Azole Assisted C‒H Bond Activation Promoted by an Osmium-Polyhydride: Discerning between N and NH
Eguillor, Beatriz; Esteruelas, Miguel A.; Fernández, Israel; Gómez-Gallego, Mar; Lledós, Agustí; Martín-Ortiz, Mamen; Oliván, Montserrat; Oñate, Enrique; Sierra, Miguel A.; Organometallics 34 (2015) 1898–; doi:10.1021/acs.organomet.5b00174

data_4085838
_publ_section_title
;
 Azole Assisted C--H Bond Activation Promoted by an Osmium-Polyhydride:
 Discerning between N and NH
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1898
_journal_paper_doi               10.1021/acs.organomet.5b00174
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C27 H52 N2 Os P2'
_chemical_formula_weight         656.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.5141(7)
_cell_length_b                   14.3683(6)
_cell_length_c                   23.0704(9)
_cell_measurement_reflns_used    17880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     5805.6(4)
_computing_cell_refinement       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_collection       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_reduction
;
  SAINT-Bruker integration program embedded in APEX2 v2008.4-0, Bruker AXS
;
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51574
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.520
_exptl_absorpt_correction_T_max  0.571
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7151
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0441
_reflns_number_gt                5555
_reflns_number_total             7151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00174_si_001.cif
_cod_data_source_block           montse25a
_cod_depositor_comments
'Adding full bibliography for 4085838--4085841.cif.'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4085838