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_1552172
_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         'C12 H16 N8 O2 Pt, 2(C H4 O)'
_chemical_formula_sum            'C14 H24 N8 O4 Pt'
_chemical_formula_weight         563.50
_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                 90.6038(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.09413(13)
_cell_length_b                   11.18048(20)
_cell_length_c                   12.3270(2)
_cell_measurement_reflns_used    6042
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3821
_cell_measurement_theta_min      2.8657
_cell_volume                     977.67(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11)'
_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      150(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega -6.00 106.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 16.3155 0.0000 -60.0000 112 #__ type_ start__ end____ width___ exp.time_ 2 omega -65.00 57.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 16.3155 -19.0000 120.0000 122 #__ type_ start__ end____ width___ exp.time_ 3 omega -1.00 86.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - 16.3155 38.0000 120.0000 87 #__ type_ start__ end____ width___ exp.time_ 4 omega -101.00 -61.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - -17.2530 -178.0000 150.0000 40 #__ type_ start__ end____ width___ exp.time_ 5 omega -25.00 0.00 1.0000 7.0000 omega____ theta____ kappa____ phi______ frames - -17.2530 -99.0000 120.0000 25'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0747008000
_diffrn_orient_matrix_UB_12      -0.0125317000
_diffrn_orient_matrix_UB_13      -0.0369644000
_diffrn_orient_matrix_UB_21      -0.0267000000
_diffrn_orient_matrix_UB_22      -0.0498134000
_diffrn_orient_matrix_UB_23      0.0319731000
_diffrn_orient_matrix_UB_31      -0.0608984000
_diffrn_orient_matrix_UB_32      0.0372245000
_diffrn_orient_matrix_UB_33      0.0303627000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         31.453
_diffrn_reflns_theta_min         3.298
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) 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    1.914
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.839
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         3003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0174P)^2^+0.5476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2333
_reflns_number_total             3003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02644d2.cif
_cod_data_source_block           es10
_cod_database_code               1552172
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O2 Pt'
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.256
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_olex2_refinement_description
;
The OHs on both the hydroxy ligand and the methanol were located in a difference map 
but 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
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C12(H12A,H12B,H12C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O11(H11)
;
_shelx_res_checksum              43117
_olex2_submission_special_instructions 'No special instructions were received'