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_7249830
_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, 4(C2 H12 Co N4 O4), 6(H2 O)'
_chemical_formula_sum            'C8 H64 Co4 Mo8 N16 O50'
_chemical_formula_weight         2187.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-19
_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                 95.0550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.99760(10)
_cell_length_b                   20.6814(3)
_cell_length_c                   13.4605(2)
_cell_measurement_reflns_used    13485
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.2060
_cell_measurement_theta_min      3.9080
_cell_volume                     2772.33(6)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.956
_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     90.00 115.00   0.50    0.08    --   46.68  77.00-150.00   50
  2  \w     88.00 113.00   0.50    0.08    --   46.68  77.00 -90.00   50
  3  \w     92.00 117.00   0.50    0.08    --   46.68  77.00 -30.00   50
  4  \w     88.00 117.00   0.50    0.08    --   46.68  77.00 120.00   58
  5  \w     99.00 166.00   0.50    0.30    --  106.38 118.00 136.00  134
  6  \w     89.00 138.00   0.50    0.30    --  106.38  77.00  30.00   98
  7  \w    114.00 151.00   0.50    0.30    --  106.38 162.00 -73.00   74
  8  \w     96.00 178.00   0.50    0.30    --  106.38 125.00 -90.00  164
  9  \w    143.00 178.00   0.50    0.30    --  106.38  19.00-120.00   70
 10  \w    111.00 136.00   0.50    0.30    --  106.38  19.00-120.00   50
 11  \w     34.00  65.00   0.50    0.30    --  106.38 -57.00-150.00   62
 12  \w     34.00  62.00   0.50    0.30    --  106.38 -57.00-180.00   56
 13  \w     34.00  65.00   0.50    0.30    --  106.38 -57.00-120.00   62
 14  \w     34.00  66.00   0.50    0.30    --  106.38 -57.00  60.00   64
 15  \w     41.00 104.00   0.50    0.30    --  106.38 -77.00  60.00  126
 16  \w     34.00  99.00   0.50    0.30    --  106.38 -99.00  60.00  130
 17  \w     41.00  66.00   0.50    0.30    --  106.38-125.00 150.00   50
 18  \w     78.00 110.00   0.50    0.30    --  106.38-118.00  49.00   64
 19  \w     75.00 106.00   0.50    0.30    --  106.38 -99.00  90.00   62
 20  \w     62.00  87.00   0.50    0.08    --   46.68-162.00-100.00   50
 21  \w     70.00  95.00   0.50    0.30    --  106.38-162.00-100.00   50
 22  \w     62.00  88.00   0.50    0.30    --  106.38-125.00 -90.00   52
 23  \w     60.00  85.00   0.50    0.08    --   46.68-118.00  49.00   50
 24  \w    -41.00 -13.00   0.50    0.30    --  -86.25  38.00   0.00   56
 25  \w    -84.00 -11.00   0.50    0.08    --  -46.68 118.00 136.00  146
 26  \w    -47.00 -22.00   0.50    0.30    --  -86.25 118.00 136.00   50
 27  \w    -43.00 -13.00   0.50    0.30    --  -86.25  38.00 -30.00   60
 28  \w   -118.00 -93.00   0.50    0.08    --  -46.68 -77.00 120.00   50
 29  \w   -114.00 -88.00   0.50    0.08    --  -46.68 -77.00  60.00   52
 30  \w   -118.00 -88.00   0.50    0.08    --  -46.68 -77.00   0.00   60
 31  \w   -149.00 -86.00   0.50    0.30    --  -86.25-118.00  49.00  126
 32  \w   -114.00 -50.00   0.50    0.08    --  -46.68-162.00-100.00  128
 33  \w   -119.00 -94.00   0.50    0.30    --  -86.25-162.00-100.00   50
;
_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  0.0687
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21910
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.288
_diffrn_reflns_theta_min         3.929
_exptl_absorpt_coefficient_mu    24.610
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    2.621
_exptl_crystal_description       plank
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.517
_refine_diff_density_min         -1.953
_refine_diff_density_rms         0.308
_refine_ls_extinction_coef       0.00015(4)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5613
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5076
_reflns_number_total             5613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_database_code               7249830
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.639
_shelx_estimated_absorpt_t_min   0.173
_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
 H24B-O25_$1
 2.269 with sigma of 0.01
 H14A-O23
 1.805 with sigma of 0.01
 O18_$1-H14B
 1.914 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O14) = Uanis(C1) = Uanis(C2)
4.a Free rotating group:
 O23(H23A,H23B), O25(H25A,H25B), O24(H24A,H24B)
4.b Rotating group:
 O14(H14A,H14B)
4.c Idealised Me refined as rotating group:
 N7(H7A,H7B,H7C), N6(H6A,H6B,H6C), N2(H2A,H2B,H2C), N5(H5A,H5B,H5C), N4(H4A,
 H4B,H4C), N8(H8A,H8B,H8C), N1(H1A,H1B,H1C), N3(H3A,H3B,H3C)
;
_shelx_res_checksum              62944
_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
;