#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:20:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179785 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/81/7008173.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_7008173
loop_
_publ_author_name
'Panda, Manashi'
'Das, Srijit'
'Mostafa, Golam'
'Castineiras, Alfonso'
'Goswami, Sreebrata'
_publ_section_title
;
 Platinum complexes of diazo ligands. Studies of regioselective
 aromatic ring amination, oxidative halogen addition and reductive
 halogen elimination reactions.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1249
_journal_page_last               1255
_journal_paper_doi               10.1039/b418470j
_journal_year                    2005
_chemical_formula_moiety         '[PtCl(L2b)]'
_chemical_formula_sum            'C18 H15 Cl N4 Pt'
_chemical_formula_weight         517.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 91.1020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7696(3)
_cell_length_b                   16.4559(8)
_cell_length_c                   14.7526(7)
_cell_measurement_temperature    173(2)
_cell_volume                     1643.13(13)
_computing_cell_refinement       'SMART Software (Bruker, 1997)'
_computing_data_collection       'SMART Software (Bruker, 1997)'
_computing_data_reduction        'SAINT Software (Bruker, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker, SMART CCD-1000'
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10140
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.708
_exptl_absorpt_correction_T_max  0.5426
_exptl_absorpt_correction_T_min  0.1323
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brown
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0239
_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)+(0.0068P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0376
_reflns_number_gt                3008
_reflns_number_total             3858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418470j.txt
_cod_data_source_block           compound_2b
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7008173
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
Pt1 Pt 0.68328(2) 0.380436(8) 0.451581(11) 0.02135(5) Uani 1 1 d . . .
Cl1 Cl 0.63414(16) 0.26284(6) 0.36879(8) 0.0386(3) Uani 1 1 d . . .
N11 N 0.6575(4) 0.33175(18) 0.5763(2) 0.0219(7) Uani 1 1 d . . .
N12 N 0.7361(4) 0.46835(18) 0.6147(2) 0.0247(8) Uani 1 1 d . . .
N13 N 0.7348(4) 0.47429(18) 0.5266(2) 0.0213(7) Uani 1 1 d . . .
N14 N 0.7261(4) 0.46228(17) 0.3508(2) 0.0229(7) Uani 1 1 d . . .
C11 C 0.6125(5) 0.2556(2) 0.6021(3) 0.0287(10) Uani 1 1 d . . .
H11 H 0.5866 0.2156 0.5569 0.034 Uiso 1 1 d R . .
C12 C 0.6030(6) 0.2341(2) 0.6925(3) 0.0348(11) Uani 1 1 d . . .
H12 H 0.5722 0.1798 0.7091 0.042 Uiso 1 1 d R . .
C13 C 0.6382(6) 0.2914(2) 0.7578(3) 0.0347(11) Uani 1 1 d . . .
H13 H 0.6324 0.2773 0.8202 0.042 Uiso 1 1 d R . .
C14 C 0.6827(5) 0.3707(2) 0.7321(3) 0.0283(9) Uani 1 1 d . . .
H14 H 0.7069 0.4114 0.7767 0.034 Uiso 1 1 d R . .
C15 C 0.6910(5) 0.3893(2) 0.6420(3) 0.0245(9) Uani 1 1 d . . .
C16 C 0.7758(5) 0.5447(2) 0.4819(3) 0.0212(9) Uani 1 1 d . . .
C17 C 0.8198(5) 0.6192(2) 0.5253(3) 0.0263(9) Uani 1 1 d . . .
H17 H 0.8255 0.6228 0.5896 0.032 Uiso 1 1 d R . .
C18 C 0.8539(5) 0.6860(2) 0.4731(3) 0.0291(10) Uani 1 1 d . . .
H18 H 0.8853 0.7365 0.5010 0.035 Uiso 1 1 d R . .
C19 C 0.8425(5) 0.6801(2) 0.3774(3) 0.0296(10) Uani 1 1 d . . .
H19 H 0.8645 0.7275 0.3421 0.036 Uiso 1 1 d R . .
C20 C 0.8009(5) 0.6086(2) 0.3343(3) 0.0268(9) Uani 1 1 d . . .
H20 H 0.7937 0.6070 0.2699 0.032 Uiso 1 1 d R . .
C21 C 0.7683(5) 0.5362(2) 0.3850(3) 0.0217(9) Uani 1 1 d . . .
C22 C 0.7175(6) 0.4483(2) 0.2571(3) 0.0266(10) Uani 1 1 d . . .
