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_7243291
_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), 4(H2 O), 1.5(C4 H6 N2)'
_chemical_formula_sum            'C34 H47 Mo10 N9 O42'
_chemical_formula_weight         2213.20
_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 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2021-07-15 deposited with the CCDC.	2021-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                100.3730(10)
_cell_angle_beta                 104.041(2)
_cell_angle_gamma                106.410(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2611(2)
_cell_length_b                   10.5249(2)
_cell_length_c                   15.9967(2)
_cell_measurement_reflns_used    28564
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.6620
_cell_measurement_theta_min      4.5340
_cell_volume                     1549.28(6)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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 0.999
_diffrn_measured_fraction_theta_max 0.973
_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     91.00 130.00   0.50    0.25    --  113.25  77.00 120.00   78
  2  \w    133.00 178.00   0.50    0.25    --  113.25  77.00 120.00   90
  3  \w     93.00 172.00   0.50    0.25    --  113.25  77.00 150.00  158
  4  \w    100.00 175.00   0.50    0.25    --  113.25  77.00  60.00  150
  5  \w     94.00 155.00   0.50    0.25    --  113.25  77.00  30.00  122
  6  \w    148.00 178.00   0.50    0.25    --  113.25  77.00 -90.00   60
  7  \w    136.00 177.00   0.50    0.25    --  113.25  77.00-120.00   82
  8  \w     91.00 136.00   0.50    0.25    --  113.25  77.00-180.00   90
  9  \w     91.00 130.00   0.50    0.25    --  113.25  77.00-120.00   78
 10  \w     94.00 139.00   0.50    0.25    --  113.25  77.00 -90.00   90
 11  \w    104.00 175.00   0.50    0.25    --  113.25  77.00-150.00  142
 12  \w    100.00 135.00   0.50    0.25    --  113.25  61.00 -30.00   70
 13  \w     91.00 173.00   0.50    0.25    --  113.25  77.00  90.00  164
 14  \w     94.00 169.00   0.50    0.25    --  113.25  77.00 -30.00  150
 15  \w    102.00 149.00   0.50    0.25    --  113.25  61.00  90.00   94
 16  \w     91.00 156.00   0.50    0.25    --  113.25  77.00 -60.00  130
 17  \w    115.00 177.00   0.50    0.25    --  113.25  61.00 -60.00  124
 18  \w    100.00 162.00   0.50    0.25    --  113.25  61.00 -90.00  124
 19  \w     98.00 171.00   0.50    0.25    --  113.25  61.00-120.00  146
 20  \w     99.00 176.00   0.50    0.25    --  113.25  61.00-180.00  154
 21  \w     97.00 150.00   0.50    0.25    --  113.25  61.00-150.00  106
 22  \w    108.00 155.00   0.50    0.25    --  113.25  61.00   0.00   94
 23  \w    127.00 167.00   0.50    0.25    --  113.25  30.00  30.00   80
 24  \w    100.00 156.00   0.50    0.25    --  113.25  61.00  60.00  112
 25  \w    107.00 176.00   0.50    0.25    --  113.25  51.00 131.00  138
 26  \w     99.00 125.00   0.50    0.25    --  113.25  61.00 150.00   52
 27  \w     34.00  67.00   0.50    0.06    --   48.02  51.00 131.00   66
 28  \w   -120.00 -79.00   0.50    0.06    --  -48.02 -77.00  30.00   82
 29  \w    -57.00 -25.00   0.50    0.06    --  -48.02 -77.00 -90.00   64
 30  \w    -54.00 -25.00   0.50    0.06    --  -48.02 -77.00 -30.00   58
 31  \w    -56.00 -25.00   0.50    0.06    --  -48.02 -77.00-150.00   62
 32  \w    -95.00 -25.00   0.50    0.06    --  -48.02 -77.00-180.00  140
 33  \w   -113.00 -87.00   0.50    0.06    --  -48.02 -77.00-150.00   52
 34  \w   -108.00 -82.00   0.50    0.06    --  -48.02 -77.00 -90.00   52
 35  \w    -61.00 -33.00   0.50    0.06    --  -48.02 -57.00 -60.00   56
 36  \w    -64.00 -26.00   0.50    0.06    --  -48.02 -77.00  30.00   76
 37  \w    -53.00 -25.00   0.50    0.06    --  -48.02 -77.00  90.00   56
