#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/36/7013635.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_7013635
loop_
_publ_author_name
'Gregorio Sánchez'
'Joaquín García'
'David Meseguer'
'José L. Serrano'
'Luis García'
'José Pérez'
'Gregorio López'
_publ_section_title
;
 Synthesis and characterisation of cyclometallated palladium(II)
 complexes with phosphine--carboxylate and phosphine--amide ligands
;
_journal_issue                   24
_journal_name_full               'Dalton Trans.'
_journal_page_first              4709
_journal_page_last               4717
_journal_paper_doi               10.1039/b310843k
_journal_year                    2003
_chemical_formula_moiety         'C33 H33 N2 O4 P Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C33.5 H34 Cl N2 O4 P Pd'
_chemical_formula_weight         701.45
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.315(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.380(2)
_cell_length_b                   9.5746(7)
_cell_length_c                   16.9787(11)
_cell_measurement_reflns_used    61
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.986
_cell_measurement_theta_min      10.038
_cell_volume                     6501.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8124
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0470P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                4440
_reflns_number_total             5715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310843k.txt
_cod_data_source_block           compound_16a
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C33.50 H34 Cl N2 O4 P Pd'
_cod_database_code               7013635
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.161209(5) 0.27777(2) 0.415977(14) 0.02371(8) Uani 1 1 d . . .
P1 P 0.133888(17) 0.47402(8) 0.42814(5) 0.02247(16) Uani 1 1 d . . .
N2 N 0.18516(6) 0.1031(3) 0.39114(16) 0.0305(6) Uani 1 1 d . . .
O1 O 0.04543(5) 0.4778(2) 0.22803(13) 0.0347(5) Uani 1 1 d . . .
C28 C 0.22479(7) 0.2753(3) 0.39059(18) 0.0303(7) Uani 1 1 d . . .
N1 N 0.08086(6) 0.2948(3) 0.27063(15) 0.0286(6) Uani 1 1 d . . .
H1 H 0.0925 0.2437 0.3135 0.034 Uiso 1 1 calc R . .
O2 O 0.22699(6) 0.0316(3) 0.34836(17) 0.0497(6) Uani 1 1 d . . .
C29 C 0.21201(7) 0.1335(3) 0.37676(19) 0.0322(7) Uani 1 1 d . . .
C23 C 0.20365(7) 0.3704(3) 0.41228(18) 0.0283(7) Uani 1 1 d . . .
C18 C 0.17218(8) 0.7899(4) 0.5978(2) 0.0380(8) Uani 1 1 d . . .
H18 H 0.1696 0.8880 0.6016 0.046 Uiso 1 1 calc R . .
C19 C 0.15344(7) 0.7178(3) 0.52690(19) 0.0314(7) Uani 1 1 d . . .
H19 H 0.1380 0.7672 0.4820 0.038 Uiso 1 1 calc R . .
C9 C 0.09943(7) 0.6993(3) 0.33074(19) 0.0305(7) Uani 1 1 d . . .
H9 H 0.0873 0.7043 0.3688 0.037 Uiso 1 1 calc R . .
C5 C 0.03342(7) 0.4005(3) 0.3871(2) 0.0330(7) Uani 1 1 d . . .
H5 H 0.0135 0.3866 0.3410 0.040 Uiso 1 1 calc R . .
C8 C 0.12414(7) 0.5972(3) 0.34140(17) 0.0255(6) Uani 1 1 d . . .
C7 C 0.06263(6) 0.4013(3) 0.28329(18) 0.0257(6) Uani 1 1 d . . .
C2 C 0.09038(7) 0.4511(3) 0.52048(18) 0.0271(7) Uani 1 1 d . . .
H2 H 0.1098 0.4711 0.5668 0.033 Uiso 1 1 calc R . .
C17 C 0.19468(8) 0.7178(4) 0.6629(2) 0.0410(8) Uani 1 1 d . . .
