Not the usual suspect – an unexpected organometallic product during the synthesis of a cytotoxic platinum(II) complex
Maier, Thomas; Wutschitz, Judith; Gajic, Natalie; Hejl, Michaela; Cseh, Klaudia; Mai, Sebastian; Jakupec, Michael; Galanski, Mathea Sophia; Keppler, Bernhard K.; Dalton Transactions  (2023) –; doi:10.1039/D3DT01736B

data_7714152
_publ_section_title
;
 Not the usual suspect -- an unexpected organometallic product during the
 synthesis of a cytotoxic platinum(II) complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01736B
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C10 H24 N2 O8 Pt'
_chemical_formula_weight         495.40
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-25
_audit_creation_method           'STOE LANA'
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                73.15(3)
_cell_angle_beta                 76.80(3)
_cell_angle_gamma                80.70(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2831(17)
_cell_length_b                   9.6777(19)
_cell_length_c                   10.192(2)
_cell_measurement_reflns_used    47101
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.86
_cell_measurement_theta_min      4.62
_cell_volume                     757.3(3)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
'  X-Area Integrate 2.5.3.0 (STOE, 2021)  X-Area LANA 2.7.5.0 (STOE, 2022)'
_computing_molecular_graphics    'ShelXle (H\"ubschle 2011)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 500K'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details      ' 15777 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15268
_diffrn_reflns_point_group_measured_fraction_full 0.592
_diffrn_reflns_point_group_measured_fraction_max 0.578
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.870
_diffrn_reflns_theta_min         5.515
_diffrn_source                   'Primux 100 micro'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    17.721
_exptl_absorpt_correction_T_max  0.4261
_exptl_absorpt_correction_T_min  0.1088
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
STOE LANA, spherical absorption correction
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'wedgy block'
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          0.050
_refine_diff_density_max         0.960
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.087(15)
_refine_ls_extinction_coef       0.00154(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         3380
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0178
_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^)+(0.0381P)^2^+0.5347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0462
_reflns_d_resolution_high        0.816
_reflns_d_resolution_low         9.572
_reflns_Friedel_coverage         0.236
_reflns_Friedel_fraction_full    0.236
_reflns_Friedel_fraction_max     0.221
_reflns_limit_h_max              10
_reflns_limit_h_min              -6
_reflns_limit_k_max              10
_reflns_limit_k_min              -11
_reflns_limit_l_max              12
_reflns_limit_l_min              -10
_reflns_number_gt                3300
_reflns_number_total             3380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01736b2.cif
_cod_data_source_block           mawa001_b
_cod_original_cell_volume        757.23(4)
_cod_database_code               7714152
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'J. Richter'
_stoe_detector_size_x            '7.7 cm'
_stoe_detector_size_y            '3.8 cm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_distance          '40.0 mm'
_stoe_measurement_identifier     MAWA001
_stoe_measurement_tube_power     '50.0 W'
_stoe_measurement_total_run_number 92
_stoe_measurement_total_frame_number 15777
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_max_exposure_per_frame '1.0 s'
_stoe_measurement_mean_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '4.4 h'
_stoe_evaluation_integration_a   15.7
_stoe_evaluation_integration_b   2.7
_stoe_evaluation_integration_ems 0.038
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_fs_max_order -
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max -
_stoe_evaluation_lana_bos_l_odd_max -
_stoe_evaluation_lana_or_c1      0.050
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      1.0
_stoe_evaluation_lana_max_2theta_available 141.8
_stoe_evaluation_lana_max_2theta_desired 141.8
_stoe_evaluation_lana_number_refls_total 18956
_stoe_evaluation_lana_number_refls_outliers 3108
_stoe_evaluation_lana_number_refls_after_or 15848
_stoe_evaluation_lana_number_refls_unique 2739
_stoe_evaluation_lana_number_refls_written 15848
_stoe_evaluation_lana_completeness 93.6
_stoe_evaluation_lana_mean_redundancy 5.8
_stoe_evaluation_lana_table
;
2Theta          16.3   31.1   45.9   60.7   75.5   90.3  105.1  119.9  134.7
<Resolution>    4.81   2.83   1.97   1.49   1.26   1.09   0.98   0.89   0.84
N(total)         386    859   1354   2639   3799   3453   2847   2389   1230
<Redundancy>     9.6    7.7    5.7    7.4    8.6    6.2    5.0    4.3    3.0
Complet. [%%]   100.0  100.0  100.0   99.0   97.2   96.9   95.8   91.6   78.0
<I/sigma>      220.8  158.6  114.2   68.4   53.2   41.0   37.7   39.4   46.3
R(int)         0.122  0.108  0.088  0.113  0.121  0.090  0.082  0.072  0.080
;
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              68046