#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/01/2240196.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_2240196
loop_
_publ_author_name
'Li, Zhi-Feng'
'Zhang, Yi-Chao'
'Hu, Xiao-Qin'
'Wang, Chun-Xiang'
_publ_section_title
;
 Crystal structure of
 poly[μ₆-adipato-diaquadi-μ₂-oxalato-didysprosium(III)]
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m399
_journal_page_last               m400
_journal_paper_doi               10.1107/S1600536814024544
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Dy2 (C6 H8 O4) (C2 O4)2 (H2 O)2]'
_chemical_formula_moiety         'C10 H12 Dy2 O14'
_chemical_formula_sum            'C10 H12 Dy2 O14'
_chemical_formula_weight         681.20
_chemical_name_systematic
;
Poly[μ₆-adipato-diaquadi-μ₂-oxalato-didysprosium(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                104.916(5)
_cell_angle_beta                 108.069(4)
_cell_angle_gamma                104.306(4)
_cell_formula_units_Z            1
_cell_length_a                   6.772(2)
_cell_length_b                   6.929(2)
_cell_length_c                   8.949(3)
_cell_measurement_reflns_used    198
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      4.6
_cell_volume                     360.50(19)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1813
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    10.369
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.446
_refine_ls_extinction_coef       0.0039(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0213
_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)+(0.0422P)²+0.1716P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                1179
_reflns_number_total             1234
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2622sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        360.5(2)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               2240196
_cod_database_fobs_code          2240196
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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy Dy 0.15576(3) 0.34496(3) 0.36280(2) 0.01182(14) Uani d . 1 1 . .
O O1 0.1519(6) 0.5222(6) 0.6470(4) 0.0145(7) Uani d . 1 1 . .
O O2 0.4801(6) 0.5972(6) 0.6395(4) 0.0162(8) Uani d . 1 1 . .
O O3 0.2699(6) 0.1546(6) 0.5391(4) 0.0154(8) Uani d . 1 1 . .
O O4 0.1535(6) -0.0812(6) 0.6512(5) 0.0181(8) Uani d . 1 1 . .
O O5 -0.0072(6) 0.2564(6) 0.0712(4) 0.0172(8) Uani d . 1 1 . .
O O6 -0.1314(7) 0.0203(6) -0.1913(5) 0.0201(8) Uani d . 1 1 . .
O O7 0.2677(6) 0.6848(6) 0.3381(5) 0.0206(8) Uani d . 1 1 . .
H H7A 0.4060 0.7539 0.3786 0.031 Uiso d . 1 1 . .
H H7B 0.1863 0.7472 0.2931 0.031 Uiso d . 1 1 . .
C C1 0.3632(9) 0.6131(8) 0.7234(6) 0.0135(11) Uani d . 1 1 . .
C C2 0.4635(9) 0.7252(9) 0.9114(7) 0.0178(12) Uani d . 1 1 . .
H H2A 0.3960 0.8298 0.9403 0.021 Uiso calc R 1 1 A 1
H H2B 0.6211 0.8016 0.9479 0.021 Uiso calc R 1 1 A 1
C C3A 0.4334(12) 0.5740(12) 1.0066(9) 0.0162(14) Uani d P 0.75 1 . 1
H H3A1 0.2770 0.4877 0.9624 0.019 Uiso calc PR 0.75 1 . 1
H H3A2 0.4788 0.6577 1.1245 0.019 Uiso calc PR 0.75 1 . 1
C C3B 0.576(4) 0.593(4) 1.005(3) 0.0162(14) Uani d P 0.25 1 . 2
H H3B1 0.6770 0.5536 0.9564 0.019 Uiso calc PR 0.25 1 . 2
H H3B2 0.6640 0.6824 1.1227 0.019 Uiso calc PR 0.25 1 . 2
C C4 0.1215(8) 0.0215(7) 0.5549(6) 0.0127(10) Uani d . 1 1 . .
