The role of stereochemistry in the anticancer activity of Re(I) tricarbonyl complexes.
Solea, Atena B.; Demirci, Gozde; Harvey, Freya M.; Crochet, Aurelien; Zobi, Fabio; Mamula Steiner, Olimpia; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13743–13755; doi:10.1039/d4dt01643b

data_7716615
_publ_section_title
;
 The role of stereochemistry in the anticancer activity of Re(I)
 tricarbonyl complexes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13743
_journal_page_last               13755
_journal_paper_doi               10.1039/d4dt01643b
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration syn
_chemical_formula_moiety
'2(C40 H34 Cl2 N4 O6 Re2), 2[C2H5OH], 1[CH2Cl2]'
_chemical_formula_sum            'C85 H82 Cl6 N8 O14 Re4'
_chemical_formula_weight         2397.186
_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_Int_Tables_number      1
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                115.332(1)
_cell_angle_beta                 94.913(1)
_cell_angle_gamma                93.345(1)
_cell_formula_units_Z            1
_cell_length_a                   12.0572(2)
_cell_length_b                   14.1674(2)
_cell_length_c                   14.4880(3)
_cell_measurement_reflns_used    90694
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      3.47
_cell_volume                     2216.21(7)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.9395
_diffrn_measured_fraction_theta_max 0.9332
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.9395
_diffrn_reflns_Laue_measured_fraction_max 0.9332
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9052
_diffrn_reflns_point_group_measured_fraction_full 0.5657
_diffrn_reflns_point_group_measured_fraction_max 0.5618
_diffrn_reflns_theta_full        67.5000
_diffrn_reflns_theta_max         67.85
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'Primux 100 micro'
_exptl_absorpt_coefficient_mu    12.616
_exptl_absorpt_correction_T_max  0.4317
_exptl_absorpt_correction_T_min  0.1396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       prism
_exptl_crystal_F_000             1149.031
_exptl_crystal_recrystallization_method
'from vapor diffusion with DCM, ethanol and diethyl ether'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
TITL ate456-2_tP 1          R = 0.06
CELL   12.0572   14.1674   14.4880    115.33     94.91     93.35
SPGR P1
C101 0.908 0.322 0.836 !       5.24 eA-3
C102 0.730 0.269 0.373 !       4.70 eA-3
C103 0.698 0.330 0.356 !       4.46 eA-3
C104 0.351 0.280 0.722 !       4.17 eA-3
C105 0.947 0.254 0.888 !       4.08 eA-3
C106 0.764 0.295 0.201 !       3.56 eA-3
C107 0.293 0.217 0.537 !       3.22 eA-3
Q108 0.502 0.292 0.452 !       3.11 eA-3
Q109 0.502 0.390 0.505 !       3.10 eA-3
Q110 0.514 0.089 0.345 !       3.08 eA-3
Q111 0.511 0.184 0.397 !       3.08 eA-3
C112 0.323 0.281 0.644 !       2.90 eA-3
Q113 0.501 0.497 0.559 !       2.80 eA-3
C114 0.891 0.229 0.063 !       2.62 eA-3
C115 0.920 0.282-0.005 !       2.49 eA-3
C116 0.376 0.391 0.776 !       2.46 eA-3
C117 0.281 0.256 0.453 !       2.45 eA-3
C118 0.888 0.326 0.109 !       2.44 eA-3
C119 0.237 0.214 0.455 !       2.38 eA-3
Q120 0.485 0.698 0.676 !       2.36 eA-3
C121 0.692 0.282 0.240 !       2.35 eA-3
Q122 0.532 0.877 0.222 !       2.29 eA-3
Q123 0.126 0.153 0.743 !       2.20 eA-3
Q124 0.125 0.060 0.688 !       2.20 eA-3
Q125 0.137 0.266 0.780 !       2.19 eA-3
C126 0.282 0.326 0.587 !       2.13 eA-3
C127 0.232 0.314 0.498 !       2.08 eA-3
Q128 0.127 0.463 0.891 !       1.96 eA-3
Q129 0.127 0.360 0.835 !       1.95 eA-3
Q130 0.893 0.128 0.003 !       1.90 eA-3
C131 0.878 0.312 0.031 !       1.87 eA-3
Q132 0.497 0.794 0.720 !       1.66 eA-3
Q133 0.519 0.781 0.177 !       1.60 eA-3
Q134 0.486 0.613 0.642 !       1.59 eA-3
Q135 0.877 0.426 0.161 !       1.52 eA-3
Q136 0.252 0.295 0.734 !       1.41 eA-3
Q137 0.503 0.019 0.351 !       1.37 eA-3
Q138 0.141 0.856 0.591 !       1.35 eA-3
Q139 0.481 0.275 0.913 !       1.29 eA-3
Q140 0.514 0.567 0.513 !       1.27 eA-3
Q141 0.137 0.939 0.581 !       1.26 eA-3
Q142 0.706 0.431 0.462 !       1.16 eA-3
C143 0.445 0.420 0.845 !       1.14 eA-3
Q144 0.139 0.181 0.432 !       1.10 eA-3
Q145 0.518 0.946 0.241 !       1.10 eA-3
Q146 0.516 0.202 0.933 !       1.09 eA-3
Q147 0.516 0.098 0.876 !       1.07 eA-3
Q148 0.155 0.544 0.864 !       1.07 eA-3
Q149 0.888 0.534 0.222 !       1.06 eA-3
Q150 0.143 0.289 0.405 !       1.05 eA-3
Q151 0.503 0.939 0.326 !       1.02 eA-3
Q152 0.496 0.875 0.686 !       1.01 eA-3
Q153 0.136 0.614 0.004 !       1.01 eA-3
Q154 0.499 0.391 0.952 !       0.98 eA-3
