#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:49:15 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180357 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/26/7202603.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_7202603
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_moiety         'C34 H30 Cl5 N O3 P2 Pd'
_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                91.922(1)
_cell_angle_beta                 102.160(1)
_cell_angle_gamma                117.036(1)
_cell_formula_units_Z            2
_cell_length_a                   10.4008(2)
_cell_length_b                   10.9060(2)
_cell_length_c                   17.6929(5)
_cell_measurement_temperature    120(2)
_cell_volume                     1728.13(7)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'φ and 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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11581
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.9020
_exptl_absorpt_correction_T_min  0.8171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV Blessing (1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6005
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0301
_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)+(0.0178P)²+1.8332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                5318
_reflns_number_total             6005
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b616337h.txt
_cod_data_source_block           2a.CHCl3
_cod_database_code               7202603
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 0.07705(2) 0.131213(18) 0.231813(10) 0.01440(8) Uani 1 1 d . . .
Cl1 Cl -0.14138(7) -0.01760(6) 0.26762(4) 0.02217(15) Uani 1 1 d . . .
Cl2 Cl -0.04467(7) 0.24679(7) 0.16369(4) 0.02286(16) Uani 1 1 d . . .
P1 P 0.18365(7) 0.02085(6) 0.30392(4) 0.01528(15) Uani 1 1 d . . .
P2 P 0.28185(7) 0.27365(6) 0.19462(4) 0.01475(15) Uani 1 1 d . . .
N1 N 0.4640(2) 0.2057(2) 0.30243(12) 0.0164(5) Uani 1 1 d . . .
O1 O 0.6586(2) 0.1364(2) 0.25263(12) 0.0303(5) Uani 1 1 d . . .
H1 H 0.7233 0.1159 0.2438 0.045 Uiso 1 1 calc R . .
O2 O 0.5048(2) 0.4376(2) 0.40311(11) 0.0373(5) Uani 1 1 d . . .
H2 H 0.4625 0.4719 0.4257 0.056 Uiso 1 1 calc R . .
O3 O 0.5914(3) 0.4138(2) 0.52530(12) 0.0386(5) Uani 1 1 d . . .
C1 C 0.0780(3) -0.1678(3) 0.28498(15) 0.0182(6) Uani 1 1 d . . .
C2 C -0.0106(3) -0.2422(3) 0.33347(17) 0.0288(7) Uani 1 1 d . . .
H2A H -0.0153 -0.1943 0.3778 0.035 Uiso 1 1 calc R . .
C3 C -0.0920(4) -0.3864(3) 0.31690(18) 0.0354(7) Uani 1 1 d . . .
H3 H -0.1532 -0.4368 0.3497 0.043 Uiso 1 1 calc R . .
C4 C -0.0846(3) -0.4570(3) 0.25317(17) 0.0291(7) Uani 1 1 d . . .
H4 H -0.1392 -0.5558 0.2427 0.035 Uiso 1 1 calc R . .
C5 C 0.0020(3) -0.3845(3) 0.20484(16) 0.0257(6) Uani 1 1 d . . .
H5 H 0.0070 -0.4331 0.1609 0.031 Uiso 1 1 calc R . .
C6 C 0.0821(3) -0.2400(3) 0.22026(15) 0.0221(6) Uani 1 1 d . . .
H6 H 0.1403 -0.1902 0.1861 0.027 Uiso 1 1 calc R . .
C7 C 0.2141(3) 0.0740(3) 0.40717(15) 0.0203(6) Uani 1 1 d U . .
C8 C 0.2720(4) 0.0147(3) 0.46407(17) 0.0331(7) Uani 1 1 d U . .
H8 H 0.2937 -0.0570 0.4492 0.040 Uiso 1 1 calc R . .
C9 C 0.2979(4) 0.0605(3) 0.54247(18) 0.0401(8) Uani 1 1 d U . .
