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#$Date: 2016-03-25 14:54:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179905 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/01/7020111.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_7020111
loop_
_publ_author_name
'Warren, Mark R.'
'Brayshaw, Simon K.'
'Hatcher, Lauren E.'
'Johnson, Andrew L.'
'Schiffers, Stefanie'
'Warren, Anna J.'
'Teat, Simon J.'
'Warren, John E.'
'Woodall, Christopher H.'
'Raithby, Paul R.'
_publ_section_title
;
 Photoactivated linkage isomerism in single crystals of nickel, palladium
 and platinum di-nitro complexes - a photocrystallographic investigation.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13173
_journal_page_last               13179
_journal_paper_doi               10.1039/c2dt30314k
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C36 H30 As2 N2 O4 Pd'
_chemical_formula_sum            'C36 H30 As2 N2 O4 Pd'
_chemical_formula_weight         810.86
_chemical_name_common
;
bis-(Triphenylarsine)dinitro-palladium(II)
;
_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                111.490(1)
_cell_angle_beta                 90.473(1)
_cell_angle_gamma                115.209(1)
_cell_formula_units_Z            1
_cell_length_a                   9.5940(7)
_cell_length_b                   9.9987(7)
_cell_length_c                   10.1274(7)
_cell_measurement_reflns_used    6896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.59
_cell_measurement_theta_min      4.02
_cell_volume                     802.14(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Beamline 13.3.1, ALS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10978
_diffrn_reflns_theta_full        33.59
_diffrn_reflns_theta_max         33.59
_diffrn_reflns_theta_min         4.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.238
_exptl_absorpt_correction_T_max  0.9684
_exptl_absorpt_correction_T_min  0.8550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 -
Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0524
_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)+(0.1255P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                4310
_reflns_number_total             4729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30314k.txt
_cod_data_source_block           3_gs
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7020111
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
Pd1 Pd 0.5000 0.5000 0.5000 0.01547(12) Uani 1 2 d S
As1 As 0.52346(3) 0.73334(3) 0.71038(3) 0.01472(12) Uani 1 1 d .
O1 O 0.7017(3) 0.6771(3) 0.3572(3) 0.0312(5) Uani 1 1 d .
O2 O 0.8279(3) 0.6968(3) 0.5463(3) 0.0312(5) Uani 1 1 d .
N1 N 0.7057(3) 0.6435(3) 0.4613(3) 0.0217(5) Uani 1 1 d .
C1 C 0.5945(3) 0.9388(3) 0.6944(3) 0.0177(5) Uani 1 1 d .
C2 C 0.7400(3) 1.0086(3) 0.6561(3) 0.0209(5) Uani 1 1 d .
H2 H 0.8060 0.9578 0.6417 0.025 Uiso 1 1 calc R
C3 C 0.7872(4) 1.1523(4) 0.6391(3) 0.0248(6) Uani 1 1 d .
H3 H 0.8863 1.2007 0.6142 0.030 Uiso 1 1 calc R
C4 C 0.6888(4) 1.2260(4) 0.6586(3) 0.0249(6) Uani 1 1 d .
H4 H 0.7210 1.3238 0.6460 0.030 Uiso 1 1 calc R
C5 C 0.5452(4) 1.1574(3) 0.6961(3) 0.0232(5) Uani 1 1 d .
H5 H 0.4793 1.2082 0.7095 0.028 Uiso 1 1 calc R
C6 C 0.4966(3) 1.0129(3) 0.7146(3) 0.0200(5) Uani 1 1 d .
H6 H 0.3980 0.9656 0.7405 0.024 Uiso 1 1 calc R
C7 C 0.6582(3) 0.7740(3) 0.8777(3) 0.0164(5) Uani 1 1 d .
C8 C 0.7649(3) 0.9304(3) 0.9729(3) 0.0216(5) Uani 1 1 d .
H8 H 0.7797 1.0201 0.9519 0.026 Uiso 1 1 calc R
C9 C 0.8501(3) 0.9550(4) 1.0995(3) 0.0238(6) Uani 1 1 d .
H9 H 0.9240 1.0614 1.1641 0.029 Uiso 1 1 calc R
C10 C 0.8263(3) 0.8231(4) 1.1306(3) 0.0244(6) Uani 1 1 d .
