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_4085839
_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_moiety         'C49 H98 N2 Os2 P4, C5 H12'
_chemical_formula_sum            'C54 H110 N2 Os2 P4'
_chemical_formula_weight         1291.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_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                 100.563(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.461(4)
_cell_length_b                   17.256(4)
_cell_length_c                   11.892(3)
_cell_measurement_reflns_used    5270
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     3119.0(13)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (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 0.999
_diffrn_measurement_device_type  'Bruker APEX DUO 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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13195
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.682
_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            green
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.348(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6324
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                5608
_reflns_number_total             6324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00174_si_001.cif
_cod_data_source_block           enriquen40cm
_cod_depositor_comments
'Adding full bibliography for 4085838--4085841.cif.'
_cod_original_cell_volume        3118.9(13)
_cod_original_sg_symbol_H-M      Cm
_cod_database_code               4085839