C23 C 0.8790(6) 0.4643(2) 0.2025(3) 0.0318(10) Uani 1 1 d . . .
H23 H 0.9980 0.4848 0.2289 0.038 Uiso 1 1 d R . .
C24 C 0.8666(7) 0.4506(2) 0.1097(3) 0.0392(12) Uani 1 1 d . . .
H24 H 0.9774 0.4629 0.0736 0.047 Uiso 1 1 d R . .
C25 C 0.6997(7) 0.4199(2) 0.0687(3) 0.0377(11) Uani 1 1 d . . .
C26 C 0.5411(7) 0.4018(2) 0.1240(3) 0.0387(11) Uani 1 1 d . . .
H26 H 0.4241 0.3798 0.0972 0.046 Uiso 1 1 d R . .
C27 C 0.5486(6) 0.4149(2) 0.2168(3) 0.0316(10) Uani 1 1 d . . .
H27 H 0.4388 0.4010 0.2529 0.038 Uiso 1 1 d R . .
C28 C 0.6848(8) 0.4064(3) -0.0334(3) 0.0560(14) Uani 1 1 d . . .
H28A H 0.6940 0.4588 -0.0647 0.084 Uiso 1 1 d R . .
H28B H 0.5580 0.3807 -0.0488 0.084 Uiso 1 1 d R . .
H28C H 0.7929 0.3710 -0.0523 0.084 Uiso 1 1 d R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pt Pt -1.7033 8.3905 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N13 Pt1 N11 79.19(13) . . y
N13 Pt1 N14 82.06(13) . . y
N11 Pt1 N14 161.25(12) . . y
N13 Pt1 Cl1 176.08(9) . . y
N11 Pt1 Cl1 97.79(9) . . y
N14 Pt1 Cl1 100.95(9) . . y
C11 N11 C15 118.6(3) . . ?
C11 N11 Pt1 130.6(3) . . ?
C15 N11 Pt1 110.8(2) . . ?
N13 N12 C15 111.1(3) . . ?
N12 N13 C16 123.2(3) . . ?
N12 N13 Pt1 120.7(2) . . ?
C16 N13 Pt1 116.1(3) . . ?
C21 N14 C22 121.5(3) . . ?
C21 N14 Pt1 111.0(3) . . ?
C22 N14 Pt1 127.5(2) . . ?
N11 C11 C12 121.7(4) . . ?
N11 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 119.4(4) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C15 C14 C13 119.1(4) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 N11 121.6(4) . . ?
C14 C15 N12 120.1(4) . . ?
N11 C15 N12 118.2(3) . . ?
N13 C16 C17 124.2(4) . . ?
N13 C16 C21 113.2(3) . . ?
C17 C16 C21 122.6(3) . . ?
C18 C17 C16 118.7(4) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 120.1(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 122.0(4) . . ?
C20 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
C19 C20 C21 120.6(4) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
N14 C21 C20 126.4(4) . . ?
N14 C21 C16 117.6(3) . . ?
C20 C21 C16 115.9(3) . . ?
C27 C22 C23 118.4(4) . . ?
C27 C22 N14 120.3(4) . . ?
C23 C22 N14 121.3(4) . . ?
C24 C23 C22 120.3(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 122.0(4) . . ?
C25 C24 H24 119.0 . . ?
C23 C24 H24 119.0 . . ?
C24 C25 C26 117.3(4) . . ?
C24 C25 C28 122.0(5) . . ?
C26 C25 C28 120.7(4) . . ?
C27 C26 C25 122.1(4) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C26 C27 C22 119.8(4) . . ?
C26 C27 H27 120.1 . . ?
C22 C27 H27 120.1 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
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 N13 1.928(3) . y
Pt1 N11 2.018(3) . y
Pt1 N14 2.031(3) . y
Pt1 Cl1 2.3090(10) . y
N11 C11 1.346(4) . ?
N11 C15 1.370(4) . ?
N12 N13 1.303(4) . ?
N12 C15 1.398(4) . ?
N13 C16 1.363(4) . ?
N14 C21 1.345(4) . ?
N14 C22 1.402(5) . ?
C11 C12 1.383(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.366(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.366(5) . ?
C14 H14 0.9500 . ?
C16 C17 1.413(5) . ?
C16 C21 1.438(5) . ?
C17 C18 1.364(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.415(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.365(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.426(5) . ?
C20 H20 0.9500 . ?
C22 C27 1.391(5) . ?
C22 C23 1.396(5) . ?
C23 C24 1.388(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.368(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.394(6) . ?
