#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:42:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179258 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/78/4317858.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_4317858
loop_
_publ_author_name
'Rong Cao'
'Daofeng Sun'
'Yucang Liang'
'Maochun Hong'
'Kazuyuki Tatsumi'
'Qian Shi'
_publ_section_title
;
 Syntheses and Characterizations of Three-Dimensional Channel-like
 Polymeric Lanthanide Complexes Constructed by
 1,2,4,5-Benzenetetracarboxylic Acid
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2087
_journal_page_last               2094
_journal_paper_doi               10.1021/ic0110124
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C15 H3 Er2 O20'
_chemical_formula_weight         837.69
_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                104.8330(10)
_cell_angle_beta                 91.0000(10)
_cell_angle_gamma                114.2570(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6739(5)
_cell_length_b                   11.0039(5)
_cell_length_c                   11.5523(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1073.27(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5541
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    7.868
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.084
_refine_diff_density_min         -2.365
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0340
_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)+(0.0581P)²+0.9693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                3228
_reflns_number_total             3713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110124_2.cif
_cod_data_source_block           Er
_cod_database_code               4317858
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
Er1 Er 0.50773(3) 1.00724(3) 0.74647(3) 0.01208(12) Uani 1 1 d . . .
Er2 Er 0.48314(3) 0.57553(3) 0.67001(3) 0.01036(12) Uani 1 1 d . . .
OW1 O 0.0375(11) 0.3434(10) 0.8498(9) 0.095(4) Uani 1 1 d . . .
O1 O 0.2828(5) 0.8612(5) 0.6015(5) 0.0185(11) Uani 1 1 d . . .
O01 O 0.4790(7) 1.1693(6) 0.6692(5) 0.0303(13) Uani 1 1 d . . .
OW2 O 0.3136(16) 0.3908(15) 0.9851(13) 0.126(5) Uani 1 1 d . . .
O2 O 0.3944(5) 0.7490(5) 0.6668(4) 0.0133(10) Uani 1 1 d . . .
O02 O 0.6078(7) 1.2171(6) 0.9110(5) 0.0310(13) Uani 1 1 d . . .
OW3 O 0.149(3) 0.505(2) 1.1018(15) 0.217(10) Uani 1 1 d . . .
O3 O 0.4012(5) 0.5533(5) 0.4664(4) 0.0148(10) Uani 1 1 d . . .
O03 O 0.2741(6) 0.5539(6) 0.7834(5) 0.0264(13) Uani 1 1 d . . .
OW4 O 0.235(5) 0.213(3) 0.843(3) 0.44(3) Uani 1 1 d . . .
O4 O 0.2578(6) 0.4416(6) 0.2903(5) 0.0220(12) Uani 1 1 d . . .
O04 O 0.4846(7) 0.4318(6) 0.8016(5) 0.0293(13) Uani 1 1 d . . .
O5 O 0.6287(6) 0.9498(5) 0.8735(5) 0.0225(12) Uani 1 1 d . . .
O6 O 0.6164(5) 0.7388(5) 0.8506(5) 0.0179(11) Uani 1 1 d . . .
O7 O 1.3188(6) 0.9710(6) 0.8599(5) 0.0296(14) Uani 1 1 d . . .
O8 O 1.1832(7) 0.7637(6) 0.8868(6) 0.0356(15) Uani 1 1 d . . .
O9 O 0.2954(6) 0.3535(5) 0.5876(5) 0.0195(11) Uani 1 1 d . . .
O10 O 0.3137(5) 0.2582(5) 0.3947(4) 0.0166(10) Uani 1 1 d . . .
O11 O 0.3877(5) 0.0481(5) 0.4320(5) 0.0167(10) Uani 1 1 d . . .
O12 O 0.2236(6) -0.1203(6) 0.2830(5) 0.0299(14) Uani 1 1 d . . .
C1 C 0.2825(8) 0.7498(7) 0.6069(6) 0.0134(14) Uani 1 1 d . . .
C2 C 0.1408(8) 0.6177(7) 0.5499(6) 0.0135(14) Uani 1 1 d . . .
C3 C 0.0047(8) 0.6097(7) 0.5928(6) 0.0136(14) Uani 1 1 d . . .
H3A H 0.0070 0.6835 0.6553 0.016 Uiso 1 1 calc R . .
C4 C 0.1344(8) 0.5052(7) 0.4547(6) 0.0136(14) Uani 1 1 d . . .
C5 C 0.2719(7) 0.5018(7) 0.3991(6) 0.0136(14) Uani 1 1 d . . .
