#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:36:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179118 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/80/4308022.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_4308022
loop_
_publ_author_name
'Liqing Ma'
'Philip M. Imbesi'
'James B. Updegraff'
'Allen D. Hunter'
'John D. Protasiewicz'
_publ_section_title
;
Synthesis and Structural Studies of NCN Diimine Palladium Pincer Complexes
Bearingm-Terphenyl Scaffolds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5220
_journal_page_last               5228
_journal_paper_doi               10.1021/ic062476a
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration rm
_chemical_formula_sum            'C36 H31 I N2 Pd'
_chemical_formula_weight         724.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.7499(2)
_cell_length_b                   15.7499(2)
_cell_length_c                   10.5822(2)
_cell_measurement_temperature    100(2)
_cell_volume                     2273.33(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            51541
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.7658
_exptl_absorpt_correction_T_min  0.7546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'AXScale in Apex2 (Bruker, 2004)'
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7199
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0196P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0336
_reflns_number_gt                7089
_reflns_number_total             7199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062476a-file001_5.cif
_cod_data_source_block           13a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_database_code               4308022
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
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 0.371634(9) 0.344075(9) 0.083686(11) 0.00996(3) Uani 1 1 d . . .
I1 I 0.331125(9) 0.156576(8) 0.049531(9) 0.01891(3) Uani 1 1 d . . .
N1 N 0.26537(10) 0.33545(10) -0.03289(13) 0.0130(3) Uani 1 1 d . . .
N2 N 0.48399(10) 0.37058(10) 0.20201(12) 0.0115(3) Uani 1 1 d . . .
C1 C 0.39502(12) 0.47445(12) 0.13424(16) 0.0121(3) Uani 1 1 d . . .
C2 C 0.37579(13) 0.48642(13) 0.26152(15) 0.0133(3) Uani 1 1 d . . .
C3 C 0.38985(14) 0.57720(14) 0.30086(17) 0.0194(4) Uani 1 1 d . . .
H3 H 0.3764 0.5857 0.3860 0.023 Uiso 1 1 calc R . .
C4 C 0.42316(15) 0.65485(14) 0.21742(18) 0.0236(4) Uani 1 1 d . . .
H4 H 0.4327 0.7164 0.2453 0.028 Uiso 1 1 calc R . .
C5 C 0.44269(14) 0.64285(13) 0.09232(17) 0.0199(4) Uani 1 1 d . . .
H5 H 0.4664 0.6966 0.0355 0.024 Uiso 1 1 calc R . .
C6 C 0.42778(13) 0.55280(13) 0.04990(15) 0.0138(3) Uani 1 1 d . . .
C7 C 0.44898(13) 0.54351(13) -0.08664(15) 0.0135(3) Uani 1 1 d . . .
C8 C 0.38150(13) 0.47056(13) -0.16827(16) 0.0134(3) Uani 1 1 d . . .
C9 C 0.40273(14) 0.47544(13) -0.29745(16) 0.0172(4) Uani 1 1 d . . .
H9 H 0.3552 0.4285 -0.3534 0.021 Uiso 1 1 calc R . .
C10 C 0.49160(15) 0.54732(14) -0.34494(17) 0.0200(4) Uani 1 1 d . . .
H10 H 0.5054 0.5491 -0.4326 0.024 Uiso 1 1 calc R . .
C11 C 0.56035(14) 0.61654(14) -0.26441(17) 0.0190(4) Uani 1 1 d . . .
H11 H 0.6225 0.6647 -0.2959 0.023 Uiso 1 1 calc R . .
C12 C 0.53822(13) 0.61549(13) -0.13683(16) 0.0164(4) Uani 1 1 d . . .
H12 H 0.5849 0.6649 -0.0827 0.020 Uiso 1 1 calc R . .
C13 C 0.33284(13) 0.40194(13) 0.35067(15) 0.0144(3) Uani 1 1 d . . .
C14 C 0.37671(12) 0.34445(13) 0.37830(15) 0.0136(3) Uani 1 1 d . . .
C15 C 0.33309(14) 0.26855(14) 0.46646(16) 0.0181(4) Uani 1 1 d . . .
H15 H 0.3651 0.2332 0.4892 0.022 Uiso 1 1 calc R . .
C16 C 0.24399(14) 0.24400(14) 0.52119(16) 0.0215(4) Uani 1 1 d . . .
H16 H 0.2129 0.1893 0.5765 0.026 Uiso 1 1 calc R . .
C17 C 0.20057(14) 0.29934(15) 0.49506(17) 0.0221(4) Uani 1 1 d . . .
H17 H 0.1398 0.2833 0.5333 0.026 Uiso 1 1 calc R . .
C18 C 0.24570(14) 0.37858(14) 0.41279(16) 0.0178(4) Uani 1 1 d . . .
