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_7217337
_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         'C60 H60 Cl1 N5 O4 P2 Ru1 S1'
_chemical_formula_sum            'C57 H56 Cl N5 O9 P2 Ru S'
_chemical_formula_weight         1185.59
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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_date             2013-11-26T02:37:28-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.800(5)
_cell_length_b                   16.008(5)
_cell_length_c                   34.268(5)
_cell_measurement_reflns_used    4522
_cell_measurement_temperature    293(2)
_cell_measurement_wavelength     0.71073
_cell_volume                     5376(3)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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      0.157217E-1
_diffrn_orient_matrix_UB_12      -0.44675E-2
_diffrn_orient_matrix_UB_13      -0.287622E-1
_diffrn_orient_matrix_UB_21      -0.100879
_diffrn_orient_matrix_UB_22      0
_diffrn_orient_matrix_UB_23      -0.45054E-2
_diffrn_orient_matrix_UB_31      0.11239E-2
_diffrn_orient_matrix_UB_32      0.624921E-1
_diffrn_orient_matrix_UB_33      -0.20562E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            5491
_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        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.737
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         5491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0801P)^2^+9.7908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1655
_reflns_number_gt                3946
_reflns_number_total             5491
_reflns_threshold_expression     >2\s(I)
_cod_duplicate_entry             7215883
_cod_data_source_file            c4ce00678j2.cif
_cod_data_source_block           cwbipylam
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7217337