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_7124562
_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 H76 N2 O6 Os'
_chemical_formula_sum            'C56 H76 N2 O6 Os'
_chemical_formula_weight         1063.38
_chemical_name_common            Os(DOPO)2
_chemical_name_systematic
;
 Bis(2,4,6,8-tetra-tert-butyl-1,9-dioxophenoxazinato)osmium
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.3740(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4119(19)
_cell_length_b                   19.7938(19)
_cell_length_c                   13.0487(12)
_cell_measurement_reflns_used    8028
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.401
_cell_measurement_theta_min      2.583
_cell_volume                     5271.9(9)
_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 0.998
_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  0.0739
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            117301
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.181
_diffrn_reflns_theta_min         1.433
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.468
_exptl_absorpt_correction_T_max  0.9046
_exptl_absorpt_correction_T_min  0.8324
_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    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             2200
_exptl_crystal_recrystallization_method
;
 Liquid-liquid diffusion of acetonitrile into CHCl3.
;
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         10557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0249P)^2^+2.9315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9028
_reflns_number_total             10557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03404j2.cif
_cod_data_source_block           osdopo
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7124562
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.715
_shelxl_version_number           2013-4
_shelx_res_checksum              73358