#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:49:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179209 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/40/4314078.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_4314078
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            'C17 H13 Cl N4 Pd'
_chemical_formula_weight         415.16
_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                 91.161(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7919(5)
_cell_length_b                   16.9123(13)
_cell_length_c                   13.8290(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1588.2(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9991
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7426
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0292
_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)+(0.0075P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                2105
_reflns_number_total             3621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034313hsi20030630_015050.cif
_cod_data_source_block           h206m
_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_database_code               4314078
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 0.18902(5) 0.382344(17) 0.95851(2) 0.04279(10) Uani 1 1 d . . .
Cl1 Cl 0.13907(18) 0.26494(6) 0.87727(8) 0.0710(4) Uani 1 1 d . . .
N1 N 0.2344(4) 0.45848(18) 0.8478(2) 0.0449(8) Uani 1 1 d . . .
N2 N 0.2339(4) 0.47686(17) 1.0340(2) 0.0374(8) Uani 1 1 d . . .
N3 N 0.2275(4) 0.47510(18) 1.1282(2) 0.0424(8) Uani 1 1 d . . .
N4 N 0.1576(4) 0.33999(19) 1.0946(2) 0.0433(8) Uani 1 1 d . . .
C1 C 0.1153(6) 0.2677(2) 1.1265(3) 0.0552(12) Uani 1 1 d . . .
H1 H 0.0971 0.2272 1.0817 0.066 Uiso 1 1 calc R . .
C2 C 0.0975(6) 0.2509(3) 1.2232(3) 0.0672(14) Uani 1 1 d . . .
H2 H 0.0667 0.2000 1.2434 0.081 Uiso 1 1 calc R . .
C3 C 0.1259(7) 0.3102(3) 1.2890(3) 0.0708(14) Uani 1 1 d . . .
H3 H 0.1166 0.2994 1.3547 0.085 Uiso 1 1 calc R . .
C4 C 0.1678(6) 0.3853(3) 1.2590(3) 0.0581(12) Uani 1 1 d . . .
H4 H 0.1851 0.4260 1.3037 0.070 Uiso 1 1 calc R . .
C5 C 0.1840(5) 0.3995(2) 1.1606(3) 0.0442(10) Uani 1 1 d . . .
C6 C 0.2748(5) 0.5437(2) 0.9836(2) 0.0367(9) Uani 1 1 d . . .
C7 C 0.3136(5) 0.6183(2) 1.0249(2) 0.0445(9) Uani 1 1 d . . .
H7 H 0.3135 0.6248 1.0917 0.053 Uiso 1 1 calc R . .
C8 C 0.3510(5) 0.6806(2) 0.9667(3) 0.0492(11) Uani 1 1 d . . .
H8 H 0.3787 0.7299 0.9934 0.059 Uiso 1 1 calc R . .
C9 C 0.3480(5) 0.6705(2) 0.8650(3) 0.0492(11) Uani 1 1 d . . .
H9 H 0.3706 0.7142 0.8258 0.059 Uiso 1 1 calc R . .
C10 C 0.3133(5) 0.5995(2) 0.8229(3) 0.0438(10) Uani 1 1 d . . .
H10 H 0.3138 0.5950 0.7559 0.053 Uiso 1 1 calc R . .
C11 C 0.2759(5) 0.5312(2) 0.8807(3) 0.0376(10) Uani 1 1 d . . .
C12 C 0.2418(6) 0.4407(2) 0.7470(3) 0.0476(11) Uani 1 1 d . . .
C13 C 0.0760(7) 0.4123(2) 0.6996(3) 0.0664(13) Uani 1 1 d . . .
H13 H -0.0392 0.4041 0.7335 0.080 Uiso 1 1 calc R . .
C14 C 0.0812(9) 0.3959(3) 0.6007(4) 0.0874(17) Uani 1 1 d . . .
H14 H -0.0309 0.3778 0.5679 0.105 Uiso 1 1 calc R . .
