Constrained Nucleic Acids (CNA). Part 2. Synthesis of Conformationally Restricted Dinucleotide Units Featuring Noncanonical α/β/γ or δ/ε/ζ Torsion Angle Combinations
Le Clézio, Ingrid; Gornitzka, Heinz; Escudier, Jean-Marc; Vigroux, Alain; The Journal of Organic Chemistry 70 (2005) 1620–1629; doi:10.1021/jo048136t

data_4028889
_publ_section_title
;
 Constrained Nucleic Acids (CNA). Part 2. Synthesis of Conformationally
 Restricted Dinucleotide Units Featuring Noncanonical \a/\b/\g or \d/\e/\z
 Torsion Angle Combinations
;
_journal_issue                   5
_journal_name_full               'The Journal of Organic Chemistry'
_journal_page_first              1620
_journal_page_last               1629
_journal_paper_doi               10.1021/jo048136t
_journal_volume                  70
_journal_year                    2005
_chemical_formula_sum            'C39 H47.25 Cl5.75 N4 O12 P Si'
_chemical_formula_weight         1026.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.397(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6695(8)
_cell_length_b                   18.7483(14)
_cell_length_c                   23.9407(18)
_cell_measurement_reflns_used    4527
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.096
_cell_measurement_theta_min      2.214
_cell_volume                     4737.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.1100
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21327
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         5.16
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.598524
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1590
_refine_ls_number_reflns         13121
_refine_ls_number_restraints     1399
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                8732
_reflns_number_total             13121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo048136tsup1.cif
_cod_data_source_block           15b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4028889