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_7054467
_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 H18 Mo N2 O7'
_chemical_formula_weight         458.27
_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
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.138(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0077(3)
_cell_length_b                   27.0442(16)
_cell_length_c                   9.7840(5)
_cell_measurement_reflns_used    7355
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.3829
_cell_measurement_theta_min      3.6875
_cell_volume                     1812.79(16)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega    4.00   56.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979  -45.0000  300.0000 52

  2 omega   -5.00   50.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979   77.0000   60.0000 55

  3 omega  -36.00   -2.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979  133.0000  212.0000 34

  4 omega   49.00  101.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979   45.0000   30.0000 52

  5 omega    4.00   56.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979  -45.0000   30.0000 52

  6 omega    0.00   50.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979   77.0000  150.0000 50

  7 omega   49.00  101.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979   45.0000  330.0000 52

  8 omega    3.00   51.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       28.4979 -135.0000  325.0000 48

  9 omega -104.00   -4.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.1542  -45.0000  150.0000 100

 10 omega  -39.00   -6.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.1542   45.0000  180.0000 33

 11 omega  -75.00  -47.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.1542  133.0000  215.0000 28

 12 omega  -44.00  -17.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.1542   45.0000  270.0000 27

 13 omega -101.00  -54.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.1542  -45.0000  240.0000 47

;
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0044956988
_diffrn_orient_matrix_UB_12      0.0261783467
_diffrn_orient_matrix_UB_13      -0.0027087955
_diffrn_orient_matrix_UB_21      0.0247097109
_diffrn_orient_matrix_UB_22      0.0009000585
_diffrn_orient_matrix_UB_23      0.0741025738
_diffrn_orient_matrix_UB_31      0.1004688714
_diffrn_orient_matrix_UB_32      -0.0013827338
_diffrn_orient_matrix_UB_33      -0.0021212011
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22974
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4814
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                3404
_reflns_number_total             4814
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4nj01394h2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7054467--7054471.cif.
;
_cod_database_code               7054467
_cell_oxdiff_length_a            7.0033(4)
_cell_oxdiff_length_b            27.0636(13)
_cell_oxdiff_length_c            9.7817(4)
_cell_oxdiff_angle_alpha         89.921(3)
_cell_oxdiff_angle_beta          102.102(4)
_cell_oxdiff_angle_gamma         90.053(4)
_cell_oxdiff_volume              1812.79(15)
_cell_oxdiff_measurement_reflns_used 7355