Synthesis, structural characterization and properties of a series of heteropolyoxomolybdates: [AlMo<sub>6</sub>(OH)<sub>6</sub>O<sub>18</sub>]<sup>3-</sup>, [GeMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>, [GeMo<sub>6</sub>O<sub>22</sub>(Hmal)<sub>3</sub>]<sup>7-</sup>, [SiMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>, and [TeMo<sub>6</sub>O<sub>24</sub>]<sup>6</sup>.
Kuzman, D.; Damjanović, V; Toplak, J.; Medak, G.; Halasz, I.; Hrenar, T.; Cindrić, M; Vrdoljak, V.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3442–3453; doi:10.1039/d5dt03064a

data_7720110
_publ_section_title
;
 Synthesis, structural characterization and properties of a series of
 heteropolyoxomolybdates:
 [AlMo<sub>6</sub>(OH)<sub>6</sub>O<sub>18</sub>]<sup>3-</sup>,
 [GeMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>,
 [GeMo<sub>6</sub>O<sub>22</sub>(Hmal)<sub>3</sub>]<sup>7-</sup>,
 [SiMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>, and
 [TeMo<sub>6</sub>O<sub>24</sub>]<sup>6</sup>.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3442
_journal_page_last               3453
_journal_paper_doi               10.1039/d5dt03064a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety
'C13 H36.5 Co2 Ge Mo6 N8 Na4 O46.75, C2 H12 Co N4 O4, 3(H2O)'
_chemical_formula_sum            'C15 H54.5 Co3 Ge Mo6 N12 Na4 O53.75'
_chemical_formula_weight         2180.17
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-12-10 deposited with the CCDC.	2026-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                106.021(2)
_cell_angle_beta                 101.646(2)
_cell_angle_gamma                91.277(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4262(2)
_cell_length_b                   14.6913(3)
_cell_length_c                   20.8988(5)
_cell_measurement_reflns_used    16942
_cell_measurement_temperature    186.8(3)
_cell_measurement_theta_max      77.9220
_cell_measurement_theta_min      3.1340
_cell_volume                     3003.13(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      186.8(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.960
_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   -116.00 -80.00   0.50    0.60    --  -47.74 -16.00  75.00   72
  2  \w     34.00  65.00   0.50    0.60    --   47.74  16.00-115.00   62
  3  \w    -27.00  23.00   0.50    0.60    --   47.74 -16.00  75.00  100
  4  \w     78.00 104.00   0.50    0.60    --   47.74  16.00-115.00   52
  5  \w   -126.00 -92.00   0.50    2.40    --  -91.75 -16.00  75.00   68
  6  \w    102.00 149.00   0.50    2.40    --  113.25  16.00-115.00   94
  7  \w    -24.00  21.00   0.50    0.60    --  -47.74  16.00-115.00   90
  8  \w    -71.00 -36.00   0.50    0.60    --  -47.74 -16.00  75.00   70
  9  \w    -86.00 -53.00   0.50    0.60    --  -47.74 125.00 120.00   66
 10  \w    -38.00  25.00   0.50    0.60    --  -47.74  38.00 -90.00  126
 11  \w    -44.00 -14.00   0.50    0.60    --  -47.74 125.00 120.00   60
 12  \w   -118.00 -88.00   0.50    0.60    --  -47.74 -77.00 150.00   60
 13  \w   -119.00 -88.00   0.50    0.60    --  -47.74 -77.00  30.00   62
 14  \w     91.00 120.00   0.50    0.60    --   47.74  77.00  30.00   58
 15  \w     -1.00  65.00   0.50    0.60    --   47.74 -99.00 120.00  132
 16  \w     63.00  89.00   0.50    0.60    --   47.74-125.00 120.00   52
 17  \w    -48.00 -23.00   0.50    2.40    --  -91.75  45.00-120.00   50
 18  \w    -83.00 -27.00   0.50    2.40    --  -91.75 125.00 -60.00  112
 19  \w    -51.00 -21.00   0.50    2.40    --  -91.75  45.00 120.00   60
 20  \w    -49.00 -23.00   0.50    2.40    --  -91.75  45.00-150.00   52
 21  \w    103.00 147.00   0.50    2.40    --  113.25  15.00  60.00   88
 22  \w     44.00  88.00   0.50    2.40    --  113.25 -77.00-180.00   88
 23  \w     45.00  71.00   0.50    2.40    --  113.25 -61.00-150.00   52
 24  \w     45.00  71.00   0.50    2.40    --  113.25 -61.00  30.00   52
 25  \w    109.00 152.00   0.50    2.40    --  113.25  45.00 -30.00   86
 26  \w     79.00 110.00   0.50    2.40    --  113.25-125.00 120.00   62
 27  \w    105.00 175.00   0.50    2.40    --  113.25  15.00 -60.00  140
 28  \w     44.00  73.00   0.50    2.40    --  113.25-125.00 120.00   58
 29  \w    108.00 158.00   0.50    2.40    --  113.25  30.00  60.00  100
 30  \w     53.00  98.00   0.50    2.40    --  113.25 -95.00  30.00   90
 31  \w    101.00 178.00   0.50    2.40    --  113.25  45.00 120.00  154
 32  \w     75.00 100.00   0.50    2.40    --  113.25 -95.00  60.00   50
 33  \w     42.00  74.00   0.50    2.40    --  113.25 -95.00-120.00   64
