A Palladium Inverse Crown: Synthesis and Characterisation
Krämer, Felix; Kennedy, Alan; Fernandez, Israel; Mulvey, Robert E.; Chemical Communications  (2026) –; doi:10.1039/D5CC06236E

data_7135329
_publ_section_title
;
 A Palladium Inverse Crown: Synthesis and Characterisation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC06236E
_journal_year                    2026
_chemical_formula_sum            'C108 H155 Cs2 O12 P7 Pd6'
_chemical_formula_weight         2766.32
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-12-04 deposited with the CCDC.	2025-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.9810(2)
_cell_length_b                   14.8646(1)
_cell_length_c                   25.5815(2)
_cell_measurement_reflns_used    39992
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      73.1810
_cell_measurement_theta_min      2.8510
_cell_volume                     11780.80(14)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_publication_material  'SHELXL in WInGX'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Synergy-i'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            86046
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.442
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'microsource tube'
_exptl_absorpt_coefficient_mu    13.304
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.076
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.94a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       plate
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.775
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 8202 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1546
_refine_ls_number_reflns         21912
_refine_ls_number_restraints     1068
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0701P)^2^+8.6282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.864
_reflns_Friedel_fraction_max     0.850
_reflns_number_gt                20375
_reflns_number_total             21912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06236e2.cif
_cod_data_source_block           compound1
_cod_database_code               7135329
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              34820