#------------------------------------------------------------------------------
#$Date: 2017-05-04 09:44:14 +0300 (Thu, 04 May 2017) $
#$Revision: 195970 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/57/4345791.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_4345791
loop_
_publ_author_name
'Gupta, Arvind Kumar'
'Akkarasamiyo, Sunisa'
'Orthaber, Andreas'
_publ_section_title
;
 Rich Coordination Chemistry of π-Acceptor Dibenzoarsole Ligands.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4505
_journal_page_last               4512
_journal_paper_doi               10.1021/acs.inorgchem.7b00100
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C32 H34 As2 Cl2 Pd'
_chemical_formula_weight         745.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.0470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6433(3)
_cell_length_b                   14.8474(4)
_cell_length_c                   10.5173(3)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.46
_cell_volume                     1431.76(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29775
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         4.076
_exptl_absorpt_coefficient_mu    3.149
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5429
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0160P)²+0.9245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3331
_reflns_number_total             3546
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00100_si_007.cif
_cod_data_source_block           06
_cod_database_code               4345791
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.5000 0.5000 0.5000 0.00836(5) Uani 1 2 d S . P
As1 As 0.52659(2) 0.47987(2) 0.28192(2) 0.00903(5) Uani 1 1 d . . .
Cl1 Cl 0.35999(5) 0.37308(3) 0.48290(4) 0.01595(9) Uani 1 1 d . . .
C1 C 0.45441(18) 0.37290(10) 0.17822(15) 0.0113(3) Uani 1 1 d . . .
C2 C 0.31207(18) 0.34206(11) 0.12809(16) 0.0136(3) Uani 1 1 d . . .
H2 H 0.2342 0.3757 0.1419 0.016 Uiso 1 1 calc R U .
C3 C 0.28434(19) 0.26136(11) 0.05745(16) 0.0153(3) Uani 1 1 d . . .
H3 H 0.1870 0.2401 0.0217 0.018 Uiso 1 1 calc R U .
C4 C 0.39872(19) 0.21187(11) 0.03921(16) 0.0155(3) Uani 1 1 d . . .
H4 H 0.3792 0.1562 -0.0075 0.019 Uiso 1 1 calc R U .
C5 C 0.54122(19) 0.24268(11) 0.08838(15) 0.0136(3) Uani 1 1 d . . .
H5 H 0.6186 0.2087 0.0742 0.016 Uiso 1 1 calc R U .
C6 C 0.57034(18) 0.32355(11) 0.15863(15) 0.0114(3) Uani 1 1 d . . .
C7 C 0.71628(17) 0.36498(10) 0.21314(15) 0.0110(3) Uani 1 1 d . . .
C8 C 0.84698(18) 0.32890(11) 0.20484(16) 0.0143(3) Uani 1 1 d . . .
H8 H 0.8476 0.2728 0.1617 0.017 Uiso 1 1 calc R U .
C9 C 0.97629(19) 0.37603(12) 0.26046(17) 0.0163(3) Uani 1 1 d . . .
H9 H 1.0655 0.3511 0.2563 0.020 Uiso 1 1 calc R U .
C10 C 0.97724(19) 0.45869(12) 0.32184(17) 0.0161(3) Uani 1 1 d . . .
H10 H 1.0663 0.4905 0.3575 0.019 Uiso 1 1 calc R U .
C11 C 0.84775(19) 0.49523(11) 0.33132(17) 0.0142(3) Uani 1 1 d . . .
H11 H 0.8478 0.5517 0.3738 0.017 Uiso 1 1 calc R U .
C12 C 0.71846(17) 0.44788(11) 0.27768(15) 0.0106(3) Uani 1 1 d . . .
C13 C 0.47663(18) 0.58460(11) 0.16359(16) 0.0139(3) Uani 1 1 d . . .
H13A H 0.5593 0.6275 0.1886 0.017 Uiso 1 1 calc R U .
H13B H 0.4630 0.5647 0.0707 0.017 Uiso 1 1 calc R U .
C14 C 0.33910(18) 0.63342(11) 0.16824(16) 0.0148(3) Uani 1 1 d . . .
H14A H 0.3538 0.6550 0.2605 0.018 Uiso 1 1 calc R U .
H14B H 0.3237 0.6868 0.1091 0.018 Uiso 1 1 calc R U .
C15 C 0.20291(19) 0.57488(12) 0.12547(17) 0.0166(3) Uani 1 1 d . . .
