#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/70/2017017.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2017017
loop_
_publ_author_name
'Muñoz, Juan Carlos'
'Atria, Ana María'
'Garland, Maria Teresa'
'Baggio, Ricardo'
_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-μ₃-itaconato-μ₂-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       'φ and ω'
_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/[σ²(Fo²)+(0.0517P)²+103.4472P] where  P=(Fo²+2Fc²)/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>2σ(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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd1 0.5000 0.21882(4) 0.2500 0.0331(2) Uani d SU 1 . .
Gd Gd2 0.5000 0.43946(3) 0.2500 0.01846(19) Uani d SU 1 . .
N N11 0.5779(8) 0.1029(6) 0.3113(13) 0.050(3) Uani d U 1 . .
C C11 0.6484(11) 0.1063(8) 0.3928(17) 0.060(4) Uani d U 1 . .
H H11 0.6760 0.1498 0.4030 0.073 Uiso calc R 1 . .
C C21 0.6816(13) 0.0458(11) 0.463(2) 0.080(5) Uani d U 1 . .
H H21 0.7330 0.0470 0.5135 0.097 Uiso calc R 1 . .
C C31 0.6368(13) -0.0141(11) 0.455(2) 0.085(6) Uani d U 1 . .
H H31 0.6532 -0.0528 0.5140 0.102 Uiso calc R 1 . .
C C41 0.5691(13) -0.0201(10) 0.366(2) 0.078(5) Uani d U 1 . .
H H41 0.5432 -0.0642 0.3529 0.093 Uiso calc R 1 . .
C C51 0.5372(8) 0.0409(7) 0.2915(15) 0.045(3) Uani d U 1 . .
O O12 0.5749(5) 0.4617(4) -0.1544(8) 0.0327(17) Uani d U 1 . .
O O22 0.5910(5) 0.4710(4) 0.0827(7) 0.0267(15) Uani d U 1 . .
O O32 0.5644(5) 0.3314(4) 0.1796(9) 0.0360(18) Uani d U 1 . .
O O42 0.6508(6) 0.2446(5) 0.2084(11) 0.054(3) Uani d U 1 . .
C C12 0.6088(6) 0.4432(5) -0.0358(11) 0.024(2) Uani d U 1 . .
C C22 0.6712(7) 0.3861(6) -0.0265(13) 0.032(2) Uani d U 1 . .
C C32 0.6989(8) 0.3539(7) 0.1154(14) 0.041(3) Uani d U 1 . .
H H32A 0.7127 0.3921 0.1842 0.050 Uiso calc R 1 . .
H H32B 0.7480 0.3261 0.1056 0.050 Uiso calc R 1 . .
C C42 0.6355(7) 0.3063(6) 0.1735(12) 0.033(2) Uani d U 1 . .
C C52 0.7024(10) 0.3670(8) -0.1438(17) 0.059(4) Uani d U 1 . .
H H52A 0.6854 0.3892 -0.2308 0.071 Uiso calc R 1 . .
H H52B 0.7419 0.3312 -0.1410 0.071 Uiso calc R 1 . .
O O13 0.5309(7) 0.1816(5) 0.0072(10) 0.060(3) Uani d U 1 . .
O O23 0.4288(6) 0.2548(4) 0.0199(9) 0.041(2) Uani d U 1 . .
C C13 0.4747(8) 0.2186(6) -0.0533(12) 0.038(3) Uani d U 1 . .
C C23 0.4674(8) 0.2241(6) -0.2172(14) 0.044(3) Uani d U 1 . .
C C53 0.4022(18) 0.2275(15) -0.269(3) 0.053(7) Uani d PU 0.50 . .
H H53A 0.3925 0.2307 -0.3688 0.064 Uiso calc PR 0.50 . .
H H53B 0.3586 0.2271 -0.2115 0.064 Uiso calc PR 0.50 . .
