Synthesis and crystal structures of three new benzotriazolylpropanamides
Amenta, Donna S.; Liebing, Phil; Biero, Julia E.; Sherman, Robert J.; Gilje, John W.; Edelmann, Frank T.; Acta Crystallographica Section E 73 (2017) 880–885; doi:10.1107/S2056989017007472

data_2242159
_publ_section_title
;
 Synthesis and crystal structures of three new benzotriazolylpropanamides
;
_journal_coeditor_code           ZL2702
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              880
_journal_page_last               885
_journal_paper_doi               10.1107/S2056989017007472
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C10 H12 N4 O'
_chemical_formula_moiety         'C10 H12 N4 O'
_chemical_formula_sum            'C10 H12 N4 O'
_chemical_formula_weight         204.24
_chemical_name_systematic
;
3-(1<i>H</i>-Benzotriazol-1-yl)-2-methylpropanamide
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                69.039(12)
_cell_angle_beta                 89.498(10)
_cell_angle_gamma                75.915(10)
_cell_formula_units_Z            2
_cell_length_a                   7.3885(9)
_cell_length_b                   8.0720(10)
_cell_length_c                   9.2976(13)
_cell_measurement_reflns_used    21215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.095
_cell_measurement_theta_min      5.096
_cell_volume                     500.37(12)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2003)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2003)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2003)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Agilent Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            28193
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.975
_diffrn_reflns_theta_min         5.113
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO, Agilent, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       prism
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.208
_refine_ls_extinction_coef       0.0117(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.1806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                2012
_reflns_number_total             2053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2702sup1.cif
_cod_data_source_block           1
_cod_database_code               2242159
_cod_database_fobs_code          2242159
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.942
_shelx_hkl_checksum              12932
_shelx_res_checksum              83517