Tris(6-carboxypyridine-2-carboxylato)terbium(III) 2.75-hydrate
Zebret, Soumaila; Besnard, Céline; Hamacek, Josef; Acta Crystallographica Section E 67 (2011) m968–m969; doi:10.1107/S1600536811024135

data_2230966
_publ_section_title
;
 Tris(6-carboxypyridine-2-carboxylato)terbium(III) 2.75-hydrate
;
_journal_coeditor_code           ZS2104
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m968
_journal_page_last               m969
_journal_paper_doi               10.1107/S1600536811024135
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Tb (C7 H4 N O4)3], 2.75H2 O'
_chemical_formula_moiety         'C21 H12 N3 O12 Tb, 2.75(H2 O)'
_chemical_formula_sum            'C21 H17.5 N3 O14.75 Tb'
_chemical_formula_weight         706.79
_chemical_name_systematic
;
Tris(6-carboxypyridine-2-carboxylato)terbium(III) 2.75-hydrate
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.0115(15)
_cell_length_b                   13.0115(15)
_cell_length_c                   9.4142(13)
_cell_measurement_reflns_used    4000
_cell_measurement_temperature    200
_cell_measurement_theta_max      32.06
_cell_measurement_theta_min      2.84
_cell_volume                     1380.3(3)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>, 2003'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3830
_diffrn_reflns_theta_full        25.328
_diffrn_reflns_theta_max         25.808
_diffrn_reflns_theta_min         2.819
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.63
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(Busing & Levy, 1957)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             694.85
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
;
_refine_diff_density_max         0.57
_refine_diff_density_min         -1.01
_refine_ls_abs_structure_details
;
Flack (1983), 679 Friedel pairs: the crystal is achiral.
;
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1566
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.0090615
_refine_ls_shift/su_mean         0.0011977
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w = 1/[\s^2^(Fo^2^) + (0.030P)^2^ + 8.38P] where P=(max(Fo^2^,0)
 + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0818
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                1464
_reflns_number_total             1569
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            zs2104.cif
_cod_data_source_block           I
_cod_original_cell_volume        1380.3(5)
_cod_database_code               2230966
_cod_database_fobs_code          2230966