#------------------------------------------------------------------------------
#$Date: 2018-09-26 05:29:44 +0200 (Wed 26 de Sep de 2018) $
#$Revision: 211175 $
#$URL: svn://www.crystallography.net/cod/cif/8/00/00/8000019.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_8000019
loop_
_publ_author_name
'Manabu Hoshino'
'Akiko Sekine'
'Hidehiro Uekusa'
'Yuji Ohashi'
_publ_section_title
;
 X-ray Analysis of Bond Elongation in VO(acac)2 at the Excited State
;
_journal_issue                   9
_journal_name_full               'Chemistry Letters'
_journal_page_first              1228
_journal_paper_doi               10.1246/cl.2005.1228
_journal_volume                  34
_journal_year                    2005
_chemical_formula_sum            'C10 H14 O5 V'
_chemical_formula_weight         265.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.973(1)
_cell_angle_beta                 72.127(1)
_cell_angle_gamma                66.860(1)
_cell_formula_units_Z            2
_cell_length_a                   7.4077(1)
_cell_length_b                   8.1943(1)
_cell_length_c                   11.2383(2)
_cell_measurement_temperature    168(2)
_cell_volume                     585.35(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT & SADABS'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Siemens SMART CCD area detector system'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku ratating anode Ultrax18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10452
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.90
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.771298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'PROGRAM SADABS was used.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         4035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0290
_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)+(0.0547P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                3539
_reflns_number_total             4035
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8000019
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
V1 V 0.14198(3) 0.29186(2) 0.722530(16) 0.01757(6) Uani 1 1 d
O1 O -0.00738(13) 0.11923(11) 0.76906(8) 0.02282(17) Uani 1 1 d
O2 O -0.06220(13) 0.41725(11) 0.85689(8) 0.02230(16) Uani 1 1 d
O3 O 0.14902(13) 0.53788(11) 0.63480(8) 0.02223(16) Uani 1 1 d
O4 O 0.22016(13) 0.22979(11) 0.55262(8) 0.02167(16) Uani 1 1 d
O5 O 0.33958(13) 0.18917(13) 0.77992(8) 0.02787(18) Uani 1 1 d
C1 C -0.2104(2) -0.06308(17) 0.88486(12) 0.0254(2) Uani 1 1 d
H1A H -0.331(3) -0.008(3) 0.8430(18) 0.038 Uiso 1 1 d
H1B H -0.250(3) -0.115(3) 0.9746(18) 0.038 Uiso 1 1 d
H1C H -0.116(3) -0.145(3) 0.8402(18) 0.038 Uiso 1 1 d
C2 C -0.13705(16) 0.08948(15) 0.87200(10) 0.01917(19) Uani 1 1 d
C3 C -0.21557(17) 0.19251(16) 0.96787(11) 0.0224(2) Uani 1 1 d
H3 H -0.312(2) 0.152(2) 1.0467(16) 0.027 Uiso 1 1 d
C4 C -0.17700(16) 0.35137(16) 0.95543(11) 0.02052(19) Uani 1 1 d
C5 C -0.2729(2) 0.4598(2) 1.05973(13) 0.0300(3) Uani 1 1 d
H5A H -0.175(3) 0.464(3) 1.0933(19) 0.045 Uiso 1 1 d
H5B H -0.377(3) 0.421(3) 1.1253(19) 0.045 Uiso 1 1 d
H5C H -0.355(3) 0.587(3) 1.0321(19) 0.045 Uiso 1 1 d
C6 C 0.22697(19) 0.78452(16) 0.48318(12) 0.0245(2) Uani 1 1 d
H6A H 0.115(3) 0.859(3) 0.4473(18) 0.037 Uiso 1 1 d
H6B H 0.345(3) 0.792(3) 0.4163(17) 0.037 Uiso 1 1 d
