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_7249826
_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         'H12 Mo8 Na2 O33, 4(C2 H12 Co N4 O4), 6(H2 O)'
_chemical_formula_sum            'C8 H72 Co4 Mo8 N16 Na2 O55'
_chemical_formula_weight         2322.03
_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
_audit_creation_date             2025-01-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                106.856(2)
_cell_angle_beta                 93.852(2)
_cell_angle_gamma                96.451(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4465(3)
_cell_length_b                   10.7769(3)
_cell_length_c                   15.2702(4)
_cell_measurement_reflns_used    11692
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.9940
_cell_measurement_theta_min      4.4880
_cell_volume                     1470.20(8)
_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    'olex2.solve 1.5 (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 0.949
_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    -65.00 -11.00   0.50    1.00    --  -46.91  92.00 171.00  108
  2  \w     -8.00  20.00   0.50    1.00    --  -46.91  92.00 171.00   56
  3  \w     12.00  39.00   0.50    1.00    --   46.91 -92.00  59.00   54
  4  \w    -71.00 -46.00   0.50    4.00    --  -86.25  92.00 171.00   50
  5  \w   -134.00 -81.00   0.50    4.00    --  -86.25 -92.00  59.00  106
  6  \w     78.00 105.00   0.50    4.00    --  106.40 -92.00  59.00   54
  7  \w    -12.00  29.00   0.50    1.00    --  -46.91  19.00-150.00   82
  8  \w    -27.00  28.00   0.50    1.00    --  -46.91  19.00  90.00  110
  9  \w   -118.00 -73.00   0.50    1.00    --  -46.91-125.00-150.00   90
 10  \w   -113.00 -74.00   0.50    1.00    --  -46.91-125.00-180.00   78
 11  \w   -103.00 -74.00   0.50    1.00    --  -46.91-125.00 -90.00   58
 12  \w    -18.00   9.00   0.50    1.00    --   46.91 -57.00  30.00   54
 13  \w     14.00  61.00   0.50    1.00    --   46.91 -57.00  30.00   94
 14  \w    -43.00 -14.00   0.50    4.00    --  -86.25  38.00 -30.00   58
 15  \w    -43.00 -14.00   0.50    4.00    --  -86.25  38.00-180.00   58
 16  \w    -86.00 -13.00   0.50    4.00    --  -86.25 125.00-180.00  146
 17  \w    -42.00 -14.00   0.50    4.00    --  -86.25  38.00 -60.00   56
 18  \w    -43.00 -13.00   0.50    4.00    --  -86.25  38.00-150.00   60
 19  \w    -41.00 -13.00   0.50    4.00    --  -86.25  38.00   0.00   56
 20  \w     34.00  60.00   0.50    4.00    --  106.40-125.00  60.00   52
 21  \w     39.00  64.00   0.50    4.00    --  106.40 -57.00 150.00   50
 22  \w     49.00 101.00   0.50    4.00    --  106.40 -99.00 -30.00  104
 23  \w     53.00 111.00   0.50    4.00    --  106.40-125.00 -60.00  116
 24  \w     35.00  94.00   0.50    4.00    --  106.40 -99.00-180.00  118
 25  \w     94.00 176.00   0.50    4.00    --  106.40  19.00  90.00  164
 26  \w     35.00  66.00   0.50    4.00    --  106.40 -57.00  90.00   62
 27  \w     34.00  66.00   0.50    4.00    --  106.40 -57.00 -30.00   64
 28  \w     36.00  63.00   0.50    4.00    --  106.40 -57.00 -90.00   54
 29  \w     45.00 110.00   0.50    4.00    --  106.40-125.00-180.00  130
 30  \w     43.00  88.00   0.50    4.00    --  106.40 -77.00-150.00   90
 31  \w    127.00 155.00   0.50    4.00    --  106.40  57.00-150.00   56
 32  \w     39.00  82.00   0.50    4.00    --  106.40 -99.00  30.00   86
 33  \w    129.00 171.00   0.50    4.00    --  106.40  38.00 120.00   84
 34  \w     40.00 111.00   0.50    4.00    --  106.40-125.00 -30.00  142
 35  \w     34.00  66.00   0.50    4.00    --  106.40 -57.00  60.00   64
 36  \w     51.00  77.00   0.50    4.00    --  106.40-125.00  90.00   52
 37  \w    120.00 176.00   0.50    4.00    --  106.40  19.00 -30.00  112
 38  \w     43.00  90.00   0.50    4.00    --  106.40 -99.00-150.00   94
 39  \w     36.00  63.00   0.50    4.00    --  106.40 -77.00   0.00   54
 40  \w     94.00 160.00   0.50    4.00    --  106.40  19.00 -90.00  132
 41  \w     44.00  96.00   0.50    4.00    --  106.40 -77.00  60.00  104
 42  \w     83.00 111.00   0.50    4.00    --  106.40-125.00  60.00   56
 43  \w     80.00 111.00   0.50    4.00    --  106.40-125.00  90.00   62
 44  \w     97.00 131.00   0.50    4.00    --  106.40 125.00 -30.00   68
 45  \w    114.00 149.00   0.50    4.00    --  106.40  92.00 171.00   70
;
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17999
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.603
_diffrn_reflns_theta_min         3.041
_exptl_absorpt_coefficient_mu    23.462
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.247
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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    2.623
_exptl_crystal_description       plate
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.005
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00021(5)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5927
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0637P)^2^+0.6935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5445
_reflns_number_total             5927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_original_cell_volume        1470.20(7)
_cod_database_code               7249826
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.549
_shelx_estimated_absorpt_t_min   0.259
_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. Restrained distances
 O7_$1-H1A_$1
 2.226 with sigma of 0.001
3.a Free rotating group:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB)
3.b Rotating group:
 O2W(H2WA,H2WB)
3.c Secondary CH2 refined with riding coordinates:
 O1W(H1WA,H1WB)
3.d Idealised Me refined as rotating group:
 N5(H5A,H5B,H5C), N2(H2A,H2B,H2C), N8(H8A,H8B,H8C), N7(H7A,H7B,H7C), N6(H6A,
 H6B,H6C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              86004
_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
;