#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/19/7011900.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_7011900
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            'C18 H24 Cl2 N2 Pd'
_chemical_formula_weight         445.69
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.666(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3555(9)
_cell_length_b                   19.140(2)
_cell_length_c                   12.969(2)
_cell_measurement_reflns_used    5806
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.65
_cell_volume                     1813.5(4)
_computing_cell_refinement       'Bruker SAINT'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Bruker SMART 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  0.043
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11373
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.318
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.154
_refine_diff_density_min         -2.037
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0427
_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)+(0.0814P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                3524
_reflns_number_total             4193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205548a.txt
_cod_data_source_block           trpdso
_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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically placed' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011900
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Pd1 Pd 0.73985(3) -0.080780(12) 0.627577(17) 0.01944(11) Uani 1 1 d . . .
Cl1 Cl 0.69363(14) -0.07698(4) 0.79802(6) 0.0311(2) Uani 1 1 d . . .
Cl2 Cl 0.78604(13) -0.19858(5) 0.64065(6) 0.0325(2) Uani 1 1 d . . .
N1 N 0.7168(3) 0.02308(14) 0.6045(2) 0.0203(5) Uani 1 1 d . . .
C2 C 0.7383(4) 0.04589(15) 0.5081(2) 0.0191(6) Uani 1 1 d . . .
C3 C 0.7393(4) 0.11686(16) 0.4852(2) 0.0217(6) Uani 1 1 d . . .
H3A H 0.7552 0.1316 0.4169 0.026 Uiso 1 1 calc R . .
C4 C 0.7173(4) 0.16650(17) 0.5609(2) 0.0230(7) Uani 1 1 d . . .
C5 C 0.6913(5) 0.14090(17) 0.6586(3) 0.0263(7) Uani 1 1 d . . .
H5A H 0.6721 0.1727 0.7126 0.032 Uiso 1 1 calc R . .
C6 C 0.6931(5) 0.07068(18) 0.6779(3) 0.0258(7) Uani 1 1 d . . .
H6A H 0.6769 0.0549 0.7457 0.031 Uiso 1 1 calc R . .
C7 C 0.7220(5) 0.24506(17) 0.5432(2) 0.0249(7) Uani 1 1 d . . .
C8 C 0.7255(5) 0.26291(18) 0.4279(3) 0.0304(8) Uani 1 1 d . . .
H8A H 0.8334 0.2415 0.4031 0.046 Uiso 1 1 calc R . .
H8B H 0.7310 0.3137 0.4196 0.046 Uiso 1 1 calc R . .
H8C H 0.6145 0.2449 0.3876 0.046 Uiso 1 1 calc R . .
C9 C 0.5532(5) 0.27927(18) 0.5803(3) 0.0328(8) Uani 1 1 d . . .
H9A H 0.4424 0.2600 0.5414 0.049 Uiso 1 1 calc R . .
H9B H 0.5575 0.3298 0.5689 0.049 Uiso 1 1 calc R . .
H9C H 0.5516 0.2699 0.6545 0.049 Uiso 1 1 calc R . .
C10 C 0.8956(5) 0.27497(18) 0.6043(3) 0.0381(9) Uani 1 1 d . . .
H10A H 1.0036 0.2532 0.5801 0.057 Uiso 1 1 calc R . .
H10B H 0.8943 0.2652 0.6784 0.057 Uiso 1 1 calc R . .
H10C H 0.8999 0.3256 0.5934 0.057 Uiso 1 1 calc R . .
N1' N 0.7688(4) -0.07528(12) 0.4747(2) 0.0189(5) Uani 1 1 d . . .
C2' C 0.7606(4) -0.01004(16) 0.4332(2) 0.0193(6) Uani 1 1 d . . .
C3' C 0.7697(4) 0.00022(16) 0.3285(2) 0.0204(6) Uani 1 1 d . . .
H3'A H 0.7662 0.0464 0.3016 0.024 Uiso 1 1 calc R . .
C4' C 0.7840(4) -0.05583(17) 0.2618(2) 0.0200(6) Uani 1 1 d . . .
C5' C 0.7909(5) -0.12241(17) 0.3072(3) 0.0244(7) Uani 1 1 d . . .
H5'A H 0.8014 -0.1626 0.2654 0.029 Uiso 1 1 calc R . .
C6' C 0.7826(5) -0.12963(17) 0.4115(3) 0.0244(7) Uani 1 1 d . . .
H6'A H 0.7868 -0.1753 0.4402 0.029 Uiso 1 1 calc R . .
C7' C 0.7810(4) -0.04853(17) 0.1454(2) 0.0215(6) Uani 1 1 d . . .