C6 C 0.6859(8) 0.8707(7) 0.8882(6) 0.0140(14) Uani 1 1 d . . .
C7 C 0.8471(8) 0.9356(7) 0.9491(6) 0.0150(14) Uani 1 1 d . . .
C8 C 0.9466(8) 0.8792(7) 0.9047(6) 0.0155(15) Uani 1 1 d . . .
H8A H 0.9102 0.7978 0.8407 0.019 Uiso 1 1 calc R . .
C9 C 1.0989(8) 0.9416(7) 0.9540(6) 0.0139(14) Uani 1 1 d . . .
C10 C 1.2096(8) 0.8871(8) 0.8972(7) 0.0187(16) Uani 1 1 d . . .
C11 C 0.2585(7) 0.2536(7) 0.4911(6) 0.0128(14) Uani 1 1 d . . .
C12 C 0.1266(8) 0.1193(7) 0.4964(6) 0.0133(14) Uani 1 1 d . . .
C13 C 0.0077(8) 0.1301(7) 0.5541(7) 0.0160(15) Uani 1 1 d . . .
H13A H 0.0126 0.2178 0.5910 0.019 Uiso 1 1 calc R . .
C14 C 0.1203(8) -0.0120(7) 0.4417(6) 0.0148(14) Uani 1 1 d . . .
C15 C 0.2496(8) -0.0299(7) 0.3824(7) 0.0158(15) Uani 1 1 d . . .
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'
Er Er -0.2586 4.9576 '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
O5 Er1 O7 88.5(2) . 1_455 ?
O5 Er1 O01 151.4(2) . . ?
O7 Er1 O01 98.9(2) 1_455 . ?
O5 Er1 O11 100.85(18) . 2_666 ?
O7 Er1 O11 153.1(2) 1_455 2_666 ?
O01 Er1 O11 85.02(19) . 2_666 ?
O5 Er1 O02 79.4(2) . . ?
O7 Er1 O02 77.6(2) 1_455 . ?
O01 Er1 O02 75.3(2) . . ?
O11 Er1 O02 128.82(19) 2_666 . ?
O5 Er1 O1 129.05(17) . . ?
O7 Er1 O1 76.7(2) 1_455 . ?
O01 Er1 O1 79.53(19) . . ?
O11 Er1 O1 77.83(17) 2_666 . ?
O02 Er1 O1 140.45(19) . . ?
O5 Er1 O12 76.7(2) . 2_666 ?
O7 Er1 O12 152.7(2) 1_455 2_666 ?
O01 Er1 O12 84.8(2) . 2_666 ?
O11 Er1 O12 53.92(17) 2_666 2_666 ?
O02 Er1 O12 77.24(19) . 2_666 ?
O1 Er1 O12 130.32(18) . 2_666 ?
O5 Er1 O2 77.36(17) . . ?
O7 Er1 O2 85.11(18) 1_455 . ?
O01 Er1 O2 130.56(18) . . ?
O11 Er1 O2 72.59(16) 2_666 . ?
O02 Er1 O2 151.25(18) . . ?
O1 Er1 O2 53.28(15) . . ?
O12 Er1 O2 113.12(16) 2_666 . ?
O5 Er1 C15 85.0(2) . 2_666 ?
O7 Er1 C15 172.9(2) 1_455 2_666 ?
O01 Er1 C15 88.2(2) . 2_666 ?
O11 Er1 C15 27.5(2) 2_666 2_666 ?
O02 Er1 C15 104.0(2) . 2_666 ?
O1 Er1 C15 105.22(19) . 2_666 ?
O12 Er1 C15 27.00(19) 2_666 2_666 ?
O2 Er1 C15 90.62(17) . 2_666 ?
O5 Er1 C1 103.34(19) . . ?
O7 Er1 C1 78.0(2) 1_455 . ?
O01 Er1 C1 105.2(2) . . ?
O11 Er1 C1 75.30(18) 2_666 . ?
O02 Er1 C1 155.3(2) . . ?
O1 Er1 C1 26.20(18) . . ?
O12 Er1 C1 127.45(18) 2_666 . ?
O2 Er1 C1 27.19(18) . . ?
C15 Er1 C1 100.7(2) 2_666 . ?
O9 Er2 O6 143.31(18) . . ?
O9 Er2 O10 137.63(17) . 2_666 ?
O6 Er2 O10 77.77(17) . 2_666 ?
O9 Er2 O3 72.18(17) . . ?
O6 Er2 O3 142.30(17) . . ?
O10 Er2 O3 72.74(16) 2_666 . ?
O9 Er2 O03 73.39(18) . . ?
