#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:57:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179712 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/14/7001483.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_7001483
loop_
_publ_author_name
'Neshat, Abdollah'
'Seambos, Cheryl L.'
'Beck, John F.'
'Schmidt, Joseph A. R.'
_publ_section_title
;
 Mono-anionic acetophenone imine ligands: synthesis, ortho-lithiation
 and first examples of group (v) metal complexes
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              4987
_journal_page_last               5000
_journal_paper_doi               10.1039/b903836a
_journal_year                    2009
_chemical_formula_sum            'C38 H49 Cl N3 Nb O4'
_chemical_formula_weight         740.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.678(1)
_cell_length_b                   11.2151(7)
_cell_length_c                   36.896(2)
_cell_measurement_reflns_used    8960
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.02
_cell_measurement_theta_min      2.21
_cell_volume                     7315.0(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       ω-scan
_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  0.1337
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            78495
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.511
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         9101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0490P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                5430
_reflns_number_total             9101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903836a.txt
_cod_data_source_block           (4)2Nb(N-2,6-iPr2C6H3)Cl_(18)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        7314.9(8)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7001483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
Nb1 Nb 0.544346(14) 0.62730(2) 0.112772(7) 0.01566(7) Uani 1 1 d . . .
Cl1 Cl 0.59384(4) 0.42934(6) 0.09786(2) 0.02351(17) Uani 1 1 d . . .
O1 O 0.34654(12) 0.5749(2) 0.09510(6) 0.0349(6) Uani 1 1 d . . .
O2 O 0.27573(12) 0.5660(2) 0.04223(6) 0.0383(6) Uani 1 1 d . . .
O3 O 0.42273(13) 0.85160(18) 0.05792(6) 0.0339(6) Uani 1 1 d . . .
O4 O 0.44189(16) 1.0505(2) 0.04719(7) 0.0502(8) Uani 1 1 d . . .
N1 N 0.47299(13) 0.5909(2) 0.14486(6) 0.0190(5) Uani 1 1 d . . .
N2 N 0.62130(13) 0.6753(2) 0.05903(6) 0.0171(5) Uani 1 1 d . . .
N3 N 0.60878(13) 0.7312(2) 0.15897(7) 0.0218(6) Uani 1 1 d . . .
C1 C 0.41499(16) 0.5658(3) 0.16963(8) 0.0204(6) Uani 1 1 d . . .
C2 C 0.39272(17) 0.4469(3) 0.17554(8) 0.0238(7) Uani 1 1 d . . .
C3 C 0.33532(19) 0.4257(3) 0.20054(9) 0.0321(8) Uani 1 1 d . . .
H3A H 0.3201 0.3477 0.2050 0.039 Uiso 1 1 calc R . .
C4 C 0.30059(19) 0.5178(3) 0.21880(9) 0.0347(8) Uani 1 1 d . . .
H4A H 0.2621 0.5017 0.2353 0.042 Uiso 1 1 calc R . .
C5 C 0.32293(18) 0.6342(3) 0.21268(9) 0.0319(8) Uani 1 1 d . . .
H5A H 0.2988 0.6955 0.2251 0.038 Uiso 1 1 calc R . .
C6 C 0.38031(17) 0.6621(3) 0.18848(8) 0.0235(7) Uani 1 1 d . . .
C7 C 0.42933(18) 0.3441(3) 0.15536(9) 0.0283(8) Uani 1 1 d . . .
H7A H 0.4669 0.3782 0.1388 0.034 Uiso 1 1 calc R . .
C8 C 0.3728(3) 0.2763(4) 0.13265(14) 0.0785(17) Uani 1 1 d . . .
H8A H 0.3980 0.2122 0.1203 0.118 Uiso 1 1 calc R . .
H8B H 0.3505 0.3291 0.1152 0.118 Uiso 1 1 calc R . .
H8C H 0.3339 0.2444 0.1480 0.118 Uiso 1 1 calc R . .
C9 C 0.4703(3) 0.2606(4) 0.18020(12) 0.0840(18) Uani 1 1 d . . .
H9A H 0.5064 0.3045 0.1943 0.126 Uiso 1 1 calc R . .
H9B H 0.4961 0.2012 0.1661 0.126 Uiso 1 1 calc R . .
H9C H 0.4346 0.2227 0.1961 0.126 Uiso 1 1 calc R . .
C10 C 0.40424(19) 0.7896(3) 0.18133(9) 0.0289(8) Uani 1 1 d . . .
H10A H 0.4559 0.7872 0.1717 0.035 Uiso 1 1 calc R . .
C11 C 0.3538(2) 0.8451(3) 0.15210(10) 0.0378(9) Uani 1 1 d . . .
