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#$Date: 2025-01-08 08:43:38 +0200 (Wed, 08 Jan 2025) $
#$Revision: 297214 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/83/4078385.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4078385
loop_
_publ_author_name
'Vicente, José'
'Abad, José-Antonio'
'Rink, Barbara'
'Hernández, Francisco-Santos'
'Ramírez de Arellano, M. Carmen'
_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]·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
;
_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            'C46 H39 Cl5 O3 P2 Pd'
_chemical_formula_weight         985.36
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   'OH difmap, others geom'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6048(12)
_cell_length_b                   17.1715(12)
_cell_length_c                   17.156(2)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.488
_cell_measurement_theta_min      5.302
_cell_volume                     4302.5(7)
_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       'ω 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  0.0126
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3945
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        2.62
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.857
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    'OH DFIX, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3866
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.043
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_obs          0.0198
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0280P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0474
_refine_ls_wR_factor_obs         0.0471
_reflns_number_observed          3685
_reflns_number_total             3866
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om970583u.cif
_cod_data_source_block           br05_compound_10x2CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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^)+(0.0280P)^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^)+(0.0280P)^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        4302.4(6)
_cod_original_sg_symbol_H-M      Cmc2(1)
_cod_database_code               4078385
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Pd Pd 0.5000 1.008061(12) 0.517500(14) 0.01325(6) Uani 1 d S
Cl1 Cl 0.5000 1.14144(4) 0.47734(5) 0.0190(2) Uani 1 d S
P P 0.33931(3) 1.01051(3) 0.52133(6) 0.01512(11) Uani 1 d .
O1 O 0.5000 0.8611(2) 0.7955(2) 0.0355(8) Uani 1 d SDU
H01 H 0.5000 0.8547(24) 0.8306(23) 0.013(12) Uiso 1 d SD
O2 O 0.5000 0.7316(2) 0.7836(2) 0.0581(10) Uani 1 d SDU
O3 O 0.5000 0.7927(2) 0.3754(2) 0.0364(8) Uani 1 d SDU
C11 C 0.5000 0.8986(2) 0.5572(2) 0.0163(7) Uani 1 d SDU
C12 C 0.5000 0.8854(2) 0.6390(2) 0.0195(7) Uani 1 d SDU
H12 H 0.5000 0.9276(2) 0.6729(2) 0.023 Uiso 1 calc SR
C13 C 0.5000 0.8098(2) 0.6691(2) 0.0240(9) Uani 1 d SDU
C14 C 0.5000 0.7458(2) 0.6193(2) 0.0294(9) Uani 1 d SDU
