#------------------------------------------------------------------------------
#$Date: 2019-11-02 08:10:00 +0200 (Sat, 02 Nov 2019) $
#$Revision: 221050 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/78/4127890.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_4127890
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            'C29.5 H43.5 N4.5 O15.5 S2 Zn4'
_chemical_formula_weight         1034.79
_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                   31.7477(14)
_cell_length_b                   31.7477(14)
_cell_length_c                   11.6653(7)
_cell_measurement_reflns_used    2311
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      3.84
_cell_volume                     10182.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8254
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.396
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.251
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             4752
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1033P)²+18.9100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1416
_reflns_number_total             2182
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b08322_si_002.cif
_cod_data_source_block           al55rrrr_sq
_cod_original_cell_volume        10182.4(11)
_cod_original_formula_sum        'C29.50 H43.50 N4.50 O15.50 S2 Zn4'
_cod_database_code               4127890
_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   0.431
_shelx_estimated_absorpt_t_max   0.877
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 0.78700(2) 0.57401(3) 0.36396(8) 0.0770(4) Uani 1 2 d DS T P . .
Zn2 Zn 0.6661(2) 0.52946(14) 0.3495(7) 0.0995(14) Uani 0.5 1 d D U P A -1
O11 O 0.75701(15) 0.60129(17) 0.4749(4) 0.1056(13) Uani 1 1 d D U . . .
O12 O 0.6758(3) 0.5755(4) 0.4700(9) 0.098(2) Uani 0.5 1 d D U P . .
O12' O 0.6821(3) 0.5776(5) 0.4393(9) 0.101(3) Uani 0.5 1 d D U P . .
C11 C 0.71899(17) 0.6017(2) 0.4989(5) 0.0896(14) Uani 1 1 d D U . . .
C12 C 0.72421(19) 0.6380(2) 0.5915(5) 0.0896(15) Uani 1 1 d . U . . .
C13 C 0.6899(2) 0.6489(3) 0.6233(4) 0.099(2) Uani 1 1 d . . . . .
H13 H 0.658147 0.634475 0.591619 0.118 Uiso 1 1 calc R U . . .
S1 S 0.77606(6) 0.666667 0.666667 0.0872(7) Uani 1 2 d S T P . .
N1 N 0.81603(9) 0.63206(19) 0.2436(4) 0.0638(13) Uani 1 2 d DS TU P . .
C1 C 0.7881(3) 0.6170(4) 0.1365(8) 0.099(3) Uani 0.5 1 d D U P . .
H1A H 0.753257 0.604109 0.154125 0.119 Uiso 0.5 1 calc R U P A .
H1B H 0.791395 0.590443 0.101281 0.119 Uiso 0.5 1 calc R U P . .
C2 C 0.8670(3) 0.6494(4) 0.2195(8) 0.083(2) Uani 0.5 1 d D U P . .
H2A H 0.871701 0.621404 0.204450 0.099 Uiso 0.5 1 calc R U P A .
H2B H 0.886800 0.667082 0.287143 0.099 Uiso 0.5 1 calc R U P . .
C3 C 0.8123(4) 0.6739(3) 0.2847(9) 0.090(3) Uani 0.5 1 d D U P . .
H3A H 0.828031 0.684401 0.360615 0.108 Uiso 0.5 1 calc R U P A .
H3B H 0.777625 0.664546 0.292771 0.108 Uiso 0.5 1 calc R U P . .
O1M O 0.7217(2) 0.5203(3) 0.3287(10) 0.105(2) Uani 0.5 1 d D U P A -1
O2M O 0.8047(3) 0.5315(3) 0.2747(8) 0.093(3) Uani 0.5 1 d D U P A -1
C1M C 0.7247(5) 0.4801(5) 0.2756(14) 0.112(4) Uani 0.5 1 d . U P A -1
H1M1 H 0.720656 0.456375 0.335835 0.134 Uiso 0.5 1 calc R U P A -1
H1M2 H 0.697486 0.463327 0.220714 0.134 Uiso 0.5 1 calc R U P A -1
C2M C 0.7698(6) 0.4952(6) 0.2162(14) 0.106(3) Uani 0.5 1 d . U P A -1
H2M1 H 0.776309 0.467765 0.211262 0.127 Uiso 0.5 1 calc R U P A -1
H2M2 H 0.768164 0.505833 0.137431 0.127 Uiso 0.5 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
O11 Zn1 O11 85.6(2) 23_655 .
O11 Zn1 N1 98.22(16) . .
O11 Zn1 N1 98.22(16) 23_655 .
O1M Zn1 O11 89.3(3) . .
O1M Zn1 O11 146.5(3) . 23_655
O1M Zn1 N1 115.3(3) . .
O1M Zn1 O2M 80.5(3) . .
O2M Zn1 O11 97.2(3) . 23_655
O2M Zn1 O11 165.5(3) . .
O2M Zn1 N1 95.5(3) . .
O12 Zn2 O12' 96.8(3) . 18_655
O12 Zn2 O1M 113.0(5) . .
O1M Zn2 O12' 117.9(6) . 18_655
O2M Zn2 O12 104.1(5) 33_545 .
O2M Zn2 O12' 108.2(5) 33_545 18_655
O2M Zn2 O1M 114.6(4) 33_545 .
C11 O11 Zn1 143.9(4) . .
Zn2 O12 Zn2 6.9(3) . 18_655
C11 O12 Zn2 112.8(7) . 18_655
C11 O12 Zn2 114.1(7) . .
