#------------------------------------------------------------------------------
#$Date: 2021-03-29 10:02:11 +0300 (Mon, 29 Mar 2021) $
#$Revision: 263401 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/13/1561316.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_1561316
loop_
_publ_author_name
'Wei, Lian-Qiang'
'Li, Yue'
'Mao, Li-Yuan'
'Chen, Qing'
'Lin, Ning'
_publ_section_title
;
 A series of porous metal--organic frameworks with hendecahedron cage:
 Structural variation and drug slow release properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              58
_journal_page_last               63
_journal_paper_doi               10.1016/j.jssc.2017.09.021
_journal_volume                  257
_journal_year                    2018
_chemical_formula_sum            'C50 H29 Cu3 N2 O13'
_chemical_formula_weight         1056.37
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6856(6)
_cell_length_b                   19.6856(6)
_cell_length_c                   59.9228(15)
_cell_measurement_reflns_used    821
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      45.5520
_cell_measurement_theta_min      4.3060
_cell_volume                     23221.5(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1234
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            19151
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        62.752
_diffrn_reflns_theta_max         62.752
_diffrn_reflns_theta_min         3.501
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.604
_exptl_crystal_description       block
_exptl_crystal_F_000             4272
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0410P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1840
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2248
_reflns_number_total             4853
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            JSSC-2018-257-58.cif
_cod_data_source_block           2
_cod_original_cell_volume        23221.5(15)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               1561316
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'
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
Cu1 Cu 0.5000 0.2500 0.14698(2) 0.0688(5) Uani 1 4 d S T P . .
Cu2 Cu 0.18372(6) 0.7500 0.24694(2) 0.0697(4) Uani 1 2 d S T P . .
O1 O 0.3169(2) 0.6813(2) 0.22929(5) 0.0897(13) Uani 1 1 d . . . . .
O2 O 0.2034(2) 0.6802(2) 0.22462(5) 0.0873(12) Uani 1 1 d . . . . .
O3 O 0.42999(19) 0.31991(19) 0.14366(5) 0.0823(12) Uani 1 1 d . . . . .
N1 N 0.0729(3) 0.7500 0.24276(8) 0.0750(19) Uani 1 2 d S T P . .
C1 C 0.2632(3) 0.6630(3) 0.22012(8) 0.0723(16) Uani 1 1 d . . . . .
C2 C 0.2727(4) 0.6138(3) 0.20076(8) 0.0868(19) Uani 1 1 d . . . . .
C3 C 0.2162(4) 0.5939(4) 0.18880(9) 0.107(2) Uani 1 1 d . . . . .
H3A H 0.1733 0.6091 0.1930 0.128 Uiso 1 1 calc R U . . .
C4 C 0.2232(4) 0.5506(4) 0.17011(10) 0.125(3) Uani 1 1 d . . . . .
H4A H 0.1852 0.5379 0.1619 0.150 Uiso 1 1 calc R U . . .
C5 C 0.2867(4) 0.5272(4) 0.16412(9) 0.102(2) Uani 1 1 d . . . . .
C6 C 0.3426(4) 0.5464(4) 0.17699(11) 0.128(3) Uani 1 1 d . . . . .
H6A H 0.3854 0.5300 0.1733 0.154 Uiso 1 1 calc R U . . .
C7 C 0.3353(4) 0.5898(4) 0.19538(9) 0.114(3) Uani 1 1 d . . . . .
H7A H 0.3730 0.6021 0.2038 0.136 Uiso 1 1 calc R U . . .
C8 C 0.2964(3) 0.4837(4) 0.14385(8) 0.101(2) Uani 1 1 d . . . . .
C10 C 0.3446(3) 0.4323(3) 0.14348(8) 0.090(2) Uani 1 1 d . . . . .
H10A H 0.3699 0.4237 0.1563 0.108 Uiso 1 1 calc R U . . .
C11 C 0.3559(3) 0.3941(3) 0.1250 0.078(2) Uani 1 2 d S T P . .
C12 C 0.4090(3) 0.3410(3) 0.1250 0.079(2) Uani 1 2 d S T P . .
C13 C 0.0381(4) 0.7500 0.26065(12) 0.111(3) Uani 1 2 d S T P . .
H13 H 0.0608 0.7500 0.2743 0.133 Uiso 1 2 calc R U P . .
C14 C 0.0390(4) 0.7500 0.22357(11) 0.098(3) Uani 1 2 d S T P . .
C15 C 0.0728(5) 0.7500 0.20291(12) 0.126(4) Uani 1 2 d S T P . .
H15A H 0.1200 0.7500 0.2024 0.151 Uiso 1 2 calc R U P . .
C16 C 0.0363(5) 0.7500 0.18348(12) 0.170(6) Uani 1 2 d S T P . .
H16 H 0.0594 0.7500 0.1699 0.204 Uiso 1 2 calc R U P . .
O1W O 0.5000 0.2500 0.18319(10) 0.135(4) Uani 1 4 d S T P . .
H1WA H 0.5289 0.2213 0.1879 0.202 Uiso 0.25 1 d R U P . .
C9 C 0.2563(3) 0.4937(3) 0.1250 0.114(4) Uani 1 2 d S T P . .
H9 H 0.2229 0.5271 0.1250 0.137 Uiso 1 2 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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 Cu1 O3 89.3(2) . 29
O3 Cu1 O3 89.5(2) . 22_655
O3 Cu1 O3 168.35(17) 29 22_655
O3 Cu1 O3 168.35(17) . 10_554
O3 Cu1 O3 89.5(2) 29 10_554
O3 Cu1 O3 89.3(2) 22_655 10_554
O3 Cu1 O1W 95.83(9) . .
O3 Cu1 O1W 95.82(9) 29 .
