#------------------------------------------------------------------------------
#$Date: 2017-02-04 15:25:49 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191487 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/92/7119275.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_7119275
loop_
_publ_author_name
'Song, Bai-Qiao'
'Chen, Da-Qin'
'Ji, Zhenguo'
'Tang, Junhong'
'Wang, Xin-Long'
'Zang, Hong-Ying'
'Su, Zhong-Min'
_publ_section_title
;
 Control of bulk homochirality and proton conductivity in isostructural
 chiral metal-organic frameworks.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1892
_journal_page_last               1895
_journal_paper_doi               10.1039/c6cc07729c
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C24 H48 Cu4 N10 O6'
_chemical_formula_weight         826.88
_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_Hall           'P 6c 2c'
_space_group_name_H-M_alt        'P 63 2 2'
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   19.603(5)
_cell_length_b                   19.603(5)
_cell_length_c                   13.939(5)
_cell_measurement_reflns_used    3637
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.988
_cell_measurement_theta_min      4.797
_cell_volume                     4639(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Diamond (Brandenburg and Putz, 2008)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26376
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.764
_diffrn_reflns_theta_max         24.764
_diffrn_reflns_theta_min         1.890
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.847
_exptl_absorpt_correction_T_max  0.7325
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2670
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0819P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.673
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1914
_reflns_number_total             2670
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc07729c2.cif
_cod_data_source_block           1P
_cod_depositor_comments
'Adding full bibliography for 7119274--7119277.cif.'
_cod_original_cell_volume        4639(3)
_cod_database_code               7119275
_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.
;
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.732
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z+1/2'
'x, x-y, -z+1/2'
'-x+y, y, -z+1/2'
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
Cu1 Cu 0.666667 0.333333 0.60138(9) 0.0599(4) Uani 1 3 d S T P
Cu2 Cu 0.73834(3) 0.26166(3) 0.750000 0.0625(4) Uani 1 2 d S T P
Cu3 Cu 1.000000 0.45958(9) 0.500000 0.0936(6) Uani 1 2 d S T P
N2 N 0.8075(3) 0.3328(4) 0.6611(4) 0.0624(15) Uani 1 1 d . . .
N1 N 0.7796(3) 0.3703(3) 0.6010(4) 0.0649(17) Uani 1 1 d . . .
N3 N 0.9033(4) 0.4090(4) 0.5641(5) 0.0783(18) Uani 1 1 d . . .
C1 C 0.8377(4) 0.4157(7) 0.5443(5) 0.079(2) Uani 1 1 d . . .
C2 C 0.8816(5) 0.3567(5) 0.6366(5) 0.073(2) Uani 1 1 d . . .
C3 C 0.9295(5) 0.3339(7) 0.6885(8) 0.121(4) Uani 1 1 d D U .
H3 H 0.894626 0.295523 0.736116 0.145 Uiso 1 1 calc R U .
C4 C 0.8232(7) 0.4649(6) 0.4730(5) 0.146(5) Uani 1 1 d D U .
H4 H 0.769656 0.455807 0.481890 0.175 Uiso 1 1 calc R U .
C5 C 0.8318(8) 0.4428(7) 0.3711(7) 0.175(6) Uani 1 1 d D U .
H5A H 0.796883 0.387416 0.361658 0.263 Uiso 1 1 calc R U .
H5B H 0.818795 0.471969 0.326677 0.263 Uiso 1 1 calc R U .
H5C H 0.885142 0.455053 0.360690 0.263 Uiso 1 1 calc R U .
C8 C 1.0016(8) 0.3934(7) 0.7440(10) 0.213(6) Uani 1 1 d D U .
H8A H 1.026150 0.367130 0.774042 0.320 Uiso 1 1 calc R U .
H8B H 1.038232 0.432919 0.700750 0.320 Uiso 1 1 calc R U .
H8C H 0.985979 0.417890 0.792155 0.320 Uiso 1 1 calc R U .
C6 C 0.8812(8) 0.5528(6) 0.4768(8) 0.173(5) Uani 1 1 d D U .
H6A H 0.879984 0.572558 0.539436 0.260 Uiso 1 1 calc R U .
H6B H 0.933287 0.562308 0.463666 0.260 Uiso 1 1 calc R U .
H6C H 0.866940 0.579224 0.429652 0.260 Uiso 1 1 calc R U .
