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#$Date: 2017-05-04 09:44:31 +0300 (Thu, 04 May 2017) $
#$Revision: 195971 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/57/4345792.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_4345792
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 Cl4 Pd2'
_chemical_formula_weight         923.03
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   34.074(5)
_cell_length_b                   34.074(5)
_cell_length_c                   7.4287(16)
_cell_measurement_reflns_used    2493
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.14
_cell_measurement_theta_min      2.39
_cell_volume                     7469(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2014 (Sheldrick 2014)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1750
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            20694
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        23.619
_diffrn_reflns_theta_max         23.619
_diffrn_reflns_theta_min         2.070
_exptl_absorpt_coefficient_mu    3.405
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.2083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       rod
_exptl_crystal_F_000             4068
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.801
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2476
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0713P)²+595.2180P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1455
_reflns_number_total             2476
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic7b00100_si_008.cif
_cod_data_source_block           05
_cod_original_cell_volume        7470(3)
_cod_database_code               4345792
_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C7 C 0.5796(5) 0.9090(5) 0.4941(19) 0.061(6) Uani 1 1 d G .
C8 C 0.5838(5) 0.8713(5) 0.459(2) 0.065(6) Uani 1 1 d G .
C9 C 0.6033(6) 0.8685(6) 0.298(2) 0.107(9) Uani 1 1 d G U
H9 H 0.6061 0.8426 0.2738 0.129 Uiso 1 1 calc R U
C10 C 0.6185(6) 0.9034(9) 0.1732(19) 0.159(14) Uani 1 1 d G U
H10 H 0.6318 0.9015 0.0635 0.191 Uiso 1 1 calc R U
C11 C 0.6143(6) 0.9412(7) 0.209(2) 0.131(11) Uani 1 1 d G U
H11 H 0.6247 0.9651 0.1234 0.157 Uiso 1 1 calc R U
C12 C 0.5949(6) 0.9440(5) 0.369(3) 0.106(10) Uani 1 1 d G .
H12 H 0.5920 0.9699 0.3936 0.127 Uiso 1 1 calc R U
Pd1 Pd 0.61003(4) 0.81527(5) 0.8142(2) 0.0479(5) Uani 1 1 d . .
As1 As 0.56146(6) 0.82884(6) 0.6427(3) 0.0498(6) Uani 1 1 d . .
C1 C 0.5437(5) 0.8659(4) 0.7645(19) 0.057(5) Uani 1 1 d G .
C2 C 0.5217(5) 0.8597(6) 0.9286(19) 0.105(11) Uani 1 1 d G .
H2 H 0.5128 0.8329 0.9965 0.127 Uiso 1 1 calc R U
C3 C 0.5127(6) 0.8927(9) 0.9935(19) 0.138(15) Uani 1 1 d G .
H3 H 0.4977 0.8884 1.1056 0.166 Uiso 1 1 calc R U
C4 C 0.5257(7) 0.9319(7) 0.894(3) 0.142(17) Uani 1 1 d G .
H4 H 0.5196 0.9544 0.9386 0.170 Uiso 1 1 calc R U
C5 C 0.5477(6) 0.9381(4) 0.730(3) 0.104(11) Uani 1 1 d G .
H5 H 0.5565 0.9649 0.6623 0.125 Uiso 1 1 calc R U
C6 C 0.5566(4) 0.9051(4) 0.6653(17) 0.056(6) Uani 1 1 d G .
C13 C 0.5092(8) 0.7768(8) 0.542(6) 0.144(16) Uani 1 1 d . .
H13A H 0.5193 0.7653 0.4399 0.173 Uiso 1 1 calc R U
H13B H 0.4962 0.7527 0.6343 0.173 Uiso 1 1 calc R U
C14 C 0.4724(7) 0.7854(7) 0.476(4) 0.084(8) Uani 1 1 d D .
H14A H 0.4841 0.8072 0.3747 0.101 Uiso 1 1 calc R U
H14B H 0.4634 0.7989 0.5739 0.101 Uiso 1 1 calc R U
C15 C 0.4298(8) 0.7400(9) 0.411(5) 0.146(12) Uani 1 1 d D U
H15A H 0.4376 0.7286 0.3018 0.175 Uiso 1 1 calc R U
H15B H 0.4206 0.7166 0.5062 0.175 Uiso 1 1 calc R U
C16 C 0.3911(11) 0.7484(13) 0.370(6) 0.185(19) Uani 1 1 d D .
