#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:24:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179109 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/71/4307147.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_4307147
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 Er N2 O9'
_chemical_formula_weight         538.58
_chemical_name_common            'Er(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                 106.979(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.4014(10)
_cell_length_b                   11.6492(10)
_cell_length_c                   19.6803(13)
_cell_measurement_temperature    293(2)
_cell_volume                     4034.8(5)
_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 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9977
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_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    4.207
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3408
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0509
_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)+(0.0818P)²+46.4113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                2976
_reflns_number_total             3408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061666i-file001_4.cif
_cod_data_source_block           Er(BTC)(DMF)2_(H2O)
_cod_database_code               4307147
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
Er1 Er 0.075168(10) 0.669750(16) 1.083308(9) 0.01980(5) Uani 1 1 d . . .
O1 O 0.02580(17) 0.4455(3) 0.93398(16) 0.0383(9) Uani 1 1 d . . .
O2 O 0.11599(17) 0.5328(3) 1.01842(14) 0.0293(8) Uani 1 1 d . . .
O3 O 0.3237(2) 0.7344(3) 0.94614(17) 0.0551(11) Uani 1 1 d . . .
O4 O 0.3486(2) 0.6806(3) 0.84996(19) 0.0522(11) Uani 1 1 d . . .
O5 O 0.15570(19) 0.4492(3) 0.67056(16) 0.0432(10) Uani 1 1 d . . .
O6 O 0.06987(16) 0.3531(2) 0.70347(15) 0.0251(8) Uani 1 1 d . . .
O7 O 0.0174(2) 0.7328(4) 0.96827(18) 0.0505(12) Uani 1 1 d . . .
O8 O -0.0200(2) 0.7992(3) 1.08880(19) 0.0461(11) Uani 1 1 d . . .
O1W O 0.0000 0.0968(17) 0.2500 0.101(6) Uani 0.50 2 d SP . .
O2W O 0.0000 0.3141(14) 0.2500 0.124(7) Uani 0.50 2 d SP . .
O3W O 0.0000 0.2040(12) 0.2500 0.077(3) Uani 0.50 2 d SPU . .
O4W O 0.0000 0.0070(9) 0.2500 0.062(4) Uani 0.50 2 d SP . .
C1 C 0.0892(2) 0.4952(4) 0.9564(2) 0.0249(11) Uani 1 1 d . . .
C2 C 0.1347(2) 0.5109(4) 0.9048(2) 0.0208(10) Uani 1 1 d . . .
C3 C 0.1115(2) 0.4579(4) 0.8391(2) 0.0224(11) Uani 1 1 d . . .
H3A H 0.0685 0.4115 0.8275 0.027 Uiso 1 1 calc R . .
C4 C 0.1527(2) 0.4738(4) 0.7897(2) 0.0221(11) Uani 1 1 d . . .
C5 C 0.2161(2) 0.5425(4) 0.8081(2) 0.0277(12) Uani 1 1 d . . .
H5A H 0.2434 0.5537 0.7757 0.033 Uiso 1 1 calc R . .
C6 C 0.2402(2) 0.5958(4) 0.8741(2) 0.0251(11) Uani 1 1 d . . .
C7 C 0.1996(2) 0.5802(4) 0.9228(2) 0.0241(11) Uani 1 1 d . . .
H7A H 0.2154 0.6156 0.9671 0.029 Uiso 1 1 calc R . .
C8 C 0.3073(3) 0.6756(4) 0.8916(2) 0.0302(12) Uani 1 1 d . . .
C9 C 0.1246(2) 0.4225(4) 0.7174(2) 0.0253(12) Uani 1 1 d . . .
C10 C -0.0456(3) 0.7241(5) 0.9262(3) 0.0471(17) Uani 1 1 d . . .
H10A H -0.0662 0.6506 0.9195 0.057 Uiso 1 1 calc R . .
C11 C -0.0623(6) 0.9211(8) 0.9038(5) 0.110(4) Uani 1 1 d . . .
H11A H -0.0135 0.9228 0.9389 0.164 Uiso 1 1 calc R . .
H11B H -0.0983 0.9627 0.9211 0.164 Uiso 1 1 calc R . .
H11C H -0.0586 0.9561 0.8608 0.164 Uiso 1 1 calc R . .
C12 C -0.1642(5) 0.7845(10) 0.8430(5) 0.125(4) Uani 1 1 d . . .
