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_7713161
_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 H36 Cl Os P'
_chemical_formula_sum            'C32 H36 Cl Os P'
_chemical_formula_weight         677.23
_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)
;
_audit_update_record
;
2023-01-23 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.834(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9540(9)
_cell_length_b                   12.9968(12)
_cell_length_c                   20.6140(18)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.62
_cell_volume                     2610.2(4)
_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      100.15
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.955
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16619
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         26.059
_diffrn_reflns_theta_min         1.913
_diffrn_source                   'ALBA XALOC beamline'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.394
_exptl_absorpt_correction_T_max  0.6397
_exptl_absorpt_correction_T_min  0.4658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1647 before and 0.1297 after correction.
The Ratio of minimum to maximum transmission is 0.7282.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.269
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.389
_refine_ls_extinction_coef       0.0196(12)
_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   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0727
_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^)+(0.1701P)^2^+7.6621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.1947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4496
_reflns_number_total             4560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00743j2.cif
_cod_data_source_block           djh8_alba_apex_0m
_cod_database_code               7713161
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.412
_shelx_estimated_absorpt_t_min   0.294
_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. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3) = Uanis(C2)
3. Others
 Sof(H30A)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(H30)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C30(H30), C30(H30A), C27(H27), C8(H8)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C4(H4), C16(H16), C15(H15), C26(H26), C6(H6), C23(H23),
 C22(H22), C7(H7), C3(H3), C25(H25)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C28(H28A,H28B,
 H28C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C32A(H32A,H32B,H32C), C32B(H32D,
 H32E,H32F)
;
_shelx_res_checksum              58887
_olex2_submission_special_instructions 'No special instructions were received'