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_7716612
_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         'C40 H34 Cl2 N4 O6 Re2, 1[CH2Cl2]'
_chemical_formula_sum            'C41 H36 Cl4 N4 O6 Re2'
_chemical_formula_weight         1194.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6887(2)
_cell_length_b                   15.7230(3)
_cell_length_c                   20.3145(3)
_cell_measurement_reflns_used    89301
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      3.55
_cell_volume                     4372.24(12)
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53947
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.536
_diffrn_reflns_theta_max         67.536
_diffrn_reflns_theta_min         3.555
_diffrn_source                   'Primux 100 micro'
_exptl_absorpt_coefficient_mu    13.319
_exptl_absorpt_correction_T_max  0.2354
_exptl_absorpt_correction_T_min  0.0761
_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    1.815
_exptl_crystal_description       needle
_exptl_crystal_F_000             2304
_exptl_crystal_preparation       'REflux under Ar'
_exptl_crystal_recrystallization_method
'vapour diffusion of Et2O into a DCM/EtOH 4/1 solution'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.451
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+19.2329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                6855
_reflns_number_total             7515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01643b2.cif
_cod_data_source_block           ate453
_cod_depositor_comments
'Adding full bibliography for 7716611--7716619.cif.'
_cod_database_code               7716612
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.502
_shelx_estimated_absorpt_t_min   0.166
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95(2)
 0.05(2)
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.a Ternary CH refined with riding coordinates:
 C12(H12), C14(H14), C29(H29), C31(H31)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C28(H28A,H28B), C32(H32A,H32B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C19(H19), C20(H20), C21(H21),
 C24(H24), C25(H25)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82185
_shelx_hkl_checksum              17875
_shelx_fab_checksum              92990
_olex2_exptl_crystal_mounting_method 'on loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'