Reactions of an Osmium-Hexahydride Complex with Cytosine, Deoxycytidine, and Cytidine: The Importance of the Minor Tautomers
Miguel A. Esteruelas; Jorge García-Raboso; Montserrat Oliván; Inorganic Chemistry 51 (2012) 9522–9528; doi:10.1021/ic3013238

data_4330272
_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
;
 Reactions of an Osmium-Hexahydride Complex with Cytosine, Deoxycytidine,
 and Cytidine: The Importance of the Minor Tautomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9522
_journal_page_last               9528
_journal_paper_doi               10.1021/ic3013238
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C46.5 H104 N6 O2 Os2 P4'
_chemical_formula_weight         1283.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.0220(10)
_cell_angle_beta                 98.4770(10)
_cell_angle_gamma                111.0880(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9800(11)
_cell_length_b                   16.5360(15)
_cell_length_c                   16.9391(16)
_cell_measurement_reflns_used    3483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     3076.3(5)
_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 0.979
_diffrn_measured_fraction_theta_max 0.907
_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  0.0827
_diffrn_reflns_av_sigmaI/netI    0.1806
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37406
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.61
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.266
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.717
_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    1.386
_exptl_crystal_description       prism
_exptl_crystal_F_000             1306
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.744
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         14297
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.825
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                7102
_reflns_number_total             14297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3013238_si_001_1.cif
_cod_data_source_block           montse15
_cod_original_formula_sum        'C46.50 H104 N6 O2 Os2 P4'
_cod_database_code               4330272