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_7243294
_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         'Mo6 O19, 2(C15 H13 Mo N4 O5), 2(C2 H3 N)'
_chemical_formula_sum            'C34 H32 Mo8 N10 O29'
_chemical_formula_weight         1812.21
_chemical_name_systematic
'[N'-(2-oxo-4-hydroxybenzylidene)isonicotinoylhydrazonato](acetonitrile)dioxomolybdenum(vi) hexamolybdate acetonitrile solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-20 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.920(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0479(4)
_cell_length_b                   8.6686(2)
_cell_length_c                   29.2039(5)
_cell_measurement_reflns_used    21240
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      78.9310
_cell_measurement_theta_min      3.0440
_cell_volume                     5300.00(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.989
_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     26.00  53.00   0.50    0.05    --   47.77  77.00  90.00   54
  2  \w     96.00 174.00   0.50    0.10    --  113.25  77.00 150.00  156
  3  \w     92.00 149.00   0.50    0.10    --  113.25  77.00  30.00  114
  4  \w     95.00 120.00   0.50    0.10    --  113.25  77.00 -60.00   50
  5  \w    123.00 172.00   0.50    0.10    --  113.25  77.00-150.00   98
  6  \w     91.00 118.00   0.50    0.10    --  113.25  77.00-150.00   54
  7  \w     92.00 162.00   0.50    0.10    --  113.25  77.00 -90.00  140
  8  \w    136.00 178.00   0.50    0.10    --  113.25  77.00 -60.00   84
  9  \w    120.00 175.00   0.50    0.10    --  113.25  77.00-180.00  110
 10  \w    136.00 178.00   0.50    0.10    --  113.25  77.00   0.00   84
 11  \w     91.00 131.00   0.50    0.10    --  113.25  77.00   0.00   80
 12  \w     99.00 176.00   0.50    0.10    --  113.25  77.00 120.00  154
 13  \w     92.00 175.00   0.50    0.10    --  113.25  77.00  90.00  166
 14  \w     96.00 142.00   0.50    0.10    --  113.25  77.00  60.00   92
 15  \w     91.00 125.00   0.50    0.10    --  113.25  77.00 -30.00   68
 16  \w    129.00 170.00   0.50    0.10    --  113.25  77.00 -30.00   82
 17  \w     99.00 151.00   0.50    0.10    --  113.25  61.00 120.00  104
 18  \w     96.00 170.00   0.50    0.10    --  113.25  77.00-120.00  148
 19  \w     98.00 162.00   0.50    0.10    --  113.25  61.00-150.00  128
 20  \w     91.00 117.00   0.50    0.10    --  113.25  77.00-180.00   52
 21  \w    103.00 129.00   0.50    0.10    --  113.25  61.00-180.00   52
 22  \w     99.00 159.00   0.50    0.10    --  113.25  61.00 -90.00  120
 23  \w     99.00 154.00   0.50    0.10    --  113.25  61.00-120.00  110
 24  \w     98.00 152.00   0.50    0.10    --  113.25  61.00   0.00  108
 25  \w     98.00 170.00   0.50    0.10    --  113.25  61.00  30.00  144
 26  \w    152.00 178.00   0.50    0.10    --  113.25  61.00  60.00   52
 27  \w     97.00 140.00   0.50    0.10    --  113.25  61.00  90.00   86
 28  \w     98.00 135.00   0.50    0.10    --  113.25  61.00  60.00   74
 29  \w     97.00 158.00   0.50    0.10    --  113.25  61.00 -30.00  122
 30  \w    140.00 178.00   0.50    0.10    --  113.25  15.00-180.00   76
 31  \w    -83.00 -14.00   0.50    0.05    --  -47.77 125.00-120.00  138
 32  \w    -74.00 -49.00   0.50    0.10    --  -91.75  93.00 -75.00   50
 33  \w    -76.00 -28.00   0.50    0.05    --  -47.77  93.00 -75.00   96
 34  \w     42.00 111.00   0.50    0.10    --  113.25-125.00 150.00  138
 35  \w     51.00  91.00   0.50    0.10    --  113.25-145.00  45.02   80
 36  \w     47.00  88.00   0.50    0.05    --   47.77-125.00 -90.00   82