 38  \w    -56.00 -25.00   0.50    0.06    --  -48.02 -77.00 120.00   62
 39  \w    -89.00 -63.00   0.50    0.06    --  -48.02 -77.00 120.00   52
 40  \w    -80.00 -34.00   0.50    0.06    --  -48.02 -51.00 -14.00   92
 41  \w    -92.00 -36.00   0.50    0.06    --  -48.02 -38.00  30.00  112
 42  \w   -119.00 -37.00   0.50    0.06    --  -48.02 -38.00  90.00  164
 43  \w   -119.00 -93.00   0.50    0.06    --  -48.02 -51.00 -14.00   52
 44  \w   -118.00 -68.00   0.50    0.06    --  -48.02 -57.00 -60.00  100
 45  \w    -64.00 -37.00   0.50    0.06    --  -48.02 -38.00-120.00   54
 46  \w    -60.00 -35.00   0.50    0.06    --  -48.02 -57.00-150.00   50
 47  \w   -121.00 -75.00   0.50    0.06    --  -48.02 -19.00-180.00   92
 48  \w    -71.00 -44.00   0.50    0.06    --  -48.02 -19.00-180.00   54
 49  \w    -57.00 -19.00   0.50    0.25    --  -91.75  61.00 -60.00   76
 50  \w    -44.00  23.00   0.50    0.06    --  -48.02  51.00 131.00  134
 51  \w    -52.00 -27.00   0.50    0.25    --  -91.75  51.00 131.00   50
 52  \w    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00  60.00   52
 53  \w   -139.00-113.00   0.50    0.25    --  -91.75 -77.00 -60.00   52
 54  \w   -105.00 -70.00   0.50    0.25    --  -91.75 -77.00 -30.00   70
 55  \w    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00 -60.00   50
 56  \w    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00 -90.00   50
 57  \w    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00-120.00   50
 58  \w   -122.00 -69.00   0.50    0.25    --  -91.75 -77.00-180.00  106
 59  \w   -163.00-129.00   0.50    0.25    --  -91.75 -77.00-180.00   68
 60  \w   -154.00-128.00   0.50    0.25    --  -91.75 -77.00   0.00   52
 61  \w    -97.00 -71.00   0.50    0.25    --  -91.75 -77.00  30.00   52
 62  \w    -94.00 -69.00   0.50    0.25    --  -91.75 -77.00   0.00   50
 63  \w    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00  94.40   52
 64  \w    -95.00 -69.00   0.50    0.25    --  -91.75 -77.00 150.00   52
 65  \w   -103.00 -69.00   0.50    0.25    --  -91.75 -76.00 123.13   68
 66  \w   -147.00-121.00   0.50    0.25    --  -91.75 -76.00 123.13   52
 67  \w   -107.00 -69.00   0.50    0.25    --  -91.75 -76.00  50.46   76
 68  \w   -100.00 -70.00   0.50    0.25    --  -91.75 -75.00 132.77   60
 69  \w    -95.00 -70.00   0.50    0.25    --  -91.75 -75.00  33.55   50
 70  \w    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00  10.45   50
 71  \w   -103.00 -70.00   0.50    0.25    --  -91.75 -75.00 -17.78   66
 72  \w    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-108.94   50
 73  \w    -96.00 -70.00   0.50    0.25    --  -91.75 -75.00-142.63   52
 74  \w    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-174.72   50
 75  \w    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00-160.09   50
 76  \w    -96.00 -70.00   0.50    0.25    --  -91.75 -74.00 -73.47   52
 77  \w   -107.00 -71.00   0.50    0.25    --  -91.75 -71.00 -52.45   72
 78  \w    -99.00 -74.00   0.50    0.25    --  -91.75 -63.00-148.79   50
 79  \w   -154.00-128.00   0.50    0.25    --  -91.75 -74.00-108.94   52
 80  \w   -145.00-120.00   0.50    0.25    --  -91.75 -51.00 -14.00   50
 81  \w    -95.00 -70.00   0.50    0.25    --  -91.75 -74.00  73.92   50
 82  \w    -98.00 -71.00   0.50    0.25    --  -91.75 -71.00 101.08   54
 83  \w    -99.00 -74.00   0.50    0.25    --  -91.75 -68.00 158.24   50
 84  \w    104.00 165.00   0.50    0.25    --  113.25 125.00   0.00  122
 85  \w    123.00 148.00   0.50    0.25    --  113.25 125.00 -30.00   50
 86  \w     43.00  68.00   0.50    0.25    --  113.25 -61.00  90.00   50
 87  \w     42.00  69.00   0.50    0.25    --  113.25 -61.00  30.00   54
 88  \w     47.00  89.00   0.50    0.25    --  113.25 -77.00 -60.00   84
 89  \w     43.00  96.00   0.50    0.25    --  113.25 -77.00 -90.00  106
