#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/80/2228014.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_2228014
loop_
_publ_author_name
'Li, Zhi-Feng'
'Wang, Chun-Xiang'
_publ_section_title
;
 Poly[μ₆-adipato-diaquadi-μ₂-oxalato-digadolinium(III)]
;
_journal_coeditor_code           SU2209
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1263
_journal_paper_doi               10.1107/S1600536810036111
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Gd2 (C6 H8 O4) (C2 O4)2 (H2 O)2]'
_chemical_formula_moiety         'C10 H12 Gd2 O14'
_chemical_formula_sum            'C10 H12 Gd2 O14'
_chemical_formula_weight         670.70
_chemical_name_systematic
;
Poly[μ₆-adipato-diaquadi-μ₂-oxalato-digadolinium(III)]
;
_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           SHELXL-97
_cell_angle_alpha                104.759(10)
_cell_angle_beta                 108.110(10)
_cell_angle_gamma                104.320(7)
_cell_formula_units_Z            1
_cell_length_a                   6.815(4)
_cell_length_b                   6.982(4)
_cell_length_c                   8.997(7)
_cell_measurement_reflns_used    238
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.6
_cell_volume                     367.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1751
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    9.021
_exptl_absorpt_correction_T_max  0.491
_exptl_absorpt_correction_T_min  0.241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.028
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1236
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0226
_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)+(0.0451P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0591
_reflns_number_gt                1157
_reflns_number_total             1236
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            su2209.cif
_cod_data_source_block           I
_cod_database_code               2228014
_cod_database_fobs_code          2228014
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 Gd 0.15528(4) 0.34583(3) 0.36187(3) 0.01206(12) Uani d . 1 . .
O O1 0.1523(6) 0.5226(6) 0.6494(4) 0.0175(8) Uani d . 1 . .
O O2 0.4788(6) 0.5964(5) 0.6393(4) 0.0156(8) Uani d . 1 . .
O O3 0.2680(6) 0.1539(6) 0.5394(4) 0.0168(8) Uani d . 1 . .
O O4 0.1538(6) -0.0817(6) 0.6500(5) 0.0191(8) Uani d . 1 . .
O O5 -0.0130(7) 0.2517(6) 0.0669(4) 0.0191(8) Uani d . 1 . .
O O6 -0.1324(7) 0.0169(6) -0.1924(5) 0.0210(9) Uani d . 1 . .
O O7 0.2703(7) 0.6881(6) 0.3356(5) 0.0218(9) Uani d D 1 . .
H H7A 0.403(5) 0.763(10) 0.370(8) 0.033 Uiso d D 1 . .
H H7B 0.218(12) 0.757(10) 0.281(8) 0.033 Uiso d D 1 . .
C C1 0.3614(9) 0.6107(8) 0.7255(7) 0.0144(11) Uani d . 1 . .
C C2 0.4651(10) 0.7225(9) 0.9107(7) 0.0193(12) Uani d . 1 . .
H H2A 0.4012 0.8285 0.9405 0.023 Uiso calc PR 0.75 A 1
H H2B 0.6218 0.7953 0.9448 0.023 Uiso calc PR 0.75 A 1
H H2C 0.3517 0.7421 0.9503 0.023 Uiso d PR 0.25 A 2
H H2D 0.5696 0.8616 0.9373 0.023 Uiso d PR 0.25 A 2
C C3A 0.4343(15) 0.5720(14) 1.0070(10) 0.0262(17) Uani d P 0.75 . 1
H H3A1 0.4800 0.6550 1.1242 0.031 Uiso calc PR 0.75 . 1
H H3A2 0.2790 0.4864 0.9633 0.031 Uiso calc PR 0.75 . 1
C C3B 0.588(4) 0.598(4) 1.005(3) 0.0262(17) Uani d P 0.25 . 2
H H3B1 0.6830 0.5544 0.9531 0.031 Uiso calc PR 0.25 . 2
H H3B2 0.6791 0.6879 1.1213 0.031 Uiso calc PR 0.25 . 2
C C4 0.1222(8) 0.0203(8) 0.5547(6) 0.0140(11) Uani d . 1 . .
C C5 -0.0433(9) 0.0774(8) -0.0367(7) 0.0143(11) Uani d . 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'
Gd Gd -0.1653 3.9035 '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'
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
O5 Gd O4 . 2_556 89.95(13) ?
O5 Gd O3 . . 133.53(13) ?
