#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:59:51 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195138 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/75/7227524.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_7227524
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 Ho2 I2 N14 O23'
_chemical_formula_weight         1923.94
_chemical_name_common            1-Ho
_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                81.3200(10)
_cell_angle_beta                 82.7230(10)
_cell_angle_gamma                63.8830(10)
_cell_formula_units_Z            1
_cell_length_a                   11.1399(9)
_cell_length_b                   12.4564(10)
_cell_length_c                   15.1237(12)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.78
_cell_measurement_theta_min      2.38
_cell_volume                     1858.5(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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13536
_diffrn_reflns_theta_full        24.76
_diffrn_reflns_theta_max         24.76
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    3.575
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.464
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0218
_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)+(0.0388P)²+5.5671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                5867
_reflns_number_total             6191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6gc02833k2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7227519--7227529.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7227524
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
Ho1 Ho 0.403528(16) 0.886586(15) 0.036968(11) 0.01982(7) Uani 1 1 d .
I1 I 0.15240(3) 1.57529(3) 0.491036(18) 0.03317(9) Uani 1 1 d .
Cu1 Cu 0.01528(5) 1.49876(5) 0.41106(3) 0.02778(12) Uani 1 1 d .
O3 O 0.4772(3) 1.1340(3) 0.10089(19) 0.0287(6) Uani 1 1 d .
O4 O 0.3360(3) 1.0464(3) 0.12359(19) 0.0301(6) Uani 1 1 d .
O2 O 0.6007(3) 0.8775(3) 0.0714(2) 0.0314(7) Uani 1 1 d .
O1 O 0.7533(3) 0.9496(2) 0.05055(19) 0.0284(6) Uani 1 1 d .
O5 O 0.5438(3) 0.6776(3) 0.0450(2) 0.0405(8) Uani 1 1 d .
O6 O 0.2940(3) 0.8115(3) -0.0416(2) 0.0336(7) Uani 1 1 d .
O7 O 0.3991(3) 0.7997(3) 0.1947(2) 0.0444(8) Uani 1 1 d .
O8 O 0.2124(3) 0.8753(3) 0.1326(2) 0.0449(8) Uani 1 1 d .
N2 N 0.1456(4) 1.3599(3) 0.3377(2) 0.0300(8) Uani 1 1 d .
N1 N 0.9143(3) 0.6284(3) 0.3096(2) 0.0294(8) Uani 1 1 d .
C9 C 0.2990(4) 1.2012(4) 0.2112(3) 0.0249(8) Uani 1 1 d .
N4 N 0.1373(4) 0.8666(4) -0.1414(3) 0.0405(9) Uani 1 1 d .
C8 C 0.3405(4) 1.2811(4) 0.2367(3) 0.0315(10) Uani 1 1 d .
H8A H 0.4222 1.2830 0.2116 0.038 Uiso 1 1 calc R
C12 C 0.3777(4) 1.1198(4) 0.1394(3) 0.0244(8) Uani 1 1 d .
C6 C 0.7072(4) 0.8781(4) 0.0898(3) 0.0243(8) Uani 1 1 d .
N5 N 0.2749(4) 0.8249(4) 0.2020(3) 0.0438(10) Uani 1 1 d .
C3 C 0.7822(4) 0.7891(4) 0.1655(3) 0.0247(8) Uani 1 1 d .
N6 N 0.4478(5) 0.5389(4) 0.6776(3) 0.0473(11) Uani 1 1 d .
C4 C 0.7384(5) 0.7054(4) 0.2088(3) 0.0356(10) Uani 1 1 d .
H4A H 0.6622 0.7016 0.1901 0.043 Uiso 1 1 calc R
C7 C 0.2611(4) 1.3581(4) 0.2995(3) 0.0314(9) Uani 1 1 d .
H7A H 0.2905 1.4127 0.3162 0.038 Uiso 1 1 calc R
C2 C 0.8950(4) 0.7899(4) 0.1952(3) 0.0316(9) Uani 1 1 d .
H2A H 0.9293 0.8449 0.1665 0.038 Uiso 1 1 calc R
N3 N 0.6947(4) 0.5210(4) -0.0275(3) 0.0478(11) Uani 1 1 d .
C10 C 0.1818(5) 1.1993(5) 0.2529(3) 0.0412(12) Uani 1 1 d .
