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_7716611
_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         'C34 H34 N4'
_chemical_formula_sum            'C34 H34 N4'
_chemical_formula_weight         498.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-18
_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                 100.364(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2640(9)
_cell_length_b                   6.1542(3)
_cell_length_c                   15.5298(10)
_cell_measurement_reflns_used    24622
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.72
_cell_measurement_theta_min      5.79
_cell_volume                     1341.02(14)
_computing_cell_refinement
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection
;
X-Area WinXpose 2.0.29.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_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 2.3, Darmstadt 2023
;
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
 810 frames, detector distance = 40 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2, 0.6 mm diameter'
_diffrn_radiation_monochromator  'multilayer optic'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18027
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.920
_diffrn_reflns_theta_min         2.893
_diffrn_source                   'Genix-Cu, 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.9670
_exptl_absorpt_correction_T_min  0.8266
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             532
_exptl_crystal_recrystallization_method 'mounted on loop with oil'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 1540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_coef       0.013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4606
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1065P)^2^+2.5021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.2388
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.918
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                3815
_reflns_number_total             4606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01643b2.cif
_cod_data_source_block           (-)-meta-l
_cod_depositor_comments
'Adding full bibliography for 7716611--7716619.cif.'
_cod_database_code               7716611
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.832
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C14(H14), C29(H29), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C28(H28A,H28B), C32(H32A,H32B)
2.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)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              57011
_shelx_hkl_checksum              7122
_olex2_exptl_crystal_mounting_method
'recrystallised from a mixture of chloroform and diethylether by solvent layering'
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.150 mm'
_stoe_detector_pixelsize_y       '0.150 mm'
_stoe_detector_size_x            '34.0 cm'
_stoe_detector_size_y            '34.0 cm'
_stoe_evaluation_integration_a   9.0
_stoe_evaluation_integration_b   0.0
_stoe_evaluation_integration_ems 0.026
_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 97.3
_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 135.9
_stoe_evaluation_lana_max_2theta_desired 135.9
_stoe_evaluation_lana_mean_redundancy 6.9
_stoe_evaluation_lana_number_refls_after_or 18033
_stoe_evaluation_lana_number_refls_outliers 7323
_stoe_evaluation_lana_number_refls_total 25356
_stoe_evaluation_lana_number_refls_unique 2611
_stoe_evaluation_lana_number_refls_written 18033
_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 2/m
_stoe_evaluation_lana_table
;
2Theta          12.4   27.0   41.6   56.2   70.8   85.4  100.0  114.6  129.2
<Resolution>    5.46   3.12   2.13   1.63   1.33   1.14   1.01   0.92   0.86
N(total)         194    990   2208   3073   4390   4854   4428   3398   1821
<Redundancy>     4.5    8.5    9.4    8.3    8.7    7.9    6.7    5.2    4.0
Complet. [%%]    84.6   98.7  100.0  100.0  100.0  100.0  100.0  100.0   83.9
<I/sigma>      266.6  277.1  182.3   80.3   44.3   38.3   19.6   10.0    1.8
R(int)         0.027  0.023  0.023  0.035  0.043  0.041  0.046  0.104  0.377
;
_stoe_measurement_identifier     (-)-Meta-L
_stoe_measurement_max_exposure_per_frame '60.0 s'
_stoe_measurement_mean_exposure_per_frame '60.0 s'
_stoe_measurement_min_exposure_per_frame '60.0 s'
_stoe_measurement_total_exposure_time '13.5 h'
_stoe_measurement_total_frame_number 810
_stoe_measurement_total_run_number 9
_stoe_measurement_tube_power     '30.0 W'