Osmium(II) Tethered Half-Sandwich Complexes: pH-dependent Aqueous Speciation and Transfer Hydrogenation in Cells
Infante-Tadeo, Sonia; Rodriguez, Vanessa; Habtemariam, Abraha; Pizarro, Ana M.; Chemical Science  (2021) –; doi:10.1039/D1SC01939B

data_1563323
_publ_section_title
;
 Osmium(II) Tethered Half-Sandwich Complexes: pH-dependent Aqueous
 Speciation and Transfer Hydrogenation in Cells
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01939B
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_sum            'C16 H18 Cl N O3.25 Os'
_chemical_formula_weight         501.96
_chemical_name_common            SIT_105_150K
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2020-09-02 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.3794(4)
_cell_length_b                   12.3794(4)
_cell_length_c                   17.8331(6)
_cell_measurement_reflns_used    8402
_cell_measurement_temperature    150.(2)
_cell_measurement_theta_max      24.8210
_cell_measurement_theta_min      2.2165
_cell_volume                     2366.77(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27375
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    8.264
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear intense yellow'
_exptl_crystal_density_diffrn    2.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.987
_refine_diff_density_min         -1.076
_refine_ls_abs_structure_details
;

Flack x determined using 1076 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2888
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0712P)^2^+4.7048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                2695
_reflns_number_total             2888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01939b2.cif
_cod_data_source_block           10_02620
_cod_original_cell_volume        2366.77(17)
_cod_database_code               1563323
_shelx_res_checksum              94499
_shelx_hkl_checksum              70476