Endogenous Alkaloids in Man. 28. (1<i>R</i>,3<i>S</i>)-1-Trichloromethyl-1,2,3,4-tetrahydro-β-carboline-3-carboxamide Methanol Solvate, a Potential Synthetic Precursor to Enantiomerically Pure TaClo
Peters, Karl; Peters, Eva-Maria; Blank, Michael; Protzen, Jens-Achim; Feineis, Doris; God, Ralf; Bringmann, Gerhard; Acta Crystallographica Section C 54 (1998) 1005–1007; doi:10.1107/S0108270198001437

data_2007441
_publ_section_title
;Endogenous Alkaloids in Man. 28.
 (1<i>R</i>,3<i>S</i>)-1-Trichloromethyl-1,2,3,4-tetrahydro-\b-carboline-3-carboxamide
 Methanol Solvate, a Potential Synthetic Precursor to Enantiomerically Pure
 TaClo
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1005
_journal_page_last               1007
_journal_paper_doi               10.1107/S0108270198001437
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C13 H12 Cl3 N3 O , C H4 O'
_chemical_formula_sum            'C14 H16 Cl3 N3 O2'
_chemical_formula_weight         364.65
_chemical_name_systematic
;(1R,3S)-1-Trichloromethyl-1,2,3,4-tetrahydro-\b-carboline-3-carboxamide
 methanol solvate
;
_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_type_scat_source           'SHELXTL-Plus (Sheldrick, 1990)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7523(6)
_cell_length_b                   11.0208(7)
_cell_length_c                   14.0493(9)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      21.1
_cell_volume                     1664.83(18)
_computing_cell_refinement       P4
_computing_data_collection       'P4 (Siemens, 1996a)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    SHELXTL-Plus
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7726
_diffrn_reflns_theta_max         32.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.56
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   '\y scan (XEMP in XSCANS; Siemens, 1996b)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.67
_refine_ls_abs_structure_Flack   '0.06(5) (Flack, 1983)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment
'H atoms refined by a mixture of independent and constrained refinement'
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5633
_refine_ls_R_factor_gt           0.045
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' w = 1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.115
_reflns_number_gt                5592
_reflns_number_total             6018
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            jz1190.cif
_cod_data_source_block           jz1190
_cod_original_cell_volume        1664.8(2)
_cod_database_code               2007441