#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:49:15 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180357 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/26/7202602.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_7202602
loop_
_publ_author_name
'Smith, Martin B.'
'Dale, Sophie H.'
'Coles, Simon J.'
'Gelbrich, Thomas'
'Hursthouse, Michael B.'
'Light, Mark E.'
'Horton, Peter N.'
_publ_section_title
;
 Hydrogen bonded supramolecular assemblies based on neutral
 square-planar palladium(ii) complexes
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              165
_journal_paper_doi               10.1039/b616337h
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C34 H30 Cl5 N O3 P2 Pd'
_chemical_formula_weight         846.18
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                86.346(5)
_cell_angle_beta                 82.333(5)
_cell_angle_gamma                69.590(5)
_cell_formula_units_Z            2
_cell_length_a                   9.657(5)
_cell_length_b                   9.830(5)
_cell_length_c                   21.630(5)
_cell_measurement_temperature    120(2)
_cell_volume                     1906.9(15)
_computing_cell_refinement       'DENZO & COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'Bruker SHELXTL and local programs'
_computing_publication_material  Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14762
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.9628
_exptl_absorpt_correction_T_min  0.8701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV Blessing (1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0456
_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)+(0.0514P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                4229
_reflns_number_total             6063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b616337h.txt
_cod_data_source_block           2e.CHCl3
_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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202602
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_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 0.58580(4) 0.08411(4) 0.197381(17) 0.01996(13) Uani 1 1 d . . .
Cl1 Cl 0.74788(13) -0.12426(12) 0.14702(6) 0.0283(3) Uani 1 1 d . . .
Cl2 Cl 0.38417(13) 0.00187(12) 0.19433(6) 0.0285(3) Uani 1 1 d . . .
P1 P 0.78310(13) 0.15248(12) 0.19853(6) 0.0198(3) Uani 1 1 d . . .
P2 P 0.43059(13) 0.27148(12) 0.25308(6) 0.0209(3) Uani 1 1 d . . .
O1 O 0.5274(4) 0.6857(3) 0.23658(15) 0.0280(8) Uani 1 1 d . . .
H1 H 0.4903 0.7760 0.2314 0.042 Uiso 1 1 calc R . .
O2 O 0.9394(5) 0.4108(4) 0.4465(2) 0.0644(14) Uani 1 1 d . . .
H2 H 1.0063 0.3988 0.4695 0.097 Uiso 1 1 calc R . .
O3 O 0.9101(4) 0.6427(4) 0.45741(17) 0.0436(10) Uani 1 1 d . . .
N1 N 0.6415(4) 0.3914(4) 0.27622(17) 0.0194(9) Uani 1 1 d . . .
C1 C 0.8894(5) 0.1531(5) 0.1242(2) 0.0254(12) Uani 1 1 d . . .
C2 C 0.8223(6) 0.1706(5) 0.0692(2) 0.0332(13) Uani 1 1 d . . .
H2A H 0.7227 0.1727 0.0714 0.040 Uiso 1 1 calc R . .
C3 C 0.8989(7) 0.1849(5) 0.0122(3) 0.0439(15) Uani 1 1 d . . .
H3 H 0.8519 0.1981 -0.0247 0.053 Uiso 1 1 calc R . .
C4 C 1.0448(8) 0.1797(6) 0.0089(3) 0.0533(18) Uani 1 1 d . . .
H4 H 1.0983 0.1883 -0.0304 0.064 Uiso 1 1 calc R . .
C5 C 1.1121(7) 0.1626(6) 0.0618(3) 0.0515(17) Uani 1 1 d . . .
H5 H 1.2123 0.1591 0.0589 0.062 Uiso 1 1 calc R . .
C6 C 1.0364(6) 0.1502(6) 0.1196(3) 0.0384(14) Uani 1 1 d . . .
H6 H 1.0841 0.1398 0.1562 0.046 Uiso 1 1 calc R . .
C7 C 0.9049(5) 0.0318(5) 0.2512(2) 0.0270(12) Uani 1 1 d . . .
