Structural Characterization of Four Members of the Electron-Transfer Series [PdII(L)2)2]n (L = o-Iminophenolate Derivative; n= 2-, 1-, 0, 1+, 2+). Ligand Mixed Valency in the Monocation and Monoanion with S=1/2 Ground States
Swarnalatha Kokatam; Thomas Weyhermüller; Eberhard Bothe; Phalguni Chaudhuri; Karl Wieghardt; Inorganic Chemistry 44 (2005) 3709–3717; doi:10.1021/ic048292i

data_1100981
_publ_section_title
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Structural Characterization of Four Members of the Electron-Transfer Series

[PdII(L)2)2]n (L = o-Iminophenolate Derivative; n= 2-, 1-, 0, 1+, 2+).

Ligand Mixed Valency in the Monocation and Monoanion with S=1/2 Ground States

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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3709
_journal_page_last               3717
_journal_paper_doi               10.1021/ic048292i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[C42 H48 F6 N2 O2 Pd]+, (B F4)-'
_chemical_formula_sum            'C42 H48 B F10 N2 O2 Pd'
_chemical_formula_weight         920.03
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.586(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.5769(6)
_cell_length_b                   13.2251(3)
_cell_length_c                   30.9126(8)
_cell_measurement_temperature    100(2)
_cell_volume                     8779.2(4)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.478
_diffrn_measured_fraction_theta_max 0.478
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'553 images at 0.6 deg. in phi, 975 images at 0.6 deg. in \w, 42 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            76289
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_type   'not measured'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         10873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+19.7222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                8927
_reflns_number_total             10873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048292isi20041206_054204_2.cif
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+19.7222P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+19.7222P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               1100981