H14 H 0.5000 0.6956(2) 0.6395(2) 0.035 Uiso 1 calc SR
C15 C 0.5000 0.7575(2) 0.5393(2) 0.0279(9) Uani 1 d SDU
H15 H 0.5000 0.7151(2) 0.5056(2) 0.033 Uiso 1 calc SR
C16 C 0.5000 0.8338(2) 0.5092(2) 0.0198(7) Uani 1 d SDU
C17 C 0.5000 0.7958(2) 0.7553(2) 0.0291(8) Uani 1 d SDU
C18 C 0.5000 0.8439(2) 0.4234(2) 0.0265(9) Uani 1 d SDU
H18 H 0.5000 0.8948(2) 0.4047(2) 0.032 Uiso 1 calc SR
C21 C 0.3000(2) 1.0598(2) 0.60950(14) 0.0172(6) Uani 1 d DU
C22 C 0.3615(2) 1.09879(14) 0.65647(14) 0.0247(5) Uani 1 d DU
H22 H 0.4232(2) 1.09966(14) 0.64305(14) 0.030 Uiso 1 calc R
C23 C 0.3324(2) 1.1369(2) 0.72364(15) 0.0300(6) Uani 1 d DU
H23 H 0.3747(2) 1.1628(2) 0.75479(15) 0.036 Uiso 1 calc R
C24 C 0.2417(2) 1.1363(2) 0.7441(2) 0.0311(7) Uani 1 d DU
H24 H 0.2221(2) 1.1618(2) 0.7890(2) 0.037 Uiso 1 calc R
C25 C 0.1791(2) 1.0973(2) 0.6971(2) 0.0333(6) Uani 1 d DU
H25 H 0.1174(2) 1.0971(2) 0.7105(2) 0.040 Uiso 1 calc R
C26 C 0.2076(2) 1.0588(2) 0.63073(14) 0.0270(6) Uani 1 d DU
H26 H 0.1654(2) 1.0321(2) 0.60017(14) 0.032 Uiso 1 calc R
C31 C 0.27405(13) 0.91958(11) 0.5217(2) 0.0183(4) Uani 1 d DU
C32 C 0.2168(2) 0.89681(14) 0.46115(14) 0.0236(5) Uani 1 d DU
H32 H 0.2097(2) 0.92890(14) 0.41790(14) 0.028 Uiso 1 calc R
C33 C 0.1701(2) 0.82632(15) 0.46486(15) 0.0287(6) Uani 1 d DU
H33 H 0.1322(2) 0.81154(15) 0.42390(15) 0.034 Uiso 1 calc R
C34 C 0.1794(2) 0.77831(13) 0.5284(2) 0.0298(6) Uani 1 d DU
H34 H 0.1478(2) 0.73135(13) 0.5306(2) 0.036 Uiso 1 calc R
C35 C 0.2361(2) 0.8003(2) 0.5891(2) 0.0296(6) Uani 1 d DU
H35 H 0.2432(2) 0.7676(2) 0.6319(2) 0.035 Uiso 1 calc R
C36 C 0.2824(2) 0.87043(14) 0.58639(14) 0.0235(5) Uani 1 d DU
H36 H 0.3194(2) 0.88512(14) 0.62798(14) 0.028 Uiso 1 calc R
C41 C 0.2911(2) 1.0633(2) 0.43894(15) 0.0191(6) Uani 1 d DU
C42 C 0.2271(2) 1.12209(14) 0.4453(2) 0.0260(6) Uani 1 d DU
H42 H 0.2074(2) 1.13813(14) 0.4943(2) 0.031 Uiso 1 calc R
C43 C 0.1919(2) 1.1575(2) 0.3788(2) 0.0370(7) Uani 1 d DU
H43 H 0.1495(2) 1.1976(2) 0.3835(2) 0.044 Uiso 1 calc R
C44 C 0.2196(2) 1.1333(2) 0.3062(2) 0.0373(8) Uani 1 d DU
H44 H 0.1953(2) 1.1567(2) 0.2619(2) 0.045 Uiso 1 calc R
C45 C 0.2833(2) 1.0747(2) 0.2989(2) 0.0364(7) Uani 1 d DU
H45 H 0.3015(2) 1.0579(2) 0.2497(2) 0.044 Uiso 1 calc R
C46 C 0.3202(2) 1.0408(2) 0.36481(14) 0.0275(6) Uani 1 d DU
H46 H 0.3649(2) 1.0025(2) 0.35976(14) 0.033 Uiso 1 calc R
C98 C 0.5000 0.4717(3) 0.8873(3) 0.0518(13) Uani 1 d S
H98A H 0.4463 0.4449(3) 0.8675(3) 0.062 Uiso 0.50 calc PR
H98B H 0.5537 0.4449(3) 0.8675(3) 0.062 Uiso 0.50 calc PR
Cl2 Cl 0.5000 0.56848(7) 0.85285(7) 0.0363(3) Uani 1 d S
Cl3 Cl 0.5000 0.46711(7) 0.98961(6) 0.0415(3) Uani 1 d S
C99 C 0.5000 0.6290(3) 0.1289(3) 0.0528(13) Uani 1 d S
H99A H 0.4463 0.6298(3) 0.0956(3) 0.063 Uiso 0.50 calc PR
H99A H 0.5537 0.6298(3) 0.0956(3) 0.063 Uiso 0.50 calc PR
Cl4 Cl 0.5000 0.71221(7) 0.18848(10) 0.0650(4) Uani 1 d S
Cl5 Cl 0.5000 0.54472(8) 0.18348(8) 0.0601(4) Uani 1 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C11 Pd P 90.42(2) . .
