#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:21:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179965 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/59/7025943.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_7025943
loop_
_publ_author_name
'Romero-Fernández, Javier'
'Carrillo-Hermosilla, Fernando'
'Antiñolo, Antonio'
'Alonso-Moreno, Carlos'
'Rodríguez, Ana M'
'López-Solera, Isabel'
'Otero, Antonio'
_publ_section_title
;
 Oxo- and imido-alkoxide vanadium complexes as precatalysts for the
 guanylation of aromatic amines.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6419
_journal_page_last               6425
_journal_paper_doi               10.1039/c0dt00064g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C36 H62 Cl2 N2 O4 V2'
_chemical_formula_sum            'C36 H62 Cl2 N2 O4 V2'
_chemical_formula_weight         759.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.638(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8392(19)
_cell_length_b                   12.0336(19)
_cell_length_c                   14.851(2)
_cell_measurement_temperature    200(2)
_cell_volume                     2097.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13776
_diffrn_reflns_theta_full        26.60
_diffrn_reflns_theta_max         26.60
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.499089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.726
_exptl_crystal_size_mid          0.562
_exptl_crystal_size_min          0.347
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0450
_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)+(0.0518P)²+0.2787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                2805
_reflns_number_total             4245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00064g.txt
_cod_data_source_block           12
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7025943
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.87471(4) 0.54172(4) 1.02084(3) 0.04016(16) Uani 1 1 d .
Cl1 Cl 0.90084(7) 0.55920(7) 1.17174(4) 0.0630(2) Uani 1 1 d .
O1 O 0.99443(14) 0.58556(14) 0.96076(11) 0.0448(4) Uani 1 1 d .
O2 O 0.78329(15) 0.42913(14) 0.98428(12) 0.0481(5) Uani 1 1 d .
N1 N 0.78820(17) 0.64817(17) 0.99066(12) 0.0394(5) Uani 1 1 d .
C1 C 0.7252(2) 0.7407(2) 0.95898(18) 0.0443(6) Uani 1 1 d .
C2 C 0.6907(2) 0.7542(2) 0.86545(19) 0.0538(7) Uani 1 1 d .
C3 C 0.6332(3) 0.8510(3) 0.8372(3) 0.0771(10) Uani 1 1 d .
H3 H 0.6099 0.8624 0.7756 0.093 Uiso 1 1 calc R
C4 C 0.6102(3) 0.9302(3) 0.8986(3) 0.0890(13) Uani 1 1 d .
H4 H 0.5721 0.9948 0.8780 0.107 Uiso 1 1 calc R
C5 C 0.6425(3) 0.9153(3) 0.9899(3) 0.0786(11) Uani 1 1 d .
H5 H 0.6254 0.9699 1.0303 0.094 Uiso 1 1 calc R
C6 C 0.6998(2) 0.8209(2) 1.0231(2) 0.0549(7) Uani 1 1 d .
C7 C 0.7109(3) 0.6670(3) 0.79597(18) 0.0668(9) Uani 1 1 d .
H7 H 0.7598 0.6092 0.8269 0.080 Uiso 1 1 calc R
C8 C 0.7710(3) 0.7147(4) 0.7189(2) 0.0952(13) Uani 1 1 d .
H8A H 0.7218 0.7673 0.6846 0.143 Uiso 1 1 calc R
H8B H 0.7886 0.6554 0.6798 0.143 Uiso 1 1 calc R
H8C H 0.8401 0.7510 0.7443 0.143 Uiso 1 1 calc R
C9 C 0.5980(3) 0.6129(4) 0.7560(2) 0.0946(12) Uani 1 1 d .
H9A H 0.5616 0.5814 0.8041 0.142 Uiso 1 1 calc R
H9B H 0.6126 0.5554 0.7142 0.142 Uiso 1 1 calc R
H9C H 0.5490 0.6680 0.7246 0.142 Uiso 1 1 calc R
C10 C 0.7314(3) 0.8011(3) 1.1236(2) 0.0666(9) Uani 1 1 d .
H10 H 0.7991 0.7534 1.1305 0.080 Uiso 1 1 calc R
C11 C 0.7629(4) 0.9050(3) 1.1785(3) 0.1185(16) Uani 1 1 d .
H11A H 0.6962 0.9502 1.1797 0.178 Uiso 1 1 calc R
H11B H 0.8190 0.9462 1.1513 0.178 Uiso 1 1 calc R
H11C H 0.7934 0.8848 1.2394 0.178 Uiso 1 1 calc R
C12 C 0.6390(4) 0.7375(4) 1.1615(3) 0.1176(16) Uani 1 1 d .
