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 76.7-79.8oC 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
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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)'