#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:22:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178780 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/34/4103475.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_4103475
loop_
_publ_author_name
'Pabitra Baran Chatterjee'
'Anandalok Audhya'
'Subhajit Bhattacharya'
'Sk Md Towsif Abtab'
'Kisholoy Bhattacharya'
'Muktimoy Chaudhury'
_publ_section_title
;
 Single Crystal-to-Single Crystal Irreversible Transformation from a
 Discrete Vanadium(V)-Alcoholate to an Aldehydic-Vanadium(IV) Oligomer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15842
_journal_page_last               15845
_journal_paper_doi               10.1021/ja103451j
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C18 H18 O8 V2'
_chemical_formula_weight         464.20
_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                 108.513(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4291(8)
_cell_length_b                   5.1473(4)
_cell_length_c                   15.9034(12)
_cell_measurement_reflns_used    1466
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      1.90
_cell_volume                     887.17(11)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'SAINT-plus (bruker, 1999)'
_computing_molecular_graphics    'Bruker SHELXTL V6.10'
_computing_publication_material  'Bruker SHELXTL V6.10'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'π and ω 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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8608
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0407
_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)+(0.0800P)²+0.4000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                1446
_reflns_number_total             1800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103451j_si_004.cif
_cod_data_source_block           MC3_DAY-12
_cod_database_code               4103475
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 0.54162(5) 0.23026(9) 0.44867(3) 0.0393(2) Uani 1 1 d .
C1 C 0.6728(3) 0.1329(6) 0.64508(18) 0.0366(6) Uani 1 1 d .
C6 C 0.6868(3) 0.0043(6) 0.72484(19) 0.0413(7) Uani 1 1 d .
C8 C 0.7404(3) 0.5015(6) 0.5626(2) 0.0469(8) Uani 1 1 d .
H7A H 0.7736 0.6731 0.5813 0.056 Uiso 1 1 calc R
H7B H 0.7887 0.4245 0.5287 0.056 Uiso 1 1 calc R
C2 C 0.7527(3) 0.3375(6) 0.6431(2) 0.0409(7) Uani 1 1 d .
C5 C 0.7812(3) 0.0793(7) 0.8005(2) 0.0508(9) Uani 1 1 d .
H5 H 0.7913 -0.0101 0.8532 0.061 Uiso 1 1 calc R
C3 C 0.8447(3) 0.4056(7) 0.7213(2) 0.0501(8) Uani 1 1 d .
H3 H 0.8978 0.5412 0.7198 0.060 Uiso 1 1 calc R
C4 C 0.8602(3) 0.2813(7) 0.8002(2) 0.0521(9) Uani 1 1 d .
C7 C 0.6022(4) -0.2056(6) 0.7340(2) 0.0493(8) Uani 1 1 d .
H8A H 0.6470 -0.3201 0.7818 0.059 Uiso 1 1 calc R
H8B H 0.5354 -0.1280 0.7506 0.059 Uiso 1 1 calc R
C9 C 0.9551(4) 0.3719(10) 0.8858(3) 0.0781(13) Uani 1 1 d .
H9A H 1.0236 0.4499 0.8727 0.117 Uiso 1 1 calc R
H9B H 0.9835 0.2260 0.9245 0.117 Uiso 1 1 calc R
H9C H 0.9181 0.4973 0.9143 0.117 Uiso 1 1 calc R
O3 O 0.61487(19) 0.5258(4) 0.50698(14) 0.0420(5) Uani 1 1 d .
O2 O 0.57826(18) 0.0650(4) 0.56949(12) 0.0382(5) Uani 1 1 d .
O1 O 0.5529(2) -0.3507(4) 0.65898(14) 0.0502(6) Uani 1 1 d .
O4 O 0.6507(2) 0.0988(4) 0.42272(15) 0.0541(6) Uani 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 V1 O1 100.46(12) . 3_656
O4 V1 O3 102.40(11) . .
O1 V1 O3 103.41(10) 3_656 .
O4 V1 O2 101.37(10) . 3_656
O1 V1 O2 87.03(9) 3_656 3_656
O3 V1 O2 151.72(10) . 3_656
O4 V1 O2 97.21(11) . .
O1 V1 O2 157.04(10) 3_656 .
O3 V1 O2 86.85(8) . .
O2 V1 O2 75.14(8) 3_656 .
O4 V1 O3 174.21(10) . 3_666
O1 V1 O3 80.08(9) 3_656 3_666
O3 V1 O3 71.93(9) . 3_666
O2 V1 O3 84.41(7) 3_656 3_666
O2 V1 O3 83.82(8) . 3_666
O2 C1 C6 120.2(3) . .
O2 C1 C2 120.4(3) . .
C6 C1 C2 119.4(3) . .
C5 C6 C1 119.2(3) . .
C5 C6 C7 117.8(3) . .
C1 C6 C7 122.9(3) . .
O3 C8 C2 112.3(3) . .
C3 C2 C1 118.7(3) . .
C3 C2 C8 117.3(3) . .
C1 C2 C8 123.8(3) . .
C4 C5 C6 122.4(3) . .
C4 C3 C2 122.8(3) . .
C3 C4 C5 117.5(3) . .
C3 C4 C9 121.7(4) . .
C5 C4 C9 120.7(4) . .
O1 C7 C6 114.3(3) . .
C8 O3 V1 116.45(19) . .
C8 O3 V1 122.94(19) . 3_666
V1 O3 V1 108.07(9) . 3_666
C1 O2 V1 128.81(18) . 3_656
C1 O2 V1 126.13(18) . .
V1 O2 V1 104.86(8) 3_656 .
C7 O1 V1 126.3(2) . 3_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O4 1.584(2) .
V1 O1 1.819(2) 3_656
V1 O3 1.839(2) .
V1 O2 2.0048(19) 3_656
V1 O2 2.020(2) .
V1 O3 2.465(2) 3_666
C1 O2 1.382(3) .
C1 C6 1.394(4) .
C1 C2 1.401(4) .
C6 C5 1.392(4) .
C6 C7 1.487(5) .
C8 O3 1.432(4) .
C8 C2 1.502(5) .
C2 C3 1.395(4) .
C5 C4 1.379(5) .
C3 C4 1.369(5) .
C4 C9 1.519(5) .
C7 O1 1.368(4) .
O3 V1 2.465(2) 3_666
O2 V1 2.0048(19) 3_656
O1 V1 1.819(2) 3_656
