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_4108622
_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_moiety         'C50 H76 N3 P2 Sc'
_chemical_formula_sum            'C50 H76 N3 P2 Sc'
_chemical_formula_weight         826.04
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.725(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.848(3)
_cell_length_b                   11.3543(18)
_cell_length_c                   22.607(3)
_cell_measurement_reflns_used    4933
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.7
_cell_volume                     4813.9(13)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31993
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.9276
_exptl_absorpt_correction_T_min  0.7850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       plates
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9769
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0628P)^2^+3.5001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                5651
_reflns_number_total             9769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806635x_si_004.cif
_cod_data_source_block           07141
_cod_database_code               4108622