#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:49:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179209 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/40/4314079.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_4314079
loop_
_publ_author_name
'Kunal K. Kamar'
'Srijit Das'
'Chen-Hsiung Hung'
'Alfonso Castiñeiras'
'Michael D. Kuz'min'
'Conrado Rillo'
'Juan Bartolomé'
'Sreebrata Goswami'
_publ_section_title
;
 Design and Synthesis of a New Binucleating Ligand via Cobalt-Promoted C-N
 Bond Fusion Reaction. Ligand Isolation and Its Coordination to Nickel,
 Palladium, and Platinum
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5367
_journal_page_last               5375
_journal_paper_doi               10.1021/ic034313h
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C32 H26 Cl2 N10 O9 Pd2'
_chemical_formula_weight         978.33
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.919(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5546(9)
_cell_length_b                   14.4884(11)
_cell_length_c                   21.2438(15)
_cell_measurement_temperature    293(2)
_cell_volume                     3766.4(5)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.1860
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23768
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7994
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         8654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0179P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                2634
_reflns_number_total             8654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034313hsi20030630_015107.cif
_cod_data_source_block           c:\xray\h204\work\h204m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3766.3(5)
_cod_database_code               4314079
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
Pd1 Pd 0.86021(5) 0.36171(5) 0.05585(3) 0.0626(2) Uani 1 1 d . . .
N1 N 0.9012(5) 0.3962(6) 0.1489(3) 0.068(2) Uani 1 1 d . . .
N2 N 0.9155(5) 0.5417(5) 0.1009(4) 0.065(2) Uani 1 1 d . . .
N3 N 0.8844(4) 0.4918(4) 0.0506(4) 0.0561(18) Uani 1 1 d . . .
N4 N 0.8291(5) 0.3733(5) -0.0388(3) 0.0583(18) Uani 1 1 d . . .
N5 N 0.7176(6) 0.2532(6) -0.0826(3) 0.075(2) Uani 1 1 d . . .
C1 C 0.9085(6) 0.3454(8) 0.2004(6) 0.094(3) Uani 1 1 d . . .
H1 H 0.8926 0.2828 0.1954 0.113 Uiso 1 1 calc R . .
C2 C 0.9388(8) 0.3810(9) 0.2614(6) 0.107(4) Uani 1 1 d . . .
H2 H 0.9436 0.3430 0.2972 0.128 Uiso 1 1 calc R . .
C3 C 0.9619(8) 0.4735(10) 0.2692(5) 0.108(4) Uani 1 1 d . . .
H3 H 0.9825 0.4988 0.3104 0.129 Uiso 1 1 calc R . .
C4 C 0.9543(7) 0.5293(7) 0.2147(5) 0.087(3) Uani 1 1 d . . .
H4 H 0.9707 0.5919 0.2185 0.105 Uiso 1 1 calc R . .
C5 C 0.9221(6) 0.4884(8) 0.1560(5) 0.068(3) Uani 1 1 d . . .
C6 C 0.8691(5) 0.5291(7) -0.0105(4) 0.055(2) Uani 1 1 d . . .
C7 C 0.8760(5) 0.6198(6) -0.0239(4) 0.064(3) Uani 1 1 d . . .
H7 H 0.8921 0.6629 0.0093 0.077 Uiso 1 1 calc R . .
C8 C 0.8594(6) 0.6473(6) -0.0864(5) 0.078(3) Uani 1 1 d . . .
H8 H 0.8634 0.7096 -0.0960 0.094 Uiso 1 1 calc R . .
C9 C 0.8359(6) 0.5818(8) -0.1368(4) 0.077(3) Uani 1 1 d . . .
H9 H 0.8274 0.6013 -0.1794 0.092 Uiso 1 1 calc R . .
C10 C 0.8258(5) 0.4909(7) -0.1240(4) 0.066(2) Uani 1 1 d . . .
H10 H 0.8082 0.4489 -0.1579 0.079 Uiso 1 1 calc R . .
C11 C 0.8419(5) 0.4596(7) -0.0591(4) 0.053(2) Uani 1 1 d . . .
C12 C 0.8110(8) 0.3003(7) -0.0807(4) 0.066(2) Uani 1 1 d . . .
C13 C 0.8860(8) 0.2669(7) -0.1138(4) 0.085(3) Uani 1 1 d . . .
H13 H 0.9498 0.3002 -0.1126 0.102 Uiso 1 1 calc R . .
C14 C 0.8694(9) 0.1865(9) -0.1484(5) 0.104(4) Uani 1 1 d . . .
