#------------------------------------------------------------------------------
#$Date: 2019-11-02 08:09:33 +0200 (Sat, 02 Nov 2019) $
#$Revision: 221049 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/78/4127889.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_4127889
loop_
_publ_author_name
'Lysova, Anna A.'
'Samsonenko, Denis G.'
'Dorovatovskii, Pavel V.'
'Lazarenko, Vladimir A.'
'Khrustalev, Victor N.'
'Kovalenko, Konstantin A.'
'Dybtsev, Danil N.'
'Fedin, Vladimir P.'
_publ_section_title
;
 Tuning the Molecular and Cationic Affinity in a Series of Multifunctional
 Metal-Organic Frameworks Based on Dodecanuclear Zn(II) Carboxylate
 Wheels.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17260
_journal_page_last               17269
_journal_paper_doi               10.1021/jacs.9b08322
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C33.1 H51.9 N3.7 O15.7 S2 Zn4'
_chemical_formula_weight         1078.48
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   32.0583(8)
_cell_length_b                   32.0583(8)
_cell_length_c                   11.5030(3)
_cell_measurement_reflns_used    4958
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.38
_cell_measurement_theta_min      3.83
_cell_volume                     10238.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9837
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.498
_diffrn_reflns_theta_min         3.363
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             4986
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2954
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0385P)²+9.7248P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2505
_reflns_number_total             2954
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b08322_si_005.cif
_cod_data_source_block           al57e_sq
_cod_original_cell_volume        10238.2(6)
_cod_database_code               4127889
_shelx_shelxl_version_number     2018/3
_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   0.400
_shelx_estimated_absorpt_t_max   0.663
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
Zn1 Zn 0.57374(2) 0.78687(2) 0.14009(2) 0.02946(9) Uani 1 2 d S T P . .
Zn2 Zn 0.52872(2) 0.666667 0.166667 0.04635(11) Uani 1 2 d S T P . .
N1 N 0.63176(7) 0.81588(3) 0.25790(16) 0.0322(4) Uani 1 2 d DS TU P . .
C1 C 0.67308(15) 0.8097(2) 0.2142(3) 0.0583(12) Uani 0.5 1 d D U P . .
H1A H 0.682519 0.823373 0.135033 0.070 Uiso 0.5 1 calc R U P . .
H1B H 0.662926 0.775071 0.210648 0.070 Uiso 0.5 1 calc R U P . .
C2 C 0.61681(15) 0.78636(15) 0.3680(3) 0.0633(13) Uani 0.5 1 d D U P . .
H2A H 0.603892 0.751978 0.348528 0.076 Uiso 0.5 1 calc R U P . .
H2B H 0.590931 0.789502 0.406706 0.076 Uiso 0.5 1 calc R U P . .
C3 C 0.64861(18) 0.86462(14) 0.2822(4) 0.0638(13) Uani 0.5 1 d D U P . .
H3A H 0.620985 0.869051 0.301559 0.077 Uiso 0.5 1 calc R U P . .
H3B H 0.664505 0.884093 0.212124 0.077 Uiso 0.5 1 calc R U P . .
O11 O 0.56288(6) 0.65436(5) 0.29186(14) 0.0587(4) Uani 1 1 d . . . . .
O12 O 0.50818(5) 0.57634(5) 0.31247(11) 0.0497(3) Uani 1 1 d . . . . .
C11 C 0.54710(7) 0.61342(6) 0.33564(14) 0.0383(4) Uani 1 1 d . . . . .
C12 C 0.57786(7) 0.60876(6) 0.42459(15) 0.0375(4) Uani 1 1 d . . . . .
C13 C 0.62380(7) 0.64186(7) 0.45718(17) 0.0491(5) Uani 1 1 d . . . . .
H13 H 0.641450 0.673401 0.425581 0.059 Uiso 1 1 calc R U . . .
S1 S 0.55596(2) 0.55596(2) 0.500000 0.03690(14) Uani 1 2 d S T P . .
O1S O 0.52611(5) 0.72293(5) 0.20296(14) 0.0559(4) Uani 1 1 d . U . . .
C1S C 0.48910(10) 0.72226(9) 0.2680(3) 0.0787(8) Uani 1 1 d . U . . .
C2S C 0.46470(19) 0.69031(18) 0.3573(5) 0.0721(13) Uani 0.5 1 d . U P A .
