#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:31:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179144 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/05/4310514.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_4310514
loop_
_publ_author_name
'Corey Seward'
'Wen-li Jia'
'Rui-Yao Wang'
'Suning Wang'
_publ_section_title
;
 Palladium(II) Complexes of Bowls, Pinwheels, Cages, and N,C,N-Pincers of
 Starburst Ligands 1,3,5-Tris(di-2-pyridylamino)benzene and
 2,4,6-Tris(di-2-pyridylamino)-1,3,5-triazene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              978
_journal_page_last               985
_journal_paper_doi               10.1021/ic034934a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C45 H37 N9 O2 Pd'
_chemical_formula_weight         842.24
_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   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.112(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.007(3)
_cell_length_b                   15.583(3)
_cell_length_c                   16.207(3)
_cell_measurement_temperature    301(2)
_cell_volume                     4011.5(13)
_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      301(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28706
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.3035
_exptl_absorpt_correction_T_min  0.2243
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .4
_refine_diff_density_max         1.512
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         9565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          2.487
_refine_ls_shift/su_mean         0.155
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0558P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                4860
_reflns_number_total             9565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034934asi20030806_023257.cif
_cod_data_source_block           cs227
_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_cell_volume        4011.5(14)
_cod_database_code               4310514
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 0.254213(19) 0.158415(17) 0.466124(16) 0.05173(11) Uani 1 1 d . . .
O1 O 0.28372(19) 0.28943(18) 0.44727(17) 0.0741(8) Uani 1 1 d . . .
O2 O 0.1611(2) 0.3281(2) 0.4743(2) 0.1170(12) Uani 1 1 d . . .
N1 N 0.28776(18) 0.16965(18) 0.59128(17) 0.0520(7) Uani 1 1 d . . .
N2 N 0.1019(2) 0.0985(2) 0.7042(3) 0.0972(13) Uani 1 1 d . . .
N3 N 0.21733(19) 0.13800(18) 0.34332(17) 0.0522(8) Uani 1 1 d . . .
N4 N 0.4040(2) 0.0401(2) 0.2634(2) 0.0874(11) Uani 1 1 d . . .
N5 N 0.1806(2) -0.3580(2) 0.5460(3) 0.0882(12) Uani 1 1 d . . .
N6 N 0.4005(3) -0.2133(3) 0.5451(2) 0.0891(11) Uani 1 1 d . . .
N7 N 0.19880(18) 0.05487(18) 0.61752(16) 0.0516(7) Uani 1 1 d . . .
N8 N 0.29991(19) 0.01338(18) 0.34745(16) 0.0528(7) Uani 1 1 d . . .
N9 N 0.25613(19) -0.23323(18) 0.51981(18) 0.0566(8) Uani 1 1 d . . .
C1 C 0.2541(2) 0.1212(2) 0.6475(2) 0.0509(9) Uani 1 1 d . . .
C2 C 0.2770(3) 0.1336(3) 0.7324(2) 0.0630(11) Uani 1 1 d . . .
H2 H 0.2540 0.0994 0.7709 0.076 Uiso 1 1 calc R . .
C3 C 0.3337(3) 0.1967(3) 0.7587(3) 0.0764(13) Uani 1 1 d . . .
H3 H 0.3484 0.2066 0.8153 0.092 Uiso 1 1 calc R . .
C4 C 0.3687(3) 0.2452(3) 0.7015(3) 0.0773(13) Uani 1 1 d . . .
H4 H 0.4078 0.2877 0.7185 0.093 Uiso 1 1 calc R . .
C5 C 0.3452(2) 0.2300(3) 0.6187(2) 0.0669(11) Uani 1 1 d . . .
H5 H 0.3696 0.2625 0.5799 0.080 Uiso 1 1 calc R . .
C6 C 0.1182(3) 0.0480(2) 0.6422(2) 0.0591(10) Uani 1 1 d . . .
C7 C 0.0577(3) -0.0065(3) 0.6032(2) 0.0741(12) Uani 1 1 d . . .
H7 H 0.0702 -0.0417 0.5600 0.089 Uiso 1 1 calc R . .
C8 C -0.0206(3) -0.0084(4) 0.6287(3) 0.0936(15) Uani 1 1 d . . .
H8 H -0.0619 -0.0446 0.6027 0.112 Uiso 1 1 calc R . .
C9 C -0.0377(4) 0.0426(4) 0.6919(4) 0.117(2) Uani 1 1 d . . .
H9 H -0.0908 0.0427 0.7096 0.140 Uiso 1 1 calc R . .
C10 C 0.0242(4) 0.0933(4) 0.7286(4) 0.133(2) Uani 1 1 d . . .
H10 H 0.0128 0.1268 0.7734 0.160 Uiso 1 1 calc R . .
