Facile Preparation of a Scandium Terminal Imido Complex Supported by a Phosphazene Ligand
Rong, Weifeng; Cheng, Jianhua; Mou, Zehuai; Xie, Hongyan; Cui, Dongmei; Organometallics 32 (2013) 5523–; doi:10.1021/om400803q

data_4081676
_publ_section_title
;
 Facile Preparation of a Scandium Terminal Imido Complex Supported by a
 Phosphazene Ligand
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5523
_journal_paper_doi               10.1021/om400803q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C72 H90 N5 O0 P2 Si0 Y'
_chemical_formula_weight         1176.34
_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                 94.2320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3417(8)
_cell_length_b                   23.5568(13)
_cell_length_c                   22.3531(13)
_cell_measurement_temperature    273(2)
_cell_volume                     7006.2(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40176
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.8821
_exptl_absorpt_correction_T_min  0.8304
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         12414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                8170
_reflns_number_total             12414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400803q_si_003.cif
_cod_data_source_block           11
_cod_original_cell_volume        7006.1(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4081676