Trisguanidinate Lanthanide Complexes: Syntheses, Structures, and Catalytic Activity for Mild Amidation of Aldehydes with Amines
Qian, Cunwei; Zhang, Xingmin; Li, Junmei; Xu, Fan; Zhang, Yong; Shen, Qi; Organometallics 28 (2009) 3856–; doi:10.1021/om900120v

data_4069279
_publ_section_title
;
 Trisguanidinate Lanthanide Complexes: Syntheses, Structures, and
 Catalytic Activity for Mild Amidation of Aldehydes with Amines
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3856
_journal_paper_doi               10.1021/om900120v
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C39 H96 N9 Nd Si6'
_chemical_formula_sum            'C39 H96 N9 Nd Si6'
_chemical_formula_weight         1004.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 97.433(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.607(2)
_cell_length_b                   23.159(3)
_cell_length_c                   17.262(3)
_cell_measurement_reflns_used    18362
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     5790.4(15)
_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      213(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41121
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         10714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0178P)^2^+22.0995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                9896
_reflns_number_total             10714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900120v_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        5790.5(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4069279