#------------------------------------------------------------------------------
#$Date: 2017-04-05 11:59:51 +0200 (Wed 05 de Apr de 2017) $
#$Revision: 195138 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/75/7227522.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_7227522
loop_
_publ_author_name
'Hu, Yue-Qiao'
'Zhang, Tao'
'Li, Mu-Qing'
'Wang, Yanyan'
'Zheng, Zhiping'
'Zheng, Yan-Zhen'
_publ_section_title
;
 Copper(i)/(ii)-redox triggered efficient and green rare-earth separation
 using a heterometallic metal--organic framework
;
_journal_issue                   5
_journal_name_full               'Green Chem.'
_journal_page_first              1250
_journal_paper_doi               10.1039/C6GC02833K
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C48 H72 Cu2 I2 N14 O23 Tb2'
_chemical_formula_weight         1911.92
_chemical_name_common            1-Tb
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.2910(10)
_cell_angle_beta                 97.1310(10)
_cell_angle_gamma                116.3470(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2008(10)
_cell_length_b                   12.5798(11)
_cell_length_c                   15.1576(14)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.38
_cell_volume                     1888.2(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15120
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    3.296
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0249
_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)+(0.0431P)²+5.5142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                5907
_reflns_number_total             6304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6gc02833k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7227519--7227529.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7227522
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tb1 Tb 0.707222(18) 0.111576(16) 0.036176(12) 0.02627(8) Uani 1 1 d .
I1 I 0.27494(3) 0.42770(3) 0.49105(2) 0.04336(10) Uani 1 1 d .
Cu1 Cu 0.48669(6) 0.50192(5) 0.41092(3) 0.03671(14) Uani 1 1 d .
O4 O 0.6174(3) -0.0477(3) 0.1248(2) 0.0397(7) Uani 1 1 d .
O3 O 0.3912(3) -0.1334(3) 0.1027(2) 0.0382(7) Uani 1 1 d .
O2 O 0.5171(3) 0.1202(3) 0.0706(2) 0.0421(8) Uani 1 1 d .
O1 O 0.2963(3) 0.0531(3) 0.0513(2) 0.0388(7) Uani 1 1 d .
O5 O 0.7724(4) 0.3212(3) 0.0431(3) 0.0548(9) Uani 1 1 d .
O6 O 0.8911(3) 0.1866(3) -0.0435(2) 0.0452(8) Uani 1 1 d .
N2 N 0.4955(4) -0.3598(4) 0.3371(3) 0.0387(9) Uani 1 1 d .
N1 N 0.4577(4) 0.3730(3) 0.3084(3) 0.0395(9) Uani 1 1 d .
O7 O 0.8020(4) 0.2009(4) 0.1939(3) 0.0603(10) Uani 1 1 d .
O8 O 0.9114(4) 0.1244(4) 0.1323(3) 0.0609(10) Uani 1 1 d .
C9 C 0.5014(4) -0.2016(4) 0.2118(3) 0.0323(9) Uani 1 1 d .
C8 C 0.3818(5) -0.2797(4) 0.2377(3) 0.0414(11) Uani 1 1 d .
H8A H 0.2991 -0.2805 0.2129 0.050 Uiso 1 1 calc R
N4 N 0.9935(4) 0.1315(4) -0.1420(3) 0.0525(11) Uani 1 1 d .
C4 C 0.4126(5) 0.1227(4) 0.0897(3) 0.0324(9) Uani 1 1 d .
C12 C 0.5043(4) -0.1196(4) 0.1409(3) 0.0321(9) Uani 1 1 d .
C3 C 0.4281(4) 0.2125(4) 0.1648(3) 0.0324(9) Uani 1 1 d .
N5 N 0.8993(5) 0.1758(5) 0.2006(3) 0.0594(12) Uani 1 1 d .
C2 C 0.3163(5) 0.2127(4) 0.1952(3) 0.0409(11) Uani 1 1 d .
H2A H 0.2277 0.1583 0.1672 0.049 Uiso 1 1 calc R
C10 C 0.6179(5) -0.2013(5) 0.2529(4) 0.0542(14) Uani 1 1 d .
H10A H 0.7027 -0.1464 0.2390 0.065 Uiso 1 1 calc R
C5 C 0.5541(5) 0.2949(5) 0.2069(3) 0.0467(12) Uani 1 1 d .
