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_7042642
_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         'C126 H84 N26 Pd6, 6(F6 P)'
_chemical_formula_sum            'C126 H84 F36 N26 P6 Pd6'
_chemical_formula_weight         3470.41
_space_group_crystal_system      hexagonal
_space_group_IT_number           175
_space_group_name_Hall           '-P 6'
_space_group_name_H-M_alt        'P 6/m'
_symmetry_space_group_name_Hall  '-P 6'
_symmetry_space_group_name_H-M   'P 6/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-10
_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                120
_cell_formula_units_Z            2
_cell_length_a                   29.983(4)
_cell_length_b                   29.983(4)
_cell_length_c                   11.399(2)
_cell_measurement_reflns_used    2016
_cell_measurement_temperature    291.15
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     8875(2)
_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      291.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            44418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.244
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.862
_refine_diff_density_min         -2.185
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0779
_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^)+(0.1347P)^2^+66.7061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4392
_reflns_number_total             5921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00179g2.cif
_cod_data_source_block           jxf111_sq
_cod_original_cell_volume        8875(3)
_cod_database_code               7042642
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P1-F2
 1.7 with sigma of 0.02
 C16-C18A
 2.4 with sigma of 0.02
 C17-C18A
 1.4 with sigma of 0.02
 C18A-C19A
 1.4 with sigma of 0.02
 F2-F8
 3 with sigma of 0.02
 F1-P1
 1.7 with sigma of 0.02
 F1-F2 \\sim F2-F5
 with sigma of 0.02
 F4-F3 \\sim F3-F2
 with sigma of 0.02
 F8-F6 \\sim F6-F10
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 P1, P2, F3, F4, F1, F2, F5, F6, F7, F8, F9, F10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20A, C20, C19, C19A, C18A, C18, C17, N5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(C20)=Sof(H20)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=FVAR(1)
 Fixed Sof: F2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C11(H11), C12(H12), C14(H14), C15(H15), C20(H20), C18(H18),
 C21(H21), C4(H4), C5(H5), C6(H6), C3(H3), C19(H19), C18A(H18A), C19A(H19A),
 C20A(H20A)
;
_shelx_res_checksum              2333
_shelx_fab_checksum              26223
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'