H10A H 0.1519 1.1437 0.2388 0.049 Uiso 1 1 calc R
C15 C 0.5748(5) 0.6074(4) -0.0133(3) 0.0376(11) Uani 1 1 d .
H15A H 0.5068 0.6171 -0.0500 0.045 Uiso 1 1 calc R
C1 C 0.9564(4) 0.7094(4) 0.2671(3) 0.0324(10) Uani 1 1 d .
H1A H 1.0324 0.7117 0.2875 0.039 Uiso 1 1 calc R
C5 C 0.8066(5) 0.6276(4) 0.2793(3) 0.0386(11) Uani 1 1 d .
H5A H 0.7756 0.5703 0.3080 0.046 Uiso 1 1 calc R
C18 C 0.2564(5) 0.8462(4) -0.1192(3) 0.0348(10) Uani 1 1 d .
H18A H 0.3172 0.8586 -0.1649 0.042 Uiso 1 1 calc R
O9 O 0.2206(5) 0.8014(6) 0.2720(3) 0.0927(18) Uani 1 1 d .
N7 N 0.4032(6) 0.1072(4) 0.5914(3) 0.0628(14) Uani 1 1 d D
C11 C 0.1088(5) 1.2789(5) 0.3151(4) 0.0437(12) Uani 1 1 d .
H11A H 0.0287 1.2763 0.3432 0.052 Uiso 1 1 calc R
O10 O 0.4029(6) 0.6068(4) 0.8142(3) 0.0894(17) Uani 1 1 d .
C21 C 0.4389(7) 0.5257(6) 0.7660(4) 0.0596(16) Uani 1 1 d .
H21A H 0.4625 0.4466 0.7949 0.072 Uiso 1 1 calc R
C17 C 0.1023(6) 0.9010(6) -0.2346(4) 0.0608(16) Uani 1 1 d .
H17A H 0.1778 0.9074 -0.2722 0.091 Uiso 1 1 calc R
H17B H 0.0236 0.9788 -0.2393 0.091 Uiso 1 1 calc R
H17C H 0.0821 0.8400 -0.2548 0.091 Uiso 1 1 calc R
C14 C 0.7231(6) 0.4361(5) -0.0932(4) 0.0580(15) Uani 1 1 d .
H14A H 0.6426 0.4589 -0.1251 0.087 Uiso 1 1 calc R
H14B H 0.7496 0.3548 -0.0622 0.087 Uiso 1 1 calc R
H14C H 0.7960 0.4377 -0.1362 0.087 Uiso 1 1 calc R
C20 C 0.4961(6) 0.4351(5) 0.6283(4) 0.0530(14) Uani 1 1 d .
H20A H 0.5138 0.3627 0.6705 0.079 Uiso 1 1 calc R
H20B H 0.5790 0.4269 0.5928 0.079 Uiso 1 1 calc R
H20C H 0.4282 0.4454 0.5884 0.079 Uiso 1 1 calc R
C19 C 0.4155(8) 0.6549(6) 0.6262(5) 0.075(2) Uani 1 1 d .
H19A H 0.3842 0.7174 0.6671 0.113 Uiso 1 1 calc R
H19B H 0.3449 0.6720 0.5864 0.113 Uiso 1 1 calc R
H19C H 0.4956 0.6540 0.5903 0.113 Uiso 1 1 calc R
C16 C 0.0378(6) 0.8524(7) -0.0745(5) 0.0681(19) Uani 1 1 d .
H16A H 0.0743 0.8292 -0.0153 0.102 Uiso 1 1 calc R
H16B H 0.0152 0.7899 -0.0893 0.102 Uiso 1 1 calc R
H16C H -0.0430 0.9287 -0.0738 0.102 Uiso 1 1 calc R
O11 O 0.3792(9) -0.0444(7) 0.6881(6) 0.165(4) Uani 1 1 d D
C13 C 0.8023(7) 0.5035(8) 0.0268(8) 0.119(4) Uani 1 1 d .
