# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is (c) The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2006



data_global
# 1. SUBMISSION DETAILS

_journal_coden_Cambridge         440

_publ_contact_letter             
;
Please consider this CIF submission for publication
in New Journal of Chemistry
;
_publ_contact_author             ' Michel Etienne '

_publ_contact_author_address     
;
Laboratoire de Chimie de Coordination CNRS
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       etienne@lcc-toulouse.fr

_publ_requested_journal          ' New Journal of Chemistry '

#=============================================================================
# 2. TITLE AND AUTHOR LIST
_publ_section_title              
;
Aromatic interactions in hydrotris(3-methylindazolyl)borate
organometallic complexes: control of an alkyne ligand
orientation in the crystal
;
loop_
_publ_author_name
_publ_author_address
'Pascal Oulie'
;
Laboratoire de Chimie de Coordination,
205 Route de Narbonne,
31077, Toulouse Cedex 04,
France
;
'Johannes Teichert'
;
Laboratoire de Chimie de Coordination,
205 Route de Narbonne,
31077, Toulouse Cedex 04,
France
;
'Laure Vendier'
;
Laboratoire de Chimie de Coordination,
205 Route de Narbonne,
31077, Toulouse Cedex 04,
France
;
'Celine Dablemont'
;
Laboratoire de Chimie de Coordination,
205 Route de Narbonne,
31077, Toulouse Cedex 04,
France
;
'Michel Etienne'
;
Laboratoire de Chimie de Coordination,
205 Route de Narbonne,
31077, Toulouse Cedex 04,
France
;
#==============================================================================
_publ_section_references         
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C.,
Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic
solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435.

Sheldrick, G. M. (1997). SHELXL97. Program for the refinement
of Crystal Structures. University of Gottingen, Germany.

MULTI SCAN - c.f. r.h. blessing, acta cryst. (1995), a51, 33-38

WINGX - 1.63 Integrated System
of Windows Programs
for the Solution, Refinement and Analysis
of Single Crystal X-Ray Diffraction Data.
Farrugia, L. J. Appl. Crystallogr., 1999, 32, 837.

Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical
Crystallography Laboratory, OXFORD, UK.
;

data_compound
_database_code_depnum_ccdc_archive 'CCDC 604264'
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C33 H30 B Cl2 N6 Nb'
_chemical_formula_sum            'C33 H30 B Cl2 N6 Nb'
_chemical_formula_weight         685.25
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.1301(14)
_cell_length_b                   19.875(2)
_cell_length_c                   16.4137(16)
_cell_angle_alpha                90
_cell_angle_beta                 109.858(10)
_cell_angle_gamma                90
_cell_volume                     3415.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    180
_cell_measurement_reflns_used    3320
_cell_measurement_theta_min      2.6892
_cell_measurement_theta_max      32.2783
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_T_max  0.9150

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180
_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  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_number            25314
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_full        26.32
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             6958
_reflns_number_gt                3929
_reflns_threshold_expression     >2\s(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6958
_refine_ls_number_parameters     392
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1105
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_restrained_S_all      0.877
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.077