C8' C 0.9363(5) -0.0903(2) 0.1064(3) 0.0349(9) Uani 1 1 d . . .
H8'A H 1.0542 -0.0722 0.1384 0.052 Uiso 1 1 calc R . .
H8'B H 0.9296 -0.0859 0.0307 0.052 Uiso 1 1 calc R . .
H8'C H 0.9248 -0.1396 0.1250 0.052 Uiso 1 1 calc R . .
C9' C 0.7959(5) 0.02769(18) 0.1126(2) 0.0297(7) Uani 1 1 d . . .
H9'A H 0.9116 0.0473 0.1451 0.044 Uiso 1 1 calc R . .
H9'B H 0.6934 0.0543 0.1347 0.044 Uiso 1 1 calc R . .
H9'C H 0.7922 0.0303 0.0369 0.044 Uiso 1 1 calc R . .
C10' C 0.5983(5) -0.07772(18) 0.0939(3) 0.0315(8) Uani 1 1 d . . .
H10D H 0.4971 -0.0514 0.1180 0.047 Uiso 1 1 calc R . .
H10E H 0.5880 -0.1271 0.1125 0.047 Uiso 1 1 calc R . .
H10F H 0.5933 -0.0733 0.0183 0.047 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'
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 Pd1 N1' 79.59(10) . . y
N1 Pd1 Cl1 95.36(8) . . y
N1' Pd1 Cl1 174.56(7) . . y
N1 Pd1 Cl2 174.02(7) . . y
N1' Pd1 Cl2 95.31(7) . . y
Cl1 Pd1 Cl2 89.84(3) . . y
C6 N1 C2 118.4(3) . . ?
C6 N1 Pd1 125.4(2) . . ?
C2 N1 Pd1 116.1(2) . . ?
N1 C2 C3 121.1(3) . . ?
N1 C2 C2' 114.3(3) . . ?
C3 C2 C2' 124.6(3) . . ?
C4 C3 C2 120.9(3) . . ?
C3 C4 C5 116.2(3) . . ?
C3 C4 C7 124.2(3) . . ?
C5 C4 C7 119.5(3) . . ?
C6 C5 C4 120.9(3) . . ?
N1 C6 C5 122.4(3) . . ?
C4 C7 C9 110.0(3) . . ?
C4 C7 C10 108.8(3) . . ?
C9 C7 C10 109.6(3) . . ?
C4 C7 C8 111.7(3) . . ?
C9 C7 C8 108.5(3) . . ?
C10 C7 C8 108.2(3) . . ?
C6' N1' C2' 118.5(3) . . ?
C6' N1' Pd1 125.8(2) . . ?
C2' N1' Pd1 115.5(2) . . ?
N1' C2' C3' 121.0(3) . . ?
N1' C2' C2 114.3(3) . . ?
C3' C2' C2 124.7(3) . . ?
C2' C3' C4' 121.2(3) . . ?
C3' C4' C5' 116.2(3) . . ?
C3' C4' C7' 123.8(3) . . ?
C5' C4' C7' 119.9(3) . . ?
C6' C5' C4' 120.2(3) . . ?
N1' C6' C5' 122.9(3) . . ?
C4' C7' C9' 111.9(3) . . ?
C4' C7' C8' 110.9(3) . . ?
C9' C7' C8' 109.1(3) . . ?
C4' C7' C10' 108.1(3) . . ?
C9' C7' C10' 108.3(3) . . ?
C8' C7' C10' 108.4(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
Pd1 N1 2.015(3) . y
Pd1 N1' 2.022(3) . y
Pd1 Cl1 2.2763(9) . y
Pd1 Cl2 2.2834(9) . y
N1 C6 1.344(4) . ?
N1 C2 1.350(4) . ?
C2 C3 1.390(4) . ?
C2 C2' 1.467(4) . ?
C3 C4 1.388(4) . ?
C4 C5 1.392(4) . ?
C4 C7 1.522(4) . ?
C5 C6 1.367(5) . ?
C7 C9 1.530(5) . ?
C7 C10 1.534(5) . ?
C7 C8 1.536(4) . ?
N1' C6' 1.335(4) . ?
N1' C2' 1.358(4) . ?
C2' C3' 1.382(4) . ?
C3' C4' 1.390(4) . ?
C4' C5' 1.402(5) . ?
C4' C7' 1.514(4) . ?
C5' C6' 1.368(5) . ?
C7' C9' 1.527(4) . ?
C7' C8' 1.528(4) . ?
C7' C10' 1.534(5) . ?
