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_7044466
_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
'C136 H168 N24 O16 Pd2, C3 H6 F, 10(C3 H6 O), 4(F6 P), 3(H2 O)'
_chemical_formula_sum            'C169 H240 F25 N24 O29 P4 Pd2'
_chemical_formula_weight         3883.54
_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                111.241(2)
_cell_angle_beta                 99.224(2)
_cell_angle_gamma                106.691(2)
_cell_formula_units_Z            2
_cell_length_a                   18.3978(4)
_cell_length_b                   23.2250(5)
_cell_length_c                   26.4301(7)
_cell_measurement_reflns_used    12269
_cell_measurement_temperature    175
_cell_measurement_theta_max      24.7600
_cell_measurement_theta_min      1.9140
_cell_volume                     9630.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (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      175
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.752
_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     29.00  73.00   1.00  185.00    --    6.16  57.00 -60.00   44
  2  \w      3.00  71.00   1.00  185.00    --    6.16  38.00 -90.00   68
  3  \w    -16.00  34.00   1.00  185.00    --   -5.46-100.00 -30.00   50
  4  \w      1.00  32.00   1.00  185.00    --   -5.46-100.00 -90.00   31
  5  \w    -19.00  45.00   1.00  185.00    --    6.16-100.00  90.00   64
  6  \w    -66.00  18.00   1.00  185.00    --    6.16 -19.00 120.00   84
;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0102456000
_diffrn_orient_matrix_UB_12      -0.0249016000
_diffrn_orient_matrix_UB_13      -0.0281091000
_diffrn_orient_matrix_UB_21      0.0399731000
_diffrn_orient_matrix_UB_22      0.0022674000
_diffrn_orient_matrix_UB_23      0.0043367000
_diffrn_orient_matrix_UB_31      -0.0085352000
_diffrn_orient_matrix_UB_32      -0.0249882000
_diffrn_orient_matrix_UB_33      0.0099881000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60277
_diffrn_reflns_theta_full        20.820
_diffrn_reflns_theta_max         24.905
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4062
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.14
_refine_diff_density_min         -0.98
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1334
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2347
_refine_ls_number_reflns         18665
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.0025015
_refine_ls_shift/su_mean         0.0000481
_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: 
 14.8 12.9 13.4 4.58 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0830
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0693
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              25
_reflns_limit_k_min              -26
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                18665
_reflns_number_total             25242
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      10.25
_oxford_refine_ls_r_factor_ref   0.0613
_oxford_refine_ls_scale          0.7491(11)
_oxford_reflns_number_all        25240
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c7dt03517a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        9630.5(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7044466
_cell_oxdiff_length_a            18.3978(4)
_cell_oxdiff_length_b            23.2250(5)
_cell_oxdiff_length_c            26.4301(7)
_cell_oxdiff_angle_alpha         111.241(2)
_cell_oxdiff_angle_beta          99.224(2)
_cell_oxdiff_angle_gamma         106.691(2)
_cell_oxdiff_volume              9630.5(4)
_oxdiff_exptl_absorpt_empirical_full_min 0.922
_oxdiff_exptl_absorpt_empirical_full_max 1.087
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_montpellier_reflns_maxres       0.84
_montpellier_reflns_completeness_maxres 75.17
_montpellier_reflns_redundancy_maxres 2.39