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_7710570
_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            Os1-Et
_chemical_name_systematic        tetrakis(2-ethylphenyl)osmium(IV)
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-28 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7666(3)
_cell_length_b                   15.7666(3)
_cell_length_c                   10.3145(2)
_cell_measurement_reflns_used    7582
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      33.4340
_cell_measurement_theta_min      3.4770
_cell_volume                     2564.04(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -7.00  22.00   0.50    1.10    --   -9.49 -99.00   0.00   58
  2  \w     -7.00  22.00   0.50    1.10    --   -9.49 -99.00 120.00   58
  3  \w    -61.00 -27.00   0.50    1.10    --   10.12 -38.00  60.00   68
  4  \w    -25.00  11.00   0.50    1.10    --   -9.49 -77.00   0.00   72
  5  \w    -17.00  64.00   0.50    1.10    --   -9.49  26.00-125.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0109823000
_diffrn_orient_matrix_UB_12      0.0414512000
_diffrn_orient_matrix_UB_13      -0.0207256000
_diffrn_orient_matrix_UB_21      0.0424218000
_diffrn_orient_matrix_UB_22      0.0134136000
_diffrn_orient_matrix_UB_23      0.0102135000
_diffrn_orient_matrix_UB_31      0.0101891000
_diffrn_orient_matrix_UB_32      -0.0111916000
_diffrn_orient_matrix_UB_33      -0.0647757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.857
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.991
_exptl_absorpt_correction_T_max  0.419
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         2114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0097P)^2^+4.2545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1863
_reflns_number_total             2114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01706g2.cif
_cod_data_source_block           C32H36Os_CCDC1
_cod_original_cell_volume        2564.04(11)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7710570
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         OsC12H24
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.380
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              52445
_shelx_hkl_checksum              61095
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.652