 34  \w     79.00 105.00   0.50    2.40    --  113.25 -95.00-120.00   52
 35  \w     61.00 104.00   0.50    2.40    --  113.25 -95.00 150.00   86
 36  \w     43.00  92.00   0.50    2.40    --  113.25 -77.00 120.00   98
 37  \w     44.00  96.00   0.50    2.40    --  113.25-125.00   0.00  104
 38  \w    101.00 154.00   0.50    2.40    --  113.25  45.00-180.00  106
 39  \w     72.00 105.00   0.50    2.40    --  113.25-125.00  90.00   66
 40  \w     73.00 100.00   0.50    2.40    --  113.25 -95.00 -90.00   54
 41  \w     42.00  68.00   0.50    2.40    --  113.25 -77.00   0.00   52
 42  \w     46.00 107.00   0.50    2.40    --  113.25-125.00 150.00  122
 43  \w     43.00  71.00   0.50    2.40    --  113.25 -95.00 -90.00   56
 44  \w    102.00 162.00   0.50    2.40    --  113.25  15.00  30.00  120
 45  \w     81.00 111.00   0.50    2.40    --  113.25-125.00-180.00   60
 46  \w    104.00 178.00   0.50    2.40    --  113.25  15.00 -90.00  148
 47  \w     52.00  78.00   0.50    2.40    --  113.25-134.00  28.17   52
 48  \w     81.00 118.00   0.50    2.40    --  113.25-134.00  28.17   74
 49  \w    119.00 172.00   0.50    2.40    --  113.25  45.00 150.00  106
 50  \w    134.00 161.00   0.50    2.40    --  113.25 125.00  30.00   54
 51  \w     66.00 111.00   0.50    2.40    --  113.25-125.00-120.00   90
 52  \w     48.00 102.00   0.50    2.40    --  113.25-125.00 -30.00  108
 53  \w     44.00  69.00   0.50    2.40    --  113.25-125.00-180.00   50
 54  \w     79.00 105.00   0.50    2.40    --  113.25 -95.00   0.00   52
 55  \w     51.00 109.00   0.50    2.40    --  113.25-125.00  30.00  116
 56  \w     80.00 111.00   0.50    2.40    --  113.25-125.00 -90.00   62
 57  \w    126.00 167.00   0.50    2.40    --  113.25 125.00  60.00   82
 58  \w     44.00  71.00   0.50    2.40    --  113.25 -95.00  60.00   54
 59  \w     49.00 108.00   0.50    2.40    --  113.25-108.00 110.20  118
 60  \w     42.00 106.00   0.50    2.40    --  113.25 -95.00-180.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0015832000
_diffrn_orient_matrix_UB_12      -0.1088582000
_diffrn_orient_matrix_UB_13      -0.0155522000
_diffrn_orient_matrix_UB_21      -0.1451290000
_diffrn_orient_matrix_UB_22      -0.0051946000
_diffrn_orient_matrix_UB_23      0.0052144000
_diffrn_orient_matrix_UB_31      -0.0430392000
_diffrn_orient_matrix_UB_32      -0.0103818000
_diffrn_orient_matrix_UB_33      -0.0768251000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46687
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.033
_diffrn_reflns_theta_min         3.140
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.270
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.394
_exptl_crystal_description       plank
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.663
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       0.00114(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         12727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1338P)^2^+10.2965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10345
_reflns_number_total             12727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03064a2.cif
_cod_data_source_block           exp_7135
_cod_depositor_comments
'Adding full bibliography for 7720101--7720111.cif.'
_cod_database_code               7720110
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ge Mo6 C15 Na4 N12 O53.75'
_cell_oxdiff_angle_alpha         106.0207(18)
_cell_oxdiff_angle_beta          101.6460(19)
_cell_oxdiff_angle_gamma         91.2767(17)
_cell_oxdiff_length_a            10.4262(2)
_cell_oxdiff_length_b            14.6913(3)
_cell_oxdiff_length_c            20.8988(5)
_cell_oxdiff_measurement_reflns_used 16942
_cell_oxdiff_volume              3003.15(11)
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.138
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Na3A) = Uanis(Na3B)
Uanis(O54C) = Uanis(O54A) = Uanis(O54B)
3. Others
 Sof(Na3A)=1-FVAR(1)
 Sof(Na3B)=FVAR(1)
 Fixed Sof: Na4B(0.5) O54A(0.25) O54B(0.25) O54C(0.25)
4.a Tetrahedral OH refined with riding coordinates:
 O26(H26), O30(H30), O34(H34)
4.b Idealised Me refined as rotating group:
 N9(H9A,H9B,H9C), N10(H10A,H10B,H10C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C),
 N11(H11A,H11B,H11C), N12(H12A,H12B,H12C), N1(H1A,H1B,H1C), N2(H2A,H2B,H2C),
 N6(H6A,H6B,H6C), N5(H5A,H5B,H5C), N7(H7A,H7B,H7C), N8(H8A,H8B,H8C)
;
_shelx_res_checksum              55127
_shelx_hkl_checksum              11688
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.183
_oxdiff_exptl_absorpt_empirical_full_min 0.561