H2S1 H 0.488515 0.697049 0.419742 0.086 Uiso 0.5 1 calc R U P . .
H2S2 H 0.454848 0.657702 0.327483 0.086 Uiso 0.5 1 calc R U P . .
C3S C 0.4201(2) 0.6872(2) 0.4157(6) 0.0931(18) Uani 0.5 1 d D U P . .
C4S C 0.4016(3) 0.6502(3) 0.5151(7) 0.111(3) Uani 0.451(4) 1 d D U P A 1
H4S1 H 0.373281 0.648997 0.550673 0.167 Uiso 0.451(4) 1 calc R U P A 1
H4S2 H 0.392903 0.618373 0.484242 0.167 Uiso 0.451(4) 1 calc R U P A 1
H4S3 H 0.426971 0.659680 0.573787 0.167 Uiso 0.451(4) 1 calc R U P A 1
C4S' C 0.3678(8) 0.657(2) 0.374(5) 0.106(8) Uani 0.049(4) 1 d D U P A 2
H4S4 H 0.346612 0.661876 0.427346 0.159 Uiso 0.049(4) 1 calc R U P A 2
H4S5 H 0.364910 0.667584 0.295767 0.159 Uiso 0.049(4) 1 calc R U P A 2
H4S6 H 0.358453 0.623085 0.372471 0.159 Uiso 0.049(4) 1 calc R U 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 0.0033 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O12 Zn1 N1 100.04(6) 27 .
O12 Zn1 N1 100.04(6) 11_565 .
O12 Zn1 O12 82.89(8) 11_565 27
O1S Zn1 N1 106.01(6) . .
O1S Zn1 N1 106.01(6) 24_565 .
O1S Zn1 O12 92.23(6) 24_565 27
O1S Zn1 O12 92.24(6) . 11_565
O1S Zn1 O12 153.95(7) . 27
O1S Zn1 O12 153.95(7) 24_565 11_565
O1S Zn1 O1S 80.95(8) 24_565 .
O11 Zn2 O11 97.74(10) 11_565 .
O1S Zn2 O11 111.13(6) . 11_565
O1S Zn2 O11 108.92(7) . .
O1S Zn2 O11 108.92(7) 11_565 11_565
O1S Zn2 O11 111.13(6) 11_565 .
O1S Zn2 O1S 117.27(9) 11_565 .
C1 N1 Zn1 111.40(17) . .
C1 N1 Zn1 111.40(17) 24_565 .
C1 N1 C1 68.9(4) 24_565 .
C2 N1 Zn1 109.27(17) . .
C2 N1 Zn1 109.27(17) 24_565 .
C2 N1 C1 138.6(2) . 24_565
C2 N1 C1 138.6(2) 24_565 .
C2 N1 C1 102.7(3) . .
C2 N1 C1 102.7(3) 24_565 24_565
C2 N1 C2 55.9(4) 24_565 .
C3 N1 Zn1 112.54(15) . .
C3 N1 Zn1 112.54(15) 24_565 .
C3 N1 C1 45.0(3) . 24_565
C3 N1 C1 45.0(3) 24_565 .
C3 N1 C1 109.6(4) . .
C3 N1 C1 109.6(4) 24_565 24_565
C3 N1 C2 59.5(3) . 24_565
C3 N1 C2 59.5(3) 24_565 .
C3 N1 C2 110.9(3) . .
C3 N1 C2 110.9(3) 24_565 24_565
C3 N1 C3 134.3(3) . 24_565
N1 C1 H1A 109.9 . .
N1 C1 H1B 109.9 . .
N1 C1 C2 108.9(3) . 18_655
N1 C1 H3B 109.7(5) . 24_565
H1A C1 H1B 108.3 . .
H1A C1 H3B 109.0 . 24_565
H1B C1 H3B 0.7 . 24_565
C2 C1 H1A 109.9 18_655 .
C2 C1 H1B 109.9 18_655 .
C2 C1 H3B 109.4(4) 18_655 24_565
N1 C2 C1 110.9(3) . 18_655
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
C1 C2 H2A 109.5 18_655 .
C1 C2 H2B 109.5 18_655 .
H2A C2 H2B 108.0 . .
N1 C3 C3 111.58(18) . 18_655
N1 C3 H3A 109.3 . .
N1 C3 H3B 109.3 . .
C3 C3 H3A 109.3 18_655 .
