#------------------------------------------------------------------------------
#$Date: 2019-11-23 08:27:46 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232558 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/78/4347879.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_4347879
loop_
_publ_author_name
'Wen, Hui-Min'
'Wang, Huizhen'
'Li, Bin'
'Cui, Yuanjing'
'Wang, Hailong'
'Qian, Guodong'
'Chen, Banglin'
_publ_section_title
;
 A Microporous Metal-Organic Framework with Lewis Basic Nitrogen Sites for
 High C2H2 Storage and Significantly Enhanced C2H2/CO2 Separation at
 Ambient Conditions.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7214
_journal_page_last               7218
_journal_paper_doi               10.1021/acs.inorgchem.6b00748
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C20 H16 Cu2 N2 O10'
_chemical_formula_weight         571.43
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_symmetry_cell_setting           trigonal
_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            9
_cell_length_a                   18.5944(6)
_cell_length_b                   18.5944(6)
_cell_length_c                   38.0120(14)
_cell_measurement_reflns_used    3561
_cell_measurement_temperature    99.98(14)
_cell_measurement_theta_max      72.2850
_cell_measurement_theta_min      3.5950
_cell_volume                     11381.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      99.98(14)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            9153
_diffrn_reflns_theta_full        72.98
_diffrn_reflns_theta_max         72.98
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54935
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.855
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2745
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.147
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1051P)²+100.1278P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2126
_reflns_number_gt                2130
_reflns_number_total             2745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00748_si_002.cif
_cod_data_source_block           platon
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4347879
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -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'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+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'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, 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'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+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'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+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
C1 C 0.5129(3) 0.4871(3) 0.53412(17) 0.072(2) Uani 1 2 d SD
C2 C 0.5264(3) 0.4736(3) 0.57055(18) 0.0641(19) Uani 1 2 d S
C3 C 0.4698(3) 0.4014(3) 0.58794(12) 0.0601(13) Uani 1 1 d .
H3 H 0.4216 0.3628 0.5765 0.072 Uiso 1 1 calc R
C4 C 0.4845(3) 0.3863(3) 0.62218(11) 0.0522(11) Uani 1 1 d .
C5 C 0.5562(2) 0.4438(2) 0.63927(15) 0.0505(14) Uani 1 2 d S
H5 H 0.5657 0.4343 0.6624 0.061 Uiso 1 2 calc SR
C6 C 0.4256(2) 0.3056(3) 0.63963(10) 0.0475(10) Uani 1 1 d .
C7 C 0.5489(8) 0.5672(4) 0.5220(2) 0.066(3) Uani 0.50 1 d PDU
H7 H 0.5790 0.6122 0.5369 0.080 Uiso 0.50 1 calc PR
Cu1 Cu 0.38082(4) 0.19041(2) 0.695394(18) 0.0373(3) Uani 1 2 d S
N1 N 0.5785(5) 0.5387(7) 0.5130(2) 0.076(3) Uani 0.50 1 d PDU
O1 O 0.44424(18) 0.29552(19) 0.67035(7) 0.0525(8) Uani 1 1 d .
O2 O 0.36460(18) 0.2557(2) 0.62219(8) 0.0575(8) Uani 1 1 d .
O3 O 0.4473(4) 0.2237(2) 0.74409(15) 0.098(2) Uani 1 2 d SD
H3A H 0.4629 0.2220 0.7649 0.147 Uiso 0.50 1 d PRD
H3B H 0.4785 0.2722 0.7361 0.147 Uiso 0.50 1 d PRD
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'
Cu Cu -1.9646 0.5888 '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'
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
N1 C1 N1 105.1(9) 24_665 .
N1 C1 C7 42.6(6) 24_665 24_665
N1 C1 C7 120.9(6) . 24_665
N1 C1 C7 120.9(6) 24_665 .
N1 C1 C7 42.6(6) . .
C7 C1 C7 103.8(11) 24_665 .
N1 C1 C2 120.7(5) 24_665 .
N1 C1 C2 120.6(5) . .
C7 C1 C2 118.3(6) 24_665 .
C7 C1 C2 118.3(6) . .
C3 C2 C3 118.9(6) 24_665 .
C3 C2 C1 120.5(3) 24_665 .
C3 C2 C1 120.5(3) . .
C2 C3 C4 120.7(4) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C5 C4 C3 119.6(4) . .
C5 C4 C6 120.3(4) . .
C3 C4 C6 119.9(4) . .
C4 C5 C4 120.4(6) . 24_665
C4 C5 H5 119.8 . .
C4 C5 H5 119.8 24_665 .
O2 C6 O1 127.0(4) . .
O2 C6 C4 116.7(4) . .
O1 C6 C4 116.2(4) . .
C1 C7 N1 117.3(8) . 6_556
C1 C7 C7 98.2(9) . 6_556
N1 C7 C7 34.0(6) 6_556 6_556
C1 C7 H7 121.3 . .
N1 C7 H7 121.3 6_556 .
C7 C7 H7 131.4 6_556 .
O1 Cu1 O1 88.7(2) 23 .
O1 Cu1 O2 90.04(15) 23 25_556
O1 Cu1 O2 167.34(12) . 25_556
O1 Cu1 O2 167.34(12) 23 11_556
O1 Cu1 O2 90.04(15) . 11_556
O2 Cu1 O2 88.4(2) 25_556 11_556
O1 Cu1 O3 99.20(17) 23 .
O1 Cu1 O3 99.21(17) . .
O2 Cu1 O3 93.42(17) 25_556 .
O2 Cu1 O3 93.44(17) 11_556 .
O1 Cu1 Cu1 84.30(9) 23 25_556
O1 Cu1 Cu1 84.30(9) . 25_556
O2 Cu1 Cu1 83.04(9) 25_556 25_556
O2 Cu1 Cu1 83.04(9) 11_556 25_556
O3 Cu1 Cu1 175.1(2) . 25_556
C1 N1 C7 121.4(7) . 6_556
C1 N1 N1 103.2(9) . 6_556
C7 N1 N1 37.8(6) 6_556 6_556
C6 O1 Cu1 121.9(3) . .
C6 O2 Cu1 123.6(3) . 25_556
Cu1 O3 H3A 162.8 . .
Cu1 O3 H3B 89.2 . .
H3A O3 H3B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.372(6) 24_665
C1 N1 1.372(6) .
C1 C7 1.372(6) 24_665
C1 C7 1.372(6) .
C1 C2 1.452(9) .
C2 C3 1.390(6) 24_665
C2 C3 1.391(6) .
C3 C4 1.387(6) .
C3 H3 0.9300 .
C4 C5 1.384(5) .
C4 C6 1.499(6) .
C5 C4 1.384(5) 24_665
C5 H5 0.9300 .
C6 O2 1.239(5) .
C6 O1 1.258(5) .
C7 N1 1.375(6) 6_556
C7 C7 1.78(2) 6_556
C7 H7 0.9300 .
Cu1 O1 1.952(3) 23
Cu1 O1 1.952(3) .
Cu1 O2 1.957(3) 25_556
Cu1 O2 1.957(3) 11_556
Cu1 O3 2.139(5) .
Cu1 Cu1 2.6662(14) 25_556
N1 C7 1.375(6) 6_556
N1 N1 1.62(2) 6_556
O2 Cu1 1.957(3) 25_556
O3 H3A 0.8483 .
O3 H3B 0.8483 .
