The role of mono- and dicarboxylic acids in the building of oxomolybdates containing {MoO4}, {Mo2O5}, {Mo2O6}, {Mo3O8}, {Mo5O17}, {Mo5O18}, {Mo8O26}, and {SiMo12O40} units
Kuzman, Dino; Damjanović, Vladimir; Stilinović, Vladimir; Cindrić, Marina; Vrdoljak, Višnja; New Journal of Chemistry 45 (2021) 19764–19774; doi:10.1039/D1NJ03280A

data_7061012
_publ_section_title
;
 The role of mono- and dicarboxylic acids in the building of oxomolybdates
 containing {MoO4}, {Mo2O5}, {Mo2O6}, {Mo3O8}, {Mo5O17}, {Mo5O18},
 {Mo8O26}, and {SiMo12O40} units
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19764
_journal_page_last               19774
_journal_paper_doi               10.1039/D1NJ03280A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'Mo8 O26, 4(C2 H12 Co N4 O4), 12(H2 O)'
_chemical_formula_sum            'C8 H72 Co4 Mo8 N16 O54'
_chemical_formula_weight         2260.05
_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             2021-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-14 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                93.0160(10)
_cell_angle_beta                 107.3180(10)
_cell_angle_gamma                103.2230(10)
_cell_formula_units_Z            1
_cell_length_a                   8.51130(10)
_cell_length_b                   13.7625(2)
_cell_length_c                   13.9561(2)
_cell_measurement_reflns_used    29528
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      76.9400
_cell_measurement_theta_min      4.3940
_cell_volume                     1506.42(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.940
_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     27.00  53.00   0.50    0.05    --   48.02  77.00   0.00   52
  2  \w     26.00  53.00   0.50    0.05    --   48.02  77.00  60.00   54
  3  \w     25.00  51.00   0.50    0.05    --   48.02  77.00 120.00   52
  4  \w     59.00  85.00   0.50    0.05    --   48.02  77.00 120.00   52
  5  \w     39.00  89.00   0.50    0.12    --  107.54 -99.00 120.00  100
  6  \w     37.00  81.00   0.50    0.12    --  107.54-125.00  60.00   88
  7  \w     86.00 111.00   0.50    0.12    --  107.54-125.00  60.00   50
  8  \w     43.00 111.00   0.50    0.12    --  107.54-125.00  30.00  136
  9  \w     38.00  63.00   0.50    0.12    --  107.54-125.00   0.00   50
 10  \w     72.00  98.00   0.50    0.12    --  107.54-125.00   0.00   52
 11  \w     35.00 108.00   0.50    0.12    --  107.54-111.00-103.00  146
 12  \w     35.00  68.00   0.50    0.12    --  107.54 -99.00-180.00   66
 13  \w     76.00 102.00   0.50    0.12    --  107.54 -99.00-180.00   52
 14  \w     68.00  93.00   0.50    0.12    --  107.54 -99.00-120.00   50
 15  \w     26.00  88.00   0.50    0.05    --   48.02-111.00-103.00  124
 16  \w     45.00  96.00   0.50    0.12    --  107.54 -99.00  60.00  102
 17  \w     35.00 105.00   0.50    0.12    --  107.54 -99.00  90.00  140
 18  \w     54.00 104.00   0.50    0.12    --  107.54 -99.00 150.00  100
 19  \w     40.00  65.00   0.50    0.12    --  107.54 -57.00 -60.00   50
 20  \w     36.00  66.00   0.50    0.12    --  107.54 -57.00-120.00   60
 21  \w     43.00 101.00   0.50    0.12    --  107.54 -77.00-120.00  116
 22  \w     -5.00  61.00   0.50    0.05    --   48.02 -57.00-120.00  132
 23  \w     39.00  66.00   0.50    0.12    --  107.54 -57.00  90.00   54
 24  \w     40.00  65.00   0.50    0.12    --  107.54 -57.00 150.00   50
 25  \w    124.00 150.00   0.50    0.12    --  107.54 111.00 -10.00   52
 26  \w     35.00  60.00   0.50    0.05    --   58.00  77.00 124.96   50
 27  \w     77.00 103.00   0.50    0.05    --   58.00  77.00 124.96   52
 28  \w     36.00  62.00   0.50    0.05    --   58.00  76.00  12.77   52
 29  \w     36.00  62.00   0.50    0.05    --   58.00  76.00 -17.42   52
 30  \w     32.00  57.00   0.50    0.05    --   54.00  76.00 -41.76   50
 31  \w     33.00  64.00   0.50    0.05    --   54.00  75.00-112.81   62
 32  \w     44.00  74.00   0.50    0.05    --   66.00  76.00 -54.28   60
 33  \w     52.00  94.00   0.50    0.05    --   74.00  75.00 -35.05   84