H17 H 0.2079 0.7670 0.7110 0.049 Uiso 1 1 calc R . .
C4 C 0.03165(7) 0.4046(4) 0.4669(2) 0.0371(8) Uani 1 1 d . . .
H4 H 0.0109 0.3905 0.4756 0.045 Uiso 1 1 calc R . .
C11 C 0.10996(9) 0.7863(4) 0.2093(2) 0.0431(9) Uani 1 1 d . . .
H11 H 0.1051 0.8504 0.1642 0.052 Uiso 1 1 calc R . .
C13 C 0.14151(7) 0.5910(3) 0.28406(18) 0.0303(7) Uani 1 1 d . . .
H13 H 0.1581 0.5215 0.2896 0.036 Uiso 1 1 calc R . .
C6 C 0.06378(6) 0.4164(3) 0.37266(18) 0.0248(6) Uani 1 1 d . . .
C1 C 0.09285(6) 0.4446(3) 0.44124(17) 0.0226(6) Uani 1 1 d . . .
C15 C 0.17936(7) 0.5029(4) 0.58798(19) 0.0336(7) Uani 1 1 d . . .
H15 H 0.1818 0.4045 0.5854 0.040 Uiso 1 1 calc R . .
C12 C 0.13438(8) 0.6867(3) 0.21919(19) 0.0362(8) Uani 1 1 d . . .
H12 H 0.1465 0.6834 0.1811 0.043 Uiso 1 1 calc R . .
C3 C 0.06016(7) 0.4291(3) 0.5336(2) 0.0351(7) Uani 1 1 d . . .
H3 H 0.0591 0.4311 0.5887 0.042 Uiso 1 1 calc R . .
C25 C 0.24748(8) 0.5424(4) 0.4251(2) 0.0440(9) Uani 1 1 d . . .
H25 H 0.2553 0.6355 0.4372 0.053 Uiso 1 1 calc R . .
C24 C 0.21601(7) 0.5063(4) 0.4296(2) 0.0355(8) Uani 1 1 d . . .
H24 H 0.2029 0.5753 0.4447 0.043 Uiso 1 1 calc R . .
C20 C 0.08202(9) 0.2609(4) 0.18752(19) 0.0382(8) Uani 1 1 d . . .
H20 H 0.0820 0.3497 0.1565 0.046 Uiso 1 1 calc R . .
C14 C 0.15693(6) 0.5746(3) 0.52062(17) 0.0245(6) Uani 1 1 d . . .
C10 C 0.09252(8) 0.7927(3) 0.2652(2) 0.0382(8) Uani 1 1 d . . .
H10 H 0.0757 0.8617 0.2585 0.046 Uiso 1 1 calc R . .
C21 C 0.11425(9) 0.1834(4) 0.1981(2) 0.0530(10) Uani 1 1 d . . .
H21A H 0.1333 0.2421 0.2289 0.080 Uiso 1 1 calc R . .
H21B H 0.1157 0.1612 0.1431 0.080 Uiso 1 1 calc R . .
H21C H 0.1146 0.0968 0.2291 0.080 Uiso 1 1 calc R . .
C31 C 0.17851(8) -0.0473(3) 0.3757(2) 0.0393(8) Uani 1 1 d . . .
H31A H 0.1553 -0.0642 0.3384 0.047 Uiso 1 1 calc R . .
H31B H 0.1824 -0.0992 0.4285 0.047 Uiso 1 1 calc R . .
C16 C 0.19803(7) 0.5761(4) 0.6585(2) 0.0417(9) Uani 1 1 d . . .
H16 H 0.2133 0.5275 0.7041 0.050 Uiso 1 1 calc R . .
C22 C 0.05161(9) 0.1740(5) 0.1389(2) 0.0602(12) Uani 1 1 d . . .
H22A H 0.0312 0.2273 0.1324 0.090 Uiso 1 1 calc R . .