O3 Cu1 O1W 95.82(9) 22_655 .
O3 Cu1 O1W 95.82(9) 10_554 .
O3 Cu1 Cu1 84.17(9) . 27_565
O3 Cu1 Cu1 84.18(9) 29 27_565
O3 Cu1 Cu1 84.18(9) 22_655 27_565
O3 Cu1 Cu1 84.18(9) 10_554 27_565
O1W Cu1 Cu1 180.0 . 27_565
O2 Cu2 O2 89.2(2) . 29_565
O2 Cu2 O1 168.70(17) . 25_565
O2 Cu2 O1 90.77(16) 29_565 25_565
O2 Cu2 O1 90.76(16) . 5
O2 Cu2 O1 168.70(17) 29_565 5
O1 Cu2 O1 87.0(2) 25_565 5
O2 Cu2 N1 96.83(16) . .
O2 Cu2 N1 96.84(15) 29_565 .
O1 Cu2 N1 94.38(16) 25_565 .
O1 Cu2 N1 94.38(16) 5 .
O2 Cu2 Cu2 84.20(13) . 25_565
O2 Cu2 Cu2 84.20(13) 29_565 25_565
O1 Cu2 Cu2 84.56(13) 25_565 25_565
O1 Cu2 Cu2 84.56(13) 5 25_565
N1 Cu2 Cu2 178.54(14) . 25_565
C1 O1 Cu2 121.0(4) . 25_565
C1 O2 Cu2 121.5(4) . .
C12 O3 Cu1 123.4(4) . .
C13 N1 C14 117.3(7) . .
C13 N1 Cu2 116.1(5) . .
C14 N1 Cu2 126.6(5) . .
O1 C1 O2 128.6(5) . .
O1 C1 C2 114.6(5) . .
O2 C1 C2 116.8(5) . .
C7 C2 C3 120.6(5) . .
C7 C2 C1 120.9(6) . .
C3 C2 C1 118.5(6) . .
C2 C3 C4 120.2(6) . .
C2 C3 H3A 119.9 . .
C4 C3 H3A 119.9 . .
C5 C4 C3 119.7(6) . .
C5 C4 H4A 120.1 . .
C3 C4 H4A 120.1 . .
C4 C5 C6 118.7(6) . .
C4 C5 C8 121.1(6) . .
C6 C5 C8 120.2(6) . .
C5 C6 C7 121.3(6) . .
C5 C6 H6A 119.3 . .
C7 C6 H6A 119.3 . .
C2 C7 C6 119.4(6) . .
C2 C7 H7A 120.3 . .
C6 C7 H7A 120.3 . .
C10 C8 C9 118.5(5) . .
C10 C8 C5 121.1(5) . .
C9 C8 C5 120.3(6) . .
C11 C10 C8 122.0(5) . .
C11 C10 H10A 119.0 . .
C8 C10 H10A 119.0 . .
C10 C11 C10 119.0(7) 16_554 .
C10 C11 C12 120.5(4) 16_554 .
C10 C11 C12 120.5(4) . .
O3 C12 O3 124.8(8) . 16_554
O3 C12 C11 117.6(4) . .
O3 C12 C11 117.6(4) 16_554 .
N1 C13 C13 122.6(4) . 10_464
N1 C13 H13 118.7 . .
C13 C13 H13 118.7 10_464 .
N1 C14 C15 121.7(8) . .
N1 C14 C14 120.1(4) . 10_464
C15 C14 C14 118.2(5) . 10_464
C16 C15 C14 120.1(9) . .
C16 C15 H15A 119.9 . .
C14 C15 H15A 119.9 . .
C15 C16 C16 121.7(5) . 10_464
C15 C16 H16 119.2 . .
C16 C16 H16 119.2 10_464 .
Cu1 O1W H1WA 109.5 . .
C8 C9 C8 119.9(8) . 16_554
C8 C9 H9 120.0 . .
C8 C9 H9 120.0 16_554 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.958(4) .
Cu1 O3 1.958(4) 29
Cu1 O3 1.958(4) 22_655
Cu1 O3 1.958(4) 10_554
Cu1 O1W 2.170(6) .
Cu1 Cu1 2.634(2) 27_565
Cu2 O2 1.956(4) .
Cu2 O2 1.956(4) 29_565
Cu2 O1 1.964(4) 25_565
Cu2 O1 1.964(4) 5
Cu2 N1 2.196(6) .
Cu2 Cu2 2.635(2) 25_565
O1 C1 1.245(6) .
O1 Cu2 1.964(4) 25_565
O2 C1 1.255(6) .
O3 C12 1.262(5) .
N1 C13 1.272(9) .
N1 C14 1.329(9) .
C1 C2 1.522(7) .
C2 C7 1.359(8) .
C2 C3 1.380(8) .
C3 C4 1.415(8) .
C3 H3A 0.9300 .
C4 C5 1.379(8) .
C4 H4A 0.9300 .
C5 C6 1.395(9) .
C5 C8 1.498(7) .
C6 C7 1.402(8) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
C8 C10 1.388(8) .
C8 C9 1.392(7) .
C10 C11 1.357(6) .
C10 H10A 0.9300 .
C11 C10 1.357(6) 16_554
C11 C12 1.479(10) .
C12 O3 1.262(5) 16_554
C13 C13 1.499(16) 10_464
C13 H13 0.9300 .
C14 C15 1.405(10) .
C14 C14 1.537(17) 10_464
C15 C16 1.368(11) .
C15 H15A 0.9300 .
C16 C16 1.430(18) 10_464
C16 H16 0.9300 .
O1W H1WA 0.8500 .
C9 C8 1.392(7) 16_554
C9 H9 0.9300 .
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
_platon_squeeze_void_content
1 -0.058 0.152 0.087 16584 3677 ' '
