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_7061008
_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         'Co2 H21 Mo5 N7 O18, 5(H2O)'
_chemical_formula_sum            'Co2 H31 Mo5 N7 O23'
_chemical_formula_weight         1094.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-09
_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                90
_cell_angle_beta                 102.988(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3392(4)
_cell_length_b                   28.0114(9)
_cell_length_c                   9.6973(4)
_cell_measurement_reflns_used    13062
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      75.7170
_cell_measurement_theta_min      3.1570
_cell_volume                     2471.95(17)
_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_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 0.9996
_diffrn_measured_fraction_theta_max 0.9519
_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   -113.00 -37.00   0.50    0.44    --  -47.77 -38.00-120.00  152
  2  \w   -103.00 -77.00   0.50    0.44    --  -47.77-125.00-120.00   52
  3  \w    -62.00  18.00   0.50    0.44    --  -47.77  57.00  30.00  160
  4  \w    -16.00  28.00   0.50    0.44    --  -47.77  19.00  60.00   88
  5  \w    -35.00  10.00   0.50    0.44    --  -47.77  38.00   0.00   90
  6  \w     -1.00  72.00   0.50    0.44    --   47.77 -99.00-120.00  146
  7  \w    -66.00 -41.00   0.50    1.75    --  -91.75  57.00-150.00   50
  8  \w   -163.00-119.00   0.50    1.75    --  -91.75 -57.00-120.00   88
  9  \w   -114.00 -88.00   0.50    1.75    --  -91.75 -57.00-120.00   52
 10  \w   -140.00 -88.00   0.50    1.75    --  -91.75 -99.00 -90.00  104
 11  \w    -83.00 -25.00   0.50    1.75    --  -91.75  77.00 120.00  116
 12  \w   -161.00 -89.00   0.50    1.75    --  -91.75 -38.00 -30.00  144
 13  \w    -52.00 -22.00   0.50    1.75    --  -91.75  57.00  60.00   60
 14  \w    -85.00 -56.00   0.50    1.75    --  -91.75 125.00 150.00   58
 15  \w   -164.00 -78.00   0.50    1.75    --  -91.75 -38.00 -90.00  172
 16  \w    -52.00 -26.00   0.50    1.75    --  -91.75 125.00 150.00   52
 17  \w    -59.00 -33.00   0.50    1.75    --  -91.75  57.00-180.00   52
 18  \w    -80.00 -34.00   0.50    1.75    --  -91.75 125.00 -30.00   92
 19  \w     39.00 103.00   0.50    1.75    --  107.54 -77.00-150.00  128
 20  \w     97.00 170.00   0.50    1.75    --  107.54  38.00 150.00  146
 21  \w     44.00  93.00   0.50    1.75    --  107.54 -99.00 -30.00   98
 22  \w     35.00  61.00   0.50    1.75    --  107.54 -57.00  30.00   52
 23  \w     39.00  64.00   0.50    1.75    --  107.54 -57.00  60.00   50
 24  \w     36.00  67.00   0.50    1.75    --  107.54 -99.00  60.00   62
 25  \w     71.00 103.00   0.50    1.75    --  107.54 -99.00  60.00   64
 26  \w     71.00 106.00   0.50    1.75    --  107.54-125.00-120.00   70
 27  \w     35.00  68.00   0.50    1.75    --  107.54-125.00-120.00   66
 28  \w    131.00 161.00   0.50    1.75    --  107.54  38.00  90.00   60
 29  \w    103.00 128.00   0.50    1.75    --  107.54  38.00  90.00   50
 30  \w     44.00 111.00   0.50    1.75    --  107.54-125.00  60.00  134
 31  \w     36.00  66.00   0.50    1.75    --  107.54 -57.00 -90.00   60
 32  \w     53.00 110.00   0.50    1.75    --  107.54-125.00-180.00  114
 33  \w     83.00 111.00   0.50    1.75    --  107.54-125.00  30.00   56
 34  \w     85.00 111.00   0.50    1.75    --  107.54-125.00 150.00   52
 35  \w     44.00  69.00   0.50    1.75    --  107.54-125.00  30.00   50
 36  \w     81.00 106.00   0.50    1.75    --  107.54 -99.00-150.00   50
 37  \w     46.00  71.00   0.50    1.75    --  107.54-125.00 150.00   50
 38  \w     81.00 108.00   0.50    1.75    --  107.54-107.00 -71.57   54
 39  \w     37.00  63.00   0.50    1.75    --  107.54-107.00 -71.57   52
;
_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      -0.0908574000
_diffrn_orient_matrix_UB_12      -0.0435584000
_diffrn_orient_matrix_UB_13      -0.0656970000
_diffrn_orient_matrix_UB_21      0.1262367000
_diffrn_orient_matrix_UB_22      -0.0333630000
_diffrn_orient_matrix_UB_23      0.0713722000
_diffrn_orient_matrix_UB_31      -0.0667642000
_diffrn_orient_matrix_UB_32      -0.0037512000
_diffrn_orient_matrix_UB_33      0.1311224000
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26766
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.236
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    31.395
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_correction_T_min  0.234
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.915
_exptl_crystal_description       plate
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.460
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.250
_refine_ls_extinction_coef       0.000100(19)
_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   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0399P)^2^+73.8004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4599
_reflns_number_total             5035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03280a2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7061007--7061013.cif.'
_cod_database_code               7061008
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.453
_shelx_estimated_absorpt_t_min   0.188
_diffrn_oxdiff_digest_frames
;
0186be8b2d6b83f011a49211b016c06f9f00034b11d
;
_diffrn_oxdiff_digest_hkl
;
019bd7cae1eb806cabb73e1134bc2bdc465b83
;
_reflns_odcompleteness_completeness 99.96
_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
2.a Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N7(H7A,
 H7B,H7C), N6(H6A,H6B,H6C), N5(H5A,H5B,H5C)
;
_shelx_res_checksum              58450
_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 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.180