#------------------------------------------------------------------------------
#$Date: 2021-03-29 10:20:34 +0300 (Mon, 29 Mar 2021) $
#$Revision: 263404 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/13/1561321.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_1561321
loop_
_publ_author_name
'Zhang, Xiu-Mei'
'Li, Peng'
'Gao, Wei'
'Liu, Feng'
'Liu, Jie-Ping'
_publ_section_title
;
 Construction of three lanthanide metal-organic frameworks: Synthesis,
 structure, magnetic properties and highly selective sensing of metal ions
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              6
_journal_page_last               11
_journal_paper_doi               10.1016/j.jssc.2016.09.009
_journal_volume                  244
_journal_year                    2016
_chemical_formula_sum            'C9 H17 N4 O11 Tb'
_chemical_formula_weight         516.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                111.761(4)
_cell_angle_beta                 99.506(4)
_cell_angle_gamma                100.499(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4990(10)
_cell_length_b                   10.9055(13)
_cell_length_c                   11.4538(15)
_cell_measurement_reflns_used    8621
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.86
_cell_volume                     827.14(19)
_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  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8760
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.340
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2875
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0272P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2749
_reflns_number_total             2875
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            mmc4.cif
_cod_data_source_block           2
_cod_database_code               1561321
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.477
_shelx_estimated_absorpt_t_max   0.723
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.66327(2) 0.75690(2) 0.66504(2) 0.01381(7) Uani 1 1 d . . . . .
N1 N 0.1132(4) 0.3734(3) -0.1639(3) 0.0250(6) Uani 1 1 d . . . . .
N2 N 0.0446(4) 0.3356(3) -0.2910(3) 0.0318(7) Uani 1 1 d . . . . .
N3 N 0.0860(5) 0.4414(3) -0.3177(3) 0.0402(8) Uani 1 1 d . . . . .
N4 N 0.1819(5) 0.5523(3) -0.2092(3) 0.0368(8) Uani 1 1 d . . . . .
O1 O 0.4938(4) 0.6471(2) 0.4588(2) 0.0333(6) Uani 1 1 d . . . . .
O2 O 0.4116(4) 0.4396(2) 0.2989(2) 0.0260(5) Uani 1 1 d . . . . .
O3 O 0.4749(3) 1.0560(2) 0.3574(2) 0.0189(5) Uani 1 1 d . . . . .
O4 O 0.2877(3) 1.0088(2) 0.1696(2) 0.0207(5) Uani 1 1 d . . . . .
O5 O 0.4010(4) 0.7555(3) 0.7517(3) 0.0471(8) Uani 1 1 d . . . . .
H5A H 0.359(8) 0.813(6) 0.777(6) 0.071 Uiso 1 1 d . U . . .
H5B H 0.330(8) 0.691(6) 0.772(5) 0.071 Uiso 1 1 d . U . . .
O6 O 0.8719(4) 0.8977(3) 0.6017(3) 0.0361(6) Uani 1 1 d D . . . .
H6C H 0.977(4) 0.894(4) 0.587(5) 0.054 Uiso 1 1 d D U . . .
H6B H 0.840(6) 0.961(4) 0.585(5) 0.054 Uiso 1 1 d D U . . .
O7 O 0.8773(5) 0.6291(3) 0.5737(3) 0.0416(8) Uani 1 1 d . . . . .
H7A H 0.889(8) 0.606(5) 0.504(5) 0.062 Uiso 1 1 d . U . . .
H7B H 0.921(8) 0.595(6) 0.603(6) 0.062 Uiso 1 1 d . U . . .
O8 O 0.9193(4) 0.7930(3) 0.8382(3) 0.0304(6) Uani 1 1 d . . . . .
H8B H 0.913(6) 0.805(5) 0.916(5) 0.046 Uiso 1 1 d . U . . .
H8C H 1.005(7) 0.828(5) 0.846(5) 0.046 Uiso 1 1 d . U . . .
O9 O 0.7055(5) 0.0244(3) 0.0929(3) 0.0532(8) Uani 1 1 d D . . . .