C8 C 1.0270(6) -0.0869(5) 0.2289(3) 0.0392(14) Uani 1 1 d . . .
H8 H 1.0501 -0.1035 0.1853 0.047 Uiso 1 1 calc R . .
C9 C 1.1144(6) -0.1806(6) 0.2703(4) 0.0529(19) Uani 1 1 d . . .
H9 H 1.1985 -0.2607 0.2551 0.064 Uiso 1 1 calc R . .
C10 C 1.0796(7) -0.1577(7) 0.3333(4) 0.058(2) Uani 1 1 d . . .
H10 H 1.1405 -0.2217 0.3615 0.069 Uiso 1 1 calc R . .
C11 C 0.9584(7) -0.0439(7) 0.3559(3) 0.0487(16) Uani 1 1 d . . .
H11 H 0.9334 -0.0303 0.3996 0.058 Uiso 1 1 calc R . .
C12 C 0.8720(6) 0.0520(6) 0.3145(3) 0.0373(14) Uani 1 1 d . . .
H12 H 0.7890 0.1325 0.3302 0.045 Uiso 1 1 calc R . .
C13 C 0.3807(5) 0.2124(5) 0.3314(2) 0.0284(12) Uani 1 1 d . . .
C14 C 0.4508(6) 0.2332(6) 0.3811(3) 0.0452(15) Uani 1 1 d . . .
H14 H 0.5189 0.2843 0.3745 0.054 Uiso 1 1 calc R . .
C15 C 0.4200(8) 0.1790(8) 0.4392(3) 0.0616(19) Uani 1 1 d . . .
H15 H 0.4694 0.1909 0.4725 0.074 Uiso 1 1 calc R . .
C16 C 0.3193(8) 0.1080(7) 0.4502(3) 0.0614(19) Uani 1 1 d . . .
H16 H 0.2985 0.0718 0.4909 0.074 Uiso 1 1 calc R . .
C17 C 0.2498(7) 0.0899(7) 0.4026(3) 0.0518(17) Uani 1 1 d . . .
H17 H 0.1787 0.0423 0.4103 0.062 Uiso 1 1 calc R . .
C18 C 0.2805(6) 0.1398(6) 0.3429(3) 0.0405(14) Uani 1 1 d . . .
H18 H 0.2326 0.1239 0.3098 0.049 Uiso 1 1 calc R . .
C19 C 0.2615(5) 0.3661(5) 0.2186(2) 0.0208(11) Uani 1 1 d . . .
C20 C 0.1329(5) 0.4523(5) 0.2540(2) 0.0283(12) Uani 1 1 d . . .
H20 H 0.1269 0.4515 0.2982 0.034 Uiso 1 1 calc R . .
C21 C 0.0141(6) 0.5389(5) 0.2240(3) 0.0343(13) Uani 1 1 d . . .
H21 H -0.0737 0.5982 0.2480 0.041 Uiso 1 1 calc R . .
C22 C 0.0207(6) 0.5409(5) 0.1603(3) 0.0368(14) Uani 1 1 d . . .
H22 H -0.0627 0.6005 0.1407 0.044 Uiso 1 1 calc R . .
C23 C 0.1481(6) 0.4568(5) 0.1242(3) 0.0345(13) Uani 1 1 d . . .
H23 H 0.1533 0.4594 0.0800 0.041 Uiso 1 1 calc R . .
C24 C 0.2684(5) 0.3684(5) 0.1539(2) 0.0287(12) Uani 1 1 d . . .
H24 H 0.3559 0.3092 0.1298 0.034 Uiso 1 1 calc R . .
C25 C 0.6654(5) 0.5100(5) 0.3054(2) 0.0215(11) Uani 1 1 d . . .
C26 C 0.7546(5) 0.4770(5) 0.3535(2) 0.0246(11) Uani 1 1 d . . .
H26 H 0.7945 0.3789 0.3673 0.030 Uiso 1 1 calc R . .
C27 C 0.7869(5) 0.5818(5) 0.3818(2) 0.0267(12) Uani 1 1 d . . .
