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_4329305
_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_absolute_configuration rm
_chemical_formula_sum            'C27 H56 N2 O5 Os P2'
_chemical_formula_weight         740.88
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_c                   17.632(2)
_cell_measurement_reflns_used    9028
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_cell_measurement_theta_min      2
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_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 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_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
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_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.53
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_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.100
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_exptl_absorpt_correction_type   multi-scan
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;
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
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_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.15
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_refine_diff_density_max         1.080
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         8389
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0200
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                8048
_reflns_number_total             8389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300639j_si_001_1.cif
_cod_data_source_block           enriquen17
_cod_original_cell_volume        3216.3(8)
_cod_database_code               4329305