#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:51:57 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180279 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/65/7116557.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_7116557
loop_
_publ_author_name
'Hyehyun Kim'
'Minhak Oh'
'Dongwook Kim'
'Jeongin Park'
'Junmo Seong'
'Sang Kyu Kwak'
'Myoung Soo Lah'
_publ_section_title
;
 Single crystalline hollow metal-organic frameworks: a metal-organic
 polyhedron single crystal as a sacrificial template
;
_journal_name_full               Chem.Commun.
_journal_page_first              3678
_journal_paper_doi               10.1039/C4cc10051D
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C216 H184 Cu24 N8 O144'
_chemical_formula_weight         6720.66
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-01-09 deposited with the CCDC.
2015-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.096(4)
_cell_length_b                   28.096(4)
_cell_length_c                   40.947(8)
_cell_measurement_reflns_used    259834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.400
_cell_measurement_theta_min      2.885
_cell_volume                     32323(9)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'Diamond 3'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            60455
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        29.997
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         2.885
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL3000
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.691
_exptl_crystal_description       block
_exptl_crystal_F_000             6768
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.446
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8507
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.476
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.1132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3621
_refine_ls_wR_factor_ref         0.4021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4439
_reflns_number_total             8507
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc10051d2.cif
_cod_data_source_block           p13_020i4m_sq
_cod_original_cell_volume        32323(11)
_cod_database_code               7116557
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_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.
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.65602(9) 0.71813(9) 0.18072(5) 0.3291(13) Uani 1 1 d . . .
Cu2 Cu 0.61840(5) 0.66417(5) 0.13487(3) 0.2528(9) Uani 1 1 d . . .
Cu3 Cu 0.87492(8) 0.5639(2) 0.0000 0.384(2) Uani 1 2 d S T P
Cu4 Cu 0.78260(5) 0.54744(9) 0.0000 0.2680(11) Uani 1 2 d S T P
O1 O 0.7151(4) 0.7164(4) 0.1521(2) 0.378(6) Uani 1 1 d D U .
O2 O 0.6823(3) 0.6688(3) 0.11452(18) 0.293(4) Uani 1 1 d D . .
O3 O 0.8594(3) 0.6108(5) 0.0342(2) 0.361(6) Uani 1 1 d D U .
O4 O 0.7816(3) 0.5992(3) 0.03363(16) 0.291(4) Uani 1 1 d D . .
O5 O 0.8769(6) 0.7494(7) 0.1121(4) 0.581(13) Uani 1 1 d D U .
C1 C 0.7620(4) 0.6890(5) 0.1100(3) 0.410(9) Uani 1 1 d DG U .
C2 C 0.7694(4) 0.6550(4) 0.0858(3) 0.372(9) Uani 1 1 d DG U .
H2 H 0.7449 0.6329 0.0806 0.446 Uiso 1 1 calc R U .
C3 C 0.8126(5) 0.6534(5) 0.0693(3) 0.400(11) Uani 1 1 d DG . .
C4 C 0.8483(4) 0.6857(6) 0.0769(3) 0.451(15) Uani 1 1 d DG . .
H4 H 0.8778 0.6846 0.0656 0.541 Uiso 1 1 calc R U .
C5 C 0.8409(4) 0.7197(5) 0.1011(3) 0.448(12) Uani 1 1 d DG U .
C6 C 0.7977(5) 0.7213(5) 0.1176(3) 0.454(11) Uani 1 1 d DG U .
H6 H 0.7927 0.7445 0.1341 0.544 Uiso 1 1 calc R U .
C7 C 0.7174(5) 0.6918(5) 0.1268(3) 0.346(8) Uani 1 1 d D U .
C8 C 0.8184(5) 0.6203(5) 0.0445(4) 0.325(7) Uani 1 1 d D U .
O6 O 0.6726(3) 0.6588(5) 0.19947(17) 0.334(5) Uani 1 1 d D . .
O7 O 0.6398(3) 0.6111(2) 0.16186(15) 0.258(3) Uani 1 1 d D . .
O8 O 0.7114(3) 0.4066(4) 0.20070(19) 0.307(4) Uani 1 1 d D . .
O9 O 0.6675(2) 0.4390(3) 0.16157(16) 0.249(3) Uani 1 1 d D . .
O10 O 0.7380(6) 0.5361(5) 0.2810(2) 0.480(9) Uani 1 1 d D . .
C9 C 0.6821(3) 0.5719(3) 0.20369(17) 0.288(6) Uani 1 1 d DG . .
C10 C 0.67659(19) 0.5275(3) 0.18930(14) 0.259(4) Uani 1 1 d DG . .
