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_2017018
_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          '[Ho2 (C5 H4 O4)3 (C10 H8 N2)2] , 2H2 O'
_chemical_formula_moiety         'C35 H28 Ho2 N4 O12 , 2H2 O'
_chemical_formula_sum            'C35 H32 Ho2 N4 O14'
_chemical_formula_weight         1062.51
_chemical_name_systematic
;
poly[[bis(2,2'-bipyridine)-\m~4~-itaconato-di-\m~3~-itaconato-diholmium(III)]
dihydrate]
;
_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                 114.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.023(5)
_cell_length_b                   9.3994(19)
_cell_length_c                   18.229(4)
_cell_measurement_reflns_used    8672
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.02
_cell_volume                     3912.8(17)
_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 0.928
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15034
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.80
_diffrn_reflns_theta_min         1.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.085
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         10.214
_refine_diff_density_min         -3.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4299
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0788
_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^)+(0.1590P)^2^+95.0201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2232
_reflns_number_gt                3770
_reflns_number_total             4299
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3282.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2017018
_cod_database_fobs_code          2017018