C28 C 0.7198(5) 0.7285(5) 0.3640(2) 0.0309(12) Uani 1 1 d . . .
H28 H 0.7367 0.8023 0.3849 0.037 Uiso 1 1 calc R . .
C29 C 0.6303(5) 0.7658(5) 0.3169(2) 0.0256(12) Uani 1 1 d . . .
H29 H 0.5847 0.8649 0.3056 0.031 Uiso 1 1 calc R . .
C30 C 0.6068(5) 0.6561(5) 0.2856(2) 0.0207(11) Uani 1 1 d . . .
C31 C 0.8843(6) 0.5457(6) 0.4315(2) 0.0320(13) Uani 1 1 d . . .
C32 C 0.7517(5) 0.3395(5) 0.2221(2) 0.0216(11) Uani 1 1 d . . .
H32A H 0.8476 0.3445 0.2312 0.026 Uiso 1 1 calc R . .
H32B H 0.7199 0.4061 0.1864 0.026 Uiso 1 1 calc R . .
C33 C 0.4882(5) 0.4278(4) 0.2614(2) 0.0216(11) Uani 1 1 d . . .
H33A H 0.4777 0.4856 0.2220 0.026 Uiso 1 1 calc R . .
H33B H 0.4194 0.4899 0.2948 0.026 Uiso 1 1 calc R . .
C34 C 0.5408(6) 0.7085(6) 0.0772(3) 0.0399(14) Uani 1 1 d . . .
Cl3 Cl 0.3902(2) 0.6520(2) 0.10398(8) 0.0715(6) Uani 1 1 d . . .
Cl4 Cl 0.7035(2) 0.55856(17) 0.05843(8) 0.0658(5) Uani 1 1 d . . .
Cl5 Cl 0.50108(16) 0.82438(15) 0.01141(7) 0.0462(4) Uani 1 1 d . . .
H34 H 0.557(6) 0.761(6) 0.112(3) 0.055 Uiso 1 1 d . . .
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'
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'
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
_geom_angle_publ_flag
P2 Pd1 P1 94.15(6) . . ?
P2 Pd1 Cl1 174.99(5) . . ?
P1 Pd1 Cl1 87.10(6) . . ?
P2 Pd1 Cl2 88.34(6) . . ?
P1 Pd1 Cl2 177.47(4) . . ?
Cl1 Pd1 Cl2 90.38(5) . . ?
C1 P1 C7 108.4(2) . . ?
C1 P1 C32 99.0(2) . . ?
C7 P1 C32 106.4(2) . . ?
C1 P1 Pd1 115.02(16) . . ?
C7 P1 Pd1 108.66(16) . . ?
C32 P1 Pd1 118.53(15) . . ?
C19 P2 C13 108.4(2) . . ?
C19 P2 C33 98.1(2) . . ?
C13 P2 C33 106.7(2) . . ?
C19 P2 Pd1 113.36(16) . . ?
C13 P2 Pd1 110.65(16) . . ?
C33 P2 Pd1 118.67(16) . . ?
C32 N1 C25 110.7(3) . . ?
C32 N1 C33 112.4(3) . . ?
C25 N1 C33 113.1(3) . . ?
C6 C1 C2 118.3(5) . . ?
C6 C1 P1 121.1(4) . . ?
C2 C1 P1 120.3(4) . . ?
C3 C2 C1 120.9(5) . . ?
C2 C3 C4 119.6(6) . . ?
C5 C4 C3 120.5(6) . . ?
C4 C5 C6 120.8(6) . . ?
C5 C6 C1 119.9(5) . . ?
C12 C7 C8 119.0(5) . . ?
C12 C7 P1 119.8(4) . . ?
C8 C7 P1 121.1(4) . . ?
C9 C8 C7 119.9(6) . . ?
C10 C9 C8 120.0(6) . . ?
C11 C10 C9 120.8(5) . . ?
C10 C11 C12 119.5(6) . . ?
C7 C12 C11 120.9(5) . . ?
C18 C13 C14 118.8(5) . . ?