C C5 -0.0395(8) 0.0806(8) -0.0350(7) 0.0150(11) Uani d . 1 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'
Dy Dy -0.1892 4.4098 '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
O5 Dy O4 . 2_556 90.45(13)
O5 Dy O3 . . 134.27(12)
O4 Dy O3 2_556 . 68.93(12)
O5 Dy O7 . . 78.20(13)
O4 Dy O7 2_556 . 142.35(13)
O3 Dy O7 . . 141.46(12)
O5 Dy O2 . 2_666 91.79(12)
O4 Dy O2 2_556 2_666 142.20(13)
O3 Dy O2 . 2_666 82.95(12)
O7 Dy O2 . 2_666 74.65(13)
O5 Dy O1 . 2_566 82.15(12)
O4 Dy O1 2_556 2_566 69.07(12)
O3 Dy O1 . 2_566 122.91(11)
O7 Dy O1 . 2_566 73.84(12)
O2 Dy O1 2_666 2_566 148.49(12)
O5 Dy O6 . 2 65.84(12)
O4 Dy O6 2_556 2 70.76(13)
O3 Dy O6 . 2 68.84(12)
O7 Dy O6 . 2 132.07(13)
O2 Dy O6 2_666 2 75.88(12)
O1 Dy O6 2_566 2 127.55(12)
O5 Dy O1 . . 146.78(12)
O4 Dy O1 2_556 . 80.36(12)
O3 Dy O1 . . 71.64(12)
O7 Dy O1 . . 89.76(13)
O2 Dy O1 2_666 . 114.93(11)
O1 Dy O1 2_566 . 64.72(14)
O6 Dy O1 2 . 137.19(12)
O5 Dy O2 . . 146.25(12)
O4 Dy O2 2_556 . 123.15(12)
O3 Dy O2 . . 69.30(12)
O7 Dy O2 . . 72.79(13)
O2 Dy O2 2_666 . 64.34(13)
O1 Dy O2 2_566 . 105.43(11)
O6 Dy O2 2 . 124.52(12)
O1 Dy O2 . . 50.76(11)
O5 Dy C1 . . 158.48(13)
O4 Dy C1 2_556 . 101.76(14)
O3 Dy C1 . . 67.18(13)
O7 Dy C1 . . 81.38(14)
O2 Dy C1 2_666 . 89.29(13)
O1 Dy C1 2_566 . 85.74(13)
O6 Dy C1 2 . 134.90(13)
O1 Dy C1 . . 25.66(13)
O2 Dy C1 . . 25.14(13)
C1 O1 Dy . 2_566 132.5(3)
C1 O1 Dy . . 95.2(3)
Dy O1 Dy 2_566 . 115.28(14)
C1 O2 Dy . 2_666 148.4(3)
C1 O2 Dy . . 95.1(3)
Dy O2 Dy 2_666 . 115.66(13)
C4 O3 Dy . . 117.8(3)
C4 O4 Dy . 2_556 118.7(3)
C5 O5 Dy . . 123.8(3)
C5 O6 Dy . 2 117.5(3)
Dy O7 H7A . . 116.9
Dy O7 H7B . . 128.4
H7A O7 H7B . . 114.8
O2 C1 O1 . . 118.8(5)
O2 C1 C2 . . 122.2(5)
O1 C1 C2 . . 119.0(4)
O2 C1 Dy . . 59.8(3)
O1 C1 Dy . . 59.1(2)
C2 C1 Dy . . 173.1(4)
C1 C2 C3A . . 113.3(5)
C1 C2 C3B . . 111.8(9)
C1 C2 H2A . . 108.9
C3A C2 H2A . . 108.9
C3B C2 H2A . . 134.9
C1 C2 H2B . . 108.9
C3A C2 H2B . . 108.9
C3B C2 H2B . . 76.5
