Scandium Carbene Complexes: Synthesis of Mixed Alkyl, Amido, and Phosphido Derivatives
Fustier, Marie; Le Goff, Xavier-Frédéric; Lutz, Martin; Slootweg, J. Chris; Mézailles, Nicolas; Organometallics 34 (2015) 63–; doi:10.1021/om500868a

data_4085113
_publ_section_title
;
 Scandium Carbene Complexes: Synthesis of Mixed Alkyl, Amido, and
 Phosphido Derivatives
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              63
_journal_paper_doi               10.1021/om500868a
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C41 H48 N2 P3 S2 Sc Si2'
_chemical_formula_sum            'C41 H48 N2 P3 S2 Sc Si2'
_chemical_formula_weight         826.98
_chemical_name_systematic
; 
 ? 
;
_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                64.9020(10)
_cell_angle_beta                 67.2485(10)
_cell_angle_gamma                70.2251(10)
_cell_formula_units_Z            4
_cell_length_a                   15.4243(6)
_cell_length_b                   17.8240(7)
_cell_length_c                   19.8192(8)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.36
_cell_volume                     4450.2(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V7.68A, SADABS-2008/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            93803
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         20302
_refine_ls_number_restraints     1030
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.8293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                14510
_reflns_number_total             20302
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om500868a_si_002.cif
_cod_data_source_block           l0189a
_cod_depositor_comments
'Adding full bibliography for 4085110--4085113.cif.'
_cod_database_code               4085113