#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:52:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180199 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/95/7109528.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_7109528
loop_
_publ_author_name
'Xingtang Rao'
'Jianfeng Cai'
'Jiancan Yu'
'Yabing He'
'Chuande Wu'
'Wei Zhou'
'Taner Yildirim'
'Banglin Chen'
'Guodong Qian'
_publ_section_title
;
 A microporous metal-organic framework with both open metal and Lewis
 basic pyridyl sites for high C2H2 and CH4 storage at room temperature
;
_journal_name_full               Chem.Commun.
_journal_page_first              6719
_journal_paper_doi               10.1039/c3cc41866a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C63 H39 Cu6 N3 O30'
_chemical_formula_weight         1699.21
_chemical_name_systematic
;
?
;
_space_group_IT_number           166
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :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            3
_cell_length_a                   18.8163(13)
_cell_length_b                   18.8163(13)
_cell_length_c                   38.079(4)
_cell_measurement_reflns_used    8052
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      3.75
_cell_volume                     11675.7(17)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd., 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω 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  0.1711
_diffrn_reflns_av_sigmaI/netI    0.1475
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            8052
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         3.75
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   CrysAlisPro
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    0.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       green
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0813P)²+12.3550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2233
_reflns_number_gt                1566
_reflns_number_total             2502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc41866a.txt
_cod_data_source_block           New
_cod_original_cell_volume        11675.7(16)
_cod_original_sg_symbol_H-M      R-3m
_cod_database_code               7109528
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-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+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-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+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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_group
Cu1 Cu 0.04598(5) 0.52299(3) 0.02875(2) 0.0336(4) Uani 1 2 d S .
O1 O 0.1115(2) 0.4830(3) 0.00459(10) 0.0508(11) Uani 1 1 d . .
O2 O 0.0319(2) 0.4446(3) -0.04409(10) 0.0495(11) Uani 1 1 d . .
O3 O 0.1083(6) 0.5541(3) 0.07814(19) 0.105(3) Uani 1 2 d S .
C1 C 0.0945(3) 0.4555(4) -0.02616(17) 0.0505(16) Uani 1 1 d . .
C2 C 0.1531(4) 0.4337(4) -0.04347(14) 0.0479(15) Uani 1 1 d . .
C3 C 0.2244(3) 0.4488(5) -0.0265(2) 0.046(2) Uani 1 2 d S .
H3A H 0.2346 0.4692 -0.0037 0.055 Uiso 1 2 calc SR .
C4 C 0.1386(4) 0.4047(4) -0.07814(15) 0.0544(16) Uani 1 1 d . .
H4A H 0.0913 0.3960 -0.0897 0.065 Uiso 1 1 calc R .
C5 C 0.1944(3) 0.3889(7) -0.0954(2) 0.065(3) Uani 1 2 d S .
C6 C 0.1810(4) 0.3620(7) -0.1327(3) 0.068(3) Uani 1 2 d S .
C7 C 0.1028(11) 0.3119(14) -0.1443(3) 0.086(5) Uani 0.38 1 d P .
N1 N 0.1028(11) 0.3119(14) -0.1443(3) 0.086(5) Uani 0.13 1 d P .
C7' C 0.1391(12) 0.3851(16) -0.1542(5) 0.101(7) Uani 0.38 1 d P 1
N1' N 0.1391(12) 0.3851(16) -0.1542(5) 0.101(7) Uani 0.13 1 d P 1
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'
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 O2 87.7(3) 19_565 6
O2 Cu1 O1 168.49(16) 19_565 .
O2 Cu1 O1 90.82(19) 6 .
O2 Cu1 O1 90.82(19) 19_565 24_565
O2 Cu1 O1 168.49(16) 6 24_565
O1 Cu1 O1 88.3(3) . 24_565
O2 Cu1 O3 92.6(2) 19_565 .
O2 Cu1 O3 92.6(2) 6 .
O1 Cu1 O3 98.9(2) . .
O1 Cu1 O3 98.9(2) 24_565 .
O2 Cu1 Cu1 83.05(12) 19_565 19_565
O2 Cu1 Cu1 83.05(12) 6 19_565
O1 Cu1 Cu1 85.44(11) . 19_565
O1 Cu1 Cu1 85.44(11) 24_565 19_565
O3 Cu1 Cu1 174.0(3) . 19_565
C1 O1 Cu1 121.0(4) . .
C1 O2 Cu1 124.5(4) . 19_565
O1 C1 O2 125.9(5) . .
O1 C1 C2 116.7(5) . .
O2 C1 C2 117.4(5) . .
C3 C2 C4 119.9(6) . .
C3 C2 C1 120.4(5) . .
C4 C2 C1 119.4(5) . .
C2 C3 C2 120.2(7) 23 .
C5 C4 C2 120.5(6) . .
C4 C5 C4 119.0(8) 23 .