H10 H 0.8826 0.8398 1.2176 0.029 Uiso 1 1 calc R
C11 C 0.7208(3) 0.6673(4) 1.0348(3) 0.0229(5) Uani 1 1 d .
H11 H 0.7054 0.5776 1.0563 0.027 Uiso 1 1 calc R
C12 C 0.6377(3) 0.6420(3) 0.9076(3) 0.0203(5) Uani 1 1 d .
H12 H 0.5671 0.5351 0.8412 0.024 Uiso 1 1 calc R
C13 C 0.3255(3) 0.6937(3) 0.7739(3) 0.0167(5) Uani 1 1 d .
C14 C 0.3095(3) 0.7002(3) 0.9125(3) 0.0182(5) Uani 1 1 d .
H14 H 0.3980 0.7302 0.9800 0.022 Uiso 1 1 calc R
C15 C 0.1625(3) 0.6625(4) 0.9517(3) 0.0219(5) Uani 1 1 d .
H15 H 0.1509 0.6664 1.0459 0.026 Uiso 1 1 calc R
C16 C 0.0336(3) 0.6192(4) 0.8527(3) 0.0234(5) Uani 1 1 d .
H16 H -0.0667 0.5914 0.8789 0.028 Uiso 1 1 calc R
C17 C 0.0504(3) 0.6162(4) 0.7157(3) 0.0234(5) Uani 1 1 d .
H17 H -0.0375 0.5902 0.6495 0.028 Uiso 1 1 calc R
C18 C 0.1950(3) 0.6512(3) 0.6755(3) 0.0202(5) Uani 1 1 d .
H18 H 0.2058 0.6464 0.5809 0.024 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 0.0040 0.0020 '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 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.7856 1.1793 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.1496 2.3280 '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
N1 Pd1 N1 180.0(2) . 2_666
N1 Pd1 As1 90.47(7) . 2_666
N1 Pd1 As1 89.53(7) 2_666 2_666
N1 Pd1 As1 89.53(7) . .
N1 Pd1 As1 90.47(7) 2_666 .
As1 Pd1 As1 180.0 2_666 .
C7 As1 C13 102.51(11) . .
C7 As1 C1 106.55(11) . .
C13 As1 C1 104.66(11) . .
C7 As1 Pd1 111.67(8) . .
C13 As1 Pd1 111.61(8) . .
C1 As1 Pd1 118.43(8) . .
O1 N1 O2 123.1(3) . .
O1 N1 Pd1 118.4(2) . .
O2 N1 Pd1 118.5(2) . .
C6 C1 C2 120.3(3) . .
C6 C1 As1 119.6(2) . .
C2 C1 As1 120.0(2) . .
C3 C2 C1 119.7(3) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
C2 C3 C4 120.0(3) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 120.4(3) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C4 C5 C6 120.2(3) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C1 C6 C5 119.5(3) . .
C1 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
C8 C7 C12 120.1(2) . .
C8 C7 As1 121.8(2) . .
C12 C7 As1 117.9(2) . .
C7 C8 C9 119.8(3) . .
C7 C8 H8 120.1 . .
C9 C8 H8 120.1 . .
C10 C9 C8 119.8(3) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C11 C10 C9 120.2(3) . .
C11 C10 H10 119.9 . .
C9 C10 H10 119.9 . .
C10 C11 C12 120.2(3) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C11 C12 C7 119.8(3) . .
C11 C12 H12 120.1 . .
C7 C12 H12 120.1 . .
C14 C13 C18 119.9(2) . .
C14 C13 As1 121.5(2) . .
C18 C13 As1 118.6(2) . .
C13 C14 C15 119.7(2) . .
C13 C14 H14 120.2 . .
C15 C14 H14 120.2 . .
C16 C15 C14 120.0(3) . .
C16 C15 H15 120.0 . .
C14 C15 H15 120.0 . .
C15 C16 C17 120.3(3) . .
C15 C16 H16 119.8 . .
C17 C16 H16 119.8 . .
C18 C17 C16 120.0(3) . .
C18 C17 H17 120.0 . .
C16 C17 H17 120.0 . .
C17 C18 C13 120.1(3) . .
C17 C18 H18 120.0 . .
C13 C18 H18 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.029(3) .
