Dioxotungsten(VI) complexes with isoniazid-related hydrazones as (pre)catalysts for olefin epoxidation: solvent and ligand substituent effects
Vrdoljak, Visnja; Pisk, Jana; Prugovečki, Biserka; Agustin, Dominique; Novak, Predrag; Matković-Čalogović, Dubravka; RSC Adv.  (2016) –; doi:10.1039/C6RA05067K

data_7224856
_publ_section_title
;
 Dioxotungsten(VI) complexes with isoniazid-related hydrazones as
 (pre)catalysts for olefin epoxidation: solvent and ligand substituent
 effects
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA05067K
_journal_year                    2016
_chemical_formula_sum            'C13.5 H18 O6 W'
_chemical_formula_weight         460.13
_chemical_name_systematic
'bis(acetylacetonato)dioxotungsten(VI) toluene solvate (2/1)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-02-19 deposited with the CCDC.
2016-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.619(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3569(4)
_cell_length_b                   16.2269(7)
_cell_length_c                   13.5020(11)
_cell_measurement_reflns_used    4849
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.4317
_cell_measurement_theta_min      3.7343
_cell_volume                     1604.12(17)
_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    'MERCURY (C.F. Macrae et al , 2008)'
_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_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Xcalibur CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14965
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.388
_diffrn_reflns_theta_min         3.749
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       prism
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.765
_refine_diff_density_min         -2.466
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2646
_reflns_number_total             3639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra05067k2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C13.50 H18 O6 W'
_cod_database_code               7224856
_shelxl_version_number           2013-4
_shelx_res_checksum              26864