#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:40:23 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178819 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/73/4107326.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_4107326
loop_
_publ_author_name
'Shengqian Ma'
'Daofeng Sun'
'Jason M. Simmons'
'Christopher D. Collier'
'Daqiang Yuan'
'Hong-Cai Zhou'
_publ_section_title
;
 Metal-Organic Framework from an Anthracene Derivative Containing
 Nanoscopic Cages Exhibiting High Methane Uptake
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1012
_journal_page_last               1016
_journal_paper_doi               10.1021/ja0771639
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'Cu18 (C30 H14 O8)9 (H2 O)18'
_chemical_formula_sum            'C270 H162 Cu18 O90'
_chemical_formula_weight         5989.9
_chemical_name_common            PCN-14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.4530(4)
_cell_length_b                   18.4530(4)
_cell_length_c                   76.976(4)
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      68.1
_cell_measurement_theta_min      3.0
_cell_volume                     22699.7(14)
_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      90(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       88
_diffrn_reflns_limit_l_min       -92
_diffrn_reflns_number            90758
_diffrn_reflns_theta_full        68.10
_diffrn_reflns_theta_max         68.10
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.9248
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   none
_exptl_crystal_colour            'blue green'
_exptl_crystal_density_diffrn    0.871
_exptl_crystal_description       block
_exptl_crystal_F_000             5976
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.000003(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1200P)²+4.7435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1658
_reflns_number_gt                3769
_reflns_number_total             4581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0771639-file001.cif
_cod_data_source_block           sq
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4107326
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Cu1 Cu 0.13354(2) 0.84812(2) 0.069247(4) 0.03924(18) Uani 1 1 d .
O1 O 0.24483(12) 0.88286(13) 0.06053(2) 0.0525(5) Uani 1 1 d .
O2 O 0.55260(11) 0.85711(12) 0.08527(2) 0.0517(4) Uani 1 1 d .
O3 O 0.28749(12) 0.84696(12) 0.08470(2) 0.0517(4) Uani 1 1 d .
O4 O 0.63651(11) 0.90333(13) 0.06194(2) 0.0552(5) Uani 1 1 d .
C5 C 0.57204(15) 0.88885(17) 0.07044(3) 0.0501(6) Uani 1 1 d .
C6 C 0.46759(16) 0.94892(18) 0.03595(4) 0.0508(7) Uani 1 1 d .
C7 C 0.29686(16) 0.87546(17) 0.06960(3) 0.0468(6) Uani 1 1 d .
C8 C 0.52654(17) 0.93798(18) 0.04487(4) 0.0524(6) Uani 1 1 d .
H8 H 0.5774 0.9504 0.0393 0.063 Uiso 1 1 calc R
C9 C 0.43660(17) 0.91771(18) 0.00427(4) 0.0504(6) Uani 1 1 d .
C10 C 0.45507(18) 0.94346(18) -0.01331(4) 0.0490(6) Uani 1 1 d .
C11 C 0.39422(17) 0.93064(17) 0.04421(3) 0.0497(6) Uani 1 1 d .
H11 H 0.3533 0.9378 0.0382 0.060 Uiso 1 1 calc R
C12 C 0.37931(16) 0.90172(16) 0.06128(3) 0.0471(6) Uani 1 1 d .
C13 C 0.48297(16) 0.97619(19) 0.01743(4) 0.0486(6) Uani 1 1 d .
O14 O 0.09416(18) 0.8843(2) 0.04659(4) 0.1025(10) Uani 1 1 d .
C15 C 0.43938(16) 0.89132(18) 0.07000(4) 0.0490(6) Uani 1 1 d .
H15 H 0.4299 0.8718 0.0817 0.059 Uiso 1 1 calc R
C16 C 0.4082(2) 0.8819(2) -0.02635(4) 0.0617(7) Uani 1 1 d .
H16 H 0.4196 0.8968 -0.0383 0.074 Uiso 1 1 calc R
C17 C 0.51270(16) 0.90934(18) 0.06172(3) 0.0506(6) Uani 1 1 d .
C18 C 0.37354(18) 0.83488(18) 0.00803(4) 0.0600(7) Uani 1 1 d .