C7 C 0.9609(7) 0.2909(8) 0.6283(10) 0.215(7) Uani 1 1 d D U .
H7A H 0.992518 0.277449 0.667790 0.323 Uiso 1 1 calc R U .
H7B H 0.917534 0.243800 0.602372 0.323 Uiso 1 1 calc R U .
H7C H 0.992350 0.324433 0.576866 0.323 Uiso 1 1 calc R U .
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'
N N 0.0061 0.0033 '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'
H H 0.0000 0.0000 '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
N1 Cu1 N1 119.998(2) . 4_665
N1 Cu1 N1 120.001(4) . 3_655
N1 Cu1 N1 119.999(3) 4_665 3_655
N2 Cu2 N2 177.9(4) . 10_666
N3 Cu3 N3 177.3(5) . 8_766
C2 N2 N1 107.9(6) . .
C2 N2 Cu2 134.2(6) . .
N1 N2 Cu2 117.8(4) . .
C1 N1 N2 106.6(6) . .
C1 N1 Cu1 134.0(5) . .
N2 N1 Cu1 118.3(4) . .
C2 N3 C1 105.5(6) . .
C2 N3 Cu3 127.7(6) . .
C1 N3 Cu3 126.7(5) . .
N1 C1 N3 110.4(8) . .
N1 C1 C4 117.2(8) . .
N3 C1 C4 132.4(7) . .
N2 C2 N3 109.5(7) . .
N2 C2 C3 122.4(8) . .
N3 C2 C3 127.8(8) . .
C2 C3 C8 121.6(10) . .
C2 C3 C7 114.0(10) . .
C8 C3 C7 103.18(13) . .
C2 C3 H3 105.6 . .
C8 C3 H3 105.6 . .
C7 C3 H3 105.6 . .
C5 C4 C6 103.25(13) . .
C5 C4 C1 110.5(9) . .
C6 C4 C1 115.4(10) . .
C5 C4 H4 109.1 . .
C6 C4 H4 109.1 . .
C1 C4 H4 109.1 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C3 C8 H8A 109.5 . .
C3 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C3 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C3 C7 H7A 109.5 . .
C3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C3 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.956(6) .
Cu1 N1 1.956(6) 4_665
Cu1 N1 1.956(6) 3_655
Cu2 N2 1.852(6) .
Cu2 N2 1.852(5) 10_666
Cu3 N3 1.870(6) .
Cu3 N3 1.870(6) 8_766
N2 C2 1.328(9) .
N2 N1 1.393(8) .
N1 C1 1.304(9) .
N3 C2 1.348(9) .
N3 C1 1.383(10) .
C1 C4 1.507(13) .
C2 C3 1.423(12) .
C3 C8 1.5193(14) .
C3 C7 1.5189(14) .
C3 H3 0.9800 .
C4 C5 1.5184(15) .
C4 C6 1.5190(14) .
C4 H4 0.9800 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C2 N2 N1 C1 -1.0(8)
Cu2 N2 N1 C1 -178.8(6)
C2 N2 N1 Cu1 168.5(5)
Cu2 N2 N1 Cu1 -9.3(7)
N2 N1 C1 N3 0.7(10)
Cu1 N1 C1 N3 -166.5(5)
N2 N1 C1 C4 -178.6(8)
Cu1 N1 C1 C4 14.3(14)
C2 N3 C1 N1 -0.1(11)
Cu3 N3 C1 N1 177.9(6)
C2 N3 C1 C4 179.0(10)
Cu3 N3 C1 C4 -3.0(16)
N1 N2 C2 N3 1.0(8)
Cu2 N2 C2 N3 178.2(5)
N1 N2 C2 C3 175.4(8)
Cu2 N2 C2 C3 -7.4(12)
C1 N3 C2 N2 -0.5(10)
Cu3 N3 C2 N2 -178.5(5)
C1 N3 C2 C3 -174.6(9)
Cu3 N3 C2 C3 7.4(13)
N2 C2 C3 C8 -113.9(11)
N3 C2 C3 C8 59.4(14)
N2 C2 C3 C7 121.5(10)
N3 C2 C3 C7 -65.2(13)
N1 C1 C4 C5 -118.3(10)
N3 C1 C4 C5 62.6(14)
N1 C1 C4 C6 125.0(10)
N3 C1 C4 C6 -54.1(15)
