Self-Assembly of Tripyrazolate-Linked [M6L2] Cages for Selective Sensing of HSO3- and gas SO2 by Turn-on Fluorescence
Wang, Pei-Pei; Tong, Jin; Meng, Cong; Yuan, Qing; Deng, Wei; Yu, Shu-Yan; Dalton Transactions  (2023) –; doi:10.1039/D3DT00083D

data_7712420
_publ_section_title
;
 Self-Assembly of Tripyrazolate-Linked [M6L2] Cages for Selective Sensing
 of HSO3- and gas SO2 by Turn-on Fluorescence
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00083D
_journal_year                    2023
_chemical_formula_moiety
'C120 H78 F18 N26 Pd6, 7(C2 H6 O S), 5(F6 P), 8(C4 H8 O2), 7(H2 O)'
_chemical_formula_sum            'C166 H198 F48 N26 O30 P5 Pd6 S7'
_chemical_formula_weight         4967.16
_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   geom
_audit_creation_date             2023-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-20 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.8350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   55.0704(4)
_cell_length_b                   31.5923(2)
_cell_length_c                   26.9571(2)
_cell_measurement_reflns_used    136187
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2290
_cell_measurement_theta_min      2.7000
_cell_volume                     42212.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_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     -2.00  24.00   0.50    1.70    --  -47.73  51.00-147.00   52
  2  \w   -114.00 -40.00   0.50    1.70    --  -47.73 -51.00  66.00  148
  3  \w      4.00  30.00   0.50    1.70    --   47.73 -51.00  66.00   52
  4  \w     78.00 103.00   0.50    1.70    --   47.73  51.00-147.00   50
  5  \w   -129.00 -96.00   0.50    8.00    --  -99.00 -51.00  66.00   66
  6  \w    -54.00 -27.00   0.50    8.00    --  -99.00  51.00-147.00   54
  7  \w     94.00 143.00   0.50    8.00    --  104.70  51.00-147.00   98
  8  \w     34.00  59.00   0.50    8.00    --  104.70 -51.00  66.00   50
  9  \w    -14.00  26.00   0.50    1.70    --  -47.73  19.00   0.00   80
 10  \w    -37.00  24.00   0.50    1.70    --  -47.73  38.00  30.00  122
 11  \w    -23.00  18.00   0.50    1.70    --  -47.73  19.00 -30.00   82
 12  \w   -119.00 -27.00   0.50    1.70    --  -47.73 -77.00  30.00  184
 13  \w     36.00  95.00   0.50    1.70    --   47.73  57.00 -30.00  118
 14  \w     77.00 119.00   0.50    1.70    --   47.73  38.00   0.00   84
 15  \w    -69.00 -27.00   0.50    8.00    --  -99.00  61.00-180.00   84
 16  \w    -69.00 -30.00   0.50    8.00    --  -99.00  61.00-120.00   78
 17  \w   -111.00 -85.00   0.50    8.00    --  -99.00 -61.00 -30.00   52
 18  \w   -111.00 -83.00   0.50    8.00    --  -99.00 -62.00 -36.97   56
 19  \w   -134.00 -82.00   0.50    8.00    --  -99.00 -72.00 -40.76  104
 20  \w   -162.00 -88.00   0.50    8.00    --  -99.00 -61.00 -60.00  148
 21  \w   -101.00 -60.00   0.50    8.00    --  -99.00  77.00 -60.00   82
 22  \w    -57.00 -29.00   0.50    8.00    --  -99.00  77.00 -60.00   56
 23  \w    -69.00 -44.00   0.50    8.00    --  -99.00  61.00   0.00   50
 24  \w   -137.00 -92.00   0.50    8.00    --  -99.00 -49.00 -36.08   90
 25  \w   -171.00-131.00   0.50    8.00    --  -99.00 -61.00 150.00   80
 26  \w   -156.00 -90.00   0.50    8.00    --  -99.00 -45.00 -90.00  132
 27  \w   -168.00-128.00   0.50    8.00    --  -99.00 -75.00 -25.10   80
 28  \w   -170.00-122.00   0.50    8.00    --  -99.00 -77.00   0.00   96
 29  \w   -151.00 -89.00   0.50    8.00    --  -99.00 -15.00 -30.00  124
 30  \w   -102.00 -77.00   0.50    8.00    --  -99.00 -77.00   0.00   50
 31  \w   -168.00-102.00   0.50    8.00    --  -99.00 -45.00  90.00  132
 32  \w   -136.00 -86.00   0.50    8.00    --  -99.00 -61.00   0.00  100
 33  \w   -116.00 -85.00   0.50    8.00    --  -99.00 -61.00 150.00   62
 34  \w   -167.00 -86.00   0.50    8.00    --  -99.00 -77.00  30.00  162
 35  \w   -153.00-103.00   0.50    8.00    --  -99.00 -61.00-180.00  100
 36  \w    -67.00 -40.00   0.50    8.00    --  -99.00  61.00  60.00   54
 37  \w   -103.00 -78.00   0.50    8.00    --  -99.00 -77.00 -30.00   50
 38  \w     34.00  70.00   0.50    8.00    --  104.70 -61.00  30.00   72
 39  \w    146.00 171.00   0.50    8.00    --  104.70  30.00  30.00   50
 40  \w     33.00  65.00   0.50    8.00    --  104.70 -61.00 -90.00   64
 41  \w    100.00 127.00   0.50    8.00    --  104.70  30.00  30.00   54
 42  \w     41.00  66.00   0.50    8.00    --  104.70 -61.00  90.00   50
 43  \w    145.00 172.00   0.50    8.00    --  104.70  30.00 150.00   54
 44  \w     94.00 120.00   0.50    8.00    --  104.70  30.00 150.00   52