 37  \w     69.00 111.00   0.50    0.10    --  113.25-125.00 -90.00   84
 38  \w     52.00 111.00   0.50    0.10    --  113.25-125.00-120.00  118
 39  \w     59.00 111.00   0.50    0.10    --  113.25-125.00-180.00  104
 40  \w     43.00  69.00   0.50    0.10    --  113.25-112.00-115.17   52
 41  \w     74.00 108.00   0.50    0.10    --  113.25-112.00-115.17   68
 42  \w     82.00 107.00   0.50    0.10    --  113.25-107.00 -39.75   50
 43  \w     75.00 106.00   0.50    0.10    --  113.25-106.00  27.75   62
 44  \w     43.00  72.00   0.50    0.10    --  113.25-106.00  27.75   58
 45  \w     65.00 108.00   0.50    0.10    --  113.25-112.00  80.53   86
 46  \w     44.00 106.00   0.50    0.10    --  113.25-110.00 103.09  124
 47  \w     61.00  88.00   0.50    0.10    --  113.25 -93.00 172.00   54
 48  \w      7.00  77.00   0.50    0.05    --   47.77 -93.00 172.00  140
 49  \w     55.00 103.00   0.50    0.10    --  113.25 -95.00 -30.00   96
 50  \w     42.00 103.00   0.50    0.10    --  113.25 -95.00 -90.00  122
 51  \w     44.00  71.00   0.50    0.10    --  113.25 -61.00-120.00   54
 52  \w     56.00  99.00   0.50    0.10    --  113.25 -77.00   0.00   86
 53  \w     43.00  76.00   0.50    0.10    --  113.25 -77.00  30.00   66
 54  \w     45.00  70.00   0.50    0.10    --  113.25 -61.00  60.00   50
 55  \w     42.00  90.00   0.50    0.10    --  113.25 -77.00 120.00   96
 56  \w    113.00 173.00   0.50    0.10    --  113.25  93.00 -75.00  120
 57  \w    153.00 178.00   0.50    0.10    --  113.25 125.00  30.00   50
 58  \w    113.00 178.00   0.50    0.10    --  113.25 125.00  60.00  130
 59  \w    106.00 134.00   0.50    0.10    --  113.25 125.00  30.00   56
 60  \w   -120.00 -36.00   0.50    0.05    --  -47.77 -19.00 -90.00  168
 61  \w   -119.00 -94.00   0.50    0.05    --  -47.77 -77.00-120.00   50
 62  \w   -116.00 -90.00   0.50    0.05    --  -47.77 -77.00   0.00   52
 63  \w    -92.00 -60.00   0.50    0.05    --  -47.77 -77.00 120.00   64
 64  \w    -64.00 -25.00   0.50    0.05    --  -47.77 -77.00 150.00   78
 65  \w    -57.00 -26.00   0.50    0.05    --  -47.77 -77.00 120.00   62
 66  \w    -83.00 -28.00   0.50    0.05    --  -47.77 -77.00  60.00  110
;
_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  0.0729
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49371
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.359
_diffrn_reflns_theta_min         3.043
_exptl_absorpt_coefficient_mu    15.881
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.173
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       plate
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.885
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.000026(6)
_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   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5738
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0607P)^2^+48.4649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5378
_reflns_number_total             5738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_1373_auto
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_original_cell_volume        5300.01(18)
_cod_database_code               7243294
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.386
_shelx_estimated_absorpt_t_min   0.138
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3
 0.86 with sigma of 0.02
 O5-H5
 0.82 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3A), C11(H11), C5(H5A), C7(H7), C13(H13), C12(H12), C6(H6)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              21942
_shelx_hkl_checksum              46069
_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
;