#------------------------------------------------------------------------------
#$Date: 2019-08-27 03:06:54 +0300 (Tue, 27 Aug 2019) $
#$Revision: 217731 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/40/7124063.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_7124063
loop_
_publ_author_name
'Shao, Kai'
'Pei, Jiyan'
'Wang, Jia-Xin'
'Yu, Yang'
'Cui, Yuanjing'
'Zhou, Wei'
'Yildirim, Taner'
'Li, Bin'
'Chen, Banglin'
'Qian, Guodong'
_publ_section_title
;
 Tailoring pore geometry and chemistry in microporous metal--organic
 frameworks for high methane storage working capacity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06239D
_journal_year                    2019
_chemical_formula_sum            'C36 H18 Cu2 N0 O10'
_chemical_formula_weight         737.58
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-07-26 deposited with the CCDC.    2019-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   18.6721(4)
_cell_length_b                   18.6721(4)
_cell_length_c                   52.020(2)
_cell_measurement_reflns_used    45987
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.863
_cell_measurement_theta_min      2.368
_cell_volume                     15706.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            18970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.863
_diffrn_reflns_theta_min         1.319
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.637
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    0.702
_exptl_crystal_description       Bloc
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00013(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3701
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1324P)²+24.8917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2863
_reflns_number_total             3701
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc06239d2.cif
_cod_data_source_block           z_sq
_cod_original_cell_volume        15706.8(10)
_cod_database_code               7124063
_shelx_shelxl_version_number     2016/6
_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'
'-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_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 0.85669(2) 0.14331(2) 0.14571(2) 0.0556(3) Uani 1 2 d S T P . .
O1 O 0.92268(19) 0.2249(2) 0.19937(5) 0.0814(8) Uani 1 1 d . . . . .
O2 O 0.96161(16) 0.18450(17) 0.16411(4) 0.0718(7) Uani 1 1 d . . . . .
O3 O 0.89290(19) 0.10710(19) 0.11108(10) 0.143(2) Uani 1 2 d S T P . .
C1 C 0.9723(2) 0.2125(2) 0.18673(6) 0.0643(9) Uani 1 1 d . . . . .
C2 C 1.11009(17) 0.2202(3) 0.18697(8) 0.0617(12) Uani 1 2 d S T P . .
H2A H 1.101525 0.203047 0.169905 0.074 Uiso 1 2 calc R U P . .
C3 C 1.0519(3) 0.2326(3) 0.19940(6) 0.0696(10) Uani 1 1 d . . . . .
C4 C 1.0656(3) 0.2581(3) 0.22506(7) 0.0954(15) Uani 1 1 d . . . . .
H4A H 1.026322 0.265887 0.233677 0.114 Uiso 1 1 calc R U . . .
C5 C 1.1360(3) 0.2720(6) 0.23789(12) 0.118(3) Uani 1 2 d DS T P . .
