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_7061007
_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         'C4 H4 Mo2 O15, 2(C2 H12 Co N4 O4), 4(H2 O)'
_chemical_formula_sum            'C8 H36 Co2 Mo2 N8 O27'
_chemical_formula_weight         986.19
_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             2021-05-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-14 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                66.911(3)
_cell_angle_beta                 74.016(3)
_cell_angle_gamma                87.852(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4297(2)
_cell_length_b                   10.3770(3)
_cell_length_c                   10.9734(4)
_cell_measurement_reflns_used    17073
_cell_measurement_temperature    169.97(10)
_cell_measurement_theta_max      79.5150
_cell_measurement_theta_min      4.5660
_cell_volume                     745.79(5)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 1.000
_diffrn_measured_fraction_theta_max 0.976
_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     67.00  93.00   0.50    0.05    --   48.02  77.00  90.00   52
  2  \w     85.00 118.00   0.50    0.05    --   48.02  77.00 150.00   66
  3  \w     26.00  52.00   0.50    0.05    --   48.02  77.00 150.00   52
  4  \w     26.00  53.00   0.50    0.05    --   48.02  77.00  90.00   54
  5  \w     64.00 102.00   0.50    0.05    --   48.02  38.00  90.00   76
  6  \w     28.00  54.00   0.50    0.05    --   50.00  75.00   0.87   52
  7  \w     61.00  88.00   0.50    0.05    --   48.02  38.00  30.00   54
  8  \w     38.00  75.00   0.50    0.05    --   48.02  38.00   0.00   74
  9  \w     25.00  60.00   0.50    0.05    --   48.02  77.00 -60.00   70
 10  \w     25.00  50.00   0.50    0.05    --   48.02  77.00-180.00   50
 11  \w     56.00  94.00   0.50    0.05    --  113.25 -95.00  30.00   76
 12  \w     56.00  82.00   0.50    0.05    --  113.25-150.00  14.00   52
 13  \w    101.00 128.00   0.50    0.05    --  113.25-150.00  14.00   54
 14  \w     44.00 110.00   0.50    0.05    --  113.25-125.00  90.00  132
 15  \w     48.00 102.00   0.50    0.05    --   48.02-150.00  14.00  108
 16  \w     42.00  68.00   0.50    0.05    --  113.25-125.00 -90.00   52
 17  \w     83.00 110.00   0.50    0.05    --  113.25-125.00 -60.00   54
 18  \w     85.00 111.00   0.50    0.05    --  113.25-125.00-150.00   52
 19  \w     76.00 111.00   0.50    0.05    --  113.25-125.00 -90.00   70
 20  \w     44.00  82.00   0.50    0.05    --  113.25-125.00-150.00   76
 21  \w     42.00  76.00   0.50    0.05    --  113.25-125.00 -60.00   68
 22  \w     60.00  86.00   0.50    0.05    --  113.25 -95.00-150.00   52
 23  \w     77.00 104.00   0.50    0.05    --  113.25-125.00  30.00   54
 24  \w     50.00  96.00   0.50    0.05    --  113.25 -95.00   0.00   92
 25  \w     71.00 108.00   0.50    0.05    --  113.25-125.00 120.00   74
 26  \w     84.00 109.00   0.50    0.05    --  113.25-124.00 177.00   50
 27  \w     42.00 106.00   0.50    0.05    --  113.25 -95.00 120.00  128
 28  \w     36.00  90.00   0.50    0.05    --   48.02-124.00 177.00  108
 29  \w     80.00 105.00   0.50    0.05    --  113.25 -95.00 -60.00   50
 30  \w     44.00  69.00   0.50    0.05    --  113.25 -95.00 -60.00   50
