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_7716618
_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, 2[C2H6O]'
_chemical_formula_sum            'C44 H46 Cl2 N4 O8 Re2'
_chemical_formula_weight         1202.15
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2023-10-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-27 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                116.153(2)
_cell_angle_beta                 95.311(2)
_cell_angle_gamma                91.952(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0797(3)
_cell_length_b                   14.3295(3)
_cell_length_c                   14.5093(3)
_cell_measurement_reflns_used    104377
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      69.92
_cell_measurement_theta_min      3.61
_cell_volume                     2236.81(10)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
 6310 frames, detector distance = 60 mm
;
_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_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            64439
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.132
_diffrn_reflns_theta_min         5.079
_diffrn_source                   'Primux 100 micro'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.980
_exptl_absorpt_correction_T_max  0.4314
_exptl_absorpt_correction_T_min  0.2668
_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    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_recrystallization_method
'crystallized by diffusion of DCM, ethanol and petroleum ether'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.038
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         11433
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1359P)^2^+8.2332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1903
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                10649
_reflns_number_total             11433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01643b2.cif
_cod_data_source_block           dcm_etoh_pe
_cod_depositor_comments
'Adding full bibliography for 7716611--7716619.cif.'
_cod_original_cell_volume        2236.81(9)
_cod_database_code               7716618
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.352
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(2)
 0.17(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. Restrained distances
 C22-C23
 1.44 with sigma of 0.05
4. Rigid bond restraints
 C2, C3, C4, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N3, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C43, C44, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C60, C65, C66
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
N3 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
C60 \\sim C65 \\sim C66: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(C50) = Uanis(C51) = Uanis(C34) = Uanis(C30) = Uanis(C13) = Uanis(C17) =
Uanis(C68) = Uanis(C67)
Uanis(C74) = Uanis(C73) = Uanis(C71) = Uanis(C70)
Uanis(C8) = Uanis(C7) = Uanis(C4) = Uanis(C3) = Uanis(C20) = Uanis(C21) =
Uanis(C24) = Uanis(C25) = Uanis(C42) = Uanis(C41) = Uanis(C38) = Uanis(C37) =
Uanis(C54) = Uanis(C55) = Uanis(C58) = Uanis(C59)
6. Rigid body (RIGU) restrains
 N2, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7.a Everything fixed:
 H17A, H17B, H17C, H34A, H34B, H34C
7.b Ternary CH refined with riding coordinates:
 C12(H12), C14(H14), C29(H29), C31(H31), C46(H46), C48(H48), C63(H63), C65(H65)
7.c 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)
7.d 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), C41(H41), C42(H42), C35(H35), C37(H37), C38(H38), C52(H52),
  C54(H54), C55(H55), C58(H58), C59(H59)
7.e Fitted hexagon refined as free rotating group:
 N2(C1,C2,C3,C4,C5), C10(N1,C6,C7,C8,C9), N5(C40,C41,C42,C43,C44)
7.f Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 122 electrons were 
found in a volume of 454\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C2H6O] per Formula Unit 
which account for 104 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6898
_shelx_hkl_checksum              76083
_shelx_fab_checksum              59258
_olex2_exptl_crystal_mounting_method 'mounted on loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   10.0
_stoe_evaluation_integration_b   2.5
_stoe_evaluation_integration_ems 0.022
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 68.5
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 138.3
_stoe_evaluation_lana_max_2theta_desired 138.3
_stoe_evaluation_lana_mean_redundancy 4.9
_stoe_evaluation_lana_number_refls_after_or 55900
_stoe_evaluation_lana_number_refls_outliers 8576
_stoe_evaluation_lana_number_refls_total 64476
_stoe_evaluation_lana_number_refls_unique 11447
_stoe_evaluation_lana_number_refls_written 64476
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 1
_stoe_evaluation_lana_table
;
2Theta          13.3   28.1   42.9   57.7   72.5   87.3  102.1  116.9  131.7
<Resolution>    5.11   2.98   2.08   1.59   1.28   1.12   0.99   0.91   0.85
N(total)         237   1323   2927   4131  10876  14583  13450  11227   5722
<Redundancy>     2.0    2.3    2.4    2.2    4.5    6.4    6.9    6.2    4.7
Complet. [%%]    76.6   95.4   96.3   93.7   90.5   72.5   58.1   53.6   43.0
<I/sigma>      151.6   80.5   55.7   32.2   17.5   12.7    9.7    7.7    6.6
R(int)         0.023  0.019  0.022  0.027  0.030  0.034  0.041  0.052  0.056
;
_stoe_measurement_identifier     DCM_EtOH_PE
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_mean_exposure_per_frame '4.2 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '7.4 h'
_stoe_measurement_total_frame_number 6310
_stoe_measurement_total_run_number 99
_stoe_measurement_tube_power     '50.0 W'