#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:47:15 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185341 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/92/7039248.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_7039248
loop_
_publ_author_name
'Haiges, Ralf'
'Vasiliu, Monica'
'Dixon, David A.'
'Christe, Karl O.'
_publ_section_title
;
 The niobium oxoazides [NbO(N3)3], [NbO(N3)3·2CH3CN],
 [(bipy)NbO(N3)3], Cs2[NbO(N3)5] and [PPh4]2[NbO(N3)5].
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10523
_journal_page_last               10529
_journal_paper_doi               10.1039/c6dt01479h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C10 H8 N11 Nb O'
_chemical_formula_sum            'C10 H8 N11 Nb O'
_chemical_formula_weight         391.18
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Heat-sensitive, explosive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2015-08-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.4600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2393(8)
_cell_length_b                   9.8720(7)
_cell_length_c                   14.4784(11)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.2142
_cell_measurement_theta_min      3.8488
_cell_volume                     1447.59(19)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS, 2014)'
_computing_data_collection
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS, 2013)'
_computing_publication_material  'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_structure_solution    'SHELXTL XT 2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13714
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Bruker AXS, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.929
_refine_ls_abs_structure_details
;
Flack x determined using 1920 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4321
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0157P)²+1.4433P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0518
_reflns_number_gt                4097
_reflns_number_total             4321
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt01479h2.cif
_cod_data_source_block           C10H8N11NbO
_cod_depositor_comments
'Adding full bibliography for 7039248--7039250.cif.'
_cod_database_code               7039248
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_posn
_atom_site_occupancy
C C1 0.6076(3) 0.0428(3) 0.4148(3) 0.0319(7) Uani d . . 1
H H1 0.6493 -0.0005 0.47 0.038 Uiso calc U R 1
C C2 0.5823(3) -0.0316(3) 0.3334(3) 0.0413(9) Uani d . . 1
H H2 0.6053 -0.1248 0.3329 0.05 Uiso calc U R 1
C C3 0.5231(3) 0.0312(4) 0.2526(3) 0.0391(9) Uani d . . 1
H H3 0.5076 -0.0176 0.1955 0.047 Uiso calc U R 1
C C4 0.4866(3) 0.1659(3) 0.2559(2) 0.0283(6) Uani d . . 1
H H4 0.4445 0.2104 0.2014 0.034 Uiso calc U R 1
C C5 0.5124(3) 0.2357(3) 0.34061(18) 0.0178(5) Uani d . . 1
C C6 0.4721(2) 0.3776(3) 0.35181(18) 0.0174(5) Uani d . . 1
C C7 0.4131(3) 0.4572(3) 0.2781(2) 0.0273(6) Uani d . . 1
H H7 0.3944 0.4208 0.2168 0.033 Uiso calc U R 1
C C8 0.3819(3) 0.5906(4) 0.2955(3) 0.0384(8) Uani d . . 1
H H8 0.3418 0.6466 0.246 0.046 Uiso calc U R 1
C C9 0.4090(4) 0.6413(3) 0.3842(3) 0.0390(8) Uani d . . 1
H H9 0.3894 0.7329 0.3969 0.047 Uiso calc U R 1
