Synthesis, Structure, and Catalytic Oxidation Chemistry from the First Oxo-Imido Schiff Base Metal Complexes
Ramkrishna Ramnauth; Salih Al-Juaid; Majid Motevalli; Bernardetta C. Parkin; Alice C. Sullivan; Inorganic Chemistry 43 (2004) 4072–4079; doi:10.1021/ic035318h

data_4311149
_publ_section_title
;
 Synthesis, Structure, and Catalytic Oxidation Chemistry from the First
 Oxo-Imido Schiff Base Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4072
_journal_page_last               4079
_journal_paper_doi               10.1021/ic035318h
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C37 H57 Mo N3 O3'
_chemical_formula_sum            'C44 H65 Mo N3 O3'
_chemical_formula_weight         779.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.28(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.299(9)
_cell_length_b                   11.798(5)
_cell_length_c                   14.3020(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      10.970
_cell_measurement_theta_min      8.887
_cell_volume                     4268(2)
_computing_cell_refinement       'CAD4 /PC (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 /PC (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_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  0.0046
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7866
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        7
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.9498
_exptl_absorpt_correction_T_min  0.8882
_exptl_absorpt_correction_type   pci-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+2.9335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                5024
_reflns_number_total             7631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035318hsi20040303_075831.cif
_cod_data_source_block           4rr196
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4311149