 31  \w     43.00  74.00   0.50    0.05    --  113.25 -77.00   0.00   62
 32  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00  60.00   50
 33  \w     45.00  70.00   0.50    0.05    --  113.25 -61.00  90.00   50
 34  \w     46.00  71.00   0.50    0.05    --  113.25 -61.00 -60.00   50
 35  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00 -90.00   50
 36  \w     44.00  69.00   0.50    0.05    --  113.25 -61.00-150.00   50
 37  \w     60.00  85.00   0.50    0.05    --  113.25 -77.00-180.00   50
 38  \w     45.00  70.00   0.50    0.05    --  113.25 -61.00-180.00   50
 39  \w    121.00 147.00   0.50    0.05    --  113.25  30.00-120.00   52
 40  \w     71.00  97.00   0.50    0.05    --   54.00  77.00-135.11   52
 41  \w     35.00  61.00   0.50    0.05    --   58.00  77.00-163.95   52
 42  \w     32.00  57.00   0.50    0.05    --   54.00  77.00-135.11   50
 43  \w     92.00 146.00   0.50    0.05    --  113.25  77.00-180.00  108
 44  \w     93.00 159.00   0.50    0.05    --  113.25  77.00-150.00  132
 45  \w     93.00 126.00   0.50    0.05    --  113.25  77.00 -60.00   66
 46  \w     97.00 123.00   0.50    0.05    --  113.25  77.00 -90.00   52
 47  \w     91.00 159.00   0.50    0.05    --  113.25  77.00   0.00  136
 48  \w     39.00  72.00   0.50    0.05    --   62.00  77.00  77.75   66
 49  \w     91.00 146.00   0.50    0.05    --  113.25  77.00 150.00  110
 50  \w    131.00 174.00   0.50    0.05    --  113.25  77.00  90.00   86
 51  \w     99.00 174.00   0.50    0.05    --  113.25  77.00 120.00  150
 52  \w     95.00 120.00   0.50    0.05    --  113.25  77.00  90.00   50
 53  \w     97.00 122.00   0.50    0.05    --  113.25  77.00  60.00   50
 54  \w     91.00 148.00   0.50    0.05    --  113.25  77.00  30.00  114
 55  \w    101.00 126.00   0.50    0.05    --   54.00  73.00  17.19   50
 56  \w     45.00  71.00   0.50    0.05    --   66.00  73.00  77.75   52
 57  \w     37.00  63.00   0.50    0.05    --   58.00  73.00  42.99   52
 58  \w     34.00  60.00   0.50    0.05    --   54.00  73.00  17.19   52
 59  \w     95.00 120.00   0.50    0.05    --  113.25  77.00-120.00   50
 60  \w    102.00 178.00   0.50    0.05    --  113.25  61.00-180.00  152
 61  \w     92.00 118.00   0.50    0.05    --   54.00  71.00 -84.50   52
 62  \w     35.00  61.00   0.50    0.05    --   54.00  71.00 -84.50   52
 63  \w     52.00  77.00   0.50    0.05    --   74.00  76.00 -70.54   50
 64  \w    111.00 136.00   0.50    0.05    --  113.25  61.00-150.00   50
 65  \w    152.00 178.00   0.50    0.05    --  113.25  61.00-150.00   52
 66  \w    100.00 177.00   0.50    0.05    --  113.25  61.00-120.00  154
 67  \w     99.00 133.00   0.50    0.05    --  113.25  61.00   0.00   68
 68  \w    107.00 156.00   0.50    0.05    --  113.25  61.00 -90.00   98
 69  \w    136.00 176.00   0.50    0.05    --  113.25  61.00  60.00   80
 70  \w    101.00 131.00   0.50    0.05    --  113.25  61.00  60.00   60
 71  \w    100.00 138.00   0.50    0.05    --  113.25  61.00  90.00   76
 72  \w     98.00 144.00   0.50    0.05    --  113.25  61.00 120.00   92
 73  \w    104.00 176.00   0.50    0.05    --  113.25  61.00 150.00  144
 74  \w    107.00 141.00   0.50    0.05    --  113.25  61.00 -60.00   68
 75  \w    146.00 171.00   0.50    0.05    --  113.25  61.00 -60.00   50
