#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:52:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179544 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/13/4501305.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_4501305
loop_
_publ_author_name
'Yang, Jin'
'Song, Shu-Yan'
'Ma, Jian-Fang'
'Liu, Ying-Ying'
'Yu, Zhen-Tao'
_publ_section_title
;
 Syntheses, Structures, Photoluminescence, and Gas Adsorption of Rare
 Earth--Organic Frameworks Based on a Flexible Tricarboxylate
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5469
_journal_paper_doi               10.1021/cg2010425
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C48 H31 Dy3 O27'
_chemical_formula_weight         1527.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.7921(9)
_cell_length_b                   19.7921(9)
_cell_length_c                   45.3830(17)
_cell_measurement_reflns_used    6042
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.46
_cell_volume                     15396.0(11)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_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  0.0775
_diffrn_reflns_av_sigmaI/netI    0.1288
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            32312
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  0.51
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4398
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         6042
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0437
_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)+(0.0759P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1514
_reflns_number_gt                3391
_reflns_number_total             6042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2010425_si_002.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4501305
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C1 C 0.4353(6) 0.1256(7) 0.6855(2) 0.046(3) Uani 1 1 d . . .
C2 C 0.5010(6) 0.1148(7) 0.69740(19) 0.047(3) Uani 1 1 d . . .
C3 C 0.5649(6) 0.1291(6) 0.67981(18) 0.042(3) Uani 1 1 d . . .
H3 H 0.5671 0.1442 0.6603 0.051 Uiso 1 1 calc R . .
C4 C 0.6240(6) 0.1209(6) 0.69138(18) 0.044(3) Uani 1 1 d . . .
C5 C 0.6915(6) 0.1369(6) 0.67196(19) 0.039(2) Uani 1 1 d . . .
C6 C 0.6237(7) 0.1009(8) 0.7204(2) 0.062(4) Uani 1 1 d . A .
H6 H 0.6656 0.0979 0.7282 0.075 Uiso 1 1 calc R . .
C7 C 0.5599(7) 0.0850(9) 0.7377(2) 0.069(4) Uani 1 1 d . . .
C8 C 0.4995(7) 0.0944(8) 0.7265(2) 0.064(4) Uani 1 1 d . A .
H8 H 0.4585 0.0870 0.7386 0.076 Uiso 1 1 calc R . .
C10 C 0.5936(9) 0.0463(13) 0.8121(3) 0.101(6) Uani 1 1 d . . .
C11 C 0.5889(12) 0.0957(12) 0.8298(3) 0.128(8) Uani 1 1 d . . .
H11 H 0.5986 0.1433 0.8221 0.154 Uiso 1 1 calc R . .
C12 C 0.5704(11) 0.0813(11) 0.8591(3) 0.109(6) Uani 1 1 d . . .
H12 H 0.5700 0.1196 0.8709 0.131 Uiso 1 1 calc R A .
C13 C 0.5527(8) 0.0121(8) 0.8709(2) 0.067(4) Uani 1 1 d . . .
C14 C 0.5259(7) -0.0078(7) 0.9026(2) 0.052(3) Uani 1 1 d . . .
C15 C 0.5610(12) -0.0382(12) 0.8541(3) 0.126(7) Uani 1 1 d . . .
H15 H 0.5550 -0.0841 0.8622 0.151 Uiso 1 1 calc R A .
C16 C 0.5794(12) -0.0211(14) 0.8235(3) 0.142(8) Uani 1 1 d . . .
H16 H 0.5815 -0.0581 0.8114 0.170 Uiso 1 1 calc R . .
O1 O 0.4451(4) 0.1535(5) 0.65973(13) 0.052(2) Uani 1 1 d . . .
O2 O 0.3785(4) 0.1076(5) 0.70165(13) 0.052(2) Uani 1 1 d . . .
O1W O 0.2750(10) 0.2554(10) 0.7286(3) 0.094(4) Uani 0.67 1 d PU . .
O3 O 0.5055(5) 0.0344(5) 0.91618(15) 0.071(3) Uani 1 1 d . . .
