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_7117179
_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            'C58 H62 Cl4 N6 O12 Pd2'
_chemical_formula_weight         1389.73
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-03-13 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.982(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8958(6)
_cell_length_b                   21.0537(7)
_cell_length_c                   11.1192(5)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3740
_cell_measurement_theta_min      4.0560
_cell_volume                     3182.1(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-2014 (Sheldrick, 2014)'
_computing_structure_solution    Superflip
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7617
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         76.318
_diffrn_reflns_theta_min         3.871
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47054
_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            yellow
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.1658
_exptl_crystal_size_mid          0.1298
_exptl_crystal_size_min          0.0837
_platon_squeeze_details
;
The crystal lattice contained a large amount of diffuse
 electron density that could not be appropriately modelled. The 
SQUEEZE routine within PLATON was employed to resolve this problem, 
resulting in void electrons
count of 116 that we assign to 2.5 DMF solvent molecules (100
electrons in total). 
;
_refine_diff_density_max         2.795
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1128P)^2^+4.7545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                2898
_reflns_number_total             3299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02226f2.cif
_cod_data_source_block           Pd2macrocyle
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 3392 2015-05-12 13:50:21Z andrius 
;
_cod_database_code               7117179
_shelxl_version_number           2014-3
_shelx_res_checksum              68231
_shelx_hkl_checksum              6227
_platon_squeeze_void_probe_radius 1.20