#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:52:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179544 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/13/4501306.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_4501306
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 O27 Tb3'
_chemical_formula_weight         1516.49
_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                   19.8558(7)
_cell_length_b                   19.8558(7)
_cell_length_c                   45.5011(14)
_cell_measurement_reflns_used    6119
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.48
_cell_volume                     15535.6(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            23235
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4380
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         6119
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1149P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                4129
_reflns_number_total             6119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2010425_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4501306
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 0.3101(5) -0.1251(6) 0.8146(2) 0.047(2) Uani 1 1 d . . .
C2 C 0.3870(5) -0.1140(6) 0.80247(19) 0.048(2) Uani 1 1 d . . .
C3 C 0.4361(5) -0.1286(6) 0.8204(2) 0.044(2) Uani 1 1 d . . .
H3 H 0.4228 -0.1436 0.8398 0.053 Uiso 1 1 calc R . .
C4 C 0.5040(5) -0.1205(6) 0.80892(19) 0.045(2) Uani 1 1 d . . .
C5 C 0.5241(6) -0.0996(7) 0.7801(2) 0.063(3) Uani 1 1 d . A .
H5 H 0.5699 -0.0946 0.7725 0.075 Uiso 1 1 calc R . .
C6 C 0.4743(7) -0.0861(9) 0.7625(2) 0.079(4) Uani 1 1 d . . .
C7 C 0.4059(6) -0.0942(8) 0.7734(2) 0.067(3) Uani 1 1 d . A .
H7 H 0.3728 -0.0864 0.7612 0.081 Uiso 1 1 calc R . .
C10 C 0.5500(8) -0.0468(10) 0.6877(3) 0.087(5) Uani 1 1 d . . .
C11 C 0.6038(11) 0.0239(11) 0.6762(4) 0.122(6) Uani 1 1 d U . .
H11 H 0.6424 0.0613 0.6882 0.146 Uiso 1 1 calc R . .
C12 C 0.6001(9) 0.0399(9) 0.6458(4) 0.100(5) Uani 1 1 d U . .
H12 H 0.6386 0.0860 0.6375 0.119 Uiso 1 1 calc R A .
C13 C 0.5399(7) -0.0128(7) 0.6292(2) 0.062(3) Uani 1 1 d . . .
C14 C 0.4910(9) -0.0817(10) 0.6410(3) 0.110(6) Uani 1 1 d . . .
H14 H 0.4519 -0.1196 0.6293 0.132 Uiso 1 1 calc R A .
C15 C 0.4970(10) -0.0986(11) 0.6703(3) 0.112(6) Uani 1 1 d . . .
H15 H 0.4624 -0.1477 0.6776 0.134 Uiso 1 1 calc R . .
C16 C 0.5539(5) -0.1371(6) 0.82822(19) 0.042(2) Uani 1 1 d . . .
C17 C 0.5337(7) 0.0071(7) 0.5978(2) 0.055(3) Uani 1 1 d . . .
O1 O 0.2717(4) -0.1069(4) 0.79846(14) 0.0543(18) Uani 1 1 d . . .
O2 O 0.2922(4) -0.1525(4) 0.84018(13) 0.0541(18) Uani 1 1 d . . .
O1W O 0.0184(9) -0.2620(10) 0.7720(4) 0.029(4) Uani 0.33 1 d PU . .
O3 O 0.5377(4) -0.1522(4) 0.85508(14) 0.0487(16) Uani 1 1 d U . .
O2W' O 0.0621(16) -0.0886(16) 0.7741(6) 0.061(8) Uani 0.33 1 d PU . .
O4 O 0.6117(3) -0.1374(4) 0.81711(13) 0.0472(16) Uani 1 1 d . . .
O3W O -0.005(3) -0.037(2) 0.7835(7) 0.143(14) Uani 0.33 1 d PU . .
O5 O 0.4722(4) -0.0341(5) 0.58441(16) 0.069(2) Uani 1 1 d . . .
