Synthesis and characterization of two isostructural 3<i>d</i>–4<i>f</i> coordination compounds based on pyridine-2,6-dicarboxylic acid and 4,4'-bipyridine
Han, Lizhi; Jin, Longyi; Wang, Enbo; Su, Zhongmin; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619006004

data_2021637
_publ_section_title
;
 Synthesis and characterization of two isostructural 3<i>d</i>--4<i>f</i>
 coordination compounds based on pyridine-2,6-dicarboxylic acid and
 4,4'-bipyridine
;
_journal_coeditor_code           LF3091
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619006004
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'(C10 H10 N2) [Co Tb2 (C7 H3 N O4)6 (C10 H9 N2)2 (H2 O)2], 8H2 O'
_chemical_formula_moiety
'C10 H10 N2 2+, C62 H40 Co N10 O26 Tb2 2-, 16(H2 O)'
_chemical_formula_sum            'C72 H82 Co N12 O42 Tb2'
_chemical_formula_weight         2164.26
_chemical_name_systematic
;4,4'-Bipyridine-1,1'-diium
diaquabis(\m~2~-pyridine-2,6-dicarboxylato)tetrakis(pyridine-2,6-dicarboxylato)bis[4-(pyridin-4-yl)pyridinium]cobalt(II)diterbium(III) octahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                98.5180(10)
_cell_angle_beta                 99.9010(10)
_cell_angle_gamma                102.7150(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8977(6)
_cell_length_b                   12.6490(6)
_cell_length_c                   14.8487(8)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     2106.78(19)
_computing_cell_refinement
;
APEX2 (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2006)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD APEXII'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12081
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.960
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1091
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.741
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         7395
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+2.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                6962
_reflns_number_total             7395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3091sup1.cif
_cod_data_source_block           Tb
_cod_database_code               2021637
_cod_database_fobs_code          2021637
_shelx_estimated_absorpt_t_min   0.651
_shelx_estimated_absorpt_t_max   0.695
_shelx_hkl_checksum              28706
_shelx_res_checksum              42292