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_4103476
_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 H16 O8 V2'
_chemical_formula_weight         462.19
_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                 108.046(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4179(17)
_cell_length_b                   5.1652(8)
_cell_length_c                   15.935(2)
_cell_measurement_reflns_used    1669
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      1.9
_cell_volume                     893.5(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0423
_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            4617
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.336
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1866
_reflns_number_gt                1241
_reflns_number_total             1751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja103451j_si_005.cif
_cod_data_source_block           MC4_DAY-14
_cod_original_cell_volume        893.6(2)
_cod_database_code               4103476