Supramolecular cations of (m-halogenated-anilinium)(dibenzo[18]crown-6) in Keggin [SMo12O402−] polyoxometallates
Xiong, J.; Kubo, K.; Noro, S.; Akutagawa, T.; Nakamura, T.; CrystEngComm 17 (2015) 856–; doi:10.1039/C4CE01988A

data_7219009
_publ_section_title
;
 Supramolecular cations of (m-halogenated-anilinium)(dibenzo[18]crown-6)
 in Keggin [SMo12O402&#x2212;] polyoxometallates
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              856
_journal_paper_doi               10.1039/C4CE01988A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C60 H72 Cl2 Mo12 N6 O52 S'
_chemical_formula_weight         2963.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-09-29 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.273(2)
_cell_length_b                   31.417(6)
_cell_length_c                   13.312(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4551.4(17)
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43588
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.777
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2888.0
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+17.0916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                8582
_reflns_number_total             10350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01988a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7219008--7219011.cif.'
_cod_original_cell_volume        4551.4(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        ' C60 H72 Cl2 Mo12 N6 O52 S'
_cod_database_code               7219009