C C10 0.4657(3) 0.5562(3) 0.4553(2) 0.0291(6) Uani d . . 1
H H10 0.4828 0.5906 0.5172 0.035 Uiso calc U R 1
N N1 0.4469(3) 0.2276(3) 0.58490(18) 0.0283(5) Uani d . . 1
N N2 0.3331(3) 0.2661(3) 0.57043(19) 0.0273(5) Uani d . . 1
N N3 0.2248(3) 0.2976(3) 0.5599(3) 0.0421(7) Uani d . . 1
N N4 0.6364(4) 0.4405(5) 0.6544(2) 0.0581(11) Uani d . . 1
N N5 0.6925(2) 0.5296(3) 0.69924(17) 0.0255(5) Uani d . . 1
N N6 0.7410(3) 0.6151(3) 0.7438(2) 0.0327(6) Uani d . . 1
N N7 0.7732(3) 0.3923(3) 0.4935(2) 0.0361(7) Uani d . . 1
N N8 0.7679(3) 0.4966(4) 0.4467(2) 0.0354(7) Uani d . . 1
N N9 0.7673(3) 0.5922(4) 0.4024(2) 0.0462(9) Uani d . . 1
N N10 0.5752(2) 0.1751(2) 0.41873(18) 0.0213(5) Uani d . . 1
N N11 0.4974(2) 0.4268(2) 0.43987(16) 0.0199(4) Uani d . . 1
Nb Nb1 0.62665(2) 0.29359(3) 0.55434(2) 0.02723(7) Uani d . . 1
O O1 0.7244(3) 0.1615(4) 0.5998(2) 0.0513(7) Uani d . . 1
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'
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
N10 C1 C2 122.3(3)
N10 C1 H1 118.9
C2 C1 H1 118.9
C1 C2 C3 119.2(3)
C1 C2 H2 120.4
C3 C2 H2 120.4
C2 C3 C4 119.2(3)
C2 C3 H3 120.4
C4 C3 H3 120.4
C3 C4 C5 119.2(3)
C3 C4 H4 120.4
C5 C4 H4 120.4
N10 C5 C4 121.3(3)
N10 C5 C6 115.7(2)
C4 C5 C6 123.0(3)
N11 C6 C7 121.5(3)
N11 C6 C5 115.2(2)
C7 C6 C5 123.3(3)
C8 C7 C6 118.9(3)
C8 C7 H7 120.6
C6 C7 H7 120.6
C9 C8 C7 119.9(3)
C9 C8 H8 120.1
C7 C8 H8 120.1
C8 C9 C10 118.6(3)
C8 C9 H9 120.7
C10 C9 H9 120.7
N11 C10 C9 122.5(3)
N11 C10 H10 118.8
C9 C10 H10 118.8
N2 N1 Nb1 136.7(2)
N3 N2 N1 176.6(3)
N5 N4 Nb1 151.9(3)
N6 N5 N4 176.9(3)
N8 N7 Nb1 130.3(2)
N9 N8 N7 177.5(4)
C1 N10 C5 118.8(3)
C1 N10 Nb1 120.3(2)
C5 N10 Nb1 120.90(18)
C10 N11 C6 118.7(3)
C10 N11 Nb1 122.4(2)
C6 N11 Nb1 118.12(18)
O1 Nb1 N4 107.66(17)
O1 Nb1 N1 99.60(13)
N4 Nb1 N1 91.41(12)
O1 Nb1 N7 95.81(14)
N4 Nb1 N7 90.26(13)
N1 Nb1 N7 163.20(11)
O1 Nb1 N10 89.31(12)
N4 Nb1 N10 163.03(14)
N1 Nb1 N10 85.53(10)
N7 Nb1 N10 88.02(10)
O1 Nb1 N11 158.00(12)
N4 Nb1 N11 93.79(15)
N1 Nb1 N11 84.30(9)
N7 Nb1 N11 78.91(10)
N10 Nb1 N11 69.31(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N10 1.350(4)
C1 C2 1.381(5)
C1 H1 0.95
C2 C3 1.383(6)
C2 H2 0.95
C3 C4 1.384(5)
C3 H3 0.95
C4 C5 1.397(4)
C4 H4 0.95
C5 N10 1.355(4)
C5 C6 1.476(4)
C6 N11 1.353(3)
C6 C7 1.390(4)
C7 C8 1.387(5)
C7 H7 0.95
C8 C9 1.368(6)
C8 H8 0.95
C9 C10 1.389(5)
C9 H9 0.95
C10 N11 1.345(4)
C10 H10 0.95
N1 N2 1.214(4)
N1 Nb1 2.061(3)
N2 N3 1.139(4)
N4 N5 1.189(4)
N4 Nb1 2.042(3)
N5 N6 1.132(4)
N7 N8 1.229(5)
N7 Nb1 2.090(3)
N8 N9 1.141(5)
N10 Nb1 2.280(2)
N11 Nb1 2.362(2)
Nb1 O1 1.715(3)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N10 C1 C2 C3 0.8(5)
C1 C2 C3 C4 -2.2(5)
C2 C3 C4 C5 1.0(5)
C3 C4 C5 N10 1.6(4)
C3 C4 C5 C6 -177.3(3)
N10 C5 C6 N11 -3.1(3)
C4 C5 C6 N11 175.9(2)
N10 C5 C6 C7 176.5(3)
C4 C5 C6 C7 -4.5(4)
N11 C6 C7 C8 1.2(4)
C5 C6 C7 C8 -178.4(3)
C6 C7 C8 C9 -0.3(5)
C7 C8 C9 C10 -1.0(5)
C8 C9 C10 N11 1.4(5)
C2 C1 N10 C5 1.8(4)
C2 C1 N10 Nb1 -177.8(2)
C4 C5 N10 C1 -3.0(4)
C6 C5 N10 C1 176.0(3)
C4 C5 N10 Nb1 176.6(2)
C6 C5 N10 Nb1 -4.3(3)
C9 C10 N11 C6 -0.5(4)
C9 C10 N11 Nb1 169.1(2)
C7 C6 N11 C10 -0.9(4)
C5 C6 N11 C10 178.8(2)
C7 C6 N11 Nb1 -170.9(2)
C5 C6 N11 Nb1 8.8(3)