O6 Er2 O03 80.76(19) . . ?
O10 Er2 O03 141.38(17) 2_666 . ?
O3 Er2 O03 108.67(18) . . ?
O9 Er2 O2 112.17(17) . . ?
O6 Er2 O2 80.67(17) . . ?
O10 Er2 O2 76.64(16) 2_666 . ?
O3 Er2 O2 70.16(16) . . ?
O03 Er2 O2 68.43(17) . . ?
O9 Er2 O3 73.08(16) . 2_666 ?
O6 Er2 O3 122.04(16) . 2_666 ?
O10 Er2 O3 73.64(16) 2_666 2_666 ?
O3 Er2 O3 71.09(18) . 2_666 ?
O03 Er2 O3 144.57(17) . 2_666 ?
O2 Er2 O3 136.48(16) . 2_666 ?
O9 Er2 O04 71.01(19) . . ?
O6 Er2 O04 76.92(19) . . ?
O10 Er2 O04 130.88(18) 2_666 . ?
O3 Er2 O04 140.68(18) . . ?
O03 Er2 O04 73.20(19) . . ?
O2 Er2 O04 138.00(17) . . ?
O3 Er2 O04 85.39(17) 2_666 . ?
O9 Er2 O4 107.90(17) . 2_666 ?
O6 Er2 O4 71.89(16) . 2_666 ?
O10 Er2 O4 68.50(17) 2_666 2_666 ?
O3 Er2 O4 116.50(16) . 2_666 ?
O03 Er2 O4 132.93(19) . 2_666 ?
O2 Er2 O4 139.15(16) . 2_666 ?
O3 Er2 O4 50.97(16) 2_666 2_666 ?
O04 Er2 O4 63.86(18) . 2_666 ?
O9 Er2 C5 93.58(18) . 2_666 ?
O6 Er2 C5 95.90(18) . 2_666 ?
O10 Er2 C5 65.07(18) 2_666 2_666 ?
O3 Er2 C5 92.53(18) . 2_666 ?
O03 Er2 C5 149.52(19) . 2_666 ?
O2 Er2 C5 141.31(18) . 2_666 ?
O3 Er2 C5 26.17(18) 2_666 2_666 ?
O04 Er2 C5 76.53(19) . 2_666 ?
O4 Er2 C5 25.35(18) 2_666 2_666 ?
O9 Er2 Er2 68.48(12) . 2_666 ?
O6 Er2 Er2 144.14(12) . 2_666 ?
O10 Er2 Er2 69.19(12) 2_666 2_666 ?
O3 Er2 Er2 36.00(11) . 2_666 ?
O03 Er2 Er2 134.49(15) . 2_666 ?
O2 Er2 Er2 104.15(11) . 2_666 ?
O3 Er2 Er2 35.09(11) 2_666 2_666 ?
O04 Er2 Er2 114.84(13) . 2_666 ?
O4 Er2 Er2 83.10(11) 2_666 2_666 ?
C5 Er2 Er2 57.94(14) 2_666 2_666 ?
C1 O1 Er1 95.3(4) . . ?
C1 O2 Er2 134.5(4) . . ?
C1 O2 Er1 90.1(4) . . ?
Er2 O2 Er1 134.47(19) . . ?
C5 O3 Er2 135.7(4) . . ?
C5 O3 Er2 96.8(4) . 2_666 ?
Er2 O3 Er2 108.91(18) . 2_666 ?
C5 O4 Er2 89.1(4) . 2_666 ?
C6 O5 Er1 147.6(5) . . ?
C6 O6 Er2 135.9(4) . . ?
C10 O7 Er1 148.7(5) . 1_655 ?
C11 O9 Er2 139.2(4) . . ?
C11 O10 Er2 135.8(4) . 2_666 ?
C15 O11 Er1 93.9(4) . 2_666 ?
C15 O12 Er1 90.4(4) . 2_666 ?
O1 C1 O2 120.8(6) . . ?
O1 C1 C2 117.8(6) . . ?
O2 C1 C2 121.3(6) . . ?
O1 C1 Er1 58.5(4) . . ?
O2 C1 Er1 62.7(3) . . ?
C2 C1 Er1 168.4(5) . . ?
C3 C2 C4 118.0(6) . . ?
C3 C2 C1 116.5(6) . . ?
C4 C2 C1 125.4(6) . . ?
C4 C3 C2 122.0(6) 2_566 . ?
C3 C4 C2 120.0(6) 2_566 . ?
C3 C4 C5 116.7(6) 2_566 . ?
C2 C4 C5 123.3(6) . . ?
