#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:02:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179822 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/18/7011897.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_7011897
loop_
_publ_author_name
'MacLean, Elizabeth J.'
'Robinson, Richard I.'
'Teat, Simon J.'
'Wilson, Claire'
'Woodward, Simon'
_publ_section_title
;
 Transformation of sulfur dioxide to sulfate at a palladium centre
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3518
_journal_paper_doi               10.1039/b205548a
_journal_year                    2002
_chemical_formula_sum            'C31 H41 Cl N4 O2 Pd'
_chemical_formula_weight         643.53
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geometrically placed, MeCN from delta-F'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.132(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0537(9)
_cell_length_b                   22.089(2)
_cell_length_c                   12.7592(11)
_cell_measurement_reflns_used    7775
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.25
_cell_volume                     3066.8(5)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26915
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.79
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        1.5
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.9191
_exptl_absorpt_correction_T_min  0.8119
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    'riding model, MeCN rigid rotating group'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0276P)²+2.4234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                6181
_reflns_number_total             7342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205548a.txt
_cod_data_source_block           pdtrac
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7011897
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.453938(13) 0.069372(6) 0.420707(12) 0.02226(5) Uani 1 1 d . . .
Cl1 Cl 0.45635(5) 0.22395(2) 0.91041(4) 0.02927(11) Uani 1 1 d . . .
N1 N 0.54856(14) 0.13039(7) 0.50699(12) 0.0213(3) Uani 1 1 d . . .
C2 C 0.52752(17) 0.14033(8) 0.60599(15) 0.0214(4) Uani 1 1 d . . .
C3 C 0.59772(17) 0.18316(9) 0.66980(15) 0.0221(4) Uani 1 1 d . . .
H3A H 0.5823 0.1913 0.7393 0.026 Uiso 1 1 calc R . .
C4 C 0.69144(17) 0.21421(8) 0.63093(15) 0.0218(4) Uani 1 1 d . . .
C5 C 0.70901(17) 0.20223(9) 0.52646(15) 0.0227(4) Uani 1 1 d . . .
H5A H 0.7710 0.2231 0.4979 0.027 Uiso 1 1 calc R . .
C6 C 0.63571(17) 0.16000(8) 0.46538(15) 0.0213(4) Uani 1 1 d . . .
C7 C 0.77722(18) 0.25976(9) 0.69735(15) 0.0241(4) Uani 1 1 d . . .
C8 C 0.9066(2) 0.23171(12) 0.7176(2) 0.0392(5) Uani 1 1 d . . .
H8A H 0.9054 0.1938 0.7574 0.059 Uiso 1 1 calc R . .
H8B H 0.9645 0.2600 0.7590 0.059 Uiso 1 1 calc R . .
H8C H 0.9324 0.2234 0.6494 0.059 Uiso 1 1 calc R . .
C9 C 0.7795(2) 0.31915(10) 0.63504(17) 0.0327(5) Uani 1 1 d . . .
H9A H 0.6972 0.3371 0.6222 0.049 Uiso 1 1 calc R . .
H9B H 0.8053 0.3108 0.5668 0.049 Uiso 1 1 calc R . .
H9C H 0.8376 0.3474 0.6764 0.049 Uiso 1 1 calc R . .
C10" C 0.3328(2) 0.06561(10) 0.94207(17) 0.0320(5) Uani 1 1 d . . .
H10A H 0.3736 0.0262 0.9427 0.048 Uiso 1 1 calc R . .
H10B H 0.2970 0.0700 1.0067 0.048 Uiso 1 1 calc R . .
H10C H 0.3929 0.0979 0.9395 0.048 Uiso 1 1 calc R . .
C10 C 0.7385(2) 0.27395(10) 0.80393(16) 0.0299(4) Uani 1 1 d . . .
H10D H 0.6559 0.2916 0.7912 0.045 Uiso 1 1 calc R . .
H10E H 0.7966 0.3028 0.8437 0.045 Uiso 1 1 calc R . .
H10F H 0.7382 0.2365 0.8452 0.045 Uiso 1 1 calc R . .
C10' C 0.9307(2) 0.16609(12) 0.17433(18) 0.0358(5) Uani 1 1 d . . .
H10G H 0.9483 0.1227 0.1827 0.054 Uiso 1 1 calc R . .
H10H H 0.9422 0.1854 0.2446 0.054 Uiso 1 1 calc R . .
H10I H 0.9866 0.1845 0.1317 0.054 Uiso 1 1 calc R . .
N1' N 0.55531(15) 0.09855(7) 0.31434(13) 0.0233(3) Uani 1 1 d . . .
C2' C 0.63958(17) 0.14192(9) 0.35382(15) 0.0223(4) Uani 1 1 d . . .
C3' C 0.71830(18) 0.16632(9) 0.29231(15) 0.0240(4) Uani 1 1 d . . .
H3'A H 0.7777 0.1955 0.3220 0.029 Uiso 1 1 calc R . .
C4' C 0.71073(18) 0.14803(9) 0.18575(15) 0.0245(4) Uani 1 1 d . . .
