Synthesis, structures, and theoretical investigation of three polyoxomolybdate-based compounds: self-assembly, fragment analysis, orbital interaction, and formation mechanism
Tong, Yi-Ping; Luo, Guo-Tian; Zhen, Jin; Shen, You; Lin, Yan-Wen; CrystEngComm 17 (2015) 2629–; doi:10.1039/C4CE02545H

data_7219585
_publ_section_title
;
 Synthesis, structures, and theoretical investigation of three
 polyoxomolybdate-based compounds: self-assembly, fragment analysis,
 orbital interaction, and formation mechanism
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2629
_journal_paper_doi               10.1039/C4CE02545H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C24 H28 Mo12 N12 O42 Si'
_chemical_formula_weight         2335.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-06 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                99.347(2)
_cell_angle_beta                 93.793(2)
_cell_angle_gamma                113.837(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6044(4)
_cell_length_b                   13.1169(4)
_cell_length_c                   20.4496(9)
_cell_measurement_temperature    293(2)
_cell_volume                     2779.28(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53969
_diffrn_reflns_theta_full        28.84
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    2.749
_exptl_absorpt_correction_T_max  0.4377
_exptl_absorpt_correction_T_min  0.3645
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.282
_refine_diff_density_min         -2.120
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         14351
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0262P)^2^+5.4131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                10702
_reflns_number_total             14351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02545h2.cif
_cod_data_source_block           l8_om
_cod_depositor_comments
'Adding full bibliography for 7219585--7219587.cif.'
_cod_original_cell_volume        2779.28(18)
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               7219585