C25 C28 1.523(6) . ?
C26 C27 1.387(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N13 Pt1 N11 C11 178.6(3) . . . . ?
N14 Pt1 N11 C11 178.0(3) . . . . ?
Cl1 Pt1 N11 C11 -3.9(3) . . . . ?
N13 Pt1 N11 C15 -0.6(2) . . . . ?
N14 Pt1 N11 C15 -1.2(5) . . . . ?
Cl1 Pt1 N11 C15 176.9(2) . . . . ?
C15 N12 N13 C16 -179.3(3) . . . . ?
C15 N12 N13 Pt1 -1.8(4) . . . . ?
N11 Pt1 N13 N12 1.4(3) . . . . ?
N14 Pt1 N13 N12 -178.8(3) . . . . ?
Cl1 Pt1 N13 N12 -38.5(15) . . . . ?
N11 Pt1 N13 C16 179.1(3) . . . . ?
N14 Pt1 N13 C16 -1.1(2) . . . . ?
Cl1 Pt1 N13 C16 139.2(13) . . . . ?
N13 Pt1 N14 C21 0.6(2) . . . . ?
N11 Pt1 N14 C21 1.2(5) . . . . ?
Cl1 Pt1 N14 C21 -176.9(2) . . . . ?
N13 Pt1 N14 C22 180.0(3) . . . . ?
N11 Pt1 N14 C22 -179.4(3) . . . . ?
Cl1 Pt1 N14 C22 2.5(3) . . . . ?
C15 N11 C11 C12 -1.2(5) . . . . ?
Pt1 N11 C11 C12 179.7(3) . . . . ?
N11 C11 C12 C13 0.6(6) . . . . ?
C11 C12 C13 C14 0.1(6) . . . . ?
C12 C13 C14 C15 -0.3(6) . . . . ?
C13 C14 C15 N11 -0.2(6) . . . . ?
C13 C14 C15 N12 -179.8(3) . . . . ?
C11 N11 C15 C14 1.0(5) . . . . ?
Pt1 N11 C15 C14 -179.7(3) . . . . ?
C11 N11 C15 N12 -179.5(3) . . . . ?
Pt1 N11 C15 N12 -0.2(4) . . . . ?
N13 N12 C15 C14 -179.3(3) . . . . ?
N13 N12 C15 N11 1.2(4) . . . . ?
N12 N13 C16 C17 -1.5(5) . . . . ?
Pt1 N13 C16 C17 -179.1(3) . . . . ?
N12 N13 C16 C21 179.1(3) . . . . ?
Pt1 N13 C16 C21 1.4(4) . . . . ?
N13 C16 C17 C18 -178.5(3) . . . . ?
C21 C16 C17 C18 0.9(5) . . . . ?
C16 C17 C18 C19 0.8(5) . . . . ?
C17 C18 C19 C20 -1.1(6) . . . . ?
C18 C19 C20 C21 -0.4(6) . . . . ?
C22 N14 C21 C20 2.7(6) . . . . ?
Pt1 N14 C21 C20 -177.9(3) . . . . ?
C22 N14 C21 C16 -179.4(3) . . . . ?
Pt1 N14 C21 C16 0.0(4) . . . . ?
C19 C20 C21 N14 179.9(3) . . . . ?
C19 C20 C21 C16 2.0(5) . . . . ?
N13 C16 C21 N14 -0.9(5) . . . . ?
C17 C16 C21 N14 179.6(3) . . . . ?
N13 C16 C21 C20 177.2(3) . . . . ?
C17 C16 C21 C20 -2.2(5) . . . . ?
C21 N14 C22 C27 -124.8(4) . . . . ?
Pt1 N14 C22 C27 55.9(5) . . . . ?
C21 N14 C22 C23 57.6(5) . . . . ?
Pt1 N14 C22 C23 -121.7(3) . . . . ?
C27 C22 C23 C24 2.9(6) . . . . ?
N14 C22 C23 C24 -179.5(4) . . . . ?
C22 C23 C24 C25 -1.2(6) . . . . ?
C23 C24 C25 C26 -0.7(6) . . . . ?
C23 C24 C25 C28 178.8(4) . . . . ?
C24 C25 C26 C27 0.7(6) . . . . ?
C28 C25 C26 C27 -178.8(4) . . . . ?
C25 C26 C27 C22 1.1(6) . . . . ?
C23 C22 C27 C26 -2.8(6) . . . . ?
N14 C22 C27 C26 179.5(3) . . . . ?