C11 C 0.2459(2) 0.0721(2) 0.3014(2) 0.0507(9) Uani 1 1 d . . .
C12 C 0.2226(2) 0.0617(3) 0.2174(2) 0.0629(10) Uani 1 1 d . . .
H12 H 0.2440 0.0162 0.1892 0.076 Uiso 1 1 calc R . .
C13 C 0.1681(3) 0.1185(3) 0.1756(3) 0.0744(12) Uani 1 1 d . . .
H13 H 0.1521 0.1124 0.1188 0.089 Uiso 1 1 calc R . .
C14 C 0.1370(3) 0.1848(3) 0.2184(3) 0.0755(12) Uani 1 1 d . . .
H14 H 0.0994 0.2239 0.1909 0.091 Uiso 1 1 calc R . .
C15 C 0.1621(3) 0.1929(3) 0.3020(2) 0.0642(10) Uani 1 1 d . . .
H15 H 0.1403 0.2374 0.3311 0.077 Uiso 1 1 calc R . .
C16 C 0.3850(3) 0.0075(2) 0.3340(2) 0.0581(10) Uani 1 1 d . . .
C17 C 0.4452(3) -0.0289(3) 0.3924(3) 0.0776(12) Uani 1 1 d . . .
H17 H 0.4300 -0.0526 0.4410 0.093 Uiso 1 1 calc R . .
C18 C 0.5275(3) -0.0295(3) 0.3772(4) 0.1020(16) Uani 1 1 d . . .
H18 H 0.5689 -0.0533 0.4158 0.122 Uiso 1 1 calc R . .
C19 C 0.5483(4) 0.0050(4) 0.3050(4) 0.116(2) Uani 1 1 d . . .
H19 H 0.6039 0.0061 0.2938 0.139 Uiso 1 1 calc R . .
C20 C 0.4855(4) 0.0376(4) 0.2502(4) 0.115(2) Uani 1 1 d . . .
H20 H 0.4995 0.0596 0.2004 0.138 Uiso 1 1 calc R . .
C21 C 0.1790(3) -0.2772(2) 0.5185(2) 0.0605(10) Uani 1 1 d . . .
C22 C 0.1058(3) -0.2358(3) 0.4902(3) 0.0732(12) Uani 1 1 d . . .
H22 H 0.1068 -0.1804 0.4692 0.088 Uiso 1 1 calc R . .
C23 C 0.0304(3) -0.2777(3) 0.4935(3) 0.0907(15) Uani 1 1 d . . .
H23 H -0.0203 -0.2504 0.4756 0.109 Uiso 1 1 calc R . .
C24 C 0.0307(3) -0.3603(4) 0.5234(4) 0.1015(17) Uani 1 1 d . . .
H24 H -0.0192 -0.3896 0.5274 0.122 Uiso 1 1 calc R . .
C25 C 0.1060(4) -0.3971(3) 0.5469(3) 0.1060(18) Uani 1 1 d . . .
H25 H 0.1063 -0.4537 0.5651 0.127 Uiso 1 1 calc R . .
C26 C 0.3377(3) -0.2699(3) 0.5314(2) 0.0624(10) Uani 1 1 d . . .
C27 C 0.3533(3) -0.3559(3) 0.5272(3) 0.0950(16) Uani 1 1 d . . .
H27 H 0.3094 -0.3953 0.5185 0.114 Uiso 1 1 calc R . .
C28 C 0.4358(4) -0.3827(4) 0.5363(4) 0.126(2) Uani 1 1 d . . .
H28 H 0.4472 -0.4411 0.5344 0.151 Uiso 1 1 calc R . .
C29 C 0.5007(4) -0.3273(4) 0.5478(4) 0.1126(19) Uani 1 1 d . . .
H29 H 0.5563 -0.3457 0.5519 0.135 Uiso 1 1 calc R . .
C30 C 0.4808(3) -0.2442(4) 0.5530(3) 0.1061(18) Uani 1 1 d . . .
H30 H 0.5247 -0.2049 0.5626 0.127 Uiso 1 1 calc R . .
C31 C 0.2244(2) -0.0009(2) 0.5544(2) 0.0464(8) Uani 1 1 d . . .
C32 C 0.2482(2) 0.0355(2) 0.48213(19) 0.0459(8) Uani 1 1 d . . .
C33 C 0.2731(2) -0.0204(2) 0.4229(2) 0.0475(8) Uani 1 1 d . . .
C34 C 0.2728(2) -0.1081(2) 0.4337(2) 0.0533(9) Uani 1 1 d . . .
H34 H 0.2866 -0.1442 0.3917 0.064 Uiso 1 1 calc R . .
C35 C 0.2519(2) -0.1421(2) 0.5072(2) 0.0516(9) Uani 1 1 d . . .