O4 Gd O3 2_556 . 68.29(13) ?
O5 Gd O7 . . 78.95(14) ?
O4 Gd O7 2_556 . 142.92(13) ?
O3 Gd O7 . . 141.60(14) ?
O5 Gd O2 . 2_666 92.50(13) ?
O4 Gd O2 2_556 2_666 142.01(12) ?
O3 Gd O2 . 2_666 83.07(12) ?
O7 Gd O2 . 2_666 74.35(13) ?
O5 Gd O1 . 2_566 81.91(12) ?
O4 Gd O1 2_556 2_566 69.18(13) ?
O3 Gd O1 . 2_566 122.76(12) ?
O7 Gd O1 . 2_566 74.25(14) ?
O2 Gd O1 2_666 2_566 148.60(13) ?
O5 Gd O6 . 2 65.44(13) ?
O4 Gd O6 2_556 2 70.90(14) ?
O3 Gd O6 . 2 68.66(13) ?
O7 Gd O6 . 2 131.77(14) ?
O2 Gd O6 2_666 2 75.79(13) ?
O1 Gd O6 2_566 2 127.57(13) ?
O5 Gd O2 . . 147.43(13) ?
O4 Gd O2 2_556 . 122.50(13) ?
O3 Gd O2 . . 69.27(13) ?
O7 Gd O2 . . 73.02(13) ?
O2 Gd O2 2_666 . 64.38(14) ?
O1 Gd O2 2_566 . 105.56(12) ?
O6 Gd O2 2 . 124.28(12) ?
O5 Gd O1 . . 147.09(13) ?
O4 Gd O1 2_556 . 80.01(13) ?
O3 Gd O1 . . 71.21(13) ?
O7 Gd O1 . . 90.34(13) ?
O2 Gd O1 2_666 . 114.63(12) ?
O1 Gd O1 2_566 . 65.20(14) ?
O6 Gd O1 2 . 136.78(12) ?
O2 Gd O1 . . 50.45(12) ?
O5 Gd C1 . . 159.72(13) ?
O4 Gd C1 2_556 . 100.86(14) ?
O3 Gd C1 . . 66.75(14) ?
O7 Gd C1 . . 82.15(15) ?
O2 Gd C1 2_666 . 89.45(14) ?
O1 Gd C1 2_566 . 85.94(14) ?
O6 Gd C1 2 . 134.31(13) ?
O2 Gd C1 . . 25.31(13) ?
O1 Gd C1 . . 25.21(14) ?
C1 O1 Gd . 2_566 133.0(3) ?
C1 O1 Gd . . 95.4(3) ?
Gd O1 Gd 2_566 . 114.80(14) ?
C1 O2 Gd . 2_666 147.7(3) ?
C1 O2 Gd . . 95.5(3) ?
Gd O2 Gd 2_666 . 115.62(14) ?
C4 O3 Gd . . 118.6(3) ?
C4 O4 Gd . 2_556 119.1(3) ?
C5 O5 Gd . . 123.7(3) ?
C5 O6 Gd . 2 117.9(3) ?
Gd O7 H7A . . 122(5) ?
Gd O7 H7B . . 139(5) ?
H7A O7 H7B . . 97(7) ?
O1 C1 O2 . . 118.3(5) ?
O1 C1 C2 . . 120.4(5) ?
O2 C1 C2 . . 121.2(5) ?
O1 C1 Gd . . 59.4(3) ?
O2 C1 Gd . . 59.1(3) ?
C2 C1 Gd . . 174.0(4) ?
C1 C2 C3A . . 112.9(5) ?
C1 C2 C3B . . 112.6(10) ?
C1 C2 H2A . . 109.0 ?
C3A C2 H2A . . 109.0 ?
C3B C2 H2A . . 135.3 ?
C1 C2 H2B . . 109.0 ?
C3A C2 H2B . . 109.0 ?
C3B C2 H2B . . 73.4 ?
H2A C2 H2B . . 107.8 ?
C1 C2 H2C . . 109.1 ?
C3A C2 H2C . . 73.3 ?
C3B C2 H2C . . 109.1 ?
H2B C2 H2C . . 136.9 ?
C1 C2 H2D . . 109.1 ?
C3A C2 H2D . . 134.9 ?
C3B C2 H2D . . 109.1 ?
H2C C2 H2D . . 107.8 ?
C3A C3A C2 2_667 . 112.2(8) ?
