#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:21:26 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179965 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/59/7025942.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_7025942
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         'C28 H46 Cl2 N2 O4 V2'
_chemical_formula_sum            'C28 H46 Cl2 N2 O4 V2'
_chemical_formula_weight         647.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.565(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.727(4)
_cell_length_b                   28.197(3)
_cell_length_c                   7.648(4)
_cell_measurement_reflns_used    1285
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      19.538
_cell_measurement_theta_min      2.659
_cell_volume                     1651.8(12)
_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      220(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10448
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.9143
_exptl_absorpt_correction_T_min  0.7930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.851
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.851
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1024P)²+3.7528P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                2056
_reflns_number_total             2910
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00064g.txt
_cod_data_source_block           8
_cod_original_cell_volume        1651.9(11)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7025942
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.06202(7) 0.458358(19) 0.37364(7) 0.0273(2) Uani 1 1 d .
Cl1 Cl -0.17155(11) 0.44971(3) 0.16821(12) 0.0399(3) Uani 1 1 d .
N1 N 0.1336(3) 0.40272(10) 0.3928(4) 0.0285(6) Uani 1 1 d .
O1 O 0.0330(3) 0.46923(8) 0.6054(3) 0.0298(5) Uani 1 1 d .
O2 O 0.2389(3) 0.48688(8) 0.2901(3) 0.0374(6) Uani 1 1 d .
C1 C 0.2002(4) 0.35719(12) 0.4162(4) 0.0302(8) Uani 1 1 d .
C2 C 0.3584(5) 0.34917(13) 0.5259(5) 0.0350(8) Uani 1 1 d .
C3 C 0.4204(5) 0.30318(14) 0.5410(5) 0.0472(10) Uani 1 1 d .
H3 H 0.5262 0.2969 0.6158 0.057 Uiso 1 1 calc R
C4 C 0.3333(6) 0.26627(14) 0.4509(6) 0.0534(11) Uani 1 1 d .
H4 H 0.3801 0.2351 0.4615 0.064 Uiso 1 1 calc R
C5 C 0.1785(5) 0.27464(13) 0.3456(6) 0.0489(11) Uani 1 1 d .
H5 H 0.1190 0.2489 0.2843 0.059 Uiso 1 1 calc R
C6 C 0.1067(5) 0.31939(13) 0.3261(5) 0.0357(8) Uani 1 1 d .
C7 C 0.4615(5) 0.38844(14) 0.6237(5) 0.0422(9) Uani 1 1 d .
H7 H 0.3955 0.4187 0.5982 0.051 Uiso 1 1 calc R
C8 C 0.4832(6) 0.38026(16) 0.8240(6) 0.0589(12) Uani 1 1 d .
H8A H 0.3679 0.3771 0.8631 0.088 Uiso 1 1 calc R
H8B H 0.5447 0.4073 0.8841 0.088 Uiso 1 1 calc R
H8C H 0.5507 0.3512 0.8527 0.088 Uiso 1 1 calc R
C9 C 0.6402(5) 0.39396(16) 0.5596(7) 0.0641(13) Uani 1 1 d .
H9A H 0.7139 0.3667 0.5990 0.096 Uiso 1 1 calc R
H9B H 0.6960 0.4232 0.6083 0.096 Uiso 1 1 calc R
H9C H 0.6250 0.3955 0.4305 0.096 Uiso 1 1 calc R
C10 C -0.0606(5) 0.32878(13) 0.2035(5) 0.0415(9) Uani 1 1 d .
H10 H -0.1164 0.3574 0.2490 0.050 Uiso 1 1 calc R
C11 C -0.0157(6) 0.34088(17) 0.0228(5) 0.0591(12) Uani 1 1 d .
H11A H 0.0675 0.3673 0.0321 0.089 Uiso 1 1 calc R
H11B H -0.1221 0.3501 -0.0539 0.089 Uiso 1 1 calc R
H11C H 0.0365 0.3132 -0.0272 0.089 Uiso 1 1 calc R
C12 C -0.1921(6) 0.28847(17) 0.1975(7) 0.0751(16) Uani 1 1 d .
H12A H -0.1440 0.2602 0.1471 0.113 Uiso 1 1 calc R
H12B H -0.3004 0.2978 0.1243 0.113 Uiso 1 1 calc R
H12C H -0.2166 0.2814 0.3173 0.113 Uiso 1 1 calc R
C13 C 0.0606(5) 0.43863(13) 0.7546(5) 0.0373(9) Uani 1 1 d .
H13A H 0.0576 0.4056 0.7149 0.056 Uiso 1 1 calc R
H13B H -0.0313 0.4438 0.8294 0.056 Uiso 1 1 calc R
H13C H 0.1747 0.4454 0.8222 0.056 Uiso 1 1 calc R
C14 C 0.3926(6) 0.47145(17) 0.2332(7) 0.0589(12) Uani 1 1 d .
H14A H 0.4919 0.4800 0.3208 0.088 Uiso 1 1 calc R
H14B H 0.4057 0.4865 0.1202 0.088 Uiso 1 1 calc R
H14C H 0.3888 0.4369 0.2185 0.088 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 101.33(12) . .
N1 V1 O1 98.82(12) . .
O2 V1 O1 117.90(11) . .
N1 V1 O1 170.69(12) . 3_566
O2 V1 O1 83.38(10) . 3_566
O1 V1 O1 71.88(10) . 3_566
N1 V1 Cl1 100.75(10) . .
O2 V1 Cl1 112.54(9) . .
O1 V1 Cl1 120.22(8) . .
O1 V1 Cl1 84.59(7) 3_566 .
C1 N1 V1 176.8(2) . .
C13 O1 V1 130.2(2) . .
C13 O1 V1 121.6(2) . 3_566
V1 O1 V1 108.12(10) . 3_566
C14 O2 V1 134.6(3) . .
N1 C1 C2 120.3(3) . .
N1 C1 C6 118.5(3) . .
C2 C1 C6 121.2(3) . .
C3 C2 C1 117.7(3) . .
C3 C2 C7 119.6(3) . .
C1 C2 C7 122.7(3) . .
C4 C3 C2 121.8(4) . .
C3 C4 C5 119.7(4) . .
C6 C5 C4 121.9(4) . .
C5 C6 C1 117.7(3) . .
C5 C6 C10 121.6(3) . .
C1 C6 C10 120.6(3) . .
C2 C7 C9 110.9(3) . .
C2 C7 C8 111.5(3) . .
C9 C7 C8 110.5(3) . .
C6 C10 C11 109.1(3) . .
C6 C10 C12 113.6(3) . .
C11 C10 C12 112.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 N1 1.663(3) .
V1 O2 1.775(2) .
V1 O1 1.842(2) .
V1 O1 2.183(2) 3_566
V1 Cl1 2.2447(12) .
N1 C1 1.386(4) .
O1 C13 1.424(4) .
O1 V1 2.183(2) 3_566
O2 C14 1.388(5) .
C1 C2 1.407(5) .
C1 C6 1.415(5) .
C2 C3 1.382(5) .
C2 C7 1.504(5) .
C3 C4 1.375(6) .
C4 C5 1.372(6) .
C5 C6 1.379(5) .
C6 C10 1.517(5) .
C7 C9 1.533(6) .
C7 C8 1.537(6) .
C10 C11 1.507(6) .
C10 C12 1.521(5) .
