#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:33:25 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179729 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/25/7002582.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_7002582
loop_
_publ_author_name
'Arbaoui, Abdessamad'
'Redshaw, Carl'
'Homden, Damien M.'
'Wright, Joseph A.'
'Elsegood, Mark R. J.'
_publ_section_title
;
 Vanadium-based imido-alkoxide pro-catalysts bearing bisphenolate
 ligands for ethylene and ε-caprolactone polymerisation
;
_journal_issue                   41
_journal_name_full               'Dalton Transactions'
_journal_page_first              8911
_journal_page_last               8922
_journal_paper_doi               10.1039/b902402f
_journal_year                    2009
_chemical_formula_moiety         'C41 H60 N O3 V'
_chemical_formula_sum            'C41 H60 N O3 V'
_chemical_formula_weight         665.84
_chemical_name_common            'Compound 1'
_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                 90.7902(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9243(7)
_cell_length_b                   18.3726(11)
_cell_length_c                   20.1620(12)
_cell_measurement_reflns_used    7087
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.17
_cell_volume                     4046.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18044
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.08, Sheldrick, G.M., (2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0526P)²+4.6627P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                4038
_reflns_number_total             5043
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b902402f.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7002582
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
V1 V 0.44552(3) 0.0000 0.624720(18) 0.01999(11) Uani 1 2 d S . .
O1 O 0.34876(14) 0.0000 0.55476(8) 0.0260(3) Uani 1 2 d S . .
C1 C 0.2251(2) 0.0000 0.52865(11) 0.0289(5) Uani 1 2 d S . .
C2 C 0.21193(17) 0.06903(11) 0.48706(9) 0.0365(4) Uani 1 1 d . . .
H2A H 0.2201 0.1118 0.5159 0.055 Uiso 1 1 calc R . .
H2B H 0.1313 0.0696 0.4651 0.055 Uiso 1 1 calc R . .
H2C H 0.2759 0.0701 0.4535 0.055 Uiso 1 1 calc R . .
C3 C 0.1355(2) 0.0000 0.58597(14) 0.0427(7) Uani 1 2 d S . .
H3A H 0.1407 0.0466 0.6094 0.064 Uiso 0.50 1 calc PR . .
H3B H 0.1563 -0.0396 0.6167 0.064 Uiso 0.50 1 calc PR . .
H3C H 0.0521 -0.0070 0.5687 0.064 Uiso 0.50 1 calc PR . .
N1 N 0.37090(17) 0.0000 0.69569(10) 0.0258(4) Uani 1 2 d S . .
C5 C 0.3169(2) 0.0000 0.75740(12) 0.0291(5) Uani 1 2 d SU . .
C6 C 0.3805(4) -0.0259(3) 0.81223(19) 0.0524(13) Uani 0.50 1 d PU . .
H6 H 0.4617 -0.0436 0.8076 0.063 Uiso 0.50 1 calc PR . .
C7 C 0.3266(5) -0.0262(3) 0.8738(2) 0.0641(17) Uani 0.50 1 d PU . .
H7 H 0.3712 -0.0447 0.9109 0.077 Uiso 0.50 1 calc PR . .
C8 C 0.2087(3) 0.0000 0.88260(15) 0.0535(8) Uani 1 2 d SU . .
C9 C 0.1473(4) 0.0270(3) 0.8283(2) 0.0491(12) Uani 0.50 1 d PU . .
H9 H 0.0670 0.0457 0.8336 0.059 Uiso 0.50 1 calc PR . .
C10 C 0.1987(3) 0.0277(2) 0.76597(18) 0.0423(10) Uani 0.50 1 d PU . .
H10 H 0.1541 0.0469 0.7292 0.051 Uiso 0.50 1 calc PR . .
C11 C 0.1495(5) 0.0000 0.95072(19) 0.0905(16) Uani 1 2 d SU . .
H11A H 0.2064 0.0211 0.9834 0.136 Uiso 0.50 1 calc PR . .
H11B H 0.1300 -0.0501 0.9635 0.136 Uiso 0.50 1 calc PR . .
H11C H 0.0742 0.0289 0.9490 0.136 Uiso 0.50 1 calc PR . .