 76  \w     97.00 178.00   0.50    0.05    --  113.25  61.00 -30.00  162
 77  \w    101.00 130.00   0.50    0.05    --  113.25  45.00   0.00   58
 78  \w    142.00 167.00   0.50    0.05    --  113.25  45.00 -30.00   50
 79  \w    144.00 169.00   0.50    0.05    --  113.25  45.00   0.00   50
 80  \w    136.00 177.00   0.50    0.05    --  113.25  45.00  30.00   82
 81  \w    122.00 147.00   0.50    0.05    --  113.25 150.00  59.00   50
 82  \w    131.00 157.00   0.50    0.05    --  113.25 124.00-103.00   52
 83  \w    104.00 153.00   0.50    0.05    --  113.25 125.00 -90.00   98
 84  \w    -14.00  20.00   0.50    0.05    --   18.00  98.00-147.69   68
 85  \w      6.00  32.00   0.50    0.05    --   34.00  94.00  70.54   52
 86  \w    -70.00 -44.00   0.50    0.05    --  -91.75  61.00 120.00   52
 87  \w   -100.00 -64.00   0.50    0.05    --  -48.02 150.00  59.00   72
 88  \w    -85.00 -48.00   0.50    0.05    --  -91.75 124.00-103.00   74
 89  \w    -81.00 -43.00   0.50    0.05    --  -48.02 124.00-103.00   76
 90  \w   -121.00 -71.00   0.50    0.05    --  -48.02 -19.00 -90.00  100
 91  \w    -95.00 -44.00   0.50    0.05    --  -48.02 -38.00-120.00  102
 92  \w    -68.00 -38.00   0.50    0.05    --  -48.02 -19.00 -90.00   60
 93  \w    -50.00 -25.00   0.50    0.05    --  -48.02 -77.00 -90.00   50
 94  \w    -72.00 -35.00   0.50    0.05    --  -48.02 -44.00  42.79   74
 95  \w    -94.00 -69.00   0.50    0.05    --  -91.75 -77.00 120.00   50
 96  \w    -97.00 -70.00   0.50    0.05    --  -91.75 -77.00  90.00   54
 97  \w   -142.00-116.00   0.50    0.05    --  -91.75 -77.00 120.00   52
 98  \w    -94.00 -69.00   0.50    0.05    --  -91.75 -77.00 -30.00   50
 99  \w    -80.00 -55.00   0.50    0.05    --  -78.00 -76.00 -67.27   50
100  \w    -81.00 -55.00   0.50    0.05    --  -78.00 -76.00-121.62   52
101  \w    -94.00 -69.00   0.50    0.05    --  -91.75 -77.00-150.00   50
102  \w   -145.00-119.00   0.50    0.05    --  -91.75 -77.00-150.00   52
103  \w   -135.00-110.00   0.50    0.05    --  -78.00 -76.00-121.62   50
104  \w   -102.00 -70.00   0.50    0.05    --  -91.75 -75.00-111.40   64
105  \w    -81.00 -56.00   0.50    0.05    --  -78.00 -75.00 -80.61   50
106  \w    -95.00 -70.00   0.50    0.05    --  -91.75 -75.00 -50.05   50
107  \w    -96.00 -71.00   0.50    0.05    --  -91.75 -74.00  11.83   50
108  \w    -76.00 -51.00   0.50    0.05    --  -74.00 -76.00  44.00   50
109  \w    -86.00 -60.00   0.50    0.05    --  -82.00 -74.00 131.73   52
110  \w   -100.00 -70.00   0.50    0.05    --  -91.75 -74.00 163.25   60
111  \w   -155.00-120.00   0.50    0.05    --  -90.00 -75.00  42.91   70
112  \w   -103.00 -73.00   0.50    0.05    --  -91.75 -71.00  65.38   60
113  \w   -112.00 -69.00   0.50    0.05    --  -90.00 -75.00  42.91   86
114  \w    -97.00 -72.00   0.50    0.05    --  -91.75 -70.00  95.89   50
115  \w    -76.00 -50.00   0.50    0.05    --  -70.00 -69.00 147.82   52
116  \w    -79.00 -54.00   0.50    0.05    --  -74.00 -69.00 136.72   50
117  \w    -76.00 -50.00   0.50    0.05    --  -70.00 -69.00 101.22   52
118  \w    -79.00 -48.00   0.50    0.05    --  -66.00 -68.00 161.59   62
119  \w    -97.00 -72.00   0.50    0.05    --  -91.75 -69.00  -6.88   50
120  \w    -81.00 -56.00   0.50    0.05    --  -78.00 -74.00 -92.06   50
