Synthesis and Structural Diversity of Heterobimetallic Lanthanide‒Potassium Complexes and Catalytic Activity for Amidation of Aldehydes with Amines
Xu, Bin; Huang, Lingling; Yang, Zijian; Yao, Yingming; Zhang, Yong; Shen, Qi; Organometallics 30 (2011) 3588–; doi:10.1021/om200283j

data_4064705
_publ_section_title
;
 Synthesis and Structural Diversity of Heterobimetallic
 Lanthanide--Potassium Complexes and Catalytic Activity for Amidation of
 Aldehydes with Amines
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3588
_journal_paper_doi               10.1021/om200283j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C66 H100 K O9 Yb '
_chemical_formula_sum            'C66 H100 K O9 Yb'
_chemical_formula_weight         1249.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.639(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0853(13)
_cell_length_b                   17.3469(15)
_cell_length_c                   28.382(3)
_cell_measurement_reflns_used    23395
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     7402.8(12)
_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      293(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            70885
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.669
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         13509
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0824
_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^)+(0.0947P)^2^+15.5940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2188
_reflns_number_gt                10501
_reflns_number_total             13509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200283j_si_002.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        7402.8(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C66 H100 K O9 Yb '
_cod_database_code               4064705