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_7720103
_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         'Ge Mo12 O40, 4(C2 H12 Co N4 O4), 6(H2 O)'
_chemical_formula_sum            'C8 H60 Co4 Ge Mo12 N16 O62'
_chemical_formula_weight         2832.31
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.67110(10)
_cell_length_b                   16.67110(10)
_cell_length_c                   23.1637(2)
_cell_measurement_reflns_used    35630
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      79.5960
_cell_measurement_theta_min      3.2520
_cell_volume                     6437.78(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.81a 64-bit (release 30-01-2023))'
_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_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -73.00 -40.00   0.50    1.00    --  -48.22  97.00 -80.00   66
  2  \w      7.00  74.00   0.50    1.00    --   48.22 -97.00 171.00  134
  3  \w    -75.00 -50.00   0.50    4.00    --  -91.75  97.00 -80.00   50
  4  \w   -149.00-123.00   0.50    4.00    --  -91.75 -97.00 171.00   52
  5  \w     43.00  77.00   0.50    4.00    --  113.25 -97.00 171.00   68
  6  \w    118.00 143.00   0.50    4.00    --  113.25  97.00 -80.00   50
  7  \w    -62.00 -35.00   0.50    1.00    --  -48.22  57.00 -30.00   54
  8  \w   -119.00 -88.00   0.50    1.00    --  -48.22 -77.00-150.00   62
  9  \w    -31.00  24.00   0.50    1.00    --  -48.22  57.00 -30.00  110
 10  \w   -119.00 -94.00   0.50    1.00    --  -48.22 -77.00 -60.00   50
 11  \w   -120.00 -89.00   0.50    1.00    --  -48.22 -77.00 -90.00   62
 12  \w   -120.00 -89.00   0.50    1.00    --  -48.22 -77.00-120.00   62
 13  \w    -36.00  15.00   0.50    1.00    --  -48.22  97.00 -80.00  102
 14  \w     40.00  93.00   0.50    1.00    --   48.22-125.00 150.00  106
 15  \w    -22.00  17.00   0.50    1.00    --   48.22 -19.00 -90.00   78
 16  \w    -12.00  14.00   0.50    1.00    --   48.22 -19.00   0.00   52
 17  \w   -159.00 -93.00   0.50    4.00    --  -91.75 -77.00 -90.00  132
 18  \w     42.00  68.00   0.50    4.00    --  113.25 -95.00-120.00   52
 19  \w     68.00 110.00   0.50    4.00    --  113.25-125.00 150.00   84
 20  \w     58.00 106.00   0.50    4.00    --  113.25 -95.00  60.00   96
 21  \w    104.00 135.00   0.50    4.00    --  113.25  45.00  90.00   62
 22  \w     75.00 107.00   0.50    4.00    --  113.25-109.00   0.86   64
 23  \w     45.00  74.00   0.50    4.00    --  113.25 -77.00-180.00   58
 24  \w     42.00  71.00   0.50    4.00    --  113.25 -61.00  30.00   58
 25  \w     46.00  71.00   0.50    4.00    --  113.25 -61.00   0.00   50
 26  \w    100.00 163.00   0.50    4.00    --  113.25  15.00  90.00  126
 27  \w     61.00 107.00   0.50    4.00    --  113.25-109.00 -34.21   92
 28  \w     42.00  87.00   0.50    4.00    --  113.25 -82.00 -11.64   90
 29  \w     46.00  73.00   0.50    4.00    --  113.25-125.00 -60.00   54
 30  \w     81.00 111.00   0.50    4.00    --  113.25-125.00 -60.00   60
 31  \w     42.00 111.00   0.50    4.00    --  113.25 -84.00-176.89  138
 32  \w    135.00 177.00   0.50    4.00    --  113.25  30.00   0.00   84
 33  \w     71.00 105.00   0.50    4.00    --  113.25 -95.00-180.00   68
 34  \w    102.00 138.00   0.50    4.00    --  113.25  45.00 120.00   72
 35  \w    145.00 177.00   0.50    4.00    --  113.25  45.00 120.00   64
 36  \w    116.00 141.00   0.50    4.00    --  113.25  45.00 -60.00   50
 37  \w    105.00 162.00   0.50    4.00    --  113.25  77.00 150.00  114
 38  \w     42.00  68.00   0.50    4.00    --  113.25 -61.00-120.00   52
 39  \w     86.00 127.00   0.50    4.00    --  113.25-146.00  89.65   82
 40  \w     49.00  79.00   0.50    4.00    --  113.25 -77.00 -60.00   60
 41  \w    101.00 174.00   0.50    4.00    --  113.25  30.00 -90.00  146
 42  \w     59.00  98.00   0.50    4.00    --  113.25 -77.00-120.00   78
 43  \w    126.00 151.00   0.50    4.00    --  113.25  30.00  90.00   50
 44  \w    128.00 169.00   0.50    4.00    --  113.25 125.00-180.00   82
 45  \w     44.00  76.00   0.50    4.00    --  113.25-125.00-120.00   64
 46  \w     86.00 111.00   0.50    4.00    --  113.25-125.00-120.00   50
 47  \w     54.00  79.00   0.50    4.00    --  113.25 -66.00-115.54   50
 48  \w     55.00  95.00   0.50    4.00    --  113.25 -95.00 150.00   80
 49  \w    131.00 156.00   0.50    4.00    --  113.25  30.00  60.00   50
 50  \w     48.00  90.00   0.50    4.00    --  113.25 -77.00 120.00   84
 51  \w    117.00 161.00   0.50    4.00    --  113.25  61.00 -90.00   88
 52  \w     97.00 126.00   0.50    4.00    --  113.25 125.00  90.00   58
