Palladium(II) complexes of a bridging amine bis(phenolate) ligand featuring κ^2^ and κ^3^ coordination modes
Graziano, Brendan J.; Wile, Bradley M.; Zeller, Matthias; Acta Crystallographica Section E 75 (2019) 1265–1269; doi:10.1107/S2056989019010454

data_2243034
_publ_section_title
;
 Palladium(II) complexes of a bridging amine bis(phenolate) ligand
 featuring \k^2^ and \k^3^ coordination modes
;
_journal_coeditor_code           LH5914
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1265
_journal_page_last               1269
_journal_paper_doi               10.1107/S2056989019010454
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Pd Cl2 (C34 H56 N2 O2)] [Pd Cl1 (C34 H55 N2 O2)], 1.685C H4 O, 0.315H2 O'
_chemical_formula_moiety
'C34 H56 Cl2 N2 O2 Pd, C34 H55 Cl N2 O2 Pd, 1.685(C H4 O), 0.315(H2 O)'
_chemical_formula_sum            'C69.68 H118.37 Cl3 N4 O6 Pd2'
_chemical_formula_weight         1427.41
_chemical_name_systematic
;Dichlorido({6,6'-[(ethane-1,2-diylbis(methylazanediyl)]bis(methylene)}bis(2,4-di-<i>tert</i>-butylphenol))palladium(II)
chlorido(2,4-di-<i>tert</i>-butyl-6-{[(2-{[(3,5-di-<i>tert</i>-butyl-2-hydroxyphenyl)methyl](methyl)amino}ethyl)(methyl)amino]methyl}phenolato)palladium(II) methanol 1.685-solvate 0.315-hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 109.5536(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8843(5)
_cell_length_b                   29.7800(10)
_cell_length_c                   16.6629(6)
_cell_measurement_reflns_used    9425
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2761
_cell_measurement_theta_min      2.9329
_cell_volume                     7427.6(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov, 2009),
<i>VESTA</i> (Momma & Izumi, 2011)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015),
<i>SHELXLE</i>  (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            87447
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.845
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6556
_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    1.276
_exptl_crystal_description       plate
_exptl_crystal_F_000             3022
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.090
_refine_diff_density_max         2.118
_refine_diff_density_min         -0.919
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         22272
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+7.3036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                18396
_reflns_number_total             22272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5914sup1.cif
_cod_data_source_block           I
_cod_database_code               2243034
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.945
_shelx_hkl_checksum              30876
_shelx_res_checksum              21318
_cod_database_fobs_code 2243034