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_7713168
_publ_section_title
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 Cytotoxicity of osmium(II) and cycloosmated half-sandwich complexes from
 1-pyrenyl-containing phosphane ligands
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00743J
_journal_year                    2023
_chemical_formula_moiety         '2(C40 H38 O P Ru S), 2(F6 P), 2(CH2Cl2)'
_chemical_formula_sum            'C82 H80 Cl4 F12 O2 P4 Ru2 S2'
_chemical_formula_weight         1857.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
;
2023-01-23 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.729(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.070(4)
_cell_length_b                   15.561(2)
_cell_length_c                   19.320(3)
_cell_measurement_reflns_used    8167
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.75
_cell_measurement_theta_min      2.29
_cell_volume                     8232(2)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72931
_diffrn_reflns_av_R_equivalents  0.1448
_diffrn_reflns_av_unetI/netI     0.1345
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62684
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.622
_diffrn_reflns_theta_max         23.622
_diffrn_reflns_theta_min         0.763
_diffrn_source                   'ALBA XALOC beamline'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1602 before and 0.1002 after correction.
The Ratio of minimum to maximum transmission is 0.7015.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.382
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0044(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         11422
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.1179
_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^)+(0.1579P)^2^+87.9289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2948
_refine_ls_wR_factor_ref         0.3069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9237
_reflns_number_total             11422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00743j2.cif
_cod_data_source_block           djh7_alba_apex_0m
_cod_original_formula_sum        'C82 H80 F12 O2 P4 Ru2 S2 Cl4'
_cod_database_code               7713168
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.864
_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. Rigid bond restraints
 F1A, F1B, F2A, F2B, F3A, F3B, F4A, F4B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 F5A, F5B, F6A, F6B, F7A, F7B, F8A, F8B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C54, C55, C56
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
3. Uiso/Uaniso restraints and constraints
F1A \\sim F1B \\sim F2A \\sim F2B \\sim F3A \\sim F3B \\sim F4A \\sim F4B:
within 2A with sigma of 0.012 and sigma for terminal atoms of 0.024 within 2A
F5A \\sim F5B \\sim F6A \\sim F6B \\sim F7A \\sim F7B \\sim F8A \\sim F8B:
within 2A with sigma of 0.012 and sigma for terminal atoms of 0.024 within 2A
C54 \\sim C55 \\sim C56: within 2A with sigma of 0.012 and sigma for terminal
atoms of 0.024 within 2A
Uanis(P4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F12) = Uanis(F11)
4. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=FVAR(1)
 Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(F8B)=1-FVAR(2)
 Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C48(H48)
5.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C32(H32), C7(H7), C12(H12), C52(H52), C4(H4), C3(H3), C6(H6),
 C35(H35), C78(H78), C37(H37), C47(H47), C18(H18), C38(H38), C31(H31), C28(H28),
  C19(H19), C77(H77), C36(H36), C74(H74), C26(H26), C61(H61), C62(H62),
 C34(H34), C21(H21), C30(H30), C76(H76), C44(H44), C68(H68), C72(H72), C75(H75),
  C43(H43), C29(H29), C22(H22), C24(H24), C25(H25), C54(H54), C69(H69),
 C65(H65), C71(H71), C66(H66), C70(H70), C56(H56), C55(H55)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C41(H41A,H41B,H41C), C79(H79A,H79B,H79C), C40(H40A,H40B,
 H40C), C49(H49A,H49B,H49C), C39(H39A,H39B,H39C), C80(H80A,H80B,H80C), C10(H10A,
 H10B,H10C), C1(H1A,H1B,H1C), C50(H50A,H50B,H50C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 302 electrons were 
found in a volume of 1480 A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2[CH2Cl2] per Formula Unit 
which account for 336 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26703
_shelx_fab_checksum              67838
_olex2_submission_special_instructions 'No special instructions were received'