Bis(pyridylimino)isoindolato (BPI) Osmium Complexes: Structural Chemistry and Reactivity
Müller, Astrid L.; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 34 (2015) 2810–; doi:10.1021/acs.organomet.5b00080

data_4085628
_publ_section_title
;
 Bis(pyridylimino)isoindolato (BPI) Osmium Complexes: Structural Chemistry
 and Reactivity
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2810
_journal_paper_doi               10.1021/acs.organomet.5b00080
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C64 H62 N7 Os P2, F6 P'
_chemical_formula_sum            'C72 H78 F6 N7 O2 Os P3'
_chemical_formula_weight         1470.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_am30a
_audit_creation_date
;
'Mon Feb 17 12:35:28 2014'
;
_audit_update_record             'Mon Feb 17 12:56:47 CET 2014'
_cell_angle_alpha                80.260(3)
_cell_angle_beta                 87.686(3)
_cell_angle_gamma                81.116(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2862(4)
_cell_length_b                   13.6767(4)
_cell_length_c                   21.7263(7)
_cell_measurement_reflns_used    11535
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      69.2300
_cell_measurement_theta_min      3.9860
_cell_volume                     3265.28(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega   -7.00   20.20   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 34

  2 omega  -68.00  -21.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 58

  3 omega  -15.00   25.00   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   60.0000 50

  4 omega   26.00   55.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 37

  5 omega  -71.00  -19.00   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   60.0000 65

  6 omega   54.00   78.80   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  -60.0000 31

  7 omega   67.00   99.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   60.0000 40

  8 omega   48.00   75.20   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -79.0000  134.2197 34

  9 omega   92.00  120.80   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -60.0000 36

 10 omega   34.00  122.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 110

 11 omega  -17.00   85.40   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000   51.6002 128

 12 omega   75.00  122.20   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 59

 13 omega   -2.00   49.20   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 64

 14 omega  -13.00   14.20   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -79.0000  134.2197 34

 15 omega  -10.00   74.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -120.0000 105

 16 omega   36.00   78.40   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 53

 17 omega   42.00   86.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 56

 18 omega   41.00  107.40   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   90.3850 83

 19 omega   87.00  149.40   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 78

 20 omega   58.00   89.20   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   30.0000 39

 21 phi    240.00  353.60   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
  40.0000  108.0000    0.0000     -     142

 22 omega   38.00  101.20   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -58.1707 79

 23 omega   67.00  106.20   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -112.4303 49

 24 omega   47.00   99.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   49.2588 65

 25 omega   45.00   83.40   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -30.0000 48

 26 omega   37.00   92.20   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  150.0000 69

 27 omega   35.00   85.40   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 63

 28 omega   37.00   91.40   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   90.0000 68

 29 omega   48.00  138.40   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  148.4241 113

 30 omega   99.00  143.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 55

 31 omega   41.00   69.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  120.0000 35

 32 omega   68.00  104.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -15.2676 46

 33 omega   46.00   89.20   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -78.0000 -146.0943 54

 34 omega  -21.00   67.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   90.0000 111

 35 phi    240.00  360.00   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
 -40.0000    0.0000    0.0000     -     150

 36 omega  -30.00   70.00   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -30.0000 125

 37 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 125

 38 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 125

 39 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 125

 40 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 125

 41 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 125

 42 omega  -15.00   73.80   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -90.0000 111

 43 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 125

 44 omega   33.00  121.80   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 111

 45 omega  -15.00   73.80   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  150.0000 111

 46 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 125

 47 omega   82.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 120

 48 omega   74.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000   60.0000 130

 49 omega   37.00  138.60   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  148.4241 127

 50 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 125

 51 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 125

 52 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 125

 53 omega   38.00  102.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -30.0000 81

 54 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 125

 55 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 125

 56 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 125

 57 omega   82.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 120

 58 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 125

 59 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 125

 60 phi    120.00  240.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
 108.0000  108.0000   40.0000     -     150

 61 omega  -69.00   19.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -150.0000 111

 62 omega  -69.00   19.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 111

 63 omega  -26.00   70.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 121

 64 omega  -16.00   84.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000    0.0000 125

 65 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 125

 66 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 125

 67 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 125

 68 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 125

 69 omega  -16.00   84.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -150.0000 125

 70 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 125

 71 omega  -15.00   73.80   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   30.0000 111

 72 omega   24.00  124.00   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 125

 73 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 125

 74 omega   37.00  138.60   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -29.1519 127

 75 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 125

 76 omega   85.00  173.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 111

 77 omega   85.00  173.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 111

 78 omega   83.00  175.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   69.0000   75.1014 115

 79 omega   84.00  176.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   67.0000  170.4499 115

 80 omega   87.00  175.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   51.2094 111

 81 omega   85.00  173.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 111

 82 omega   82.00  175.60   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   70.0000   -4.2420 117

 83 omega   82.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   36.0000 -123.7325 120

 84 omega   81.00  177.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000   24.0664 120

 85 omega   82.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 120

 86 omega   85.00  173.80   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 111

 87 omega   78.00  178.00   0.8000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 125

 88 omega  -73.00   71.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  120.0000 181

 89 omega  -69.00   19.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -90.0000 111

 90 omega  -73.00   71.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000    0.0000 181

 91 omega   33.00   56.20   0.8000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 29

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0753857000
_diffrn_orient_matrix_UB_12      0.0194663000
_diffrn_orient_matrix_UB_13      -0.0603055000
_diffrn_orient_matrix_UB_21      -0.1086412000
_diffrn_orient_matrix_UB_22      -0.0064175000
_diffrn_orient_matrix_UB_23      -0.0390486000
_diffrn_orient_matrix_UB_31      -0.0400713000
_diffrn_orient_matrix_UB_32      0.1137627000
_diffrn_orient_matrix_UB_33      -0.0039514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1500
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            99072
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.769
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.960
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       plate
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.1868
_exptl_crystal_size_mid          0.1160
_exptl_crystal_size_min          0.0266
_refine_diff_density_max         2.067
_refine_diff_density_min         -2.738
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         12232
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+1.8794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9307
_reflns_number_total             12232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00080_si_002.cif
_cod_data_source_block           ga_am30a_sq
_cod_depositor_comments
'Adding full bibliography for 4085628--4085631.cif.'
_cod_original_cell_volume        3265.3(2)
_cod_database_code               4085628
_audit_block_refno               1967
_audit_block_usercomment         'AM589 yellow plate'
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.637
_shelx_estimated_absorpt_t_min   0.637
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P3-F1 \\sim P3-F2 \\sim P3-F3 \\sim P3-F6 \\sim P3-F4 \\sim P3-F5
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F1-F5 \\sim F2-F3 \\sim F2-F5 \\sim F2-F6
\\sim F3-F4 \\sim F3-F6 \\sim F4-F5
 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13(H13), C19(H19), C21(H21), C22(H22),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38),
  C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              12914
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_cell_oxdiff_length_a            11.2862(4)
_cell_oxdiff_length_b            13.6767(4)
_cell_oxdiff_length_c            21.7263(7)
_cell_oxdiff_angle_alpha         80.260(3)
_cell_oxdiff_angle_beta          87.686(3)
_cell_oxdiff_angle_gamma         81.116(3)
_cell_oxdiff_volume              3265.27(19)
_cell_oxdiff_measurement_reflns_used 11535
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1