#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/72/4317267.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_4317267
loop_
_publ_author_name
'Yinfeng Han'
'Xiaoyan Li'
'Liqing Li'
'Chunlin Ma'
'Zhen Shen'
'You Song'
'Xiaozeng You'
_publ_contact_author_email       hanyfeng@yahoo.cn
_publ_contact_author_name        'Yinfeng Han'
_publ_section_title
;
 Structures and Properties of Porous Coordination Polymers Based on
 Lanthanide Carboxylate Building Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10781
_journal_page_last               10787
_journal_paper_doi               10.1021/ic902194g
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C15 H15 Dy N O8'
_chemical_formula_sum            'C15 H15 Dy N O8'
_chemical_formula_weight         499.78
_chemical_name_systematic
;
?
;
_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                64.726(5)
_cell_angle_beta                 71.738(6)
_cell_angle_gamma                79.581(6)
_cell_formula_units_Z            2
_cell_length_a                   8.522(3)
_cell_length_b                   10.154(3)
_cell_length_c                   11.067(4)
_cell_measurement_reflns_used    926
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.28
_cell_volume                     821.1(5)
_computing_cell_refinement       'SAINTPLUS(Bruker, 2003)'
_computing_data_collection       'SMART(Bruker, 2003)'
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    'SHELXTL(Bruker, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0910
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4227
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    4.594
_exptl_absorpt_correction_T_max  0.4052
_exptl_absorpt_correction_T_min  0.3395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Sheldrick,2003)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.267
_refine_diff_density_min         -2.402
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0353
_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/[σ²(Fo²)+(0.0529P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                2831
_reflns_number_total             2987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902194g_si_002_05.cif
_cod_data_source_block           5Dy
_cod_original_sg_symbol_Hall     '-p 1'
_cod_database_code               4317267
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.63217(2) 0.93817(2) 0.65651(2) 0.02008(11) Uani 1 1 d . . .
C1 C 0.5637(6) 0.7402(6) 0.5489(5) 0.0229(10) Uani 1 1 d . . .
C2 C 0.5303(6) 0.6162(6) 0.5217(5) 0.0241(10) Uani 1 1 d . . .
C3 C 0.5382(6) 0.6327(6) 0.3895(6) 0.0284(11) Uani 1 1 d . . .
H3A H 0.5650 0.7214 0.3151 0.034 Uiso 1 1 calc R . .
C4 C 0.4938(7) 0.4831(6) 0.6314(6) 0.0287(11) Uani 1 1 d . . .
H4A H 0.4908 0.4717 0.7200 0.034 Uiso 1 1 calc R . .
C5 C 0.3248(6) 0.9581(6) 0.8339(5) 0.0240(10) Uani 1 1 d . . .
C6 C 0.1555(6) 0.9801(6) 0.9199(5) 0.0256(11) Uani 1 1 d . . .
C7 C 0.0233(7) 0.9114(7) 0.9286(6) 0.0297(12) Uani 1 1 d . . .
H7A H 0.0393 0.8528 0.8797 0.036 Uiso 1 1 calc R . .
C8 C -0.1319(7) 0.9301(7) 1.0097(6) 0.0318(12) Uani 1 1 d . . .
H8A H -0.2203 0.8826 1.0171 0.038 Uiso 1 1 calc R . .
C9 C 0.8249(6) 0.7310(6) 0.8198(6) 0.0261(11) Uani 1 1 d . . .
C10 C 0.9174(7) 0.6110(6) 0.9109(5) 0.0251(11) Uani 1 1 d . . .
C11 C 0.8369(7) 0.5361(7) 1.0495(6) 0.0364(13) Uani 1 1 d . . .
H11A H 0.7260 0.5602 1.0831 0.044 Uiso 1 1 calc R . .
C12 C 1.0808(7) 0.5735(7) 0.8620(6) 0.0356(13) Uani 1 1 d . . .
H12A H 1.1358 0.6219 0.7693 0.043 Uiso 1 1 calc R . .
C13 C 0.7514(8) 1.1719(7) 0.7455(7) 0.0388(15) Uani 1 1 d . . .
H13 H 0.6565 1.1576 0.8189 0.047 Uiso 1 1 calc R . .
C14 C 0.8146(12) 1.3547(9) 0.8032(11) 0.075(3) Uani 1 1 d . . .
H14A H 0.7128 1.3259 0.8740 0.112 Uiso 1 1 calc R . .
H14B H 0.8038 1.4560 0.7444 0.112 Uiso 1 1 calc R . .
H14C H 0.9026 1.3397 0.8455 0.112 Uiso 1 1 calc R . .
C15 C 1.0044(10) 1.2922(11) 0.6096(11) 0.082(3) Uani 1 1 d . . .
H15A H 1.0129 1.2291 0.5631 0.123 Uiso 1 1 calc R . .
H15B H 1.0974 1.2717 0.6475 0.123 Uiso 1 1 calc R . .
H15C H 1.0034 1.3920 0.5448 0.123 Uiso 1 1 calc R . .
N1 N 0.8519(8) 1.2676(7) 0.7211(7) 0.0536(16) Uani 1 1 d . . .
