Octahedral to trigonal prismatic distortion driven by subjacent orbital π antibonding interactions and modulated by ligand redox noninnocence.
Cipressi, Jacqueline; Brown, Seth N.; Chemical communications (Cambridge, England) 50 (2014) 7956–7959; doi:10.1039/c4cc03404j

data_7124563
_publ_section_title
;
 Octahedral to trigonal prismatic distortion driven by subjacent orbital
 \p antibonding interactions and modulated by ligand redox noninnocence.
;
_journal_issue                   59
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7956
_journal_page_last               7959
_journal_paper_doi               10.1039/c4cc03404j
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C56 H80 N2 O4 Os, 2 (C H Cl3)'
_chemical_formula_sum            'C58 H82 Cl6 N2 O4 Os'
_chemical_formula_weight         1274.15
_chemical_name_common            'Os(ONO)2 . 2 CHCl3'
_chemical_name_systematic
;
 Bis[bis(3,5-di-tert-butyl-2-oxyphenyl)amido]osmium  
dichloroform solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.211(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   59.4673(19)
_cell_length_b                   21.5249(6)
_cell_length_c                   19.0986(5)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.711
_cell_measurement_theta_min      4.108
_cell_volume                     24345.7(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       73
_diffrn_reflns_limit_h_min       -72
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            238998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.868
_diffrn_reflns_theta_min         1.492
_diffrn_source                   'micro-focus source'
_exptl_absorpt_coefficient_mu    6.721
_exptl_absorpt_correction_T_max  0.9710
_exptl_absorpt_correction_T_min  0.5099
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. 
Madison, WI USA.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade-like
_exptl_crystal_F_000             10464
_exptl_crystal_recrystallization_method
;
 Vapor diffusion of acetonitrile into CHCl3.
;
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.018
_platon_squeeze_details
;
;
_refine_diff_density_max         2.726
_refine_diff_density_min         -3.901
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         23772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0580P)^2^+446.6057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20325
_reflns_number_total             23772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03404j2.cif
_cod_data_source_block           osono2_sqz
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7124563
_shelx_estimated_absorpt_t_min   0.411
_shelx_estimated_absorpt_t_max   0.889
_shelxl_version_number           2013-4
_shelx_res_checksum              74709