 90  \w    -23.00  53.00   0.50    0.06    --   48.02 -51.00 -14.00  152
 91  \w     43.00  97.00   0.50    0.25    --  113.25 -95.00  90.00  108
 92  \w     71.00 117.00   0.50    0.25    --  113.25-132.00 172.24   92
 93  \w     85.00 111.00   0.50    0.25    --  113.25-125.00  90.00   52
 94  \w     42.00  81.00   0.50    0.25    --  113.25-125.00  90.00   78
 95  \w     76.00 111.00   0.50    0.25    --  113.25-125.00   0.00   70
 96  \w     45.00  71.00   0.50    0.25    --  113.25-125.00   0.00   52
 97  \w     43.00 111.00   0.50    0.25    --  113.25-125.00 -90.00  136
 98  \w     43.00 111.00   0.50    0.25    --  113.25-125.00-120.00  136
 99  \w     44.00 107.00   0.50    0.25    --  113.25-125.00-150.00  126
100  \w     36.00  78.00   0.50    0.06    --   48.02-125.00-150.00   84
101  \w     46.00 111.00   0.50    0.25    --  113.25-125.00 -60.00  130
102  \w     78.00 108.00   0.50    0.25    --  113.25-112.00  43.18   60
103  \w     47.00 102.00   0.50    0.25    --  113.25-125.00  30.00  110
104  \w     45.00  75.00   0.50    0.25    --  113.25-112.00  43.18   60
105  \w     81.00 106.00   0.50    0.25    --  113.25-102.00  36.80   50
106  \w     86.00 111.00   0.50    0.25    --  113.25-125.00 120.00   50
107  \w     44.00  69.00   0.50    0.25    --  113.25-125.00 120.00   50
108  \w     64.00  90.00   0.50    0.25    --  113.25 -95.00 150.00   52
109  \w     51.00  76.00   0.50    0.25    --  113.25-102.00  36.80   50
110  \w      6.00  82.00   0.50    0.06    --   48.02 -99.00-180.00  152
;
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44714
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.744
_diffrn_reflns_theta_min         4.545
_exptl_absorpt_coefficient_mu    17.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47651
_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    2.372
_exptl_crystal_description       block
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.398
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00072(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   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6624
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0473P)^2^+5.7164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6244
_reflns_number_total             6624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_653
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_original_cell_volume        1549.28(5)
_cod_database_code               7243291
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.343
_shelx_estimated_absorpt_t_min   0.256
_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,H) groups
2. Restrained distances
 H3-N3
 0.86 with sigma of 0.02
 N4-C15
 1.14 with sigma of 0.02
 C16-N4
 2.593 with sigma of 0.02
 C15-N4
 1.137 with sigma of 0.01
 C15-C16
 1.456 with sigma of 0.01
 N4-C16
 2.59 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N4 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C17) = Uanis(C18A)
Uanis(C15) = Uanis(C16)
Uanis(C17) = Uanis(C18)
Uanis(N5) = Uanis(C17)
4. Rigid body (RIGU) restrains
 N4, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C15(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C18A(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) C18(0.5) H18D(0.5) H18E(0.5) H18F(0.5) O21(0.5)
 H21A(0.5) H21B(0.5) O21A(0.5) H21C(0.5) H21D(0.5)
6.a Free rotating group:
 O20(H20A,H20B), O21(H21A,H21B), O21A(H21C,H21D)
6.b Rotating group:
 O5(H5A,H5B)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C13(H13), C10(H10), C7(H7), C11(H11), C6(H6), C12(H12), C3(H3A), C5(H5)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18A(H18A,H18B,H18C), C18(H18D,H18E,
 H18F)
;
_shelx_res_checksum              27970
_shelx_hkl_checksum              51253
_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
;