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_7249829
_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         'C4 H4 Mo4 O16, 2(C2 H12 Co N4 O4), 3(H2O)'
_chemical_formula_sum            'C8 H34 Co2 Mo4 N8 O27'
_chemical_formula_weight         1176.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-21
_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                90
_cell_angle_beta                 92.8440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.0622(3)
_cell_length_b                   7.36240(10)
_cell_length_c                   33.9652(4)
_cell_measurement_reflns_used    33621
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      77.1250
_cell_measurement_theta_min      2.6020
_cell_volume                     6758.98(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_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    -64.00 -14.00   0.50    0.40    --  -86.25  57.00-120.00  100
  2  \w    -83.00 -16.00   0.50    0.10    --  -47.29 125.00 -60.00  134
  3  \w    -41.00 -16.00   0.50    0.40    --  -86.25  61.00  75.00   50
  4  \w    -62.00  21.00   0.50    0.10    --  -47.29  61.00  75.00  166
  5  \w     82.00 113.00   0.50    0.10    --   47.29  64.00  14.56   62
  6  \w     86.00 120.00   0.50    0.10    --   47.29  61.00  75.00   68
  7  \w     31.00  82.00   0.50    0.10    --   47.29  61.00  75.00  102
  8  \w     33.00  72.00   0.50    0.10    --   47.29  57.00 150.00   78
  9  \w     31.00  77.00   0.50    0.10    --   47.29  64.00  14.56   92
 10  \w     32.00  58.00   0.50    0.10    --   47.29  57.00 120.00   52
 11  \w     33.00  63.00   0.50    0.10    --   47.29  57.00 -30.00   60
 12  \w     33.00  58.00   0.50    0.10    --   47.29  57.00   0.00   50
 13  \w     34.00  70.00   0.50    0.10    --   47.29  57.00 -60.00   72
 14  \w     33.00  65.00   0.50    0.10    --   47.29  57.00 -90.00   64
 15  \w     32.00  82.00   0.50    0.10    --   47.29  57.00-120.00  100
 16  \w     32.00  94.00   0.50    0.10    --   47.29  62.00-179.02  124
 17  \w     41.00  69.00   0.50    0.10    --   47.29  38.00 -60.00   56
 18  \w     86.00 119.00   0.50    0.10    --   47.29  57.00 -60.00   66
 19  \w     37.00  80.00   0.50    0.10    --   47.29  57.00  60.00   86
 20  \w     88.00 178.00   0.50    0.40    --  106.90  77.00  30.00  180
 21  \w    143.00 169.00   0.50    0.40    --  106.90  77.00 150.00   52
 22  \w     90.00 135.00   0.50    0.40    --  106.90  77.00 150.00   90
 23  \w     92.00 152.00   0.50    0.40    --  106.90  61.00  75.00  120
 24  \w     87.00 178.00   0.50    0.40    --  106.90  72.00 -73.76  182
 25  \w     96.00 177.00   0.50    0.40    --  106.90  57.00-180.00  162
 26  \w    118.00 178.00   0.50    0.40    --  106.90  77.00-150.00  120
 27  \w     92.00 155.00   0.50    0.40    --  106.90  57.00 -90.00  126
 28  \w     92.00 172.00   0.50    0.40    --  106.90  57.00 -30.00  160
 29  \w     99.00 175.00   0.50    0.40    --  106.90  57.00   0.00  152
 30  \w     96.00 167.00   0.50    0.40    --  106.90  57.00 120.00  142
 31  \w     98.00 172.00   0.50    0.40    --  106.90  57.00  90.00  148
 32  \w    137.00 165.00   0.50    0.40    --  106.90  57.00-150.00   56
 33  \w     98.00 129.00   0.50    0.40    --  106.90  57.00-150.00   62
 34  \w     35.00  65.00   0.50    0.40    --  106.90 -57.00 -90.00   60
 35  \w     36.00  71.00   0.50    0.40    --  106.90 -61.00 -62.00   70
 36  \w     34.00 103.00   0.50    0.40    --  106.90 -77.00  30.00  138
 37  \w    -19.00  21.00   0.50    0.10    --   47.29 -61.00 -62.00   80
 38  \w     35.00  78.00   0.50    0.10    --   47.29-125.00 -30.00   86
 39  \w     44.00 112.00   0.50    0.40    --  106.90-125.00-180.00  136
 40  \w     55.00 112.00   0.50    0.40    --  106.90-125.00-150.00  114
 41  \w     82.00 112.00   0.50    0.40    --  106.90-125.00 -90.00   60
 42  \w     78.00 111.00   0.50    0.40    --  106.90-125.00 -30.00   66
 43  \w     64.00 112.00   0.50    0.40    --  106.90-125.00   0.00   96
 44  \w     36.00 112.00   0.50    0.40    --  106.90-125.00  30.00  152
 45  \w     37.00 105.00   0.50    0.40    --  106.90 -99.00  30.00  136
 46  \w     35.00  73.00   0.50    0.40    --  106.90-125.00 -30.00   76
 47  \w     51.00 104.00   0.50    0.40    --  106.90-125.00 -60.00  106
 48  \w     41.00  84.00   0.50    0.40    --  106.90 -99.00-150.00   86
 49  \w     34.00  79.00   0.50    0.40    --  106.90-125.00 -90.00   90
 50  \w     35.00  88.00   0.50    0.40    --  106.90 -99.00 120.00  106
 51  \w    -86.00 -35.00   0.50    0.10    --  -47.29 -19.00 -60.00  102