H2A C2 H2B . . 107.7
C2 C3A C3A . 2_667 113.2(7)
C2 C3A H3A1 . . 108.9
C3A C3A H3A1 2_667 . 108.9
C2 C3A H3A2 . . 108.9
C3A C3A H3A2 2_667 . 108.9
H3A1 C3A H3A2 . . 107.8
C3B C3B C2 2_667 . 113(2)
C3B C3B H3B1 2_667 . 108.9
C2 C3B H3B1 . . 108.9
C3B C3B H3B2 2_667 . 108.9
C2 C3B H3B2 . . 108.9
H3B1 C3B H3B2 . . 107.7
O4 C4 O3 . . 125.9(5)
O4 C4 C4 . 2_556 116.9(5)
O3 C4 C4 . 2_556 117.2(5)
O6 C5 O5 . . 127.2(5)
O6 C5 C5 . 2 116.0(6)
O5 C5 C5 . 2 116.8(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Dy O5 . 2.336(4)
Dy O4 2_556 2.360(4)
Dy O3 . 2.376(4)
Dy O7 . 2.379(4)
Dy O2 2_666 2.406(3)
Dy O1 2_566 2.464(4)
Dy O6 2 2.535(4)
Dy O1 . 2.535(3)
Dy O2 . 2.552(4)
O1 C1 . 1.279(7)
O2 C1 . 1.255(6)
O3 C4 . 1.256(6)
O4 C4 . 1.253(6)
O5 C5 . 1.256(6)
O6 C5 . 1.245(7)
O6 Dy 2 2.535(4)
O7 H7A . 0.8468
O7 H7B . 0.8496
C1 C2 . 1.501(7)
C2 C3A . 1.525(9)
C2 C3B . 1.57(2)
C2 H2A . 0.9700
C2 H2B . 0.9700
C3A C3A 2_667 1.529(14)
C3A H3A1 . 0.9700
C3A H3A2 . 0.9700
C3B C3B 2_667 1.40(4)
C3B H3B1 . 0.9700
C3B H3B2 . 0.9700
C4 C4 2_556 1.538(10)
C5 C5 2 1.540(11)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_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 0.85 1.96 2.787(4) 166 yes
O7 H7B O6 2_565 0.85 2.10 2.883(5) 153 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_4
_geom_torsion
O5 Dy O1 C1 . . -138.0(3)
O4 Dy O1 C1 2_556 . 146.2(3)
O3 Dy O1 C1 . . 75.4(3)
O7 Dy O1 C1 . . -70.3(3)
O2 Dy O1 C1 2_666 . 2.6(3)
O1 Dy O1 C1 2_566 . -142.5(4)
O6 Dy O1 C1 2 . 98.7(3)
O2 Dy O1 C1 . . -2.5(3)
O5 Dy O1 Dy . 2_566 4.5(3)
O4 Dy O1 Dy 2_556 2_566 -71.31(15)
O3 Dy O1 Dy . 2_566 -142.17(17)
O7 Dy O1 Dy . 2_566 72.19(15)
O2 Dy O1 Dy 2_666 2_566 145.10(14)
O1 Dy O1 Dy 2_566 2_566 0.0
O6 Dy O1 Dy 2 2_566 -118.82(18)
O2 Dy O1 Dy . 2_566 139.9(2)
C1 Dy O1 Dy . 2_566 142.5(4)
O5 Dy O2 C1 . . 138.8(3)
O4 Dy O2 C1 2_556 . -35.1(3)
O3 Dy O2 C1 . . -80.2(3)
O7 Dy O2 C1 . . 106.9(3)
O2 Dy O2 C1 2_666 . -172.2(4)
O1 Dy O2 C1 2_566 . 39.7(3)
