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_7249831
_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), 12(H2O)'
_chemical_formula_sum            'C8 H76 Co4 Mo8 N16 O56'
_chemical_formula_weight         2296.01
_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                89.529(2)
_cell_angle_beta                 65.036(2)
_cell_angle_gamma                70.299(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5178(3)
_cell_length_b                   12.4160(3)
_cell_length_c                   12.6190(2)
_cell_measurement_reflns_used    13174
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      77.0650
_cell_measurement_theta_min      3.8340
_cell_volume                     1521.10(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.53a 64-bit (release 15-04-2022))'
_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_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.950
_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    -25.00  22.00   0.50    0.05    --  -46.68  41.00-169.00   94
  2  \w    -46.00 -20.00   0.50    0.15    --  -86.25  41.00-169.00   52
  3  \w    -62.00 -25.00   0.50    0.15    --  -86.25  57.00 -30.00   74
  4  \w    -43.00 -13.00   0.50    0.15    --  -86.25  38.00 -60.00   60
  5  \w    -52.00 -26.00   0.50    0.15    --  -86.25  57.00   0.00   52
  6  \w    -43.00 -14.00   0.50    0.15    --  -86.25  38.00   0.00   58
  7  \w    -43.00 -14.00   0.50    0.15    --  -86.25  38.00  30.00   58
  8  \w    -43.00 -18.00   0.50    0.15    --  -86.25  38.00 120.00   50
  9  \w    -43.00 -14.00   0.50    0.15    --  -86.25  38.00 150.00   58
 10  \w    -12.00  46.00   0.50    0.05    --   46.68 -41.00  37.00  116
 11  \w     96.00 138.00   0.50    0.15    --  106.38 125.00  30.00   84
 12  \w     97.00 152.00   0.50    0.15    --  106.38 125.00   0.00  110
 13  \w     34.00  61.00   0.50    0.05    --   46.68 -57.00   0.00   54
 14  \w    -24.00  30.00   0.50    0.05    --   46.68 -57.00   0.00  108
 15  \w     40.00  84.00   0.50    0.05    --   46.68-125.00 -90.00   88
 16  \w     85.00 110.00   0.50    0.15    --  106.38-125.00-120.00   50
 17  \w     34.00  70.00   0.50    0.15    --  106.38-125.00-120.00   72
 18  \w     39.00  64.00   0.50    0.15    --  106.38-125.00 -30.00   50
 19  \w     82.00 111.00   0.50    0.15    --  106.38-125.00 -30.00   58
 20  \w     75.00 105.00   0.50    0.15    --  106.38-125.00  60.00   60
 21  \w     35.00  69.00   0.50    0.15    --  106.38-125.00  60.00   68
 22  \w     37.00  62.00   0.50    0.15    --  106.38-107.00 150.85   50
 23  \w     55.00 109.00   0.50    0.15    --  106.38-114.00 132.72  108
 24  \w     82.00 107.00   0.50    0.15    --  106.38-107.00 150.85   50
 25  \w     78.00 104.00   0.50    0.15    --  106.38 -99.00  30.00   52
 26  \w     73.00 106.00   0.50    0.15    --  106.38 -99.00 -30.00   66
 27  \w     34.00  61.00   0.50    0.15    --  106.38 -99.00 -30.00   54
 28  \w     61.00  96.00   0.50    0.15    --  106.38 -99.00-180.00   70
 29  \w     36.00 101.00   0.50    0.15    --  106.38 -99.00-120.00  130
 30  \w     76.00 101.00   0.50    0.15    --  106.38 -99.00 -90.00   50
 31  \w     41.00  66.00   0.50    0.15    --  106.38 -57.00 -60.00   50
 32  \w     43.00  70.00   0.50    0.15    --  106.38 -77.00 -60.00   54
 33  \w     79.00 104.00   0.50    0.15    --  106.38 -77.00 -60.00   50
 34  \w     76.00 103.00   0.50    0.15    --  106.38 -77.00  30.00   54
 35  \w     68.00 105.00   0.50    0.15    --  106.38 -77.00  90.00   74
 36  \w     37.00  65.00   0.50    0.15    --  106.38 -57.00 120.00   56
 37  \w     39.00  66.00   0.50    0.15    --  106.38 -77.00  30.00   54
 38  \w     36.00  63.00   0.50    0.15    --  106.38 -57.00  30.00   54
 39  \w     38.00  63.00   0.50    0.15    --  106.38 -57.00 -30.00   50
 40  \w     36.00  61.00   0.50    0.15    --  106.38 -57.00-120.00   50
 41  \w     37.00  62.00   0.50    0.15    --  106.38 -57.00-180.00   50
 42  \w     56.00  88.00   0.50    0.05    --   46.68  41.00-169.00   64
 43  \w     95.00 170.00   0.50    0.15    --  106.38  41.00-169.00  150
 44  \w     94.00 178.00   0.50    0.15    --  106.38  19.00 120.00  168
 45  \w    144.00 178.00   0.50    0.15    --  106.38  19.00 150.00   68
 46  \w     94.00 122.00   0.50    0.15    --  106.38  19.00 150.00   56
 47  \w   -118.00 -38.00   0.50    0.05    --  -46.68 -41.00  37.00  160
 48  \w   -114.00 -83.00   0.50    0.05    --  -46.68-125.00   0.00   62
 49  \w   -156.00 -77.00   0.50    0.15    --  -86.25 -41.00  37.00  158
 50  \w    -81.00 -56.00   0.50    0.15    --  -86.25 125.00-120.00   50
 51  \w    -38.00 -13.00   0.50    0.15    --  -86.25 125.00-120.00   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  0.0534
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18740
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.156
_diffrn_reflns_theta_min         3.829
_exptl_absorpt_coefficient_mu    22.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18079
_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_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.485
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       0.00033(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   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0627P)^2^+2.1956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5749
_reflns_number_total             6119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_database_code               7249831
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.551
_shelx_estimated_absorpt_t_min   0.301
_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(O11) = Uanis(O1)
Uanis(O27A) = Uanis(O27B)
Uanis(O24B) = Uanis(O24A)
3. Others
 Sof(O24A)=1-FVAR(1)
 Sof(O24B)=FVAR(1)
 Fixed Sof: O27B(0.666667) O27A(0.333333)
4.a Rotating group:
 O14(H14A,H14B)
4.b Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N7(H7A,H7B,H7C), N5(H5A,H5B,H5C), N1(H1A,H1B,H1C), N6(H6A,
 H6B,H6C), N3(H3A,H3B,H3C), N8(H8A,H8B,H8C), N2(H2A,H2B,H2C)
;
_shelx_res_checksum              86543
_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
;