Bis[4,4,5,5-tetramethyl-2-(pyridin-2-yl-κ^2^<i>N</i>)imidazoline-1-oxyl 3-oxide-κ<i>O</i>]tris(nitrato-κ^2^<i>O</i>,<i>O</i>')terbium(III)
Li, Dong-jiao; Acta Crystallographica Section E 68 (2012) m1341–; doi:10.1107/S1600536812040287

data_2236485
_publ_section_title
;
 Bis[4,4,5,5-tetramethyl-2-(pyridin-2-yl-\k^2^<i>N</i>)imidazoline-1-oxyl
 3-oxide-\k<i>O</i>]tris(nitrato-\k^2^<i>O</i>,<i>O</i>')terbium(III)
;
_journal_coeditor_code           MW2078
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1341
_journal_paper_doi               10.1107/S1600536812040287
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Tb (N O3)3 (C12 H16 N3 O2)2]'
_chemical_formula_moiety         'C24 H32 N9 O13 Tb'
_chemical_formula_sum            'C24 H32 N9 O13 Tb'
_chemical_formula_weight         813.51
_chemical_name_systematic
;
Bis[4,4,5,5-tetramethyl-2-(pyridin-2-yl-\k^2^<i>N</i>)imidazoline-1-oxyl
3-oxide-\k<i>O</i>]tris(nitrato-\k^2^<i>O</i>,<i>O</i>')terbium(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.292(3)
_cell_length_b                   11.114(2)
_cell_length_c                   23.264(5)
_cell_measurement_reflns_used    9251
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8864
_cell_measurement_theta_min      3.00
_cell_volume                     3144.3(12)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn CCD area-detector'
_diffrn_measurement_method       '\w--\q scans'
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25443
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.327
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.945
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                4726
_reflns_number_total             5554
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            mw2078.cif
_cod_data_source_block           I
_cod_original_cell_volume        3144.6(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2236485
_cod_database_fobs_code          2236485