#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:27:15 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234854 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/95/4349524.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_4349524
loop_
_publ_author_name
'Liu, Bo'
'Zhou, Hui-Fang'
'Hou, Lei'
'Zhu, Zhonghua'
'Wang, Yao-Yu'
_publ_section_title
;
 A chiral metal--organic framework with polar channels: unique
 interweaving six-fold helices and high CO2/CH4 separation
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1326
_journal_paper_doi               10.1039/C6QI00282J
_journal_volume                  3
_journal_year                    2016
_chemical_formula_sum            'C25 H25 Cu N3 O8'
_chemical_formula_weight         559.02
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-07-08 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.4258(16)
_cell_length_b                   22.4258(16)
_cell_length_c                   10.9190(15)
_cell_measurement_reflns_used    7478
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.60
_cell_volume                     4755.6(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25299
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.9304
_exptl_absorpt_correction_T_min  0.8857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1734
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6211
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0803
_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)+(0.1668P)²+3.0415P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2286
_reflns_number_gt                5382
_reflns_number_total             6211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00282j2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P3121
_cod_database_code               4349524
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'-x, -x+y, -z+1/3'
'x-y, -y, -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
Cu1 Cu 0.33696(4) 0.0000 0.3333 0.0347(2) Uani 1 2 d S
Cu2 Cu 0.33679(4) 0.33679(4) 0.0000 0.0368(2) Uani 1 2 d S
C1 C 0.4427(3) 0.3260(3) 0.0799(6) 0.0442(13) Uani 1 1 d .
C2 C 0.4808(3) 0.2899(3) 0.1231(6) 0.0471(13) Uani 1 1 d .
C3 C 0.4441(3) 0.2225(3) 0.1638(5) 0.0402(10) Uani 1 1 d .
H3 H 0.3962 0.1993 0.1669 0.048 Uiso 1 1 calc R
C4 C 0.4816(3) 0.1894(3) 0.2011(5) 0.0469(13) Uani 1 1 d .
C5 C 0.5505(4) 0.2221(4) 0.1851(9) 0.071(2) Uani 1 1 d .
H5 H 0.5741 0.1995 0.2079 0.085 Uiso 1 1 calc R
C6 C 0.5859(5) 0.2849(6) 0.1384(11) 0.089(3) Uani 1 1 d .
C7 C 0.5515(4) 0.3230(4) 0.1125(9) 0.067(2) Uani 1 1 d .
H7 H 0.5763 0.3690 0.0891 0.081 Uiso 1 1 calc R
C8 C 0.4408(3) 0.1169(3) 0.2461(6) 0.0456(13) Uani 1 1 d .
C9 C 0.6629(4) 0.3215(5) 0.1110(6) 0.068(2) Uani 1 1 d .
C10 C 0.7069(4) 0.3915(5) 0.1125(8) 0.074(2) Uani 1 1 d .
H10 H 0.6883 0.4199 0.1246 0.089 Uiso 1 1 calc R
C11 C 0.7715(5) 0.4194(5) 0.0983(10) 0.086(3) Uani 1 1 d .
H11 H 0.7988 0.4672 0.0986 0.103 Uiso 1 1 calc R
C12 C 0.8019(5) 0.3780(5) 0.0819(9) 0.081(2) Uani 1 1 d .
H12 H 0.8493 0.3970 0.0746 0.097 Uiso 1 1 calc R
C13 C 0.7576(4) 0.3078(5) 0.0774(8) 0.070(2) Uani 1 1 d .
C14 C 0.7825(4) 0.2585(5) 0.0500(8) 0.072(2) Uani 1 1 d .
C15 C 0.7538(5) 0.1944(5) 0.1054(11) 0.092(3) Uani 1 1 d .
H15 H 0.7187 0.1820 0.1624 0.111 Uiso 1 1 calc R
C16 C 0.7766(4) 0.1477(4) 0.0774(7) 0.0615(19) Uani 1 1 d .
C17 C 0.8340(4) 0.1679(4) 0.0006(6) 0.0553(14) Uani 1 1 d .
H17 H 0.8537 0.1402 -0.0076 0.066 Uiso 1 1 calc R
C18 C 0.8603(4) 0.2286(4) -0.0618(7) 0.0646(19) Uani 1 1 d U
C19 C 0.8363(5) 0.2769(5) -0.0306(9) 0.078(2) Uani 1 1 d U
H19 H 0.8577 0.3205 -0.0658 0.094 Uiso 1 1 calc R
C20 C 0.7482(4) 0.0813(4) 0.1494(7) 0.0567(17) Uani 1 1 d .
C21 C 0.9194(4) 0.2515(4) -0.1481(7) 0.0547(16) Uani 1 1 d .
O8 O 0.9493(2) 0.3152(3) -0.1802(4) 0.0577(11) Uani 1 1 d .
