Discrete mononuclear and dinuclear compounds containing a MoO22+ core and 4-aminobenzhydrazone ligands: synthesis, structure and organic-solvent-free epoxidation activity
Cvijanović, Danijela; Pisk, Jana; Pavlović, Gordana; Šišak-Jung, Dubravka; Matković-Čalogović, Dubravka; Cindrić, Marina; Agustin, Dominique; Vrdoljak, Višnja; New Journal of Chemistry 43 (2019) 1791–; doi:10.1039/C8NJ04074E

data_7058984
_publ_section_title
;
 Discrete mononuclear and dinuclear compounds containing a MoO22+ core and
 4-aminobenzhydrazone ligands: synthesis, structure and
 organic-solvent-free epoxidation activity
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1791
_journal_paper_doi               10.1039/C8NJ04074E
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C16 H17 Mo N3 O6'
_chemical_formula_sum            'C16 H17 Mo N3 O6'
_chemical_formula_weight         443.26
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-10 deposited with the CCDC.
2018-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.484(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7385(3)
_cell_length_b                   21.1670(6)
_cell_length_c                   10.5127(5)
_cell_measurement_reflns_used    2356
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.0670
_cell_measurement_theta_min      4.5500
_cell_volume                     1703.15(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 

;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 

;
_computing_molecular_graphics    'MERCURY 3.8. (CCDC, 2016)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9733
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         4.321
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91439
_exptl_absorpt_correction_type   multi-scan
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4940
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0509P)^2^+0.0478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3650
_reflns_number_total             4940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04074e2.cif
_cod_data_source_block           1843
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7058984
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              91579