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_7239981
_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         'C34 H26 N4 O12 Zn'
_chemical_formula_sum            'C34 H26 N4 O12 Zn'
_chemical_formula_weight         747.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-05 deposited with the CCDC.	2020-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8776(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1613(2)
_cell_length_b                   8.55650(14)
_cell_length_c                   27.6390(5)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      70.3200
_cell_measurement_theta_min      4.8590
_cell_volume                     3101.28(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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    -67.00 -21.00   1.00    1.00    --    0.00 -57.00  60.00   46
  2  \w     -5.00  21.00   1.00    1.00    --    0.00 -57.00  60.00   26
  3  \w     31.00  64.00   1.00    1.00    --    0.00  57.00-150.00   33
  4  \w    -34.00  11.00   1.00    1.00    --    0.00  93.00-170.00   45
  5  \w      5.00  67.00   1.00    2.00    --   54.00 -57.00   0.00   62
  6  \w     35.00 108.00   1.00    2.00    --   54.00-125.00 -60.00   73
  7  \w     23.00  72.00   1.00    2.00    --   54.00-125.00 120.00   49
  8  \w     10.00 127.00   1.00    2.00    --   54.00  19.00 -60.00  117
  9  \w    -10.00  69.00   1.00    2.00    --   54.00 -57.00 120.00   79
 10  \w     28.00 118.00   1.00    2.00    --   54.00  77.00 -30.00   90
 11  \w     65.00 134.00   1.00    2.00    --  108.00 178.00 -60.00   69
 12  \w    148.00 177.00   1.00    2.00    --  108.00  25.00  60.00   29
 13  \w    118.00 159.00   1.00    2.00    --  108.00 111.00 -60.00   41
 14  \w     35.00 140.00   1.00    2.00    --  108.00 -25.00   0.00  105
 15  \w     41.00 113.00   1.00    2.00    --  108.00 -63.00  30.00   72
 16  \w     36.00 113.00   1.00    2.00    --  108.00-111.00 -90.00   77
 17  \w     39.00 110.00   1.00    2.00    --  108.00-111.00-180.00   71
 18  \w     40.00 101.00   1.00    2.00    --  108.00 -63.00-120.00   61
 19  \w    114.00 178.00   1.00    2.00    --  108.00  50.00  30.00   64
 20  \w     56.00  84.00   1.00    2.00    --  108.00 -25.00 120.00   28
 21  \w     48.00 113.00   1.00    2.00    --  108.00-111.00  60.00   65
 22  \w     75.00 104.00   1.00    2.00    --  108.00  25.00  60.00   29
 23  \w     39.00 129.00   1.00    2.00    --  108.00 -38.00 -90.00   90
 24  \w     75.00 178.00   1.00    2.00    --  108.00  25.00 -30.00  103
 25  \w    105.00 136.00   1.00    2.00    --  108.00 -91.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0258361000
_diffrn_orient_matrix_UB_12      0.1361668000
_diffrn_orient_matrix_UB_13      -0.0353895000
_diffrn_orient_matrix_UB_21      0.0486842000
_diffrn_orient_matrix_UB_22      0.1160160000
_diffrn_orient_matrix_UB_23      0.0378100000
_diffrn_orient_matrix_UB_31      0.1037054000
_diffrn_orient_matrix_UB_32      -0.0205577000
_diffrn_orient_matrix_UB_33      -0.0211815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            19904
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.501
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         5886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0545P)^2^+0.9765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5151
_reflns_number_total             5886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00177e2.cif
_cod_data_source_block           complex-4
_cod_database_code               7239981
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Zn'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_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:
 C4(H4), C5(H5), C7(H7), C13(H13), C14(H14), C18(H18), C19(H19), C23(H23),
 C26(H26), C27(H27), C29(H29), C32(H32)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O10(H10)
;
_shelx_res_checksum              47379
_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 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.575