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_7239982
_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         '0.5(C64 H48 Cd2 N4 O24 S4)'
_chemical_formula_sum            'C32 H24 Cd N2 O12 S2'
_chemical_formula_weight         805.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 95.607(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5349(8)
_cell_length_b                   8.6599(6)
_cell_length_c                   26.4575(17)
_cell_measurement_reflns_used    3282
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      73.4440
_cell_measurement_theta_min      3.8320
_cell_volume                     3086.3(3)
_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      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_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    -35.00  34.00   1.00    1.00    --  -40.84  38.00 -30.00   69
  2  \w    -69.00  28.00   1.00    1.00    --  -40.84  57.00  90.00   97
  3  \w   -102.00 -40.00   1.00    1.00    --  -40.84 -77.00-180.00   62
  4  \w     30.00  86.00   1.00    1.00    --  108.54 -77.00 -90.00   56
  5  \w     36.00 118.00   1.00    1.00    --  108.54 -45.00 -60.00   82
  6  \w    109.00 160.00   1.00    1.00    --  108.54  45.00  60.00   51
  7  \w     81.00 178.00   1.00    1.00    --  108.54  30.00 150.00   97
  8  \w    107.00 172.00   1.00    1.00    --  108.54 125.00-150.00   65
  9  \w     33.00  91.00   1.00    1.00    --  108.54 -95.00-180.00   58
;
_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      0.0604571000
_diffrn_orient_matrix_UB_12      -0.0947408000
_diffrn_orient_matrix_UB_13      0.0415102000
_diffrn_orient_matrix_UB_21      0.0969459000
_diffrn_orient_matrix_UB_22      0.0520817000
_diffrn_orient_matrix_UB_23      -0.0208378000
_diffrn_orient_matrix_UB_31      0.0045961000
_diffrn_orient_matrix_UB_32      0.1413386000
_diffrn_orient_matrix_UB_33      0.0355690000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5674
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.747
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18483
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.434
_refine_diff_density_min         -1.522
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0327
_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/[\s^2^(Fo^2^)+(0.0546P)^2^+5.4683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2940
_reflns_number_total             3074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00177e2.cif
_cod_data_source_block           complex-2
_cod_original_cell_volume        3086.3(4)
_cod_database_code               7239982
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cd C H O N'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C14(H14), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              50695
_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 4.098
_oxdiff_exptl_absorpt_empirical_full_min 0.702