Synthesis, Reactivity, and Characterization of Sodium and Rare-Earth Metal Complexes Bearing a Dianionic N-Aryloxo-Functionalized β-Ketoiminate Ligand
Hongmei Peng; Zhenqin Zhang; Ruipeng Qi; Yingming Yao; Yong Zhang; Qi Shen; Yanxiang Cheng; Inorganic Chemistry 47 (2008) 9828–9835; doi:10.1021/ic8011469

data_4306304
_publ_contact_author_email       yaoym@suda.edu.cn
_publ_contact_author_fax         86-512-65880305
_publ_contact_author_name        'Dr. Yingming Yao'
_publ_contact_author_phone       86-512-65882806
_publ_section_title
;
Synthesis, Reactivity, and Characterization of Sodium and Rare-Earth Metal
Complexes Bearing a Dianionic N-Aryloxo-Functionalized \b-Ketoiminate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9828
_journal_page_last               9835
_journal_paper_doi               10.1021/ic8011469
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C32 H46 Cl2 N2 O8 Tb2,2/3(C4 H8 O)'
_chemical_formula_sum            'C34.66667 H51.33333 Cl2 N2 O8.66667 Tb2'
_chemical_formula_weight         1023.52
_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                 97.889(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   13.1389(11)
_cell_length_b                   15.0689(12)
_cell_length_c                   31.425(3)
_cell_measurement_reflns_used    22231
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6162.9(9)
_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      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            56812
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    3.593
_exptl_absorpt_correction_T_max  0.5335
_exptl_absorpt_correction_T_min  0.2667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         13954
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0362P)^2^+17.9447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                12612
_reflns_number_total             13954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8011469_si_001_3.cif
_cod_data_source_block           complex5
_cod_depositor_comments
;

2021-04-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_original_formula_moiety     '3(C32 H46 Cl2 N2 O8 Tb2),2(C4 H8 O)'
_cod_original_formula_sum        'C104 H154 Cl6 N6 O26 Tb6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     3070.55
_cod_database_code               4306304