Single crystal X-ray structure of virescenine hydrochloride

Authorship and data citation: Phurpa Wangchuk, John B. Bremner, Bryan W. Skelton. CCDC 1574634: Experimental Crystal Structure Determination, 2017,  DOI: 10.5517/ccdc.csd.cc1pvjnqMethod: Virescenine hydrochloride was isolated from a Bhutanese medicinal plant, Aconitum orochryseum. Needle-like colourless crystals were obtained from acetone/diethyl ether. This compound had a melting point of  76.7-79.8oC and  an optical rotation of  [α]D24 = +16.9o (c 1.095, EtOH). Its single crystal X-ray crystallographic structure was presented here for the first time. X-ray diffraction images were measured on a Nonius KappaCCD diffractometer (Mo Kα radiation, graphite monochromator, λ=0.71073 Å) and data extracted using the DENZO package (Otwinowski and Minor, 1997). Structure solution was by direct methods (SUPERFLIP, SIR92) (Altomare et al., 1994, Palatinus and Chapuis, 2007). The structure was refined using the CRYSTALS program package (Betteridge et al., 2003). Atomic coordinates, bond lengths and angles and displacement parameters have been deposited at the Cambridge Crystallographic Data Centre (CCDC).Crystal data: The crystal structure of virescenine hydrochloride has been assigned CCDC no. 1574634  (DOI: 10.5517/ccdc.csd.cc1pvjnq). Molecular formula: C23H38ClNO6. Chemical formula weight = 459. UNIT CELL INFORMATION                                    ---------------------------------------------------------------------------symmetry_cell_setting                              triclinicsymmetry_space_group_name_H-M     'P 1'symmetry_space_group_name_Hall      'P 1'symmetry_Int_Tables_number                1loop_symmetry_equiv_pos_as_              xyzcell_length_a                                               8.6730(10)cell_length_b                                               8.7250(10)cell_length_c                                                8.8670(10)cell_angle_alpha                                         61.467(5)cell_angle_beta                                           73.372(6)cell_angle_gamma                                      79.072(6)cell_volume                                                  563.72(12)cell_formula_units_Z                                  1cell_measurement_temperature              101(2)cell_measurement_reflns_used                2132cell_measurement_theta_min                  2.32cell_measurement_theta_max                 18.06---------------------------------------------------------------------------                   CRYSTAL INFORMATION                                      --------------------------------------------------------------------------exptl_crystal_description            prismexptl_crystal_colour                   colourlessexptl_crystal_size_max                0.12exptl_crystal_size_mid                 0.1exptl_crystal_size_min                 0.08exptl_crystal_density_diffrn        1.355exptl_crystal_F_000                     248 ----------------------------------------------------------------------------                   ABSORPTION CORRECTION                                    ----------------------------------------------------------------------------exptl_absorpt_coefficient_mu           0.116exptl_absorpt_correction_type         multi-scanexptl_absorpt_process_details          SADABS; Sheldrick, 1996exptl_transmission_factor_max          1.00exptl_transmission_factor_min          0.817---------------------------------------------------------------------------                  DATA COLLECTION                                          ---------------------------------------------------------------------------diffrn_ambient_temperature             101(2)diffrn_radiation_type                           'synchrotron'diffrn_radiation_wavelength               0.48595diffrn_measurement_device_type;   Bruker SMART CCDdiffrn_measurement_method             '\f and \w scans'diffrn_reflns_av_R_equivalents         0.0338diffrn_reflns_av_unetI/netI                0.0604diffrn_reflns_number                         10439diffrn_reflns_limit_h_min               -13diffrn_reflns_limit_h_max               13diffrn_reflns_limit_k_min                -13diffrn_reflns_limit_k_max                13diffrn_reflns_limit_l_min                 -12diffrn_reflns_limit_l_max                 13diffrn_reflns_theta_min                   1.679diffrn_reflns_theta_max                  22.622diffrn_reflns_theta_full                  16.952diffrn_measured_fraction_theta_full                          0.999diffrn_measured_fraction_theta_max                         0.817diffrn_reflns_Laue_measured_fraction_full                0.999diffrn_reflns_Laue_measured_fraction_max              0.817diffrn_reflns_point_group_measured_fraction_full   0.92_diffrn_reflns_point_group_measured_fraction_max 0.681_reflns_Friedel_fraction_full           0.841_reflns_Friedel_fraction_max            0.545_reflns_Friedel_coverage                0.667_reflns_number_total                    6392_reflns_number_gt                       5763_reflns_threshold_expression            'I > 2\s(I)' ---------------------------------------------------------------------------                   COMPUTER PROGRAMS USED                                   ----------------------------------------------------------------------------computing_data_collection             'Siemens SMART (Siemens, 1995)'computing_cell_refinement             'Siemens SAINT (Siemens, 1995)' computing_structure_refinement         'SHELXL-2014/7 (Sheldrick, 2014)'computing_structure_solution           'Sir92 (Altomare, A.,et. al. 1994)'computing_publication_material        'WinGX Farrugia, L. J. (1999)'