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_7714215
_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         'C12 H13 N Re, F6 P'
_chemical_formula_sum            'C12 H13 F6 N P Re'
_chemical_formula_weight         502.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2023-09-06 deposited with the CCDC.	2023-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0918(1)
_cell_length_b                   12.2476(2)
_cell_length_c                   7.0155(1)
_cell_measurement_reflns_used    3609
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.1430
_cell_measurement_theta_min      6.5190
_cell_volume                     695.272(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5'
_computing_structure_refinement  'SHELXL 2018/3 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     34.00 123.00   0.50    0.10    --   52.02  66.00 -55.00  178
  2  \w   -101.00 -13.00   0.50    0.20    --  -86.25  57.00 149.00  176
  3  \w   -162.00 -80.00   0.50    0.20    --  -86.25-112.00 -69.00  164
  4  \w     37.00 126.00   0.50    0.20    --  107.75 -66.00 169.00  178
  5  \w    -86.00 -12.00   0.50    0.10    --  -52.02 125.00 -90.00  148
  6  \w   -127.00 -73.00   0.50    0.10    --  -52.02-125.00  90.00  108
  7  \w     94.00 178.00   0.50    0.20    --  107.75  30.00 -90.00  168
  8  \w    102.00 178.00   0.50    0.20    --  107.75 111.00 150.00  152
  9  \w     31.00 106.00   0.50    0.20    --  107.75 -94.00  90.00  150
 10  \w     94.00 178.00   0.50    0.20    --  107.75  30.00 -60.00  168
 11  \w     94.00 178.00   0.50    0.20    --  107.75  30.00-120.00  168
 12  \w     31.00 106.00   0.50    0.20    --  107.75 -94.00-180.00  150
 13  \w     93.00 178.00   0.50    0.20    --  107.75  57.00 149.00  170
 14  \w   -125.00 -30.00   0.50    0.10    --  -52.02 -77.00 120.00  190
 15  \w   -125.00 -37.00   0.50    0.10    --  -52.02 -57.00   8.00  176
 16  \w   -125.00 -30.00   0.50    0.10    --  -52.02 -77.00-150.00  190
 17  \w     94.00 119.00   0.50    0.20    --  107.75  30.00   0.00   50
 18  \w     96.00 178.00   0.50    0.20    --  107.75  15.00  90.00  164
;
_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      0.0255588000
_diffrn_orient_matrix_UB_12      0.1134496000
_diffrn_orient_matrix_UB_13      -0.0901376000
_diffrn_orient_matrix_UB_21      0.1277001000
_diffrn_orient_matrix_UB_22      -0.0487417000
_diffrn_orient_matrix_UB_23      -0.1388673000
_diffrn_orient_matrix_UB_31      -0.1388626000
_diffrn_orient_matrix_UB_32      -0.0240256000
_diffrn_orient_matrix_UB_33      -0.1442506000
_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  0.0280
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3744
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.320
_diffrn_reflns_theta_min         6.557
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.792
_exptl_absorpt_correction_T_max  0.337
_exptl_absorpt_correction_T_min  0.133
_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    2.400
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0087(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         436
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0162
_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^)+(0.0216P)^2^+1.3906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                436
_reflns_number_total             436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03011c2.cif
_cod_data_source_block           2
_cod_database_code               7714215
_shelx_estimated_absorpt_t_max   0.283
_shelx_estimated_absorpt_t_min   0.133
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All F(H,H) groups
2. Restrained distances
 C1A-C2A = C2B-C1B
 1.4 with sigma of 0.01
 C1B_$1-C1B_$2
 1.4 with sigma of 0.01
 N1-H1D = N1-H1C
 0.82 with sigma of 0.005
 H1D-H1C
 1.34 with sigma of 0.01
 P1-F2A \\sim P1-F1A \\sim P1-F1B \\sim P1-F2B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Re1 \\sim C1A \\sim C2A \\sim C1B \\sim C2B: within 3A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3A
F1A \\sim F2A \\sim F1B \\sim F2B: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3A
4. Others
 Sof(F1B)=0.5*(1-FVAR(2))
 Sof(F2B)=0.25*(1-FVAR(2))
 Sof(F1A)=0.25*FVAR(2)
 Sof(F2A)=0.5*FVAR(2)
 Sof(C2A)=Sof(H2A)=1-FVAR(2)
 Sof(C1A)=0.5*(1-FVAR(3))
 Sof(C2B)=Sof(H2B)=0.5*FVAR(3)
 Sof(C1B)=Sof(H1B)=FVAR(2)
 Fixed Sof: H1A(0.28425) H1D(0.125) H1C(0.125) N1(0.125)
5.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C1B(H1B), C2B(H2B)
;
_shelx_res_checksum              43231