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_4064704
_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         'C62 H92 K O8 Sm, 0.5(C7 H8), 0.5(C4 H8 O)'
_chemical_formula_sum            'C67.5 H100 K O8.5 Sm'
_chemical_formula_weight         1236.92
_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                111.279(4)
_cell_angle_beta                 92.015(2)
_cell_angle_gamma                107.289(4)
_cell_formula_units_Z            2
_cell_length_a                   13.071(2)
_cell_length_b                   16.239(3)
_cell_length_c                   18.208(3)
_cell_measurement_reflns_used    12085
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     3393.9(10)
_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 0.992
_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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0919
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33076
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         12344
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0828
_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^)+(0.0741P)^2^+4.0218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                9757
_reflns_number_total             12344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200283j_si_002.cif
_cod_data_source_block           complex3
_cod_original_cell_volume        3394.0(10)
_cod_original_formula_sum        'C67.50 H100 K O8.50 Sm'
_cod_database_code               4064704