#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:06:34 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178549 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/56/4065629.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_4065629
loop_
_publ_author_name
'Xiao, Xu-Qiong'
'Jia, Ai-Quan'
'Lin, Yue-Jian'
'Jin, Guo-Xin'
_publ_section_title
;
 Self-Assembly of Palladium-Based Macrocycles with N-Heterocyclic Carbene
 as the “Corner” Ligand†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4842
_journal_paper_doi               10.1021/om100040g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C17 H21 F6 N7 O6 Pd S2'
_chemical_formula_weight         703.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.423(7)
_cell_length_b                   10.167(5)
_cell_length_c                   19.551(10)
_cell_measurement_reflns_used    890
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.563
_cell_measurement_theta_min      2.720
_cell_volume                     2668(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0906
_diffrn_reflns_av_sigmaI/netI    0.1101
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12543
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        9.68
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  0.9118
_exptl_absorpt_correction_T_min  0.8342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.811
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.811
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0350P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                1619
_reflns_number_total             3108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100040g_si_001.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4065629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.17919(3) 0.2500 0.65273(2) 0.04213(16) Uani 1 2 d S
S1 S 0.53464(16) 0.2500 0.56523(10) 0.0701(5) Uani 1 2 d S
S2 S -0.04507(15) 0.2500 0.32319(9) 0.0761(6) Uani 1 2 d S
F1 F 0.3610(4) 0.2500 0.5090(3) 0.159(3) Uani 1 2 d S
F2 F 0.4606(4) 0.1537(6) 0.4582(2) 0.244(3) Uani 1 1 d .
F3 F 0.1370(5) 0.2500 0.2924(5) 0.235(4) Uani 1 2 d S
F4 F 0.0475(4) 0.1467(7) 0.2267(3) 0.257(3) Uani 1 1 d .
N1 N 0.2214(2) 0.0122(3) 0.56657(15) 0.0433(8) Uani 1 1 d .
N2 N 0.1101(2) 0.1356(3) 0.52477(15) 0.0408(8) Uani 1 1 d .
N3 N 0.1821(3) 0.1120(3) 0.72909(16) 0.0516(9) Uani 1 1 d .
O1 O 0.5094(4) 0.1370(5) 0.6017(2) 0.155(2) Uani 1 1 d .
O2 O 0.6278(4) 0.2500 0.5370(3) 0.115(2) Uani 1 2 d S
O3 O -0.1310(3) 0.2500 0.2821(2) 0.0899(17) Uani 1 2 d S
O4 O -0.0279(4) 0.1330(6) 0.3596(2) 0.159(2) Uani 1 1 d .
C1 C 0.1712(3) 0.1212(4) 0.57854(17) 0.0388(9) Uani 1 1 d .
C2 C 0.1913(3) -0.0431(4) 0.50568(19) 0.0527(12) Uani 1 1 d .
H2 H 0.2151 -0.1207 0.4865 0.063 Uiso 1 1 calc R
C3 C 0.1223(3) 0.0350(4) 0.4796(2) 0.0499(11) Uani 1 1 d .
H3 H 0.0886 0.0234 0.4385 0.060 Uiso 1 1 calc R
C4 C 0.0485(4) 0.2500 0.5160(3) 0.0446(15) Uani 1 2 d S
H4A H 0.0189 0.2500 0.4708 0.053 Uiso 1 2 calc SR
H4B H -0.0048 0.2500 0.5496 0.053 Uiso 1 2 calc SR
C5 C 0.2990(3) -0.0442(4) 0.6099(2) 0.0591(12) Uani 1 1 d .
H5A H 0.3357 0.0252 0.6315 0.089 Uiso 1 1 calc R
H5B H 0.3433 -0.0962 0.5824 0.089 Uiso 1 1 calc R
H5C H 0.2689 -0.0989 0.6442 0.089 Uiso 1 1 calc R
C6 C 0.1817(3) 0.0474(4) 0.7747(2) 0.0500(11) Uani 1 1 d .
C7 C 0.1815(4) -0.0355(5) 0.83512(19) 0.0799(15) Uani 1 1 d .
