Tetrakis(1,10-phenanthroline)bis(μ-pyridine-2,6-dicarboxylato)(pyridine-2,6-dicarboxylato)dicopper(II)terbium(III) nitrate tetrahydrate
Zhang, Wei; Acta Crystallographica Section E 68 (2012) m1084–m1085; doi:10.1107/S1600536812031686

data_2235812
_publ_section_title
;
 Tetrakis(1,10-phenanthroline)bis(\m-pyridine-2,6-dicarboxylato)(pyridine-2,6-dicarboxylato)dicopper(II)terbium(III)
 nitrate tetrahydrate
;
_journal_coeditor_code           GK2483
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1084
_journal_page_last               m1085
_journal_paper_doi               10.1107/S1600536812031686
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Cu2 Tb (C7 H3 N O4)3 (C12 H8 N2)4] N O3 , 4H2 O'
_chemical_formula_moiety         'C69 H41 Cu2 N11 O12 Tb +, N O3 -, 4(H2 O)'
_chemical_formula_sum            'C69 H49 Cu2 N12 O19 Tb'
_chemical_formula_weight         1636.20
_chemical_name_systematic
;
Tetrakis(1,10-phenanthroline)-
1\k^4^<i>N</i>,<i>N</i>';3\k^4^<i>N</i>,<i>N</i>'-bis(\m-pyridine-2,6-
dicarboxylato)-1:2\k^5^<i>O</i>^2^,<i>O</i>^2'^:
<i>O</i>^2^,<i>N</i>,<i>O</i>^6^;2:3\k^5^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^:
<i>O</i>^6^,<i>O</i>^6-^-(pyridine-2,6-dicarboxylato)-
2\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^-1,3-dicopper(II)-2-terbium(III)
nitrate tetrahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.289(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.058(4)
_cell_length_b                   19.574(5)
_cell_length_c                   19.927(5)
_cell_measurement_reflns_used    5232
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.32
_cell_volume                     6600(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17945
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  0.7757
_exptl_absorpt_correction_T_min  0.7280
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6454
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0792P)^2^+8.9094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                4952
_reflns_number_total             6454
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2483.cif
_cod_data_source_block           I
_cod_original_cell_volume        6599(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2235812
_cod_database_fobs_code          2235812