Selective 15N-Labeling and Analysis of 13C-15N J Couplings as an Effective Tool for Studying the Structure and Azide-Tetrazole Equilibrium in a Series of Tetrazolo[1,5-b][1,2,4]triazines and Tetrazolo[1,5-a]pyrimidines
Sergey L. Deev; Zakhar O. Shenkarev; Tatyana S. Shestakova; Oleg N. Chupakhin; Vladimir L. Rusinov; Alexander S. Arseniev; Journal of Organic Chemistry 75 (2010) 8487–8497; doi:10.1021/jo1017876

data_4025878
_publ_section_title
;
 Selective 15N-Labeling and Analysis of 13C-15N J Couplings as an
 Effective Tool for Studying the Structure and Azide-Tetrazole Equilibrium
 in a Series of Tetrazolo[1,5-b][1,2,4]triazines and
 Tetrazolo[1,5-a]pyrimidines
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8487
_journal_page_last               8497
_journal_paper_doi               10.1021/jo1017876
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C4 H3 N5'
_chemical_formula_sum            'C4 H3 N5'
_chemical_formula_weight         121.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.457(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0702(4)
_cell_length_b                   5.6183(2)
_cell_length_c                   13.1708(8)
_cell_measurement_temperature    295(2)
_cell_volume                     516.07(5)
_computing_cell_refinement       'CrysAlis CCD 171.28c4'
_computing_data_collection       'CrysAlis CCD 171.28c4'
_computing_data_reduction        'CrysAlis RED 171.28c4'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Xcalibur 3 CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6446
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         31.63
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             248
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.113(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                1251
_reflns_number_total             1562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1017876_si_002.cif
_cod_data_source_block           dc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4025878