Synthesis of Mercury(II) and Palladium(II) Organometallic Derivatives of Terephthaldehyde by Metalation, Transmetalation, Oxidation, and Condensation Reactions. X-ray Crystal Structures oftrans-[PdCl{C6H3(CO2H)2-2,5}(PPh3)2]·Me2CO·2MeOH,trans-[PdCl{C6H3(CHO)-2-(CO2H)-5}(PPh3)2]·2CH2Cl2, and [Pd{C6H3(CHNC6H4NH2-4)-2-(CHO)-5}(N,N,N',N'-Tetramethylethylenediamine)]CF3SO3. Molecular Assemblies through [Pd]–Cl···HO2C–Aryl and [Pd]–Cl···HOMe HO(O)C–Aryl Hydrogen Bonds
Vicente, José; Abad, José-Antonio; Rink, Barbara; Hernández, Francisco-Santos; Ramírez de Arellano, M. Carmen; Organometallics 16 (1997) 5269–5282; doi:10.1021/om970583u

data_4078386
_publ_section_title
;
 Synthesis of Mercury(II) and Palladium(II) Organometallic Derivatives of
 Terephthaldehyde by Metalation, Transmetalation, Oxidation, and
 Condensation Reactions. X-ray Crystal Structures
 oftrans-[PdCl{C6H3(CO2H)2-2,5}(PPh3)2]&#x00B7;Me2CO&#x00B7;2MeOH,trans-[PdCl{C6H3(CHO)-2-(CO2H)-5}(PPh3)2]&#x00B7;2CH2Cl2,
 and
 [Pd{C6H3(CHNC6H4NH2-4)-2-(CHO)-5}(N,N,N',N'-Tetramethylethylenediamine)]CF3SO3.
 Molecular Assemblies through
 [Pd]--Cl&#x00B7;&#x00B7;&#x00B7;HO2C--Aryl and
 [Pd]--Cl&#x00B7;&#x00B7;&#x00B7;HOMe HO(O)C--Aryl
 Hydrogen Bonds
;
_journal_coden_ASTM              ORGND7
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5269
_journal_page_last               5282
_journal_paper_doi               10.1021/om970583u
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C21 H27 F3 N4 O4 Pd S'
_chemical_formula_weight         594.93
_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                74.991(12)
_cell_angle_beta                 75.398(10)
_cell_angle_gamma                82.864(14)
_cell_formula_units_Z            2
_cell_length_a                   10.786(2)
_cell_length_b                   10.998(2)
_cell_length_c                   11.140(2)
_cell_measurement_reflns_used    81
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      13.50
_cell_measurement_theta_min      4.73
_cell_volume                     1232.7(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5507
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        2.90
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.894
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       tablet
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.945
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     405
_refine_ls_restrained_S_all      0.919
_refine_ls_restrained_S_obs      0.991
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_obs          0.0362
_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^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0782
_refine_ls_wR_factor_obs         0.0742
_reflns_number_observed          3299
_reflns_number_total             4266
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om970583u.cif
_cod_data_source_block           br01_compound_12c'
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0424P)^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^)+(0.0424P)^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        1232.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078386