#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:59:51 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195138 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/75/7227521.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_7227521
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 Gd2 I2 N14 O23'
_chemical_formula_weight         1908.58
_chemical_name_common            1-Gd
_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                92.438(2)
_cell_angle_beta                 96.979(2)
_cell_angle_gamma                116.3080(10)
_cell_formula_units_Z            1
_cell_length_a                   11.1994(12)
_cell_length_b                   12.5884(14)
_cell_length_c                   15.1740(17)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.28
_cell_volume                     1892.3(4)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       13
_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            15372
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.280
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.107
_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     407
_refine_ls_number_reflns         6323
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0261
_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)+(0.0454P)²+4.6446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                5806
_reflns_number_total             6323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6gc02833k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7227519--7227529.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7227521
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
Gd1 Gd 0.793235(19) 0.388903(16) 0.963898(12) 0.02715(8) Uani 1 1 d .
I1 I 1.22489(3) 0.07185(3) 0.50866(2) 0.04439(10) Uani 1 1 d .
Cu1 Cu 1.01313(6) -0.00180(5) 0.58895(4) 0.03779(14) Uani 1 1 d .
O4 O 0.8826(3) 0.5485(3) 0.8743(2) 0.0418(7) Uani 1 1 d .
O2 O 0.9864(3) 0.3823(3) 0.9301(2) 0.0428(8) Uani 1 1 d .
O3 O 1.1088(3) 0.6346(3) 0.8969(2) 0.0403(7) Uani 1 1 d .
O1 O 1.2068(3) 0.4469(3) 0.9484(2) 0.0403(7) Uani 1 1 d .
O5 O 0.7286(4) 0.1787(3) 0.9563(3) 0.0563(9) Uani 1 1 d .
O6 O 0.6079(3) 0.3122(3) 1.0443(2) 0.0461(8) Uani 1 1 d .
N2 N 1.0044(4) 0.8604(3) 0.6627(2) 0.0389(9) Uani 1 1 d .
N1 N 1.0424(4) 0.1273(3) 0.6911(3) 0.0398(9) Uani 1 1 d .
O7 O 0.6986(4) 0.2993(4) 0.8052(3) 0.0614(10) Uani 1 1 d .
O8 O 0.5872(4) 0.3737(4) 0.8675(3) 0.0621(10) Uani 1 1 d .
C9 C 0.9990(4) 0.7025(4) 0.7876(3) 0.0334(9) Uani 1 1 d .
N4 N 0.5062(5) 0.3684(4) 1.1430(3) 0.0553(11) Uani 1 1 d .
C8 C 1.1185(5) 0.7808(4) 0.7622(3) 0.0431(11) Uani 1 1 d .
H8A H 1.2012 0.7821 0.7872 0.052 Uiso 1 1 calc R
C6 C 1.0901(5) 0.3779(4) 0.9103(3) 0.0335(9) Uani 1 1 d .
C12 C 0.9964(5) 0.6211(4) 0.8588(3) 0.0341(9) Uani 1 1 d .
N5 N 0.5998(5) 0.3237(4) 0.7993(3) 0.0613(13) Uani 1 1 d .
C3 C 1.0737(4) 0.2883(4) 0.8351(3) 0.0329(9) Uani 1 1 d .
C2 C 1.1849(5) 0.2872(4) 0.8047(3) 0.0421(11) Uani 1 1 d .
H2A H 1.2736 0.3410 0.8326 0.051 Uiso 1 1 calc R
C10 C 0.8824(5) 0.7017(5) 0.7464(4) 0.0565(15) Uani 1 1 d .
H10A H 0.7976 0.6467 0.7603 0.068 Uiso 1 1 calc R
C4 C 0.9472(5) 0.2065(5) 0.7931(3) 0.0473(12) Uani 1 1 d .
H4A H 0.8687 0.2041 0.8127 0.057 Uiso 1 1 calc R
C1 C 1.1647(5) 0.2061(4) 0.7326(3) 0.0441(11) Uani 1 1 d .
H1A H 1.2416 0.2066 0.7117 0.053 Uiso 1 1 calc R
C7 C 1.1168(5) 0.8573(4) 0.7001(3) 0.0443(11) Uani 1 1 d .