C3 C3 H3B 109.3 18_655 .
H3A C3 H3B 108.0 . .
C11 O11 Zn2 122.11(13) . .
C11 O12 Zn1 143.42(12) . 26_455
O11 C11 C12 116.33(16) . .
O12 C11 O11 126.86(17) . .
O12 C11 C12 116.81(15) . .
C11 C12 S1 119.11(13) . .
C13 C12 C11 128.64(16) . .
C13 C12 S1 112.26(14) . .
C12 C13 C13 112.20(11) . 4_556
C12 C13 H13 123.9 . .
C13 C13 H13 123.9 4_556 .
C12 S1 C12 91.07(13) 4_556 .
Zn2 O1S Zn1 121.78(7) . .
C1S O1S Zn1 114.94(13) . .
C1S O1S Zn2 123.12(13) . .
O1S C1S C1S 114.21(12) . 24_565
C2S C1S O1S 124.9(3) . .
C2S C1S C1S 117.2(2) . 24_565
C1S C2S H2S1 106.7 . .
C1S C2S H2S2 106.7 . .
C1S C2S C3S 122.4(4) . .
H2S1 C2S H2S2 106.6 . .
C3S C2S H2S1 106.7 . .
C3S C2S H2S2 106.7 . .
C2S C3S C4S 111.2(6) . .
C2S C3S H4S6 107(2) . 22_665
C4S C3S H4S6 71.6(17) . 22_665
C4S' C3S C2S 126(2) . .
C4S' C3S H4S6 26.4(3) . 22_665
C3S C4S H4S1 109.5 . .
C3S C4S H4S2 109.5 . .
C3S C4S H4S3 109.5 . .
H4S1 C4S H4S2 109.5 . .
H4S1 C4S H4S3 109.5 . .
H4S2 C4S H4S3 109.5 . .
C3S C4S' C4S' 85(2) . 24_565
C3S C4S' H4S4 109.5 . .
C3S C4S' H4S5 109.5 . .
C3S C4S' H4S6 75(4) . 22_665
C3S C4S' H4S6 109.5 . .
C4S' C4S' H4S4 60.1 24_565 .
C4S' C4S' H4S5 67.3 24_565 .
C4S' C4S' H4S6 159(6) 24_565 22_665
C4S' C4S' H4S6 164.6 24_565 .
H4S4 C4S' H4S5 109.5 . .
H4S4 C4S' H4S6 109.5 . .
H4S4 C4S' H4S6 134.3 . 22_665
H4S5 C4S' H4S6 109.5 . .
H4S5 C4S' H4S6 111.4 . 22_665
H4S6 C4S' H4S6 36.7 . 22_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.1050(19) . yes
Zn1 O12 2.0466(13) 11_565 yes
Zn1 O12 2.0468(13) 27 ?
Zn1 O1S 1.9814(13) . yes
Zn1 O1S 1.9814(13) 24_565 ?
Zn2 O11 1.9650(14) . yes
Zn2 O11 1.9650(14) 11_565 ?
Zn2 O1S 1.8936(14) 11_565 ?
Zn2 O1S 1.8937(14) . yes
N1 C1 1.519(4) . ?
N1 C1 1.519(4) 24_565 ?
N1 C2 1.509(4) . ?
N1 C2 1.509(4) 24_565 ?
N1 C3 1.403(4) . ?
N1 C3 1.403(4) 24_565 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.556(5) 18_655 ?
C1 H3B 0.837(6) 24_565 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C3 1.546(6) 18_655 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O11 C11 1.252(2) . ?
O12 C11 1.248(2) . ?
C11 C12 1.479(2) . ?
C12 C13 1.369(3) . ?
C12 S1 1.7094(17) . ?
C13 C13 1.406(4) 4_556 ?
C13 H13 0.9500 . ?
O1S C1S 1.394(3) . ?
C1S C1S 1.429(5) 24_565 ?
C1S C2S 1.384(5) . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?
C2S C3S 1.536(7) . ?
C3S C4S 1.537(8) . ?
C3S C4S' 1.535(13) . ?
C3S H4S6 1.51(4) 22_665 ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
C4S' C4S' 1.71(13) 24_565 ?
C4S' H4S4 0.9800 . ?
C4S' H4S5 0.9800 . ?
C4S' H4S6 0.697(10) 22_665 ?
C4S' H4S6 0.9800 . ?
