The first 3':5'-cyclic nucleotide–amino acid complex: <small>L</small>-His–cIMP
Ślepokura, Katarzyna; Acta Crystallographica Section C 68 (2012) o311–o316; doi:10.1107/S0108270112030041

data_2018582
_publ_section_title
;
 The first 3':5'-cyclic nucleotide--amino acid complex:
 <small>L</small>-His--cIMP
;
_journal_coeditor_code           QS3016
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o311
_journal_page_last               o316
_journal_paper_doi               10.1107/S0108270112030041
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 H10 N3 O2 + , C10 H10 N4 O7 P -'
_chemical_formula_moiety         'C6 H10 N3 O2 +, C10 H10 N4 O7 P -'
_chemical_formula_sum            'C16 H20 N7 O9 P'
_chemical_formula_weight         485.36
_chemical_name_common
;
<i>L</i>-Histdinium inosine 3':5'-cyclic phosphate
;
_chemical_name_systematic
;
5-(2-amino-2-carboxyethyl)-1<i>H</i>-imidazol-3-ium
7-hydroxy-2-oxo-6-(6-oxo-6,9-dihydro-1<i>H</i>-purin-9-yl)-4a,6,7,7a-tetrahydro-
4<i>H</i>-1,3,5,2\l^5^-furo[3,2-<i>d</i>][1,3,2\l^5^]dioxaphosphinin-2-olate
;
_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   difmap
_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                   5.709(2)
_cell_length_b                   10.284(3)
_cell_length_c                   32.795(9)
_cell_measurement_reflns_used    14525
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      38.50
_cell_measurement_theta_min      2.71
_cell_volume                     1925.4(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type
;
Oxford Xcalibur PX \k-geometry diffractometer with an Onyx CCD camera
;
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            17935
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.273
_refine_ls_abs_structure_details
;
from known absolute configuration and anomalous dispersion effects
(Flack, 1983), with 1877 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.20(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.2437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                4778
_reflns_number_total             5114
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qs3016.cif
_cod_data_source_block           I
_cod_database_code               2018582
_cod_database_fobs_code          2018582