C6 C 1.1488(17) 0.2981(11) 0.26551(16) 0.207(4) Uani 0.5 1 d D U P A -1
C7 C 1.1665(9) 0.2527(10) 0.28252(14) 0.208(4) Uani 0.5 1 d D U P A -1
H7A H 1.171173 0.208137 0.276663 0.249 Uiso 0.5 1 calc R U P A -1
C8 C 1.1773(10) 0.2734(10) 0.30861(16) 0.216(4) Uani 0.5 1 d D U P A -1
H8A H 1.192709 0.244772 0.319862 0.259 Uiso 0.5 1 calc R U P A -1
C9 C 1.165(2) 0.3357(13) 0.31778(16) 0.223(4) Uani 0.5 1 d D U P A -1
C10 C 1.1681(12) 0.3939(9) 0.30013(18) 0.243(5) Uani 0.5 1 d D U P A -1
C11 C 1.1613(11) 0.3755(9) 0.27396(18) 0.238(5) Uani 0.5 1 d D U P A -1
C12 C 1.1570(15) 0.4310(10) 0.2568(2) 0.274(6) Uani 0.5 1 d D U P A -1
H12A H 1.131376 0.412609 0.240875 0.329 Uiso 0.5 1 calc R U P A -1
C13 C 1.1915(16) 0.5146(10) 0.2636(3) 0.297(6) Uani 0.5 1 d D U P A -1
H13A H 1.215393 0.556641 0.251461 0.357 Uiso 0.5 1 calc R U P A -1
C14 C 1.1883(17) 0.5310(10) 0.2893(3) 0.295(6) Uani 0.5 1 d D U P A -1
H14A H 1.191018 0.579982 0.294413 0.354 Uiso 0.5 1 calc R U P A -1
C15 C 1.1808(15) 0.4722(10) 0.3075(3) 0.277(6) Uani 0.5 1 d D U P A -1
H15A H 1.184191 0.485080 0.324909 0.332 Uiso 0.5 1 calc R U P A -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 88.26(16) . 22_665
O2 Cu1 O1 167.87(10) . 25_655
O2 Cu1 O1 90.04(13) 22_665 25_655
O2 Cu1 O1 90.04(13) . 10_545
O2 Cu1 O1 167.87(10) 22_665 10_545
O1 Cu1 O1 89.12(19) 25_655 10_545
O2 Cu1 O3 97.06(15) . .
O2 Cu1 O3 97.06(15) 22_665 .
O1 Cu1 O3 95.07(15) 25_655 .
O1 Cu1 O3 95.07(15) 10_545 .
O2 Cu1 Cu1 84.15(7) . 25_655
O2 Cu1 Cu1 84.15(7) 22_665 25_655
O1 Cu1 Cu1 83.73(7) 25_655 25_655
O1 Cu1 Cu1 83.73(7) 10_545 25_655
O3 Cu1 Cu1 178.30(19) . 25_655
C1 O1 Cu1 123.1(2) . 25_655
C1 O2 Cu1 122.5(2) . .
O1 C1 O2 126.1(3) . .
O1 C1 C3 117.3(3) . .
O2 C1 C3 116.6(3) . .
C3 C2 C3 121.2(4) . 23_755
C2 C3 C4 118.7(3) . .
C2 C3 C1 121.3(3) . .
C4 C3 C1 119.8(3) . .
C5 C4 C3 121.4(4) . .
C4 C5 C4 118.6(5) 23_755 .
C4 C5 C6 120.9(9) 23_755 .
C4 C5 C6 120.5(9) . .
C7 C6 C11 117.6(8) . .
C7 C6 C5 117.7(7) . .
C11 C6 C5 123.3(8) . .
C6 C7 C8 120.0(8) . .
C9 C8 C7 120.6(8) . .
C8 C9 C10 118.1(10) . .
C11 C10 C9 118.9(8) . .
C11 C10 C15 118.0(8) . .
C9 C10 C15 123.1(8) . .
C10 C11 C12 118.2(8) . .
C10 C11 C6 120.3(8) . .
C12 C11 C6 121.1(8) . .
C11 C12 C13 119.7(11) . .
C14 C13 C12 116.5(12) . .
C13 C14 C15 118.6(11) . .
C14 C15 C10 121.6(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.959(2) .
Cu1 O2 1.959(2) 22_665
Cu1 O1 1.964(3) 25_655
Cu1 O1 1.964(3) 10_545
Cu1 O3 2.149(4) .
Cu1 Cu1 2.6525(9) 25_655
O1 C1 1.248(4) .
O2 C1 1.263(4) .
C1 C3 1.492(5) .
C2 C3 1.380(4) .
C2 C3 1.381(4) 23_755
C3 C4 1.397(5) .
C4 C5 1.379(5) .
C5 C6 1.498(8) .
C6 C7 1.376(8) .
C6 C11 1.413(8) .
C7 C8 1.398(8) .
C8 C9 1.373(9) .
C9 C10 1.405(8) .
C10 C11 1.394(8) .
C10 C15 1.412(8) .
C11 C12 1.402(8) .
C12 C13 1.403(9) .
C13 C14 1.378(9) .
C14 C15 1.404(9) .
