#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:17:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179718 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/20/7002090.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_7002090
loop_
_publ_author_name
'Huynh, Han Vinh'
'Yuan, Dan'
'Han, Yuan'
_publ_section_title
;
 Syntheses and catalytic activities of pseudo-pincer and CSC
 pincer-type Pd(II) complexes derived from benzannulated N-heterocyclic
 carbenes
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              7262
_journal_paper_doi               10.1039/b907887h
_journal_year                    2009
_chemical_formula_sum            'C32 H30 Br N5 O3 Pd S'
_chemical_formula_weight         750.98
_chemical_name_systematic
;
?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   31.2166(19)
_cell_length_b                   11.1730(7)
_cell_length_c                   17.0257(10)
_cell_measurement_reflns_used    1712
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      20.03
_cell_measurement_theta_min      2.28
_cell_volume                     5938.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1100
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32991
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_T_max  0.8510
_exptl_absorpt_correction_T_min  0.7054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.176
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5235
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0530
_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)+(0.0658P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                3337
_reflns_number_total             5235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907887h.txt
_cod_data_source_block           7580a
_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.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' 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      Pbcn
_cod_database_code               7002090
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.640000(14) 0.72518(4) 0.57830(3) 0.02995(16) Uani 1 1 d . . .
S1 S 0.67960(5) 0.70946(16) 0.46430(10) 0.0395(4) Uani 1 1 d . . .
Br1 Br 0.59676(2) 0.77416(7) 0.69284(4) 0.0421(2) Uani 1 1 d . . .
N1 N 0.67528(16) 0.5286(5) 0.6912(3) 0.0351(13) Uani 1 1 d . . .
N2 N 0.72439(16) 0.6321(5) 0.6334(3) 0.0379(13) Uani 1 1 d . . .
N3 N 0.55982(16) 0.8198(4) 0.4954(3) 0.0317(12) Uani 1 1 d . . .
N4 N 0.61596(15) 0.9283(4) 0.4770(3) 0.0330(13) Uani 1 1 d . . .
C1 C 0.68130(18) 0.6212(6) 0.6405(4) 0.0317(15) Uani 1 1 d . . .
C2 C 0.7146(2) 0.4807(6) 0.7155(4) 0.0392(17) Uani 1 1 d . . .
C3 C 0.7244(3) 0.3850(7) 0.7640(4) 0.053(2) Uani 1 1 d . . .
H3 H 0.7031 0.3385 0.7880 0.064 Uiso 1 1 calc R . .
C4 C 0.7676(3) 0.3620(8) 0.7751(4) 0.062(2) Uani 1 1 d . . .
H4 H 0.7759 0.2977 0.8073 0.074 Uiso 1 1 calc R . .
C5 C 0.7983(2) 0.4309(8) 0.7400(5) 0.062(2) Uani 1 1 d . . .
H5 H 0.8272 0.4133 0.7502 0.074 Uiso 1 1 calc R . .
C6 C 0.7890(2) 0.5242(7) 0.6910(4) 0.050(2) Uani 1 1 d . . .
H6 H 0.8106 0.5701 0.6669 0.060 Uiso 1 1 calc R . .
C7 C 0.7459(2) 0.5468(6) 0.6789(4) 0.0400(18) Uani 1 1 d . . .
C8 C 0.6342(2) 0.4853(6) 0.7221(4) 0.0422(17) Uani 1 1 d . . .
H8A H 0.6114 0.5389 0.7040 0.051 Uiso 1 1 calc R . .
H8B H 0.6350 0.4895 0.7796 0.051 Uiso 1 1 calc R . .
C9 C 0.62313(19) 0.3594(6) 0.6983(4) 0.0361(16) Uani 1 1 d . . .
C10 C 0.6047(2) 0.2829(7) 0.7524(5) 0.056(2) Uani 1 1 d . . .
H10 H 0.6002 0.3082 0.8044 0.067 Uiso 1 1 calc R . .
C11 C 0.5928(2) 0.1663(8) 0.7290(6) 0.064(2) Uani 1 1 d . . .
