Incorporating highly basic polyoxometalate anions comprising Nb or Ta into nanoscale reaction fields of porous ionic crystals.
Weng, Zhewei; Ogiwara, Naoki; Kitao, Takashi; Kikukawa, Yuji; Gao, Yu; Yan, Likai; Uchida, Sayaka; Nanoscale 13 (2021) 18451–18457; doi:10.1039/d1nr04762k

data_1564793
_publ_section_title
;
 Incorporating highly basic polyoxometalate anions comprising Nb or Ta
 into nanoscale reaction fields of porous ionic crystals.
;
_journal_issue                   44
_journal_name_full               Nanoscale
_journal_page_first              18451
_journal_page_last               18457
_journal_paper_doi               10.1039/d1nr04762k
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C12 H6 Cr6 K7.5 Nb3 O103 P2 W15, 1.5(H4 O2)'
_chemical_formula_sum            'C12 H12 Cr6 K7.5 Nb3 O106 P2 W15'
_chemical_formula_weight         5555.89
_space_group_crystal_system      trigonal
_space_group_IT_number           164
_space_group_name_Hall           '-P 3 2"'
_space_group_name_H-M_alt        'P -3 m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-19 deposited with the CCDC.	2021-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.1712(4)
_cell_length_b                   16.1712(4)
_cell_length_c                   24.9066(7)
_cell_measurement_reflns_used    11605
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2040
_cell_measurement_theta_min      2.8490
_cell_volume                     5640.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  79.00   0.50   14.03    --  -10.30  59.00 -47.00  182
  2  \w    -25.00  19.00   0.50   14.03    --  -10.30  60.00 -30.00   88
  3  \w    -71.00  48.00   0.50   14.03    --  -10.30  57.00-180.00  238
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0091588000
_diffrn_orient_matrix_UB_12      0.0340916000
_diffrn_orient_matrix_UB_13      0.0204259000
_diffrn_orient_matrix_UB_21      0.0157022000
_diffrn_orient_matrix_UB_22      0.0365306000
_diffrn_orient_matrix_UB_23      -0.0196675000
_diffrn_orient_matrix_UB_31      -0.0472767000
_diffrn_orient_matrix_UB_32      -0.0084314000
_diffrn_orient_matrix_UB_33      -0.0025537000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            40304
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.011
_diffrn_reflns_theta_min         2.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.486
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_density_diffrn    3.271
_exptl_crystal_description       plate
_exptl_crystal_F_000             4963
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.023
_refine_diff_density_max         2.474
_refine_diff_density_min         -2.519
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5704
_refine_ls_number_restraints     1140
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+182.3912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4509
_reflns_number_total             5704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nr04762k2.cif
_cod_data_source_block           exp_231_sq
_cod_depositor_comments
'Adding full bibliography for 1564793--1564795.cif.'
_cod_original_formula_sum        'C12 H12 Cr6 K7.50 Nb3 O106 P2 W15'
_cod_database_code               1564793
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cr3 Nb3 W15 O62'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{C20, O20}
{C21, O21}
{W2, Nb2}
{W1, Nb1}
3. Restrained distances
 Cr7-O37
 2.063 with sigma of 0.02
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C20) = Uanis(O20)
Uanis(C21) = Uanis(O21)
Uanis(W1) = Uanis(Nb1)
Uanis(W2) = Uanis(Nb2)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(W1)=Sof(Nb2)=0.5*(1-FVAR(2))
 Sof(W2)=Sof(Nb1)=0.5*FVAR(2)
 Fixed Sof: O20(0.5) O21(0.5) Cr1(0.5) O18(0.5) O22(0.5) O23(0.5) C20(0.5)
 H20(0.5) C21(0.5) K3(0.5) O27(0.5) O29(0.125) O30(0.25) O32(0.25) O14(0.16667)
 H28A(0.5) H28B(0.5) O35(0.125) O37(0.5) O12(0.25) O26(0.33333) K25(0.25)
8.a Free rotating group:
 O28(H28A,H28B)
8.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3442
_shelx_fab_checksum              50622
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.628
_oxdiff_exptl_absorpt_empirical_full_min 0.688