#------------------------------------------------------------------------------
#$Date: 2019-11-23 14:58:47 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 233917 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/61/7236102.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_7236102
loop_
_publ_author_name
'Han, Yun-Hu'
'Tian, Chong-Bin'
'Lin, Ping'
'Du, Shao-Wu'
_publ_section_title
;
 An unprecedented anionic Ln-MOF with a cage-within-cage motif:
 spontaneous reduction and immobilization of ion-exchanged Pd(ii) to
 Pd-NPs in the framework
;
_journal_issue                   48
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              24525
_journal_paper_doi               10.1039/C5TA04937G
_journal_volume                  3
_journal_year                    2015
_chemical_formula_sum            'C240 H288 N36 O90 Tb6'
_chemical_formula_weight         6070.58
_space_group_IT_number           204
_space_group_name_Hall           '-I 2 2 3'
_space_group_name_H-M_alt        'I m -3'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I m -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-02 deposited with the CCDC.
2015-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   26.7264(13)
_cell_length_b                   26.7264(13)
_cell_length_c                   26.7264(13)
_cell_measurement_reflns_used    24310
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.1536
_cell_volume                     19090.7(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            80259
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.64
_diffrn_standards_number         3873
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6180
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_platon_squeeze_details
;
;
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00136(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3867
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0628
_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)+(0.0400P)²+98.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                3259
_reflns_number_total             3867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ta04937g2.cif
_cod_data_source_block           x
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'CUBIC' was changed to
'cubic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      Im-3
_cod_database_code               7236102
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+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
Tb1 Tb 0.0000 0.5000 0.372971(15) 0.0411(2) Uani 1 4 d S . .
O1 O 0.0573(5) 0.4281(5) 0.3938(3) 0.065(3) Uani 0.502(9) 1 d PDU A 1
O2 O 0.0369(3) 0.4318(3) 0.3202(3) 0.067(2) Uani 0.502(9) 1 d PDU A 1
O1B O 0.0679(6) 0.4453(4) 0.3940(2) 0.068(3) Uani 0.498(9) 1 d PDU A 2
O2B O 0.0668(3) 0.4674(3) 0.3205(3) 0.063(2) Uani 0.498(9) 1 d PDU . 2
N1 N 0.2734(2) 0.3279(2) 0.2588(2) 0.0896(19) Uani 1 1 d . . .
C1 C 0.0741(2) 0.4303(2) 0.3505(2) 0.0749(17) Uani 1 1 d D . .
C2 C 0.1190(2) 0.3984(2) 0.3383(2) 0.0748(17) Uani 1 1 d . A .
C3 C 0.1378(3) 0.3994(3) 0.2905(3) 0.121(3) Uani 1 1 d . . .
H3A H 0.1218 0.4182 0.2660 0.145 Uiso 1 1 calc R A .
C4 C 0.1802(3) 0.3725(3) 0.2785(3) 0.118(3) Uani 1 1 d . A .
H4A H 0.1932 0.3745 0.2463 0.141 Uiso 1 1 calc R . .
C5 C 0.2032(2) 0.3431(3) 0.3128(2) 0.085(2) Uani 1 1 d . . .
C6 C 0.1839(3) 0.3404(3) 0.3611(2) 0.090(2) Uani 1 1 d . A .
H6A H 0.1987 0.3199 0.3850 0.108 Uiso 1 1 calc R . .
C7 C 0.1420(2) 0.3689(3) 0.3728(2) 0.081(2) Uani 1 1 d . . .
H7A H 0.1292 0.3677 0.4052 0.097 Uiso 1 1 calc R A .
C8 C 0.2471(2) 0.3131(3) 0.2989(2) 0.086(2) Uani 1 1 d . A .
O3 O 0.0000 0.5000 0.4577(2) 0.073(2) Uani 1 4 d SD . .
C9 C 0.0175(7) 0.5000 0.5000 0.066(6) Uani 0.50 4 d SPD . .
N2 N 0.0000 0.3275(5) 0.5000 0.098(4) Uani 1 4 d S . .
C10 C 0.0392(14) 0.3677(9) 0.5000 0.160(13) Uani 0.50 2 d SP . .
C11 C 0.0000 0.2997(11) 0.4538(11) 0.148(12) Uani 0.50 2 d SP . .
O1W O 0.3726(2) 0.3726(2) 0.3726(2) 0.046(2) Uiso 0.50 3 d SP . .
O7W O 0.2549(16) 0.5000 0.3669(15) 0.145(13) Uiso 0.25 2 d SP . .
N3 N 0.1612(11) 0.5000 0.5000 0.147(14) Uani 0.50 4 d SP . .
C12 C 0.1285(14) 0.4507(16) 0.5000 0.087(12) Uani 0.25 2 d SP . .
C13 C 0.186(2) 0.5000 0.449(2) 0.14(2) Uani 0.25 2 d SP . .
