Extending the structural landscape of Mo(vi) hydrazonato inorganic–organic POM-hybrids: an experimental and computational study
Bebić, Nikol; Topić, Edi; Mandarić, Mirna; Hrenar, Tomica; Vrdoljak, Višnja; CrystEngComm 23 (2021) 6349–6358; doi:10.1039/D1CE00861G

data_7243293
_publ_section_title
;
 Extending the structural landscape of Mo(vi) hydrazonato
 inorganic--organic POM-hybrids: an experimental and computational study
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              6349
_journal_page_last               6358
_journal_paper_doi               10.1039/D1CE00861G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'Mo8 O26, 2(C14 H15 Mo N3 O6), 2(C2 H3 N), 3(H2 O)'
_chemical_formula_sum            'C32 H42 Mo10 N8 O41'
_chemical_formula_weight         2154.13
_chemical_name_systematic
'[N-(2-oxo-4-methoxybenzylidene)isonicotinoylhydrazonato](aqua)dioxomolybdenum(vi) octamolybdate acetonitrile solvate hydrate'
_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             2021-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                107.1590(10)
_cell_angle_beta                 102.4120(10)
_cell_angle_gamma                105.877(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5703(2)
_cell_length_b                   11.3121(2)
_cell_length_c                   14.2003(2)
_cell_measurement_reflns_used    27176
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      79.3330
_cell_measurement_theta_min      3.4250
_cell_volume                     1477.54(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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   -119.00 -70.00   0.50    0.16    --  -48.02-164.00 104.00   98
  2  \w    -80.00  -8.00   0.50    0.16    --  -48.02 117.00 -19.00  144
  3  \w     29.00  92.00   0.50    0.16    --   48.02-117.00-106.00  126
  4  \w     87.00 116.00   0.50    0.16    --   48.02 164.00 129.00   58
  5  \w     88.00 119.00   0.50    0.16    --   48.02-164.00 104.00   62
  6  \w    -93.00 -68.00   0.50    0.65    --  -91.75-164.00 104.00   50
  7  \w    -75.00 -50.00   0.50    0.65    --  -91.75 117.00 -19.00   50
  8  \w   -145.00-120.00   0.50    0.65    --  -91.75-117.00-106.00   50
  9  \w    100.00 137.00   0.50    0.65    --  113.25-164.00 104.00   74
 10  \w     52.00  78.00   0.50    0.65    --  113.25-117.00-106.00   52
 11  \w     90.00 116.00   0.50    0.65    --  113.25 164.00 129.00   52
 12  \w    125.00 150.00   0.50    0.65    --  113.25 117.00 -19.00   50
 13  \w     81.00 109.00   0.50    0.65    --  113.25-117.00-106.00   56
 14  \w    -87.00 -33.00   0.50    0.16    --  -48.02 -57.00   0.00  108
 15  \w   -118.00 -91.00   0.50    0.16    --  -48.02 -57.00 -60.00   54
 16  \w   -117.00 -37.00   0.50    0.16    --  -48.02 -19.00-180.00  160
 17  \w    -82.00 -33.00   0.50    0.16    --  -48.02 -57.00 -60.00   98
 18  \w    -51.00 -25.00   0.50    0.16    --  -48.02 -77.00-120.00   52
 19  \w   -103.00 -35.00   0.50    0.16    --  -48.02 -38.00 150.00  136
 20  \w   -107.00 -82.00   0.50    0.16    --  -48.02 -77.00-120.00   50
 21  \w    -54.00 -26.00   0.50    0.16    --  -48.02 -77.00  90.00   56
 22  \w    -69.00 -36.00   0.50    0.16    --  -48.02 -38.00  60.00   66
 23  \w    -85.00 -60.00   0.50    0.16    --  -48.02 -77.00 120.00   50
 24  \w    -97.00 -72.00   0.50    0.16    --  -48.02 164.00 129.00   50
 25  \w    -51.00 -25.00   0.50    0.16    --  -48.02 -77.00 120.00   52
 26  \w    -63.00 -25.00   0.50    0.16    --  -48.02 -77.00  30.00   76
 27  \w   -118.00 -37.00   0.50    0.16    --  -48.02 -43.00  47.35  162
 28  \w   -118.00 -93.00   0.50    0.16    --  -48.02 -57.00   0.00   50
 29  \w   -112.00 -86.00   0.50    0.16    --  -48.02 -77.00  90.00   52