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0494(4) 0.10125(19) 0.4658(3) 0.0524(12) Uani 1 1 d . . .
H1A H -0.0896 0.0816 0.5034 0.079 Uiso 1 1 calc R . .
H1B H -0.005 0.0669 0.4461 0.079 Uiso 1 1 calc R . .
H1C H -0.1131 0.1214 0.4169 0.079 Uiso 1 1 calc R . .
C2 C 0.0432(4) 0.15366(18) 0.5139(2) 0.0382(10) Uani 1 1 d . . .
C3 C 0.0612(4) 0.21840(18) 0.5242(2) 0.0342(9) Uani 1 1 d . . .
C4 C -0.0021(4) 0.28207(18) 0.4958(2) 0.0347(9) Uani 1 1 d . . .
C5 C 0.0607(4) 0.34187(18) 0.5264(3) 0.0437(11) Uani 1 1 d . . .
H5 H 0.1445 0.3411 0.5644 0.052 Uiso 1 1 calc R . .
C6 C -0.0010(5) 0.4029(2) 0.5007(3) 0.0532(12) Uani 1 1 d . . .
H6 H 0.0415 0.4429 0.5219 0.064 Uiso 1 1 calc R . .
C7 C -0.1260(5) 0.4046(2) 0.4435(3) 0.0618(14) Uani 1 1 d . . .
H7 H -0.1672 0.4456 0.4266 0.074 Uiso 1 1 calc R . .
C8 C -0.1873(5) 0.3466(2) 0.4127(3) 0.0734(16) Uani 1 1 d . . .
H8 H -0.271 0.3478 0.3745 0.088 Uiso 1 1 calc R . .
C9 C -0.1264(4) 0.2847(2) 0.4377(3) 0.0583(13) Uani 1 1 d . . .
H9 H -0.1694 0.2451 0.4153 0.07 Uiso 1 1 calc R . .
C11 C 0.2223(4) 0.11100(19) 0.3943(2) 0.0485(11) Uani 1 1 d . . .
H11A H 0.1595 0.1402 0.4037 0.073 Uiso 1 1 calc R . .
H11B H 0.1845 0.0864 0.3414 0.073 Uiso 1 1 calc R . .
H11C H 0.2924 0.1374 0.3904 0.073 Uiso 1 1 calc R . .
C12 C 0.2693(4) 0.06328(19) 0.4673(3) 0.0370(10) Uani 1 1 d . . .
C13 C 0.3195(3) -0.00160(18) 0.4643(3) 0.0345(9) Uani 1 1 d . . .
C14 C 0.3491(3) -0.02788(18) 0.5485(3) 0.0343(9) Uani 1 1 d . . .
C15 C 0.4010(4) -0.09233(18) 0.5703(3) 0.0413(10) Uani 1 1 d . . .
H15 H 0.4196 -0.1099 0.6257 0.05 Uiso 1 1 calc R . .
C16 C 0.4227(4) -0.1281(2) 0.5052(3) 0.0508(12) Uani 1 1 d . . .
H16 H 0.4559 -0.1714 0.5168 0.061 Uiso 1 1 calc R . .
C17 C 0.3967(4) -0.1016(2) 0.4217(3) 0.0504(12) Uani 1 1 d . . .
H17 H 0.4142 -0.1275 0.3799 0.061 Uiso 1 1 calc R . .
C18 C 0.3467(4) -0.0392(2) 0.4004(3) 0.0441(11) Uani 1 1 d . . .
H18 H 0.3309 -0.0219 0.3452 0.053 Uiso 1 1 calc R . .
C21 C 0.5288(4) 0.2481(2) 0.7650(3) 0.0570(13) Uani 1 1 d . . .
H21A H 0.5929 0.2593 0.7402 0.085 Uiso 1 1 calc R . .
