#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:24:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179109 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/71/4307148.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_4307148
loop_
_publ_author_name
'Zhongyue Li'
'Guangshan Zhu'
'Xiaodan Guo'
'Xiaojun Zhao'
'Zhao Jin'
'Shilun Qiu'
_publ_section_title
;
Synthesis, Structure, and Luminescent and Magnetic Properties of Novel
Lanthanide Metal-Organic Frameworks with Zeolite-like Topology
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5174
_journal_page_last               5178
_journal_paper_doi               10.1021/ic061666i
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C15 H19 N2 O9 Tm'
_chemical_formula_weight         540.25
_chemical_name_common            Tm(BTC)(DMF)2(H2O)
_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                 107.086(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.382(2)
_cell_length_b                   11.5929(15)
_cell_length_c                   19.632(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3998.9(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_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  0.0995
_diffrn_reflns_av_sigmaI/netI    0.1233
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11699
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.485
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_refine_diff_density_max         2.002
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4323
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0269P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1240
_reflns_number_gt                3064
_reflns_number_total             4323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061666i-file001_5.cif
_cod_data_source_block           Tm(BTC)(DMF)2(H2O)
_cod_original_cell_volume        3998.8(9)
_cod_database_code               4307148
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.07492(2) 0.82928(4) 0.08307(2) 0.02043(15) Uani 1 1 d . . .
O1 O 0.1759(5) 0.7332(8) 0.0528(4) 0.053(3) Uani 1 1 d . . .
O2 O 0.1509(4) 0.6803(8) 0.1488(4) 0.050(2) Uani 1 1 d . . .
O3 O 0.1560(4) 0.9478(7) 0.1698(3) 0.038(2) Uani 1 1 d . . .
O4 O 0.0698(4) 0.8534(6) 0.2034(3) 0.0253(17) Uani 1 1 d . . .
O5 O -0.0261(4) 0.9464(7) 0.0663(3) 0.038(2) Uani 1 1 d . . .
O6 O 0.1155(3) 0.9658(6) 0.0190(3) 0.0281(17) Uani 1 1 d . . .
O7 O 0.0171(5) 0.7668(8) -0.0322(4) 0.045(2) Uani 1 1 d . . .
O8 O -0.0198(5) 0.6981(7) 0.0881(4) 0.048(2) Uani 1 1 d . . .
O1W O 0.0000 0.482(2) 0.2500 0.069(7) Uani 0.60 2 d SP . .
O2W O 0.0000 0.388(4) 0.2500 0.090(14) Uani 0.40 2 d SP . .
O3W O 0.0000 0.297(4) 0.2500 0.129(14) Uani 0.60 2 d SPU . .
O4W O 0.0000 0.186(4) 0.2500 0.110(15) Uani 0.40 2 d SPU . .
C1 C 0.3082(5) 1.1764(10) 0.3921(5) 0.026(2) Uani 1 1 d . . .
C2 C 0.2398(5) 1.0968(9) 0.3746(5) 0.022(2) Uani 1 1 d . . .
C3 C 0.1995(5) 1.0818(9) 0.4235(5) 0.021(2) Uani 1 1 d . . .
H3A H 0.2154 1.1170 0.4680 0.025 Uiso 1 1 calc R . .
C4 C 0.1347(5) 1.0129(9) 0.4048(4) 0.022(2) Uani 1 1 d . . .
C5 C 0.1114(5) 0.9596(9) 0.3392(4) 0.022(2) Uani 1 1 d . . .
H5A H 0.0681 0.9133 0.3275 0.027 Uiso 1 1 calc R . .
C6 C 0.1531(5) 0.9751(10) 0.2896(5) 0.027(2) Uani 1 1 d . . .
C7 C 0.2169(5) 1.0429(9) 0.3087(5) 0.026(2) Uani 1 1 d . . .
H7A H 0.2453 1.0530 0.2769 0.031 Uiso 1 1 calc R . .
C8 C 0.1246(6) 0.9202(9) 0.2170(5) 0.025(2) Uani 1 1 d . . .
C9 C 0.0881(5) 0.9968(10) 0.4562(5) 0.026(2) Uani 1 1 d . . .
C10 C -0.0468(8) 0.7768(13) -0.0759(6) 0.048(3) Uani 1 1 d . . .
H10A H -0.0670 0.8509 -0.0825 0.057 Uiso 1 1 calc R . .
C11 C -0.0590(11) 0.5845(17) -0.1030(10) 0.121(8) Uani 1 1 d . . .