H10A H 0.6632 0.5249 0.1681 0.310 Uiso 1 1 calc R U .
C11 C 0.6907(2) 0.4867(3) 0.20597(15) 0.301(7) Uani 1 1 d DG . .
C12 C 0.7103(3) 0.4905(4) 0.23703(13) 0.373(8) Uani 1 1 d DG U .
H12 H 0.7200 0.4626 0.2484 0.447 Uiso 1 1 calc R U .
C13 C 0.7158(3) 0.5349(4) 0.25141(14) 0.397(10) Uani 1 1 d DG U .
C14 C 0.7017(3) 0.5757(4) 0.23474(18) 0.389(10) Uani 1 1 d DG . .
H14 H 0.7055 0.6061 0.2446 0.467 Uiso 1 1 calc R U .
C15 C 0.6634(5) 0.6146(5) 0.1881(3) 0.300(6) Uani 1 1 d D . .
C16 C 0.6902(5) 0.4408(5) 0.1879(3) 0.273(5) Uani 1 1 d D . .
O11 O 0.8758(3) 0.5146(5) 0.0325(3) 0.393(8) Uani 1 1 d D . .
O12 O 0.7973(2) 0.5007(3) 0.03312(16) 0.274(3) Uani 1 1 d D . .
O13 O 0.7698(3) 0.3693(4) 0.1530(2) 0.356(5) Uani 1 1 d D . .
O14 O 0.7245(2) 0.3975(3) 0.11450(17) 0.276(3) Uani 1 1 d D . .
O15 O 0.9380(4) 0.4042(9) 0.1183(4) 0.658(16) Uani 1 1 d D U .
C17 C 0.8425(3) 0.4612(4) 0.07163(16) 0.386(12) Uani 1 1 d DG . .
C18 C 0.8024(3) 0.4403(3) 0.08543(14) 0.315(7) Uani 1 1 d DG U .
H18 H 0.7716 0.4501 0.0787 0.378 Uiso 1 1 calc R U .
C19 C 0.8075(3) 0.4050(3) 0.10900(18) 0.334(8) Uani 1 1 d DG U .
C20 C 0.8527(3) 0.3907(4) 0.11878(19) 0.540(15) Uani 1 1 d DG U .
H20 H 0.8561 0.3666 0.1349 0.648 Uiso 1 1 calc R U .
C21 C 0.8928(3) 0.4116(4) 0.10498(19) 0.553(13) Uani 1 1 d DG U .
C22 C 0.8877(3) 0.4468(4) 0.08141(19) 0.526(14) Uani 1 1 d DG U .
H22 H 0.9151 0.4611 0.0720 0.631 Uiso 1 1 calc R U .
C23 C 0.8408(5) 0.4937(6) 0.0455(4) 0.422(15) Uani 1 1 d D . .
C24 C 0.7651(5) 0.3916(5) 0.1251(3) 0.323(8) Uani 1 1 d D . .
O1S O 0.6858(4) 0.7627(4) 0.2189(2) 0.338(5) Uani 1 1 d D U .
N1S N 0.6858(5) 0.7776(6) 0.2733(5) 0.451(10) Uani 1 1 d D U .
C1S C 0.6725(5) 0.7514(7) 0.2437(4) 0.417(9) Uani 1 1 d D U .
H1S H 0.6523 0.7245 0.2454 0.501 Uiso 1 1 calc R U .
C2S C 0.7153(8) 0.8158(6) 0.2670(6) 0.465(14) Uani 1 1 d D U .
H2S1 H 0.7215 0.8178 0.2435 0.698 Uiso 1 1 calc R U .
H2S2 H 0.6999 0.8452 0.2743 0.698 Uiso 1 1 calc R U .
H2S3 H 0.7455 0.8117 0.2787 0.698 Uiso 1 1 calc R U .
C3S C 0.6645(10) 0.7565(13) 0.3023(6) 0.71(3) Uani 1 1 d D U .
H3S1 H 0.6454 0.7288 0.2960 1.058 Uiso 1 1 calc R U .
H3S2 H 0.6897 0.7465 0.3174 1.058 Uiso 1 1 calc R U .
H3S3 H 0.6441 0.7801 0.3130 1.058 Uiso 1 1 calc R U .
O1W O 0.5912(4) 0.6174(3) 0.09796(16) 0.336(5) Uani 1 1 d . . .
O2W O 0.7080(3) 0.5344(4) 0.0000 0.374(9) Uani 1 2 d S T P
O3W O 0.9545(4) 0.5822(9) 0.0000 0.479(14) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0074 0.0035 '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 0.0135 0.0071 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0225 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -0.0744 2.2856 '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
O6 Cu1 O8 88.1(4) . 3_655
O6 Cu1 O13 165.6(4) . 3_655
O8 Cu1 O13 89.3(5) 3_655 3_655
O6 Cu1 O1 90.6(5) . .
