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_4064703
_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         'C100 H136 K2 Nd2 O10, 4(C7 H8)'
_chemical_formula_sum            'C128 H168 K2 Nd2 O10'
_chemical_formula_weight         2233.30
_chemical_name_systematic
; 
 ? 
;
_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                75.615(5)
_cell_angle_beta                 68.163(5)
_cell_angle_gamma                77.512(6)
_cell_formula_units_Z            1
_cell_length_a                   13.7855(7)
_cell_length_b                   15.4725(11)
_cell_length_c                   15.9167(9)
_cell_measurement_reflns_used    12438
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     3023.5(3)
_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 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29550
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         11000
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0506P)^2^+2.8796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                10350
_reflns_number_total             11000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200283j_si_002.cif
_cod_data_source_block           complex2
_cod_database_code               4064703