H14 H 0.9206 0.1653 -0.1705 0.125 Uiso 1 1 calc R . .
C15 C 0.7756(11) 0.1381(8) -0.1495(5) 0.111(4) Uani 1 1 d . . .
H15 H 0.7620 0.0830 -0.1723 0.134 Uiso 1 1 calc R . .
C16 C 0.7014(8) 0.1723(8) -0.1162(5) 0.097(3) Uani 1 1 d . . .
H16 H 0.6380 0.1388 -0.1167 0.116 Uiso 1 1 calc R . .
Pd2 Pd 0.60357(5) 0.30955(5) -0.03874(3) 0.0748(3) Uani 1 1 d . . .
N6 N 0.5136(5) 0.3807(5) -0.1142(4) 0.076(2) Uani 1 1 d . . .
N7 N 0.4188(6) 0.4157(6) -0.0327(4) 0.092(3) Uani 1 1 d . . .
N8 N 0.4919(5) 0.3609(6) -0.0006(4) 0.080(2) Uani 1 1 d . . .
N9 N 0.6576(7) 0.2572(6) 0.0497(4) 0.082(2) Uani 1 1 d . . .
N10 N 0.8393(7) 0.2249(5) 0.0640(3) 0.077(2) Uani 1 1 d . . .
C17 C 0.5244(7) 0.3925(7) -0.1750(5) 0.089(3) Uani 1 1 d . . .
H17 H 0.5818 0.3637 -0.1884 0.107 Uiso 1 1 calc R . .
C18 C 0.4520(9) 0.4466(8) -0.2185(5) 0.109(4) Uani 1 1 d . . .
H18 H 0.4592 0.4508 -0.2611 0.130 Uiso 1 1 calc R . .
C19 C 0.3708(8) 0.4935(8) -0.1998(5) 0.123(5) Uani 1 1 d . . .
H19 H 0.3238 0.5315 -0.2286 0.148 Uiso 1 1 calc R . .
C20 C 0.3598(7) 0.4836(7) -0.1383(6) 0.108(4) Uani 1 1 d . . .
H20 H 0.3045 0.5146 -0.1243 0.130 Uiso 1 1 calc R . .
C21 C 0.4307(8) 0.4277(8) -0.0966(5) 0.083(3) Uani 1 1 d . . .
C22 C 0.4965(8) 0.3341(7) 0.0631(5) 0.088(3) Uani 1 1 d . . .
C23 C 0.4202(7) 0.3618(8) 0.0988(5) 0.118(4) Uani 1 1 d . . .
H23 H 0.3620 0.4001 0.0806 0.142 Uiso 1 1 calc R . .
C24 C 0.4338(9) 0.3308(10) 0.1610(6) 0.146(5) Uani 1 1 d . . .
H24 H 0.3838 0.3471 0.1854 0.176 Uiso 1 1 calc R . .
C25 C 0.5233(10) 0.2745(8) 0.1878(5) 0.121(4) Uani 1 1 d . . .
H25 H 0.5317 0.2554 0.2305 0.146 Uiso 1 1 calc R . .
C26 C 0.5990(8) 0.2463(7) 0.1542(5) 0.105(4) Uani 1 1 d . . .
H26 H 0.6573 0.2091 0.1741 0.126 Uiso 1 1 calc R . .
C27 C 0.5876(8) 0.2746(7) 0.0877(5) 0.083(3) Uani 1 1 d . . .
C28 C 0.7398(10) 0.1939(8) 0.0661(4) 0.084(3) Uani 1 1 d . . .
C29 C 0.7245(9) 0.1010(10) 0.0790(5) 0.129(4) Uani 1 1 d . . .
H29 H 0.6561 0.0794 0.0821 0.154 Uiso 1 1 calc R . .
C30 C 0.8138(13) 0.0409(8) 0.0871(6) 0.150(5) Uani 1 1 d . . .
H30 H 0.8057 -0.0216 0.0949 0.180 Uiso 1 1 calc R . .
C31 C 0.9114(10) 0.0752(10) 0.0835(5) 0.131(5) Uani 1 1 d . . .
H31 H 0.9723 0.0371 0.0888 0.158 Uiso 1 1 calc R . .
C32 C 0.9195(9) 0.1669(8) 0.0720(5) 0.102(4) Uani 1 1 d . . .
H32 H 0.9878 0.1897 0.0698 0.122 Uiso 1 1 calc R . .
Cl1 Cl 0.7902(2) 0.8714(2) 0.80282(13) 0.0931(8) Uani 1 1 d . . .
