Synthesis, Characterisation and Potent Cytotoxicity of Unconventional Platinum(IV) Complexes with Modified Lipophilicity
Deo, Krishant Moneesh; Sakoff, Jennette; Gilbert, Jayne; Zhang, Yingjie; Aldrich-Wright, Janice R; Dalton Transactions  (2019) –; doi:10.1039/C9DT03339D

data_7701388
_publ_section_title
;
 Synthesis, Characterisation and Potent Cytotoxicity of Unconventional
 Platinum(IV) Complexes with Modified Lipophilicity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03339D
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C26 H36 N4 O4 Pt, 0.5(O), 2(N O3)'
_chemical_formula_sum            'C26 H36 N6 O10.5 Pt'
_chemical_formula_weight         795.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-09-12 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.036(2)
_cell_length_b                   13.168(3)
_cell_length_c                   20.936(4)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.827
_cell_volume                     3042.5(11)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Eiga Detector'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30726
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.827
_diffrn_source                   'Australian Synchrotron MX2'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.678
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.2936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1906 before and 0.1013 after correction.
The Ratio of minimum to maximum transmission is 0.3934.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         3.012
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.224
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.18(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5347
_refine_ls_number_restraints     351
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1483P)^2^+0.7448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2081
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5101
_reflns_number_total             5347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03339d2.cif
_cod_data_source_block           p212121_a
_cod_original_cell_volume        3042.5(10)
_cod_original_formula_sum        'C26 H36 N6 O10.50 Pt'
_cod_database_code               7701388
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.82(3)
 0.18(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O1W(0.5)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C18(H18)
5.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B), C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              30407
_olex2_submission_special_instructions 'No special instructions were received'