H13A H 0.7696 0.5665 0.0672 0.179 Uiso 1 1 calc R
H13B H 0.8776 0.5075 -0.0124 0.179 Uiso 1 1 calc R
H13C H 0.8320 0.4246 0.0622 0.179 Uiso 1 1 calc R
C24 C 0.3569(12) 0.0318(8) 0.6365(7) 0.135(4) Uani 1 1 d DU
H24A H 0.2716 0.0520 0.6162 0.162 Uiso 1 1 calc R
C23 C 0.3414(13) 0.1858(11) 0.5211(7) 0.144(4) Uani 1 1 d U
H23A H 0.2602 0.1781 0.5119 0.216 Uiso 1 1 calc R
H23B H 0.4021 0.1683 0.4669 0.216 Uiso 1 1 calc R
H23C H 0.3173 0.2680 0.5337 0.216 Uiso 1 1 calc R
C22 C 0.5190(14) 0.1137(18) 0.6097(12) 0.227(10) Uani 1 1 d .
H22A H 0.5596 0.0545 0.6604 0.340 Uiso 1 1 calc R
H22B H 0.4963 0.1945 0.6247 0.340 Uiso 1 1 calc R
H22C H 0.5825 0.0966 0.5568 0.340 Uiso 1 1 calc R
O1W O 0.0000 1.0000 -0.5000 0.379(19) Uani 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'
Ho Ho -0.2175 4.6783 '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 Ho1 O3 78.22(10) . 2_675
O2 Ho1 O4 76.76(10) . .
O3 Ho1 O4 126.98(10) 2_675 .
O2 Ho1 O6 147.79(11) . .
O3 Ho1 O6 77.75(11) 2_675 .
O4 Ho1 O6 135.31(11) . .
O2 Ho1 O1 123.89(11) . 2_675
O3 Ho1 O1 79.96(10) 2_675 2_675
O4 Ho1 O1 76.64(10) . 2_675
O6 Ho1 O1 72.05(10) . 2_675
O2 Ho1 O5 77.92(11) . .
O3 Ho1 O5 77.17(11) 2_675 .
O4 Ho1 O5 139.34(11) . .
O6 Ho1 O5 76.08(11) . .
O1 Ho1 O5 143.94(11) 2_675 .
O2 Ho1 O8 131.54(11) . .
O3 Ho1 O8 148.60(11) 2_675 .
O4 Ho1 O8 76.82(11) . .
O6 Ho1 O8 70.97(11) . .
O1 Ho1 O8 87.79(11) 2_675 .
O5 Ho1 O8 97.50(13) . .
O2 Ho1 O7 82.34(11) . .
O3 Ho1 O7 145.90(11) 2_675 .
O4 Ho1 O7 74.03(11) . .
O6 Ho1 O7 106.73(12) . .
O1 Ho1 O7 134.00(10) 2_675 .
O5 Ho1 O7 71.49(12) . .
O8 Ho1 O7 51.53(11) . .
O2 Ho1 N5 107.13(12) . .
O3 Ho1 N5 159.46(11) 2_675 .
O4 Ho1 N5 73.34(11) . .
O6 Ho1 N5 88.99(12) . .
O1 Ho1 N5 111.03(11) 2_675 .
O5 Ho1 N5 84.51(12) . .
O8 Ho1 N5 25.61(12) . .
O7 Ho1 N5 25.93(11) . .
Cu1 I1 Cu1 61.28(2) . 2_586
N2 Cu1 N1 101.11(14) . 1_465
N2 Cu1 I1 109.41(10) . .
N1 Cu1 I1 109.57(10) 1_465 .
N2 Cu1 I1 107.31(10) . 2_586
N1 Cu1 I1 109.26(10) 1_465 2_586
I1 Cu1 I1 118.72(2) . 2_586
N2 Cu1 Cu1 128.16(11) . 2_586
N1 Cu1 Cu1 130.71(11) 1_465 2_586
I1 Cu1 Cu1 59.83(2) . 2_586
I1 Cu1 Cu1 58.89(2) 2_586 2_586
C12 O3 Ho1 139.2(3) . 2_675
C12 O4 Ho1 138.4(3) . .
C6 O2 Ho1 177.2(3) . .
C6 O1 Ho1 113.1(2) . 2_675
C15 O5 Ho1 129.5(3) . .
C18 O6 Ho1 127.5(3) . .
N5 O7 Ho1 95.9(3) . .
N5 O8 Ho1 96.6(3) . .
C7 N2 C11 116.9(4) . .
