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_1564794
_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
'C6 H6 Cr3 K2 Nb1 O82.5 P2 W17, C6 H6 Cr3 O16, 6(O)'
_chemical_formula_sum            'C12 H12 Cr6 K2 Nb O104.5 P2 W17'
_chemical_formula_weight         5498.72
_chemical_name_systematic        'PIC 2'
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-22 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                   15.8474(3)
_cell_length_b                   15.8474(3)
_cell_length_c                   21.4754(6)
_cell_measurement_reflns_used    10570
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      30.5170
_cell_measurement_theta_min      2.3680
_cell_volume                     4670.76(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Rigaku HyPix-6000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.954
_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  37.00   0.50   34.50    --  -14.60  45.00   0.00   50
  2  \w    -73.00 -33.00   0.50   34.50    --  -14.60  45.00  30.00   80
  3  \w   -102.00  65.00   0.50   34.50    --  -14.60  45.00  60.00  334
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016108000
_diffrn_orient_matrix_UB_12      0.0301601000
_diffrn_orient_matrix_UB_13      -0.0238248000
_diffrn_orient_matrix_UB_21      -0.0436980000
_diffrn_orient_matrix_UB_22      -0.0398739000
_diffrn_orient_matrix_UB_23      -0.0116021000
_diffrn_orient_matrix_UB_31      -0.0275375000
_diffrn_orient_matrix_UB_32      0.0130461000
_diffrn_orient_matrix_UB_33      0.0197274000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27338
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.457
_diffrn_reflns_theta_min         2.408
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Ultrax 18'
_exptl_absorpt_coefficient_mu    21.875
_exptl_absorpt_correction_T_max  0.03025
_exptl_absorpt_correction_T_min  0.01014
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.910
_exptl_crystal_description       block
_exptl_crystal_F_000             4862
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         3.064
_refine_diff_density_min         -2.962
_refine_diff_density_rms         0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2552
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+294.9114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2195
_reflns_number_total             2552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nr04762k2.cif
_cod_data_source_block           exp_18
_cod_depositor_comments
'Adding full bibliography for 1564793--1564795.cif.'
_cod_original_cell_volume        4670.8(2)
_cod_original_formula_sum        'C12 H12 Cr6 K2 Nb O104.50 P2 W17'
_cod_database_code               1564794
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cr P2W17Nb'
_shelx_estimated_absorpt_t_max   0.097
_shelx_estimated_absorpt_t_min   0.059
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Nb1, W1}
3. 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
4. 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(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Nb1) = Uanis(W1)
5. 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
6. Others
 Fixed Sof: W1(0.41665) Cr2(0.25) O9(0.08333) O12(0.5) H9(0.25) O13(0.25)
 O15(0.5) C10(0.25) H10(0.25) Nb1(0.08335) K1(0.16665) O17(0.25) O18(0.25)
 O16(0.25) O19(0.25) O20(0.125)
7.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C2(H2)
;
_shelx_res_checksum              45893
_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 1.969
_oxdiff_exptl_absorpt_empirical_full_min 0.647