C11 Pd P 90.42(2) . 4_655
P Pd P 176.19(4) . 4_655
C11 Pd Cl1 176.80(10) . .
P Pd Cl1 89.48(2) . .
P Pd Cl1 89.48(2) 4_655 .
C41 P C21 106.89(11) . .
C41 P C31 103.09(13) . .
C21 P C31 103.21(13) . .
C41 P Pd 111.96(10) . .
C21 P Pd 110.22(9) . .
C31 P Pd 120.37(7) . .
C16 C11 C12 117.3(3) . .
C16 C11 Pd 123.5(3) . .
C12 C11 Pd 119.2(2) . .
C13 C12 C11 121.0(3) . .
C14 C13 C12 120.4(3) . .
C14 C13 C17 118.6(3) . .
C12 C13 C17 121.0(4) . .
C15 C14 C13 119.5(3) . .
C14 C15 C16 119.8(3) . .
C11 C16 C15 122.0(3) . .
C11 C16 C18 119.8(3) . .
C15 C16 C18 118.2(3) . .
O2 C17 O1 124.6(4) . .
O2 C17 C13 123.1(4) . .
O1 C17 C13 112.3(3) . .
O3 C18 C16 126.4(4) . .
C22 C21 C26 118.8(2) . .
C22 C21 P 120.3(2) . .
C26 C21 P 120.9(2) . .
C21 C22 C23 120.8(2) . .
C24 C23 C22 120.3(3) . .
C23 C24 C25 119.3(3) . .
C26 C25 C24 120.7(3) . .
C25 C26 C21 120.0(3) . .
C32 C31 C36 118.4(2) . .
C32 C31 P 123.4(2) . .
C36 C31 P 118.2(2) . .
C31 C32 C33 120.4(2) . .
C34 C33 C32 120.7(2) . .
C33 C34 C35 119.6(2) . .
C36 C35 C34 120.4(2) . .
C35 C36 C31 120.7(2) . .
C42 C41 C46 118.8(2) . .
C42 C41 P 124.4(2) . .
C46 C41 P 116.8(2) . .
C41 C42 C43 120.3(3) . .
C44 C43 C42 120.2(3) . .
C43 C44 C45 120.2(3) . .
C44 C45 C46 119.8(3) . .
C45 C46 C41 120.6(3) . .
Cl3 C98 Cl2 112.1(3) . .
Cl5 C99 Cl4 111.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd C11 1.999(3) .
Pd P 2.3482(5) .
Pd P 2.3482(5) 4_655
Pd Cl1 2.3917(8) .
P C41 1.821(3) .
P C21 1.826(3) .
P C31 1.829(2) .
O1 C17 1.316(5) .
O2 C17 1.204(4) .
O3 C18 1.205(4) .
C11 C16 1.385(5) .
C11 C12 1.420(5) .
C12 C13 1.397(5) .
C13 C14 1.392(5) .
C13 C17 1.499(5) .
C14 C15 1.387(5) .
C15 C16 1.408(5) .
C16 C18 1.483(5) .
C21 C22 1.380(4) .
C21 C26 1.398(4) .
C22 C23 1.392(3) .
C23 C24 1.371(4) .
C24 C25 1.391(4) .
C25 C26 1.381(4) .
C31 C32 1.390(3) .
C31 C36 1.399(3) .
C32 C33 1.391(3) .
C33 C34 1.374(4) .
C34 C35 1.382(4) .
C35 C36 1.382(3) .
C41 C42 1.379(4) .
C41 C46 1.396(3) .
C42 C43 1.390(4) .
C43 C44 1.373(4) .
C44 C45 1.377(4) .
C45 C46 1.382(4) .
C98 Cl3 1.758(5) .
C98 Cl2 1.764(5) .
C99 Cl5 1.724(5) .
C99 Cl4 1.757(5) .
