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_7249832
_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
'H4 Mo8 O28, Mo8 O26, 8(C2 H12 Co N4 O4), 12(H2O)'
_chemical_formula_sum            'C16 H124 Co8 Mo16 N32 O98'
_chemical_formula_weight         4339.94
_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             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                91.8640(10)
_cell_angle_beta                 101.574(2)
_cell_angle_gamma                99.735(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7837(3)
_cell_length_b                   12.5652(2)
_cell_length_c                   20.6823(4)
_cell_measurement_reflns_used    22769
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.6480
_cell_measurement_theta_min      3.8820
_cell_volume                     2949.84(11)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.957
_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    -61.00 -17.00   0.50    0.40    --  -86.25  57.00 -30.00   88
  2  \w    -43.00 -17.00   0.50    0.40    --  -86.25  38.00  60.00   52
  3  \w    -20.00  29.00   0.50    0.10    --  -46.80  19.00 150.00   98
  4  \w     63.00 105.00   0.50    0.10    --   46.80-149.00 -31.00   84
  5  \w     76.00 129.00   0.50    0.40    --  106.38-149.00 -31.00  106
  6  \w     86.00 111.00   0.50    0.40    --  106.38-125.00-120.00   50
  7  \w     53.00 110.00   0.50    0.40    --  106.38-125.00-180.00  114
  8  \w     36.00  67.00   0.50    0.40    --  106.38-125.00-120.00   62
  9  \w     75.00 104.00   0.50    0.40    --  106.38-125.00 -30.00   58
 10  \w     34.00  61.00   0.50    0.40    --  106.38-125.00 -30.00   54
 11  \w     37.00  78.00   0.50    0.40    --  106.38-125.00 120.00   82
 12  \w     55.00 110.00   0.50    0.40    --  106.38-124.00 132.00  110
 13  \w     45.00 102.00   0.50    0.40    --  106.38-125.00 150.00  114
 14  \w     42.00  93.00   0.50    0.10    --   46.80-124.00 132.00  102
 15  \w     36.00 105.00   0.50    0.40    --  106.38 -99.00  30.00  138
 16  \w     58.00  91.00   0.50    0.40    --  106.38 -99.00   0.00   66
 17  \w     50.00 104.00   0.50    0.40    --  106.38 -99.00 -30.00  108
 18  \w     77.00 102.00   0.50    0.40    --  106.38 -99.00 -60.00   50
 19  \w     39.00  99.00   0.50    0.40    --  106.38 -99.00-180.00  120
 20  \w     -5.00  23.00   0.50    0.10    --   46.80 -19.00-150.00   56
 21  \w     34.00  64.00   0.50    0.40    --  106.38 -57.00-150.00   60
 22  \w     41.00  66.00   0.50    0.40    --  106.38 -57.00 -90.00   50
 23  \w     37.00  66.00   0.50    0.40    --  106.38 -57.00-120.00   58
 24  \w     39.00  66.00   0.50    0.40    --  106.38 -57.00 -60.00   54
 25  \w     34.00  60.00   0.50    0.40    --  106.38 -57.00 -30.00   52
 26  \w     36.00  61.00   0.50    0.40    --  106.38 -77.00   0.00   50
 27  \w     36.00  62.00   0.50    0.40    --  106.38 -57.00   0.00   52
 28  \w     76.00 105.00   0.50    0.40    --  106.38 -77.00   0.00   58
 29  \w     34.00  65.00   0.50    0.40    --  106.38 -57.00 150.00   62
 30  \w     94.00 178.00   0.50    0.40    --  106.38  38.00  90.00  168
 31  \w    119.00 167.00   0.50    0.40    --  106.38  57.00 120.00   96
 32  \w     93.00 176.00   0.50    0.40    --  106.38  38.00 150.00  166
 33  \w    102.00 173.00   0.50    0.40    --  106.38  77.00-180.00  142
 34  \w     96.00 125.00   0.50    0.40    --  106.38 124.00-148.00   58
 35  \w     99.00 135.00   0.50    0.40    --  106.38 125.00 -30.00   72
 36  \w    151.00 177.00   0.50    0.40    --  106.38 125.00   0.00   52