C3A C3A H2C 2_667 . 148.3 ?
C3A C3A H3A1 2_667 . 109.2 ?
C2 C3A H3A1 . . 109.2 ?
H2C C3A H3A1 . . 91.7 ?
C3A C3A H3A2 2_667 . 109.2 ?
C2 C3A H3A2 . . 109.2 ?
H2C C3A H3A2 . . 85.5 ?
H3A1 C3A H3A2 . . 107.9 ?
C3B C3B C2 2_667 . 108(2) ?
C3B C3B H3B1 2_667 . 110.1 ?
C2 C3B H3B1 . . 110.1 ?
C3B C3B H3B2 2_667 . 110.1 ?
C2 C3B H3B2 . . 110.1 ?
H3B1 C3B H3B2 . . 108.4 ?
O4 C4 O3 . . 126.3(5) ?
O4 C4 C4 . 2_556 117.1(6) ?
O3 C4 C4 . 2_556 116.6(6) ?
O6 C5 O5 . . 127.0(5) ?
O6 C5 C5 . 2 116.6(6) ?
O5 C5 C5 . 2 116.4(6) ?
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
Gd O1 . 2.575(4) no
Gd O1 2_566 2.473(4) no
Gd O2 . 2.569(4) no
Gd O2 2_666 2.430(4) no
Gd O3 . 2.403(4) no
Gd O4 2_556 2.385(4) no
Gd O5 . 2.374(4) no
Gd O6 2 2.540(4) no
Gd O7 . 2.420(4) no
O1 C1 . 1.274(7) ?
O2 C1 . 1.279(6) ?
O3 C4 . 1.252(7) ?
O4 C4 . 1.249(6) ?
O5 C5 . 1.253(6) ?
O6 C5 . 1.246(7) ?
O7 H7A . 0.84(6) ?
O7 H7B . 0.83(7) ?
C1 C2 . 1.489(8) ?
C2 C3A . 1.538(10) ?
C2 C3B . 1.57(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C2 H2C . 0.9700 ?
C2 H2D . 0.9700 ?
C3A C3A 2_667 1.510(16) ?
C3A H3A1 . 0.9700 ?
C3A H3A2 . 0.9700 ?
C3B C3B 2_667 1.54(5) ?
C3B H3B1 . 0.9700 ?
C3B H3B2 . 0.9700 ?
C4 C4 2_556 1.558(10) ?
C5 C5 2 1.546(10) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O7 H7A O3 . . 2_666 0.84(6) 2.00(5) 2.799(4) 160 yes
O7 H7B O6 . . 2_565 0.83(7) 2.07(7) 2.888(5) 168 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O5 Gd O1 C1 . . . . -140.5(3) ?
O4 Gd O1 C1 2_556 . . . 145.4(3) ?
O3 Gd O1 C1 . . . . 75.1(3) ?
O7 Gd O1 C1 . . . . -70.5(3) ?
O2 Gd O1 C1 2_666 . . . 2.4(3) ?
O1 Gd O1 C1 2_566 . . . -143.0(4) ?
O6 Gd O1 C1 2 . . . 97.7(3) ?
O2 Gd O1 C1 . . . . -3.1(3) ?
O5 Gd O1 Gd . . . 2_566 2.5(3) ?
O4 Gd O1 Gd 2_556 . . 2_566 -71.57(16) ?
O3 Gd O1 Gd . . . 2_566 -141.88(18) ?
O7 Gd O1 Gd . . . 2_566 72.44(17) ?
O2 Gd O1 Gd 2_666 . . 2_566 145.34(15) ?
O1 Gd O1 Gd 2_566 . . 2_566 -0.001(2) ?
O6 Gd O1 Gd 2 . . 2_566 -119.29(18) ?
O2 Gd O1 Gd . . . 2_566 139.9(2) ?
C1 Gd O1 Gd . . . 2_566 143.0(4) ?
O5 Gd O2 C1 . . . . 139.9(3) ?
O4 Gd O2 C1 2_556 . . . -34.5(3) ?
O3 Gd O2 C1 . . . . -79.2(3) ?
O7 Gd O2 C1 . . . . 108.2(3) ?
O2 Gd O2 C1 2_666 . . . -171.4(4) ?
O1 Gd O2 C1 2_566 . . . 40.5(3) ?
O6 Gd O2 C1 2 . . . -122.4(3) ?
