#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:02:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179228 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/48/4314885.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_4314885
loop_
_publ_author_name
'Xia Li'
'Hao-Ling Sun'
'Xiao-Shuo Wu'
'Xiao Qiu'
'Miao Du'
_publ_section_title
;
 Unique (3,12)-Connected Porous Lanthanide-Organic Frameworks Based on
 Ln4O4 Clusters: Synthesis, Crystal Structures, Luminescence, and
 Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1865
_journal_page_last               1871
_journal_paper_doi               10.1021/ic902241n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C28 H44 O36 S4 Tb4'
_chemical_formula_weight         1720.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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            2
_cell_length_a                   17.1205(7)
_cell_length_b                   17.1205(7)
_cell_length_c                   8.4672(6)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.63
_cell_measurement_theta_min      3.37
_cell_volume                     2481.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  '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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5558
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    5.903
_exptl_absorpt_correction_T_max  0.7568
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2866
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0174P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                2606
_reflns_number_total             2866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902241n_si_004.cif
_cod_data_source_block           090418a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314885
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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 0.2588(3) 0.3730(3) 1.0377(8) 0.0241(13) Uani 1 1 d . . .
C2 C 0.2237(3) 0.3020(3) 1.0021(7) 0.0245(14) Uani 1 1 d . . .
H2 H 0.2513 0.2640 0.9469 0.029 Uiso 1 1 calc R . .
C3 C 0.1474(4) 0.2882(3) 1.0493(8) 0.0273(14) Uani 1 1 d . . .
C4 C 0.1079(4) 0.2136(4) 1.0081(7) 0.0284(14) Uani 1 1 d . . .
C5 C 0.1094(4) 0.3443(4) 1.1376(10) 0.0416(17) Uani 1 1 d . . .
H5 H 0.0586 0.3351 1.1721 0.050 Uiso 1 1 calc R . .
C6 C 0.1460(4) 0.4143(4) 1.1757(10) 0.046(2) Uani 1 1 d . . .
H6 H 0.1202 0.4512 1.2372 0.055 Uiso 1 1 calc R . .
C7 C 0.2196(4) 0.4289(4) 1.1230(9) 0.0367(18) Uani 1 1 d . . .
H7 H 0.2434 0.4765 1.1446 0.044 Uiso 1 1 calc R . .
Tb1 Tb 0.390183(14) 0.537329(14) 0.64980(4) 0.01683(7) Uani 1 1 d . . .
O1 O 0.3491(2) 0.4506(2) 0.8530(6) 0.0322(9) Uani 1 1 d . . .
O2 O 0.3952(2) 0.4247(2) 1.1157(5) 0.0267(10) Uani 1 1 d . . .
O3 O 0.3904(3) 0.3205(2) 0.9181(5) 0.0316(10) Uani 1 1 d . . .
O4 O 0.1482(3) 0.1587(3) 0.9562(6) 0.0377(11) Uani 1 1 d . . .
O5 O 0.0339(3) 0.2108(2) 1.0307(5) 0.0335(10) Uani 1 1 d . . .
O6 O 0.4741(2) 0.4275(2) 0.6208(5) 0.0202(9) Uani 1 1 d D . .
O7 O 0.2638(3) 0.5794(3) 0.7657(6) 0.0380(12) Uani 1 1 d D . .
O8 O 0.3625(5) 0.1720(6) 0.7979(18) 0.173(6) Uani 1 1 d D . .
O9 O 0.9302(8) 0.3535(10) -0.0371(17) 0.200(6) Uani 1 1 d D . .
S1 S 0.35614(8) 0.39234(9) 0.97636(17) 0.0203(3) Uani 1 1 d . . .
H1W H 0.466(6) 0.404(6) 0.720(6) 0.113(17) Uiso 1 1 d D . .
H5W H 0.380(7) 0.182(6) 0.691(5) 0.113(17) Uiso 1 1 d D . .
H3W H 0.227(4) 0.615(4) 0.726(10) 0.113(17) Uiso 1 1 d D . .
