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_7243292
_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(C13 H12 Mo N3 O6)'
_chemical_formula_sum            'C26 H24 Mo8 N6 O31'
_chemical_formula_weight         1684.03
_chemical_name_systematic
'bis((aquo)-dioxo-(N-(2-oxy-3-hydroxybenzylidene)isonicotinylhydrazonato)-molybdenum(vi)) hexamolybdate'
_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             2021-06-18
_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                90
_cell_angle_beta                 89.706(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6794(2)
_cell_length_b                   9.3605(3)
_cell_length_c                   29.2326(9)
_cell_measurement_reflns_used    7205
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.7240
_cell_measurement_theta_min      4.4030
_cell_volume                     2101.30(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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      150.0
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.916
_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     46.00 108.00   1.00   30.00    --   28.19 179.00  90.00   62
  2  \w    -20.00  12.00   1.00   30.00    --   28.19  19.00 -60.00   32
  3  \w   -101.00 -24.00   1.00   30.00    --  -31.15 -37.00-120.00   77
  4  \w     19.00  45.00   1.00   30.00    --   28.19 -57.00  30.00   26
  5  \w    -53.00 -26.00   1.00   30.00    --  -31.15 -57.00   0.00   27
  6  \w   -102.00 -56.00   1.00   30.00    --  -31.15 -57.00   0.00   46
  7  \w     80.00 106.00   1.00   30.00    --   28.19-179.00  30.00   26
  8  \w      0.00  35.00   1.00   30.00    --  -31.15 -19.00 -90.00   35
  9  \w    -81.00 -28.00   1.00   30.00    --  -31.15 -19.00 -90.00   53
 10  \w     38.00  69.00   1.00   30.00    --   28.19 179.00-120.00   31
 11  \w     42.00  77.00   1.00   30.00    --   28.19 179.00 -30.00   35
 12  \w    -85.00 -39.00   1.00   30.00    --  -31.15-179.00   0.00   46
 13  \w    -56.00  -2.00   1.00   30.00    --  -31.15 -77.00   0.00   54
 14  \w   -109.00 -81.00   1.00   30.00    --  -31.15-179.00  30.00   28
 15  \w    -87.00 -38.00   1.00   30.00    --  -31.15-179.00 -60.00   49
 16  \w    -35.00  -8.00   1.00   30.00    --  -31.15 -57.00  30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            31071
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.737
_diffrn_reflns_theta_min         4.026
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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    2.662
_exptl_crystal_description       prism
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.887
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7112
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0287P)^2^+6.0964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5238
_reflns_number_total             7112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_5000_autored
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_database_code               7243292
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.713
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H) groups
2. Restrained distances
 N3-H3
 0.82 with sigma of 0.02
 O6-H6A
 0.82 with sigma of 0.02
 O6-H6B
 0.82 with sigma of 0.02
 O5-H5
 0.82 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C7(H7), C11(H11), C5(H5A), C10(H10), C6(H6), C4(H4)
;
_shelx_res_checksum              26604
_shelx_hkl_checksum              38381
_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
;