#------------------------------------------------------------------------------
#$Date: 2017-05-04 09:43:54 +0300 (Thu, 04 May 2017) $
#$Revision: 195969 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/57/4345790.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_4345790
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            'C36 H24 As2 Cl2 Pd'
_chemical_formula_weight         783.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.26(3)
_cell_length_b                   10.488(19)
_cell_length_c                   20.49(4)
_cell_measurement_reflns_used    980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.44
_cell_volume                     2961(10)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.2436
_diffrn_reflns_av_unetI/netI     0.2145
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8014
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        23.348
_diffrn_reflns_theta_max         23.348
_diffrn_reflns_theta_min         2.057
_exptl_absorpt_coefficient_mu    3.051
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.2741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.680
_refine_diff_density_min         -1.912
_refine_diff_density_rms         0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2071
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.2344
_refine_ls_R_factor_gt           0.1662
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3866
_refine_ls_wR_factor_ref         0.4322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1054
_reflns_number_total             2071
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00100_si_006.cif
_cod_data_source_block           07
_cod_database_code               4345790
_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, 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_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 0.1915(3) 0.2500 0.0488(12) Uani 1 2 d S T P
As1 As 0.5094(2) 0.3505(3) 0.33376(18) 0.0530(12) Uani 1 1 d . . .
Cl1 Cl 0.4775(6) 0.0349(6) 0.1647(4) 0.061(2) Uani 1 1 d . . .
C18 C 0.3372(16) 0.505(3) 0.3180(17) 0.060(9) Uani 1 1 d D . .
H18 H 0.3214 0.4390 0.3452 0.072 Uiso 1 1 calc R U .
C9 C 0.7194(19) 0.436(2) 0.3667(19) 0.061(10) Uani 1 1 d D . .
H9 H 0.7142 0.4501 0.3202 0.073 Uiso 1 1 calc R U .
C15 C 0.3876(19) 0.701(3) 0.2408(17) 0.065(9) Uani 1 1 d D . .
H15 H 0.4065 0.7716 0.2179 0.078 Uiso 1 1 calc R U .
C14 C 0.4506(18) 0.595(2) 0.2581(14) 0.047(8) Uani 1 1 d D . .
C8 C 0.636(2) 0.401(2) 0.3878(15) 0.058(9) Uani 1 1 d D . .
C7 C 0.642(2) 0.389(3) 0.4571(14) 0.078(10) Uani 1 1 d D U .
C10 C 0.809(2) 0.449(3) 0.4137(17) 0.074(11) Uani 1 1 d D . .
H10 H 0.8670 0.4634 0.3998 0.089 Uiso 1 1 calc R U .
C6 C 0.552(2) 0.343(3) 0.4717(14) 0.054(8) Uani 1 1 d D U .
C5 C 0.534(2) 0.321(3) 0.5342(18) 0.085(11) Uani 1 1 d D U .
H5 H 0.5842 0.3385 0.5738 0.102 Uiso 1 1 calc R U .
C16 C 0.297(2) 0.704(3) 0.257(2) 0.116(19) Uani 1 1 d D . .
H16 H 0.2547 0.7748 0.2437 0.139 Uiso 1 1 calc R U .
C12 C 0.730(2) 0.406(3) 0.5049(19) 0.073(10) Uani 1 1 d D U .
H12 H 0.7359 0.3930 0.5516 0.088 Uiso 1 1 calc R U .
C1 C 0.4756(19) 0.305(2) 0.4189(18) 0.077(12) Uani 1 1 d D . .
C17 C 0.270(2) 0.604(3) 0.2937(19) 0.088(14) Uani 1 1 d D . .
H17 H 0.2071 0.6020 0.3018 0.106 Uiso 1 1 calc R U .
C2 C 0.386(2) 0.260(3) 0.4231(18) 0.073(10) Uani 1 1 d D U .
H2 H 0.3362 0.2407 0.3835 0.088 Uiso 1 1 calc R U .
C13 C 0.4278(17) 0.503(2) 0.3021(14) 0.047(8) Uani 1 1 d D . .
C11 C 0.811(3) 0.442(3) 0.4819(19) 0.085(12) Uani 1 1 d D . .
H11 H 0.8692 0.4626 0.5145 0.102 Uiso 1 1 calc R U .
C4 C 0.4464(19) 0.275(3) 0.5408(18) 0.067(9) Uani 1 1 d D U .
H4 H 0.4380 0.2635 0.5849 0.081 Uiso 1 1 calc R U .