H11 H 0.5802 0.1141 0.7656 0.077 Uiso 1 1 calc R . .
C12 C 0.5995(2) 0.1292(7) 0.6544(5) 0.056(2) Uani 1 1 d . . .
H12 H 0.5918 0.0511 0.6396 0.068 Uiso 1 1 calc R . .
C13 C 0.6176(2) 0.2060(7) 0.5996(5) 0.056(2) Uani 1 1 d . . .
H13 H 0.6221 0.1806 0.5476 0.068 Uiso 1 1 calc R . .
C14 C 0.6288(2) 0.3198(7) 0.6225(5) 0.0485(19) Uani 1 1 d . . .
H14 H 0.6408 0.3721 0.5852 0.058 Uiso 1 1 calc R . .
C15 C 0.7450(2) 0.7114(6) 0.5757(4) 0.0464(18) Uani 1 1 d . . .
H15A H 0.7762 0.7085 0.5824 0.056 Uiso 1 1 calc R . .
H15B H 0.7356 0.7941 0.5844 0.056 Uiso 1 1 calc R . .
C16 C 0.73350(19) 0.6732(7) 0.4933(4) 0.0444(18) Uani 1 1 d . . .
H16A H 0.7375 0.5865 0.4890 0.053 Uiso 1 1 calc R . .
H16B H 0.7534 0.7113 0.4565 0.053 Uiso 1 1 calc R . .
C17 C 0.60164(19) 0.8296(6) 0.5138(3) 0.0307(15) Uani 1 1 d . . .
C18 C 0.54716(19) 0.9110(6) 0.4445(4) 0.0330(15) Uani 1 1 d . . .
C19 C 0.5086(2) 0.9373(6) 0.4092(4) 0.0435(18) Uani 1 1 d . . .
H19 H 0.4845 0.8882 0.4168 0.052 Uiso 1 1 calc R . .
C20 C 0.5064(2) 1.0376(6) 0.3626(4) 0.0451(18) Uani 1 1 d . . .
H20 H 0.4805 1.0582 0.3379 0.054 Uiso 1 1 calc R . .
C21 C 0.5424(2) 1.1084(6) 0.3518(4) 0.0447(18) Uani 1 1 d . . .
H21 H 0.5401 1.1763 0.3196 0.054 Uiso 1 1 calc R . .
C22 C 0.5816(2) 1.0840(6) 0.3862(4) 0.0407(17) Uani 1 1 d . . .
H22 H 0.6057 1.1331 0.3782 0.049 Uiso 1 1 calc R . .
C23 C 0.5832(2) 0.9826(6) 0.4331(4) 0.0331(15) Uani 1 1 d . . .
C24 C 0.5318(2) 0.7203(6) 0.5194(4) 0.0375(16) Uani 1 1 d . . .
H24A H 0.5027 0.7507 0.5282 0.045 Uiso 1 1 calc R . .
H24B H 0.5422 0.6866 0.5690 0.045 Uiso 1 1 calc R . .
C25 C 0.53052(19) 0.6231(6) 0.4577(4) 0.0356(16) Uani 1 1 d . . .
C26 C 0.5636(2) 0.5419(6) 0.4499(5) 0.048(2) Uani 1 1 d . . .
H26 H 0.5874 0.5479 0.4834 0.058 Uiso 1 1 calc R . .
C27 C 0.5627(3) 0.4536(7) 0.3952(5) 0.056(2) Uani 1 1 d . . .
H27 H 0.5852 0.3980 0.3919 0.067 Uiso 1 1 calc R . .
C28 C 0.5278(3) 0.4466(7) 0.3440(5) 0.060(2) Uani 1 1 d . . .
H28 H 0.5274 0.3878 0.3046 0.071 Uiso 1 1 calc R . .
C29 C 0.4943(3) 0.5247(7) 0.3508(5) 0.058(2) Uani 1 1 d . . .
H29 H 0.4706 0.5189 0.3170 0.070 Uiso 1 1 calc R . .
