Synthesis and characterization of fluorinated β-ketoiminate and imino-alcoholate Pd complexes: precursors for palladium chemical vapor deposition
Liu, Yan-Hsiu; Cheng, Yi-Ching; Tung, Yung-Liang; Chi, Yun; Chen, Yao-Lun; Liu, Chao-Shiuan; Peng, Shie-Ming; Lee, Gene-Hsiang; Journal of Materials Chemistry 13 (2003) 135–142; doi:10.1039/b208535f

data_7204521
_publ_section_title
;
 Synthesis and characterization of fluorinated \b-ketoiminate and
 imino-alcoholate Pd complexes: precursors for palladium chemical
 vapor deposition
;
_journal_issue                   1
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              135
_journal_page_last               142
_journal_paper_doi               10.1039/b208535f
_journal_volume                  13
_journal_year                    2003
_chemical_formula_sum            'C18 H24 F12 N2 O4 Pd'
_chemical_formula_weight         666.79
_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
_cell_angle_alpha                77.307(1)
_cell_angle_beta                 89.906(1)
_cell_angle_gamma                75.714(1)
_cell_formula_units_Z            1
_cell_length_a                   5.8906(1)
_cell_length_b                   10.2740(2)
_cell_length_c                   10.9422(1)
_cell_measurement_reflns_used    5903
_cell_measurement_temperature    295(2)
_cell_volume                     625.091(18)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8392
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.8087
_exptl_absorpt_correction_type   'empirical used sadabs'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0111(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_obs          0.0262
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0636
_refine_ls_wR_factor_obs         0.0630
_reflns_number_observed          2811
_reflns_number_total             2874
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b208535f.txt
_cod_data_source_block           ic6753
_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:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] 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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        625.09(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204521