Aqueous solution as a playground of {MoO4}, {Mo4O12}, {Mo8O26}, {Mo8V5O40} and {V7Mo2O27} species in the presence of carboxylic acids and [Co(C2O4)(NH3)4]+ or [Co(en)3]3+ cations
Kuzman, D.; Damjanović, V.; Cindrić, M.; Vrdoljak, V.; CrystEngComm 27 (2025) 1128–1138; doi:10.1039/D4CE01187B

data_7249827
_publ_section_title
;
 Aqueous solution as a playground of {MoO4}, {Mo4O12}, {Mo8O26},
 {Mo8V5O40} and {V7Mo2O27} species in the presence of carboxylic acids and
 [Co(C2O4)(NH3)4]+ or [Co(en)3]3+ cations
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1128
_journal_page_last               1138
_journal_paper_doi               10.1039/D4CE01187B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'Mo8 O26, 4(C2 H12 Co N4 O4), 9(H2O)'
_chemical_formula_sum            'C8 H66 Co4 Mo8 N16 O51'
_chemical_formula_weight         2206.00
_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
_audit_creation_date             2024-11-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-22 deposited with the CCDC.	2025-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                108.216(2)
_cell_angle_beta                 94.540(2)
_cell_angle_gamma                103.045(2)
_cell_formula_units_Z            1
_cell_length_a                   7.9160(2)
_cell_length_b                   12.5833(3)
_cell_length_c                   15.4115(3)
_cell_measurement_reflns_used    25534
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.6790
_cell_measurement_theta_min      3.8340
_cell_volume                     1401.85(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_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     43.00 110.00   0.50    0.30    --  113.25-125.00  30.00  134
  2  \w     42.00 111.00   0.50    0.30    --  113.25-125.00 150.00  138
  3  \w     25.00  51.00   0.50    0.30    --   48.02  77.00   0.00   52
  4  \w     25.00  51.00   0.50    0.30    --   48.02  77.00  60.00   52
  5  \w     37.00  63.00   0.50    0.30    --   48.02  77.00  90.00   52
  6  \w     60.00 111.00   0.50    0.30    --  113.25-125.00  60.00  102
  7  \w     44.00 111.00   0.50    0.30    --  113.25-125.00   0.00  134
  8  \w     77.00 111.00   0.50    0.30    --  113.25-125.00  90.00   68
  9  \w     43.00 111.00   0.50    0.30    --  113.25-125.00 -90.00  136
 10  \w     80.00 105.00   0.50    0.30    --  113.25-100.00-150.48   50
 11  \w     77.00 111.00   0.50    0.30    --  113.25-125.00-180.00   68
 12  \w     45.00  72.00   0.50    0.30    --  113.25-125.00-180.00   54
 13  \w     44.00  69.00   0.50    0.30    --  113.25-100.00-150.48   50
 14  \w     50.00  96.00   0.50    0.30    --  113.25 -95.00-150.00   92
 15  \w     81.00 106.00   0.50    0.30    --  113.25 -95.00 -90.00   50
 16  \w     45.00  70.00   0.50    0.30    --  113.25 -95.00 -90.00   50
 17  \w     75.00 111.00   0.50    0.30    --  113.25-125.00 -60.00   72
 18  \w     81.00 106.00   0.50    0.30    --  113.25 -95.00  60.00   50
 19  \w     55.00  80.00   0.50    0.30    --  113.25 -95.00  60.00   50
 20  \w     60.00  86.00   0.50    0.30    --  113.25 -86.00  93.00   52
 21  \w     47.00  72.00   0.50    0.30    --  113.25-125.00  90.00   50
 22  \w     60.00 102.00   0.50    0.30    --  113.25 -95.00 150.00   84
 23  \w     -2.00  61.00   0.50    0.30    --   48.02 -86.00  93.00  126
