#------------------------------------------------------------------------------
#$Date: 2019-11-02 08:10:29 +0200 (Sat, 02 Nov 2019) $
#$Revision: 221051 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/78/4127891.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_4127891
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            'C31.4 H48.6 N3.8 O15.8 S2 Zn4'
_chemical_formula_weight         1057.74
_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                   31.8116(9)
_cell_length_b                   31.8116(9)
_cell_length_c                   11.6096(4)
_cell_measurement_reflns_used    3132
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      3.44
_cell_volume                     10174.6(5)
_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 0.875
_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  0.0181
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7717
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.508
_diffrn_reflns_theta_min         3.389
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82779
_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            yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             4878
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2656
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0318
_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)+(0.0473P)²+15.9630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2272
_reflns_number_total             2656
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b08322_si_004.cif
_cod_data_source_block           bu_sq
_cod_original_cell_volume        10174.6(7)
_cod_database_code               4127891
_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   0.625
_shelx_estimated_absorpt_t_max   0.714
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 0.57468(2) 0.78734(2) 0.14027(3) 0.03138(12) Uani 1 2 d S T P A .
Zn2 Zn 0.52997(2) 0.666667 0.166667 0.04409(14) Uani 1 2 d S T P A .
N1 N 0.63208(9) 0.81604(5) 0.2583(2) 0.0371(6) Uani 1 2 d S TU P . .
C1 C 0.6730(2) 0.8089(3) 0.2181(5) 0.0621(14) Uani 0.5 1 d D U P . .
H1A H 0.682860 0.822066 0.139270 0.075 Uiso 0.5 1 calc R U P . .
H1B H 0.662272 0.773885 0.216345 0.075 Uiso 0.5 1 calc R U P . .
C2 C 0.6168(2) 0.7857(2) 0.3650(5) 0.0762(19) Uani 0.5 1 d D U P . .
H2A H 0.604050 0.751259 0.344308 0.091 Uiso 0.5 1 calc R U P . .
H2B H 0.590486 0.788460 0.403500 0.091 Uiso 0.5 1 calc R U P . .
C3 C 0.6483(2) 0.8632(2) 0.2826(6) 0.0652(14) Uani 0.5 1 d D U P . .
H3A H 0.620431 0.867447 0.302496 0.078 Uiso 0.5 1 calc R U P . .
H3B H 0.664194 0.883048 0.213430 0.078 Uiso 0.5 1 calc R U P . .
O11 O 0.56424(7) 0.65396(7) 0.28958(17) 0.0575(5) Uani 1 1 d . . . . .
O12 O 0.50902(7) 0.57605(6) 0.31124(15) 0.0491(4) Uani 1 1 d . . . . .
C11 C 0.54800(8) 0.61312(8) 0.3341(2) 0.0392(5) Uani 1 1 d . . . . .
C12 C 0.57859(8) 0.60878(8) 0.42380(19) 0.0379(5) Uani 1 1 d . . . . .
C13 C 0.62432(9) 0.64190(9) 0.4569(2) 0.0502(6) Uani 1 1 d . . . . .
H13 H 0.642318 0.673529 0.424796 0.060 Uiso 1 1 calc R U . . .
S1 S 0.55614(2) 0.55614(2) 0.500000 0.03835(19) Uani 1 2 d S T P . .
O1S O 0.52684(6) 0.72303(6) 0.20317(17) 0.0508(4) Uani 1 1 d . U . . .
