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_7716619
_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'
_chemical_formula_sum            'C40 H34 Cl2 N4 O6 Re2'
_chemical_formula_weight         1110.058
_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'
_symmetry_Int_Tables_number      19
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8365(2)
_cell_length_b                   16.5716(4)
_cell_length_c                   17.2135(3)
_cell_measurement_reflns_used    77055
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      2.26
_cell_volume                     3946.93(13)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.9975
_diffrn_measured_fraction_theta_max 0.9035
_diffrn_measurement_details
;
 761 frames, detector distance = 85 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 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.9975
_diffrn_reflns_Laue_measured_fraction_max 0.9035
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            73035
_diffrn_reflns_point_group_measured_fraction_full 0.9983
_diffrn_reflns_point_group_measured_fraction_max 0.8692
_diffrn_reflns_theta_full        19.6637
_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         2.26
_diffrn_source                   'Axo Ag'
_diffrn_source_current           0.670
_diffrn_source_power             0.044
_diffrn_source_voltage           65
_exptl_absorpt_coefficient_mu    3.390
_exptl_absorpt_correction_T_max  0.5231
_exptl_absorpt_correction_T_min  0.1481
_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    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2135.501
_exptl_crystal_recrystallization_method
'crystallized by layering of methanol and petroleum ether'
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.363
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.4842
_refine_diff_density_min         -1.2046
_refine_diff_density_rms         0.1987
_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   -0.009(7)
_refine_ls_d_res_high            0.6270
_refine_ls_d_res_low             7.1087
_refine_ls_goodness_of_fit_ref   1.0282
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    59
_refine_ls_number_parameters     507
_refine_ls_number_reflns         14575
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.0279
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+1.3484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.828
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              26
_reflns_limit_k_min              -25
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                12012
_reflns_number_total             14575
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt01643b2.cif
_cod_data_source_block           ate515-d1-pe
_cod_depositor_comments
'Adding full bibliography for 7716611--7716619.cif.'
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7716619
_olex2_refinement_description
;
1. 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
2. Restrained distances
 Re1-Cl1 \\sim Re1-Cl1A
 with sigma of 0.02
 Re1-C35 \\sim Re1-C35A
 with sigma of 0.02
 O1-C35 \\sim O1A-C35A
 with sigma of 0.02
 Re1-O1 \\sim Re1-O1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C35) = Uanis(C35A)
Uanis(O1) = Uanis(O1A)
4. Others
 Sof(Cl1A)=Sof(O1A)=Sof(C35A)=1-FVAR(1)
 Sof(Cl1)=Sof(O1)=Sof(C35)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C14(H14), C29(H29), C31(H31)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C15(H15a,H15b), C28(H28a,H28b), C32(H32a,H32b)
5.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)
5.d Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C33(H33a,H33b,H33c), C34(H34a,H34b,
 H34c)
;
_olex2_exptl_crystal_mounting_method 'mounted on loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '85.0 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   7.0
_stoe_evaluation_integration_b   0.5
_stoe_evaluation_integration_ems 0.012
_stoe_evaluation_lana_bis_l_even_max 4
_stoe_evaluation_lana_bis_l_odd_max 1
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 86.7
_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 53.2
_stoe_evaluation_lana_max_2theta_desired 53.2
_stoe_evaluation_lana_mean_redundancy 4.0
_stoe_evaluation_lana_number_refls_after_or 58275
_stoe_evaluation_lana_number_refls_outliers 14760
_stoe_evaluation_lana_number_refls_total 73035
_stoe_evaluation_lana_number_refls_unique 14577
_stoe_evaluation_lana_number_refls_written 73035
_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 222
_stoe_evaluation_lana_table
;
2Theta           6.5   12.1   17.7   23.3   28.9   34.5   40.1   45.7   51.3
<Resolution>    4.20   2.60   1.80   1.38   1.12   0.94   0.82   0.73   0.66
N(total)         572   2145   4414   6261  10201  14263  16653  15301   3225
<Redundancy>     4.5    5.2    4.8    4.1    4.6    4.7    4.5    3.6    1.8
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0   96.5   45.1
<I/sigma>       96.9   59.9   43.8   31.0   17.9   10.4    5.5    3.0    1.7
R(int)         0.029  0.023  0.032  0.033  0.047  0.058  0.085  0.126  0.187
;
_stoe_measurement_identifier     ATE515-D1-PE
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '10.0 s'
_stoe_measurement_min_exposure_per_frame '10.0 s'
_stoe_measurement_total_exposure_time '2.1 h'
_stoe_measurement_total_frame_number 761
_stoe_measurement_total_run_number 16
_stoe_measurement_tube_power     '43.6 W'