Three lanthanide complexes derived from itaconic acid and 2,2'-bipyridine
Muñoz, Juan Carlos; Atria, Ana María; Garland, Maria Teresa; Baggio, Ricardo; Acta Crystallographica Section C 65 (2009) m121–m127; doi:10.1107/S0108270109002534

data_2017016
_publ_section_title
;
 Three lanthanide complexes derived from itaconic acid and
 2,2'-bipyridine
;
_journal_coeditor_code           SK3282
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m121
_journal_page_last               m127
_journal_paper_doi               10.1107/S0108270109002534
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Gd2 (C5 H4 O4)3 (C10 H8 N2)2] , 4H2 O'
_chemical_formula_moiety         'C35 H28 Gd2 N4 O12 , 4H2 O'
_chemical_formula_sum            'C35 H36 Gd2 N4 O16'
_chemical_formula_weight         1083.18
_chemical_name_systematic
;Poly[[bis(2,2'-bipyridine)-\m~4~-itaconato-di-\m~3~-itaconato-digadolinium(III)]
tetrahydrate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                71.60(3)
_cell_angle_beta                 82.32(3)
_cell_angle_gamma                68.39(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5507(19)
_cell_length_b                   12.598(3)
_cell_length_c                   17.582(4)
_cell_measurement_reflns_used    8754
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.01
_cell_volume                     1865.9(9)
_computing_cell_refinement       'SAINT-NT (Bruker, 2002)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        'SAINT-NT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL-NT (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL-NT (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.785
_diffrn_measurement_device_type  'Bruker SMART? CCD area-detector'
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.604
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         7.157
_refine_diff_density_min         -3.024
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         6922
_refine_ls_number_restraints     541
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0748
_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^)+(0.1319P)^2^+23.4752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2043
_reflns_number_gt                5639
_reflns_number_total             6922
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3282.cif
_cod_data_source_block           I
_cod_database_code               2017016
_cod_database_fobs_code          2017016