#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:19:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179810 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/06/7010674.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_7010674
loop_
_publ_author_name
'Manos, Manolis J.'
'Tasiopoulos, Anastasios J.'
'Raptopoulou, Catherine'
'Terzis, Aris'
'Woollins, J. Derek'
'Slawin, Alexandra M. Z.'
'Keramidas, Anastasios D.'
'Kabanos, Themistoklis A.'
_publ_section_title
;
 Unexpected reduction of vanadium(IV) to vanadium(III) in the presence
 of the chelate ligands 2,2'-bipyridine (bpy) and 1,8-hydroxyquinoline
 (Hquin)
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1556
_journal_paper_doi               10.1039/b102095l
_journal_year                    2001
_chemical_formula_analytical     '[V(III)Cl2(acac)(bpy)].CH3COCH3'
_chemical_formula_sum            'C18 H21 Cl2 N2 O3 V'
_chemical_formula_weight         435.21
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 115.699(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.616(2)
_cell_length_b                   12.451(2)
_cell_length_c                   14.337(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11
_cell_measurement_theta_min      5.5
_cell_volume                     2029.3(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'P21 Nicolet upgraded by Crystal Logic'
_diffrn_measurement_method       'theta-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3921
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      1.40
_exptl_crystal_density_method    'floating method'
_exptl_crystal_F_000             896
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_obs   1.141
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_obs          0.0690
_refine_ls_shift/esd_max         0.182
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0970P)²+4.3016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2357
_refine_ls_wR_factor_obs         0.1840
_reflns_number_observed          2226
_reflns_number_total             3766
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b102095l.txt
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+4.3016P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+4.3016P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2029.3(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7010674
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V V 0.73875(10) 0.20730(9) 0.97820(9) 0.0506(4) Uani 1 d . .
Cl1 Cl 0.5817(2) 0.28554(14) 0.99804(15) 0.0591(5) Uani 1 d . .
Cl2 Cl 0.8684(2) 0.3319(2) 1.0721(2) 0.0786(6) Uani 1 d . .
O1 O 0.6916(4) 0.2788(4) 0.8439(3) 0.0586(13) Uani 1 d . .
O2 O 0.8612(4) 0.1327(4) 0.9508(3) 0.0516(11) Uani 1 d . .
N1 N 0.6285(4) 0.0720(4) 0.9068(4) 0.0448(12) Uani 1 d . .
N2 N 0.7744(4) 0.0975(4) 1.1031(4) 0.0458(12) Uani 1 d . .
C1 C 0.5549(7) 0.0646(7) 0.8066(6) 0.059(2) Uani 1 d . .
C2 C 0.4867(8) -0.0240(8) 0.7643(7) 0.071(2) Uani 1 d . .
C3 C 0.4955(8) -0.1088(7) 0.8273(8) 0.075(3) Uani 1 d . .
C4 C 0.5690(8) -0.1033(7) 0.9285(8) 0.063(2) Uani 1 d . .
C5 C 0.6353(6) -0.0111(5) 0.9693(5) 0.0475(15) Uani 1 d . .
C6 C 0.7161(6) 0.0048(5) 1.0798(5) 0.0468(15) Uani 1 d . .
C7 C 0.7296(9) -0.0697(8) 1.1574(8) 0.067(2) Uani 1 d . .
C8 C 0.8011(9) -0.0468(9) 1.2581(7) 0.076(3) Uani 1 d . .
C9 C 0.8610(9) 0.0473(8) 1.2812(7) 0.070(2) Uani 1 d . .
C10 C 0.8474(7) 0.1184(7) 1.2041(6) 0.060(2) Uani 1 d . .
C11 C 0.6964(8) 0.3673(7) 0.7015(6) 0.076(2) Uani 1 d . .
H11A H 0.7371(48) 0.3618(51) 0.6587(35) 0.158(29) Uiso 1 calc R .
H11B H 0.7009(66) 0.4398(10) 0.7257(6) 0.158(29) Uiso 1 calc R .
H11C H 0.6154(22) 0.3477(43) 0.6621(37) 0.158(29) Uiso 1 calc R .
C12 C 0.7519(6) 0.2932(5) 0.7923(5) 0.0483(15) Uani 1 d . .
C13 C 0.8562(7) 0.2413(6) 0.8163(6) 0.056(2) Uani 1 d . .
C14 C 0.9054(5) 0.1627(5) 0.8904(5) 0.0436(14) Uani 1 d . .
C15 C 1.0162(6) 0.1065(6) 0.9006(6) 0.057(2) Uani 1 d . .
H15A H 1.0080(29) 0.0860(60) 0.8333(8) 0.159(29) Uiso 1 calc R .
H15B H 1.0289(40) 0.0436(37) 0.9429(54) 0.159(29) Uiso 1 calc R .
H15C H 1.0821(13) 0.1542(24) 0.9322(59) 0.159(29) Uiso 1 calc R .
O3 O 0.2138(7) 0.3137(7) -0.0558(7) 0.126(3) Uani 1 d . .
C16 C 0.2348(7) 0.3775(6) 0.0159(7) 0.072(2) Uani 1 d . .
C17 C 0.3520(8) 0.4286(8) 0.0685(8) 0.085(3) Uani 1 d . .