 34  \w     97.00 128.00   0.50    0.05    --   58.00  76.00 -17.42   62
 35  \w     41.00  70.00   0.50    0.05    --   62.00  72.00-174.07   58
 36  \w     40.00  66.00   0.50    0.05    --   62.00  75.00  76.30   52
 37  \w     48.00  74.00   0.50    0.05    --   70.00  76.00 124.01   52
 38  \w     33.00  59.00   0.50    0.05    --   54.00  75.00 167.12   52
 39  \w     46.00  76.00   0.50    0.05    --   66.00  71.00 178.21   60
 40  \w     88.00 139.00   0.50    0.05    --   66.00  71.00 178.21  102
 41  \w     35.00  65.00   0.50    0.05    --   54.00  71.00 -84.49   60
 42  \w     43.00  88.00   0.50    0.05    --   62.00  71.00-145.79   90
 43  \w     42.00  79.00   0.50    0.05    --   62.00  70.00 108.40   74
 44  \w     12.00  38.00   0.50    0.05    --   38.00  86.00  79.54   52
 45  \w     -1.00  26.00   0.50    0.05    --   30.00  97.00 116.96   54
 46  \w    -40.00 -11.00   0.50    0.05    --    6.00 123.00  56.08   58
 47  \w    -12.00  16.00   0.50    0.05    --   22.00 100.00  -9.88   56
 48  \w     13.00  38.00   0.50    0.05    --   42.00  90.00 -96.48   50
 49  \w     15.00  40.00   0.50    0.05    --   42.00  87.00-164.89   50
 50  \w    -16.00  22.00   0.50    0.05    --   14.00  96.00-117.33   76
 51  \w    -58.00 -13.00   0.50    0.05    --  -48.02 111.00 -10.00   90
 52  \w    -85.00 -20.00   0.50    0.12    --  -91.75 125.00 -90.00  130
 53  \w    -74.00 -49.00   0.50    0.12    --  -91.75 111.00 -10.00   50
 54  \w    -87.00 -35.00   0.50    0.05    --  -48.02 -19.00-120.00  104
 55  \w    -79.00 -41.00   0.50    0.05    --  -48.02 -19.00  30.00   76
 56  \w   -121.00 -85.00   0.50    0.05    --  -48.02 -19.00  30.00   72
 57  \w   -138.00 -73.00   0.50    0.12    --  -91.75 -77.00 120.00  130
 58  \w   -152.00 -69.00   0.50    0.12    --  -91.75 -77.00  30.00  166
 59  \w   -162.00-122.00   0.50    0.12    --  -91.75 -77.00   0.00   80
 60  \w   -124.00 -69.00   0.50    0.12    --  -91.75 -77.00-120.00  110
 61  \w   -140.00 -69.00   0.50    0.12    --  -91.75 -77.00 -11.10  142
 62  \w   -106.00 -69.00   0.50    0.12    --  -91.75 -77.00   0.00   74
 63  \w   -106.00 -70.00   0.50    0.12    --  -91.75 -77.00 -30.00   72
 64  \w   -162.00 -69.00   0.50    0.12    --  -91.75 -77.00 -60.00  186
 65  \w   -142.00-116.00   0.50    0.12    --  -91.75 -77.00 -30.00   52
 66  \w   -157.00 -65.00   0.50    0.12    --  -86.00 -75.00-103.25  184
 67  \w    -78.00 -52.00   0.50    0.12    --  -74.00 -75.00  42.05   52
 68  \w    -85.00 -60.00   0.50    0.12    --  -82.00 -75.00 150.74   50
 69  \w    -94.00 -69.00   0.50    0.12    --  -91.75 -77.00 150.00   50
 70  \w    -84.00 -58.00   0.50    0.12    --  -78.00 -74.00 176.35   52
 71  \w   -162.00-121.00   0.50    0.12    --  -91.75 -77.00 150.00   82
 72  \w   -152.00-127.00   0.50    0.12    --  -91.75 -74.00  59.39   50
 73  \w   -117.00 -70.00   0.50    0.12    --  -91.75 -74.00  59.39   94
 74  \w   -162.00 -70.00   0.50    0.12    --  -91.75 -74.00 161.34  184
 75  \w    -65.00 -40.00   0.50    0.05    --  -62.00 -75.00   2.90   50
 76  \w    -88.00 -62.00   0.50    0.12    --  -82.00 -73.00 118.52   52
 77  \w    -89.00 -64.00   0.50    0.12    --  -86.00 -74.00-124.61   50
 78  \w    -78.00 -53.00   0.50    0.12    --  -74.00 -73.00-101.86   50
 79  \w    -91.00 -61.00   0.50    0.12    --  -82.00 -74.00-159.08   60
 80  \w   -100.00 -64.00   0.50    0.12    --  -86.00 -75.00-166.36   72
 81  \w   -141.00 -71.00   0.50    0.12    --  -91.75 -74.00-173.08  140
 82  \w   -144.00-118.00   0.50    0.12    --  -74.00 -73.00-101.86   52
 83  \w   -162.00-101.00   0.50    0.12    --  -91.75 -72.00 -52.06  122
 84  \w    -97.00 -72.00   0.50    0.12    --  -91.75 -72.00 -52.06   50
 85  \w    -98.00 -73.00   0.50    0.12    --  -91.75 -71.00 -79.56   50
 86  \w   -158.00-133.00   0.50    0.12    --  -91.75 -71.00 -79.56   50
 87  \w    -81.00 -49.00   0.50    0.12    --  -70.00 -72.00 -33.28   64
 88  \w    -84.00 -58.00   0.50    0.12    --  -78.00 -71.00  -5.20   52
 89  \w   -163.00 -71.00   0.50    0.12    --  -91.75 -71.00 102.22  184
 90  \w   -163.00-126.00   0.50    0.12    --  -91.75 -70.00  69.28   74
