Stereoselective preparation of (RP)-8-hetaryladenosine-3',5'-cyclic phosphorothioic acids.
Andrei, Mioara; Bjørnstad, Vidar; Langli, Geir; Rømming, Christian; Klaveness, Jo; Taskén, Kjetil; Undheim, Kjell; Organic & biomolecular chemistry 5 (2007) 2070–2080; doi:10.1039/b702403g

data_7151107
_publ_section_title
;
 Stereoselective preparation of (RP)-8-hetaryladenosine-3',5'-cyclic
 phosphorothioic acids.
;
_journal_issue                   13
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2070
_journal_page_last               2080
_journal_paper_doi               10.1039/b702403g
_journal_volume                  5
_journal_year                    2007
_chemical_formula_sum            'C27 H35 N6 O6 P Si'
_chemical_formula_weight         598.67
_chemical_name_common
;
(Sp)-8-(2-Furyrl)adenosine-2'-O-(tert-butylmethylsilyl)-3',5'-
cyclic N-benzylphosphoramidate
;
_chemical_name_systematic
;
(Sp)-8-(2-Furyrl)adenosine-2'-O-(tert-butylmethylsilyl)-3',5'-cyclic N-
benzylphosphoramidate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8533(5)
_cell_length_b                   13.3879(6)
_cell_length_c                   20.9242(9)
_cell_measurement_temperature    120(2)
_cell_volume                     3040.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            57613
_diffrn_reflns_theta_full        36.32
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         14434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.0869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                12632
_reflns_number_total             14434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702403g.txt
_cod_data_source_block           8a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7151107