H21B H 0.5532 0.2656 0.8228 0.085 Uiso 1 1 calc R . .
H21C H 0.4485 0.2674 0.7304 0.085 Uiso 1 1 calc R . .
C22 C 0.5160(4) 0.1741(2) 0.7672(2) 0.0399(10) Uani 1 1 d . . .
C23 C 0.6072(4) 0.1297(2) 0.8211(2) 0.0412(10) Uani 1 1 d . . .
C24 C 0.7315(4) 0.1388(3) 0.8836(3) 0.0580(13) Uani 1 1 d . . .
H24 H 0.7703 0.1809 0.8946 0.07 Uiso 1 1 calc R . .
C25 C 0.7922(5) 0.0810(3) 0.9277(3) 0.0675(15) Uani 1 1 d . . .
H25 H 0.8726 0.0849 0.9698 0.081 Uiso 1 1 calc R . .
C26 C 0.7355(5) 0.0185(3) 0.9101(3) 0.0661(15) Uani 1 1 d . . .
H26 H 0.779 -0.018 0.9421 0.079 Uiso 1 1 calc R . .
C27 C 0.6155(4) 0.0070(2) 0.8466(3) 0.0472(11) Uani 1 1 d . . .
H27 H 0.5797 -0.0357 0.8343 0.057 Uiso 1 1 calc R . .
C28 C 0.5541(4) 0.0650(2) 0.8030(2) 0.0371(10) Uani 1 1 d . . .
C31 C -0.0568(4) 0.1472(2) 0.6863(3) 0.0552(12) Uani 1 1 d . . .
H31A H -0.016 0.1876 0.7144 0.083 Uiso 1 1 calc R . .
H31B H -0.124 0.1351 0.7078 0.083 Uiso 1 1 calc R . .
H31C H -0.0921 0.1547 0.6249 0.083 Uiso 1 1 calc R . .
C32 C 0.0400(4) 0.09106(18) 0.7046(3) 0.0368(10) Uani 1 1 d . . .
C33 C 0.0393(4) 0.03323(19) 0.7523(2) 0.0354(9) Uani 1 1 d . . .
C34 C -0.0415(4) 0.0077(2) 0.7954(3) 0.0436(11) Uani 1 1 d . . .
H34 H -0.1132 0.0316 0.7958 0.052 Uiso 1 1 calc R . .
C35 C -0.0110(4) -0.0533(2) 0.8368(3) 0.0488(11) Uani 1 1 d . . .
H35 H -0.0621 -0.071 0.8662 0.059 Uiso 1 1 calc R . .
C36 C 0.0979(4) -0.0892(2) 0.8349(3) 0.0481(11) Uani 1 1 d . . .
H36 H 0.1154 -0.1306 0.8628 0.058 Uiso 1 1 calc R . .
C37 C 0.1789(4) -0.06628(19) 0.7943(2) 0.0402(10) Uani 1 1 d . . .
H37 H 0.2501 -0.0907 0.7944 0.048 Uiso 1 1 calc R . .
C38 C 0.1481(4) -0.00363(18) 0.7524(2) 0.0323(9) Uani 1 1 d . . .
N1 N 0.2696(3) 0.07539(14) 0.5486(2) 0.0335(8) Uani 1 1 d . . .
N2 N 0.3175(3) 0.01967(14) 0.59808(19) 0.0326(8) Uani 1 1 d . . .
N3 N 0.4136(3) 0.13943(15) 0.7195(2) 0.0356(8) Uani 1 1 d . . .
N4 N 0.4351(3) 0.07219(15) 0.74133(19) 0.0349(8) Uani 1 1 d . . .
N5 N 0.1433(3) 0.09133(14) 0.6797(2) 0.0370(8) Uani 1 1 d . . .
N6 N 0.2093(3) 0.03175(14) 0.70851(19) 0.0329(8) Uani 1 1 d . . .