H7A H 1.2000 0.9104 0.6831 0.053 Uiso 1 1 calc R
N6 N 0.5140(5) 0.9615(5) 0.6793(4) 0.0688(14) Uani 1 1 d .
C5 C 0.9355(5) 0.1279(5) 0.7223(4) 0.0505(13) Uani 1 1 d .
H5A H 0.8478 0.0717 0.6944 0.061 Uiso 1 1 calc R
N3 N 0.7195(6) 0.0220(4) 1.0278(4) 0.0695(14) Uani 1 1 d .
C18 C 0.6044(5) 0.3472(5) 1.1213(4) 0.0472(12) Uani 1 1 d .
H18A H 0.6766 0.3593 1.1670 0.057 Uiso 1 1 calc R
C11 C 0.8887(5) 0.7804(5) 0.6854(4) 0.0570(15) Uani 1 1 d .
H11A H 0.8067 0.7782 0.6577 0.068 Uiso 1 1 calc R
C15 C 0.6869(6) 0.1080(4) 1.0124(4) 0.0523(13) Uani 1 1 d .
H15A H 0.6263 0.1168 1.0472 0.063 Uiso 1 1 calc R
O9 O 0.5213(7) 0.2982(7) 0.7300(4) 0.127(2) Uani 1 1 d .
N7 N -0.0071(7) 0.3924(5) 0.5914(4) 0.0855(18) Uani 1 1 d D
O10 O 0.4920(8) 0.8964(6) 0.8148(4) 0.138(3) Uani 1 1 d .
C17 C 0.5043(8) 0.4045(8) 1.2346(5) 0.086(2) Uani 1 1 d .
H17A H 0.5849 0.4109 1.2727 0.128 Uiso 1 1 calc R
H17B H 0.4236 0.3450 1.2549 0.128 Uiso 1 1 calc R
H17C H 0.5032 0.4819 1.2382 0.128 Uiso 1 1 calc R
C20 C 0.5659(7) 1.0623(7) 0.6304(5) 0.0773(19) Uani 1 1 d .
H20A H 0.6186 1.1346 0.6721 0.116 Uiso 1 1 calc R
H20B H 0.4910 1.0691 0.5949 0.116 Uiso 1 1 calc R
H20C H 0.6239 1.0525 0.5906 0.116 Uiso 1 1 calc R
C21 C 0.5358(9) 0.9756(7) 0.7667(5) 0.093(2) Uani 1 1 d .
H21A H 0.5903 1.0543 0.7950 0.111 Uiso 1 1 calc R
C14 C 0.6606(8) -0.0635(6) 1.0922(5) 0.083(2) Uani 1 1 d .
H14A H 0.5996 -0.0425 1.1216 0.125 Uiso 1 1 calc R
H14B H 0.7329 -0.0608 1.1371 0.125 Uiso 1 1 calc R
H14C H 0.6102 -0.1440 1.0608 0.125 Uiso 1 1 calc R
C19 C 0.4348(9) 0.8466(7) 0.6286(6) 0.110(3) Uani 1 1 d .
H19A H 0.4052 0.7849 0.6694 0.165 Uiso 1 1 calc R
H19B H 0.4895 0.8306 0.5892 0.165 Uiso 1 1 calc R
H19C H 0.3557 0.8462 0.5925 0.165 Uiso 1 1 calc R
C16 C 0.3953(8) 0.3548(8) 1.0757(6) 0.097(3) Uani 1 1 d .
H16A H 0.4090 0.3300 1.0172 0.145 Uiso 1 1 calc R
H16B H 0.3916 0.4310 1.0738 0.145 Uiso 1 1 calc R
H16C H 0.3104 0.2942 1.0906 0.145 Uiso 1 1 calc R
O11 O 0.1761(11) 0.5323(11) 0.6691(8) 0.200(4) Uani 1 1 d DU
C24 C 0.0617(14) 0.4758(13) 0.6634(10) 0.230(8) Uani 1 1 d DU
H24A H 0.0151 0.4868 0.7084 0.276 Uiso 1 1 calc R
C13 C 0.8152(12) 0.0062(10) 0.9778(10) 0.165(6) Uani 1 1 d .
