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_7061011
_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), 10(H2 O)'
_chemical_formula_sum            'C8 H68 Co4 Mo8 N16 O52'
_chemical_formula_weight         2224.02
_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             2021-05-12
_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                95.0810(10)
_cell_angle_beta                 107.1720(10)
_cell_angle_gamma                102.5790(10)
_cell_formula_units_Z            1
_cell_length_a                   8.51020(10)
_cell_length_b                   13.7353(2)
_cell_length_c                   13.95510(10)
_cell_measurement_reflns_used    26599
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.8590
_cell_measurement_theta_min      3.3310
_cell_volume                     1500.51(3)
_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 1.3 (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 0.998
_diffrn_measured_fraction_theta_max 0.939
_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     59.00  84.00   0.50    0.05    --   48.02  77.00 -30.00   50
  2  \w     25.00  70.00   0.50    0.05    --   48.02  77.00-150.00   90
  3  \w     82.00 119.00   0.50    0.05    --   48.02  77.00-150.00   74
  4  \w     26.00  56.00   0.50    0.05    --   48.02  77.00 -30.00   60
  5  \w     29.00  55.00   0.50    0.05    --   48.02  68.00 -70.00   52
  6  \w     76.00 102.00   0.50    0.05    --   48.02  68.00 -70.00   52
  7  \w     25.00  62.00   0.50    0.05    --   48.02  77.00  30.00   74
  8  \w     38.00  63.00   0.50    0.05    --   48.02  38.00  60.00   50
  9  \w     36.00  62.00   0.50    0.05    --   48.02  38.00 120.00   52
 10  \w     25.00  75.00   0.50    0.05    --   48.02  77.00  90.00  100
 11  \w     25.00 109.00   0.50    0.05    --   48.02  77.00 150.00  168
 12  \w     82.00 121.00   0.50    0.05    --   48.02  38.00 120.00   78
 13  \w     36.00  65.00   0.50    0.20    --  107.54 -99.00 -30.00   58
 14  \w     34.00  95.00   0.50    0.05    --   48.02-125.00-180.00  122
 15  \w     39.00 111.00   0.50    0.20    --  107.54-125.00 -30.00  144
 16  \w     38.00 111.00   0.50    0.20    --  107.54-125.00  60.00  146
 17  \w     42.00 110.00   0.50    0.20    --  107.54-125.00  90.00  136
 18  \w     39.00 111.00   0.50    0.20    --  107.54-125.00 150.00  144
 19  \w     74.00 111.00   0.50    0.20    --  107.54-125.00 -60.00   74
 20  \w     36.00  61.00   0.50    0.20    --  107.54 -99.00-120.00   50
 21  \w     67.00 111.00   0.50    0.20    --  107.54-125.00-180.00   88
 22  \w     53.00 102.00   0.50    0.20    --  107.54 -99.00-150.00   98
 23  \w     69.00 101.00   0.50    0.20    --  107.54 -99.00 -30.00   64
 24  \w     38.00  79.00   0.50    0.20    --  107.54 -99.00   0.00   82
 25  \w     35.00  81.00   0.50    0.20    --  107.54 -99.00  90.00   92
 26  \w     76.00 104.00   0.50    0.20    --  107.54 -99.00 150.00   56
 27  \w     35.00  61.00   0.50    0.20    --  107.54 -99.00 150.00   52
 28  \w     35.00  66.00   0.50    0.20    --  107.54 -57.00 120.00   62
 29  \w     37.00  76.00   0.50    0.20    --  107.54 -68.00 156.00   78
 30  \w    -22.00  33.00   0.50    0.05    --   48.02 -68.00 156.00  110
 31  \w    122.00 161.00   0.50    0.20    --  107.54  68.00 -70.00   78
 32  \w    -97.00 -36.00   0.50    0.05    --  -48.02 -19.00   0.00  122
 33  \w    -62.00 -25.00   0.50    0.05    --  -48.02 -77.00-120.00   74
 34  \w    -83.00 -35.00   0.50    0.20    --  -91.75  68.00 -70.00   96
 35  \w    -65.00  24.00   0.50    0.05    --  -48.02  68.00 -70.00  178
 36  \w    -58.00 -30.00   0.50    0.05    --  -48.02 -66.00 -82.63   56
 37  \w   -120.00 -85.00   0.50    0.05    --  -48.02 -66.00 -82.63   70
 38  \w    -68.00 -33.00   0.50    0.05    --  -48.02 -57.00 -30.00   70
 39  \w    -74.00 -36.00   0.50    0.05    --  -48.02 -43.00-132.23   76
 40  \w    -74.00 -35.00   0.50    0.05    --  -48.02 -38.00 -30.00   78
 41  \w   -106.00 -80.00   0.50    0.05    --  -48.02 -68.00 156.00   52
 42  \w    -55.00 -29.00   0.50    0.05    --  -48.02 -68.00 156.00   52
 43  \w    -79.00 -35.00   0.50    0.05    --  -48.02 -43.00 134.14   88
 44  \w   -118.00 -92.00   0.50    0.05    --  -48.02 -38.00 -30.00   52
 45  \w   -141.00 -78.00   0.50    0.20    --  -91.75 -57.00 -90.00  126
 46  \w   -163.00-116.00   0.50    0.20    --  -91.75 -77.00-120.00   94