C30 C 0.4958(2) 0.6128(6) 0.4085(4) 0.0452(18) Uani 1 1 d . . .
H30 H 0.4727 0.6662 0.4139 0.054 Uiso 1 1 calc R . .
C31 C 0.6616(2) 0.9576(6) 0.4745(4) 0.0414(17) Uani 1 1 d . . .
H31A H 0.6728 0.9626 0.5281 0.050 Uiso 1 1 calc R . .
H31B H 0.6655 1.0357 0.4493 0.050 Uiso 1 1 calc R . .
C32 C 0.6860(2) 0.8626(6) 0.4288(4) 0.0486(19) Uani 1 1 d . . .
H32A H 0.7165 0.8828 0.4300 0.058 Uiso 1 1 calc R . .
H32B H 0.6767 0.8655 0.3739 0.058 Uiso 1 1 calc R . .
N5A N 0.8146(3) 0.8636(13) 1.4377(7) 0.0331(16) Uani 0.613(13) 1 d PDU A 1
O1A O 0.8350(7) 0.7710(18) 1.4240(16) 0.091(8) Uani 0.613(13) 1 d PDU A 1
O2A O 0.7960(4) 0.9048(11) 1.4899(8) 0.118(5) Uani 0.613(13) 1 d PDU A 1
O3A O 0.8169(5) 0.9145(12) 1.3786(8) 0.118(5) Uani 0.613(13) 1 d PDU A 1
N5B N 0.8195(5) 0.8629(18) 1.4257(8) 0.0331(16) Uani 0.387(13) 1 d PDU A 2
O1B O 0.8265(9) 0.755(2) 1.4335(19) 0.051(7) Uani 0.387(13) 1 d PDU A 2
O2B O 0.7850(4) 0.8898(13) 1.3927(10) 0.070(6) Uani 0.387(13) 1 d PDU A 2
O3B O 0.8415(5) 0.9474(13) 1.4458(10) 0.082(6) Uani 0.387(13) 1 d PDU A 2
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
C17 Pd1 C1 177.3(2) . . ?
C17 Pd1 S1 84.46(17) . . ?
C1 Pd1 S1 93.16(18) . . ?
C17 Pd1 Br1 88.66(17) . . ?
C1 Pd1 Br1 93.59(18) . . ?
S1 Pd1 Br1 171.10(5) . . ?
C16 S1 C32 101.5(3) . . ?
C16 S1 Pd1 106.7(2) . . ?
C32 S1 Pd1 105.4(2) . . ?
C1 N1 C2 110.9(5) . . ?
C1 N1 C8 126.8(5) . . ?
C2 N1 C8 122.2(5) . . ?
C1 N2 C7 111.5(5) . . ?
C1 N2 C15 123.2(5) . . ?
C7 N2 C15 124.7(5) . . ?
C17 N3 C18 111.1(5) . . ?
C17 N3 C24 125.0(5) . . ?
C18 N3 C24 123.7(5) . . ?
C17 N4 C23 111.1(5) . . ?
C17 N4 C31 121.4(5) . . ?
C23 N4 C31 126.6(5) . . ?
N2 C1 N1 105.2(5) . . ?
N2 C1 Pd1 122.1(5) . . ?
N1 C1 Pd1 132.6(4) . . ?
C7 C2 C3 121.8(7) . . ?
C7 C2 N1 106.5(6) . . ?
C3 C2 N1 131.7(7) . . ?
C4 C3 C2 116.2(7) . . ?
C5 C4 C3 121.2(7) . . ?
C6 C5 C4 123.2(7) . . ?
C5 C6 C7 115.8(7) . . ?
C2 C7 C6 121.7(7) . . ?
C2 C7 N2 106.0(5) . . ?
C6 C7 N2 132.3(7) . . ?
N1 C8 C9 114.3(5) . . ?
C14 C9 C10 118.7(7) . . ?
C14 C9 C8 121.6(6) . . ?
C10 C9 C8 119.6(6) . . ?
