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_4085630
_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         'C72 H69 N5 Os P2, 2(B F4)'
_chemical_formula_sum            'C73 H71 B2 Cl2 F8 N5 Os P2'
_chemical_formula_weight         1515.00
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_am37
_audit_creation_date             2014-05-05
_audit_update_record             'Mon May  5 18:25:34 CEST 2014'
_cell_angle_alpha                108.001(8)
_cell_angle_beta                 98.002(12)
_cell_angle_gamma                95.292(11)
_cell_formula_units_Z            2
_cell_length_a                   12.407(5)
_cell_length_b                   15.235(7)
_cell_length_c                   18.640(9)
_cell_measurement_reflns_used    8113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.95
_cell_measurement_theta_min      2.62
_cell_volume                     3284(3)
_computing_cell_refinement
;
SAINT 8.x (Bruker AXS, 1997-2012). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT 8.x (Bruker AXS, 1997-2011)'
_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      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            85212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.506
_diffrn_reflns_theta_min         1.167
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.447
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         22138
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0381P)^2^+2.0281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19425
_reflns_number_total             22138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00080_si_002.cif
_cod_data_source_block           ga_am37_sq
_cod_depositor_comments
'Adding full bibliography for 4085628--4085631.cif.'
_cod_database_code               4085630
_audit_block_refno               2026
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.768
_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
 C23-C24A \\sim C23-C24B \\sim C23-C25A \\sim C23-C25B \\sim C23-C26A \\sim
C23-C26B
 with sigma of 0.02
 C24A-C25A \\sim C24A-C26A \\sim C25A-C26A \\sim C24B-C25B \\sim C24B-C26B
\\sim C25B-C26B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24A \\sim C24B \\sim C25A \\sim C25B \\sim C26A \\sim C26B: within 1.25A with
sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C24A) \\sim Ueq, Uanis(C24B) \\sim Ueq, Uanis(C25A) \\sim Ueq,
Uanis(C25B) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C26B) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.01
4. Same fragment restrains
{F11, F12, F13, F14, B1}
as
{F21, F22, F23, F24, B2}
5. Others
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
6.a Me refined with riding coordinates:
 C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C26A(H26A,H26B,H26C), C24B(H24D,
 H24E,H24F), C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F)
6.b 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), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              38497
_shelx_fab_checksum              72001