Cl2 Cl 0.7717(3) 0.7789(3) 0.1435(2) 0.1258(11) Uani 1 1 d . . .
O1 O 0.6865(7) 0.8620(8) 0.7758(5) 0.259(6) Uani 1 1 d . . .
O2 O 0.8508(8) 0.7973(6) 0.7893(4) 0.197(4) Uani 1 1 d . . .
O3 O 0.8278(6) 0.9518(5) 0.7775(3) 0.150(3) Uani 1 1 d . . .
O4 O 0.8053(6) 0.8787(5) 0.8689(3) 0.142(3) Uani 1 1 d . . .
O5 O 0.8623(10) 0.7690(11) 0.1311(7) 0.355(10) Uani 1 1 d . . .
O6 O 0.7747(10) 0.8604(7) 0.1685(5) 0.247(6) Uani 1 1 d . . .
O7 O 0.7570(9) 0.7128(7) 0.1884(5) 0.254(6) Uani 1 1 d . . .
O8 O 0.6935(10) 0.7726(9) 0.0928(5) 0.320(9) Uani 1 1 d . . .
O9 O 0.4847(9) 0.0918(9) -0.0512(5) 0.124(4) Uiso 0.50 1 d P . .
O10 O 1.0964(10) 0.5692(9) 0.4357(6) 0.141(5) Uiso 0.50 1 d P . .
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'
Cl Cl 0.1484 0.1585 '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
N3 Pd1 N4 81.6(3) . . ?
N3 Pd1 N1 78.6(3) . . ?
N4 Pd1 N1 160.2(3) . . ?
N3 Pd1 N10 178.0(3) . . ?
N4 Pd1 N10 99.9(3) . . ?
N1 Pd1 N10 99.9(3) . . ?
C1 N1 C5 119.0(9) . . ?
C1 N1 Pd1 130.1(8) . . ?
C5 N1 Pd1 110.9(7) . . ?
N3 N2 C5 109.8(8) . . ?
N2 N3 C6 121.1(8) . . ?
N2 N3 Pd1 122.1(6) . . ?
C6 N3 Pd1 116.7(6) . . ?
C11 N4 C12 121.6(7) . . ?
C11 N4 Pd1 113.4(6) . . ?
C12 N4 Pd1 124.4(6) . . ?
C12 N5 C16 118.4(9) . . ?
C12 N5 Pd2 118.5(7) . . ?
C16 N5 Pd2 122.9(8) . . ?
N1 C1 C2 122.3(11) . . ?
C3 C2 C1 119.3(11) . . ?
C2 C3 C4 119.4(11) . . ?
C5 C4 C3 117.4(11) . . ?
N1 C5 C4 122.7(9) . . ?
N1 C5 N2 118.5(9) . . ?
C4 C5 N2 118.7(11) . . ?
C7 C6 N3 125.3(8) . . ?
C7 C6 C11 123.4(9) . . ?
N3 C6 C11 111.4(8) . . ?
C6 C7 C8 119.2(9) . . ?
C7 C8 C9 120.5(9) . . ?
C10 C9 C8 120.8(9) . . ?
C9 C10 C11 120.3(8) . . ?
N4 C11 C10 127.3(8) . . ?
N4 C11 C6 116.8(8) . . ?
C10 C11 C6 115.8(9) . . ?
N5 C12 C13 119.7(9) . . ?
N5 C12 N4 115.2(9) . . ?
C13 C12 N4 124.7(9) . . ?
C14 C13 C12 122.0(10) . . ?
C13 C14 C15 118.3(11) . . ?
C14 C15 C16 119.0(11) . . ?
N5 C16 C15 122.5(10) . . ?
N8 Pd2 N9 82.9(4) . . ?
N8 Pd2 N6 78.8(3) . . ?
N9 Pd2 N6 161.7(4) . . ?
N8 Pd2 N5 177.6(3) . . ?
N9 Pd2 N5 98.7(3) . . ?
N6 Pd2 N5 99.6(3) . . ?
C17 N6 C21 116.6(8) . . ?
C17 N6 Pd2 132.1(7) . . ?
C21 N6 Pd2 111.2(7) . . ?
N8 N7 C21 111.7(8) . . ?
N7 N8 C22 123.7(9) . . ?
N7 N8 Pd2 121.1(6) . . ?
C22 N8 Pd2 115.2(7) . . ?
C27 N9 C28 122.0(9) . . ?
C27 N9 Pd2 111.3(7) . . ?
C28 N9 Pd2 125.0(7) . . ?
C32 N10 C28 118.9(10) . . ?