 53  \w    133.00 167.00   0.50    4.00    --  113.25 125.00  90.00   68
 54  \w     79.00 111.00   0.50    4.00    --  113.25-125.00 -90.00   64
 55  \w     44.00  75.00   0.50    4.00    --  113.25-125.00  60.00   62
 56  \w     86.00 111.00   0.50    4.00    --  113.25-125.00  60.00   50
 57  \w    105.00 161.00   0.50    4.00    --  113.25  45.00  30.00  112
 58  \w    101.00 131.00   0.50    4.00    --  113.25  30.00   0.00   60
 59  \w     61.00  86.00   0.50    4.00    --  113.25 -77.00  90.00   50
 60  \w     86.00 111.00   0.50    4.00    --  113.25-125.00-180.00   50
 61  \w     63.00  88.00   0.50    4.00    --  113.25-136.00  91.21   50
 62  \w     95.00 120.00   0.50    4.00    --  113.25-136.00  91.21   50
 63  \w     42.00  67.00   0.50    4.00    --  113.25 -61.00 -90.00   50
 64  \w     43.00  80.00   0.50    4.00    --  113.25 -77.00 -30.00   74
 65  \w     83.00 108.00   0.50    4.00    --  113.25-108.00 -74.96   50
 66  \w     44.00  70.00   0.50    4.00    --  113.25-125.00-150.00   52
 67  \w     86.00 111.00   0.50    4.00    --  113.25-125.00-150.00   50
 68  \w     51.00  96.00   0.50    4.00    --  113.25   0.00  60.00   90
 69  \w     60.00  86.00   0.50    4.00    --  113.25 -77.00  60.00   52
 70  \w     92.00 118.00   0.50    4.00    --  113.25 -87.00  51.92   52
 71  \w     43.00  70.00   0.50    4.00    --  113.25 -77.00-150.00   54
 72  \w     42.00  89.00   0.50    4.00    --  113.25 -88.00 -43.51   94
 73  \w     45.00  92.00   0.50    4.00    --  113.25-125.00  30.00   94
 74  \w     61.00 107.00   0.50    4.00    --  113.25 -78.00  71.21   92
 75  \w    143.00 174.00   0.50    4.00    --  113.25  15.00-120.00   62
 76  \w    117.00 145.00   0.50    4.00    --  113.25  30.00 -60.00   56
 77  \w    153.00 178.00   0.50    4.00    --  113.25  45.00 -60.00   50
 78  \w     52.00  77.00   0.50    4.00    --  113.25-125.00-180.00   50
 79  \w    116.00 143.00   0.50    4.00    --  113.25  30.00 150.00   54
 80  \w    153.00 178.00   0.50    4.00    --  113.25  30.00 150.00   50
 81  \w     99.00 124.00   0.50    4.00    --  113.25  61.00  60.00   50
 82  \w    103.00 178.00   0.50    4.00    --  113.25  61.00  90.00  150
 83  \w    135.00 161.00   0.50    4.00    --  113.25 125.00-120.00   52
 84  \w    116.00 162.00   0.50    4.00    --  113.25 125.00 -30.00   92
 85  \w    140.00 168.00   0.50    4.00    --  113.25 125.00   0.00   56
 86  \w    104.00 156.00   0.50    4.00    --  113.25  77.00 -30.00  104
 87  \w    123.00 159.00   0.50    4.00    --  113.25  77.00   0.00   72
 88  \w    113.00 138.00   0.50    4.00    --  113.25 -82.00 118.80   50
 89  \w     46.00  71.00   0.50    4.00    --  113.25 -61.00 -30.00   50
;
_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      0.0368297000
_diffrn_orient_matrix_UB_12      0.0587980000
_diffrn_orient_matrix_UB_13      -0.0439312000
_diffrn_orient_matrix_UB_21      0.0071510000
_diffrn_orient_matrix_UB_22      -0.0684514000
_diffrn_orient_matrix_UB_23      -0.0443767000
_diffrn_orient_matrix_UB_31      -0.0844553000
_diffrn_orient_matrix_UB_32      0.0198607000
_diffrn_orient_matrix_UB_33      -0.0229085000
_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  0.0804
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65855
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.961
_diffrn_reflns_theta_min         5.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    28.045
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.298
_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    2.918
_exptl_crystal_description       block
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+42.6173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3267
_reflns_number_total             3492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03064a2.cif
_cod_data_source_block           exp_5954
_cod_depositor_comments
'Adding full bibliography for 7720101--7720111.cif.'
_cod_original_cell_volume        6437.78(10)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7720103
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ge Mo12 Co4 C8 N16 O56'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.284
_diffrn_oxdiff_ac3_digest_hkl    01c5cf0e9f5c56ef201dd244ae2df64c1c03f0
_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,H) groups
2.a Free rotating group:
 O16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N3(H3A,H3B,H3C), N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              15055
_shelx_hkl_checksum              42064
_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 2.585
_oxdiff_exptl_absorpt_empirical_full_min 0.471