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_7243289
_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(C14 H14 Mo N3 O6), 4(C2 H3 N)'
_chemical_formula_sum            'C36 H40 Mo8 N10 O31'
_chemical_formula_weight         1876.30
_chemical_name_systematic
'bis((aquo)-dioxo-(N-(2-oxy-4-methoxybenzylidene)isonicotinylhydrazonato)-molybdenum(vi)) hexamolybdate acetonitrile solvate'
_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
_audit_creation_date             2021-07-15
_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                97.652(3)
_cell_angle_beta                 107.915(3)
_cell_angle_gamma                114.577(4)
_cell_formula_units_Z            1
_cell_length_a                   10.8617(4)
_cell_length_b                   10.9074(4)
_cell_length_c                   13.8765(6)
_cell_measurement_reflns_used    7355
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.0980
_cell_measurement_theta_min      4.2240
_cell_volume                     1356.26(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.996
_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     69.00 101.00   1.00    1.00    --   28.65 179.00 -90.00   32
  2  \w     49.00  88.00   1.00    1.00    --   28.65 179.00  90.00   39
  3  \w    -96.00  43.00   1.00    1.00    --  -31.62  19.00 -60.00  139
  4  \w   -111.00 -44.00   1.00    1.00    --  -31.62-179.00 -30.00   67
  5  \w    -70.00  -8.00   1.00    1.00    --  -31.62 -57.00  30.00   62
  6  \w    -64.00 -36.00   1.00    1.00    --  -31.62 -57.00 -30.00   28
  7  \w   -107.00 -80.00   1.00    1.00    --  -31.62 179.00  60.00   27
  8  \w    -58.00 -32.00   1.00    1.00    --  -31.62 179.00  60.00   26
  9  \w   -107.00   3.00   1.00    1.00    --  -31.62 -19.00-180.00  110
 10  \w    -76.00 -32.00   1.00    1.00    --  -31.62 179.00  30.00   44
 11  \w     43.00  71.00   1.00    1.00    --   28.65 -99.00 150.00   28
 12  \w     16.00  73.00   1.00    1.00    --   28.65 -99.00 -90.00   57
 13  \w    -46.00  -7.00   1.00    1.00    --  -31.62 -77.00   0.00   39
 14  \w     12.00  39.00   1.00    1.00    --  -31.62  77.00 150.00   27
 15  \w   -102.00 -44.00   1.00    1.00    --  -31.62 -57.00 -60.00   58
;
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22244
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.259
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    2.297
_exptl_crystal_description       irregular
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.443
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0338P)^2^+0.3977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6501
_reflns_number_total             7891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00861g3.cif
_cod_data_source_block           exp_5005
_cod_depositor_comments
'Adding full bibliography for 7243285--7243294.cif.'
_cod_original_cell_volume        1356.26(10)
_cod_database_code               7243289
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.692
_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
2. Restrained distances
 H6A-O6
 0.86 with sigma of 0.02
 O6-H6B
 0.86 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C7(H7), C5(H5), C3(H3A), C6(H6), C13(H13), C12(H12), C11(H11), C10(H10)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              18855
_shelx_hkl_checksum              31118
_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
;