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_4069277
_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_sum            'C43 H65 Cl3 La N9 O'
_chemical_formula_weight         969.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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                80.505(4)
_cell_angle_beta                 89.947(4)
_cell_angle_gamma                86.812(5)
_cell_formula_units_Z            2
_cell_length_a                   10.463(2)
_cell_length_b                   13.118(2)
_cell_length_c                   17.912(3)
_cell_measurement_temperature    223(2)
_cell_volume                     2421.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17336
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.8281
_exptl_absorpt_correction_T_min  0.5517
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         8828
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                7747
_reflns_number_total             8828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900120v_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2421.0(8)
_cod_database_code               4069277