Smart crystalline framework materials with a triazole carboxylic acid ligand: fluorescence sensing and catalytic reduction of PNP.
Lv, Qiu; Guan, Qing Lin; Li, Jin Long; Li, Jin Xiao; Jin, Jing; Bai, Feng Ying; Xing, Yong Heng; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02406g

data_7714429
_publ_section_title
;
 Smart crystalline framework materials with a triazole carboxylic acid
 ligand: fluorescence sensing and catalytic reduction of PNP.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02406g
_journal_year                    2023
_chemical_formula_moiety         '0.5(C22 H18 N6 O10 Pb2)'
_chemical_formula_sum            'C11 H9 N3 O5 Pb'
_chemical_formula_weight         470.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-09-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.151(2)
_cell_length_b                   6.596(2)
_cell_length_c                   25.646(8)
_cell_measurement_reflns_used    3773
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.96
_cell_volume                     1209.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            5562
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.957
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.972
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1445 before and 0.0868 after correction.
The Ratio of minimum to maximum transmission is 0.6899.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.686
_refine_diff_density_min         -2.371
_refine_diff_density_rms         0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1306
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0686
_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^)+(0.0795P)^2^+103.6095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1190
_reflns_number_total             1306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt02406g2.cif
_cod_data_source_block           123
_cod_original_cell_volume        1209.7(7)
_cod_database_code               7714429
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.336
_shelx_estimated_absorpt_t_min   0.264
_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,H) groups
2. Restrained distances
 O4-C2 = C2-O16
 1.25 with sigma of 0.02
 C5-C2
 1.48 with sigma of 0.02
 O4-O16
 2.165 with sigma of 0.04
3. Restrained planarity
 O4, C12, C15, C13, C5, C18, C10, O16, C2
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N19) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9) = Uanis(C17)
5. Rigid body (RIGU) restrains
 O11, C1, C7, N3, N19, N14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C12, C5, C13, C18, C15, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, O4, C12, C15, C13, C18, C10, O16, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C9, C17, C7, C2, N14, O11, O16, C1, O20, N3, C15, O4, C13, O8, C5, N19, C18,
 C10, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C1(0.5) O4(0.5) N19(0.5) C12(0.5) C15(0.5) H15(0.5) C13(0.5)
 H13(0.5) C5(0.5) C18(0.5) H18(0.5) C10(0.5) H10(0.5) N3(0.5) N14(0.5) O11(0.5)
 C7(0.5) O8(0.5) O16(0.5) C2(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
 C9(0.5) O20(0.5) H20A(0.5) H20B(0.5)
 Fixed X: O8(0.3174)
 Fixed Y: O8(0.905449)
 Fixed Z: O8(0.45088)
7.a Rotating group:
 O20(H20A,H20B)
7.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C18(H18), C10(H10)
7.c Fitted hexagon refined as free rotating group:
 C12(C15,C13,C5,C18,C10)
7.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              90553
_olex2_submission_special_instructions 'No special instructions were received'