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_7710392
_publ_section_title
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 Phosphorus guiding palladium: [4+4] metallomacrocyclic PdII complex and
 self-assembly of heterometallic PdII/ZnII grid-type complex
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01176J
_journal_year                    2022
_chemical_formula_moiety
'C124 H112 N28 P4 Pd4, 8(C F3 O3 S), C Cl2, 4(C2 H3 N)'
_chemical_formula_sum            'C141 H124 Cl2 F24 N32 O24 P4 Pd4 S8'
_chemical_formula_weight         3983.57
_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     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
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2022-05-27 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 95.3690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.4899(3)
_cell_length_b                   21.7388(3)
_cell_length_c                   32.7073(3)
_cell_measurement_reflns_used    46470
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.0340
_cell_measurement_theta_min      1.9390
_cell_volume                     18752.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.927
_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  0.0689
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            251333
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.367
_diffrn_reflns_theta_min         1.794
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       prism
_exptl_crystal_F_000             8032
_exptl_crystal_recrystallization_method
'Vapour diffusion of CH2Cl2 into CH3CN solution'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2237
_refine_ls_number_reflns         39418
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+35.4849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27477
_reflns_number_total             39418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01176j2.cif
_cod_data_source_block           '[Pd(1)]4(OTf)8_(3)'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710392
_extra_info
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PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
RESPONSE: The solid state structure of [Pd(1)]4(CF3SO3)8_4(C2H3N)_2(CH2Cl2) ?(CF3SO3)_x(CH2Cl2)_y(C2H3N) contained
significant electron density in the asymmetric unit which could not resolved sufficiently. 
This density was therefore removed by the SQUEEZE procedure of PLATON.  
One void per asymmetric unit with the volume of 1042 A^3 and 318 electrons was identified relating to one triflate anion (CF3SO3 = 74 electrons) 
and significat unidentified high number of solvent molecules dichloromethane x(CH2Cl2) and acetonitrile y(CH3CN) (0 < x < 5, 0 < y < 11).
Due to this the exact amount of lattice solvent molecules could not be determined.

PLAT910 Problem: Missing reflections below Theta(Min).
Response: The unit cell is reasonable large and these low angle reflections are probably missing due to the beam stop.

PLAT934 Problem: Report number of outliers.
Response: Some reflections were omitted due to the beam stop.

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_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              14583
_shelx_fab_checksum              96668