H15A H 0.1965 0.5456 0.0393 0.020 Uiso 1 1 calc R U .
H15B H 0.2118 0.5268 0.1928 0.020 Uiso 1 1 calc R U .
C16 C 0.0635(2) 0.62722(12) 0.10986(18) 0.0195(4) Uani 1 1 d . . .
H16A H 0.0688 0.6564 0.1948 0.029 Uiso 1 1 calc R U .
H16B H -0.0199 0.5859 0.0843 0.029 Uiso 1 1 calc R U .
H16C H 0.0514 0.6731 0.0403 0.029 Uiso 1 1 calc R U .
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl1 Pd1 Cl1 180.0 3_666 .
Cl1 Pd1 As1 86.717(11) 3_666 .
Cl1 Pd1 As1 93.283(11) . .
Cl1 Pd1 As1 93.284(11) 3_666 3_666
Cl1 Pd1 As1 86.716(11) . 3_666
As1 Pd1 As1 180.0 . 3_666
C12 As1 C1 87.98(7) . .
C12 As1 C13 103.33(7) . .
C1 As1 C13 108.65(7) . .
C12 As1 Pd1 116.13(4) . .
C1 As1 Pd1 121.00(5) . .
C13 As1 Pd1 115.47(5) . .
C2 C1 C6 120.74(14) . .
C2 C1 As1 128.88(13) . .
C6 C1 As1 110.37(11) . .
C1 C2 C3 119.42(16) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C4 C3 C2 120.03(15) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C3 C4 C5 120.80(15) . .
C3 C4 H4 119.6 . .
C5 C4 H4 119.6 . .
C4 C5 C6 119.73(16) . .
C4 C5 H5 120.1 . .
C6 C5 H5 120.1 . .
C5 C6 C1 119.28(15) . .
C5 C6 C7 125.14(15) . .
C1 C6 C7 115.55(14) . .
C8 C7 C12 119.22(15) . .
C8 C7 C6 125.80(15) . .
C12 C7 C6 114.98(14) . .
C9 C8 C7 119.31(15) . .
C9 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
C10 C9 C8 121.15(16) . .
C10 C9 H9 119.4 . .
C8 C9 H9 119.4 . .
C9 C10 C11 120.11(16) . .
C9 C10 H10 119.9 . .
C11 C10 H10 119.9 . .
C12 C11 C10 119.03(15) . .
C12 C11 H11 120.5 . .
C10 C11 H11 120.5 . .
C11 C12 C7 121.16(15) . .
C11 C12 As1 127.87(12) . .
C7 C12 As1 110.95(12) . .
C14 C13 As1 113.74(11) . .
C14 C13 H13A 108.8 . .
As1 C13 H13A 108.8 . .
C14 C13 H13B 108.8 . .
As1 C13 H13B 108.8 . .
H13A C13 H13B 107.7 . .
C15 C14 C13 113.48(14) . .
C15 C14 H14A 108.9 . .
C13 C14 H14A 108.9 . .
C15 C14 H14B 108.9 . .
C13 C14 H14B 108.9 . .
H14A C14 H14B 107.7 . .
C16 C15 C14 113.22(14) . .
C16 C15 H15A 108.9 . .
C14 C15 H15A 108.9 . .
C16 C15 H15B 108.9 . .
C14 C15 H15B 108.9 . .
H15A C15 H15B 107.7 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl1 2.2925(4) 3_666
Pd1 Cl1 2.2925(4) .
Pd1 As1 2.40414(17) .
Pd1 As1 2.40417(17) 3_666
As1 C12 1.9241(16) .
As1 C1 1.9303(15) .
As1 C13 1.9563(16) .
C1 C2 1.387(2) .
C1 C6 1.404(2) .
C2 C3 1.391(2) .
C2 H2 0.9500 .
C3 C4 1.387(2) .
C3 H3 0.9500 .
C4 C5 1.387(2) .
C4 H4 0.9500 .
C5 C6 1.392(2) .
C5 H5 0.9500 .
C6 C7 1.479(2) .
C7 C8 1.397(2) .
C7 C12 1.403(2) .
C8 C9 1.391(2) .
C8 H8 0.9500 .
C9 C10 1.385(2) .
C9 H9 0.9500 .
C10 C11 1.393(2) .
C10 H10 0.9500 .
C11 C12 1.390(2) .
C11 H11 0.9500 .
C13 C14 1.525(2) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.522(2) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.517(2) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
