Two new polyoxometalate-templated supramolecular compounds constructed by a new tridentate ligand 2,4,6-tris[1-(4-oxidroxypyridinium)-ylmethyl]-mesitylene
Jiao Guo; Jin Yang; Ying-Ying Liu; Jian-Fang Ma; Inorganica Chimica Acta 400 (2013) 51–58; doi:

data_1516912
_publ_section_title
;
 Two new polyoxometalate-templated supramolecular compounds constructed by
 a new tridentate ligand
 2,4,6-tris[1-(4-oxidroxypyridinium)-ylmethyl]-mesitylene
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              51
_journal_page_last               58
_journal_volume                  400
_journal_year                    2013
_chemical_formula_moiety         'O40 Si W12, 2(C27 H29 N3 O3), 6(H2 O)'
_chemical_formula_sum            'C54 H70 N6 O52 Si W12'
_chemical_formula_weight         3869.23
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 111.482(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.756(5)
_cell_length_b                   23.821(8)
_cell_length_c                   12.814(5)
_cell_measurement_reflns_used    7018
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.2
_cell_volume                     3907(2)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15753
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    17.711
_exptl_absorpt_correction_T_max  0.041
_exptl_absorpt_correction_T_min  0.041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis (Oxford Diffraction, 2006)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3484
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.782
_refine_diff_density_min         -2.893
_refine_diff_density_rms         0.384
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7106
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0764
_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^)+(0.0297P)^2^+212.5332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                6002
_reflns_number_total             7106
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2013-400-51-58-2.cif
_cod_data_source_block           compound-2
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_sg_symbol_H-M      'p 21/c'
_cod_database_code               1516912