O1 O 0.5270(4) 0.8699(4) 0.4756(4) 0.0282(8) Uani 1 1 d . . .
O2 O 0.6288(5) 0.7112(5) 0.6439(5) 0.0365(10) Uani 1 1 d . . .
O3 O 0.3453(4) 0.8784(4) 0.7670(4) 0.0265(8) Uani 1 1 d . . .
O4 O 0.4438(4) 1.0182(4) 0.8291(4) 0.0290(8) Uani 1 1 d . . .
O5 O 0.8968(4) 0.8020(4) 0.6934(4) 0.0302(8) Uani 1 1 d . . .
O6 O 0.6760(4) 0.7619(5) 0.8700(4) 0.0324(9) Uani 1 1 d . . .
O7 O 0.7763(5) 1.0993(5) 0.6755(4) 0.0370(9) Uani 1 1 d . . .
O1W O 0.8164(5) 1.0358(5) 0.4336(4) 0.0355(9) Uani 1 1 d . . .
H1A H 0.7738 1.0494 0.3690 0.042(19) Uiso 1 1 d R . .
H1B H 0.8991 1.0887 0.3982 0.08(3) Uiso 1 1 d R . .
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'
N N 0.0061 0.0033 '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
O7 Dy1 O1W 76.99(15) . . ?
O7 Dy1 O6 88.30(15) . . ?
O1W Dy1 O6 131.31(13) . . ?
O7 Dy1 O1 92.62(14) . 2_676 ?
O1W Dy1 O1 75.77(13) . 2_676 ?
O6 Dy1 O1 152.05(13) . 2_676 ?
O7 Dy1 O2 148.66(15) . . ?
O1W Dy1 O2 93.33(15) . . ?
O6 Dy1 O2 75.77(14) . . ?
O1 Dy1 O2 114.08(13) 2_676 . ?
O7 Dy1 O4 74.48(14) . . ?
O1W Dy1 O4 139.76(15) . . ?
O6 Dy1 O4 75.54(13) . . ?
O1 Dy1 O4 77.81(13) 2_676 . ?
O2 Dy1 O4 125.23(15) . . ?
O7 Dy1 O3 128.22(14) . . ?
O1W Dy1 O3 140.55(12) . . ?
O6 Dy1 O3 84.01(12) . . ?
O1 Dy1 O3 73.54(13) 2_676 . ?
O2 Dy1 O3 77.45(14) . . ?
O4 Dy1 O3 53.99(12) . . ?
O7 Dy1 O5 75.72(14) . . ?
O1W Dy1 O5 77.54(13) . . ?
O6 Dy1 O5 53.80(12) . . ?
O1 Dy1 O5 152.68(13) 2_676 . ?
O2 Dy1 O5 73.09(14) . . ?
O4 Dy1 O5 120.97(12) . . ?
O3 Dy1 O5 132.96(12) . . ?
O7 Dy1 C5 101.00(15) . . ?
O1W Dy1 C5 148.10(14) . . ?
O6 Dy1 C5 79.89(13) . . ?
O1 Dy1 C5 72.52(14) 2_676 . ?
O2 Dy1 C5 102.47(16) . . ?
O4 Dy1 C5 26.80(14) . . ?
O3 Dy1 C5 27.26(14) . . ?
O5 Dy1 C5 133.45(13) . . ?
O7 Dy1 C9 82.44(15) . . ?
O1W Dy1 C9 104.68(15) . . ?
O6 Dy1 C9 26.72(14) . . ?
O1 Dy1 C9 174.74(13) 2_676 . ?
O2 Dy1 C9 71.17(15) . . ?
O4 Dy1 C9 99.05(14) . . ?
O3 Dy1 C9 108.15(14) . . ?
O5 Dy1 C9 27.15(14) . . ?
C5 Dy1 C9 106.59(15) . . ?
O7 Dy1 O1 145.53(13) . . ?
O1W Dy1 O1 71.70(13) . . ?
O6 Dy1 O1 123.35(13) . . ?
O1 Dy1 O1 66.22(14) 2_676 . ?
O2 Dy1 O1 49.10(12) . . ?
O4 Dy1 O1 122.92(11) . . ?
O3 Dy1 O1 73.58(11) . . ?
O5 Dy1 O1 110.34(12) . . ?
C5 Dy1 O1 98.08(13) . . ?
C9 Dy1 O1 118.97(14) . . ?
O7 Dy1 C1 158.46(15) . . ?
O1W Dy1 C1 83.15(14) . . ?
O6 Dy1 C1 98.79(15) . . ?
O1 Dy1 C1 90.49(14) 2_676 . ?
O2 Dy1 C1 23.99(14) . . ?
O4 Dy1 C1 126.95(13) . . ?
O3 Dy1 C1 73.00(13) . . ?
O5 Dy1 C1 92.04(13) . . ?
C5 Dy1 C1 100.26(15) . . ?
C9 Dy1 C1 94.77(15) . . ?
O1 Dy1 C1 25.15(13) . . ?
O2 C1 O1 121.4(5) . . ?
