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_7713159
_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 Cl2 Os P'
_chemical_formula_sum            'C32 H37 Cl2 Os P'
_chemical_formula_weight         713.68
_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             2022-09-02
_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                68.196(2)
_cell_angle_beta                 85.911(2)
_cell_angle_gamma                72.520(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4570(5)
_cell_length_b                   12.5735(6)
_cell_length_c                   13.3284(7)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.74
_cell_volume                     1402.07(13)
_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 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16036
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.405
_diffrn_reflns_theta_min         3.255
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.815
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1392 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.4653.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.818
_refine_diff_density_min         -3.630
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0444P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5325
_reflns_number_total             5718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00743j2.cif
_cod_data_source_block           1955_djh1_dcmhex_0m
_cod_database_code               7713159
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.532
_shelx_estimated_absorpt_t_min   0.197
_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.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29), C25(H25), C16(H16), C11(H11), C26(H26), C15(H15), C8(H8),
 C12(H12), C14(H14), C7(H7), C3(H3), C2(H2)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C17(H17A,H17B,
 H17C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              37304
_olex2_submission_special_instructions 'No special instructions were received'