O4W O 0.3333 -0.3333 0.7529(12) 0.31(3) Uani 1 3 d S . .
O6 O 0.5896(4) 0.0654(4) 0.58564(14) 0.062(2) Uani 1 1 d . . .
Tb1 Tb 0.14041(2) -0.14788(2) 0.792647(8) 0.03303(19) Uani 1 1 d . . .
O7 O 0.4768(8) -0.0855(9) 0.7315(3) 0.050(4) Uani 0.50 1 d PU A 1
C9 C 0.5611(9) -0.0500(11) 0.7210(4) 0.030(4) Uani 0.50 1 d PU A 1
H9A H 0.5827 -0.0830 0.7258 0.036 Uiso 0.50 1 calc PR A 1
H9B H 0.5940 0.0014 0.7292 0.036 Uiso 0.50 1 calc PR A 1
O7' O 0.4986(7) -0.0455(8) 0.7353(3) 0.038(3) Uani 0.50 1 d PU A 2
C9' C 0.5383(15) -0.0943(16) 0.7179(5) 0.067(6) Uani 0.50 1 d PU A 2
H9'1 H 0.5869 -0.0849 0.7266 0.080 Uiso 0.50 1 calc PR A 2
H9'2 H 0.5024 -0.1497 0.7160 0.080 Uiso 0.50 1 calc PR A 2
O1W' O 0.0455(18) -0.1157(18) 0.7700(7) 0.076(9) Uani 0.33 1 d PU . .
O2W O 0.0259(14) -0.2214(15) 0.7665(6) 0.070(7) Uani 0.33 1 d PU . .
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'
Tb Tb -0.1723 4.1537 '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
O1 C1 O2 126.5(8) . .
O1 C1 C2 117.3(8) . .
O2 C1 C2 116.2(8) . .
C7 C2 C3 119.7(8) . .
C7 C2 C1 119.8(8) . .
C3 C2 C1 120.3(8) . .
C4 C3 C2 119.7(8) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C5 C4 C3 121.1(8) . .
C5 C4 C16 120.5(8) . .
C3 C4 C16 118.4(8) . .
C4 C5 C6 118.5(9) . .
C4 C5 H5 120.8 . .
C6 C5 H5 120.8 . .
C7 C6 C5 121.6(9) . .
C7 C6 O7 112.8(10) . .
C5 C6 O7 123.2(10) . .
C7 C6 O7' 114.4(10) . .
C5 C6 O7' 122.3(10) . .
O7 C6 O7' 29.0(6) . .
C6 C7 C2 119.4(9) . .
C6 C7 H7 120.3 . .
C2 C7 H7 120.3 . .
C15 C10 C11 118.8(14) . .
C15 C10 C9 129.8(15) . .
C11 C10 C9 111.3(16) . .
C15 C10 C9' 103.5(16) . .
C11 C10 C9' 137.0(18) . .
C9 C10 C9' 28.3(9) . .
C10 C11 C12 119.7(17) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C13 C12 C11 119.3(15) . .
C13 C12 H12 120.4 . .
C11 C12 H12 120.4 . .
C14 C13 C12 118.6(12) . .
C14 C13 C17 122.5(12) . .
C12 C13 C17 118.8(12) . .
C13 C14 C15 121.6(15) . .
C13 C14 H14 119.2 . .
C15 C14 H14 119.2 . .
C10 C15 C14 121.5(16) . .
C10 C15 H15 119.3 . .
C14 C15 H15 119.3 . .
O4 C16 O3 120.9(8) . .
O4 C16 C4 118.5(8) . .
O3 C16 C4 120.5(8) . .
O4 C16 Tb1 72.3(5) . 18_546
O3 C16 Tb1 48.9(4) . 18_546
C4 C16 Tb1 167.3(6) . 18_546
O5 C17 O6 121.0(9) . .
O5 C17 C13 118.5(10) . .
O6 C17 C13 120.5(10) . .
