Synthesis and crystal structure of a PdII complex of ortho-xylylenebis(pyridyltriazole)
Pokharel, Uttam; Naquin, Aaron; Fronczek, Frank; IUCrData 8 (2023) x230362–; doi:10.1107/S2414314623003620

data_1568964
_publ_section_title
;
 Synthesis and crystal structure of a PdII complex of
 ortho-xylylenebis(pyridyltriazole)
;
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x230362
_journal_paper_doi               10.1107/S2414314623003620
_journal_volume                  8
_journal_year                    2023
_chemical_formula_iupac
'[Pd2 (C22 H18 N8)2] (B F4)4, 2C3 H7 N O, C4 H10 O'
_chemical_formula_moiety
'C44 H36 N16 Pd2 4+, 4(B F4 -), 2(C3 H7 N O), C4 H10 O'
_chemical_formula_sum            'C54 H60 B4 F16 N18 O3 Pd2'
_chemical_formula_weight         1569.24
_chemical_name_systematic
;Bis{\m-1,1'-(<i>o</i>-xylylene)bis[4-(pyridin-2-yl)triazole]-\k<i>N</i>^3^:<i>N</i>^3'^}dipalladium(II)
tetrakis(tetrafluoridoborate)--dimethylformamide--diethyl ether (1/2/1)
;
_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
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                85.540(2)
_cell_angle_beta                 79.660(2)
_cell_angle_gamma                76.997(2)
_cell_formula_units_Z            1
_cell_length_a                   8.3546(4)
_cell_length_b                   12.4468(5)
_cell_length_c                   15.4504(6)
_cell_measurement_reflns_used    7868
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      2.91
_cell_volume                     1538.86(11)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_radiation_source         'I\mS microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17544
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         68.453
_diffrn_reflns_theta_min         3.647
_exptl_absorpt_coefficient_mu    5.683
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       fragment
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.409
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.0220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                4983
_reflns_number_total             5427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xu4050.cif
_cod_data_source_block           I
_cod_database_code               1568964
_shelx_estimated_absorpt_t_min   0.659
_shelx_estimated_absorpt_t_max   0.945
_shelx_hkl_checksum              28350
_shelx_res_checksum              31887