C36 C 0.2289(2) -0.0886(2) 0.5686(2) 0.0520(9) Uani 1 1 d . . .
H36 H 0.2166 -0.1111 0.6188 0.062 Uiso 1 1 calc R . .
C37 C 0.2324(3) 0.3443(3) 0.4607(2) 0.0685(11) Uani 1 1 d . . .
C38 C 0.2610(4) 0.4354(3) 0.4656(3) 0.137(2) Uani 1 1 d . . .
H38A H 0.2156 0.4721 0.4434 0.206 Uiso 1 1 calc R . .
H38B H 0.3075 0.4424 0.4340 0.206 Uiso 1 1 calc R . .
H38C H 0.2785 0.4504 0.5226 0.206 Uiso 1 1 calc R . .
C39 C 0.3004(4) -0.2831(5) 0.2745(4) 0.213(5) Uani 1 1 d G . .
C40 C 0.2396(6) -0.2292(3) 0.2335(3) 0.198(5) Uani 1 1 d G . .
H40 H 0.2558 -0.1797 0.2076 0.237 Uiso 1 1 calc R . .
C41 C 0.1548(5) -0.2493(5) 0.2312(3) 0.283(8) Uani 1 1 d G . .
H41 H 0.1141 -0.2133 0.2037 0.339 Uiso 1 1 calc R . .
C42 C 0.1306(4) -0.3234(6) 0.2698(5) 0.194(4) Uani 1 1 d G . .
H42 H 0.0739 -0.3368 0.2682 0.233 Uiso 1 1 calc R . .
C43 C 0.1914(7) -0.3773(4) 0.3108(4) 0.277(8) Uani 1 1 d G . .
H43 H 0.1752 -0.4268 0.3366 0.333 Uiso 1 1 calc R . .
C44 C 0.2762(6) -0.3571(4) 0.3131(3) 0.196(5) Uani 1 1 d G . .
H44 H 0.3169 -0.3932 0.3406 0.236 Uiso 1 1 calc R . .
C45 C 0.3807(5) -0.2589(7) 0.2850(6) 0.246(6) Uani 1 1 d . . .
H45A H 0.4114 -0.2909 0.2481 0.369 Uiso 1 1 calc R . .
H45B H 0.4043 -0.2695 0.3415 0.369 Uiso 1 1 calc R . .
H45C H 0.3844 -0.1988 0.2731 0.369 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'
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
C32 Pd1 N3 87.88(12) . . ?
C32 Pd1 N1 87.88(12) . . ?
N3 Pd1 N1 175.53(11) . . ?
C32 Pd1 O1 169.89(13) . . ?
N3 Pd1 O1 93.00(11) . . ?
N1 Pd1 O1 91.41(11) . . ?
C37 O1 Pd1 118.7(3) . . ?
C1 N1 C5 118.7(3) . . ?
C1 N1 Pd1 123.2(2) . . ?
C5 N1 Pd1 118.1(3) . . ?
C6 N2 C10 117.4(4) . . ?
C15 N3 C11 118.6(3) . . ?
C15 N3 Pd1 118.7(3) . . ?
C11 N3 Pd1 122.7(2) . . ?
C16 N4 C20 117.2(4) . . ?
C21 N5 C25 116.8(4) . . ?
C26 N6 C30 117.6(4) . . ?
C6 N7 C1 121.3(3) . . ?
C6 N7 C31 120.6(3) . . ?
C1 N7 C31 117.8(3) . . ?
C11 N8 C16 120.1(3) . . ?
C11 N8 C33 117.3(3) . . ?
C16 N8 C33 120.1(3) . . ?
C21 N9 C26 126.7(3) . . ?
C21 N9 C35 116.9(3) . . ?
C26 N9 C35 116.4(3) . . ?
N1 C1 C2 120.8(4) . . ?
N1 C1 N7 117.7(3) . . ?
C2 C1 N7 121.3(3) . . ?
C3 C2 C1 119.3(4) . . ?
C4 C3 C2 119.7(4) . . ?
C3 C4 C5 118.9(4) . . ?
N1 C5 C4 122.4(4) . . ?
N2 C6 C7 121.3(4) . . ?
N2 C6 N7 116.4(4) . . ?
C7 C6 N7 122.3(4) . . ?
C8 C7 C6 119.4(4) . . ?
C9 C8 C7 119.7(5) . . ?
C8 C9 C10 118.2(5) . . ?
C9 C10 N2 123.9(5) . . ?
N3 C11 C12 121.6(3) . . ?
N3 C11 N8 117.0(3) . . ?
C12 C11 N8 121.4(3) . . ?
C13 C12 C11 119.4(4) . . ?
C12 C13 C14 119.3(4) . . ?
