Synthesis, crystal structure and Hirshfeld analysis of trans-bis(2-{1-[(6R,S)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamidato-κ2 N 2,S)palladium(II) ethanol monosolvate
Melo, Ana Paula Lopes de; Bresolin, Leandro; Tirloni, Bárbara; Farias, Renan Lira de; Oliveira, Adriano Bof de; Acta Crystallographica Section E Crystallographic Communications 79 (2023) 1166–1172; doi:10.1107/S2056989023009908

data_2022945
_publ_section_title
;
 Synthesis, crystal structure and Hirshfeld analysis of
 trans-bis(2-{1-[(6R,S)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-N-methylhydrazinecarbothioamidato-\k2
 N 2,S)palladium(II) ethanol monosolvate
;
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1166
_journal_page_last               1172
_journal_paper_doi               10.1107/S2056989023009908
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Pd (C20 H30 N3 S1)2], C2 H6 O1'
_chemical_formula_moiety         'C40 H60 N6 Pd1 S2, C2 H6 O1'
_chemical_formula_sum            'C42 H66 N6 O Pd S2'
_chemical_formula_weight         841.52
_chemical_name_systematic
'<i>trans</i>-Bis(2-{1-[(6<i>R</i>,<i>S</i>)-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl]ethylidene}-<i>N</i>-methylhydrazinecarbothioamidato-\k^2^<i>N</i>^2^,<i>S</i>)palladium(II) ethanol monosolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                69.021(5)
_cell_angle_beta                 86.730(6)
_cell_angle_gamma                75.348(9)
_cell_formula_units_Z            2
_cell_length_a                   12.412(3)
_cell_length_b                   12.430(4)
_cell_length_c                   15.700(5)
_cell_measurement_reflns_used    9602
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.73
_cell_volume                     2186.6(11)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006), CrystalExplorer (Wolff <i>et al.</i>,
2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), publCIF (Westrip, 2010) and
enCIFer (Allen <i>et al.</i>,
2004)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            102991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_min         2.152
_diffrn_source                   'microfocus X ray tube'
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.852
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         10905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+2.3103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                10009
_reflns_number_total             10905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zn2034sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022945.cif.'
_cod_original_formula_sum        'C42 H66 N6 O1 Pd1 S2'
_cod_database_code               2022945
_cod_database_fobs_code          2022945
_shelx_hkl_checksum              92788
_shelx_res_checksum              3175