In Situ Solvothermal Generation of 1,2,4-Triazolates and Related Compounds from Organonitrile and Hydrazine Hydrate: A Mechanism Study
Lin Cheng; Wei-Xiong Zhang; Bao-Hui Ye; Jian-Bin Lin; Xiao-Ming Chen; Inorganic Chemistry 46 (2007) 1135–1143; doi:10.1021/ic061303i

data_4306949
_publ_section_title
;
In Situ Solvothermal Generation of 1,2,4-Triazolates and Related Compounds
from Organonitrile and Hydrazine Hydrate: A Mechanism Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1135
_journal_page_last               1143
_journal_paper_doi               10.1021/ic061303i
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C26 H20 Mn2 N12 O2 S2'
_chemical_formula_weight         706.54
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.841(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.612(3)
_cell_length_b                   7.5526(9)
_cell_length_c                   15.0059(17)
_cell_measurement_temperature    293(2)
_cell_volume                     2978.9(6)
_computing_cell_refinement
;
     'SAINT-PLUS for Windows NT, Ver. 6.0, Bruker AXS Inc., 1997.'
;
_computing_data_collection
;
          'SMART for Windows NT, Bruker AXS Inc., 1998.' 
;
_computing_molecular_graphics
;
     'XP-Interactive Molecular Graphics, Ver. 6.10, Bruker AXS Inc., 2000.'
;
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APX CCD'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8152
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.9035
_exptl_absorpt_correction_T_min  0.8118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+1.2640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                2507
_reflns_number_total             3144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061303isi20060714_094810_4.cif
_cod_data_source_block           3
_cod_database_code               4306949