O6 Dy O2 C1 2 . -123.4(3)
O1 Dy O2 C1 . . 2.6(3)
O5 Dy O2 Dy . 2_666 -49.0(3)
O4 Dy O2 Dy 2_556 2_666 137.16(15)
O3 Dy O2 Dy . 2_666 92.06(16)
O7 Dy O2 Dy . 2_666 -80.87(16)
O2 Dy O2 Dy 2_666 2_666 0.0010(10)
O1 Dy O2 Dy 2_566 2_666 -148.06(15)
O6 Dy O2 Dy 2 2_666 48.8(2)
O1 Dy O2 Dy . 2_666 174.8(2)
C1 Dy O2 Dy . 2_666 172.2(4)
O5 Dy O3 C4 . . -74.6(4)
O4 Dy O3 C4 2_556 . -5.9(3)
O7 Dy O3 C4 . . 145.5(3)
O2 Dy O3 C4 2_666 . -160.2(3)
O1 Dy O3 C4 2_566 . 39.2(4)
O6 Dy O3 C4 2 . -82.6(3)
O1 Dy O3 C4 . . 80.6(3)
O2 Dy O3 C4 . . 134.6(4)
C1 Dy O3 C4 . . 107.6(4)
O4 Dy O5 C5 2_556 . -66.7(4)
O3 Dy O5 C5 . . -6.3(5)
O7 Dy O5 C5 . . 149.5(4)
O2 Dy O5 C5 2_666 . 75.6(4)
O1 Dy O5 C5 2_566 . -135.5(4)
O6 Dy O5 C5 2 . 1.9(4)
O1 Dy O5 C5 . . -139.6(4)
O2 Dy O5 C5 . . 118.4(4)
C1 Dy O5 C5 . . 168.2(4)
Dy O2 C1 O1 2_666 . -171.1(4)
Dy O2 C1 O1 . . -4.5(5)
Dy O2 C1 C2 2_666 . 5.7(9)
Dy O2 C1 C2 . . 172.3(4)
Dy O2 C1 Dy 2_666 . -166.6(6)
Dy O1 C1 O2 2_566 . -127.1(4)
Dy O1 C1 O2 . . 4.5(5)
Dy O1 C1 C2 2_566 . 56.0(6)
Dy O1 C1 C2 . . -172.3(4)
Dy O1 C1 Dy 2_566 . -131.7(4)
O5 Dy C1 O2 . . -86.1(5)
O4 Dy C1 O2 2_556 . 150.6(3)
O3 Dy C1 O2 . . 89.7(3)
O7 Dy C1 O2 . . -67.6(3)
O2 Dy C1 O2 2_666 . 7.0(3)
O1 Dy C1 O2 2_566 . -141.9(3)
O6 Dy C1 O2 2 . 76.1(3)
O1 Dy C1 O2 . . -175.4(5)
O5 Dy C1 O1 . . 89.3(5)
O4 Dy C1 O1 2_556 . -34.1(3)
O3 Dy C1 O1 . . -95.0(3)
O7 Dy C1 O1 . . 107.8(3)
O2 Dy C1 O1 2_666 . -177.6(3)
O1 Dy C1 O1 2_566 . 33.5(3)
O6 Dy C1 O1 2 . -108.5(3)
O2 Dy C1 O1 . . 175.4(5)
O2 C1 C2 C3A . . -110.4(6)
O1 C1 C2 C3A . . 66.3(7)
O2 C1 C2 C3B . . -71.7(11)
O1 C1 C2 C3B . . 105.1(10)
C1 C2 C3A C3A . 2_667 68.2(9)
C3B C2 C3A C3A . 2_667 -27.2(14)
C1 C2 C3B C3B . 2_667 -70(2)
C3A C2 C3B C3B . 2_667 29.9(15)
Dy O4 C4 O3 2_556 . -174.4(4)
Dy O4 C4 C4 2_556 2_556 4.9(7)
Dy O3 C4 O4 . . -175.0(4)
Dy O3 C4 C4 . 2_556 5.8(7)
Dy O6 C5 O5 2 . 178.5(4)
Dy O6 C5 C5 2 2 -2.6(7)
Dy O5 C5 O6 . . 177.5(4)
Dy O5 C5 C5 . 2 -1.4(7)