H12A H -0.1747 0.7036 0.8401 0.188 Uiso 1 1 calc R . .
H12B H -0.1682 0.8138 0.7965 0.188 Uiso 1 1 calc R . .
H12C H -0.2002 0.8230 0.8619 0.188 Uiso 1 1 calc R . .
C13 C -0.0524(3) 0.8197(4) 1.1325(3) 0.0415(16) Uani 1 1 d . . .
H13A H -0.0244 0.8060 1.1794 0.050 Uiso 1 1 calc R . .
C14 C -0.1662(7) 0.8850(12) 1.0497(7) 0.144(3) Uani 1 1 d U . .
H14A H -0.1362 0.8687 1.0183 0.216 Uiso 1 1 calc R . .
H14B H -0.1801 0.9647 1.0460 0.216 Uiso 1 1 calc R . .
H14C H -0.2114 0.8387 1.0367 0.216 Uiso 1 1 calc R . .
C15 C -0.1564(4) 0.8758(7) 1.1784(4) 0.083(2) Uani 1 1 d . . .
H15A H -0.1207 0.8568 1.2233 0.125 Uiso 1 1 calc R . .
H15B H -0.2003 0.8275 1.1703 0.125 Uiso 1 1 calc R . .
H15C H -0.1713 0.9547 1.1789 0.125 Uiso 1 1 calc R . .
N1 N -0.0869(3) 0.8043(4) 0.8899(3) 0.0610(18) Uani 1 1 d . . .
N2 N -0.1218(3) 0.8588(5) 1.1233(3) 0.0606(17) 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'
Er Er -0.2586 4.9576 '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
O1 Er1 O2 83.73(12) 5_567 . ?
O1 Er1 O7 85.31(13) 5_567 . ?
O2 Er1 O7 78.97(13) . . ?
O1 Er1 O8 78.10(13) 5_567 . ?
O2 Er1 O8 147.45(11) . . ?
O7 Er1 O8 72.86(14) . . ?
O1 Er1 O5 94.32(12) 5_567 6_566 ?
O2 Er1 O5 76.09(11) . 6_566 ?
O7 Er1 O5 154.94(14) . 6_566 ?
O8 Er1 O5 131.64(13) . 6_566 ?
O1 Er1 O4 148.63(13) 5_567 7_567 ?
O2 Er1 O4 125.39(12) . 7_567 ?
O7 Er1 O4 109.55(14) . 7_567 ?
O8 Er1 O4 80.23(13) . 7_567 ?
O5 Er1 O4 83.41(13) 6_566 7_567 ?
O1 Er1 O3 156.59(12) 5_567 7_567 ?
O2 Er1 O3 77.60(12) . 7_567 ?
O7 Er1 O3 77.40(13) . 7_567 ?
O8 Er1 O3 110.98(14) . 7_567 ?
O5 Er1 O3 94.77(13) 6_566 7_567 ?
O4 Er1 O3 54.14(13) 7_567 7_567 ?
O1 Er1 O6 79.23(10) 5_567 6_566 ?
O2 Er1 O6 125.53(10) . 6_566 ?
O7 Er1 O6 148.63(13) . 6_566 ?
O8 Er1 O6 77.30(11) . 6_566 ?
O5 Er1 O6 54.44(11) 6_566 6_566 ?
O4 Er1 O6 74.05(12) 7_567 6_566 ?
O3 Er1 O6 123.28(10) 7_567 6_566 ?
O1 Er1 C9 86.50(12) 5_567 6_566 ?
O2 Er1 C9 101.05(12) . 6_566 ?
O7 Er1 C9 171.76(14) . 6_566 ?
O8 Er1 C9 104.51(13) . 6_566 ?
O5 Er1 C9 27.19(13) 6_566 6_566 ?
O4 Er1 C9 77.27(13) 7_567 6_566 ?
O3 Er1 C9 110.72(12) 7_567 6_566 ?
O6 Er1 C9 27.26(12) 6_566 6_566 ?
O1 Er1 C8 175.39(14) 5_567 7_567 ?
O2 Er1 C8 100.78(13) . 7_567 ?
O7 Er1 C8 94.59(14) . 7_567 ?
O8 Er1 C8 97.46(14) . 7_567 ?
O5 Er1 C8 87.72(13) 6_566 7_567 ?
O4 Er1 C8 27.55(14) 7_567 7_567 ?
O3 Er1 C8 26.66(13) 7_567 7_567 ?