C7 N2 Cu1 120.9(3) . .
C11 N2 Cu1 121.4(3) . .
C1 N1 C5 116.8(4) . .
C1 N1 Cu1 123.4(3) . 1_645
C5 N1 Cu1 119.6(3) . 1_645
C10 C9 C8 117.8(4) . .
C10 C9 C12 120.9(4) . .
C8 C9 C12 121.3(4) . .
C18 N4 C16 121.1(5) . .
C18 N4 C17 120.8(4) . .
C16 N4 C17 118.0(4) . .
C7 C8 C9 119.0(4) . .
O4 C12 O3 126.8(4) . .
O4 C12 C9 116.9(4) . .
O3 C12 C9 116.3(4) . .
O2 C6 O1 124.1(4) . .
O2 C6 C3 117.7(4) . .
O1 C6 C3 118.2(3) . .
O9 N5 O8 122.4(5) . .
O9 N5 O7 121.6(5) . .
O8 N5 O7 116.0(4) . .
O9 N5 Ho1 178.5(4) . .
O8 N5 Ho1 57.8(2) . .
O7 N5 Ho1 58.2(2) . .
C4 C3 C2 117.9(4) . .
C4 C3 C6 120.5(4) . .
C2 C3 C6 121.5(4) . .
C21 N6 C20 120.3(5) . .
C21 N6 C19 122.2(5) . .
C20 N6 C19 117.4(5) . .
C5 C4 C3 119.3(4) . .
N2 C7 C8 123.6(4) . .
C1 C2 C3 119.0(4) . .
C15 N3 C13 119.5(5) . .
C15 N3 C14 122.1(5) . .
C13 N3 C14 118.2(5) . .
C11 C10 C9 119.5(4) . .
O5 C15 N3 124.6(5) . .
N1 C1 C2 123.5(4) . .
N1 C5 C4 123.6(4) . .
O6 C18 N4 123.8(4) . .
C24 N7 C23 122.6(10) . .
C24 N7 C22 124.3(11) . .
C23 N7 C22 113.1(11) . .
N2 C11 C10 123.1(4) . .
O10 C21 N6 125.6(6) . .
O11 C24 N7 144.1(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ho1 O2 2.272(3) .
Ho1 O3 2.311(3) 2_675
Ho1 O4 2.338(3) .
Ho1 O6 2.341(3) .
Ho1 O1 2.367(3) 2_675
Ho1 O5 2.367(3) .
Ho1 O8 2.463(3) .
Ho1 O7 2.470(3) .
Ho1 N5 2.892(4) .
I1 Cu1 2.6082(6) .
I1 Cu1 2.6338(6) 2_586
Cu1 N2 2.071(3) .
Cu1 N1 2.078(3) 1_465
Cu1 I1 2.6338(6) 2_586
Cu1 Cu1 2.6716(10) 2_586
O3 C12 1.256(5) .
O3 Ho1 2.311(3) 2_675
O4 C12 1.255(5) .
O2 C6 1.255(5) .
O1 C6 1.255(5) .
O1 Ho1 2.367(3) 2_675
O5 C15 1.245(6) .
O6 C18 1.246(6) .
O7 N5 1.271(5) .
O8 N5 1.258(5) .
N2 C7 1.335(6) .
N2 C11 1.344(6) .
N1 C1 1.340(6) .
N1 C5 1.343(6) .
N1 Cu1 2.078(3) 1_645
C9 C10 1.384(6) .
C9 C8 1.385(6) .
C9 C12 1.511(5) .
N4 C18 1.315(6) .
N4 C16 1.456(7) .
N4 C17 1.459(7) .
C8 C7 1.385(6) .
C6 C3 1.510(5) .
N5 O9 1.214(6) .
C3 C4 1.384(6) .
C3 C2 1.392(6) .
N6 C21 1.319(7) .
N6 C20 1.447(7) .
N6 C19 1.448(7) .
C4 C5 1.378(6) .
C2 C1 1.383(6) .
N3 C15 1.311(6) .
N3 C13 1.457(9) .
N3 C14 1.466(7) .
C10 C11 1.381(7) .
N7 C24 1.325(8) .
N7 C23 1.356(11) .
N7 C22 1.391(13) .
O10 C21 1.226(7) .
O11 C24 1.091(8) .
