Oxygen activation and catalytic aerobic oxidation by Mo(iv)/(vi) complexes with functionalized iminophenolate ligands.
Zwettler, Niklas; Judmaier, Martina E.; Strohmeier, Lara; Belaj, Ferdinand; Mösch-Zanetti, Nadia C; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14549–14560; doi:10.1039/c6dt01692h

data_7039708
_publ_section_title
;
 Oxygen activation and catalytic aerobic oxidation by Mo(iv)/(vi)
 complexes with functionalized iminophenolate ligands.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14549
_journal_page_last               14560
_journal_paper_doi               10.1039/c6dt01692h
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C76 H120 Mo2 N4 O11, 2(C2 H3 N)'
_chemical_formula_sum            'C80 H126 Mo2 N6 O11'
_chemical_formula_weight         1539.74
_chemical_name_common
'tetrakis(2,4-di-tert-butyl-6-{(E)-[(3-methoxypropyl)imino]methyl}phe-nolato)-(mu2-oxo)-dioxo-di-molybdenum(V) acetonitrile solvate (1:2)'
_chemical_name_systematic
'tetrakis(2,4-di-tert-butyl-6-{(E)-[(3-methoxypropyl)imino]methyl}phe-nolato)-(mu2-oxo)-dioxo-di-molybdenum(V) acetonitrile solvate (1:2)'
_space_group_crystal_system      hexagonal
_space_group_IT_number           171
_space_group_name_Hall           'P 62'
_space_group_name_H-M_alt        'P 62'
_symmetry_space_group_name_Hall  'P 62'
_symmetry_space_group_name_H-M   'P 62'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.8493(5)
_cell_length_b                   20.8493(5)
_cell_length_c                   17.0636(6)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.55
_cell_volume                     6423.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41606
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       hexag.prism
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.842
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 2331 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7534
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+2.2270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5744
_reflns_number_total             7534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01692h2.cif
_cod_data_source_block           NZ372
_cod_depositor_comments
'Adding full bibliography for 7039702--7039708.cif.'
_cod_original_cell_volume        6423.7(4)
_cod_database_code               7039708
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.966
_shelxl_version_number           2014/6
_shelx_res_checksum              63311