O O1W 0.5856(5) 0.3969(4) 0.4555(8) 0.0347(18) Uani d U 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O23 Gd1 O23 2_655 . 148.2(4) ?
O23 Gd1 O13 2_655 . 139.6(3) ?
O23 Gd1 O13 . . 52.7(3) ?
O23 Gd1 O13 2_655 2_655 52.7(3) ?
O23 Gd1 O13 . 2_655 139.6(3) ?
O13 Gd1 O13 . 2_655 147.2(5) ?
O23 Gd1 O32 2_655 2_655 73.6(3) ?
O23 Gd1 O32 . 2_655 79.3(3) ?
O13 Gd1 O32 . 2_655 127.8(3) ?
O13 Gd1 O32 2_655 2_655 82.5(3) ?
O23 Gd1 O32 2_655 . 79.3(3) ?
O23 Gd1 O32 . . 73.6(3) ?
O13 Gd1 O32 . . 82.5(3) ?
O13 Gd1 O32 2_655 . 127.8(3) ?
O32 Gd1 O32 2_655 . 63.2(4) ?
O23 Gd1 N11 2_655 2_655 128.4(3) ?
O23 Gd1 N11 . 2_655 81.0(4) ?
O13 Gd1 N11 . 2_655 72.2(4) ?
O13 Gd1 N11 2_655 2_655 80.0(3) ?
O32 Gd1 N11 2_655 2_655 124.2(3) ?
O32 Gd1 N11 . 2_655 151.7(3) ?
O23 Gd1 N11 2_655 . 81.0(4) ?
O23 Gd1 N11 . . 128.4(3) ?
O13 Gd1 N11 . . 80.0(3) ?
O13 Gd1 N11 2_655 . 72.2(4) ?
O32 Gd1 N11 2_655 . 151.7(3) ?
O32 Gd1 N11 . . 124.2(3) ?
N11 Gd1 N11 2_655 . 64.1(6) ?
O23 Gd1 O42 2_655 2_655 102.2(3) ?
O23 Gd1 O42 . 2_655 71.8(3) ?
O13 Gd1 O42 . 2_655 117.8(4) ?
O13 Gd1 O42 2_655 2_655 68.8(4) ?
O32 Gd1 O42 2_655 2_655 50.4(3) ?
O32 Gd1 O42 . 2_655 108.7(3) ?
N11 Gd1 O42 2_655 2_655 73.9(3) ?
N11 Gd1 O42 . 2_655 126.3(3) ?
O23 Gd1 O42 2_655 . 71.8(3) ?
O23 Gd1 O42 . . 102.2(3) ?
O13 Gd1 O42 . . 68.8(4) ?
O13 Gd1 O42 2_655 . 117.8(4) ?
O32 Gd1 O42 2_655 . 108.7(3) ?
O32 Gd1 O42 . . 50.4(3) ?
N11 Gd1 O42 2_655 . 126.3(3) ?
N11 Gd1 O42 . . 73.9(3) ?
O42 Gd1 O42 2_655 . 158.6(4) ?
O23 Gd1 C13 2_655 . 153.7(3) ?
O23 Gd1 C13 . . 26.4(3) ?
O13 Gd1 C13 . . 26.3(3) ?
O13 Gd1 C13 2_655 . 153.6(3) ?
O32 Gd1 C13 2_655 . 103.7(3) ?
O32 Gd1 C13 . . 76.4(3) ?
N11 Gd1 C13 2_655 . 75.3(4) ?
N11 Gd1 C13 . . 104.5(4) ?
O42 Gd1 C13 2_655 . 95.1(4) ?
O42 Gd1 C13 . . 84.9(4) ?
O23 Gd1 C13 2_655 2_655 26.4(3) ?
O23 Gd1 C13 . 2_655 153.7(3) ?
O13 Gd1 C13 . 2_655 153.6(3) ?
O13 Gd1 C13 2_655 2_655 26.3(3) ?
