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_7054997
_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            'C17 H23 Cl Mo N4 O6'
_chemical_formula_weight         510.78
_chemical_name_systematic
'cis-dioxido-aqua-(diethylamino-salicylaldehyde4-phenylthiosemicarbazonato)molybdenum(VI)chloride hydrate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-10 deposited with the CCDC.
2015-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.225(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9580(4)
_cell_length_b                   11.4043(2)
_cell_length_c                   12.2325(3)
_cell_measurement_reflns_used    23679
_cell_measurement_temperature    295
_cell_measurement_theta_max      32.5802
_cell_measurement_theta_min      4.1663
_cell_volume                     2102.04(9)
_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-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45544
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         4.17
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+1.0950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                4947
_reflns_number_total             5580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01567g2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7054993--7055000.cif.'
_cod_original_cell_volume        2102.04(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7054997