A triangular palladium(II) supramolecular coordination complex based on 1,4-bis(1<i>H</i>-imidazol-1-yl)benzene and (2,2'-bipyridyl)palladium(II) nitrate: synthesis and crystal structure
Daran, Jean-Claude; Gimeno, Nicolas; Gouygou, Maryse; Volkman, Jérôme; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619004212

data_2021565
_publ_section_title
;
 A triangular palladium(II) supramolecular coordination complex based on
 1,4-bis(1<i>H</i>-imidazol-1-yl)benzene and (2,2'-bipyridyl)palladium(II)
 nitrate: synthesis and crystal structure
;
_journal_coeditor_code           QP3020
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619004212
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Pd3 (C10 H8 N2)3 (C12 H10 N4)3] (P F6)6, 7C2 H3 N'
_chemical_formula_moiety         'C66 H54 N18 Pd3 6+, 6(F6 P -), 7(C2 H3 N)'
_chemical_formula_sum            'C80 H75 F36 N25 P6 Pd3'
_chemical_formula_weight         2575.67
_chemical_name_systematic
;Tris[\m-bis(1<i>H</i>-imidazol-1-yl)benzene-\k^2^<i>N</i>^3^:<i>N</i>^3'^]-<i>triangulo</i>-tris[(2,2'-bipyridyl-\k^2^<i>N</i>,<i>N</i>')palladium(II)]
hexakis(hexafluoridophosphate) acetonitrile heptasolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                105.211(2)
_cell_angle_beta                 93.579(2)
_cell_angle_gamma                100.586(2)
_cell_formula_units_Z            2
_cell_length_a                   17.8173(4)
_cell_length_b                   18.0361(4)
_cell_length_c                   18.0674(4)
_cell_measurement_reflns_used    16442
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.1470
_cell_measurement_theta_min      3.5790
_cell_volume                     5469.7(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2016)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2016)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2016)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Xcalibur Eos Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50923
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.164
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2564
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.236
_refine_diff_density_min         -0.984
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         19228
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0833P)^2^+7.4981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                15197
_reflns_number_total             19228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qp3020sup1.cif
_cod_data_source_block           I
_cod_database_code               2021565
_cod_database_fobs_code          2021565
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.874
_shelx_hkl_checksum              79113
_shelx_res_checksum              69790
_shelxl_version_number           2014/6