#------------------------------------------------------------------------------
#$Date: 2019-12-25 22:10:52 +0200 (Wed, 25 Dec 2019) $
#$Revision: 245846 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/13/2311390.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2311390
loop_
_publ_author_name
'Konno, Yosuke'
'Matsushita, Nobuyuki'
_publ_section_title
;
 Crystal structure of
 di-chlorido-(1,2-phenyl-enedi-amine-κ²N,N')platinum(II).
;
_journal_coeditor_code           WM5396
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1009
_journal_page_last               1012
_journal_paper_doi               10.1107/S2056989017008477
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Pt Cl2 (C6 H8 N2)]'
_chemical_formula_moiety         'C6 H8 Cl2 N2 Pt'
_chemical_formula_sum            'C6 H8 Cl2 N2 Pt'
_chemical_formula_weight         374.13
_chemical_name_systematic
;
Dichlorido(1,2-phenylenediamine-κ²N,N')platinum(II)
;
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 116.61(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.087(2)
_cell_length_b                   10.446(3)
_cell_length_c                   6.6920(16)
_cell_measurement_reflns_used    12924
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      1.95
_cell_volume                     442.9(2)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 1998)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2017)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare et al.,  1994)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging-plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10875
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    16.377
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    2.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.073
_refine_diff_density_max         4.621
_refine_diff_density_min         -1.744
_refine_ls_extinction_coef       0.0039(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         1587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0341
_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)+(0.0669P)²+0.3105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                1480
_reflns_number_total             1587
_reflns_threshold_expression     F²>2σ(F²)
_iucr_refine_instructions_details
;
TITL  PtCl2(opda)-01
CELL  0.71075 7.0873 10.4457 6.6920 90.000 116.614 90.000
ZERR  2 0.0020 0.0033 0.0016 0.000 0.021 0.000
LATT 1
SYMM    -X,    +Y, .50-Z
SFAC C H N CL PT
UNIT 12 16 4 4 2
L.S. 60
FMAP 2
PLAN 20
OMIT 0 1 0
EQIV $1 1-X, 1-Y, 1-Z
EQIV $2 1-X, 1-Y, -Z
EQIV $3 X, 1-Y, .50+Z
EQIV $4 X, 1-Y, -.50+Z
EQIV $5 -X, 1-Y, -Z
EQIV $6 1-X, Y, .50-Z
BIND Pt1 Pt1_$1
BIND Pt1 Pt1_$2
RTAB deg. Pt1_$1 Pt1 Pt1_$2
HTAB N1 Cl1_$3
HTAB N1 Cl1_$4
HTAB N1 Cl1_$5
HTAB
MPLA Pt1 Cl1 N1 C1 C2 C3 Cl1_$6 N1_$6 C1_$6 C2_$6 C3_$6
ACTA
TEMP 23
BOND $H
CONF
REM WGHT    0.066700    0.315800
WGHT    0.066900    0.310500
EXTI    0.003908
FVAR       1.37110
PT1   5    0.500000    0.504875    0.250000    10.50000    0.02635    0.02835 =
         0.03208    0.00000    0.00944    0.00000
CL1   4    0.233265    0.656867    0.139239    11.00000    0.03351    0.03829 =
         0.05129    0.00116    0.01399    0.00584
N1    3    0.286315    0.359205    0.166571    11.00000    0.03474    0.03714 =
         0.04278   -0.00112    0.01085   -0.00167
AFIX  23
H1A   2    0.214403    0.365322    0.248038    11.00000   -1.20000
H1B   2    0.193383    0.365703    0.021280    11.00000   -1.20000
AFIX   0
C1    1    0.390967    0.236441    0.206599    11.00000    0.04968    0.03281 =
         0.03654   -0.00118    0.01849   -0.00277
C2    1    0.283481    0.122468    0.162080    11.00000    0.06700    0.04624 =
         0.05377   -0.00520    0.02550   -0.01837
AFIX  43
H2    2    0.137019    0.122448    0.101610    11.00000   -1.20000
AFIX   0
C3    1    0.391442    0.008092    0.206512    11.00000    0.11219    0.03731 =
         0.06321   -0.00650    0.04721   -0.01667
AFIX  43
H3    2    0.318174   -0.068950    0.177958    11.00000   -1.20000
HKLF 4
REM   PtCl2(opda)-01
