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_7243287
_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, 4(C13 H12 Mo N3 O6), 10(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C56 H74 Mo12 N14 O60'
_chemical_formula_weight         3054.57
_chemical_name_systematic
'bis((aquo)-dioxo-(N-(2-oxy-4-hydroxybenzylidene)isonicotinylhydrazonium)-molybdenum(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             2021-05-28
_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                116.276(3)
_cell_angle_beta                 95.232(3)
_cell_angle_gamma                93.035(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4085(4)
_cell_length_b                   16.2433(5)
_cell_length_c                   17.3878(4)
_cell_measurement_reflns_used    23681
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.7510
_cell_measurement_theta_min      3.0260
_cell_volume                     2359.80(15)
_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 0.972
_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     28.00 121.00   0.50    0.10    --   47.77  72.00-138.00  186
  2  \w    116.00 178.00   0.50    0.15    --  113.25  72.00-138.00  124
  3  \w    101.00 178.00   0.50    0.15    --  113.25  45.00-150.00  154
  4  \w    101.00 173.00   0.50    0.15    --  113.25  45.00 -90.00  144
  5  \w    143.00 178.00   0.50    0.15    --  113.25  30.00-180.00   70
  6  \w    104.00 174.00   0.50    0.15    --  113.25  45.00 -60.00  140
  7  \w    101.00 135.00   0.50    0.15    --  113.25  30.00   0.00   68
  8  \w    139.00 178.00   0.50    0.15    --  113.25  30.00  60.00   78
  9  \w    130.00 165.00   0.50    0.15    --  113.25  45.00  90.00   70
 10  \w    103.00 128.00   0.50    0.15    --  113.25  30.00  60.00   50
 11  \w    100.00 175.00   0.50    0.15    --  113.25  15.00 150.00  150
 12  \w    118.00 172.00   0.50    0.15    --  113.25  15.00  30.00  108
 13  \w    142.00 168.00   0.50    0.15    --  113.25  30.00   0.00   52
 14  \w    101.00 126.00   0.50    0.15    --  113.25  30.00-180.00   50
 15  \w    -68.00 -25.00   0.50    0.10    --  -47.77  72.00-138.00   86
 16  \w    -79.00 -54.00   0.50    0.15    --  -91.75  72.00-138.00   50
 17  \w    -16.00  11.00   0.50    0.10    --  -47.77  72.00-138.00   54
 18  \w    -50.00 -20.00   0.50    0.15    --  -91.75  45.00   0.00   60
 19  \w    -51.00 -20.00   0.50    0.15    --  -91.75  45.00  30.00   62
 20  \w     88.00 130.00   0.50    0.15    --  113.25-151.00-132.23   84
 21  \w     36.00  81.00   0.50    0.10    --   47.77-125.00 -60.00   90
 22  \w     76.00 101.00   0.50    0.15    --  113.25-125.00  30.00   50
 23  \w     42.00  68.00   0.50    0.15    --  113.25-125.00  30.00   52
 24  \w     72.00  98.00   0.50    0.15    --  113.25-125.00 -30.00   52
 25  \w     43.00  81.00   0.50    0.15    --  113.25-125.00 -60.00   76
 26  \w     52.00 110.00   0.50    0.15    --  113.25-125.00-120.00  116
 27  \w     51.00 106.00   0.50    0.15    --  113.25-108.00 -64.43  110
 28  \w     55.00 122.00   0.50    0.15    --  113.25-139.00   9.82  134
 29  \w     85.00 111.00   0.50    0.15    --  113.25-125.00  60.00   52
 30  \w     86.00 111.00   0.50    0.15    --  113.25-125.00 150.00   50
 31  \w     48.00 111.00   0.50    0.15    --  113.25-125.00 120.00  126
 32  \w     46.00  72.00   0.50    0.15    --  113.25 -95.00  60.00   52
 33  \w     76.00 102.00   0.50    0.15    --  113.25 -95.00  90.00   52
 34  \w     47.00  85.00   0.50    0.15    --  113.25 -95.00   0.00   76
