Lewis Acid Stabilized Methylidene and Oxoscandium Complexes
Jennifer Scott; Hongjun Fan; Benjamin F. Wicker; Alison R. Fout; Mu-Hyun Baik; Daniel J. Mindiola; Journal of the American Chemical Society 130 (2008) 14438–14439; doi:10.1021/ja806635x

data_4108623
_publ_section_title
;
 Lewis Acid Stabilized Methylidene and Oxoscandium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14438
_journal_page_last               14439
_journal_paper_doi               10.1021/ja806635x
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C99 H156 Al4 N2 O2 P4 Sc2'
_chemical_formula_weight         1727.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.519(6)
_cell_angle_beta                 104.568(5)
_cell_angle_gamma                106.793(5)
_cell_formula_units_Z            1
_cell_length_a                   10.822(4)
_cell_length_b                   14.580(5)
_cell_length_c                   17.981(7)
_cell_measurement_reflns_used    5781
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.75
_cell_volume                     2575.2(16)
_computing_cell_refinement       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_collection       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_reduction        'APEX II v.2.2 (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2007)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker SMART APEXII'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
'0.30 degree frames measured for 120 seconds each'
_diffrn_measurement_device       'APEX II Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi 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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40739
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_correction_T_min  0.9526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         10504
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+3.1350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1847
_reflns_number_gt                7151
_reflns_number_total             10504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806635x_si_005.cif
_cod_data_source_block           08096
_cod_database_code               4108623