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_7249833
_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
'Mo2 Na2.5 O38 V7, C6 H24 Co N6, 4(O), Na0.5 O3'
_chemical_formula_sum            'C6 H24 Co Mo2 N6 Na3 O45 V7'
_chemical_formula_weight         1576.67
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-24
_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                92.9430(10)
_cell_angle_beta                 97.9090(10)
_cell_angle_gamma                91.0120(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1225(2)
_cell_length_b                   13.4878(2)
_cell_length_c                   14.4274(2)
_cell_measurement_reflns_used    19670
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.2530
_cell_measurement_theta_min      3.1120
_cell_volume                     2332.71(6)
_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      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 0.988
_diffrn_measured_fraction_theta_max 0.965
_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   -118.00 -70.00   0.50    0.31    --  -47.74-131.00  67.00   96
  2  \w    -87.00 -62.00   0.50    0.31    --  -47.74 140.00 -47.00   50
  3  \w    -72.00 -46.00   0.50    0.31    --  -47.74 131.00 138.00   52
  4  \w   -104.00 -63.00   0.50    0.31    --  -47.74-140.00-106.00   82
  5  \w     38.00  98.00   0.50    0.31    --   47.74-131.00  67.00  120
  6  \w     52.00  96.00   0.50    0.31    --   47.74-140.00-106.00   88
  7  \w    -83.00 -58.00   0.50    1.26    --  -91.75 140.00 -47.00   50
  8  \w   -128.00-102.00   0.50    1.26    --  -91.75-131.00  67.00   52
  9  \w   -134.00-109.00   0.50    1.26    --  -91.75-140.00-106.00   50
 10  \w    -80.00 -55.00   0.50    1.26    --  -91.75 131.00 138.00   50
 11  \w     81.00 115.00   0.50    1.26    --  113.25-131.00  67.00   68
 12  \w    105.00 130.00   0.50    1.26    --  113.25 140.00 -47.00   50
 13  \w     81.00 122.00   0.50    1.26    --  113.25-140.00-106.00   82
 14  \w    118.00 144.00   0.50    1.26    --  113.25 131.00 138.00   52
 15  \w   -117.00 -90.00   0.50    0.31    --  -47.74 -77.00  90.00   54
 16  \w   -119.00 -92.00   0.50    0.31    --  -47.74 -77.00-120.00   54
 17  \w   -119.00 -90.00   0.50    0.31    --  -47.74 -77.00-180.00   58
 18  \w   -114.00 -88.00   0.50    0.31    --  -47.74 -77.00  30.00   52
 19  \w   -117.00 -88.00   0.50    0.31    --  -47.74 -77.00 150.00   58
 20  \w    -20.00  27.00   0.50    0.31    --  -47.74  19.00 120.00   94
 21  \w    -26.00  26.00   0.50    0.31    --   47.74 -19.00 -30.00  104
 22  \w     35.00  78.00   0.50    0.31    --   47.74-125.00-180.00   86
 23  \w     90.00 119.00   0.50    0.31    --   47.74  77.00 -60.00   58
 24  \w   -162.00 -98.00   0.50    1.26    --  -91.75 -45.00 120.00  128
 25  \w    145.00 171.00   0.50    1.26    --  113.25  61.00  30.00   52
 26  \w    138.00 164.00   0.50    1.26    --  113.25  30.00  90.00   52
 27  \w     77.00 111.00   0.50    1.26    --  113.25-125.00-150.00   68
 28  \w     51.00  96.00   0.50    1.26    --  113.25 -95.00  60.00   90
 29  \w    133.00 176.00   0.50    1.26    --  113.25  30.00-120.00   86
 30  \w     98.00 143.00   0.50    1.26    --  113.25  61.00  30.00   90
 31  \w     42.00  71.00   0.50    1.26    --  113.25 -61.00-150.00   58
 32  \w     64.00 107.00   0.50    1.26    --  113.25-103.00 -77.11   86
 33  \w     99.00 155.00   0.50    1.26    --  113.25  61.00 120.00  112
 34  \w     42.00 104.00   0.50    1.26    --  113.25 -77.00  90.00  124
 35  \w     45.00  81.00   0.50    1.26    --  113.25-125.00   0.00   72
 36  \w     86.00 111.00   0.50    1.26    --  113.25-125.00   0.00   50
 37  \w    105.00 176.00   0.50    1.26    --  113.25  45.00-150.00  142
