#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:49:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179209 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/40/4314081.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_4314081
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            'C16 H12 Cl3 N5 Pt'
_chemical_formula_weight         575.75
_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                 105.817(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.641(3)
_cell_length_b                   8.486(2)
_cell_length_c                   18.402(5)
_cell_measurement_temperature    150(2)
_cell_volume                     1749.0(8)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8411
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.82
_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         1.417
_refine_diff_density_min         -1.740
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0156P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                3230
_reflns_number_total             3920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034313hsi20030630_015141.cif
_cod_data_source_block           c:\xray\h708\work\h708m
_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        1749.0(7)
_cod_original_sg_symbol_H-M      'P 1 21/n 1'
_cod_database_code               4314081
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
Pt1 Pt 0.782829(16) 0.135169(19) 0.128745(9) 0.01363(6) Uani 1 1 d . . .
Cl3 Cl 0.59755(10) 0.01593(13) 0.08694(7) 0.0215(3) Uani 1 1 d . . .
Cl2 Cl 0.80153(11) 0.05357(14) 0.25238(6) 0.0230(3) Uani 1 1 d . . .
Cl1 Cl 0.96807(10) 0.25695(14) 0.16550(6) 0.0213(3) Uani 1 1 d . . .
N1 N 0.8561(3) -0.0602(4) 0.0933(2) 0.0163(8) Uani 1 1 d . . .
N2 N 0.8081(3) 0.0991(4) -0.0187(2) 0.0185(9) Uani 1 1 d . . .
N3 N 0.7721(3) 0.1943(4) 0.0237(2) 0.0136(8) Uani 1 1 d . . .
N4 N 0.7042(4) 0.3502(4) 0.1286(2) 0.0179(8) Uani 1 1 d . . .
N5 N 0.7304(4) 0.5648(5) 0.2131(2) 0.0253(10) Uani 1 1 d . . .
C1 C 0.9005(4) -0.1923(5) 0.1305(3) 0.0225(11) Uani 1 1 d . . .
H1 H 0.9010 -0.2047 0.1819 0.027 Uiso 1 1 calc R . .
C2 C 0.9453(4) -0.3098(6) 0.0948(3) 0.0264(12) Uani 1 1 d . . .
H2 H 0.9767 -0.4032 0.1213 0.032 Uiso 1 1 calc R . .
C3 C 0.9445(4) -0.2912(6) 0.0199(3) 0.0250(12) Uani 1 1 d . . .
H3 H 0.9773 -0.3712 -0.0046 0.030 Uiso 1 1 calc R . .
C4 C 0.8971(4) -0.1593(5) -0.0190(3) 0.0230(11) Uani 1 1 d . . .
H4 H 0.8936 -0.1482 -0.0709 0.028 Uiso 1 1 calc R . .
C5 C 0.8540(4) -0.0415(5) 0.0187(2) 0.0167(10) Uani 1 1 d . . .
C6 C 0.7249(4) 0.3395(5) 0.0031(2) 0.0180(10) Uani 1 1 d . . .
C7 C 0.7084(4) 0.4019(5) -0.0698(3) 0.0213(11) Uani 1 1 d . . .
H7 H 0.7318 0.3442 -0.1077 0.026 Uiso 1 1 calc R . .
C8 C 0.6573(4) 0.5494(6) -0.0848(3) 0.0239(11) Uani 1 1 d . . .
H8 H 0.6449 0.5945 -0.1336 0.029 Uiso 1 1 calc R . .
C9 C 0.6235(4) 0.6334(5) -0.0275(3) 0.0233(11) Uani 1 1 d . . .
H9 H 0.5875 0.7340 -0.0395 0.028 Uiso 1 1 calc R . .
C10 C 0.6399(4) 0.5779(5) 0.0431(3) 0.0194(10) Uani 1 1 d . . .
H10 H 0.6180 0.6398 0.0802 0.023 Uiso 1 1 calc R . .
C11 C 0.6915(4) 0.4222(5) 0.0619(3) 0.0164(10) Uani 1 1 d . . .
C12 C 0.6820(4) 0.4225(5) 0.1928(2) 0.0157(10) Uani 1 1 d . . .
C13 C 0.6110(4) 0.3426(5) 0.2306(3) 0.0211(11) Uani 1 1 d . . .
H13 H 0.5796 0.2413 0.2144 0.025 Uiso 1 1 calc R . .
C14 C 0.5876(5) 0.4138(6) 0.2917(3) 0.0256(12) Uani 1 1 d . . .
