Controlled introduction of metal cations into polymerizable ionic liquid-polyoxomolybdate hybrid crystals
Kobayashi, Jun; Misawa, Toshiyuki; Umeda, Chihiro; Isono, Toru; Ono, Seiji; Naruke, Haruo; Okamura, Yosuke; Koguchi, Shinichi; Higuchi, Masashi; Nagase, Yu; Ito, Takeru; CrystEngComm 21 (2019) 629–; doi:10.1039/C8CE01658E

data_7231964
_publ_section_title
;
 Controlled introduction of metal cations into polymerizable ionic
 liquid-polyoxomolybdate hybrid crystals
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              629
_journal_paper_doi               10.1039/C8CE01658E
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C30 H45 Mo8 N6 Na O32'
_chemical_formula_sum            'C30 H45 Mo8 N6 Na O32'
_chemical_formula_weight         1792.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_update_record
;
2018-09-28 deposited with the CCDC.
2018-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                112.2762(14)
_cell_angle_beta                 93.2135(15)
_cell_angle_gamma                105.0974(15)
_cell_formula_units_Z            2
_cell_length_a                   12.4487(7)
_cell_length_b                   14.0216(8)
_cell_length_c                   17.0849(9)
_cell_measurement_reflns_used    22201
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.01
_cell_volume                     2624.1(3)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2002)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2002)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2002)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      193
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41831
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         3.010
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1740.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.90
_refine_diff_density_min         -3.88
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     700
_refine_ls_number_reflns         11944
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0396P)^2^+40.1161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9043
_reflns_number_total             11944
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8ce01658e1.cif
_cod_data_source_block           150210
_cod_depositor_comments
'Adding full bibliography for 7231962--7231964.cif.'
_cod_database_code               7231964
_150210
;
PROBLEM: Check Calcd Resid. Dens. 1.02A From Mo8 -3.72 eA-3
RESPONSE: There is no twin law detected for this structure.  The chemical 
components including molecular structures are supported by infrared spectra 
and CHN elemental analysis.  Therefore, all atoms are assigned accurately 
and no model error is included.  The larger residual density and atomic 
displacement parameters are observed only near the ab plane of the unit 
cell.  A kind of molecular misfit may occur around the ab plane at the 
measured temperature, which might be a reason of the large residual density 
around one metal atom.
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_shelx_res_checksum              73037