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#$Date: 2019-11-17 10:05:16 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229252 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045592.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_7045592
loop_
_publ_author_name
'Bartalucci, Niccolò'
'Bortoluzzi, Marco'
'Pampaloni, Guido'
'Pinzino, Calogero'
'Zacchini, Stefano'
'Marchetti, Fabio'
_publ_section_title
;
 Stable coordination complexes of α-diimines with Nb(v) and Ta(v)
 halides.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3346
_journal_page_last               3355
_journal_paper_doi               10.1039/c8dt00122g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C26 H36 Cl3 N2 Nb O'
_chemical_formula_weight         591.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-04 deposited with the CCDC.
2018-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5172(8)
_cell_length_b                   21.3437(14)
_cell_length_c                   10.4112(6)
_cell_measurement_reflns_used    5773
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.007
_cell_measurement_theta_min      2.376
_cell_volume                     2781.5(3)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0903
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            37999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.908
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.9431
_exptl_absorpt_correction_T_min  0.9033
_exptl_absorpt_correction_type   empirical
_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_crystal_colour            orange
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       needle
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.896
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2528
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0475
_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)+(0.0427P)²+10.1718P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1956
_reflns_number_total             2528
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00122g2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7045585--7045593.cif.'
_cod_database_code               7045592
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.943
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'
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 . . .
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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_4
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) .
