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_7720109
_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
'2(H2 Mo4 O14), 2(C6 H24 Co N6), 6(H2 O), 2(Cl)'
_chemical_formula_sum            'C12 H64 Cl2 Co2 Mo8 N12 O34'
_chemical_formula_weight         1877.02
_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             2025-06-17
_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                88.228(4)
_cell_angle_beta                 87.964(4)
_cell_angle_gamma                82.297(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4453(6)
_cell_length_b                   14.1720(7)
_cell_length_c                   15.4608(6)
_cell_measurement_reflns_used    5804
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.6550
_cell_measurement_theta_min      2.8670
_cell_volume                     2482.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 41.123a 64-bit (release 20-01-2022))'
_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      169.99(10)
_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 0.944
_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     97.00 126.00   0.50    0.80    --  113.25  61.00   0.00   58
  2  \w    130.00 174.00   0.50    0.80    --  113.25  61.00   0.00   88
  3  \w    118.00 167.00   0.50    0.80    --  113.25  45.00  60.00   98
  4  \w     93.00 140.00   0.50    0.80    --  113.25  77.00 120.00   94
  5  \w    103.00 173.00   0.50    0.80    --  113.25  79.00  85.00  140
  6  \w    101.00 177.00   0.50    0.80    --  113.25  45.00  30.00  152
  7  \w    105.00 146.00   0.50    0.80    --  113.25  30.00 -60.00   82
  8  \w    102.00 173.00   0.50    0.80    --  113.25  45.00 -30.00  142
  9  \w    142.00 167.00   0.50    0.80    --  113.25  30.00 -90.00   50
 10  \w    127.00 178.00   0.50    0.80    --  113.25  45.00-120.00  102
 11  \w    103.00 142.00   0.50    0.80    --  113.25  30.00-150.00   78
 12  \w    101.00 139.00   0.50    0.80    --  113.25  15.00-180.00   76
 13  \w    141.00 166.00   0.50    0.80    --  113.25  15.00-180.00   50
 14  \w    103.00 137.00   0.50    0.80    --  113.25  30.00 -90.00   68
 15  \w    121.00 177.00   0.50    0.80    --  113.25  15.00 150.00  112
 16  \w     41.00  88.00   0.50    0.20    --   47.74-125.00 -60.00   94
 17  \w     43.00 111.00   0.50    0.80    --  113.25-125.00  30.00  136
 18  \w     65.00 111.00   0.50    0.80    --  113.25-125.00   0.00   92
 19  \w     43.00  68.00   0.50    0.80    --  113.25-125.00  90.00   50
 20  \w     79.00 111.00   0.50    0.80    --  113.25-125.00 120.00   64
 21  \w     77.00 107.00   0.50    0.80    --  113.25-125.00  90.00   60
 22  \w     61.00 111.00   0.50    0.80    --  113.25-125.00 -60.00  100
 23  \w     43.00 111.00   0.50    0.80    --  113.25-125.00 -90.00  136
 24  \w     69.00 106.00   0.50    0.80    --  113.25-125.00-180.00   74
 25  \w     84.00 109.00   0.50    0.80    --  113.25-113.00-165.97   50
 26  \w     73.00 111.00   0.50    0.80    --  113.25-125.00 -30.00   76
 27  \w     54.00 102.00   0.50    0.80    --  113.25 -95.00 -60.00   96
 28  \w     58.00 107.00   0.50    0.80    --  113.25-109.00  47.02   98
 29  \w     42.00  68.00   0.50    0.80    --  113.25 -95.00  90.00   52
 30  \w     42.00  75.00   0.50    0.80    --  113.25-125.00 150.00   66
 31  \w     70.00 109.00   0.50    0.80    --  113.25-114.00 134.17   78
 32  \w     67.00 102.00   0.50    0.80    --  113.25 -95.00 150.00   70
 33  \w     76.00 102.00   0.50    0.80    --  113.25 -95.00  90.00   52
 34  \w     42.00 103.00   0.50    0.80    --  113.25 -95.00-180.00  122
 35  \w     45.00  83.00   0.50    0.80    --  113.25 -95.00-150.00   76
 36  \w    111.00 137.00   0.50    0.80    --  113.25 -79.00 -38.00   52
 37  \w     43.00  69.00   0.50    0.80    --  113.25 -61.00-120.00   52
 38  \w     42.00  89.00   0.50    0.80    --  113.25 -77.00-150.00   94