 38  \w    107.00 135.00   0.50    1.26    --  113.25  30.00  90.00   56
 39  \w     74.00 111.00   0.50    1.26    --  113.25-125.00 150.00   74
 40  \w     43.00  68.00   0.50    1.26    --  113.25 -61.00  60.00   50
 41  \w     45.00 109.00   0.50    1.26    --  113.25-125.00-180.00  128
 42  \w     85.00 111.00   0.50    1.26    --  113.25-125.00 -90.00   52
 43  \w     46.00 102.00   0.50    1.26    --  113.25 -77.00-150.00  112
 44  \w     65.00 108.00   0.50    1.26    --  113.25-125.00 120.00   86
 45  \w     42.00  70.00   0.50    1.26    --  113.25 -61.00 -60.00   56
 46  \w    122.00 153.00   0.50    1.26    --  113.25 125.00  60.00   62
 47  \w     51.00 108.00   0.50    1.26    --  113.25-125.00  30.00  114
 48  \w    101.00 175.00   0.50    1.26    --  113.25  45.00-180.00  148
 49  \w    111.00 136.00   0.50    1.26    --  113.25 125.00 120.00   50
 50  \w     45.00 100.00   0.50    1.26    --  113.25 -77.00   0.00  110
 51  \w    126.00 174.00   0.50    1.26    --  113.25  45.00 -90.00   96
 52  \w    122.00 165.00   0.50    1.26    --  113.25  45.00 -30.00   86
 53  \w    103.00 175.00   0.50    1.26    --  113.25  45.00 -60.00  144
 54  \w     50.00  80.00   0.50    1.26    --  113.25 -95.00-180.00   60
 55  \w     42.00  71.00   0.50    1.26    --  113.25 -61.00-120.00   58
 56  \w     79.00 104.00   0.50    1.26    --  113.25 -95.00 -90.00   50
 57  \w     80.00 105.00   0.50    1.26    --  113.25 -95.00 -30.00   50
 58  \w    105.00 130.00   0.50    1.26    --  113.25  61.00 150.00   50
 59  \w    133.00 178.00   0.50    1.26    --  113.25  61.00 150.00   90
 60  \w     46.00  71.00   0.50    1.26    --  113.25 -61.00  90.00   50
 61  \w    129.00 155.00   0.50    1.26    --  113.25  15.00 -90.00   52
 62  \w     52.00  87.00   0.50    1.26    --  113.25 -77.00-180.00   70
 63  \w     58.00  99.00   0.50    1.26    --  113.25 -95.00 -60.00   82
 64  \w     45.00  70.00   0.50    1.26    --  113.25 -61.00  30.00   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      -0.0033383000
_diffrn_orient_matrix_UB_12      -0.1097379000
_diffrn_orient_matrix_UB_13      0.0245365000
_diffrn_orient_matrix_UB_21      -0.0146816000
_diffrn_orient_matrix_UB_22      -0.0321349000
_diffrn_orient_matrix_UB_23      -0.1050778000
_diffrn_orient_matrix_UB_31      0.1274571000
_diffrn_orient_matrix_UB_32      -0.0036961000
_diffrn_orient_matrix_UB_33      0.0036191000
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36368
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.008
_diffrn_reflns_theta_min         3.282
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34259
_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_density_diffrn    2.245
_exptl_crystal_F_000             1534
_refine_diff_density_max         5.878
_refine_diff_density_min         -1.865
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         9832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0751
_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^)+(0.1451P)^2^+16.3019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2170
_refine_ls_wR_factor_ref         0.2225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8908
_reflns_number_total             9832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_database_code               7249833
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O V Co Mo Na'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N014(H01A,H01B), N016(H01C,H01D), N017(H01E,H01F), N018(H01G,H01H), N019(H01I,
 H01J), N01A(H01K,H01L), C01E(H01M,H01N), C01G(H01O,H01P), C01H(H01Q,H01R),
 C01I(H01S,H01T), C01J(H01U,H01V), C01K(H01W,H01X)
;
_shelx_res_checksum              43727
_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 2.441
_oxdiff_exptl_absorpt_empirical_full_min 0.603