H11A H 0.3541 0.7952 0.1309 0.057 Uiso 1 1 calc R . .
H11B H 0.3727 0.9227 0.1459 0.057 Uiso 1 1 calc R . .
H11C H 0.3031 0.8520 0.1611 0.057 Uiso 1 1 calc R . .
C12 C 0.4055(2) 0.8677(3) 0.21541(10) 0.0455(10) Uani 1 1 d . . .
H12A H 0.4381 0.8322 0.2332 0.068 Uiso 1 1 calc R . .
H12B H 0.3553 0.8741 0.2251 0.068 Uiso 1 1 calc R . .
H12C H 0.4240 0.9456 0.2093 0.068 Uiso 1 1 calc R . .
C13 C 0.46968(15) 0.6211(3) 0.06614(8) 0.0192(6) Uani 1 1 d . . .
C14 C 0.39354(17) 0.5956(3) 0.06566(8) 0.0234(7) Uani 1 1 d . . .
C15 C 0.35098(17) 0.5909(3) 0.03413(9) 0.0274(7) Uani 1 1 d . . .
C16 C 0.38131(18) 0.6083(3) 0.00076(9) 0.0278(7) Uani 1 1 d . . .
H16A H 0.3523 0.6037 -0.0202 0.033 Uiso 1 1 calc R . .
C17 C 0.45874(18) 0.6336(3) -0.00020(8) 0.0258(6) Uani 1 1 d . . .
H17A H 0.4821 0.6453 -0.0225 0.031 Uiso 1 1 calc R . .
C18 C 0.50185(16) 0.6419(2) 0.03122(8) 0.0198(6) Uani 1 1 d . . .
C19 C 0.27250(19) 0.5691(4) 0.08111(10) 0.0487(11) Uani 1 1 d . . .
H19A H 0.2438 0.6381 0.0890 0.058 Uiso 1 1 calc R . .
H19B H 0.2473 0.4981 0.0901 0.058 Uiso 1 1 calc R . .
C20 C 0.58300(17) 0.6764(2) 0.02932(8) 0.0202(6) Uani 1 1 d . . .
C21 C 0.61116(19) 0.7140(3) -0.00754(8) 0.0298(8) Uani 1 1 d . . .
H21A H 0.6639 0.7340 -0.0060 0.045 Uiso 1 1 calc R . .
H21B H 0.5831 0.7822 -0.0157 0.045 Uiso 1 1 calc R . .
H21C H 0.6044 0.6496 -0.0244 0.045 Uiso 1 1 calc R . .
C22 C 0.70356(16) 0.7115(3) 0.05998(8) 0.0217(7) Uani 1 1 d . . .
C23 C 0.70823(19) 0.8474(3) 0.05783(10) 0.0337(8) Uani 1 1 d . . .
H23A H 0.6767 0.8819 0.0763 0.051 Uiso 1 1 calc R . .
H23B H 0.6912 0.8735 0.0344 0.051 Uiso 1 1 calc R . .
H23C H 0.7596 0.8722 0.0615 0.051 Uiso 1 1 calc R . .
C24 C 0.75342(18) 0.6502(3) 0.03117(9) 0.0289(8) Uani 1 1 d . . .
H24A H 0.7369 0.6736 0.0074 0.043 Uiso 1 1 calc R . .
H24B H 0.7492 0.5653 0.0336 0.043 Uiso 1 1 calc R . .
H24C H 0.8052 0.6736 0.0346 0.043 Uiso 1 1 calc R . .
C25 C 0.73397(18) 0.6710(3) 0.09667(9) 0.0351(8) Uani 1 1 d . . .
H25A H 0.7047 0.7070 0.1157 0.053 Uiso 1 1 calc R . .
H25B H 0.7859 0.6949 0.0990 0.053 Uiso 1 1 calc R . .
H25C H 0.7304 0.5858 0.0984 0.053 Uiso 1 1 calc R . .
C26 C 0.52242(16) 0.8260(3) 0.10535(8) 0.0189(6) Uani 1 1 d . . .
C27 C 0.48135(17) 0.8919(3) 0.08013(8) 0.0238(7) Uani 1 1 d . . .
C28 C 0.4896(2) 1.0131(3) 0.07394(9) 0.0313(8) Uani 1 1 d . . .
C29 C 0.5378(2) 1.0827(3) 0.09384(10) 0.0333(8) Uani 1 1 d . . .
H29A H 0.5450 1.1632 0.0888 0.040 Uiso 1 1 calc R . .
C30 C 0.57517(18) 1.0256(3) 0.12196(9) 0.0282(8) Uani 1 1 d . . .
