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_4085841
_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            'C31 H53 N Os P2 S'
_chemical_formula_weight         723.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.0250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1952(6)
_cell_length_b                   16.2072(10)
_cell_length_c                   19.8843(12)
_cell_measurement_reflns_used    6679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3187.7(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.918
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28888
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.186
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.628
_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            red
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.951
_refine_diff_density_min         -1.713
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+6.4029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                6099
_reflns_number_total             7538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00174_si_001.cif
_cod_data_source_block           enrique137
_cod_depositor_comments
'Adding full bibliography for 4085838--4085841.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4085841