Activation of Carbodiimide and Transformation with Amine to Guanidinate Group by Ln(OAr)3(THF)2 (Ln: Lanthanide and Yttrium) and Ln(OAr)3(THF)2 as a Novel Precatalyst for Addition of Amines to Carbodiimides: Influence of Aryloxide Group
Yang Cao; Zhu Du; Wenbo Li; Junmei Li; Yong Zhang; Fan Xu; Qi Shen; Inorganic Chemistry 50 (2011) 3729–3737; doi:10.1021/ic200091s

data_4324904
_publ_contact_author_email       qshen@suda.edu.cn
_publ_contact_author_fax         86-512-65880305
_publ_contact_author_name        'Dr. Qi Shen'
_publ_contact_author_phone       86-512-65880306
_publ_section_title
;
 Activation of Carbodiimide and Transformation with Amine to Guanidinate
 Group by Ln(OAr)3(THF)2 (Ln: Lanthanide and Yttrium) and Ln(OAr)3(THF)2
 as a Novel Precatalyst for Addition of Amines to Carbodiimides: Influence
 of Aryloxide Group
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3729
_journal_page_last               3737
_journal_paper_doi               10.1021/ic200091s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C58 H91 N2 O3 Y, C7 H8'
_chemical_formula_sum            'C65 H99 N2 O3 Y'
_chemical_formula_weight         1045.37
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                79.534(5)
_cell_angle_beta                 75.579(5)
_cell_angle_gamma                71.112(4)
_cell_formula_units_Z            2
_cell_length_a                   14.2961(4)
_cell_length_b                   14.8441(5)
_cell_length_c                   15.7236(6)
_cell_measurement_reflns_used    13768
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3039.0(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26299
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11250
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0562P)^2^+2.9211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                9528
_reflns_number_total             11250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200091s_si_001_4.cif
_cod_data_source_block           complex3
_cod_original_cell_volume        3038.96(18)
_cod_database_code               4324904