 0.0200(16) Uani 1 1 d . . . . .
Br1 Br 0.34186(17) 0.51215(10) 0.57307(14) 0.0235(5) Uani 0.703(9) 1 d . . P .
.
Br2 Br 0.59873(17) 0.75107(11) 0.59950(14) 0.0178(5) Uani 0.577(10) 1 d . . P .
.
Br3 Br 0.92813(16) 0.60896(10) 0.82898(13) 0.0251(5) Uani 0.769(9) 1 d . . P .
.
Cl1 Cl 0.34186(17) 0.51215(10) 0.57307(14) 0.0235(5) Uani 0.297(9) 1 d . . P .
.
Cl2 Cl 0.59873(17) 0.75107(11) 0.59950(14) 0.0178(5) Uani 0.423(10) 1 d . . P .
.
Cl3 Cl 0.92813(16) 0.60896(10) 0.82898(13) 0.0251(5) Uani 0.231(9) 1 d . . P .
.
C1 C 0.7976(12) 0.4409(8) 0.5517(10) 0.015(2) Uani 1 1 d . . . . .
C2 C 0.9590(14) 0.4112(10) 0.3496(11) 0.025(3) Uani 1 1 d . . . . .
H2A H 1.0003 0.4876 0.3598 0.030 Uiso 1 1 calc R U . . .
H2B H 1.0627 0.3659 0.3300 0.030 Uiso 1 1 calc R U . . .
C3 C 0.8147(17) 0.4030(14) 0.2311(12) 0.045(4) Uani 1 1 d . . . . .
H3A H 0.8617 0.4276 0.1455 0.068 Uiso 1 1 calc R U . . .
H3B H 0.7752 0.3272 0.2202 0.068 Uiso 1 1 calc R U . . .
H3C H 0.7128 0.4487 0.2499 0.068 Uiso 1 1 calc R U . . .
C4 C 0.9139(13) 0.2608(8) 0.5260(10) 0.019(2) Uani 1 1 d . . . . .
H4A H 0.9557 0.2178 0.4490 0.023 Uiso 1 1 calc R U . . .
H4B H 0.7968 0.2309 0.5466 0.023 Uiso 1 1 calc R U . . .
C5 C 1.0487(14) 0.2495(11) 0.6539(12) 0.027(3) Uani 1 1 d . . . . .
H5A H 1.0609 0.1727 0.6800 0.040 Uiso 1 1 calc R U . . .
H5B H 1.1654 0.2778 0.6333 0.040 Uiso 1 1 calc R U . . .
H5C H 1.0067 0.2909 0.7309 0.040 Uiso 1 1 calc R U . . .
C6 C 0.4861(13) 0.5542(9) 0.9188(11) 0.019(2) Uani 1 1 d . . . . .
C7 C 0.3316(14) 0.6393(9) 1.0947(11) 0.021(2) Uani 1 1 d . . . . .
H7A H 0.2166 0.6202 1.1308 0.025 Uiso 1 1 calc R U . . .
H7B H 0.3074 0.6975 1.0247 0.025 Uiso 1 1 calc R U . . .
C8 C 0.4605(17) 0.6810(11) 1.2120(12) 0.037(3) Uani 1 1 d . . . . .
H8A H 0.4087 0.7448 1.2537 0.056 Uiso 1 1 calc R U . . .
H8B H 0.4829 0.6240 1.2824 0.056 Uiso 1 1 calc R U . . .
H8C H 0.5737 0.7013 1.1765 0.056 Uiso 1 1 calc R U . . .
C9 C 0.3701(14) 0.4339(9) 1.0853(11) 0.020(2) Uani 1 1 d . . . . .
H9A H 0.3473 0.4402 1.1839 0.024 Uiso 1 1 calc R U . . .
H9B H 0.4788 0.3887 1.0807 0.024 Uiso 1 1 calc R U . . .
C10 C 0.2104(15) 0.3791(10) 1.0032(15) 0.036(3) Uani 1 1 d . . . . .
H10A H 0.1922 0.3068 1.0421 0.053 Uiso 1 1 calc R U . . .
H10B H 0.1026 0.4233 1.0089 0.053 Uiso 1 1 calc R U . . .
H10C H 0.2339 0.3719 0.9059 0.053 Uiso 1 1 calc R U . . .
N1 N 0.8907(10) 0.3740(7) 0.4825(9) 0.0164(18) Uani 1 1 d . . . . .
