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#$Date: 2016-03-25 13:52:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179868 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/64/7016428.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_7016428
loop_
_publ_author_name
'Chuchuryukin, Alexey V.'
'Huang, Rubin'
'van Faassen, Ernst E.'
'van Klink, Gerard P. M.'
'Lutz, Martin'
'Chadwick, John C.'
'Spek, Anthony L.'
'van Koten, Gerard'
_publ_section_title
;
 Mono N,C,N-pincer complexes of titanium, vanadium and niobium.
 Synthesis, structure and catalytic activity in olefin polymerisation.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8887
_journal_page_last               8895
_journal_paper_doi               10.1039/c1dt10482a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C12 H19 Cl2 N2 V, C6 H6'
_chemical_formula_sum            'C18 H25 Cl2 N2 V'
_chemical_formula_weight         391.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.975(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1127(3)
_cell_length_b                   16.9371(7)
_cell_length_c                   14.3078(4)
_cell_measurement_reflns_used    12849
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.40
_cell_volume                     1941.90(12)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19466
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0290
_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)+(0.0309P)²+2.4050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                1926
_reflns_number_total             2240
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c1dt10482a.txt
_cod_data_source_block           s3665a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7016428
loop_
_symmetry_equiv_pos_as_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'
'-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_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
V1 V 0.5000 0.68314(2) 0.2500 0.01637(11) Uani 1 2 d S
Cl1 Cl 0.28887(6) 0.74473(3) 0.15420(3) 0.03502(13) Uani 1 1 d .
N1 N 0.65604(16) 0.65432(8) 0.13675(9) 0.0202(3) Uani 1 1 d .
C1 C 0.5000 0.56524(12) 0.2500 0.0160(4) Uani 1 2 d S
C2 C 0.61575(18) 0.52462(9) 0.20521(10) 0.0186(3) Uani 1 1 d .
C3 C 0.6151(2) 0.44218(10) 0.20458(12) 0.0253(3) Uani 1 1 d .
C4 C 0.5000 0.40240(14) 0.2500 0.0295(5) Uani 1 2 d S
C5 C 0.7378(2) 0.57665(10) 0.16463(12) 0.0229(3) Uani 1 1 d .
C6 C 0.5490(2) 0.64356(11) 0.04331(12) 0.0266(4) Uani 1 1 d .
C7 C 0.7872(2) 0.71311(12) 0.12502(14) 0.0315(4) Uani 1 1 d .
H3 H 0.690(2) 0.4137(12) 0.1732(14) 0.031(5) Uiso 1 1 d .
H4 H 0.5000 0.3438(19) 0.2500 0.036(8) Uiso 1 2 d S
H5A H 0.833(2) 0.5864(11) 0.2131(13) 0.025(5) Uiso 1 1 d .
H5B H 0.778(2) 0.5539(11) 0.1118(14) 0.026(5) Uiso 1 1 d .
H6A H 0.492(3) 0.6917(13) 0.0236(15) 0.036(6) Uiso 1 1 d .
H6B H 0.615(2) 0.6262(12) -0.0040(14) 0.030(5) Uiso 1 1 d .
H6C H 0.467(2) 0.6052(12) 0.0482(13) 0.026(5) Uiso 1 1 d .
H7A H 0.865(3) 0.7186(12) 0.1841(15) 0.033(5) Uiso 1 1 d .
H7B H 0.848(3) 0.6962(12) 0.0763(15) 0.033(5) Uiso 1 1 d .
H7C H 0.730(3) 0.7649(13) 0.1054(15) 0.038(6) Uiso 1 1 d .
C8 C 0.1321(2) 0.52366(13) 0.06667(13) 0.0349(4) Uani 1 1 d .
C9 C 0.0593(2) 0.45064(13) 0.07471(13) 0.0336(4) Uani 1 1 d .
C10 C -0.0730(2) 0.42682(12) 0.00784(14) 0.0335(4) Uani 1 1 d .
H8 H 0.218(3) 0.5413(13) 0.1122(17) 0.045(6) Uiso 1 1 d .
H9 H 0.095(3) 0.4198(14) 0.1239(17) 0.044(6) Uiso 1 1 d .
H10 H -0.120(3) 0.3781(14) 0.0135(16) 0.044(6) Uiso 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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'
V V 0.3005 0.5294 '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
C1 V1 N1 77.53(3) . 2_655
C1 V1 N1 77.53(3) . .
N1 V1 N1 155.05(7) 2_655 .
C1 V1 Cl1 117.315(15) . .
N1 V1 Cl1 94.46(3) 2_655 .
N1 V1 Cl1 96.92(4) . .
C1 V1 Cl1 117.314(15) . 2_655
N1 V1 Cl1 96.92(4) 2_655 2_655
N1 V1 Cl1 94.46(4) . 2_655
Cl1 V1 Cl1 125.37(3) . 2_655
C7 N1 C6 107.97(13) . .
C7 N1 C5 108.86(13) . .
C6 N1 C5 107.68(13) . .
C7 N1 V1 115.31(11) . .
C6 N1 V1 110.93(10) . .
C5 N1 V1 105.83(9) . .
