Crystal structure of an eight-coordinate terbium(III) ion chelated by <i>N</i>,<i>N</i>'-bis(2-hydroxybenzyl)-<i>N</i>,<i>N</i>'-bis(pyridin-2-ylmethyl)ethylenediamine (bbpen^2{-^}) and nitrate
Gregório, Thaiane; Rüdiger, André Luis; Nunes, Giovana G.; Soares, Jaísa F.; Hughes, David L.; Acta Crystallographica Section E 71 (2015) 65–68; doi:10.1107/S2056989014026826

data_2240315
_publ_section_title
;
 Crystal structure of an eight-coordinate terbium(III) ion chelated by
 <i>N</i>,<i>N</i>'-bis(2-hydroxybenzyl)-<i>N</i>,<i>N</i>'-bis(pyridin-2-ylmethyl)ethylenediamine
 (bbpen^2{-^}) and nitrate
;
_journal_coeditor_code           LH5741
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              65
_journal_page_last               68
_journal_paper_doi               10.1107/S2056989014026826
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Tb (C28 H28 N4 O2) (N O3)]'
_chemical_formula_moiety         'C28 H28 N5 O5 Tb'
_chemical_formula_structural     'Terbium complex'
_chemical_formula_sum            'C28 H28 N5 O5 Tb'
_chemical_formula_weight         673.47
_chemical_name_systematic
'[<i>N</i>,<i>N</i>'-Bis(2-oxidobenzyl-\k<i>O</i>)-<i>N</i>,<i>N</i>'-bis(pyridin-2-ylmethyl-\k<i>N</i>)ethylenediamine-\k^2^<i>N</i>,<i>N</i>'](nitrato-\k^2^<i>O</i>,<i>O</i>')terbium(III)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5947(6)
_cell_length_b                   18.2401(17)
_cell_length_c                   16.9272(13)
_cell_measurement_reflns_used    9558
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.88
_cell_volume                     2653.6(4)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) and ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2008) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            75009
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_min         2.883
_exptl_absorpt_coefficient_mu    2.713
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS2014/2; Bruker, 2014)
;
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.301
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1431 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.0107(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0105
_refine_ls_R_factor_gt           0.0102
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+1.0428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0265
_refine_ls_wR_factor_ref         0.0266
_reflns_number_gt                3289
_reflns_number_total             3320
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5741sup1.cf
_cod_data_source_block           I
_cod_database_code               2240315
_cod_database_fobs_code          2240315
_shelx_estimated_absorpt_t_min   0.387
_shelx_estimated_absorpt_t_max   0.618
_shelx_hkl_checksum              58903
_shelx_res_checksum              4226
_shelxl_version_number           .2013