Different nucleobase orientations in two cyclic 2',3'-phosphates of purine ribonucleosides: Et~3~NH(2',3'-cAMP) and Et~3~NH(2',3'-cGMP)·H~2~O
Krzysztof Sierosławski; Katarzyna Ślepokura; Tadeusz Lis; Małgorzata Bogucka; Joanna Lutomska; Adam Kraszewski; Acta Crystallographica Section C 62 (2006) o405–o409; doi:10.1107/S0108270106017811

data_2015425
_publ_section_title
;
 Different nucleobase orientations in two cyclic 2',3'-phosphates of
 purine ribonucleosides: Et~3~NH(2',3'-cAMP) and
 Et~3~NH(2',3'-cGMP)&#x00B7;H~2~O
;
_journal_coeditor_code           FG3019
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o405
_journal_page_last               o409
_journal_paper_doi               10.1107/S0108270106017811
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C6 H16 N +, C10 H11 N5 O7 P -, H2 O'
_chemical_formula_moiety         'C6 H16 N +, C10 H11 N5 O7 P -, H2 O'
_chemical_formula_sum            'C16 H29 N6 O8 P'
_chemical_formula_weight         464.42
_chemical_name_common
;
triethylammonium guanosine cyclic 2',3'-phosphate monohydrate
;
_chemical_name_systematic
;
triethylammonium
4-(6-oxo-1,6-dihydropurin-7-yl)-6-hydroxymethyl-2-oxido-2-
oxoperhydrofurano[3,4-c][1,3,2]dioxaphosphole monohydrate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.89(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.611(3)
_cell_length_b                   7.931(3)
_cell_length_c                   12.585(3)
_cell_measurement_reflns_used    9219
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      36.61
_cell_measurement_theta_min      3.04
_cell_volume                     1051.5(6)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type
'KUMA KM4 \k-geometry diffractometer with Saphire CCD camera'
_diffrn_measurement_method       \w
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21121
_diffrn_reflns_theta_full        34.99
_diffrn_reflns_theta_max         34.99
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details
;
(Flack, 1983), 2054 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6943
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                5239
_reflns_number_total             6943
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3019.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2015425
_cod_database_fobs_code          2015425