#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:55:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179084 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/46/4304633.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_4304633
loop_
_publ_author_name
'Natalia Moldovan'
'Peter Lönnecke'
'Ioan Silaghi-Dumitrescu'
'Luminita Silaghi-Dumitrescu'
'Evamarie Hey-Hawkins'
_publ_section_title
;
Palladium(II) and Platinum(II) Complexes with Heteroditopic
10-(Aryl)phenoxarsine (Aryl = 2-C6H4OR, R = H, Me, Pri) Ligands:
Solvent-Oriented Crystallization of cis Isomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1524
_journal_page_last               1531
_journal_paper_doi               10.1021/ic7021648
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C42 H38 As2 Cl2 O4 Pd'
_chemical_formula_weight         933.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.956(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.865(2)
_cell_length_b                   12.586(3)
_cell_length_c                   14.840(3)
_cell_measurement_reflns_used    861
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      4.08
_cell_volume                     1907.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia, 1997)'
_computing_publication_material  'WINGX  (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick,1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11761
_diffrn_reflns_theta_full        29.07
_diffrn_reflns_theta_max         29.07
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    2.390
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0317
_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)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                3679
_reflns_number_total             4684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7021648-file003.cif
_cod_data_source_block           c1915fin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4304633
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 1.0000 0.0000 1.0000 0.02452(8) Uani 1 2 d S . .
As1 As 0.89603(2) 0.01935(2) 1.118440(19) 0.02646(8) Uani 1 1 d . . .
Cl1 Cl 0.81211(7) -0.06393(6) 0.88853(5) 0.04227(19) Uani 1 1 d . . .
O1 O 1.0275(2) -0.17834(17) 1.19319(16) 0.0493(6) Uani 1 1 d . . .
O2 O 0.6542(2) 0.1098(2) 1.16929(18) 0.0574(6) Uani 1 1 d . . .
C1 C 1.0019(3) -0.0117(2) 1.2501(2) 0.0312(6) Uani 1 1 d . . .
C2 C 1.0641(3) -0.1090(2) 1.2693(2) 0.0397(7) Uani 1 1 d . . .
C3 C 1.1511(3) -0.1319(3) 1.3611(2) 0.0533(9) Uani 1 1 d . . .
H3 H 1.1973 -0.1965 1.3737 0.064 Uiso 1 1 calc R . .
C4 C 1.1679(4) -0.0574(3) 1.4333(2) 0.0591(10) Uani 1 1 d . . .
H4 H 1.2271 -0.0714 1.4951 0.071 Uiso 1 1 calc R . .
C5 C 1.1003(4) 0.0354(3) 1.4160(2) 0.0587(10) Uani 1 1 d . . .
H5 H 1.1094 0.0833 1.4664 0.070 Uiso 1 1 calc R . .
C6 C 1.0175(3) 0.0598(3) 1.3237(2) 0.0443(7) Uani 1 1 d . . .
H6 H 0.9722 0.1248 1.3115 0.053 Uiso 1 1 calc R . .
C7 C 1.1033(4) -0.2743(3) 1.1962(3) 0.0587(10) Uani 1 1 d . . .
H7 H 1.1292 -0.3064 1.2609 0.070 Uiso 1 1 calc R . .
C8 C 1.2233(4) -0.2423(3) 1.1743(3) 0.0723(12) Uani 1 1 d . . .
H8A H 1.1975 -0.2133 1.1100 0.109 Uiso 1 1 calc R . .
H8B H 1.2787 -0.3039 1.1789 0.109 Uiso 1 1 calc R . .
H8C H 1.2712 -0.1888 1.2200 0.109 Uiso 1 1 calc R . .
C9 C 1.0115(4) -0.3476(3) 1.1242(3) 0.0798(14) Uani 1 1 d . . .
H9A H 0.9378 -0.3646 1.1444 0.120 Uiso 1 1 calc R . .
H9B H 1.0574 -0.4124 1.1197 0.120 Uiso 1 1 calc R . .
H9C H 0.9802 -0.3131 1.0620 0.120 Uiso 1 1 calc R . .
C10 C 0.6373(3) 0.0085(3) 1.1303(2) 0.0429(7) Uani 1 1 d . . .
C11 C 0.5185(3) -0.0389(3) 1.1215(2) 0.0553(9) Uani 1 1 d . . .
H11 H 0.4551 -0.0015 1.1389 0.066 Uiso 1 1 calc R . .
C12 C 0.4941(3) -0.1404(3) 1.0873(3) 0.0564(10) Uani 1 1 d . . .
H12 H 0.4143 -0.1729 1.0828 0.068 Uiso 1 1 calc R . .
C13 C 0.5833(3) -0.1952(3) 1.0596(2) 0.0529(9) Uani 1 1 d . . .
H13 H 0.5642 -0.2643 1.0348 0.063 Uiso 1 1 calc R . .
C14 C 0.7028(3) -0.1485(2) 1.0683(2) 0.0417(7) Uani 1 1 d . . .
