Bis{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(iminomethylene)]diphenolato(1.5{-})-κ^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}terbium(III)
Xia, Hai-Tao; Liu, Yu-Fen; Yang, Shu-Ping; Wang, Da-Qi; Acta Crystallographica Section E 65 (2009) m201–; doi:10.1107/S1600536809001494

data_2220672
_publ_section_title
Bis{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(iminomethylene)]diphenolato(1.5{-})-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}terbium(III)
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m201
_journal_paper_doi               10.1107/S1600536809001494
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Tb (C18 H22.5 N2 O4)2]'
_chemical_formula_moiety         'C36 H45 N4 O8 Tb'
_chemical_formula_sum            'C36 H45 N4 O8 Tb'
_chemical_formula_weight         820.68
_chemical_name_systematic
;Bis{6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(iminomethylene)]diphenolato(1.5-)-
\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>'}terbium(III)
;
_space_group_IT_number           45
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.885(2)
_cell_length_b                   11.1407(10)
_cell_length_c                   14.0928(14)
_cell_measurement_reflns_used    3398
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.891
_cell_volume                     3436.0(6)
_computing_cell_refinement       '<i>SAINT</i> (Siemens, 1996)'
_computing_data_collection       '<i>SMART</i> (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Siemens SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7735
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.8006
_exptl_absorpt_correction_T_min  0.5331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.603
_refine_ls_abs_structure_details 'Flack (1983), 1230  Freidel pairs'
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2820
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0351P)^2^+45.2805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                1893
_reflns_number_total             2820
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2682.cif
_cod_data_source_block           I
_cod_database_code               2220672
_cod_database_fobs_code          2220672