Purine 3':5'-cyclic nucleotides with the nucleobase in a <i>syn</i> orientation: cAMP, cGMP and cIMP
Ślepokura, Katarzyna Anna; Acta Crystallographica Section C 72 (2016) –; doi:10.1107/S2053229616006999

data_2020503
_publ_section_title
;
 Purine 3':5'-cyclic nucleotides with the nucleobase in a <i>syn</i>
 orientation: cAMP, cGMP and cIMP
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229616006999
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C10 H12 N5 O6 P, 0.3H2 O'
_chemical_formula_moiety         'C10 H12 N5 O6 P, 0.3(H2 O)'
_chemical_formula_sum            'C10 H12.6 N5 O6.3 P'
_chemical_formula_weight         334.62
_chemical_name_common
;
Adenosine 3':5'-cyclic phosphate 0.3-hydrate
;
_chemical_name_systematic
;
Adenosine 3':5'-cyclic phosphate 0.3-hydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.786(2)
_cell_length_b                   10.638(3)
_cell_length_c                   29.887(8)
_cell_measurement_reflns_used    5879
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.56
_cell_measurement_theta_min      4.15
_cell_volume                     2475.5(12)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1956
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur PX \k-geometry diffractometer
with an Onyx CCD camera
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            22972
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         67.985
_diffrn_reflns_theta_min         4.412
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012), based on expressions
derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.446
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1568 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.020(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0922P)^2^+0.9260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                4090
_reflns_number_total             4505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3622sup1.cif
_cod_data_source_block           II_camp1ab
_cod_original_formula_sum        'C10 H12.60 N5 O6.30 P'
_cod_database_code               2020503
_shelx_estimated_absorpt_t_min   0.654
_shelx_estimated_absorpt_t_max   0.953
_shelx_hkl_checksum              72751
_shelx_res_checksum              7299
_cod_database_fobs_code 2020503