C1S C 0.4834(3) 0.7226(4) 0.2513(9) 0.0574(17) Uani 0.5 1 d D U P A -1
C2S C 0.4952(3) 0.7731(3) 0.2761(10) 0.0584(19) Uani 0.5 1 d D U P A -1
C3S C 0.4549(5) 0.7704(6) 0.3286(15) 0.060(3) Uani 0.25 1 d D U P A -1
H3S1 H 0.446036 0.789894 0.278014 0.072 Uiso 0.25 1 calc R U P A -1
H3S2 H 0.467850 0.789789 0.399839 0.072 Uiso 0.25 1 calc R U P A -1
C4S C 0.4068(5) 0.7282(6) 0.3646(16) 0.081(3) Uani 0.25 1 d D U P A -1
H4S1 H 0.386889 0.740324 0.399729 0.122 Uiso 0.25 1 calc R U P A -1
H4S2 H 0.390072 0.708477 0.297019 0.122 Uiso 0.25 1 calc R U P A -1
H4S3 H 0.412221 0.708371 0.420713 0.122 Uiso 0.25 1 calc R U P A -1
C2S' C 0.4674(5) 0.6922(7) 0.3536(13) 0.061(3) Uani 0.25 1 d D U P A -1
H2S1 H 0.494338 0.705481 0.409967 0.073 Uiso 0.25 1 calc R U P A -1
H2S2 H 0.460797 0.659320 0.332019 0.073 Uiso 0.25 1 calc R U P A -1
C3S' C 0.4226(5) 0.6873(6) 0.4126(14) 0.081(3) Uani 0.25 1 d D U P A -1
H3S3 H 0.414851 0.666161 0.480160 0.122 Uiso 0.25 1 calc R U P A -1
H3S4 H 0.428816 0.719366 0.437012 0.122 Uiso 0.25 1 calc R U P A -1
H3S5 H 0.395182 0.673077 0.358849 0.122 Uiso 0.25 1 calc R U P A -1
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 100.67(8) 27 .
O12 Zn1 N1 100.67(8) 11_565 .
O12 Zn1 O12 82.81(10) 11_565 27
O1S Zn1 N1 105.16(8) . .
O1S Zn1 N1 105.16(8) 24_565 .
O1S Zn1 O12 92.40(7) . 11_565
O1S Zn1 O12 92.40(7) 24_565 27
O1S Zn1 O12 154.17(8) . 27
O1S Zn1 O12 154.17(8) 24_565 11_565
O1S Zn1 O1S 80.91(10) . 24_565
O11 Zn2 O11 97.34(12) 11_565 .
O1S Zn2 O11 111.35(7) . 11_565
O1S Zn2 O11 109.33(9) . .
O1S Zn2 O11 109.34(9) 11_565 11_565
O1S Zn2 O11 111.35(7) 11_565 .
O1S Zn2 O1S 116.49(11) 11_565 .
C1 N1 Zn1 111.3(2) . .
C1 N1 Zn1 111.3(2) 24_565 .
C1 N1 C1 71.4(6) . 24_565
C2 N1 Zn1 109.3(2) . .
C2 N1 Zn1 109.3(2) 24_565 .
C2 N1 C1 138.7(3) . 24_565
C2 N1 C1 138.7(3) 24_565 .
C2 N1 C1 100.8(4) . .
C2 N1 C1 100.8(4) 24_565 24_565
C2 N1 C2 57.7(6) . 24_565
C3 N1 Zn1 112.8(2) . .
C3 N1 Zn1 112.8(2) 24_565 .
C3 N1 C1 43.9(4) . 24_565
C3 N1 C1 43.9(4) 24_565 .
C3 N1 C1 110.7(5) . .
C3 N1 C1 110.7(5) 24_565 24_565
C3 N1 C2 58.4(4) . 24_565
C3 N1 C2 58.4(4) 24_565 .
C3 N1 C2 111.3(5) . .
C3 N1 C2 111.3(5) 24_565 24_565
C3 N1 C3 133.8(5) 24_565 .
N1 C1 H1A 109.9 . .
N1 C1 H1B 109.9 . .
N1 C1 C2 109.1(4) . 18_655
N1 C1 C3 86.1(4) . 31_665
N1 C1 H3B 110.1(7) . 24_565
H1A C1 H1B 108.3 . .
H1A C1 H3B 105.7 . 24_565
H1B C1 H3B 2.9 . 24_565
C2 C1 H1A 109.9 18_655 .
C2 C1 H1B 109.9 18_655 .
C2 C1 C3 44.3(3) 18_655 31_665
C2 C1 H3B 112.2(7) 18_655 24_565
C3 C1 H1A 154.0 31_665 .
C3 C1 H1B 84.0 31_665 .
C3 C1 H3B 86.8(7) 31_665 24_565
N1 C2 C1 110.4(4) . 18_655
N1 C2 H2A 109.6 . .
N1 C2 H2B 109.6 . .
N1 C2 C3 87.2(4) . 31_665
C1 C2 H2A 109.6 18_655 .
C1 C2 H2B 109.6 18_655 .
C1 C2 C3 33.1(3) 18_655 31_665
H2A C2 H2B 108.1 . .
C3 C2 H2A 97.3 31_665 .
C3 C2 H2B 141.7 31_665 .