O8 Cu1 O1 167.6(3) 3_655 .
O13 Cu1 O1 88.9(5) 3_655 .
O6 Cu1 O1S 96.9(4) . .
O8 Cu1 O1S 95.8(4) 3_655 .
O13 Cu1 O1S 97.4(4) 3_655 .
O1 Cu1 O1S 96.6(4) . .
O6 Cu1 Cu2 83.2(2) . .
O8 Cu1 Cu2 83.2(2) 3_655 .
O13 Cu1 Cu2 82.4(3) 3_655 .
O1 Cu1 Cu2 84.4(2) . .
O1S Cu1 Cu2 179.0(3) . .
O14 Cu2 O9 90.5(3) 3_655 3_655
O14 Cu2 O7 169.0(3) 3_655 .
O9 Cu2 O7 88.5(3) 3_655 .
O14 Cu2 O2 88.3(4) 3_655 .
O9 Cu2 O2 168.7(3) 3_655 .
O7 Cu2 O2 90.5(4) . .
O14 Cu2 O1W 98.6(3) 3_655 .
O9 Cu2 O1W 97.4(3) 3_655 .
O7 Cu2 O1W 92.4(3) . .
O2 Cu2 O1W 93.9(3) . .
O14 Cu2 Cu1 84.0(2) 3_655 .
O9 Cu2 Cu1 84.5(2) 3_655 .
O7 Cu2 Cu1 84.95(18) . .
O2 Cu2 Cu1 84.2(2) . .
O1W Cu2 Cu1 176.7(3) . .
O11 Cu3 O11 87.8(8) . 10
O11 Cu3 O3 89.6(5) . .
O11 Cu3 O3 167.7(4) 10 .
O11 Cu3 O3 167.7(4) . 10
O11 Cu3 O3 89.6(5) 10 10
O3 Cu3 O3 90.4(8) . 10
O11 Cu3 O3W 98.6(5) . .
O11 Cu3 O3W 98.6(5) 10 .
O3 Cu3 O3W 93.7(5) . .
O3 Cu3 O3W 93.7(5) 10 .
O11 Cu3 Cu4 83.5(3) . .
O11 Cu3 Cu4 83.5(3) 10 .
O3 Cu3 Cu4 84.3(3) . .
O3 Cu3 Cu4 84.3(3) 10 .
O3W Cu3 Cu4 177.2(7) . .
O12 Cu4 O12 89.1(5) 10 .
O12 Cu4 O4 90.8(4) 10 10
O12 Cu4 O4 168.2(3) . 10
O12 Cu4 O4 168.2(3) 10 .
O12 Cu4 O4 90.8(4) . .
O4 Cu4 O4 86.8(5) 10 .
O12 Cu4 O2W 95.4(3) 10 .
O12 Cu4 O2W 95.4(3) . .
O4 Cu4 O2W 96.4(3) 10 .
O4 Cu4 O2W 96.4(3) . .
O12 Cu4 Cu3 84.8(2) 10 .
O12 Cu4 Cu3 84.8(2) . .
O4 Cu4 Cu3 83.4(2) 10 .
O4 Cu4 Cu3 83.4(2) . .
O2W Cu4 Cu3 179.8(4) . .
C7 O1 Cu1 122.4(8) . .
C7 O2 Cu2 124.3(7) . .
C8 O3 Cu3 125.6(9) . .
C8 O4 Cu4 124.6(8) . .
C2 C1 C6 120.0 . .
C2 C1 C7 120.8(9) . .
C6 C1 C7 119.1(9) . .
C3 C2 C1 120.0 . .
C8 C3 C2 118.8(10) . .
C8 C3 C4 121.1(10) . .
C2 C3 C4 120.0 . .
C5 C4 C3 120.0 . .
O5 C5 C4 122.4(12) . .
O5 C5 C6 117.2(11) . .
C4 C5 C6 120.0 . .
C5 C6 C1 120.0 . .
O1 C7 O2 124.5(12) . .
O1 C7 C1 118.5(12) . .
O2 C7 C1 117.0(11) . .
O3 C8 O4 122.1(13) . .
O3 C8 C3 119.7(12) . .
O4 C8 C3 118.1(12) . .
C15 O6 Cu1 128.5(7) . .
C15 O7 Cu2 125.7(7) . .
C16 O8 Cu1 124.5(8) . 4_565
C16 O9 Cu2 122.6(7) . 4_565
C10 C9 C14 120.0 . .