H5A H 0.6330 0.2981 0.1874 0.056 Uiso 1 1 calc R
C1 C 0.3359(5) 0.2932(5) 0.2670(3) 0.0431(11) Uani 1 1 d .
H1A H 0.2587 0.2917 0.2879 0.052 Uiso 1 1 calc R
N6 N 0.0142(5) 0.4612(5) 0.6795(4) 0.0656(13) Uani 1 1 d .
C7 C 0.3833(5) -0.3562(4) 0.2997(3) 0.0433(11) Uani 1 1 d .
H7A H 0.3001 -0.4093 0.3168 0.052 Uiso 1 1 calc R
C6 C 0.5646(5) 0.3729(5) 0.2778(4) 0.0490(13) Uani 1 1 d .
H6A H 0.6521 0.4293 0.3061 0.059 Uiso 1 1 calc R
N3 N 0.7813(6) 0.4782(4) -0.0291(4) 0.0664(14) Uani 1 1 d .
C18 C 0.8955(5) 0.1516(5) -0.1206(3) 0.0447(11) Uani 1 1 d .
H18A H 0.8231 0.1388 -0.1666 0.054 Uiso 1 1 calc R
C15 C 0.8143(6) 0.3921(4) -0.0133(4) 0.0513(13) Uani 1 1 d .
H15A H 0.8751 0.3833 -0.0480 0.062 Uiso 1 1 calc R
C11 C 0.6117(5) -0.2807(5) 0.3143(4) 0.0566(15) Uani 1 1 d .
H11A H 0.6935 -0.2792 0.3417 0.068 Uiso 1 1 calc R
O9 O 0.9788(7) 0.2011(7) 0.2697(4) 0.125(3) Uani 1 1 d .
N7 N 0.4896(7) 0.8921(6) 0.5925(4) 0.0825(17) Uani 1 1 d D
O10 O -0.0092(8) 0.3955(6) 0.8154(4) 0.132(3) Uani 1 1 d .
C17 C 0.9957(8) 0.0954(8) -0.2339(5) 0.083(2) Uani 1 1 d .
H17A H 0.9150 0.0887 -0.2723 0.124 Uiso 1 1 calc R
H17B H 0.9971 0.0180 -0.2372 0.124 Uiso 1 1 calc R
H17C H 1.0765 0.1551 -0.2541 0.124 Uiso 1 1 calc R
C21 C 0.0368(9) 0.4752(7) 0.7668(5) 0.091(2) Uani 1 1 d .
H21A H 0.0936 0.5536 0.7951 0.109 Uiso 1 1 calc R
C20 C 0.0662(8) 0.5624(7) 0.6303(5) 0.0756(19) Uani 1 1 d .
H20A H 0.1182 0.6348 0.6720 0.113 Uiso 1 1 calc R
H20B H -0.0087 0.5687 0.5942 0.113 Uiso 1 1 calc R
H20C H 0.1249 0.5530 0.5910 0.113 Uiso 1 1 calc R
C14 C 0.8396(8) 0.5628(6) -0.0937(5) 0.085(2) Uani 1 1 d .
H14A H 0.8998 0.5412 -0.1234 0.127 Uiso 1 1 calc R
H14B H 0.8909 0.6435 -0.0626 0.127 Uiso 1 1 calc R
H14C H 0.7670 0.5604 -0.1385 0.127 Uiso 1 1 calc R
C16 C 1.1051(8) 0.1462(8) -0.0750(6) 0.094(3) Uani 1 1 d .
H16A H 1.0915 0.1708 -0.0164 0.141 Uiso 1 1 calc R
H16B H 1.1895 0.2074 -0.0901 0.141 Uiso 1 1 calc R
H16C H 1.1099 0.0704 -0.0730 0.141 Uiso 1 1 calc R
C19 C -0.0655(9) 0.3462(8) 0.6282(6) 0.107(3) Uani 1 1 d .
H19A H -0.0955 0.2842 0.6690 0.160 Uiso 1 1 calc R
H19B H -0.0107 0.3302 0.5890 0.160 Uiso 1 1 calc R
H19C H -0.1443 0.3461 0.5919 0.160 Uiso 1 1 calc R
O11 O 0.6619(12) 1.0406(10) 0.6859(7) 0.186(4) Uani 1 1 d DU
C24 C 0.6173(13) 0.9645(12) 0.6308(10) 0.200(7) Uani 1 1 d DU
H24A H 0.6827 0.9484 0.6068 0.240 Uiso 1 1 calc R
C13 C 0.6863(13) 0.4926(11) 0.0218(10) 0.167(6) Uani 1 1 d .