 91  \w   -146.00-119.00   0.50    0.12    --  -91.75 -72.00 124.04   54
 92  \w   -101.00 -74.00   0.50    0.12    --  -91.75 -72.00 124.04   54
 93  \w    -78.00 -50.00   0.50    0.12    --  -70.00 -70.00 178.21   56
 94  \w   -107.00 -72.00   0.50    0.12    --  -91.75 -70.00  69.28   70
 95  \w    -76.00 -50.00   0.50    0.12    --  -70.00 -69.00  58.57   52
 96  \w   -159.00 -72.00   0.50    0.12    --  -91.75 -69.00  39.61  174
 97  \w   -163.00-125.00   0.50    0.12    --  -91.75 -68.00  90.89   76
 98  \w   -119.00 -73.00   0.50    0.12    --  -91.75 -68.00  90.89   92
 99  \w    -91.00 -65.00   0.50    0.12    --  -82.00 -66.00  64.43   52
100  \w   -155.00 -74.00   0.50    0.12    --  -91.75 -69.00 -95.63  162
101  \w    -90.00 -65.00   0.50    0.12    --  -82.00 -66.00-152.30   50
102  \w    -81.00 -56.00   0.50    0.12    --  -74.00 -65.00-130.65   50
103  \w   -106.00 -55.00   0.50    0.12    --  -74.00 -68.00-138.07  102
104  \w   -144.00-118.00   0.50    0.12    --  -74.00 -65.00-130.65   52
105  \w   -162.00-125.00   0.50    0.12    --  -91.75 -63.00-156.39   74
106  \w   -163.00-117.00   0.50    0.12    --  -91.75 -57.00-150.00   92
107  \w   -117.00 -79.00   0.50    0.12    --  -91.75 -63.00-156.39   76
108  \w    -95.00 -61.00   0.50    0.12    --  -78.00 -63.00 -92.69   68
109  \w    -90.00 -64.00   0.50    0.12    --  -82.00 -64.00 -25.92   52
110  \w    -84.00 -59.00   0.50    0.12    --  -74.00 -62.00   3.80   50
111  \w   -146.00-121.00   0.50    0.12    --  -91.75-111.00-103.00   50
;
_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      -0.0670216000
_diffrn_orient_matrix_UB_12      0.0622156000
_diffrn_orient_matrix_UB_13      0.0664468000
_diffrn_orient_matrix_UB_21      -0.1357343000
_diffrn_orient_matrix_UB_22      -0.0950630000
_diffrn_orient_matrix_UB_23      0.0015603000
_diffrn_orient_matrix_UB_31      0.1247377000
_diffrn_orient_matrix_UB_32      -0.0232650000
_diffrn_orient_matrix_UB_33      0.0958208000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1427
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45721
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.244
_diffrn_reflns_theta_min         4.403
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.726
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.058
_refine_diff_density_max         2.752
_refine_diff_density_min         -2.062
_refine_diff_density_rms         0.290
_refine_ls_extinction_coef       0.00091(14)
_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   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6014
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0613
_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^)+(0.1348P)^2^+1.3294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5424
_reflns_number_total             6014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03280a2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7061007--7061013.cif.'
_cod_database_code               7061012
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo8 Co4 C8 N16 O52'
_chemical_oxdiff_usercomment     kapilara
_shelx_estimated_absorpt_t_max   0.352
_shelx_estimated_absorpt_t_min   0.035
_diffrn_oxdiff_digest_frames
;
01391db3b9ec5e3dc1c8c3147682869fff08562085c
;
_diffrn_oxdiff_digest_hkl
;
019ff60b95250cd385e72f809ab7fbbdb1f141
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 O6W-H5WB
 1.913 with sigma of 0.02
 O16-H6WB
 1.93 with sigma of 0.02
 O2W-H3WA
 1.915 with sigma of 0.1
 O21-H2WB
 2.047 with sigma of 0.02
 O4W-H3WB
 2.102 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(O3W) = Uanis(O2W)
4.a Free rotating group:
 O1W(H1WA,H1WB), O6W(H6WA,H6WB), O4W(H4WA,H4WB), O2W(H2WA,H2WB), O5W(H5WA,
 H5WB), O3W(H3WA,H3WB)
4.b Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N3(H3A,H3B,H3C), N1(H1A,H1B,H1C), N5(H5A,H5B,H5C), N8(H8A,
 H8B,H8C), N2(H2A,H2B,H2C), N7(H7A,H7B,H7C), N6(H6A,H6B,H6C)
;
_shelx_res_checksum              31158
_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 5.073
_oxdiff_exptl_absorpt_empirical_full_min 0.443