Synthesis, Structure, and Catalytic Properties of VIV, MnIII, MoVI, and UVI Complexes Containing Bidentate (N, O) Oxazine and Oxazoline Ligands
Karuppasamy Kandasamy; Harkesh B. Singh; Ray J. Butcher; Jerry P. Jasinski; Inorganic Chemistry 43 (2004) 5704–5713; doi:10.1021/ic0352093

data_4311468
_publ_section_title
;
 Synthesis, Structure, and Catalytic Properties of VIV, MnIII, MoVI, and
 UVI Complexes Containing Bidentate (N, O) Oxazine and Oxazoline Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5704
_journal_page_last               5713
_journal_paper_doi               10.1021/ic0352093
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C22 H24 Mo N2 O6'
_chemical_formula_weight         508.37
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.585(2)
_cell_length_b                   14.807(3)
_cell_length_c                   27.670(6)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      7.75
_cell_measurement_theta_min      6.25
_cell_volume                     4336.8(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       'omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1179
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2681
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.37
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'cloudy yellow'
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1596
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+93.0134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                1464
_reflns_number_total             2681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0352093si20031022_020809_3.cif
_cod_data_source_block           5
_cod_original_cell_volume        4337.0(15)
_cod_database_code               4311468