O2 C1 C2 118.4(5) . . ?
O1 C1 C2 120.2(5) . . ?
O2 C1 Dy1 50.9(3) . . ?
O1 C1 Dy1 70.6(3) . . ?
C2 C1 Dy1 168.6(4) . . ?
C3 C2 C4 119.9(5) . . ?
C3 C2 C1 121.2(5) . . ?
C4 C2 C1 119.0(5) . . ?
C4 C3 C2 119.6(5) 2_666 . ?
C4 C3 H3A 120.2 2_666 . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C2 120.6(5) 2_666 . ?
C3 C4 H4A 119.7 2_666 . ?
C2 C4 H4A 119.7 . . ?
O4 C5 O3 121.0(5) . . ?
O4 C5 C6 119.7(5) . . ?
O3 C5 C6 119.3(5) . . ?
O4 C5 Dy1 60.4(3) . . ?
O3 C5 Dy1 60.9(3) . . ?
C6 C5 Dy1 175.2(4) . . ?
C8 C6 C7 120.3(5) 2_577 . ?
C8 C6 C5 119.5(5) 2_577 . ?
C7 C6 C5 120.2(5) . . ?
C8 C7 C6 120.0(5) . . ?
C8 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C7 C8 C6 119.7(5) . 2_577 ?
C7 C8 H8A 120.2 . . ?
C6 C8 H8A 120.2 2_577 . ?
O6 C9 O5 120.6(5) . . ?
O6 C9 C10 119.2(5) . . ?
O5 C9 C10 120.2(5) . . ?
O6 C9 Dy1 58.0(3) . . ?
O5 C9 Dy1 62.8(3) . . ?
C10 C9 Dy1 175.1(4) . . ?
C12 C10 C11 119.0(5) . . ?
C12 C10 C9 121.7(5) . . ?
C11 C10 C9 119.2(5) . . ?
C12 C11 C10 121.0(5) 2_767 . ?
C12 C11 H11A 119.5 2_767 . ?
C10 C11 H11A 119.5 . . ?
C10 C12 C11 120.0(5) . 2_767 ?
C10 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 2_767 . ?
O7 C13 N1 122.7(7) . . ?
O7 C13 H13 118.6 . . ?
N1 C13 H13 118.6 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 N1 C14 120.9(8) . . ?
C13 N1 C15 121.1(7) . . ?
C14 N1 C15 118.0(7) . . ?
C1 O1 Dy1 156.1(3) . 2_676 ?
C1 O1 Dy1 84.2(3) . . ?
Dy1 O1 Dy1 113.78(14) 2_676 . ?
C1 O2 Dy1 105.1(3) . . ?
C5 O3 Dy1 91.9(3) . . ?
C5 O4 Dy1 92.8(3) . . ?
C9 O5 Dy1 90.1(3) . . ?
C9 O6 Dy1 95.3(3) . . ?
C13 O7 Dy1 137.1(4) . . ?
Dy1 O1W H1A 113.0 . . ?
Dy1 O1W H1B 134.8 . . ?
H1A O1W H1B 107.7 . . ?
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 O7 2.327(4) . ?
Dy1 O1W 2.362(4) . ?
Dy1 O6 2.372(4) . ?
Dy1 O1 2.372(4) 2_676 ?
Dy1 O2 2.373(4) . ?
Dy1 O4 2.412(4) . ?
Dy1 O3 2.422(3) . ?
Dy1 O5 2.476(4) . ?
Dy1 C5 2.771(5) . ?
Dy1 C9 2.784(5) . ?
Dy1 O1 2.798(4) . ?
Dy1 C1 2.951(5) . ?
C1 O2 1.242(7) . ?
C1 O1 1.261(6) . ?
C1 C2 1.504(7) . ?
C2 C3 1.380(7) . ?
C2 C4 1.382(7) . ?
C3 C4 1.378(8) 2_666 ?
C3 H3A 0.9300 . ?
C4 C3 1.378(8) 2_666 ?
C4 H4A 0.9300 . ?
C5 O4 1.251(6) . ?
C5 O3 1.270(6) . ?
C5 C6 1.497(7) . ?
C6 C8 1.387(8) 2_577 ?
C6 C7 1.387(8) . ?
C7 C8 1.379(8) . ?
C7 H7A 0.9300 . ?
C8 C6 1.387(8) 2_577 ?
C8 H8A 0.9300 . ?
C9 O6 1.257(6) . ?
C9 O5 1.270(7) . ?
C9 C10 1.491(8) . ?
C10 C12 1.374(8) . ?
C10 C11 1.391(8) . ?
C11 C12 1.381(8) 2_767 ?
C11 H11A 0.9300 . ?
C12 C11 1.381(8) 2_767 ?
C12 H12A 0.9300 . ?
C13 O7 1.232(8) . ?
C13 N1 1.297(9) . ?
C13 H13 0.9300 . ?
C14 N1 1.453(10) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N1 1.457(11) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
O1 Dy1 2.372(4) 2_676 ?
O1W H1A 0.8501 . ?
O1W H1B 0.8500 . ?