Pd1 N1 2.029(3) 2_666
Pd1 As1 2.4364(3) 2_666
Pd1 As1 2.4364(3) .
As1 C7 1.928(3) .
As1 C13 1.935(3) .
As1 C1 1.941(3) .
O1 N1 1.223(3) .
O2 N1 1.231(3) .
C1 C6 1.399(4) .
C1 C2 1.401(4) .
C2 C3 1.389(4) .
C2 H2 0.9500 .
C3 C4 1.401(5) .
C3 H3 0.9500 .
C4 C5 1.381(4) .
C4 H4 0.9500 .
C5 C6 1.402(4) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.392(4) .
C7 C12 1.395(4) .
C8 C9 1.397(4) .
C8 H8 0.9500 .
C9 C10 1.393(4) .
C9 H9 0.9500 .
C10 C11 1.387(4) .
C10 H10 0.9500 .
C11 C12 1.390(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.394(4) .
C13 C18 1.399(4) .
C14 C15 1.397(4) .
C14 H14 0.9500 .
C15 C16 1.388(4) .
C15 H15 0.9500 .
C16 C17 1.390(4) .
C16 H16 0.9500 .
C17 C18 1.383(4) .
C17 H17 0.9500 .
C18 H18 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N1 Pd1 As1 C7 -82.56(11) .
N1 Pd1 As1 C7 97.44(11) 2_666
As1 Pd1 As1 C7 0(100) 2_666
N1 Pd1 As1 C13 163.36(11) .
N1 Pd1 As1 C13 -16.64(11) 2_666
As1 Pd1 As1 C13 0(100) 2_666
N1 Pd1 As1 C1 41.76(12) .
N1 Pd1 As1 C1 -138.24(12) 2_666
As1 Pd1 As1 C1 0(100) 2_666
N1 Pd1 N1 O1 -45(100) 2_666
As1 Pd1 N1 O1 71.4(2) 2_666
As1 Pd1 N1 O1 -108.6(2) .
N1 Pd1 N1 O2 133(100) 2_666
As1 Pd1 N1 O2 -110.9(2) 2_666
As1 Pd1 N1 O2 69.1(2) .
C7 As1 C1 C6 -113.9(2) .
C13 As1 C1 C6 -5.8(2) .
Pd1 As1 C1 C6 119.30(19) .
C7 As1 C1 C2 69.1(2) .
C13 As1 C1 C2 177.3(2) .
Pd1 As1 C1 C2 -57.7(2) .
C6 C1 C2 C3 0.4(4) .
As1 C1 C2 C3 177.4(2) .
C1 C2 C3 C4 -0.7(4) .
C2 C3 C4 C5 0.6(4) .
C3 C4 C5 C6 -0.2(4) .
C2 C1 C6 C5 0.0(4) .
As1 C1 C6 C5 -177.0(2) .
C4 C5 C6 C1 -0.1(4) .
C13 As1 C7 C8 -100.8(2) .
C1 As1 C7 C8 8.9(3) .
Pd1 As1 C7 C8 139.6(2) .
C13 As1 C7 C12 74.4(2) .
C1 As1 C7 C12 -175.9(2) .
Pd1 As1 C7 C12 -45.2(2) .
C12 C7 C8 C9 -0.8(4) .
As1 C7 C8 C9 174.3(2) .
C7 C8 C9 C10 -0.8(4) .
C8 C9 C10 C11 1.3(4) .
C9 C10 C11 C12 -0.3(4) .
C10 C11 C12 C7 -1.3(4) .
C8 C7 C12 C11 1.8(4) .
As1 C7 C12 C11 -173.5(2) .
C7 As1 C13 C14 0.5(2) .
C1 As1 C13 C14 -110.6(2) .
Pd1 As1 C13 C14 120.1(2) .
C7 As1 C13 C18 -176.9(2) .
C1 As1 C13 C18 72.0(2) .
Pd1 As1 C13 C18 -57.3(2) .
C18 C13 C14 C15 0.7(4) .
As1 C13 C14 C15 -176.6(2) .
C13 C14 C15 C16 -0.2(4) .
C14 C15 C16 C17 -1.3(4) .
C15 C16 C17 C18 2.2(4) .
C16 C17 C18 C13 -1.7(4) .
C14 C13 C18 C17 0.2(4) .
As1 C13 C18 C17 177.6(2) .