C18 C13 P2 121.2(4) . . ?
C14 C13 P2 119.9(4) . . ?
C15 C14 C13 119.4(6) . . ?
C14 C15 C16 121.3(6) . . ?
C17 C16 C15 119.4(6) . . ?
C16 C17 C18 121.2(6) . . ?
C13 C18 C17 119.9(5) . . ?
C24 C19 C20 119.8(4) . . ?
C24 C19 P2 118.0(4) . . ?
C20 C19 P2 121.6(4) . . ?
C21 C20 C19 119.1(5) . . ?
C22 C21 C20 121.1(5) . . ?
C21 C22 C23 120.7(5) . . ?
C22 C23 C24 118.7(5) . . ?
C19 C24 C23 120.6(5) . . ?
C26 C25 C30 118.3(4) . . ?
C26 C25 N1 118.6(4) . . ?
C30 C25 N1 123.1(4) . . ?
C27 C26 C25 122.1(4) . . ?
C26 C27 C28 118.8(4) . . ?
C26 C27 C31 121.8(4) . . ?
C28 C27 C31 119.3(4) . . ?
C29 C28 C27 120.8(4) . . ?
C28 C29 C30 119.5(4) . . ?
O1 C30 C29 122.1(4) . . ?
O1 C30 C25 117.7(4) . . ?
C29 C30 C25 120.3(4) . . ?
O3 C31 O2 122.8(5) . . ?
O3 C31 C27 120.8(5) . . ?
O2 C31 C27 116.4(4) . . ?
N1 C32 P1 115.4(3) . . ?
N1 C33 P2 115.1(3) . . ?
Cl3 C34 Cl4 110.9(3) . . ?
Cl3 C34 Cl5 110.2(3) . . ?
Cl4 C34 Cl5 109.9(3) . . ?
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 P2 2.2285(14) . ?
Pd1 P1 2.2340(16) . ?
Pd1 Cl1 2.3292(14) . ?
Pd1 Cl2 2.3640(16) . ?
P1 C1 1.789(5) . ?
P1 C7 1.817(5) . ?
P1 C32 1.849(4) . ?
P2 C19 1.807(4) . ?
P2 C13 1.815(5) . ?
P2 C33 1.834(4) . ?
O1 C30 1.348(5) . ?
O2 C31 1.282(6) . ?
O3 C31 1.248(6) . ?
N1 C32 1.459(6) . ?
N1 C25 1.459(5) . ?
N1 C33 1.472(5) . ?
C1 C6 1.400(7) . ?
C1 C2 1.402(7) . ?
C2 C3 1.377(7) . ?
C3 C4 1.385(8) . ?
C4 C5 1.363(8) . ?
C5 C6 1.382(8) . ?
C7 C12 1.375(7) . ?
C7 C8 1.395(7) . ?
C8 C9 1.386(8) . ?
C9 C10 1.372(9) . ?
C10 C11 1.365(9) . ?
C11 C12 1.388(7) . ?
C13 C18 1.379(7) . ?
C13 C14 1.406(7) . ?
C14 C15 1.369(8) . ?
C15 C16 1.372(9) . ?
C16 C17 1.354(8) . ?
C17 C18 1.384(8) . ?
C19 C24 1.390(7) . ?
C19 C20 1.394(6) . ?
C20 C21 1.382(7) . ?
C21 C22 1.370(7) . ?
C22 C23 1.388(7) . ?
C23 C24 1.394(6) . ?
C25 C26 1.389(6) . ?
C25 C30 1.410(6) . ?
C26 C27 1.374(6) . ?
C27 C28 1.411(7) . ?
C27 C31 1.469(6) . ?
C28 C29 1.373(6) . ?
C29 C30 1.406(6) . ?
C34 Cl3 1.748(6) . ?
C34 Cl4 1.760(6) . ?
C34 Cl5 1.762(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 Cl2 0.84 2.24 3.064(3) 165.8 1_565
O2 H2 O3 0.84 1.83 2.616(5) 155.5 2_766