 52  \w   -119.00 -94.00   0.50    0.10    --  -47.29 -77.00  60.00   50
 53  \w   -101.00 -66.00   0.50    0.10    --  -47.29 -61.00 -62.00   70
 54  \w    -91.00 -39.00   0.50    0.10    --  -47.29 -19.00-180.00  104
 55  \w    -97.00 -71.00   0.50    0.40    --  -86.25 -57.00-128.38   52
 56  \w    -94.00 -68.00   0.50    0.40    --  -86.25 -66.00   8.54   52
 57  \w   -133.00-107.00   0.50    0.40    --  -86.25 -65.00  76.09   52
 58  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -66.00 143.36   50
 59  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -66.00 166.20   50
 60  \w    -94.00 -68.00   0.50    0.40    --  -86.25 -66.00 157.82   52
 61  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -65.00  94.60   50
 62  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -65.00  76.09   50
 63  \w   -113.00 -68.00   0.50    0.40    --  -86.25 -65.00  49.11   90
 64  \w   -156.00-130.00   0.50    0.40    --  -86.25 -65.00  17.94   52
 65  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -65.00  33.54   50
 66  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -65.00  -7.82   50
 67  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -65.00  17.94   50
 68  \w    -95.00 -69.00   0.50    0.40    --  -86.25 -64.00 -22.31   52
 69  \w    -95.00 -69.00   0.50    0.40    --  -86.25 -65.00-131.43   52
 70  \w   -116.00 -68.00   0.50    0.40    --  -86.25 -65.00 -93.31   96
 71  \w   -156.00-131.00   0.50    0.40    --  -86.25 -65.00  33.54   50
 72  \w   -152.00-122.00   0.50    0.40    --  -86.25 -64.00  62.34   60
 73  \w    -93.00 -68.00   0.50    0.40    --  -86.25 -65.00 131.37   50
 74  \w    -95.00 -69.00   0.50    0.40    --  -86.25 -64.00  62.34   52
 75  \w    -95.00 -69.00   0.50    0.40    --  -86.25 -64.00 -48.62   52
 76  \w    -94.00 -69.00   0.50    0.40    --  -86.25 -63.00 -79.69   50
 77  \w   -158.00-118.00   0.50    0.40    --  -86.25 -63.00-145.72   80
 78  \w    -96.00 -70.00   0.50    0.40    --  -86.25 -63.00-145.72   52
 79  \w   -153.00-127.00   0.50    0.40    --  -86.25 -63.00 -79.69   52
 80  \w   -147.00-122.00   0.50    0.40    --  -86.25 -61.00 -62.00   50
 81  \w   -159.00-113.00   0.50    0.40    --  -86.25 -64.00 -22.31   92
 82  \w   -155.00-130.00   0.50    0.40    --  -86.25 -63.00 103.26   50
 83  \w   -117.00 -69.00   0.50    0.40    --  -86.25 -63.00 173.36   96
 84  \w    -95.00 -70.00   0.50    0.40    --  -86.25 -61.00 109.33   50
 85  \w    -94.00 -69.00   0.50    0.40    --  -86.25 -63.00 103.26   50
 86  \w   -159.00-134.00   0.50    0.40    --  -86.25 -61.00 109.33   50
 87  \w   -156.00-131.00   0.50    0.40    --  -86.25 -60.00 -37.67   50
 88  \w   -120.00 -72.00   0.50    0.40    --  -86.25 -60.00 -20.24   96
 89  \w   -100.00 -70.00   0.50    0.40    --  -86.25 -60.00 -37.67   60
 90  \w    -95.00 -70.00   0.50    0.40    --  -86.25 -61.00 -62.00   50
 91  \w   -101.00 -70.00   0.50    0.40    --  -86.25 -60.00-115.82   62
 92  \w    -95.00 -70.00   0.50    0.40    --  -86.25 -60.00-173.69   50
 93  \w    -95.00 -70.00   0.50    0.40    --  -86.25 -59.00-161.55   50
 94  \w   -132.00-106.00   0.50    0.40    --  -86.25 -60.00-173.69   52
 95  \w    -96.00 -70.00   0.50    0.40    --  -86.25 -59.00 -75.35   52
 96  \w   -118.00 -70.00   0.50    0.40    --  -86.25 -59.00  49.29   96
;
_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  0.1088
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            88875
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.368
_diffrn_reflns_theta_min         3.270
_exptl_absorpt_coefficient_mu    20.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
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    2.300
_exptl_crystal_description       needle
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.710
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0683P)^2^+67.6760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5787
_reflns_number_total             7055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_database_code               7249829
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.178
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) = Uanis(O2W)
Uanis(O4W) = Uanis(O2W) = Uanis(O3W) = Uanis(O1W)
3. Others
 Fixed Sof: O2W(0.5) O3W(0.5) O4W(0.5) O1W(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B)
4.b Idealised Me refined as rotating group:
 N8(H8A,H8B,H8C), N7(H7A,H7B,H7C), N5(H5A,H5B,H5C), N6(H6A,H6B,H6C), N1(H1A,
 H1B,H1C), N4(H4C,H4D,H4E), N3(H3A,H3B,H3C), N2(H2C,H2D,H2E)
;
_shelx_res_checksum              75970
_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
;