H13A H 0.8472 0.0688 0.9378 0.248 Uiso 1 1 calc R
H13B H 0.7706 -0.0720 0.9425 0.248 Uiso 1 1 calc R
H13C H 0.8920 0.0113 1.0196 0.248 Uiso 1 1 calc R
C23 C -0.0155(17) 0.3207(13) 0.5239(10) 0.190(6) Uani 1 1 d U
H23A H 0.0754 0.3353 0.5146 0.284 Uiso 1 1 calc R
H23B H -0.0619 0.3349 0.4701 0.284 Uiso 1 1 calc R
H23C H -0.0662 0.2379 0.5362 0.284 Uiso 1 1 calc R
C22 C -0.1417(19) 0.3683(18) 0.6021(13) 0.248(9) Uani 1 1 d U
H22A H -0.2056 0.3097 0.5533 0.372 Uiso 1 1 calc R
H22B H -0.1508 0.4422 0.6008 0.372 Uiso 1 1 calc R
H22C H -0.1610 0.3365 0.6593 0.372 Uiso 1 1 calc R
O1W O 0.5000 0.5000 1.5000 0.289(10) Uiso 1 2 d S
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'
Gd Gd -0.1653 3.9035 '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 Gd1 O3 77.79(11) . 2_767
O2 Gd1 O6 147.45(12) . .
O3 Gd1 O6 77.05(12) 2_767 .
O2 Gd1 O4 76.76(11) . .
O3 Gd1 O4 128.54(11) 2_767 .
O6 Gd1 O4 135.62(12) . .
O2 Gd1 O5 78.09(13) . .
O3 Gd1 O5 75.97(12) 2_767 .
O6 Gd1 O5 76.03(13) . .
O4 Gd1 O5 138.81(12) . .
O2 Gd1 O1 124.14(11) . 2_767
O3 Gd1 O1 81.39(11) 2_767 2_767
O6 Gd1 O1 71.60(11) . 2_767
O4 Gd1 O1 77.22(11) . 2_767
O5 Gd1 O1 143.82(12) . 2_767
O2 Gd1 O8 132.18(12) . .
O3 Gd1 O8 147.92(12) 2_767 .
O6 Gd1 O8 70.90(13) . .
O4 Gd1 O8 76.95(13) . .
O5 Gd1 O8 97.12(14) . .
O1 Gd1 O8 87.30(12) 2_767 .
O2 Gd1 O7 83.96(13) . .
O3 Gd1 O7 145.23(12) 2_767 .
O6 Gd1 O7 105.85(14) . .
O4 Gd1 O7 73.94(13) . .
O5 Gd1 O7 71.42(13) . .
O1 Gd1 O7 132.97(12) 2_767 .
O8 Gd1 O7 50.54(13) . .
O2 Gd1 N5 108.37(14) . .
O3 Gd1 N5 157.81(13) 2_767 .
O6 Gd1 N5 88.43(14) . .
O4 Gd1 N5 73.42(13) . .
O5 Gd1 N5 84.36(14) . .
O1 Gd1 N5 110.11(13) 2_767 .
O8 Gd1 N5 25.01(13) . .
O7 Gd1 N5 25.54(13) . .
Cu1 I1 Cu1 61.60(2) . 2_756
N2 Cu1 N1 100.45(16) 1_545 .
N2 Cu1 I1 109.48(11) 1_545 .
N1 Cu1 I1 109.57(11) . .
N2 Cu1 I1 107.88(11) 1_545 2_756
N1 Cu1 I1 109.54(11) . 2_756
I1 Cu1 I1 118.40(2) . 2_756
N2 Cu1 Cu1 128.71(11) 1_545 2_756
N1 Cu1 Cu1 130.82(12) . 2_756
I1 Cu1 Cu1 59.57(2) . 2_756
I1 Cu1 Cu1 58.83(2) 2_756 2_756
C12 O4 Gd1 137.5(3) . .
C6 O2 Gd1 178.9(3) . .
C12 O3 Gd1 139.0(3) . 2_767
C6 O1 Gd1 110.5(3) . 2_767
C15 O5 Gd1 130.2(3) . .
C18 O6 Gd1 127.3(3) . .
C7 N2 C11 116.5(4) . .
C7 N2 Cu1 121.0(3) . 1_565
C11 N2 Cu1 121.9(3) . 1_565
C1 N1 C5 117.2(4) . .
