#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:41:51 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179858 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/54/7015480.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_7015480
loop_
_publ_author_name
'Mu, Jing-Shan'
'Wang, Yong-Xia'
'Li, Bai-Xiang'
'Li, Yue-Sheng'
_publ_section_title
;
 Synthesis of vanadium(III) complexes bearing iminopyrrolyl ligands and
 their role as thermal robust ethylene (co)polymerization catalysts.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3490
_journal_page_last               3497
_journal_paper_doi               10.1039/c0dt01650k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C38 H50 Cl N4 O V'
_chemical_formula_weight         665.21
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0190(9)
_cell_length_b                   14.8900(12)
_cell_length_c                   22.0694(18)
_cell_measurement_reflns_used    3417
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.34
_cell_volume                     3534.5(5)
_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      185(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX 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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9803
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.9709
_exptl_absorpt_correction_T_min  0.9109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0513
_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)+(0.0782P)²+5.1968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                2999
_reflns_number_total             3489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01650k.txt
_cod_data_source_block           t012
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7015480
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
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V -1.0000 -0.15245(4) -0.7500 0.02273(19) Uani 1 2 d S . .
Cl1 Cl -1.0000 -0.00020(6) -0.7500 0.0398(3) Uani 1 2 d S . .
O1 O -1.0000 -0.29581(15) -0.7500 0.0272(5) Uani 1 2 d S . .
N1 N -1.15821(18) -0.16037(13) -0.71578(9) 0.0249(4) Uani 1 1 d . . .
N2 N -0.92016(18) -0.15413(12) -0.65106(9) 0.0221(4) Uani 1 1 d . . .
C1 C -1.2833(2) -0.16093(17) -0.73453(12) 0.0311(6) Uani 1 1 d . . .
H1 H -1.3269 -0.1639 -0.7766 0.037 Uiso 1 1 calc R . .
C2 C -1.3399(2) -0.15653(17) -0.68438(13) 0.0349(6) Uani 1 1 d . . .
H2 H -1.4267 -0.1560 -0.6859 0.042 Uiso 1 1 calc R . .
C3 C -1.2448(2) -0.15295(17) -0.63125(12) 0.0320(6) Uani 1 1 d . . .
H3 H -1.2539 -0.1496 -0.5895 0.038 Uiso 1 1 calc R . .
C4 C -1.1338(2) -0.15526(15) -0.65152(11) 0.0247(5) Uani 1 1 d . . .
C5 C -1.0078(2) -0.15157(15) -0.61997(11) 0.0245(5) Uani 1 1 d . . .
H5 H -0.9870 -0.1472 -0.5760 0.029 Uiso 1 1 calc R . .
C6 C -0.7927(2) -0.14166(17) -0.61815(10) 0.0256(5) Uani 1 1 d . . .
C7 C -0.7117(2) -0.21610(19) -0.61030(11) 0.0330(6) Uani 1 1 d . . .
C8 C -0.5864(3) -0.2012(2) -0.58327(13) 0.0449(8) Uani 1 1 d . . .
H8 H -0.5301 -0.2504 -0.5772 0.054 Uiso 1 1 calc R . .
C9 C -0.5430(3) -0.1159(3) -0.56515(14) 0.0508(8) Uani 1 1 d . . .
H9 H -0.4569 -0.1064 -0.5488 0.061 Uiso 1 1 calc R . .
C10 C -0.6245(2) -0.0452(2) -0.57085(12) 0.0401(7) Uani 1 1 d . . .
H10 H -0.5940 0.0126 -0.5568 0.048 Uiso 1 1 calc R . .
C11 C -0.7510(2) -0.05586(18) -0.59677(11) 0.0295(5) Uani 1 1 d . . .
C12 C -0.7608(3) -0.30993(19) -0.62630(13) 0.0390(7) Uani 1 1 d . . .
H12 H -0.8340 -0.3048 -0.6620 0.047 Uiso 1 1 calc R . .
C13 C -0.6670(4) -0.3734(3) -0.6463(2) 0.0678(11) Uani 1 1 d . . .
H13A H -0.6324 -0.3445 -0.6788 0.102 Uiso 1 1 calc R . .
H13B H -0.7089 -0.4292 -0.6625 0.102 Uiso 1 1 calc R . .
H13C H -0.5997 -0.3869 -0.6105 0.102 Uiso 1 1 calc R . .
C14 C -0.8073(4) -0.3490(2) -0.57169(16) 0.0611(10) Uani 1 1 d . . .
H14A H -0.7379 -0.3539 -0.5356 0.092 Uiso 1 1 calc R . .
H14B H -0.8426 -0.4088 -0.5827 0.092 Uiso 1 1 calc R . .
H14C H -0.8714 -0.3096 -0.5616 0.092 Uiso 1 1 calc R . .
C15 C -0.8371(2) 0.02436(18) -0.59811(12) 0.0324(6) Uani 1 1 d . . .
H15 H -0.9211 0.0072 -0.6228 0.039 Uiso 1 1 calc R . .
C16 C -0.7942(3) 0.1069(2) -0.62793(19) 0.0587(9) Uani 1 1 d . . .
H16A H -0.7134 0.1265 -0.6034 0.088 Uiso 1 1 calc R . .
H16B H -0.8551 0.1552 -0.6294 0.088 Uiso 1 1 calc R . .
H16C H -0.7863 0.0922 -0.6702 0.088 Uiso 1 1 calc R . .
C17 C -0.8500(3) 0.0474(2) -0.53193(14) 0.0476(8) Uani 1 1 d . . .
