#------------------------------------------------------------------------------
#$Date: 2019-08-09 03:20:12 +0300 (Fri, 09 Aug 2019) $
#$Revision: 217469 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/21/1552173.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_1552173
loop_
_publ_author_name
'Shaili, Evyenia'
'Salassa, Luca'
'Woods, Julie A.'
'Clarkson, Guy'
'Sadler, Peter J.'
'Farrer, Nicola J.'
_publ_section_title
;
 Platinum(iv) dihydroxido diazido N-(heterocyclic)imine complexes are
 potently photocytotoxic when irradiated with visible light
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02644D
_journal_year                    2019
_chemical_formula_moiety         'C6 H6 N8 Pt S2'
_chemical_formula_sum            'C6 H6 N8 Pt S2'
_chemical_formula_weight         449.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-03 deposited with the CCDC.    2019-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                88.995(3)
_cell_angle_beta                 86.555(3)
_cell_angle_gamma                76.997(3)
_cell_formula_units_Z            1
_cell_length_a                   3.79960(10)
_cell_length_b                   8.1562(3)
_cell_length_c                   9.0053(3)
_cell_measurement_reflns_used    3936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      3.40
_cell_volume                     271.427(16)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3931
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.061
_diffrn_reflns_theta_min         3.415
_exptl_absorpt_coefficient_mu    13.298
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.756
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0233P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1314
_reflns_number_total             1314
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc02644d2.cif
_cod_data_source_block           nf2
_cod_database_code               1552173
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5)
;
_shelx_res_file
;
TITL nf2 in P1
    nf2.res
    created by SHELXL-2018/3 at 16:06:33 on 30-Mar-2019
REM yellow block 0.32 0.08 0.04
REM yellow block 032 0.08 0.04 3936 refs 3.40 28.99 0.49 1.00
REM ACTA 54
CELL 0.71073 3.7996 8.1562 9.0053 88.995 86.555 76.997
ZERR 1 0.0001 0.0003 0.0003 0.003 0.003 0.003
LATT 1
SFAC C H N Pt S
UNIT 6 6 8 1 2
EQIV $1 2-X,1-Y,1-Z
EQIV $2 -1+X,+Y,+Z
EQIV $3 -X,2-Y,1-Z
EQIV $4 +X,+Y,-1+Z
EQIV $5 -X,2-Y,-Z
EQIV $6 1+X,+Y,+Z
EQIV $7 1-X,1-Y,1-Z

L.S. 4
PLAN  20
TEMP -173
HTAB C2 N8_$1
HTAB C5 N6
HTAB C5 N6_$2
HTAB C4 N6_$3
RTAB dist S3 N8_$4
RTAB dist S3 S3_$5
RTAB dist S3 C4_$6
RTAB dist Pt1 Pt1_$2
RTAB tors C2 N1 Pt1 N6_$7
BOND $H
fmap 2
ACTA
REM <olex2.extras>
REM <HklSrc "%./nf2.hkl">
REM </olex2.extras>

WGHT    0.023300
FVAR       8.71165
PT1   4    0.500000    0.500000    0.500000    10.50000    0.01107    0.00482 =
         0.00605    0.00158   -0.00024    0.00042
N1    3    0.345476    0.678583    0.345034    11.00000    0.01289    0.00765 =
         0.00769    0.00143   -0.00158   -0.00160
C2    1    0.469237    0.675142    0.204471    11.00000    0.01288    0.00712 =
         0.01049    0.00315   -0.00241   -0.00286
AFIX  43
H2    2    0.637525    0.581737    0.161177    11.00000   -1.20000
AFIX   0
S3    5    0.298347    0.853855    0.108695    11.00000    0.01491    0.01085 =
         0.00999    0.00370   -0.00154   -0.00159
C4    1    0.047957    0.941162    0.263748    11.00000    0.00997    0.00959 =
         0.01529   -0.00110   -0.00155   -0.00055
AFIX  43
H4    2   -0.105733    1.050526    0.268645    11.00000   -1.20000
AFIX   0
C5    1    0.103207    0.829426    0.379206    11.00000    0.01421    0.00818 =
         0.01078   -0.00226   -0.00119   -0.00162
AFIX  43
H5    2   -0.014474    0.852976    0.475046    11.00000   -1.20000
AFIX   0
N6    3    0.542723    0.690213    0.635874    11.00000    0.01809    0.00674 =
         0.01134   -0.00012   -0.00276   -0.00047
N7    3    0.691163    0.667677    0.752397    11.00000    0.01203    0.00543 =
         0.01380   -0.00059    0.00098   -0.00075
N8    3    0.826538    0.659239    0.864651    11.00000    0.01991    0.01697 =
         0.01336    0.00000   -0.00407   -0.00324
HKLF 4




REM  nf2 in P1
REM wR2 = 0.0392, GooF = S = 1.080, Restrained GooF = 1.080 for all data
REM R1 = 0.0175 for 1314 Fo > 4sig(Fo) and 0.0175 for all 1314 data
REM 79 parameters refined using 0 restraints

