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_7243285
_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
'4(C13 H12 Mo N3 O6), Mo8 O26, 4(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C56 H62 Mo12 N14 O54'
_chemical_formula_weight         2946.47
_chemical_name_systematic
'tetrakis(((aquo)-N-(2-oxo-3-hydroxybenzylidene)isonicotinylhydrazonato)dioxomolybdenum(vi)) octamolybdate acetonitrile solvate hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 108.137(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0881(2)
_cell_length_b                   33.6789(5)
_cell_length_c                   12.0491(2)
_cell_measurement_reflns_used    21463
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      79.2710
_cell_measurement_theta_min      3.8720
_cell_volume                     4275.99(13)
_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 0.975
_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    102.00 159.00   0.50    0.84    --  113.25  61.00 120.00  114
  2  \w    113.00 178.00   0.50    0.84    --  113.25  45.00  90.00  130
  3  \w    102.00 174.00   0.50    0.84    --  113.25  30.00  60.00  144
  4  \w    100.00 142.00   0.50    0.84    --  113.25  15.00 -60.00   84
  5  \w    121.00 169.00   0.50    0.84    --  113.25  30.00-150.00   96
  6  \w    153.00 178.00   0.50    0.84    --  113.25  15.00-180.00   50
  7  \w    120.00 146.00   0.50    0.84    --  113.25  15.00-180.00   52
  8  \w    -12.00  13.00   0.50    0.21    --  -48.02  19.00-150.00   50
  9  \w    -82.00 -52.00   0.50    0.84    --  -91.75 107.00-167.00   60
 10  \w    -71.00 -42.00   0.50    0.21    --  -48.02 107.00-167.00   58
 11  \w    -36.00  -3.00   0.50    0.21    --  -48.02 107.00-167.00   66
 12  \w    -38.00  25.00   0.50    0.21    --  -48.02  38.00 -60.00  126
 13  \w   -148.00-122.00   0.50    0.84    --  -91.75-107.00  94.00   52
 14  \w   -116.00 -89.00   0.50    0.21    --  -48.02-125.00 150.00   54
 15  \w   -118.00 -77.00   0.50    0.21    --  -48.02-125.00 -30.00   82
 16  \w   -117.00 -74.00   0.50    0.21    --  -48.02-125.00 -60.00   86
 17  \w   -110.00 -74.00   0.50    0.21    --  -48.02-125.00-180.00   72
 18  \w     45.00  70.00   0.50    0.84    --  113.25 -61.00 -90.00   50
 19  \w     61.00  86.00   0.50    0.84    --  113.25 -77.00-180.00   50
 20  \w     65.00 105.00   0.50    0.84    --  113.25 -77.00-120.00   80
 21  \w     42.00  69.00   0.50    0.84    --  113.25 -61.00-180.00   54
 22  \w     42.00  71.00   0.50    0.84    --  113.25 -61.00   0.00   58
 23  \w     44.00  71.00   0.50    0.84    --  113.25 -61.00 120.00   54
 24  \w     46.00  72.00   0.50    0.84    --  113.25 -77.00  90.00   52
 25  \w     43.00  70.00   0.50    0.84    --  113.25 -61.00 -30.00   54
 26  \w     43.00  69.00   0.50    0.84    --  113.25 -61.00-150.00   52
 27  \w     96.00 176.00   0.50    0.84    --  113.25 125.00 -60.00  160
 28  \w    117.00 143.00   0.50    0.84    --  113.25 107.00-167.00   52
 29  \w     51.00  98.00   0.50    0.84    --  113.25 -95.00 150.00   94
 30  \w     45.00 101.00   0.50    0.84    --  113.25-107.00  94.00  112
 31  \w     49.00 111.00   0.50    0.84    --  113.25-125.00 150.00  124
 32  \w     61.00  97.00   0.50    0.84    --  113.25 -95.00 120.00   72
 33  \w     23.00  80.00   0.50    0.21    --   48.02-107.00  94.00  114
 34  \w     42.00  78.00   0.50    0.84    --  113.25-125.00   0.00   72
 35  \w     62.00 109.00   0.50    0.84    --  113.25-125.00-150.00   94
;
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37508
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.131
_diffrn_reflns_theta_min         4.078
_exptl_absorpt_coefficient_mu    14.926
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.244
_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    2.288
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.741
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0786P)^2^+14.0679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8184
_reflns_number_total             9113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_649_auto
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_database_code               7243285
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.201
_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.a Free rotating group:
 O20(H20A,H20B), O21(H21A,H21B)
2.b Rotating group:
 O5(H5B,H5C), O5A(H5AA,H5AB)
2.c Aromatic/amide H refined with riding coordinates:
 N3A(H3A), N3(H3), C13A(H13A), C10(H10), C13(H13), C7(H7), C5(H5), C7A(H7A),
 C6(H6B), C12(H12), C11A(H11A), C10A(H10A), C4(H4), C12A(H12A), C6A(H6AA),
 C11(H11), C5A(H5A), C4A(H4A)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
2.e Idealised tetrahedral OH refined as rotating group:
 O6A(H6A), O6(H6)
;
_shelx_res_checksum              88473
_shelx_hkl_checksum              5818
_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
;