Quasi-enantiomeric single-nucleoside and quasi-racemic two-nucleoside hydrochloride salts and ruthenium complexes of cytidine and 2′,3′-dideoxycytidine analogs unveiling the negligible structure-driving role of the 2′,3′-moieties
Martins, Felipe Terra; Corrêa, Rodrigo S.; Batista, Alzir Azevedo; Ellena, Javier; CrystEngComm 16 (2014) 7013–; doi:10.1039/C4CE00678J

data_7217338
_publ_section_title
;
 Quasi-enantiomeric single-nucleoside and quasi-racemic two-nucleoside
 hydrochloride salts and ruthenium complexes of cytidine and
 2&#x2032;,3&#x2032;-dideoxycytidine analogs unveiling the negligible
 structure-driving role of the 2&#x2032;,3&#x2032;-moieties
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              7013
_journal_paper_doi               10.1039/C4CE00678J
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C55 H56 Cl1 N5 O9 P2 Ru1'
_chemical_formula_sum            'C114.5 H115 Cl2 N10 O21 P4 Ru2'
_chemical_formula_weight         2364.08
_chemical_name_common            ctd_cwbpy
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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_date             2013-11-26T03:23:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.20(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.432(1)
_cell_length_b                   20.600(3)
_cell_length_c                   27.012(5)
_cell_measurement_reflns_used    23923
_cell_measurement_temperature    293(2)
_cell_measurement_wavelength     0.71073
_cell_volume                     5745.5(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.2503E-2
_diffrn_orient_matrix_UB_12      0.448477E-1
_diffrn_orient_matrix_UB_13      -0.142754E-1
_diffrn_orient_matrix_UB_21      0.966286E-1
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      0.2822E-2
_diffrn_orient_matrix_UB_31      -0.60415E-2
_diffrn_orient_matrix_UB_32      -0.185807E-1
_diffrn_orient_matrix_UB_33      -0.344562E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44046
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
   P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         22785
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.108
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                15972
_reflns_number_total             22785
_reflns_threshold_expression     >2\s(I)
_cod_duplicate_entry             7215884
_cod_data_source_file            c4ce00678j2.cif
_cod_data_source_block           ctd_cwbipy
_cod_original_cell_volume        5745.5(1)
_cod_original_sg_symbol_H-M      P21
_cod_original_formula_sum        'C114.50 H115 Cl2 N10 O21 P4 Ru2'
_cod_database_code               7217338