Fluorescent Zn(II) frameworks with multicarboxylate and pyridyl N-donor ligands for sensing specific anions and organic molecules
Zhao, Shu-Man; Qiu, Zhao-Feng; Xu, Zou-Hong; huang, ziqing; Zhao, Yue; Sun, Wei-Yin; Dalton Transactions  (2022) –; doi:10.1039/D1DT04052A

data_7709392
_publ_section_title
;
 Fluorescent Zn(II) frameworks with multicarboxylate and pyridyl N-donor
 ligands for sensing specific anions and organic molecules
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04052A
_journal_year                    2022
_chemical_formula_moiety         'C56 H38 N6 O8 Zn2, 1[C3H7NO], 1[C3H7NO]'
_chemical_formula_sum            'C62 H52 N8 O10 Zn2'
_chemical_formula_weight         1199.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-27 deposited with the CCDC.	2022-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.559(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   45.953(3)
_cell_length_b                   6.8308(4)
_cell_length_c                   18.9183(12)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      59.477
_cell_measurement_theta_min      4.071
_cell_volume                     5522.9(6)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2019)
;
_computing_data_collection       'Bruker BIS V6.2.14'
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2019)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON III'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.404
_diffrn_reflns_theta_min         1.799
_diffrn_source                   MetalJet
_diffrn_source_type              'Liquid Metal source'
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1095 before and 0.0842 after correction.
The Ratio of minimum to maximum transmission is 0.8654.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0618P)^2^+5.1361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4336
_reflns_number_total             6184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04052a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        5523.0(6)
_cod_database_code               7709392
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
N4A \\sim N4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
3. Others
 Sof(C27A)=Sof(H27A)=Sof(C28A)=1-FVAR(1)
 Sof(C27)=Sof(C28)=Sof(H28)=FVAR(1)
 Sof(N4A)=Sof(H4AA)=Sof(H4AB)=0.5*(1-FVAR(3))
 Sof(N4)=Sof(H4A)=Sof(H4B)=0.5*FVAR(3)
 Fixed Sof: H19(0.5) H27(0.27936) N3(0.5) H3A(0.5) H3B(0.5) H28A(0.22063)
4.a Riding coordinates:
 C27(H27), C28A(H28A)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C20(H20), C19(H19), C13(H13), C3(H3), C14(H14), C8(H8),
 C22(H22), C21(H21), C4(H4), C25(H25), C11(H11), C24(H24), C9(H9), C10(H10),
 C28(H28), C27A(H27A)
4.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N4A(H4AA,H4AB)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 232 electrons were
found in a volume of 1144\%A^3^ in 2 voids per unit cell.
This is consistent with the presence of 1[C3H7NO], 1[C3H7NO] per Formula Unit
which account for 320 electrons per unit cell.
The electron count is a little lower than expected - this is due to the disorder
present in this structure. There is no doubt that two molecules of DMF exist
here (and these could even be modeled, at a push).
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46872
_shelx_fab_checksum              62238
_olex2_submission_special_instructions 'No special instructions were received'