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_7124564
_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 Ru'
_chemical_formula_sum            'C56 H76 N2 O6 Ru'
_chemical_formula_weight         974.25
_chemical_name_common            (DOPO)2Ru
_chemical_name_systematic
; 
 Bis(2,4,6,8-tetra-tert-butyl-1,9-dioxophenoxazinato)ruthenium
;
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.575(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3495(11)
_cell_length_b                   19.7245(11)
_cell_length_c                   12.9833(7)
_cell_measurement_reflns_used    9057
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.21
_cell_measurement_theta_min      2.59
_cell_volume                     5211.0(5)
_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 0.999
_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  0.0853
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            149553
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.271
_diffrn_reflns_theta_min         1.438
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_correction_T_min  0.9168
_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/black'
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             2072
_exptl_crystal_recrystallization_method
;
Slow evaporation from deuteriochloroform 
;
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+4.6873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8809
_reflns_number_total             11697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03404j2.cif
_cod_data_source_block           rudopo2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7124564
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2013-4
_shelx_res_checksum              7907