Selective separation of planar and non-planar hydrocarbons using an aqueous Pd6 interlocked cage
Chakraborty, Debsena; Saha, Rupak; Clegg, Jack Kay; Mukherjee, Partha Sarathi; Chemical Science  (2022) –; doi:10.1039/D2SC04660A

data_1567640
_publ_section_title
;
 Selective separation of planar and non-planar hydrocarbons using an
 aqueous Pd6 interlocked cage
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04660A
_journal_year                    2022
_chemical_formula_moiety         '2(C80 H102 N30 Pd3), 24(N O3), x(H2 O)'
_chemical_formula_sum            'C160 H204 N84 O72 Pd6'
_chemical_formula_weight         5094.46
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-04-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-24 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   27.653(4)
_cell_length_b                   27.653(4)
_cell_length_c                   44.488(9)
_cell_measurement_reflns_used    456097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.284
_cell_measurement_theta_min      2.250
_cell_volume                     29462(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'MX2 Beamline Australian Synchrotron'
_diffrn_measurement_method       'phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            456097
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         28.284
_diffrn_reflns_theta_min         2.250
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             10416
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.202
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         24357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0910
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2931
_refine_ls_wR_factor_ref         0.3221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14626
_reflns_number_total             24357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04660a2.cif
_cod_data_source_block           p3barc1_a
_cod_original_cell_volume        29463(10)
_cod_database_code               1567640
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C3(H3A,H3B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N20(H20A), N8(H8), N16(H16), C29(H29), C28(H28), C40(H40), C17(H17),
  C42(H42), C010(H010), C32(H32), C31(H31), C24(H24), C44(H44), C20(H20),
 C25(H25), C22(H22), C35(H35), C13(H13), C43(H43), C46(H46), C18(H18), C51(H51),
  C47(H47), C50(H50), C39(H39), C37(H37), C33(H33), C21(H21), C54(H54),
 C15(H15), C14(H14), C53(H53), C48(H48), C36(H36), C55(H55)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C12(H12A,
 H12B,H12C), C7(H7A,H7B,H7C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60461
_shelx_hkl_checksum              64128
_shelx_fab_checksum              13692
_olex2_submission_special_instructions 'No special instructions were received'