Single Crystal-to-Single Crystal Irreversible Transformation from a Discrete Vanadium(V)-Alcoholate to an Aldehydic-Vanadium(IV) Oligomer
Pabitra Baran Chatterjee; Anandalok Audhya; Subhajit Bhattacharya; Sk Md Towsif Abtab; Kisholoy Bhattacharya; Muktimoy Chaudhury; Journal of the American Chemical Society 132 (2010) 15842–15845; doi:10.1021/ja103451j

data_4103475
_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
_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  '\p and \w 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/[\s^2^(Fo^2^)+(0.0800P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/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