O2W' O 0.1570(10) 0.1034(10) 0.7277(3) 0.031(4) Uani 0.33 1 d PU . .
O4 O 0.5241(5) -0.0653(5) 0.91480(13) 0.065(2) Uani 1 1 d . . .
O5 O 0.7494(4) 0.1374(4) 0.68342(13) 0.0478(18) Uani 1 1 d . . .
O6 O 0.6902(4) 0.1526(5) 0.64520(12) 0.0504(19) Uani 1 1 d . . .
Dy1 Dy 0.28851(3) 0.14771(3) 0.707171(8) 0.03257(17) Uani 1 1 d . . .
O2W O 0.2277(14) 0.1985(15) 0.7348(4) 0.059(6) Uani 0.33 1 d PU . .
O3W O 0.6667 0.3333 0.764(2) 0.54(6) Uiso 1 3 d S . .
O4W O 0.6667 0.3333 0.731(2) 0.50(5) Uiso 1 3 d S . .
O7 O 0.5625(8) 0.0862(9) 0.7688(3) 0.042(4) Uani 0.50 1 d PU A 1
C9 C 0.608(2) 0.0454(17) 0.7789(7) 0.045(9) Uani 0.50 1 d PU A 1
H9A H 0.5859 -0.0072 0.7712 0.053 Uiso 0.50 1 calc PR A 1
H9B H 0.6631 0.0753 0.7740 0.053 Uiso 0.50 1 calc PR A 1
O7' O 0.5425(8) 0.0441(9) 0.7649(3) 0.033(3) Uani 0.50 1 d PU A 2
C9' C 0.6245(18) 0.083(2) 0.7823(5) 0.069(11) Uani 0.50 1 d P A 2
H9'1 H 0.6601 0.0679 0.7740 0.083 Uiso 0.50 1 calc PR A 2
H9'2 H 0.6494 0.1395 0.7829 0.083 Uiso 0.50 1 calc PR A 2
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
O2 C1 O1 126.4(9) . .
O2 C1 C2 118.0(8) . .
O1 C1 C2 115.7(9) . .
C8 C2 C3 119.4(9) . .
C8 C2 C1 119.1(9) . .
C3 C2 C1 121.4(8) . .
C4 C3 C2 119.9(8) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C6 121.6(9) . .
C3 C4 C5 118.4(8) . .
C6 C4 C5 120.0(9) . .
O5 C5 O6 122.0(8) . .
O5 C5 C4 118.2(8) . .
O6 C5 C4 119.7(9) . .
O5 C5 Dy1 73.2(5) . 14_556
O6 C5 Dy1 49.0(4) . 14_556
C4 C5 Dy1 166.6(7) . 14_556
C4 C6 C7 118.8(10) . .
C4 C6 H6 120.6 . .
C7 C6 H6 120.6 . .
C6 C7 C8 120.5(9) . .
C6 C7 O7 122.9(11) . .
C8 C7 O7 112.9(10) . .
C6 C7 O7' 123.8(10) . .
C8 C7 O7' 114.5(10) . .
O7 C7 O7' 30.5(7) . .
C2 C8 C7 119.7(9) . .
C2 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C11 C10 C16 117.1(14) . .
C11 C10 C9' 111(2) . .
C16 C10 C9' 132(2) . .
C11 C10 C9 134.2(19) . .
C16 C10 C9 109(2) . .
C9' C10 C9 25.2(19) . .
C10 C11 C12 123.6(18) . .
C10 C11 H11 118.2 . .
C12 C11 H11 118.2 . .
C13 C12 C11 120.2(16) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C15 C13 C12 118.1(12) . .
C15 C13 C14 120.6(13) . .
C12 C13 C14 121.3(13) . .
O4 C14 O3 121.1(9) . .
O4 C14 C13 120.1(11) . .
O3 C14 C13 118.7(11) . .
O4 C14 Dy1 60.2(5) . 18_546
O3 C14 Dy1 60.9(5) . 18_546
C13 C14 Dy1 178.7(8) . 18_546
C13 C15 C16 119.4(17) . .