O1 Gd O2 C1 . . . . 3.1(3) ?
O5 Gd O2 Gd . . . 2_666 -48.6(3) ?
O4 Gd O2 Gd 2_556 . . 2_666 136.96(15) ?
O3 Gd O2 Gd . . . 2_666 92.21(16) ?
O7 Gd O2 Gd . . . 2_666 -80.42(17) ?
O2 Gd O2 Gd 2_666 . . 2_666 0.0 ?
O1 Gd O2 Gd 2_566 . . 2_666 -148.11(15) ?
O6 Gd O2 Gd 2 . . 2_666 49.0(2) ?
O1 Gd O2 Gd . . . 2_666 174.5(2) ?
C1 Gd O2 Gd . . . 2_666 171.4(4) ?
O5 Gd O3 C4 . . . . -72.7(4) ?
O4 Gd O3 C4 2_556 . . . -5.0(4) ?
O7 Gd O3 C4 . . . . 146.7(3) ?
O2 Gd O3 C4 2_666 . . . -159.5(4) ?
O1 Gd O3 C4 2_566 . . . 39.7(4) ?
O6 Gd O3 C4 2 . . . -82.1(4) ?
O2 Gd O3 C4 . . . . 135.3(4) ?
O1 Gd O3 C4 . . . . 81.5(4) ?
C1 Gd O3 C4 . . . . 108.1(4) ?
O4 Gd O5 C5 2_556 . . . -67.3(4) ?
O3 Gd O5 C5 . . . . -8.0(5) ?
O7 Gd O5 C5 . . . . 148.3(4) ?
O2 Gd O5 C5 2_666 . . . 74.8(4) ?
O1 Gd O5 C5 2_566 . . . -136.2(4) ?
O6 Gd O5 C5 2 . . . 1.7(4) ?
O2 Gd O5 C5 . . . . 117.5(4) ?
O1 Gd O5 C5 . . . . -138.6(4) ?
C1 Gd O5 C5 . . . . 170.0(4) ?
Gd O1 C1 O2 2_566 . . . -126.2(4) ?
Gd O1 C1 O2 . . . . 5.5(5) ?
Gd O1 C1 C2 2_566 . . . 55.3(6) ?
Gd O1 C1 C2 . . . . -173.1(4) ?
Gd O1 C1 Gd 2_566 . . . -131.6(4) ?
Gd O2 C1 O1 2_666 . . . -170.9(4) ?
Gd O2 C1 O1 . . . . -5.5(5) ?
Gd O2 C1 C2 2_666 . . . 7.6(9) ?
Gd O2 C1 C2 . . . . 173.0(4) ?
Gd O2 C1 Gd 2_666 . . . -165.4(6) ?
O5 Gd C1 O1 . . . . 86.4(5) ?
O4 Gd C1 O1 2_556 . . . -34.7(3) ?
O3 Gd C1 O1 . . . . -95.2(3) ?
O7 Gd C1 O1 . . . . 107.9(3) ?
O2 Gd C1 O1 2_666 . . . -177.9(3) ?
O1 Gd C1 O1 2_566 . . . 33.2(3) ?
O6 Gd C1 O1 2 . . . -108.5(3) ?
O2 Gd C1 O1 . . . . 174.4(5) ?
O5 Gd C1 O2 . . . . -88.0(5) ?
O4 Gd C1 O2 2_556 . . . 150.9(3) ?
O3 Gd C1 O2 . . . . 90.4(3) ?
O7 Gd C1 O2 . . . . -66.5(3) ?
O2 Gd C1 O2 2_666 . . . 7.7(3) ?
O1 Gd C1 O2 2_566 . . . -141.2(3) ?
O6 Gd C1 O2 2 . . . 77.1(3) ?
O1 Gd C1 O2 . . . . -174.4(5) ?
O1 C1 C2 C3A . . . . 66.3(7) ?
Gd O4 C4 O3 2_556 . . . -175.4(4) ?
Gd O4 C4 C4 2_556 . . 2_556 5.3(7) ?
Gd O3 C4 O4 . . . . -175.0(4) ?
Gd O3 C4 C4 . . . 2_556 4.3(7) ?
Gd O6 C5 O5 2 . . . 178.4(4) ?
Gd O6 C5 C5 2 . . 2 -0.3(7) ?
Gd O5 C5 O6 . . . . 179.1(4) ?
Gd O5 C5 C5 . . . 2 -2.1(8) ?