H13A H 0.6551 0.4293 0.0614 0.251 Uiso 1 1 calc R
H13B H 0.6090 0.4877 -0.0195 0.251 Uiso 1 1 calc R
H13C H 0.7310 0.5705 0.0576 0.251 Uiso 1 1 calc R
C23 C 0.4744(17) 0.8167(13) 0.5229(9) 0.185(6) Uani 1 1 d U
H23A H 0.5632 0.8276 0.5116 0.277 Uiso 1 1 calc R
H23B H 0.4275 0.8326 0.4699 0.277 Uiso 1 1 calc R
H23C H 0.4212 0.7346 0.5358 0.277 Uiso 1 1 calc R
C22 C 0.367(2) 0.8781(19) 0.6109(14) 0.248(9) Uani 1 1 d U
H22A H 0.2950 0.8164 0.5674 0.371 Uiso 1 1 calc R
H22B H 0.3624 0.9537 0.6071 0.371 Uiso 1 1 calc R
H22C H 0.3567 0.8542 0.6713 0.371 Uiso 1 1 calc R
O1W O 1.0000 0.0000 -0.5000 0.287(10) Uani 1 2 d SU
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
O2 Tb1 O3 78.09(11) . 2_655
O2 Tb1 O6 147.60(12) . .
O3 Tb1 O6 77.34(11) 2_655 .
O2 Tb1 O4 76.86(11) . .
O3 Tb1 O4 127.82(11) 2_655 .
O6 Tb1 O4 135.39(12) . .
O2 Tb1 O1 124.05(11) . 2_655
O3 Tb1 O1 80.70(11) 2_655 2_655
O6 Tb1 O1 71.89(11) . 2_655
O4 Tb1 O1 76.79(11) . 2_655
O2 Tb1 O5 77.78(13) . .
O3 Tb1 O5 76.32(12) 2_655 .
O6 Tb1 O5 76.14(13) . .
O4 Tb1 O5 139.21(12) . .
O1 Tb1 O5 143.91(12) 2_655 .
O2 Tb1 O7 83.49(13) . .
O3 Tb1 O7 145.58(12) 2_655 .
O6 Tb1 O7 105.81(13) . .
O4 Tb1 O7 74.34(13) . .
O1 Tb1 O7 133.38(12) 2_655 .
O5 Tb1 O7 71.48(13) . .
O2 Tb1 O8 131.84(12) . .
O3 Tb1 O8 148.21(12) 2_655 .
O6 Tb1 O8 70.94(13) . .
O4 Tb1 O8 76.80(13) . .
O1 Tb1 O8 87.47(12) 2_655 .
O5 Tb1 O8 97.65(15) . .
O7 Tb1 O8 50.78(13) . .
O2 Tb1 N5 107.77(14) . .
O3 Tb1 N5 158.40(13) 2_655 .
O6 Tb1 N5 88.55(14) . .
O4 Tb1 N5 73.57(13) . .
O1 Tb1 N5 110.61(13) 2_655 .
O5 Tb1 N5 84.53(14) . .
O7 Tb1 N5 25.45(13) . .
O8 Tb1 N5 25.34(13) . .
Cu1 I1 Cu1 61.60(2) . 2_666
N2 Cu1 N1 100.42(16) 1_565 .
N2 Cu1 I1 109.57(11) 1_565 .
N1 Cu1 I1 109.66(11) . .
N2 Cu1 I1 107.77(11) 1_565 2_666
N1 Cu1 I1 109.51(11) . 2_666
I1 Cu1 I1 118.40(2) . 2_666
N2 Cu1 Cu1 128.67(12) 1_565 2_666
N1 Cu1 Cu1 130.89(12) . 2_666
I1 Cu1 Cu1 59.62(2) . 2_666
I1 Cu1 Cu1 58.78(2) 2_666 2_666
C12 O4 Tb1 138.0(3) . .
C12 O3 Tb1 139.0(3) . 2_655
C4 O2 Tb1 178.8(3) . .
C4 O1 Tb1 111.8(3) . 2_655
C15 O5 Tb1 130.3(3) . .
C18 O6 Tb1 127.9(3) . .
C7 N2 C11 116.8(4) . .