H9B H 0.736(8) -0.040(4) 0.101(6) 0.080 Uiso 1 1 d D U . . .
O10 O 0.0945(4) 0.1617(3) 0.9150(3) 0.0353(6) Uani 1 1 d D . . . .
H10A H 0.114(6) 0.214(4) 0.878(4) 0.053 Uiso 1 1 d D U . . .
H10B H -0.013(4) 0.106(4) 0.878(4) 0.053 Uiso 1 1 d D U . . .
O11 O 0.8287(4) 1.0890(3) 0.5052(3) 0.0281(5) Uani 1 1 d . . . . .
H11A H 0.874(6) 1.168(5) 0.573(5) 0.042 Uiso 1 1 d . U . . .
H11B H 0.743(7) 1.090(5) 0.468(5) 0.042 Uiso 1 1 d . U . . .
C1 C 0.4399(4) 0.5665(3) 0.3410(3) 0.0180(6) Uani 1 1 d . . . . .
C2 C 0.4032(4) 0.6268(3) 0.2438(3) 0.0158(6) Uani 1 1 d . . . . .
C3 C 0.4331(4) 0.7683(3) 0.2867(3) 0.0157(6) Uani 1 1 d . . . . .
H3A H 0.487(5) 0.818(4) 0.368(4) 0.019 Uiso 1 1 d . U . . .
C4 C 0.3814(4) 0.8226(3) 0.1983(3) 0.0154(6) Uani 1 1 d . . . . .
C5 C 0.3854(4) 0.9708(3) 0.2446(3) 0.0148(6) Uani 1 1 d . . . . .
C6 C 0.3082(4) 0.7367(3) 0.0675(3) 0.0177(6) Uani 1 1 d . . . . .
H6A H 0.270(5) 0.771(4) 0.006(4) 0.021 Uiso 1 1 d . U . . .
C7 C 0.2826(4) 0.5955(3) 0.0226(3) 0.0164(6) Uani 1 1 d . . . . .
C8 C 0.3298(4) 0.5416(3) 0.1127(3) 0.0179(6) Uani 1 1 d . . . . .
H8A H 0.308(5) 0.452(4) 0.085(3) 0.021 Uiso 1 1 d . U . . .
C9 C 0.1954(4) 0.5074(3) -0.1149(3) 0.0187(6) 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'
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'
Tb Tb -0.1723 4.1537 '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'
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 Tb1 O2 91.57(8) . 2_666
O1 Tb1 O5 94.28(12) . .
O2 Tb1 O5 70.73(9) 2_666 .
O1 Tb1 O6 89.31(10) . .
O2 Tb1 O6 148.21(9) 2_666 .
O5 Tb1 O6 140.87(9) . .
O1 Tb1 O8 152.11(10) . .
O2 Tb1 O8 76.83(9) 2_666 .
O5 Tb1 O8 105.29(12) . .
O6 Tb1 O8 87.82(10) . .
O1 Tb1 O7 81.00(11) . .
O2 Tb1 O7 76.51(10) 2_666 .
O5 Tb1 O7 146.77(10) . .
O6 Tb1 O7 72.25(10) . .
O8 Tb1 O7 71.71(10) . .
O1 Tb1 O4 132.31(8) . 2_676
O2 Tb1 O4 124.38(7) 2_666 2_676
O5 Tb1 O4 73.33(9) . 2_676
O6 Tb1 O4 75.62(9) . 2_676
O8 Tb1 O4 73.45(8) . 2_676
O7 Tb1 O4 132.82(10) . 2_676
O1 Tb1 O3 80.38(8) . 2_676
O2 Tb1 O3 141.24(8) 2_666 2_676
O5 Tb1 O3 72.16(9) . 2_676
O6 Tb1 O3 70.09(8) . 2_676
O8 Tb1 O3 124.20(8) . 2_676
O7 Tb1 O3 137.88(9) . 2_676
O4 Tb1 O3 51.93(7) 2_676 2_676
O1 Tb1 C5 106.23(9) . 2_676
O2 Tb1 C5 139.68(8) 2_666 2_676
O5 Tb1 C5 72.08(9) . 2_676
O6 Tb1 C5 69.53(8) . 2_676
O8 Tb1 C5 98.69(9) . 2_676
O7 Tb1 C5 140.91(10) . 2_676
O4 Tb1 C5 26.10(8) 2_676 2_676
O3 Tb1 C5 25.90(8) 2_676 2_676
C9 N1 N2 105.7(3) . .