Cl1 Cl 0.35169(10) 0.23008(5) 0.54953(7) 0.0427(3) Uani 1 1 d . . .
Cl2 Cl 0.19930(10) 0.24758(5) 0.71449(7) 0.0450(3) Uani 1 1 d . . .
Nb1 Nb 0.21837(3) 0.168522(16) 0.60928(2) 0.03357(12) Uani 1 1 d . . .
B1 B 0.3373(4) 0.0184(2) 0.6954(3) 0.0359(11) Uani 1 1 d . . .
H1 H 0.3693 -0.026 0.719 0.043 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.044(3) 0.038(2) 0.062(3) -0.005(2) 0.002(2) -0.008(2)
C2 0.034(2) 0.040(2) 0.039(2) 0.0049(19) 0.0099(19) 0.0027(19)
C3 0.037(2) 0.031(2) 0.038(2) 0.0016(18) 0.0168(19) 0.0034(18)
C4 0.042(2) 0.035(2) 0.027(2) -0.0013(17) 0.0123(19) 0.0034(19)
C5 0.050(3) 0.038(2) 0.047(3) 0.004(2) 0.022(2) 0.004(2)
C6 0.071(3) 0.038(2) 0.056(3) 0.003(2) 0.028(3) 0.004(2)
C7 0.094(4) 0.042(3) 0.047(3) 0.007(2) 0.020(3) 0.028(3)
C8 0.070(4) 0.061(3) 0.061(3) -0.003(3) -0.013(3) 0.025(3)
C9 0.055(3) 0.046(3) 0.055(3) -0.009(2) -0.007(3) 0.007(2)
C11 0.059(3) 0.043(2) 0.038(2) 0.000(2) 0.008(2) 0.002(2)
C12 0.035(2) 0.036(2) 0.035(2) -0.0015(19) 0.0052(19) -0.0055(18)
C13 0.029(2) 0.032(2) 0.040(2) -0.0051(19) 0.0080(19) -0.0044(17)
C14 0.024(2) 0.034(2) 0.043(2) -0.0065(19) 0.0098(19) -0.0056(17)
C15 0.038(2) 0.034(2) 0.053(3) -0.002(2) 0.016(2) 0.0035(19)
C16 0.040(3) 0.038(2) 0.074(3) -0.006(2) 0.019(3) -0.002(2)
C17 0.043(3) 0.050(3) 0.060(3) -0.018(2) 0.019(2) -0.002(2)
C18 0.034(2) 0.047(3) 0.048(3) -0.015(2) 0.011(2) -0.010(2)
C21 0.049(3) 0.057(3) 0.057(3) -0.002(2) 0.009(2) -0.015(2)
C22 0.039(2) 0.046(2) 0.032(2) -0.006(2) 0.010(2) -0.004(2)
C23 0.032(2) 0.061(3) 0.031(2) -0.005(2) 0.0114(19) -0.006(2)
C24 0.041(3) 0.080(3) 0.048(3) -0.018(3) 0.008(2) -0.006(3)
C25 0.045(3) 0.113(5) 0.040(3) -0.009(3) 0.010(2) 0.005(3)
C26 0.048(3) 0.100(4) 0.050(3) 0.012(3) 0.015(3) 0.019(3)
C27 0.035(2) 0.066(3) 0.041(3) 0.012(2) 0.013(2) 0.006(2)
C28 0.028(2) 0.052(3) 0.030(2) 0.000(2) 0.0092(18) 0.003(2)
C31 0.045(3) 0.053(3) 0.071(3) 0.004(2) 0.025(3) 0.003(2)
C32 0.035(2) 0.031(2) 0.043(2) -0.0009(18) 0.011(2) -0.0006(18)
C33 0.036(2) 0.035(2) 0.035(2) -0.0036(18) 0.0110(19) -0.0062(19)
