Phosphorus guiding palladium: [4+4] metallomacrocyclic PdII complex and self-assembly of heterometallic PdII/ZnII grid-type complex
Clauss, Reike; Hey-Hawkins, Evamarie; Dalton Transactions  (2022) –; doi:10.1039/D2DT01176J

data_7710390
_publ_section_title
;
 Phosphorus guiding palladium: [4+4] metallomacrocyclic PdII complex and
 self-assembly of heterometallic PdII/ZnII grid-type complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01176J
_journal_year                    2022
_chemical_formula_moiety         'C62 H56 N14 P2 Pd, 2(C F3 O3 S), 5(C H2 Cl2)'
_chemical_formula_sum            'C69 H66 Cl10 F6 N14 O6 P2 Pd S2'
_chemical_formula_weight         1888.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.90150(10)
_cell_length_b                   38.1339(4)
_cell_length_c                   14.9542(2)
_cell_measurement_reflns_used    27449
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.6790
_cell_measurement_theta_min      2.1140
_cell_volume                     7846.74(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Mercury version 3.10.3 (Macrae et al., 2006)'
_computing_publication_material  'Mercury version 3.10.3 (Macrae et al., 2006)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.3560
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            82553
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.033
_diffrn_reflns_theta_min         1.825
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       prism
_exptl_crystal_F_000             3832
_exptl_crystal_recrystallization_method
'Vapour diffusion of Et2O into CH2Cl2 solution'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.213
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         17579
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+24.8975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14203
_reflns_number_total             17579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01176j2.cif
_cod_data_source_block           '[Pd(1)2](OTf)2_(4)'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710390
_extra_info
; The solid state structure of [Pd(1)2](OTf)2_3(CH2Cl2) ?2(CH2Cl2) contained significant 
electron density in the asymmetric unit which could not resolved sufficiently. 
This density was therefore removed by the SQUEEZE procedure of PLATON.
Two voids with each size of 91 A^3 and 41 electrons were removed from the asymmetric unit of 
[Pd(1)2](OTf)2_3(CH2Cl2) ?2(CH2Cl2) corresponding to two CH2Cl2 solvent molecules (42 electrons/molecule).
Therefore, the exact number of lattice solvent molecules should be taken with care.
;
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              42458
_shelx_fab_checksum              14198