H30A H 0.6060 1.0698 0.1373 0.034 Uiso 1 1 calc R . .
C31 C 0.56736(16) 0.9028(2) 0.12764(8) 0.0198(6) Uani 1 1 d . . .
C32 C 0.4113(2) 0.9429(3) 0.03196(10) 0.0417(10) Uani 1 1 d . . .
H32A H 0.3578 0.9525 0.0270 0.050 Uiso 1 1 calc R . .
H32B H 0.4369 0.9233 0.0095 0.050 Uiso 1 1 calc R . .
C33 C 0.60458(16) 0.8467(3) 0.15881(8) 0.0224(7) Uani 1 1 d . . .
C34 C 0.6316(2) 0.9296(3) 0.18847(10) 0.0381(9) Uani 1 1 d . . .
H34A H 0.6551 0.8838 0.2074 0.057 Uiso 1 1 calc R . .
H34B H 0.5893 0.9726 0.1982 0.057 Uiso 1 1 calc R . .
H34C H 0.6676 0.9849 0.1786 0.057 Uiso 1 1 calc R . .
C35 C 0.64344(19) 0.6627(3) 0.19020(8) 0.0276(7) Uani 1 1 d . . .
C36 C 0.72513(19) 0.7038(3) 0.19823(10) 0.0383(9) Uani 1 1 d . . .
H36A H 0.7248 0.7863 0.2052 0.057 Uiso 1 1 calc R . .
H36B H 0.7556 0.6940 0.1769 0.057 Uiso 1 1 calc R . .
H36C H 0.7457 0.6567 0.2176 0.057 Uiso 1 1 calc R . .
C37 C 0.5913(2) 0.6708(3) 0.22355(9) 0.0408(9) Uani 1 1 d . . .
H37A H 0.5414 0.6441 0.2171 0.061 Uiso 1 1 calc R . .
H37B H 0.5889 0.7519 0.2317 0.061 Uiso 1 1 calc R . .
H37C H 0.6109 0.6213 0.2426 0.061 Uiso 1 1 calc R . .
C38 C 0.6480(2) 0.5316(3) 0.17968(9) 0.0336(8) Uani 1 1 d . . .
H38A H 0.5981 0.5021 0.1746 0.050 Uiso 1 1 calc R . .
H38B H 0.6696 0.4868 0.1993 0.050 Uiso 1 1 calc R . .
H38C H 0.6790 0.5231 0.1585 0.050 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 0.0000 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
_geom_angle_publ_flag
N1 Nb1 C13 95.12(11) . . ?
N1 Nb1 C26 100.60(10) . . ?
C13 Nb1 C26 80.36(10) . . ?
N1 Nb1 N3 88.56(10) . . ?
C13 Nb1 N3 151.99(9) . . ?
C26 Nb1 N3 71.68(9) . . ?
N1 Nb1 Cl1 101.24(8) . . ?
C13 Nb1 Cl1 90.59(8) . . ?
C26 Nb1 Cl1 157.00(7) . . ?
N3 Nb1 Cl1 115.96(6) . . ?
N1 Nb1 N2 167.94(9) . . ?
C13 Nb1 N2 72.82(9) . . ?
C26 Nb1 N2 77.50(9) . . ?
N3 Nb1 N2 101.94(8) . . ?
Cl1 Nb1 N2 79.64(6) . . ?
C14 O1 C19 106.1(3) . . ?
C15 O2 C19 104.3(2) . . ?
C27 O3 C32 105.6(2) . . ?
C28 O4 C32 105.0(2) . . ?
C1 N1 Nb1 177.8(2) . . ?
C20 N2 C22 121.5(2) . . ?
C20 N2 Nb1 113.37(19) . . ?
C22 N2 Nb1 124.87(18) . . ?
C33 N3 C35 122.2(3) . . ?
C33 N3 Nb1 117.6(2) . . ?
C35 N3 Nb1 119.65(18) . . ?
N1 C1 C2 119.7(3) . . ?
N1 C1 C6 118.7(3) . . ?
C2 C1 C6 121.5(3) . . ?
C3 C2 C1 118.0(3) . . ?
C3 C2 C7 120.4(3) . . ?
C1 C2 C7 121.6(3) . . ?
C4 C3 C2 121.4(3) . . ?
C3 C4 C5 120.1(3) . . ?
C4 C5 C6 121.8(3) . . ?
C5 C6 C1 117.3(3) . . ?
C5 C6 C10 121.9(3) . . ?
C1 C6 C10 120.7(3) . . ?
C9 C7 C8 110.2(4) . . ?
C9 C7 C2 112.4(3) . . ?
C8 C7 C2 111.9(3) . . ?