 24  \w     42.00  67.00   0.50    0.30    --  113.25 -61.00 -60.00   50
 25  \w     45.00  70.00   0.50    0.30    --  113.25 -77.00-120.00   50
 26  \w    133.00 178.00   0.50    0.30    --  113.25  86.00-148.00   90
 27  \w     44.00  86.00   0.50    0.30    --  113.25 -77.00 -90.00   84
 28  \w     80.00 105.00   0.50    0.30    --  113.25 -77.00  30.00   50
 29  \w     44.00  74.00   0.50    0.30    --  113.25 -77.00 150.00   60
 30  \w     42.00  71.00   0.50    0.30    --  113.25 -61.00  30.00   58
 31  \w     46.00  71.00   0.50    0.30    --  113.25 -61.00-180.00   50
 32  \w    114.00 150.00   0.50    0.30    --  113.25 125.00 150.00   72
 33  \w    124.00 164.00   0.50    0.30    --  113.25  45.00 -60.00   80
 34  \w    142.00 174.00   0.50    0.30    --  113.25  77.00-150.00   64
 35  \w     32.00  80.00   0.50    0.30    --   54.00  77.00-118.30   96
 36  \w     94.00 133.00   0.50    0.30    --  113.25  77.00-150.00   78
 37  \w     91.00 174.00   0.50    0.30    --  113.25  77.00 -60.00  166
 38  \w    139.00 175.00   0.50    0.30    --  113.25  77.00 -30.00   72
 39  \w    152.00 177.00   0.50    0.30    --  113.25  77.00  60.00   50
 40  \w     95.00 145.00   0.50    0.30    --  113.25  77.00  90.00  100
 41  \w     91.00 133.00   0.50    0.30    --  113.25  77.00 120.00   84
 42  \w     95.00 142.00   0.50    0.30    --  113.25  77.00  60.00   94
 43  \w     92.00 118.00   0.50    0.30    --  113.25  77.00  30.00   52
 44  \w     91.00 117.00   0.50    0.30    --  113.25  77.00   0.00   52
 45  \w     98.00 133.00   0.50    0.30    --  113.25  77.00 -30.00   70
 46  \w     91.00 159.00   0.50    0.30    --  113.25  77.00-120.00  136
 47  \w    128.00 153.00   0.50    0.30    --  113.25  77.00   0.00   50
 48  \w    130.00 155.00   0.50    0.30    --  113.25  77.00  30.00   50
 49  \w     52.00  80.00   0.50    0.30    --   74.00  76.00 131.70   56
 50  \w     91.00 123.00   0.50    0.30    --  113.25  77.00 150.00   64
 51  \w    129.00 170.00   0.50    0.30    --  113.25  77.00 150.00   82
 52  \w    113.00 139.00   0.50    0.30    --   74.00  76.00 131.70   52
 53  \w     76.00 102.00   0.50    0.30    --   54.00  76.00  32.81   52
 54  \w     36.00  61.00   0.50    0.30    --   58.00  76.00  67.01   50
 55  \w     32.00  57.00   0.50    0.30    --   54.00  76.00  32.81   50
 56  \w     37.00  62.00   0.50    0.30    --   58.00  74.00 -30.59   50
 57  \w     36.00  62.00   0.50    0.30    --   58.00  75.00 -87.36   52
 58  \w     32.00  57.00   0.50    0.30    --   54.00  76.00-168.18   50
 59  \w     45.00  71.00   0.50    0.30    --   66.00  75.00-155.69   52
 60  \w     45.00  70.00   0.50    0.30    --   66.00  73.00-126.56   50
 61  \w     49.00  75.00   0.50    0.30    --   70.00  74.00-175.31   52
 62  \w     94.00 120.00   0.50    0.30    --   70.00  74.00-175.31   52
 63  \w    101.00 165.00   0.50    0.30    --  113.25  61.00  60.00  128
 64  \w    139.00 175.00   0.50    0.30    --  113.25  61.00 150.00   72
 65  \w     99.00 134.00   0.50    0.30    --  113.25  61.00 150.00   70
 66  \w     45.00  90.00   0.50    0.30    --   66.00  73.00 117.78   90
 67  \w    101.00 176.00   0.50    0.30    --  113.25  61.00  90.00  150
 68  \w     97.00 122.00   0.50    0.30    --  113.25  61.00 -60.00   50