H6C H 0.217(3) 0.831(3) 0.5526(18) 0.037 Uiso 1 1 d
C7 C 0.22638(16) 0.59332(14) 0.51795(11) 0.01893(19) Uani 1 1 d
C8 C 0.30054(18) 0.48984(15) 0.42248(11) 0.0219(2) Uani 1 1 d
H8 H 0.352(2) 0.546(2) 0.3360(16) 0.026 Uiso 1 1 d
C9 C 0.29167(16) 0.31527(15) 0.44395(10) 0.01936(19) Uani 1 1 d
C10 C 0.3663(2) 0.21562(18) 0.33582(12) 0.0295(3) Uani 1 1 d
H10A H 0.499(3) 0.128(3) 0.3395(19) 0.044 Uiso 1 1 d
H10B H 0.377(3) 0.285(3) 0.2517(19) 0.044 Uiso 1 1 d
H10C H 0.290(3) 0.157(3) 0.3390(19) 0.044 Uiso 1 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'
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
O5 V1 O4 104.83(4)
O5 V1 O2 104.88(4)
O4 V1 O2 150.28(4)
O5 V1 O3 106.91(5)
O4 V1 O3 87.81(3)
O2 V1 O3 84.09(3)
O5 V1 O1 106.83(4)
O4 V1 O1 83.65(3)
O2 V1 O1 87.37(3)
O3 V1 O1 146.25(4)
C2 O1 V1 128.45(7)
C4 O2 V1 127.80(7)
C7 O3 V1 129.00(7)
C9 O4 V1 128.99(7)
C2 C1 H1A 106.4(11)
C2 C1 H1B 109.8(11)
H1A C1 H1B 110.7(15)
C2 C1 H1C 109.6(12)
H1A C1 H1C 107.1(16)
H1B C1 H1C 113.0(17)
O1 C2 C3 124.38(10)
O1 C2 C1 116.01(10)
C3 C2 C1 119.58(10)
C4 C3 C2 123.16(10)
C4 C3 H3 119.5(9)
C2 C3 H3 117.2(9)
O2 C4 C3 124.24(10)
O2 C4 C5 115.26(10)
C3 C4 C5 120.49(10)
C4 C5 H5A 110.5(12)
C4 C5 H5B 113.9(12)
H5A C5 H5B 112.7(16)
C4 C5 H5C 114.3(11)
H5A C5 H5C 106.4(16)
H5B C5 H5C 98.3(16)
C7 C6 H6A 108.3(12)
C7 C6 H6B 109.2(11)
H6A C6 H6B 106.2(15)
C7 C6 H6C 113.9(12)
H6A C6 H6C 107.2(16)
H6B C6 H6C 111.7(16)
O3 C7 C8 124.32(10)
O3 C7 C6 116.33(10)
C8 C7 C6 119.30(10)
C9 C8 C7 123.27(10)
C9 C8 H8 118.7(10)
C7 C8 H8 117.9(10)
O4 C9 C8 124.47(10)
O4 C9 C10 115.23(10)
C8 C9 C10 120.30(10)
C9 C10 H10A 109.8(12)
C9 C10 H10B 117.5(12)
H10A C10 H10B 106.0(16)
C9 C10 H10C 112.4(13)
H10A C10 H10C 107.0(17)
H10B C10 H10C 103.4(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V1 O5 1.6001(9)
V1 O4 1.9745(8)
V1 O2 1.9770(8)
V1 O3 1.9814(8)
V1 O1 1.9850(8)
O1 C2 1.2873(13)
O2 C4 1.2937(13)
O3 C7 1.2855(13)
O4 C9 1.2869(13)
C1 C2 1.5028(16)
C1 H1A 1.021(19)
C1 H1B 0.974(19)
C1 H1C 0.90(2)
C2 C3 1.4050(16)
C3 C4 1.3989(16)
C3 H3 1.016(17)
C4 C5 1.5068(16)
C5 H5A 0.93(2)
C5 H5B 0.97(2)
C5 H5C 0.99(2)
C6 C7 1.5011(15)
C6 H6A 0.944(19)
C6 H6B 0.975(18)
C6 H6C 0.935(19)
C7 C8 1.4060(15)
C8 C9 1.4038(15)
C8 H8 0.975(17)
C9 C10 1.5044(16)
C10 H10A 0.97(2)
C10 H10B 0.95(2)
C10 H10C 0.86(2)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1A O5 1.021(19) 2.521(19) 3.5139(16) 163.8(15) 1_455
C1 H1B O5 0.974(19) 2.575(19) 3.5300(16) 166.8(15) 2_557
C5 H5A O2 0.93(2) 2.57(2) 3.4644(16) 161.2(17) 2_567
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
O5 V1 O1 C2 86.58(10)
O4 V1 O1 C2 -169.81(10)
O2 V1 O1 C2 -18.18(10)
O3 V1 O1 C2 -93.45(11)
O5 V1 O2 C4 -83.66(10)
O4 V1 O2 C4 95.37(11)
O3 V1 O2 C4 170.37(10)
O1 V1 O2 C4 23.06(10)
O5 V1 O3 C7 90.35(10)
O4 V1 O3 C7 -14.49(10)
O2 V1 O3 C7 -165.86(10)
O1 V1 O3 C7 -89.62(11)
O5 V1 O4 C9 -91.96(10)
O2 V1 O4 C9 89.01(11)
O3 V1 O4 C9 14.96(10)
O1 V1 O4 C9 162.26(10)
V1 O1 C2 C3 7.67(16)
V1 O1 C2 C1 -174.35(8)
O1 C2 C3 C4 7.06(18)
C1 C2 C3 C4 -170.85(11)
V1 O2 C4 C3 -17.75(16)
V1 O2 C4 C5 162.94(9)
C2 C3 C4 O2 -1.82(19)
C2 C3 C4 C5 177.45(11)
V1 O3 C7 C8 9.16(16)
V1 O3 C7 C6 -173.61(8)
O3 C7 C8 C9 2.25(18)
C6 C7 C8 C9 -174.90(11)
V1 O4 C9 C8 -10.15(17)
V1 O4 C9 C10 170.61(9)
C7 C8 C9 O4 -1.77(18)
C7 C8 C9 C10 177.45(12)