H18 H 0.2164 0.4178 0.3985 0.021 Uiso 1 1 calc R . .
C19 C 0.28407(13) 0.39003(13) -0.13077(15) 0.0143(3) Uani 1 1 d . . .
H19 H 0.2304 0.3775 -0.1838 0.017 Uiso 1 1 calc R . .
C20 C 0.46945(13) 0.36331(12) 0.32148(15) 0.0136(3) Uani 1 1 d . . .
H20 H 0.5208 0.3704 0.3755 0.016 Uiso 1 1 calc R . .
C21 C 0.16081(13) 0.26242(14) -0.00116(16) 0.0177(4) Uani 1 1 d . . .
H21 H 0.1618 0.2083 0.0469 0.021 Uiso 1 1 calc R . .
C22 C 0.12327(16) 0.31185(18) 0.09010(19) 0.0321(5) Uani 1 1 d . . .
H22A H 0.1679 0.3385 0.1624 0.048 Uiso 1 1 calc R . .
H22B H 0.0577 0.2635 0.1199 0.048 Uiso 1 1 calc R . .
H22C H 0.1202 0.3651 0.0463 0.048 Uiso 1 1 calc R . .
C23 C 0.09639(13) 0.21599(14) -0.11585(16) 0.0174(4) Uani 1 1 d . . .
C24 C 0.09401(15) 0.13382(14) -0.16940(18) 0.0228(4) Uani 1 1 d . . .
H24 H 0.1332 0.1094 -0.1345 0.027 Uiso 1 1 calc R . .
C25 C 0.03481(17) 0.08754(16) -0.27326(18) 0.0302(5) Uani 1 1 d . . .
H25 H 0.0327 0.0309 -0.3078 0.036 Uiso 1 1 calc R . .
C26 C -0.02098(16) 0.12336(17) -0.32660(18) 0.0312(5) Uani 1 1 d . . .
H26 H -0.0612 0.0916 -0.3978 0.037 Uiso 1 1 calc R . .
C27 C -0.01808(14) 0.20554(17) -0.27605(18) 0.0287(5) Uani 1 1 d . . .
H27 H -0.0556 0.2310 -0.3132 0.034 Uiso 1 1 calc R . .
C28 C 0.03965(14) 0.25098(15) -0.17089(17) 0.0218(4) Uani 1 1 d . . .
H28 H 0.0404 0.3069 -0.1359 0.026 Uiso 1 1 calc R . .
C29 C 0.58012(13) 0.39077(13) 0.14772(15) 0.0137(3) Uani 1 1 d . . .
H29 H 0.5734 0.3270 0.1200 0.016 Uiso 1 1 calc R . .
C30 C 0.60245(13) 0.45610(14) 0.03058(15) 0.0181(4) Uani 1 1 d . . .
H30A H 0.5503 0.4223 -0.0320 0.027 Uiso 1 1 calc R . .
H30B H 0.6652 0.4698 -0.0059 0.027 Uiso 1 1 calc R . .
H30C H 0.6061 0.5179 0.0549 0.027 Uiso 1 1 calc R . .
C31 C 0.66428(13) 0.43794(13) 0.24060(15) 0.0141(3) Uani 1 1 d . . .
C32 C 0.72368(12) 0.39747(13) 0.26224(15) 0.0148(3) Uani 1 1 d . . .
H32 H 0.7097 0.3383 0.2210 0.018 Uiso 1 1 calc R . .
C33 C 0.80380(13) 0.44311(15) 0.34413(16) 0.0198(4) Uani 1 1 d . . .
H33 H 0.8445 0.4154 0.3580 0.024 Uiso 1 1 calc R . .
C34 C 0.82372(14) 0.52922(15) 0.40523(16) 0.0209(4) Uani 1 1 d . . .
H34 H 0.8777 0.5602 0.4617 0.025 Uiso 1 1 calc R . .
C35 C 0.76455(14) 0.57000(15) 0.38364(16) 0.0211(4) Uani 1 1 d . . .
H35 H 0.7781 0.6288 0.4254 0.025 Uiso 1 1 calc R . .
C36 C 0.68612(14) 0.52513(14) 0.30153(16) 0.0177(4) Uani 1 1 d . . .
H36 H 0.6466 0.5540 0.2864 0.021 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'
I I -0.4742 1.8119 '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
C1 Pd1 N1 87.30(6) . . ?
C1 Pd1 N2 85.92(6) . . ?
N1 Pd1 N2 172.98(6) . . ?
C1 Pd1 I1 171.62(5) . . ?
N1 Pd1 I1 96.25(4) . . ?
N2 Pd1 I1 90.71(4) . . ?
C19 N1 C21 119.37(15) . . ?
C19 N1 Pd1 122.75(12) . . ?
C21 N1 Pd1 117.88(11) . . ?