H7A H 0.2464 -0.0344 0.8558 0.120 Uiso 1 1 calc R
H7B H 0.1647 -0.1240 0.8224 0.120 Uiso 1 1 calc R
H7C H 0.1332 -0.0031 0.8672 0.120 Uiso 1 1 calc R
C8 C 0.4516(6) 0.2500 0.4961(4) 0.075(2) Uani 1 2 d S
C9 C 0.0505(8) 0.2500 0.2649(7) 0.136(4) Uani 1 2 d S
N4 N 0.8632(6) 0.2500 0.6339(4) 0.126(3) Uani 1 2 d S
C10 C 0.8939(6) 0.2500 0.6844(4) 0.091(3) Uani 1 2 d S
C11 C 0.9329(6) 0.2500 0.7515(4) 0.179(6) Uani 1 2 d S
H11A H 0.8796 0.2387 0.7838 0.269 Uiso 0.50 1 calc PR
H11B H 0.9659 0.3321 0.7601 0.269 Uiso 0.50 1 calc PR
H11C H 0.9796 0.1792 0.7564 0.269 Uiso 0.50 1 calc PR
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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C1 Pd1 C1 84.0(2) . 7_565
C1 Pd1 N3 177.63(16) . 7_565
C1 Pd1 N3 94.75(14) 7_565 7_565
C1 Pd1 N3 94.75(14) . .
C1 Pd1 N3 177.63(16) 7_565 .
N3 Pd1 N3 86.43(18) 7_565 .
O2 S1 O1 115.4(3) . 7_565
O2 S1 O1 115.4(3) . .
O1 S1 O1 111.0(5) 7_565 .
O2 S1 C8 105.7(4) . .
O1 S1 C8 103.9(3) 7_565 .
O1 S1 C8 103.9(3) . .
O4 S2 O4 115.6(4) 7_565 .
O4 S2 O3 115.1(2) 7_565 .
O4 S2 O3 115.1(2) . .
O4 S2 C9 102.4(3) 7_565 .
O4 S2 C9 102.4(3) . .
O3 S2 C9 103.5(5) . .
C1 N1 C2 110.2(4) . .
C1 N1 C5 126.3(4) . .
C2 N1 C5 123.4(4) . .
C1 N2 C3 110.6(3) . .
C1 N2 C4 122.3(4) . .
C3 N2 C4 126.9(4) . .
C6 N3 Pd1 173.0(3) . .
N1 C1 N2 105.4(3) . .
N1 C1 Pd1 131.8(3) . .
N2 C1 Pd1 122.8(3) . .
C3 C2 N1 107.1(4) . .
C2 C3 N2 106.6(4) . .
N2 C4 N2 108.0(4) 7_565 .
N3 C6 C7 179.2(5) . .
F2 C8 F2 105.2(9) . 7_565
F2 C8 F1 102.6(6) . .
F2 C8 F1 102.6(6) 7_565 .
F2 C8 S1 113.6(5) . .
F2 C8 S1 113.6(5) 7_565 .
F1 C8 S1 117.7(6) . .
F3 C9 F4 105.8(7) . .
F3 C9 F4 105.8(7) . 7_565
F4 C9 F4 109.0(13) . 7_565
F3 C9 S2 113.6(10) . .
F4 C9 S2 111.2(7) . .
F4 C9 S2 111.2(7) 7_565 .
N4 C10 C11 179.1(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 1.957(4) .
Pd1 C1 1.957(4) 7_565
Pd1 N3 2.049(3) 7_565
Pd1 N3 2.049(3) .
S1 O2 1.367(5) .
S1 O1 1.394(4) 7_565
S1 O1 1.394(4) .
S1 C8 1.753(8) .
S2 O4 1.406(5) 7_565
S2 O4 1.406(5) .
S2 O3 1.406(4) .
S2 C9 1.716(13) .
F1 C8 1.242(8) .
F2 C8 1.233(5) .
F3 C9 1.279(12) .
F4 C9 1.289(8) .
N1 C1 1.319(5) .
N1 C2 1.377(5) .
N1 C5 1.459(5) .
N2 C1 1.341(4) .
N2 C3 1.361(5) .
N2 C4 1.437(4) .
N3 C6 1.108(4) .
C2 C3 1.323(5) .
C4 N2 1.437(4) 7_565
C6 C7 1.451(5) .
C8 F2 1.233(5) 7_565
C9 F4 1.289(8) 7_565
N4 C10 1.070(8) .
C10 C11 1.413(10) .