O5 C17 Tb1 60.9(5) . 14_556
O6 C17 Tb1 60.2(5) . 14_556
C13 C17 Tb1 178.0(8) . 14_556
C1 O1 Tb1 135.4(6) . .
C1 O2 Tb1 138.7(6) . 16_546
O2W O1W Tb1 66(2) . .
C16 O3 Tb1 107.2(5) . 18_546
O1W' O2W' Tb1 82(6) . .
C16 O4 Tb1 174.7(6) . 3_655
C16 O4 Tb1 82.9(5) . 18_546
Tb1 O4 Tb1 101.6(2) 3_655 18_546
O3W O3W O3W 60.00(4) 3 2
C17 O5 Tb1 92.5(6) . 14_556
C17 O6 Tb1 92.7(6) . 14_556
O4 Tb1 O2 77.7(2) 2_545 16_546
O4 Tb1 O2W 96.1(7) 2_545 .
O2 Tb1 O2W 74.7(6) 16_546 .
O4 Tb1 O1 77.5(2) 2_545 .
O2 Tb1 O1 131.9(2) 16_546 .
O2W Tb1 O1 148.4(6) . .
O4 Tb1 O3 126.9(2) 2_545 17_556
O2 Tb1 O3 81.4(2) 16_546 17_556
O2W Tb1 O3 124.3(7) . 17_556
O1 Tb1 O3 81.6(2) . 17_556
O4 Tb1 O6 138.6(2) 2_545 15_446
O2 Tb1 O6 141.0(2) 16_546 15_446
O2W Tb1 O6 85.5(7) . 15_446
O1 Tb1 O6 79.9(2) . 15_446
O3 Tb1 O6 82.6(2) 17_556 15_446
O4 Tb1 O5 87.2(2) 2_545 15_446
O2 Tb1 O5 142.2(3) 16_546 15_446
O2W Tb1 O5 72.7(6) . 15_446
O1 Tb1 O5 76.1(3) . 15_446
O3 Tb1 O5 133.5(2) 17_556 15_446
O6 Tb1 O5 53.8(2) 15_446 15_446
O4 Tb1 O1W' 137.7(8) 2_545 .
O2 Tb1 O1W' 72.7(8) 16_546 .
O2W Tb1 O1W' 47.3(10) . .
O1 Tb1 O1W' 144.6(8) . .
O3 Tb1 O1W' 77.8(7) 17_556 .
O6 Tb1 O1W' 69.2(8) 15_446 .
O5 Tb1 O1W' 98.0(8) 15_446 .
O4 Tb1 O2W' 146.0(7) 2_545 .
O2 Tb1 O2W' 73.6(6) 16_546 .
O2W Tb1 O2W' 58.9(9) . .
O1 Tb1 O2W' 136.1(7) . .
O3 Tb1 O2W' 66.3(7) 17_556 .
O6 Tb1 O2W' 67.4(7) 15_446 .
O5 Tb1 O2W' 104.4(7) 15_446 .
O1W' Tb1 O2W' 11.6(9) . .
O4 Tb1 O1W 78.3(4) 2_545 .
O2 Tb1 O1W 72.3(4) 16_546 .
O2W Tb1 O1W 17.9(6) . .
O1 Tb1 O1W 139.5(4) . .
O3 Tb1 O1W 138.7(4) 17_556 .
O6 Tb1 O1W 98.0(4) 15_446 .
O5 Tb1 O1W 70.7(4) 15_446 .
O1W' Tb1 O1W 64.4(8) . .
O2W' Tb1 O1W 75.8(8) . .
