N-Acyl-1,2,3-triazoles – key intermediates in denitrogenative transformations
Motornov, Vladimir; Pohl, Radek; Klepetarova, Blanka; Beier, Petr; Chemical Communications  (2023) –; doi:10.1039/D3CC00987D

data_7131790
_publ_section_title
;
 N-Acyl-1,2,3-triazoles -- key intermediates in denitrogenative
 transformations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC00987D
_journal_year                    2023
_chemical_formula_moiety         'C11 H11 N3 O'
_chemical_formula_sum            'C11 H11 N3 O'
_chemical_formula_weight         201.23
_chemical_name_systematic
' 1-(4-(p-tolyl)-2H-1,2,3-triazol-2-yl)ethan-1-one'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2023-02-27 deposited with the CCDC.	2023-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.9689(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7087(2)
_cell_length_b                   11.2855(2)
_cell_length_c                   12.0893(2)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    180
_cell_measurement_theta_max      70.0476
_cell_measurement_theta_min      3.9170
_cell_volume                     1024.90(4)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19496
_diffrn_reflns_theta_full        68.224
_diffrn_reflns_theta_max         68.224
_diffrn_reflns_theta_min         5.428
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.14
_refine_ls_extinction_coef       24(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0701
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1807
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.0003834
_refine_ls_shift/su_mean         0.0000595
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.174 0.140 0.453E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0429
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0404
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1807
_reflns_number_total             1876
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.28
_oxford_diffrn_Wilson_scale      14.58
_oxford_refine_ls_r_factor_ref   0.0379
_oxford_refine_ls_scale          0.2859(7)
_oxford_reflns_number_all        1876
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            d3cc00987d2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7131790