 69  \w    103.00 159.00   0.50    0.30    --  113.25  61.00 -30.00  112
 70  \w    153.00 178.00   0.50    0.30    --  113.25  61.00 -60.00   50
 71  \w     98.00 176.00   0.50    0.30    --  113.25  61.00 -90.00  156
 72  \w     99.00 140.00   0.50    0.30    --  113.25  61.00-150.00   82
 73  \w    102.00 138.00   0.50    0.30    --  113.25  61.00-120.00   72
 74  \w     99.00 129.00   0.50    0.30    --  113.25  61.00-180.00   60
 75  \w    135.00 175.00   0.50    0.30    --  113.25  61.00-180.00   80
 76  \w    104.00 167.00   0.50    0.30    --  113.25  45.00-150.00  126
 77  \w     97.00 174.00   0.50    0.30    --  113.25  61.00   0.00  154
 78  \w    102.00 175.00   0.50    0.30    --  113.25  61.00  30.00  146
 79  \w    101.00 172.00   0.50    0.30    --  113.25  61.00 120.00  142
 80  \w     17.00  42.00   0.50    0.30    --   46.00  90.00 148.62   50
 81  \w     14.00  39.00   0.50    0.30    --   42.00  89.00 179.04   50
 82  \w      2.00  27.00   0.50    0.30    --   26.00  81.00 170.72   50
 83  \w     -3.00  22.00   0.50    0.30    --   30.00  98.00  62.53   50
 84  \w     15.00  41.00   0.50    0.30    --   42.00  87.00 -89.74   52
 85  \w    -10.00  18.00   0.50    0.30    --   22.00  99.00-125.02   56
 86  \w    -55.00 -30.00   0.50    0.30    --   10.00 154.00 -46.37   50
 87  \w    -75.00  25.00   0.50    0.30    --  -48.02  86.00-148.00  200
 88  \w    -93.00 -68.00   0.50    0.30    --  -91.75  86.00-148.00   50
 89  \w    -51.00 -22.00   0.50    0.30    --  -91.75  45.00-150.00   58
 90  \w    -51.00 -21.00   0.50    0.30    --  -91.75  45.00  30.00   60
 91  \w    -43.00  22.00   0.50    0.30    --  -48.02  38.00 150.00  130
 92  \w    -92.00 -37.00   0.50    0.30    --  -48.02 -19.00  30.00  110
 93  \w    -73.00 -38.00   0.50    0.30    --  -48.02 -38.00 150.00   70
 94  \w    -61.00 -35.00   0.50    0.30    --  -48.02 -38.00   0.00   52
 95  \w    -99.00 -69.00   0.50    0.30    --  -48.02 -38.00   0.00   60
 96  \w   -118.00 -48.00   0.50    0.30    --  -48.02 -19.00-150.00  140
 97  \w    -95.00 -69.00   0.50    0.30    --  -91.75 -77.00 -90.00   52
 98  \w    -94.00 -69.00   0.50    0.30    --  -91.75 -77.00-150.00   50
 99  \w    -94.00 -69.00   0.50    0.30    --  -91.75 -77.00-141.74   50
100  \w   -162.00-111.00   0.50    0.30    --  -91.75 -77.00-141.74  102
101  \w   -132.00-107.00   0.50    0.30    --  -62.00 -76.00  59.47   50
102  \w   -160.00-135.00   0.50    0.30    --  -91.75 -77.00 120.00   50
103  \w    -96.00 -69.00   0.50    0.30    --  -91.75 -77.00 150.00   54
104  \w    -94.00 -69.00   0.50    0.30    --  -91.75 -77.00 120.00   50
105  \w    -70.00 -39.00   0.50    0.30    --  -62.00 -76.00  59.47   62
106  \w    -73.00 -47.00   0.50    0.30    --  -70.00 -76.00  30.60   52
107  \w    -75.00 -47.00   0.50    0.30    --  -70.00 -76.00 -29.29   56
108  \w    -94.00 -69.00   0.50    0.30    --  -91.75 -76.00  31.85   50
109  \w    -64.00 -39.00   0.50    0.30    --  -62.00 -76.00 -24.79   50
110  \w    -77.00 -51.00   0.50    0.30    --  -74.00 -76.00-139.81   52
111  \w    -82.00 -56.00   0.50    0.30    --  -78.00 -75.00 -68.47   52
112  \w    -95.00 -69.00   0.50    0.30    --  -91.75 -76.00 -50.04   52
113  \w   -139.00-114.00   0.50    0.30    --  -66.00 -74.00  -4.38   50
114  \w    -69.00 -44.00   0.50    0.30    --  -66.00 -74.00 -82.75   50
