#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:23:38 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180076 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/22/7052261.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7052261
loop_
_publ_author_name
'Pascal Oulié'
'Johannes Teichert'
'Laure Vendier'
'Céline Dablemont'
'Michel Etienne'
_publ_section_title
;
 Aromatic interactions in hydrotris(3-methylindazolyl)borate
 organoniobium complexes: control of an alkyne ligand orientation in
 the crystal
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              679
_journal_paper_doi               10.1039/b601652a
_journal_volume                  30
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H30 B Cl2 N6 Nb'
_chemical_formula_sum            'C33 H30 B Cl2 N6 Nb'
_chemical_formula_weight         685.25
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 109.858(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1301(14)
_cell_length_b                   19.875(2)
_cell_length_c                   16.4137(16)
_cell_measurement_reflns_used    3320
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.2783
_cell_measurement_theta_min      2.6892
_cell_measurement_wavelength     0.71073
_cell_volume                     3415.0(7)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25314
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         3.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.54
_exptl_absorpt_correction_T_max  0.9150
_exptl_absorpt_correction_T_min  0.8812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0472P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                3929
_reflns_number_total             6958
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b601652a.txt
_cod_data_source_block           compound
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7052261
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'
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_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_
_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) . . ?
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) . ?
