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_1100983
_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
'3 [C42 H48 F6 N2 O2 Pd]2+, 6 (B F4)-, 2 HBF4, 4 CH2Cl2'
_chemical_formula_sum            'C43.33 H51.33 B2.67 Cl2.67 F16.67 N2 O2 Pd'
_chemical_formula_weight         1178.62
_chemical_name_systematic
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 ? 

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_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.548(5)
_cell_angle_beta                 72.946(5)
_cell_angle_gamma                78.209(5)
_cell_formula_units_Z            3
_cell_length_a                   13.5833(5)
_cell_length_b                   16.8101(7)
_cell_length_c                   18.3743(7)
_cell_measurement_temperature    100(2)
_cell_volume                     3883.1(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'851 images at 0.5 deg. in \w and 726 images at 0.5 deg. in phi, 15 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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54535
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.9065
_exptl_absorpt_correction_T_min  0.7185
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            'deep green'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       transparent
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.178
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         17684
_refine_ls_number_restraints     415
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0436P)^2^+12.9878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                15319
_reflns_number_total             17684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048292isi20041206_054204_4.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0436P)^2^+12.9878P] 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^)+(0.0436P)^2^+12.9878P] 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               1100983