Multiple hydrogen bonded three-dimensional supramolecular architecture composed of unique three-fold interlocked anionic Zn(II)-coordination architecture
Ke, Hua; Chen, Qi-Hua; Liao, Jian-Zhen; Lu, Can-Zhong; CrystEngComm  (2020) –; doi:10.1039/D0CE00177E

data_7239979
_publ_section_title
;
 Multiple hydrogen bonded three-dimensional supramolecular architecture
 composed of unique three-fold interlocked anionic Zn(II)-coordination
 architecture
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00177E
_journal_year                    2020
_chemical_formula_moiety
'C84 H40 N6 O32 Zn2, C12 H36 O6 S6 Zn, 6(C2 H6 O S)'
_chemical_formula_sum            'C108 H112 N6 O44 S12 Zn3'
_chemical_formula_weight         2778.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-09 deposited with the CCDC.	2020-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                88.535(3)
_cell_angle_beta                 73.381(4)
_cell_angle_gamma                61.238(4)
_cell_formula_units_Z            1
_cell_length_a                   12.7067(6)
_cell_length_b                   13.0794(4)
_cell_length_c                   21.0583(8)
_cell_measurement_reflns_used    9313
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      74.1630
_cell_measurement_theta_min      3.8660
_cell_volume                     2913.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -55.00  32.00   1.00    3.00    --  -40.97  57.00 -90.00   87
  2  \w    103.00 129.00   1.00    3.00    --   40.97 175.00 -91.00   26
  3  \w     96.00 178.00   1.00   12.00    --  108.22 125.00-120.00   82
  4  \w    121.00 166.00   1.00   12.00    --  108.22  45.00-120.00   45
  5  \w     85.00 176.00   1.00   12.00    --  108.22  30.00-150.00   91
  6  \w     79.00 161.00   1.00   12.00    --  108.22  61.00 -60.00   82
  7  \w    102.00 128.00   1.00   12.00    --  108.22 125.00 120.00   26
  8  \w     41.00 132.00   1.00   12.00    --  108.22 -45.00 150.00   91
  9  \w     44.00 120.00   1.00   12.00    --  108.22-125.00 120.00   76
 10  \w     61.00 140.00   1.00   12.00    --  108.22 -77.00 -60.00   79
 11  \w     54.00 109.00   1.00   12.00    --  108.22 -95.00 -90.00   55
 12  \w     44.00 135.00   1.00   12.00    --  108.22 -45.00 -90.00   91
 13  \w     31.00 107.00   1.00   12.00    --  108.22 -95.00-180.00   76
 14  \w      2.00  80.00   1.00    3.00    --   40.97 -99.00   0.00   78
 15  \w   -114.00 -17.00   1.00    3.00    --  -40.97 -38.00 120.00   97
 16  \w   -111.00 -26.00   1.00    3.00    --  -40.97 -38.00  30.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1274373000
_diffrn_orient_matrix_UB_12      -0.0948948000
_diffrn_orient_matrix_UB_13      0.0068306000
_diffrn_orient_matrix_UB_21      -0.0631695000
_diffrn_orient_matrix_UB_22      0.0104634000
_diffrn_orient_matrix_UB_23      0.0756259000
_diffrn_orient_matrix_UB_31      -0.0310637000
_diffrn_orient_matrix_UB_32      -0.0962596000
_diffrn_orient_matrix_UB_33      -0.0129912000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20344
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.074
_diffrn_reflns_theta_min         3.890
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.903
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         11462
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0591
_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/[\s^2^(Fo^2^)+(0.0768P)^2^+6.7870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9791
_reflns_number_total             11462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00177e2.cif
_cod_data_source_block           complex-1
_cod_database_code               7239979
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn C H O N S'
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.473
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 S3A-C47A
 1.79 with sigma of 0.02
 S3A-C48A
 1.79 with sigma of 0.02
 C51A-S5A
 1.79 with sigma of 0.02
 S5A-C52A
 1.79 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C47A) = Uanis(C47)
Uanis(C48A) = Uanis(C48)
Uanis(O19A) = Uanis(O19)
Uanis(C51A) = Uanis(C51)
Uanis(C52) = Uanis(C52A)
Uanis(S5A) = Uanis(S5)
Uanis(O21) = Uanis(O21A)
4. Others
 Sof(S3A)=Sof(O19A)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C48A)=
 Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(S3)=Sof(O19)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(H48A)=
 Sof(H48B)=Sof(H48C)=FVAR(1)
 Sof(S5A)=Sof(O21A)=Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C52A)=
 Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(2)
 Sof(S5)=Sof(O21)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C52)=Sof(H52A)=
 Sof(H52B)=Sof(H52C)=FVAR(2)
5.a Rotating group:
 O16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C13(H13A), C14(H14), C18(H18), C19(H19), C21(H21),
 C27(H27), C28(H28), C32(H32), C33(H33), C35(H35), C41(H41), C42(H42)
5.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C47A(H47D,H47E,H47F),
 C48A(H48D,H48E,H48F), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              11979
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.629
_oxdiff_exptl_absorpt_empirical_full_min 0.685