Computational, ^1^H NMR, and X-ray structural studies on 1-arylurazole tetrazane dimers
Martin, Kenneth L.; Breton, Gary W.; Acta Crystallographica Section C 73 (2017) –; doi:10.1107/S2053229617010786

data_2020843
_publ_section_title
;
 Computational, ^1^H NMR, and X-ray structural studies on 1-arylurazole
 tetrazane dimers
;
_journal_coeditor_code           FN3238
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229617010786
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C24 H28 N6 O4'
_chemical_formula_moiety         'C24 H28 N6 O4'
_chemical_formula_sum            'C24 H28 N6 O4'
_chemical_formula_weight         464.52
_chemical_melting_point          433
_chemical_name_common            'A646 (Breton2016)'
_chemical_name_systematic
4-Methyl-1-[4-methyl-3,5-dioxo-2-(2,4,6-trimethylphenyl)-1,2,4-triazolidin-1-yl]-2-(2,4,6-trimethylphenyl)-1,2,4-triazolidine-3,5-dione
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1077(7)
_cell_length_b                   13.5893(11)
_cell_length_c                   19.4760(16)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6804
_cell_measurement_theta_min      2.5732
_cell_volume                     2410.5(3)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
ShelXle (H\"ubschle <i>et al.</i>,  2011)
;
_computing_publication_material
;
ShelXle (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20363
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.680
_diffrn_reflns_theta_min         2.573
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.842
_exptl_crystal_size_mid          0.503
_exptl_crystal_size_min          0.341
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3721
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.8555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                3323
_reflns_number_total             3721
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           I
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_shelx_res_checksum              27869
_cod_database_fobs_code 2020843