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_7720105
_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(C6 H16 Co N4 O4), 12H2O'
_chemical_formula_sum            'C24 H88 Co4 Ge Mo12 N16 O68'
_chemical_formula_weight         3148.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-10
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-10 deposited with the CCDC.	2026-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.300(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1320(7)
_cell_length_b                   12.0745(7)
_cell_length_c                   25.9671(16)
_cell_measurement_reflns_used    3815
_cell_measurement_temperature    177.1(2)
_cell_measurement_theta_max      77.4250
_cell_measurement_theta_min      3.4180
_cell_volume                     4110.6(4)
_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      177.1(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.970
_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    -78.00 -35.00   0.50    1.50    --  -47.74 -42.00  13.00   86
  2  \w    -45.00  19.00   0.50    1.50    --  -47.74  42.00 165.00  128
  3  \w     11.00  47.00   0.50    1.50    --   47.74 -42.00  13.00   72
  4  \w     41.00 120.00   0.50    1.50    --   47.74  42.00 165.00  158
  5  \w   -146.00-121.00   0.50    6.00    --  -91.75 -42.00  13.00   50
  6  \w    -47.00 -20.00   0.50    6.00    --  -91.75  42.00 165.00   54
  7  \w    137.00 177.00   0.50    6.00    --  113.25  42.00 165.00   80
  8  \w   -119.00 -88.00   0.50    1.50    --  -47.74 -77.00-120.00   62
  9  \w   -119.00 -89.00   0.50    1.50    --  -47.74 -77.00 -90.00   60
 10  \w    -83.00 -14.00   0.50    1.50    --  -47.74 125.00-120.00  138
 11  \w   -118.00 -89.00   0.50    1.50    --  -47.74 -77.00   0.00   58
 12  \w   -118.00 -88.00   0.50    1.50    --  -47.74 -77.00 -60.00   60
 13  \w    -51.00 -21.00   0.50    6.00    --  -91.75  61.00 -30.00   60
 14  \w    102.00 177.00   0.50    6.00    --  113.25  15.00 -60.00  150
 15  \w     42.00  67.00   0.50    6.00    --  113.25 -61.00   0.00   50
 16  \w    140.00 178.00   0.50    6.00    --  113.25  30.00-120.00   76
 17  \w     42.00  67.00   0.50    6.00    --  113.25 -61.00 150.00   50
 18  \w     50.00  91.00   0.50    6.00    --  113.25 -77.00 -90.00   82
 19  \w     45.00 104.00   0.50    6.00    --  113.25 -95.00 150.00  118
 20  \w     45.00  70.00   0.50    6.00    --  113.25 -61.00-180.00   50
 21  \w     42.00  67.00   0.50    6.00    --  113.25 -61.00-150.00   50
 22  \w     48.00  97.00   0.50    6.00    --  113.25 -77.00   0.00   98
 23  \w     44.00 104.00   0.50    6.00    --  113.25 -77.00  60.00  120
 24  \w     44.00  92.00   0.50    6.00    --  113.25 -77.00  30.00   96
 25  \w    153.00 178.00   0.50    6.00    --  113.25  61.00-180.00   50
 26  \w     42.00  70.00   0.50    6.00    --  113.25 -61.00  90.00   56
 27  \w     44.00  88.00   0.50    6.00    --  113.25 -95.00 120.00   88
 28  \w     45.00 102.00   0.50    6.00    --  113.25-125.00   0.00  114
 29  \w     42.00  67.00   0.50    6.00    --  113.25 -61.00 -90.00   50
 30  \w     97.00 140.00   0.50    6.00    --  113.25  61.00-180.00   86
 31  \w    104.00 130.00   0.50    6.00    --  113.25  30.00 -60.00   52
 32  \w     45.00  70.00   0.50    6.00    --  113.25 -61.00  60.00   50
 33  \w     42.00  67.00   0.50    6.00    --  113.25 -61.00 -60.00   50
 34  \w    121.00 173.00   0.50    6.00    --  113.25  15.00 150.00  104
 35  \w     57.00  83.00   0.50    6.00    --  113.25 -77.00-150.00   52
 36  \w     47.00  97.00   0.50    6.00    --  113.25 -77.00-120.00  100
 37  \w    104.00 136.00   0.50    6.00    --  113.25  30.00-120.00   64
;
_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      0.0298196000
_diffrn_orient_matrix_UB_12      -0.0004240000
_diffrn_orient_matrix_UB_13      -0.0564989000
_diffrn_orient_matrix_UB_21      0.0966086000
_diffrn_orient_matrix_UB_22      0.0673346000
_diffrn_orient_matrix_UB_23      0.0155160000
_diffrn_orient_matrix_UB_31      0.0598333000
_diffrn_orient_matrix_UB_32      -0.1084302000
_diffrn_orient_matrix_UB_33      0.0098770000
_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  0.1005
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35687
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.239
_diffrn_reflns_theta_min         4.039
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.121
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.153
_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    2.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.878
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.00022(3)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         8715
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0881
_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^)+(0.0898P)^2^+63.1675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2148
_refine_ls_wR_factor_ref         0.2299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6396
_reflns_number_total             8715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03064a2.cif
_cod_data_source_block           exp_7093
_cod_depositor_comments
'Adding full bibliography for 7720101--7720111.cif.'
_cod_database_code               7720105
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 Co4 Mo12 N16 O68 Ge'
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.177
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups, All N(H,H,H,H)
  groups
2. Restrained distances
 Mo4-O16B
 1.65 with sigma of 0.001
 N8-C12A \\sim N8-C12B
 with sigma of 0.02
 C11-C12A \\sim C11-C12B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O7A) = Uanis(O7B)
Uanis(O11B) = Uanis(O11A)
Uanis(O8A) = Uanis(O8B)
Uanis(O12A) = Uanis(O12B)
Uanis(O10B) = Uanis(O10A)
Uanis(O20A) = Uanis(O20B)
Uanis(O16A) = Uanis(O16B)
Uanis(O21B) = Uanis(O21A)
Uanis(O19B) = Uanis(O19A)
Uanis(O18B) = Uanis(O18A)
Uanis(O8B) = Uanis(O8A) = Uanis(O17)
Uanis(C11) = Uanis(C12A) = Uanis(C12B)
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Fixed Sof: O4(0.5) O7B(0.5) O8B(0.5) O3(0.5) O11B(0.5) O2(0.5) O1(0.5)
 O8A(0.5) O11A(0.5) O7A(0.5) O12A(0.5) O12B(0.5) O10A(0.5) O10B(0.5) O20A(0.5)
 O20B(0.5) O16B(0.5) O16A(0.5) O21A(0.5) O21B(0.5) O19B(0.5) O19A(0.5)
 O18B(0.5) O18A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), N3(H3A,H3B), N1(H1A,H1B), N7(H7A,H7B), N6(H6A,H6B),
 N5(H5A,H5B), N8(H8AA,H8AB), N8(H8BC,H8BD), C6(H6C,H6D), C5(H5C,H5D), C9(H9A,
 H9B), C10(H10A,H10B), C3(H3C,H3D), C4(H4C,H4D), C11(H11A,H11B), C11(H11C,H11D),
  C12A(H12A,H12B), C12B(H12C,H12D)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 244 electrons were 
found in a volume of 724\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
12[H2O] per Formula Unit 
which account for 240 electrons 
per unit cell.
;
_shelx_res_checksum              11555
_shelx_hkl_checksum              863
_shelx_fab_checksum              51478
_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 1.962
_oxdiff_exptl_absorpt_empirical_full_min 0.544