N1 N 0.6893(3) 0.2789(4) 0.0978(6) 0.0660(17) Uani 1 1 d .
O1 O 0.3759(2) 0.2896(3) 0.0870(4) 0.0533(11) Uani 1 1 d .
O2 O 0.4723(3) 0.3845(3) 0.0427(6) 0.0803(18) Uani 1 1 d .
O3 O 0.3760(2) 0.0887(2) 0.2465(5) 0.0534(10) Uani 1 1 d .
O4 O 0.4714(3) 0.0860(3) 0.2819(6) 0.0759(17) Uani 1 1 d .
O5 O 0.6870(3) 0.0535(2) 0.1832(4) 0.0622(12) Uani 1 1 d .
O6 O 0.7867(4) 0.0585(4) 0.1802(7) 0.098(2) Uani 1 1 d .
O7 O 0.9352(4) 0.2084(4) -0.1818(7) 0.097(2) Uani 1 1 d .
N2 N 0.5398(8) 0.0342(8) 0.1487(14) 0.155(5) Uani 1 1 d DU
H2A H 0.5339 0.0609 0.2031 0.186 Uiso 1 1 calc R
H2B H 0.5684 0.0214 0.1820 0.186 Uiso 1 1 calc R
C22 C 0.4697(9) -0.0303(8) 0.1203(17) 0.168(6) Uani 1 1 d DU
H22A H 0.4546 -0.0602 0.1902 0.253 Uiso 1 1 calc R
H22B H 0.4745 -0.0541 0.0514 0.253 Uiso 1 1 calc R
H22C H 0.4364 -0.0166 0.1016 0.253 Uiso 1 1 calc R
C23 C 0.5710(11) 0.0742(13) 0.033(2) 0.235(10) Uani 1 1 d DU
H23A H 0.6150 0.1135 0.0517 0.352 Uiso 1 1 calc R
H23B H 0.5412 0.0892 -0.0003 0.352 Uiso 1 1 calc R
H23C H 0.5768 0.0454 -0.0248 0.352 Uiso 1 1 calc R
C24 C 0.9240(12) 0.1628(9) 0.5520(19) 0.196(9) Uani 1 1 d DU
H24A H 0.9674 0.2050 0.5524 0.294 Uiso 1 1 calc R
H24B H 0.9279 0.1284 0.5980 0.294 Uiso 1 1 calc R
H24C H 0.8895 0.1706 0.5884 0.294 Uiso 1 1 calc R
C25 C 0.8383(11) 0.0657(10) 0.427(2) 0.205(9) Uani 1 1 d DU
H25A H 0.8229 0.0513 0.3442 0.308 Uiso 1 1 calc R
H25B H 0.8026 0.0673 0.4724 0.308 Uiso 1 1 calc R
H25C H 0.8490 0.0335 0.4643 0.308 Uiso 1 1 calc R
N3 N 0.9044(13) 0.1391(10) 0.425(2) 0.255(9) Uani 1 1 d DU
H3A H 0.9390 0.1372 0.3871 0.306 Uiso 1 1 calc R
H3B H 0.8957 0.1687 0.3837 0.306 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 0.0033 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'
Cu Cu 0.3201 1.2651 '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'
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
O8 Cu1 O8 175.3(3) 4_545 3_665
O8 Cu1 O3 91.8(2) 4_545 .
O8 Cu1 O3 88.5(2) 3_665 .
O8 Cu1 O3 88.5(2) 4_545 6
O8 Cu1 O3 91.8(2) 3_665 6
O3 Cu1 O3 173.1(3) . 6
O1 Cu2 O1 174.6(3) 4 .
O1 Cu2 O5 92.9(2) 4 3_664
O1 Cu2 O5 87.3(2) . 3_664
O1 Cu2 O5 87.3(2) 4 5_665
O1 Cu2 O5 92.9(2) . 5_665
O5 Cu2 O5 176.0(4) 3_664 5_665
O2 C1 O1 122.4(6) . .
O2 C1 C2 122.3(6) . .
O1 C1 C2 115.2(5) . .
C7 C2 C3 120.8(5) . .
C7 C2 C1 119.3(5) . .
C3 C2 C1 119.7(5) . .
C2 C3 C4 118.3(5) . .
C2 C3 H3 120.9 . .
C4 C3 H3 120.9 . .
C5 C4 C3 119.5(6) . .
C5 C4 C8 122.9(5) . .
C3 C4 C8 117.3(5) . .
C6 C5 C4 122.7(7) . .
C6 C5 H5 118.6 . .
C4 C5 H5 118.6 . .
C5 C6 C7 119.6(8) . .
C5 C6 C9 124.3(8) . .
C7 C6 C9 116.2(9) . .
C2 C7 C6 118.5(7) . .
C2 C7 H7 120.7 . .
C6 C7 H7 120.7 . .
O4 C8 O3 122.1(6) . .
