#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/62/4506284.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_4506284
loop_
_publ_author_name
'Wang, Hao'
'Liu, Sui-Jun'
'Tian, Dan'
'Jia, Ji-Min'
'Hu, Tong-Liang'
_publ_section_title
;
 Temperature-Dependent Structures of Lanthanide Metal--Organic Frameworks
 Based on Furan-2,5-Dicarboxylate and Oxalate
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3263
_journal_paper_doi               10.1021/cg3004036
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C7 H6 Tb O9,H2 O'
_chemical_formula_sum            'C7 H8 O10 Tb'
_chemical_formula_weight         411.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 117.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.775(3)
_cell_length_b                   10.569(2)
_cell_length_c                   13.697(3)
_cell_measurement_reflns_used    10340
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.20
_cell_volume                     2153.4(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       ω
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9284
_diffrn_reflns_theta_full        25.19
_diffrn_reflns_theta_max         25.19
_diffrn_reflns_theta_min         3.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.617
_exptl_absorpt_correction_T_max  0.2781
_exptl_absorpt_correction_T_min  0.2588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Higashi,1995
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         1930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0260
_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)+(0.0193P)²+17.7186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                1704
_reflns_number_total             1930
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3004036_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2153.4(7)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4506284
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
O2 O 0.1429(3) 1.1913(4) 0.9619(3) 0.0322(10) Uani 1 1 d .
O1 O 0.2313(2) 1.0223(3) 0.9960(3) 0.0244(9) Uani 1 1 d .
C1 C 0.1556(3) 1.0751(5) 0.9615(4) 0.0191(11) Uani 1 1 d .
O9 O -0.1171(2) 0.3806(4) 0.6881(3) 0.0240(9) Uani 1 1 d .
O4 O -0.0591(2) 0.6213(3) 0.9005(3) 0.0232(9) Uani 1 1 d .
Tb1 Tb 0.135388(16) 0.40327(2) 0.99748(2) 0.01580(9) Uani 1 1 d .
O3 O 0.0918(2) 0.8645(3) 0.9285(3) 0.0204(8) Uani 1 1 d .
C5 C 0.0097(3) 0.8080(5) 0.8898(4) 0.0194(11) Uani 1 1 d .
O5 O 0.0768(2) 0.6068(3) 0.9112(3) 0.0305(9) Uani 1 1 d .
O8 O -0.0187(2) 0.3559(3) 0.8646(3) 0.0213(8) Uani 1 1 d .
O1W O 0.2717(3) 0.7976(4) 0.1374(3) 0.0344(10) Uani 1 1 d G
H1WA H 0.3263 0.7899 0.1509 0.052 Uiso 1 1 d G
H1WB H 0.2441 0.8445 0.0812 0.052 Uiso 1 1 d G
O3W O 0.2487(3) 0.3091(4) 1.1691(3) 0.0378(11) Uani 1 1 d .
H3WB H 0.2286 0.3068 1.2159 0.057 Uiso 1 1 d R
H3WA H 0.2601 0.2343 1.1563 0.057 Uiso 1 1 d R
C3 C -0.0133(3) 1.0153(5) 0.8705(4) 0.0221(12) Uani 1 1 d .
H3 H -0.0410 1.0941 0.8532 0.026 Uiso 1 1 calc R
C6 C 0.0096(3) 0.6672(5) 0.9012(4) 0.0187(12) Uani 1 1 d .
C4 C -0.0567(4) 0.8957(5) 0.8523(4) 0.0242(12) Uani 1 1 d .
H4 H -0.1183 0.8807 0.8210 0.029 Uiso 1 1 calc R
C7 C -0.0392(3) 0.3702(5) 0.7656(4) 0.0178(11) Uani 1 1 d .
C2 C 0.0751(3) 0.9926(5) 0.9171(4) 0.0169(11) Uani 1 1 d .
O2W O 0.1894(3) 0.5649(4) 1.1403(4) 0.0366(11) Uani 1 1 d .
H2WA H 0.2116 0.6281 1.1206 0.055 Uiso 1 1 d R
H2WB H 0.1456 0.5923 1.1515 0.055 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'
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
C1 O2 Tb1 169.4(4) . 1_565
C1 O1 Tb1 130.3(3) . 7_567
O2 C1 O1 125.3(5) . .
O2 C1 C2 117.1(5) . .
O1 C1 C2 117.6(4) . .