O4 O 0.1625(10) 0.3197(11) 0.5000 0.185(9) Uiso 0.50 2 d SPD . .
N5 N 0.1916(10) 0.2394(10) 0.5000 0.136(8) Uiso 0.50 2 d SPD . .
C14 C 0.1541(12) 0.2731(10) 0.5000 0.191(16) Uiso 0.50 2 d SPD . .
C15 C 0.1912(15) 0.1862(10) 0.5000 0.188(15) Uiso 0.50 2 d SPD . .
C16 C 0.2393(13) 0.2629(16) 0.5000 0.222(19) Uiso 0.50 2 d SPD . .
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'
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
O3 Tb1 O1B 76.43(16) . 2_565
O3 Tb1 O1B 76.43(16) . 27_565
O1B Tb1 O1B 98.4(7) 2_565 27_565
O3 Tb1 O1B 76.43(16) . 28
O1B Tb1 O1B 75.1(7) 2_565 28
O1B Tb1 O1B 152.9(3) 27_565 28
O3 Tb1 O1B 76.43(16) . .
O1B Tb1 O1B 152.9(3) 2_565 .
O1B Tb1 O1B 75.1(7) 27_565 .
O1B Tb1 O1B 98.4(7) 28 .
O3 Tb1 O2B 125.21(16) . 2_565
O1B Tb1 O2B 50.3(2) 2_565 2_565
O1B Tb1 O2B 118.2(4) 27_565 2_565
O1B Tb1 O2B 78.3(4) 28 2_565
O1B Tb1 O2B 155.4(3) . 2_565
O3 Tb1 O2B 125.21(16) . 27_565
O1B Tb1 O2B 118.2(4) 2_565 27_565
O1B Tb1 O2B 50.3(2) 27_565 27_565
O1B Tb1 O2B 155.4(3) 28 27_565
O1B Tb1 O2B 78.3(4) . 27_565
O2B Tb1 O2B 94.5(4) 2_565 27_565
O3 Tb1 O2B 125.21(16) . 28
O1B Tb1 O2B 78.3(4) 2_565 28
O1B Tb1 O2B 155.4(3) 27_565 28
O1B Tb1 O2B 50.3(2) 28 28
O1B Tb1 O2B 118.2(4) . 28
O2B Tb1 O2B 41.9(4) 2_565 28
O2B Tb1 O2B 109.6(3) 27_565 28
O3 Tb1 O2B 125.21(16) . .
O1B Tb1 O2B 155.4(3) 2_565 .
O1B Tb1 O2B 78.3(4) 27_565 .
O1B Tb1 O2B 118.2(4) 28 .
O1B Tb1 O2B 50.3(2) . .
O2B Tb1 O2B 109.6(3) 2_565 .
O2B Tb1 O2B 41.9(4) 27_565 .
O2B Tb1 O2B 94.5(4) 28 .
O3 Tb1 O2 124.24(17) . 2_565
O1B Tb1 O2 52.5(3) 2_565 2_565
O1B Tb1 O2 89.2(4) 27_565 2_565
O1B Tb1 O2 106.1(4) 28 2_565
O1B Tb1 O2 150.8(3) . 2_565
O2B Tb1 O2 29.1(2) 2_565 2_565
O2B Tb1 O2 72.8(3) 27_565 2_565
O2B Tb1 O2 69.3(3) 28 2_565
O2B Tb1 O2 103.0(2) . 2_565
O3 Tb1 O2 124.24(18) . 27_565
O1B Tb1 O2 89.2(4) 2_565 27_565
O1B Tb1 O2 52.5(3) 27_565 27_565
O1B Tb1 O2 150.8(3) 28 27_565
O1B Tb1 O2 106.1(4) . 27_565
O2B Tb1 O2 72.8(3) 2_565 27_565
O2B Tb1 O2 29.1(2) 27_565 27_565
O2B Tb1 O2 103.0(2) 28 27_565
O2B Tb1 O2 69.3(3) . 27_565
O2 Tb1 O2 46.3(3) 2_565 27_565
O3 Tb1 O2 124.24(18) . 28
O1B Tb1 O2 106.1(4) 2_565 28
O1B Tb1 O2 150.8(3) 27_565 28
O1B Tb1 O2 52.5(3) 28 28
O1B Tb1 O2 89.2(4) . 28
O2B Tb1 O2 69.3(3) 2_565 28
O2B Tb1 O2 103.0(2) 27_565 28
O2B Tb1 O2 29.1(2) 28 28
O2B Tb1 O2 72.8(3) . 28
O2 Tb1 O2 93.3(4) 2_565 28
O2 Tb1 O2 111.5(3) 27_565 28
C1 O1 Tb1 88.7(7) . .
C1 O2 Tb1 88.4(4) . .
C1 O1B Tb1 94.4(7) . .
