DMAP-catalyzed esterification of pentaerythritol-derivatized POMs: a new route for the functionalization of polyoxometalates
Pingfan Wu; Zicheng Xiao; Jin Zhang; Jian Hao; Jiake Chen; Panchao Yin; Yongge Wei; Chem.Commun. 47 (2011) 5557–; doi:10.1039/c1cc10650c

data_7106362
_publ_section_title
;
 DMAP-catalyzed esterification of pentaerythritol-derivatized POMs: a new
 route for the functionalization of polyoxometalates
;
_journal_name_full               Chem.Commun.
_journal_page_first              5557
_journal_paper_doi               10.1039/c1cc10650c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C48 H98 N2 O23 V6'
_chemical_formula_weight         1376.92
_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                 97.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.135(2)
_cell_length_b                   14.900(3)
_cell_length_c                   19.855(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3265.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31068
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0079(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7439
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0576
_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/[\s^2^(Fo^2^)+(0.0883P)^2^+1.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1995
_reflns_number_gt                4175
_reflns_number_total             7439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc10650c.txt
_cod_data_source_block           c3
_cod_original_cell_volume        3265.1(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7106362