O4 C5 O3 120.5(6) . . ?
O4 C5 C4 119.7(6) . . ?
O3 C5 C4 119.6(6) . . ?
O4 C5 Er2 65.5(4) . 2_666 ?
O3 C5 Er2 57.0(3) . 2_666 ?
C4 C5 Er2 161.2(5) . 2_666 ?
O5 C6 O6 123.7(6) . . ?
O5 C6 C7 117.8(6) . . ?
O6 C6 C7 118.4(6) . . ?
C8 C7 C9 119.8(7) . 2_777 ?
C8 C7 C6 119.6(6) . . ?
C9 C7 C6 120.5(6) 2_777 . ?
C9 C8 C7 121.1(7) . . ?
C8 C9 C7 119.1(6) . 2_777 ?
C8 C9 C10 120.5(6) . . ?
C7 C9 C10 120.1(6) 2_777 . ?
O8 C10 O7 125.5(7) . . ?
O8 C10 C9 118.7(6) . . ?
O7 C10 C9 115.7(7) . . ?
O10 C11 O9 126.8(6) . . ?
O10 C11 C12 119.0(6) . . ?
O9 C11 C12 114.1(6) . . ?
C13 C12 C14 119.7(6) . . ?
C13 C12 C11 117.5(6) . . ?
C14 C12 C11 122.8(6) . . ?
C12 C13 C14 121.0(7) . 2_556 ?
C13 C14 C12 119.3(6) 2_556 . ?
C13 C14 C15 118.7(6) 2_556 . ?
C12 C14 C15 122.0(6) . . ?
O12 C15 O11 119.4(6) . . ?
O12 C15 C14 120.4(6) . . ?
O11 C15 C14 120.2(6) . . ?
O12 C15 Er1 62.6(4) . 2_666 ?
O11 C15 Er1 58.6(4) . 2_666 ?
C14 C15 Er1 165.6(5) . 2_666 ?
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
Er1 O5 2.223(5) . ?
Er1 O7 2.229(5) 1_455 ?
Er1 O01 2.295(5) . ?
Er1 O11 2.362(5) 2_666 ?
Er1 O02 2.395(5) . ?
Er1 O1 2.397(5) . ?
Er1 O12 2.452(5) 2_666 ?
Er1 O2 2.488(4) . ?
Er1 C15 2.761(7) 2_666 ?
Er1 C1 2.800(7) . ?
Er2 O9 2.297(5) . ?
Er2 O6 2.308(5) . ?
Er2 O10 2.359(5) 2_666 ?
Er2 O3 2.388(5) . ?
Er2 O03 2.391(5) . ?
Er2 O2 2.401(4) . ?
Er2 O3 2.442(5) 2_666 ?
Er2 O04 2.462(6) . ?
Er2 O4 2.630(5) 2_666 ?
Er2 C5 2.890(7) 2_666 ?
Er2 Er2 3.9301(6) 2_666 ?
O1 C1 1.242(8) . ?
O2 C1 1.279(9) . ?
O3 C5 1.284(8) . ?
O3 Er2 2.442(5) 2_666 ?
O4 C5 1.237(8) . ?
O4 Er2 2.630(5) 2_666 ?
O5 C6 1.249(9) . ?
O6 C6 1.270(8) . ?
O7 C10 1.254(9) . ?
O7 Er1 2.229(5) 1_655 ?
O8 C10 1.246(9) . ?
O9 C11 1.271(8) . ?
O10 C11 1.247(8) . ?
O10 Er2 2.359(4) 2_666 ?
O11 C15 1.276(9) . ?
O11 Er1 2.362(5) 2_666 ?
O12 C15 1.253(9) . ?
O12 Er1 2.452(5) 2_666 ?
C1 C2 1.506(10) . ?
C2 C3 1.391(9) . ?
C2 C4 1.408(9) . ?
C3 C4 1.390(10) 2_566 ?
C4 C3 1.390(10) 2_566 ?
C4 C5 1.497(9) . ?
C5 Er2 2.890(7) 2_666 ?
C6 C7 1.492(10) . ?
C7 C8 1.386(10) . ?
C7 C9 1.406(10) 2_777 ?
C8 C9 1.380(10) . ?
C9 C7 1.406(10) 2_777 ?
C9 C10 1.513(9) . ?
C11 C12 1.522(9) . ?
C12 C13 1.372(9) . ?
C12 C14 1.396(10) . ?
C13 C14 1.392(9) 2_556 ?
C14 C13 1.392(9) 2_556 ?
C14 C15 1.496(9) . ?
C15 Er1 2.761(7) 2_666 ?