H9 H 0.3366 0.0192 0.5811 0.048 Uiso 1 1 calc R . .
C10 C 0.2685(3) 0.1649(3) 0.56513(17) 0.0354(7) Uani 1 1 d U . .
H10 H 0.2869 0.1955 0.6191 0.043 Uiso 1 1 calc R . .
C11 C 0.2122(3) 0.2249(3) 0.50936(17) 0.0342(7) Uani 1 1 d U . .
H11 H 0.1915 0.2970 0.5248 0.041 Uiso 1 1 calc R . .
C12 C 0.1856(3) 0.1801(3) 0.43060(16) 0.0275(6) Uani 1 1 d U . .
H12 H 0.1475 0.2224 0.3923 0.033 Uiso 1 1 calc R . .
C13 C 0.3488(3) 0.4578(3) 0.22189(14) 0.0189(6) Uani 1 1 d . . .
C14 C 0.2900(3) 0.5074(3) 0.27109(15) 0.0216(6) Uani 1 1 d . . .
H14 H 0.2113 0.4440 0.2913 0.026 Uiso 1 1 calc R . .
C15 C 0.3462(3) 0.6501(3) 0.29087(16) 0.0284(7) Uani 1 1 d . . .
H15 H 0.3080 0.6842 0.3259 0.034 Uiso 1 1 calc R . .
C16 C 0.4573(3) 0.7418(3) 0.25959(17) 0.0311(7) Uani 1 1 d . . .
H16 H 0.4932 0.8391 0.2720 0.037 Uiso 1 1 calc R . .
C17 C 0.5168(3) 0.6938(3) 0.21047(17) 0.0316(7) Uani 1 1 d . . .
H17 H 0.5936 0.7576 0.1892 0.038 Uiso 1 1 calc R . .
C18 C 0.4640(3) 0.5522(3) 0.19247(16) 0.0252(6) Uani 1 1 d . . .
H18 H 0.5065 0.5189 0.1597 0.030 Uiso 1 1 calc R . .
C19 C 0.2415(3) 0.2413(3) 0.08898(15) 0.0183(5) Uani 1 1 d . . .
C20 C 0.2319(3) 0.3377(3) 0.04208(16) 0.0289(7) Uani 1 1 d . . .
H20 H 0.2475 0.4249 0.0651 0.035 Uiso 1 1 calc R . .
C21 C 0.1995(4) 0.3064(3) -0.03874(17) 0.0392(8) Uani 1 1 d . . .
H21 H 0.1944 0.3732 -0.0707 0.047 Uiso 1 1 calc R . .
C22 C 0.1747(3) 0.1801(3) -0.07270(17) 0.0351(8) Uani 1 1 d . . .
H22 H 0.1542 0.1602 -0.1279 0.042 Uiso 1 1 calc R . .
C23 C 0.1795(3) 0.0820(3) -0.02674(17) 0.0341(7) Uani 1 1 d . . .
H23 H 0.1600 -0.0063 -0.0503 0.041 Uiso 1 1 calc R . .
C24 C 0.2127(3) 0.1123(3) 0.05385(16) 0.0269(6) Uani 1 1 d . . .
H24 H 0.2158 0.0444 0.0854 0.032 Uiso 1 1 calc R . .
C25 C 0.6124(3) 0.2534(3) 0.34981(16) 0.0213(6) Uani 1 1 d . . .
C26 C 0.7096(3) 0.2130(3) 0.32436(16) 0.0234(6) Uani 1 1 d . . .
C27 C 0.8498(3) 0.2496(3) 0.37187(17) 0.0296(7) Uani 1 1 d . . .
H27 H 0.9171 0.2277 0.3531 0.036 Uiso 1 1 calc R . .
C28 C 0.8907(3) 0.3188(3) 0.44717(18) 0.0323(7) Uani 1 1 d . . .
H28 H 0.9844 0.3395 0.4809 0.039 Uiso 1 1 calc R . .
