#------------------------------------------------------------------------------
#$Date: 2019-11-02 08:10:59 +0200 (Sat, 02 Nov 2019) $
#$Revision: 221052 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/78/4127892.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_4127892
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            'C29.7 H43.3 N3.9 O14.9 S2 Zn4'
_chemical_formula_weight         1018.98
_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                   31.7683(6)
_cell_length_b                   31.7683(6)
_cell_length_c                   11.8414(4)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      3.6
_cell_volume                     10349.6(4)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_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      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rayonix SX-165 CCD'
_diffrn_measurement_method       'φ scan'
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80246
_diffrn_reflns_av_R_equivalents  0.1514
_diffrn_reflns_av_unetI/netI     0.1276
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11820
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        28.782
_diffrn_reflns_theta_max         29.290
_diffrn_reflns_theta_min         3.586
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    3.073
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2292
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0774
_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)+(0.1193P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2070
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1776
_reflns_number_total             2292
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b08322_si_003.cif
_cod_data_source_block           pr_sq
_cod_original_cell_volume        10349.5(5)
_cod_original_formula_sum        'C29.70 H43.30 N3.90 O14.90 S2 Zn4'
_cod_database_code               4127892
_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   0.749
_shelx_estimated_absorpt_t_max   0.941
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
Zn1 Zn 0.42470(3) 0.21235(2) 0.86162(8) 0.0468(4) Uani 1 2 d S T P
Zn2 Zn 0.46875(3) 0.333333 0.833333 0.0563(4) Uani 1 2 d S T P
S1 S 0.44349(6) 0.44349(6) 0.500000 0.0527(6) Uani 1 2 d S T P
O11 O 0.43495(16) 0.34669(16) 0.7125(5) 0.0727(14) Uani 1 1 d . . .
O12 O 0.48973(16) 0.42499(14) 0.6917(4) 0.0648(12) Uani 1 1 d . . .
C11 C 0.4508(2) 0.3873(2) 0.6681(5) 0.0529(13) Uani 1 1 d . . .
C12 C 0.4205(2) 0.39105(19) 0.5761(6) 0.0547(14) Uani 1 1 d . . .
C13 C 0.3751(2) 0.3581(2) 0.5440(6) 0.0647(16) Uani 1 1 d . . .
H13 H 0.356601 0.326921 0.577378 0.078 Uiso 1 1 calc R U .
O21 O 0.47204(15) 0.27706(14) 0.7988(4) 0.0651(12) Uani 1 1 d D U .
C21 C 0.5143(6) 0.2786(7) 0.763(2) 0.084(4) Uani 0.5 1 d D U P
H21 H 0.538355 0.290686 0.826416 0.101 Uiso 0.5 1 calc R U P
C22 C 0.5057(5) 0.2291(6) 0.7256(15) 0.069(4) Uani 0.5 1 d D U P
H22A H 0.493243 0.222237 0.647191 0.083 Uiso 0.5 1 calc R U P
H22B H 0.536504 0.228348 0.728355 0.083 Uiso 0.5 1 calc R U P
C23 C 0.5366(6) 0.3124(6) 0.6612(15) 0.096(5) Uani 0.5 1 d D U P
H23A H 0.545382 0.345584 0.682737 0.144 Uiso 0.5 1 calc R U P
H23B H 0.512884 0.301351 0.599506 0.144 Uiso 0.5 1 calc R U P
H23C H 0.565740 0.311854 0.636364 0.144 Uiso 0.5 1 calc R U P
N1 N 0.3674(2) 0.18372(11) 0.7412(5) 0.0449(13) Uani 1 2 d S TU P
C1 C 0.3839(4) 0.1721(5) 0.6372(11) 0.064(3) Uani 0.5 1 d . U P
H1A H 0.398247 0.151501 0.655112 0.077 Uiso 0.5 1 calc R U P
H1B H 0.409613 0.202560 0.602572 0.077 Uiso 1 2 calc R U P
C2 C 0.3519(5) 0.2176(4) 0.7138(12) 0.057(3) Uani 0.5 1 d . U P
H2A H 0.380428 0.248791 0.690490 0.068 Uiso 0.5 1 calc R U P
H2B H 0.337647 0.223800 0.781666 0.068 Uiso 0.5 1 calc R U P
C3 C 0.3245(5) 0.1365(4) 0.7813(12) 0.068(3) Uani 0.5 1 d . U P
H3A H 0.314139 0.140954 0.857172 0.081 Uiso 0.5 1 calc R U P
H3B H 0.333522 0.110959 0.786247 0.081 Uiso 0.5 1 calc R U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0050 0.0020 '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 0.0090 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0150 0.0080 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1500 0.1580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2120 1.8140 '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 O12 83.1(2) 17_556 33_546
O12 Zn1 N1 100.09(19) 17_556 .