 39  \w     43.00  70.00   0.50    0.80    --  113.25 -61.00 -90.00   54
 40  \w     57.00 100.00   0.50    0.80    --  113.25 -79.00 -38.00   86
 41  \w     57.00  82.00   0.50    0.80    --  113.25 -77.00 -30.00   50
 42  \w     46.00  71.00   0.50    0.80    --  113.25 -61.00   0.00   50
 43  \w     42.00  67.00   0.50    0.80    --  113.25 -61.00  60.00   50
 44  \w     44.00  70.00   0.50    0.80    --  113.25 -61.00  90.00   52
 45  \w     46.00  71.00   0.50    0.80    --  113.25 -61.00 120.00   50
 46  \w     -4.00  70.00   0.50    0.20    --   47.74 -79.00 -38.00  148
 47  \w    -11.00  40.00   0.50    0.20    --   47.74 -38.00   0.00  102
 48  \w    -17.00  12.00   0.50    0.20    --   47.74 -19.00  60.00   58
 49  \w    -60.00  14.00   0.50    0.20    --  -47.74  79.00  85.00  148
 50  \w    -91.00 -66.00   0.50    0.80    --  -91.75  79.00  85.00   50
 51  \w    -23.00  26.00   0.50    0.20    --  -47.74  19.00 -30.00   98
 52  \w    -51.00 -26.00   0.50    0.80    --  -91.75  45.00 -60.00   50
 53  \w    -50.00 -24.00   0.50    0.80    --  -91.75  45.00-150.00   52
 54  \w   -154.00-120.00   0.50    0.80    --  -91.75 -79.00 -38.00   68
 55  \w   -116.00 -88.00   0.50    0.20    --  -47.74 -77.00   0.00   56
 56  \w   -118.00 -89.00   0.50    0.20    --  -47.74 -77.00  30.00   58
 57  \w   -119.00 -88.00   0.50    0.20    --  -47.74 -77.00  60.00   62
 58  \w   -154.00-128.00   0.50    0.80    --  -91.75 -77.00  60.00   52
 59  \w   -112.00 -83.00   0.50    0.20    --  -47.74-125.00  30.00   58
 60  \w   -117.00 -80.00   0.50    0.20    --  -47.74-125.00  90.00   74
;
_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      -0.0682844000
_diffrn_orient_matrix_UB_12      -0.0252597000
_diffrn_orient_matrix_UB_13      -0.0782960000
_diffrn_orient_matrix_UB_21      0.1112818000
_diffrn_orient_matrix_UB_22      -0.0626337000
_diffrn_orient_matrix_UB_23      -0.0345478000
_diffrn_orient_matrix_UB_31      -0.0376996000
_diffrn_orient_matrix_UB_32      -0.0864887000
_diffrn_orient_matrix_UB_33      0.0512297000
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36477
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         82.381
_diffrn_reflns_theta_min         3.148
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.007
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10433
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+16.8971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9589
_reflns_number_total             10433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03064a2.cif
_cod_data_source_block           exp_7358
_cod_depositor_comments
'Adding full bibliography for 7720101--7720111.cif.'
_cod_database_code               7720109
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co2 Mo8 C12 N12 O34'
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.460
_olex2_refinement_description
;
1. Restrained distances
 H14A-H15B
 2.1 with sigma of 0.00001
 Mo4-H14A \\sim Mo4-H14B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O31B) = Uanis(O31A)
Uanis(O32B) = Uanis(O32A)
Uanis(O33A) = Uanis(O33B)
Uanis(O34A) = Uanis(O34B)
3. Others
 Sof(O32A)=1-FVAR(1)
 Sof(O32B)=FVAR(1)
 Sof(O33B)=1-FVAR(2)
 Sof(O33A)=FVAR(2)
 Sof(O34B)=1-FVAR(3)
 Sof(O34A)=FVAR(3)
 Fixed Sof: O31B(0.5) O31A(0.5)
4.a Free rotating group:
 O14(H14A,H14B)
4.b Rotating group:
 O15(H15A,H15B)
4.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), N8(H8A,H8B), N7(H7A,H7B), N5(H5A,H5B), N6(H6A,H6B),
 N9(H9A,H9B), N12(H12A,H12B), N10(H10A,H10B), N11(H11A,H11B), N1(H1A,H1B),
 N4(H4A,H4B), C7(H7C,H7D), C6(H6C,H6D), C5(H5C,H5D), C10(H10C,H10D), C2(H2C,
 H2D), C8(H8C,H8D), C11(H11C,H11D), C9(H9C,H9D), C1(H1C,H1D), C12(H12C,H12D),
 C4(H4C,H4D), C3(H3C,H3D)
;
_shelx_res_checksum              32095
_shelx_hkl_checksum              75197
_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 2.794
_oxdiff_exptl_absorpt_empirical_full_min 0.685