 45  \w     34.00  71.00   0.50    8.00    --  104.70 -61.00 -60.00   74
 46  \w     33.00  58.00   0.50    8.00    --  104.70 -61.00-120.00   50
 47  \w     79.00 105.00   0.50    8.00    --  104.70 -95.00-120.00   52
 48  \w     41.00  67.00   0.50    8.00    --  104.70 -95.00-120.00   52
 49  \w    103.00 178.00   0.50    8.00    --  104.70  30.00 120.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0164143000
_diffrn_orient_matrix_UB_12      0.0231522000
_diffrn_orient_matrix_UB_13      0.0253137000
_diffrn_orient_matrix_UB_21      0.0438281000
_diffrn_orient_matrix_UB_22      -0.0199563000
_diffrn_orient_matrix_UB_23      0.0168256000
_diffrn_orient_matrix_UB_31      0.0329168000
_diffrn_orient_matrix_UB_32      0.0380085000
_diffrn_orient_matrix_UB_33      -0.0065641000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            301265
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.116
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             20088
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         4.082
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1946
_refine_ls_number_reflns         42932
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.1317
_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^)+(0.1100P)^2^+999.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3211
_refine_ls_wR_factor_ref         0.3255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                36391
_reflns_number_total             42932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00083d2.cif
_cod_data_source_block           a_sq
_cod_original_cell_volume        42212.4(6)
_cod_database_code               7712420
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     2207168977
_shelx_estimated_absorpt_t_max   0.410
_shelx_estimated_absorpt_t_min   0.364
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 F1-C10 \\sim F3-C10 \\sim F2-C10 \\sim F78-C10 \\sim F77-C10 \\sim F79-C10
 with sigma of 0.02
 F77-F78 \\sim F78-F79 \\sim F77-F79
 with sigma of 0.02
 F2-F1 \\sim F1-F3 \\sim F2-F3
 with sigma of 0.02
 F41-F38 \\sim F38-F40
 with sigma of 0.02
 P6-F80 \\sim P6-F81 \\sim P6-F82 \\sim P6-F85 \\sim P6-F83 \\sim P6-F84
 with sigma of 0.02
 F82-F81 \\sim F81-F83 \\sim F82-F80 \\sim F80-F83 \\sim F80-F85 \\sim F85-F81
 with sigma of 0.02
 F16-F18 \\sim F18-F17 \\sim F16-F17
 with sigma of 0.01
 F17-C04A \\sim F16-C04A \\sim F18-C04A
 with sigma of 0.02
3. Rigid bond restraints
 P5, F44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N17 \\sim C75 \\sim C74 \\sim C73 \\sim C72 \\sim C71: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F81 \\sim P6 \\sim F82 \\sim F83 \\sim F85 \\sim F84 \\sim F80: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
N15 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C30) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(F43) \\sim Ueq, Uanis(F44) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F18) \\sim Ueq, Uanis(F11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(F77)=Sof(F78)=Sof(F79)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Fixed Sof: P6(0.5) F82(0.5) F83(0.5) F85(0.5) F84(0.5) F80(0.5) F81(0.5)
6.a Me refined with riding coordinates:
 C30(H30A,H30B,H30C)
6.b Aromatic/amide H refined with riding coordinates:
 C64(H64), C63(H63), C62(H62), C61(H61), C74(H74), C73(H73), C72(H72),
 C71(H71), C104(H104), C103(H103), C102(H102), C101(H101), C01K(H01K), C2(H2),
 C02B(H02B), C02C(H02C), C02Q(H02Q), C3(H3), C5(H5), C6(H6), C8(H8), C12(H12),
 C13(H13), C15(H15), C16(H16), C18(H18), C32(H32), C033(H033), C33(H33),
 C35(H35), C36(H36), C38(H38), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48),
  C52(H52), C53(H53), C55(H55), C56(H56), C58(H58), C67(H67), C68(H68),
 C69(H69), C70(H70), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82),
  C83(H83), C84(H84), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91),
 C92(H92), C93(H93), C94(H94), C97(H97), C98(H98), C99(H99), C100(H100),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C117(H117), C118(H118), C119(H119), C120(H120)
6.c Fitted hexagon refined as free rotating group:
 N15(C65,C64,C63,C62,C61), N17(C75,C74,C73,C72,C71), N23(C105,C104,C103,C102,
 C101)
6.d Idealised Me refined as rotating group:
 C03S(H03A,H03B,H03C), C05U(H05A,H05B,H05C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              25221
_shelx_hkl_checksum              66074
_shelx_fab_checksum              29030
_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 1.867
_oxdiff_exptl_absorpt_empirical_full_min 0.597