O2 O 0.54323(9) 0.07962(6) 0.62839(5) 0.0212(2) Uani 1 1 d . . .
C12 C 0.58743(13) 0.10960(8) 0.68647(7) 0.0204(3) Uani 1 1 d . . .
C13 C 0.54666(14) 0.17873(9) 0.70697(8) 0.0238(3) Uani 1 1 d . . .
C14 C 0.58841(15) 0.20297(9) 0.76883(8) 0.0277(3) Uani 1 1 d . . .
H14 H 0.5606 0.2489 0.7842 0.033 Uiso 1 1 calc R . .
C15 C 0.66925(15) 0.16316(9) 0.80947(8) 0.0266(3) Uani 1 1 d . . .
C16 C 0.71187(14) 0.09727(9) 0.78503(8) 0.0244(3) Uani 1 1 d . . .
H16 H 0.7685 0.0699 0.8111 0.029 Uiso 1 1 calc R . .
C17 C 0.67427(13) 0.07007(8) 0.72363(7) 0.0200(3) Uani 1 1 d . . .
C18 C 0.45664(16) 0.22445(9) 0.66442(9) 0.0298(4) Uani 1 1 d . . .
C19 C 0.50034(19) 0.23150(11) 0.59220(9) 0.0392(4) Uani 1 1 d . . .
H19A H 0.4429 0.2621 0.5670 0.059 Uiso 1 1 calc R . .
H19B H 0.5040 0.1831 0.5719 0.059 Uiso 1 1 calc R . .
H19C H 0.5819 0.2537 0.5919 0.059 Uiso 1 1 calc R . .
C20 C 0.32868(17) 0.18946(12) 0.66525(11) 0.0427(5) Uani 1 1 d . . .
H20A H 0.3020 0.1842 0.7112 0.064 Uiso 1 1 calc R . .
H20B H 0.3319 0.1414 0.6442 0.064 Uiso 1 1 calc R . .
H20C H 0.2706 0.2205 0.6409 0.064 Uiso 1 1 calc R . .
C21 C 0.4448(2) 0.30231(11) 0.69145(11) 0.0456(5) Uani 1 1 d . . .
H21A H 0.3915 0.3308 0.6618 0.068 Uiso 1 1 calc R . .
H21B H 0.5259 0.3250 0.6940 0.068 Uiso 1 1 calc R . .
H21C H 0.4093 0.3008 0.7358 0.068 Uiso 1 1 calc R . .
C22 C 0.70629(18) 0.19140(11) 0.87870(9) 0.0372(4) Uani 1 1 d . . .
C23 C 0.6052(3) 0.1743(3) 0.92605(12) 0.1048(15) Uani 1 1 d . . .
H23A H 0.5976 0.1214 0.9308 0.157 Uiso 1 1 calc R . .
H23B H 0.5280 0.1943 0.9089 0.157 Uiso 1 1 calc R . .
H23C H 0.6242 0.1960 0.9694 0.157 Uiso 1 1 calc R . .
C24 C 0.8251(2) 0.15740(16) 0.90353(12) 0.0616(7) Uani 1 1 d . . .
H24A H 0.8480 0.1787 0.9465 0.092 Uiso 1 1 calc R . .
H24B H 0.8900 0.1668 0.8716 0.092 Uiso 1 1 calc R . .
H24C H 0.8141 0.1048 0.9086 0.092 Uiso 1 1 calc R . .
C25 C 0.7295(4) 0.27385(15) 0.87685(15) 0.0896(12) Uani 1 1 d . . .
H25A H 0.6527 0.2992 0.8665 0.134 Uiso 1 1 calc R . .
H25B H 0.7898 0.2849 0.8427 0.134 Uiso 1 1 calc R . .
H25C H 0.7608 0.2900 0.9202 0.134 Uiso 1 1 calc R . .
C26 C 0.72948(19) 0.0000 0.69564(11) 0.0204(4) Uani 1 2 d S . .
H26 H 0.7110 0.0000 0.6469 0.024 Uiso 1 2 calc SR . .
C27 C 0.8701(2) 0.0000 0.70339(13) 0.0270(5) Uani 1 2 d S . .