C7 N2 Cu1 121.1(3) . 1_545
C11 N2 Cu1 121.4(3) . 1_545
C1 N1 C6 117.0(4) . .
C1 N1 Cu1 123.2(3) . .
C6 N1 Cu1 119.6(3) . .
N5 O7 Tb1 96.2(3) . .
N5 O8 Tb1 96.3(3) . .
C10 C9 C8 117.4(4) . .
C10 C9 C12 121.2(4) . .
C8 C9 C12 121.4(4) . .
C7 C8 C9 119.4(4) . .
C18 N4 C16 120.9(5) . .
C18 N4 C17 121.4(5) . .
C16 N4 C17 117.6(5) . .
O1 C4 O2 123.5(4) . .
O1 C4 C3 118.4(4) . .
O2 C4 C3 118.1(4) . .
O4 C12 O3 126.8(4) . .
O4 C12 C9 117.2(4) . .
O3 C12 C9 116.0(4) . .
C5 C3 C2 117.9(4) . .
C5 C3 C4 120.9(4) . .
C2 C3 C4 121.2(4) . .
O9 N5 O8 121.5(5) . .
O9 N5 O7 121.8(6) . .
O8 N5 O7 116.7(4) . .
O9 N5 Tb1 179.1(6) . .
O8 N5 Tb1 58.4(2) . .
O7 N5 Tb1 58.4(2) . .
C1 C2 C3 119.0(4) . .
C9 C10 C11 120.0(5) . .
C3 C5 C6 119.3(4) . .
N1 C1 C2 123.4(4) . .
C21 N6 C20 120.1(6) . .
C21 N6 C19 122.9(7) . .
C20 N6 C19 116.9(6) . .
N2 C7 C8 123.4(4) . .
N1 C6 C5 123.3(4) . .
C15 N3 C13 118.7(6) . .
C15 N3 C14 122.5(6) . .
C13 N3 C14 118.7(6) . .
O6 C18 N4 123.9(5) . .
O5 C15 N3 125.2(6) . .
N2 C11 C10 122.9(5) . .
C23 N7 C24 116.2(12) . .
C23 N7 C22 111.0(12) . .
C24 N7 C22 132.8(13) . .
O10 C21 N6 125.4(8) . .
O11 C24 N7 132.6(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O2 2.301(3) .
Tb1 O3 2.337(3) 2_655
Tb1 O6 2.361(3) .
Tb1 O4 2.365(3) .
Tb1 O1 2.398(3) 2_655
Tb1 O5 2.398(3) .
Tb1 O7 2.491(4) .
Tb1 O8 2.491(4) .
Tb1 N5 2.908(4) .
I1 Cu1 2.6101(7) .
I1 Cu1 2.6329(7) 2_666
Cu1 N2 2.078(4) 1_565
Cu1 N1 2.087(4) .
Cu1 I1 2.6329(7) 2_666
Cu1 Cu1 2.6846(11) 2_666
O4 C12 1.249(5) .
O3 C12 1.259(5) .
O3 Tb1 2.337(3) 2_655
O2 C4 1.255(5) .
O1 C4 1.250(5) .
O1 Tb1 2.398(3) 2_655
O5 C15 1.239(6) .
O6 C18 1.247(6) .
N2 C7 1.334(6) .
N2 C11 1.339(6) .
N2 Cu1 2.078(4) 1_545
N1 C1 1.337(6) .
N1 C6 1.337(6) .
O7 N5 1.257(6) .
O8 N5 1.252(6) .
C9 C10 1.372(7) .
C9 C8 1.382(6) .
C9 C12 1.512(6) .
C8 C7 1.376(6) .
N4 C18 1.305(6) .
N4 C16 1.447(8) .
N4 C17 1.454(8) .
C4 C3 1.507(6) .
C3 C5 1.378(7) .
C3 C2 1.389(6) .
N5 O9 1.217(6) .
C2 C1 1.383(7) .
C10 C11 1.378(7) .
C5 C6 1.383(7) .
N6 C21 1.306(9) .
N6 C20 1.429(9) .
N6 C19 1.444(9) .
N3 C15 1.313(7) .
N3 C13 1.457(11) .
N3 C14 1.464(8) .
N7 C23 1.332(14) .
N7 C24 1.344(9) .
N7 C22 1.369(18) .
O10 C21 1.228(9) .
O11 C24 1.127(9) .