H17A H -0.7677 0.0600 -0.5060 0.071 Uiso 1 1 calc R . .
H17B H -0.8875 -0.0034 -0.5145 0.071 Uiso 1 1 calc R . .
H17C H -0.9032 0.1005 -0.5331 0.071 Uiso 1 1 calc R . .
C18 C -1.0663(3) -0.35255(17) -0.71369(13) 0.0342(6) Uani 1 1 d . . .
H18A H -1.1571 -0.3501 -0.7308 0.041 Uiso 1 1 calc R . .
H18B H -1.0494 -0.3327 -0.6698 0.041 Uiso 1 1 calc R . .
C19 C -1.0172(3) -0.44690(19) -0.71864(14) 0.0456(7) Uani 1 1 d . . .
H19A H -0.9437 -0.4590 -0.6849 0.055 Uiso 1 1 calc R . .
H19B H -1.0820 -0.4924 -0.7170 0.055 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'
V V 0.3005 0.5294 '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'
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 N1 173.40(11) . 2_353 ?
N1 V1 O1 86.70(6) . . ?
N1 V1 O1 86.70(6) 2_353 . ?
N1 V1 N2 79.62(7) . . ?
N1 V1 N2 100.31(7) 2_353 . ?
O1 V1 N2 89.34(5) . . ?
N1 V1 N2 100.31(7) . 2_353 ?
N1 V1 N2 79.61(7) 2_353 2_353 ?
O1 V1 N2 89.34(5) . 2_353 ?
N2 V1 N2 178.68(10) . 2_353 ?
N1 V1 Cl1 93.30(6) . . ?
N1 V1 Cl1 93.30(6) 2_353 . ?
O1 V1 Cl1 180.0 . . ?
N2 V1 Cl1 90.66(5) . . ?
N2 V1 Cl1 90.66(5) 2_353 . ?
C18 O1 C18 109.5(3) . 2_353 ?
C18 O1 V1 125.24(13) . . ?
C18 O1 V1 125.24(13) 2_353 . ?
C1 N1 C4 105.8(2) . . ?
C1 N1 V1 141.39(17) . . ?
C4 N1 V1 112.47(15) . . ?
C5 N2 C6 118.83(19) . . ?
C5 N2 V1 110.21(15) . . ?
C6 N2 V1 129.88(15) . . ?
N1 C1 C2 111.2(2) . . ?
N1 C1 H1 124.4 . . ?
C2 C1 H1 124.4 . . ?
C1 C2 C3 106.7(2) . . ?
C1 C2 H2 126.6 . . ?
C3 C2 H2 126.6 . . ?
C4 C3 C2 106.4(2) . . ?
C4 C3 H3 126.8 . . ?
C2 C3 H3 126.8 . . ?
N1 C4 C3 109.9(2) . . ?
N1 C4 C5 117.2(2) . . ?
C3 C4 C5 132.8(2) . . ?
N2 C5 C4 120.1(2) . . ?
N2 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C11 C6 C7 121.4(2) . . ?
C11 C6 N2 119.8(2) . . ?
C7 C6 N2 118.7(2) . . ?
C8 C7 C6 117.9(3) . . ?
C8 C7 C12 121.1(2) . . ?
C6 C7 C12 120.9(2) . . ?
C9 C8 C7 121.0(3) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 121.7(3) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C6 117.8(2) . . ?
C10 C11 C15 118.8(2) . . ?
C6 C11 C15 123.4(2) . . ?
C7 C12 C14 109.4(2) . . ?
C7 C12 C13 114.0(3) . . ?
C14 C12 C13 110.9(3) . . ?
C7 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C13 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C11 113.1(2) . . ?
C16 C15 C17 109.5(3) . . ?
C11 C15 C17 110.1(2) . . ?
C16 C15 H15 108.0 . . ?
C11 C15 H15 108.0 . . ?
C17 C15 H15 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O1 C18 C19 105.5(2) . . ?
O1 C18 H18A 110.6 . . ?
C19 C18 H18A 110.6 . . ?
O1 C18 H18B 110.6 . . ?
C19 C18 H18B 110.6 . . ?
H18A C18 H18B 108.8 . . ?
C19 C19 C18 103.30(17) 2_353 . ?
C19 C19 H19A 111.1 2_353 . ?
C18 C19 H19A 111.1 . . ?
C19 C19 H19B 111.1 2_353 . ?
C18 C19 H19B 111.1 . . ?
H19A C19 H19B 109.1 . . ?
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 2.0483(19) . ?
V1 N1 2.0483(19) 2_353 ?
V1 O1 2.135(2) . ?
V1 N2 2.1697(19) . ?
V1 N2 2.1697(19) 2_353 ?
V1 Cl1 2.2671(10) . ?
O1 C18 1.464(3) . ?
O1 C18 1.464(3) 2_353 ?
N1 C1 1.351(3) . ?
N1 C4 1.387(3) . ?
N2 C5 1.301(3) . ?
N2 C6 1.446(3) . ?
C1 C2 1.385(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.393(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.413(3) . ?
C5 H5 0.9500 . ?
C6 C11 1.404(4) . ?
C6 C7 1.410(3) . ?
C7 C8 1.398(4) . ?
C7 C12 1.512(4) . ?
C8 C9 1.385(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.396(4) . ?
C10 H10 0.9500 . ?
C11 C15 1.522(4) . ?
C12 C14 1.524(5) . ?
C12 C13 1.534(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.517(4) . ?
C15 C17 1.537(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.518(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C19 1.513(6) 2_353 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