C29 C 0.7978(3) 0.3578(3) 0.47374(16) 0.0245(6) Uani 1 1 d . . .
H29 H 0.8268 0.4040 0.5256 0.029 Uiso 1 1 calc R . .
C30 C 0.6604(3) 0.3293(3) 0.42410(16) 0.0239(6) Uani 1 1 d . . .
C31 C 0.5784(3) 0.3936(3) 0.45428(17) 0.0243(6) Uani 1 1 d . . .
C32 C 0.3699(3) 0.0556(3) 0.29622(15) 0.0188(6) Uani 1 1 d . . .
H32A H 0.4146 0.0189 0.3385 0.023 Uiso 1 1 calc R . .
H32B H 0.3624 0.0086 0.2454 0.023 Uiso 1 1 calc R . .
C33 C 0.4521(3) 0.2534(3) 0.22649(15) 0.0190(6) Uani 1 1 d . . .
H33A H 0.4504 0.1857 0.1871 0.023 Uiso 1 1 calc R . .
H33B H 0.5411 0.3439 0.2294 0.023 Uiso 1 1 calc R . .
Cl3 Cl 0.41169(10) 0.70488(9) -0.02806(5) 0.0463(2) Uani 1 1 d . . .
Cl4 Cl 0.44074(10) 0.92043(8) 0.08405(5) 0.0425(2) Uani 1 1 d . . .
Cl5 Cl 0.16364(10) 0.66377(11) 0.03437(5) 0.0535(2) Uani 1 1 d . . .
C34 C 0.3188(3) 0.7861(3) 0.00533(17) 0.0322(7) Uani 1 1 d . . .
H34 H 0.2830 0.8278 -0.0384 0.039 Uiso 1 1 calc R . .
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
Cl1 Pd1 Cl2 90.68(2) . . ?
Cl1 Pd1 P1 85.91(2) . . ?
Cl1 Pd1 P2 178.46(2) . . ?
Cl2 Pd1 P1 175.52(2) . . ?
Cl2 Pd1 P2 88.01(2) . . ?
P1 Pd1 P2 95.44(2) . . ?
Pd1 P1 C1 114.90(8) . . ?
Pd1 P1 C7 110.15(9) . . ?
Pd1 P1 C32 117.14(9) . . ?
C1 P1 C7 107.49(12) . . ?
C1 P1 C32 103.25(12) . . ?
C7 P1 C32 102.82(12) . . ?
Pd1 P2 C13 115.51(9) . . ?
Pd1 P2 C19 108.58(8) . . ?
Pd1 P2 C33 118.37(8) . . ?
C13 P2 C19 107.01(12) . . ?
C13 P2 C33 103.46(12) . . ?
C19 P2 C33 102.69(12) . . ?
C25 N1 C32 113.0(2) . . ?
C25 N1 C33 116.0(2) . . ?
C32 N1 C33 111.9(2) . . ?
P1 C1 C2 121.2(2) . . ?
P1 C1 C6 119.8(2) . . ?
C2 C1 C6 118.9(2) . . ?
C1 C2 C3 120.0(3) . . ?
C2 C3 C4 120.5(3) . . ?
C3 C4 C5 120.0(3) . . ?
C4 C5 C6 120.0(3) . . ?
C1 C6 C5 120.6(3) . . ?
P1 C7 C8 121.2(2) . . ?
P1 C7 C12 119.8(2) . . ?
C8 C7 C12 118.9(3) . . ?
C7 C8 C9 119.7(3) . . ?
C8 C9 C10 121.0(3) . . ?
C9 C10 C11 119.7(3) . . ?
C10 C11 C12 120.0(3) . . ?
C7 C12 C11 120.7(3) . . ?
P2 C13 C14 122.2(2) . . ?
P2 C13 C18 118.5(2) . . ?
C14 C13 C18 119.3(2) . . ?
C13 C14 C15 120.0(3) . . ?
