#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:30:50 +0100 (Wed, 23 Mar 2016) $
#$Revision: 179249 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/31/69/4316929.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_4316929
loop_
_publ_author_name
'Hai-Long Jiang'
'Nobuko Tsumori'
'Qiang Xu'
_publ_section_title
;
 A Series of (6,6)-Connected Porous Lanthanide-Organic Framework
 Enantiomers with High Thermostability and Exposed Metal Sites: Scalable
 Syntheses, Structures, and Sorption Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10001
_journal_page_last               10006
_journal_paper_doi               10.1021/ic101294s
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C9 H5 Dy O7'
_chemical_formula_weight         387.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           95
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw 2c'
_symmetry_space_group_name_H-M   'P 43 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3200(15)
_cell_length_b                   10.3200(15)
_cell_length_c                   14.500(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1544.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15151
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.95
_exptl_absorpt_coefficient_mu    4.853
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7651
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.000
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+3.2824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                1647
_reflns_number_total             1767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101294s_si_002_3.cif
_cod_data_source_block           3b-Dy-P4322
_cod_original_cell_volume        1544.3(4)
_cod_database_code               4316929
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+1/4'
'-y, -x, -z+3/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.14787(2) 0.14787(2) 0.1250 0.01283(10) Uani 1 2 d S . .
C3 C 0.0431(6) 0.6042(5) 0.0773(4) 0.0230(12) Uani 1 1 d . . .
H3A H 0.0715 0.5589 0.1289 0.028 Uiso 1 1 calc R . .
C4 C 0.0000 0.5373(7) 0.0000 0.0197(16) Uani 1 2 d S . .
C6 C 0.0000 0.3896(8) 0.0000 0.0231(17) Uani 1 2 d S . .
O2 O 0.0952(5) 0.7564(5) 0.2357(3) 0.0405(13) Uani 1 1 d . . .
C2 C 0.0436(6) 0.7391(5) 0.0771(3) 0.0196(11) Uani 1 1 d . . .
C5 C 0.0870(6) 0.8146(6) 0.1611(4) 0.0236(12) Uani 1 1 d . . .
O3 O 0.0709(5) 0.3364(4) 0.0584(3) 0.0358(11) Uani 1 1 d . . .
O1 O 0.1096(5) 0.9307(4) 0.1514(3) 0.0427(14) Uani 1 1 d . . .
C1 C 0.0000 0.8070(8) 0.0000 0.0248(18) Uani 1 2 d S . .
H1A H 0.0000 0.8971 0.0000 0.030 Uiso 1 2 calc SR . .
O4 O 0.3125(5) 0.3125(5) 0.1250 0.084(3) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.01444(11) 0.01444(11) 0.00960(14) 0.00004(10) -0.00004(10) 0.00229(13)
C3 0.035(3) 0.019(3) 0.015(2) 0.002(2) -0.008(2) 0.000(2)
C4 0.029(4) 0.011(4) 0.019(4) 0.000 -0.011(3) 0.000
C6 0.034(5) 0.014(4) 0.021(4) 0.000 -0.007(4) 0.000
O2 0.065(3) 0.043(3) 0.014(2) -0.003(2) -0.009(2) -0.015(3)
C2 0.033(3) 0.015(3) 0.011(2) -0.002(2) -0.007(2) -0.002(2)
C5 0.022(3) 0.024(3) 0.025(3) -0.007(2) -0.004(2) -0.003(2)
O3 0.060(3) 0.015(2) 0.033(2) 0.0041(18) -0.023(2) 0.000(2)
O1 0.062(3) 0.016(2) 0.050(3) -0.010(2) -0.022(2) -0.003(2)
C1 0.045(5) 0.015(4) 0.015(4) 0.000 0.000(4) 0.000
O4 0.044(3) 0.044(3) 0.164(10) 0.020(5) -0.020(5) -0.022(4)
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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O1 72.2(2) 7_455 1_545 ?
O1 Dy1 O3 145.83(16) 7_455 7 ?
O1 Dy1 O3 75.00(18) 1_545 7 ?
O1 Dy1 O3 75.00(18) 7_455 . ?
O1 Dy1 O3 145.83(16) 1_545 . ?
O3 Dy1 O3 138.8(2) 7 . ?
O1 Dy1 O2 89.41(19) 7_455 6_565 ?
O1 Dy1 O2 103.28(18) 1_545 6_565 ?
O3 Dy1 O2 88.86(17) 7 6_565 ?
O3 Dy1 O2 85.66(16) . 6_565 ?
O1 Dy1 O2 103.28(18) 7_455 3_654 ?
O1 Dy1 O2 89.41(19) 1_545 3_654 ?
O3 Dy1 O2 85.66(16) 7 3_654 ?
O3 Dy1 O2 88.86(17) . 3_654 ?
O2 Dy1 O2 164.4(3) 6_565 3_654 ?
O1 Dy1 O4 143.88(12) 7_455 . ?
O1 Dy1 O4 143.88(12) 1_545 . ?
O3 Dy1 O4 69.39(12) 7 . ?
O3 Dy1 O4 69.39(12) . . ?
O2 Dy1 O4 82.20(14) 6_565 . ?
O2 Dy1 O4 82.20(14) 3_654 . ?
C4 C3 C2 119.8(5) . . ?
C3 C4 C3 120.4(7) . 5 ?
C3 C4 C6 119.8(4) . . ?
C3 C4 C6 119.8(4) 5 . ?
O3 C6 O3 127.8(8) 5 . ?
O3 C6 C4 116.1(4) 5 . ?
O3 C6 C4 116.1(4) . . ?
C5 O2 Dy1 124.8(4) . 4_565 ?
C3 C2 C1 120.2(5) . . ?
C3 C2 C5 121.0(5) . . ?
C1 C2 C5 118.8(5) . . ?
O1 C5 O2 124.0(6) . . ?
O1 C5 C2 117.8(5) . . ?
O2 C5 C2 118.2(5) . . ?
C6 O3 Dy1 148.8(4) . . ?
C5 O1 Dy1 176.9(4) . 1_565 ?
C2 C1 C2 119.6(8) 5 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.308(4) 7_455 ?
Dy1 O1 2.308(4) 1_545 ?
Dy1 O3 2.313(4) 7 ?
Dy1 O3 2.313(4) . ?
Dy1 O2 2.313(4) 6_565 ?
Dy1 O2 2.313(4) 3_654 ?
Dy1 O4 2.403(7) . ?
C3 C4 1.389(7) . ?
C3 C2 1.393(8) . ?
C4 C3 1.389(7) 5 ?
C4 C6 1.524(11) . ?
C6 O3 1.247(5) 5 ?
C6 O3 1.247(5) . ?
O2 C5 1.240(7) . ?
O2 Dy1 2.313(4) 4_565 ?
C2 C1 1.395(7) . ?
C2 C5 1.513(7) . ?
C5 O1 1.228(7) . ?
O1 Dy1 2.308(4) 1_565 ?
C1 C2 1.395(7) 5 ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.500 0.761 678.4 33.0