O12 Zn1 N1 100.09(19) 33_546 .
O21 Zn1 O12 92.64(17) . 17_556
O21 Zn1 O12 92.64(17) 24 33_546
O21 Zn1 O12 156.3(2) . 33_546
O21 Zn1 O12 156.3(2) 24 17_556
O21 Zn1 O21 82.0(2) 24 .
O21 Zn1 N1 103.6(2) . .
O21 Zn1 N1 103.6(2) 24 .
O11 Zn2 O11 97.9(3) 17_556 .
O21 Zn2 O11 110.1(2) . .
O21 Zn2 O11 110.1(2) 17_556 17_556
O21 Zn2 O11 110.59(18) . 17_556
O21 Zn2 O11 110.60(18) 17_556 .
O21 Zn2 O21 116.1(3) . 17_556
C12 S1 C12 90.6(4) 4_556 .
C11 O11 Zn2 123.5(4) . .
C11 O12 Zn1 143.4(4) . 32_556
O11 C11 O12 126.5(6) . .
O11 C11 C12 116.5(5) . .
O12 C11 C12 117.1(5) . .
C11 C12 S1 118.9(4) . .
C13 C12 S1 112.3(5) . .
C13 C12 C11 128.8(5) . .
C12 C13 C13 112.4(4) . 4_556
C12 C13 H13 123.8 . .
C13 C13 H13 123.8 4_556 .
Zn2 O21 Zn1 121.8(2) . .
C21 O21 Zn1 111.7(7) . .
C21 O21 Zn2 123.0(9) . .
C22 O21 Zn1 114.4(9) 24 .
C22 O21 Zn2 123.7(9) 24 .
C22 O21 C21 21.2(15) 24 .
O21 C21 H21 108.9 . .
O21 C21 C22 112.5(15) . .
O21 C21 H22B 113.4(18) . 24
O21 C21 C23 111.4(13) . .
H21 C21 H22B 84.1 . 24
C22 C21 H21 108.9 . .
C22 C21 H22B 124.2(18) . 24
C22 C21 C23 106.0(16) . .
C23 C21 H21 108.9 . .
C23 C21 H22B 26.4(18) . 24
O21 C22 C21 107.2(14) 24 .
O21 C22 H22A 110.3 24 .
O21 C22 H22B 110.3 24 .
C21 C22 H22A 110.3 . .
C21 C22 H22B 110.3 . .
H22A C22 H22B 108.5 . .
C21 C23 H22B 31(2) . 24
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H22B 84.2 . 24
H23A C23 H23B 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H22B 137.6 . 24
H23B C23 H23C 109.5 . .
H23C C23 H22B 102.6 . 24
C1 N1 Zn1 109.7(6) . .
C1 N1 Zn1 109.7(6) 24 .
C1 N1 C1 51.3(12) . 24
C1 N1 C3 106.0(8) . .
C1 N1 C3 106.0(8) 24 24
C1 N1 C3 137.9(8) . 24
C1 N1 C3 137.9(8) 24 .
C2 N1 Zn1 112.0(5) . .
C2 N1 Zn1 112.0(5) 24 .
C2 N1 C1 60.0(8) . 24
C2 N1 C1 60.0(8) 24 .