 30  \w    -75.00 -26.00   0.50    0.16    --  -48.02 -77.00-180.00   98
 31  \w    -60.00 -25.00   0.50    0.16    --  -48.02 -77.00 -30.00   70
 32  \w   -112.00 -79.00   0.50    0.16    --  -48.02 -77.00 -30.00   66
 33  \w     27.00  54.00   0.50    0.16    --   48.02  77.00 -60.00   54
 34  \w     25.00  72.00   0.50    0.16    --   48.02  77.00-120.00   94
 35  \w    -96.00 -71.00   0.50    0.65    --  -91.75 -72.00  40.76   50
 36  \w    -95.00 -69.00   0.50    0.65    --  -91.75 -76.00-143.60   52
 37  \w   -113.00 -76.00   0.50    0.65    --  -91.75 -61.00 114.47   74
 38  \w    -97.00 -71.00   0.50    0.65    --  -91.75 -72.00  68.10   52
 39  \w    -99.00 -71.00   0.50    0.65    --  -91.75 -74.00 -18.69   56
 40  \w    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00  60.00   52
 41  \w   -161.00-135.00   0.50    0.65    --  -91.75 -72.00  40.76   52
 42  \w   -136.00-110.00   0.50    0.65    --  -91.75 -72.00  68.10   52
 43  \w    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00  90.00   52
 44  \w    -99.00 -69.00   0.50    0.65    --  -91.75 -77.00  30.00   60
 45  \w   -149.00-123.00   0.50    0.65    --  -91.75 -76.00-143.60   52
 46  \w    -99.00 -73.00   0.50    0.65    --  -91.75 -68.00-176.64   52
 47  \w   -110.00 -73.00   0.50    0.65    --  -91.75 -68.00 146.56   74
 48  \w    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00 -49.38   52
 49  \w   -158.00-117.00   0.50    0.65    --  -91.75 -71.00 160.68   82
 50  \w    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00   0.00   52
 51  \w   -101.00 -69.00   0.50    0.65    --  -91.75 -76.00 104.29   64
 52  \w   -100.00 -72.00   0.50    0.65    --  -91.75 -69.00 -84.60   56
 53  \w    -97.00 -71.00   0.50    0.65    --  -91.75 -72.00  73.72   52
 54  \w   -100.00 -74.00   0.50    0.65    --  -91.75 -67.00-122.90   52
 55  \w    -96.00 -71.00   0.50    0.65    --  -91.75 -71.00 160.68   50
 56  \w   -152.00-125.00   0.50    0.65    --  -91.75 -64.00 -44.04   54
 57  \w    -94.00 -69.00   0.50    0.65    --  -91.75 -76.00-128.85   50
 58  \w    -96.00 -70.00   0.50    0.65    --  -91.75 -77.00-150.00   52
 59  \w    -94.00 -69.00   0.50    0.65    --  -91.75 -77.00 120.00   50
 60  \w    -95.00 -70.00   0.50    0.65    --  -91.75 -74.00-175.37   50
 61  \w    -95.00 -69.00   0.50    0.65    --  -91.75 -77.00 -60.00   52
 62  \w   -113.00 -69.00   0.50    0.65    --  -91.75 -77.00 -90.00   88
 63  \w    -94.00 -69.00   0.50    0.65    --  -91.75 -77.00 150.00   50
 64  \w   -100.00 -74.00   0.50    0.65    --  -91.75 -69.00-112.01   52
 65  \w    -94.00 -69.00   0.50    0.65    --  -91.75 -76.00  10.80   50
 66  \w   -100.00 -74.00   0.50    0.65    --  -91.75 -64.00 -44.04   52
 67  \w    -99.00 -73.00   0.50    0.65    --  -91.75 -66.00 -53.02   52
 68  \w     43.00  70.00   0.50    0.65    --  113.25 -95.00 -30.00   54
 69  \w     91.00 176.00   0.50    0.65    --  113.25  77.00 -60.00  170
 70  \w     82.00 107.00   0.50    0.65    --  113.25-109.00 -49.41   50
 71  \w     99.00 177.00   0.50    0.65    --  113.25  61.00-150.00  156
 72  \w     42.00  77.00   0.50    0.65    --  113.25-109.00 -49.41   70
 73  \w    135.00 178.00   0.50    0.65    --  113.25  15.00-180.00   86
 74  \w     93.00 127.00   0.50    0.65    --  113.25  77.00  30.00   68
 75  \w    131.00 156.00   0.50    0.65    --  113.25  77.00  30.00   50
 76  \w    100.00 128.00   0.50    0.65    --  113.25  15.00-180.00   56
 77  \w     43.00 106.00   0.50    0.65    --  113.25 -95.00 150.00  126
 78  \w     42.00  77.00   0.50    0.65    --  113.25 -95.00   0.00   70
 79  \w    136.00 175.00   0.50    0.65    --  113.25  77.00 -90.00   78
 80  \w     92.00 128.00   0.50    0.65    --  113.25  77.00 -90.00   72