C3 C 0.371(3) 0.244(4) 0.4865(15) 0.094(12) Uani 1 1 d D U .
H3 H 0.3109 0.2137 0.4923 0.113 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 91.8(4) 2_655 .
Cl1 Pd1 As1 175.6(2) 2_655 2_655
Cl1 Pd1 As1 88.9(3) . 2_655
Cl1 Pd1 As1 88.9(3) 2_655 .
Cl1 Pd1 As1 175.6(2) . .
As1 Pd1 As1 90.7(2) 2_655 .
C8 As1 C1 88.0(11) . .
C8 As1 C13 110.6(10) . .
C1 As1 C13 103.0(10) . .
C8 As1 Pd1 118.3(7) . .
C1 As1 Pd1 119.1(8) . .
C13 As1 Pd1 114.2(8) . .
C13 C18 C17 120(3) . .
C13 C18 H18 119.8 . .
C17 C18 H18 119.8 . .
C10 C9 C8 121(3) . .
C10 C9 H9 119.7 . .
C8 C9 H9 119.7 . .
C16 C15 C14 121(3) . .
C16 C15 H15 119.5 . .
C14 C15 H15 119.5 . .
C13 C14 C15 117(2) . .
C13 C14 C14 121(2) . 2_655
C15 C14 C14 120.3(18) . 2_655
C7 C8 C9 120(3) . .
C7 C8 As1 111(2) . .
C9 C8 As1 129(2) . .
C12 C7 C8 120(3) . .
C12 C7 C6 125(3) . .
C8 C7 C6 114(2) . .
C11 C10 C9 117(3) . .
C11 C10 H10 121.4 . .
C9 C10 H10 121.4 . .
C1 C6 C5 112(3) . .
C1 C6 C7 119(3) . .
C5 C6 C7 128(3) . .
C4 C5 C6 122(3) . .
C4 C5 H5 118.8 . .
C6 C5 H5 118.8 . .
C17 C16 C15 120(3) . .
C17 C16 H16 119.8 . .
C15 C16 H16 119.8 . .
C7 C12 C11 118(4) . .
C7 C12 H12 121.0 . .
C11 C12 H12 121.0 . .
C6 C1 C2 127(3) . .
C6 C1 As1 107(2) . .
C2 C1 As1 125(2) . .
C16 C17 C18 119(3) . .
C16 C17 H17 120.6 . .
C18 C17 H17 120.6 . .
C3 C2 C1 118(3) . .
C3 C2 H2 121.1 . .
C1 C2 H2 121.1 . .
C14 C13 C18 121(2) . .
C14 C13 As1 123.0(15) . .
C18 C13 As1 115.3(16) . .
C10 C11 C12 124(4) . .
C10 C11 H11 118.2 . .
C12 C11 H11 118.2 . .
C3 C4 C5 123(4) . .
C3 C4 H4 118.5 . .
C5 C4 H4 118.5 . .
C4 C3 C2 117(4) . .
C4 C3 H3 121.4 . .
C2 C3 H3 121.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Cl1 2.358(9) 2_655
Pd1 Cl1 2.358(9) .
Pd1 As1 2.372(5) 2_655
Pd1 As1 2.372(5) .
As1 C8 1.94(3) .
As1 C1 1.98(4) .
As1 C13 1.99(2) .
C18 C13 1.411(18) .
C18 C17 1.415(18) .
C18 H18 0.9500 .
C9 C10 1.398(19) .
C9 C8 1.408(19) .
C9 H9 0.9500 .
C15 C16 1.416(18) .
C15 C14 1.422(17) .
C15 H15 0.9500 .
C14 C13 1.410(18) .
C14 C14 1.53(5) 2_655
C8 C7 1.408(19) .
C7 C12 1.394(19) .
C7 C6 1.47(4) .
C10 C11 1.394(19) .
C10 H10 0.9500 .
C6 C1 1.380(19) .
C6 C5 1.39(2) .
C5 C4 1.38(2) .
C5 H5 0.9500 .
C16 C17 1.405(18) .
C16 H16 0.9500 .
C12 C11 1.398(19) .
C12 H12 0.9500 .
C1 C2 1.388(19) .
C17 H17 0.9500 .
C2 C3 1.38(2) .
C2 H2 0.9500 .
C11 H11 0.9500 .
C4 C3 1.37(2) .
C4 H4 0.9500 .
C3 H3 0.9500 .
