Dioxidomolybdenum(vi) complexes with isoniazid-related hydrazones: solution-based, mechanochemical and UV-light assisted deprotonation
Vrdoljak, Višnja; Prugovečki, Biserka; Pulić, Ivana; Cigler, Marko; Sviben, Dora; Parlov Vuković, Jelena; Novak, Predrag; Matković-Čalogović, Dubravka; Cindrić, Marina; New J. Chem. 39 (2015) 7322–; doi:10.1039/C5NJ01567G

data_7054996
_publ_section_title
;
 Dioxidomolybdenum(vi) complexes with isoniazid-related hydrazones:
 solution-based, mechanochemical and UV-light assisted deprotonation
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7322
_journal_paper_doi               10.1039/C5NJ01567G
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C18 H16 Cl Mo N3 O5'
_chemical_formula_weight         485.73
_chemical_name_systematic
'cis-dioxido-methanol-(2-oxo-1-naphthaldehyde isonicotinylhydrazonato-O,N,O)molybdenum(VI) chloride'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-10 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                96.890(6)
_cell_angle_beta                 90.248(5)
_cell_angle_gamma                97.558(7)
_cell_formula_units_Z            2
_cell_length_a                   7.5013(5)
_cell_length_b                   9.4538(9)
_cell_length_c                   13.3244(7)
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      3.71
_cell_volume                     929.74(12)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2010)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2010)'
_computing_molecular_graphics    'PLATON98 (Spek, 1990)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean CCD
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       'Xcalibur CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25507
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.573
_diffrn_reflns_theta_min         3.706
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0487P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4762
_reflns_number_total             6216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01567g2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7054993--7055000.cif.'
_cod_database_code               7054996
_shelxl_version_number           2013-4
_shelx_res_checksum              22297