 37  \w    143.00 174.00   0.50    0.40    --  106.38 125.00 -30.00   62
 38  \w     97.00 142.00   0.50    0.40    --  106.38 125.00   0.00   90
 39  \w     92.00 117.00   0.50    0.40    --  106.38 149.00  15.00   50
 40  \w    -64.00 -23.00   0.50    0.10    --  -46.80 124.00-148.00   82
 41  \w    -73.00 -48.00   0.50    0.40    --  -86.25 124.00-148.00   50
 42  \w    -88.00 -63.00   0.50    0.10    --  -46.80 149.00  15.00   50
 43  \w    -83.00 -57.00   0.50    0.40    --  -86.25 149.00  15.00   52
 44  \w   -117.00 -91.00   0.50    0.10    --  -46.80 -77.00-150.00   52
 45  \w   -118.00 -93.00   0.50    0.10    --  -46.80 -77.00-120.00   50
 46  \w   -118.00 -90.00   0.50    0.10    --  -46.80 -77.00 -60.00   56
 47  \w   -116.00 -88.00   0.50    0.10    --  -46.80 -77.00 120.00   56
 48  \w   -118.00 -89.00   0.50    0.10    --  -46.80 -77.00  90.00   58
 49  \w   -114.00 -89.00   0.50    0.10    --  -46.80 -77.00  60.00   50
 50  \w   -118.00 -92.00   0.50    0.10    --  -46.80 -77.00-180.00   52
 51  \w   -132.00 -73.00   0.50    0.40    --  -86.25 -38.00-180.00  118
 52  \w   -115.00 -58.00   0.50    0.10    --  -46.80-149.00 -31.00  114
 53  \w   -104.00 -65.00   0.50    0.40    --  -86.25-149.00 -31.00   78
 54  \w   -110.00 -83.00   0.50    0.10    --  -46.80-125.00  90.00   54
 55  \w   -141.00-116.00   0.50    0.40    --  -86.25-124.00 132.00   50
 56  \w   -159.00 -92.00   0.50    0.40    --  -86.25 -57.00 150.00  134
;
_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      0.0408418000
_diffrn_orient_matrix_UB_12      -0.0038304000
_diffrn_orient_matrix_UB_13      0.0753335000
_diffrn_orient_matrix_UB_21      0.1211089000
_diffrn_orient_matrix_UB_22      -0.0198345000
_diffrn_orient_matrix_UB_23      -0.0098225000
_diffrn_orient_matrix_UB_31      0.0454487000
_diffrn_orient_matrix_UB_32      0.1230453000
_diffrn_orient_matrix_UB_33      0.0060775000
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42828
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.457
_diffrn_reflns_theta_min         3.577
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33744
_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    2.429
_exptl_crystal_description       prism
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.328
_refine_diff_density_min         -2.010
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         11992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0974P)^2^+10.1206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10532
_reflns_number_total             11992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_database_code               7249832
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo Co N C O'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.338
_shelx_estimated_absorpt_t_min   0.206
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O45) = Uanis(O44) = Uanis(O49) = Uanis(O50) = Uanis(O51) = Uanis(O47) =
Uanis(O48) = Uanis(O52)
3. Others
 Fixed Sof: O44(0.333333) O52(0.5) O48(0.5) O47(0.333333) O45(0.333333)
4.a Rotating group:
 O27(H27A,H27B)
4.b Idealised Me refined as rotating group:
 N5(H5A,H5B,H5C), N12(H12A,H12B,H12C), N16(H16A,H16B,H16C), N14(H14A,H14B,
 H14C), N15(H15A,H15B,H15C), N11(H11A,H11B,H11C), N10(H10A,H10B,H10C), N8(H8A,
 H8B,H8C), N6(H6A,H6B,H6C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N13(H13A,H13B,
 H13C), N4(H4A,H4B,H4C), N7(H7A,H7B,H7C), N9(H9A,H9B,H9C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              20568
_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 2.323
_oxdiff_exptl_absorpt_empirical_full_min 0.632