H22B H 0.0513 0.0873 0.1694 0.090 Uiso 1 1 calc R . .
H22C H 0.0529 0.1514 0.0837 0.090 Uiso 1 1 calc R . .
C26 C 0.26718(7) 0.4459(4) 0.4034(2) 0.0466(9) Uani 1 1 d . . .
H26 H 0.2884 0.4720 0.4008 0.056 Uiso 1 1 calc R . .
C30 C 0.20410(11) -0.0873(4) 0.3335(3) 0.0646(12) Uani 1 1 d . . .
H30A H 0.2162 -0.1735 0.3584 0.077 Uiso 1 1 calc R . .
H30B H 0.1930 -0.1026 0.2729 0.077 Uiso 1 1 calc R . .
C27 C 0.25589(7) 0.3124(4) 0.3857(2) 0.0419(9) Uani 1 1 d . . .
H27 H 0.2692 0.2449 0.3701 0.050 Uiso 1 1 calc R . .
O3 O 0.12028(5) 0.1545(2) 0.41420(12) 0.0284(5) Uani 1 1 d . . .
O4 O 0.14104(6) 0.1259(3) 0.55167(14) 0.0473(6) Uani 1 1 d . . .
C32 C 0.11882(7) 0.1100(3) 0.48444(19) 0.0290(7) Uani 1 1 d . . .
C33 C 0.08633(8) 0.0375(4) 0.4776(2) 0.0443(9) Uani 1 1 d . . .
H33A H 0.0718 0.0366 0.4191 0.067 Uiso 1 1 calc R . .
H33B H 0.0752 0.0875 0.5113 0.067 Uiso 1 1 calc R . .
H33C H 0.0910 -0.0588 0.4978 0.067 Uiso 1 1 calc R . .
Cl1 Cl 0.01207(5) -0.1711(3) 0.3392(2) 0.284(2) Uani 1 1 d . . .
C34 C 0.0000 -0.2709(7) 0.2500 0.106(3) Uani 1 2 d S . .
H34A H -0.0188 -0.3318 0.2504 0.127 Uiso 0.50 1 calc PR . .
H34B H 0.0188 -0.3318 0.2496 0.127 Uiso 0.50 1 calc PR . .
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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
_geom_angle_publ_flag
C23 Pd1 N2 81.21(11) . . ?
C23 Pd1 O3 171.26(10) . . ?
N2 Pd1 O3 90.09(9) . . ?
C23 Pd1 P1 97.25(9) . . ?
N2 Pd1 P1 173.71(7) . . ?
O3 Pd1 P1 91.31(6) . . ?
C8 P1 C14 105.48(13) . . ?
C8 P1 C1 103.01(12) . . ?
C14 P1 C1 103.54(12) . . ?
C8 P1 Pd1 116.83(10) . . ?
C14 P1 Pd1 111.98(9) . . ?
C1 P1 Pd1 114.64(9) . . ?
C29 N2 C31 108.6(3) . . ?
C29 N2 Pd1 112.5(2) . . ?
C31 N2 Pd1 138.4(2) . . ?
C27 C28 C23 123.1(3) . . ?
C27 C28 C29 122.5(3) . . ?
C23 C28 C29 114.3(3) . . ?
C7 N1 C20 121.9(3) . . ?
C29 O2 C30 105.3(2) . . ?
N2 C29 O2 117.5(3) . . ?
N2 C29 C28 119.5(3) . . ?
O2 C29 C28 123.0(3) . . ?
C24 C23 C28 115.5(3) . . ?
C24 C23 Pd1 132.6(2) . . ?
C28 C23 Pd1 111.9(2) . . ?
C17 C18 C19 119.4(3) . . ?
C14 C19 C18 120.9(3) . . ?
C10 C9 C8 120.4(3) . . ?
C4 C5 C6 121.4(3) . . ?
C9 C8 C13 118.8(3) . . ?
