Classical and non-classical redox reactions of Pd(II) complexes containing redox-active ligands
Corey A. Sanz; Michael J. Ferguson; Robert McDonald; Brian O. Patrick; Robin G. Hicks; Chem.Commun. 50 (2014) 11676–; doi:10.1039/C4cc04863F

data_7115700
_publ_section_title
;
 Classical and non-classical redox reactions of Pd(II) complexes
 containing redox-active ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              11676
_journal_paper_doi               10.1039/C4cc04863F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C26 H28 Cl2 N4 O P Pd, H2 O'
_chemical_formula_sum            'C26 H30 Cl2 N4 O2 P Pd'
_chemical_formula_weight         638.81
_chemical_name_systematic
;
 ?
;
_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   mixed
_audit_creation_date             2013-06-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                101.704(14)
_cell_angle_beta                 100.030(14)
_cell_angle_gamma                94.767(13)
_cell_formula_units_Z            2
_cell_length_a                   8.972(5)
_cell_length_b                   9.771(5)
_cell_length_c                   16.661(9)
_cell_measurement_reflns_used    8678
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.42
_cell_volume                     1397.7(13)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27787
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.508
_diffrn_reflns_theta_min         1.273
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0579 after correction.
The Ratio of minimum to maximum transmission is 0.7254.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.645
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5055
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0490
_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^)+9.3271P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4202
_reflns_number_total             5055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc04863f2.cif
_cod_data_source_block           rh111
_cod_database_code               7115700
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.9584 with sigma of 0.001
 H2A-H2B
 1.515 with sigma of 0.001
3.a Ternary CH refined with riding coordinates:
 C6(H6), C3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C20(H20), C22(H22), C24(H24), C19(H19), C18(H18), C25(H25),
 C17(H17), C26(H26), C23(H23), C13(H13), C12(H12), C14(H14), C11(H11)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.693
_shelxl_version_number           2012-9