Dioxomolybdenum(vi) and dioxotungsten(vi) complexes chelated with the ONO tridentate hydrazone ligand: synthesis, structure and catalytic epoxidation activity
Vrdoljak, Višnja; Pisk, Jana; Agustin, Dominique; Novak, Predrag; Parlov Vuković, Jelena; Matković-Čalogović, Dubravka; New J. Chem. 38 (2014) 6176–; doi:10.1039/C4NJ01394H

data_7054468
_publ_section_title
;
 Dioxomolybdenum(vi) and dioxotungsten(vi) complexes chelated with the ONO
 tridentate hydrazone ligand: synthesis, structure and catalytic
 epoxidation activity
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              6176
_journal_paper_doi               10.1039/C4NJ01394H
_journal_volume                  38
_journal_year                    2014
_chemical_formula_sum            'C17 H15 Mo N3 O6'
_chemical_formula_weight         453.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.342(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.97920(10)
_cell_length_b                   10.3039(3)
_cell_length_c                   21.3511(9)
_cell_measurement_reflns_used    3057
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6570
_cell_measurement_theta_min      4.4050
_cell_volume                     871.62(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6290
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         28.926
_diffrn_reflns_theta_min         4.315
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.315
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.1248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                3308
_reflns_number_total             3373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4nj01394h2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7054467--7054471.cif.'
_cod_database_code               7054468
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              54010