Cooperativity of steric bulk and H-bonding in coordination sphere engineering: heteroleptic PdII cages and bowls by design
Chen, Bin; Holstein, Julian J.; Platzek, André; Schneider, Laura; Wu, Kai; Clever, Guido H.; Chemical Science  (2022) –; doi:10.1039/D1SC06931D

data_1566162
_publ_section_title
;
 Cooperativity of steric bulk and H-bonding in coordination sphere
 engineering: heteroleptic PdII cages and bowls by design
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC06931D
_journal_year                    2022
_chemical_formula_moiety
;
C138 H90 N14 O16 Pd2, C70, 2(C6 H6), 2(B F4) [+ solvent]
;
_chemical_formula_sum            'C220 H102 B2 F8 N14 O16 Pd2'
_chemical_formula_weight         3583.57
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           'FinalCif by Daniel Kratzert, Freiburg 2019'
_audit_update_record
;
2020-04-16 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.20(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.755(6)
_cell_length_b                   16.741(3)
_cell_length_c                   41.053(8)
_cell_measurement_reflns_used    68636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.834
_cell_measurement_theta_min      1.013
_cell_volume                     20079(7)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'costum designed P11 GUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
;
Pilatus 6M fast, High Precision 1-Axis Goniostat with Sta\"ubli sample changing
robot
;
_diffrn_measurement_method       '360\deg \p scan'
_diffrn_radiation_monochromator
'double crystal monochromator (Si-111 and Si-113 reflections)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0332
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68636
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.834
_diffrn_reflns_theta_max         24.834
_diffrn_reflns_theta_min         1.013
_diffrn_source                   'P11@PETRA III, DESY, Hamburg, Germany'
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       neddle
_exptl_crystal_F_000             7288
_exptl_crystal_recrystallization_method
'Diffussion of 2ml benzene into 100yl of 0.64 mmol/l solution of compound in acetonitrile'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.665
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2990
_refine_ls_number_reflns         11207
_refine_ls_number_restraints     30712
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1443
_refine_ls_R_factor_gt           0.1188
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3434
_refine_ls_wR_factor_ref         0.3706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7745
_reflns_number_total             11207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06931d2.cif
_cod_data_source_block           bc31a_sq
_cod_original_cell_volume        20080(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1566162
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.907
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              4060
_shelx_hkl_checksum              70819
_shelx_fab_checksum              62444