H14 H 0.7648 -0.1866 1.0498 0.050 Uiso 1 1 calc R . .
C15 C 0.7311(2) -0.0459(2) 1.10410(19) 0.0327(6) Uani 1 1 d . . .
C16 C 0.7355(3) 0.1852(3) 1.1531(2) 0.0427(7) Uani 1 1 d . . .
C17 C 0.8444(3) 0.1632(2) 1.12875(19) 0.0349(6) Uani 1 1 d . . .
C18 C 0.9199(3) 0.2473(2) 1.1163(2) 0.0458(8) Uani 1 1 d . . .
H18 H 0.9941 0.2334 1.0993 0.055 Uiso 1 1 calc R . .
C19 C 0.8874(4) 0.3512(3) 1.1286(2) 0.0597(10) Uani 1 1 d . . .
H19 H 0.9385 0.4077 1.1195 0.072 Uiso 1 1 calc R . .
C20 C 0.7797(4) 0.3707(3) 1.1543(2) 0.0612(11) Uani 1 1 d . . .
H20 H 0.7583 0.4412 1.1639 0.073 Uiso 1 1 calc R . .
C21 C 0.7033(4) 0.2899(3) 1.1660(2) 0.0562(10) Uani 1 1 d . . .
H21 H 0.6291 0.3047 1.1828 0.067 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
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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 Cl1 180.0 . 3_757 ?
Cl1 Pd1 As1 92.19(3) . . ?
Cl1 Pd1 As1 87.81(3) 3_757 . ?
Cl1 Pd1 As1 87.81(3) . 3_757 ?
Cl1 Pd1 As1 92.19(3) 3_757 3_757 ?
As1 Pd1 As1 180.0 . 3_757 ?
C15 As1 C17 97.21(13) . . ?
C15 As1 C1 103.67(11) . . ?
C17 As1 C1 101.49(11) . . ?
C15 As1 Pd1 122.03(9) . . ?
C17 As1 Pd1 112.17(9) . . ?
C1 As1 Pd1 116.81(8) . . ?
C2 O1 C7 120.0(2) . . ?
C16 O2 C10 124.4(2) . . ?
C2 C1 C6 119.7(3) . . ?
C2 C1 As1 117.9(2) . . ?
C6 C1 As1 122.4(2) . . ?
O1 C2 C1 114.2(3) . . ?
O1 C2 C3 125.4(3) . . ?
C1 C2 C3 120.3(3) . . ?
C4 C3 C2 118.7(3) . . ?
C5 C4 C3 121.0(3) . . ?
C4 C5 C6 120.2(3) . . ?
C1 C6 C5 119.9(3) . . ?
O1 C7 C8 107.1(3) . . ?
O1 C7 C9 104.9(3) . . ?
C8 C7 C9 115.2(4) . . ?
O2 C10 C11 114.9(3) . . ?
O2 C10 C15 124.4(3) . . ?
C11 C10 C15 120.6(3) . . ?
C12 C11 C10 119.6(3) . . ?
C13 C12 C11 121.2(3) . . ?
C12 C13 C14 119.7(3) . . ?
C13 C14 C15 120.3(3) . . ?
C10 C15 C14 118.5(3) . . ?
C10 C15 As1 120.4(2) . . ?
C14 C15 As1 121.1(2) . . ?
O2 C16 C17 124.6(3) . . ?
O2 C16 C21 115.1(3) . . ?
C17 C16 C21 120.3(3) . . ?
C16 C17 C18 118.7(3) . . ?
C16 C17 As1 120.8(2) . . ?
C18 C17 As1 120.4(2) . . ?
C19 C18 C17 120.9(3) . . ?
C20 C19 C18 119.2(4) . . ?
C21 C20 C19 121.1(3) . . ?
C20 C21 C16 119.8(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 Cl1 2.2904(7) . ?
Pd1 Cl1 2.2904(7) 3_757 ?
Pd1 As1 2.4042(5) . ?
Pd1 As1 2.4042(5) 3_757 ?
As1 C15 1.915(3) . ?
As1 C17 1.917(3) . ?
As1 C1 1.939(3) . ?
O1 C2 1.375(4) . ?
O1 C7 1.455(4) . ?
O2 C16 1.372(4) . ?
O2 C10 1.387(4) . ?
C1 C2 1.380(4) . ?
C1 C6 1.380(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.388(5) . ?
C4 C5 1.357(5) . ?
C5 C6 1.393(4) . ?
C7 C8 1.502(5) . ?
C7 C9 1.503(5) . ?
C10 C11 1.387(4) . ?
C10 C15 1.389(4) . ?
C11 C12 1.366(5) . ?
C12 C13 1.362(5) . ?
C13 C14 1.391(4) . ?
C14 C15 1.391(4) . ?
C16 C17 1.378(4) . ?
C16 C21 1.393(4) . ?
C17 C18 1.390(4) . ?
C18 C19 1.382(4) . ?
C19 C20 1.370(5) . ?
C20 C21 1.361(5) . ?