C1 O2B O2B 140.2(5) . 27_565
C1 O2B Tb1 91.5(4) . .
O2B O2B Tb1 69.03(18) 27_565 .
C8 N1 C8 115.2(6) . 9
O1B C1 O1 25.2(8) . .
O1B C1 O2 118.6(9) . .
O1 C1 O2 108.1(7) . .
O1B C1 O2B 108.4(7) . .
O1 C1 O2B 124.2(9) . .
O2 C1 O2B 57.8(5) . .
O1B C1 C2 119.4(8) . .
O1 C1 C2 117.5(8) . .
O2 C1 C2 119.8(6) . .
O2B C1 C2 114.8(6) . .
O1B C1 Tb1 59.2(6) . .
O1 C1 Tb1 64.8(7) . .
O2 C1 Tb1 64.2(4) . .
O2B C1 Tb1 60.9(4) . .
C2 C1 Tb1 172.3(5) . .
C7 C2 C3 118.5(5) . .
C7 C2 C1 122.7(5) . .
C3 C2 C1 118.8(5) . .
C2 C3 C4 120.4(6) . .
C2 C3 H3A 119.8 . .
C4 C3 H3A 119.8 . .
C5 C4 C3 121.2(6) . .
C5 C4 H4A 119.4 . .
C3 C4 H4A 119.4 . .
C4 C5 C6 119.3(5) . .
C4 C5 C8 120.5(5) . .
C6 C5 C8 120.1(5) . .
C7 C6 C5 118.6(6) . .
C7 C6 H6A 120.7 . .
C5 C6 H6A 120.7 . .
C2 C7 C6 121.9(5) . .
C2 C7 H7A 119.0 . .
C6 C7 H7A 119.0 . .
N1 C8 N1 124.8(6) . 5
N1 C8 C5 117.3(5) . .
N1 C8 C5 117.9(5) 5 .
C9 O3 C9 44.8(17) 25_566 .
C9 O3 Tb1 157.6(8) 25_566 .
C9 O3 Tb1 157.6(8) . .
C9 C9 O3 67.6(8) 25_566 .
C9 C9 O3 67.6(8) 25_566 25_566
O3 C9 O3 135.2(17) . 25_566
C11 N2 C11 118(3) . 26_556
C11 N2 C10 111.6(11) . 3_556
C11 N2 C10 111.6(11) 26_556 3_556
C11 N2 C10 111.6(11) . .
C11 N2 C10 111.6(11) 26_556 .
C10 N2 C10 89(3) 3_556 .
C13 N3 C13 128(5) 26_556 .
C13 N3 C12 104.0(14) 26_556 27_565
C13 N3 C12 104.0(14) . 27_565
C13 N3 C12 104.0(14) 26_556 .
C13 N3 C12 104.0(14) . .
C12 N3 C12 113(4) 27_565 .
C14 N5 C16 112(3) . .
C14 N5 C15 131(3) . .
C16 N5 C15 117(3) . .
O4 C14 N5 122(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O3 2.264(7) .
Tb1 O1B 2.397(13) 2_565
Tb1 O1B 2.397(13) 27_565
Tb1 O1B 2.397(13) 28
Tb1 O1B 2.397(13) .
Tb1 O2B 2.431(6) 2_565
Tb1 O2B 2.431(6) 27_565
Tb1 O2B 2.431(6) 28
Tb1 O2B 2.431(6) .
Tb1 O2 2.505(7) 2_565
Tb1 O2 2.505(7) 27_565
Tb1 O2 2.505(7) 28
O1 C1 1.243(8) .
O2 C1 1.282(7) .
O1B C1 1.240(9) .
O2B C1 1.290(7) .
O2B O2B 1.740(15) 27_565
N1 C8 1.343(7) .
N1 C8 1.350(7) 9
C1 C2 1.510(7) .
C2 C7 1.361(8) .
C2 C3 1.373(8) .
C3 C4 1.380(8) .
C3 H3A 0.9300 .
C4 C5 1.355(8) .
C4 H4A 0.9300 .
C5 C6 1.392(8) .
C5 C8 1.469(7) .
C6 C7 1.391(8) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
C8 N1 1.350(7) 5
O3 C9 1.223(7) 25_566
O3 C9 1.223(7) .
C9 C9 0.93(4) 25_566
C9 O3 1.223(7) 25_566
N2 C11 1.44(2) .
N2 C11 1.44(2) 26_556
N2 C10 1.50(2) 3_556
N2 C10 1.50(2) .
N3 C13 1.52(5) 26_556
N3 C13 1.52(5) .
N3 C12 1.58(4) 27_565
N3 C12 1.58(4) .
O4 C14 1.266(10) .
N5 C14 1.350(10) .
N5 C16 1.419(10) .
N5 C15 1.422(10) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 2078.9 22.6
2 0.500 0.500 0.500 2079.1 22.6