C34 0.038(2) 0.051(3) 0.042(3) -0.002(2) 0.014(2) -0.003(2)
C35 0.045(3) 0.055(3) 0.050(3) 0.006(2) 0.021(2) -0.005(2)
C36 0.059(3) 0.040(2) 0.041(3) 0.010(2) 0.012(2) 0.000(2)
C37 0.042(2) 0.039(2) 0.040(2) 0.0055(19) 0.014(2) 0.000(2)
C38 0.035(2) 0.030(2) 0.030(2) -0.0023(17) 0.0083(18) -0.0063(18)
N1 0.0296(18) 0.0274(17) 0.042(2) 0.0017(15) 0.0097(16) -0.0004(14)
N2 0.0307(18) 0.0294(17) 0.0354(19) -0.0017(14) 0.0084(15) -0.0006(14)
N3 0.0370(19) 0.0348(18) 0.0343(18) -0.0012(15) 0.0113(16) -0.0031(16)
N4 0.0324(19) 0.0391(19) 0.0340(19) 0.0053(15) 0.0122(16) 0.0009(15)
N5 0.040(2) 0.0272(17) 0.046(2) 0.0044(15) 0.0170(17) -0.0008(15)
N6 0.0315(18) 0.0283(17) 0.0382(19) 0.0035(14) 0.0109(16) 0.0023(14)
Cl1 0.0448(6) 0.0359(5) 0.0488(6) 0.0029(5) 0.0178(5) -0.0022(5)
Cl2 0.0540(7) 0.0388(6) 0.0409(6) -0.0041(5) 0.0145(5) -0.0005(5)
Nb1 0.0339(2) 0.02793(18) 0.0355(2) 0.00067(17) 0.00751(16) -0.00074(17)
B1 0.039(3) 0.029(2) 0.038(3) -0.001(2) 0.011(2) 0.002(2)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.489(5) . ?
C2 C3 1.304(5) . ?
C2 Nb1 2.065(4) . ?
C3 C4 1.446(5) . ?
C3 Nb1 2.082(4) . ?
C4 C5 1.384(5) . ?
C4 C9 1.389(5) . ?
C5 C6 1.388(5) . ?
C6 C7 1.389(6) . ?
C7 C8 1.347(6) . ?
C8 C9 1.397(6) . ?
C11 C12 1.478(5) . ?
C12 N1 1.354(5) . ?
C12 C13 1.413(5) . ?
C13 C18 1.402(5) . ?
C13 C14 1.408(5) . ?
C14 N2 1.369(4) . ?
C14 C15 1.400(5) . ?
C15 C16 1.371(5) . ?
C16 C17 1.404(6) . ?
C17 C18 1.355(5) . ?
C21 C22 1.479(5) . ?
C22 N3 1.334(4) . ?
C22 C23 1.407(5) . ?
C23 C28 1.405(5) . ?
C23 C24 1.427(5) . ?
C24 C25 1.403(7) . ?
C25 C26 1.377(7) . ?
C26 C27 1.406(6) . ?
C27 C28 1.405(5) . ?
C28 N4 1.374(4) . ?
C31 C32 1.509(5) . ?
C32 N5 1.345(5) . ?
C32 C33 1.392(5) . ?
C33 C34 1.414(5) . ?
C33 C38 1.415(5) . ?
C34 C35 1.375(5) . ?
C35 C36 1.417(5) . ?
C36 C37 1.367(5) . ?
C37 C38 1.407(5) . ?
C38 N6 1.346(4) . ?
N1 N2 1.370(4) . ?
N1 Nb1 2.265(3) . ?
N2 B1 1.537(5) . ?
N3 N4 1.383(4) . ?
N3 Nb1 2.379(3) . ?
N4 B1 1.530(5) . ?
N5 N6 1.389(4) . ?
N5 Nb1 2.246(3) . ?
N6 B1 1.534(5) . ?
Cl1 Nb1 2.3768(11) . ?
Cl2 Nb1 2.3969(11) . ?

