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_2017017
_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) (H2 O)2]'
_chemical_formula_moiety         'C25 H24 Gd2 N2 O14'
_chemical_formula_sum            'C25 H24 Gd2 N2 O14'
_chemical_formula_weight         890.96
_chemical_name_systematic
;
Poly[diaqua(2,2'-bipyridine)di-\m~3~-itaconato-\m~2~-itaconato-
digadolinium(III)]
;
_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                 94.949(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.427(5)
_cell_length_b                   18.645(5)
_cell_length_c                   9.300(3)
_cell_measurement_reflns_used    8794
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.88
_cell_measurement_theta_min      1.90
_cell_volume                     2837.8(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.923
_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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9298
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.833
_refine_diff_density_min         -4.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3098
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0517P)^2^+103.4472P] where  P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                2689
_reflns_number_total             3098
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3282.cif
_cod_data_source_block           II
_cod_original_cell_volume        2837.7(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2017017
_cod_database_fobs_code          2017017