C4 C5 C6 120.4(4) 23 .
C4 C5 C6 120.4(4) . .
N1' C6 C7' 0.0(17) 23 23
N1' C6 C7' 96.2(19) 23 .
C7' C6 C7' 96.2(19) 23 .
N1' C6 N1 54.8(11) 23 23
C7' C6 N1 54.8(11) 23 23
C7' C6 N1 121.0(11) . 23
N1' C6 C7 54.8(11) 23 23
C7' C6 C7 54.8(11) 23 23
C7' C6 C7 121.0(11) . 23
N1 C6 C7 0.0(15) 23 23
N1' C6 C7 121.0(11) 23 .
C7' C6 C7 121.0(11) 23 .
C7' C6 C7 54.8(11) . .
N1 C6 C7 94.2(17) 23 .
C7 C6 C7 94.2(17) 23 .
N1' C6 C5 119.9(10) 23 .
C7' C6 C5 119.9(10) 23 .
C7' C6 C5 119.9(9) . .
N1 C6 C5 119.1(8) 23 .
C7 C6 C5 119.1(8) 23 .
C7 C6 C5 119.1(8) . .
C7' C7 C6 62.0(13) . .
C7' C7 N1' 93(2) . 17_554
C6 C7 N1' 121.1(15) . 17_554
C7' C7 C7' 93(2) . 17_554
C6 C7 C7' 121.1(15) . 17_554
N1' C7 C7' 0.0(5) 17_554 17_554
C7' C7 C7 50.1(13) . 17_554
C6 C7 C7 94.2(15) . 17_554
N1' C7 C7 42.7(11) 17_554 17_554
C7' C7 C7 42.7(11) 17_554 17_554
C7' C7 N1 50.1(13) . 17_554
C6 C7 N1 94.2(15) . 17_554
N1' C7 N1 42.7(11) 17_554 17_554
C7' C7 N1 42.7(11) 17_554 17_554
C7 C7 N1 0.0(13) 17_554 17_554
C7' C7 C7 90.3(12) . 23
C6 C7 C7 42.9(9) . 23
N1' C7 C7 90.2(10) 17_554 23
C7' C7 C7 90.2(10) 17_554 23
C7 C7 C7 89.996(2) 17_554 23
N1 C7 C7 89.996(2) 17_554 23
C7 C7' C6 63.1(14) . .
C7 C7' N1 87(2) . 17_554
C6 C7' N1 118.0(17) . 17_554
C7 C7' C7 87(2) . 17_554
C6 C7' C7 118.0(17) . 17_554
N1 C7' C7 0.0(18) 17_554 17_554
C7 C7' N1' 46.9(13) . 17_554
C6 C7' N1' 93.2(17) . 17_554
N1 C7' N1' 40.2(10) 17_554 17_554
C7 C7' N1' 40.2(10) 17_554 17_554
C7 C7' C7' 46.9(13) . 17_554
C6 C7' C7' 93.2(17) . 17_554
N1 C7' C7' 40.2(10) 17_554 17_554
C7 C7' C7' 40.2(10) 17_554 17_554
N1' C7' C7' 0.0(13) 17_554 17_554
C7 C7' C7' 89.7(12) . 23
C6 C7' C7' 41.9(9) . 23
N1 C7' C7' 89.8(10) 17_554 23
C7 C7' C7' 89.8(10) 17_554 23
N1' C7' C7' 89.997(2) 17_554 23
C7' C7' C7' 89.997(2) 17_554 23
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.936(4) 19_565
Cu1 O2 1.937(4) 6
Cu1 O1 1.965(4) .
Cu1 O1 1.965(4) 24_565
Cu1 O3 2.137(6) .
Cu1 Cu1 2.6531(17) 19_565
O1 C1 1.255(7) .
O2 C1 1.287(7) .
O2 Cu1 1.937(4) 19_565
C1 C2 1.508(8) .
C2 C3 1.384(7) .
C2 C4 1.402(8) .
C3 C2 1.384(7) 23
C4 C5 1.393(7) .
C5 C4 1.393(7) 23
C5 C6 1.485(13) .
C6 N1' 1.351(18) 23
C6 C7' 1.351(18) 23
C6 C7' 1.351(18) .
C6 N1 1.364(19) 23
C6 C7 1.364(19) 23
C6 C7 1.364(19) .
C7 C7' 1.25(3) .
C7 N1' 1.414(17) 17_554
C7 C7' 1.414(17) 17_554
C7 C7 1.84(3) 17_554
C7 N1 1.84(3) 17_554
C7 C7 2.00(4) 23
C7' N1 1.414(17) 17_554
C7' C7 1.414(17) 17_554
C7' N1' 1.93(4) 17_554
C7' C7' 1.93(4) 17_554
C7' C7' 2.01(3) 23
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 -0.049 -0.033 -0.002 8241 1447 ' '
