Pushing steric limits in osmium(IV) tetraaryl complexes
Parr, Joseph Michael; Olivar, Clarissa; Saal, Thomas; Haiges, Ralf; Inkpen , Michael Stephen; Dalton Transactions  (2022) –; doi:10.1039/D2DT01706G

data_7710569
_publ_section_title
;
 Pushing steric limits in osmium(IV) tetraaryl complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01706G
_journal_year                    2022
_chemical_formula_moiety         'C32 H36 Os'
_chemical_formula_sum            'C32 H36 Os'
_chemical_formula_weight         610.81
_chemical_name_common            Os(2,5-xylyl)4
_chemical_name_systematic        tetrakis(2,5-dimethylphenyl)osmium(IV)
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2020-08-19 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.736(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9059(19)
_cell_length_b                   12.9355(18)
_cell_length_c                   15.837(2)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.5925
_cell_measurement_theta_min      2.4679
_cell_volume                     2613.2(6)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS, 2019)'
_computing_data_collection
'Bruker Instrument Service v2013.12.0.0 (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS, 2013)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'
_computing_structure_refinement  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32067
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    4.897
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.535
_refine_ls_abs_structure_details
;

Flack x determined using 3368 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         7862
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0012P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0416
_reflns_number_gt                7265
_reflns_number_total             7862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01706g2.cif
_cod_data_source_block           C32H36Os
_cod_original_cell_volume        2613.2(7)
_cod_database_code               7710569
_shelx_res_checksum              63131
_shelx_hkl_checksum              10962