C2 C1 C2 121.02(19) 2_655 .
C2 C1 V1 119.49(9) 2_655 .
C2 C1 V1 119.49(10) . .
C3 C2 C1 119.54(15) . .
C3 C2 C5 125.73(14) . .
C1 C2 C5 114.67(14) . .
C4 C3 C2 118.89(16) . .
C4 C3 H3 120.1(12) . .
C2 C3 H3 121.0(13) . .
C3 C4 C3 122.1(2) 2_655 .
C3 C4 H4 118.95(11) 2_655 .
C3 C4 H4 118.95(11) . .
N1 C5 C2 109.00(12) . .
N1 C5 H5A 108.1(11) . .
C2 C5 H5A 108.7(11) . .
N1 C5 H5B 109.7(12) . .
C2 C5 H5B 113.3(11) . .
H5A C5 H5B 107.9(15) . .
N1 C6 H6A 110.3(13) . .
N1 C6 H6B 110.9(12) . .
H6A C6 H6B 110.1(17) . .
N1 C6 H6C 109.8(12) . .
H6A C6 H6C 107.4(17) . .
H6B C6 H6C 108.3(16) . .
N1 C7 H7A 110.2(12) . .
N1 C7 H7B 110.0(12) . .
H7A C7 H7B 108.5(17) . .
N1 C7 H7C 108.0(12) . .
H7A C7 H7C 111.4(18) . .
H7B C7 H7C 108.8(17) . .
C10 C8 C9 120.38(17) 5_565 .
C10 C8 H8 118.6(14) 5_565 .
C9 C8 H8 121.0(14) . .
C10 C9 C8 119.94(19) . .
C10 C9 H9 120.0(15) . .
C8 C9 H9 120.0(15) . .
C9 C10 C8 119.69(19) . 5_565
C9 C10 H10 119.4(14) . .
C8 C10 H10 120.9(14) 5_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 C1 1.997(2) .
V1 N1 2.2596(13) 2_655
V1 N1 2.2597(13) .
V1 Cl1 2.2734(4) .
V1 Cl1 2.2734(4) 2_655
N1 C7 1.486(2) .
N1 C6 1.487(2) .
N1 C5 1.499(2) .
C1 C2 1.3976(17) 2_655
C1 C2 1.3977(17) .
C2 C3 1.396(2) .
C2 C5 1.508(2) .
C3 C4 1.392(2) .
C3 H3 0.94(2) .
C4 C3 1.392(2) 2_655
C4 H4 0.99(3) .
C5 H5A 0.966(19) .
C5 H5B 0.95(2) .
C6 H6A 0.96(2) .
C6 H6B 0.97(2) .
C6 H6C 0.94(2) .
C7 H7A 0.98(2) .
C7 H7B 0.96(2) .
C7 H7C 1.01(2) .
C8 C10 1.382(3) 5_565
C8 C9 1.383(3) .
C8 H8 0.93(2) .
C9 C10 1.382(3) .
C9 H9 0.89(2) .
C10 C8 1.382(3) 5_565
C10 H10 0.92(2) .
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_1
_geom_torsion_site_symmetry_4
C1 V1 N1 C7 -149.74(12) . .
N1 V1 N1 C7 -149.74(12) 2_655 .
Cl1 V1 N1 C7 93.73(12) . .
Cl1 V1 N1 C7 -32.74(12) 2_655 .
C1 V1 N1 C6 87.15(10) . .
N1 V1 N1 C6 87.15(10) 2_655 .
Cl1 V1 N1 C6 -29.37(11) . .
Cl1 V1 N1 C6 -155.84(10) 2_655 .
C1 V1 N1 C5 -29.36(9) . .
N1 V1 N1 C5 -29.36(9) 2_655 .
Cl1 V1 N1 C5 -145.89(9) . .
Cl1 V1 N1 C5 87.65(9) 2_655 .
N1 V1 C1 C2 15.16(8) 2_655 2_655
N1 V1 C1 C2 -164.84(8) . 2_655
Cl1 V1 C1 C2 -73.44(7) . 2_655
Cl1 V1 C1 C2 106.56(7) 2_655 2_655
N1 V1 C1 C2 -164.84(8) 2_655 .
N1 V1 C1 C2 15.15(8) . .
Cl1 V1 C1 C2 106.56(7) . .
Cl1 V1 C1 C2 -73.44(7) 2_655 .
C2 C1 C2 C3 0.46(10) 2_655 .
V1 C1 C2 C3 -179.54(10) . .
C2 C1 C2 C5 -176.98(14) 2_655 .
V1 C1 C2 C5 3.03(14) . .
C1 C2 C3 C4 -0.9(2) . .
C5 C2 C3 C4 176.22(13) . .
C2 C3 C4 C3 0.45(10) . 2_655
C7 N1 C5 C2 162.82(13) . .
C6 N1 C5 C2 -80.38(15) . .
V1 N1 C5 C2 38.31(14) . .
C3 C2 C5 N1 153.13(15) . .
C1 C2 C5 N1 -29.63(17) . .
C10 C8 C9 C10 0.2(3) 5_565 .
C8 C9 C10 C8 -0.2(3) . 5_565