H12A H 0.5715 0.7824 1.1576 0.176 Uiso 1 1 calc R
H12B H 0.6639 0.7192 1.2238 0.176 Uiso 1 1 calc R
H12C H 0.6227 0.6705 1.1271 0.176 Uiso 1 1 calc R
C13 C 1.0097(2) 0.6893(2) 0.91656(18) 0.0510(7) Uani 1 1 d .
H13A H 0.9398 0.7083 0.8778 0.061 Uiso 1 1 calc R
H13B H 1.0694 0.6812 0.8782 0.061 Uiso 1 1 calc R
C14 C 1.0408(3) 0.7830(2) 0.9839(2) 0.0679(9) Uani 1 1 d .
H14A H 0.9805 0.7928 1.0214 0.082 Uiso 1 1 calc R
H14B H 1.1102 0.7641 1.0233 0.082 Uiso 1 1 calc R
C15 C 1.0582(4) 0.8900(3) 0.9341(3) 0.1232(18) Uani 1 1 d .
H15A H 0.9877 0.9118 0.8990 0.185 Uiso 1 1 calc R
H15B H 1.1150 0.8789 0.8944 0.185 Uiso 1 1 calc R
H15C H 1.0830 0.9472 0.9773 0.185 Uiso 1 1 calc R
C16 C 0.6631(2) 0.4246(3) 0.9601(2) 0.0578(8) Uani 1 1 d .
H16A H 0.6450 0.3788 0.9063 0.069 Uiso 1 1 calc R
H16B H 0.6340 0.4987 0.9458 0.069 Uiso 1 1 calc R
C17 C 0.6066(3) 0.3771(3) 1.0365(2) 0.0738(9) Uani 1 1 d .
H17A H 0.6241 0.4244 1.0894 0.089 Uiso 1 1 calc R
H17B H 0.5247 0.3787 1.0191 0.089 Uiso 1 1 calc R
C18 C 0.6417(3) 0.2605(3) 1.0622(3) 0.1093(15) Uani 1 1 d .
H18A H 0.6298 0.2139 1.0094 0.164 Uiso 1 1 calc R
H18B H 0.5970 0.2335 1.1070 0.164 Uiso 1 1 calc R
H18C H 0.7209 0.2595 1.0868 0.164 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'
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
N1 V1 O2 100.19(9) . .
N1 V1 O1 97.71(9) . .
O2 V1 O1 123.09(8) . .
N1 V1 O1 168.80(8) . 3_767
O2 V1 O1 84.02(8) . 3_767
O1 V1 O1 71.46(7) . 3_767
N1 V1 Cl1 101.31(7) . .
O2 V1 Cl1 112.15(6) . .
O1 V1 Cl1 116.41(6) . .
O1 V1 Cl1 86.49(5) 3_767 .
C13 O1 V1 128.38(15) . .
C13 O1 V1 122.77(14) . 3_767
V1 O1 V1 108.55(7) . 3_767
C16 O2 V1 131.04(17) . .
C1 N1 V1 173.35(17) . .
N1 C1 C2 120.0(2) . .
N1 C1 C6 118.1(2) . .
C2 C1 C6 121.8(2) . .
C3 C2 C1 117.6(3) . .
C3 C2 C7 119.5(3) . .
C1 C2 C7 122.9(2) . .
C4 C3 C2 121.1(3) . .
C5 C4 C3 120.8(3) . .
C4 C5 C6 121.4(3) . .
C5 C6 C1 117.3(3) . .
C5 C6 C10 122.0(3) . .
C1 C6 C10 120.7(2) . .
C2 C7 C9 110.5(3) . .
C2 C7 C8 112.4(3) . .
C9 C7 C8 109.6(3) . .
C12 C10 C6 110.7(3) . .
C12 C10 C11 111.0(3) . .
C6 C10 C11 114.4(3) . .
O1 C13 C14 112.3(2) . .
C15 C14 C13 110.3(3) . .
O2 C16 C17 110.7(3) . .
C18 C17 C16 114.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 N1 1.664(2) .
V1 O2 1.7736(18) .
V1 O1 1.8491(16) .
V1 O1 2.1699(17) 3_767
V1 Cl1 2.2311(8) .
O1 C13 1.433(3) .
O1 V1 2.1698(17) 3_767
O2 C16 1.422(3) .
N1 C1 1.387(3) .
C1 C2 1.404(4) .
C1 C6 1.416(4) .
C2 C3 1.385(4) .
C2 C7 1.512(4) .
C3 C4 1.371(5) .
C4 C5 1.371(5) .
C5 C6 1.380(4) .
C6 C10 1.508(4) .
C7 C9 1.534(5) .
C7 C8 1.536(4) .
C10 C12 1.504(5) .
C10 C11 1.513(5) .
C13 C14 1.520(4) .
C14 C15 1.513(4) .
C16 C17 1.504(4) .
C17 C18 1.498(5) .
