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_4306950
_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            'C56 H54 Mn4 N34 O2'
_chemical_formula_weight         1455.09
_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                 131.062(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4385(11)
_cell_length_b                   16.8446(15)
_cell_length_c                   18.7956(13)
_cell_measurement_temperature    293(2)
_cell_volume                     2969.3(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15889
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1487
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0998P)^2^+4.7630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.1842
_reflns_number_gt                4672
_reflns_number_total             5830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061303isi20060714_094810_5.cif
_cod_data_source_block           5
_cod_original_cell_volume        2969.3(4)
_cod_database_code               4306950