121  \w   -109.00 -71.00   0.50    0.05    --  -91.75 -74.00-100.28   76
122  \w   -111.00 -73.00   0.50    0.05    --  -91.75 -68.00-174.29   76
123  \w    -89.00 -63.00   0.50    0.05    --  -82.00 -73.00-100.82   52
124  \w   -102.00 -74.00   0.50    0.05    --  -91.75 -66.00-151.29   56
125  \w   -110.00 -73.00   0.50    0.05    --  -91.75 -67.00 -86.81   74
126  \w    -73.00 -47.00   0.50    0.05    --  -66.00 -67.00 -25.55   52
127  \w    -81.00 -55.00   0.50    0.05    --  -70.00 -66.00 -16.33   52
128  \w    -86.00 -51.00   0.50    0.05    --  -66.00 -63.00-169.75   70
129  \w    -82.00 -56.00   0.50    0.05    --  -74.00 -67.00  -3.38   52
130  \w   -135.00-109.00   0.50    0.05    --  -66.00 -68.00 161.59   52
131  \w    -95.00 -70.00   0.50    0.05    --  -86.00 -65.00 162.47   50
132  \w    -86.00 -57.00   0.50    0.05    --  -74.00 -65.00 157.40   58
133  \w    -75.00 -50.00   0.50    0.05    --  -66.00 -63.00 -64.09   50
134  \w    -76.00 -50.00   0.50    0.05    --  -66.00 -62.00 -78.84   52
135  \w    -82.00 -54.00   0.50    0.05    --  -70.00 -63.00-179.50   56
136  \w   -130.00-105.00   0.50    0.05    --  -66.00 -63.00-169.75   50
137  \w    -78.00 -53.00   0.50    0.05    --  -70.00 -62.00 -50.68   50
138  \w    -93.00 -68.00   0.50    0.05    --  -82.00 -61.00 -32.19   50
139  \w   -107.00 -81.00   0.50    0.05    --  -91.75 -61.00 -30.00   52
140  \w    -92.00 -67.00   0.50    0.05    --  -82.00 -58.00 -50.80   50
141  \w    -87.00 -61.00   0.50    0.05    --  -74.00 -60.00  52.22   52
142  \w    -79.00 -54.00   0.50    0.05    --  -70.00 -61.00  75.39   50
143  \w   -101.00 -75.00   0.50    0.05    --  -91.75 -62.00 111.29   52
144  \w   -143.00-118.00   0.50    0.05    --  -91.75-124.00 177.00   50
145  \w   -120.00 -95.00   0.50    0.05    --  -48.02-124.00 177.00   50
146  \w   -107.00 -82.00   0.50    0.05    --  -48.02-150.00  14.00   50
147  \w   -127.00-102.00   0.50    0.05    --  -91.75-150.00  14.00   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  0.0904
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23798
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.263
_diffrn_reflns_theta_min         4.568
_exptl_absorpt_coefficient_mu    16.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55758
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_description       block
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.030
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0037(3)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0580P)^2^+0.5808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3057
_reflns_number_total             3180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03280a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7061007--7061013.cif.'
_cod_original_cell_volume        745.79(4)
_cod_database_code               7061007
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.266
_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.a Free rotating group:
 O3W(H3WA,H3WB), O2W(H2WA,H2WB)
2.b Rotating group:
 O1W(H1WA,H1WB)
2.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N4(H4A,H4B,H4C), N3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              72329
_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
;