C9 C8 P1 121.0(2) . . ?
C13 C8 P1 120.2(2) . . ?
O1 C7 N1 124.2(3) . . ?
O1 C7 C6 121.8(3) . . ?
N1 C7 C6 114.0(3) . . ?
C1 C2 C3 121.3(3) . . ?
C16 C17 C18 120.6(3) . . ?
C3 C4 C5 119.6(3) . . ?
C12 C11 C10 119.8(3) . . ?
C12 C13 C8 119.8(3) . . ?
C5 C6 C1 118.7(3) . . ?
C5 C6 C7 116.1(2) . . ?
C1 C6 C7 125.2(2) . . ?
C2 C1 C6 118.9(3) . . ?
C2 C1 P1 119.1(2) . . ?
C6 C1 P1 121.9(2) . . ?
C16 C15 C14 119.7(3) . . ?
C11 C12 C13 120.8(3) . . ?
C4 C3 C2 120.0(3) . . ?
C26 C25 C24 121.5(3) . . ?
C23 C24 C25 120.9(3) . . ?
N1 C20 C21 108.1(3) . . ?
N1 C20 C22 110.5(3) . . ?
C21 C20 C22 111.4(3) . . ?
C19 C14 C15 118.9(3) . . ?
C19 C14 P1 123.2(2) . . ?
C15 C14 P1 117.9(2) . . ?
C9 C10 C11 120.3(3) . . ?
N2 C31 C30 101.8(3) . . ?
C17 C16 C15 120.5(3) . . ?
C27 C26 C25 119.3(3) . . ?
O2 C30 C31 104.8(3) . . ?
C26 C27 C28 119.7(3) . . ?
C32 O3 Pd1 117.90(18) . . ?
O4 C32 O3 124.3(3) . . ?
O4 C32 C33 121.9(3) . . ?
O3 C32 C33 113.7(3) . . ?
Cl1 C34 Cl1 112.5(5) . 2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C23 2.025(3) . ?
Pd1 N2 2.071(2) . ?
Pd1 O3 2.0897(19) . ?
Pd1 P1 2.2521(8) . ?
P1 C8 1.824(3) . ?
P1 C14 1.826(3) . ?
P1 C1 1.847(3) . ?
N2 C29 1.274(4) . ?
N2 C31 1.474(4) . ?
O1 C7 1.223(3) . ?
C28 C27 1.394(4) . ?
C28 C23 1.409(4) . ?
C28 C29 1.452(5) . ?
N1 C7 1.339(4) . ?
N1 C20 1.465(4) . ?
O2 C29 1.338(4) . ?
O2 C30 1.462(5) . ?
C23 C24 1.397(4) . ?
C18 C17 1.382(5) . ?
C18 C19 1.387(4) . ?
C19 C14 1.386(4) . ?
C9 C10 1.382(4) . ?
C9 C8 1.400(4) . ?
C5 C4 1.382(4) . ?
C5 C6 1.395(4) . ?
C8 C13 1.403(4) . ?
C7 C6 1.509(4) . ?
C2 C1 1.385(4) . ?
C2 C3 1.387(4) . ?
C17 C16 1.369(5) . ?
C4 C3 1.376(4) . ?
C11 C12 1.376(5) . ?
C11 C10 1.384(5) . ?
C13 C12 1.387(4) . ?
C6 C1 1.413(4) . ?
C15 C16 1.387(4) . ?
C15 C14 1.402(4) . ?
C25 C26 1.374(5) . ?
C25 C24 1.404(4) . ?
C20 C21 1.512(5) . ?
C20 C22 1.527(5) . ?
C31 C30 1.534(5) . ?
C26 C27 1.363(5) . ?
O3 C32 1.287(3) . ?
O4 C32 1.226(4) . ?
C32 C33 1.511(4) . ?
Cl1 C34 1.719(4) . ?
C34 Cl1 1.719(4) 2 ?