C5' C 0.62137(19) 0.10541(9) 0.14708(16) 0.0270(4) Uani 1 1 d . . .
H5'A H 0.6111 0.0929 0.0748 0.032 Uiso 1 1 calc R . .
C6' C 0.54740(19) 0.08115(9) 0.21317(16) 0.0264(4) Uani 1 1 d . . .
H6'A H 0.4889 0.0511 0.1857 0.032 Uiso 1 1 calc R . .
C7' C 0.7975(2) 0.17501(10) 0.11794(16) 0.0277(4) Uani 1 1 d . . .
C8' C 0.7690(2) 0.24308(10) 0.10454(18) 0.0355(5) Uani 1 1 d . . .
H8'A H 0.7787 0.2623 0.1748 0.053 Uiso 1 1 calc R . .
H8'B H 0.6844 0.2485 0.0672 0.053 Uiso 1 1 calc R . .
H8'C H 0.8259 0.2618 0.0632 0.053 Uiso 1 1 calc R . .
C9' C 0.7811(2) 0.14526(11) 0.00743(16) 0.0346(5) Uani 1 1 d . . .
H9'A H 0.7993 0.1019 0.0154 0.052 Uiso 1 1 calc R . .
H9'B H 0.8372 0.1641 -0.0344 0.052 Uiso 1 1 calc R . .
H9'C H 0.6961 0.1508 -0.0292 0.052 Uiso 1 1 calc R . .
N1" N 0.38031(15) 0.06136(7) 0.55319(13) 0.0227(3) Uani 1 1 d . . .
C2" C 0.42719(17) 0.10157(8) 0.63242(15) 0.0216(4) Uani 1 1 d . . .
C3" C 0.38100(17) 0.10425(9) 0.72588(16) 0.0234(4) Uani 1 1 d . . .
H3"A H 0.4137 0.1326 0.7794 0.028 Uiso 1 1 calc R . .
C4" C 0.28534(18) 0.06506(9) 0.74227(16) 0.0244(4) Uani 1 1 d . . .
C5" C 0.24270(18) 0.02398(9) 0.66147(17) 0.0268(4) Uani 1 1 d . . .
H5"A H 0.1799 -0.0039 0.6702 0.032 Uiso 1 1 calc R . .
C6" C 0.29103(18) 0.02350(9) 0.56867(17) 0.0256(4) Uani 1 1 d . . .
H6"A H 0.2598 -0.0046 0.5143 0.031 Uiso 1 1 calc R . .
C7" C 0.23010(19) 0.06993(9) 0.84342(17) 0.0271(4) Uani 1 1 d . . .
C8" C 0.1352(2) 0.01976(11) 0.84942(19) 0.0377(5) Uani 1 1 d . . .
H8"A H 0.1755 -0.0198 0.8509 0.057 Uiso 1 1 calc R . .
H8"B H 0.0696 0.0222 0.7870 0.057 Uiso 1 1 calc R . .
H8"C H 0.1001 0.0249 0.9142 0.057 Uiso 1 1 calc R . .
C9" C 0.1655(2) 0.13182(10) 0.84188(19) 0.0349(5) Uani 1 1 d . . .
H9"A H 0.1006 0.1344 0.7789 0.052 Uiso 1 1 calc R . .
H9"B H 0.2255 0.1642 0.8395 0.052 Uiso 1 1 calc R . .
H9"C H 0.1292 0.1362 0.9062 0.052 Uiso 1 1 calc R . .
O1 O 0.36682(16) 0.00061(7) 0.33001(14) 0.0377(4) Uani 1 1 d . . .
O2 O 0.2023(2) 0.05394(10) 0.28765(19) 0.0667(6) Uani 1 1 d . . .
C1A C 0.2681(3) 0.00847(10) 0.28404(19) 0.0401(6) Uani 1 1 d . . .
C2A C 0.2126(3) -0.04480(14) 0.2124(3) 0.0569(8) Uani 1 1 d . . .
H2A1 H 0.2782 -0.0656 0.1839 0.085 Uiso 1 1 calc R . .
H2A2 H 0.1517 -0.0292 0.1534 0.085 Uiso 1 1 calc R . .
H2A3 H 0.1729 -0.0733 0.2545 0.085 Uiso 1 1 calc R . .
N1S N -0.0939(3) 0.07627(13) 0.5460(3) 0.0771(9) Uani 1 1 d . . .
C2S C -0.0170(2) 0.09853(12) 0.5124(2) 0.0450(6) Uani 1 1 d . . .
C3S C 0.0801(3) 0.12902(12) 0.4705(2) 0.0473(6) Uani 1 1 d . . .
H3S1 H 0.0504 0.1684 0.4412 0.071 Uiso 1 1 calc R . .
H3S2 H 0.1050 0.1043 0.4142 0.071 Uiso 1 1 calc R . .
H3S3 H 0.1507 0.1351 0.5278 0.071 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 0.0033 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'
Pd Pd -0.9988 1.0072 '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'
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
_geom_angle_publ_flag
N1 Pd N1" 80.82(7) . . y
N1 Pd N1' 81.41(7) . . y
N1" Pd N1' 162.18(6) . . y
N1 Pd O1 175.23(7) . . y
N1" Pd O1 100.99(6) . . y
N1' Pd O1 96.83(6) . . y
C2 N1 C6 123.05(16) . . ?
