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_1566161
_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         'C38 H24 N6 O4'
_chemical_formula_sum            'C38 H24 N6 O4'
_chemical_formula_weight         628.63
_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                 103.069(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0425(5)
_cell_length_b                   11.2236(4)
_cell_length_c                   19.5237(7)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.34
_cell_measurement_theta_min      2.72
_cell_volume                     2997.38(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PYMOL (Schr\"odinger, LLC 2019)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS with Photon 2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            90407
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.380
_diffrn_reflns_theta_min         2.107
_diffrn_source_type              'INCOATEC microfocus sealed tube, Iys 3.0'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       needle
_exptl_crystal_F_000             1304
_exptl_crystal_recrystallization_method
'Evaporation from of 1.00 mmol solution of compound in 1:1 mixture of CH3CN (200yl) and CH2Cl2 (200yl)'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         14541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0761P)^2^+0.3173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10433
_reflns_number_total             14541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06931d2.cif
_cod_data_source_block           bc18a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1566161
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.998
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_shelx_res_checksum              29393
_shelx_hkl_checksum              21172