H18 H 0.3613 0.8175 0.0198 0.072 Uiso 1 1 calc R
C19 C 0.3488(2) 0.8039(2) -0.02215(4) 0.0691(8) Uani 1 1 d .
H19 H 0.3189 0.7646 -0.0311 0.083 Uiso 1 1 calc R
C21 C 0.3306(2) 0.7802(2) -0.00463(4) 0.0689(8) Uani 1 1 d .
H21 H 0.2876 0.7252 -0.0018 0.083 Uiso 1 1 calc R
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
O2 Cu1 O1 170.73(7) 17_564 .
O2 Cu1 O4 89.89(9) 17_564 2_665
O1 Cu1 O4 89.76(9) . 2_665
O2 Cu1 O3 89.19(9) 17_564 16_454
O1 Cu1 O3 88.74(8) . 16_454
O4 Cu1 O3 164.93(8) 2_665 16_454
O2 Cu1 O14 94.40(10) 17_564 .
O1 Cu1 O14 94.84(10) . .
O4 Cu1 O14 96.71(12) 2_665 .
O3 Cu1 O14 98.36(11) 16_454 .
O2 Cu1 Cu1 85.44(5) 17_564 16_454
O1 Cu1 Cu1 85.33(5) . 16_454
O4 Cu1 Cu1 82.35(5) 2_665 16_454
O3 Cu1 Cu1 82.58(5) 16_454 16_454
O14 Cu1 Cu1 179.05(10) . 16_454
C7 O1 Cu1 121.05(17) . .
C5 O2 Cu1 121.84(16) . 17_664
C7 O3 Cu1 123.13(16) . 16_454
C5 O4 Cu1 123.82(17) . 3_565
O2 C5 O4 126.2(2) . .
O2 C5 C17 117.1(2) . .
O4 C5 C17 116.6(2) . .
C11 C6 C8 118.9(3) . .
C11 C6 C13 121.5(2) . .
C8 C6 C13 119.5(2) . .
O1 C7 O3 127.8(2) . .
O1 C7 C12 116.1(2) . .
O3 C7 C12 116.1(2) . .
C17 C8 C6 121.0(2) . .
C18 C9 C13 122.4(3) . .
C18 C9 C10 119.2(3) . .
C13 C9 C10 118.4(3) . .
C13 C10 C9 120.6(3) 19_675 .
C13 C10 C16 122.4(3) 19_675 .
C9 C10 C16 117.0(3) . .
C6 C11 C12 120.8(2) . .
C15 C12 C11 119.4(2) . .
C15 C12 C7 120.2(2) . .
C11 C12 C7 120.2(2) . .
C10 C13 C9 121.0(3) 19_675 .
C10 C13 C6 119.8(3) 19_675 .
C9 C13 C6 119.1(3) . .
C17 C15 C12 119.9(3) . .
C19 C16 C10 121.7(3) . .
C8 C17 C15 120.0(2) . .
C8 C17 C5 120.3(2) . .
C15 C17 C5 119.3(2) . .
C21 C18 C9 121.5(3) . .
C16 C19 C21 120.4(3) . .
C18 C21 C19 120.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.9336(18) 17_564
Cu1 O1 1.9396(18) .
Cu1 O4 1.9582(18) 2_665
Cu1 O3 1.9606(18) 16_454
Cu1 O14 2.122(2) .
Cu1 Cu1 2.6547(6) 16_454
O1 C7 1.248(3) .
O2 C5 1.251(3) .
O2 Cu1 1.9337(18) 17_664
O3 C7 1.252(3) .
O3 Cu1 1.9606(18) 16_454
O4 C5 1.263(3) .
O4 Cu1 1.9582(18) 3_565
C5 C17 1.485(4) .
C6 C11 1.376(4) .
C6 C8 1.384(4) .
C6 C13 1.491(4) .
C7 C12 1.491(3) .
C8 C17 1.375(4) .
C9 C18 1.412(4) .
C9 C13 1.414(4) .
C9 C10 1.418(4) .
C10 C13 1.382(4) 19_675
C10 C16 1.436(4) .
C11 C12 1.393(4) .
C12 C15 1.389(4) .
C13 C10 1.382(4) 19_675
C15 C17 1.377(4) .
C16 C19 1.342(4) .
C18 C21 1.340(4) .
C19 C21 1.406(4) .