END

WGHT      0.0233      0.0000

REM Highest difference peak  0.756,  deepest hole -1.372,  1-sigma level  0.180
Q1    1   0.4511  0.3991  0.4951  11.00000  0.05    0.76
Q2    1   0.1908  0.4593  0.5339  11.00000  0.05    0.71
Q3    1   0.5504  0.6042  0.6111  11.00000  0.05    0.68
Q4    1   0.0794  0.4754  0.4297  11.00000  0.05    0.66
Q5    1   0.2561  0.4248  0.4922  11.00000  0.05    0.61
Q6    1   0.0000  0.5000  0.5000  10.50000  0.05    0.60
Q7    1   0.7432  0.6594  0.4184  11.00000  0.05    0.58
Q8    1   0.2411  0.4948  0.6222  11.00000  0.05    0.58
Q9    1   0.8995  0.5104  0.2840  11.00000  0.05    0.56
Q10   1   0.2531  0.5180  0.5366  11.00000  0.05    0.56
Q11   1   0.8918  0.6386  0.2399  11.00000  0.05    0.55
Q12   1   0.6033  0.8655  0.0711  11.00000  0.05    0.54
Q13   1   0.9090  0.5921  0.0509  11.00000  0.05    0.54
Q14   1   0.5262  0.5649  0.7164  11.00000  0.05    0.54
Q15   1   0.0076  0.5212  0.3952  11.00000  0.05    0.52
Q16   1   0.3938  0.6198  0.3918  11.00000  0.05    0.52
Q17   1   0.7180  0.6423  1.0039  11.00000  0.05    0.52
Q18   1   0.8892  0.6438  0.6077  11.00000  0.05    0.51
Q19   1   0.9473  0.7384  0.9985  11.00000  0.05    0.51
Q20   1   0.3097  0.6194  0.7807  11.00000  0.05    0.51
;
_shelx_res_checksum              15629
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pt1 Pt 0.500000 0.500000 0.500000 0.00769(7) Uani 1 2 d S T P
N1 N 0.3455(7) 0.6786(4) 0.3450(3) 0.0095(5) Uani 1 1 d . . .
C2 C 0.4692(9) 0.6751(4) 0.2045(4) 0.0100(6) Uani 1 1 d . . .
H2 H 0.637525 0.581737 0.161177 0.012 Uiso 1 1 calc R . .
S3 S 0.2983(2) 0.85386(11) 0.10869(9) 0.01213(17) Uani 1 1 d . . .
C4 C 0.0480(9) 0.9412(4) 0.2637(4) 0.0118(7) Uani 1 1 d . . .
H4 H -0.105733 1.050526 0.268645 0.014 Uiso 1 1 calc R . .
C5 C 0.1032(9) 0.8294(4) 0.3792(4) 0.0112(6) Uani 1 1 d . . .
H5 H -0.014474 0.852976 0.475046 0.013 Uiso 1 1 calc R . .
N6 N 0.5427(8) 0.6902(4) 0.6359(3) 0.0123(6) Uani 1 1 d . . .
N7 N 0.6912(7) 0.6677(4) 0.7524(3) 0.0107(6) Uani 1 1 d . . .
N8 N 0.8265(8) 0.6592(4) 0.8647(3) 0.0168(6) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01107(10) 0.00482(10) 0.00605(9) 0.00158(6) -0.00024(6) 0.00042(6)
N1 0.0129(13) 0.0076(14) 0.0077(13) 0.0014(10) -0.0016(10) -0.0016(11)
C2 0.0129(16) 0.0071(16) 0.0105(16) 0.0032(12) -0.0024(12) -0.0029(13)
S3 0.0149(4) 0.0108(4) 0.0100(4) 0.0037(3) -0.0015(3) -0.0016(3)
C4 0.0100(15) 0.0096(17) 0.0153(16) -0.0011(13) -0.0015(12) -0.0006(13)
C5 0.0142(16) 0.0082(16) 0.0108(16) -0.0023(12) -0.0012(12) -0.0016(13)
N6 0.0181(14) 0.0067(14) 0.0113(14) -0.0001(11) -0.0028(11) -0.0005(11)
N7 0.0120(13) 0.0054(14) 0.0138(14) -0.0006(11) 0.0010(11) -0.0008(11)
N8 0.0199(16) 0.0170(16) 0.0134(15) 0.0000(12) -0.0041(12) -0.0032(13)
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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N1 Pt1 N1 180.00(16) 2_666 .
N1 Pt1 N6 86.62(11) 2_666 2_666
N1 Pt1 N6 93.38(11) 2_666 .
N1 Pt1 N6 86.62(11) . .
N1 Pt1 N6 93.38(11) . 2_666
N6 Pt1 N6 180.0 . 2_666
C2 N1 Pt1 126.4(2) . .
C2 N1 C5 111.4(3) . .
C5 N1 Pt1 122.0(2) . .
N1 C2 H2 123.2 . .
N1 C2 S3 113.5(3) . .
S3 C2 H2 123.2 . .
C2 S3 C4 91.09(17) . .
S3 C4 H4 125.2 . .
C5 C4 S3 109.5(3) . .
C5 C4 H4 125.2 . .
N1 C5 H5 122.8 . .
C4 C5 N1 114.4(3) . .
C4 C5 H5 122.8 . .
N7 N6 Pt1 123.4(2) . .
N8 N7 N6 174.8(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N1 2.014(3) 2_666
Pt1 N1 2.014(3) .
Pt1 N6 2.033(3) 2_666
Pt1 N6 2.033(3) .
N1 C2 1.322(4) .
N1 C5 1.388(4) .
C2 H2 0.9500 .
C2 S3 1.699(3) .
S3 C4 1.712(4) .
C4 H4 0.9500 .
C4 C5 1.365(5) .
C5 H5 0.9500 .
N6 N7 1.213(4) .
N7 N8 1.156(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2 N8 0.95 2.49 3.400(5) 159.4 2_766 yes
C4 H4 N6 0.95 2.51 3.422(4) 161.9 2_576 yes
C5 H5 N6 0.95 2.71 3.402(5) 130.4 1_455 yes
C5 H5 N6 0.95 2.72 2.990(4) 97.3 . yes