N3 N2 N1 109.1(3) . .
N2 N3 N4 110.1(3) . .
C9 N4 N3 104.7(3) . .
C1 O1 Tb1 161.6(2) . .
C1 O2 Tb1 148.3(2) . 2_666
C5 O3 Tb1 92.77(17) . 2_676
C5 O4 Tb1 95.10(17) . 2_676
Tb1 O5 H5A 127(5) . .
Tb1 O5 H5B 132(3) . .
H5A O5 H5B 100(5) . .
Tb1 O6 H6C 131(3) . .
Tb1 O6 H6B 120(3) . .
H6C O6 H6B 108(3) . .
Tb1 O7 H7A 128(4) . .
Tb1 O7 H7B 122(5) . .
H7A O7 H7B 109(6) . .
Tb1 O8 H8B 126(3) . .
Tb1 O8 H8C 123(5) . .
H8B O8 H8C 104(5) . .
H10A O10 H10B 110(3) . .
H11A O11 H11B 109(5) . .
O2 C1 O1 124.7(3) . .
O2 C1 C2 117.8(3) . .
O1 C1 C2 117.5(3) . .
C8 C2 C3 120.2(3) . .
C8 C2 C1 120.1(3) . .
C3 C2 C1 119.7(3) . .
C4 C3 C2 119.5(3) . .
C4 C3 H3A 124(2) . .
C2 C3 H3A 117(2) . .
C3 C4 C6 119.8(3) . .
C3 C4 C5 120.4(3) . .
C6 C4 C5 119.5(3) . .
O3 C5 O4 119.9(3) . .
O3 C5 C4 121.5(3) . .
O4 C5 C4 118.5(3) . .
O3 C5 Tb1 61.33(15) . 2_676
O4 C5 Tb1 58.80(15) . 2_676
C4 C5 Tb1 171.5(2) . 2_676
C4 C6 C7 121.2(3) . .
C4 C6 H6A 121(2) . .
C7 C6 H6A 118(2) . .
C8 C7 C6 118.5(3) . .
C8 C7 C9 121.7(3) . .
C6 C7 C9 119.6(3) . .
C2 C8 C7 120.7(3) . .
C2 C8 H8A 121(2) . .
C7 C8 H8A 119(2) . .
N1 C9 N4 110.4(3) . .
N1 C9 C7 125.5(3) . .
N4 C9 C7 124.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.233(2) .
Tb1 O2 2.318(2) 2_666
Tb1 O5 2.345(3) .
Tb1 O6 2.379(2) .
Tb1 O8 2.380(3) .
Tb1 O7 2.429(3) .
Tb1 O4 2.468(2) 2_676
Tb1 O3 2.525(2) 2_676
Tb1 C5 2.874(3) 2_676
N1 C9 1.334(4) .
N1 N2 1.336(4) .
N2 N3 1.297(4) .
N3 N4 1.341(4) .
N4 C9 1.338(4) .
O1 C1 1.252(4) .
O2 C1 1.248(4) .
O2 Tb1 2.318(2) 2_666
O3 C5 1.257(4) .
O3 Tb1 2.525(2) 2_676
O4 C5 1.270(4) .
O4 Tb1 2.468(2) 2_676
O5 H5A 0.74(6) .
O5 H5B 0.92(6) .
O6 H6C 0.837(19) .
O6 H6B 0.843(19) .
O7 H7A 0.77(6) .
O7 H7B 0.67(6) .
O8 H8B 0.87(5) .
O8 H8C 0.66(5) .
O9 H9B 0.80(2) .
O10 H10A 0.838(19) .
O10 H10B 0.848(19) .
O11 H11A 0.88(5) .
O11 H11B 0.71(5) .
C1 C2 1.502(4) .
