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_2020502
_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, 2H2 O'
_chemical_formula_moiety         'C10 H12 N5 O6 P, 2(H2 O)'
_chemical_formula_sum            'C10 H16 N5 O8 P'
_chemical_formula_weight         365.25
_chemical_name_common
;
Adenosine 3':5'-cyclic phosphate dihydrate
;
_chemical_name_systematic
;
Adenosine 3':5'-cyclic phosphate dihydrate
;
_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                   7.715(2)
_cell_length_b                   10.598(3)
_cell_length_c                   35.481(9)
_cell_measurement_reflns_used    7087
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.77
_cell_measurement_theta_min      2.87
_cell_volume                     2901.1(13)
_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      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Kuma KM-4 CCD \k-geometry diffractometer with a Sapphire2
CCD camera
;
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            27238
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         2.879
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.328
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1672 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6322
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0363P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                4907
_reflns_number_total             6322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3622sup1.cif
_cod_data_source_block           I_camp
_cod_database_code               2020502
_cod_database_fobs_code          2020502
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.998
_shelx_hkl_checksum              43823
_shelx_res_checksum              33037