C20 N2 C29 120.98(14) . . ?
C20 N2 Pd1 119.45(12) . . ?
C29 N2 Pd1 119.41(10) . . ?
C6 C1 C2 120.02(15) . . ?
C6 C1 Pd1 122.78(12) . . ?
C2 C1 Pd1 117.19(12) . . ?
C3 C2 C1 119.06(16) . . ?
C3 C2 C13 119.65(15) . . ?
C1 C2 C13 121.08(15) . . ?
C4 C3 C2 120.76(16) . . ?
C3 C4 C5 119.94(17) . . ?
C6 C5 C4 120.58(17) . . ?
C5 C6 C1 119.62(15) . . ?
C5 C6 C7 118.41(16) . . ?
C1 C6 C7 121.96(15) . . ?
C12 C7 C8 118.22(15) . . ?
C12 C7 C6 117.90(15) . . ?
C8 C7 C6 123.73(16) . . ?
C9 C8 C7 119.54(16) . . ?
C9 C8 C19 115.29(15) . . ?
C7 C8 C19 125.04(15) . . ?
C10 C9 C8 121.09(17) . . ?
C11 C10 C9 119.72(17) . . ?
C10 C11 C12 119.75(17) . . ?
C11 C12 C7 121.52(17) . . ?
C18 C13 C14 117.64(17) . . ?
C18 C13 C2 118.79(16) . . ?
C14 C13 C2 123.56(16) . . ?
C15 C14 C13 119.77(16) . . ?
C15 C14 C20 117.47(16) . . ?
C13 C14 C20 122.72(16) . . ?
C16 C15 C14 121.02(18) . . ?
C17 C16 C15 119.62(18) . . ?
C16 C17 C18 120.03(18) . . ?
C17 C18 C13 121.72(18) . . ?
N1 C19 C8 125.81(16) . . ?
N2 C20 C14 122.60(15) . . ?
N1 C21 C23 113.83(14) . . ?
N1 C21 C22 107.81(15) . . ?
C23 C21 C22 114.49(16) . . ?
C28 C23 C24 118.21(17) . . ?
C28 C23 C21 123.52(17) . . ?
C24 C23 C21 118.27(17) . . ?
C25 C24 C23 120.5(2) . . ?
C26 C25 C24 120.4(2) . . ?
C27 C26 C25 119.70(19) . . ?
C26 C27 C28 120.0(2) . . ?
C27 C28 C23 121.10(19) . . ?
N2 C29 C31 113.55(13) . . ?
N2 C29 C30 108.70(13) . . ?
C31 C29 C30 110.15(14) . . ?
C32 C31 C36 118.95(16) . . ?
C32 C31 C29 120.48(16) . . ?
C36 C31 C29 120.51(16) . . ?
C31 C32 C33 120.55(17) . . ?
C34 C33 C32 119.72(17) . . ?
C33 C34 C35 119.89(17) . . ?
C36 C35 C34 120.12(17) . . ?
C35 C36 C31 120.77(17) . . ?
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 C1 1.9702(17) . ?
Pd1 N1 2.0283(14) . ?
Pd1 N2 2.0334(14) . ?
Pd1 I1 2.71557(16) . ?
N1 C19 1.283(2) . ?
N1 C21 1.501(2) . ?
N2 C20 1.280(2) . ?
N2 C29 1.497(2) . ?
C1 C6 1.396(2) . ?
C1 C2 1.414(2) . ?
C2 C3 1.396(3) . ?
C2 C13 1.489(2) . ?
C3 C4 1.382(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.391(2) . ?
C6 C7 1.506(2) . ?
C7 C12 1.396(2) . ?
C7 C8 1.405(2) . ?
C8 C9 1.400(2) . ?
C8 C19 1.475(2) . ?
C9 C10 1.382(3) . ?
C10 C11 1.381(3) . ?
C11 C12 1.392(2) . ?
C13 C18 1.395(2) . ?
C13 C14 1.417(2) . ?
C14 C15 1.396(2) . ?
C14 C20 1.466(2) . ?
C15 C16 1.383(3) . ?
C16 C17 1.378(3) . ?
C17 C18 1.391(3) . ?
C21 C23 1.515(2) . ?
C21 C22 1.533(3) . ?
C23 C28 1.391(3) . ?
C23 C24 1.396(3) . ?
C24 C25 1.389(3) . ?
C25 C26 1.380(3) . ?
C26 C27 1.380(3) . ?
C27 C28 1.388(3) . ?
C29 C31 1.513(2) . ?
C29 C30 1.535(2) . ?
C31 C32 1.389(2) . ?
C31 C36 1.395(2) . ?
C32 C33 1.398(2) . ?
C33 C34 1.389(3) . ?
C34 C35 1.390(3) . ?
C35 C36 1.381(3) . ?
