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_7704224
_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         'C63 H78 N4 O3 Os'
_chemical_formula_sum            'C63 H78 N4 O3 Os'
_chemical_formula_weight         1129.49
_chemical_name_common            (MeClamp)Os
_chemical_name_systematic
;
 [Tris(2-(3',5'-di-tert-butyl-2'-oxyphenyl)amido-4-
methylphenyl)amine]osmium(VI)
;
_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   difmap
_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                 92.9257(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2048(11)
_cell_length_b                   28.050(3)
_cell_length_c                   17.3586(16)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      56.522
_cell_measurement_theta_min      4.919
_cell_volume                     5934.9(10)
_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 1.000
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            159593
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         1.381
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.189
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7157
_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    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_recrystallization_method
;
 Crystals were grown by diffusion of acetonitrile into
a dichloromethane solution of the complex.
;
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.108
_exptl_transmission_factor_max   0.8621
_exptl_transmission_factor_min   0.7157
_refine_diff_density_max         1.685
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         14762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0289P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11650
_reflns_number_total             14762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01287d2.cif
_cod_data_source_block           meclampos
_cod_depositor_comments
'Adding full bibliography for 7704222--7704225.cif.'
_cod_original_cell_volume        5934.9(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7704224
_shelx_estimated_absorpt_t_min   0.7157
_shelx_estimated_absorpt_t_max   0.8621
_shelxl_version_number           2013-4
_shelx_res_checksum              80755