C1 N1 Cu1 122.9(3) . .
C5 N1 Cu1 119.7(3) . .
N5 O7 Gd1 95.9(3) . .
N5 O8 Gd1 96.7(3) . .
C10 C9 C8 117.5(4) . .
C10 C9 C12 121.2(4) . .
C8 C9 C12 121.3(4) . .
C18 N4 C17 121.3(5) . .
C18 N4 C16 120.7(5) . .
C17 N4 C16 117.9(5) . .
C9 C8 C7 119.4(4) . .
O1 C6 O2 123.2(4) . .
O1 C6 C3 118.3(4) . .
O2 C6 C3 118.5(4) . .
O4 C12 O3 126.9(4) . .
O4 C12 C9 116.8(4) . .
O3 C12 C9 116.3(4) . .
O9 N5 O8 122.2(6) . .
O9 N5 O7 121.0(6) . .
O8 N5 O7 116.8(4) . .
O9 N5 Gd1 178.7(6) . .
O8 N5 Gd1 58.3(2) . .
O7 N5 Gd1 58.5(2) . .
C4 C3 C2 118.0(4) . .
C4 C3 C6 120.9(4) . .
C2 C3 C6 121.1(4) . .
C3 C2 C1 119.0(4) . .
C11 C10 C9 119.8(5) . .
C3 C4 C5 119.5(4) . .
N1 C1 C2 123.2(4) . .
N2 C7 C8 123.4(4) . .
C21 N6 C20 120.1(6) . .
C21 N6 C19 122.6(7) . .
C20 N6 C19 117.2(6) . .
N1 C5 C4 123.0(5) . .
C15 N3 C13 119.6(6) . .
C15 N3 C14 122.8(6) . .
C13 N3 C14 117.6(6) . .
O6 C18 N4 123.5(5) . .
N2 C11 C10 123.4(5) . .
O5 C15 N3 125.4(6) . .
C23 N7 C24 153.3(13) . .
C23 N7 C22 107.4(12) . .
C24 N7 C22 99.0(12) . .
O10 C21 N6 125.5(8) . .
O11 C24 N7 119.6(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O2 2.319(3) .
Gd1 O3 2.351(3) 2_767
Gd1 O6 2.381(3) .
Gd1 O4 2.381(3) .
Gd1 O5 2.407(3) .
Gd1 O1 2.411(3) 2_767
Gd1 O8 2.503(4) .
Gd1 O7 2.506(4) .
Gd1 N5 2.922(4) .
I1 Cu1 2.6110(7) .
I1 Cu1 2.6312(7) 2_756
Cu1 N2 2.077(4) 1_545
Cu1 N1 2.084(4) .
Cu1 I1 2.6312(7) 2_756
Cu1 Cu1 2.6841(11) 2_756
O4 C12 1.254(5) .
O2 C6 1.258(5) .
O3 C12 1.254(5) .
O3 Gd1 2.351(3) 2_767
O1 C6 1.250(5) .
O1 Gd1 2.411(3) 2_767
O5 C15 1.237(6) .
O6 C18 1.243(6) .
N2 C7 1.334(6) .
N2 C11 1.339(6) .
N2 Cu1 2.077(4) 1_565
N1 C1 1.337(6) .
N1 C5 1.343(6) .
O7 N5 1.267(6) .
O8 N5 1.244(6) .
C9 C10 1.373(7) .
C9 C8 1.378(6) .
C9 C12 1.515(6) .
N4 C18 1.315(7) .
N4 C17 1.449(8) .
N4 C16 1.451(8) .
C8 C7 1.379(7) .
C6 C3 1.504(6) .
N5 O9 1.216(6) .
C3 C4 1.381(6) .
C3 C2 1.386(6) .
C2 C1 1.390(6) .
C10 C11 1.371(7) .
C4 C5 1.382(7) .
N6 C21 1.309(9) .
N6 C20 1.425(9) .
N6 C19 1.439(9) .
N3 C15 1.308(7) .
N3 C13 1.462(11) .
N3 C14 1.471(8) .
N7 C23 1.302(14) .
N7 C24 1.367(10) .
N7 C22 1.432(18) .
O10 C21 1.218(9) .
O11 C24 1.146(9) .
