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_7249828
_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), C4 H6 O4, 4(H2 O)'
_chemical_formula_sum            'C12 H62 Co4 Mo8 N16 O50'
_chemical_formula_weight         2234.01
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-11-22 deposited with the CCDC.	2025-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                84.2600(10)
_cell_angle_beta                 73.105(2)
_cell_angle_gamma                71.519(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4824(2)
_cell_length_b                   13.3673(2)
_cell_length_c                   14.0305(2)
_cell_measurement_reflns_used    26504
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      76.6750
_cell_measurement_theta_min      3.2930
_cell_volume                     1443.65(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (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_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_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     24.00  61.00   0.50    0.20    --   47.03  77.00  60.00   74
  2  \w     25.00  53.00   0.50    0.20    --   47.03  77.00 120.00   56
  3  \w     84.00 120.00   0.50    0.20    --   47.03  77.00  60.00   72
  4  \w     24.00  84.00   0.50    0.20    --   47.03  77.00   0.00  120
  5  \w     32.00  74.00   0.50    0.20    --   47.03  57.00 -30.00   84
  6  \w     24.00  50.00   0.50    0.20    --   47.03  77.00 -60.00   52
  7  \w     36.00  65.00   0.50    0.20    --   47.03  50.00 -62.00   58
  8  \w     24.00  60.00   0.50    0.20    --   47.03  77.00-120.00   72
  9  \w     24.00  55.00   0.50    0.20    --   47.03  77.00-180.00   62
 10  \w     84.00 110.00   0.50    0.20    --   47.03  77.00-180.00   52
 11  \w     95.00 120.00   0.50    0.20    --   47.03  50.00 -62.00   50
 12  \w     84.00 138.00   0.50    0.50    --  106.40  77.00 -60.00  108
 13  \w     84.00 139.00   0.50    0.50    --  106.40  77.00-180.00  110
 14  \w    143.00 176.00   0.50    0.50    --  106.40  77.00-180.00   66
 15  \w     93.00 131.00   0.50    0.50    --  106.40  57.00-150.00   76
 16  \w     87.00 177.00   0.50    0.50    --  106.40  77.00 -30.00  180
 17  \w     98.00 178.00   0.50    0.50    --  106.40  57.00  30.00  160
 18  \w     98.00 172.00   0.50    0.50    --  106.40  57.00  90.00  148
 19  \w    138.00 167.00   0.50    0.50    --  106.40  57.00  60.00   58
 20  \w     95.00 134.00   0.50    0.50    --  106.40  57.00  60.00   78
 21  \w     96.00 128.00   0.50    0.50    --  106.40  57.00 150.00   64
 22  \w     93.00 177.00   0.50    0.50    --  106.40  38.00 150.00  168
 23  \w     91.00 168.00   0.50    0.50    --  106.40  77.00   0.00  154
 24  \w    101.00 177.00   0.50    0.50    --  106.40  50.00 -62.00  152
 25  \w     96.00 141.00   0.50    0.50    --  106.40  19.00 -60.00   90
 26  \w    139.00 178.00   0.50    0.50    --  106.40  19.00-120.00   78
 27  \w    141.00 170.00   0.50    0.50    --  106.40  57.00-150.00   58
 28  \w    151.00 177.00   0.50    0.50    --  106.40 125.00-120.00   52
 29  \w     97.00 142.00   0.50    0.50    --  106.40 125.00-120.00   90
 30  \w     24.00  57.00   0.50    0.20    --   47.03 -50.00 150.00   66
 31  \w    -24.00  19.00   0.50    0.20    --   47.03 -50.00 150.00   86
 32  \w     34.00  66.00   0.50    0.50    --  106.40 -57.00  60.00   64
 33  \w     34.00  59.00   0.50    0.50    --  106.40 -57.00 -30.00   50
 34  \w     39.00  65.00   0.50    0.50    --  106.40 -57.00 -60.00   52
 35  \w     34.00  66.00   0.50    0.50    --  106.40 -57.00-120.00   64
 36  \w     34.00 103.00   0.50    0.50    --  106.40 -99.00-120.00  138
 37  \w     44.00 108.00   0.50    0.50    --  106.40-125.00-180.00  128
 38  \w     34.00  94.00   0.50    0.20    --   47.03-125.00-180.00  120
 39  \w     34.00  65.00   0.50    0.50    --  106.40 -99.00-180.00   62
 40  \w     45.00 110.00   0.50    0.50    --  106.40-125.00 -30.00  130
 41  \w     79.00 105.00   0.50    0.50    --  106.40 -99.00 -30.00   52
 42  \w     37.00  62.00   0.50    0.50    --  106.40-125.00   0.00   50
 43  \w     35.00  62.00   0.50    0.50    --  106.40 -99.00 -30.00   54
 44  \w     78.00 105.00   0.50    0.50    --  106.40-125.00   0.00   54
 45  \w     41.00  88.00   0.50    0.50    --  106.40 -99.00  60.00   94
 46  \w     37.00 111.00   0.50    0.50    --  106.40-125.00  60.00  148
 47  \w     80.00 105.00   0.50    0.50    --  106.40 -99.00  90.00   50
 48  \w     38.00  72.00   0.50    0.50    --  106.40 -99.00  90.00   68
 49  \w     35.00  87.00   0.50    0.50    --  106.40 -99.00-150.00  104
 50  \w     69.00 106.00   0.50    0.50    --  106.40 -99.00-180.00   74
 51  \w    -60.00 -17.00   0.50    0.50    --  -86.25  57.00 150.00   86
 52  \w    -51.00  16.00   0.50    0.20    --  -47.03  50.00 -62.00  134
 53  \w    -57.00 -16.00   0.50    0.50    --  -86.25  50.00 -62.00   82