 35  \w     78.00 106.00   0.50    0.15    --  113.25 -95.00  30.00   56
 36  \w     43.00 106.00   0.50    0.15    --  113.25 -95.00 150.00  126
 37  \w     43.00  75.00   0.50    0.15    --  113.25 -95.00  30.00   64
 38  \w     47.00 108.00   0.50    0.15    --  113.25-108.00-115.90  122
 39  \w     64.00 103.00   0.50    0.15    --  113.25 -95.00 -30.00   78
 40  \w     69.00 106.00   0.50    0.15    --  113.25 -95.00-150.00   74
 41  \w     81.00 106.00   0.50    0.15    --  113.25 -95.00-180.00   50
 42  \w     46.00  76.00   0.50    0.15    --  113.25 -95.00-180.00   60
 43  \w     68.00  94.00   0.50    0.15    --  113.25 -77.00-150.00   52
 44  \w     42.00  67.00   0.50    0.15    --  113.25 -61.00-150.00   50
 45  \w     45.00  71.00   0.50    0.15    --  113.25 -61.00  30.00   52
 46  \w     42.00  93.00   0.50    0.15    --  113.25 -77.00  90.00  102
 47  \w     42.00  67.00   0.50    0.15    --  113.25 -72.00  91.00   50
 48  \w     44.00  70.00   0.50    0.15    --  113.25 -61.00  90.00   52
 49  \w     11.00  65.00   0.50    0.10    --   47.77 -72.00  91.00  108
 50  \w     44.00  70.00   0.50    0.15    --  113.25 -61.00 -30.00   52
 51  \w     46.00  71.00   0.50    0.15    --  113.25 -61.00 -90.00   50
 52  \w     96.00 128.00   0.50    0.15    --  113.25 125.00-180.00   64
 53  \w    140.00 165.00   0.50    0.15    --  113.25 125.00-180.00   50
 54  \w     97.00 168.00   0.50    0.15    --  113.25 125.00 -60.00  142
 55  \w    -68.00 -14.00   0.50    0.10    --  -47.77 125.00 120.00  108
 56  \w    -77.00 -18.00   0.50    0.10    --  -47.77 125.00   0.00  118
 57  \w   -118.00 -28.00   0.50    0.10    --  -47.77 -72.00  91.00  180
 58  \w   -141.00-115.00   0.50    0.15    --  -91.75 -72.00  91.00   52
 59  \w   -102.00 -73.00   0.50    0.10    --  -47.77-125.00-120.00   58
 60  \w   -115.00 -89.00   0.50    0.10    --  -47.77-125.00-150.00   52
;
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37525
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.466
_diffrn_reflns_theta_min         2.858
_exptl_absorpt_coefficient_mu    13.601
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.114
_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    2.149
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.290
_refine_diff_density_min         -1.719
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.00031(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   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0764P)^2^+17.1814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9372
_reflns_number_total             10049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_947_auto
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_database_code               7243287
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.091
_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. Uiso/Uaniso restraints and constraints
Uanis(O11) = Uanis(Mo3)
3.a Free rotating group:
 O24(H24A,H24B), O20(H20A,H20B), O23(H23A,H23B), O22(H22A,H22B), O21(H21A,H21B)
3.b Rotating group:
 O5A(H5AA,H5AB), O5(H5A,H5B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N3A(H3AA), C6(H6A), C3A(H3AB), C10(H10), C13(H13), C5(H5), C12(H12),
 C11(H11), C6A(H6AB), C7(H7), C7A(H7A), C5A(H5AC), C10A(H10A), C3(H3A),
 C11A(H11A), C13A(H13A), C12A(H12A)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
3.e Idealised tetrahedral OH refined as rotating group:
 O6A(H6AA), O6(H6)
;
_shelx_res_checksum              35430
_shelx_hkl_checksum              97239
_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
;