O32 Gd1 C13 2_655 2_655 76.4(3) ?
O32 Gd1 C13 . 2_655 103.7(3) ?
N11 Gd1 C13 2_655 2_655 104.5(4) ?
N11 Gd1 C13 . 2_655 75.3(4) ?
O42 Gd1 C13 2_655 2_655 84.9(4) ?
O42 Gd1 C13 . 2_655 95.1(4) ?
C13 Gd1 C13 . 2_655 179.8(5) ?
O22 Gd2 O22 2_655 . 150.7(3) ?
O22 Gd2 O12 2_655 5_665 73.0(2) ?
O22 Gd2 O12 . 5_665 83.9(3) ?
O22 Gd2 O12 2_655 6_566 83.9(3) ?
O22 Gd2 O12 . 6_566 73.0(2) ?
O12 Gd2 O12 5_665 6_566 76.6(4) ?
O22 Gd2 O32 2_655 2_655 72.9(2) ?
O22 Gd2 O32 . 2_655 136.2(2) ?
O12 Gd2 O32 5_665 2_655 122.3(3) ?
O12 Gd2 O32 6_566 2_655 141.9(3) ?
O22 Gd2 O32 2_655 . 136.2(2) ?
O22 Gd2 O32 . . 72.9(2) ?
O12 Gd2 O32 5_665 . 141.9(3) ?
O12 Gd2 O32 6_566 . 122.3(3) ?
O32 Gd2 O32 2_655 . 65.3(4) ?
O22 Gd2 O1W 2_655 2_655 104.4(3) ?
O22 Gd2 O1W . 2_655 85.3(3) ?
O12 Gd2 O1W 5_665 2_655 73.0(3) ?
O12 Gd2 O1W 6_566 2_655 144.1(3) ?
O32 Gd2 O1W 2_655 2_655 72.4(3) ?
O32 Gd2 O1W . 2_655 75.4(3) ?
O22 Gd2 O1W 2_655 . 85.3(3) ?
O22 Gd2 O1W . . 104.4(3) ?
O12 Gd2 O1W 5_665 . 144.1(3) ?
O12 Gd2 O1W 6_566 . 73.0(3) ?
O32 Gd2 O1W 2_655 . 75.4(3) ?
O32 Gd2 O1W . . 72.4(3) ?
O1W Gd2 O1W 2_655 . 141.5(4) ?
C51 N11 C11 . . 121.3(13) ?
C51 N11 Gd1 . . 117.7(9) ?
C11 N11 Gd1 . . 118.8(10) ?
N11 C11 C21 . . 121.0(17) ?
N11 C11 H11 . . 119.5 ?
C21 C11 H11 . . 119.5 ?
C31 C21 C11 . . 117(2) ?
C31 C21 H21 . . 121.3 ?
C11 C21 H21 . . 121.3 ?
C21 C31 C41 . . 122(2) ?
C21 C31 H31 . . 119.0 ?
C41 C31 H31 . . 119.0 ?
C31 C41 C51 . . 119.6(18) ?
C31 C41 H41 . . 120.2 ?
C51 C41 H41 . . 120.2 ?
N11 C51 C51 . 2_655 118.8(8) ?
N11 C51 C41 . . 117.9(14) ?
C51 C51 C41 2_655 . 123.1(11) ?
C12 O12 Gd2 . 5_665 137.3(7) ?
C12 O22 Gd2 . . 133.2(6) ?
C42 O32 Gd2 . . 139.1(8) ?
C42 O32 Gd1 . . 96.7(6) ?
Gd2 O32 Gd1 . . 115.7(3) ?
C42 O42 Gd1 . . 92.1(7) ?
O12 C12 O22 . . 122.5(9) ?
O12 C12 C22 . . 120.6(10) ?
O22 C12 C22 . . 117.0(9) ?
C52 C22 C12 . . 118.2(12) ?
