Platinum(iv) dihydroxido diazido N-(heterocyclic)imine complexes are potently photocytotoxic when irradiated with visible light
Shaili, Evyenia; Salassa, Luca; Woods, Julie A.; Clarkson, Guy; Sadler, Peter J.; Farrer, Nicola J.; Chemical Science  (2019) –; doi:10.1039/C9SC02644D

data_1552171
_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         '2(C4 H7 N5 O Pt0.5), H2 O'
_chemical_formula_sum            'C8 H16 N10 O3 Pt'
_chemical_formula_weight         495.40
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 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                71.076(5)
_cell_angle_beta                 79.831(4)
_cell_angle_gamma                84.892(6)
_cell_formula_units_Z            2
_cell_length_a                   8.4653(5)
_cell_length_b                   8.7128(6)
_cell_length_c                   10.9563(4)
_cell_measurement_reflns_used    2793
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.5220
_cell_measurement_theta_min      3.3260
_cell_volume                     751.97(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00  47.00   1.00   10.00    --   12.37 -19.00-150.00  115
  2  \w     -6.00  86.00   1.00   10.00    --   12.37  38.00  30.00   92
  3  \w     46.00  93.00   1.00   10.00    --   12.37 178.00 -90.00   47
  4  \w   -102.00 -61.00   1.00   10.00    --  -13.30-178.00   0.00   41
  5  \w    -17.00  28.00   1.00   10.00    --  -13.30 -99.00-180.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0315086000
_diffrn_orient_matrix_UB_12      0.0698943000
_diffrn_orient_matrix_UB_13      0.0053615000
_diffrn_orient_matrix_UB_21      0.0791255000
_diffrn_orient_matrix_UB_22      -0.0315700000
_diffrn_orient_matrix_UB_23      -0.0128314000
_diffrn_orient_matrix_UB_31      0.0011597000
_diffrn_orient_matrix_UB_32      0.0391549000
_diffrn_orient_matrix_UB_33      -0.0678847000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6671
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.703
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.361
_exptl_absorpt_correction_T_max  0.422
_exptl_absorpt_correction_T_min  0.079
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.176
_refine_diff_density_min         -2.158
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3708
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0396
_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/[\s^2^(Fo^2^)+(0.0624P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2572
_reflns_number_total             3708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02644d2.cif
_cod_data_source_block           es9
_cod_database_code               1552171
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N4 O5 Pt'
_shelx_estimated_absorpt_t_max   0.604
_shelx_estimated_absorpt_t_min   0.256
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
;
The hydrogens on the OH ligands were detected in a difference map but these 
and the water OHs were placed at calculated positions for the refinement.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 N7-H2A
 2.2 with sigma of 0.02
 O2-H1
 2.2 with sigma of 0.02
 H3B-O1
 2 with sigma of 0.02
3.a Free rotating group:
 O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C12(H12), C14(H14), C15(H15)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C16(H16A,H16B,H16C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_shelx_res_checksum              2815
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.974
_oxdiff_exptl_absorpt_empirical_full_min 0.604