Single crystal X-ray structure of virescenine hydrochloride

Full description

Authorship and data citation: Phurpa Wangchuk, John B. Bremner, Bryan W. Skelton. CCDC 1574634: Experimental Crystal Structure Determination, 2017,  DOI: 10.5517/ccdc.csd.cc1pvjnq

Method: 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  76.7-79.8^oC and  an optical rotation of  [α]_D²⁴ = +16.9^o (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                                    

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symmetry_cell_setting                              triclinic

symmetry_space_group_name_H-M     'P 1'

symmetry_space_group_name_Hall      'P 1'

symmetry_Int_Tables_number                1

loop_symmetry_equiv_pos_as_              xyz

cell_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                                  1

cell_measurement_temperature              101(2)

cell_measurement_reflns_used                2132

cell_measurement_theta_min                  2.32

cell_measurement_theta_max                 18.06

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                   CRYSTAL INFORMATION                                      

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exptl_crystal_description            prism

exptl_crystal_colour                   colourless

exptl_crystal_size_max                0.12

exptl_crystal_size_mid                 0.1

exptl_crystal_size_min                 0.08

exptl_crystal_density_diffrn        1.355

exptl_crystal_F_000                     248

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                   ABSORPTION CORRECTION                                    

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exptl_absorpt_coefficient_mu           0.116

exptl_absorpt_correction_type         multi-scan

exptl_absorpt_process_details          SADABS; Sheldrick, 1996

exptl_transmission_factor_max          1.00

exptl_transmission_factor_min          0.817

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                  DATA COLLECTION                                          

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diffrn_ambient_temperature             101(2)

diffrn_radiation_type                           'synchrotron'

diffrn_radiation_wavelength               0.48595

diffrn_measurement_device_type;   Bruker SMART CCD

diffrn_measurement_method             '\f and \w scans'

diffrn_reflns_av_R_equivalents         0.0338

diffrn_reflns_av_unetI/netI                0.0604

diffrn_reflns_number                         10439

diffrn_reflns_limit_h_min               -13

diffrn_reflns_limit_h_max               13

diffrn_reflns_limit_k_min                -13

diffrn_reflns_limit_k_max                13

diffrn_reflns_limit_l_min                 -12

diffrn_reflns_limit_l_max                 13

diffrn_reflns_theta_min                   1.679

diffrn_reflns_theta_max                  22.622

diffrn_reflns_theta_full                  16.952

diffrn_measured_fraction_theta_full                          0.999

diffrn_measured_fraction_theta_max                         0.817

diffrn_reflns_Laue_measured_fraction_full                0.999

diffrn_reflns_Laue_measured_fraction_max              0.817

diffrn_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)'

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                   COMPUTER PROGRAMS USED                                   

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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)'