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_7245949
_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             2022-11-04
_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                   29.9967(4)
_cell_length_b                   17.1308(2)
_cell_length_c                   14.7811(2)
_cell_measurement_reflns_used    10484
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      76.9440
_cell_measurement_theta_min      2.9240
_cell_volume                     7595.53(17)
_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      100.00(14)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18600
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.507
_diffrn_reflns_theta_min         3.333
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57423
_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    1.033
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 2619 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.044(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7626
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0518
_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^)+(0.1031P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.922
_reflns_number_gt                6610
_reflns_number_total             7626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01530g2.cif
_cod_data_source_block           R-1
_cod_depositor_comments
'Adding full bibliography for 7245949--7245950.cif.'
_cod_original_formula_sum        'C30 H28 N4 O3 Zn1.50'
_cod_database_code               7245949
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.760
_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. Uiso/Uaniso restraints and constraints
C30 \\sim C29 \\sim C28: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
3.a Rotating group:
 O3(H3a,H3b)
3.b Ternary CH refined with riding coordinates:
 C13(H13), C18(H18)
3.c Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C17(H17a,H17b), C15(H15a,H15b), C16(H16a,H16b)
3.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C8(H8), C19(H19), C12(H12), C7(H7), C5(H5), C21(H21), C1(H1),
 C24(H24), C2(H2), C4(H4), C22(H22), C29(H29), C28(H28), C27(H27), C30(H30)
3.e Fitted hexagon refined as free rotating group:
 C29(N4,C28,C27,C26,C30)
;
_shelx_res_checksum              71717
_shelx_hkl_checksum              85964
_shelx_fab_checksum              12436
_olex2_submission_special_instructions 'No special instructions were received'