Hydrophobic metallo-supramolecular Pd2L4 Cages for zwitterionic guest encapsulation in organic solvents
Li, Yuhao; Zhang, Yan; Legrand, Yves-Marie; Van der Lee, Arie; Jiang, Ji-Jun; Chen, Cheng-Xia; Su, Cheng-Yong; Barboiu, Mihail; Dalton Trans.  (2017) –; doi:10.1039/C7DT03517A

data_7044467
_publ_section_title
;
 Hydrophobic metallo-supramolecular Pd2L4 Cages for zwitterionic guest
 encapsulation in organic solvents
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03517A
_journal_year                    2017
_chemical_formula_moiety         'C88 H70 N24 O8 Pd2, 4(C2 H6 O S)'
_chemical_formula_sum            'C96 H94 N24 O12 Pd2 S4'
_chemical_formula_weight         2117.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_update_record
;
2017-08-31 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                64.366(2)
_cell_angle_beta                 86.1457(17)
_cell_angle_gamma                65.272(2)
_cell_formula_units_Z            2
_cell_length_a                   19.2335(4)
_cell_length_b                   21.0093(5)
_cell_length_c                   23.2406(5)
_cell_measurement_reflns_used    15417
_cell_measurement_temperature    150
_cell_measurement_theta_max      65.1750
_cell_measurement_theta_min      3.9250
_cell_volume                     7615.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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    -44.00  33.00   1.00   30.00    --  -40.95  38.00 -30.00   77
  2  \w    -50.00  33.00   1.00   30.00    --  -40.95  38.00  90.00   83
  3  \w    -66.00  22.00   1.00   30.00    --  -40.95  57.00-150.00   88
  4  \w     63.00 166.00   1.00   90.00    --   89.96  30.00 -90.00  103
  5  \w     64.00 163.00   1.00   90.00    --   89.96  45.00   0.00   99
  6  \w     17.00  98.00   1.00   90.00    --   89.96 -45.00   0.00   81
  7  \w     94.00 133.00   1.00   90.00    --   89.96 125.00 -60.00   39
  8  \w     34.00 123.00   1.00   90.00    --   89.96 -77.00-180.00   89
  9  \w     23.00 121.00   1.00   90.00    --   89.96-125.00-180.00   98
 10  \w     15.00 120.00   1.00   90.00    --   89.96 -77.00 -60.00  105
;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0079286000
_diffrn_orient_matrix_UB_12      -0.0717085000
_diffrn_orient_matrix_UB_13      0.0039009000
_diffrn_orient_matrix_UB_21      -0.0367667000
_diffrn_orient_matrix_UB_22      -0.0086558000
_diffrn_orient_matrix_UB_23      0.0623277000
_diffrn_orient_matrix_UB_31      -0.0807141000
_diffrn_orient_matrix_UB_32      0.0540532000
_diffrn_orient_matrix_UB_33      -0.0401519000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24869
_diffrn_reflns_theta_full        65.338
_diffrn_reflns_theta_max         65.338
_diffrn_reflns_theta_min         3.546
_exptl_absorpt_coefficient_mu    2.804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.80
_refine_diff_density_min         -1.09
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         20197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.0018073
_refine_ls_shift/su_mean         0.0001900
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 14.1 -4.01 10.6 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0744
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0673
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              24
_reflns_limit_k_min              -21
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                20197
_reflns_number_total             24869
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.78
_oxford_diffrn_Wilson_scale      0.22
_oxford_refine_ls_r_factor_ref   0.0654
_oxford_refine_ls_scale          2.170(2)
_oxford_reflns_number_all        24869
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c7dt03517a2.cif
_cod_data_source_block           1_CCDC1
_cod_original_cell_volume        7615.89(18)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7044467
_cell_oxdiff_length_a            19.2335(4)
_cell_oxdiff_length_b            21.0093(5)
_cell_oxdiff_length_c            23.2406(5)
_cell_oxdiff_angle_alpha         64.366(2)
_cell_oxdiff_angle_beta          86.1457(17)
_cell_oxdiff_angle_gamma         65.272(2)
_cell_oxdiff_volume              7615.9(3)
_oxdiff_exptl_absorpt_empirical_full_min 0.788
_oxdiff_exptl_absorpt_empirical_full_max 1.314
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_montpellier_reflns_maxres       0.85
_montpellier_reflns_completeness_maxres 95.17
_montpellier_reflns_redundancy_maxres 1.66