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_2015424
_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 O6 P -'
_chemical_formula_moiety         'C6 H16 N +, C10 H11 N5 O6 P -'
_chemical_formula_sum            'C16 H27 N6 O6 P'
_chemical_formula_weight         430.41
_chemical_name_common
;
triethylammonium adenosine cyclic 2',3'-phosphate
;
_chemical_name_systematic
;
Triethylammonium
4-(6-aminopurin-7-yl)-6-hydroxymethyl-2-oxido-2-
oxoperhydrofurano[3,4-c][1,3,2]dioxaphosphole
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.704(2)
_cell_length_b                   10.493(3)
_cell_length_c                   28.536(7)
_cell_measurement_reflns_used    11796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.80
_cell_measurement_theta_min      4.49
_cell_volume                     2007.4(10)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type
'Xcalibur PX \k-geometry diffractometer with Onyx CCD camera'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            14174
_diffrn_reflns_theta_full        75.80
_diffrn_reflns_theta_max         75.80
_diffrn_reflns_theta_min         4.49
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.43
_refine_ls_abs_structure_details
;
(Flack, 1983), 1481 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0714P)^2^+0.7467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                3559
_reflns_number_total             3911
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3019.cif
_cod_data_source_block           I
_cod_database_code               2015424
_cod_database_fobs_code          2015424