Synthesis and Crystal Structure of a Terbium(III) Complex of Tris(2-(2-hydroxy-3-methylbenzylideneamino)ethyl)amine
NAGAHARA, Keiko; KANESATO, Masatoshi; SATO, Ken-ichi; GOTO, Midori; X-ray Structure Analysis Online 27 (2011) 9–; doi:10.2116/xraystruct.27.9

data_1551740
_publ_section_title
;
 Synthesis and Crystal Structure of a Terbium(III) Complex of
 Tris(2-(2-hydroxy-3-methylbenzylideneamino)ethyl)amine
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              9
_journal_paper_doi               10.2116/xraystruct.27.9
_journal_volume                  27
_journal_year                    2011
_chemical_formula_sum            'C30 H33 N4 O3 Tb'
_chemical_formula_weight         656.52
_chemical_name_systematic
' (tris(2-(3-methyl-2-oxy-benzylideneamino)ethyl)amine)terbium(III)'
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   12.2874(4)
_cell_length_b                   12.2874(4)
_cell_length_c                   10.8085(5)
_cell_measurement_reflns_used    7373
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.246
_cell_measurement_theta_min      2.686
_cell_volume                     1413.24(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8815
_diffrn_reflns_theta_full        26.22
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  563
_diffrn_standards_number         239
_exptl_absorpt_coefficient_mu    2.539
_exptl_absorpt_correction_T_max  0.7019
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+0.4415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0426
_reflns_number_gt                2132
_reflns_number_total             2186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            27_9_1.cif
_cod_data_source_block           natb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 6524 2018-11-02 12:15:13Z antanas 
;
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               1551740