Chiral two-dimensional metal–organic frameworks based on Zn(salen) ligands: subcomponent self-assembly and circularly polarised luminescence
Wang, Xue-Zhi; Zhou, Chuang-Wei; Wang, Bei; Lai, Ya-Liang; Lian, Zhao-Xia; Liu, Yi-Tong; Li, Yan Yan; Zhou, Xiao-Ping; CrystEngComm 25 (2023) 484–489; doi:10.1039/D2CE01530G

data_7245950
_publ_section_title
;
 Chiral two-dimensional metal--organic frameworks based on Zn(salen)
 ligands: subcomponent self-assembly and circularly polarised luminescence
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              484
_journal_page_last               489
_journal_paper_doi               10.1039/D2CE01530G
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C30 H28 N4 O3 Zn1.5'
_chemical_formula_sum            'C30 H28 N4 O3 Zn1.5'
_chemical_formula_weight         590.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-30 deposited with the CCDC.	2022-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7259(2)
_cell_length_b                   17.3191(2)
_cell_length_c                   30.0077(4)
_cell_measurement_reflns_used    10757
_cell_measurement_temperature    99.98(12)
_cell_measurement_theta_max      74.6680
_cell_measurement_theta_min      2.9590
_cell_volume                     7653.14(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(12)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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     10.00  37.00   0.50    4.00    --    0.00  33.00-175.00   54
  2  \w    -39.00  -8.00   0.50    4.00    --    0.00 -33.00  25.00   62
  3  \w     46.00  71.00   0.50   17.00    --  102.90 -33.00  25.00   50
  4  \w     98.00 162.00   0.50   17.00    --  102.90  33.00-175.00  128
  5  \w    -17.00  34.00   0.50    4.00    --    0.00  82.00-180.00  102
  6  \w    -28.00  36.00   0.50    4.00    --    0.00  82.00  60.00  128
  7  \w    121.00 192.00   0.50   17.00    --  102.90  38.00 -90.00  142
  8  \w     15.00 125.00   0.50   17.00    --  102.90 -38.00 -60.00  220
  9  \w     14.00 127.00   0.50   17.00    --  102.90 -57.00-150.00  226
 10  \w     66.00 123.00   0.50   17.00    --  102.90 -57.00   0.00  114
 11  \w     17.00 125.00   0.50   17.00    --  102.90 -38.00-150.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0636403000
_diffrn_orient_matrix_UB_12      0.0095962000
_diffrn_orient_matrix_UB_13      0.0403756000
_diffrn_orient_matrix_UB_21      0.0726405000
_diffrn_orient_matrix_UB_22      -0.0361046000
_diffrn_orient_matrix_UB_23      0.0304600000
_diffrn_orient_matrix_UB_31      0.0401146000
_diffrn_orient_matrix_UB_32      0.0807827000
_diffrn_orient_matrix_UB_33      0.0087594000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            19488
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.574
_diffrn_reflns_theta_min         2.946
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 3080 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7630
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0756P)^2^+8.2668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                7300
_reflns_number_total             7630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01530g2.cif
_cod_data_source_block           S-1
_cod_depositor_comments
'Adding full bibliography for 7245949--7245950.cif.'
_cod_original_formula_sum        'C30 H28 N4 O3 Zn1.50'
_cod_database_code               7245950
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         CHONZn
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.762
_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, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 C4, C5, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C5 \\sim N1 \\sim C4: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
4.a Rotating group:
 O3(H3a,H3b)
4.b Ternary CH refined with riding coordinates:
 C18(H18), C13(H13)
4.c Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C14(H14a,H14b), C16(H16a,H16b), C15(H15a,H15b)
4.d Aromatic/amide H refined with riding coordinates:
 C24(H24), C12(H12), C21(H21), C11(H11), C22(H22), C19(H19), C30(H30),
 C27(H27), C28(H28), C29(H29), C8(H8), C7(H7), C2(H2), C1(H1), C5(H5), C4(H4)
4.e Fitted hexagon refined as free rotating group:
 C30(C26,C27,C28,N4,C29), C2(C1,N1,C5,C4,C3)
;
_shelx_res_checksum              26563
_shelx_hkl_checksum              80956
_shelx_fab_checksum              24149
_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 1.915
_oxdiff_exptl_absorpt_empirical_full_min 0.681