C7 O9 Tb1 118.3(3) . 2_556
C6 O4 Tb1 144.1(3) . 5_567
O4 Tb1 O2 96.80(13) 5_567 1_545
O4 Tb1 O1 143.71(13) 5_567 7_567
O2 Tb1 O1 100.97(13) 1_545 7_567
O4 Tb1 O9 141.91(13) 5_567 2_556
O2 Tb1 O9 71.08(14) 1_545 2_556
O1 Tb1 O9 74.23(13) 7_567 2_556
O4 Tb1 O8 74.58(13) 5_567 .
O2 Tb1 O8 77.59(13) 1_545 .
O1 Tb1 O8 140.14(13) 7_567 .
O9 Tb1 O8 67.62(12) 2_556 .
O4 Tb1 O5 100.45(13) 5_567 .
O2 Tb1 O5 143.61(15) 1_545 .
O1 Tb1 O5 83.41(13) 7_567 .
O9 Tb1 O5 75.62(13) 2_556 .
O8 Tb1 O5 76.52(13) . .
O4 Tb1 O2W 72.32(13) 5_567 .
O2 Tb1 O2W 144.50(15) 1_545 .
O1 Tb1 O2W 74.86(13) 7_567 .
O9 Tb1 O2W 136.97(13) 2_556 .
O8 Tb1 O2W 128.21(13) . .
O5 Tb1 O2W 71.74(15) . .
O4 Tb1 O3W 76.95(14) 5_567 .
O2 Tb1 O3W 73.40(15) 1_545 .
O1 Tb1 O3W 78.21(14) 7_567 .
O9 Tb1 O3W 129.15(13) 2_556 .
O8 Tb1 O3W 136.11(14) . .
O5 Tb1 O3W 141.79(15) . .
O2W Tb1 O3W 71.24(15) . .
C5 O3 C2 105.6(4) . .
C4 C5 O3 110.7(5) . .
C4 C5 C6 132.8(5) . .
O3 C5 C6 116.4(4) . .
C6 O5 Tb1 130.4(3) . .
C7 O8 Tb1 117.0(3) . .
H1WA O1W H1WB 109.5 . .
Tb1 O3W H3WB 109.5 . .
Tb1 O3W H3WA 109.2 . .
H3WB O3W H3WA 109.5 . .
C2 C3 C4 106.8(5) . .
C2 C3 H3 126.6 . .
C4 C3 H3 126.6 . .
O5 C6 O4 126.0(5) . .
O5 C6 C5 118.5(4) . .
O4 C6 C5 115.6(5) . .
C5 C4 C3 106.0(5) . .
C5 C4 H4 127.0 . .
C3 C4 H4 127.0 . .
O8 C7 O9 126.1(5) . .
O8 C7 C7 117.1(6) . 2_556
O9 C7 C7 116.8(6) . 2_556
C3 C2 O3 110.7(4) . .
C3 C2 C1 133.6(5) . .
O3 C2 C1 115.6(4) . .
Tb1 O2W H2WA 110.1 . .
Tb1 O2W H2WB 110.2 . .
H2WA O2W H2WB 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O2 C1 1.247(6) .
O2 Tb1 2.308(4) 1_565
O1 C1 1.262(6) .
O1 Tb1 2.333(3) 7_567
C1 C2 1.482(7) .
O9 C7 1.251(6) .
O9 Tb1 2.427(4) 2_556
O4 C6 1.247(6) .
O4 Tb1 2.304(4) 5_567
Tb1 O4 2.304(4) 5_567
Tb1 O2 2.308(4) 1_545
Tb1 O1 2.333(3) 7_567
Tb1 O9 2.427(4) 2_556
Tb1 O8 2.428(4) .
Tb1 O5 2.432(4) .
Tb1 O2W 2.434(4) .
Tb1 O3W 2.449(4) .
O3 C5 1.364(6) .
O3 C2 1.377(6) .
C5 C4 1.355(7) .
C5 C6 1.496(7) .
O5 C6 1.247(6) .
O8 C7 1.245(6) .
O1W H1WA 0.8501 .
O1W H1WB 0.8499 .
O3W H3WB 0.8505 .
O3W H3WA 0.8502 .
C3 C2 1.337(7) .
C3 C4 1.422(7) .
C3 H3 0.9300 .
C4 H4 0.9300 .
C7 C7 1.559(10) 2_556
O2W H2WA 0.8669 .
O2W H2WB 0.8668 .