N2 N 0.4010(11) 0.5441(7) 1.0284(9) 0.021(2) 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 O2 2.077(7) . ?
Nb1 O4 2.085(7) . ?
Nb1 O3 2.104(7) . ?
Nb1 O1 2.111(7) . ?
Nb1 Br1 2.4637(16) . ?
Nb1 Br2 2.4726(17) . ?
Nb1 Br3 2.5017(15) . ?
O1 C1 1.302(12) . ?
O2 C1 1.288(12) . ?
O3 C6 1.293(13) . ?
O4 C6 1.307(13) . ?
C1 N1 1.306(13) . ?
C2 C3 1.498(16) . ?
C2 N1 1.504(14) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 N1 1.459(13) . ?
C4 C5 1.523(14) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.298(12) . ?
C7 N2 1.456(13) . ?
C7 C8 1.504(15) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.490(13) . ?
C9 C10 1.524(16) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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
O2 Nb1 O4 74.8(3) . . ?
O2 Nb1 O3 137.3(3) . . ?
O4 Nb1 O3 62.7(3) . . ?
O2 Nb1 O1 62.0(3) . . ?
O4 Nb1 O1 136.8(3) . . ?
O3 Nb1 O1 160.2(3) . . ?
O2 Nb1 Br1 89.2(2) . . ?
O4 Nb1 Br1 86.9(2) . . ?
O3 Nb1 Br1 92.8(2) . . ?
O1 Nb1 Br1 91.74(19) . . ?
O2 Nb1 Br2 143.0(2) . . ?
O4 Nb1 Br2 142.1(2) . . ?
O3 Nb1 Br2 79.6(2) . . ?
O1 Nb1 Br2 81.04(19) . . ?
Br1 Nb1 Br2 90.54(5) . . ?
O2 Nb1 C6 106.4(3) . . ?
O4 Nb1 C6 31.6(3) . . ?
O3 Nb1 C6 31.2(3) . . ?
O1 Nb1 C6 168.4(3) . . ?
Br1 Nb1 C6 88.2(2) . . ?
Br2 Nb1 C6 110.6(3) . . ?
O2 Nb1 Br3 87.7(2) . . ?
O4 Nb1 Br3 90.9(2) . . ?
O3 Nb1 Br3 88.5(2) . . ?
O1 Nb1 Br3 88.07(19) . . ?
Br1 Nb1 Br3 176.63(6) . . ?
Br2 Nb1 Br3 92.75(5) . . ?
C6 Nb1 Br3 91.3(2) . . ?
O2 Nb1 C1 30.8(3) . . ?
O4 Nb1 C1 105.6(3) . . ?
O3 Nb1 C1 167.4(3) . . ?
O1 Nb1 C1 31.2(3) . . ?
Br1 Nb1 C1 91.1(2) . . ?
Br2 Nb1 C1 112.3(2) . . ?
C6 Nb1 C1 137.2(4) . . ?
Br3 Nb1 C1 87.0(2) . . ?
C1 O1 Nb1 91.6(6) . . ?
C1 O2 Nb1 93.6(6) . . ?
C6 O3 Nb1 91.3(6) . . ?
C6 O4 Nb1 91.7(6) . . ?
O2 C1 O1 112.8(8) . . ?
O2 C1 N1 122.0(10) . . ?
O1 C1 N1 125.2(9) . . ?
O2 C1 Nb1 55.6(5) . . ?
O1 C1 Nb1 57.2(5) . . ?
N1 C1 Nb1 176.3(7) . . ?
C3 C2 N1 110.7(9) . . ?
C3 C2 H2A 109.5 . . ?
N1 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C5 111.8(9) . . ?
N1 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C6 N2 124.1(10) . . ?
O3 C6 O4 114.0(8) . . ?
N2 C6 O4 121.9(10) . . ?
O3 C6 Nb1 57.5(5) . . ?
N2 C6 Nb1 175.7(8) . . ?
O4 C6 Nb1 56.7(5) . . ?
N2 C7 C8 112.1(9) . . ?
N2 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 110.6(9) . . ?
N2 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
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 . . ?
C1 N1 C4 120.5(9) . . ?
C1 N1 C2 119.5(9) . . ?
C4 N1 C2 119.7(8) . . ?
C6 N2 C7 120.7(9) . . ?
C6 N2 C9 119.8(9) . . ?
C7 N2 C9 119.5(8) . . ?

_refine_diff_density_max         1.368
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.159



