In vivo and in vitro studies of [M(η6-pseudoerlotinib)2]+ sandwich complexes (M = Re, 99mTc)
Battistin, Federica; Fernandes, Célia; Raposinho, Paula D.; Blacque, Olivier; Paulo, António Rocha; Alberto, Roger; Dalton Transactions  (2023) –; doi:10.1039/D3DT03011C

data_7714216
_publ_section_title
;
 In vivo and in vitro studies of [M(\h6-pseudoerlotinib)2]+ sandwich
 complexes (M = Re, 99mTc)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03011C
_journal_year                    2023
_chemical_formula_moiety         'C40 H48 N6 O8 Re, F6 P, 2(Cl), 2(H2 O)'
_chemical_formula_sum            'C40 H52 Cl2 F6 N6 O10 P Re'
_chemical_formula_weight         1178.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-09-06 deposited with the CCDC.	2023-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                73.359(2)
_cell_angle_beta                 71.7530(10)
_cell_angle_gamma                75.7690(10)
_cell_formula_units_Z            2
_cell_length_a                   11.06150(10)
_cell_length_b                   13.8305(3)
_cell_length_c                   16.0904(3)
_cell_measurement_reflns_used    39858
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.7810
_cell_measurement_theta_min      2.9680
_cell_volume                     2206.68(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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   -126.00 -78.00   0.50    1.00    --  -51.79 -85.00  79.00   96
  2  \w    -78.00  23.00   0.50    1.00    --  -51.79  85.00-161.00  202
  3  \w    -22.00  78.00   0.50    1.00    --   51.79 -85.00  79.00  200
  4  \w   -161.00 -78.00   0.50    2.00    --  -86.25 -85.00  79.00  166
  5  \w   -112.00 -11.00   0.50    2.00    --  -86.25  85.00-161.00  202
  6  \w     33.00 134.00   0.50    2.00    --  107.75 -85.00  79.00  202
  7  \w    100.00 178.00   0.50    2.00    --  107.75  85.00-161.00  156
  8  \w   -126.00 -73.00   0.50    1.00    --  -51.79-125.00 -90.00  106
  9  \w   -125.00 -29.00   0.50    1.00    --  -51.79 -77.00-180.00  192
 10  \w   -126.00 -73.00   0.50    1.00    --  -51.79-125.00   0.00  106
 11  \w   -124.00 -37.00   0.50    1.00    --  -51.79 -57.00-150.00  174
 12  \w     29.00 125.00   0.50    1.00    --   51.79  77.00  90.00  192
 13  \w   -164.00 -73.00   0.50    2.00    --  -86.25 -30.00  90.00  182
 14  \w    -99.00 -10.00   0.50    2.00    --  -86.25  45.00  30.00  178
 15  \w     91.00 178.00   0.50    2.00    --  107.75  63.00 178.81  174
 16  \w     92.00 178.00   0.50    2.00    --  107.75  61.00 120.00  172
 17  \w     31.00 106.00   0.50    2.00    --  107.75 -94.00-180.00  150
 18  \w     31.00 109.00   0.50    2.00    --  107.75-111.00  60.00  156
 19  \w     94.00 178.00   0.50    2.00    --  107.75  30.00-150.00  168
 20  \w     31.00 109.00   0.50    2.00    --  107.75-111.00  30.00  156
 21  \w     34.00 130.00   0.50    2.00    --  107.75 -77.00-120.00  192
 22  \w     31.00 106.00   0.50    2.00    --  107.75 -94.00 120.00  150
 23  \w     31.00 106.00   0.50    2.00    --  107.75 -94.00 -30.00  150
 24  \w     40.00  91.00   0.50    2.00    --  107.75 -94.00-120.00  102
 25  \w     31.00  77.00   0.50    2.00    --  107.75 -94.00  30.00   92
 26  \w     86.00 116.00   0.50    2.00    --  107.75 -45.00  90.00   60
 27  \w     99.00 133.00   0.50    2.00    --  107.75  77.00  30.00   68
 28  \w    138.00 178.00   0.50    2.00    --  107.75  77.00  30.00   80
 29  \w     32.00 109.00   0.50    2.00    --  107.75-111.00 120.00  154
 30  \w     33.00 108.00   0.50    2.00    --  107.75-111.00 -60.00  150
 31  \w     95.00 120.00   0.50    2.00    --  107.75 -30.00-120.00   50
 32  \w     35.00 108.00   0.50    2.00    --  107.75-102.00  -9.58  146
 33  \w     63.00 100.00   0.50    2.00    --  107.75 -94.00  60.00   74
 34  \w     46.00 109.00   0.50    2.00    --  107.75-111.00 -30.00  126
 35  \w     96.00 178.00   0.50    2.00    --  107.75  45.00  90.00  164
 36  \w     50.00 109.00   0.50    2.00    --  107.75-111.00-180.00  118
 37  \w     38.00  67.00   0.50    2.00    --  107.75 -30.00-120.00   58
 38  \w     96.00 174.00   0.50    2.00    --  107.75  15.00-180.00  156
 39  \w     83.00 109.00   0.50    2.00    --  107.75-111.00-120.00   52
 40  \w    122.00 177.00   0.50    2.00    --  107.75  61.00   0.00  110
 41  \w    112.00 167.00   0.50    2.00    --  107.75  15.00 -60.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0492896000
_diffrn_orient_matrix_UB_12      0.0923596000
_diffrn_orient_matrix_UB_13      -0.0685644000
_diffrn_orient_matrix_UB_21      -0.0108476000
_diffrn_orient_matrix_UB_22      0.0715707000
_diffrn_orient_matrix_UB_23      0.0607848000
_diffrn_orient_matrix_UB_31      0.1400431000
_diffrn_orient_matrix_UB_32      0.0165255000
_diffrn_orient_matrix_UB_33      -0.0481890000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46323
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.499
_diffrn_reflns_theta_min         2.970
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.636
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         8981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+7.2006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8836
_reflns_number_total             8981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03011c2.cif
_cod_data_source_block           1
_cod_database_code               7714216
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.394
_olex2_refinement_description
;
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 C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(O10B)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(O10A)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Fixed X: H10C(0.046109) H10D(0.05418)
 Fixed Y: H10C(0.88909) H10D(0.80179)
 Fixed Z: H10C(0.380449) H10D(0.35281)
3.a Free rotating group:
 O9(H9A,H9B), O10A(H10A,H10B)
3.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C35(H35A,
 H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4A), C5(H5), C6(H6A), C8(H8), C11(H11), C14(H14),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C31(H31), C34(H34)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C37(H37A,H37B,H37C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              58395