Platinum(IV)-azido monocarboxylato complexes are photocytotoxic under irradiation with visible light.
Shaili, Evyenia; Romero, Mar\ía J; Salassa, Luca; Woods, Julie A.; Butler, Jennifer S.; Romero-Canelón, Isolda; Clarkson, Guy; Habtemariam, Abraha; Sadler, Peter J.; Farrer, Nicola J.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10593–10607; doi:10.1039/d1dt01730f

data_7707831
_publ_section_title
;
 Platinum(IV)-azido monocarboxylato complexes are photocytotoxic under
 irradiation with visible light.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10593
_journal_page_last               10607
_journal_paper_doi               10.1039/d1dt01730f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C18 H19 N9 O3 Pt'
_chemical_formula_sum            'C18 H19 N9 O3 Pt'
_chemical_formula_weight         604.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-05 deposited with the CCDC.	2021-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.184(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.54127(18)
_cell_length_b                   35.8789(6)
_cell_length_c                   8.17745(19)
_cell_measurement_reflns_used    18581
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2270
_cell_measurement_theta_min      3.1260
_cell_volume                     2089.72(9)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.999
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega 40.00 96.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 18.3155 178.0000 90.0000 56 #__ type_ start__ end____ width___ exp.time_ 2 omega -22.00 15.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 18.3155 -38.0000 120.0000 37 #__ type_ start__ end____ width___ exp.time_ 3 omega -56.00 45.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - 18.3155 -38.0000 -120.0000 101 #__ type_ start__ end____ width___ exp.time_ 4 omega -73.00 -46.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -19.2530 -57.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 5 omega -24.00 18.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -19.2530 -99.0000 90.0000 42 #__ type_ start__ end____ width___ exp.time_ 6 omega -108.00 -53.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -19.2530 178.0000 60.0000 55 #__ type_ start__ end____ width___ exp.time_ 7 omega -95.00 7.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -19.2530 -38.0000 -60.0000 102 #__ type_ start__ end____ width___ exp.time_ 8 omega -93.00 10.00 1.0000 40.0000 omega____ theta____ kappa____ phi______ frames - -19.2530 -57.0000 -150.0000 103'
_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      -0.0601265000
_diffrn_orient_matrix_UB_12      0.0103742000
_diffrn_orient_matrix_UB_13      -0.0702906000
_diffrn_orient_matrix_UB_21      0.0687396000
_diffrn_orient_matrix_UB_22      0.0142487000
_diffrn_orient_matrix_UB_23      0.0153076000
_diffrn_orient_matrix_UB_31      0.0397833000
_diffrn_orient_matrix_UB_32      -0.0089393000
_diffrn_orient_matrix_UB_33      -0.0571002000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.499
_diffrn_reflns_theta_min         2.698
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) 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    1.921
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+1.0229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5686
_reflns_number_total             6362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01730f2.cif
_cod_data_source_block           es11
_cod_depositor_comments
'Adding full bibliography for 7707830--7707832.cif.'
_cod_database_code               7707831
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O2 Pt'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;

The amide NH and the OH were located in a difference map but refined
at calculated positions

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(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:
 C5(H5), C6(H6), C7(H7), C8(H8), N10(H10), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              45256
_shelx_hkl_checksum              47095
_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 1.880
_oxdiff_exptl_absorpt_empirical_full_min 0.837