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_4085631
_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         'C48 H46 N5 O2 Os P, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H50 Cl4 N5 O2 Os P'
_chemical_formula_weight         1115.92
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_am39
_audit_creation_date
;
'Thu May 15 14:22:59 2014'
;
_audit_update_record             'Thu May 15 14:41:42 CEST 2014'
_cell_angle_alpha                90
_cell_angle_beta                 101.5353(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.46720(8)
_cell_length_b                   21.53543(15)
_cell_length_c                   21.50542(18)
_cell_measurement_reflns_used    117337
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.7970
_cell_measurement_theta_min      3.6800
_cell_volume                     4749.74(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); 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      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega  -35.00   -1.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -79.0000  -81.9526 68

  2 omega   10.00   50.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -79.0000  -81.9526 80

  3 omega  -46.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  172.6369 194

  4 omega  -33.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000 -125.1642 168

  5 omega  -39.00    3.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  115.7085 84

  6 omega   26.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  115.7085 50

  7 omega  -11.00   66.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000 -150.0000 154

  8 omega   -6.00   63.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000  -30.0000 138

  9 omega   -3.00   88.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000  120.0000 182

 10 omega  -50.00   -6.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000  -30.0000 88

 11 omega   51.00   77.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000   30.0000 52

 12 omega   23.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000  -60.0000 52

 13 omega    5.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000   84.2703 92

 14 omega   -6.00   43.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   38.0000   90.0000 98

 15 omega   12.00   38.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000    0.0000 52

 16 omega   -4.00   91.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   38.0000  -60.0000 190

 17 omega   23.00   48.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000  -30.0000 50

 18 omega  -44.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000   28.2512 190

 19 omega   -3.00   88.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000  120.0000 182

 20 omega   -7.00   91.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   38.0000    0.0000 196

 21 omega  -46.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000 -125.1642 194

 22 omega  -50.00   40.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -57.0000  -30.0000 180

 23 omega   -3.00   88.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000  -90.0000 182

 24 omega   -3.00   88.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   57.0000   30.0000 182

 25 omega  -46.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  115.7085 194

 26 omega  -51.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000    0.0000 200

 27 omega  -11.00   89.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505   77.0000 -120.0000 200

 28 omega  -46.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000   28.2512 194

 29 omega  -46.00   51.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -80.0000  172.6369 194

 30 omega  -47.00   50.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -79.0000  -81.9526 194

 31 omega  -51.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000  -60.0000 200

 32 omega  -51.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505  -77.0000   60.0000 200

 33 omega  -54.00   92.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000  120.0000 292

 34 omega  -54.00   92.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000  240.0000 292

 35 phi      0.00  120.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

 36 phi      0.00  120.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -20.0000     -     240

 37 phi      0.00  120.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   20.0000     -     240

 38 phi      0.00  120.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -40.0000     -     240

 39 phi      0.00  120.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   40.0000     -     240

 40 phi      0.00  120.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505  -60.0000     -     240

 41 phi      0.00  120.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  18.8505   18.8505   60.0000     -     240

 42 phi    120.00  240.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.8505    0.0000     -     240

 43 omega  -54.00   92.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8505    0.0000    0.0000 292

;
_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      0.0331514000
_diffrn_orient_matrix_UB_12      0.0118436000
_diffrn_orient_matrix_UB_13      -0.0231953000
_diffrn_orient_matrix_UB_21      -0.0471010000
_diffrn_orient_matrix_UB_22      0.0239574000
_diffrn_orient_matrix_UB_23      -0.0072447000
_diffrn_orient_matrix_UB_31      0.0382542000
_diffrn_orient_matrix_UB_32      0.0192387000
_diffrn_orient_matrix_UB_33      0.0233096000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            357038
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.122
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.1809
_exptl_crystal_size_mid          0.1493
_exptl_crystal_size_min          0.0964
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         12503
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+11.3385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11931
_reflns_number_total             12503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00080_si_002.cif
_cod_data_source_block           ga_am39
_cod_depositor_comments
'Adding full bibliography for 4085628--4085631.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4085631
_audit_block_refno               2041
_audit_block_usercomment         'AM569, irregular, red'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C50 H50 Cl4 N5 O2 Os1 P1'
_chemical_oxdiff_usercomment     'AM569, irregular, red'
_shelx_estimated_absorpt_t_max   0.754
_shelx_estimated_absorpt_t_min   0.754
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C15A \\sim C14-C15B \\sim C14-C16A \\sim C14-C16B \\sim C14-C17A \\sim
C14-C17B
 with sigma of 0.02
 C15A-C16A \\sim C15A-C17A \\sim C16A-C17A \\sim C15B-C16B \\sim C15B-C17B
\\sim C16B-C17B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15A \\sim C16A \\sim C17A \\sim C15B \\sim C16B \\sim C17B: within 1.3A with
sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq,
Uanis(C15B) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C17B) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C51(H51A,H51B)
6.b Me refined with riding coordinates:
 C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C15B(H15D,
 H15E,H15F), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13(H13), C19(H19), C21(H21), C22(H22),
 C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
6.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              94355
_cell_oxdiff_length_a            10.46825(9)
_cell_oxdiff_length_b            21.53991(17)
_cell_oxdiff_length_c            21.4957(2)
_cell_oxdiff_angle_alpha         90.0078(7)
_cell_oxdiff_angle_beta          101.4946(8)
_cell_oxdiff_angle_gamma         90.0027(7)
_cell_oxdiff_volume              4749.74(7)
_cell_oxdiff_measurement_reflns_used 117337