115  \w    -86.00 -60.00   0.50    0.30    --  -82.00 -75.00  49.81   52
116  \w    -90.00 -64.00   0.50    0.30    --  -86.00 -74.00   3.95   52
117  \w    -70.00 -45.00   0.50    0.30    --  -66.00 -74.00  -4.38   50
118  \w    -96.00 -70.00   0.50    0.30    --  -91.75 -74.00-112.35   52
119  \w    -82.00 -57.00   0.50    0.30    --  -78.00 -73.00-101.82   50
120  \w    -90.00 -62.00   0.50    0.30    --  -82.00 -73.00 -42.48   56
121  \w    -97.00 -71.00   0.50    0.30    --  -91.75 -73.00  49.25   52
122  \w   -155.00-129.00   0.50    0.30    --  -91.75 -75.00 172.32   52
123  \w   -103.00 -71.00   0.50    0.30    --  -91.75 -75.00 172.32   64
124  \w    -97.00 -65.00   0.50    0.30    --  -86.00 -74.00 175.99   64
125  \w    -97.00 -71.00   0.50    0.30    --  -91.75 -71.00  99.06   52
126  \w   -158.00-133.00   0.50    0.30    --  -91.75 -71.00  99.06   50
127  \w   -157.00-128.00   0.50    0.30    --  -86.00 -71.00 -14.52   58
128  \w    -92.00 -66.00   0.50    0.30    --  -86.00 -71.00 -14.52   52
129  \w    -91.00 -65.00   0.50    0.30    --  -86.00 -72.00 -48.94   52
130  \w    -93.00 -65.00   0.50    0.30    --  -86.00 -73.00-175.36   56
131  \w    -96.00 -71.00   0.50    0.30    --  -91.75 -72.00 -74.59   50
132  \w    -84.00 -58.00   0.50    0.30    --  -78.00 -70.00 -45.45   52
133  \w    -97.00 -72.00   0.50    0.30    --  -91.75 -69.00 -29.48   50
134  \w    -80.00 -55.00   0.50    0.30    --  -74.00 -68.00  70.13   50
135  \w    -90.00 -58.00   0.50    0.30    --  -78.00 -69.00 123.51   64
136  \w   -111.00 -74.00   0.50    0.30    --  -91.75 -69.00 124.03   74
137  \w   -162.00-127.00   0.50    0.30    --  -91.75 -69.00 124.03   70
138  \w   -154.00-128.00   0.50    0.30    --  -82.00 -66.00  59.57   52
139  \w   -109.00 -76.00   0.50    0.30    --  -91.75 -60.00  -5.04   66
140  \w    -81.00 -56.00   0.50    0.30    --  -74.00 -65.00  47.76   50
141  \w    -90.00 -64.00   0.50    0.30    --  -82.00 -66.00  59.57   52
142  \w   -104.00 -79.00   0.50    0.30    --  -91.75 -86.00  93.00   50
143  \w   -155.00-129.00   0.50    0.30    --  -91.75 -86.00  93.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1433
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44452
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.961
_diffrn_reflns_theta_min         3.835
_exptl_absorpt_coefficient_mu    24.355
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_description       needle
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.937
_refine_diff_density_rms         0.262
_refine_ls_extinction_coef       0.00050(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   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0917P)^2^+2.1992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5245
_reflns_number_total             5928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_database_code               7249827
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.049
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Others
 Fixed Sof: O22(0.5)
3.a Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N8(H8A,H8B,H8C), N1(H1A,H1B,H1C), N4(H4A,H4B,H4C), N2(H2A,
 H2B,H2C), N7(H7A,H7B,H7C), N5(H5A,H5B,H5C), N6(H6A,H6B,H6C)
;
_shelx_res_checksum              40004
_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
;