C52 C22 C32 . . 121.7(12) ?
C12 C22 C32 . . 120.1(10) ?
C22 C32 C42 . . 112.9(11) ?
C22 C32 H32A . . 109.0 ?
C42 C32 H32A . . 109.0 ?
C22 C32 H32B . . 109.0 ?
C42 C32 H32B . . 109.0 ?
H32A C32 H32B . . 107.8 ?
O42 C42 O32 . . 120.5(11) ?
O42 C42 C32 . . 121.4(11) ?
O32 C42 C32 . . 118.0(10) ?
O42 C42 Gd1 . . 63.1(7) ?
O32 C42 Gd1 . . 57.6(6) ?
C32 C42 Gd1 . . 172.3(9) ?
C22 C52 H52A . . 120.0 ?
C22 C52 H52B . . 120.0 ?
H52A C52 H52B . . 120.0 ?
C13 O13 Gd1 . . 93.1(7) ?
C13 O23 Gd1 . . 93.6(8) ?
O13 C13 O23 . . 120.6(11) ?
O13 C13 C23 . . 118.7(10) ?
O23 C13 C23 . . 120.5(11) ?
O13 C13 Gd1 . . 60.6(6) ?
O23 C13 Gd1 . . 60.0(6) ?
C23 C13 Gd1 . . 174.4(9) ?
C53 C23 C23 . 2_654 127(2) ?
C53 C23 C13 . . 114.6(19) ?
C23 C23 C13 2_654 . 118.8(15) ?
C23 C53 H53A . . 120.0 ?
C23 C53 H53B . . 120.0 ?
H53A C53 H53B . . 120.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Gd1 O23 2_655 2.443(9) ?
Gd1 O23 . 2.443(9) y
Gd1 O13 . 2.456(9) y
Gd1 O13 2_655 2.456(9) ?
Gd1 O32 2_655 2.464(7) ?
Gd1 O32 . 2.464(7) y
Gd1 N11 2_655 2.551(11) ?
Gd1 N11 . 2.551(11) y
Gd1 O42 2_655 2.585(10) ?
Gd1 O42 . 2.585(10) y
Gd1 Gd2 . 4.1139(15) y
Gd2 O22 2_655 2.324(7) ?
Gd2 O22 . 2.324(7) y
Gd2 O12 5_665 2.348(8) y
Gd2 O12 6_566 2.348(8) ?
Gd2 O32 2_655 2.394(8) ?
Gd2 O32 . 2.394(8) y
Gd2 O1W 2_655 2.407(8) ?
Gd2 O1W . 2.407(8) y
N11 C51 . 1.339(17) ?
N11 C11 . 1.33(2) ?
C11 C21 . 1.39(2) ?
C11 H11 . 0.9300 ?
C21 C31 . 1.34(3) ?
C21 H21 . 0.9300 ?
C31 C41 . 1.33(3) ?
C31 H31 . 0.9300 ?
C41 C51 . 1.41(2) ?
C41 H41 . 0.9300 ?
C51 C51 2_655 1.39(3) ?
O12 C12 . 1.241(13) ?
O12 Gd2 5_665 2.348(8) ?
O22 C12 . 1.275(12) ?
O32 C42 . 1.264(13) ?
O42 C42 . 1.216(13) ?
C12 C22 . 1.476(14) ?
C22 C52 . 1.294(18) ?
C22 C32 . 1.485(16) ?
C32 C42 . 1.504(16) ?
C32 H32A . 0.9700 ?
C32 H32B . 0.9700 ?
C52 H52A . 0.9300 ?
C52 H52B . 0.9300 ?
O13 C13 . 1.248(16) ?
O23 C13 . 1.254(14) ?
C13 C23 . 1.522(17) ?
C23 C53 . 1.14(3) ?
C23 C23 2_654 1.28(3) ?
C53 H53A . 0.9300 ?
C53 H53B . 0.9300 ?
