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_1552170
_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         'C11 H14 N8 O2 Pt'
_chemical_formula_sum            'C11 H14 N8 O2 Pt'
_chemical_formula_weight         485.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_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                90
_cell_angle_beta                 92.473(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6152(3)
_cell_length_b                   9.1982(3)
_cell_length_c                   17.2275(5)
_cell_measurement_reflns_used    4557
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2970
_cell_measurement_theta_min      3.8160
_cell_volume                     1522.22(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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(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 0.874
_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 -10.00 91.00 1.00 15.00 -- 12.32 77.00 120.00 101 2 \w 30.00 59.00 1.00 15.00 -- 12.32 77.00-150.00 29 3 \w -21.00 64.00 1.00 15.00 -- 12.32 77.00 0.00 85'
_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      0.0408330000
_diffrn_orient_matrix_UB_12      -0.0557394000
_diffrn_orient_matrix_UB_13      0.0180243000
_diffrn_orient_matrix_UB_21      0.0294371000
_diffrn_orient_matrix_UB_22      -0.0159952000
_diffrn_orient_matrix_UB_23      -0.0360685000
_diffrn_orient_matrix_UB_31      0.0540307000
_diffrn_orient_matrix_UB_32      0.0508711000
_diffrn_orient_matrix_UB_33      0.0084186000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.757
_diffrn_reflns_theta_min         3.066
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.238
_exptl_absorpt_correction_T_max  0.047
_exptl_absorpt_correction_T_min  0.005
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.137
_refine_diff_density_max         6.245
_refine_diff_density_min         -2.457
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3790
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0886P)^2^+6.2355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3266
_reflns_number_total             3790
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 174.5869\% 
 around [-0.01 1.00 -0.03] (reciprocal) or [-0.01 1.00 -0.01] (direct)
;
_cod_data_source_file            c9sc02644d2.cif
_cod_data_source_block           es2
_cod_original_cell_volume        1522.21(8)
_cod_database_code               1552170
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N8 O2 Pt'
_shelx_estimated_absorpt_t_max   0.364
_shelx_estimated_absorpt_t_min   0.117
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
;
The OHs were not located but placed a positions to form H bonds 
with a suitable electronegative atoms

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
2. Restrained distances
 H1-N6
 2.7 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C105(H105), C106(H106), C202(H202), C203(H203),
 C204(H204), C205(H205), C206(H206)
3.b Idealised Me refined as rotating group:
 C107(H10A,H10B,H10C)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_shelx_res_checksum              83260
_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 3.158
_oxdiff_exptl_absorpt_empirical_full_min 0.475
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2