Structure-directing effect of aqueous alkali metal ion (Li+, Na+ and K+) clusters on the polyoxoanion configuration in vanadium–molybdenum polyoxometalate solid solutions
Yao, Zhi-Yuan; Zhang, Guo-Qin; Li, Zi-Han; Shen, Lin-Jiang; Ren, Xiao-Ming; CrystEngComm 23 (2021) 6533–6540; doi:10.1039/D1CE00875G

data_7243347
_publ_section_title
;
 Structure-directing effect of aqueous alkali metal ion (Li+, Na+ and K+)
 clusters on the polyoxoanion configuration in vanadium--molybdenum
 polyoxometalate solid solutions
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              6533
_journal_page_last               6540
_journal_paper_doi               10.1039/D1CE00875G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'Mo0.95 O28 V9.05, H20 Na2 O10, 3.05(H4 N)'
_chemical_formula_sum            'H32.2 Mo0.95 N3.05 Na2 O38 V9.05'
_chemical_formula_weight         1281.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-25 deposited with the CCDC.	2021-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                69.078(2)
_cell_angle_beta                 87.216(2)
_cell_angle_gamma                66.729(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6373(5)
_cell_length_b                   10.4700(7)
_cell_length_c                   11.2282(6)
_cell_measurement_reflns_used    7118
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.564
_cell_measurement_theta_min      2.277
_cell_volume                     866.21(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13623
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.278
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1076 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.7602.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.456
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_refine_diff_density_max         1.594
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.198
_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     255
_refine_ls_number_reflns         3964
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0966P)^2^+9.8944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1965
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3250
_reflns_number_total             3964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00875g2.cif
_cod_data_source_block           yao
_cod_depositor_comments
'Adding full bibliography for 7243347--7243348.cif.'
_cod_original_formula_sum        'H32.20 Mo0.95 N3.05 Na2 O38 V9.05'
_cod_database_code               7243347
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Shared sites
{V1, Mo1}
{V2, Mo2}
{V3, Mo3}
{V4, Mo4}
{V5, Mo5}
2. Restrained distances
 N2-H2B = N2-H2A = N2-H2C
 0.9 with sigma of 0.02
 N2-H2D
 0.9 with sigma of 0.02
 Na1-H16A \\sim Na1-H16B
 with sigma of 0.02
 Na1-H18A \\sim Na1-H18B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(V1) = Uanis(Mo1)
Uanis(V2) = Uanis(Mo2)
Uanis(V3) = Uanis(Mo3)
Uanis(V4) = Uanis(Mo4)
Uanis(V5) = Uanis(Mo5)
4. Others
 Fixed Sof: V2(0.905) Mo2(0.095) V3(0.905) Mo3(0.095) V1(0.905) Mo1(0.095)
 V5(0.905) Mo5(0.095) N1(0.7625) H1A(0.7625) H1B(0.7625) H1C(0.7625)
 H1D(0.7625) N2(0.7625) H2A(0.7625) H2B(0.7625) H2C(0.7625) H2D(0.7625)
 V4(0.905) Mo4(0.095)
5.a Riding coordinates:
 N1(H1A,H1B,H1C), N1(H1D), N2(H2A,H2B,H2C)
5.b Free rotating group:
 O18(H18A,H18B), O16(H16A,H16B)
5.c Rotating group:
 O14(H14A,H14B)
5.d Secondary CH2 refined with riding coordinates:
 O17(H17A,H17B)
5.e X=CH2 refined with riding coordinates:
 O15(H15A,H15B)
;
_shelx_res_checksum              12336
_olex2_submission_special_instructions 'No special instructions were received'