C15 C14 C13 119.2(4) . . ?
N3 C15 C14 121.8(4) . . ?
N4 C16 C17 122.2(4) . . ?
N4 C16 N8 116.1(4) . . ?
C17 C16 N8 121.7(3) . . ?
C18 C17 C16 118.9(4) . . ?
C19 C18 C17 119.6(5) . . ?
C18 C19 C20 118.0(5) . . ?
N4 C20 C19 124.1(5) . . ?
N5 C21 C22 122.5(4) . . ?
N5 C21 N9 118.2(4) . . ?
C22 C21 N9 119.3(4) . . ?
C21 C22 C23 118.9(4) . . ?
C24 C23 C22 119.4(5) . . ?
C25 C24 C23 117.6(5) . . ?
C24 C25 N5 124.8(5) . . ?
N6 C26 C27 121.3(4) . . ?
N6 C26 N9 114.7(4) . . ?
C27 C26 N9 124.0(4) . . ?
C26 C27 C28 118.0(5) . . ?
C29 C28 C27 122.3(5) . . ?
C30 C29 C28 116.4(5) . . ?
C29 C30 N6 124.3(5) . . ?
C36 C31 C32 121.7(3) . . ?
C36 C31 N7 119.4(3) . . ?
C32 C31 N7 118.8(3) . . ?
C33 C32 C31 117.2(3) . . ?
C33 C32 Pd1 120.2(2) . . ?
C31 C32 Pd1 122.5(2) . . ?
C32 C33 C34 121.9(3) . . ?
C32 C33 N8 119.8(3) . . ?
C34 C33 N8 118.3(3) . . ?
C35 C34 C33 119.6(3) . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 N9 119.4(3) . . ?
C36 C35 N9 120.4(3) . . ?
C35 C36 C31 119.3(3) . . ?
O2 C37 O1 123.6(5) . . ?
O2 C37 C38 118.5(4) . . ?
O1 C37 C38 117.8(4) . . ?
C45 C39 C40 119.9(9) . . ?
C45 C39 C44 119.7(9) . . ?
C40 C39 C44 120.0 . . ?
C41 C40 C39 120.0 . . ?
C42 C41 C40 120.0 . . ?
C41 C42 C43 120.0 . . ?
C44 C43 C42 120.0 . . ?
C43 C44 C39 120.0 . . ?
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 C32 1.937(3) . ?
Pd1 N3 2.030(3) . ?
Pd1 N1 2.041(3) . ?
Pd1 O1 2.126(3) . ?
O1 C37 1.224(4) . ?
O2 C37 1.216(5) . ?
N1 C1 1.346(4) . ?
N1 C5 1.351(4) . ?
N2 C6 1.326(5) . ?
N2 C10 1.354(6) . ?
N3 C15 1.347(5) . ?
N3 C11 1.342(4) . ?
N4 C16 1.321(5) . ?
N4 C20 1.349(6) . ?
N5 C21 1.335(5) . ?
N5 C25 1.343(6) . ?
N6 C26 1.334(5) . ?
N6 C30 1.365(6) . ?
N7 C6 1.402(4) . ?
N7 C1 1.408(4) . ?
N7 C31 1.440(4) . ?
N8 C11 1.408(4) . ?
N8 C16 1.409(5) . ?
N8 C33 1.445(4) . ?
N9 C21 1.410(5) . ?
N9 C26 1.417(5) . ?
N9 C35 1.435(4) . ?
C1 C2 1.393(5) . ?
C2 C3 1.370(6) . ?
C3 C4 1.369(6) . ?
C4 C5 1.367(5) . ?
C6 C7 1.381(5) . ?
C7 C8 1.369(6) . ?
C8 C9 1.351(7) . ?
C9 C10 1.346(7) . ?
C11 C12 1.377(5) . ?
C12 C13 1.364(5) . ?
C13 C14 1.371(6) . ?
C14 C15 1.371(5) . ?
C16 C17 1.386(5) . ?
C17 C18 1.368(6) . ?
C18 C19 1.367(6) . ?
C19 C20 1.355(7) . ?
C21 C22 1.366(5) . ?
C22 C23 1.379(6) . ?
C23 C24 1.375(7) . ?
C24 C25 1.347(7) . ?
C26 C27 1.367(5) . ?
C27 C28 1.376(7) . ?
C28 C29 1.344(7) . ?
C29 C30 1.338(7) . ?
C31 C36 1.385(5) . ?
C31 C32 1.396(4) . ?
C32 C33 1.389(4) . ?
C33 C34 1.378(5) . ?
C34 C35 1.382(5) . ?
C35 C36 1.384(5) . ?
C37 C38 1.491(6) . ?
C39 C45 1.331(9) . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C40 C41 1.3900 . ?
C41 C42 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