C15 C 0.2535(10) 0.4069(3) 0.5526(3) 0.093(2) Uani 1 1 d . . .
H15 H 0.2578 0.3955 0.4869 0.111 Uiso 1 1 calc R . .
C16 C 0.4189(8) 0.4342(3) 0.5992(3) 0.0797(16) Uani 1 1 d . . .
H16 H 0.5347 0.4413 0.5655 0.096 Uiso 1 1 calc R . .
C17 C 0.4134(7) 0.4511(2) 0.6962(3) 0.0572(12) Uani 1 1 d . . .
H17 H 0.5260 0.4697 0.7282 0.069 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'
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
N2 Pd1 N4 79.00(13) . . ?
N2 Pd1 N1 81.83(13) . . ?
N4 Pd1 N1 160.82(13) . . ?
N2 Pd1 Cl1 176.35(9) . . ?
N4 Pd1 Cl1 97.52(10) . . ?
N1 Pd1 Cl1 101.65(9) . . ?
C11 N1 C12 120.9(3) . . ?
C11 N1 Pd1 111.1(2) . . ?
C12 N1 Pd1 127.8(3) . . ?
N3 N2 C6 122.8(3) . . ?
N3 N2 Pd1 120.9(2) . . ?
C6 N2 Pd1 116.3(2) . . ?
N2 N3 C5 110.8(3) . . ?
C1 N4 C5 118.7(3) . . ?
C1 N4 Pd1 131.2(3) . . ?
C5 N4 Pd1 110.1(3) . . ?
N4 C1 C2 122.4(4) . . ?
C3 C2 C1 118.8(4) . . ?
C2 C3 C4 120.5(4) . . ?
C3 C4 C5 118.6(4) . . ?
N4 C5 N3 119.2(3) . . ?
N4 C5 C4 121.0(4) . . ?
N3 C5 C4 119.8(4) . . ?
N2 C6 C7 125.2(3) . . ?
N2 C6 C11 112.9(3) . . ?
C7 C6 C11 121.9(3) . . ?
C8 C7 C6 119.5(3) . . ?
C7 C8 C9 119.9(4) . . ?
C10 C9 C8 122.1(4) . . ?
C9 C10 C11 120.6(3) . . ?
N1 C11 C10 126.2(3) . . ?
N1 C11 C6 117.8(3) . . ?
C10 C11 C6 115.9(3) . . ?
C13 C12 C17 119.5(4) . . ?
C13 C12 N1 119.5(4) . . ?
C17 C12 N1 121.0(4) . . ?
C12 C13 C14 119.9(5) . . ?
C15 C14 C13 119.1(5) . . ?
C16 C15 C14 121.3(5) . . ?
C15 C16 C17 119.6(5) . . ?
C16 C17 C12 120.6(4) . . ?
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 N2 1.930(3) . ?
Pd1 N4 2.029(3) . ?
Pd1 N1 2.029(3) . ?
Pd1 Cl1 2.3031(11) . ?
N1 C11 1.338(4) . ?
N1 C12 1.428(4) . ?
N2 N3 1.305(3) . ?
N2 C6 1.360(4) . ?
N3 C5 1.388(4) . ?
N4 C1 1.333(4) . ?
N4 C5 1.369(4) . ?
C1 C2 1.375(5) . ?
C2 C3 1.366(5) . ?
C3 C4 1.368(5) . ?
C4 C5 1.389(4) . ?
C6 C7 1.408(4) . ?
C6 C11 1.440(4) . ?
C7 C8 1.353(4) . ?
C8 C9 1.416(4) . ?
C9 C10 1.354(4) . ?
C10 C11 1.430(5) . ?
C12 C13 1.378(5) . ?
C12 C17 1.383(5) . ?
C13 C14 1.397(5) . ?
C14 C15 1.371(6) . ?
C15 C16 1.364(6) . ?
C16 C17 1.373(5) . ?