O4 C8 C4 119.8(6) . .
O3 C8 C4 118.1(5) . .
N1 C9 C10 119.1(8) . .
N1 C9 C6 114.6(8) . .
C10 C9 C6 125.9(9) . .
C11 C10 C9 123.7(10) . .
C11 C10 H10 118.2 . .
C9 C10 H10 118.2 . .
C10 C11 C12 119.9(10) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C13 C12 C11 116.5(9) . .
C13 C12 H12 121.7 . .
C11 C12 H12 121.7 . .
N1 C13 C12 122.6(8) . .
N1 C13 C14 115.6(7) . .
C12 C13 C14 121.8(8) . .
C19 C14 C15 118.2(8) . .
C19 C14 C13 120.0(8) . .
C15 C14 C13 121.8(7) . .
C14 C15 C16 121.5(8) . .
C14 C15 H15 119.2 . .
C16 C15 H15 119.2 . .
C17 C16 C15 120.2(6) . .
C17 C16 C20 119.6(6) . .
C15 C16 C20 119.2(6) . .
C18 C17 C16 119.2(6) . .
C18 C17 H17 120.4 . .
C16 C17 H17 120.4 . .
C17 C18 C19 119.0(6) . .
C17 C18 C21 121.6(7) . .
C19 C18 C21 118.8(6) . .
C14 C19 C18 121.0(7) . .
C14 C19 H19 119.5 . .
C18 C19 H19 119.5 . .
O5 C20 O6 122.0(6) . .
O5 C20 C16 117.5(6) . .
O6 C20 C16 120.2(7) . .
O7 C21 O8 126.2(6) . .
O7 C21 C18 118.1(7) . .
O8 C21 C18 115.7(6) . .
C21 O8 Cu1 115.4(4) . 2_654
C13 N1 C9 118.0(7) . .
C1 O1 Cu2 108.8(4) . .
C8 O3 Cu1 109.1(4) . .
C20 O5 Cu2 116.9(5) . 2_655
C23 N2 C22 110.1(12) . .
C23 N2 H2A 109.6 . .
C22 N2 H2A 109.6 . .
C23 N2 H2B 109.6 . .
C22 N2 H2B 109.6 . .
H2A N2 H2B 108.2 . .
N2 C22 H22A 109.5 . .
N2 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
N2 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
N2 C23 H23A 109.5 . .
N2 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
N2 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N3 C24 H24A 109.5 . .
N3 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
N3 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
N3 C25 H25A 109.5 . .
N3 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
N3 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 N3 C25 108.9(16) . .
C24 N3 H3A 109.9 . .
C25 N3 H3A 109.9 . .
C24 N3 H3B 109.9 . .
C25 N3 H3B 109.9 . .
H3A N3 H3B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O8 1.942(4) 4_545
Cu1 O8 1.942(4) 3_665
Cu1 O3 1.970(4) .
Cu1 O3 1.970(4) 6
Cu2 O1 1.930(4) 4
Cu2 O1 1.930(4) .
Cu2 O5 1.942(4) 3_664
Cu2 O5 1.942(4) 5_665
C1 O2 1.208(8) .
C1 O1 1.301(8) .
C1 C2 1.517(8) .
C2 C7 1.378(10) .
C2 C3 1.384(8) .
C3 C4 1.431(8) .
C3 H3 0.9300 .
C4 C5 1.350(11) .
C4 C8 1.495(9) .
C5 C6 1.326(13) .
C5 H5 0.9300 .
C6 C7 1.438(12) .
C6 C9 1.525(12) .
C7 H7 0.9300 .
C8 O4 1.256(8) .
C8 O3 1.262(8) .
C9 N1 1.361(12) .
C9 C10 1.373(13) .
C10 C11 1.268(13) .
C10 H10 0.9300 .
C11 C12 1.413(14) .
C11 H11 0.9300 .
C12 C13 1.380(13) .
C12 H12 0.9300 .
C13 N1 1.350(11) .
C13 C14 1.497(13) .
C14 C19 1.379(12) .
C14 C15 1.385(12) .
C15 C16 1.410(12) .
C15 H15 0.9300 .
C16 C17 1.407(9) .
C16 C20 1.515(9) .
C17 C18 1.365(10) .
C17 H17 0.9300 .
C18 C19 1.468(13) .
C18 C21 1.494(9) .
C19 H19 0.9300 .
C20 O5 1.246(9) .
C20 O6 1.249(10) .
C21 O7 1.239(10) .
C21 O8 1.286(9) .
O8 Cu1 1.942(4) 2_654
O5 Cu2 1.942(4) 2_655
N2 C23 1.499(19) .
N2 C22 1.545(16) .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 N3 1.47(2) .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 N3 1.571(19) .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
N3 H3A 0.9000 .
N3 H3B 0.9000 .
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 0.000 0.000 -0.052 1425 281 ' '
