Highly covalent metal-ligand π bonding in chelated bis- and tris(iminoxolene) complexes of osmium and ruthenium.
Gianino, Jacqueline; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7015–7027; doi:10.1039/d0dt01287d

data_7704223
_publ_section_title
;
 Highly covalent metal-ligand \p bonding in chelated bis- and
 tris(iminoxolene) complexes of osmium and ruthenium.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7015
_journal_page_last               7027
_journal_paper_doi               10.1039/d0dt01287d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C50 H58 N4 O2 Os'
_chemical_formula_sum            'C50 H58 N4 O2 Os'
_chemical_formula_weight         937.20
_chemical_name_common            (Clip)Os(py)2
_chemical_name_systematic
2,2'-Biphenylbis((2-oxy-3,5-di-tert-butylphenyl)amido)-bis(pyridine)osmium(IV)
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-04-02 deposited with the CCDC.	2020-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.10(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.870(7)
_cell_length_b                   23.816(19)
_cell_length_c                   19.126(14)
_cell_measurement_reflns_used    9021
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.162
_cell_measurement_theta_min      2.492
_cell_volume                     4496(6)
_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 0.997
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            80737
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         1.710
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.879
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6282
_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            teal
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_recrystallization_method
'Crystals were grown by vapor diffusion of acetonitrileinto a solution of the compound in benzene.'
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.074
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6282
_refine_diff_density_max         8.846
_refine_diff_density_min         -2.047
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         11154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0490P)^2^+54.7625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9598
_reflns_number_total             11154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01287d2.cif
_cod_data_source_block           clipospy
_cod_depositor_comments
'Adding full bibliography for 7704222--7704225.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7704223
_shelx_estimated_absorpt_t_min   0.470
_shelx_estimated_absorpt_t_max   0.815
_shelxl_version_number           2013-4
_shelx_res_checksum              50719