N-H and N-C Bond Activation of Pyrimidinic Nucleobases and Nucleosides Promoted by an Osmium Polyhydride
Miguel A. Esteruelas; Jorge García-Raboso; Montserrat Oliván; Enrique Oñate; Inorganic Chemistry 51 (2012) 5975–5984; doi:10.1021/ic300639j

data_4329306
_publ_contact_author
;
  Dr. Montserrat Oliv\'an
  Departamento de Qu\'imica Inorg\'anica - ISQCH
  Universidad de Zaragoza - CSIC
  50009 Zaragoza, Spain
;
_publ_contact_author_email       molivan@unizar.es
_publ_section_title
;
 N-H and N-C Bond Activation of Pyrimidinic Nucleobases and Nucleosides
 Promoted by an Osmium Polyhydride
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5975
_journal_page_last               5984
_journal_paper_doi               10.1021/ic300639j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C41 H94 N2 O2 Os2 P4'
_chemical_formula_weight         1151.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.2180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6768(7)
_cell_length_b                   16.0063(7)
_cell_length_c                   21.5187(10)
_cell_measurement_reflns_used    9598
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     4989.9(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 0.997
_diffrn_measured_fraction_theta_max 0.937
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59788
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    5.249
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_correction_T_min  0.445
_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            colorless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       prism
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         12026
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                9745
_reflns_number_total             12026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300639j_si_001_2.cif
_cod_data_source_block           montse13s
_cod_database_code               4329306