H16A H 0.3869 0.7643 0.4719 0.277 Uiso 1 1 calc R U
H16B H 0.3632 0.7194 0.3509 0.277 Uiso 1 1 calc R U
H16C H 0.3982 0.7671 0.2616 0.277 Uiso 1 1 calc R U
Cl1 Cl 0.67357(15) 0.86110(16) 0.6469(6) 0.0506(12) Uani 1 1 d . .
Cl2 Cl 0.54631(19) 0.7703(3) 0.9727(13) 0.131(4) Uani 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'
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_3
C8 C7 C12 120.0 .
C8 C7 C6 112.3(12) .
C12 C7 C6 127.7(12) .
C9 C8 C7 120.0 .
C9 C8 As1 127.1(10) .
C7 C8 As1 112.9(10) .
C10 C9 C8 120.0 .
C10 C9 H9 120.0 .
C8 C9 H9 120.0 .
C9 C10 C11 120.0 .
C9 C10 H10 120.0 .
C11 C10 H10 120.0 .
C12 C11 C10 120.0 .
C12 C11 H11 120.0 .
C10 C11 H11 120.0 .
C11 C12 C7 120.0 .
C11 C12 H12 120.0 .
C7 C12 H12 120.0 .
Cl2 Pd1 Cl1 178.4(2) .
Cl2 Pd1 As1 83.21(17) .
Cl1 Pd1 As1 95.26(13) .
Cl2 Pd1 Cl1 94.5(2) 16_666
Cl1 Pd1 Cl1 87.01(16) 16_666
As1 Pd1 Cl1 173.81(14) 16_666
C8 As1 C1 88.7(6) .
C8 As1 C13 105.1(13) .
C1 As1 C13 110.1(10) .
C8 As1 Pd1 120.4(4) .
C1 As1 Pd1 111.9(4) .
C13 As1 Pd1 117.1(8) .
C2 C1 C6 120.0 .
C2 C1 As1 130.4(9) .
C6 C1 As1 109.6(9) .
C1 C2 C3 120.0 .
C1 C2 H2 120.0 .
C3 C2 H2 120.0 .
C2 C3 C4 120.0 .
C2 C3 H3 120.0 .
C4 C3 H3 120.0 .
C5 C4 C3 120.0 .
C5 C4 H4 120.0 .
C3 C4 H4 120.0 .
C6 C5 C4 120.0 .
C6 C5 H5 120.0 .
C4 C5 H5 120.0 .
C5 C6 C1 120.0 .
C5 C6 C7 123.4(11) .
C1 C6 C7 116.6(11) .
C14 C13 As1 115.2(15) .
C14 C13 H13A 108.5 .
As1 C13 H13A 108.5 .
C14 C13 H13B 108.5 .
As1 C13 H13B 108.5 .
H13A C13 H13B 107.5 .
C13 C14 C15 110.9(18) .
C13 C14 H14A 109.5 .
C15 C14 H14A 109.5 .
C13 C14 H14B 109.5 .
C15 C14 H14B 109.5 .
H14A C14 H14B 108.1 .
C16 C15 C14 110(2) .
C16 C15 H15A 109.8 .
C14 C15 H15A 109.8 .
C16 C15 H15B 109.8 .
C14 C15 H15B 109.8 .
H15A C15 H15B 108.2 .
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 .
Pd1 Cl1 Pd1 92.98(16) 16_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C7 C8 1.3900 .
C7 C12 1.3900 .
C7 C6 1.464(18) .
C8 C9 1.3900 .
C8 As1 1.855(13) .
C9 C10 1.3900 .
C9 H9 0.9500 .
C10 C11 1.3900 .
C10 H10 0.9500 .
C11 C12 1.3900 .
C11 H11 0.9500 .
C12 H12 0.9500 .
Pd1 Cl2 2.264(6) .
Pd1 Cl1 2.300(5) .
Pd1 As1 2.311(2) .
Pd1 Cl1 2.424(5) 16_666
As1 C1 1.884(11) .
As1 C13 1.93(2) .
C1 C2 1.3900 .
C1 C6 1.3900 .
C2 C3 1.3900 .
C2 H2 0.9500 .
C3 C4 1.3900 .
C3 H3 0.9500 .
C4 C5 1.3900 .
C4 H4 0.9500 .
C5 C6 1.3900 .
C5 H5 0.9500 .
C13 C14 1.50(3) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.577(18) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.515(19) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
Cl1 Pd1 2.424(5) 16_666
