Molybdenum Oxo and Imido Complexes of β-Diketiminate Ligands: Synthesis and Structural Aspects
Ganna Lyashenko; Regine Herbst-Irmer; Vojtech Jancik; Aritra Pal; Nadia C. Mösch-Zanetti; Inorganic Chemistry 47 (2008) 113–120; doi:10.1021/ic701534a

data_4304114
_publ_section_title
;
Molybdenum Oxo and Imido Complexes of \b-Diketiminate Ligands: Synthesis
and Structural Aspects
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              113
_journal_page_last               120
_journal_paper_doi               10.1021/ic701534a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C42 H50 Mo2 N4 O4'
_chemical_formula_weight         866.74
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 109.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.982(3)
_cell_length_b                   8.848(2)
_cell_length_c                   23.761(2)
_cell_measurement_reflns_used    7217
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.959
_cell_measurement_theta_min      3.955
_cell_volume                     3952.4(12)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'Proteum (v 1.40, Bruker 2002)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18849
_diffrn_reflns_theta_full        58.95
_diffrn_reflns_theta_max         58.95
_diffrn_reflns_theta_min         3.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.558
_exptl_absorpt_correction_T_max  0.6064
_exptl_absorpt_correction_T_min  0.4894
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.000275(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+5.1407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                2704
_reflns_number_total             2806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701534a-file001.cif
_cod_data_source_block           test
_cod_original_cell_volume        3952.4(11)
_cod_database_code               4304114