3':5'-Cyclic nucleotides: two sodium salts of cdTMP
Ślepokura, Katarzyna Anna; Acta Crystallographica Section C 72 (2016) 35–47; doi:10.1107/S2053229615022536

data_2020318
_publ_section_title
;
 3':5'-Cyclic nucleotides: two sodium salts of cdTMP
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              35
_journal_page_last               47
_journal_paper_doi               10.1107/S2053229615022536
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'Na + , C10 H12 N2 O7 P - , 3.7H2 O'
_chemical_formula_moiety         'Na +, C10 H12 N2 O7 P -, 3.7(H2 O)'
_chemical_formula_sum            'C10 H19.4 N2 Na O10.7 P'
_chemical_formula_weight         392.83
_chemical_name_common
;
Thymidine 3':5'-cyclic phosphate sodium salt 3.7-hydrate
;
_chemical_name_systematic
;
Sodium thymidine 3':5'-cyclic phosphate 3.7-hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL2013
_cell_angle_alpha                90
_cell_angle_beta                 112.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   32.936(8)
_cell_length_b                   19.718(4)
_cell_length_c                   21.569(5)
_cell_measurement_reflns_used    18866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.76
_cell_volume                     12971(6)
_computing_cell_refinement
;
(CrysAlis RED; Oxford Diffraction, 2010)
;
_computing_data_collection
;
(CrysAlis CCD; Oxford Diffraction, 2010)
;
_computing_data_reduction
;
(CrysAlis RED; Oxford Diffraction, 2010)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Oxford Xcalibur PX \k-geometry diffractometer with Onyx CCD camera
;
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            82355
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.054
_diffrn_reflns_theta_min         2.829
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       plate
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.442
_refine_ls_abs_structure_details
;
Flack <i>x</i> parameter determined using 4968 quotients
[(I^+^) - (I^-^)]/[(I^+^) + (I^-^)] (Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1954
_refine_ls_number_reflns         25620
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                13487
_reflns_number_total             25620
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3608sup1.cif
_cod_data_source_block           II_tmpna1
_cod_depositor_comments
;Adding full bibliography for 2020317--2020318.cif.

 Adding full bibliography for 2020317--2020318.cif.
;
_cod_original_formula_sum        'C10 H19.40 N2 Na O10.70 P'
_cod_database_code               2020318
_cod_database_fobs_code          2020318
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              85271
_shelx_res_checksum              48350
_shelxl_version_number           .2013