Self-Assembly and Anion sensing of Metal-organic [M6L2] Cages from Fluorescent Triphenylamine Tri-pyrazoles with Dipalladium(II,II) Corners
Cui, Yu; Chen, Zi-Man; Jiang, Xuan-Feng; Tong, Jin; Yu, Shu-Yan; Dalton Trans.  (2017) –; doi:10.1039/C7DT00179G

data_7042641
_publ_section_title
;
 Self-Assembly and Anion sensing of Metal-organic [M6L2] Cages from
 Fluorescent Triphenylamine Tri-pyrazoles with Dipalladium(II,II) Corners
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00179G
_journal_year                    2017
_chemical_formula_moiety         'C63 H53 N13 Pd3, 12(F1.5 P0.25), C2 H3 N'
_chemical_formula_sum            'C65 H56 F18 N14 P3 Pd3'
_chemical_formula_weight         1787.34
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   58.295(7)
_cell_length_b                   11.9914(14)
_cell_length_c                   24.911(3)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.736
_cell_measurement_theta_min      2.197
_cell_volume                     17414(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1759
_diffrn_reflns_av_unetI/netI     0.1789
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92048
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.151
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       Prism
_exptl_crystal_F_000             7112
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.681
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         16623
_refine_ls_number_restraints     1203
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.2202
_refine_ls_R_factor_gt           0.1171
_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^)+(0.1358P)^2^+235.8990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2768
_refine_ls_wR_factor_ref         0.3293
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8031
_reflns_number_total             16623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00179g2.cif
_cod_data_source_block           w_sq
_cod_database_code               7042641
_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
 F28-P7
 1.9 with sigma of 0.02
 C64-N14
 1.2 with sigma of 0.02
 C64-C65
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(Pd3) \\sim Ueq, Uanis(Pd4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(F3) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F2) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(F7) \\sim Ueq, Uanis(P2) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F8) \\sim
Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: P1(0.25) F1(0.25) F2(0.25) F3(0.25) F4(0.25) F5(0.5) P2(0.25)
 F6(0.25) F7(0.5) F8(0.25) F9(0.5) P4(0.375) F15(0.375) F16(0.75) F17(0.75)
 F18(0.375) P5(0.375) F19(0.375) F20(0.375) F21(0.375) F22(0.375) F23(0.75)
 P7(0.25) F28(0.25) F29(0.25) F30(0.25) F31(0.25) F32(0.5) H65A(0.5) H65B(0.5)
 H65C(0.5) H67A(0.5) H67B(0.5) H67C(0.5)
6.a Riding coordinates:
 C65(H65A,H65B,H65C)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26),
  C27(H27), C29(H29), C31(H31), C32(H32), C35(H35), C37(H37), C38(H38),
 C41(H41), C43(H43), C47(H47), C49(H49), C50(H50), C53(H53), C55(H55), C56(H56),
  C58(H58), C59(H59), C61(H61)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C39(H39A,H39B,H39C), C45(H45A,H45B,H45C), C51(H51A,H51B,
 H51C), C57(H57A,H57B,H57C), C63(H63A,H63B,H63C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              26665
_shelx_fab_checksum              93457
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'