#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:01:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178969 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/98/4119860.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_4119860
loop_
_publ_author_name
'Thomas L. Gianetti'
'Robert G. Bergman'
'John Arnold'
_publ_section_title
;
 Dis-assembly of a Benzylic CF3 Group Mediated by a Niobium(III) Imido
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8145
_journal_page_last               8148
_journal_paper_doi               10.1021/ja4033007
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C66 H102 N6 Nb2'
_chemical_formula_sum            'C66 H102 N6 Nb2'
_chemical_formula_weight         1165.36
_chemical_melting_point          468(1)
_chemical_name_common            'Complex 4'
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 120.0960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.7537(15)
_cell_length_b                   19.0483(16)
_cell_length_c                   11.5495(9)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.95
_cell_volume                     3379.2(5)
_computing_cell_refinement       'Bruker APEX2 v.2009.1'
_computing_data_collection       'Bruker APEX2 v.2009.1'
_computing_data_reduction        'Bruker APEX2 v.2009.1'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0107
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30549
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_correction_T_min  0.9140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       rode
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
;
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0343P)²+5.3762P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                3082
_reflns_number_total             3204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4033007_si_002_4.cif
_cod_data_source_block           (4)
_cod_database_code               4119860
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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 0.446657(12) 0.0000 0.361415(19) 0.01479(8) Uani 1 2 d S . .
N1 N 0.34890(8) 0.07895(7) 0.22478(13) 0.0166(3) Uani 1 1 d . . .
N2 N 0.53087(13) 0.0000 0.3226(2) 0.0217(4) Uani 1 2 d S . .
C14 C 0.31247(10) 0.06641(9) 0.09344(16) 0.0195(3) Uani 1 1 d . . .
C15 C 0.30561(15) 0.0000 0.0378(2) 0.0209(5) Uani 1 2 d S . .
H15 H 0.2948 0.0000 -0.0497 0.025 Uiso 1 2 calc SR . .
C6 C 0.38851(12) 0.20490(9) 0.26861(16) 0.0237(4) Uani 1 1 d . . .
C7 C 0.46500(12) 0.19588(10) 0.24604(18) 0.0267(4) Uani 1 1 d . . .
H7 H 0.4653 0.1473 0.2184 0.032 Uiso 1 1 calc R . .
C1 C 0.33517(11) 0.14877(9) 0.26096(16) 0.0208(3) Uani 1 1 d . . .
C2 C 0.26468(12) 0.15991(10) 0.28224(18) 0.0277(4) Uani 1 1 d . B .
C4 C 0.30126(15) 0.28327(11) 0.3181(2) 0.0375(5) Uani 1 1 d . B .
H4 H 0.2899 0.3282 0.3369 0.045 Uiso 1 1 calc R . .
C5 C 0.36994(14) 0.27176(10) 0.29719(18) 0.0321(4) Uani 1 1 d . . .
H5 H 0.4048 0.3094 0.3022 0.039 Uiso 1 1 calc R . .
C16 C 0.59403(18) 0.0000 0.2772(3) 0.0375(7) Uani 1 2 d S . .
C13 C 0.27358(13) 0.12563(10) -0.00754(18) 0.0292(4) Uani 1 1 d . . .
H13A H 0.2460 0.1588 0.0219 0.044 Uiso 1 1 calc R . .
H13B H 0.2313 0.1069 -0.0929 0.044 Uiso 1 1 calc R . .
H13C H 0.3189 0.1487 -0.0155 0.044 Uiso 1 1 calc R . .
C9 C 0.55041(12) 0.20934(11) 0.37598(19) 0.0308(4) Uani 1 1 d . . .
H9A H 0.5509 0.2565 0.4054 0.046 Uiso 1 1 calc R . .
H9B H 0.5984 0.2029 0.3608 0.046 Uiso 1 1 calc R . .
H9C H 0.5556 0.1770 0.4434 0.046 Uiso 1 1 calc R . .
C8 C 0.45901(15) 0.24503(12) 0.1357(2) 0.0409(5) Uani 1 1 d . . .
