Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate)
Shapovalov, Sergey; Tikhonova, Olga; Skabitsky, Ivan; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021009270

data_2243919
_publ_section_title
;
 Crystal structure of the new palladium complexes
 tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II)
 hexadecacarbonyltetrarhenium diethyl ether disolvate and
 octa-\m-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium
 (unknown solvate)
;
_journal_coeditor_code           TX2041
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021009270
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Pd (C5 H8 N2)4] [Re4 (C O)16], 2C4 H10 O'
_chemical_formula_moiety
'C20 H32 N8 Pd 2+, C16 O16 Re4 2-, 2(C4 H10 O)'
_chemical_formula_sum            'C44 H52 N8 O18 Pd Re4'
_chemical_formula_weight         1832.13
_chemical_name_systematic
;
Tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II)
hexadecacarbonyltetrarhenium diethyl ether disolvate
;
_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
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.3420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1079(9)
_cell_length_b                   14.0026(6)
_cell_length_c                   19.4346(8)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      2.91
_cell_volume                     5420.0(4)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            128368
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.525
_diffrn_reflns_theta_min         1.778
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.302
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.2851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_density_diffrn    2.245
_exptl_crystal_description       plate
_exptl_crystal_F_000             3448
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.831
_refine_ls_extinction_coef       0.000167(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2014/7 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9046
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0239P)^2^+18.7547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                7392
_reflns_number_total             9046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2041sup1.cif
_cod_data_source_block           1
_cod_database_code               2243919
_shelx_estimated_absorpt_t_min   0.301
_shelx_estimated_absorpt_t_max   0.768
_shelx_hkl_checksum              22665
_shelx_res_checksum              88879
_cod_database_fobs_code 2243919