N1 C3 C1 95.1(4) . 31_665
N1 C3 C2 95.6(4) . 31_665
N1 C3 C3 112.0(3) . 18_655
N1 C3 H3A 109.2 . .
N1 C3 H3B 109.2 . .
C1 C3 H3A 90.6 31_665 .
C1 C3 H3B 141.6 31_665 .
C2 C3 C1 71.5(3) 31_665 31_665
C2 C3 H3A 150.8 31_665 .
C2 C3 H3B 76.8 31_665 .
C3 C3 C1 32.5(4) 18_655 31_665
C3 C3 C2 44.8(4) 18_655 31_665
C3 C3 H3A 109.2 18_655 .
C3 C3 H3B 109.2 18_655 .
H3A C3 H3B 107.9 . .
C11 O11 Zn2 122.35(17) . .
C11 O12 Zn1 143.45(16) . 26_455
O11 C11 C12 116.2(2) . .
O12 C11 O11 126.8(2) . .
O12 C11 C12 117.0(2) . .
C11 C12 S1 119.05(17) . .
C13 C12 C11 128.8(2) . .
C13 C12 S1 112.12(18) . .
C12 C13 C13 112.41(14) . 4_556
C12 C13 H13 123.8 . .
C13 C13 H13 123.8 4_556 .
C12 S1 C12 90.94(16) . 4_556
Zn2 O1S Zn1 121.25(9) . .
C1S O1S Zn1 112.3(4) . .
C1S O1S Zn2 124.4(4) . .
C2S C1S O1S 109.5(9) . .
C2S' C1S O1S 109.1(8) . .
C2S' C1S C2S 112.2(14) . .
O1S C2S C1S 111.5(9) 24_565 .
O1S C2S C3S 132.7(12) 24_565 .
C3S C2S C1S 107.1(12) . .
C2S C3S H3S1 104.1 . .
C2S C3S H3S2 104.1 . .
C2S C3S C4S 132.4(14) . .
H3S1 C3S H3S2 105.5 . .
C4S C3S H3S1 104.1 . .
C4S C3S H3S2 104.1 . .
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 . .
C1S C2S' H2S1 108.3 . .
C1S C2S' H2S2 108.3 . .
C1S C2S' C3S' 115.8(13) . .
H2S1 C2S' H2S2 107.4 . .
C3S' C2S' H2S1 108.3 . .
C3S' C2S' H2S2 108.3 . .
C2S' C3S' H3S3 109.5 . .
C2S' C3S' H3S4 109.5 . .
C2S' C3S' H3S5 109.5 . .
H3S3 C3S' H3S4 109.5 . .
H3S3 C3S' H3S5 109.5 . .
H3S4 C3S' H3S5 109.5 . .
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 2.092(3) . yes
Zn1 O12 2.0460(17) 11_565 ?
Zn1 O12 2.0461(17) 27 yes
Zn1 O1S 1.9801(16) . yes
Zn1 O1S 1.9801(16) 24_565 ?
Zn2 O11 1.9565(18) 11_565 ?
Zn2 O11 1.9566(18) . yes
Zn2 O1S 1.8929(17) 11_565 ?
Zn2 O1S 1.8930(17) . yes
N1 C1 1.502(5) . ?
N1 C1 1.502(6) 24_565 ?
N1 C2 1.494(6) . ?
N1 C2 1.494(6) 24_565 ?
N1 C3 1.350(5) . ?
N1 C3 1.350(5) 24_565 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.551(7) 18_655 ?
C1 C3 1.988(9) 31_665 ?
C1 H3B 0.785(9) 24_565 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.962(9) 31_665 ?
C3 C3 1.551(11) 18_655 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O11 C11 1.245(3) . ?
O12 C11 1.239(3) . ?
C11 C12 1.478(3) . ?
C12 C13 1.357(3) . ?
C12 S1 1.703(2) . ?
C13 C13 1.394(5) 4_556 ?
C13 H13 0.9500 . ?
O1S C1S 1.485(8) . ?
C1S C2S 1.484(8) . ?
C1S C2S' 1.455(15) . ?
C2S C3S 1.383(13) . ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C3S C4S 1.504(14) . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
C2S' H2S1 0.9900 . ?
C2S' H2S2 0.9900 . ?
C2S' C3S' 1.516(14) . ?
C3S' H3S3 0.9800 . ?
C3S' H3S4 0.9800 . ?
C3S' H3S5 0.9800 . ?