C9 C10 C11 119.5(7) . . ?
C12 C11 C10 120.5(8) . . ?
C11 C12 C13 120.3(8) . . ?
C14 C13 C12 119.0(8) . . ?
C13 C14 C9 122.0(7) . . ?
N2 C15 C16 110.2(6) . . ?
C15 C16 S1 114.5(5) . . ?
N4 C17 N3 106.3(5) . . ?
N4 C17 Pd1 122.4(4) . . ?
N3 C17 Pd1 131.3(5) . . ?
C19 C18 C23 121.5(6) . . ?
C19 C18 N3 132.4(6) . . ?
C23 C18 N3 106.1(5) . . ?
C20 C19 C18 118.0(7) . . ?
C19 C20 C21 120.1(7) . . ?
C22 C21 C20 123.3(7) . . ?
C21 C22 C23 115.8(7) . . ?
C22 C23 C18 121.3(6) . . ?
C22 C23 N4 133.3(6) . . ?
C18 C23 N4 105.4(5) . . ?
N3 C24 C25 111.4(5) . . ?
C30 C25 C26 118.4(7) . . ?
C30 C25 C24 120.2(6) . . ?
C26 C25 C24 121.4(6) . . ?
C27 C26 C25 122.0(7) . . ?
C26 C27 C28 119.0(7) . . ?
C29 C28 C27 120.5(8) . . ?
C28 C29 C30 119.1(8) . . ?
C25 C30 C29 121.0(7) . . ?
N4 C31 C32 110.3(5) . . ?
C31 C32 S1 115.5(5) . . ?
O2A N5A O3A 120.2(17) . . ?
O2A N5A O1A 137.5(17) . . ?
O3A N5A O1A 102.4(17) . . ?
O3B N5B O1B 129(2) . . ?
O3B N5B O2B 115.2(19) . . ?
O1B N5B O2B 115.9(19) . . ?
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 C17 2.000(6) . ?
Pd1 C1 2.033(6) . ?
Pd1 S1 2.3078(18) . ?
Pd1 Br1 2.4341(8) . ?
S1 C16 1.800(7) . ?
S1 C32 1.825(7) . ?
N1 C1 1.361(8) . ?
N1 C2 1.402(8) . ?
N1 C8 1.468(7) . ?
N2 C1 1.356(7) . ?
N2 C7 1.400(8) . ?
N2 C15 1.472(8) . ?
N3 C17 1.347(7) . ?
N3 C18 1.395(8) . ?
N3 C24 1.472(8) . ?
N4 C17 1.345(8) . ?
N4 C23 1.404(7) . ?
N4 C31 1.461(7) . ?
C2 C7 1.375(9) . ?
C2 C3 1.385(9) . ?
C3 C4 1.384(9) . ?
C4 C5 1.368(11) . ?
C5 C6 1.366(11) . ?
C6 C7 1.385(8) . ?
C8 C9 1.503(9) . ?
C9 C14 1.377(9) . ?
C9 C10 1.382(9) . ?
C10 C11 1.412(11) . ?
C11 C12 1.352(11) . ?
C12 C13 1.388(11) . ?
C13 C14 1.376(10) . ?
C15 C16 1.509(10) . ?
C18 C19 1.377(9) . ?
C18 C23 1.395(8) . ?
C19 C20 1.375(9) . ?
C20 C21 1.385(9) . ?
C21 C22 1.384(9) . ?
C22 C23 1.387(9) . ?
C24 C25 1.511(9) . ?
C25 C30 1.375(9) . ?
C25 C26 1.381(9) . ?
C26 C27 1.356(10) . ?
C27 C28 1.397(11) . ?
C28 C29 1.366(10) . ?
C29 C30 1.392(10) . ?
C31 C32 1.520(9) . ?
N5A O2A 1.156(13) . ?
N5A O3A 1.159(14) . ?
N5A O1A 1.236(14) . ?
N5B O3B 1.217(16) . ?
N5B O1B 1.233(17) . ?
N5B O2B 1.251(17) . ?