H14 H 0.5380 0.3642 0.3182 0.031 Uiso 1 1 calc R . .
C15 C 0.6385(4) 0.5618(6) 0.3143(3) 0.0258(12) Uani 1 1 d . . .
H15 H 0.6256 0.6132 0.3573 0.031 Uiso 1 1 calc R . .
C16 C 0.7072(5) 0.6312(6) 0.2734(3) 0.0292(12) Uani 1 1 d . . .
H16 H 0.7402 0.7321 0.2888 0.035 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'
Pt Pt -1.7033 8.3905 '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 Pt1 N4 82.05(14) . . ?
N3 Pt1 N1 79.32(14) . . ?
N4 Pt1 N1 161.37(14) . . ?
N3 Pt1 Cl3 88.91(11) . . ?
N4 Pt1 Cl3 90.75(11) . . ?
N1 Pt1 Cl3 88.39(11) . . ?
N3 Pt1 Cl1 88.74(11) . . ?
N4 Pt1 Cl1 89.04(11) . . ?
N1 Pt1 Cl1 91.05(11) . . ?
Cl3 Pt1 Cl1 177.65(4) . . ?
N3 Pt1 Cl2 176.98(11) . . ?
N4 Pt1 Cl2 100.94(10) . . ?
N1 Pt1 Cl2 97.69(11) . . ?
Cl3 Pt1 Cl2 91.44(4) . . ?
Cl1 Pt1 Cl2 90.90(4) . . ?
C1 N1 C5 120.3(4) . . ?
C1 N1 Pt1 130.5(3) . . ?
C5 N1 Pt1 109.2(3) . . ?
N3 N2 C5 112.5(4) . . ?
N2 N3 C6 125.5(4) . . ?
N2 N3 Pt1 119.8(3) . . ?
C6 N3 Pt1 114.7(3) . . ?
C11 N4 C12 124.4(4) . . ?
C11 N4 Pt1 110.3(3) . . ?
C12 N4 Pt1 124.7(3) . . ?
C16 N5 C12 116.5(4) . . ?
N1 C1 C2 120.4(4) . . ?
C1 C2 C3 119.6(5) . . ?
C4 C3 C2 120.5(5) . . ?
C3 C4 C5 118.7(5) . . ?
N1 C5 C4 120.4(4) . . ?
N1 C5 N2 119.1(4) . . ?
C4 C5 N2 120.5(4) . . ?
N3 C6 C7 123.2(4) . . ?
N3 C6 C11 113.9(4) . . ?
C7 C6 C11 122.9(4) . . ?
C6 C7 C8 118.1(5) . . ?
C7 C8 C9 120.0(4) . . ?
C10 C9 C8 123.2(4) . . ?
C9 C10 C11 119.3(5) . . ?
N4 C11 C6 118.9(4) . . ?
N4 C11 C10 124.6(4) . . ?
C6 C11 C10 116.5(4) . . ?
N5 C12 C13 124.0(4) . . ?
N5 C12 N4 117.6(4) . . ?
C13 C12 N4 118.3(4) . . ?
C14 C13 C12 118.3(4) . . ?
C13 C14 C15 118.5(5) . . ?
C16 C15 C14 118.9(5) . . ?
N5 C16 C15 123.7(5) . . ?
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
Pt1 N3 1.967(4) . ?
Pt1 N4 2.041(4) . ?
Pt1 N1 2.050(4) . ?
Pt1 Cl3 2.3159(12) . ?
Pt1 Cl1 2.3196(12) . ?
Pt1 Cl2 2.3309(12) . ?
N1 C1 1.342(6) . ?
N1 C5 1.376(5) . ?
N2 N3 1.272(5) . ?
N2 C5 1.408(5) . ?
N3 C6 1.360(5) . ?
N4 C11 1.342(6) . ?
N4 C12 1.416(5) . ?
N5 C16 1.336(6) . ?
N5 C12 1.342(6) . ?
C1 C2 1.372(6) . ?
C2 C3 1.386(7) . ?
C3 C4 1.361(6) . ?
C4 C5 1.386(6) . ?
C6 C7 1.406(6) . ?
C6 C11 1.430(6) . ?
C7 C8 1.381(6) . ?
C8 C9 1.414(7) . ?
C9 C10 1.346(6) . ?
C10 C11 1.453(6) . ?
C12 C13 1.394(6) . ?
C13 C14 1.367(6) . ?
C14 C15 1.402(7) . ?
C15 C16 1.371(7) . ?