C2 N1 Pd 119.04(13) . . ?
C6 N1 Pd 117.89(12) . . ?
N1 C2 C3 119.38(17) . . ?
N1 C2 C2" 112.28(16) . . ?
C3 C2 C2" 128.34(17) . . ?
C2 C3 C4 119.71(17) . . ?
C3 C4 C5 118.47(17) . . ?
C3 C4 C7 123.29(17) . . ?
C5 C4 C7 118.23(16) . . ?
C6 C5 C4 119.77(17) . . ?
N1 C6 C5 119.59(17) . . ?
N1 C6 C2' 112.94(16) . . ?
C5 C6 C2' 127.47(17) . . ?
C10 C7 C4 112.59(16) . . ?
C10 C7 C9 108.55(17) . . ?
C4 C7 C9 109.85(16) . . ?
C10 C7 C8 109.31(17) . . ?
C4 C7 C8 107.16(16) . . ?
C9 C7 C8 109.34(18) . . ?
C6' N1' C2' 118.81(17) . . ?
C6' N1' Pd 127.63(14) . . ?
C2' N1' Pd 113.56(12) . . ?
N1' C2' C3' 121.36(17) . . ?
N1' C2' C6 114.08(16) . . ?
C3' C2' C6 124.55(17) . . ?
C2' C3' C4' 120.09(18) . . ?
C5' C4' C3' 117.07(18) . . ?
C5' C4' C7' 122.88(17) . . ?
C3' C4' C7' 120.05(18) . . ?
C6' C5' C4' 120.38(18) . . ?
N1' C6' C5' 122.23(19) . . ?
C4' C7' C10' 109.40(17) . . ?
C4' C7' C9' 111.66(17) . . ?
C10' C7' C9' 108.95(18) . . ?
C4' C7' C8' 107.96(17) . . ?
C10' C7' C8' 109.78(19) . . ?
C9' C7' C8' 109.07(17) . . ?
C6" N1" C2" 119.23(17) . . ?
C6" N1" Pd 126.83(14) . . ?
C2" N1" Pd 113.91(13) . . ?
N1" C2" C3" 120.94(17) . . ?
N1" C2" C2 113.87(17) . . ?
C3" C2" C2 125.19(17) . . ?
C2" C3" C4" 120.21(18) . . ?
C5" C4" C3" 117.09(18) . . ?
C5" C4" C7" 122.60(18) . . ?
C3" C4" C7" 120.28(18) . . ?
C6" C5" C4" 120.54(18) . . ?
N1" C6" C5" 121.96(18) . . ?
C4" C7" C8" 111.68(17) . . ?
C4" C7" C9" 107.78(16) . . ?
C8" C7" C9" 108.76(18) . . ?
C4" C7" C10" 109.85(16) . . ?
C8" C7" C10" 108.98(18) . . ?
C9" C7" C10" 109.76(18) . . ?
C1A O1 Pd 118.93(16) . . ?
O1 C1A O2 127.4(2) . . ?
O1 C1A C2A 115.2(2) . . ?
O2 C1A C2A 117.4(3) . . ?
N1S C2S C3S 178.0(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd N1 1.9280(16) . y
Pd N1' 2.0119(17) . y
Pd N1" 2.0087(17) . y
Pd O1 2.0448(15) . y
N1 C2 1.342(2) . ?
N1 C6 1.348(2) . ?
C2 C3 1.392(3) . ?
C2 C2" 1.486(3) . ?
C3 C4 1.404(3) . ?
C4 C5 1.406(3) . ?
C4 C7 1.532(3) . ?
C5 C6 1.383(3) . ?
C6 C2' 1.486(3) . ?
C7 C10 1.528(3) . ?
C7 C9 1.537(3) . ?
C7 C8 1.539(3) . ?
C10" C7" 1.542(3) . ?
C10' C7' 1.533(3) . ?
N1' C6' 1.335(3) . ?
N1' C2' 1.369(2) . ?
C2' C3' 1.380(3) . ?
C3' C4' 1.407(3) . ?
C4' C5' 1.391(3) . ?
C4' C7' 1.522(3) . ?
C5' C6' 1.382(3) . ?
C7' C9' 1.537(3) . ?
C7' C8' 1.540(3) . ?
N1" C6" 1.335(2) . ?
N1" C2" 1.377(2) . ?
C2" C3" 1.379(3) . ?
C3" C4" 1.410(3) . ?
C4" C5" 1.392(3) . ?
C4" C7" 1.526(3) . ?
C5" C6" 1.382(3) . ?
C7" C8" 1.537(3) . ?
C7" C9" 1.541(3) . ?
O1 C1A 1.157(3) . ?
O2 C1A 1.246(3) . ?
C1A C2A 1.549(3) . ?
N1S C2S 1.130(4) . ?
C2S C3S 1.447(4) . ?