 47  \w    -94.00 -69.00   0.50    0.20    --  -91.75 -77.00-120.00   50
 48  \w    -94.00 -69.00   0.50    0.20    --  -91.75 -77.00 -30.00   50
 49  \w   -163.00-100.00   0.50    0.20    --  -91.75 -77.00 -30.00  126
 50  \w    -94.00 -69.00   0.50    0.20    --  -91.75 -77.00  90.00   50
 51  \w   -159.00 -69.00   0.50    0.20    --  -91.75 -77.00  60.00  180
 52  \w   -150.00-124.00   0.50    0.20    --  -91.75 -77.00  90.00   52
 53  \w   -144.00-119.00   0.50    0.20    --  -91.75 -77.00  30.00   50
 54  \w    -95.00 -70.00   0.50    0.20    --  -91.75 -77.00  30.00   50
 55  \w   -101.00 -70.00   0.50    0.20    --  -91.75 -77.00 -60.00   62
 56  \w   -158.00-127.00   0.50    0.20    --  -91.75 -77.00 -60.00   62
 57  \w    -96.00 -70.00   0.50    0.20    --  -91.75 -77.00-150.00   52
 58  \w   -127.00 -69.00   0.50    0.20    --  -91.75 -77.00-180.00  116
 59  \w   -159.00-132.00   0.50    0.20    --  -91.75 -77.00-180.00   54
 60  \w   -157.00-131.00   0.50    0.20    --  -91.75 -77.00-150.00   52
 61  \w   -162.00 -70.00   0.50    0.20    --  -91.75 -74.00 -12.45  184
 62  \w   -118.00 -71.00   0.50    0.20    --  -91.75 -74.00  35.23   94
 63  \w   -157.00-121.00   0.50    0.20    --  -91.75 -74.00  35.23   72
 64  \w   -144.00-116.00   0.50    0.20    --  -91.75 -73.00 133.60   56
 65  \w   -109.00 -71.00   0.50    0.20    --  -91.75 -73.00 133.60   76
 66  \w   -103.00 -71.00   0.50    0.20    --  -91.75 -72.00 145.69   64
 67  \w   -163.00 -72.00   0.50    0.20    --  -91.75 -73.00   9.21  182
 68  \w    -99.00 -71.00   0.50    0.20    --  -91.75 -72.00  -4.22   56
 69  \w   -163.00 -71.00   0.50    0.20    --  -91.75 -72.00 122.34  184
 70  \w   -154.00 -71.00   0.50    0.20    --  -91.75 -73.00 -89.35  166
 71  \w    -97.00 -72.00   0.50    0.20    --  -91.75 -70.00-113.17   50
 72  \w   -161.00-106.00   0.50    0.20    --  -91.75 -70.00-113.17  110
 73  \w   -163.00 -71.00   0.50    0.20    --  -91.75 -73.00-171.15  184
 74  \w   -134.00 -71.00   0.50    0.20    --  -91.75 -72.00-163.80  126
 75  \w   -103.00 -74.00   0.50    0.20    --  -91.75 -68.00  41.33   58
 76  \w   -162.00 -72.00   0.50    0.20    --  -91.75 -69.00 103.23  180
 77  \w   -148.00-121.00   0.50    0.20    --  -91.75 -68.00 156.00   54
 78  \w   -117.00 -74.00   0.50    0.20    --  -91.75 -68.00 156.00   86
 79  \w   -159.00 -72.00   0.50    0.20    --  -91.75 -69.00  63.51  174
 80  \w    -98.00 -73.00   0.50    0.20    --  -91.75 -66.00  85.08   50
 81  \w   -153.00-115.00   0.50    0.20    --  -91.75 -66.00 -56.44   76
 82  \w   -110.00 -73.00   0.50    0.20    --  -91.75 -66.00 -56.44   74
 83  \w   -101.00 -76.00   0.50    0.20    --  -91.75 -64.00 -40.25   50
 84  \w    -99.00 -74.00   0.50    0.20    --  -91.75 -68.00-149.01   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  0.0515
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38779
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.457
_diffrn_reflns_theta_min         3.342
_exptl_absorpt_coefficient_mu    22.775
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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            'dark pink'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.892
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00093(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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5998
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0442P)^2^+6.3231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5676
_reflns_number_total             5998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03280a2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7061007--7061013.cif.'
_cod_database_code               7061011
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.463
_shelx_estimated_absorpt_t_min   0.113
_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
 H5WA-O21
 1.52 with sigma of 0.2
 O5W-H3WA
 1.931 with sigma of 0.02
 O17-H4WB
 2.582 with sigma of 0.02
3.a Free rotating group:
 O1W(H1WA,H1WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
3.b Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), N8(H8A,H8B,H8C), N5(H5A,H5B,H5C), N6(H6A,H6B,H6C), N2(H2A,
 H2B,H2C), N7(H7A,H7B,H7C), N3(H3A,H3B,H3C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              1170
_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
;