Cytotoxicity of osmium(II) and cycloosmated half-sandwich complexes from 1-pyrenyl-containing phosphane ligands
Josa, Dana; Aguilà, David; Fontava, Pere; Soto-Cerrato, Vanessa; Herrera-Ramírez, Piedad; Rafols, Laia; Grabulosa, Arnald; Gamez, Patrick; Dalton Transactions  (2023) –; doi:10.1039/D3DT00743J

data_7713160
_publ_section_title
;
 Cytotoxicity of osmium(II) and cycloosmated half-sandwich complexes from
 1-pyrenyl-containing phosphane ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00743J
_journal_year                    2023
_chemical_formula_moiety         'C32 H37 I2 Os P, 2(C H2 Cl2)'
_chemical_formula_sum            'C34 H41 Cl4 I2 Os P'
_chemical_formula_weight         1066.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-23 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                66.410(3)
_cell_angle_beta                 63.882(3)
_cell_angle_gamma                75.842(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4778(10)
_cell_length_b                   13.0153(10)
_cell_length_c                   13.4334(10)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.87
_cell_volume                     1788.9(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34316
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.780
_diffrn_reflns_theta_min         3.256
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.657
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1441 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.6153.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         9183
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+2.3855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8501
_reflns_number_total             9183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00743j2.cif
_cod_data_source_block           2003djs21_0m
_cod_database_code               7713160
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl8-Cl10
 2.9 with sigma of 0.04
 Cl5-Cl10
 2.9 with sigma of 0.04
 C34-Cl5 \\sim C34-Cl6 \\sim C34-Cl7 \\sim C34-Cl8 \\sim C34-Cl9 \\sim C34-Cl10
 with sigma of 0.02
 C33-Cl2 \\sim C33-Cl11 \\sim C33-Cl1 \\sim C33-Cl12 \\sim C33-Cl4 \\sim C33-Cl3
 with sigma of 0.02
3. Rigid bond restraints
 Cl2, Cl4, Cl3, Cl12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl4 \\sim Cl3 \\sim Cl12: within 2A with sigma of 0.008 and sigma for
terminal atoms of 0.016 within 2A
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(Cl7) \\sim Ueq, Uanis(Cl11)
\\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.02
5. Others
 1*[Sof(Cl1)+Sof(Cl4)]+1*[Sof(Cl2)+Sof(Cl3)]+1*[Sof(Cl12)+Sof(Cl11)]=1 with
 esd of 0.001
 1*[Sof(Cl5)+Sof(Cl8)]+1*[Sof(Cl7)+Sof(Cl10)]+1*[Sof(Cl6)+Sof(Cl9)]=1 with esd
 of 0.001
 Sof(Cl1)=Sof(Cl4)=FVAR(1)
 Sof(Cl2)=Sof(Cl3)=FVAR(2)
 Sof(Cl12)=Sof(Cl11)=FVAR(3)
 Sof(Cl5)=Sof(Cl8)=FVAR(4)
 Sof(Cl7)=Sof(Cl10)=FVAR(5)
 Sof(Cl6)=Sof(Cl9)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C8(H8)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C4(H4), C3(H3), C24(H24), C23(H23), C6(H6), C32(H32), C19(H19),
 C27(H27), C7(H7), C31(H31), C28(H28), C30(H30)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C), C13(H13A,H13B,
 H13C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              58779
_olex2_submission_special_instructions 'No special instructions were received'