H8A H 0.4039 0.2386 0.0556 0.061 Uiso 1 1 calc R . .
H8B H 0.5051 0.2342 0.1180 0.061 Uiso 1 1 calc R . .
H8C H 0.4643 0.2929 0.1648 0.061 Uiso 1 1 calc R . .
C10 C 0.20278(14) 0.10139(11) 0.2673(2) 0.0407(5) Uani 1 1 d . . .
H10 H 0.2352 0.0571 0.2888 0.049 Uiso 1 1 calc R A 8
C3 C 0.24952(14) 0.22789(11) 0.3112(2) 0.0367(5) Uani 1 1 d . . .
H3 H 0.2034 0.2359 0.3262 0.044 Uiso 1 1 calc R B .
C18 C 0.6787(3) -0.0389(3) 0.3925(5) 0.0363(13) Uani 0.500(8) 1 d P . 1
C17 C 0.5590(4) -0.0577(3) 0.1546(6) 0.0352(14) Uani 0.500(8) 1 d P . 1
H17A H 0.5946 -0.0554 0.1138 0.053 Uiso 0.500(8) 1 calc PR . 1
H17B H 0.4997 -0.0474 0.0890 0.053 Uiso 0.500(8) 1 calc PR . 1
H17C H 0.5624 -0.1040 0.1897 0.053 Uiso 0.500(8) 1 calc PR . 1
C17A C 0.6103(3) -0.0637(2) 0.2398(6) 0.0325(13) Uani 0.500(8) 1 d P . 2
H17D H 0.5589 -0.0799 0.1613 0.049 Uiso 0.500(8) 1 calc PR . 2
H17E H 0.6267 -0.0968 0.3111 0.049 Uiso 0.500(8) 1 calc PR . 2
H17F H 0.6568 -0.0590 0.2206 0.049 Uiso 0.500(8) 1 calc PR . 2
C11 C 0.1670(2) 0.10905(16) 0.3632(4) 0.0853(12) Uani 1 1 d . B 8
H11A H 0.2140 0.1190 0.4517 0.128 Uiso 1 1 calc R B 8
H11B H 0.1390 0.0661 0.3643 0.128 Uiso 1 1 calc R B 8
H11C H 0.1256 0.1468 0.3335 0.128 Uiso 1 1 calc R B 8
C12 C 0.12782(16) 0.09644(15) 0.1233(3) 0.0643(8) Uani 1 1 d . B .
H12A H 0.0873 0.0612 0.1174 0.096 Uiso 1 1 calc R . .
H12B H 0.1502 0.0840 0.0657 0.096 Uiso 1 1 calc R . .
H12C H 0.0988 0.1410 0.0962 0.096 Uiso 1 1 calc R . .
H1 H 0.5000 0.0692(15) 0.5000 0.025(7) Uiso 1 2 d S . .
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'
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
N2 Nb1 N1 106.09(6) . 6
N2 Nb1 N1 106.09(6) . .
N1 Nb1 N1 84.34(7) 6 .
N2 Nb1 Nb1 96.76(7) . 5_656
N1 Nb1 Nb1 130.54(3) 6 5_656
N1 Nb1 Nb1 130.54(3) . 5_656
N2 Nb1 H1 94.90(7) . .
N1 Nb1 H1 159.00(8) 6 .
N1 Nb1 H1 90.6(6) . .
Nb1 Nb1 H1 43.4(6) 5_656 .
C14 N1 C1 115.75(13) . .
C14 N1 Nb1 116.22(11) . .
C1 N1 Nb1 126.53(10) . .
C16 N2 Nb1 174.56(18) . .
N1 C14 C15 124.34(16) . .
N1 C14 C13 120.89(15) . .
C15 C14 C13 114.76(16) . .
C14 C15 C14 129.9(2) . 6
C14 C15 H15 115.0 . .
C14 C15 H15 115.0 6 .
C5 C6 C1 118.60(17) . .
C5 C6 C7 118.84(17) . .
C1 C6 C7 122.56(16) . .
C6 C7 C9 110.21(15) . .
C6 C7 C8 112.15(17) . .