C13 C15 H15 120.3 . .
C16 C15 H15 120.3 . .
C10 C16 C15 121.1(18) . .
C10 C16 H16 119.4 . .
C15 C16 H16 119.4 . .
C1 O1 Dy1 138.2(6) . 13_556
C1 O2 Dy1 135.7(7) . .
O2W O1W Dy1 67.4(15) . .
C14 O3 Dy1 91.8(6) . 18_546
O2W O2W' Dy1 63.1(9) . .
C14 O4 Dy1 92.6(6) . 18_546
C5 O5 Dy1 176.0(6) . 2_655
C5 O5 Dy1 82.0(5) . 14_556
Dy1 O5 Dy1 101.2(2) 2_655 14_556
C5 O6 Dy1 107.0(6) . 14_556
O5 Dy1 O2W 106.0(7) 3_665 .
O5 Dy1 O2 77.5(3) 3_665 .
O2W Dy1 O2 151.7(6) . .
O5 Dy1 O1 78.4(2) 3_665 13_556
O2W Dy1 O1 74.9(6) . 13_556
O2 Dy1 O1 132.4(2) . 13_556
O5 Dy1 O6 127.5(2) 3_665 15_446
O2W Dy1 O6 114.1(7) . 15_446
O2 Dy1 O6 82.3(3) . 15_446
O1 Dy1 O6 80.8(3) 13_556 15_446
O5 Dy1 O4 138.3(3) 3_665 17_556
O2W Dy1 O4 79.5(6) . 17_556
O2 Dy1 O4 79.9(3) . 17_556
O1 Dy1 O4 140.5(3) 13_556 17_556
O6 Dy1 O4 82.9(2) 15_446 17_556
O5 Dy1 O3 86.1(3) 3_665 17_556
O2W Dy1 O3 76.2(6) . 17_556
O2 Dy1 O3 76.0(3) . 17_556
O1 Dy1 O3 141.8(3) 13_556 17_556
O6 Dy1 O3 134.5(3) 15_446 17_556
O4 Dy1 O3 54.4(3) 17_556 17_556
O5 Dy1 O2W' 141.4(4) 3_665 .
O2W Dy1 O2W' 42.2(7) . .
O2 Dy1 O2W' 141.1(4) . .
O1 Dy1 O2W' 72.5(4) 13_556 .
O6 Dy1 O2W' 72.3(4) 15_446 .
O4 Dy1 O2W' 68.3(4) 17_556 .
O3 Dy1 O2W' 101.3(4) 17_556 .
O5 Dy1 O1W 80.4(4) 3_665 .
O2W Dy1 O1W 25.9(6) . .
O2 Dy1 O1W 140.9(4) . .
O1 Dy1 O1W 72.4(4) 13_556 .
O6 Dy1 O1W 136.3(4) 15_446 .
O4 Dy1 O1W 96.3(4) 17_556 .
O3 Dy1 O1W 70.7(4) 17_556 .
O2W' Dy1 O1W 67.1(6) . .