REM R1 =  0.0341 for   1480 Fo > 4sig(Fo)  and  0.0359 for all   1587 data
REM     52 parameters refined using      0 restraints
END
WGHT      0.0669      0.3109
REM Highest difference peak  4.621,  deepest hole -1.744,  1-sigma level  0.229
Q1    1   0.4810  0.5058  0.1228  11.00000  0.05    4.62
Q2    1   0.5000  0.5000  0.0000  10.50000  0.05    3.34
Q3    1   0.5000  0.4404  0.2500  10.50000  0.05    1.65
Q4    1   0.2242  0.6574  0.0029  11.00000  0.05    1.33
Q5    1   0.5000  0.5752  0.2500  10.50000  0.05    1.33
Q6    1   0.3552  0.5022  0.2224  11.00000  0.05    0.70
Q7    1   0.3588  0.4955 -0.0034  11.00000  0.05    0.61
Q8    1   0.2798  0.3661  0.0450  11.00000  0.05    0.57
Q9    1   0.3824  0.1637  0.2250  11.00000  0.05    0.52
Q10   1   0.3402  0.4983  0.1128  11.00000  0.05    0.51
Q11   1   0.3423  0.3969  0.0135  11.00000  0.05    0.46
Q12   1   0.6426  0.5108  0.1343  11.00000  0.05    0.43
Q13   1   0.3224  0.3984  0.2934  11.00000  0.05    0.43
Q14   1   0.6231  0.5773  0.2256  11.00000  0.05    0.43
Q15   1   0.1984  0.3541  0.1198  11.00000  0.05    0.43
Q16   1   0.3577  0.4436  0.2528  11.00000  0.05    0.43
Q17   1   0.4250  0.2330  0.1078  11.00000  0.05    0.42
Q18   1   0.3600  0.4187  0.1593  11.00000  0.05    0.42
Q19   1   0.0467  0.1331  0.0267  11.00000  0.05    0.40
Q20   1   0.3565  0.3057  0.1856  11.00000  0.05    0.40
;
_cod_data_source_file            wm5396sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2311390
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Pt Pt1 0.5000 0.504875(16) 0.2500 0.03029(13) Uani d S 1 2
Cl Cl1 0.23327(19) 0.65687(13) 0.1392(2) 0.0429(3) Uani d . 1 1
N N1 0.2863(7) 0.3592(4) 0.1666(8) 0.0407(9) Uani d . 1 1
H H1A 0.2144 0.3653 0.2480 0.049 Uiso calc R 1 1
H H1B 0.1934 0.3657 0.0213 0.049 Uiso calc R 1 1
C C1 0.3910(7) 0.2364(4) 0.2066(6) 0.0400(8) Uani d . 1 1
C C2 0.2835(10) 0.1225(5) 0.1621(9) 0.0563(12) Uani d . 1 1
H H2 0.1370 0.1224 0.1016 0.068 Uiso calc R 1 1
C C3 0.391(3) 0.0081(5) 0.207(2) 0.068(3) Uani d . 1 1
H H3 0.3182 -0.0690 0.1780 0.082 Uiso calc R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pt1 0.02635(17) 0.02835(16) 0.03208(18) 0.000 0.00944(11) 0.000
Cl1 0.0335(5) 0.0383(5) 0.0513(6) 0.0058(4) 0.0140(4) 0.0012(4)
N1 0.0347(18) 0.0371(18) 0.043(2) -0.0017(14) 0.0108(16) -0.0011(15)
C1 0.050(2) 0.0328(18) 0.0365(18) -0.0028(15) 0.0185(17) -0.0012(14)
C2 0.067(3) 0.046(3) 0.054(3) -0.018(2) 0.026(2) -0.005(2)
C3 0.112(10) 0.037(3) 0.063(6) -0.017(3) 0.047(6) -0.006(2)
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Pt1 N1 . 2_655 83.6(3) y
N1 Pt1 Cl1 . 2_655 174.82(12) ?
N1 Pt1 Cl1 2_655 2_655 91.39(15) ?
N1 Pt1 Cl1 . . 91.39(15) y
N1 Pt1 Cl1 2_655 . 174.82(12) ?
Cl1 Pt1 Cl1 2_655 . 93.69(7) y
N1 Pt1 Pt1 . 3_665 92.07(14) y
N1 Pt1 Pt1 2_655 3_665 85.32(14) ?
Cl1 Pt1 Pt1 2_655 3_665 88.59(4) ?
Cl1 Pt1 Pt1 . 3_665 93.80(4) y
N1 Pt1 Pt1 . 3_666 85.32(14) y
N1 Pt1 Pt1 2_655 3_666 92.07(14) ?
Cl1 Pt1 Pt1 2_655 3_666 93.80(4) ?
Cl1 Pt1 Pt1 . 3_666 88.59(4) y
Pt1 Pt1 Pt1 3_665 3_666 176.513(11) y
C1 N1 Pt1 . . 110.8(3) y
C1 N1 H1A . . 109.5 ?
Pt1 N1 H1A . . 109.5 ?
C1 N1 H1B . . 109.5 ?
Pt1 N1 H1B . . 109.5 ?
H1A N1 H1B . . 108.1 ?
C2 C1 C1 . 2_655 119.8(3) y
C2 C1 N1 . . 122.7(5) y
C1 C1 N1 2_655 . 117.4(2) y
C1 C2 C3 . . 120.3(8) y
C1 C2 H2 . . 119.8 ?
C3 C2 H2 . . 119.8 ?
C2 C3 C3 . 2_655 119.8(6) y
C2 C3 H3 . . 120.1 ?
C3 C3 H3 2_655 . 120.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 N1 . 2.040(4) y
Pt1 N1 2_655 2.040(4) ?
Pt1 Cl1 2_655 2.3213(13) ?
Pt1 Cl1 . 2.3213(13) y
Pt1 Pt1 3_665 3.3475(8) y
Pt1 Pt1 3_666 3.3475(8) ?
N1 C1 . 1.445(6) y
N1 H1A . 0.9000 ?
N1 H1B . 0.9000 ?
C1 C2 . 1.372(6) y
C1 C1 2_655 1.386(9) y
C2 C3 . 1.377(11) y
C2 H2 . 0.9300 ?
C3 C3 2_655 1.38(3) y
C3 H3 . 0.9300 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A Cl1 4_566 0.90 2.57 3.353(4) 145.6
N1 H1B Cl1 4_565 0.90 2.71 3.381(4) 132.7
N1 H1B Cl1 3_565 0.90 2.73 3.320(5) 124.4
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_site_symmetry_1
_geom_torsion
Pt1 Pt1 N1 C1 3_665 84.8(3)
Pt1 Pt1 N1 C1 3_666 -92.9(3)
