Poly[[aqua-μ~3~-picolinato-μ~2~-picolinato-dipicolinatopotassium(I)terbium(III)] 2.5-hydrate]
Cunha-Silva, Luís; Soares-Santos, Paula C. R.; Nogueira, Helena I. S.; Trindade, Tito; Klinowski, Jacek; Rocha, João; Almeida Paz, Filipe A.; Acta Crystallographica Section E 64 (2008) m529–m530; doi:10.1107/S1600536808005758

data_2217894
_publ_section_title
;Poly[[aqua-\m~3~-picolinato-\m~2~-picolinato-dipicolinatopotassium(I)terbium(III)]
 2.5-hydrate]
;
_journal_coeditor_code           CV2369
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m529
_journal_page_last               m530
_journal_paper_doi               10.1107/S1600536808005758
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[K Tb (C6 H4 N O2)4 (H2 O)], 2.5H2 O'
_chemical_formula_moiety         'C24 H18 K1 N4 O9 Tb1, 2.5(H2 O)'
_chemical_formula_sum            'C24 H23 K N4 O11.5 Tb'
_chemical_formula_weight         1498.97
_chemical_name_systematic
;
Poly[[aqua-\m~3~-picolinato-\m~2~-picolinato-
dipicolinatopotassium(I)terbium(III)] 2.5-hydrate]
;
_space_group_IT_number           179
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXTL, manual editing plus enCIFer'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   12.7187(2)
_cell_length_b                   12.7187(2)
_cell_length_c                   62.2321(9)
_cell_measurement_reflns_used    28400
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.02
_cell_volume                     8718.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            31023
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.642
_exptl_absorpt_correction_T_max  0.5818
_exptl_absorpt_correction_T_min  0.4257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4452
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.700
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.020(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+2.1846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                4488
_reflns_number_total             5031
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2369.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C24 H23 K1 N4 O11.5 Tb1'
_cod_database_code               2217894
_cod_database_fobs_code          2217894