O5 Dy1 C14 112.6(3) 3_665 17_556
O2W Dy1 C14 76.0(6) . 17_556
O2 Dy1 C14 76.7(3) . 17_556
O1 Dy1 C14 150.8(3) 13_556 17_556
O6 Dy1 C14 108.9(3) 15_446 17_556
O4 Dy1 C14 27.2(3) 17_556 17_556
O3 Dy1 C14 27.3(3) 17_556 17_556
O2W' Dy1 C14 84.2(4) . 17_556
O1W Dy1 C14 82.6(4) . 17_556
O5 Dy1 O5 78.8(2) 3_665 15_446
O2W Dy1 O5 139.6(6) . 15_446
O2 Dy1 O5 68.7(2) . 15_446
O1 Dy1 O5 66.7(2) 13_556 15_446
O6 Dy1 O5 48.7(2) 15_446 15_446
O4 Dy1 O5 123.8(2) 17_556 15_446
O3 Dy1 O5 143.8(3) 17_556 15_446
O2W' Dy1 O5 111.0(4) . 15_446
O1W Dy1 O5 136.9(4) . 15_446
C14 Dy1 O5 140.3(3) 17_556 15_446
O5 Dy1 C5 103.6(2) 3_665 15_446
O2W Dy1 C5 128.7(6) . 15_446
O2 Dy1 C5 75.4(3) . 15_446
O1 Dy1 C5 71.2(3) 13_556 15_446
O6 Dy1 C5 23.9(2) 15_446 15_446
O4 Dy1 C5 104.0(3) 17_556 15_446
O3 Dy1 C5 146.9(3) 17_556 15_446
O2W' Dy1 C5 90.6(4) . 15_446
O1W Dy1 C5 141.7(4) . 15_446
C14 Dy1 C5 127.5(3) 17_556 15_446
O5 Dy1 C5 24.8(2) 15_446 15_446
O1W O2W O2W' 154(2) . .
O1W O2W Dy1 86.7(16) . .
O2W' O2W Dy1 74.7(10) . .
C7 O7 C9 108.3(15) . .
C10 C9 O7 97(2) . .
C10 C9 H9A 112.3 . .
O7 C9 H9A 112.3 . .
C10 C9 H9B 112.3 . .
O7 C9 H9B 112.3 . .
H9A C9 H9B 109.9 . .
C7 O7' C9' 104.7(15) . .
C10 C9' O7' 98.1(19) . .
C10 C9' H9'1 112.2 . .
O7' C9' H9'1 112.2 . .
C10 C9' H9'2 112.2 . .
O7' C9' H9'2 112.2 . .
H9'1 C9' H9'2 109.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.234(11) .
C1 O1 1.268(11) .
C1 C2 1.519(14) .
C2 C8 1.378(13) .
C2 C3 1.400(13) .
C3 C4 1.363(13) .
C3 H3 0.9300 .
C4 C6 1.373(12) .
C4 C5 1.496(13) .
C5 O5 1.255(11) .
C5 O6 1.257(10) .
C5 Dy1 2.961(9) 14_556
C6 C7 1.386(14) .
C6 H6 0.9300 .
C7 C8 1.394(14) .
C7 O7 1.410(15) .
C7 O7' 1.420(15) .
C8 H8 0.9300 .
C10 C11 1.31(2) .
C10 C16 1.32(3) .
C10 C9' 1.51(3) .
C10 C9 1.53(3) .
C11 C12 1.371(18) .
C11 H11 0.9300 .
C12 C13 1.344(19) .
C12 H12 0.9300 .
C13 C15 1.325(19) .
C13 C14 1.517(14) .
C14 O4 1.251(13) .
C14 O3 1.255(13) .
C14 Dy1 2.738(9) 18_546
C15 C16 1.435(18) .
C15 H15 0.9300 .
C16 H16 0.9300 .
O1 Dy1 2.307(6) 13_556
O2 Dy1 2.298(7) .
O1W O2W 1.08(2) .
O1W Dy1 2.476(15) .
O3 Dy1 2.395(7) 18_546
O2W' O2W 1.72(3) .
O2W' Dy1 2.476(17) .
O4 Dy1 2.379(7) 18_546
O5 Dy1 2.275(7) 2_655
O5 Dy1 2.863(6) 14_556
O6 Dy1 2.339(6) 14_556
Dy1 O5 2.275(7) 3_665
Dy1 O2W 2.29(2) .
Dy1 O1 2.307(6) 13_556
Dy1 O6 2.339(6) 15_446
Dy1 O4 2.379(7) 17_556
Dy1 O3 2.395(7) 17_556
Dy1 C14 2.738(9) 17_556
Dy1 O5 2.863(6) 15_446
Dy1 C5 2.961(9) 15_446
O3W O4W 1.46(10) .
O7 C9 1.55(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
O7' C9' 1.61(3) .
C9' H9'1 0.9700 .
C9' H9'2 0.9700 .