C10 C9 C15 121.0(7) . .
C14 C9 C15 118.8(7) . .
C9 C10 C11 120.0 . .
C10 C11 C12 120.0 . .
C10 C11 C16 117.9(6) . .
C12 C11 C16 121.6(6) . .
C13 C12 C11 120.0 . .
O10 C13 C12 116.7(8) . .
O10 C13 C14 123.1(8) . .
C12 C13 C14 120.0 . .
C13 C14 C9 120.0 . .
O7 C15 O6 117.6(11) . .
O7 C15 C9 119.8(10) . .
O6 C15 C9 122.5(11) . .
O8 C16 O9 125.0(11) . .
O8 C16 C11 117.2(11) . .
O9 C16 C11 117.8(10) . .
C23 O11 Cu3 128.0(9) . .
C23 O12 Cu4 124.1(8) . .
C24 O13 Cu1 126.8(8) . 4_565
C24 O14 Cu2 128.7(7) . 4_565
C18 C17 C22 120.0 . .
C18 C17 C23 123.7(7) . .
C22 C17 C23 116.0(7) . .
C19 C18 C17 120.0 . .
C18 C19 C20 120.0 . .
C18 C19 C24 115.3(6) . .
C20 C19 C24 123.9(6) . .
C19 C20 C21 120.0 . .
C22 C21 C20 120.0 . .
C22 C21 O15 118.0(11) . .
C20 C21 O15 121.0(10) . .
C21 C22 C17 120.0 . .
O11 C23 O12 119.0(13) . .
O11 C23 C17 126.4(11) . .
O12 C23 C17 114.5(12) . .
O14 C24 O13 117.8(12) . .
O14 C24 C19 125.5(10) . .
O13 C24 C19 116.6(11) . .
C1S O1S Cu1 111.0(14) . .
C2S N1S C3S 135.8(19) . .
C2S N1S C1S 112.7(16) . .
C3S N1S C1S 111.5(17) . .
O1S C1S N1S 121(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O6 1.894(13) .
Cu1 O8 1.949(12) 3_655
Cu1 O13 1.977(10) 3_655
Cu1 O1 2.033(11) .
Cu1 O1S 2.171(7) .
Cu1 Cu2 2.6346(15) .
Cu2 O14 1.941(7) 3_655
Cu2 O9 1.951(7) 3_655
Cu2 O7 1.951(7) .
Cu2 O2 1.984(8) .
Cu2 O1W 2.144(5) .
Cu3 O11 1.921(15) .
Cu3 O11 1.921(15) 10
Cu3 O3 1.971(12) .
Cu3 O3 1.971(12) 10
Cu3 O3W 2.294(12) .
Cu3 Cu4 2.635(3) .
Cu4 O12 1.933(8) 10
Cu4 O12 1.934(8) .
Cu4 O4 2.003(8) 10
Cu4 O4 2.003(8) .
Cu4 O2W 2.128(7) .
O1 C7 1.245(11) .
O2 C7 1.282(11) .
O3 C8 1.256(12) .
O4 C8 1.270(11) .
O5 C5 1.388(10) .
C1 C2 1.3900 .
C1 C6 1.3900 .
C1 C7 1.432(12) .
C2 C3 1.3900 .
C3 C8 1.387(13) .
C3 C4 1.3900 .
C4 C5 1.3900 .
C5 C6 1.3900 .
O6 C15 1.351(11) .
O7 C15 1.267(11) .
O8 C16 1.246(11) .
O8 Cu1 1.949(12) 4_565
O9 C16 1.254(12) .
O9 Cu2 1.951(7) 4_565
O10 C13 1.364(9) .
C9 C10 1.3900 .
C9 C14 1.3900 .
C9 C15 1.455(12) .
C10 C11 1.3900 .
C11 C12 1.3900 .
C11 C16 1.488(11) .
C12 C13 1.3900 .
C13 C14 1.3900 .
O11 C23 1.263(14) .
O12 C23 1.335(11) .
O13 C24 1.308(11) .
O13 Cu1 1.977(10) 4_565
O14 C24 1.232(11) .
O14 Cu2 1.941(7) 4_565
O15 C21 1.397(10) .
C17 C18 1.3900 .
C17 C22 1.3900 .
C17 C23 1.409(14) .
C18 C19 1.3900 .
C19 C20 1.3900 .
C19 C24 1.414(12) .
C20 C21 1.3900 .
C21 C22 1.3900 .
O1S C1S 1.127(15) .
N1S C2S 1.382(15) .
N1S C3S 1.455(16) .
N1S C1S 1.468(15) .