 54  \w   -117.00 -71.00   0.50    0.20    --  -47.03 -38.00 -60.00   92
 55  \w    -76.00 -33.00   0.50    0.20    --  -47.03 -52.00 103.40   86
 56  \w    -77.00 -45.00   0.50    0.20    --  -47.03 -50.00 150.00   64
 57  \w   -114.00 -86.00   0.50    0.20    --  -47.03 -38.00 120.00   56
 58  \w   -117.00 -85.00   0.50    0.20    --  -47.03 -52.00 103.40   64
 59  \w    -59.00 -34.00   0.50    0.20    --  -47.03 -38.00 120.00   50
 60  \w    -67.00 -37.00   0.50    0.20    --  -47.03 -38.00 -60.00   60
 61  \w    -74.00 -34.00   0.50    0.20    --  -47.03 -38.00-150.00   80
 62  \w    -65.00 -35.00   0.50    0.20    --  -47.03 -19.00-180.00   60
 63  \w   -105.00 -74.00   0.50    0.20    --  -47.03 -19.00-180.00   62
 64  \w    -90.00 -63.00   0.50    0.50    --  -86.25 -77.00  60.00   54
 65  \w    -88.00 -63.00   0.50    0.50    --  -86.25 -77.00  90.00   50
 66  \w    -88.00 -63.00   0.50    0.50    --  -86.25 -77.00  81.30   50
 67  \w    -88.00 -63.00   0.50    0.50    --  -86.25 -77.00 150.00   50
 68  \w   -151.00-125.00   0.50    0.50    --  -86.25 -77.00  90.00   52
 69  \w   -153.00-128.00   0.50    0.50    --  -86.25 -77.00 150.00   50
 70  \w   -156.00-126.00   0.50    0.50    --  -86.25 -77.00  60.00   60
 71  \w    -90.00 -64.00   0.50    0.50    --  -86.25 -77.00   0.00   52
 72  \w    -88.00 -63.00   0.50    0.50    --  -86.25 -77.00 -30.00   50
 73  \w    -88.00 -63.00   0.50    0.50    --  -86.25 -77.00 -60.00   50
 74  \w    -93.00 -68.00   0.50    0.50    --  -86.25 -77.00-120.00   50
 75  \w    -88.00 -63.00   0.50    0.50    --  -86.25 -77.00-180.00   50
 76  \w    -95.00 -65.00   0.50    0.50    --  -86.25 -77.00-150.00   60
 77  \w   -154.00-129.00   0.50    0.50    --  -86.25 -77.00-150.00   50
 78  \w   -159.00-120.00   0.50    0.50    --  -86.25 -77.00-120.00   78
 79  \w   -148.00 -66.00   0.50    0.50    --  -86.25 -74.00-113.16  164
 80  \w    -91.00 -64.00   0.50    0.50    --  -86.25 -75.00 -97.19   54
 81  \w    -91.00 -66.00   0.50    0.50    --  -86.25 -75.00 -42.06   50
 82  \w   -147.00-121.00   0.50    0.50    --  -86.25 -75.00 -42.06   52
 83  \w   -144.00-118.00   0.50    0.50    --  -86.25 -74.00  37.41   52
 84  \w    -92.00 -65.00   0.50    0.50    --  -86.25 -76.00 109.74   54
 85  \w    -96.00 -65.00   0.50    0.50    --  -86.25 -72.00 117.66   62
 86  \w    -91.00 -65.00   0.50    0.50    --  -86.25 -74.00  37.41   52
 87  \w    -93.00 -67.00   0.50    0.50    --  -86.25 -69.00 -22.41   52
 88  \w   -150.00-124.00   0.50    0.50    --  -86.25 -68.00  10.58   52
 89  \w   -109.00 -73.00   0.50    0.50    --  -86.25 -57.00 137.36   72
 90  \w    -93.00 -67.00   0.50    0.50    --  -86.25 -68.00  10.58   52
 91  \w    -99.00 -73.00   0.50    0.50    --  -86.25 -50.00 150.00   52
 92  \w    -91.00 -65.00   0.50    0.50    --  -86.25 -72.00 -79.12   52
 93  \w    -91.00 -66.00   0.50    0.50    --  -86.25 -71.00-137.41   50
 94  \w   -148.00-123.00   0.50    0.50    --  -86.25 -71.00-137.41   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      0.0487304000
_diffrn_orient_matrix_UB_12      0.0787286000
_diffrn_orient_matrix_UB_13      0.0504140000
_diffrn_orient_matrix_UB_21      -0.1929995000
_diffrn_orient_matrix_UB_22      0.0556290000
_diffrn_orient_matrix_UB_23      0.0479040000
_diffrn_orient_matrix_UB_31      0.0056680000
_diffrn_orient_matrix_UB_32      -0.0739886000
_diffrn_orient_matrix_UB_33      0.0912838000
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34979
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.053
_diffrn_reflns_theta_min         3.292
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.654
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
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            'dark pink'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.570
_exptl_crystal_description       plank
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.645
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00092(6)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0571P)^2^+2.6459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5734
_reflns_number_total             5921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_database_code               7249828
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo8 C12 Co4 O46 N16'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.378
_shelx_estimated_absorpt_t_min   0.076
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O8-H1WA
 2.031 with sigma of 0.1
3.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6D,H6E)
3.c Idealised Me refined as rotating group:
 N5(H5A,H5B,H5C), N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N4(H4A,H4B,H4C), N6(H6A,
 H6B,H6C), N3(H3A,H3B,H3C), N7(H7A,H7B,H7C), N8(H8A,H8B,H8C)
3.d Idealised tetrahedral OH refined as rotating group:
 O22(H22)
;
_shelx_res_checksum              1775
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.647