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
C3 C2 C1 143.8(4) . . ?
C3 C2 Nb1 72.4(2) . . ?
C1 C2 Nb1 143.8(3) . . ?
C2 C3 C4 141.7(4) . . ?
C2 C3 Nb1 71.0(2) . . ?
C4 C3 Nb1 147.1(3) . . ?
C5 C4 C9 118.6(4) . . ?
C5 C4 C3 120.3(4) . . ?
C9 C4 C3 121.1(4) . . ?
C4 C5 C6 120.3(4) . . ?
C5 C6 C7 120.3(4) . . ?
C8 C7 C6 119.8(4) . . ?
C7 C8 C9 120.6(4) . . ?
C4 C9 C8 120.4(4) . . ?
N1 C12 C13 109.2(3) . . ?
N1 C12 C11 124.5(4) . . ?
C13 C12 C11 126.3(4) . . ?
C18 C13 C14 119.9(4) . . ?
C18 C13 C12 134.5(4) . . ?
C14 C13 C12 105.5(3) . . ?
N2 C14 C15 130.3(4) . . ?
N2 C14 C13 107.8(3) . . ?
C15 C14 C13 121.9(4) . . ?
C16 C15 C14 116.3(4) . . ?
C15 C16 C17 122.2(4) . . ?
C18 C17 C16 121.7(4) . . ?
C17 C18 C13 118.0(4) . . ?
N3 C22 C23 109.6(4) . . ?
N3 C22 C21 124.7(4) . . ?
C23 C22 C21 125.7(4) . . ?
C28 C23 C22 106.2(3) . . ?
C28 C23 C24 120.2(4) . . ?
C22 C23 C24 133.6(4) . . ?
C25 C24 C23 116.5(4) . . ?
C26 C25 C24 121.6(4) . . ?
C25 C26 C27 123.6(5) . . ?
C28 C27 C26 114.8(4) . . ?
N4 C28 C23 106.9(3) . . ?
N4 C28 C27 129.9(4) . . ?
C23 C28 C27 123.1(4) . . ?
N5 C32 C33 110.1(3) . . ?
N5 C32 C31 124.3(4) . . ?
C33 C32 C31 125.6(4) . . ?
C32 C33 C34 134.7(4) . . ?
C32 C33 C38 105.0(3) . . ?
C34 C33 C38 120.3(4) . . ?
C35 C34 C33 118.1(4) . . ?
C34 C35 C36 120.2(4) . . ?
C37 C36 C35 123.6(4) . . ?
C36 C37 C38 116.2(4) . . ?
N6 C38 C37 129.9(4) . . ?
N6 C38 C33 108.5(3) . . ?
C37 C38 C33 121.6(4) . . ?
C12 N1 N2 108.1(3) . . ?
C12 N1 Nb1 131.4(3) . . ?
N2 N1 Nb1 120.4(2) . . ?
C14 N2 N1 109.4(3) . . ?
C14 N2 B1 129.1(3) . . ?
N1 N2 B1 121.3(3) . . ?
C22 N3 N4 108.0(3) . . ?
C22 N3 Nb1 134.3(3) . . ?
N4 N3 Nb1 117.7(2) . . ?
C28 N4 N3 109.3(3) . . ?
C28 N4 B1 129.6(3) . . ?
N3 N4 B1 121.1(3) . . ?
C32 N5 N6 107.5(3) . . ?
C32 N5 Nb1 131.7(3) . . ?
N6 N5 Nb1 120.7(2) . . ?
C38 N6 N5 108.8(3) . . ?
C38 N6 B1 130.3(3) . . ?
N5 N6 B1 120.6(3) . . ?
C2 Nb1 C3 36.66(13) . . ?
C2 Nb1 N5 82.63(13) . . ?
C3 Nb1 N5 107.18(13) . . ?
C2 Nb1 N1 82.17(13) . . ?
C3 Nb1 N1 111.97(13) . . ?
N5 Nb1 N1 82.03(11) . . ?
C2 Nb1 Cl1 108.77(11) . . ?
C3 Nb1 Cl1 88.77(11) . . ?
N5 Nb1 Cl1 163.25(8) . . ?
N1 Nb1 Cl1 87.33(8) . . ?
C2 Nb1 N3 157.67(13) . . ?
C3 Nb1 N3 165.55(12) . . ?
N5 Nb1 N3 81.17(11) . . ?
N1 Nb1 N3 80.46(10) . . ?
Cl1 Nb1 N3 84.35(8) . . ?
C2 Nb1 Cl2 110.37(11) . . ?
C3 Nb1 Cl2 84.90(10) . . ?
N5 Nb1 Cl2 86.43(8) . . ?
N1 Nb1 Cl2 161.76(8) . . ?
Cl1 Nb1 Cl2 100.39(4) . . ?
N3 Nb1 Cl2 83.87(8) . . ?
N4 B1 N6 110.4(3) . . ?
N4 B1 N2 109.1(3) . . ?
N6 B1 N2 109.3(3) . . ?