Tuning the photoactivated anticancer activity of Pt(iv) compounds <i>via</i> distant ferrocene conjugation.
Shi, Huayun; Ponte, Fortuna; Grewal, Jaspreet S.; Clarkson, Guy J.; Imberti, Cinzia; Hands-Portman, Ian; Dallmann, Robert; Sicilia, Emilia; Sadler, Peter J.; Chemical science 15 (2024) 4121–4134; doi:10.1039/d3sc03092j

data_1571000
_publ_section_title
;
 Tuning the photoactivated anticancer activity of Pt(iv) compounds
 <i>via</i> distant ferrocene conjugation.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              4121
_journal_page_last               4134
_journal_paper_doi               10.1039/d3sc03092j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C23 H23 Fe N9 O4 Pt'
_chemical_formula_sum            'C23 H23 Fe N9 O4 Pt'
_chemical_formula_weight         740.44
_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     dual
_audit_creation_date             2018-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2023-01-05 deposited with the CCDC.	2024-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4247(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1269(3)
_cell_length_b                   10.50172(17)
_cell_length_c                   16.1559(3)
_cell_measurement_reflns_used    13646
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1160
_cell_measurement_theta_min      3.1430
_cell_volume                     2515.65(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.895
_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    -61.00  41.00   1.00    2.23    --   12.41 -78.00 -92.00  102
  2  \w    -16.00  68.00   1.00    2.23    --   12.41  78.00  32.00   84
  3  \w     18.00  59.00   1.00    2.23    --   12.41-114.00-171.00   41
  4  \w     10.00  82.00   1.00    2.23    --   12.41  38.00-180.00   72
  5  \w    -93.00 -57.00   1.00    2.23    --  -13.35-178.00   0.00   36
;
_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      0.0112673000
_diffrn_orient_matrix_UB_12      -0.0494316000
_diffrn_orient_matrix_UB_13      -0.0259893000
_diffrn_orient_matrix_UB_21      -0.0279630000
_diffrn_orient_matrix_UB_22      0.0283095000
_diffrn_orient_matrix_UB_23      -0.0356736000
_diffrn_orient_matrix_UB_31      0.0371423000
_diffrn_orient_matrix_UB_32      0.0363090000
_diffrn_orient_matrix_UB_33      -0.0075694000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.314
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.706
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+0.7783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5890
_reflns_number_total             6758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03092j2.cif
_cod_data_source_block           hs32
_cod_depositor_comments          'Adding full bibliography for 1571000.cif.'
_cod_original_cell_volume        2515.64(8)
_cod_database_code               1571000
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O2 Fe Pt'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
The NH and OH 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, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C18(H18), C14(H14), N22(H22), C17(H17), C11(H11), C30(H30), C8(H8),
 C28(H28), C33(H33), C15(H15), C26(H26), C29(H29), C25(H25), C31(H31), C16(H16),
  C32(H32), C10(H10), C27(H27), C9(H9)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              43690
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.901