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_7710391
_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
'(C35 H34 N9 P Pd2), 4 (C F3 O3 S), 2 (C2 H3 N)'
_chemical_formula_sum            'C43 H40 F12 N11 O12 P Pd2 S4'
_chemical_formula_weight         1502.87
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 94.3660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.1345(3)
_cell_length_b                   19.3453(2)
_cell_length_c                   50.1762(6)
_cell_measurement_reflns_used    20891
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.1000
_cell_measurement_theta_min      2.1830
_cell_volume                     22390.9(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.951
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            87278
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.344
_diffrn_reflns_theta_min         2.309
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99062
_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    1.783
_exptl_crystal_description       plate
_exptl_crystal_F_000             12000
_exptl_crystal_recrystallization_method
'Vapour diffusion of Et2O into CH3CN solution'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1398
_refine_ls_number_reflns         24085
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0610P)^2^+103.5645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19191
_reflns_number_total             24085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01176j2.cif
_cod_data_source_block           '[Pd2(1)](OTf)4_(2)'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7710391
_extra_info
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PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
RESPONSE: The solid state structure of 2[Pd2(1)(CH3CN)2](CF3SO3)4_2(C2H3N) ?2(CF3SO3)_2(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.  
Two voids per asymmetric unit with the same volume of 247 A^3 and 98 electrons have been identified.
Each void related to one triflate anion (CF3SO3) and one acetonitrile solvent molecule (CH3CN) (calculated 96 electrons/void).
However, the exact number of lattice solvent molecules should be taken with care.

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

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_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              76433
_shelx_fab_checksum              95098