C32 N10 Pd1 122.6(8) . . ?
C28 N10 Pd1 118.3(8) . . ?
N6 C17 C18 121.5(9) . . ?
C19 C18 C17 120.8(10) . . ?
C18 C19 C20 118.5(10) . . ?
C21 C20 C19 119.7(11) . . ?
C20 C21 N6 122.9(9) . . ?
C20 C21 N7 120.1(11) . . ?
N6 C21 N7 117.0(10) . . ?
N8 C22 C23 123.9(11) . . ?
N8 C22 C27 112.2(10) . . ?
C23 C22 C27 123.9(10) . . ?
C24 C23 C22 118.3(10) . . ?
C23 C24 C25 119.9(11) . . ?
C26 C25 C24 123.1(11) . . ?
C25 C26 C27 119.6(10) . . ?
N9 C27 C22 118.0(10) . . ?
N9 C27 C26 126.8(10) . . ?
C22 C27 C26 115.0(10) . . ?
N10 C28 C29 120.1(11) . . ?
N10 C28 N9 115.0(10) . . ?
C29 C28 N9 124.6(12) . . ?
C30 C29 C28 118.8(12) . . ?
C31 C30 C29 118.6(13) . . ?
C30 C31 C32 118.7(13) . . ?
N10 C32 C31 124.8(11) . . ?
O1 Cl1 O4 110.6(6) . . ?
O1 Cl1 O2 111.6(7) . . ?
O4 Cl1 O2 108.4(4) . . ?
O1 Cl1 O3 107.7(6) . . ?
O4 Cl1 O3 110.1(5) . . ?
O2 Cl1 O3 108.4(5) . . ?
O5 Cl2 O8 112.3(9) . . ?
O5 Cl2 O6 104.5(9) . . ?
O8 Cl2 O6 110.8(8) . . ?
O5 Cl2 O7 109.6(9) . . ?
O8 Cl2 O7 109.4(7) . . ?
O6 Cl2 O7 110.1(7) . . ?
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 N3 1.916(6) . ?
Pd1 N4 1.967(6) . ?
Pd1 N1 1.992(7) . ?
Pd1 N10 2.012(7) . ?
N1 C1 1.304(10) . ?
N1 C5 1.363(10) . ?
N2 N3 1.277(7) . ?
N2 C5 1.390(9) . ?
N3 C6 1.379(8) . ?
N4 C11 1.343(9) . ?
N4 C12 1.370(10) . ?
N5 C12 1.350(9) . ?
N5 C16 1.365(10) . ?
N5 Pd2 2.044(7) . ?
C1 C2 1.368(11) . ?
C2 C3 1.373(12) . ?
C3 C4 1.398(11) . ?
C4 C5 1.358(10) . ?
C6 C7 1.353(9) . ?
C6 C11 1.427(10) . ?
C7 C8 1.356(9) . ?
C8 C9 1.412(10) . ?
C9 C10 1.356(10) . ?
C10 C11 1.424(9) . ?
C12 C13 1.382(10) . ?
C13 C14 1.368(11) . ?
C14 C15 1.365(12) . ?
C15 C16 1.382(11) . ?
Pd2 N8 1.919(7) . ?
Pd2 N9 1.999(7) . ?
Pd2 N6 2.024(7) . ?
N6 C17 1.341(8) . ?
N6 C21 1.364(10) . ?
N7 N8 1.288(8) . ?
N7 C21 1.410(9) . ?
N8 C22 1.396(9) . ?
N9 C27 1.344(10) . ?
N9 C28 1.366(11) . ?
N10 C32 1.293(11) . ?
N10 C28 1.337(10) . ?
C17 C18 1.385(10) . ?
C18 C19 1.357(11) . ?
C19 C20 1.351(10) . ?
C20 C21 1.372(11) . ?
C22 C23 1.406(11) . ?
C22 C27 1.435(11) . ?
C23 C24 1.369(11) . ?
C24 C25 1.402(13) . ?
C25 C26 1.374(11) . ?
C26 C27 1.447(11) . ?
C28 C29 1.395(12) . ?
C29 C30 1.400(14) . ?
C30 C31 1.340(13) . ?
C31 C32 1.358(12) . ?
Cl1 O1 1.307(8) . ?
Cl1 O4 1.379(6) . ?
Cl1 O2 1.382(7) . ?
Cl1 O3 1.408(7) . ?
Cl2 O5 1.232(9) . ?
Cl2 O8 1.289(8) . ?
Cl2 O6 1.292(9) . ?
Cl2 O7 1.392(9) . ?