H6W H 0.370(6) 0.221(3) 0.850(10) 0.113(17) Uiso 1 1 d D . .
H4W H 0.254(6) 0.575(6) 0.876(3) 0.113(17) Uiso 1 1 d D . .
H8W H 0.976(4) 0.322(6) -0.018(12) 0.113(17) Uiso 1 1 d D . .
H7W H 0.905(6) 0.358(7) 0.066(7) 0.113(17) Uiso 1 1 d 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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
C7 C1 C2 120.9(6) . . ?
C7 C1 S1 118.8(4) . . ?
C2 C1 S1 120.4(5) . . ?
C3 C2 C1 119.6(6) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C5 C3 C2 118.8(5) . . ?
C5 C3 C4 120.7(6) . . ?
C2 C3 C4 120.5(6) . . ?
O4 C4 O5 124.9(5) . . ?
O4 C4 C3 118.6(6) . . ?
O5 C4 C3 116.5(6) . . ?
C3 C5 C6 120.8(6) . . ?
C3 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C7 C6 C5 120.0(6) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C1 119.8(6) . . ?
C6 C7 H7 120.1 . . ?
C1 C7 H7 120.1 . . ?
O5 Tb1 O4 95.13(16) 7_554 5_556 ?
O5 Tb1 O2 142.88(14) 7_554 3_567 ?
O4 Tb1 O2 87.65(16) 5_556 3_567 ?
O5 Tb1 O6 89.41(14) 7_554 . ?
O4 Tb1 O6 145.68(15) 5_556 . ?
O2 Tb1 O6 108.70(14) 3_567 . ?
O5 Tb1 O1 76.60(15) 7_554 . ?
O4 Tb1 O1 138.02(15) 5_556 . ?
O2 Tb1 O1 76.84(15) 3_567 . ?
O6 Tb1 O1 76.09(14) . . ?
O5 Tb1 O6 75.03(14) 7_554 3_566 ?
O4 Tb1 O6 77.36(14) 5_556 3_566 ?
O2 Tb1 O6 140.97(14) 3_567 3_566 ?
O6 Tb1 O6 71.01(16) . 3_566 ?
O1 Tb1 O6 136.23(14) . 3_566 ?
O5 Tb1 O6 142.80(15) 7_554 2_665 ?
O4 Tb1 O6 90.54(15) 5_556 2_665 ?
O2 Tb1 O6 73.95(14) 3_567 2_665 ?
O6 Tb1 O6 66.76(15) . 2_665 ?
O1 Tb1 O6 120.94(14) . 2_665 ?
O6 Tb1 O6 70.43(16) 3_566 2_665 ?
O5 Tb1 O7 71.22(17) 7_554 . ?
O4 Tb1 O7 69.63(16) 5_556 . ?
O2 Tb1 O7 75.24(16) 3_567 . ?
O6 Tb1 O7 142.77(15) . . ?
O1 Tb1 O7 68.75(16) . . ?
O6 Tb1 O7 129.53(15) 3_566 . ?
O6 Tb1 O7 143.82(16) 2_665 . ?
O5 Tb1 Tb1 66.87(11) 7_554 4_656 ?
O4 Tb1 Tb1 115.03(12) 5_556 4_656 ?
O2 Tb1 Tb1 143.46(9) 3_567 4_656 ?
O6 Tb1 Tb1 37.50(10) . 4_656 ?
O1 Tb1 Tb1 99.56(11) . 4_656 ?
O6 Tb1 Tb1 38.21(9) 3_566 4_656 ?
O6 Tb1 Tb1 77.42(9) 2_665 4_656 ?
O7 Tb1 Tb1 138.06(12) . 4_656 ?
O5 Tb1 Tb1 111.92(11) 7_554 3_566 ?
O4 Tb1 Tb1 68.97(11) 5_556 3_566 ?
O2 Tb1 Tb1 103.62(10) 3_567 3_566 ?
O6 Tb1 Tb1 77.77(9) . 3_566 ?
O1 Tb1 Tb1 152.40(10) . 3_566 ?
