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_4308859
_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_sum            'C42 H48 F6 N2 O2 Pd'
_chemical_formula_weight         833.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.81(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1042(3)
_cell_length_b                   8.1767(3)
_cell_length_c                   21.8740(5)
_cell_measurement_reflns_used    4892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      138.3
_cell_measurement_theta_min      8.08
_cell_volume                     1985.07(10)
_computing_cell_refinement       SAINT
_computing_data_collection       'SMART Collect Software'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       '\w-scans at 0.3 deg and 5 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11753
_diffrn_reflns_theta_max         68.96
_diffrn_reflns_theta_min         4.04
_exptl_absorpt_coefficient_mu    4.327
_exptl_absorpt_correction_type   'SADABS (G.Sheldrick 2004)'
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.752
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.151
_refine_ls_goodness_of_fit_obs   1.160
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_restrained_S_obs      1.160
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_obs          0.0464
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+2.8327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1373
_refine_ls_wR_factor_obs         0.1352
_reflns_number_observed          3322
_reflns_number_total             3439
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic048292isi20041206_054204_1.cif
_cod_data_source_block           1
_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^)+(0.0832P)^2^+2.8327P] 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^)+(0.0832P)^2^+2.8327P] 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_original_cell_volume        1985.1(2)
_cod_database_code               4308859