O6 Er1 C8 98.70(12) 6_566 7_567 ?
C9 Er1 C8 93.50(13) 6_566 7_567 ?
C1 O1 Er1 166.3(3) . 5_567 ?
C1 O2 Er1 133.1(3) . . ?
C8 O3 Er1 93.4(3) . 7_567 ?
C8 O4 Er1 92.6(3) . 7_567 ?
C9 O5 Er1 93.7(3) . 6_565 ?
C9 O6 Er1 91.4(3) . 6_565 ?
C10 O7 Er1 135.4(4) . . ?
C13 O8 Er1 133.9(3) . . ?
O4W O1W O3W 180.000(3) . . ?
O1W O3W O2W 180.000(4) . . ?
O2 C1 O1 124.1(4) . . ?
O2 C1 C2 118.5(4) . . ?
O1 C1 C2 117.4(3) . . ?
C3 C2 C7 120.1(4) . . ?
C3 C2 C1 119.7(4) . . ?
C7 C2 C1 120.1(4) . . ?
C2 C3 C4 120.3(4) . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 C9 121.1(4) . . ?
C3 C4 C9 120.0(4) . . ?
C4 C5 C6 121.5(4) . . ?
C7 C6 C5 119.7(4) . . ?
C7 C6 C8 119.6(4) . . ?
C5 C6 C8 120.5(4) . . ?
C6 C7 C2 119.5(4) . . ?
O3 C8 O4 119.6(4) . . ?
O3 C8 C6 121.2(5) . . ?
O4 C8 C6 119.1(4) . . ?
O3 C8 Er1 60.0(3) . 7_567 ?
O4 C8 Er1 59.9(2) . 7_567 ?
C6 C8 Er1 176.4(3) . 7_567 ?
O5 C9 O6 120.5(4) . . ?
O5 C9 C4 119.7(4) . . ?
O6 C9 C4 119.8(4) . . ?
O5 C9 Er1 59.1(2) . 6_565 ?
O6 C9 Er1 61.3(2) . 6_565 ?
C4 C9 Er1 178.8(3) . 6_565 ?
O7 C10 N1 127.6(5) . . ?
O8 C13 N2 129.1(5) . . ?
C10 N1 C11 118.9(6) . . ?
C10 N1 C12 122.9(6) . . ?
C11 N1 C12 117.5(7) . . ?
C13 N2 C15 125.0(5) . . ?
C13 N2 C14 116.4(7) . . ?
C15 N2 C14 118.6(7) . . ?
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
Er1 O1 2.236(3) 5_567 ?
Er1 O2 2.302(3) . ?
Er1 O7 2.321(3) . ?
Er1 O8 2.338(4) . ?
Er1 O5 2.362(3) 6_566 ?
Er1 O4 2.378(4) 7_567 ?
Er1 O3 2.382(4) 7_567 ?
Er1 O6 2.410(3) 6_566 ?
Er1 C9 2.746(4) 6_566 ?
Er1 C8 2.747(5) 7_567 ?
O1 C1 1.262(5) . ?
O1 Er1 2.236(3) 5_567 ?
O2 C1 1.254(5) . ?
O3 C8 1.235(6) . ?
O3 Er1 2.382(4) 7_567 ?
O4 C8 1.272(7) . ?
O4 Er1 2.378(4) 7_567 ?
O5 C9 1.257(6) . ?
O5 Er1 2.362(3) 6_565 ?
O6 C9 1.258(5) . ?
O6 Er1 2.410(3) 6_565 ?
O7 C10 1.217(6) . ?
O8 C13 1.205(7) . ?
O1W O4W 1.05(2) . ?
O1W O3W 1.25(2) . ?
O2W O3W 1.28(2) . ?
C1 C2 1.503(6) . ?
C2 C3 1.383(6) . ?
C2 C7 1.399(6) . ?
C3 C4 1.410(6) . ?
C4 C5 1.373(6) . ?
C4 C9 1.490(6) . ?
C5 C6 1.390(6) . ?
C6 C7 1.390(7) . ?
C6 C8 1.502(6) . ?
C8 Er1 2.747(5) 7_567 ?
C9 Er1 2.746(4) 6_565 ?
C10 N1 1.281(7) . ?
C11 N1 1.436(11) . ?
C12 N1 1.471(9) . ?
C13 N2 1.319(8) . ?
C14 N2 1.473(13) . ?
C15 N2 1.422(10) . ?
