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_7704222
_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         'C40 H48 Cl2 N2 O2 Os, C4 H8 O2'
_chemical_formula_sum            'C44 H56 Cl2 N2 O4 Os'
_chemical_formula_weight         938.00
_chemical_name_common            '(Clip)OsCl2 . EtOAc'
_chemical_name_systematic
'2,2'-biphenylenediamido-N,N'-bis(2-oxy-3,5-di-tertbutylphenyl)-dichloroosmium(VI) ethyl acetate solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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                 98.4471(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5267(6)
_cell_length_b                   10.3290(5)
_cell_length_c                   36.2615(19)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.27
_cell_volume                     4270.4(4)
_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 0.990
_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  0.0649
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            58745
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.596
_diffrn_reflns_theta_min         1.793
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.153
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_type   multi-scan
_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            purple
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_recrystallization_method
'Slow evaporation of a solution of the compound in a hexane/ethyl acetate mixture.'
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.084
_exptl_transmission_factor_max   0.8620
_exptl_transmission_factor_min   0.6783
_refine_diff_density_max         1.196
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         8851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0202P)^2^+6.5746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7202
_reflns_number_total             8851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01287d2.cif
_cod_data_source_block           cliposcl2
_cod_depositor_comments
'Adding full bibliography for 7704222--7704225.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7704222
_shelx_estimated_absorpt_t_min   0.6783
_shelx_estimated_absorpt_t_max   0.8620
_shelxl_version_number           2013-4
_shelx_res_checksum              63020