C2 N1 C1 107.5(9) . .
C2 N1 C1 107.5(9) 24 24
C2 N1 C2 135.9(10) 24 .
C2 N1 C3 48.5(8) . 24
C2 N1 C3 48.5(8) 24 .
C2 N1 C3 109.7(9) . .
C2 N1 C3 109.7(9) 24 24
C3 N1 Zn1 111.6(6) . .
C3 N1 Zn1 111.6(6) 24 .
C3 N1 C3 65.3(13) . 24
N1 C1 H1A 109.2 . .
N1 C1 H1B 109.2 . .
N1 C1 C2 86.7(8) . 25_556
N1 C1 C3 112.0(9) . 12_556
H1A C1 H1B 107.9 . .
C2 C1 H1A 95.2 25_556 .
C2 C1 H1B 144.8 25_556 .
C3 C1 H1A 109.2 12_556 .
C3 C1 H1B 109.2 12_556 .
C3 C1 C2 36.4(7) 12_556 25_556
N1 C2 C1 89.3(7) . 25_556
N1 C2 C2 111.7(5) . 12_556
N1 C2 H2A 109.3 . .
N1 C2 H2B 109.3 . .
N1 C2 C3 91.3(8) . 25_556
C1 C2 H2A 153.7 25_556 .
C1 C2 H2B 81.8 25_556 .
C2 C2 C1 45.0(9) 12_556 25_556
C2 C2 H2A 109.3 12_556 .
C2 C2 H2B 109.3 12_556 .
C2 C2 C3 37.2(8) 12_556 25_556
H2A C2 H2B 107.9 . .
C3 C2 C1 71.9(6) 25_556 25_556
C3 C2 H2A 88.7 25_556 .
C3 C2 H2B 146.4 25_556 .
N1 C3 C1 108.1(9) . 12_556
N1 C3 C2 86.6(8) . 25_556
N1 C3 H2B 102.7(13) . 24
N1 C3 H3A 110.1 . .
N1 C3 H3B 110.1 . .
C1 C3 C2 45.8(7) 12_556 25_556
C1 C3 H2B 112.7(14) 12_556 24
C1 C3 H3A 110.1 12_556 .
C1 C3 H3B 110.1 12_556 .
C2 C3 H2B 79.4(12) 25_556 24
C2 C3 H3A 155.3 25_556 .
C2 C3 H3B 81.1 25_556 .
H3A C3 H2B 112.8 . 24
H3A C3 H3B 108.4 . .
H3B C3 H2B 7.4 . 24
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 O12 2.043(4) 17_556 yes
Zn1 O12 2.043(4) 33_546 ?
Zn1 O21 1.987(4) . yes
Zn1 O21 1.987(4) 24 ?
Zn1 N1 2.125(6) . yes
Zn2 O11 1.959(5) . yes
Zn2 O11 1.959(5) 17_556 ?
Zn2 O21 1.887(4) . yes
Zn2 O21 1.887(4) 17_556 ?
S1 C12 1.704(6) . ?
S1 C12 1.704(6) 4_556 ?
O11 C11 1.243(7) . ?
O12 C11 1.248(7) . ?
C11 C12 1.498(9) . ?
C12 C13 1.346(8) . ?
C13 C13 1.398(13) 4_556 ?
C13 H13 0.9500 . ?
O21 C21 1.386(11) . ?
O21 C22 1.383(10) 24 ?
C21 H21 1.0000 . ?
C21 C22 1.520(16) . ?
C21 H22B 0.94(3) 24 ?
C21 C23 1.532(17) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
N1 C1 1.456(13) . ?
N1 C1 1.456(13) 24 ?
N1 C2 1.428(10) . ?
N1 C2 1.428(10) 24 ?
N1 C3 1.513(12) . ?
N1 C3 1.513(12) 24 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 2.036(18) 25_556 ?
C1 C3 1.540(17) 12_556 ?
C2 C2 1.51(2) 12_556 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 2.00(2) 25_556 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
