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_7219587
_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            'C54 H59 Mo12 N27 O45 Si'
_chemical_formula_weight         2985.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                90.00
_cell_angle_beta                 94.9490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.3171(13)
_cell_length_b                   15.7546(9)
_cell_length_c                   12.0657(7)
_cell_measurement_temperature    293(2)
_cell_volume                     4415.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16040
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  0.5613
_exptl_absorpt_correction_T_min  0.4974
_exptl_crystal_density_diffrn    2.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2900
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.859
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5149
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      18.201
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+33.2096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                4234
_reflns_number_total             5149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02545h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7219585--7219587.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7219587