H11A H -0.0105 0.5832 -0.0671 0.182 Uiso 1 1 calc R . .
H11B H -0.0534 0.5566 -0.1472 0.182 Uiso 1 1 calc R . .
H11C H -0.0941 0.5362 -0.0884 0.182 Uiso 1 1 calc R . .
C12 C -0.1577(9) 0.7199(17) -0.1643(9) 0.118(8) Uani 1 1 d . . .
H12A H -0.1694 0.8008 -0.1655 0.176 Uiso 1 1 calc R . .
H12B H -0.1971 0.6770 -0.1526 0.176 Uiso 1 1 calc R . .
H12C H -0.1546 0.6961 -0.2102 0.176 Uiso 1 1 calc R . .
C13 C -0.0524(7) 0.6802(11) 0.1321(6) 0.045(3) Uani 1 1 d . . .
H13A H -0.0257 0.6997 0.1787 0.053 Uiso 1 1 calc R . .
C14 C -0.1633(12) 0.593(2) 0.0526(10) 0.144(8) Uani 1 1 d U . .
H14A H -0.1362 0.6098 0.0188 0.216 Uiso 1 1 calc R . .
H14B H -0.2125 0.6288 0.0377 0.216 Uiso 1 1 calc R . .
H14C H -0.1693 0.5108 0.0553 0.216 Uiso 1 1 calc R . .
C15 C -0.1573(10) 0.6157(17) 0.1791(9) 0.104(6) Uani 1 1 d . . .
H15A H -0.1248 0.6424 0.2241 0.156 Uiso 1 1 calc R . .
H15B H -0.1664 0.5345 0.1821 0.156 Uiso 1 1 calc R . .
H15C H -0.2049 0.6563 0.1678 0.156 Uiso 1 1 calc R . .
N1 N -0.0870(7) 0.6991(10) -0.1121(6) 0.062(3) Uani 1 1 d . . .
N2 N -0.1204(6) 0.6369(12) 0.1230(6) 0.070(4) 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'
N N 0.0061 0.0033 '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'
Tm Tm -0.3139 5.2483 '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 Tm1 O6 83.7(2) . . ?
O5 Tm1 O7 85.6(3) . . ?
O6 Tm1 O7 79.0(3) . . ?
O5 Tm1 O8 78.8(3) . . ?
O6 Tm1 O8 147.6(2) . . ?
O7 Tm1 O8 72.7(3) . . ?
O5 Tm1 O3 94.3(3) . . ?
O6 Tm1 O3 75.7(2) . . ?
O7 Tm1 O3 154.5(3) . . ?
O8 Tm1 O3 132.3(2) . . ?
O5 Tm1 O2 148.9(2) . . ?
O6 Tm1 O2 125.1(2) . . ?
O7 Tm1 O2 109.5(3) . . ?
O8 Tm1 O2 80.1(3) . . ?
O3 Tm1 O2 83.3(3) . . ?
O5 Tm1 O1 156.4(2) . . ?
O6 Tm1 O1 77.4(3) . . ?
O7 Tm1 O1 77.2(3) . . ?
O8 Tm1 O1 110.6(3) . . ?
O3 Tm1 O1 94.5(3) . . ?
O2 Tm1 O1 54.2(2) . . ?
O5 Tm1 O4 78.8(2) . . ?
O6 Tm1 O4 125.1(2) . . ?
O7 Tm1 O4 148.9(3) . . ?
O8 Tm1 O4 77.9(2) . . ?
O3 Tm1 O4 54.5(2) . . ?
O2 Tm1 O4 74.6(2) . . ?
O1 Tm1 O4 123.8(2) . . ?
O5 Tm1 C1 175.8(3) . 4_545 ?
O6 Tm1 C1 100.5(3) . 4_545 ?
O7 Tm1 C1 94.8(3) . 4_545 ?
O8 Tm1 C1 97.3(3) . 4_545 ?
O3 Tm1 C1 87.2(3) . 4_545 ?
O2 Tm1 C1 27.4(2) . 4_545 ?
O1 Tm1 C1 26.8(2) . 4_545 ?
O4 Tm1 C1 99.0(3) . 4_545 ?
O5 Tm1 C8 86.3(3) . . ?
O6 Tm1 C8 101.1(3) . . ?
O7 Tm1 C8 171.9(3) . . ?
O8 Tm1 C8 104.7(3) . . ?
O3 Tm1 C8 27.6(3) . . ?