Q155 0.515 0.999 0.823 !       0.98 eA-3
Q156 0.109 1.003 0.713 !       0.98 eA-3
Q157 0.499 0.595 0.057 !       0.97 eA-3
Q158 0.500 0.302 0.986 !       0.97 eA-3
Q159 0.609 0.295 0.175 !       0.97 eA-3
C160 0.081 0.287 0.043 !       0.97 eA-3
Q161 0.496 0.190 0.850 !       0.96 eA-3
Q162 0.611 0.366 0.402 !       0.96 eA-3
Q163 0.107 0.669-0.002 !       0.96 eA-3
Q164 0.471 0.902 0.787 !       0.96 eA-3
Q165 0.109 0.467 0.355 !       0.95 eA-3
Q166 0.874 0.643 0.278 !       0.94 eA-3
Q167 0.860 0.738 0.331 !       0.93 eA-3
Q168 0.859 0.394 0.893 !       0.92 eA-3
C169 0.965 0.310 0.100 !       0.92 eA-3
Q170 0.500 0.988 0.730 !       0.91 eA-3
Q171 0.501 0.497 0.009 !       0.90 eA-3
Q172 0.143 0.064 0.223 !       0.90 eA-3
Q173 0.499 0.767 0.629 !       0.89 eA-3
Q174 0.264 0.287 0.350 !       0.89 eA-3
Q175 0.905 0.031 0.950 !       0.88 eA-3
Q176 0.519 0.687 0.130 !       0.87 eA-3
Q177 0.468 0.984 0.788 !       0.86 eA-3
Q178 0.919 0.926 0.890 !       0.86 eA-3
Q179 0.515 0.808 0.268 !       0.86 eA-3
C180 0.734 0.183 0.145 !       0.84 eA-3
Q181 0.234 0.197 0.690 !       0.84 eA-3
Q182 0.138 0.287 0.482 !       0.84 eA-3
Q183 0.127 0.270 0.329 !       0.84 eA-3
Q184 0.499 0.083 0.783 !       0.83 eA-3
Q185 0.751 0.130 0.033 !       0.83 eA-3
Q186 0.127 0.256 0.236 !       0.83 eA-3
Q187 0.779 0.020 0.987 !       0.83 eA-3
Q188 0.043 0.908 0.612 !       0.82 eA-3
C189 0.496 0.269 0.158 !       0.81 eA-3
Q190 0.861 0.845 0.386 !       0.81 eA-3
Q191 0.127 0.765 0.541 !       0.80 eA-3
C192 0.780 0.223 0.154 !       0.80 eA-3
C193 0.840 0.282 0.249 !       0.79 eA-3
Q194 0.265 0.169 0.317 !       0.79 eA-3
Q195 0.424 0.331 0.193 !       0.79 eA-3
Q196 0.969 0.232 0.050 !       0.79 eA-3
Q197 0.604 0.969 0.372 !       0.79 eA-3
Q198 0.154 0.970 0.171 !       0.78 eA-3
Q199 0.580 0.515 0.659 !       0.78 eA-3
;
_refine_diff_density_max         1.9099
_refine_diff_density_min         -1.5352
_refine_diff_density_rms         0.1331
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.059(8)
_refine_ls_d_res_high            0.8323
_refine_ls_d_res_low             12.1015
_refine_ls_goodness_of_fit_ref   1.0428
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    115
_refine_ls_number_parameters     814
_refine_ls_number_reflns         9052
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.0427
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+6.6952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.190
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -16
_reflns_limit_l_max              13
_reflns_limit_l_min              -17
_reflns_number_gt                8721
_reflns_number_total             9052
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt01643b2.cif
_cod_data_source_block           ATE456-2_tw_sq
_cod_depositor_comments
'Adding full bibliography for 7716611--7716619.cif.'
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               7716615
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.582(11)
 0.418(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 O5, C73
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Uiso/Uaniso restraints and constraints
Uanis(C73) = Uanis(C72) = Uanis(C74)
Uanis(C59) = Uanis(C58) = Uanis(C55) = Uanis(C54) = Uanis(C37) = Uanis(C38) =
Uanis(C42) = Uanis(C41) = Uanis(C25) = Uanis(C24) = Uanis(C21) = Uanis(C20) =
Uanis(C3) = Uanis(C4) = Uanis(C7) = Uanis(C8)
Uanis(C56) = Uanis(C57) = Uanis(C53) = Uanis(C36) = Uanis(C39) = Uanis(C40) =
Uanis(C23) = Uanis(C22) = Uanis(C19) = Uanis(C2) = Uanis(C5) = Uanis(C6)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C14(H14), C29(H29), C31(H31), C46(H46), C48(H48), C63(H63), C65(H65)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C13(H13a,H13b), C28(H28a,H28b), C30(H30a,H30b), C45(H45a,
 H45b), C47(H47a,H47b), C62(H62a,H62b), C64(H64a,H64b)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C18(H18), C20(H20), C21(H21),
 C24(H24), C25(H25), C35(H35), C37(H37), C38(H38), C41(H41), C42(H42), C52(H52),
  C54(H54), C55(H55), C58(H58), C59(H59)
5.d Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C33(H33a,H33b,H33c), C34(H34a,H34b,
 H34c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C67(H67a,H67b,H67c), C68(H68a,
 H68b,H68c)
;
_platon_squeeze_special_details
;
A solvent mask was calculated and 94 electrons were 
found in a volume of 410\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2 ethanol, 1 dichloromethane per formula unit 
which account for 94 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_exptl_crystal_mounting_method 'on loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'