Chloride triggered reversible switching from a metallosupramolecular [Pd2L4]^4+^ cage to a [Pd2L2Cl4] metallo-macrocycle with release of endo- and exo-hedrally bound guests
Dan Preston; Alyssa Fox-Charles; Warrick K. C. Lo; James D. Crowley; Chem.Commun. 51 (2015) 9042–; doi:10.1039/C5cc02226F

data_7117180
_publ_section_title
;
 Chloride triggered reversible switching from a metallosupramolecular
 [Pd2L4]^4+^ cage to a [Pd2L2Cl4] metallo-macrocycle with release of endo-
 and exo-hedrally bound guests
;
_journal_name_full               Chem.Commun.
_journal_page_first              9042
_journal_paper_doi               10.1039/C5cc02226F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C126 H150 N16 O38 Pd2 S4'
_chemical_formula_weight         2837.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-13 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.566(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.099
_cell_length_b                   17.179
_cell_length_c                   32.2500(10)
_cell_measurement_reflns_used    37475
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.4700
_cell_measurement_theta_min      3.0970
_cell_volume                     7254.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir-2011
_diffrn_ambient_temperature      100.01(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            105476
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63630
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2956
_exptl_crystal_size_max          0.3331
_exptl_crystal_size_mid          0.1913
_exptl_crystal_size_min          0.1555
_platon_squeeze_details
;
there was residual electron density which could not be
resolved consisting of a total electron count of 868,
which we attribute to the missing ends (CH2CH2OCH3) of two
diglyme chains per cage (4 in total, 156 electrons) and 18 
DMF solvent molecules (720 electrons).
;
_refine_diff_density_max         4.230
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.860
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         14267
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.871
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.1103
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3733
_refine_ls_wR_factor_ref         0.3871
_reflns_number_gt                12733
_reflns_number_total             14267
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5cc02226f2.cif
_cod_data_source_block           dp217mes
_cod_database_code               7117180
_platon_squeeze_void_probe_radius 1.20