H27A H 0.9026 0.0467 0.6881 0.040 Uiso 0.50 1 calc PR . .
H27B H 0.9044 -0.0395 0.6769 0.040 Uiso 0.50 1 calc PR . .
H27C H 0.8925 -0.0071 0.7502 0.040 Uiso 0.50 1 calc PR . .
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'
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
_geom_angle_publ_flag
N1 V1 O1 113.39(9) . . ?
N1 V1 O2 105.15(5) . . ?
O1 V1 O2 112.44(4) . . ?
O2 V1 O2 107.69(7) . 6 ?
C1 O1 V1 147.73(14) . . ?
O1 C1 C3 109.30(19) . . ?
O1 C1 C2 106.31(13) . 6 ?
C3 C1 C2 111.12(13) . 6 ?
O1 C1 C2 106.31(13) . . ?
C3 C1 C2 111.12(13) . . ?
C2 C1 C2 112.4(2) 6 . ?
C5 N1 V1 175.73(17) . . ?
N1 C5 C6 120.2(2) . . ?
N1 C5 C10 121.0(2) . . ?
C6 C5 C10 103.3(3) 6 . ?
C6 C5 C10 118.7(3) . . ?
C5 C6 C7 120.3(4) . . ?
C6 C7 C8 121.4(4) . . ?
C9 C8 C7 102.5(3) 6 . ?
C9 C8 C7 117.9(3) . . ?
C9 C8 C11 120.7(3) 6 . ?
C9 C8 C11 120.7(3) . . ?
C7 C8 C11 121.4(3) . . ?
C8 C9 C10 122.0(3) . . ?
C9 C10 C5 119.6(3) . . ?
C12 O2 V1 123.90(9) . . ?
O2 C12 C17 118.30(13) . . ?
O2 C12 C13 120.11(13) . . ?
C17 C12 C13 121.59(14) . . ?
C14 C13 C12 116.67(14) . . ?
C14 C13 C18 121.39(14) . . ?
C12 C13 C18 121.91(14) . . ?
C13 C14 C15 123.47(15) . . ?
C16 C15 C14 117.30(15) . . ?
C16 C15 C22 122.03(15) . . ?
C14 C15 C22 120.67(15) . . ?
C15 C16 C17 122.13(15) . . ?
C16 C17 C12 118.56(14) . . ?
C16 C17 C26 121.08(15) . . ?
C12 C17 C26 120.32(14) . . ?
C21 C18 C20 107.69(16) . . ?
C21 C18 C19 106.57(16) . . ?
C20 C18 C19 109.75(16) . . ?
C21 C18 C13 111.43(14) . . ?
C20 C18 C13 109.77(15) . . ?
C19 C18 C13 111.51(14) . . ?
C23 C22 C24 109.7(2) . . ?
C23 C22 C15 108.63(17) . . ?
C24 C22 C15 111.92(16) . . ?
C23 C22 C25 110.2(3) . . ?
C24 C22 C25 105.8(2) . . ?
C15 C22 C25 110.61(18) . . ?
C17 C26 C17 114.28(17) 6 . ?
C17 C26 C27 111.05(11) . . ?
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
V1 N1 1.657(2) . ?
V1 O1 1.7509(15) . ?
V1 O2 1.8118(11) . ?
O1 C1 1.444(3) . ?
C1 C3 1.524(3) . ?
C1 C2 1.526(2) 6 ?
C1 C2 1.526(2) . ?
N1 C5 1.384(3) . ?
C5 C6 1.382(4) . ?
C5 C10 1.401(4) . ?
C6 C7 1.380(6) . ?
C7 C8 1.389(6) . ?
C8 C9 1.369(5) . ?
C8 C11 1.526(4) . ?
C9 C10 1.383(5) . ?
O2 C12 1.3756(18) . ?
C12 C17 1.403(2) . ?
C12 C13 1.410(2) . ?
C13 C14 1.395(2) . ?
C13 C18 1.544(2) . ?
C14 C15 1.402(2) . ?
C15 C16 1.390(2) . ?
C15 C22 1.538(2) . ?
C16 C17 1.392(2) . ?
C17 C26 1.5326(19) . ?
C18 C21 1.537(2) . ?
