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_7249834
_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         'C6 H42 Co3 Mo8 N12 Na2 O57.017 V5, 4.5(O)'
_chemical_formula_sum            'C6 H42 Co3 Mo8 N12 Na2 O61.52 V5'
_chemical_formula_weight         2511.82
_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             2024-11-22
_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                86.364(2)
_cell_angle_beta                 81.442(2)
_cell_angle_gamma                88.936(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2251(3)
_cell_length_b                   15.9667(3)
_cell_length_c                   16.2567(5)
_cell_measurement_reflns_used    20817
_cell_measurement_temperature    170.00(11)
_cell_measurement_theta_max      76.2240
_cell_measurement_theta_min      3.7620
_cell_volume                     3387.58(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 41.92a 64-bit (release 05-12-2020))'
_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      170.00(11)
_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 0.953
_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    -78.00  -6.00   0.50    0.70    --  -47.03 108.00  50.00  144
  2  \w     21.00  78.00   0.50    0.70    --   47.03-108.00 -46.00  114
  3  \w   -126.00-100.00   0.50    2.80    --  -86.25-108.00 -46.00   52
  4  \w    -53.00 -27.00   0.50    2.80    --  -86.25 108.00  50.00   52
  5  \w     81.00 107.00   0.50    2.80    --  106.40-108.00 -46.00   52
  6  \w    105.00 132.00   0.50    2.80    --  106.40 108.00  50.00   54
  7  \w   -114.00 -88.00   0.50    0.70    --  -47.03-125.00 150.00   52
  8  \w    -23.00  19.00   0.50    0.70    --  -47.03  19.00  60.00   84
  9  \w   -103.00 -77.00   0.50    0.70    --  -47.03-125.00 120.00   52
 10  \w   -102.00 -76.00   0.50    0.70    --  -47.03-125.00 -30.00   52
 11  \w    -59.00  21.00   0.50    0.70    --  -47.03  57.00   0.00  160
 12  \w    -23.00  24.00   0.50    0.70    --  -47.03  19.00 120.00   94
 13  \w    -18.00  24.00   0.50    0.70    --  -47.03  19.00 -30.00   84
 14  \w     45.00  71.00   0.50    0.70    --   47.03-125.00  90.00   52
 15  \w    -65.00 -39.00   0.50    2.80    --  -86.25  57.00 -60.00   52
 16  \w    -41.00 -14.00   0.50    2.80    --  -86.25  38.00  90.00   54
 17  \w   -154.00 -73.00   0.50    2.80    --  -86.25 -38.00   0.00  162
 18  \w    -41.00 -13.00   0.50    2.80    --  -86.25  38.00-120.00   56
 19  \w     39.00  64.00   0.50    2.80    --  106.40 -57.00 -60.00   50
 20  \w     35.00 103.00   0.50    2.80    --  106.40 -99.00  90.00  136
 21  \w     72.00 103.00   0.50    2.80    --  106.40 -99.00-150.00   62
 22  \w     93.00 145.00   0.50    2.80    --  106.40  38.00-180.00  104
 23  \w     35.00  61.00   0.50    2.80    --  106.40 -57.00-180.00   52
 24  \w     36.00  62.00   0.50    2.80    --  106.40 -57.00  90.00   52
 25  \w     94.00 175.00   0.50    2.80    --  106.40  19.00 150.00  162
 26  \w    102.00 175.00   0.50    2.80    --  106.40  19.00 120.00  146
 27  \w    111.00 165.00   0.50    2.80    --  106.40  57.00  30.00  108
 28  \w     37.00  63.00   0.50    2.80    --  106.40 -57.00-150.00   52
 29  \w     38.00 111.00   0.50    2.80    --  106.40-125.00  30.00  146
 30  \w     34.00  66.00   0.50    2.80    --  106.40 -99.00-150.00   64
 31  \w     35.00  99.00   0.50    2.80    --  106.40 -99.00 -30.00  128
 32  \w     94.00 176.00   0.50    2.80    --  106.40  19.00  60.00  164
 33  \w     45.00 102.00   0.50    2.80    --  106.40 -99.00-180.00  114
 34  \w     50.00  94.00   0.50    2.80    --  106.40 -99.00  30.00   88
 35  \w    110.00 160.00   0.50    2.80    --  106.40  19.00  30.00  100
 36  \w     38.00  64.00   0.50    2.80    --  106.40-125.00 -30.00   52
 37  \w     47.00 111.00   0.50    2.80    --  106.40-125.00 150.00  128
 38  \w     66.00 111.00   0.50    2.80    --  106.40-125.00 -30.00   90
 39  \w     34.00  66.00   0.50    2.80    --  106.40 -57.00-120.00   64
 40  \w     61.00 110.00   0.50    2.80    --  106.40-125.00  90.00   98
 41  \w     42.00 101.00   0.50    2.80    --  106.40 -99.00-120.00  118
 42  \w     34.00  59.00   0.50    2.80    --  106.40 -77.00 -60.00   50
 43  \w     47.00 110.00   0.50    2.80    --  106.40-125.00-180.00  126
;
_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      -0.0080466000
_diffrn_orient_matrix_UB_12      0.0155734000
_diffrn_orient_matrix_UB_13      0.0933172000
_diffrn_orient_matrix_UB_21      0.1037333000
_diffrn_orient_matrix_UB_22      -0.0447070000
_diffrn_orient_matrix_UB_23      0.0030294000
_diffrn_orient_matrix_UB_31      0.0552496000
_diffrn_orient_matrix_UB_32      0.0843013000
_diffrn_orient_matrix_UB_33      -0.0223877000
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44397
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.552
_diffrn_reflns_theta_min         3.380
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.036
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
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_density_diffrn    2.463
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.759
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.368
_refine_ls_extinction_coef       0.00052(6)
_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   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         13752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0951
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1430P)^2^+88.1793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11842
_reflns_number_total             13752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01187b2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7249826--7249834.cif.'
_cod_original_cell_volume        3387.59(15)
_cod_database_code               7249834
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Na V5 Mo8 Co3 C6 N12 O60'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.532
_shelx_estimated_absorpt_t_min   0.123
_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(O60) = Uanis(O61)
Uanis(O57) = Uanis(O56)
Uanis(O63) = Uanis(O57)
3. Others
 Fixed Sof: Na58(0.5) O57(0.5) H57A(0.5) H57B(0.5) O49(0.5) O48(0.5) Na62(0.5)
 O59(0.5) H59A(0.5) H59B(0.5) C5(0.5) O50(0.5) O51(0.5) O54(0.5) C6(0.5)
 C23(0.5) O58(0.5) O65(0.5) O64(0.5) C29(0.5) O62(0.5) O68(0.5) O66(0.5)
 O69(0.5) O67(0.5)
4.a Rotating group:
 O53(H53A,H53B), O52(H52A,H52B)
4.b X=CH2 refined with riding coordinates:
 O57(H57A,H57B), O59(H59A,H59B)
4.c Idealised Me refined as rotating group:
 N5(H5A,H5B,H5C), N9(H9A,H9B,H9C), N3(H3A,H3B,H3C), N6(H6A,H6B,H6C), N2(H2A,
 H2B,H2C), N1(H1A,H1B,H1C), N10(H10A,H10B,H10C), N8(H8A,H8B,H8C), N4(H4A,H4B,
 H4C), N7(H7A,H7B,H7C), N11(H11A,H11B,H11C), N12(H12A,H12B,H12C)
;
_shelx_res_checksum              80662
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.983
_oxdiff_exptl_absorpt_empirical_full_min 0.525