C11 O12' Zn2 132.4(9) . 18_655
O11 C11 C12 115.3(5) . .
O12 C11 O11 133.0(8) . .
O12 C11 C12 111.4(6) . .
O12' C11 O11 119.1(8) . .
O12' C11 O12 18.5(8) . .
O12' C11 C12 125.1(7) . .
C11 C12 S1 119.1(4) . .
C13 C12 C11 126.2(5) . .
C13 C12 S1 114.6(5) . .
C12 C13 C13 110.6(4) . 11_566
C12 C13 H13 124.7 . .
C13 C13 H13 124.7 11_566 .
C12 S1 C12 89.5(4) . 11_566
C1 N1 Zn1 110.5(5) . .
C1 N1 Zn1 110.5(5) 23_655 .
C1 N1 C1 52.4(9) 23_655 .
C1 N1 C3 105.2(6) . .
C1 N1 C3 105.2(6) 23_655 23_655
C1 N1 C3 137.1(6) . 23_655
C1 N1 C3 137.1(6) 23_655 .
C2 N1 Zn1 112.0(3) . .
C2 N1 Zn1 112.0(3) 23_655 .
C2 N1 C1 61.3(6) . 23_655
C2 N1 C1 61.3(6) 23_655 .
C2 N1 C1 109.7(6) . .
C2 N1 C1 109.7(6) 23_655 23_655
C2 N1 C2 135.1(7) . 23_655
C2 N1 C3 46.7(6) . 23_655
C2 N1 C3 46.7(6) 23_655 .
C2 N1 C3 107.3(7) . .
C2 N1 C3 107.3(7) 23_655 23_655
C3 N1 Zn1 111.8(5) . .
C3 N1 Zn1 111.8(5) 23_655 .
C3 N1 C3 64.3(9) 23_655 .
N1 C1 H1A 109.0 . .
N1 C1 H1B 109.0 . .
N1 C1 C2 90.4(6) . 25_665
N1 C1 C3 112.8(7) . 11_565
H1A C1 H1B 107.8 . .
C2 C1 H1A 92.4 25_665 .
C2 C1 H1B 144.6 25_665 .
C3 C1 H1A 109.0 11_565 .
C3 C1 H1B 109.0 11_565 .
C3 C1 C2 35.7(6) 11_565 25_665
N1 C2 C1 90.5(5) . 25_665
N1 C2 C2 110.7(4) . 11_565
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
C1 C2 H2A 155.4 25_665 .
C1 C2 H2B 77.0 25_665 .
C2 C2 C1 47.9(6) 11_565 25_665
C2 C2 H2A 109.5 11_565 .
C2 C2 H2B 109.5 11_565 .
H2A C2 H2B 108.1 . .
N1 C3 C1 109.0(7) . 11_565
N1 C3 H2B 112.0(9) . 23_655
N1 C3 H3A 109.9 . .
N1 C3 H3B 109.9 . .
C1 C3 H2B 104.9(9) 11_565 23_655
C1 C3 H3A 109.9 11_565 .
C1 C3 H3B 109.9 11_565 .
H3A C3 H2B 111.2 . 23_655
H3A C3 H3B 108.3 . .
H3B C3 H2B 5.1 . 23_655
Zn2 O1M Zn1 119.2(5) . .
C1M O1M Zn1 110.2(7) . .
C1M O1M Zn2 130.1(7) . .
Zn2 O2M Zn1 118.5(5) 32 .
C2M O2M Zn1 117.6(8) . .
C2M O2M Zn2 120.4(7) . 32
O1M C1M H1M1 108.8 . .
O1M C1M H1M2 108.8 . .
H1M1 C1M H1M2 107.7 . .
C2M C1M O1M 113.7(13) . .
C2M C1M H1M1 108.8 . .
C2M C1M H1M2 108.8 . .
O2M C2M C1M 107.6(13) . .
O2M C2M H2M1 110.2 . .
O2M C2M H2M2 110.2 . .
C1M C2M H2M1 110.2 . .
C1M C2M H2M2 110.2 . .
H2M1 C2M H2M2 108.5 . .
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 O11 2.038(4) . yes
Zn1 O11 2.038(4) 23_655 ?
Zn1 N1 2.126(6) . yes
Zn1 O1M 1.961(6) . yes
Zn1 O2M 1.996(6) . yes
Zn2 O12 1.938(8) . yes
Zn2 O12' 1.954(7) 18_655 yes
Zn2 O1M 1.942(6) . yes
Zn2 O2M 1.932(6) 33_545 yes
O11 C11 1.246(5) . ?
O12 C11 1.244(8) . ?
O12' C11 1.243(8) . ?
C11 C12 1.525(9) . ?
C12 C13 1.348(8) . ?
C12 S1 1.676(6) . ?
C13 C13 1.408(13) 11_566 ?
C13 H13 0.9500 . ?
N1 C1 1.467(8) . ?
N1 C1 1.467(8) 23_655 ?
N1 C2 1.451(8) . ?
N1 C2 1.451(8) 23_655 ?
N1 C3 1.472(8) . ?
N1 C3 1.472(8) 23_655 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.982(16) 25_665 ?
C1 C3 1.558(13) 11_565 ?
C2 C2 1.554(13) 11_565 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O1M C1M 1.463(16) . ?
O2M C2M 1.321(16) . ?
C1M H1M1 0.9900 . ?
C1M H1M2 0.9900 . ?
C1M C2M 1.442(17) . ?
C2M H2M1 0.9900 . ?
C2M H2M2 0.9900 . ?