H17A H 0.3710(41) 0.4389(77) 0.1403(19) 0.195(38) Uiso 1 calc R .
H17B H 0.3509(28) 0.4969(39) 0.0369(54) 0.195(38) Uiso 1 calc R .
H17C H 0.4101(16) 0.3832(40) 0.0622(71) 0.195(38) Uiso 1 calc R .
C18 C 0.1444(8) 0.4069(9) 0.0506(9) 0.099(3) Uani 1 d . .
H18A H 0.1349(38) 0.4835(9) 0.0478(45) 0.111(20) Uiso 1 calc R .
H18B H 0.1685(26) 0.3827(44) 0.1205(19) 0.111(20) Uiso 1 calc R .
H18C H 0.0711(16) 0.3737(40) 0.0063(30) 0.111(20) Uiso 1 calc R .
H1 H 0.5507(49) 0.1165(48) 0.7700(45) 0.030(15) Uiso 1 d . .
H2 H 0.4407(71) -0.0237(66) 0.7065(64) 0.068(26) Uiso 1 d . .
H3 H 0.4539(65) -0.1664(64) 0.7973(58) 0.061(21) Uiso 1 d . .
H4 H 0.5814(77) -0.1365(70) 0.9673(66) 0.064(32) Uiso 1 d . .
H7 H 0.6935(62) -0.1166(57) 1.1404(55) 0.044(23) Uiso 1 d . .
H8 H 0.8051(89) -0.0907(84) 1.2948(79) 0.100(35) Uiso 1 d . .
H9 H 0.9113(79) 0.0618(74) 1.3409(71) 0.087(31) Uiso 1 d . .
H10 H 0.9135(93) 0.1633(92) 1.2153(80) 0.121(38) Uiso 1 d . .
H13 H 0.8842(59) 0.2542(55) 0.7748(51) 0.051(19) Uiso 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'
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
_geom_angle_publ_flag
O1 V O2 87.1(2) . . ?
O1 V N2 166.9(2) . . ?
O2 V N2 88.1(2) . . ?
O1 V N1 91.7(2) . . ?
O2 V N1 86.4(2) . . ?
N2 V N1 75.8(2) . . ?
O1 V Cl2 96.1(2) . . ?
O2 V Cl2 90.9(2) . . ?
N2 V Cl2 96.1(2) . . ?
N1 V Cl2 171.5(2) . . ?
O1 V Cl1 91.02(15) . . ?
O2 V Cl1 174.7(2) . . ?
N2 V Cl1 92.64(14) . . ?
N1 V Cl1 88.67(14) . . ?
Cl2 V Cl1 94.32(9) . . ?
C12 O1 V 128.7(4) . . ?
C14 O2 V 127.3(4) . . ?
C1 N1 C5 118.5(6) . . ?
C1 N1 V 125.0(5) . . ?
C5 N1 V 116.4(4) . . ?
C6 N2 C10 118.5(6) . . ?
C6 N2 V 116.8(4) . . ?
C10 N2 V 124.6(5) . . ?
N1 C1 C2 122.9(8) . . ?
C3 C2 C1 118.4(8) . . ?
C4 C3 C2 119.8(8) . . ?
C3 C4 C5 120.3(9) . . ?
N1 C5 C4 120.1(7) . . ?
N1 C5 C6 115.1(6) . . ?
C4 C5 C6 124.8(7) . . ?
N2 C6 C7 120.8(7) . . ?
N2 C6 C5 115.7(5) . . ?
C7 C6 C5 123.5(7) . . ?
C8 C7 C6 120.0(9) . . ?
C9 C8 C7 118.9(8) . . ?
C8 C9 C10 120.1(9) . . ?
N2 C10 C9 121.7(8) . . ?
O1 C12 C13 122.3(6) . . ?
O1 C12 C11 114.6(6) . . ?
C13 C12 C11 123.1(6) . . ?
C12 C13 C14 126.3(6) . . ?
O2 C14 C13 123.3(6) . . ?
O2 C14 C15 117.2(6) . . ?
C13 C14 C15 119.5(6) . . ?
O3 C16 C18 121.5(9) . . ?
O3 C16 C17 120.5(9) . . ?
C18 C16 C17 117.9(9) . . ?
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
V O1 1.964(4) . ?
V O2 1.982(4) . ?
V N2 2.140(5) . ?
V N1 2.142(6) . ?
V Cl2 2.233(3) . ?
V Cl1 2.333(2) . ?
O1 C12 1.284(8) . ?
O2 C14 1.273(7) . ?
N1 C1 1.332(9) . ?
N1 C5 1.348(8) . ?
N2 C6 1.331(8) . ?
N2 C10 1.362(9) . ?
C1 C2 1.368(12) . ?
C2 C3 1.363(13) . ?
C3 C4 1.342(13) . ?
C4 C5 1.391(11) . ?
C5 C6 1.480(10) . ?
C6 C7 1.400(10) . ?
C7 C8 1.360(14) . ?
C8 C9 1.355(14) . ?
C9 C10 1.367(11) . ?
C11 C12 1.498(9) . ?
C12 C13 1.369(10) . ?
C13 C14 1.377(9) . ?
C14 C15 1.513(9) . ?
O3 C16 1.233(11) . ?
C16 C18 1.476(13) . ?
C16 C17 1.481(12) . ?