C2 C8 1.388(4) .
C2 C3 1.396(4) .
C3 C4 1.387(4) .
C3 H3A 0.87(4) .
C4 C6 1.388(4) .
C4 C5 1.496(4) .
C5 Tb1 2.874(3) 2_676
C6 C7 1.394(4) .
C6 H6A 0.95(4) .
C7 C8 1.393(4) .
C7 C9 1.463(4) .
C8 H8A 0.89(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O9 0.74(6) 2.05(6) 2.751(4) 160(6) 2_666
O5 H5B N4 0.92(6) 1.81(6) 2.732(4) 173(5) 1_556
O6 H6B O11 0.843(19) 1.94(3) 2.742(4) 159(4) .
O6 H6C O11 0.837(19) 1.96(3) 2.735(3) 155(4) 2_776
O7 H7A N3 0.77(6) 2.05(6) 2.818(4) 175(6) 2_665
O7 H7B N3 0.67(6) 2.59(6) 3.256(4) 172(6) 1_656
O8 H8B O10 0.87(5) 1.84(5) 2.707(4) 177(4) 2_667
O8 H8C O9 0.66(5) 2.28(5) 2.926(5) 170(6) 2_766
O9 H9B O10 0.80(2) 1.98(3) 2.720(4) 152(6) 2_656
O10 H10B O4 0.848(19) 2.07(2) 2.901(3) 167(5) 2_566
O10 H10A N1 0.838(19) 1.96(3) 2.763(4) 159(5) 1_556
O11 H11A N2 0.88(5) 1.94(5) 2.795(4) 163(4) 1_666
O11 H11B O3 0.71(5) 2.08(5) 2.784(3) 170(5) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C9 N1 N2 N3 0.9(4) . . . .
N1 N2 N3 N4 -0.4(5) . . . .
N2 N3 N4 C9 -0.3(5) . . . .
Tb1 O2 C1 O1 25.6(6) 2_666 . . .
Tb1 O2 C1 C2 -153.1(3) 2_666 . . .
Tb1 O1 C1 O2 55.2(9) . . . .
Tb1 O1 C1 C2 -126.1(6) . . . .
O2 C1 C2 C8 3.7(5) . . . .
O1 C1 C2 C8 -175.2(3) . . . .
O2 C1 C2 C3 180.0(3) . . . .
O1 C1 C2 C3 1.1(5) . . . .
C8 C2 C3 C4 2.7(5) . . . .
C1 C2 C3 C4 -173.5(3) . . . .
C2 C3 C4 C6 -2.7(5) . . . .
C2 C3 C4 C5 170.9(3) . . . .
Tb1 O3 C5 O4 5.5(3) 2_676 . . .
Tb1 O3 C5 C4 -170.7(2) 2_676 . . .
Tb1 O4 C5 O3 -5.6(3) 2_676 . . .
Tb1 O4 C5 C4 170.7(2) 2_676 . . .
C3 C4 C5 O3 17.1(4) . . . .
C6 C4 C5 O3 -169.3(3) . . . .
C3 C4 C5 O4 -159.2(3) . . . .
C6 C4 C5 O4 14.5(4) . . . .
C3 C4 C6 C7 0.9(5) . . . .
C5 C4 C6 C7 -172.8(3) . . . .
C4 C6 C7 C8 0.9(5) . . . .
C4 C6 C7 C9 176.7(3) . . . .
C3 C2 C8 C7 -0.9(5) . . . .
C1 C2 C8 C7 175.4(3) . . . .
C6 C7 C8 C2 -0.9(5) . . . .
C9 C7 C8 C2 -176.6(3) . . . .
N2 N1 C9 N4 -1.1(4) . . . .
N2 N1 C9 C7 176.8(3) . . . .
N3 N4 C9 N1 0.9(4) . . . .
N3 N4 C9 C7 -177.1(3) . . . .
C8 C7 C9 N1 16.5(5) . . . .
C6 C7 C9 N1 -159.1(3) . . . .
C8 C7 C9 N4 -165.9(3) . . . .
C6 C7 C9 N4 18.5(5) . . . .