C9 C7 C8 109.47(15) . .
C6 C7 H7 108.3 . .
C9 C7 H7 108.3 . .
C8 C7 H7 108.3 . .
C6 C1 C2 120.41(16) . .
C6 C1 N1 120.78(15) . .
C2 C1 N1 118.75(15) . .
C3 C2 C1 118.46(18) . .
C3 C2 C10 119.60(17) . .
C1 C2 C10 121.86(17) . .
C5 C4 C3 119.57(18) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.2 . .
C4 C5 C6 121.52(19) . .
C4 C5 H5 119.2 . .
C6 C5 H5 119.2 . .
C17A C16 C17A 125.2(4) . 6
C17A C16 N2 115.9(2) . .
C17A C16 N2 115.9(2) 6 .
C17A C16 C18 114.4(3) . 6
C17A C16 C18 66.1(3) 6 6
N2 C16 C18 105.8(2) . 6
C17A C16 C18 66.1(3) . .
C17A C16 C18 114.4(3) 6 .
N2 C16 C18 105.8(2) . .
C18 C16 C18 54.9(4) 6 .
C17A C16 C17 35.4(2) . .
C17A C16 C17 111.7(3) 6 .
N2 C16 C17 106.4(2) . .
C18 C16 C17 144.4(3) 6 .
C18 C16 C17 101.4(3) . .
C17A C16 C17 111.7(3) . 6
C17A C16 C17 35.4(2) 6 6
N2 C16 C17 106.4(2) . 6
C18 C16 C17 101.4(3) 6 6
C18 C16 C17 144.4(3) . 6
C17 C16 C17 83.7(4) . 6
C14 C13 H13A 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C14 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C2 C10 C12 110.87(19) . .
C2 C10 C11 112.8(2) . .
C12 C10 C11 110.0(2) . .
C2 C10 H10 107.7 . .
C12 C10 H10 107.7 . .
C11 C10 H10 107.7 . .
C4 C3 C2 121.46(19) . .
C4 C3 H3 119.3 . .
C2 C3 H3 119.3 . .
C18 C18 C16 62.53(18) 6 .
C18 C18 H18C 49.1(15) 6 .
C16 C18 H18C 102.6(18) . .
C18 C18 H18B 165(5) 6 .
C16 C18 H18B 131(5) . .
H18C C18 H18B 116(5) . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
C16 C17A H17D 109.5 . .
C16 C17A H17E 109.5 . .
H17D C17A H17E 109.5 . .
C16 C17A H17F 109.5 . .
H17D C17A H17F 109.5 . .
H17E C17A H17F 109.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 N2 1.763(2) .
Nb1 N1 2.2399(13) 6
Nb1 N1 2.2399(13) .
Nb1 Nb1 2.7846(4) 5_656
Nb1 H1 1.92(2) .
N1 C14 1.339(2) .
N1 C1 1.451(2) .
N2 C16 1.457(3) .
C14 C15 1.396(2) .
C14 C13 1.517(2) .
C15 C14 1.396(2) 6
C15 H15 0.9300 .
C6 C5 1.396(3) .
C6 C1 1.401(3) .
C6 C7 1.516(3) .
C7 C9 1.528(3) .
C7 C8 1.541(3) .
C7 H7 0.9800 .
C1 C2 1.407(2) .
C2 C3 1.397(3) .
C2 C10 1.513(3) .
C4 C5 1.374(3) .
C4 C3 1.375(3) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C16 C17A 1.366(4) .
C16 C17A 1.366(4) 6
C16 C18 1.604(5) 6
C16 C18 1.604(5) .
C16 C17 1.648(5) .
C16 C17 1.648(5) 6
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C10 C12 1.525(4) .
C10 C11 1.535(3) .
C10 H10 0.9800 .
C3 H3 0.9300 .
C18 C18 1.480(10) 6
C18 H18C 1.13(3) .
C18 H18B 0.74(8) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C17A H17D 0.9600 .
C17A H17E 0.9600 .
C17A H17F 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 232 51 ' '
2 1.000 0.000 0.500 232 51 ' '
