Versatile Reactivity of a Four-Coordinate Scandium Phosphinidene Complex: Reduction, Addition, and CO Activation Reactions
Yingdong Lv; Christos E. Kefalidis; Jiliang Zhou; Laurent Maron; Xuebing Leng; Yaofeng Chen; Journal of the American Chemical Society 135 (2013) 14784–14796; doi:10.1021/ja406413d

data_4120881
_publ_section_title
;
 Versatile Reactivity of a Four-Coordinate Scandium Phosphinidene Complex:
 Reduction, Addition, and CO Activation Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14784
_journal_page_last               14796
_journal_paper_doi               10.1021/ja406413d
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C90 H136 N8 P2 Sc2'
_chemical_formula_weight         1481.93
_chemical_name_systematic
; 
 ? 
;
_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                 102.052(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.7351(19)
_cell_length_b                   14.0886(15)
_cell_length_c                   19.026(2)
_cell_measurement_reflns_used    9153
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.28
_cell_volume                     4649.1(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40348
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.9398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         12451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1074P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                8832
_reflns_number_total             12451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja406413d_11.cif
_cod_data_source_block           mo_dm12591_0m
_cod_original_cell_volume        4649.0(9)
_cod_database_code               4120881