C6 C10 C11 110.1(3) . . ?
C6 C10 C12 113.6(3) . . ?
C11 C10 C12 110.8(3) . . ?
C14 C13 C18 114.3(3) . . ?
C14 C13 Nb1 127.7(2) . . ?
C18 C13 Nb1 117.92(19) . . ?
C13 C14 C15 123.3(3) . . ?
C13 C14 O1 127.6(3) . . ?
C15 C14 O1 109.0(3) . . ?
C16 C15 C14 122.8(3) . . ?
C16 C15 O2 127.0(3) . . ?
C14 C15 O2 110.3(3) . . ?
C15 C16 C17 116.0(3) . . ?
C18 C17 C16 121.9(3) . . ?
C17 C18 C13 121.6(3) . . ?
C17 C18 C20 120.4(3) . . ?
C13 C18 C20 118.0(3) . . ?
O1 C19 O2 109.3(3) . . ?
N2 C20 C18 117.7(3) . . ?
N2 C20 C21 126.6(3) . . ?
C18 C20 C21 115.7(3) . . ?
N2 C22 C25 106.3(2) . . ?
N2 C22 C23 108.6(2) . . ?
C25 C22 C23 108.9(3) . . ?
N2 C22 C24 114.5(2) . . ?
C25 C22 C24 106.1(3) . . ?
C23 C22 C24 112.2(3) . . ?
C27 C26 C31 110.7(3) . . ?
C27 C26 Nb1 133.5(2) . . ?
C31 C26 Nb1 115.2(2) . . ?
C28 C27 C26 125.1(3) . . ?
C28 C27 O3 107.4(3) . . ?
C26 C27 O3 127.4(3) . . ?
O4 C28 C29 126.7(3) . . ?
O4 C28 C27 110.8(3) . . ?
C29 C28 C27 122.4(3) . . ?
C28 C29 C30 115.8(3) . . ?
C29 C30 C31 121.3(3) . . ?
C30 C31 C26 124.1(3) . . ?
C30 C31 C33 119.7(3) . . ?
C26 C31 C33 116.2(3) . . ?
O3 C32 O4 106.8(3) . . ?
N3 C33 C31 117.2(3) . . ?
N3 C33 C34 126.3(3) . . ?
C31 C33 C34 116.5(3) . . ?
N3 C35 C38 108.5(2) . . ?
N3 C35 C37 109.6(3) . . ?
C38 C35 C37 107.0(3) . . ?
N3 C35 C36 111.9(3) . . ?
C38 C35 C36 106.8(3) . . ?
C37 C35 C36 112.9(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
Nb1 N1 1.777(2) . ?
Nb1 C13 2.170(3) . ?
Nb1 C26 2.278(3) . ?
Nb1 N3 2.358(2) . ?
Nb1 Cl1 2.4489(7) . ?
Nb1 N2 2.464(2) . ?
O1 C14 1.387(4) . ?
O1 C19 1.408(4) . ?
O2 C15 1.392(4) . ?
O2 C19 1.436(4) . ?
O3 C27 1.396(4) . ?
O3 C32 1.417(4) . ?
O4 C28 1.364(4) . ?
O4 C32 1.437(4) . ?
N1 C1 1.402(4) . ?
N2 C20 1.289(4) . ?
N2 C22 1.510(4) . ?
N3 C33 1.298(4) . ?
N3 C35 1.514(4) . ?
C1 C2 1.407(4) . ?
C1 C6 1.423(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.518(4) . ?
C3 C4 1.378(5) . ?
C4 C5 1.382(5) . ?
C5 C6 1.387(4) . ?
C6 C10 1.514(4) . ?
C7 C9 1.496(5) . ?
C7 C8 1.510(5) . ?
C10 C11 1.531(5) . ?
C10 C12 1.532(4) . ?
C13 C14 1.376(4) . ?
C13 C18 1.427(4) . ?
C14 C15 1.386(4) . ?
C15 C16 1.357(4) . ?
C16 C17 1.399(4) . ?
C17 C18 1.390(4) . ?
C18 C20 1.488(4) . ?
C20 C21 1.508(4) . ?
C22 C25 1.526(5) . ?
C22 C23 1.529(4) . ?
C22 C24 1.542(4) . ?
C26 C27 1.393(4) . ?
C26 C31 1.431(4) . ?
C27 C28 1.387(4) . ?
C28 C29 1.368(5) . ?
C29 C30 1.387(5) . ?
C30 C31 1.400(4) . ?
C31 C33 1.467(4) . ?
C33 C34 1.513(4) . ?
C35 C38 1.523(4) . ?
C35 C37 1.541(5) . ?
C35 C36 1.545(5) . ?