 81  \w     98.00 161.00   0.50    0.65    --  113.25 125.00-150.00  126
 82  \w     93.00 151.00   0.50    0.65    --  113.25  77.00 150.00  116
 83  \w     43.00  68.00   0.50    0.65    --  113.25 -77.00 120.00   50
 84  \w     97.00 138.00   0.50    0.65    --  113.25  61.00 -90.00   82
 85  \w     42.00  67.00   0.50    0.65    --  113.25 -61.00  90.00   50
 86  \w     95.00 172.00   0.50    0.65    --  113.25  67.00 -31.14  154
 87  \w     76.00 111.00   0.50    0.65    --  113.25-125.00-180.00   70
 88  \w     91.00 178.00   0.50    0.65    --  113.25  77.00-180.00  174
 89  \w    140.00 178.00   0.50    0.65    --  113.25  77.00 120.00   76
 90  \w     78.00 106.00   0.50    0.65    --  113.25 -95.00  30.00   56
 91  \w     42.00  71.00   0.50    0.65    --  113.25 -95.00  30.00   58
 92  \w     86.00 111.00   0.50    0.65    --  113.25-125.00 -30.00   50
 93  \w     42.00 106.00   0.50    0.65    --  113.25-125.00-120.00  128
 94  \w     43.00  77.00   0.50    0.65    --  113.25-125.00 -30.00   68
 95  \w    146.00 172.00   0.50    0.65    --  113.25  77.00  90.00   52
 96  \w     91.00 117.00   0.50    0.65    --  113.25  77.00 120.00   52
 97  \w     74.00 100.00   0.50    0.65    --  113.25 -95.00  60.00   52
 98  \w    106.00 138.00   0.50    0.65    --  113.25  45.00 -90.00   64
 99  \w    147.00 173.00   0.50    0.65    --  113.25  45.00 -90.00   52
100  \w     91.00 142.00   0.50    0.65    --  113.25  77.00  90.00  102
101  \w     91.00 152.00   0.50    0.65    --  113.25  77.00  60.00  122
102  \w     48.00  93.00   0.50    0.65    --  113.25 -95.00 -90.00   90
103  \w     93.00 150.00   0.50    0.65    --  113.25  77.00 -30.00  114
104  \w    152.00 177.00   0.50    0.65    --  113.25  61.00 150.00   50
105  \w     99.00 125.00   0.50    0.65    --  113.25  61.00 150.00   52
106  \w    104.00 162.00   0.50    0.65    --  113.25 125.00  90.00  116
107  \w     99.00 178.00   0.50    0.65    --  113.25  61.00   0.00  158
108  \w    100.00 158.00   0.50    0.65    --  113.25  61.00  30.00  116
109  \w     46.00  71.00   0.50    0.65    --  113.25 -61.00-150.00   50
110  \w     43.00  89.00   0.50    0.65    --  113.25-125.00 -60.00   92
111  \w     42.00  71.00   0.50    0.65    --  113.25 -61.00-180.00   58
112  \w     92.00 115.00   0.50    0.65    --  113.25  77.00   0.00   46
;
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40227
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.134
_diffrn_reflns_theta_min         3.440
_exptl_absorpt_coefficient_mu    17.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38682
_exptl_absorpt_correction_type   multi-scan
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_description       block
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.00039(4)
_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   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+4.0660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5812
_reflns_number_total             6253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_449_auto
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_database_code               7243293
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.330
_shelx_estimated_absorpt_t_min   0.176
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H3-N3
 0.86 with sigma of 0.02
 H20B-O20
 0.82 with sigma of 0.02
3. Others
 Fixed Sof: O21(0.5) H21A(0.5) H21B(0.5)
4.a Free rotating group:
 O20(H20A), O21(H21A,H21B)
4.b Rotating group:
 O5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3A), C5(H5), C6(H6), C7(H7), C13(H13), C10(H10), C11(H11), C12(H12)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              19273
_shelx_hkl_checksum              67173
_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
;