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_7243348
_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         'Mo0.13 O28 V9.87, H20 Li2 O10, 3.87(H4 N1)'
_chemical_formula_sum            'H35.48 Li2 Mo0.13 N3.87 O38 V9.87'
_chemical_formula_weight         1227.11
_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             2021-06-25
_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                68.641(2)
_cell_angle_beta                 87.059(2)
_cell_angle_gamma                67.707(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5037(5)
_cell_length_b                   10.2366(6)
_cell_length_c                   11.0539(7)
_cell_measurement_reflns_used    9388
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.549
_cell_measurement_theta_min      3.432
_cell_volume                     824.94(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      273.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_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  0.0204
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.983
_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            12457
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         3.431
_exptl_absorpt_coefficient_mu    2.842
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0812 before and 0.0366 after correction.
The Ratio of minimum to maximum transmission is 0.7736.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.470
_exptl_crystal_description       block
_exptl_crystal_F_000             605
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3755
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0438P)^2^+1.1106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3443
_reflns_number_total             3755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00875g2.cif
_cod_data_source_block           licl
_cod_depositor_comments
'Adding full bibliography for 7243347--7243348.cif.'
_cod_database_code               7243348
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Shared sites
{V1, Mo1}
{V2, Mo2}
{V3, Mo3}
{V4, Mo4}
{V5, Mo5}
3. Restrained distances
 O17-H17B
 0.98 with sigma of 0.02
 Li1-H16A \\sim Li1-H16B
 with sigma of 0.02
 Li1-H14A \\sim Li1-H14B
 with sigma of 0.02
4. 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)
5. Others
 Fixed Sof: V2(0.987) Mo2(0.013) V3(0.987) Mo3(0.013) V4(0.987) Mo4(0.013)
 V1(0.987) Mo1(0.013) V5(0.987) Mo5(0.013) N2(0.9675) H2A(0.9675) H2B(0.9675)
 H2C(0.9675) H2D(0.9675) N1(0.9675) H1A(0.9675) H1B(0.9675) H1C(0.9675)
 H1D(0.9675)
6.a Riding coordinates:
 N2(H2A,H2B,H2C), N2(H2D), N1(H1A,H1B,H1C), N1(H1D)
6.b Free rotating group:
 O16(H16A,H16B), O14(H14A,H14B)
6.c Rotating group:
 O15(H15A)
6.d X=CH2 refined with riding coordinates:
 O18(H18A,H18B)
;
_shelx_res_checksum              73853
_olex2_submission_special_instructions 'No special instructions were received'