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_7713164
_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 H33 Cl2 Os P'
_chemical_formula_sum            'C38 H33 Cl2 Os P'
_chemical_formula_weight         781.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-01-10
_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                 94.909(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9947(5)
_cell_length_b                   13.9336(5)
_cell_length_c                   15.7966(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.92
_cell_volume                     3068.98(19)
_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      100.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27677
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.772
_diffrn_reflns_theta_min         2.504
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.408
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6159
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1240 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.8263.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         6509
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0140P)^2^+8.8241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5511
_reflns_number_total             6509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00743j2.cif
_cod_data_source_block           test
_cod_database_code               7713164
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.539
_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 planarity
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B
 with sigma of 0.1
 C23B, C24B, C25B, C26B, C27B, C28B, C29B, C30B, C31B, C32B, C33B, C34B, C35B,
 C36B, C37B, C38B
 with sigma of 0.1
3. Rigid bond restraints
 Os1B, Cl1B, Cl2B, P1B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Os1B \\sim Cl1B \\sim Cl2B \\sim P1B: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.016 within 2A
Uanis(Os1B) \\sim Ueq, Uanis(Cl1B) \\sim Ueq, Uanis(Cl2B) \\sim Ueq, Uanis(P1B)
\\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.012
5. Same fragment restrains
{C1, C2, C3, C4, C5, C6, C7, C8, C9, C10} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B}
{C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37,
C38} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23B, C24B, C25B, C26B, C27B, C28B, C29B, C30B, C31B, C32B, C33B, C34B, C35B,
C36B, C37B, C38B}
6. Others
 Sof(Os1B)=Sof(Cl1B)=Sof(Cl2B)=Sof(P1B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=
 Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=
 Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=
 Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11B)=Sof(C12B)=Sof(H12B)=
 Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=
 Sof(H16B)=Sof(C17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=
 Sof(H20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(C24B)=
 Sof(H24B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(C27B)=Sof(C28B)=Sof(C29B)=
 Sof(H29B)=Sof(C30B)=Sof(H30B)=Sof(C31B)=Sof(C32B)=Sof(C33B)=Sof(H33B)=
 Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(C37B)=Sof(H37B)=
 Sof(C38B)=Sof(H38B)=1-FVAR(1)
 Sof(Os1)=Sof(Cl1)=Sof(Cl2)=Sof(P1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(C18)=Sof(H18)=
 Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=
 Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(C27)=Sof(C28)=
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(C32)=Sof(C33)=Sof(H33)=
 Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(C37)=Sof(H37)=Sof(C38)=
 Sof(H38)=FVAR(1)
 Uiso(C1B)=Uiso(C2B)=Uiso(C3B)=Uiso(C4B)=Uiso(C5B)=Uiso(C6B)=Uiso(C7B)=
 Uiso(C8B)=Uiso(C9B)=Uiso(C10B)=Uiso(C11B)=Uiso(C12B)=Uiso(C13B)=Uiso(C14B)=
 Uiso(C15B)=Uiso(C16B)=Uiso(C17B)=Uiso(C18B)=Uiso(C19B)=Uiso(C20B)=Uiso(C21B)=
 Uiso(C22B)=Uiso(C23B)=Uiso(C24B)=Uiso(C25B)=Uiso(C26B)=Uiso(C27B)=Uiso(C28B)=
 Uiso(C29B)=Uiso(C30B)=Uiso(C31B)=Uiso(C32B)=Uiso(C33B)=Uiso(C34B)=Uiso(C35B)=
 Uiso(C36B)=Uiso(C37B)=Uiso(C38B)=FVAR(2)
7.a Riding coordinates:
 C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F)
7.b Ternary CH refined with riding coordinates:
 C8(H8), C8B(H8B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B), C12B(H12B), C13B(H13B), C14B(H14B),
 C15B(H15B), C16B(H16B), C18B(H18B), C19B(H19B), C20B(H20B), C21B(H21B),
 C22B(H22B), C24B(H24B), C25B(H25B), C29B(H29B), C30B(H30B), C33B(H33B),
 C34B(H34B), C35B(H35B), C37B(H37B), C38B(H38B)
7.d Fitted hexagon refined as free rotating group:
 C11B(C12B,C13B,C14B,C15B,C16B), C17B(C18B,C19B,C20B,C21B,C22B)
7.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C1B(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              9479
_olex2_submission_special_instructions 'No special instructions were received'