C14 C15 C16 119.9(3) . . ?
C15 C16 C17 120.6(3) . . ?
C16 C17 C18 119.5(3) . . ?
C13 C18 C17 120.6(3) . . ?
P2 C19 C20 122.5(2) . . ?
P2 C19 C24 118.4(2) . . ?
C20 C19 C24 119.1(2) . . ?
C19 C20 C21 119.8(3) . . ?
C20 C21 C22 120.6(3) . . ?
C21 C22 C23 120.0(3) . . ?
C22 C23 C24 119.9(3) . . ?
C19 C24 C23 120.5(3) . . ?
N1 C25 C26 120.0(2) . . ?
N1 C25 C30 121.5(2) . . ?
C26 C25 C30 118.3(2) . . ?
O1 C26 C25 117.0(2) . . ?
O1 C26 C27 122.2(3) . . ?
C25 C26 C27 120.8(3) . . ?
C26 C27 C28 119.2(3) . . ?
C27 C28 C29 121.1(3) . . ?
C28 C29 C30 119.8(3) . . ?
C25 C30 C29 120.6(3) . . ?
C25 C30 C31 123.8(2) . . ?
C29 C30 C31 115.5(2) . . ?
O2 C31 O3 122.8(3) . . ?
O2 C31 C30 116.7(2) . . ?
O3 C31 C30 120.3(2) . . ?
P1 C32 N1 109.21(17) . . ?
P2 C33 N1 112.30(17) . . ?
Cl3 C34 Cl4 110.53(17) . . ?
Cl3 C34 Cl5 110.25(17) . . ?
Cl4 C34 Cl5 110.13(17) . . ?
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 Cl1 2.3495(6) . ?
Pd1 Cl2 2.3566(6) . ?
Pd1 P1 2.2419(7) . ?
Pd1 P2 2.2437(7) . ?
P1 C1 1.815(3) . ?
P1 C7 1.815(3) . ?
P1 C32 1.833(3) . ?
P2 C13 1.809(3) . ?
P2 C19 1.812(3) . ?
P2 C33 1.856(3) . ?
N1 C25 1.432(3) . ?
N1 C32 1.462(3) . ?
N1 C33 1.458(3) . ?
O1 C26 1.354(3) . ?
O2 C31 1.306(3) . ?
O3 C31 1.236(3) . ?
C1 C2 1.394(4) . ?
C1 C6 1.387(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.379(4) . ?
C4 C5 1.374(4) . ?
C5 C6 1.391(4) . ?
C7 C8 1.392(4) . ?
C7 C12 1.389(4) . ?
C8 C9 1.386(4) . ?
C9 C10 1.374(5) . ?
C10 C11 1.376(5) . ?
C11 C12 1.388(4) . ?
C13 C14 1.385(4) . ?
C13 C18 1.394(4) . ?
C14 C15 1.391(4) . ?
C15 C16 1.377(4) . ?
C16 C17 1.380(4) . ?
C17 C18 1.381(4) . ?
C19 C20 1.386(4) . ?
C19 C24 1.392(4) . ?
C20 C21 1.391(4) . ?
C21 C22 1.372(4) . ?
C22 C23 1.377(5) . ?
C23 C24 1.385(4) . ?
C25 C26 1.415(4) . ?
C25 C30 1.392(4) . ?
C26 C27 1.387(4) . ?
C27 C28 1.388(4) . ?
C28 C29 1.373(4) . ?
C29 C30 1.400(4) . ?
C30 C31 1.489(4) . ?
Cl3 C34 1.747(3) . ?
Cl4 C34 1.768(3) . ?
Cl5 C34 1.756(3) . ?
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 Cl1 0.84 2.44 3.192(2) 150.3 1_655
O1 H1 Cl2 0.84 2.88 3.499(2) 131.7 1_655
O2 H2 O3 0.84 1.84 2.665(3) 166.4 2_666
