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#$Date: 2017-09-15 02:03:24 +0300 (Fri, 15 Sep 2017) $
#$Revision: 200898 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/64/4126406.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_4126406
loop_
_publ_author_name
'Park, Sarah S.'
'Tulchinsky, Yuri'
'Dincă, Mircea'
_publ_section_title
;
 Single-Ion Li(+), Na(+), and Mg(2+) Solid Electrolytes Supported by a
 Mesoporous Anionic Cu-Azolate Metal-Organic Framework.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b06197
_journal_year                    2017
_chemical_formula_sum            'C4.5 H1.5 Cl0.75 Cu0.75 N2.25 O0.75'
_chemical_formula_weight         173.32
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            24
_cell_length_a                   38.819(4)
_cell_length_b                   38.819(4)
_cell_length_c                   7.7932(12)
_cell_measurement_reflns_used    660
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      34.29
_cell_measurement_theta_min      2.28
_cell_volume                     10170(2)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      373(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1983
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9731
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        37.333
_diffrn_reflns_theta_max         37.333
_diffrn_reflns_theta_min         2.276
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    2.314
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.5461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2034
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.699
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         622
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      0.589
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1821P)²+15.2817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                439
_reflns_number_total             622
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b06197_si_003.cif
_cod_data_source_block           MIT-20d
_cod_original_cell_volume        10170(3)
_cod_original_formula_sum        'C4.50 H1.50 Cl0.75 Cu0.75 N2.25 O0.75'
_cod_database_code               4126406
_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   0.802
_shelx_estimated_absorpt_t_max   0.995
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 0.666667 0.63467(5) 0.833333 0.0625(13) Uani 1 2 d S T P . .
Cl1 Cl 0.72512(10) 0.666667 0.666667 0.0940(19) Uani 1 2 d S T P A .
N1 N 0.6430(3) 0.6430(3) 0.500000 0.057(4) Uani 1 2 d DS TU P . .
N2A N 0.6295(12) 0.6177(10) 0.633(5) 0.052(10) Uani 0.5 1 d D U P A 1
C1A C 0.5936(9) 0.5870(7) 0.588(6) 0.051(10) Uani 0.5 1 d D U P A 1
C2A C 0.5678(11) 0.5536(8) 0.674(6) 0.058(13) Uani 0.5 1 d D U P A 1
H2A H 0.574374 0.548706 0.782545 0.070 Uiso 0.5 1 calc R U P A 1
C3A C 0.5334(12) 0.5278(12) 0.604(7) 0.072(13) Uani 0.5 1 d D U P A 1
O1A O 0.5069(9) 0.4931(9) 0.690(6) 0.093(14) Uani 0.5 2 d DS TU P A 1
N2B N 0.6335(12) 0.6137(11) 0.614(5) 0.049(9) Uani 0.5 1 d D U P A 2
C1B C 0.5974(9) 0.5835(7) 0.570(6) 0.044(8) Uani 0.5 1 d D U P A 2
C2B C 0.5735(11) 0.5475(9) 0.643(6) 0.048(10) Uani 0.5 1 d D U P A 2
H2B H 0.580650 0.539868 0.743997 0.058 Uiso 0.5 1 calc R U P A 2
C3B C 0.5392(13) 0.5238(12) 0.564(7) 0.073(13) Uani 0.5 1 d D U P A 2
O1B O 0.5143(9) 0.4857(9) 0.627(5) 0.088(15) Uani 0.5 2 d DS TU P A 2
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'
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'
Cl Cl 0.3639 0.7018 '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'
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
N2A Cu1 N2A 176(3) 18_656 .
N2A Cu1 N2B 9(4) 18_656 18_656
N2A Cu1 N2B 174(2) . 18_656
N2B Cu1 N2B 170(3) . 18_656
N2A Cu1 N1 88.2(15) 18_656 9_565
N2A Cu1 N1 88.2(15) . 9_565
N2B Cu1 N1 94.8(15) . 9_565
N2B Cu1 N1 94.8(15) 18_656 9_565
N2A Cu1 Cl1 84.6(14) 18_656 .
N2A Cu1 Cl1 95.2(13) . .
N2B Cu1 Cl1 89.9(12) . .
N2B Cu1 Cl1 90.6(13) 18_656 .
N1 Cu1 Cl1 87.38(7) 9_565 .
N2A Cu1 Cl1 95.2(13) 18_656 9_565
N2A Cu1 Cl1 84.6(14) . 9_565
N2B Cu1 Cl1 90.6(13) . 9_565
N2B Cu1 Cl1 89.9(12) 18_656 9_565
N1 Cu1 Cl1 87.38(7) 9_565 9_565
Cl1 Cu1 Cl1 174.76(15) . 9_565
Cu1 Cl1 Cu1 91.33(16) 14_654 .
N2A N1 N2A 112(3) . 4_556
N2A N1 N2B 110.1(16) . 4_556
N2A N1 N2B 13(6) 4_556 4_556
N2B N1 N2B 112(3) 4_556 .
N2A N1 Cu1 124.1(14) . 14_654
N2A N1 Cu1 124.1(14) 4_556 14_654
N2B N1 Cu1 124.1(15) 4_556 14_654
N2B N1 Cu1 124.1(15) . 14_654
N1 N2A C1A 107.1(19) . .
N1 N2A Cu1 114.1(18) . .
C1A N2A Cu1 139(2) . .
N2A C1A C2A 131(3) . .
N2A C1A C1A 106.9(18) . 4_556
C2A C1A C1A 122.0(18) . 4_556
C3A C2A C1A 120(2) . .
C3A C2A H2A 119.9 . .
C1A C2A H2A 120.0 . .
C2A C3A O1A 120(2) . .
C2A C3A C3A 117(2) . 4_556
O1A C3A C3A 121(2) . 4_556
C3A O1A C3A 117(4) 22_665 .
N1 N2B C1B 107(2) . .
N1 N2B Cu1 111(2) . .
C1B N2B Cu1 137(2) . .
N2B C1B C2B 132(3) . .
N2B C1B C1B 106.9(18) . 4_556
C2B C1B C1B 120.9(17) . 4_556
C3B C2B C1B 117(2) . .
C3B C2B H2B 121.6 . .
C1B C2B H2B 121.6 . .
C2B C3B O1B 120(2) . .
C2B C3B C3B 121(2) . 4_556
O1B C3B C3B 118.4(19) . 4_556
C3B O1B C3B 123(4) 22_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2A 2.00(3) 18_656
Cu1 N2A 2.00(3) .
Cu1 N2B 2.05(3) .
Cu1 N2B 2.05(3) 18_656
Cu1 N1 2.162(12) 9_565
Cu1 Cl1 2.358(3) .
Cu1 Cl1 2.358(3) 9_565
N1 N2A 1.343(17) .
N1 N2A 1.343(17) 4_556
N1 N2B 1.341(17) 4_556
N1 N2B 1.341(17) .
N2A C1A 1.352(18) .
C1A C2A 1.355(18) .
C1A C1A 1.44(10) 4_556
C2A C3A 1.323(17) .
C2A H2A 0.9300 .
C3A O1A 1.395(18) .
C3A C3A 1.66(11) 4_556
N2B C1B 1.347(17) .
C1B C2B 1.358(18) .
C1B C1B 1.43(10) 4_556
C2B C3B 1.330(18) .
C2B H2B 0.9300 .
C3B O1B 1.392(18) .
C3B C3B 1.44(12) 4_556