C18 C20 1.539(3) . ?
C18 C19 1.544(3) . ?
C22 C23 1.503(3) . ?
C22 C24 1.519(3) . ?
C22 C25 1.536(4) . ?
C26 C27 1.541(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 V1 O1 C1 0.0 . . . . ?
O2 V1 O1 C1 -119.13(4) . . . . ?
O2 V1 O1 C1 119.13(4) 6 . . . ?
V1 O1 C1 C3 0.0 . . . . ?
V1 O1 C1 C2 -120.01(13) . . . 6 ?
V1 O1 C1 C2 120.01(13) . . . . ?
N1 C5 C6 C7 -179.8(4) . . . . ?
C6 C5 C6 C7 77.9(5) 6 . . . ?
C10 C5 C6 C7 -41.1(5) 6 . . . ?
C10 C5 C6 C7 1.8(6) . . . . ?
C5 C6 C7 C8 -0.7(7) . . . . ?
C6 C7 C8 C9 41.8(6) . . . 6 ?
C6 C7 C8 C9 -0.6(6) . . . . ?
C6 C7 C8 C7 -76.7(5) . . . 6 ?
C6 C7 C8 C11 -179.7(4) . . . . ?
C9 C8 C9 C10 -76.7(4) 6 . . . ?
C7 C8 C9 C10 41.1(5) 6 . . . ?
C7 C8 C9 C10 0.9(6) . . . . ?
C11 C8 C9 C10 179.9(3) . . . . ?
C8 C9 C10 C5 0.2(6) . . . . ?
N1 C5 C10 C9 -180.0(3) . . . . ?
C6 C5 C10 C9 -41.7(4) 6 . . . ?
C6 C5 C10 C9 -1.6(5) . . . . ?
C10 C5 C10 C9 76.4(4) 6 . . . ?
N1 V1 O2 C12 27.60(13) . . . . ?
O1 V1 O2 C12 151.44(11) . . . . ?
O2 V1 O2 C12 -84.15(12) 6 . . . ?
V1 O2 C12 C17 68.58(16) . . . . ?
V1 O2 C12 C13 -112.20(14) . . . . ?
O2 C12 C13 C14 175.20(14) . . . . ?
C17 C12 C13 C14 -5.6(2) . . . . ?
O2 C12 C13 C18 -2.7(2) . . . . ?
C17 C12 C13 C18 176.50(14) . . . . ?
C12 C13 C14 C15 1.5(2) . . . . ?
C18 C13 C14 C15 179.43(16) . . . . ?
C13 C14 C15 C16 2.1(3) . . . . ?
C13 C14 C15 C22 -176.80(17) . . . . ?
C14 C15 C16 C17 -1.7(2) . . . . ?
C22 C15 C16 C17 177.10(16) . . . . ?
C15 C16 C17 C12 -2.1(2) . . . . ?
C15 C16 C17 C26 175.61(15) . . . . ?
O2 C12 C17 C16 -174.82(13) . . . . ?
C13 C12 C17 C16 6.0(2) . . . . ?
O2 C12 C17 C26 7.4(2) . . . . ?
C13 C12 C17 C26 -171.80(14) . . . . ?
C14 C13 C18 C21 12.3(2) . . . . ?
C12 C13 C18 C21 -169.88(16) . . . . ?
C14 C13 C18 C20 -106.89(18) . . . . ?
C12 C13 C18 C20 70.9(2) . . . . ?
C14 C13 C18 C19 131.27(17) . . . . ?
C12 C13 C18 C19 -50.9(2) . . . . ?
C16 C15 C22 C23 -99.0(3) . . . . ?
C14 C15 C22 C23 79.8(3) . . . . ?
C16 C15 C22 C24 22.2(3) . . . . ?
C14 C15 C22 C24 -159.0(2) . . . . ?
C16 C15 C22 C25 139.9(2) . . . . ?
C14 C15 C22 C25 -41.3(3) . . . . ?
C16 C17 C26 C17 80.8(2) . . . 6 ?
C12 C17 C26 C17 -101.52(19) . . . 6 ?
C16 C17 C26 C27 -45.8(2) . . . . ?
C12 C17 C26 C27 131.90(17) . . . . ?
