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_7713163
_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         'C38 H32 I2 Os P, C H2 Cl2'
_chemical_formula_sum            'C39 H34 Cl2 I2 Os P'
_chemical_formula_weight         1048.53
_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             2022-12-28
_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                88.816(6)
_cell_angle_beta                 76.115(5)
_cell_angle_gamma                73.322(6)
_cell_formula_units_Z            2
_cell_length_a                   9.1684(11)
_cell_length_b                   13.9992(15)
_cell_length_c                   14.6343(16)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      3.04
_cell_volume                     1744.4(3)
_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 0.984
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30291
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.646
_diffrn_reflns_theta_min         2.036
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.652
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1486 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.7506.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_description       plate
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7978
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+4.3743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6959
_reflns_number_total             7978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00743j2.cif
_cod_data_source_block           2009djs31_0m
_cod_database_code               7713163
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-Cl1B
 1.7 with sigma of 0.01
 C39-Cl1A
 1.7 with sigma of 0.01
3. Rigid bond restraints
 Cl1A, C39
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C8, C30A, C31B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4. Uiso/Uaniso restraints and constraints
Cl1A \\sim C39: within 2A with sigma of 0.012 and sigma for terminal atoms of
0.024 within 2A
C8 \\sim C30A \\sim C31B: within 2A with sigma of 0.012 and sigma for terminal
atoms of 0.024 within 2A
5. Others
 Sof(Cl1B)=Sof(H39C)=Sof(H39D)=1-FVAR(1)
 Sof(Cl1A)=Sof(H39A)=Sof(H39B)=FVAR(1)
 Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=1-FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39(H39C,H39D)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C21(H21), C24(H24), C15(H15), C12(H12), C38(H38), C16(H16),
 C3(H3), C18(H18), C20(H20), C25(H25), C29(H29), C4(H4), C19(H19), C14(H14),
 C13(H13), C37(H37), C30(H30), C22(H22), C33(H33), C35(H35), C34(H34)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C31A(H31A,H31B,H31C), C30A(H30A,H30B,H30C), C31B(H31D,H31E,
 H31F), C30B(H30D,H30E,H30F)
;
_shelx_res_checksum              42682
_olex2_submission_special_instructions 'No special instructions were received'