O6 Tb1 Tb1 37.36(9) 3_566 3_566 ?
O6 Tb1 Tb1 37.71(9) 2_665 3_566 ?
O7 Tb1 Tb1 138.60(12) . 3_566 ?
Tb1 Tb1 Tb1 63.299(9) 4_656 3_566 ?
O5 Tb1 Tb1 122.08(11) 7_554 2_665 ?
O4 Tb1 Tb1 123.20(12) 5_556 2_665 ?
O2 Tb1 Tb1 85.44(9) 3_567 2_665 ?
O6 Tb1 Tb1 34.31(9) . 2_665 ?
O1 Tb1 Tb1 94.53(10) . 2_665 ?
O6 Tb1 Tb1 73.76(9) 3_566 2_665 ?
O6 Tb1 Tb1 33.76(9) 2_665 2_665 ?
O7 Tb1 Tb1 156.71(12) . 2_665 ?
Tb1 Tb1 Tb1 58.350(5) 4_656 2_665 ?
Tb1 Tb1 Tb1 58.350(5) 3_566 2_665 ?
S1 O1 Tb1 157.8(3) . . ?
S1 O2 Tb1 143.3(2) . 4_657 ?
C4 O4 Tb1 130.2(4) . 5_546 ?
C4 O5 Tb1 127.3(4) . 7 ?
Tb1 O6 Tb1 105.14(15) . 4_656 ?
Tb1 O6 Tb1 111.94(14) . 2_665 ?
Tb1 O6 Tb1 104.08(15) 4_656 2_665 ?
Tb1 O6 H1W 99(7) . . ?
Tb1 O6 H1W 137(7) 4_656 . ?
Tb1 O6 H1W 99(7) 2_665 . ?
Tb1 O7 H3W 129(6) . . ?
Tb1 O7 H4W 121(6) . . ?
H3W O7 H4W 106(3) . . ?
H5W O8 H6W 103(3) . . ?
H8W O9 H7W 105(3) . . ?
O1 S1 O3 111.9(3) . . ?
O1 S1 O2 111.0(3) . . ?
O3 S1 O2 114.3(3) . . ?
O1 S1 C1 105.1(3) . . ?
O3 S1 C1 108.7(3) . . ?
O2 S1 C1 105.3(3) . . ?
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
C1 C7 1.373(8) . ?
C1 C2 1.388(8) . ?
C1 S1 1.777(6) . ?
C2 C3 1.387(8) . ?
C2 H2 0.9300 . ?
C3 C5 1.380(8) . ?
C3 C4 1.486(8) . ?
C4 O4 1.245(8) . ?
C4 O5 1.282(8) . ?
C5 C6 1.391(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.360(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
Tb1 O5 2.344(4) 7_554 ?
Tb1 O4 2.357(4) 5_556 ?
Tb1 O2 2.372(4) 3_567 ?
Tb1 O6 2.379(4) . ?
Tb1 O1 2.379(4) . ?
Tb1 O6 2.387(4) 3_566 ?
Tb1 O6 2.413(4) 2_665 ?
Tb1 O7 2.482(5) . ?
Tb1 Tb1 3.7844(5) 4_656 ?
Tb1 Tb1 3.7844(5) 3_566 ?
Tb1 Tb1 3.9715(5) 2_665 ?
O1 S1 1.449(5) . ?
O2 S1 1.465(4) . ?
O2 Tb1 2.372(4) 4_657 ?
O3 S1 1.449(4) . ?
O4 Tb1 2.357(4) 5_546 ?
O5 Tb1 2.344(4) 7 ?
O6 Tb1 2.387(4) 4_656 ?
O6 Tb1 2.413(4) 2_665 ?
O6 H1W 0.94(2) . ?
O7 H3W 0.95(2) . ?
O7 H4W 0.95(2) . ?
O8 H5W 0.97(2) . ?
O8 H6W 0.96(2) . ?
O9 H8W 0.96(2) . ?
O9 H7W 0.97(2) . ?