O4 Tb1 C17 112.9(3) 2_545 15_446
O2 Tb1 C17 151.3(3) 16_546 15_446
O2W Tb1 C17 77.6(6) . 15_446
O1 Tb1 C17 76.7(3) . 15_446
O3 Tb1 C17 108.6(3) 17_556 15_446
O6 Tb1 C17 27.2(3) 15_446 15_446
O5 Tb1 C17 26.6(3) 15_446 15_446
O1W' Tb1 C17 83.1(8) . 15_446
O2W' Tb1 C17 85.7(7) . 15_446
O1W Tb1 C17 83.6(4) . 15_446
O4 Tb1 O4 78.4(2) 2_545 17_556
O2 Tb1 O4 66.9(2) 16_546 17_556
O2W Tb1 O4 141.6(6) . 17_556
O1 Tb1 O4 68.1(2) . 17_556
O3 Tb1 O4 48.5(2) 17_556 17_556
O6 Tb1 O4 123.5(2) 15_446 17_556
O5 Tb1 O4 143.5(2) 15_446 17_556
O1W' Tb1 O4 115.3(8) . 17_556
O2W' Tb1 O4 106.2(7) . 17_556
O1W Tb1 O4 136.3(4) . 17_556
C17 Tb1 O4 139.8(3) 15_446 17_556
C6 O7 C9 109.9(12) . .
O7 C9 C10 100.3(12) . .
O7 C9 H9A 111.7 . .
C10 C9 H9A 111.7 . .
O7 C9 H9B 111.7 . .
C10 C9 H9B 111.7 . .
H9A C9 H9B 109.5 . .
C6 O7' C9' 101.7(12) . .
C10 C9' O7' 92.1(14) . .
C10 C9' H9'1 113.3 . .
O7' C9' H9'1 113.3 . .
C10 C9' H9'2 113.3 . .
O7' C9' H9'2 113.3 . .
H9'1 C9' H9'2 110.6 . .
O2W' O1W' Tb1 87(6) . .
O1W O2W Tb1 96(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.236(10) .
C1 O2 1.258(11) .
C1 C2 1.532(12) .
C2 C7 1.379(13) .
C2 C3 1.407(12) .
C3 C4 1.378(12) .
C3 H3 0.9300 .
C4 C5 1.373(12) .
C4 C16 1.479(12) .
C5 C6 1.399(14) .
C5 H5 0.9300 .
C6 C7 1.376(14) .
C6 O7 1.415(17) .
C6 O7' 1.423(16) .
C7 H7 0.9300 .
C10 C15 1.31(2) .
C10 C11 1.37(2) .
C10 C9 1.54(2) .
C10 C9' 1.62(3) .
C11 C12 1.43(2) .
C11 H11 0.9300 .
C12 C13 1.357(18) .
C12 H12 0.9300 .
C13 C14 1.331(18) .
C13 C17 1.507(13) .
C14 C15 1.394(18) .
C14 H14 0.9300 .
C15 H15 0.9300 .
C16 O4 1.257(10) .
C16 O3 1.261(10) .
C16 Tb1 2.978(9) 18_546
C17 O5 1.238(13) .
C17 O6 1.262(13) .
C17 Tb1 2.761(10) 14_556
O1 Tb1 2.325(6) .
O2 Tb1 2.322(6) 16_546
O1W O2W 0.78(2) .
O1W Tb1 2.530(16) .
O3 Tb1 2.351(6) 18_546
O2W' O1W' 0.51(4) .
O2W' Tb1 2.52(3) .
O4 Tb1 2.303(6) 3_655
O4 Tb1 2.859(6) 18_546
O3W O3W 1.20(5) 3
O3W O3W 1.20(5) 2
O5 Tb1 2.414(7) 14_556
O6 Tb1 2.399(7) 14_556
Tb1 O4 2.303(6) 2_545
Tb1 O2 2.322(6) 16_546
Tb1 O2W 2.32(2) .
Tb1 O3 2.351(6) 17_556
Tb1 O6 2.399(7) 15_446
Tb1 O5 2.414(7) 15_446
Tb1 O1W' 2.50(3) .
Tb1 C17 2.761(10) 15_446
Tb1 O4 2.859(6) 17_556
O7 C9 1.53(2) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
O7' C9' 1.72(3) .
C9' H9'1 0.9700 .
C9' H9'2 0.9700 .