O2 Tm1 C8 77.2(3) . . ?
O1 Tm1 C8 110.9(3) . . ?
O4 Tm1 C8 26.9(2) . . ?
C1 Tm1 C8 93.2(3) 4_545 . ?
C1 O1 Tm1 91.8(6) 4_545 . ?
C1 O2 Tm1 92.6(6) 4_545 . ?
C8 O3 Tm1 93.1(6) . . ?
C8 O4 Tm1 91.2(5) . . ?
C9 O5 Tm1 166.1(7) 2 . ?
C9 O6 Tm1 132.5(6) 6_575 . ?
C10 O7 Tm1 135.9(8) . . ?
C13 O8 Tm1 132.5(8) . . ?
O3W O2W O1W 180.000(11) . . ?
O2W O3W O4W 180.000(14) . . ?
O1 C1 O2 121.0(9) 4 4 ?
O1 C1 C2 119.5(8) 4 . ?
O2 C1 C2 119.4(9) 4 . ?
O1 C1 Tm1 61.4(5) 4 4 ?
O2 C1 Tm1 60.0(5) 4 4 ?
C2 C1 Tm1 176.1(7) . 4 ?
C7 C2 C3 120.9(9) . . ?
C7 C2 C1 119.3(8) . . ?
C3 C2 C1 119.8(8) . . ?
C2 C3 C4 118.6(8) . . ?
C5 C4 C3 120.8(8) . . ?
C5 C4 C9 119.0(9) . . ?
C3 C4 C9 120.2(8) . . ?
C4 C5 C6 120.1(9) . . ?
C7 C6 C5 118.6(9) . . ?
C7 C6 C8 122.2(8) . . ?
C5 C6 C8 119.2(9) . . ?
C6 C7 C2 120.9(9) . . ?
O4 C8 O3 121.2(9) . . ?
O4 C8 C6 120.3(9) . . ?
O3 C8 C6 118.5(9) . . ?
O4 C8 Tm1 61.9(5) . . ?
O3 C8 Tm1 59.3(5) . . ?
C6 C8 Tm1 177.5(7) . . ?
O5 C9 O6 124.7(8) 2 6_576 ?
O5 C9 C4 117.5(8) 2 . ?
O6 C9 C4 117.8(8) 6_576 . ?
O7 C10 N1 127.6(14) . . ?
O8 C13 N2 128.5(11) . . ?
C10 N1 C11 118.1(13) . . ?
C10 N1 C12 123.6(14) . . ?
C11 N1 C12 118.2(13) . . ?
C13 N2 C14 119.4(13) . . ?
C13 N2 C15 126.3(12) . . ?
C14 N2 C15 114.0(14) . . ?
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
Tm1 O5 2.245(7) . ?
Tm1 O6 2.279(7) . ?
Tm1 O7 2.315(7) . ?
Tm1 O8 2.336(8) . ?
Tm1 O3 2.349(7) . ?
Tm1 O2 2.354(8) . ?
Tm1 O1 2.385(7) . ?
Tm1 O4 2.408(6) . ?
Tm1 C1 2.716(9) 4_545 ?
Tm1 C8 2.729(9) . ?
O1 C1 1.227(11) 4_545 ?
O2 C1 1.251(11) 4_545 ?
O3 C8 1.268(11) . ?
O4 C8 1.235(11) . ?
O5 C9 1.241(10) 2 ?
O6 C9 1.264(10) 6_575 ?
O7 C10 1.239(13) . ?
O8 C13 1.205(13) . ?
O1W O2W 1.08(4) . ?
O2W O3W 1.06(5) . ?
O3W O4W 1.29(5) . ?
C1 O1 1.227(11) 4 ?
C1 O2 1.251(11) 4 ?
C1 C2 1.516(13) . ?
C1 Tm1 2.716(9) 4 ?
C2 C7 1.386(12) . ?
C2 C3 1.387(12) . ?
C3 C4 1.390(12) . ?
C4 C5 1.378(12) . ?
C4 C9 1.515(12) . ?
C5 C6 1.417(12) . ?
C6 C7 1.369(13) . ?
C6 C8 1.508(13) . ?
C9 O5 1.241(10) 2 ?
C9 O6 1.264(10) 6_576 ?
C10 N1 1.247(15) . ?
C11 N1 1.42(2) . ?
C12 N1 1.419(16) . ?
C13 N2 1.309(15) . ?
C14 N2 1.466(19) . ?
C15 N2 1.477(17) . ?
